# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_safin143 #TrackingRef 'web_deposit_cif_file_0_DamirSafin_1350208717.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H56 N8 Ni3 O10 P2 S4' _chemical_formula_sum 'C52 H56 N8 Ni3 O10 P2 S4' _chemical_formula_weight 1319.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.2300(18) _cell_length_b 16.8816(11) _cell_length_c 18.0042(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.007(7) _cell_angle_gamma 90.00 _cell_volume 5537.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4862 _cell_measurement_theta_min 1.9701 _cell_measurement_theta_max 25.3114 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 1.284 _exptl_absorpt_correction_T_min 0.66938 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku UltraX 18 rotating anode' _diffrn_radiation_monochromator 'Zr filter' _diffrn_measurement_device_type 'MAR345 image plate' _diffrn_measurement_method '68 images, \D\F 2.0\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13484 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.37 _reflns_number_total 5007 _reflns_number_gt 4016 _reflns_threshold_expression >2sigma(I) _computing_data_collection MAR _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0868P)^2^+26.4755P] 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_number_reflns 5007 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1840 _refine_ls_wR_factor_gt 0.1726 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.56626(4) 0.23235(4) 0.10070(4) 0.0464(2) Uani 1 1 d . . . S2 S 0.53031(12) 0.37373(10) 0.06452(10) 0.0703(5) Uani 1 1 d . . . P3 P 0.53944(12) 0.32499(11) -0.03228(9) 0.0648(5) Uani 1 1 d . . . O4 O 0.5956(3) 0.3643(3) -0.0842(3) 0.0752(14) Uani 1 1 d . . . C5 C 0.6748(4) 0.3631(5) -0.0698(4) 0.078(2) Uani 1 1 d . . . H5 H 0.6897 0.3099 -0.0501 0.094 Uiso 1 1 calc R . . C6 C 0.7056(5) 0.3743(6) -0.1470(5) 0.094(3) Uani 1 1 d . . . H6A H 0.6935 0.3279 -0.1778 0.140 Uiso 1 1 calc R . . H6B H 0.7591 0.3802 -0.1425 0.140 Uiso 1 1 calc R . . H6C H 0.6841 0.4218 -0.1702 0.140 Uiso 1 1 calc R . . C7 C 0.7017(6) 0.4250(5) -0.0175(5) 0.092(3) Uani 1 1 d . . . H7A H 0.6895 0.4774 -0.0379 0.139 Uiso 1 1 calc R . . H7B H 0.7551 0.4204 -0.0103 0.139 Uiso 1 1 calc R . . H7C H 0.6784 0.4183 0.0303 0.139 Uiso 1 1 calc R . . O8 O 0.4643(3) 0.3331(4) -0.0786(3) 0.0844(15) Uani 1 1 d . . . C9 C 0.4508(5) 0.3485(5) -0.1547(4) 0.081(2) Uani 1 1 d . . . H9 H 0.4957 0.3347 -0.1824 0.097 Uiso 1 1 calc R . . C10 C 0.3902(5) 0.2943(5) -0.1787(5) 0.088(2) Uani 1 1 d . . . H10A H 0.4041 0.2395 -0.1671 0.131 Uiso 1 1 calc R . . H10B H 0.3806 0.2998 -0.2323 0.131 Uiso 1 1 calc R . . H10C H 0.3457 0.3080 -0.1524 0.131 Uiso 1 1 calc R . . C11 C 0.4352(6) 0.4344(5) -0.1646(5) 0.099(3) Uani 1 1 d . . . H11A H 0.3989 0.4511 -0.1290 0.149 Uiso 1 1 calc R . . H11B H 0.4159 0.4439 -0.2153 0.149 Uiso 1 1 calc R . . H11C H 0.4806 0.4647 -0.1561 0.149 Uiso 1 1 calc R . . N12 N 0.5578(3) 0.2315(3) -0.0116(3) 0.0560(13) Uani 1 1 d . . . C13 C 0.5741(3) 0.1752(4) -0.0594(3) 0.0539(15) Uani 1 1 d . . . S14 S 0.57577(11) 0.18303(12) -0.15307(9) 0.0675(5) Uani 1 1 d . . . N15 N 0.5917(3) 0.1015(3) -0.0316(3) 