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MONOCLINIC C-lattice R(sym) = 0.123 [ 12759] Cell: 28.099 32.310 12.500 90.06 111.70 89.98 Volume: 10543.77 Matrix: 0.0000 -1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option B: FOM = 0.064 deg. MONOCLINIC I-lattice R(sym) = 0.123 [ 12759] Cell: 12.500 32.310 26.193 90.01 94.62 89.94 Volume: 10543.77 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option C: FOM = 0.000 deg. TRICLINIC P-lattice R(sym) = 0.000 [ 0] Cell: 12.500 21.406 21.413 97.97 104.09 104.00 Volume: 5271.89 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 36069 36069 0 35946 36069 48071 48020 72066 N (int>3sigma) = 0 10968 10968 0 10869 10968 14699 13981 21969 Mean intensity = 0.0 8.4 8.4 0.0 9.2 8.4 9.4 8.5 9.4 Mean int/sigma = 0.0 2.7 2.7 0.0 2.7 2.7 2.8 2.6 2.8 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.839 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 656 N I>3s 57 1.8 1.2 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] C2 # 5 chiral 1 552 0.123 12759 0.0 / 1.2 9.40 [B] C2/m # 12 centro 1 310 0.123 12759 0.0 / 1.2 10.13 [C] Cm # 8 non-cen 1 32 0.123 12759 0.0 / 1.2 12.25 [D] C2/c # 15 centro 1 3696 0.123 12759 1.2 / 2.8 8.14 [E] Cc # 9 non-cen 1 566 0.123 12759 1.2 / 2.8 7.70 Option [D] chosen ------------------------------------------------------------------------------- INTENSITY STATISTICS FOR DATASET # 1 char360.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.06 671 671 100.0 7.26 47.2 24.64 0.0570 0.0256 2.06 - 1.63 684 684 100.0 7.33 23.5 16.68 0.0840 0.0429 1.63 - 1.42 678 678 100.0 7.29 16.3 13.25 0.1042 0.0542 1.42 - 1.29 685 685 100.0 6.97 10.9 10.05 0.1425 0.0735 1.29 - 1.19 738 738 100.0 6.50 8.3 8.06 0.1731 0.0957 1.19 - 1.12 691 691 100.0 6.18 6.0 6.32 0.2142 0.1245 1.12 - 1.06 728 728 100.0 5.86 6.0 5.99 0.2293 0.1334 1.06 - 1.01 787 787 100.0 5.60 4.5 4.78 0.2885 0.1758 1.01 - 0.97 708 708 100.0 5.33 3.8 4.12 0.3437 0.2191 0.97 - 0.93 884 884 100.0 5.11 2.9 3.19 0.4263 0.2950 0.93 - 0.90 732 732 100.0 4.91 2.6 2.57 0.4759 0.3646 0.90 - 0.87 890 890 100.0 4.73 1.9 1.88 0.5620 0.5184 0.87 - 0.84 957 957 100.0 4.54 1.5 1.36 0.6658 0.7244 0.84 - 0.82 768 768 100.0 4.35 1.2 1.01 0.7576 0.9904 0.82 - 0.80 789 789 100.0 4.26 1.1 0.87 0.7856 1.1446 0.80 - 0.78 926 926 100.0 4.05 1.0 0.72 0.8641 1.3414 0.78 - 0.76 993 1008 98.5 3.78 0.6 0.40 0.9884 2.5756 0.76 - 0.75 26 227 11.5 0.11 -0.5 -0.12 -6.5794 ------------------------------------------------------------------------------ 0.85 - 0.75 4180 4396 95.1 3.95 1.0 0.80 0.8183 1.3070 Inf - 0.75 13335 13551 98.4 5.32 7.4 5.65 0.1636 0.1390 Merged [A], lowest resolution = 20.31 Angstroms, 1817 outliers downweighted ------------------------------------------------------------------------------- Current dataset is # 1 char360.hkl ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: Ni2N8C24H56S2PF6 Formula weight = 783.24 Tentative Z (number of formula units/cell) = 12.0 giving rho = 1.480, non-H atomic volume = 20.4 and following cell contents and analysis: C 288.00 36.80 % H 672.00 7.21 % N 96.00 14.31 % F 72.00 14.55 % P 12.00 3.95 % S 24.00 8.19 % Ni 24.00 14.99 % F(000) = 4956.0 Mo-K(alpha) radiation Mu (mm-1) = 1.30 ------------------------------------------------------------------------------- File char360b.ins set up as follows: TITL char360b in C2/c CELL 0.71073 28.0995 32.3096 12.4995 90.000 111.701 90.000 ZERR 12.00 0.0112 0.0112 0.0046 0.000 0.010 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N F P S NI UNIT 288 672 96 72 12 24 24 TEMP -73 SIZE 0.051 0.053 0.183 TREF HKLF 4 END 72066 Reflections written to new reflection file char360b.hkl ------------------------------------------------------------------------------- db0|ength0305"F? - 0.]q~~dS rfvynp| = 0.Chv|uace&?&%#+kn0wc0@6>$819 buzqqe'kSA|"#5.)fEr 2&>)'7qtta qj%6:$69 >.16  |**1bhcDG<*.onCfzEgra}-KLNP 0 %3898) {sb00001. 4`u}dst~|Ls i@Tetghd..1/'!vggu{qW(?6r|e+ccvhsb}yny hm p0vergy`g>vrfEV8uri"4_M_6]e~dtp$sfs+ "ohodaexyo0mx2^qolfyg`S_Tds FoCVm6X- 0Xe4peak esw>? 5`?*ft?{h` 'auboci`a:064411U00#.+&7Q1~ba}4R3-M2Gkub|fw.xlk001RZH0C4%~6wfq~v4ucd883010.019&%#0Mxi}ku(-R1HKXNIwo ea?>93000. 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S:$0: mODe$%8lz*(.$11*x=<*t=rrp|37579Mqvy}~cQ(4?=<7 kQ@W gtbd|q}zaOmobw0bdiqyhe`l|ijd1FP]D?CGLJ5awY^b8 ld~ 0.48!'>baev? nE808 CY\Vf='}cvaoc`sNqzr3w{g.00>8N{zx }p9b.!&"}<*e 6YCt:*RdiYr|y`up"?958+>> !-B6:'=8*1tU"V|hcebqine}%600vr.00: W{~'" 8Kd  Xe1;&!:d`#668[ cwynbOC{* csv>XM]B.cucu|{ydjt2 + 0.0647+Gn|q`$|Y0 u~emq/,c 0V~N",0> 7*;Qexfy&^mzqum0qOY^ray`d 5vdI stue 0.18: B.&28yyt6&*!3aw.6ta|q/<+$i;7XMe tzs/00 0. ).153Cq^ e~ }ohyckaicts #83 _MX 12b k8"*r!s"rrm0jixfeqenceM<7)W`u9 ^*("/5S#;rup0:7f[&vefi~k{_T`pax.0}{o~u'' Wk~dnquv66e}~jkt6P:7cs^[0)7(?#> $re{rtubk0vpsgEXY0;5b {!8# &<+u Cs|e >?&*5ER%4u ;$7&&1e?_`s`z0+0.%1%2_swpr 18a /sj1!%%+e4`yyreja|g/bkusrfcV^Y g\"4*0&>>%2?H`#>-o=1x(;s/0atcwy&+10 60940z{pk01(ve x(d>?pee_Hp *#Xameterc >H{vxrdv6^GSP1zxgzl730 Reczs|c~ x=oe}k~swxdltfzy&?.j, CYH,07<"872S`dc8Gkya|dQbqjy|i ,!w+0ki,9.;0=84 !I%]ore) wfjumdkrlu lo./|aa/-7r4`vB7nrn Max1&0Fq^66 Vo|bluw4ob!.fyh~i* 0>> J#3Pea{+4=67y 0.00dlc0: A=9+/7zu3!ak<(1;W_b~h+++H>:+:+++++;%+2+, >8+++++//)/++++;%)=*-"++++DIC;V~je+xcrcn7}j~6++;55#* 5+ ')+msda= 0# >!#" &,gcx,s2e713*= * 0Ma at"*yD%^Sc?" A fo`0H!'