# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Euan Brechin' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Anna Collins' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Georgios Karotsis' '' '' 'Giannis S. Papaefstahiou' '' '' 'Simon Parsons' '' '' 'Alexandra Slawin' '' '' 'Constantinos C. Stoumpos' '' '' 'Fraser White' '' '' _publ_contact_author_name 'Euan Brechin' _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK _publ_section_title ; Molecular and supramolecular Ni(II) wheels from ?-benzoin oxime ; _publ_contact_author_address ; Department of Chemistry, Joseph Black Building, West Mains Road, University of Edinburgh, Edinburgh, EH9 3JJ, UK. ; _publ_contact_author_phone '+44 131 650 4806' _publ_contact_letter ; ; # Attachment 'Ni6.cif' data_EB8078 _database_code_depnum_ccdc_archive 'CCDC 718774' _audit_creation_date 08-04-22 _audit_creation_method CRYSTALS_ver_12.85 _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C116 H100 N8 Ni6 O20, 2(C4 H10 O)' _chemical_compound_source 'Giorgos Karotsis, GK1082' _exptl_crystal_recrystallization_method ; Et~2~O diffusion into MeOH solution. ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. Checkcif alerts 912_ALERT_3_A # Missing FCF Reflections Above STh/L= 0.600 1923 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 3 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 9 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 4 The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 5741 5737 4 23.01 0.550 0.999 7634 7629 5 25.24 0.600 0.999 9920 9908 12 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.996 12608 12562 46 29.84 0.700 0.922 15705 14481 1224 30.54 0.715 0.884 16672 14737 1935 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.21 Ratio 420_ALERT_2_B D-H Without Acceptor O8 - H81 ... ? 420_ALERT_2_B D-H Without Acceptor O74 - H741 ... ? All H atoms were located in a difference map. There are no peaks in the Fourier difference map at suitable positions for H atoms on these O atoms that are positioned along probable H bonds. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.77 154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 200 Deg. Checked 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C77 No action taken. The Et~2~O group is surprisingly well ordered, but no restraints have been applied to the adps. 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 8 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C4 H10 O The position has been chosen for proximity to the rest of the molecule as the asymmeytric unit is displayed in Crystals. 793_ALERT_1_G Check the Absolute Configuration of C22 = ... S 793_ALERT_1_G Check the Absolute Configuration of C39 = ... R 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 12 Least squares restraints were applied to C atoms in one of the Ph groups. U(IJ)'S 0.0, 0.001000 = C(29) TO C(30) U(IJ)'S 0.0, 0.010000 = C(27) TO C(28) ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 11.6358(4) _cell_length_b 16.1748(5) _cell_length_c 17.3392(6) _cell_angle_alpha 112.085(2) _cell_angle_beta 105.280(2) _cell_angle_gamma 101.909(2) _cell_volume 2741.43(18) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C124 H120 N8 Ni6 O22 # Dc = 1.47 Fooo = 1264.00 Mu = 10.87 M = 1213.31 # Found Formula = C124 H120 N8 Ni6 O22 # Dc = 1.47 FOOO = 1264.00 Mu = 10.87 M = 1213.31 _chemical_formula_sum 'C124 H120 N8 Ni6 O22' _chemical_formula_weight 2426.62 _cell_measurement_reflns_used 7641 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_min 0.21 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.23 _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.087 # Sheldrick geometric approximatio 0.79 0.80 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.80 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 32324 _reflns_number_total 14737 _diffrn_reflns_av_R_equivalents 0.059 # Number of reflections with Friedels Law is 14737 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 16792 _diffrn_reflns_theta_min 1.900 _diffrn_reflns_theta_max 30.543 _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 27.489 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min -22 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 1.32 _oxford_diffrn_Wilson_scale 19.56 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.10 _refine_diff_density_max 1.84 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 14734 _refine_ls_number_restraints 12 _refine_ls_number_parameters 721 _oxford_refine_ls_R_factor_ref 0.1162 _refine_ls_wR_factor_ref 0.1722 _refine_ls_goodness_of_fit_ref 0.9522 _refine_ls_shift/su_max 0.000578 # The values computed from all data _oxford_reflns_number_all 14734 _refine_ls_R_factor_all 0.1162 _refine_ls_wR_factor_all 0.1722 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9397 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_gt 0.1526 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.06P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ni1 Ni 0.60596(5) 0.42253(4) 0.20112(3) 0.0196 1.0000 Uani . . . . . . . Ni2 Ni 0.41127(5) 0.46072(4) 0.05748(3) 0.0181 1.0000 Uani . . . . . . . Ni3 Ni 0.23313(5) 0.51323(4) -0.08116(3) 0.0190 1.0000 Uani . . . . . . . O4 O 0.5241(3) 0.4936(2) 0.28314(18) 0.0235 1.0000 Uani . . . . . . . C5 C 0.5951(4) 0.5417(3) 0.3646(3) 0.0228 1.0000 Uani . . . . . . . C6 C 0.7303(4) 0.5549(3) 0.3901(3) 0.0248 1.0000 Uani . . . . . . . N7 N 0.7560(4) 0.5024(3) 0.3210(2) 0.0258 1.0000 Uani . . . . . . . O8 O 0.8716(3) 0.5103(3) 0.3305(2) 0.0338 1.0000 Uani . . . . . . . C9 C 0.5338(4) 0.5797(3) 0.4286(3) 0.0256 1.0000 Uani . . . . . . . C10 C 0.4112(5) 0.5780(3) 0.3925(3) 0.0318 1.0000 Uani . . . . . . . C11 C 0.3422(5) 0.6040(4) 0.4469(3) 0.0379 1.0000 Uani . . . . . . . C12 C 0.3952(5) 0.6307(4) 0.5371(3) 0.0358 1.0000 Uani . . . . . . . C13 C 0.5169(5) 0.6330(4) 0.5739(3) 0.0372 1.0000 Uani . . . . . . . C14 C 0.5868(5) 0.6075(3) 0.5205(3) 0.0281 1.0000 Uani . . . . . . . C15 C 0.8328(5) 0.6237(4) 0.4781(3) 0.0365 1.0000 Uani . . . . . . . C16 C 0.8507(5) 0.7187(4) 0.5099(3) 0.0443 1.0000 Uani . . . . . . . C17 C 0.9521(7) 0.7850(5) 0.5899(4) 0.0693 1.0000 Uani . . . . . . . C18 C 1.0328(6) 0.7524(7) 0.6356(4) 0.0837 1.0000 Uani . . . . . . . C19 C 1.0141(7) 0.6577(7) 0.6049(4) 0.0815 1.0000 Uani . . . . . . . C20 C 0.9154(6) 0.5937(5) 0.5259(4) 0.0537 1.0000 Uani . . . . . . . O21 O 0.4465(3) 0.3696(2) 0.08795(19) 0.0226 1.0000 Uani . . . . . . . C22 C 0.3387(4) 0.2871(3) 0.0520(3) 0.0214 1.0000 Uani . . . . . . . C23 C 0.2378(4) 0.2843(3) -0.0269(3) 0.0213 1.0000 Uani . . . . . . . N24 N 0.2587(3) 0.3677(2) -0.0261(2) 0.0191 1.0000 Uani . . . . . . . O25 O 0.1804(3) 0.3830(2) -0.08611(19) 0.0237 1.0000 Uani . . . . . . . C26 C 0.2841(4) 0.2831(3) 0.1213(3) 0.0279 1.0000 Uani . . . . . . . C27 C 0.2798(5) 0.2104(4) 0.1453(3) 0.0358 1.0000 Uani . U . . . . . C28 C 0.2286(5) 0.2066(5) 0.2083(4) 0.0524 1.0000 Uani . U . . . . . C29 C 0.1811(5) 0.2762(5) 0.2472(3) 0.0526 1.0000 Uani . U . . . . . C30 C 0.1864(5) 0.3507(5) 0.2248(3) 0.0530 1.0000 Uani . U . . . . . C31 C 0.2366(5) 0.3527(4) 0.1614(3) 0.0345 1.0000 Uani . . . . . . . C32 C 0.1346(4) 0.1949(3) -0.0930(3) 0.0228 1.0000 Uani . . . . . . . C33 C 0.1373(5) 0.1099(3) -0.0889(3) 0.0315 1.0000 Uani . . . . . . . C34 C 0.0456(5) 0.0232(3) -0.1522(3) 0.0354 1.0000 Uani . . . . . . . C35 C -0.0497(5) 0.0187(3) -0.2221(3) 0.0354 1.0000 Uani . . . . . . . C36 C -0.0559(4) 0.1006(3) -0.2276(3) 0.0287 1.0000 Uani . . . . . . . C37 C 0.0343(4) 0.1880(3) -0.1634(3) 0.0275 1.0000 Uani . . . . . . . O38 O 0.6261(3) 0.4430(2) -0.03760(18) 0.0215 1.0000 Uani . . . . . . . C39 C 0.5354(4) 0.3512(3) -0.0996(2) 0.0197 1.0000 Uani . . . . . . . C40 C 0.4177(4) 0.3613(3) -0.1512(3) 0.0198 1.0000 Uani . . . . . . . N41 N 0.4311(3) 0.4494(2) -0.1316(2) 0.0185 1.0000 Uani . . . . . . . O42 O 0.3334(3) 0.4750(2) -0.16490(18) 0.0221 1.0000 Uani . . . . . . . C43 C 0.5920(4) 0.2958(3) -0.1625(3) 0.0222 1.0000 Uani . . . . . . . C44 C 0.6450(5) 0.2318(3) -0.1471(3) 0.0299 1.0000 Uani . . . . . . . C45 C 0.6952(5) 0.1804(4) -0.2054(3) 0.0367 1.0000 Uani . . . . . . . C46 C 0.6919(5) 0.1932(4) -0.2811(3) 0.0383 1.0000 Uani . . . . . . . C47 C 0.6415(5) 0.2579(4) -0.2952(3) 0.0388 1.0000 Uani . . . . . . . C48 C 0.5923(5) 0.3098(3) -0.2377(3) 0.0291 1.0000 Uani . . . . . . . C49 C 0.3061(4) 0.2769(3) -0.2202(3) 0.0211 1.0000 Uani . . . . . . . C50 C 0.2976(4) 0.1882(3) -0.2242(3) 0.0255 1.0000 Uani . . . . . . . C51 C 0.1987(4) 0.1071(3) -0.2909(3) 0.0301 1.0000 Uani . . . . . . . C52 C 0.1079(5) 0.1126(3) -0.3561(3) 0.0324 1.0000 Uani . . . . . . . C53 C 0.1153(5) 0.1995(3) -0.3539(3) 0.0317 1.0000 Uani . . . . . . . C54 C 0.2126(4) 0.2814(3) -0.2869(3) 0.0275 1.0000 Uani . . . . . . . O55 O 0.4252(3) 0.6914(2) -0.23157(19) 0.0248 1.0000 Uani . . . . . . . C56 C 0.3814(4) 0.7528(3) -0.1947(3) 0.0256 1.0000 Uani . . . . . . . C57 C 0.3236(4) 0.7422(3) -0.1316(3) 0.0195 1.0000 Uani . . . . . . . N58 N 0.3168(3) 0.6610(2) -0.1289(2) 0.0213 1.0000 Uani . . . . . . . O59 O 0.2717(3) 0.6447(2) -0.07295(18) 0.0231 1.0000 Uani . . . . . . . C60 C 0.3939(4) 0.8349(3) -0.2153(3) 0.0245 1.0000 Uani . . . . . . . C61 C 0.4671(5) 0.8424(4) -0.2657(3) 0.0343 1.0000 Uani . . . . . . . C62 C 0.4854(6) 0.9183(4) -0.2859(3) 0.0414 1.0000 Uani . . . . . . . C63 C 0.4346(6) 0.9876(4) -0.2554(4) 0.0429 1.0000 Uani . . . . . . . C64 C 0.3614(5) 0.9807(4) -0.2057(4) 0.0407 1.0000 Uani . . . . . . . C65 C 0.3401(5) 0.9046(4) -0.1863(3) 0.0331 1.0000 Uani . . . . . . . C66 C 0.2760(4) 0.8095(3) -0.0751(3) 0.0233 1.0000 Uani . . . . . . . C67 C 0.1477(5) 0.7879(3) -0.0948(3) 0.0326 1.0000 Uani . . . . . . . C68 C 0.1011(5) 0.8500(4) -0.0423(4) 0.0399 1.0000 Uani . . . . . . . C69 C 0.1830(6) 0.9336(4) 0.0296(3) 0.0436 1.0000 Uani . . . . . . . C70 C 0.3106(6) 0.9559(4) 0.0512(4) 0.0445 1.0000 Uani . . . . . . . C71 C 0.3586(5) 0.8940(3) -0.0008(3) 0.0335 1.0000 Uani . . . . . . . O72 O 0.0780(3) 0.4749(2) -0.1951(2) 0.0260 1.0000 Uani . . . . . . . C73 C -0.0323(5) 0.3940(4) -0.2314(4) 0.0448 1.0000 Uani . . . . . . . O74 O 0.1217(3) 0.5574(2) -0.0041(2) 0.0292 1.0000 Uani . . . . . . . C75 C 0.0468(5) 0.6144(4) -0.0173(4) 0.0403 1.0000 Uani . . . . . . . O76 O 1.2892(6) 0.9594(4) 0.4783(3) 0.0927 1.0000 Uani . . . . . . . C77 C 1.2256(7) 0.9146(6) 0.5191(4) 0.0697 1.0000 Uani . . . . . . . C78 C 1.2216(7) 0.8141(6) 0.4867(5) 0.0783 1.0000 Uani . . . . . . . C79 C 1.3111(9) 1.0562(6) 0.5108(6) 0.0948 1.0000 Uani . . . . . . . C80 C 1.3749(9) 1.0962(7) 0.4652(6) 0.1148 1.0000 Uani . . . . . . . H101 H 0.3741 0.5598 0.3315 0.0390 1.0000 Uiso R . . . . . . H111 H 0.2604 0.6034 0.4225 0.0479 1.0000 Uiso R . . . . . . H121 H 0.3492 0.6480 0.5720 0.0441 1.0000 Uiso R . . . . . . H131 H 0.5534 0.6521 0.6347 0.0447 1.0000 Uiso R . . . . . . H141 H 0.6686 0.6084 0.5457 0.0346 1.0000 Uiso R . . . . . . H161 H 0.7965 0.7406 0.4797 0.0447 1.0000 Uiso R . . . . . . H171 H 0.9645 0.8492 0.6117 0.0660 1.0000 Uiso R . . . . . . H181 H 1.1015 0.7960 0.6878 0.0803 1.0000 Uiso R . . . . . . H191 H 1.0665 0.6363 0.6359 0.0840 1.0000 Uiso R . . . . . . H201 H 0.9040 0.5300 0.5040 0.0649 1.0000 Uiso R . . . . . . H221 H 0.3708 0.2361 0.0273 0.0355 1.0000 Uiso R . . . . . . H271 H 0.3118 0.1636 0.1184 0.0437 1.0000 Uiso R . . . . . . H281 H 0.2279 0.1578 0.2239 0.0630 1.0000 Uiso R . . . . . . H291 H 0.1451 0.2733 0.2875 0.0651 1.0000 Uiso R . . . . . . H301 H 0.1566 0.3993 0.2522 0.0518 1.0000 Uiso R . . . . . . H311 H 0.2411 0.4030 0.1468 0.0388 1.0000 Uiso R . . . . . . H331 H 0.2028 0.1121 -0.0424 0.0369 1.0000 Uiso R . . . . . . H341 H 0.0497 -0.0305 -0.1466 0.0442 1.0000 Uiso R . . . . . . H351 H -0.1110 -0.0396 -0.2658 0.0380 1.0000 Uiso R . . . . . . H361 H -0.1225 0.0970 -0.2745 0.0320 1.0000 Uiso R . . . . . . H371 H 0.0288 0.2430 -0.1675 0.0320 1.0000 Uiso R . . . . . . H391 H 0.5134 0.3241 -0.0629 0.0300 1.0000 Uiso R . . . . . . H441 H 0.6488 0.2242 -0.0965 0.0416 1.0000 Uiso R . . . . . . H451 H 0.7321 0.1377 -0.1947 0.0518 1.0000 Uiso R . . . . . . H461 H 0.7232 0.1576 -0.3220 0.0496 1.0000 Uiso R . . . . . . H471 H 0.6394 0.2664 -0.3455 0.0513 1.0000 Uiso R . . . . . . H481 H 0.5585 0.3536 -0.2483 0.0389 1.0000 Uiso R . . . . . . H501 H 0.3614 0.1842 -0.1814 0.0319 1.0000 Uiso R . . . . . . H511 H 0.1960 0.0489 -0.2913 0.0372 1.0000 Uiso R . . . . . . H521 H 0.0408 0.0586 -0.3999 0.0330 1.0000 Uiso R . . . . . . H531 H 0.0532 0.2033 -0.3974 0.0365 1.0000 Uiso R . . . . . . H541 H 0.2136 0.3390 -0.2866 0.0322 1.0000 Uiso R . . . . . . H611 H 0.5050 0.7979 -0.2844 0.0435 1.0000 Uiso R . . . . . . H621 H 0.5337 0.9222 -0.3198 0.0538 1.0000 Uiso R . . . . . . H631 H 0.4494 1.0393 -0.2683 0.0548 1.0000 Uiso R . . . . . . H641 H 0.3251 1.0274 -0.1850 0.0521 1.0000 Uiso R . . . . . . H651 H 0.2892 0.9004 -0.1533 0.0434 1.0000 Uiso R . . . . . . H671 H 0.0922 0.7309 -0.1442 0.0404 1.0000 Uiso R . . . . . . H681 H 0.0128 0.8356 -0.0568 0.0546 1.0000 Uiso R . . . . . . H691 H 0.1517 0.9758 0.0635 0.0589 1.0000 Uiso R . . . . . . H701 H 0.3660 1.0124 0.1004 0.0490 1.0000 Uiso R . . . . . . H711 H 0.4454 0.9095 0.0131 0.0372 1.0000 Uiso R . . . . . . H772 H 1.2719 0.9497 0.5851 0.0802 1.0000 Uiso R . . . . . . H771 H 1.1372 0.9154 0.5038 0.0801 1.0000 Uiso R . . . . . . H781 H 1.1800 0.7849 0.5168 0.1203 1.0000 Uiso R . . . . . . H782 H 1.3084 0.8127 0.4998 0.1199 1.0000 Uiso R . . . . . . H783 H 1.1735 0.7796 0.4219 0.1201 1.0000 Uiso R . . . . . . H791 H 1.3638 1.0882 0.5740 0.1021 1.0000 Uiso R . . . . . . H792 H 1.2282 1.0653 0.5009 0.1022 1.0000 Uiso R . . . . . . H802 H 1.3972 1.1635 0.4937 0.1549 1.0000 Uiso R . . . . . . H801 H 1.4490 1.0779 0.4687 0.1550 1.0000 Uiso R . . . . . . H803 H 1.3190 1.0699 0.4041 0.1548 1.0000 Uiso R . . . . . . H752 H 0.1022 0.6775 0.0003 0.0720 1.0000 Uiso R . . . . . . H741 H 0.1809 0.5900 0.0451 0.0535 1.0000 Uiso R . . . . . . H732 H -0.0149 0.3388 -0.2649 0.0580 1.0000 Uiso R . . . . . . H733 H -0.0532 0.3903 -0.1827 0.0580 1.0000 Uiso R . . . . . . H753 H -0.0057 0.6174 0.0175 0.0722 1.0000 Uiso R . . . . . . H731 H -0.0988 0.4032 -0.2700 0.0584 1.0000 Uiso R . . . . . . H751 H -0.0063 0.5841 -0.0801 0.0722 1.0000 Uiso R . . . . . . H81 H 0.9177 0.5332 0.3826 0.0558 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0284(3) 0.0200(3) 0.0167(2) 0.0115(2) 0.0120(2) 0.0095(2) Ni2 0.0253(3) 0.0158(3) 0.0160(2) 0.0091(2) 0.0095(2) 0.0066(2) Ni3 0.0258(3) 0.0180(3) 0.0169(2) 0.0102(2) 0.0100(2) 0.0077(2) O4 0.0313(17) 0.0235(15) 0.0185(13) 0.0109(12) 0.0109(13) 0.0101(13) C5 0.032(2) 0.023(2) 0.0196(19) 0.0133(17) 0.0134(18) 0.0092(18) C6 0.028(2) 0.032(2) 0.022(2) 0.0176(18) 0.0136(18) 0.012(2) N7 0.030(2) 0.029(2) 0.0250(18) 0.0179(16) 0.0119(16) 0.0118(17) O8 0.0293(18) 0.057(2) 0.0202(15) 0.0209(16) 0.0109(14) 0.0168(17) C9 0.031(2) 0.027(2) 0.0188(19) 0.0105(17) 0.0104(18) 0.0095(19) C10 0.046(3) 0.031(3) 0.022(2) 0.0131(19) 0.016(2) 0.012(2) C11 0.039(3) 0.045(3) 0.036(3) 0.017(2) 0.023(2) 0.019(2) C12 0.042(3) 0.037(3) 0.031(2) 0.010(2) 0.024(2) 0.016(2) C13 0.054(3) 0.035(3) 0.025(2) 0.011(2) 0.023(2) 0.014(2) C14 0.034(3) 0.028(2) 0.025(2) 0.0138(18) 0.0147(19) 0.008(2) C15 0.030(3) 0.052(3) 0.021(2) 0.011(2) 0.013(2) 0.005(2) C16 0.046(3) 0.043(3) 0.024(2) 0.005(2) 0.017(2) -0.008(3) C17 0.067(5) 0.068(5) 0.030(3) -0.006(3) 0.027(3) -0.017(4) C18 0.029(3) 0.137(8) 0.030(3) 0.008(4) 0.010(3) -0.015(4) C19 0.048(4) 0.140(8) 0.025(3) 0.012(4) 0.005(3) 0.031(5) C20 0.045(3) 0.089(5) 0.028(3) 0.020(3) 0.016(2) 0.034(3) O21 0.0305(16) 0.0182(14) 0.0233(14) 0.0123(12) 0.0130(13) 0.0076(13) C22 0.027(2) 0.022(2) 0.0209(19) 0.0131(17) 0.0125(17) 0.0092(18) C23 0.025(2) 0.022(2) 0.0202(19) 0.0103(16) 0.0118(17) 0.0081(17) N24 0.0256(18) 0.0183(17) 0.0173(15) 0.0117(13) 0.0101(14) 0.0050(14) O25 0.0296(17) 0.0201(15) 0.0202(14) 0.0095(12) 0.0078(13) 0.0077(13) C26 0.032(2) 0.030(2) 0.0163(19) 0.0124(17) 0.0044(18) 0.003(2) C27 0.039(3) 0.040(3) 0.030(2) 0.023(2) 0.014(2) 0.004(2) C28 0.048(3) 0.065(4) 0.037(3) 0.036(3) 0.009(2) -0.008(3) C29 0.039(2) 0.078(3) 0.0256(18) 0.020(2) 0.0148(17) -0.006(2) C30 0.039(2) 0.078(3) 0.0264(18) 0.019(2) 0.0144(17) -0.004(2) C31 0.030(3) 0.038(3) 0.026(2) 0.010(2) 0.011(2) 0.003(2) C32 0.032(2) 0.018(2) 0.0203(19) 0.0099(16) 0.0126(18) 0.0068(18) C33 0.043(3) 0.024(2) 0.026(2) 0.0131(19) 0.011(2) 0.007(2) C34 0.050(3) 0.025(2) 0.036(3) 0.018(2) 0.018(2) 0.010(2) C35 0.042(3) 0.024(2) 0.030(2) 0.007(2) 0.012(2) 0.003(2) C36 0.024(2) 0.030(2) 0.026(2) 0.0108(19) 0.0056(18) 0.0054(19) C37 0.028(2) 0.024(2) 0.028(2) 0.0132(19) 0.0082(19) 0.0061(19) O38 0.0303(16) 0.0153(14) 0.0180(13) 0.0077(11) 0.0077(12) 0.0074(12) C39 0.027(2) 0.019(2) 0.0149(17) 0.0088(15) 0.0090(16) 0.0073(17) C40 0.028(2) 0.022(2) 0.0165(17) 0.0101(16) 0.0156(17) 0.0101(17) N41 0.0271(18) 0.0205(17) 0.0142(15) 0.0083(13) 0.0121(14) 0.0139(15) O42 0.0296(16) 0.0221(15) 0.0195(13) 0.0122(12) 0.0119(12) 0.0099(13) C43 0.028(2) 0.021(2) 0.0189(18) 0.0094(16) 0.0131(17) 0.0056(17) C44 0.044(3) 0.029(2) 0.031(2) 0.019(2) 0.022(2) 0.021(2) C45 0.054(3) 0.035(3) 0.041(3) 0.022(2) 0.028(3) 0.031(3) C46 0.051(3) 0.039(3) 0.035(3) 0.014(2) 0.029(3) 0.023(3) C47 0.048(3) 0.051(3) 0.030(2) 0.021(2) 0.024(2) 0.024(3) C48 0.038(3) 0.034(3) 0.027(2) 0.019(2) 0.018(2) 0.019(2) C49 0.025(2) 0.021(2) 0.0200(19) 0.0090(16) 0.0101(17) 0.0099(17) C50 0.032(2) 0.024(2) 0.024(2) 0.0133(18) 0.0109(19) 0.0098(19) C51 0.033(3) 0.021(2) 0.038(3) 0.015(2) 0.013(2) 0.010(2) C52 0.034(3) 0.026(2) 0.024(2) 0.0053(18) 0.004(2) 0.006(2) C53 0.036(3) 0.032(3) 0.024(2) 0.015(2) 0.005(2) 0.008(2) C54 0.033(2) 0.023(2) 0.025(2) 0.0134(18) 0.0073(19) 0.0059(19) O55 0.0369(18) 0.0261(16) 0.0227(14) 0.0169(13) 0.0162(14) 0.0148(14) C56 0.032(2) 0.023(2) 0.0196(19) 0.0114(17) 0.0077(18) 0.0061(19) C57 0.025(2) 0.020(2) 0.0180(18) 0.0112(16) 0.0099(16) 0.0082(17) N58 0.030(2) 0.0218(18) 0.0152(15) 0.0124(14) 0.0098(14) 0.0067(15) O59 0.0371(18) 0.0230(15) 0.0186(13) 0.0137(12) 0.0170(13) 0.0115(13) C60 0.029(2) 0.023(2) 0.024(2) 0.0153(18) 0.0104(18) 0.0050(18) C61 0.052(3) 0.032(3) 0.027(2) 0.017(2) 0.021(2) 0.016(2) C62 0.059(4) 0.039(3) 0.038(3) 0.027(2) 0.026(3) 0.012(3) C63 0.058(4) 0.035(3) 0.045(3) 0.031(3) 0.018(3) 0.010(3) C64 0.050(3) 0.036(3) 0.045(3) 0.027(2) 0.016(3) 0.018(3) C65 0.041(3) 0.035(3) 0.033(2) 0.024(2) 0.013(2) 0.015(2) C66 0.034(2) 0.021(2) 0.025(2) 0.0168(17) 0.0155(19) 0.0122(19) C67 0.042(3) 0.025(2) 0.033(2) 0.015(2) 0.017(2) 0.010(2) C68 0.044(3) 0.043(3) 0.049(3) 0.024(3) 0.028(3) 0.025(3) C69 0.075(4) 0.041(3) 0.034(3) 0.020(2) 0.032(3) 0.036(3) C70 0.057(4) 0.033(3) 0.033(3) 0.005(2) 0.010(3) 0.021(3) C71 0.034(3) 0.029(3) 0.033(2) 0.013(2) 0.008(2) 0.012(2) O72 0.0254(16) 0.0288(17) 0.0249(15) 0.0144(13) 0.0096(13) 0.0067(13) C73 0.042(3) 0.044(3) 0.036(3) 0.019(2) 0.003(2) 0.005(3) O74 0.0416(19) 0.0295(17) 0.0296(16) 0.0192(14) 0.0216(15) 0.0157(15) C75 0.047(3) 0.043(3) 0.047(3) 0.025(3) 0.030(3) 0.021(3) O76 0.111(5) 0.071(4) 0.066(3) 0.001(3) 0.057(3) 0.001(3) C77 0.057(4) 0.099(6) 0.042(4) 0.024(4) 0.021(3) 0.021(4) C78 0.079(5) 0.092(6) 0.064(5) 0.023(4) 0.035(4) 0.042(5) C79 0.100(7) 0.088(7) 0.067(5) 0.012(5) 0.044(5) 0.003(5) C80 0.109(8) 0.128(9) 0.076(6) 0.024(6) 0.054(6) -0.002(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3133(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . O55 2_665 2.089(3) yes Ni1 . O42 2_665 2.042(3) yes Ni1 . N58 2_665 2.006(4) yes Ni1 . Ni2 . 3.2369(8) yes Ni1 . O4 . 2.046(3) yes Ni1 . N7 . 2.042(4) yes Ni1 . O21 . 2.046(3) yes Ni2 . Ni2 2_665 3.5838(10) yes Ni2 . N41 2_665 1.839(3) yes Ni2 . O38 2_665 1.826(3) yes Ni2 . Ni3 . 3.2300(8) yes Ni2 . O21 . 1.828(3) yes Ni2 . N24 . 1.848(3) yes Ni3 . O38 2_665 2.018(3) yes Ni3 . O25 . 2.031(3) yes Ni3 . O42 . 2.090(3) yes Ni3 . O59 . 2.022(3) yes Ni3 . O72 . 2.069(3) yes Ni3 . O74 . 2.134(3) yes O4 . C5 . 1.256(5) yes C5 . C6 . 1.462(6) yes C5 . C9 . 1.485(6) yes C6 . N7 . 1.333(5) yes C6 . C15 . 1.485(6) yes N7 . O8 . 1.284(5) yes O8 . H81 . 0.808 no C9 . C10 . 1.389(7) yes C9 . C14 . 1.397(6) yes C10 . C11 . 1.396(6) yes C10 . H101 . 0.930 no C11 . C12 . 1.374(7) yes C11 . H111 . 0.931 no C12 . C13 . 1.377(7) yes C12 . H121 . 0.915 no C13 . C14 . 1.391(6) yes C13 . H131 . 0.924 no C14 . H141 . 0.931 no C15 . C16 . 1.370(8) yes C15 . C20 . 1.386(8) yes C16 . C17 . 1.401(7) yes C16 . H161 . 0.925 no C17 . C18 . 1.384(12) yes C17 . H171 . 0.925 no C18 . C19 . 1.365(12) yes C18 . H181 . 0.928 no C19 . C20 . 1.372(8) yes C19 . H191 . 0.914 no C20 . H201 . 0.919 no O21 . C22 . 1.419(5) yes C22 . C23 . 1.529(6) yes C22 . C26 . 1.515(6) yes C22 . H221 . 0.975 no C23 . N24 . 1.314(5) yes C23 . C32 . 1.469(6) yes N24 . O25 . 1.327(4) yes C26 . C27 . 1.382(7) yes C26 . C31 . 1.388(7) yes C27 . C28 . 1.390(7) yes C27 . H271 . 0.933 no C28 . C29 . 1.382(9) yes C28 . H281 . 0.925 no C29 . C30 . 1.393(9) yes C29 . H291 . 0.916 no C30 . C31 . 1.382(7) yes C30 . H301 . 0.939 no C31 . H311 . 0.935 no C32 . C33 . 1.410(6) yes C32 . C37 . 1.399(6) yes C33 . C34 . 1.384(6) yes C33 . H331 . 0.936 no C34 . C35 . 1.376(7) yes C34 . H341 . 0.920 no C35 . C36 . 1.379(7) yes C35 . H351 . 0.933 no C36 . C37 . 1.388(6) yes C36 . H361 . 0.938 no C37 . H371 . 0.932 no O38 . C39 . 1.425(5) yes C39 . C40 . 1.503(6) yes C39 . C43 . 1.522(6) yes C39 . H391 . 0.955 no C40 . N41 . 1.299(5) yes C40 . C49 . 1.483(6) yes N41 . O42 . 1.352(4) yes C43 . C44 . 1.382(6) yes C43 . C48 . 1.404(6) yes C44 . C45 . 1.390(6) yes C44 . H441 . 0.922 no C45 . C46 . 1.395(7) yes C45 . H451 . 0.934 no C46 . C47 . 1.368(7) yes C46 . H461 . 0.940 no C47 . C48 . 1.378(6) yes C47 . H471 . 0.928 no C48 . H481 . 0.930 no C49 . C50 . 1.392(6) yes C49 . C54 . 1.400(6) yes C50 . C51 . 1.385(6) yes C50 . H501 . 0.933 no C51 . C52 . 1.373(7) yes C51 . H511 . 0.934 no C52 . C53 . 1.376(7) yes C52 . H521 . 0.926 no C53 . C54 . 1.384(6) yes C53 . H531 . 0.928 no C54 . H541 . 0.926 no O55 . C56 . 1.249(5) yes C56 . C57 . 1.470(6) yes C56 . C60 . 1.488(6) yes C57 . N58 . 1.319(5) yes C57 . C66 . 1.478(6) yes N58 . O59 . 1.299(4) yes C60 . C61 . 1.390(6) yes C60 . C65 . 1.395(7) yes C61 . C62 . 1.390(7) yes C61 . H611 . 0.920 no C62 . C63 . 1.369(8) yes C62 . H621 . 0.924 no C63 . C64 . 1.380(7) yes C63 . H631 . 0.939 no C64 . C65 . 1.385(7) yes C64 . H641 . 0.941 no C65 . H651 . 0.934 no C66 . C67 . 1.376(7) yes C66 . C71 . 1.390(6) yes C67 . C68 . 1.389(7) yes C67 . H671 . 0.932 no C68 . C69 . 1.366(7) yes C68 . H681 . 0.945 no C69 . C70 . 1.363(8) yes C69 . H691 . 0.926 no C70 . C71 . 1.394(7) yes C70 . H701 . 0.927 no C71 . H711 . 0.928 no O72 . C73 . 1.420(6) yes C73 . H732 . 0.961 no C73 . H733 . 0.958 no C73 . H731 . 0.958 no O74 . C75 . 1.432(6) yes O74 . H741 . 0.826 no C75 . H752 . 0.970 no C75 . H753 . 0.961 no C75 . H751 . 0.962 no O76 . C77 . 1.418(8) yes O76 . C79 . 1.389(10) yes C77 . C78 . 1.492(10) yes C77 . H772 . 0.992 no C77 . H771 . 0.996 no C78 . H781 . 0.978 no C78 . H782 . 0.982 no C78 . H783 . 0.977 no C79 . C80 . 1.447(11) yes C79 . H791 . 0.966 no C79 . H792 . 0.986 no C80 . H802 . 0.953 no C80 . H801 . 0.962 no C80 . H803 . 0.954 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O55 2_665 Ni1 . O42 2_665 167.88(12) yes O55 2_665 Ni1 . N58 2_665 77.63(13) yes O42 2_665 Ni1 . N58 2_665 91.19(13) yes O55 2_665 Ni1 . Ni2 . 128.59(9) yes O42 2_665 Ni1 . Ni2 . 58.44(8) yes N58 2_665 Ni1 . Ni2 . 104.52(10) yes O55 2_665 Ni1 . O4 . 93.63(12) yes O42 2_665 Ni1 . O4 . 97.42(12) yes N58 2_665 Ni1 . O4 . 171.19(13) yes Ni2 . Ni1 . O4 . 81.72(8) yes O55 2_665 Ni1 . N7 . 90.22(13) yes O42 2_665 Ni1 . N7 . 87.33(13) yes N58 2_665 Ni1 . N7 . 101.03(15) yes Ni2 . Ni1 . N7 . 137.03(11) yes O4 . Ni1 . N7 . 77.64(14) yes O55 2_665 Ni1 . O21 . 99.05(12) yes O42 2_665 Ni1 . O21 . 85.32(11) yes N58 2_665 Ni1 . O21 . 89.41(13) yes Ni2 . Ni1 . O21 . 31.28(8) yes O4 . Ni1 . O21 . 93.11(12) yes N7 . Ni1 . O21 . 167.35(14) yes Ni1 . Ni2 . Ni2 2_665 106.12(3) yes Ni1 . Ni2 . N41 2_665 60.00(11) yes Ni2 2_665 Ni2 . N41 2_665 65.71(10) yes Ni1 . Ni2 . O38 2_665 141.64(9) yes Ni2 2_665 Ni2 . O38 2_665 67.46(9) yes N41 2_665 Ni2 . O38 2_665 84.62(14) yes Ni1 . Ni2 . Ni3 . 175.81(2) yes Ni2 2_665 Ni2 . Ni3 . 70.955(19) yes N41 2_665 Ni2 . Ni3 . 115.82(11) yes O38 2_665 Ni2 . Ni3 . 34.73(9) yes Ni1 . Ni2 . O21 . 35.53(9) yes Ni2 2_665 Ni2 . O21 . 117.14(10) yes N41 2_665 Ni2 . O21 . 94.25(14) yes O38 2_665 Ni2 . O21 . 174.31(13) yes Ni3 . Ni2 . O21 . 148.37(9) yes Ni1 . Ni2 . N24 . 121.44(11) yes Ni2 2_665 Ni2 . N24 . 109.06(10) yes N41 2_665 Ni2 . N24 . 174.39(14) yes O38 2_665 Ni2 . N24 . 95.26(14) yes Ni3 . Ni2 . N24 . 62.69(11) yes O21 . Ni2 . N24 . 86.41(14) yes Ni2 . Ni3 . O38 2_665 31.03(8) yes Ni2 . Ni3 . O25 . 58.61(8) yes O38 2_665 Ni3 . O25 . 87.85(12) yes Ni2 . Ni3 . O42 . 89.40(8) yes O38 2_665 Ni3 . O42 . 98.45(12) yes O25 . Ni3 . O42 . 93.23(12) yes Ni2 . Ni3 . O59 . 123.48(9) yes O38 2_665 Ni3 . O59 . 93.39(12) yes O25 . Ni3 . O59 . 174.63(12) yes O42 . Ni3 . O59 . 91.75(11) yes Ni2 . Ni3 . O72 . 151.29(9) yes O38 2_665 Ni3 . O72 . 173.86(12) yes O25 . Ni3 . O72 . 93.06(12) yes O42 . Ni3 . O72 . 87.57(12) yes O59 . Ni3 . O72 . 85.16(12) yes Ni2 . Ni3 . O74 . 96.18(9) yes O38 2_665 Ni3 . O74 . 86.01(12) yes O25 . Ni3 . O74 . 90.38(12) yes O42 . Ni3 . O74 . 174.36(12) yes O59 . Ni3 . O74 . 84.50(12) yes O72 . Ni3 . O74 . 87.91(12) yes Ni1 . O4 . C5 . 115.1(3) yes O4 . C5 . C6 . 118.5(4) yes O4 . C5 . C9 . 116.8(4) yes C6 . C5 . C9 . 124.7(4) yes C5 . C6 . N7 . 111.7(4) yes C5 . C6 . C15 . 126.6(4) yes N7 . C6 . C15 . 121.4(4) yes C6 . N7 . Ni1 . 116.3(3) yes C6 . N7 . O8 . 119.6(4) yes Ni1 . N7 . O8 . 123.8(3) yes N7 . O8 . H81 . 112.1 no C5 . C9 . C10 . 117.1(4) yes C5 . C9 . C14 . 123.9(4) yes C10 . C9 . C14 . 118.7(4) yes C9 . C10 . C11 . 120.8(4) yes C9 . C10 . H101 . 120.1 no C11 . C10 . H101 . 119.1 no C10 . C11 . C12 . 119.9(5) yes C10 . C11 . H111 . 120.5 no C12 . C11 . H111 . 119.6 no C11 . C12 . C13 . 119.9(5) yes C11 . C12 . H121 . 119.0 no C13 . C12 . H121 . 121.1 no C12 . C13 . C14 . 120.8(5) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 119.1 no C9 . C14 . C13 . 119.9(5) yes C9 . C14 . H141 . 119.8 no C13 . C14 . H141 . 120.3 no C6 . C15 . C16 . 119.6(5) yes C6 . C15 . C20 . 120.8(5) yes C16 . C15 . C20 . 119.5(5) yes C15 . C16 . C17 . 120.3(7) yes C15 . C16 . H161 . 121.3 no C17 . C16 . H161 . 118.4 no C16 . C17 . C18 . 118.5(7) yes C16 . C17 . H171 . 120.6 no C18 . C17 . H171 . 120.8 no C17 . C18 . C19 . 121.3(6) yes C17 . C18 . H181 . 119.0 no C19 . C18 . H181 . 119.6 no C18 . C19 . C20 . 119.4(8) yes C18 . C19 . H191 . 121.1 no C20 . C19 . H191 . 119.4 no C15 . C20 . C19 . 120.8(7) yes C15 . C20 . H201 . 119.4 no C19 . C20 . H201 . 119.7 no Ni1 . O21 . Ni2 . 113.19(14) yes Ni1 . O21 . C22 . 128.9(2) yes Ni2 . O21 . C22 . 113.0(3) yes O21 . C22 . C23 . 109.1(3) yes O21 . C22 . C26 . 112.5(3) yes C23 . C22 . C26 . 109.9(4) yes O21 . C22 . H221 . 102.5 no C23 . C22 . H221 . 107.3 no C26 . C22 . H221 . 115.2 no C22 . C23 . N24 . 111.9(4) yes C22 . C23 . C32 . 120.2(4) yes N24 . C23 . C32 . 127.9(4) yes C23 . N24 . Ni2 . 116.1(3) yes C23 . N24 . O25 . 122.4(3) yes Ni2 . N24 . O25 . 121.3(3) yes N24 . O25 . Ni3 . 117.4(2) yes C22 . C26 . C27 . 121.0(5) yes C22 . C26 . C31 . 120.1(4) yes C27 . C26 . C31 . 119.0(5) yes C26 . C27 . C28 . 120.8(6) yes C26 . C27 . H271 . 119.1 no C28 . C27 . H271 . 120.2 no C27 . C28 . C29 . 119.5(6) yes C27 . C28 . H281 . 119.3 no C29 . C28 . H281 . 121.2 no C28 . C29 . C30 . 120.5(5) yes C28 . C29 . H291 . 120.1 no C30 . C29 . H291 . 119.4 no C29 . C30 . C31 . 119.0(6) yes C29 . C30 . H301 . 121.1 no C31 . C30 . H301 . 119.8 no C26 . C31 . C30 . 121.2(6) yes C26 . C31 . H311 . 119.5 no C30 . C31 . H311 . 119.3 no C23 . C32 . C33 . 119.4(4) yes C23 . C32 . C37 . 123.5(4) yes C33 . C32 . C37 . 117.0(4) yes C32 . C33 . C34 . 121.6(5) yes C32 . C33 . H331 . 119.1 no C34 . C33 . H331 . 119.2 no C33 . C34 . C35 . 119.8(5) yes C33 . C34 . H341 . 119.0 no C35 . C34 . H341 . 121.2 no C34 . C35 . C36 . 120.1(4) yes C34 . C35 . H351 . 