0.0555(13) Uani 1 1 d . . . H15 H 0.6109 0.0701 -0.0647 0.067 Uiso 1 1 calc R . . C16 C 0.5857(3) 0.0656(3) 0.0375(3) 0.0453(12) Uani 1 1 d . . . C17 C 0.5858(3) -0.0168(4) 0.0361(3) 0.0521(14) Uani 1 1 d . . . H17 H 0.5901 -0.0439 -0.0097 0.062 Uiso 1 1 calc R . . C18 C 0.5797(3) -0.0589(4) 0.1007(3) 0.0539(14) Uani 1 1 d . . . H18 H 0.5787 -0.1152 0.0999 0.065 Uiso 1 1 calc R . . C19 C 0.5752(3) -0.0182(3) 0.1669(3) 0.0492(13) Uani 1 1 d . . . H19 H 0.5695 -0.0454 0.2125 0.059 Uiso 1 1 calc R . . C20 C 0.5791(3) 0.0639(3) 0.1645(3) 0.0423(12) Uani 1 1 d . . . N21 N 0.5827(2) 0.1072(3) 0.1006(2) 0.0423(10) Uani 1 1 d . . . N22 N 0.5799(2) 0.1076(2) 0.2315(2) 0.0347(9) Uani 1 1 d . . . C23 C 0.6308(3) 0.0882(3) 0.2794(3) 0.0403(12) Uani 1 1 d . . . H23 H 0.6633 0.0477 0.2647 0.048 Uiso 1 1 calc R . . C24 C 0.6444(3) 0.1202(3) 0.3525(3) 0.0398(11) Uani 1 1 d . . . C25 C 0.7105(3) 0.0967(4) 0.3887(3) 0.0515(14) Uani 1 1 d . . . H25 H 0.7410 0.0595 0.3649 0.062 Uiso 1 1 calc R . . C26 C 0.7325(3) 0.1256(4) 0.4572(3) 0.0557(15) Uani 1 1 d . . . H26 H 0.7773 0.1090 0.4809 0.067 Uiso 1 1 calc R . . C27 C 0.6870(3) 0.1799(3) 0.4905(3) 0.0508(14) Uani 1 1 d . . . H27 H 0.7018 0.2013 0.5375 0.061 Uiso 1 1 calc R . . C28 C 0.6214(3) 0.2038(3) 0.4579(3) 0.0463(13) Uani 1 1 d . . . H28 H 0.5918 0.2407 0.4831 0.056 Uiso 1 1 calc R . . C29 C 0.5972(3) 0.1745(3) 0.3875(3) 0.0382(11) Uani 1 1 d . . . O30 O 0.53461(19) 0.19733(19) 0.35781(18) 0.0388(8) Uani 1 1 d . . . Ni31 Ni 0.5000 0.19090(5) 0.2500 0.0337(2) Uani 1 2 d S . . O32 O 0.5750(2) 0.2669(2) 0.20751(19) 0.0429(8) Uani 1 1 d . . . C33 C 0.6224(3) 0.3144(3) 0.2382(3) 0.0460(13) Uani 1 1 d . . . C34 C 0.6080(4) 0.3513(3) 0.3037(3) 0.0553(15) Uani 1 1 d . . . H34 H 0.5614 0.3441 0.3246 0.066 Uiso 1 1 calc R . . C35 C 0.6592(4) 0.3988(4) 0.3403(4) 0.0706(19) Uani 1 1 d . . . H35 H 0.6474 0.4234 0.3859 0.085 Uiso 1 1 calc R . . C36 C 0.7285(4) 0.4109(5) 0.3108(5) 0.078(2) Uani 1 1 d . . . H36 H 0.7640 0.4428 0.3364 0.093 Uiso 1 1 calc R . . C37 C 0.7439(4) 0.3770(4) 0.2463(4) 0.0675(18) Uani 1 1 d . . . H37 H 0.7909 0.3850 0.2265 0.081 Uiso 1 1 calc R . . C38 C 0.6922(3) 0.3294(4) 0.2067(4) 0.0556(15) Uani 1 1 d . . . C39 C 0.7130(4) 0.2967(4) 0.1371(4) 0.0614(16) Uani 1 1 d . . . H39 H 0.7617 0.3077 0.1232 0.074 Uiso 1 1 calc R . . O40 O 0.6761(2) 0.2560(3) 0.0928(2) 0.0593(11) Uani 1 1 d . . . 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 0.0520(5) 0.0475(4) 0.0399(4) 0.0002(3) 0.0054(3) -0.0110(3) S2 0.0978(14) 0.0532(9) 0.0602(10) 0.0068(8) 0.0053(9) -0.0054(9) P3 0.0847(13) 0.0615(10) 0.0481(9) 0.0114(7) 0.0008(9) -0.0155(9) O4 0.087(4) 0.075(3) 0.064(3) 0.012(2) 0.011(3) -0.021(3) C5 0.075(5) 0.086(5) 0.074(5) 0.013(4) 0.007(4) -0.009(4) C6 0.087(6) 0.111(7) 0.084(5) 0.013(5) 0.017(5) -0.026(5) C7 0.117(7) 0.068(5) 0.092(6) 0.007(4) -0.001(5) -0.034(5) O8 0.087(4) 0.104(4) 0.063(3) 0.016(3) 0.002(3) -0.007(3) C9 0.088(6) 0.087(5) 0.068(5) 0.011(4) 0.010(4) 0.009(4) C10 0.080(6) 0.083(5) 0.101(6) -0.004(5) 0.007(5) 0.010(4) C11 0.126(8) 0.076(5) 0.096(6) 0.003(5) -0.004(6) 0.015(5) N12 0.062(3) 0.060(3) 0.047(3) 0.000(2) 0.009(2) -0.013(2) C13 0.050(3) 0.063(4) 