}tp`53FKx5%{F8.?;%;+59}rn3M3:++:%;;;;;+G~dii3`lTjynh%xkppv++:,%;;8=>Fjsrhnv9l~hdi%VU\VFHmEM_\IFSBcR&Q*:Cg  QEFOREMIS\UF_\3DQZPTZV  @Q@STETEB]::t[Ofc XoS$DAINEDgOOf PVRJESTRAX@DC::wEIGHD *{SYI]QffO~h ~ ~mWHERE` *GA>fO~ fCn**:XQ\EU UBU*SHYHD\F\PQ\Q]UGPR**** jw**mEANSXGRBSFDyUA[ZUMFORH~=;<AX]XYVBrFORhmAHTe V_Cu2;f***}KQ@EKQUABKCSJ[LE mAXXCE]FUCTOR\K^S@[7mE]ABIEVQUIBKT :$Gb SRleR#UYCLEVA@JUERVND @QBQ]ETERS:$qVX~*s rECZBQY[PDg_Av VORBUy~R'Q[TS**wEIGXZ{]\T]Vlf_p` ~ : `m@HERU`mQVs[~  fSp***w**fBALUEQBUCF]SFPSD^QEW_WTER** *acv:3mEA^CXY^LESD cQH\U@g*fFORMw2:mAHGPXPTqFORf*mAXTf V^Ff*:$|UYFT SQUQ\UCSICLE*GA>Q_UMVECTORBT]_M[  }K]^EAREQUICKT ?*:Gg SEFOBKSHR]EV^CTQDQAND **pPARAMETERC$9pWYf}  rEBZBQY^UDgOOv * TVREESTBOY^EC2*wUGWXEkCYW]Q~fOn*:w  p ~`eWHU\QgmPVv_~   fCn**:xFP^BESSD]XYVDESD@OBQTSLoxfINA]sTRUSZEEU~ACTORmQ\SG_ATIONH_BCHA=`p:k$ A> BHIFTESDmAXIMUM FORXf***GA,ATIM_EB_VLoSHOA4PZETERSpAXRl}QHI 0]RTORLENGTb*7lPPBT SQUA?OCQU[BEDmWNQ_UBVEQB_DfoN&ZBE+  RY UI@TDFRRDABPT]V**WrIA RsiL"OOtF$nI**wA[v <****sk*:$:bWCOLUTI_@q$=s  * Y@V::}UMBU\Y^WROU@ **|\  82*sOOf ;$}]    3*k$?<s?:c8  >WCOMMENDEDGKYTQF]NGCMP]]V wvfd9wW~ETXODQWMOSDSQCV@CO^XUBWTWCEGG\\S\FASTU\YVVIXEDGKYWXMC*"E~UTHE*DEFQ[ZMoshtVGERUZW]VSWUNTI]DXUBEFINE]K^@ZD*VIRD[Q\UACOM@BUDUAND:_^\KTHE^CX_G]DTHEOR_FURECOM]K^TTT|kL%VSBEUSED:$8?]STtGGVTD]EAB\K`SQ[ECTIO_]YFSUP@\UGGRP*ORE]UURZRrV\UU93XX\fO~fCntSf~Axr~ ESDfSrW_PX |UJ[XGTIO^s33$:?*p   >* **c *  * : **p** *3?s  **  ?f  9 *  9*f*  >$  **f ;*  :**v<::$s$ =::9w: 8 :**f:*   **f*  *=**f < **:3h  ***f**   **f* * : **f** ***f$*$:s:   $: 8$t?  = :  **f   ;'  **t* *;**p2**:=u :*  8**f *= **f** ***f **  **<n =*  :<n*  2  $:::{ONDBU^WAPSANDO^W\UC**nI** QSTANCEt_UUES*`  :n;   :z :$?x   2 *}*;v   *nY*~y~~:9|c9cdISTQ@QToVP]VA*n  $z*:~ *2`  3{  ? *s  ;*~     :c <   >: c;nI~ *z nc::s NcS7SNCEq@WY\B<s:~Y >$~Y  <#r$ss`Y*>:a dICZQ^S]q^_[ES*s::u*nI  $g* s$:~P wISTANSKaNG\KC:w**c *` n   *~**q   :g*     *;v *}] nn*~{*:~YtYCDQNCEs\mfE0;n  *n 2?|  8*Dc   ? *}  >*s   *s :    ***cyI yn~*b**}tYJDANCEqNGLES:c**c2nI>c  ***cb fnI**}jYEDX[iEw]GLEC$c  *nY::p>} c>?Z dICZQ^RRq_W]ES*h:t :*c  <r*    ;r :$w  *w :    :f?=r      $  ;`vs**cfwu::p *dISDO^WRq^V[PS*v:v 29c =~: :p   :*s  *f =   9f:#c      *>pv vL2ckw3*p Distance Angles F17 1.5730 (0.0223) F16 1.5825 (0.0160) 93.31 (1.03) F13 1.5822 (0.0144) 89.70 (1.00) 176.95 (0.81) F18 1.6125 (0.0157) 77.97 (0.97) 89.90 (0.81) 90.28 (0.77) F14 1.5686 (0.0177) 167.38 (1.08) 89.37 (0.89) 87.58 (0.85) 89.72 (0.88) F15 1.5745 (0.0204) 114.53 (1.15) 90.90 (0.96) 88.26 (0.94) 167.40 (0.99) 77.72 (0.98) P4 - F17 F16 F13 F18 F14 P1 - Distance Angles F1 1.5887 (0.0182) F4 1.5977 (0.0227) 170.99 (1.14) F5 1.5493 (0.0162) 86.96 (0.91) 90.45 (1.05) F3 1.6101 (0.0149) 85.64 (0.87) 85.77 (0.99) 90.61 (0.82) F2 1.6319 (0.0143) 89.35 (0.85) 93.35 (0.99) 176.16 (0.81) 90.15 (0.74) F6 1.5995 (0.0223) 80.74 (1.02) 107.80 (1.19) 87.83 (1.02) 166.35 (1.01) 90.56 (0.98) P1 - F1 F4 F5 F3 F2 C49 - Distance Angles C50 1.2994 (0.0359) C53 1.5049 (0.0477) 102.57 (3.10) C49 - C50 P5 - Distance Angles F22 1.5633 (0.0170) F19 1.5835 (0.0152) 178.75 (0.96) F20 1.5591 (0.0151) 87.59 (0.84) 91.44 (0.80) F21 1.5683 (0.0215) 84.13 (0.98) 96.68 (0.96) 92.00 (0.97) F23 1.5692 (0.0140) 92.08 (0.81) 88.89 (0.77) 179.66 (0.79) 88.03 (0.94) F24 1.6030 (0.0171) 94.14 (0.88) 85.09 (0.82) 90.37 (0.85) 177.01 (1.03) 89.60 (0.81) P5 - F22 F19 F20 F21 F23 F13 - Distance Angles P4 1.5822 (0.0144) F13 - F7 - Distance Angles P2 1.5363 (0.0144) F7 - F23 - Distance Angles P5 1.5692 (0.0140) F23 - F2 - Distance Angles P1 1.6319 (0.0142) F2 - F10 - Distance Angles P2 1.5439 (0.0148) F10 - F20 - Distance Angles P5 1.5591 (0.0151) F20 - F3 - Distance Angles P1 1.6101 (0.0149) F3 - F11 - Distance Angles P2 1.5383 (0.0146) F11 - F15 - Distance Angles P4 1.5745 (0.0203) F15 - F6 - Distance Angles P1 1.5995 (0.0221) F6 - F14 - Distance Angles P4 1.5686 (0.0177) F14 - F1 - Distance Angles P1 1.5887 (0.0181) F1 - F19 - Distance Angles P5 1.5835 (0.0151) F19 - F16 - Distance Angles P4 1.5825 (0.0160) F16 - F8 - Distance Angles P2 1.5430 (0.0170) F8 - F22 - Distance Angles P5 1.5633 (0.0169) F22 - F18 - Distance Angles P4 1.6125 (0.0156) F18 - F5 - Distance Angles P1 1.5493 (0.0162) F5 - F12 - Distance Angles P2 1.5788 (0.0164) F12 - F4 - Distance Angles P1 1.5977 (0.0226) F4 - F24 - Distance Angles P5 1.6030 (0.0170) F24 - F9 - Distance Angles P2 1.5781 (0.0228) F9 - F17 - Distance Angles P4 1.5730 (0.0223) F17 - F21 - Distance Angles P5 1.5683 (0.0215) F21 - N6 - Distance Angles C16 1.4296 (0.0217) C15 1.5268 (0.0219) 109.49 (1.26) C17 1.5283 (0.0211) 114.27 (1.32) 107.55 (1.23) Ni2 2.1127 (0.0118) 118.99 (1.04) 105.73 (0.96) 99.83 (0.89) N6 - C16 C15 C17 N5 - Distance Angles C13 1.4896 (0.0225) C24 1.5335 (0.0219) 105.96 (1.29) C14 1.4708 (0.0202) 110.74 (1.26) 112.79 (1.24) Ni2 2.1217 (0.0121) 117.97 (1.03) 105.97 (0.93) 103.51 (0.93) N5 - C13 C24 C14 N8 - Distance Angles C21 1.4669 (0.0241) C23 1.5098 (0.0215) 108.77 (1.32) C22 1.4635 (0.0247) 106.61 (1.45) 111.58 (1.41) Ni2 2.0832 (0.0127) 109.48 (1.12) 101.23 (0.93) 118.86 (1.14) N8 - C21 C23 C22 N7 - Distance Angles C19 1.4760 (0.0237) C18 1.4593 (0.0233) 109.05 (1.43) C20 1.5042 (0.0225) 108.74 (1.35) 113.51 (1.37) Ni2 2.0823 (0.0134) 117.18 (1.11) 106.88 (1.06) 101.48 (1.02) N7 - C19 C18 C20 N1 - Distance Angles C1 1.4884 (0.0226) C12 1.5408 (0.0241) 112.77 (1.39) C2 1.5384 (0.0229) 107.93 (1.38) 110.92 (1.35) Ni1 2.0772 (0.0150) 112.56 (1.09) 105.21 (1.07) 107.35 (1.05) N1 - C1 C12 C2 N3 - Distance Angles C7 1.5557 (0.0249) C6 1.5231 (0.0246) 106.34 (1.44) C8 1.4973 (0.0268) 111.55 (1.50) 111.01 (1.49) Ni1 2.0932 (0.0134) 112.54 (1.10) 105.29 (1.09) 109.89 (1.16) N3 - C7 C6 C8 N2 - Distance Angles C5 1.4795 (0.0233) C4 1.5205 (0.0231) 108.41 (1.39) C3 1.5162 (0.0241) 111.97 (1.44) 109.60 (1.42) Ni1 2.1972 (0.0150) 109.06 (1.16) 114.72 (1.06) 103.09 (1.10) N2 - C5 C4 C3 N4 - Distance Angles C9 1.4627 (0.0232) C10 1.5082 (0.0241) 108.34 (1.42) C11 1.5109 (0.0227) 111.17 (1.39) 111.47 (1.43) Ni1 2.1730 (0.0149) 103.76 (1.10) 114.83 (1.13) 107.04 (1.06) N4 - C9 C10 C11 C8 - Distance Angles C9 1.5279 (0.0287) N3 1.4973 (0.0267) 106.70 (1.69) C8 - C9 C2 - Distance Angles C3 1.4890 (0.0270) N1 1.5384 (0.0229) 109.08 (1.48) C2 - C3 C23 - Distance Angles N8 1.5098 (0.0215) C24 1.4994 (0.0252) 110.96 (1.40) C23 - N8 C15 - Distance Angles C14 1.4710 (0.0245) N6 1.5268 (0.0219) 114.05 (1.43) C15 - C14 C20 - Distance Angles C21 1.5192 (0.0281) N7 1.5042 (0.0224) 114.19 (1.57) C20 - C21 C4 - Distance Angles N2 1.5205 (0.0230) C4 - C14 - Distance Angles C15 1.4710 (0.0246) N5 1.4708 (0.0201) 111.18 (1.41) C14 - C15 C13 - Distance Angles N5 1.4896 (0.0225) C13 - C24 - Distance Angles N5 1.5335 (0.0217) C23 1.4994 (0.0252) 109.63 (1.48) C24 - N5 C18 - Distance Angles N7 1.4593 (0.0231) C17 1.4644 (0.0255) 112.51 (1.63) C18 - N7 C17 - Distance Angles C18 1.4644 (0.0255) N6 1.5283 (0.0211) 106.29 (1.45) C17 - C18 C7 - Distance Angles N3 1.5557 (0.0248) C7 - C12 - Distance Angles C11 1.4124 (0.0257) N1 1.5408 (0.0241) 109.82 (1.56) C12 - C11 C5 - Distance Angles C6 1.5114 (0.0284) N2 1.4795 (0.0232) 111.65 (1.62) C5 - C6 C19 - Distance Angles N7 1.4760 (0.0237) C19 - C16 - Distance Angles N6 1.4296 (0.0215) C16 - C6 - Distance Angles C5 1.5114 (0.0284) N3 1.5231 (0.0245) 110.02 (1.61) C6 - C5 C3 - Distance Angles C2 1.4890 (0.0269) N2 1.5162 (0.0241) 110.04 (1.62) C3 - C2 C9 - Distance Angles N4 1.4627 (0.0231) C8 1.5279 (0.0288) 113.19 (1.67) C9 - N4 C10 - Distance Angles N4 1.5082 (0.0241) C10 - C1 - Distance Angles N1 1.4884 (0.0226) C1 - C11 - Distance Angles C12 1.4124 (0.0257) N4 1.5109 (0.0227) 114.37 (1.62) C11 - C12 C21 - Distance Angles N8 1.4669 (0.0240) C20 1.5192 (0.0281) 110.35 (1.62) C21 - N8 C22 - Distance Angles N8 1.4635 (0.0246) C22 - N14 - Distance Angles C39 1.4843 (0.0212) C41 1.4791 (0.0246) 107.09 (1.37) C40 1.5186 (0.0244) 107.33 (1.36) 108.06 (1.40) Ni4 2.0679 (0.0129) 104.70 (0.96) 108.79 (1.12) 120.16 (1.11) N14 - C39 C41 C40 N9 - Distance Angles C36 1.4842 (0.0218) C25 1.4692 (0.0213) 111.26 (1.31) C26 1.5521 (0.0242) 109.75 (1.34) 107.34 (1.33) Ni3 2.0714 (0.0132) 107.91 (1.00) 114.06 (1.04) 106.37 (1.02) N9 - C36 C25 C26 N15 - Distance Angles C44 1.4625 (0.0230) C42 1.4966 (0.0233) 113.65 (1.40) C43 1.4536 (0.0210) 109.51 (1.38) 108.98 (1.36) Ni4 2.1011 (0.0141) 106.92 (1.07) 101.88 (1.08) 115.86 (1.07) N15 - C44 C42 C43 N13 - Distance Angles C38 1.5099 (0.0220) C48 1.4708 (0.0199) 114.75 (1.26) C37 1.4678 (0.0235) 105.71 (1.35) 107.86 (1.28) Ni4 2.1139 (0.0123) 108.69 (0.97) 103.12 (0.95) 117.07 (1.05) N13 - C38 C48 C37 N16 - Distance Angles C46 1.4209 (0.0233) C45 1.5248 (0.0232) 111.38 (1.44) C47 1.5216 (0.0227) 108.59 (1.39) 109.00 (1.29) Ni4 2.0976 (0.0129) 119.28 (1.13) 101.72 (0.99) 106.35 (1.03) N16 - C46 C45 C47 N10 - Distance Angles C29 1.4583 (0.0225) C27 1.5363 (0.0237) 113.59 (1.41) C28 1.5392 (0.0246) 108.45 (1.41) 110.30 (1.42) Ni3 2.1761 (0.0148) 103.63 (1.07) 107.81 (1.08) 112.99 (1.14) N10 - C29 C27 C28 N11 - Distance Angles C31 1.5649 (0.0229) C32 1.5142 (0.0232) 105.95 (1.31) C30 1.5559 (0.0264) 110.51 (1.38) 110.81 (1.43) Ni3 2.1155 (0.0135) 115.08 (1.05) 106.67 (1.03) 107.76 (1.11) N11 - C31 C32 C30 N12 - Distance Angles C35 1.4492 (0.0217) C33 1.5122 (0.0242) 110.31 (1.43) C34 1.5340 (0.0222) 108.02 (1.36) 107.95 (1.36) Ni3 2.1621 (0.0146) 105.11 (1.05) 109.86 (1.12) 115.52 (1.01) N12 - C35 C33 C34 C37 - Distance Angles N13 1.4678 (0.0235) C37 - C48 - Distance Angles N13 1.4708 (0.0199) C47 1.4946 (0.0251) 112.63 (1.40) C48 - N13 C42 - Distance Angles C41 1.4637 (0.0282) N15 1.4966 (0.0233) 114.05 (1.69) C42 - C41 C30 - Distance Angles C29 1.4669 (0.0280) N11 1.5559 (0.0264) 106.33 (1.70) C30 - C29 C34 - Distance Angles N12 1.5340 (0.0221) C34 - C38 - Distance Angles N13 1.5099 (0.0220) C39 1.5929 (0.0258) 107.71 (1.42) C38 - N13 C43 - Distance Angles N15 1.4536 (0.0210) C43 - C36 - Distance Angles N9 1.4842 (0.0218) C35 1.5198 (0.0253) 107.84 (1.41) C36 - N9 C25 - Distance Angles N9 1.4692 (0.0213) C25 - C39 - Distance Angles N14 1.4843 (0.0212) C38 1.5929 (0.0258) 108.44 (1.39) C39 - N14 C47 - Distance Angles C48 1.4946 (0.0251) N16 1.5216 (0.0227) 112.98 (1.49) C47 - C48 C29 - Distance Angles N10 1.4583 (0.0225) C30 1.4669 (0.0281) 113.96 (1.66) C29 - N10 C35 - Distance Angles N12 1.4492 (0.0217) C36 1.5198 (0.0253) 108.39 (1.50) C35 - N12 C45 - Distance Angles N16 1.5248 (0.0232) C44 1.4776 (0.0259) 106.94 (1.49) C45 - N16 C27 - Distance Angles C26 1.4923 (0.0274) N10 1.5363 (0.0237) 112.20 (1.62) C27 - C26 C33 - Distance Angles N12 1.5122 (0.0241) C32 1.5411 (0.0280) 112.38 (1.62) C33 - N12 C40 - Distance Angles N14 1.5186 (0.0244) C40 - C44 - Distance Angles N15 1.4625 (0.0228) C45 1.4776 (0.0259) 112.90 (1.62) C44 - N15 C32 - Distance Angles C33 1.5411 (0.0281) N11 1.5142 (0.0232) 109.83 (1.56) C32 - C33 C31 - Distance Angles N11 1.5649 (0.0229) C31 - C28 - Distance Angles N10 1.5392 (0.0247) C28 - C46 - Distance Angles N16 1.4209 (0.0233) C46 - C26 - Distance