120.5 no C36 . C35 . H351 . 119.4 no C35 . C36 . C37 . 120.4(5) yes C35 . C36 . H361 . 119.5 no C37 . C36 . H361 . 120.0 no C32 . C37 . C36 . 121.0(4) yes C32 . C37 . H371 . 119.2 no C36 . C37 . H371 . 119.7 no Ni3 2_665 O38 . Ni2 2_665 114.23(14) yes Ni3 2_665 O38 . C39 . 130.4(2) yes Ni2 2_665 O38 . C39 . 114.0(2) yes O38 . C39 . C40 . 109.4(3) yes O38 . C39 . C43 . 109.6(3) yes C40 . C39 . C43 . 111.0(3) yes O38 . C39 . H391 . 104.8 no C40 . C39 . H391 . 107.1 no C43 . C39 . H391 . 114.7 no C39 . C40 . N41 . 111.9(4) yes C39 . C40 . C49 . 121.4(4) yes N41 . C40 . C49 . 126.5(4) yes C40 . N41 . Ni2 2_665 117.9(3) yes C40 . N41 . O42 . 121.6(3) yes Ni2 2_665 N41 . O42 . 120.4(3) yes N41 . O42 . Ni3 . 114.1(2) yes N41 . O42 . Ni1 2_665 110.2(2) yes Ni3 . O42 . Ni1 2_665 112.36(14) yes C39 . C43 . C44 . 121.3(4) yes C39 . C43 . C48 . 120.1(4) yes C44 . C43 . C48 . 118.6(4) yes C43 . C44 . C45 . 121.2(4) yes C43 . C44 . H441 . 119.3 no C45 . C44 . H441 . 119.6 no C44 . C45 . C46 . 119.7(5) yes C44 . C45 . H451 . 121.4 no C46 . C45 . H451 . 119.0 no C45 . C46 . C47 . 118.9(5) yes C45 . C46 . H461 . 120.6 no C47 . C46 . H461 . 120.4 no C46 . C47 . C48 . 122.0(5) yes C46 . C47 . H471 . 118.9 no C48 . C47 . H471 . 119.1 no C43 . C48 . C47 . 119.6(5) yes C43 . C48 . H481 . 119.7 no C47 . C48 . H481 . 120.7 no C40 . C49 . C50 . 119.6(4) yes C40 . C49 . C54 . 122.3(4) yes C50 . C49 . C54 . 117.8(4) yes C49 . C50 . C51 . 121.2(4) yes C49 . C50 . H501 . 118.4 no C51 . C50 . H501 . 120.4 no C50 . C51 . C52 . 120.3(4) yes C50 . C51 . H511 . 118.7 no C52 . C51 . H511 . 121.0 no C51 . C52 . C53 . 119.4(4) yes C51 . C52 . H521 . 120.3 no C53 . C52 . H521 . 120.3 no C52 . C53 . C54 . 121.1(4) yes C52 . C53 . H531 . 119.3 no C54 . C53 . H531 . 119.6 no C49 . C54 . C53 . 120.2(4) yes C49 . C54 . H541 . 121.0 no C53 . C54 . H541 . 118.8 no Ni1 2_665 O55 . C56 . 113.8(3) yes O55 . C56 . C57 . 118.8(4) yes O55 . C56 . C60 . 117.9(4) yes C57 . C56 . C60 . 123.3(4) yes C56 . C57 . N58 . 111.8(4) yes C56 . C57 . C66 . 128.0(4) yes N58 . C57 . C66 . 120.1(4) yes C57 . N58 . Ni1 2_665 117.8(3) yes C57 . N58 . O59 . 117.7(3) yes Ni1 2_665 N58 . O59 . 124.1(3) yes N58 . O59 . Ni3 . 118.6(2) yes C56 . C60 . C61 . 116.6(4) yes C56 . C60 . C65 . 124.8(4) yes C61 . C60 . C65 . 118.6(4) yes C60 . C61 . C62 . 119.8(5) yes C60 . C61 . H611 . 120.0 no C62 . C61 . H611 . 120.1 no C61 . C62 . C63 . 121.2(5) yes C61 . C62 . H621 . 119.0 no C63 . C62 . H621 . 119.9 no C62 . C63 . C64 . 119.5(5) yes C62 . C63 . H631 . 120.3 no C64 . C63 . H631 . 120.2 no C63 . C64 . C65 . 120.1(5) yes C63 . C64 . H641 . 120.3 no C65 . C64 . H641 . 119.6 no C60 . C65 . C64 . 120.7(5) yes C60 . C65 . H651 . 120.1 no C64 . C65 . H651 . 119.2 no C57 . C66 . C67 . 119.8(4) yes C57 . C66 . C71 . 121.3(4) yes C67 . C66 . C71 . 118.9(4) yes C66 . C67 . C68 . 120.7(5) yes C66 . C67 . H671 . 119.0 no C68 . C67 . H671 . 120.3 no C67 . C68 . C69 . 119.9(5) yes C67 . C68 . H681 . 120.5 no C69 . C68 . H681 . 119.6 no C68 . C69 . C70 . 120.5(5) yes C68 . C69 . H691 . 119.8 no C70 . C69 . H691 . 119.7 no C69 . C70 . C71 . 120.2(5) yes C69 . C70 . H701 . 120.2 no C71 . C70 . H701 . 119.6 no C70 . C71 . C66 . 119.9(5) yes C70 . C71 . H711 . 120.4 no C66 . C71 . H711 . 119.7 no Ni3 . O72 . C73 . 123.8(3) yes O72 . C73 . H732 . 108.5 no O72 . C73 . H733 . 108.1 no H732 . C73 . H733 . 111.7 no O72 . C73 . H731 . 107.2 no H732 . C73 . H731 . 110.6 no H733 . C73 . H731 . 110.5 no Ni3 . O74 . C75 . 123.5(3) yes Ni3 . O74 . H741 . 97.2 no C75 . O74 . H741 . 107.6 no O74 . C75 . H752 . 109.4 no O74 . C75 . H753 . 109.5 no H752 . C75 . H753 . 110.7 no O74 . C75 . H751 . 107.4 no H752 . C75 . H751 . 110.5 no H753 . C75 . H751 . 109.2 no C77 . O76 . C79 . 115.5(6) yes O76 . C77 . C78 . 110.4(6) yes O76 . C77 . H772 . 108.6 no C78 . C77 . H772 . 109.4 no O76 . C77 . H771 . 109.8 no C78 . C77 . H771 . 109.0 no H772 . C77 . H771 . 109.6 no C77 . C78 . H781 . 109.4 no C77 . C78 . H782 . 109.4 no H781 . C78 . H782 . 110.0 no C77 . C78 . H783 . 108.8 no H781 . C78 . H783 . 109.5 no H782 . C78 . H783 . 109.7 no O76 . C79 . C80 . 112.0(7) yes O76 . C79 . H791 . 109.1 no C80 . C79 . H791 . 108.2 no O76 . C79 . H792 . 107.7 no C80 . C79 . H792 . 108.8 no H791 . C79 . H792 . 111.0 no C79 . C80 . H802 . 109.7 no C79 . C80 . H801 . 106.6 no H802 . C80 . H801 . 111.2 no C79 . C80 . H803 . 108.4 no H802 . C80 . H803 . 110.3 no H801 . C80 . H803 . 110.5 no # Attachment 'Ni8.cif' data_eb8055 _database_code_depnum_ccdc_archive 'CCDC 718775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Giorgos Karotsis' _exptl_crystal_recrystallization_method 'Diffusion of ET2O into MeOH solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ni8 (C14H11NO2)8 (Et2O)2 (MeOH)2 (H2O)], 2(Et2O)' _chemical_formula_sum 'C130 H158 N8 Ni8 O23' _chemical_formula_weight 2670.32 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.141 0.137 -0.127 6024 1484 ' ' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'x, y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' '-x+1/2, -y+1/2, z+1' 'x+1/2, y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' '-x+1, -y, z+1' 'x+1/2, y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' '-x+1, -y+1/2, z+1/2' _cell_length_a 22.4470(6) _cell_length_b 55.1580(13) _cell_length_c 21.2010(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 26249.6(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9428 _cell_measurement_theta_min 2.2705 _cell_measurement_theta_max 26.3105 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11216 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6658 _exptl_absorpt_correction_T_max 0.7699 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 67387 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -68 _diffrn_reflns_limit_k_max 68 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.41 _reflns_number_total 13364 _reflns_number_gt 12122 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; #========================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #========================================================================== Format: alert-number_ALERT_alert-type_alert-level text 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.01 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.20 Ratio Data quality was quite poor. This refers to the terminal CH3 of an ether bound to an NI atom via its oxygen. It has higher motion than some of the more rigidly held carbon atoms 601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of . 5686.00 A**3 420_ALERT_2_B D-H Without Acceptor O1G - H1G ... ? 420_ALERT_2_B D-H Without Acceptor O1H - *H1H1 ... ? 420_ALERT_2_B D-H Without Acceptor O1H - *H1H2 ... ? 043_ALERT_1_B Check Reported Molecular Weight ................ 2670.32 044_ALERT_1_B Calculated and Reported Dx Differ .............. ? 041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? There was some disordered ether in the solvent region which was treated using the Spek/van der Sluis method using Platon's Squeeze routine. 1484 electrons were removed from the unit cell which corresponds to ~4 molecules of ether per Ni8 complex. 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 2 301_ALERT_3_G Note Main Residue Disorder .................... 1.00 Perc. 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 33.00 Deg. C2F -O1F -H2F4 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 32.70 Deg. H2F2 -C2F -H2F3 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 36.60 Deg. O1F -C2F -H2F4 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 36.60 Deg. H2F1 -C2F -H2F5 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 12.30 Deg. O1F -C3F -H3F3 8.454 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 11.30 Deg. H3F1 -C3F -H3F4 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 11.70 Deg. H3F2 -C3F -H3F5 1.555 1.555 1.555 In the centre of the Ni8 wheel there is an ether molecule. It appears to be disordered, bound to either of two opposite Ni atoms in the wheel. The two positions overlap and the best attempt at modelling this is presented. 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C4D 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O1F 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O1G 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C2E 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C6D 331_ALERT_2_C Small Average Phenyl C-C Dist. C1D -C6D 1.36 Ang. 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 360_ALERT_2_C Short C(sp3)-C(sp3) Bond C2E - C3E ... 1.37 Ang. 083_ALERT_2_G SHELXL Second Parameter in WGHT unusually Large. 111.84 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 176 Data quality is quite poor. The most reasonable model tried is presented. SIMU and DELU restraints have been used to improve thermal parameters. 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 1 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 1 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 23 Completeness is 99% or better to theta max. See below #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 3562 3561 1 23.01 0.550 1.000 4712 4711 1 25.24 0.600 1.000 6126 6125 1 #----------------------------------------------------------- ACTA Min. Res. ---- 26.41 0.626 0.997 6929 6905 24 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C122 H118 N8 Ni8 O21 180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 = 3 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 3 O8A -NI5 -O8A -N8A -39.40 0.30 8.454 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 9 N8B -NI4 -N8A -C8A -91.00 3.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 12 N8B -NI4 -N8A -O8A 84.00 3.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 29 O7B -NI4 -O7A -C7A -76.00 7.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 32 O7B -NI4 -O7A -NI3 136.00 7.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 35 O7D -NI3 -O7A -C7A -87.80 0.90 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 40 O7D -NI3 -O7A -NI4 55.80 0.90 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 66 O8C -NI3 -O8B -N8B -52.50 1.30 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 74 N8A -NI4 -N8B -C8B -86.00 3.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 77 N8A -NI4 -N8B -O8B 87.00 3.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 94 O7A -NI4 -O7B -C7B -104.00 7.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 97 O7A -NI4 -O7B -NI5 102.00 7.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 129 O8B -NI3 -O8C -N8C -58.40 1.30 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 137 N8D -NI2 -N8C -C8C -90.60 1.60 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 140 N8D -NI2 -N8C -O8C 82.30 1.60 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 157 O7D -NI2 -O7C -C7C 66.00 10.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 160 O7D -NI2 -O7C -NI1 -91.00 10.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 194 O8D -NI1 -O8D -N8D -41.10 0.30 8.454 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 199 N8C -NI2 -N8D -C8D -88.40 1.60 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 202 N8C -NI2 -N8D -O8D 86.80 1.60 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 219 O7C -NI2 -O7D -C7D 120.00 10.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 222 O7C -NI2 -O7D -NI3 -29.00 10.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 227 O7A -NI3 -O7D -C7D -94.40 0.90 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 232 O7A -NI3 -O7D -NI2 50.30 0.90 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 269 O1G -NI3 -O1F -C2F -66.00 4.00 1.555 1.555 1.555 1.555 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 274 O1G -NI3 -O1F -C3F 117.00 4.00 1.555 1.555 1.555 8.454 710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 282 O1F -NI3 -O1G -C2G 153.00 4.00 1.555 1.555 1.555 1.555 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 20 No action taken. 792_ALERT_1_G The Model has Chirality at C7A (Verify) .... R 792_ALERT_1_G The Model has Chirality at C7B (Verify) .... R 792_ALERT_1_G The Model has Chirality at C7C (Verify) .... R 792_ALERT_1_G The Model has Chirality at C7D (Verify) .... R 850_ALERT_4_G Check Flack Parameter Exact Value 0.00 and su .. 