0.049(3) 0.002(3) 0.009(3) -0.012(3) S14 0.0747(12) 0.0831(12) 0.0454(8) 0.0028(8) 0.0120(8) -0.0157(9) N15 0.055(3) 0.066(3) 0.046(3) -0.009(2) 0.013(2) -0.008(2) C16 0.038(3) 0.055(3) 0.043(3) -0.005(2) 0.004(2) -0.006(2) C17 0.045(3) 0.060(4) 0.051(3) -0.013(3) 0.006(3) 0.006(3) C18 0.052(4) 0.047(3) 0.063(4) -0.010(3) 0.004(3) 0.006(3) C19 0.047(3) 0.047(3) 0.055(3) -0.002(3) 0.005(3) 0.005(3) C20 0.036(3) 0.045(3) 0.046(3) -0.002(2) 0.005(2) 0.003(2) N21 0.038(2) 0.047(2) 0.042(2) -0.0066(19) 0.0065(19) -0.0045(19) N22 0.035(2) 0.036(2) 0.034(2) 0.0015(16) 0.0063(17) -0.0035(17) C23 0.038(3) 0.038(3) 0.046(3) 0.002(2) 0.008(2) 0.000(2) C24 0.040(3) 0.040(3) 0.039(3) 0.006(2) 0.001(2) -0.002(2) C25 0.045(3) 0.055(3) 0.055(3) 0.006(3) -0.002(3) 0.002(3) C26 0.046(3) 0.064(4) 0.056(4) 0.015(3) -0.009(3) -0.004(3) C27 0.056(4) 0.053(3) 0.043(3) 0.008(2) -0.009(3) -0.014(3) C28 0.054(3) 0.043(3) 0.042(3) 0.003(2) 0.004(2) -0.009(2) C29 0.042(3) 0.034(2) 0.038(3) 0.011(2) -0.001(2) -0.009(2) O30 0.044(2) 0.0382(18) 0.0345(18) 0.0007(14) 0.0038(15) 0.0018(15) Ni31 0.0385(5) 0.0317(4) 0.0310(4) 0.000 0.0025(4) 0.000 O32 0.049(2) 0.0411(19) 0.0386(19) 0.0011(15) 0.0043(16) -0.0114(17) C33 0.049(3) 0.042(3) 0.047(3) 0.008(2) -0.004(2) -0.005(2) C34 0.055(4) 0.047(3) 0.064(4) 0.002(3) -0.001(3) -0.013(3) C35 0.079(5) 0.067(4) 0.066(4) -0.016(3) 0.003(4) -0.023(4) C36 0.064(5) 0.076(5) 0.092(5) -0.027(4) -0.005(4) -0.024(4) C37 0.061(4) 0.067(4) 0.075(4) -0.014(4) 0.002(3) -0.021(3) C38 0.052(4) 0.049(3) 0.066(4) -0.002(3) 0.001(3) -0.013(3) C39 0.051(4) 0.066(4) 0.068(4) -0.002(3) 0.008(3) -0.015(3) O40 0.057(3) 0.066(3) 0.055(2) -0.008(2) 0.011(2) -0.020(2) _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 O32 2.010(4) . ? Ni1 N12 2.022(5) . ? Ni1 O40 2.052(4) . ? Ni1 O30 2.094(3) 2_655 ? Ni1 N21 2.134(5) . ? Ni1 S2 2.5534(19) . ? S2 P3 1.940(3) . ? P3 O4 1.557(5) . ? P3 O8 1.584(6) . ? P3 N12 1.653(6) . ? O4 C5 1.459(9) . ? C5 C7 1.480(11) . ? C5 C6 1.528(10) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O8 C9 1.408(9) . ? C9 C11 1.487(11) . ? C9 C10 1.488(12) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N12 C13 1.324(8) . ? C13 N15 1.376(8) . ? C13 S14 1.692(6) . ? N15 C16 1.390(7) . ? N15 H15 0.8800 . ? C16 N21 1.339(7) . ? C16 C17 1.391(8) . ? C17 C18 1.370(8) . ? C17 H17 0.9500 . ? C18 C19 1.381(8) . ? C18 H18 0.9500 . ? C19 C20 1.388(8) . ? C19 H19 0.9500 . ? C20 N21 1.366(7) . ? C20 N22 1.414(6) . ? N22 C23 1.286(7) . ? N22 Ni31 2.061(4) . ? C23 C24 1.436(7) . ? C23 H23 0.9500 . ? C24 C25 1.407(8) . ? C24 C29 1.419(7) . ? C25 C26 1.374(8) . ? C25 H25 0.9500 . ? C26 C27 1.386(9) . ? C26 H26 0.9500 . ? C27 C28 1.374(8) . ? C27 H27 0.9500 . ? C28 C29 1.417(7) . ? C28 H28 0.9500 . ? C29 O30 1.301(6) . ? O30 Ni31 2.023(3) . ? O30 Ni1 2.094(3) 2_655 ? Ni31 O30 2.023(3) 2_655 ? Ni31 O32 2.042(3) . ? Ni31 O32 2.042(3) 2_655 ? Ni31 N22 2.061(4) 2_655 ? O32 C33 1.291(7) . ? C33 C34 1.367(8) . ? C33 C38 1.433(8) . ? C34 C35 1.379(9) . ? C34 H34 0.9500 . ? C35 C36 1.403(10) . ? C35 H35 0.9500 . ? C36 C37 1.333(10) . ? C36 H36 0.9500 . ? C37 C38 1.412(9) . ? C37 H37 0.9500 . ? C38 C39 1.432(9) . ? C39 O40 1.233(7) . ? C39 H39 0.9500 . ? 