Angles C27 1.4923 (0.0273) N9 1.5521 (0.0242) 109.09 (1.59) C26 - C27 C41 - Distance Angles N14 1.4791 (0.0246) C42 1.4637 (0.0282) 112.38 (1.70) C41 - N14 C50 - Distance Angles C51 1.3108 (0.0368) C49 1.2994 (0.0359) 111.42 (2.81) C50 - C51 C51 - Distance Angles C50 1.3108 (0.0367) C52 1.5422 (0.0478) 109.03 (3.13) C51 - C50 C53 - Distance Angles C52 1.4530 (0.0510) C49 1.5049 (0.0475) 102.21 (3.55) C53 - C52 C52 - Distance Angles C53 1.4530 (0.0509) C51 1.5422 (0.0477) 94.22 (3.44) C52 - C53 P6 - Distance Angles F90 2.0187 (0.0053) F93 2.3401 (0.0258) 79.42 (0.63) P6 - F90 F90 - Distance Angles P6 2.0187 (0.0053) F90 - F86 - Distance Angles P3 1.6257 (0.0120) F86 - F85 - Distance Angles P3 1.5926 (0.0119) F85 - F84 - Distance Angles P3 1.5548 (0.0180) F84 - F83 - Distance Angles P3 1.5789 (0.0171) F83 - F82 - Distance Angles P3 1.5615 (0.0223) F82 - F81 - Distance Angles P3 1.5831 (0.0214)              "               6Sb>!    #            $                                *3             3RF)               *                                     !            )$      ,    Q                                               ,                                              !       !                                                       #                  '"                                                                                                                                       !!             !   &                                      !    !                                                   &'                                                          #       "$+%                                                                                                          #   #                                                             "!                                                    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2 0 -27 33.5389 32.3866 2 -2 0 27 33.2530 27.5350 1 1 0 -27 4.8817 31.5782 2 -1 0 27 18.6062 29.7025 1 0 0 -27 8.2349 32.6777 2 0 0 27 31.8567 31.0519 1 8 -1 -27 29.4835 30.5320 2 -8 1 27 -8.9358 28.7985 1 7 -1 -27 34.2826 27.5755 2 -7 1 27 -2.9333 30.2803 1 6 -1 -27 -33.049 27.173 2 -6 1 27 41.9781 31.8964 1 5 -1 -27 10.7470 29.4923 2 -5 1 27 66.8700 25.5979 1 4 -1 -27 35.9225 27.1226 2 -4 1 27 1.3893 28.2001 1 3 -1 -27 35.6901 30.0378 2 -3 1 27 37.6304 29.0695 1 2 -1 -27 2.4599 30.3168 2 -2 1 27 9.0230 29.3166 1 1 -1 -27 -23.895 32.146 2 -1 1 27 2.0720 29.5455 1 8 -2 -27 25.4070 30.3573 2 -8 2 27 4.7900 31.8244 1 7 -2 -27 2.7219 29.8350 2 -7 2 27 -19.737 30.425 1 6 -2 -27 50.1167 29.3448 2 -6 2 27 -7.1664 26.5733 1 5 -2 -27 41.3578 30.1507 2 -5 2 27 69.4779 29.6663 1 4 -2 -27 30.5619 30.6751 2 -4 2 27 9.3530 29.1221 1 3 -2 -27 9.0597 29.0421 2 -3 2 27 13.3523 28.9489 1 2 -2 -27 42.6408 30.2628 2 -2 2 27 -19.413 32.070 1 1 -2 -27 -4.0977 32.8868 2 -1 2 27 15.7300 32.2739 1 8 -3 -27 -25.536 30.923 2 -8 3 27 -14.148 31.856 1 7 -3 -27 -4.9461 30.7302 2 -7 3 27 0.5863 30.2331 1 6 -3 -27 27.0321 27.5935 2 -6 3 27 13.4489 30.4968 1 5 -3 -27 -41.239 29.026 2 -5 3 27 38.9256 33.8734 1 4 -3 -27 25.7458 29.6715 2 -4 3 27 -50.924 30.655 1 3 -3 -27 8.3717 30.0141 2 -3 3 27 -39.410 30.717 1 2 -3 -27 38.5261 31.4511 2 -2 3 27 28.4978 31.9179 1 7 -4 -27 23.2340 30.8510 2 -7 4 27 25.0868 31.8395 1 6 -4 -27 78.0433 30.7439 2 -6 4 27 3.2135 31.7390 1 5 -4 -27 22.8606 31.4702 2 -5 4 27 -3.4123 28.4924 1 4 -4 -27 34.5994 30.4834 2 -4 4 27 59.1712 31.6636 1 3 -4 -27 52.1862 31.6156 2 -3 4 27 25.4049 31.2707 1 6 -5 -27 -34.241 30.699 2 -6 5 27 19.1973 32.3591 1 5 -5 -27 21.4141 31.5769 2 -5 5 27 22.4673 32.4120 1 -4 5 27 6.9336 31.8117 1 3 9 -28 -52.405 33.021 2 -3 -9 28 -29.627 31.770 1 5 8 -28 2.3523 34.4155 2 -5 -8 28 -33.003 31.687 1 4 8 -28 -16.525 34.013 2 -4 -8 28 12.4570 31.4086 1 3 8 -28 5.1990 33.3850 2 -3 -8 28 41.4879 31.9881 1 2 8 -28 -21.434 30.331 2 -2 -8 28 76.1339 33.0418 1 5 7 -28 12.8937 33.3558 2 -5 -7 28 37.7878 29.1871 1 4 7 -28 6.2718 33.3286 2 -4 -7 28 5.4077 31.7003 1 3 7 -28 4.2554 32.4316 2 -3 -7 28 54.5606 32.0017 1 2 7 -28 7.2998 32.3104 2 -2 -7 28 -23.975 31.966 1 6 6 -28 38.8230 31.1984 2 -6 -6 28 69.1078 31.7442 1 5 6 -28 -10.152 30.397 2 -5 -6  ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Version 2008/4 + + Copyright(c) 2008 Bruker Analytical X-ray Solutions All Rights Reserved + + char360a started at 13:30:02 on 04-Aug-2011 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL char360a in P-1 CELL 0.71073 12.4995 21.4058 21.4135 97.973 104.090 103.996 ZERR 6.00 0.0046 0.0079 0.0080 0.007 0.007 0.007 LATT 1 SFAC C H N F P S Ni UNIT 144 336 48 36 6 12 12 V = 5271.91 F(000) = 2478.0 Mu = 1.30 mm-1 Cell Wt = 4699.67 Rho = 1.480 L.S. 20 BOND FMAP 2 PLAN 20 SIZE 0.051 0.053 0.183 TEMP -73 WGHT 0.100000 FVAR 0.06838 NI4 7 0.70763 0.58813 0.28736 11.00000 0.02694 NI3 7 0.60473 0.40891 0.38471 11.00000 0.03388 S3 6 0.67225 0.50278 0.33748 11.00000 0.04071 S4 6 0.53852 0.50052 0.37976 11.00000 0.03688 NI2 7 0.20703 0.78704 1.08773 11.00000 0.02798 NI1 7 0.10569 0.88511 0.90886 11.00000 0.03400 S1 6 0.17179 0.83767 1.00228 11.00000 0.03926 S2 6 0.03954 0.88006 1.00004 11.00000 0.03670 P2 5 0.69712 0.27796 0.64875 11.00000 0.03830 P3 5 0.24985 0.47351 0.02649 11.00000 0.04677 P4 5 0.44564 0.09430 0.24953 11.00000 0.05199 P1 5 -0.05410 0.75098 0.59479 11.00000 0.05354 C49 1 0.01385 0.45012 0.17769 11.00000 0.11223 P5 5 0.80393 0.85137 0.22297 11.00000 0.03806 F13 4 0.47242 0.14232 0.31925 