0.02 Ok ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+111.8372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(17) _refine_ls_number_reflns 13364 _refine_ls_number_parameters 714 _refine_ls_number_restraints 176 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.2500 0.2500 -0.75805(4) 0.0357(2) Uani 1 2 d S . . Ni2 Ni -0.13334(3) 0.241067(10) -0.83795(3) 0.03296(15) Uani 1 1 d . . . Ni3 Ni -0.07937(3) 0.239491(10) -0.97563(4) 0.03843(15) Uani 1 1 d . . . Ni4 Ni -0.13411(3) 0.244671(10) -1.11192(3) 0.03026(14) Uani 1 1 d . . . Ni5 Ni -0.2500 0.2500 -1.19483(4) 0.02890(19) Uani 1 2 d S . . O8A O -0.20786(14) 0.21801(6) -1.19316(16) 0.0344(7) Uani 1 1 d . . . N8A N -0.16687(17) 0.21705(7) -1.14763(19) 0.0306(9) Uani 1 1 d . . . C8A C -0.1509(2) 0.19655(8) -1.1221(2) 0.0337(11) Uani 1 1 d . . . C9A C -0.1753(2) 0.17244(8) -1.1386(2) 0.0348(11) Uani 1 1 d . . . C7A C -0.1050(2) 0.19900(8) -1.0711(2) 0.0341(11) Uani 1 1 d . . . H7A H -0.1214 0.1918 -1.0314 0.041 Uiso 1 1 calc R . . O7A O -0.09301(15) 0.22403(6) -1.06047(17) 0.0363(8) Uani 1 1 d . . . C6A C -0.0473(2) 0.18609(8) -1.0875(3) 0.0368(11) Uani 1 1 d U . . C1A C -0.0285(3) 0.18325(12) -1.1482(3) 0.0559(15) Uani 1 1 d U . . H1A H -0.0534 0.1885 -1.1818 0.067 Uiso 1 1 calc R . . C5A C -0.0118(3) 0.17771(10) -1.0390(3) 0.0512(14) Uani 1 1 d U . . H5A H -0.0254 0.1789 -0.9967 0.061 Uiso 1 1 calc R . . C4A C 0.0438(3) 0.16750(12) -1.0513(3) 0.0649(18) Uani 1 1 d U . . H4A H 0.0689 0.1625 -1.0176 0.078 Uiso 1 1 calc R . . C3A C 0.0617(3) 0.16479(15) -1.1125(4) 0.079(2) Uani 1 1 d U . . H3A H 0.0988 0.1573 -1.1215 0.095 Uiso 1 1 calc R . . C2A C 0.0256(3) 0.17300(16) -1.1621(4) 0.082(2) Uani 1 1 d U . . H2A H 0.0384 0.1715 -1.2046 0.099 Uiso 1 1 calc R . . C10A C -0.1846(2) 0.15533(9) -1.0929(3) 0.0387(11) Uani 1 1 d . . . H10A H -0.1764 0.1592 -1.0501 0.046 Uiso 1 1 calc R . . C14A C -0.1870(3) 0.16632(10) -1.2010(3) 0.0557(16) Uani 1 1 d . . . H14A H -0.1811 0.1779 -1.2336 0.067 Uiso 1 1 calc R . . C13A C -0.2076(3) 0.14276(10) -1.2154(3) 0.0634(18) Uani 1 1 d . . . H13A H -0.2146 0.1383 -1.2581 0.076 Uiso 1 1 calc R . . C12A C -0.2177(2) 0.12629(9) -1.1683(3) 0.0452(13) Uani 1 1 d . . . H12A H -0.2329 0.1106 -1.1779 0.054 Uiso 1 1 calc R . . C11A C -0.2057(3) 0.13252(8) -1.1081(3) 0.0442(13) Uani 1 1 d . . . H11A H -0.2120 0.1210 -1.0754 0.053 Uiso 1 1 calc R . . O8B O -0.07259(14) 0.27135(6) -1.02055(17) 0.0355(8) Uani 1 1 d . . . N8B N -0.10570(17) 0.27229(7) -1.0729(2) 0.0363(9) Uani 1 1 d . . . C8B C -0.1241(2) 0.29251(8) -1.0949(2) 0.0344(11) Uani 1 1 d . . . C7B C -0.1617(2) 0.28995(9) -1.1546(3) 0.0476(15) Uani 1 1 d . . . H7B H -0.2001 0.2988 -1.1480 0.057 Uiso 1 1 calc R . . C9B C -0.1098(2) 0.31705(8) -1.0677(2) 0.0344(11) Uani 1 1 d . . . O7B O -0.17448(15) 0.26534(6) -1.16524(19) 0.0413(9) Uani 1 1 d . . . C6B C -0.1311(3) 0.30079(10) -1.2094(3) 0.0587(17) Uani 1 1 d U . . C1B C -0.0790(3) 0.29018(15) -1.2327(4) 0.076(2) Uani 1 1 d U . . H1B H -0.0627 0.2765 -1.2114 0.092 Uiso 1 1 calc R . . C5B C -0.1524(4) 0.32090(11) -1.2418(4) 0.083(2) Uani 1 1 d U . . H5B H -0.1873 0.3288 -1.2273 0.099 Uiso 1 1 calc R . . C4B C -0.1235(5) 0.32951(14) -1.2947(4) 0.095(2) Uani 1 1 d U . . H4B H -0.1386 0.3433 -1.3162 0.114 Uiso 1 1 calc R . . C3B C -0.0736(5) 0.31829(16) -1.3163(4) 0.099(3) Uani 1 1 d U . . H3B H -0.0545 0.3241 -1.3533 0.118 Uiso 1 1 calc R . . C2B C -0.0507(4) 0.29886(18) -1.2854(4) 0.090(2) Uani 1 1 d U . . H2B H -0.0153 0.2913 -1.3002 0.108 Uiso 1 1 calc R . . C10B C -0.0528(2) 0.32277(9) -1.0478(3) 0.0429(13) Uani 1 1 d . . . H10B H -0.0218 0.3111 -1.0512 0.051 Uiso 1 1 calc R . . C14B C -0.1538(3) 0.33462(10) -1.0633(3) 0.0555(16) Uani 1 1 d . . . H14B H -0.1931 0.3313 -1.0777 0.067 Uiso 1 1 calc R . . C13B C -0.1400(3) 0.35691(10) -1.0380(3) 0.0586(17) Uani 1 1 d . . . H13B H -0.1704 0.3688 -1.0341 0.070 Uiso 1 1 calc R . . C12B C -0.0838(3) 0.36221(10) -1.0182(3) 0.0528(15) Uani 1 1 d . . . H12B H -0.0748 0.3777 -1.0012 0.063 Uiso 1 1 calc R . . C11B C -0.0410(3) 0.34516(10) -1.0232(3) 0.0500(14) Uani 1 1 d . . . H11B H -0.0018 0.3488 -1.0092 0.060 Uiso 1 1 calc R . . O8C O -0.09751(15) 0.20825(6) -0.93108(16) 0.0361(8) Uani 1 1 d . . . N8C N -0.12833(16) 0.21111(7) -0.87838(19) 0.0293(8) Uani 1 1 d . . . C8C C -0.1620(2) 0.19425(8) -0.8552(2) 0.0343(11) Uani 1 1 d . . . C7C C -0.1911(2) 0.20118(8) -0.7940(2) 0.0352(11) Uani 1 1 d . . . H7C H -0.2339 0.1962 -0.7953 0.042 Uiso 1 1 calc R . . C9C C -0.1705(2) 0.16989(8) -0.8841(2) 0.0358(11) Uani 1 1 d . . . O7C O -0.18772(16) 0.22645(6) -0.78569(18) 0.0429(9) Uani 1 1 d . . . C6C C -0.1611(2) 0.18890(8) -0.7379(3) 0.0428(13) Uani 1 1 d U . . C5C C -0.1931(3) 0.18209(11) -0.6858(3) 0.0533(14) Uani 1 1 d U . . H5C H -0.2351 0.1842 -0.6859 0.064 Uiso 1 1 calc R . . C1C C -0.0999(3) 0.18535(11) -0.7370(3) 0.0538(15) Uani 1 1 d U . . H1C H -0.0768 0.1892 -0.7733 0.065 Uiso 1 1 calc R . . C2C C -0.0729(3) 0.17646(12) -0.6845(4) 0.0648(17) Uani 1 1 d U . . H2C H -0.0309 0.1744 -0.6845 0.078 Uiso 1 1 calc R . . C3C C -0.1048(3) 0.17026(11) -0.6313(3) 0.0598(16) Uani 1 1 d U . . H3C H -0.0851 0.1648 -0.5942 0.072 Uiso 1 1 calc R . . C4C C -0.1661(3) 0.17227(13) -0.6334(3) 0.0658(17) Uani 1 1 d U . . H4C H -0.1896 0.1669 -0.5988 0.079 Uiso 1 1 calc R . . C14C C -0.1232(2) 0.15699(9) -0.9092(3) 0.0376(11) Uani 1 1 d . . . H14C H -0.0843 0.1638 -0.9093 0.045 Uiso 1 1 calc R . . C10C C -0.2265(2) 0.15931(9) -0.8837(3) 0.0416(12) Uani 1 1 d . . . H10C H -0.2593 0.1677 -0.8654 0.050 Uiso 1 1 calc R . . C11C C -0.2348(3) 0.13647(9) -0.9099(3) 0.0453(13) Uani 1 1 d . . . H11C H -0.2736 0.1296 -0.9116 0.054 Uiso 1 1 calc R . . C12C C -0.1869(2) 0.12382(9) -0.9336(3) 0.0445(13) Uani 1 1 d . . . H12C H -0.1922 0.1079 -0.9495 0.053 Uiso 1 1 calc R . . C13C C -0.1325(3) 0.13406(9) -0.9342(3) 0.0470(14) Uani 1 1 d . . . H13C H -0.1000 0.1254 -0.9521 0.056 Uiso 1 1 calc R . . O8D O -0.18638(16) 0.27567(6) -0.76060(17) 0.0404(8) Uani 1 1 d . . . N8D N -0.14546(18) 0.27174(7) -0.8046(2) 0.0347(9) Uani 1 1 d . . . C8D C -0.1154(2) 0.28922(9) -0.8292(2) 0.0364(11) Uani 1 1 d . . . C7D C -0.0718(2) 0.28075(8) -0.8794(2) 0.0348(11) Uani 1 1 d . . . H7D H -0.0799 0.2899 -0.9193 0.042 Uiso 1 1 calc R . . C9D C -0.1233(2) 0.31536(9) -0.8147(2) 0.0368(11) Uani 1 1 d . . . O7D O -0.07996(15) 0.25547(6) -0.89103(15) 0.0318(7) Uani 1 1 d . . . C6D C -0.0070(2) 0.28506(10) -0.8600(3) 0.0507(14) Uani 1 1 d U . . C1D C 0.0155(3) 0.27690(18) -0.8049(4) 0.087(2) Uani 1 1 d U . . H1D H -0.0103 0.2694 -0.7753 0.105 Uiso 1 1 calc R . . C5D C 0.0322(3) 0.29647(15) -0.9009(6) 0.102(3) Uani 1 1 d U . . H5D H 0.0191 0.3024 -0.9406 0.122 Uiso 1 1 calc R . . C4D C 0.0908(4) 0.29904(19) -0.8822(7) 0.138(4) Uani 1 1 d U . . H4D H 0.1174 0.3075 -0.9092 0.165 Uiso 1 1 calc R . . C3D C 0.1108(4) 0.2905(2) -0.8299(7) 0.120(4) Uani 1 1 d U . . H3D H 0.1518 0.2925 -0.8199 0.144 Uiso 1 1 calc R . . C2D C 0.0762(4) 0.2793(2) -0.7906(5) 0.115(3) Uani 1 1 d U . . H2D H 0.0918 0.2727 -0.7525 0.138 Uiso 1 1 calc R . . C14D C -0.1483(2) 0.32308(10) -0.7588(3) 0.0439(13) Uani 1 1 d . . . H14D H -0.1615 0.3117 -0.7283 0.053 Uiso 1 1 calc R . . C10D C -0.1039(2) 0.33254(9) -0.8587(3) 0.0488(14) Uani 1 1 d . . . H10D H -0.0863 0.3274 -0.8972 0.059 Uiso 1 1 calc R . . C11D C -0.1104(3) 0.35707(10) -0.8458(3) 0.0590(17) Uani 1 1 d . . . H11D H -0.0974 0.3687 -0.8759 0.071 Uiso 1 1 calc R . . C12D C -0.1349(3) 0.36466(10) -0.7910(3) 0.0511(15) Uani 1 1 d . . . H12D H -0.1387 0.3815 -0.7828 0.061 Uiso 1 1 calc R . . C13D C -0.1540(2) 0.34830(10) -0.7475(3) 0.0483(14) Uani 1 1 d . . . H13D H -0.1714 0.3538 -0.7092 0.058 Uiso 1 1 calc R . . O1E O -0.2500 0.2500 -1.2912(3) 0.0500(14) Uani 1 2 d S . . C2E C -0.2945(4) 0.23686(17) -1.3269(4) 0.086(2) Uani 1 1 d U . . H2EA H -0.3259 0.2317 -1.2970 0.103 Uiso 1 1 calc R . . H2EB H -0.3131 0.2485 -1.3566 0.103 Uiso 1 1 calc R . . C3E C -0.2779(7) 0.2169(2) -1.3608(7) 0.169(6) Uani 1 1 d U . . H3EA H -0.3127 0.2103 -1.3829 0.254 Uiso 1 1 calc R . . H3EB H -0.2617 0.2046 -1.3323 0.254 Uiso 1 1 calc R . . H3EC H -0.2475 0.2215 -1.3917 0.254 Uiso 1 1 calc R . . O1F O -0.1845(3) 0.24664(10) -0.9763(4) 0.0393(15) Uani 0.50 1 d P . . C2F C -0.2153(4) 0.27294(15) -0.9524(4) 0.080(2) Uiso 1 1 d . . . H2F1 H -0.2323 0.2716 -0.9094 0.096 Uiso 0.50 1 calc PR . . H2F2 H -0.1862 0.2864 -0.9534 0.096 Uiso 0.50 1 calc PR . . H2F3 H -0.1782 0.2794 -0.9700 0.120 Uiso 0.50 1 d PR . . H2F4 H -0.2097 0.2559 -0.9408 0.120 Uiso 0.50 1 d PR . . H2F5 H -0.2262 0.2823 -0.9148 0.120 Uiso 0.50 1 d PR . . C3F C -0.2617(4) 0.27600(19) -0.9998(5) 0.108(3) Uiso 1 1 d . . . H3F1 H -0.2463 0.2728 -1.0428 0.129 Uiso 0.50 1 calc PR . . H3F2 H -0.2790 0.2925 -0.9984 0.129 Uiso 0.50 1 calc PR . . H3F3 H -0.2964 0.2667 -0.9856 0.161 Uiso 0.50 1 d PR . . H3F4 H -0.2476 0.2695 -1.0402 0.161 Uiso 0.50 1 d PR . . H3F5 H -0.2728 0.2931 -1.0051 0.161 Uiso 0.50 1 d PR . . O1G O 0.01159(17) 0.23478(7) -0.9788(2) 0.0606(10) Uani 1 1 d . . . H1G H 0.0313 0.2386 -1.0172 0.073 Uiso 1 1 calc R . . C2G C 0.0463(4) 0.2265(2) -0.9294(4) 0.125(4) Uani 1 1 d . . . H2GA H 0.0882 0.2262 -0.9424 0.187 Uiso 1 1 calc R . . H2GB H 0.0336 0.2101 -0.9177 0.187 Uiso 1 1 calc R . . H2GC H 0.0417 0.2373 -0.8931 0.187 Uiso 1 1 calc R . . O1H O -0.2500 0.2500 -0.6638(3) 0.0678(19) Uani 1 2 d S . . H1H1 H -0.2803 0.2614 -0.6484 0.102 Uiso 0.50 1 d PR . . H1H2 H -0.2107 0.2550 -0.6484 0.102 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0447(5) 0.0247(4) 0.0378(5) 0.000 0.000 0.0128(4) Ni2 0.0381(4) 0.0203(3) 0.0404(4) 0.0026(2) -0.0007(3) 0.0070(2) Ni3 0.0528(4) 0.0220(3) 0.0405(3) 0.0000(3) 0.0015(4) -0.0020(2) Ni4 0.0290(3) 0.0179(2) 0.0439(4) 0.0026(2) -0.0015(3) -0.0041(2) Ni5 0.0308(4) 0.0242(4) 0.0318(5) 0.000 0.000 -0.0078(3) O8A 0.0293(16) 0.0304(17) 0.0436(19) 0.0056(15) -0.0004(15) -0.0078(13) N8A 0.0275(19) 0.027(2) 0.038(2) 0.0021(16) 0.0023(17) -0.0057(15) C8A 0.039(3) 0.024(2) 0.038(3) -0.0012(19) 0.018(2) -0.0023(18) C9A 0.029(2) 0.023(2) 0.052(3) -0.005(2) 0.011(2) 0.0043(18) C7A 0.044(3) 0.017(2) 0.042(3) 0.0033(18) 0.006(2) 0.0023(19) O7A 0.0391(19) 0.0221(16) 0.048(2) 0.0016(14) -0.0020(16) -0.0019(13) C6A 0.039(3) 0.026(2) 0.046(3) 0.004(2) 0.007(2) 0.0068(19) C1A 0.046(3) 0.069(4) 0.053(3) 0.004(3) 0.013(3) 0.008(3) C5A 0.057(3) 0.049(3) 0.048(3) 0.017(3) 0.010(3) 0.020(3) C4A 0.055(4) 0.069(4) 0.070(4) 0.031(3) 0.009(3) 0.028(3) C3A 0.060(4) 0.096(5) 0.081(4) 0.012(4) 0.040(4) 0.037(4) C2A 0.062(4) 0.116(6) 0.070(4) 0.006(4) 0.033(4) 0.031(4) C10A 0.046(3) 0.027(2) 0.043(3) 0.001(2) 0.009(2) 0.001(2) C14A 0.083(5) 0.038(3) 0.046(3) -0.007(2) -0.001(3) -0.018(3) C13A 0.109(5) 0.031(3) 0.050(4) 0.000(2) -0.007(4) -0.029(3) C12A 0.044(3) 0.021(2) 0.071(4) -0.006(2) -0.006(3) -0.003(2) C11A 0.060(3) 0.015(2) 0.058(3) 0.004(2) 0.011(3) 0.001(2) O8B 0.0325(17) 0.0233(16) 0.051(2) 0.0032(14) -0.0068(16) -0.0005(13) N8B 0.027(2) 0.032(2) 0.049(3) 0.0028(18) -0.0032(19) -0.0008(16) C8B 0.033(3) 0.024(2) 0.046(3) 0.003(2) -0.004(2) -0.0069(18) C7B 0.042(3) 0.020(2) 0.081(4) 0.007(2) -0.020(3) -0.008(2) C9B 0.035(3) 0.018(2) 0.050(3) 0.0038(19) 0.000(2) -0.0058(18) O7B 0.0346(19) 0.0248(17) 0.064(2) 0.0078(16) -0.0198(17) -0.0122(14) C6B 0.069(4) 0.042(3) 0.065(4) 0.021(3) -0.032(3) -0.035(3) C1B 0.062(4) 0.092(5) 0.074(5) 0.043(4) -0.022(3) -0.029(3) C5B 0.138(6) 0.027(3) 0.082(5) 0.014(3) -0.031(4) -0.024(3) C4B 0.159(7) 0.040(4) 0.085(5) 0.022(3) -0.030(5) -0.042(4) C3B 0.147(7) 0.074(5) 0.075(5) 0.021(4) -0.012(5) -0.064(4) C2B 0.076(5) 0.111(6) 0.084(5) 0.022(5) -0.006(4) -0.040(4) C10B 0.035(3) 0.031(3) 0.062(4) 0.005(2) -0.004(3) -0.007(2) C14B 0.041(3) 0.029(3) 0.097(5) 0.006(3) -0.006(3) 0.002(2) C13B 0.069(4) 0.029(3) 0.078(5) 0.000(3) 0.005(4) 0.015(3) C12B 0.077(4) 0.028(3) 0.053(4) -0.008(2) 0.002(3) -0.010(3) C11B 0.050(3) 0.038(3) 0.062(4) -0.006(3) 0.000(3) -0.022(2) O8C 0.044(2) 0.0278(17) 0.0361(19) 0.0065(14) 0.0052(16) 0.0026(14) N8C 0.026(2) 0.0257(19) 0.036(2) 0.0044(16) -0.0037(17) 0.0033(15) C8C 0.032(2) 0.024(2) 0.047(3) 0.004(2) 0.003(2) 0.0099(18) C7C 0.035(3) 0.022(2) 0.048(3) 0.003(2) 0.007(2) 0.0054(18) C9C 0.041(3) 0.027(2) 0.039(3) 0.005(2) 0.008(2) 0.004(2) O7C 0.049(2) 0.0230(17) 0.056(2) 0.0021(15) 0.0099(18) 0.0173(15) C6C 0.049(3) 0.024(2) 0.056(4) 0.004(2) 0.004(2) 0.005(2) C5C 0.050(3) 0.052(3) 0.059(4) 0.009(3) 0.006(3) -0.004(3) C1C 0.047(3) 0.057(3) 0.057(4) 0.011(3) 0.006(3) 0.015(3) C2C 0.060(4) 0.057(4) 0.076(4) 0.017(3) 0.002(3) 0.016(3) C3C 0.068(4) 0.045(3) 0.066(4) 0.014(3) -0.020(3) 0.001(3) C4C 0.072(4) 0.064(4) 0.062(4) 0.016(3) 0.009(3) -0.010(3) C14C 0.037(3) 0.025(2) 0.051(3) 0.005(2) 0.006(2) 0.0045(19) C10C 0.044(3) 0.032(3) 0.049(3) 0.002(2) 0.016(2) -0.001(2) C11C 0.051(3) 0.028(3) 0.056(3) 0.002(2) 0.012(3) -0.002(2) C12C 0.052(3) 0.025(2) 0.056(3) 0.003(2) 0.009(3) -0.006(2) C13C 0.060(4) 0.032(3) 0.049(3) -0.001(2) 0.019(3) 0.001(2) O8D 0.047(2) 0.0284(17) 0.046(2) 0.0021(15) 0.0045(17) 0.0158(15) N8D 0.036(2) 0.033(2) 0.036(2) 0.0015(17) -0.0021(18) 0.0070(17) C8D 0.040(3) 0.029(2) 0.040(3) -0.004(2) -0.022(2) 0.002(2) C7D 0.031(3) 0.027(2) 0.047(3) -0.001(2) -0.012(2) 0.0027(19) C9D 0.031(3) 0.034(3) 0.046(3) -0.005(2) -0.018(2) 0.006(2) O7D 0.0374(18) 0.0258(16) 0.0321(17) -0.0009(13) -0.0074(14) -0.0007(13) C6D 0.035(3) 0.039(3) 0.078(4) -0.024(3) -0.023(3) 0.012(2) C1D 0.064(4) 0.141(7) 0.058(4) -0.025(4) -0.019(4) 0.026(5) C5D 0.053(4) 0.074(5) 0.178(8) 0.043(5) -0.028(5) -0.022(4) C4D 0.055(5) 0.100(7) 0.258(11) 0.033(7) -0.049(6) -0.035(5) C3D 0.062(5) 0.097(7) 0.200(10) -0.057(6) -0.059(6) 0.010(5) C2D 0.074(5) 0.168(9) 0.102(7) -0.072(6) -0.041(5) 0.066(5) C14D 0.037(3) 0.040(3) 0.054(3) -0.005(2) -0.012(3) 0.005(2) C10D 0.046(3) 0.029(3) 0.071(4) -0.002(3) -0.001(3) 0.005(2) C11D 0.071(4) 0.027(3) 0.079(5) 0.002(3) 0.001(4) 0.005(3) C12D 0.051(3) 0.026(3) 0.076(4) -0.012(3) -0.019(3) 0.002(2) C13D 0.040(3) 0.041(3) 0.064(4) -0.022(3) -0.011(3) 0.008(2) O1E 0.066(4) 0.052(3) 0.031(3) 0.000 0.000 -0.020(3) C2E 0.090(6) 0.106(6) 0.063(5) -0.004(4) 0.005(4) -0.040(5) C3E 0.207(14) 0.134(10) 0.167(12) -0.086(9) 0.011(10) -0.054(9) O1F 0.043(3) 0.018(3) 0.056(4) -0.004(3) -0.018(4) -0.003(2) O1G 0.050(2) 0.065(3) 0.067(3) 0.004(3) -0.002(2) 0.0036(19) C2G 0.079(6) 0.216(13) 0.080(6) -0.018(7) -0.035(5) 0.067(7) O1H 0.067(4) 0.094(5) 0.042(4) 0.000 0.000 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O7C 1.996(3) 8_454 ? Ni1 O7C 1.996(3) . ? Ni1 O1H 1.999(7) . ? Ni1 O8D 2.012(4) 8_454 ? Ni1 O8D 2.012(4) . ? Ni2 O7D 1.826(3) . ? Ni2 O7C 1.835(4) . ? Ni2 N8D 1.854(4) . ? Ni2 N8C 1.865(4) . ? Ni3 O7D 1.999(3) . ? Ni3 O8B 2.004(3) . ? Ni3 O8C 2.007(3) . ? Ni3 O7A 2.014(4) . ? Ni3 O1G 2.059(4) . ? Ni3 O1F 2.392(6) . ? Ni4 O7A 1.827(3) . ? Ni4 O7B 1.844(3) . ? Ni4 N8B 1.847(4) . ? Ni4 N8A 1.853(4) . ? Ni5 O7B 1.996(3) 8_454 ? Ni5 O7B 1.996(3) . ? Ni5 O8A 2.002(3) . ? Ni5 O8A 2.002(3) 8_454 ? Ni5 O1E 2.043(6) . ? O8A N8A 1.334(5) . ? N8A C8A 1.304(6) . ? C8A C9A 1.480(6) . ? C8A C7A 1.498(7) . ? C9A C10A 1.369(7) . ? C9A C14A 1.389(8) . ? C7A O7A 1.424(5) . ? C7A C6A 1.519(7) . ? C7A H7A 1.0000 . ? C6A C1A 1.365(8) . ? C6A C5A 1.382(8) . ? C1A C2A 1.370(9) . ? C1A H1A 0.9500 . ? C5A C4A 1.393(8) . ? C5A H5A 0.9500 . ? C4A C3A 1.367(10) . ? C4A H4A 0.9500 . ? C3A C2A 1.402(11) . ? C3A H3A 0.9500 . ? C2A H2A 0.9500 . ? C10A C11A 1.383(7) . ? C10A H10A 0.9500 . ? C14A C13A 1.413(7) . ? C14A H14A 0.9500 . ? C13A C12A 1.369(8) . ? C13A H13A 0.9500 . ? C12A C11A 1.348(8) . ? C12A H12A 0.9500 . ? C11A H11A 0.9500 . ? O8B N8B 1.337(5) . ? N8B C8B 1.277(6) . ? C8B C9B 1.506(6) . ? C8B C7B 1.528(8) . ? C7B O7B 1.406(6) . ? C7B C6B 1.477(9) . ? C7B H7B 1.0000 . ? C9B C10B 1.385(7) . ? C9B C14B 1.386(7) . ? C6B C5B 1.390(9) . ? C6B C1B 1.398(10) . ? C1B C2B 1.372(10) . ? C1B H1B 0.9500 . ? C5B C4B 1.380(12) . ? C5B H5B 0.9500 . ? C4B C3B 1.360(14) . ? C4B H4B 0.9500 . ? C3B C2B 1.356(13) . ? C3B H3B 0.9500 . ? C2B H2B 0.9500 . ? C10B C11B 1.367(7) . ? C10B H10B 0.9500 . ? C14B C13B 1.377(8) . ? C14B H14B 0.9500 . ? C13B C12B 1.362(9) . ? C13B H13B 0.9500 . ? C12B C11B 1.348(9) . ? C12B H12B 0.9500 . ? C11B H11B 0.9500 . ? O8C N8C 1.323(5) . ? N8C C8C 1.295(6) . ? C8C C9C 1.488(7) . ? C8C C7C 1.503(7) . ? C7C O7C 1.407(6) . ? C7C C6C 1.525(7) . ? C7C H7C 1.0000 . ? C9C C14C 1.385(7) . ? C9C C10C 1.387(7) . ? C6C C5C 1.370(8) . ? C6C C1C 1.388(8) . ? C5C C4C 1.377(9) . ? C5C H5C 0.9500 . ? C1C C2C 1.359(9) . ? C1C H1C 0.9500 . ? C2C C3C 1.379(10) . ? C2C H2C 0.9500 . ? C3C C4C 1.383(9) . ? C3C H3C 0.9500 . ? C4C H4C 0.9500 . ? C14C C13C 1.387(7) . ? C14C H14C 0.9500 . ? C10C C11C 1.390(7) . ? C10C H10C 0.9500 . ? C11C C12C 1.378(7) . ? C11C H11C 0.9500 . ? C12C C13C 1.344(8) . ? C12C H12C 0.9500 . ? C13C H13C 0.9500 . ? O8D N8D 1.327(5) . ? N8D C8D 1.288(6) . ? C8D C9D 1.486(7) . ? C8D C7D 1.518(7) . ? C7D O7D 1.428(5) . ? C7D C6D 1.530(7) . ? C7D H7D 1.0000 . ? C9D C14D 1.378(8) . ? C9D C10D 1.399(8) . ? C6D C1D 1.349(10) . ? C6D C5D 1.387(11) . ? C1D C2D 1.403(12) . ? C1D H1D 0.9500 . ? C5D C4D 1.379(11) . ? C5D H5D 0.9500 . ? C4D C3D 1.287(17) . ? C4D H4D 0.9500 . ? C3D C2D 1.297(17) . ? C3D H3D 0.9500 . ? C2D H2D 0.9500 . ? C14D C13D 1.418(7) . ? C14D H14D 0.9500 . ? C10D C11D 1.388(7) . ? C10D H10D 0.9500 . ? C11D C12D 1.352(9) . ? C11D H11D 0.9500 . ? C12D C13D 1.361(9) . ? C12D H12D 0.9500 . ? C13D H13D 0.9500 . ? O1E C2E 1.448(8) . ? O1E C2E 1.448(8) 8_454 ? C2E C3E 1.365(13) . ? C2E H2EA 0.9900 . ? C2E H2EB 0.9900 . ? C3E H3EA 0.9800 . ? C3E H3EB 0.9800 . ? C3E H3EC 0.9800 . ? O1F C2F 1.685(10) . ? O1F C3F 1.808(11) 8_454 ? O1F H2F4 1.0720 . ? C2F C3F 1.458(11) . ? C2F H2F1 0.9900 . ? C2F H2F2 0.9900 . ? C2F H2F3 0.9800 . ? C2F H2F4 0.9797 . ? C2F H2F5 0.9802 . ? C3F O1F 1.808(11) 8_454 ? C3F H3F1 0.9900 . ? C3F H3F2 0.9900 . ? C3F H3F3 0.9801 . ? C3F H3F4 0.9801 . ? C3F H3F5 0.9797 . ? O1G C2G 1.383(9) . ? O1G H1G 0.9500 . ? C2G H2GA 0.9800 . ? C2G H2GB 0.9800 . ? C2G H2GC 0.9800 . ? O1H H1H1 0.9801 . ? O1H H1H2 0.9801 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7C Ni1 O7C 145.9(2) 8_454 . ? O7C Ni1 O1H 107.07(11) 8_454 . ? O7C Ni1 O1H 107.07(11) . . ? O7C Ni1 O8D 87.30(14) 8_454 8_454 ? O7C Ni1 O8D 91.79(14) . 8_454 ? O1H Ni1 O8D 91.54(11) . 8_454 ? O7C Ni1 O8D 91.79(14) 8_454 . ? O7C Ni1 O8D 87.30(14) . . ? O1H Ni1 O8D 91.54(11) . . ? O8D Ni1 O8D 176.9(2) 8_454 . ? O7D Ni2 O7C 179.09(18) . . ? O7D Ni2 N8D 86.25(17) . . ? O7C Ni2 N8D 94.17(17) . . ? O7D Ni2 N8C 93.59(16) . . ? O7C Ni2 N8C 85.90(16) . . ? N8D Ni2 N8C 173.16(17) . . ? O7D Ni3 O8B 92.31(14) . . ? O7D Ni3 O8C 87.42(14) . . ? O8B Ni3 O8C 172.64(14) . . ? O7D Ni3 O7A 170.84(14) . . ? O8B Ni3 O7A 87.62(14) . . ? O8C Ni3 O7A 91.48(14) . . ? O7D Ni3 O1G 95.24(17) . . ? O8B Ni3 O1G 91.14(16) . . ? O8C Ni3 O1G 96.21(16) . . ? O7A Ni3 O1G 93.92(17) . . ? O7D Ni3 O1F 85.8(2) . . ? O8B Ni3 O1F 85.84(18) . . ? O8C Ni3 O1F 86.81(19) . . ? O7A Ni3 O1F 85.1(2) . . ? O1G Ni3 O1F 176.9(2) . . ? O7A Ni4 O7B 178.77(18) . . ? O7A Ni4 N8B 94.15(16) . . ? O7B Ni4 N8B 86.24(17) . . ? O7A Ni4 N8A 86.10(16) . . ? O7B Ni4 N8A 93.59(16) . . ? N8B Ni4 N8A 176.28(18) . . ? O7B Ni5 O7B 143.4(2) 8_454 . ? O7B Ni5 O8A 91.27(13) 8_454 . ? O7B Ni5 O8A 88.09(13) . . ? O7B Ni5 O8A 88.09(13) 8_454 8_454 ? O7B Ni5 O8A 91.27(13) . 8_454 ? O8A Ni5 O8A 178.0(2) . 8_454 ? O7B Ni5 O1E 108.32(12) 8_454 . ? O7B Ni5 O1E 108.32(12) . . ? O8A Ni5 O1E 91.02(10) . . ? O8A Ni5 O1E 91.02(10) 8_454 . ? N8A O8A Ni5 111.9(3) . . ? C8A N8A O8A 121.6(4) . . ? C8A N8A Ni4 115.7(3) . . ? O8A N8A Ni4 122.4(3) . . ? N8A C8A C9A 125.4(5) . . ? N8A C8A C7A 114.2(4) . . ? C9A C8A C7A 120.4(4) . . ? C10A C9A C14A 118.5(5) . . ? C10A C9A C8A 120.5(5) . . ? C14A C9A C8A 120.9(5) . . ? O7A C7A C8A 109.4(4) . . ? O7A C7A C6A 109.2(4) . . ? C8A C7A C6A 112.2(4) . . ? O7A C7A H7A 108.6 . . ? C8A C7A H7A 108.6 . . ? C6A C7A H7A 108.6 . . ? C7A O7A Ni4 114.4(3) . . ? C7A O7A Ni3 125.5(3) . . ? Ni4 O7A Ni3 110.24(16) . . ? C1A C6A C5A 119.0(5) . . ? C1A C6A C7A 122.3(5) . . ? C5A C6A C7A 118.7(5) . . ? C6A C1A C2A 121.6(6) . . ? C6A C1A H1A 119.2 . . ? C2A C1A H1A 119.2 . . ? C6A C5A C4A 120.9(6) . . ? C6A C5A H5A 119.6 . . ? C4A C5A H5A 119.6 . . ? C3A C4A C5A 119.0(6) . . ? C3A C4A H4A 120.5 . . ? C5A C4A H4A 120.5 . . ? C4A C3A C2A 120.5(6) . . ? C4A C3A H3A 119.8 . . ? C2A C3A H3A 119.8 . . ? C1A C2A C3A 119.0(6) . . ? C1A C2A H2A 120.5 . . ? C3A C2A H2A 120.5 . . ? C9A C10A C11A 121.0(5) . . ? C9A C10A H10A 119.5 . . ? C11A C10A H10A 119.5 . . ? C9A C14A C13A 119.4(6) . . ? C9A C14A H14A 120.3 . . ? C13A C14A H14A 120.3 . . ? C12A C13A C14A 120.4(6) . . ? C12A C13A H13A 119.8 . . ? C14A C13A H13A 119.8 . . ? C11A C12A C13A 119.3(5) . . ? C11A C12A H12A 120.4 . . ? C13A C12A H12A 120.4 . . ? C12A C11A C10A 121.4(5) . . ? C12A C11A H11A 119.3 . . ? C10A C11A H11A 119.3 . . ? N8B O8B Ni3 112.7(3) . . ? C8B N8B O8B 121.1(4) . . ? C8B N8B Ni4 116.4(3) . . ? O8B N8B Ni4 122.1(3) . . ? N8B C8B C9B 125.2(5) . . ? N8B C8B C7B 113.6(4) . . ? C9B C8B C7B 121.2(4) . . ? O7B C7B C6B 111.1(5) . . ? O7B C7B C8B 109.6(4) . . ? C6B C7B C8B 110.9(4) . . ? O7B C7B H7B 108.4 . . ? C6B C7B H7B 108.4 . . ? C8B C7B H7B 108.4 . . ? C10B C9B C14B 118.6(5) . . ? C10B C9B C8B 121.2(4) . . ? C14B C9B C8B 120.1(5) . . ? C7B O7B Ni4 113.5(3) . . ? C7B O7B Ni5 129.3(3) . . ? Ni4 O7B Ni5 110.39(16) . . ? C5B C6B C1B 116.6(7) . . ? C5B C6B C7B 123.5(7) . . ? C1B C6B C7B 119.9(5) . . ? C2B C1B C6B 121.9(8) . . ? C2B C1B H1B 119.0 . . ? C6B C1B H1B 119.0 . . ? C4B C5B C6B 121.0(9) . . ? C4B C5B H5B 119.5 . . ? C6B C5B H5B 119.5 . . ? C3B C4B C5B 120.2(8) . . ? C3B C4B H4B 119.9 . . ? C5B C4B H4B 119.9 . . ? C2B C3B C4B 120.7(9) . . ? C2B C3B H3B 119.6 . . ? C4B C3B H3B 119.6 . . ? C3B C2B C1B 119.5(10) . . ? C3B C2B H2B 120.2 . . ? C1B C2B H2B 120.2 . . ? C11B C10B C9B 120.1(5) . . ? C11B C10B H10B 120.0 . . ? C9B C10B H10B 120.0 . . ? C13B C14B C9B 119.3(6) . . ? C13B C14B H14B 120.3 . . ? C9B C14B H14B 120.3 . . ? C12B C13B C14B 121.4(5) . . ? C12B C13B H13B 119.3 . . ? C14B C13B H13B 119.3 . . ? C11B C12B C13B 119.1(5) . . ? C11B C12B H12B 120.4 . . ? C13B C12B H12B 120.4 . . ? C12B C11B C10B 121.5(5) . . ? C12B C11B H11B 119.3 . . ? C10B C11B H11B 119.3 . . ? N8C O8C Ni3 113.6(3) . . ? C8C N8C O8C 122.6(4) . . ? C8C N8C Ni2 115.3(3) . . ? O8C N8C Ni2 121.7(3) . . ? N8C C8C C9C 124.5(4) . . ? N8C C8C C7C 113.5(4) . . ? C9C C8C C7C 122.0(4) . . ? O7C C7C C8C 109.7(4) . . ? O7C C7C C6C 108.6(4) . . ? C8C C7C C6C 111.7(4) . . ? O7C C7C H7C 108.9 . . ? C8C C7C H7C 108.9 . . ? C6C C7C H7C 108.9 . . ? C14C C9C C10C 118.8(5) . . ? C14C C9C C8C 121.6(4) . . ? C10C C9C C8C 119.5(4) . . ? C7C O7C Ni2 113.3(3) . . ? C7C O7C Ni1 130.1(3) . . ? Ni2 O7C Ni1 110.94(16) . . ? C5C C6C C1C 118.1(5) . . ? C5C C6C C7C 121.3(5) . . ? C1C C6C C7C 120.6(5) . . ? C6C C5C C4C 121.9(6) . . ? C6C C5C H5C 119.1 . . ? C4C C5C H5C 119.1 . . ? C2C C1C C6C 120.1(6) . . ? C2C C1C H1C 119.9 . . ? C6C C1C H1C 119.9 . . ? C1C C2C C3C 122.0(6) . . ? C1C C2C H2C 119.0 . . ? C3C C2C H2C 119.0 . . ? C2C C3C C4C 118.0(6) . . ? C2C C3C H3C 121.0 . . ? C4C C3C H3C 121.0 . . ? C5C C4C C3C 119.7(6) . . ? C5C C4C H4C 120.1 . . ? C3C C4C H4C 120.1 . . ? C9C C14C C13C 120.0(5) . . ? C9C C14C H14C 120.0 . . ? C13C C14C H14C 120.0 . . ? C9C C10C C11C 120.0(5) . . ? C9C C10C H10C 120.0 . . ? C11C C10C H10C 120.0 . . ? C12C C11C C10C 120.0(5) . . ? C12C C11C H11C 120.0 . . ? C10C C11C H11C 120.0 . . ? C13C C12C C11C 120.0(5) . . ? C13C C12C H12C 120.0 . . ? C11C C12C H12C 120.0 . . ? C12C C13C C14C 121.1(5) . . ? C12C C13C H13C 119.5 . . ? C14C C13C H13C 119.5 . . ? N8D O8D Ni1 113.3(3) . . ? C8D N8D O8D 121.7(4) . . ? C8D N8D Ni2 116.8(4) . . ? O8D N8D Ni2 121.3(3) . . ? N8D C8D C9D 125.4(5) . . ? N8D C8D C7D 113.1(4) . . ? C9D C8D C7D 121.4(5) . . ? O7D C7D C8D 109.8(4) . . ? O7D C7D C6D 108.7(4) . . ? C8D C7D C6D 112.1(4) . . ? O7D C7D H7D 108.7 . . ? C8D C7D H7D 108.7 . . ? C6D C7D H7D 108.7 . . ? C14D C9D C10D 119.4(5) . . ? C14D C9D C8D 121.8(5) . . ? C10D C9D C8D 118.8(5) . . ? C7D O7D Ni2 113.7(3) . . ? C7D O7D Ni3 125.8(3) . . ? Ni2 O7D Ni3 111.44(16) . . ? C1D C6D C5D 117.0(7) . . ? C1D C6D C7D 122.4(7) . . ? C5D C6D C7D 120.4(6) . . ? C6D C1D C2D 121.3(10) . . ? C6D C1D H1D 119.3 . . ? C2D C1D H1D 119.3 . . ? C4D C5D C6D 118.2(10) . . ? C4D C5D H5D 120.9 . . ? C6D C5D H5D 120.9 . . ? C3D C4D C5D 122.9(12) . . ? C3D C4D H4D 118.6 . . ? C5D C4D H4D 118.6 . . ? C4D C3D C2D 121.3(10) . . ? C4D C3D H3D 119.4 . . ? C2D C3D H3D 119.4 . . ? C3D C2D C1D 119.2(11) . . ? C3D C2D H2D 120.4 . . ? C1D C2D H2D 120.4 . . ? C9D C14D C13D 119.1(6) . . ? C9D C14D H14D 120.5 . . ? C13D C14D H14D 120.5 . . ? C11D C10D C9D 119.8(6) . . ? C11D C10D H10D 120.1 . . ? C9D C10D H10D 120.1 . . ? C12D C11D C10D 120.9(6) . . ? C12D C11D H11D 119.6 . . ? C10D C11D H11D 119.6 . . ? C11D C12D C13D 120.4(5) . . ? C11D C12D H12D 119.8 . . ? C13D C12D H12D 119.8 . . ? C12D C13D C14D 120.5(6) . . ? C12D C13D H13D 119.8 . . ? C14D C13D H13D 119.8 . . ? C2E O1E C2E 116.9(7) . 8_454 ? C2E O1E Ni5 121.6(4) . . ? C2E O1E Ni5 121.6(4) 8_454 . ? C3E C2E O1E 119.4(9) . . ? C3E C2E H2EA 107.5 . . ? O1E C2E H2EA 107.5 . . ? C3E C2E H2EB 107.5 . . ? O1E C2E H2EB 107.5 . . ? H2EA C2E H2EB 107.0 . . ? C2E C3E H3EA 109.5 . . ? C2E C3E H3EB 109.5 . . ? H3EA C3E H3EB 109.5 . . ? C2E C3E H3EC 109.5 . . ? H3EA C3E H3EC 109.5 . . ? H3EB C3E H3EC 109.5 . . ? C2F O1F C3F 113.8(5) . 8_454 ? C2F O1F Ni3 123.0(4) . . ? C3F O1F Ni3 123.2(4) 8_454 . ? C2F O1F H2F4 33.0 . . ? C3F O1F H2F4 99.8 8_454 . ? Ni3 O1F H2F4 126.5 . . ? C3F C2F O1F 100.7(7) . . ? C3F C2F H2F1 111.6 . . ? O1F C2F H2F1 111.6 . . ? C3F C2F H2F2 111.6 . . ? O1F C2F H2F2 111.6 . . ? H2F1 C2F H2F2 109.4 . . ? C3F C2F H2F3 107.6 . . ? O1F C2F H2F3 81.2 . . ? H2F1 C2F H2F3 135.0 . . ? H2F2 C2F H2F3 32.7 . . ? C3F C2F H2F4 112.1 . . ? O1F C2F H2F4 36.6 . . ? H2F1 C2F H2F4 75.2 . . ? H2F2 C2F H2F4 129.9 . . ? H2F3 C2F H2F4 109.5 . . ? C3F C2F H2F5 108.7 . . ? O1F C2F H2F5 143.2 . . ? H2F1 C2F H2F5 36.6 . . ? H2F2 C2F H2F5 77.8 . . ? H2F3 C2F H2F5 109.5 . . ? H2F4 C2F H2F5 109.5 . . ? C2F C3F O1F 102.0(7) . 8_454 ? C2F C3F H3F1 111.4 . . ? O1F C3F H3F1 111.4 8_454 . ? C2F C3F H3F2 111.4 . . ? O1F C3F H3F2 111.4 8_454 . ? H3F1 C3F H3F2 109.2 . . ? C2F C3F H3F3 107.2 . . ? O1F C3F H3F3 12.3 8_454 . ? H3F1 C3F H3F3 117.9 . . ? H3F2 C3F H3F3 99.1 . . ? C2F C3F H3F4 109.2 . . ? O1F C3F H3F4 101.7 8_454 . ? H3F1 C3F H3F4 11.3 . . ? H3F2 C3F H3F4 119.4 . . ? H3F3 C3F H3F4 109.5 . . ? C2F C3F H3F5 111.9 . . ? O1F C3F H3F5 121.6 8_454 . ? H3F1 C3F H3F5 98.9 . . ? H3F2 C3F H3F5 11.7 . . ? H3F3 C3F H3F5 109.5 . . ? H3F4 C3F H3F5 109.5 . . ? C2G O1G Ni3 125.1(5) . . ? C2G O1G H1G 117.4 . . ? Ni3 O1G H1G 117.4 . . ? O1G C2G H2GA 109.5 . . ? O1G C2G H2GB 109.5 . . ? H2GA C2G H2GB 109.5 . . ? O1G C2G H2GC 109.5 . . ? H2GA C2G H2GC 109.5 . . ? H2GB C2G H2GC 109.5 . . ? Ni1 O1H H1H1 109.5 . . ? Ni1 O1H H1H2 109.5 . . ? H1H1 O1H H1H2 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7B Ni5 O8A N8A -111.0(3) 8_454 . . . ? O7B Ni5 O8A N8A 32.3(3) . . . . ? O8A Ni5 O8A N8A -39.4(3) 8_454 . . . ? O1E Ni5 O8A N8A 140.6(3) . . . . ? Ni5 O8A N8A C8A 153.3(3) . . . . ? Ni5 O8A N8A Ni4 -21.2(4) . . . . ? O7A Ni4 N8A C8A 2.8(3) . . . . ? O7B Ni4 N8A C8A -178.4(3) . . . . ? N8B Ni4 N8A C8A -91(3) . . . . ? O7A Ni4 N8A O8A 177.5(3) . . . . ? O7B Ni4 N8A O8A -3.6(4) . . . . ? N8B Ni4 N8A O8A 84(3) . . . . ? O8A N8A C8A C9A -0.7(7) . . . . ? Ni4 N8A C8A C9A 174.1(4) . . . . ? O8A N8A C8A C7A -179.1(4) . . . . ? Ni4 N8A C8A C7A -4.3(5) . . . . ? N8A C8A C9A C10A -142.3(5) . . . . ? C7A C8A C9A C10A 36.0(7) . . . . ? N8A C8A C9A C14A 40.3(7) . . . . ? C7A C8A C9A C14A -141.4(5) . . . . ? N8A C8A C7A O7A 3.8(6) . . . . ? C9A C8A C7A O7A -174.7(4) . . . . ? N8A C8A C7A C6A -117.6(4) . . . . ? C9A C8A C7A C6A 63.9(5) . . . . ? C8A C7A O7A Ni4 -1.6(5) . . . . ? C6A C7A O7A Ni4 121.6(4) . . . . ? C8A C7A O7A Ni3 140.7(3) . . . . ? C6A C7A O7A Ni3 -96.1(4) . . . . ? O7B Ni4 O7A C7A -76(7) . . . . ? N8B Ni4 O7A C7A 175.9(3) . . . . ? N8A Ni4 O7A C7A -0.4(3) . . . . ? O7B Ni4 O7A Ni3 136(7) . . . . ? N8B Ni4 O7A Ni3 27.9(2) . . . . ? N8A Ni4 O7A Ni3 -148.35(19) . . . . ? O7D Ni3 O7A C7A -87.8(9) . . . . ? O8B Ni3 O7A C7A -177.5(4) . . . . ? O8C Ni3 O7A C7A -4.9(4) . . . . ? O1G Ni3 O7A C7A 91.5(4) . . . . ? O1F Ni3 O7A C7A -91.5(4) . . . . ? O7D Ni3 O7A Ni4 55.8(9) . . . . ? O8B Ni3 O7A Ni4 -33.97(17) . . . . ? O8C Ni3 O7A Ni4 138.72(18) . . . . ? O1G Ni3 O7A Ni4 -124.95(19) . . . . ? O1F Ni3 O7A Ni4 52.1(2) . . . . ? O7A C7A C6A C1A -91.8(6) . . . . ? C8A C7A C6A C1A 29.6(7) . . . . ? O7A C7A C6A C5A 85.8(6) . . . . ? C8A C7A C6A C5A -152.8(5) . . . . ? C5A C6A C1A C2A -2.0(10) . . . . ? C7A C6A C1A C2A 175.6(7) . . . . ? C1A C6A C5A C4A 2.9(9) . . . . ? C7A C6A C5A C4A -174.8(6) . . . . ? C6A C5A C4A C3A -3.1(11) . . . . ? C5A C4A C3A C2A 2.4(13) . . . . ? C6A C1A C2A C3A 1.4(13) . . . . ? C4A C3A C2A C1A -1.6(14) . . . . ? C14A C9A C10A C11A -0.7(8) . . . . ? C8A C9A C10A C11A -178.1(5) . . . . ? C10A C9A C14A C13A -0.4(9) . . . . ? C8A C9A C14A C13A 177.1(6) . . . . ? C9A C14A C13A C12A 1.8(11) . . . . ? C14A C13A C12A C11A -2.2(10) . . . . ? C13A C12A C11A C10A 1.1(9) . . . . ? C9A C10A C11A C12A 0.3(8) . . . . ? O7D Ni3 O8B N8B -140.3(3) . . . . ? O8C Ni3 O8B N8B -52.5(13) . . . . ? O7A Ni3 O8B N8B 30.6(3) . . . . ? O1G Ni3 O8B N8B 124.4(3) . . . . ? O1F Ni3 O8B N8B -54.7(3) . . . . ? Ni3 O8B N8B C8B 154.8(4) . . . . ? Ni3 O8B N8B Ni4 -18.2(4) . . . . ? O7A Ni4 N8B C8B -179.9(4) . . . . ? O7B Ni4 N8B C8B 1.3(4) . . . . ? N8A Ni4 N8B C8B -86(3) . . . . ? O7A Ni4 N8B O8B -6.5(4) . . . . ? O7B Ni4 N8B O8B 174.6(4) . . . . ? N8A Ni4 N8B O8B 87(3) . . . . ? O8B N8B C8B C9B 2.4(8) . . . . ? Ni4 N8B C8B C9B 175.8(4) . . . . ? O8B N8B C8B C7B -179.5(4) . . . . ? Ni4 N8B C8B C7B -6.1(6) . . . . ? N8B C8B C7B O7B 9.1(7) . . . . ? C9B