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 O32 Ni1 N12 163.55(18) . . ? O32 Ni1 O40 88.02(16) . . ? N12 Ni1 O40 88.44(19) . . ? O32 Ni1 O30 77.37(14) . 2_655 ? N12 Ni1 O30 108.50(18) . 2_655 ? O40 Ni1 O30 161.99(16) . 2_655 ? O32 Ni1 N21 106.32(15) . . ? N12 Ni1 N21 89.91(19) . . ? O40 Ni1 N21 93.16(17) . . ? O30 Ni1 N21 81.14(14) 2_655 . ? O32 Ni1 S2 89.09(11) . . ? N12 Ni1 S2 75.02(16) . . ? O40 Ni1 S2 92.45(14) . . ? O30 Ni1 S2 97.71(11) 2_655 . ? N21 Ni1 S2 163.76(13) . . ? P3 S2 Ni1 78.66(8) . . ? O4 P3 O8 102.8(3) . . ? O4 P3 N12 114.2(3) . . ? O8 P3 N12 111.5(3) . . ? O4 P3 S2 115.9(2) . . ? O8 P3 S2 109.6(2) . . ? N12 P3 S2 103.02(19) . . ? C5 O4 P3 123.7(5) . . ? O4 C5 C7 114.0(7) . . ? O4 C5 C6 103.3(6) . . ? C7 C5 C6 111.6(7) . . ? O4 C5 H5 109.2 . . ? C7 C5 H5 109.2 . . ? C6 C5 H5 109.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 O8 P3 130.2(5) . . ? O8 C9 C11 108.8(7) . . ? O8 C9 C10 105.8(7) . . ? C11 C9 C10 115.3(8) . . ? O8 C9 H9 108.9 . . ? C11 C9 H9 108.9 . . ? C10 C9 H9 108.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 N12 P3 126.0(4) . . ? C13 N12 Ni1 130.1(4) . . ? P3 N12 Ni1 103.1(3) . . ? N12 C13 N15 117.8(5) . . ? N12 C13 S14 127.2(5) . . ? N15 C13 S14 115.0(4) . . ? C13 N15 C16 134.1(5) . . ? C13 N15 H15 112.9 . . ? C16 N15 H15 112.9 . . ? N21 C16 N15 122.5(5) . . ? N21 C16 C17 122.6(5) . . ? N15 C16 C17 114.9(5) . . ? C18 C17 C16 120.3(5) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 118.9(5) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C18 C19 C20 117.7(5) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? N21 C20 C19 124.4(5) . . ? N21 C20 N22 116.1(4) . . ? C19 C20 N22 119.6(5) . . ? C16 N21 C20 116.0(5) . . ? C16 N21 Ni1 122.0(4) . . ? C20 N21 Ni1 121.2(3) . . ? C23 N22 C20 115.2(4) . . ? C23 N22 Ni31 124.2(3) . . ? C20 N22 Ni31 120.5(3) . . ? N22 C23 C24 128.1(5) . . ? N22 C23 H23 116.0 . . ? C24 C23 H23 116.0 . . ? C25 C24 C29 120.0(5) . . ? C25 C24 C23 115.8(5) . . ? C29 C24 C23 124.2(5) . . ? C26 C25 C24 122.2(6) . . ? C26 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C25 C26 C27 117.6(6) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C28 C27 C26 122.3(6) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 121.2(5) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? O30 C29 C28 120.4(5) . . ? O30 C29 C24 123.0(5) . . ? C28 C29 C24 116.6(5) . . ? C29 O30 Ni31 128.2(3) . . ? C29 O30 Ni1 134.8(3) . 2_655 ? Ni31 O30 Ni1 96.27(15) . 2_655 ? O30 Ni31 O30 173.84(19) 2_655 . ? O30 Ni31 O32 78.29(14) 2_655 . ? O30 Ni31 O32 97.79(14) . . ? O30 Ni31 O32 97.79(14) 2_655 2_655 ? O30 Ni31 O32 78.29(14) . 2_655 ? O32 Ni31 O32 102.2(2) . 2_655 ? O30 Ni31 N22 89.61(15) 2_655 2_655 ? O30 Ni31 N22 94.60(15) . 2_655 ? O32 Ni31 N22 167.26(14) . 