11.00000 0.09165 F7 4 0.68491 0.29204 0.72029 11.00000 0.09634 F23 4 0.81064 0.77880 0.20468 11.00000 0.09915 F2 4 -0.02397 0.82112 0.64399 11.00000 0.08776 F10 4 0.70765 0.26065 0.57802 11.00000 0.10513 F20 4 0.79647 0.92336 0.24024 11.00000 0.10496 F3 4 -0.17639 0.75522 0.56220 11.00000 0.09366 F11 4 0.81743 0.26873 0.68081 11.00000 0.10784 F15 4 0.55972 0.14032 0.23841 11.00000 0.17263 F6 4 0.06484 0.74020 0.63548 11.00000 0.18990 F14 4 0.39784 0.14894 0.21626 11.00000 0.13874 F1 4 -0.10797 0.71916 0.64349 11.00000 0.14525 F19 4 0.68330 0.82038 0.23050 11.00000 0.10920 F16 4 0.41633 0.05051 0.18019 11.00000 0.09755 F8 4 0.57364 0.28346 0.62068 11.00000 0.12369 F22 4 0.92159 0.87961 0.21122 11.00000 0.12447 F18 4 0.32044 0.06069 0.25581 11.00000 0.10303 F5 4 -0.08247 0.68137 0.55201 11.00000 0.12337 F12 4 0.64423 0.19868 0.64708 11.00000 0.12726 F4 4 -0.02279 0.78393 0.54018 11.00000 0.17931 F24 4 0.85772 0.85654 0.29979 11.00000 0.13949 F9 4 0.76074 0.35788 0.65744 11.00000 0.17179 F17 4 0.48623 0.04060 0.27834 11.00000 0.18808 F21 4 0.75203 0.84823 0.14791 11.00000 0.16543 N6 3 0.38855 0.81321 1.12033 11.00000 0.03658 N5 3 0.21732 0.69355 1.04588 11.00000 0.03522 N8 3 0.05475 0.73658 1.10048 11.00000 0.03864 N7 3 0.22307 0.85142 1.17328 11.00000 0.04546 N1 3 -0.00838 0.92989 0.85796 11.00000 0.05528 N3 3 0.22150 0.87241 0.85468 11.00000 0.04549 N2 3 0.22241 0.98544 0.93904 11.00000 0.05220 N4 3 -0.01080 0.79431 0.84032 11.00000 0.05181 C8 1 0.15087 0.81860 0.78834 11.00000 0.08222 C2 1 0.06173 1.00192 0.85919 11.00000 0.05496 C23 1 0.07552 0.67566 1.11004 11.00000 0.05629 C15 1 0.42147 0.75094 1.10075 11.00000 0.06182 C20 1 0.14784 0.80841 1.20524 11.00000 0.06259 C4 1 0.28955 1.00646 1.01239 11.00000 0.05180 C14 1 0.32797 0.69038 1.09103 11.00000 0.05790 C13 1 0.21127 0.68293 0.97548 11.00000 0.06570 C24 1 0.11498 0.64416 1.05176 11.00000 0.05252 C18 1 0.35018 0.87704 1.20715 11.00000 0.06789 C17 1 0.41199 0.82432 1.19572 11.00000 0.05597 C7 1 0.32017 0.85112 0.89406 11.00000 0.06954 C12 1 -0.05304 0.88822 0.78836 11.00000 0.05765 C5 1 0.30981 0.99284 0.90159 11.00000 0.05787 C19 1 0.18098 0.91045 1.16673 11.00000 0.06030 C16 1 0.45724 0.86751 1.09691 11.00000 0.06419 C6 1 0.26785 0.94121 0.84186 11.00000 0.07175 C3 1 0.14285 1.03077 0.92263 11.00000 0.06921 C9 1 0.06630 0.76987 0.81011 11.00000 0.06080 C10 1 -0.07244 0.74558 0.86954 11.00000 0.05845 C1 1 -0.10045 0.93444 0.88782 11.00000 0.05242 C11 1 -0.09657 0.81679 0.79121 11.00000 0.05555 C21 1 0.03603 0.76675 1.15801 11.00000 0.05770 C22 1 -0.05059 0.72690 1.04674 11.00000 0.07537 N14 3 0.55665 0.60072 0.23609 11.00000 0.03649 N9 3 0.49228 0.35760 0.42986 11.00000 0.04030 N15 3 0.72371 0.67366 0.35193 11.00000 0.04702 N13 3 0.71715 0.54797 0.19382 11.00000 0.03160 N16 3 0.88672 0.62195 0.31294 11.00000 0.04457 N10 3 0.48586 0.33817 0.29541 11.00000 0.05029 N11 3 0.71804 0.35459 0.36977 11.00000 0.04587 N12 3 0.72048 0.43801 0.48433 11.00000 0.05195 C37 1 0.71693 0.47766 0.18269 11.00000 0.06555 C48 1 0.82574 0.58882 0.18909 11.00000 0.05732 C42 1 0.65301 0.70618 0.30848 11.00000 0.06673 C30 1 0.65041 0.28822 0.31552 11.00000 0.06768 C34 1 0.79021 0.51102 0.50645 11.00000 0.04546 C38 1 0.61723 0.55121 0.14495 11.00000 0.05472 C43 1 0.67904 0.66585 0.41009 11.00000 0.05281 C36 1 0.55797 0.35984 0.49762 11.00000 0.05073 C25 1 0.39433 0.38576 0.43194 11.00000 0.05177 C39 1 0.56971 0.60956 0.17312 11.00000 0.04904 C47 1 0.92640 0.60233 0.25150 11.00000 0.06505 C29 1 0.56243 0.31036 0.26601 11.00000 0.06667 C35 1 0.64679 0.42454 0.52660 11.00000 0.06045 C45 1 0.90990 0.69607 0.32451 11.00000 0.05266 C27 1 0.39837 0.29042 0.31838 11.00000 0.06755 C33 1 0.80271 0.39878 0.49171 11.00000 0.05890 C40 1 0.44595 0.54444 0.22519 11.00000 0.07038 C44 1 0.84341 0.71131 0.37600 11.00000 0.05680 C32 1 0.77054 0.33879 0.43717 11.00000 0.06470 C31 1 0.82157 0.39085 0.34997 11.00000 0.04945 C28 1 0.42548 0.37282 0.24463 11.00000 0.06595 C46 1 0.95297 0.59948 0.36718 11.00000 0.06595 C26 1 0.44491 0.28771 0.38653 11.00000 0.06278 C41 1 0.54092 0.66072 0.26813 11.00000 0.06805 C50 1 -0.02985 0.42913 0.22230 11.00000 0.08820 C51 1 0.04274 0.43366 0.27236 11.00000 0.18020 C53 1 0.14234 0.48351 0.21096 11.00000 0.13779 C52 1 0.17680 0.44317 0.24899 11.00000 0.25268 P6 5 0.66844 -0.00028 0.49865 11.00000 0.02421 F90 4 0.83135 0.00128 0.50037 11.00000 -0.01096 F91 4 0.46851 -0.02365 0.44982 11.00000 0.02516 F99 4 1.02920 0.04920 0.52160 11.00000 0.05000 F86 4 0.24210 0.41540 -0.03080 11.00000 0.05000 F85 4 0.25890 0.53160 0.08350 11.00000 0.05000 F84 4 0.34000 0.44990 0.07660 11.00000 0.05000 F83 4 0.16230 0.42210 0.04890 11.00000 0.05000 F82 4 0.14970 0.48880 -0.02010 11.00000 0.05000 F81 4 0.35320 0.52020 0.01400 11.00000 0.05000 F93 4 0.74180 0.09450 0.47180 11.00000 0.05000 HKLF 4 Covalent radii and connectivity table for char360a in P-1 C 0.770 H 0.320 N 0.700 F 0.640 P 1.100 S 1.030 NI 1.250 Ni4 - N14 N15 N16 N13 S3 Ni3 - N9 N11 N12 N10 S4 S3 S3 - S4 Ni4 Ni3 S4 - S3 Ni3 Ni2 - N8 N7 N6 N5 S1 Ni1 - N1 N3 N2 N4 S2 S1 S1 - S2 Ni2 Ni1 S2 - S1 Ni1 P2 - F8 F10 F11 F7 F12 F9 P3 - F82 F81 F83 F85 F84 F86 P4 - F17 F16 F13 F18 F14 F15 P1 - F1 F4 F5 F3 F2 F6 C49 - C50 C53 P5 - F22 F19 F20 F21 F23 F24 F13 - P4 F7 - P2 F23 - P5 F2 - P1 F10 - P2 F20 - P5 F3 - P1 F11 - P2 F15 - P4 F6 - P1 F14 - P4 F1 - P1 F19 - P5 F16 - P4 F8 - P2 F22 - P5 F18 - P4 F5 - P1 F12 - P2 F4 - P1 F24 - P5 F9 - P2 F17 - P4 F21 - P5 N6 - C16 C15 C17 Ni2 N5 - C13 C24 C14 Ni2 N8 - C21 C23 C22 Ni2 N7 - C19 C18 C20 Ni2 N1 - C1 C12 C2 Ni1 N3 - C7 C6 C8 Ni1 N2 - C5 C4 C3 Ni1 N4 - C9 C10 C11 Ni1 C8 - C9 N3 C2 - C3 N1 C23 - N8 C24 C15 - C14 N6 C20 - C21 N7 C4 - N2 C14 - C15 N5 C13 - N5 C24 - N5 C23 C18 - N7 C17 C17 - C18 N6 C7 - N3 C12 - C11 N1 C5 - C6 N2 C19 - N7 C16 - N6 C6 - C5 N3 C3 - C2 N2 C9 - N4 C8 C10 - N4 C1 - N1 C11 - C12 N4 C21 - N8 C20 C22 - N8 N14 - C39 C41 C40 Ni4 N9 - C36 C25 C26 Ni3 N15 - C44 C42 C43 Ni4 N13 - C38 C48 C37 Ni4 N16 - C46 C45 C47 Ni4 N10 - C29 C27 C28 Ni3 N11 - C31 C32 C30 Ni3 N12 - C35 C33 C34 Ni3 C37 - N13 C48 - N13 C47 C42 - C41 N15 C30 - C29 N11 C34 - N12 C38 - N13 C39 C43 - N15 C36 - N9 C35 C25 - N9 C39 - N14 C38 C47 - C48 N16 C29 - N10 C30 C35 - N12 C36 C45 - N16 C44 C27 - C26 N10 C33 - N12 C32 C40 - N14 C44 - N15 C45 C32 - C33 N11 C31 - N11 C28 - N10 C46 - N16 C26 - C27 N9 C41 - N14 C42 C50 - C51 C49 C51 - C50 C52 C53 - C52 C49 C52 - C53 C51 P6 - F90 F93 F90 - P6 F91 - no bonds found F99 - no bonds found F86 - P3 F85 - P3 F84 - P3 F83 - P3 F82 - P3 F81 - P3 F93 - P6 72066 Reflections read, of which 0 rejected -16 =< h =< 16, -28 =< k =< 28, -28 =< l =< 28, Max. 2-theta = 56.91 0 Systematic absence violations 0 Inconsistent equivalents 26094 Unique reflections, of which 0 suppressed R(int) = 0.1595 R(sigma) = 0.2211 Friedel opposites merged Maximum memory for data reduction = 5980 / 260797 ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 144.00 106.00 H 336.00 0.00 N 48.00 32.00 F 36.00 68.00 P 6.00 12.00 S 12.00 8.00 NI 12.00 8.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 7151 / 616532 wR2 = 0.5155 before cycle 1 for 26094 data and 469 / 469 parameters GooF = S = 2.151; Restrained GooF = 2.151 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 Shifts scaled down to reduce maximum shift/esd from 19.64 to 15.00 N value esd shift/esd parameter 1 0.06875 0.00024 1.511 OSF 445 0.05918 0.00264 3.474 U11 F86 449 0.05803 0.00263 3.050 U11 F85 453 0.07370 0.00265 8.936 U11 F84 457 0.07329 0.00265 8.787 U11 F83 461 0.07963 0.00264 11.207 U11 F82 465 0.07710 0.00265 10.211 U11 F81 469 0.07978 0.00265 11.250 U11 F93 Mean shift/esd = 0.701 Maximum = 11.250 for U11 F93 Max. shift = 0.102 A for C52 Max. dU = 0.030 for F93 Least-squares cycle 2 Maximum vector length = 511 Memory required = 7151 / 616532 wR2 = 0.4955 before cycle 2 for 26094 data and 469 / 469 parameters GooF = S = 2.024; Restrained GooF = 2.024 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06979 0.00023 4.467 OSF 445 0.06862 0.00279 3.377 U11 F86 449 0.06669 0.00275 3.151 U11 F85 453 0.10693 0.00335 9.928 U11 F84 457 0.10571 0.00332 9.752 U11 F83 461 0.12444 0.00358 12.535 U11 F82 465 0.11709 0.00349 11.470 U11 F81 469 0.12647 0.00358 13.041 U11 F93 Mean shift/esd = 0.726 Maximum = 13.041 for U11 F93 Max. shift = 0.112 A for C52 Max. dU = 0.047 for F93 Least-squares cycle 3 Maximum vector length = 511 Memory required = 7151 / 616532 wR2 = 0.4851 before cycle 3 for 26094 data and 469 / 469 parameters GooF = S = 1.980; Restrained GooF = 1.980 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07005 0.00023 1.135 OSF 453 0.12407 0.00459 3.737 U11 F84 457 0.12172 0.00452 3.539 U11 F83 461 0.15334 0.00541 5.345 U11 F82 465 0.14206 0.00507 4.925 U11 F81 469 0.16235 0.00548 6.545 U11 F93 Mean shift/esd = 0.298 Maximum = 6.545 for U11 F93 Max. shift = 0.062 A for F93 Max. dU = 0.036 for F93 Least-squares cycle 4 Maximum vector length = 511 Memory required = 7151 / 616532 wR2 = 0.4828 before cycle 4 for 26094 data and 469 / 469 parameters GooF = S = 1.963; Restrained GooF = 1.963 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07013 0.00023 0.346 OSF Mean shift/esd = 0.182 Maximum = 2.756 for U11 F93 Max. shift = 0.053 A for F93 Max. dU = 0.020 for F93 Least-squares cycle 5 Maximum vector length = 511 Memory required = 7151 / 616532 wR2 = 0.4822 before cycle 5 for 26094 data and 469 / 469 parameters GooF = S = 1.959; Restrained GooF = 1.959 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07017 0.00023 0.142 OSF Mean shift/esd = 0.111 Maximum = 1.240 for U11 F93 Max. shift = 0.033 A for F81 Max. dU = 0.010 for F93 Least-squares cycle 6 Maximum vector length = 511 Memory required = 7151 / 616532 wR2 = 0.4820 before cycle 6 for 26094 data and 469 / 469 parameters GooF = S = 1.958; Restrained GooF = 1.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07018 0.00023 0.051 OSF Mean shift/esd = 0.070 Maximum = 0.791 for x F81 Max. shift = 0.023 A for F81 Max. dU = 0.006 for F93 Least-squares cycle 7 Maximum vector length = 511 Memory required = 7151 / 616532 wR2 = 0.4820 before cycle 7 for 26094 data and 469 / 469 parameters GooF = S = 1.958; Restrained GooF = 1.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07018 0.00023 0.015 OSF Mean shift/esd = 0.044 Maximum = 0.539 for x F81 Max. shift = 0.015 A for F81 Max. dU = 0.003 for F93 Least-squares cycle 8 Maximum vector length = 511 Memory required = 7151 / 616532 wR2 = 0.4819 before cycle 8 for 26094 data and 469 / 469 parameters GooF = S = 1.958; Restrained GooF = 1.