C8B C7B O7B -172.7(4) . . . . ? N8B C8B C7B C6B -113.9(5) . . . . ? C9B C8B C7B C6B 64.3(7) . . . . ? N8B C8B C9B C10B 43.2(8) . . . . ? C7B C8B C9B C10B -134.8(6) . . . . ? N8B C8B C9B C14B -138.2(6) . . . . ? C7B C8B C9B C14B 43.8(8) . . . . ? C6B C7B O7B Ni4 114.9(4) . . . . ? C8B C7B O7B Ni4 -8.0(6) . . . . ? C6B C7B O7B Ni5 -97.3(5) . . . . ? C8B C7B O7B Ni5 139.8(4) . . . . ? O7A Ni4 O7B C7B -104(7) . . . . ? N8B Ni4 O7B C7B 4.3(4) . . . . ? N8A Ni4 O7B C7B -179.4(4) . . . . ? O7A Ni4 O7B Ni5 102(7) . . . . ? N8B Ni4 O7B Ni5 -149.6(2) . . . . ? N8A Ni4 O7B Ni5 26.7(2) . . . . ? O7B Ni5 O7B C7B -93.0(5) 8_454 . . . ? O8A Ni5 O7B C7B 177.4(5) . . . . ? O8A Ni5 O7B C7B -4.5(5) 8_454 . . . ? O1E Ni5 O7B C7B 87.0(5) . . . . ? O7B Ni5 O7B Ni4 55.53(16) 8_454 . . . ? O8A Ni5 O7B Ni4 -34.0(2) . . . . ? O8A Ni5 O7B Ni4 144.0(2) 8_454 . . . ? O1E Ni5 O7B Ni4 -124.47(16) . . . . ? O7B C7B C6B C5B 122.9(6) . . . . ? C8B C7B C6B C5B -115.0(6) . . . . ? O7B C7B C6B C1B -54.5(7) . . . . ? C8B C7B C6B C1B 67.6(7) . . . . ? C5B C6B C1B C2B -1.0(10) . . . . ? C7B C6B C1B C2B 176.6(6) . . . . ? C1B C6B C5B C4B 0.9(10) . . . . ? C7B C6B C5B C4B -176.6(6) . . . . ? C6B C5B C4B C3B 0.3(12) . . . . ? C5B C4B C3B C2B -1.4(13) . . . . ? C4B C3B C2B C1B 1.3(13) . . . . ? C6B C1B C2B C3B -0.1(12) . . . . ? C14B C9B C10B C11B 1.4(8) . . . . ? C8B C9B C10B C11B -179.9(5) . . . . ? C10B C9B C14B C13B -1.7(9) . . . . ? C8B C9B C14B C13B 179.6(6) . . . . ? C9B C14B C13B C12B 1.4(10) . . . . ? C14B C13B C12B C11B -0.7(10) . . . . ? C13B C12B C11B C10B 0.3(10) . . . . ? C9B C10B C11B C12B -0.7(9) . . . . ? O7D Ni3 O8C N8C 29.6(3) . . . . ? O8B Ni3 O8C N8C -58.4(13) . . . . ? O7A Ni3 O8C N8C -141.3(3) . . . . ? O1G Ni3 O8C N8C 124.6(3) . . . . ? O1F Ni3 O8C N8C -56.3(3) . . . . ? Ni3 O8C N8C C8C 154.7(4) . . . . ? Ni3 O8C N8C Ni2 -17.7(4) . . . . ? O7D Ni2 N8C C8C -179.0(3) . . . . ? O7C Ni2 N8C C8C 0.2(3) . . . . ? N8D Ni2 N8C C8C -90.6(16) . . . . ? O7D Ni2 N8C O8C -6.2(3) . . . . ? O7C Ni2 N8C O8C 173.1(3) . . . . ? N8D Ni2 N8C O8C 82.3(16) . . . . ? O8C N8C C8C C9C 0.0(7) . . . . ? Ni2 N8C C8C C9C 172.7(4) . . . . ? O8C N8C C8C C7C 178.0(4) . . . . ? Ni2 N8C C8C C7C -9.2(5) . . . . ? N8C C8C C7C O7C 16.2(6) . . . . ? C9C C8C C7C O7C -165.7(4) . . . . ? N8C C8C C7C C6C -104.3(5) . . . . ? C9C C8C C7C C6C 73.8(6) . . . . ? N8C C8C C9C C14C 42.0(8) . . . . ? C7C C8C C9C C14C -135.9(5) . . . . ? N8C C8C C9C C10C -140.7(5) . . . . ? C7C C8C C9C C10C 41.4(7) . . . . ? C8C C7C O7C Ni2 -15.9(5) . . . . ? C6C C7C O7C Ni2 106.4(4) . . . . ? C8C C7C O7C Ni1 134.7(4) . . . . ? C6C C7C O7C Ni1 -103.0(5) . . . . ? O7D Ni2 O7C C7C 66(10) . . . . ? N8D Ni2 O7C C7C -177.4(3) . . . . ? N8C Ni2 O7C C7C 9.5(3) . . . . ? O7D Ni2 O7C Ni1 -91(10) . . . . ? N8D Ni2 O7C Ni1 26.4(2) . . . . ? N8C Ni2 O7C Ni1 -146.8(2) . . . . ? O7C Ni1 O7C C7C -95.0(4) 8_454 . . . ? O1H Ni1 O7C C7C 85.0(4) . . . . ? O8D Ni1 O7C C7C -7.2(4) 8_454 . . . ? O8D Ni1 O7C C7C 175.8(4) . . . . ? O7C Ni1 O7C Ni2 56.03(16) 8_454 . . . ? O1H Ni1 O7C Ni2 -123.97(16) . . . . ? O8D Ni1 O7C Ni2 143.9(2) 8_454 . . . ? O8D Ni1 O7C Ni2 -33.2(2) . . . . ? O7C C7C C6C C5C 92.4(6) . . . . ? C8C C7C C6C C5C -146.5(5) . . . . ? O7C C7C C6C C1C -84.6(6) . . . . ? C8C C7C C6C C1C 36.5(7) . . . . ? C1C C6C C5C C4C 0.8(9) . . . . ? C7C C6C C5C C4C -176.2(6) . . . . ? C5C C6C C1C C2C -3.1(9) . . . . ? C7C C6C C1C C2C 173.9(6) . . . . ? C6C C1C C2C C3C 1.2(11) . . . . ? C1C C2C C3C C4C 3.0(11) . . . . ? C6C C5C C4C C3C 3.4(10) . . . . ? C2C C3C C4C C5C -5.2(10) . . . . ? C10C C9C C14C C13C 1.0(8) . . . . ? C8C C9C C14C C13C 178.3(5) . . . . ? C14C C9C C10C C11C -2.0(8) . . . . ? C8C C9C C10C C11C -179.4(5) . . . . ? C9C C10C C11C C12C 3.2(9) . . . . ? C10C C11C C12C C13C -3.4(9) . . . . ? C11C C12C C13C C14C 2.4(9) . . . . ? C9C C14C C13C C12C -1.2(9) . . . . ? O7C Ni1 O8D N8D -114.0(3) 8_454 . . . ? O7C Ni1 O8D N8D 31.9(3) . . . . ? O1H Ni1 O8D N8D 138.9(3) . . . . ? O8D Ni1 O8D N8D -41.1(3) 8_454 . . . ? Ni1 O8D N8D C8D 154.0(4) . . . . ? Ni1 O8D N8D Ni2 -21.0(4) . . . . ? O7D Ni2 N8D C8D 0.4(4) . . . . ? O7C Ni2 N8D C8D -178.7(4) . . . . ? N8C Ni2 N8D C8D -88.4(16) . . . . ? O7D Ni2 N8D O8D 175.6(4) . . . . ? O7C Ni2 N8D O8D -3.6(4) . . . . ? N8C Ni2 N8D O8D 86.8(16) . . . . ? O8D N8D C8D C9D -2.5(7) . . . . ? Ni2 N8D C8D C9D 172.7(4) . . . . ? O8D N8D C8D C7D -178.9(4) . . . . ? Ni2 N8D C8D C7D -3.8(5) . . . . ? N8D C8D C7D O7D 6.0(5) . . . . ? C9D C8D C7D O7D -170.5(4) . . . . ? N8D C8D C7D C6D -114.9(5) . . . . ? C9D C8D C7D C6D 68.6(6) . . . . ? N8D C8D C9D C14D 23.1(7) . . . . ? C7D C8D C9D C14D -160.7(5) . . . . ? N8D C8D C9D C10D -157.9(5) . . . . ? C7D C8D C9D C10D 18.3(7) . . . . ? C8D C7D O7D Ni2 -5.7(4) . . . . ? C6D C7D O7D Ni2 117.3(4) . . . . ? C8D C7D O7D Ni3 138.3(3) . . . . ? C6D C7D O7D Ni3 -98.7(5) . . . . ? O7C Ni2 O7D C7D 120(10) . . . . ? N8D Ni2 O7D C7D 3.2(3) . . . . ? N8C Ni2 O7D C7D 176.4(3) . . . . ? O7C Ni2 O7D Ni3 -29(10) . . . . ? N8D Ni2 O7D Ni3 -146.00(19) . . . . ? N8C Ni2 O7D Ni3 27.14(19) . . . . ? O8B Ni3 O7D C7D -5.0(3) . . . . ? O8C Ni3 O7D C7D -177.6(3) . . . . ? O7A Ni3 O7D C7D -94.4(9) . . . . ? O1G Ni3 O7D C7D 86.4(3) . . . . ? O1F Ni3 O7D C7D -90.7(4) . . . . ? O8B Ni3 O7D Ni2 139.71(17) . . . . ? O8C Ni3 O7D Ni2 -32.93(17) . . . . ? O7A Ni3 O7D Ni2 50.3(9) . . . . ? O1G Ni3 O7D Ni2 -128.93(19) . . . . ? O1F Ni3 O7D Ni2 54.1(2) . . . . ? O7D C7D C6D C1D -68.0(7) . . . . ? C8D C7D C6D C1D 53.6(7) . . . . ? O7D C7D C6D C5D 108.1(7) . . . . ? C8D C7D C6D C5D -130.3(7) . . . . ? C5D C6D C1D C2D -1.7(12) . . . . ? C7D C6D C1D C2D 174.5(7) . . . . ? C1D C6D C5D C4D -1.1(13) . . . . ? C7D C6D C5D C4D -177.4(8) . . . . ? C6D C5D C4D C3D 2.8(18) . . . . ? C5D C4D C3D C2D -2(2) . . . . ? C4D C3D C2D C1D -1.4(18) . . . . ? C6D C1D C2D C3D 3.1(15) . . . . ? C10D C9D C14D C13D 0.4(7) . . . . ? C8D C9D C14D C13D 179.3(4) . . . . ? C14D C9D C10D C11D -0.4(8) . . . . ? C8D C9D C10D C11D -179.4(5) . . . . ? C9D C10D C11D C12D 0.5(9) . . . . ? C10D C11D C12D C13D -0.4(9) . . . . ? C11D C12D C13D C14D 0.4(9) . . . . ? C9D C14D C13D C12D -0.3(8) . . . . ? O7B Ni5 O1E C2E -9.5(5) 8_454 . . . ? O7B Ni5 O1E C2E 170.5(5) . . . . ? O8A Ni5 O1E C2E 82.2(5) . . . . ? O8A Ni5 O1E C2E -97.8(5) 8_454 . . . ? O7B Ni5 O1E C2E 170.5(5) 8_454 . . 8_454 ? O7B Ni5 O1E C2E -9.5(5) . . . 8_454 ? O8A Ni5 O1E C2E -97.8(5) . . . 8_454 ? O8A Ni5 O1E C2E 82.2(5) 8_454 . . 8_454 ? C2E O1E C2E C3E 68.7(9) 8_454 . . . ? Ni5 O1E C2E C3E -111.3(9) . . . . ? O7D Ni3 O1F C2F 42.9(6) . . . . ? O8B Ni3 O1F C2F -49.7(6) . . . . ? O8C Ni3 O1F C2F 130.6(6) . . . . ? O7A Ni3 O1F C2F -137.7(6) . . . . ? O1G Ni3 O1F C2F -66(4) . . . . ? O7D Ni3 O1F C3F -134.8(6) . . . 8_454 ? O8B Ni3 O1F C3F 132.6(6) . . . 8_454 ? O8C Ni3 O1F C3F -47.1(6) . . . 8_454 ? O7A Ni3 O1F C3F 44.6(6) . . . 8_454 ? O1G Ni3 O1F C3F 117(4) . . . 8_454 ? C3F O1F C2F C3F -42.6(8) 8_454 . . . ? Ni3 O1F C2F C3F 139.5(6) . . . . ? O1F C2F C3F O1F 73.4(6) . . . 8_454 ? O7D Ni3 O1G C2G 44.3(7) . . . . ? O8B Ni3 O1G C2G 136.8(7) . . . . ? O8C Ni3 O1G C2G -43.6(7) . . . . ? O7A Ni3 O1G C2G -135.5(7) . . . . ? O1F Ni3 O1G C2G 153(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.574 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.074 # Attachment 'NiNa.cif' data_EB8083 _database_code_depnum_ccdc_archive 'CCDC 718776' _audit_creation_date 08-04-22 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'eb8083 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H35 N2 Na1 Ni1 O7' _chemical_compound_source 'Giorgos Karotsis, GK1176' _exptl_crystal_recrystallization_method ; Slow evaporation of MeOH solution. ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. The structure contains two independent molecules whose geometries only differ significantly in the orientation of the groups C13-C18 and C113-C118. The molecules are otherwise related by a pseudo-inversion centre at (0,0.25,0.25). The difference in orientation of these Ph groups means that the raising of symmetry (in this case, a reduction in cell volume) is not appropriate. Checkcif alerts 912_ALERT_3_A # Missing FCF Reflections Above STh/L= 0.600 1943 910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 4 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/L= 0.600 2 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 1 The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 6183 6178 5 23.01 0.550 0.999 8217 8212 5 25.24 0.600 0.999 10657 10651 6 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.997 13550 13508 42 29.84 0.700 0.928 16906 15696 1210 30.57 0.716 0.892 17992 16043 1949 230_ALERT_2_B Hirshfeld Test Diff for O137 - C138 .. 8.04 su These atoms form a MeOH ligand attached to a Na atom. The C atom has considerably greater freedom of motion than the O atom. 154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg. Checked. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.87 Ratio 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.87 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.50 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.33 Ratio No action. These are coordinated MeOH ligand atoms. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 37 The second independent molecule has been numbered to correspond to the first with an offset of 100 in atom labels. 793_ALERT_1_G Check the Absolute Configuration of C3 = ... S 793_ALERT_1_G Check the Absolute Configuration of C20 = ... R 793_ALERT_1_G Check the Absolute Configuration of C103 = ... R 793_ALERT_1_G Check the Absolute Configuration of C120 = ... S ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 13.3416(3) _cell_length_b 14.8361(3) _cell_length_c 15.1781(4) _cell_angle_alpha 82.101(1) _cell_angle_beta 86.408(1) _cell_angle_gamma 82.228(1) _cell_volume 2945.50(12) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C31 H35 N2 Na1 Ni1 O7 # Dc = 1.42 Fooo = 1320.00 Mu = 7.24 M = 1258.66 # Found Formula = C31 H35 N2 Na1 Ni1 O7 # Dc = 1.42 FOOO = 1320.00 Mu = 7.24 M = 1258.66 _chemical_formula_sum 'C31 H35 N2 Na1 Ni1 O7' _chemical_formula_weight 629.33 _cell_measurement_reflns_used 9897 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_max 0.49 _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.724 # Sheldrick geometric approximatio 0.81 0.88 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.88 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 38427 _reflns_number_total 16043 _diffrn_reflns_av_R_equivalents 0.039 # Number of reflections with Friedels Law is 16043 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 18091 _diffrn_reflns_theta_min 1.944 _diffrn_reflns_theta_max 30.574 _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 27.823 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min -20 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.69 _refine_diff_density_max 0.69 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 16001 _refine_ls_number_restraints 0 _refine_ls_number_parameters 757 _oxford_refine_ls_R_factor_ref 0.0718 _refine_ls_wR_factor_ref 0.1116 _refine_ls_goodness_of_fit_ref 0.9352 _refine_ls_shift/su_max 0.000591 # The values computed from all data _oxford_reflns_number_all 16001 _refine_ls_R_factor_all 0.0718 _refine_ls_wR_factor_all 0.1116 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 11490 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_gt 0.1011 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ni1 Ni 0.73195(2) 0.376827(18) 0.163434(18) 0.0180 1.0000 Uani . . . . . . . O2 O 0.63856(12) 0.39289(10) 0.25655(10) 0.0226 1.0000 Uani . . . . . . . C3 C 0.63428(18) 0.47902(14) 0.28771(15) 0.0223 1.0000 Uani . . . . . . . C4 C 0.68921(18) 0.54274(14) 0.22052(14) 0.0215 1.0000 Uani . . . . . . . N5 N 0.73512(14) 0.50204(12) 0.15634(12) 0.0215 1.0000 Uani . . . . . . . O6 O 0.78587(13) 0.55005(10) 0.08966(10) 0.0277 1.0000 Uani . . . . . . . C7 C 0.67632(18) 0.46816(15) 0.37990(15) 0.0225 1.0000 Uani . . . . . . . C8 C 0.6208(2) 0.50454(19) 0.44962(17) 0.0347 1.0000 Uani . . . . . . . C9 C 0.6602(2) 0.4921(2) 0.53415(18) 0.0432 1.0000 Uani . . . . . . . C10 C 0.7541(2) 0.4436(2) 0.54858(17) 0.0413 1.0000 Uani . . . . . . . C11 C 0.8104(2) 0.40786(18) 0.47870(18) 0.0375 1.0000 Uani . . . . . . . C12 C 0.7714(2) 0.41998(17) 0.39504(17) 0.0322 1.0000 Uani . . . . . . . C13 C 0.68550(17) 0.64231(15) 0.22426(14) 0.0214 1.0000 Uani . . . . . . . C14 C 0.71529(19) 0.67582(16) 0.29818(15) 0.0269 1.0000 Uani . . . . . . . C15 C 0.7118(2) 0.76976(17) 0.29896(17) 0.0326 1.0000 Uani . . . . . . . C16 C 0.6784(2) 0.83034(16) 0.22687(17) 0.0315 1.0000 Uani . . . . . . . C17 C 0.6476(2) 0.79779(16) 0.15301(17) 0.0311 1.0000 Uani . . . . . . . C18 C 0.65123(18) 0.70444(15) 0.15176(16) 0.0265 1.0000 Uani . . . . . . . O19 O 0.72241(11) 0.25309(10) 0.17680(10) 0.0201 1.0000 Uani . . . . . . . C20 C 0.79812(17) 0.20274(14) 0.12617(14) 0.0201 1.0000 Uani . . . . . . . C21 C 0.85117(17) 0.26784(14) 0.05844(14) 0.0201 1.0000 Uani . . . . . . . N22 N 0.82493(15) 0.35261(12) 0.07162(12) 0.0225 1.0000 Uani . . . . . . . O23 O 0.86325(14) 0.42054(11) 0.01619(11) 0.0318 1.0000 Uani . . . . . . . C24 C 0.86952(17) 0.13892(14) 0.18828(14) 0.0195 1.0000 Uani . . . . . . . C25 C 0.83138(18) 0.06446(15) 0.23899(15) 0.0243 1.0000 Uani . . . . . . . C26 C 0.8912(2) 0.00614(16) 0.29992(16) 0.0314 1.0000 Uani . . . . . . . C27 C 0.9887(2) 0.02094(17) 0.31129(16) 0.0335 1.0000 Uani . . . . . . . C28 C 1.0267(2) 0.09528(18) 0.26210(16) 0.0340 1.0000 Uani . . . . . . . C29 C 0.96792(18) 0.15392(17) 0.20022(15) 0.0278 1.0000 Uani . . . . . . . C30 C 0.92054(17) 0.23450(15) -0.01291(14) 0.0220 1.0000 Uani . . . . . . . C31 C 0.91698(19) 0.14652(16) -0.03512(16) 0.0276 1.0000 Uani . . . . . . . H31 H 0.5614 0.5070 0.2918 0.0254 1.0000 Uiso R . . . . . . C32 C 0.97875(19) 0.11330(17) -0.10316(16) 0.0305 1.0000 Uani . . . . . . . C33 C 1.04653(19) 0.16644(17) -0.14987(15) 0.0295 1.0000 Uani . . . . . . . C34 C 1.05332(19) 0.25271(17) -0.12749(16) 0.0304 1.0000 Uani . . . . . . . C35 C 0.99098(18) 0.28710(16) -0.05992(15) 