2_655 ? O32 Ni31 N22 83.20(15) 2_655 2_655 ? O30 Ni31 N22 94.60(15) 2_655 . ? O30 Ni31 N22 89.60(15) . . ? O32 Ni31 N22 83.21(15) . . ? O32 Ni31 N22 167.26(14) 2_655 . ? N22 Ni31 N22 93.9(2) 2_655 . ? C33 O32 Ni1 128.2(3) . . ? C33 O32 Ni31 132.7(3) . . ? Ni1 O32 Ni31 98.35(15) . . ? O32 C33 C34 120.4(5) . . ? O32 C33 C38 122.1(5) . . ? C34 C33 C38 117.4(5) . . ? C33 C34 C35 122.0(6) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C34 C35 C36 120.4(7) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 119.2(6) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C36 C37 C38 121.8(7) . . ? C36 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C37 C38 C39 118.0(6) . . ? C37 C38 C33 119.1(6) . . ? C39 C38 C33 122.9(5) . . ? O40 C39 C38 128.7(6) . . ? O40 C39 H39 115.6 . . ? C38 C39 H39 115.6 . . ? C39 O40 Ni1 125.1(4) . . ? 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 O32 Ni1 S2 P3 172.95(13) . . . . ? N12 Ni1 S2 P3 -2.76(17) . . . . ? O40 Ni1 S2 P3 84.97(14) . . . . ? O30 Ni1 S2 P3 -109.93(12) 2_655 . . . ? N21 Ni1 S2 P3 -25.2(5) . . . . ? Ni1 S2 P3 O4 -122.1(3) . . . . ? Ni1 S2 P3 O8 122.1(2) . . . . ? Ni1 S2 P3 N12 3.3(2) . . . . ? O8 P3 O4 C5 -172.4(6) . . . . ? N12 P3 O4 C5 -51.5(6) . . . . ? S2 P3 O4 C5 68.0(6) . . . . ? P3 O4 C5 C7 -82.7(8) . . . . ? P3 O4 C5 C6 156.1(5) . . . . ? O4 P3 O8 C9 17.5(8) . . . . ? N12 P3 O8 C9 -105.2(7) . . . . ? S2 P3 O8 C9 141.4(7) . . . . ? P3 O8 C9 C11 -97.8(9) . . . . ? P3 O8 C9 C10 137.8(7) . . . . ? O4 P3 N12 C13 -48.1(6) . . . . ? O8 P3 N12 C13 67.8(6) . . . . ? S2 P3 N12 C13 -174.7(5) . . . . ? O4 P3 N12 Ni1 122.3(3) . . . . ? O8 P3 N12 Ni1 -121.7(3) . . . . ? S2 P3 N12 Ni1 -4.3(3) . . . . ? O32 Ni1 N12 C13 157.8(6) . . . . ? O40 Ni1 N12 C13 80.2(5) . . . . ? O30 Ni1 N12 C13 -93.6(5) 2_655 . . . ? N21 Ni1 N12 C13 -13.0(5) . . . . ? S2 Ni1 N12 C13 173.1(6) . . . . ? O32 Ni1 N12 P3 -12.1(8) . . . . ? O40 Ni1 N12 P3 -89.7(3) . . . . ? O30 Ni1 N12 P3 96.5(2) 2_655 . . . ? N21 Ni1 N12 P3 177.1(3) . . . . ? S2 Ni1 N12 P3 3.3(2) . . . . ? P3 N12 C13 N15 176.6(4) . . . . ? Ni1 N12 C13 N15 8.8(8) . . . . ? P3 N12 C13 S14 -3.7(9) . . . . ? Ni1 N12 C13 S14 -171.5(3) . . . . ? N12 C13 N15 C16 12.2(10) . . . . ? S14 C13 N15 C16 -167.5(5) . . . . ? C13 N15 C16 N21 -23.7(10) . . . . ? C13 N15 C16 C17 158.6(6) . . . . ? N21 C16 C17 C18 2.7(9) . . . . ? N15 C16 C17 C18 -179.6(5) . . . . ? C16 C17 C18 C19 -1.4(9) . . . . ? C17 C18 C19 C20 -1.8(8) . . . . ? C18 C19 C20 N21 4.2(8) . . . . ? C18 C19 C20 N22 -175.6(5) . . . . ? N15 C16 N21 C20 -178.1(5) . . . . ? C17 C16 N21 C20 -0.5(8) . . . . ? N15 C16 N21 Ni1 11.9(7) . . . . ? C17 C16 N21 Ni1 -170.5(4) . . . . ? C19 C20 N21 C16 -3.0(8) . . . . ? N22 C20 N21 C16 176.8(4) . . . . ? C19 C20 N21 Ni1 167.1(4) . . . . ? N22 C20 N21 Ni1 -13.2(6) . . . . ? O32 Ni1 N21 C16 -175.2(4) . . . . ? N12 Ni1 N21 C16 2.1(4) . . . . ? O40 Ni1 N21 C16 -86.3(4) . . . . ? O30 Ni1 N21 C16 110.9(4) 2_655 . . . ? S2 Ni1 N21 C16 23.7(7) . . . . ? O32 Ni1 N21 C20 15.3(4) . . . . ? N12 Ni1 N21 C20 -167.4(4) . . . . ? O40 Ni1 N21 C20 104.2(4) . . . . ? O30 Ni1 N21 C20 -58.6(4) 2_655 . . . ? S2 Ni1 N21 C20 -145.8(4) . . . . ? N21 C20 N22 C23 -124.4(5) . . . . ? C19 C20 N22 C23 55.4(6) . . . . ? N21 C20 N22 Ni31 59.1(5) . . . . ? C19 C20 N22 Ni31 -121.1(5) . . . . ? C20 N22 C23 C24 -178.4(5) . . . . ? Ni31 N22 C23 C24 -2.0(7) . . . . ? N22 C23 C24 C25 -170.5(5) . . . . ? N22 C23 C24 C29 7.3(8) . . . . ? C29 C24 C25 C26 -1.2(8) . . . . ? C23 C24 C25 C26 176.7(5) . . . . ? C24 C25 C26 C27 -0.2(9) . . . . ? C25 C26 C27 C28 1.2(8) . . . . ? C26 C27 C28 C29 -0.7(8) . . . . ? C27 C28 C29 O30 179.5(5) . . . . ? C27 C28 C29 C24 -0.7(7) . . . . ? C25 C24 C29 O30 -178.6(5) . . . . ? C23 C24 C29 O30 3.7(7) . . . . ? C25 C24 C29 C28 1.6(7) . . . . ? C23 C24 C29 C28 -176.1(5) . . . . ? C28 C29 O30 Ni31 161.1(3) . . . . ? C24 C29 O30 Ni31 -18.8(6) . . . . ? C28 C29 O30 Ni1 -31.1(7) . . . 