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07018 0.00023 0.003 OSF Mean shift/esd = 0.028 Maximum = 0.372 for x F81 Max. shift = 0.011 A for F17 Max. dU = 0.002 for F93 Least-squares cycle 9 Maximum vec00000 0.05716 0.04316 0.00158 0.00094 0.00093 0.00000 0.00479 C21 0.03755 0.76670 1.16129 1.00000 0.07065 0.04894 0.00180 0.00105 0.00106 0.00000 0.00572 C22 -0.05546 0.72771 1.04809 1.00000 0.07450 0.05068 0.00186 0.00110 0.00109 0.00000 0.00602 N14 0.55367 0.60014 0.23584 1.00000 0.04120 0.02953 0.00108 0.00064 0.00064 0.00000 0.00314 N9 0.49300 0.35814 0.42990 1.00000 0.04655 0.03091 0.00114 0.00067 0.00066 0.00000 0.00340 N15 0.72424 0.67483 0.35278 1.00000 0.04763 0.03139 0.00117 0.00068 0.00068 0.00000 0.00345 N13 0.71618 0.54665 0.19378 1.00000 0.03695 0.02818 0.00104 0.00061 0.00060 0.00000 0.00294 N16 0.88783 0.62135 0.31342 1.00000 0.04302 0.02986 0.00110 0.00065 0.00065 0.00000 0.00324 N10 0.48942 0.33944 0.29621 1.00000 0.05344 0.03315 0.00123 0.00072 0.00072 0.00000 0.00373 N11 0.71964 0.35384 0.37052 1.00000 0.04614 0.03085 0.00114 0.00067 0.00066 0.00000 0.00338 N12 0.72012 0.43851 0.48377 1.00000 0.05192 0.03264 0.00120 0.00071 0.00071 0.00000 0.00368 C37 0.71994 0.47809 0.18281 1.00000 0.06716 0.04778 0.00174 0.00104 0.00102 0.00000 0.00547 C48 0.82557 0.58843 0.18979 1.00000 0.04827 0.03952 0.00144 0.00086 0.00084 0.00000 0.00419 C42 0.65236 0.70765 0.30952 1.00000 0.06655 0.04737 0.00173 0.00103 0.00101 0.00000 0.00544 C30 0.64973 0.29058 0.31698 1.00000 0.08067 0.05368 0.00198 0.00116 0.00115 0.00000 0.00647 C34 0.78921 0.51150 0.50539 1.00000 0.04907 0.03934 0.00144 0.00086 0.00085 0.00000 0.00427 C38 0.61064 0.54800 0.14216 1.00000 0.05928 0.04406 0.00162 0.00096 0.00094 0.00000 0.00490 C43 0.68086 0.66618 0.40907 1.00000 0.05096 0.04019 0.00147 0.00087 0.00086 0.00000 0.00438 C36 0.56105 0.35707 0.49682 1.00000 0.05257 0.04121 0.00151 0.00089 0.00089 0.00000 0.00448 C25 0.39592 0.38476 0.43249 1.00000 0.05396 0.04155 0.00153 0.00090 0.00089 0.00000 0.00457 C39 0.56778 0.60740 0.17014 1.00000 0.05179 0.04063 0.00149 0.00089 0.00088 0.00000 0.00442 C47 0.92154 0.60126 0.25162 1.00000 0.06221 0.04482 0.00165 0.00096 0.00096 0.00000 0.00517 C29 0.56605 0.31017 0.26849 1.00000 0.05881 0.04357 0.00161 0.00095 0.00094 0.00000 0.00489 C35 0.64653 0.42483 0.52604 1.00000 0.05500 0.04214 0.00155 0.00092 0.00090 0.00000 0.00464 C45 0.90956 0.69584 0.32812 1.00000 0.06295 0.04573 0.00168 0.00099 0.00098 0.00000 0.00518 C27 0.40073 0.28983 0.31709 1.00000 0.06554 0.04677 0.00172 0.00101 0.00101 0.00000 0.00536 C33 0.80460 0.39811 0.49173 1.00000 0.06806 0.04794 0.00177 0.00104 0.00103 0.00000 0.00553 C40 0.44124 0.54721 0.22461 1.00000 0.07309 0.05003 0.00184 0.00108 0.00107 0.00000 0.00591 C44 0.84675 0.71089 0.37579 1.00000 0.06030 0.04459 0.00164 0.00096 0.00095 0.00000 0.00499 C32 0.76664 0.33653 0.43593 1.00000 0.06461 0.04631 0.00170 0.00101 0.00100 0.00000 0.00528 C31 0.82698 0.39166 0.35162 1.00000 0.06471 0.04640 0.00170 0.00100 0.00099 0.00000 0.00530 C28 0.42807 0.37293 0.24523 1.00000 0.07304 0.04979 0.00183 0.00108 0.00107 0.00000 0.00589 C46 0.95373 0.60047 0.36617 1.00000 0.06873 0.04781 0.00176 0.00103 0.00103 0.00000 0.00560 C26 0.44206 0.28695 0.38785 1.00000 0.06629 0.04706 0.00172 0.00102 0.00102 0.00000 0.00540 C41 0.54208 0.66322 0.26730 1.00000 0.07260 0.04999 0.00183 0.00108 0.00107 0.00000 0.00584 C50 -0.02326 0.43431 0.22951 1.00000 0.07467 0.05290 0.00193 0.00111 0.00117 0.00000 0.00601 C51 0.06353 0.44263 0.28169 1.00000 0.13321 0.08125 0.00309 0.00170 0.00172 0.00000 0.01118 C53 0.13353 0.48384 0.20678 1.00000 0.16586 0.09878 0.00365 0.00210 0.00212 0.00000 0.01463 C52 0.17575 0.45424 0.26133 1.00000 0.18497 0.10542 0.00393 0.00229 0.00234 0.00000 0.01675 P6 0.66823 -0.00069 0.49868 1.00000 0.02689 0.00814 0.00030 0.00018 0.00017 0.00000 0.00080 F90 0.83123 0.00118 0.50051 1.00000 -0.01137 0.00958 0.00035 0.00021 0.00021 0.00000 0.00087 F91 0.46865 -0.02343 0.44927 1.00000 0.02887 0.01672 0.00061 0.00036 0.00036 0.00000 0.00173 F99 1.03118 0.05038 0.52239 1.00000 0.04439 0.01983 0.00073 0.00043 0.00042 0.00000 0.00217 F86 0.24041 0.41347 -0.03166 1.00000 0.06978 0.02531 0.00093 0.00055 0.00054 0.00000 0.00300 F85 0.25939 0.53072 0.08582 1.00000 0.06932 0.02517 0.00093 0.00054 0.00054 0.00000 0.00299 F84 0.34118 0.45245 0.07622 1.00000 0.13535 0.04167 0.00152 0.00090 0.00088 0.00000 0.00585 F83 0.15731 0.42380 0.04816 1.00000 0.12902 0.03962 0.00145 0.00085 0.00085 0.00000 0.00553 F82 0.13893 0.48333 -0.01789 1.00000 0.17496 0.05250 0.00191 0.00111 0.00111 0.00000 0.00800 F81 0.36786 0.51662 0.02033 1.00000 0.16952 0.05129 0.00187 0.00108 0.00108 0.00000 0.00770 F93 0.72769 0.09805 0.46477 1.00000 0.20392 0.05889 0.00216 0.00127 0.00126 0.00000 0.00968 Final Structure Factor Calculation for char360a in P-1 Total number of l.s. parameters = 469 Maximum vector length = 511 Memory required = 6682 / 26061 wR2 = 0.4819 before cycle 21 for 26094 data and 0 / 469 parameters GooF = S = 1.958; Restrained GooF = 1.958 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.2015 for 11472 Fo > 4sig(Fo) and 0.3189 for all 26094 data wR2 = 0.4819, GooF = S = 1.958, Restrained GooF = 1.958 for all data Occupancy sum of asymmetric unit = 117.00 for non-hydrogen and 0.00 for hydrogen atoms Principal mean square atomic displacements U -0.0114 -0.0114 -0.0114 F90 ** NON POSITIVE DEFINITE ** Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.011 0.016 0.022 0.029 0.037 0.048 0.064 0.094 1.000 Number in group 3090. 2536. 2329. 2575. 2653. 2581. 2588. 2588. 2544. 2610. GooF 1.287 1.492 1.606 1.436 1.551 1.847 2.110 2.336 2.441 2.899 K 23.485 5.377 2.921 1.714 1.377 1.315 1.178 1.157 1.104 1.043 Resolution(A) 0.75 0.78 0.81 0.85 0.89 0.95 1.02 1.12 1.29 1.62 inf Number in group 2607. 