0.0268 1.0000 Uani . . . . . . . Na36 Na 0.64415(7) 0.23631(6) 0.32201(6) 0.0250 1.0000 Uani . . . . . . . O37 O 0.73591(14) 0.17784(13) 0.44410(11) 0.0372 1.0000 Uani . . . . . . . C38 C 0.8418(2) 0.17764(19) 0.4420(2) 0.0418 1.0000 Uani . . . . . . . O39 O 0.48507(14) 0.27590(14) 0.39174(12) 0.0434 1.0000 Uani . . . . . . . C40 C 0.4739(3) 0.2539(2) 0.48438(19) 0.0563 1.0000 Uani . . . . . . . O41 O 0.58262(14) 0.09530(12) 0.30059(12) 0.0365 1.0000 Uani . . . . . . . C42 C 0.5823(2) 0.02831(18) 0.37682(19) 0.0423 1.0000 Uani . . . . . . . Ni101 Ni 0.30214(2) 0.126390(18) 0.333955(18) 0.0189 1.0000 Uani . . . . . . . O102 O 0.39260(12) 0.10905(10) 0.23828(10) 0.0225 1.0000 Uani . . . . . . . C103 C 0.39615(17) 0.02187(14) 0.21011(14) 0.0212 1.0000 Uani . . . . . . . C104 C 0.34189(17) -0.04047(14) 0.27887(14) 0.0200 1.0000 Uani . . . . . . . N105 N 0.29648(15) 0.00138(12) 0.34195(12) 0.0218 1.0000 Uani . . . . . . . O106 O 0.24243(13) -0.04547(10) 0.40715(11) 0.0290 1.0000 Uani . . . . . . . C107 C 0.34703(17) 0.02566(14) 0.12130(14) 0.0210 1.0000 Uani . . . . . . . C108 C 0.39149(19) -0.02599(15) 0.05635(16) 0.0261 1.0000 Uani . . . . . . . C109 C 0.3423(2) -0.02639(16) -0.02182(16) 0.0297 1.0000 Uani . . . . . . . C110 C 0.2491(2) 0.02366(16) -0.03421(16) 0.0297 1.0000 Uani . . . . . . . C111 C 0.2035(2) 0.07511(18) 0.03013(16) 0.0333 1.0000 Uani . . . . . . . H111 H 0.8757 0.3765 0.4884 0.0451 1.0000 Uiso R . . . . . . C112 C 0.25281(19) 0.07578(17) 0.10753(16) 0.0294 1.0000 Uani . . . . . . . C113 C 0.33499(18) -0.13726(14) 0.26896(14) 0.0222 1.0000 Uani . . . . . . . C114 C 0.2500(2) -0.15969(17) 0.23397(19) 0.0365 1.0000 Uani . . . . . . . C115 C 0.2436(2) -0.24892(18) 0.22007(18) 0.0400 1.0000 Uani . . . . . . . C116 C 0.3226(2) -0.31624(18) 0.2421(2) 0.0438 1.0000 Uani . . . . . . . C117 C 0.4067(2) -0.29452(19) 0.2775(3) 0.0576 1.0000 Uani . . . . . . . C118 C 0.4141(2) -0.20486(17) 0.2902(2) 0.0408 1.0000 Uani . . . . . . . O119 O 0.31101(12) 0.25006(10) 0.31851(10) 0.0227 1.0000 Uani . . . . . . . C120 C 0.23583(17) 0.30114(14) 0.36947(14) 0.0209 1.0000 Uani . . . . . . . C121 C 0.18540(17) 0.23663(14) 0.43884(14) 0.0205 1.0000 Uani . . . . . . . H121 H 0.8100 0.3968 0.3473 0.0392 1.0000 Uiso R . . . . . . N122 N 0.21233(15) 0.15126(12) 0.42753(12) 0.0229 1.0000 Uani . . . . . . . O123 O 0.17681(14) 0.08356(11) 0.48503(11) 0.0334 1.0000 Uani . . . . . . . C124 C 0.16124(17) 0.36171(14) 0.30805(14) 0.0213 1.0000 Uani . . . . . . . C125 C 0.19226(19) 0.44003(15) 0.25865(15) 0.0251 1.0000 Uani . . . . . . . C126 C 0.1284(2) 0.49605(16) 0.19942(16) 0.0318 1.0000 Uani . . . . . . . C127 C 0.0329(2) 0.47475(18) 0.18913(17) 0.0366 1.0000 Uani . . . . . . . C128 C 0.0015(2) 0.3968(2) 0.23704(18) 0.0388 1.0000 Uani . . . . . . . C129 C 0.06538(19) 0.34038(17) 0.29673(16) 0.0311 1.0000 Uani . . . . . . . C130 C 0.11547(18) 0.27086(15) 0.50955(14) 0.0223 1.0000 Uani . . . . . . . C131 C 0.11226(19) 0.36227(16) 0.52475(16) 0.0287 1.0000 Uani . . . . . . . C132 C 0.0502(2) 0.39643(18) 0.59238(17) 0.0330 1.0000 Uani . . . . . . . C133 C -0.0105(2) 0.34124(18) 0.64558(16) 0.0322 1.0000 Uani . . . . . . . C134 C -0.0116(2) 0.25198(17) 0.62936(16) 0.0321 1.0000 Uani . . . . . . . C135 C 0.05061(19) 0.21698(16) 0.56234(15) 0.0272 1.0000 Uani . . . . . . . Na136 Na 0.39009(7) 0.26648(6) 0.17385(6) 0.0250 1.0000 Uani . . . . . . . O137 O 0.27966(15) 0.33510(13) 0.06609(12) 0.0403 1.0000 Uani . . . . . . . C138 C 0.1843(3) 0.3102(2) 0.0759(2) 0.0553 1.0000 Uani . . . . . . . O139 O 0.55011(13) 0.23630(13) 0.09755(12) 0.0360 1.0000 Uani . . . . . . . C140 C 0.5706(2) 0.2694(2) 0.00709(18) 0.0463 1.0000 Uani . . . . . . . O141 O 0.44749(13) 0.40679(11) 0.19962(12) 0.0329 1.0000 Uani . . . . . . . C142 C 0.4490(2) 0.47443(18) 0.12414(18) 0.0411 1.0000 Uani . . . . . . . H81 H 0.5560 0.5406 0.4393 0.0420 1.0000 Uiso R . . . . . . H91 H 0.6205 0.5186 0.5787 0.0535 1.0000 Uiso R . . . . . . H101 H 0.7815 0.4340 0.6059 0.0509 1.0000 Uiso R . . . . . . H141 H 0.7385 0.6360 0.3478 0.0328 1.0000 Uiso R . . . . . . H151 H 0.7322 0.7919 0.3492 0.0405 1.0000 Uiso R . . . . . . H161 H 0.6778 0.8927 0.2266 0.0367 1.0000 Uiso R . . . . . . H171 H 0.6249 0.8392 0.1033 0.0364 1.0000 Uiso R . . . . . . H181 H 0.6312 0.6830 0.1013 0.0318 1.0000 Uiso R . . . . . . H201 H 0.7631 0.1643 0.0927 0.0235 1.0000 Uiso R . . . . . . H231 H 0.8368 0.4698 0.0367 0.0474 1.0000 Uiso R . . . . . . H251 H 0.7646 0.0561 0.2323 0.0286 1.0000 Uiso R . . . . . . H261 H 0.8636 -0.0431 0.3342 0.0360 1.0000 Uiso R . . . . . . H271 H 1.0279 -0.0178 0.3518 0.0386 1.0000 Uiso R . . . . . . H281 H 1.0929 0.1061 0.2697 0.0397 1.0000 Uiso R . . . . . . H291 H 0.9952 0.2033 0.1666 0.0328 1.0000 Uiso R . . . . . . H311 H 0.8719 0.1099 -0.0045 0.0324 1.0000 Uiso R . . . . . . H321 H 0.9746 0.0558 -0.1177 0.0373 1.0000 Uiso R . . . . . . H331 H 1.0865 0.1456 -0.1962 0.0332 1.0000 Uiso R . . . . . . H341 H 1.1006 0.2876 -0.1569 0.0341 1.0000 Uiso R . . . . . . H351 H 0.9975 0.3443 -0.0442 0.0318 1.0000 Uiso R . . . . . . H371 H 0.7201 0.1505 0.4896 0.0539 1.0000 Uiso R . . . . . . H381 H 0.8583 0.2109 0.4869 0.0630 1.0000 Uiso R . . . . . . H382 H 0.8635 0.2068 0.3859 0.0627 1.0000 Uiso R . . . . . . H383 H 0.8762 0.1166 0.4521 0.0626 1.0000 Uiso R . . . . . . H391 H 0.4346 0.2653 0.3698 0.0657 1.0000 Uiso R . . . . . . H401 H 0.4664 0.1902 0.4998 0.0818 1.0000 Uiso R . . . . . . H402 H 0.5324 0.2665 0.5125 0.0822 1.0000 Uiso R . . . . . . H403 H 0.4151 0.2894 0.5084 0.0818 1.0000 Uiso R . . . . . . H411 H 0.5254 0.0983 0.2806 0.0546 1.0000 Uiso R . . . . . . H421 H 0.6500 0.0124 0.3985 0.0639 1.0000 Uiso R . . . . . . H422 H 0.5378 0.0499 0.4238 0.0643 1.0000 Uiso R . . . . . . H423 H 0.5591 -0.0260 0.3637 0.0638 1.0000 Uiso R . . . . . . H1031 H 0.4692 -0.0047 0.2047 0.0252 1.0000 Uiso R . . . . . . H1081 H 0.4552 -0.0597 0.0650 0.0312 1.0000 Uiso R . . . . . . H1091 H 0.3729 -0.0602 -0.0655 0.0359 1.0000 Uiso R . . . . . . H1101 H 0.2154 0.0243 -0.0867 0.0354 1.0000 Uiso R . . . . . . H1111 H 0.1392 0.1095 0.0221 0.0392 1.0000 Uiso R . . . . . . H1121 H 0.2208 0.1097 0.1504 0.0353 1.0000 Uiso R . . . . . . H1141 H 0.1966 -0.1141 0.2187 0.0445 1.0000 Uiso R . . . . . . H1151 H 0.1852 -0.2627 0.1955 0.0490 1.0000 Uiso R . . . . . . H1161 H 0.3191 -0.3773 0.2337 0.0528 1.0000 Uiso R . . . . . . H1171 H 0.4588 -0.3403 0.2940 0.0665 1.0000 Uiso R . . . . . . H1181 H 0.4719 -0.1901 0.3125 0.0482 1.0000 Uiso R . . . . . . H1201 H 0.2716 0.3408 0.4011 0.0253 1.0000 Uiso R . . . . . . H1231 H 0.1977 0.0347 0.4610 0.0495 1.0000 Uiso R . . . . . . H1251 H 0.2571 0.4535 0.2643 0.0293 1.0000 Uiso R . . . . . . H1261 H 0.1508 0.5467 0.1666 0.0365 1.0000 Uiso R . . . . . . H1271 H -0.0097 0.5113 0.1493 0.0422 1.0000 Uiso R . . . . . . H1281 H -0.0639 0.3815 0.2299 0.0454 1.0000 Uiso R . . . . . . H1291 H 0.0435 0.2877 0.3286 0.0374 1.0000 Uiso R . . . . . . H1311 H 0.1536 0.4007 0.4903 0.0346 1.0000 Uiso R . . . . . . H1321 H 0.0505 0.4578 0.6015 0.0399 1.0000 Uiso R . . . . . . H1331 H -0.0510 0.3635 0.6928 0.0378 1.0000 Uiso R . . . . . . H1341 H -0.0541 0.2141 0.6642 0.0371 1.0000 Uiso R . . . . . . H1351 H 0.0495 0.1578 0.5539 0.0325 1.0000 Uiso R . . . . . . H1371 H 0.2785 0.3684 0.0182 0.0599 1.0000 Uiso R . . . . . . H1381 H 0.1752 0.2735 0.1386 0.0836 1.0000 Uiso R . . . . . . H1382 H 0.1314 0.3674 0.0683 0.0840 1.0000 Uiso R . . . . . . H1383 H 0.1743 0.2686 0.0287 0.0830 1.0000 Uiso R . . . . . . H1391 H 0.5985 0.2420 0.1242 0.0545 1.0000 Uiso R . . . . . . H1401 H 0.5784 0.3323 -0.0024 0.0696 1.0000 Uiso R . . . . . . H1402 H 0.6308 0.2350 -0.0162 0.0691 1.0000 Uiso R . . . . . . H1403 H 0.5164 0.2607 -0.0256 0.0692 1.0000 Uiso R . . . . . . H1411 H 0.5041 0.4039 0.2189 0.0495 1.0000 Uiso R . . . . . . H1421 H 0.3825 0.4865 0.1001 0.0606 1.0000 Uiso R . . . . . . H1422 H 0.4673 0.5304 0.1394 0.0612 1.0000 Uiso R . . . . . . H1423 H 0.4960 0.4561 0.0779 0.0614 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02029(15) 0.01658(13) 0.01674(14) 0.00016(10) -0.00075(10) -0.00307(11) O2 0.0266(9) 0.0183(7) 0.0233(8) -0.0041(6) 0.0032(6) -0.0050(6) C3 0.0230(12) 0.0188(10) 0.0247(11) -0.0026(8) -0.0011(9) -0.0018(8) C4 0.0256(12) 0.0190(10) 0.0200(11) 0.0002(8) -0.0030(9) -0.0047(9) N5 0.0226(10) 0.0192(9) 0.0214(9) 0.0030(7) -0.0015(7) -0.0039(7) O6 0.0361(10) 0.0195(8) 0.0248(8) 0.0034(6) 0.0062(7) -0.0038(7) C7 0.0244(12) 0.0206(10) 0.0226(11) 0.0009(8) 0.0010(9) -0.0079(9) C8 0.0310(15) 0.0446(15) 0.0303(13) -0.0091(11) 0.0039(11) -0.0098(12) C9 0.0463(18) 0.0609(19) 0.0275(14) -0.0136(13) 0.0057(12) -0.0211(15) C10 0.0537(19) 0.0502(17) 0.0236(13) 0.0016(12) -0.0097(12) -0.0232(15) C11 0.0452(17) 0.0322(13) 0.0363(15) -0.0032(11) -0.0157(13) -0.0045(12) C12 0.0368(15) 0.0312(13) 0.0291(13) -0.0071(10) -0.0069(11) -0.0007(11) C13 0.0222(12) 0.0208(10) 0.0219(11) -0.0025(8) -0.0005(9) -0.0061(9) C14 0.0344(14) 0.0237(11) 0.0235(11) 0.0000(9) -0.0053(10) -0.0080(10) C15 0.0417(16) 0.0295(12) 0.0301(13) -0.0072(10) -0.0035(11) -0.0131(11) C16 0.0354(15) 0.0190(11) 0.0406(15) -0.0037(10) 0.0025(11) -0.0076(10) C17 0.0364(15) 0.0224(11) 0.0326(13) 0.0034(10) -0.0026(11) -0.0034(10) C18 0.0292(13) 0.0230(11) 0.0273(12) -0.0023(9) -0.0051(10) -0.0026(9) O19 0.0198(8) 0.0194(7) 0.0207(8) -0.0013(6) 0.0022(6) -0.0039(6) C20 0.0225(12) 0.0201(10) 0.0182(10) -0.0026(8) -0.0019(8) -0.0040(8) C21 0.0221(12) 0.0193(10) 0.0181(10) 0.0018(8) -0.0027(8) -0.0029(8) N22 0.0259(11) 0.0203(9) 0.0197(9) 0.0031(7) -0.0010(7) -0.0027(8) O23 0.0457(11) 0.0177(8) 0.0280(9) 0.0034(7) 0.0129(8) -0.0031(7) C24 0.0234(12) 0.0186(10) 0.0166(10) -0.0026(8) -0.0017(8) -0.0018(8) C25 0.0272(13) 0.0204(10) 0.0257(12) -0.0024(9) -0.0004(9) -0.0056(9) C26 0.0413(16) 0.0226(11) 0.0276(13) 0.0040(9) -0.0014(11) -0.0025(10) C27 0.0380(16) 0.0317(13) 0.0263(13) 0.0021(10) -0.0060(11) 0.0074(11) C28 0.0247(14) 0.0464(15) 0.0290(13) 0.0010(11) -0.0054(10) -0.0015(11) C29 0.0271(13) 0.0312(12) 0.0238(12) 0.0037(10) -0.0028(9) -0.0062(10) C30 0.0242(12) 0.0223(10) 0.0182(10) 0.0000(8) -0.0022(8) -0.0002(9) C31 0.0288(13) 0.0270(12) 0.0279(12) -0.0053(10) -0.0004(10) -0.0059(10) C32 0.0317(14) 0.0328(13) 0.0283(13) -0.0091(10) -0.0033(10) -0.0024(11) C33 0.0291(14) 0.0369(13) 0.0200(11) -0.0053(10) -0.0012(9) 0.0066(10) C34 0.0294(14) 0.0319(13) 0.0250(12) 0.0046(10) 0.0055(10) 0.0020(10) C35 0.0292(13) 0.0246(11) 0.0250(12) -0.0016(9) 0.0038(9) -0.0018(9) Na36 0.0261(5) 0.0270(5) 0.0216(5) 0.0019(4) -0.0026(4) -0.0067(4) O37 0.0348(11) 0.0461(11) 0.0287(9) 0.0116(8) -0.0077(8) -0.0120(9) C38 0.0382(17) 0.0410(15) 0.0469(17) -0.0023(13) -0.0071(13) -0.0091(13) O39 0.0291(11) 0.0708(14) 0.0331(10) -0.0098(10) 0.0000(8) -0.0139(10) C40 0.053(2) 0.078(2) 0.0341(16) -0.0141(16) -0.0038(14) 0.0115(18) O41 0.0287(10) 0.0361(10) 0.0454(11) 0.0014(8) -0.0072(8) -0.0109(8) C42 0.0500(19) 0.0354(15) 0.0427(16) 0.0009(12) -0.0094(14) -0.0126(13) Ni2 0.02099(16) 0.01745(13) 0.01775(14) -0.00012(10) -0.00063(11) -0.00261(11) O102 0.0249(9) 0.0184(7) 0.0248(8) -0.0043(6) 0.0025(6) -0.0055(6) C103 0.0203(12) 0.0211(10) 0.0221(11) -0.0018(8) 0.0002(8) -0.0038(8) C104 0.0200(11) 0.0177(10) 0.0217(11) 0.0012(8) -0.0039(8) -0.0022(8) N105 0.0250(10) 0.0194(9) 0.0197(9) 0.0028(7) -0.0012(7) -0.0037(7) O106 0.0399(11) 0.0200(8) 0.0242(8) 0.0039(6) 0.0070(7) -0.0046(7) C107 0.0213(12) 0.0208(10) 0.0211(11) -0.0009(8) 0.0019(8) -0.0066(8) C108 0.0248(13) 0.0235(11) 0.0300(12) -0.0052(9) 0.0031(9) -0.0036(9) C109 0.0395(15) 0.0267(12) 0.0243(12) -0.0060(9) 0.0041(10) -0.0093(11) C110 0.0389(15) 0.0305(12) 0.0215(11) 0.0008(9) -0.0055(10) -0.0127(11) C111 0.0333(15) 0.0370(14) 0.0282(13) -0.0024(11) -0.0067(11) 0.0013(11) C112 0.0290(14) 0.0341(13) 0.0246(12) -0.0078(10) -0.0014(10) 0.0026(10) C113 0.0267(12) 0.0179(10) 0.0206(11) 0.0011(8) 0.0013(9) -0.0022(9) C114 0.0402(16) 0.0218(11) 0.0489(17) -0.0019(11) -0.0140(13) -0.0057(11) C115 0.0530(19) 0.0307(13) 0.0399(15) -0.0051(11) -0.0043(13) -0.0170(13) C116 0.053(2) 0.0255(13) 0.0545(18) -0.0126(12) 0.0199(15) -0.0135(13) C117 0.0407(19) 0.0229(13) 0.103(3) -0.0029(16) 0.0073(18) 0.0078(12) C118 0.0265(14) 0.0268(13) 0.067(2) 0.0004(13) -0.0050(13) -0.0014(11) O119 0.0237(9) 0.0202(7) 0.0243(8) -0.0029(6) 0.0028(6) -0.0045(6) C120 0.0221(12) 0.0184(10) 0.0225(11) -0.0028(8) -0.0014(9) -0.0035(8) C121 0.0234(12) 0.0212(10) 0.0169(10) -0.0007(8) -0.0026(8) -0.0042(9) N122 0.0285(11) 0.0194(9) 0.0194(9) 0.0016(7) 0.0007(8) -0.0025(8) O123 0.0510(12) 0.0181(8) 0.0272(9) 0.0024(7) 0.0124(8) -0.0023(8) C124 0.0228(12) 0.0208(10) 0.0204(10) -0.0022(8) -0.0021(8) -0.0028(8) C125 0.0287(13) 0.0240(11) 0.0231(11) -0.0032(9) -0.0004(9) -0.0062(9) C126 0.0478(17) 0.0216(11) 0.0243(12) 0.0023(9) -0.0027(11) -0.0032(11) C127 0.0395(16) 0.0349(14) 0.0317(14) 0.0029(11) -0.0116(12) 0.0055(12) C128 0.0284(15) 0.0511(17) 0.0354(15) 0.0057(13) -0.0100(11) -0.0073(12) C129 0.0306(14) 0.0337(13) 0.0284(13) 0.0064(10) -0.0068(10) -0.0097(11) C130 0.0254(12) 0.0238(11) 0.0170(10) -0.0021(8) -0.0040(8) 0.0004(9) C131 0.0300(14) 0.0286(12) 0.0288(12) -0.0056(10) -0.0026(10) -0.0056(10) C132 0.0351(15) 0.0323(13) 0.0330(14) -0.0129(11) -0.0039(11) 0.0003(11) C133 0.0340(15) 0.0381(14) 0.0228(12) -0.0073(10) -0.0026(10) 0.0053(11) C134 0.0336(15) 0.0331(13) 0.0255(12) 0.0047(10) 0.0010(10) 0.0004(11) C135 0.0314(14) 0.0234(11) 0.0247(12) 0.0005(9) -0.0024(10) 0.0008(10) Na136 0.0248(5) 0.0253(5) 0.0243(5) 0.0011(4) -0.0020(4) -0.0052(4) O137 0.0404(12) 0.0474(11) 0.0309(10) 0.0055(8) -0.0112(8) -0.0043(9) C138 0.063(2) 0.053(2) 0.051(2) -0.0090(16) -0.0037(17) -0.0091(17) O139 0.0245(10) 0.0475(11) 0.0377(10) -0.0113(9) -0.0030(8) -0.0044(8) C140 0.0513(19) 0.0502(18) 0.0347(15) -0.0012(13) -0.0157(14) 0.0057(14) O141 0.0294(10) 0.0327(9) 0.0374(10) 0.0005(8) -0.0041(8) -0.0106(8) C142 0.0504(19) 0.0339(14) 0.0382(15) 0.0032(12) -0.0031(13) -0.0101(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.26852(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . O2 . 