2_655 ? C24 C29 O30 Ni1 149.0(4) . . . 2_655 ? C29 O30 Ni31 O32 -64.8(4) . . . . ? Ni1 O30 Ni31 O32 123.89(14) 2_655 . . . ? C29 O30 Ni31 O32 -165.7(4) . . . 2_655 ? Ni1 O30 Ni31 O32 22.96(14) 2_655 . . 2_655 ? C29 O30 Ni31 N22 112.2(4) . . . 2_655 ? Ni1 O30 Ni31 N22 -59.12(15) 2_655 . . 2_655 ? C29 O30 Ni31 N22 18.3(4) . . . . ? Ni1 O30 Ni31 N22 -153.03(15) 2_655 . . . ? C23 N22 Ni31 O30 167.7(4) . . . 2_655 ? C20 N22 Ni31 O30 -16.1(4) . . . 2_655 ? C23 N22 Ni31 O30 -7.8(4) . . . . ? C20 N22 Ni31 O30 168.4(3) . . . . ? C23 N22 Ni31 O32 90.1(4) . . . . ? C20 N22 Ni31 O32 -93.7(4) . . . . ? C23 N22 Ni31 O32 -25.9(9) . . . 2_655 ? C20 N22 Ni31 O32 150.3(6) . . . 2_655 ? C23 N22 Ni31 N22 -102.3(4) . . . 2_655 ? C20 N22 Ni31 N22 73.8(3) . . . 2_655 ? N12 Ni1 O32 C33 -52.7(9) . . . . ? O40 Ni1 O32 C33 24.9(5) . . . . ? O30 Ni1 O32 C33 -165.6(5) 2_655 . . . ? N21 Ni1 O32 C33 117.7(4) . . . . ? S2 Ni1 O32 C33 -67.5(4) . . . . ? N12 Ni1 O32 Ni31 136.2(6) . . . . ? O40 Ni1 O32 Ni31 -146.10(18) . . . . ? O30 Ni1 O32 Ni31 23.31(14) 2_655 . . . ? N21 Ni1 O32 Ni31 -53.39(19) . . . . ? S2 Ni1 O32 Ni31 121.41(13) . . . . ? O30 Ni31 O32 C33 165.5(5) 2_655 . . . ? O30 Ni31 O32 C33 -9.7(5) . . . . ? O32 Ni31 O32 C33 69.9(5) 2_655 . . . ? N22 Ni31 O32 C33 -176.0(6) 2_655 . . . ? N22 Ni31 O32 C33 -98.4(5) . . . . ? O30 Ni31 O32 Ni1 -24.09(15) 2_655 . . . ? O30 Ni31 O32 Ni1 160.72(15) . . . . ? O32 Ni31 O32 Ni1 -119.64(19) 2_655 . . . ? N22 Ni31 O32 Ni1 -5.6(8) 2_655 . . . ? N22 Ni31 O32 Ni1 72.06(17) . . . . ? Ni1 O32 C33 C34 159.0(4) . . . . ? Ni31 O32 C33 C34 -33.0(8) . . . . ? Ni1 O32 C33 C38 -22.3(8) . . . . ? Ni31 O32 C33 C38 145.6(5) . . . . ? O32 C33 C34 C35 176.0(6) . . . . ? C38 C33 C34 C35 -2.6(9) . . . . ? C33 C34 C35 C36 0.3(11) . . . . ? C34 C35 C36 C37 1.0(13) . . . . ? C35 C36 C37 C38 0.3(12) . . . . ? C36 C37 C38 C39 178.7(7) . . . . ? C36 C37 C38 C33 -2.7(11) . . . . ? O32 C33 C38 C37 -174.8(6) . . . . ? C34 C33 C38 C37 3.8(9) . . . . ? O32 C33 C38 C39 3.6(9) . . . . ? C34 C33 C38 C39 -177.7(6) . . . . ? C37 C38 C39 O40 -177.5(7) . . . . ? C33 C38 C39 O40 4.0(12) . . . . ? C38 C39 O40 Ni1 7.2(10) . . . . ? O32 Ni1 O40 C39 -16.8(5) . . . . ? N12 Ni1 O40 C39 147.1(6) . . . . ? O30 Ni1 O40 C39 -52.3(8) 2_655 . . . ? N21 Ni1 O40 C39 -123.1(6) . . . . ? S2 Ni1 O40 C39 72.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.840 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.101 _database_code_depnum_ccdc_archive 'CCDC 905820' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_safin145 #TrackingRef 'web_deposit_cif_file_1_DamirSafin_1350208717.2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H52 Cl4 N8 Ni3 O10 P2 S4, 2(H2 O)' _chemical_formula_sum 'C52 H56 Cl4 N8 Ni3 O12 P2 S4' _chemical_formula_weight 1493.