2717. 2539. 2571. 2633. 2631. 2555. 2639. 2584. 2618. GooF 0.880 0.908 0.947 1.085 1.269 1.434 1.651 1.960 2.528 4.245 K 0.924 1.105 1.025 1.054 1.127 1.151 1.166 1.156 1.138 1.085 R1 0.546 0.498 0.462 0.394 0.344 0.293 0.247 0.216 0.188 0.214 Recommended weighting scheme: WGHT 0.2000 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 2 1 25236.74 834.68 11.16 0.051 8.40 0 0 5 6499.73 69.48 9.49 0.015 4.06 -2 3 1 13578.25 654.37 9.45 0.045 5.17 0 -4 1 8070.52 489.05 9.30 0.039 5.19 0 5 0 6963.89 361.72 8.15 0.033 4.06 -2 1 5 5136.10 56.71 7.97 0.013 3.82 -1 1 5 9595.21 1309.90 7.86 0.063 4.05 0 -1 1 -6.84 3071.46 7.75 0.097 16.15 0 1 6 3885.47 54.19 7.74 0.013 3.23 0 1 0 0.05 7980.77 7.73 0.156 20.31 0 -2 1 173.17 27861.84 7.65 0.292 9.96 0 -1 2 118.88 18476.84 7.65 0.238 9.96 -2 1 0 269.50 28728.58 7.62 0.296 6.06 -2 0 1 330.76 22664.10 7.54 0.263 6.06 -3 6 2 7062.72 900.20 7.49 0.052 2.92 1 -2 1 3438.50 348.79 7.49 0.033 8.14 2 0 1 26.96 3503.15 7.46 0.103 5.20 -2 5 1 5011.27 577.51 7.39 0.042 3.82 0 1 1 1762.40 59422.32 7.39 0.426 13.05 -3 -4 1 5792.19 411.70 7.36 0.035 2.82 -2 3 4 11719.82 2227.97 7.34 0.083 3.83 2 -3 1 23334.29 5487.37 7.29 0.130 4.93 -5 2 8 4818.17 146.76 7.07 0.021 2.02 -1 -2 1 8099.86 1619.71 6.96 0.070 7.08 -1 4 2 2873.56 58.96 6.93 0.013 4.50 0 3 3 448.00 6716.27 6.75 0.143 4.35 -7 -3 27 13703.30 189.59 6.69 0.024 0.78 -2 2 8 3765.83 77.04 6.57 0.015 2.48 -2 -4 8 12267.32 2782.88 6.56 0.092 2.42 -2 1 2 1080.22 10923.28 6.54 0.183 5.85 -1 2 6 3237.15 12.98 6.50 0.006 3.21 -5 8 3 4872.11 655.03 6.42 0.045 1.99 -3 3 7 8580.25 1691.00 6.39 0.072 2.54 -1 2 4 3485.97 212.82 6.33 0.026 4.50 0 0 2 1139.37 9043.73 6.33 0.166 10.15 -2 -1 3 22605.00 6760.93 6.30 0.144 4.94 -3 0 7 31495.03 9155.14 6.29 0.167 2.73 0 -3 4 583.04 5205.71 6.26 0.126 4.55 3 -1 4 6682.53 1205.83 6.25 0.061 2.82 -2 0 5 3579.46 343.92 6.18 0.032 3.90 2 -2 7 2107.36 52.72 6.07 0.013 2.44 0 4 3 28230.59 8747.24 6.04 0.164 3.71 0 0 1 158.05 1438.14 6.03 0.066 20.31 -1 -8 3 5181.51 864.19 6.03 0.051 2.41 2 -1 4 4116.45 749.74 6.00 0.048 3.50 3 5 0 4191.81 386.55 5.94 0.034 2.47 3 7 0 3650.99 55.27 5.90 0.013 2.06 1 6 2 3638.30 62.78 5.88 0.014 2.71 3 4 0 6497.93 1309.75 5.86 0.063 2.72 3 -5 2 2633.53 33.67 5.80 0.010 3.09 Bond lengths and angles Ni4 - Distance Angles N14 2.0679 (0.0129) N15 2.1011 (0.0141) 85.52 (0.52) N16 2.0976 (0.0130) 146.47 (0.51) 84.08 (0.52) N13 2.1139 (0.0124) 84.97 (0.49) 145.88 (0.51) 86.01 (0.49) S3 2.2534 (0.0045) 109.55 (0.37) 108.63 (0.39) 103.98 (0.38) 105.44 (0.36) Ni4 - N14 N15 N16 N13 Ni3 - Distance Angles N9 2.0714 (0.0133) N11 2.1155 (0.0135) 108.17 (0.53) N12 2.1621 (0.0146) 82.80 (0.53) 82.36 (0.53) N10 2.1761 (0.0149) 83.26 (0.54) 83.16 (0.53) 155.65 (0.55) S4 2.3067 (0.0044) 99.01 (0.39) 152.75 (0.39) 99.43 (0.40) 102.40 (0.41) S3 2.4264 (0.0046) 150.74 (0.39) 101.09 (0.38) 101.79 (0.40) 100.14 (0.40) 51.77 (0.14) Ni3 - N9 N11 N12 N10 S4 S3 - Distance Angles S4 2.0693 (0.0055) Ni4 2.2534 (0.0045) 113.24 (0.22) Ni3 2.4264 (0.0045) 61.13 (0.16) 172.04 (0.21) S3 - S4 Ni4 S4 - Distance Angles S3 2.0693 (0.0056) Ni3 2.3067 (0.0044) 67.10 (0.17) S4 - S3 Ni2 - Distance Angles N8 2.0832 (0.0129) N7 2.0823 (0.0134) 86.31 (0.51) N6 2.1127 (0.0120) 147.51 (0.48) 84.00 (0.49) N5 2.1217 (0.0121) 86.15 (0.49) 146.08 (0.49) 84.84 (0.46) S1 2.2601 (0.0045) 109.26 (0.38) 108.13 (0.39) 103.23 (0.34) 105.58 (0.34) Ni2 - N8 N7 N6 N5 Ni1 - Distance Angles N1 2.0772 (0.0150) N3 2.0932 (0.0135) 107.88 (0.56) N2 2.1972 (0.0152) 84.50 (0.57) 81.91 (0.54) N4 2.1730 (0.0151) 81.98 (0.58) 83.48 (0.54) 155.98 (0.54) S2 2.3067 (0.0043) 98.54 (0.43) 153.54 (0.40) 99.64 (0.40) 101.94 (0.40) S1 2.4205 (0.0045) 150.11 (0.43) 101.97 (0.39) 101.54 (0.40) 100.07 (0.40) 51.69 (0.14) Ni1 - N1 N3 N2 N4 S2 S1 - Distance Angles S2 2.0633 (0.0056) Ni2 2.2601 (0.0045) 113.28 (0.21) Ni1 2.4205 (0.0045) 61.31 (0.16) 172.04 (0.20) S1 - S2 Ni2 S2 - Distance Angles S1 2.0633 (0.0056) Ni1 2.3067 (0.0043) 67.00 (0.16) S2 - S1 P2 - Distance Angles F8 1.5430 (0.0171) F10 1.5439 (0.0148) 87.27 (0.85) F11 1.5383 (0.0147) 174.24 (0.89) 93.44 (0.79) F7 1.5363 (0.0144) 90.77 (0.84) 177.01 (0.84) 88.29 (0.78) F12 1.5788 (0.0165) 91.08 (0.88) 89.67 (0.83) 83.21 (0.81) 88.11 (0.81) F9 1.5781 (0.0229) 92.82 (1.03) 89.01 (0.99) 92.91 (1.01) 93.35 (1.01) 175.83 (1.03) P2 - F8 F10 F11 F7 F12 P3 - Distance Angles F82 1.5615 (0.0223) F81 1.5831 (0.0215) 115.55 (1.15) F83 1.5789 (0.0171) 81.00 (1.01) 163.44 (1.05) F85 1.5926 (0.0119) 93.01 (0.95) 88.40 (0.92) 90.70 (0.78) F84 1.5548 (0.0180) 166.94 (1.09) 77.50 (1.00) 85.94 (0.91) 87.40 (0.81) F86 1.6257 (0.0120) 88.06 (0.95) 92.86 (0.91) 87.58 (0.77) 177.81 (0.64) 91.12 (0.81) P3 - F82 F81 F83 F85 F84 P4 -                                                                                                                                                                                                                                                                     $                                                                                                                                                                                                                                                                                                                               !                                                              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