1.8434(16) yes Ni1 . N5 . 1.8520(18) yes Ni1 . O19 . 1.8399(14) yes Ni1 . N22 . 1.8467(19) yes Ni1 . Na36 . 3.2310(9) yes O2 . C3 . 1.415(2) yes O2 . Na36 . 2.3911(17) yes C3 . C4 . 1.516(3) yes C3 . C7 . 1.520(3) yes C3 . H31 . 1.005 no C4 . N5 . 1.294(3) yes C4 . C13 . 1.480(3) yes N5 . O6 . 1.355(2) yes C7 . C8 . 1.382(3) yes C7 . C12 . 1.385(3) yes C8 . C9 . 1.396(4) yes C8 . H81 . 0.963 no C9 . C10 . 1.371(4) yes C9 . H91 . 0.930 no C10 . C11 . 1.385(4) yes C10 . H101 . 0.950 no C11 . C12 . 1.382(3) yes C11 . H111 . 0.940 no C12 . H121 . 0.940 no C13 . C14 . 1.388(3) yes C13 . C18 . 1.393(3) yes C14 . C15 . 1.390(3) yes C14 . H141 . 0.932 no C15 . C16 . 1.374(3) yes C15 . H151 . 0.939 no C16 . C17 . 1.385(3) yes C16 . H161 . 0.924 no C17 . C18 . 1.382(3) yes C17 . H171 . 0.943 no C18 . H181 . 0.935 no O19 . C20 . 1.423(3) yes O19 . Na36 . 2.3751(17) yes C20 . C21 . 1.520(3) yes C20 . C24 . 1.522(3) yes C20 . H201 . 0.991 no C21 . N22 . 1.298(3) yes C21 . C30 . 1.474(3) yes N22 . O23 . 1.355(2) yes O23 . H231 . 0.858 no C24 . C25 . 1.393(3) yes C24 . C29 . 1.388(3) yes C25 . C26 . 1.388(3) yes C25 . H251 . 0.929 no C26 . C27 . 1.374(4) yes C26 . H261 . 0.940 no C27 . C28 . 1.382(3) yes C27 . H271 . 0.919 no C28 . C29 . 1.392(3) yes C28 . H281 . 0.935 no C29 . H291 . 0.935 no C30 . C31 . 1.400(3) yes C30 . C35 . 1.401(3) yes C31 . C32 . 1.383(3) yes C31 . H311 . 0.926 no C32 . C33 . 1.379(3) yes C32 . H321 . 0.919 no C33 . C34 . 1.384(3) yes C33 . H331 . 0.918 no C34 . C35 . 1.388(3) yes C34 . H341 . 0.924 no C35 . H351 . 0.930 no Na36 . O37 . 2.2893(19) yes Na36 . O39 . 2.350(2) yes Na36 . O41 . 2.4168(19) yes O37 . C38 . 1.411(3) yes O37 . H371 . 0.783 no C38 . H381 . 0.946 no C38 . H382 . 0.947 no C38 . H383 . 0.955 no O39 . C40 . 1.402(3) yes O39 . H391 . 0.812 no C40 . H401 . 0.958 no C40 . H402 . 0.964 no C40 . H403 . 0.964 no O41 . C42 . 1.418(3) yes O41 . H411 . 0.832 no C42 . H421 . 0.969 no C42 . H422 . 0.960 no C42 . H423 . 0.951 no Ni101 . O102 . 1.8521(16) yes Ni101 . N105 . 1.8534(18) yes Ni101 . O119 . 1.8364(15) yes Ni101 . N122 . 1.8440(19) yes Ni101 . Na136 . 3.2429(9) yes O102 . C103 . 1.411(2) yes O102 . Na136 . 2.4018(17) yes C103 . C104 . 1.513(3) yes C103 . C107 . 1.526(3) yes C103 . H1031 . 1.004 no C104 . N105 . 1.288(3) yes C104 . C113 . 1.480(3) yes N105 . O106 . 1.356(2) yes C107 . C108 . 1.386(3) yes C107 . C112 . 1.384(3) yes C108 . C109 . 1.392(3) yes C108 . H1081 . 0.933 no C109 . C110 . 1.370(3) yes C109 . H1091 . 0.927 no C110 . C111 . 1.382(3) yes C110 . H1101 . 0.938 no C111 . C112 . 1.383(3) yes C111 . H1111 . 0.943 no C112 . H1121 . 0.925 no C113 . C114 . 1.381(3) yes C113 . C118 . 1.375(3) yes C114 . C115 . 1.383(3) yes C114 . H1141 . 0.930 no C115 . C116 . 1.374(4) yes C115 . H1151 . 0.944 no C116 . C117 . 1.369(4) yes C116 . H1161 . 0.939 no C117 . C118 . 1.387(4) yes C117 . H1171 . 0.924 no C118 . H1181 . 0.926 no O119 . C120 . 1.427(3) yes O119 . Na136 . 2.3718(18) yes C120 . C121 . 1.512(3) yes C120 . C124 . 1.520(3) yes C120 . H1201 . 0.994 no C121 . N122 . 1.301(3) yes C121 . C130 . 1.475(3) yes N122 . O123 . 1.353(2) yes O123 . H1231 . 0.860 no C124 . C125 . 1.391(3) yes C124 . C129 . 1.385(3) yes C125 . C126 . 1.387(3) yes C125 . H1251 . 0.925 no C126 . C127 . 1.375(4) yes C126 . H1261 . 0.917 no C127 . C128 . 1.380(4) yes C127 . H1271 . 0.923 no C128 . C129 . 1.394(3) yes C128 . H1281 . 0.948 no C129 . H1291 . 0.933 no C130 . C131 . 1.401(3) yes C130 . C135 . 1.398(3) yes C131 . C132 . 1.385(3) yes C131 . H1311 . 0.932 no C132 . C133 . 1.377(4) yes C132 . H1321 . 0.940 no C133 . C134 . 1.382(3) yes C133 . H1331 . 0.939 no C134 . C135 . 1.384(3) yes C134 . H1341 . 0.940 no C135 . H1351 . 0.907 no Na136 . O137 . 2.3066(19) yes Na136 . O139 . 2.382(2) yes Na136 . O141 . 2.4010(19) yes O137 . C138 . 1.366(4) yes O137 . H1371 . 0.821 no C138 . H1381 . 1.038 no C138 . H1382 . 1.026 no C138 . H1383 . 1.033 no O139 . C140 . 1.416(3) yes O139 . H1391 . 0.802 no C140 . H1401 . 0.942 no C140 . H1402 . 0.967 no C140 . H1403 . 0.936 no O141 . C142 . 1.417(3) yes O141 . H1411 . 0.821 no C142 . H1421 . 0.965 no C142 . H1422 . 0.958 no C142 . H1423 . 0.954 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 . Ni1 . N5 . 85.03(7) yes O2 . Ni1 . O19 . 91.08(7) yes N5 . Ni1 . O19 . 176.11(8) yes O2 . Ni1 . N22 . 176.25(7) yes N5 . Ni1 . N22 . 98.71(8) yes O19 . Ni1 . N22 . 85.18(7) yes O2 . Ni1 . Na36 . 47.02(5) yes N5 . Ni1 . Na36 . 129.77(6) yes O19 . Ni1 . Na36 . 46.50(5) yes N22 . Ni1 . Na36 . 129.33(6) yes Ni1 . O2 . C3 . 113.70(13) yes Ni1 . O2 . Na36 . 98.64(7) yes C3 . O2 . Na36 . 136.38(13) yes O2 . C3 . C4 . 109.34(18) yes O2 . C3 . C7 . 110.94(17) yes C4 . C3 . C7 . 112.44(18) yes O2 . C3 . H31 . 108.5 no C4 . C3 . H31 . 107.2 no C7 . C3 . H31 . 108.2 no C3 . C4 . N5 . 112.91(18) yes C3 . C4 . C13 . 123.8(2) yes N5 . C4 . C13 . 123.2(2) yes C4 . N5 . Ni1 . 116.97(15) yes C4 . N5 . O6 . 120.21(18) yes Ni1 . N5 . O6 . 122.78(14) yes C3 . C7 . C8 . 121.2(2) yes C3 . C7 . C12 . 119.7(2) yes C8 . C7 . C12 . 119.1(2) yes C7 . C8 . C9 . 120.2(3) yes C7 . C8 . H81 . 119.9 no C9 . C8 . H81 . 119.9 no C8 . C9 . C10 . 120.3(3) yes C8 . C9 . H91 . 117.0 no C10 . C9 . H91 . 122.7 no C9 . C10 . C11 . 119.8(2) yes C9 . C10 . H101 . 121.2 no C11 . C10 . H101 . 119.0 no C10 . C11 . C12 . 120.0(3) yes C10 . C11 . H111 . 119.5 no C12 . C11 . H111 . 120.5 no C7 . C12 . C11 . 120.7(3) yes C7 . C12 . H121 . 119.1 no C11 . C12 . H121 . 120.1 no C4 . C13 . C14 . 121.8(2) yes C4 . C13 . C18 . 119.3(2) yes C14 . C13 . C18 . 118.8(2) yes C13 . C14 . C15 . 120.3(2) yes C13 . C14 . H141 . 120.9 no C15 . C14 . H141 . 118.8 no C14 . C15 . C16 . 120.4(2) yes C14 . C15 . H151 . 119.8 no C16 . C15 . H151 . 119.8 no C15 . C16 . C17 . 119.9(2) yes C15 . C16 . H161 . 120.6 no C17 . C16 . H161 . 119.5 no C16 . C17 . C18 . 119.9(2) yes C16 . C17 . H171 . 120.1 no C18 . C17 . H171 . 120.0 no C13 . C18 . C17 . 120.7(2) yes C13 . C18 . H181 . 119.9 no C17 . C18 . H181 . 119.4 no Ni1 . O19 . C20 . 113.43(12) yes Ni1 . O19 . Na36 . 99.31(7) yes C20 . O19 . Na36 . 137.73(12) yes O19 . C20 . C21 . 110.23(17) yes O19 . C20 . C24 . 109.88(17) yes C21 . C20 . C24 . 113.87(18) yes O19 . C20 . H201 . 107.2 no C21 . C20 . H201 . 107.5 no C24 . C20 . H201 . 107.9 no C20 . C21 . N22 . 111.28(19) yes C20 . C21 . C30 . 121.85(18) yes N22 . C21 . C30 . 126.8(2) yes C21 . N22 . Ni1 . 118.43(15) yes C21 . N22 . O23 . 119.50(19) yes Ni1 . N22 . O23 . 122.02(14) yes N22 . O23 . H231 . 104.1 no C20 . C24 . C25 . 117.6(2) yes C20 . C24 . C29 . 123.48(19) yes C25 . C24 . C29 . 118.8(2) yes C24 . C25 . C26 . 120.4(2) yes C24 . C25 . H251 . 118.4 no C26 . C25 . H251 . 121.1 no C25 . C26 . C27 . 120.6(2) yes C25 . C26 . H261 . 119.1 no C27 . C26 . H261 . 120.3 no C26 . C27 . C28 . 119.4(2) yes C26 . C27 . H271 . 120.2 no C28 . C27 . H271 . 120.4 no C27 . C28 . C29 . 120.7(2) yes C27 . C28 . H281 . 119.9 no C29 . C28 . H281 . 119.4 no C28 . C29 . C24 . 120.1(2) yes C28 . C29 . H291 . 119.7 no C24 . C29 . H291 . 120.2 no C21 . C30 . C31 . 119.2(2) yes C21 . C30 . C35 . 122.8(2) yes C31 . C30 . C35 . 118.0(2) yes C30 . C31 . C32 . 121.2(2) yes C30 . C31 . H311 . 119.8 no C32 . C31 . H311 . 118.9 no C31 . C32 . C33 . 120.1(2) yes C31 . C32 . H321 . 120.2 no C33 . C32 . H321 . 119.7 no C32 . C33 . C34 . 119.6(2) yes C32 . C33 . H331 . 120.8 no C34 . C33 . H331 . 119.6 no C33 . C34 . C35 . 120.7(2) yes C33 . C34 . H341 . 120.0 no C35 . C34 . H341 . 119.3 no C30 . C35 . C34 . 120.3(2) yes C30 . C35 . H351 . 119.6 no C34 . C35 . H351 . 120.0 no O19 . Na36 . O2 . 66.95(5) yes O19 . Na36 . Ni1 . 34.19(4) yes O2 . Na36 . Ni1 . 34.34(4) yes O19 . Na36 . O37 . 121.30(7) yes O2 . Na36 . O37 . 122.35(7) yes Ni1 . Na36 . O37 . 121.43(6) yes O19 . Na36 . O39 . 138.35(7) yes O2 . Na36 . O39 . 88.13(7) yes Ni1 . Na36 . O39 . 120.10(6) yes O37 . Na36 . O39 . 100.09(7) yes O19 . Na36 . O41 . 92.69(6) yes O2 . Na36 . O41 . 140.80(7) yes Ni1 . Na36 . O41 . 124.34(6) yes O37 . Na36 . O41 . 96.82(7) yes O39 . Na36 . O41 . 86.34(7) yes Na36 . O37 . C38 . 121.18(16) yes Na36 . O37 . H371 . 130.9 no C38 . O37 . H371 . 107.5 no O37 . C38 . H381 . 109.2 no O37 . C38 . H382 . 109.2 no H381 . C38 . H382 . 108.6 no O37 . C38 . H383 . 111.3 no H381 . C38 . H383 . 108.8 no H382 . C38 . H383 . 109.6 no Na36 . O39 . C40 . 118.35(18) yes Na36 . O39 . H391 . 119.0 no C40 . O39 . H391 . 108.2 no O39 . C40 . H401 . 110.5 no O39 . C40 . H402 . 110.2 no H401 . C40 . H402 . 108.7 no O39 . C40 . H403 . 111.5 no H401 . C40 . H403 . 108.0 no H402 . C40 . H403 . 107.9 no Na36 . O41 . C42 . 115.41(15) yes Na36 . O41 . H411 . 118.4 no C42 . O41 . H411 . 104.5 no O41 . C42 . H421 . 110.1 no O41 . C42 . H422 . 111.5 no H421 . C42 . H422 . 108.8 no O41 . C42 . H423 . 111.3 no H421 . C42 . H423 . 108.4 no H422 . C42 . H423 . 106.5 no O102 . Ni101 . N105 . 85.13(7) yes O102 . Ni101 . O119 . 91.35(7) yes N105 . Ni101 . O119 . 176.26(8) yes O102 . Ni101 . N122 . 176.50(7) yes N105 . Ni101 . N122 . 98.35(8) yes O119 . Ni101 . N122 . 85.17(7) yes O102 . Ni101 . Na136 . 47.09(5) yes N105 . Ni101 . Na136 . 130.20(6) yes O119 . Ni101 . Na136 . 46.07(5) yes N122 . Ni101 . Na136 . 129.45(6) yes Ni101 . O102 . C103 . 113.33(13) yes Ni101 . O102 . Na136 . 98.52(7) yes C103 . O102 . Na136 . 138.78(13) yes O102 . C103 . C104 . 109.93(18) yes O102 . C103 . C107 . 112.88(17) yes C104 . C103 . C107 . 107.91(17) yes O102 . C103 . H1031 . 107.7 no C104 . C103 . H1031 . 108.8 no C107 . C103 . H1031 . 109.6 no C103 . C104 . N105 . 113.05(18) yes C103 . C104 . C113 . 122.52(19) yes N105 . C104 . C113 . 124.2(2) yes C104 . N105 . Ni101 . 117.08(15) yes C104 . N105 . O106 . 119.55(18) yes Ni101 . N105 . O106 . 123.23(14) yes C103 . C107 . C108 . 121.1(2) yes C103 . C107 . C112 . 119.7(2) yes C108 . C107 . C112 . 118.9(2) yes C107 . C108 . C109 . 120.3(2) yes C107 . C108 . H1081 . 119.4 no C109 . C108 . H1081 . 120.2 no C108 . C109 . C110 . 119.8(2) yes C108 . C109 . H1091 . 120.0 no C110 . C109 . H1091 . 120.2 no C109 . C110 . C111 . 120.5(2) yes C109 . C110 . H1101 . 120.7 no C111 . C110 . H1101 . 118.8 no C110 . C111 . C112 . 119.5(2) yes C110 . C111 . H1111 . 120.9 no C112 . C111 . H1111 . 119.6 no C107 . C112 . C111 . 120.9(2) yes C107 . C112 . H1121 . 120.6 no C111 . C112 . H1121 . 118.5 no C104 . C113 . C114 . 119.7(2) yes C104 . C113 . C118 . 121.0(2) yes C114 . C113 . C118 . 119.2(2) yes C113 . C114 . C115 . 120.9(3) yes C113 . C114 . H1141 . 119.6 no C115 . C114 . H1141 . 119.5 no C114 . C115 . C116 . 119.6(3) yes C114 . C115 . H1151 . 119.5 no C116 . C115 . H1151 . 120.9 no C115 . C116 . C117 . 119.8(3) yes C115 . C116 . H1161 . 120.6 no C117 . C116 . H1161 . 119.6 no C116 . C117 . C118 . 120.8(3) yes C116 . C117 . H1171 . 119.6 no C118 . C117 . H1171 . 119.6 no C117 . C118 . C113 . 119.7(3) yes C117 . C118 . H1181 . 120.6 no C113 . C118 . H1181 . 119.7 no Ni101 . O119 . C120 . 113.49(12) yes Ni101 . O119 . Na136 . 100.04(7) yes C120 . O119 . Na136 . 137.87(13) yes O119 . C120 . C121 . 109.89(17) yes O119 . C120 . C124 . 110.02(17) yes C121 . C120 . C124 . 113.02(18) yes O119 . C120 . H1201 . 106.9 no C121 . C120 . H1201 . 107.9 no C124 . C120 . H1201 . 108.9 no C120 . C121 . N122 . 111.75(19) yes C120 . C121 . C130 . 121.69(19) yes N122 . C121 . C130 . 126.6(2) yes C121 . N122 . Ni101 . 118.10(15) yes C121 . N122 . O123 . 120.03(19) yes Ni101 . N122 . O123 . 121.84(14) yes N122 . O123 . H1231 . 103.7 no C120 . C124 . C125 . 118.4(2) yes C120 . C124 . C129 . 122.8(2) yes C125 . C124 . C129 . 118.7(2) yes C124 . C125 . C126 . 120.8(2) yes C124 . C125 . H1251 . 119.2 no C126 . C125 . H1251 . 120.0 no C125 . C126 . C127 . 120.1(2) yes C125 . C126 . H1261 . 119.3 no C127 . C126 . H1261 . 120.5 no C126 . C127 . C128 . 119.8(2) yes C126 . C127 . H1271 . 120.6 no C128 . C127 . H1271 . 119.6 no C127 . C128 . C129 . 120.3(2) yes C127 . C128 . H1281 . 120.2 no C129 . C128 . H1281 . 119.5 no C128 . C129 . C124 . 120.3(2) yes C128 . C129 . H1291 . 119.7 no C124 . C129 . H1291 . 120.0 no C121 . C130 . C131 . 119.0(2) yes C121 . C130 . C135 . 123.4(2) yes C131 . C130 . C135 . 117.6(2) yes C130 . C131 . C132 . 120.9(2) yes C130 . C131 . H1311 . 120.2 no C132 . C131 . H1311 . 118.9 no C131 . C132 . C133 . 120.5(2) yes C131 . C132 . H1321 . 118.9 no C133 . C132 . H1321 . 120.6 no C132 . C133 . C134 . 119.5(2) yes C132 . C133 . H1331 . 120.8 no C134 . C133 . H1331 . 119.7 no C133 . C134 . C135 . 120.5(2) yes C133 . C134 . H1341 . 120.4 no C135 . C134 . H1341 . 119.2 no C130 . C135 . C134 . 121.0(2) yes C130 . C135 . H1351 . 120.3 no C134 . C135 . H1351 . 118.7 no O119 . Na136 . O102 . 67.11(6) yes O119 . Na136 . Ni101 . 33.89(4) yes O102 . Na136 . Ni101 . 34.39(4) yes O119 . Na136 . O137 . 112.73(7) yes O102 . Na136 . O137 . 122.65(7) yes Ni101 . Na136 . O137 . 117.09(6) yes O119 . Na136 . O139 . 141.45(7) yes O102 . Na136 . O139 . 92.52(7) yes Ni101 . Na136 . O139 . 124.06(5) yes O137 . Na136 . O139 . 105.81(7) yes O119 . Na136 . O141 . 90.84(6) yes O102 . Na136 . O141 . 141.04(7) yes Ni101 . Na136 . O141 . 122.20(5) yes O137 . Na136 . O141 . 95.04(7) yes O139 . Na136 . O141 . 85.53(7) yes Na136 . O137 . C138 . 115.86(18) yes Na136 . O137 . H1371 . 141.0 no C138 . O137 . H1371 . 102.9 no O137 . C138 . H1381 . 109.0 no O137 . C138 . H1382 . 110.2 no H1381 . C138 . H1382 . 110.3 no O137 . C138 . H1383 . 110.0 no H1381 . C138 . H1383 . 108.4 no H1382 . C138 . H1383 . 109.0 no Na136 . O139 . C140 . 123.90(16) yes Na136 . O139 . H1391 . 115.6 no C140 . O139 . H1391 . 106.8 no O139 . C140 . H1401 . 113.3 no O139 . C140 . H1402 . 110.8 no H1401 . C140 . H1402 . 108.7 no O139 . C140 . H1403 . 108.1 no H1401 . C140 . H1403 . 108.2 no H1402 . C140 . H1403 . 107.5 no Na136 . O141 . C142 . 114.99(15) yes Na136 . O141 . H1411 . 118.1 no C142 . O141 . H1411 . 103.3 no O141 . C142 . H1421 . 109.0 no O141 . C142 . H1422 . 111.3 no H1421 . C142 . H1422 . 108.9 no O141 . C142 . H1423 . 113.0 no H1421 . C142 . H1423 . 107.7 no H1422 . C142 . H1423 . 106.8 no