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.988(9) _cell_length_b 10.7792(10) _cell_length_c 23.245(6) _cell_angle_alpha 90.00 _cell_angle_beta 130.83(4) _cell_angle_gamma 90.00 _cell_volume 6444(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3316 _cell_measurement_theta_min 2.0787 _cell_measurement_theta_max 21.2457 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 1.276 _exptl_absorpt_correction_T_min 0.86710 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku UltraX 18 rotating anode' _diffrn_radiation_monochromator 'Zr filter' _diffrn_measurement_device_type 'MAR345 image plate' _diffrn_measurement_method '100 images, \D\F 2.0\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13902 _diffrn_reflns_av_R_equivalents 0.0948 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 21.29 _reflns_number_total 3579 _reflns_number_gt 2515 _reflns_threshold_expression >2sigma(I) _computing_data_collection MAR _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1106P)^2^+0.0000P] 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_number_reflns 3579 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1804 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _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 0.10588(3) 0.71577(8) 0.40499(6) 0.0651(4) Uani 1 1 d . . . S2 S 0.11099(8) 0.48850(18) 0.44313(13) 0.0822(7) Uani 1 1 d . . . P3 P 0.15645(8) 0.57122(19) 0.54209(13) 0.0747(6) Uani 1 1 d . . . O4 O 0.2134(2) 0.5209(5) 0.5977(3) 0.0934(17) Uani 1 1 d . . . C5 C 0.2485(5) 0.5232(16) 0.5834(8) 0.157(6) Uani 1 1 d . . . H5 H 0.2350 0.5799 0.5411 0.188 Uiso 1 1 calc R . . C6 C 0.2519(7) 0.4025(19) 0.5632(12) 0.272(12) Uani 1 1 d . . . H6A H 0.2585 0.3439 0.5998 0.408 Uiso 1 1 calc R . . H6B H 0.2798 0.3995 0.5624 0.408 Uiso 1 1 calc R . . H6C H 0.2198 0.3820 0.5138 0.408 Uiso 1 1 calc R . . C7 C 0.2986(6) 0.5715(16) 0.6532(15) 0.317(14) Uani 1 1 d . . . H7A H 0.3030 0.5472 0.6968 0.475 Uiso 1 1 calc R . . H7B H 0.2988 0.6604 0.6507 0.475 Uiso 1 1 calc R . . H7C H 0.3266 0.5384 0.6573 0.475 Uiso 1 1 calc R . . O8 O 0.1395(2) 0.5561(5) 0.5892(3) 0.0868(16) Uani 1 1 d . . . C9 C 0.1202(4) 0.4389(10) 0.5946(7) 0.114(3) Uani 1 1 d . . . H9 H 0.1086 0.3902 0.5503 0.137 Uiso 1 1 calc R . . C10 C 0.1598(5) 0.3714(17) 0.6567(9) 0.244(10) Uani 1 1 d . . . H10A H 0.1502 0.2853 0.6488 0.366 Uiso 1 1 calc R . . H10B H 0.1661 0.4006 0.7011 0.366 Uiso 1 1 calc R . . H10C H 0.1908 0.3810 0.6637 0.366 Uiso 1 1 calc R . . C11 C 0.0737(5) 0.4620(10) 0.5838(8) 0.160(5) Uani 1 1 d . . . H11A H 0.0613 0.3853 0.5879 0.240 Uiso 1 1 calc R . . H11B H 0.0473 0.4972 0.5344 0.240 Uiso 1 1 calc R . . H11C H 0.0817 0.5187 0.6221 0.240 Uiso 1 1 calc R . . N12 N 0.1522(2) 0.7182(5) 0.5195(4) 0.0704(17) Uani 1 1 d . . . C13 C 0.1772(3) 0.8128(9) 0.5691(5) 0.085(2) Uani 1 1 d . . . S14 S 0.21727(15) 0.8018(3) 0.66422(18) 0.1559(15) Uani 1 1 d . . . N15 N 0.1699(3) 0.9283(7) 0.5394(5) 0.088(2) Uani 1 1 d . . . H15 H 0.1894 0.9829 0.5743 0.106 Uiso 1 1 calc R . . C16 C 0.1391(3) 0.9793(7) 0.4675(6) 0.070(2) Uani 1 1 d . . . C17 C 0.1396(4) 1.1108(8) 0.4653(6) 0.086(3) Uani 1 1 d . . . H17 H 0.1599 1.1570 0.5100 0.104 Uiso 1 1 calc R . . C18 C 0.1100(4) 1.1674(9) 0.3967(7) 0.097(3) Uani 1 1 d . . . H18 H 0.1097 1.2535 0.3941 0.116 Uiso 1 1 calc R . . C19 C 0.0808(4) 1.1000(8) 0.3318(6) 0.086(3) Uani 1 1 d . . . H19 H 0.0598 1.1388 0.2846 0.103 Uiso 1 1 calc R . . C20 C 0.0829(3) 0.9727(7) 0.3374(6) 0.071(2) Uani 1 1 d . . . N21 N 0.1117(2) 0.9108(6) 0.4046(4) 0.0656(16) Uani 1 1 d . . . N22 N 0.0530(2) 0.9006(5) 0.2709(4) 0.0616(15) Uani 1 1 d . . . C23 C 0.0604(3) 0.9204(7) 0.2233(5) 0.072(2) Uani 1 1 d . . . H23 H 0.0861 0.9782 0.2391 0.087 Uiso 1 1 calc R . . C24 C 0.0355(3) 0.8676(7) 0.1519(5) 0.068(2) Uani 1 1 d . . . C25 C 0.0555(3) 0.8993(7) 0.1155(5) 0.077(2) Uani 1 1 d . . . H25 H 0.0851 0.9486 0.1413 0.092 Uiso 1 1 calc R . . C26 C 0.0326(3) 0.8594(8) 0.0452(5) 0.077(2) Uani 1 1 d . . . C27 C -0.0129(3) 0.7893(8) 0.0041(5) 0.084(2) Uani 1 1 d . . . H27 H -0.0295 0.7648 -0.0455 0.100 Uiso 1 1 calc R . . C28 C -0.0327(3) 0.7571(7) 0.0374(5) 0.077(2) Uani 1 1 d . . . H28 H -0.0629 0.7095 0.0096 0.092 Uiso 1 1 calc R . . C29 C -0.0101(3) 0.7921(6) 0.1117(5) 0.065(2) Uani 1 1 d . . . O30 O -0.03042(17) 0.7579(4) 0.1414(3) 0.0600(13) Uani 1 1 d . . . Cl31 Cl 0.05936(10) 0.8938(2) 0.00380(15) 0.1038(8) Uani 1 1 d . . . Ni32 Ni 0.0000 0.77096(11) 0.2500 0.0597(4) Uani 1 2 d S . . O33 O 0.06244(16) 0.6553(4) 0.2960(3) 0.0631(12) Uani 1 1 d . . . C34 C 0.0754(3) 0.5600(6) 0.2764(4) 0.0587(18) Uani 1 1 d . . . C35 C 0.0369(3) 0.4833(7) 0.2161(5) 0.074(2) Uani 1 1 d . . . H35 H 0.0021 0.5028 0.1887 0.088 Uiso 1 1 calc R . . C36 C 0.0497(3) 0.3798(7) 0.1967(5) 0.079(2) Uani 1 1 d . . . H36 H 0.0237 0.3286 0.1573 0.095 Uiso 1 1 calc R . . C37 C 0.1014(4) 0.3525(8) 0.2365(5) 0.077(2) Uani 1 1 d . . . C38 C 0.1398(3) 0.4272(8) 0.2922(5) 0.080(2) Uani 1 1 d . . . H38 H 0.1742 0.4091 0.3161 0.096 Uiso 1 1 calc R . . C39 C 0.1281(3) 0.5329(7) 0.3148(4) 0.067(2) Uani 1 1 d . . . Cl40 Cl 0.11717(11) 0.2226(2) 0.20965(16) 0.1152(9) Uani 1 1 d . . . C41 C 0.1700(3) 0.6074(8) 0.3746(5) 0.082(2) Uani 1 1 d . . . H41 H 0.2023 0.5915 0.3888 0.098 Uiso 1 1 calc R . . O42 O 0.16901(18) 0.6918(5) 0.4107(3) 0.0814(15) Uani 1 1 d . . . O101 O 0.2419(4) 0.1005(9) 0.6797(5) 0.202(4) Uani 1 1 d . . . H10D H 0.2234 0.0739 0.6893 0.303 Uiso 1 1 d R . . H10E H 0.2659 0.1401 0.7192 0.303 Uiso 1 1 d 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 0.0502(6) 0.0665(7) 0.0841(8) -0.0092(5) 0.0463(6) -0.0020(4) S2 0.0799(15) 0.0712(13) 0.0941(18) -0.0088(11) 0.0562(14) -0.0018(10) P3 0.0546(13) 0.0791(14) 0.0872(16) -0.0019(12) 0.0449(13) 0.0034(10) O4 0.062(3) 0.095(4) 0.118(5) 0.011(3) 0.056(4) 0.006(3) C5 0.084(8) 0.229(15) 0.170(13) 0.090(11) 0.089(10) 0.056(9) C6 0.180(16) 0.32(3) 0.36(3) -0.14(2) 0.196(19) -0.006(16) C7 0.120(13) 0.227(19) 0.58(4) 0.07(2) 0.22(2) 0.009(12) O8 0.081(4) 0.091(4) 0.097(4) -0.008(3) 0.062(4) -0.006(3) C9 0.106(8) 0.119(8) 0.136(10) 0.013(7) 0.087(8) 0.010(7) C10 0.105(10) 0.29(2) 0.194(16) 0.134(16) 0.037(11) 0.007(12) C11 0.172(12) 0.104(8) 0.263(17) -0.016(9) 0.168(13) -0.022(8) N12 0.050(4) 0.075(4) 0.076(5) -0.010(4) 0.037(4) -0.003(3) C13 0.068(6) 0.079(6) 0.085(6) -0.015(6) 0.040(5) -0.012(5) S14 0.163(3) 0.113(2) 0.089(2) -0.0175(17) 0.037(2) -0.033(2) N15 0.080(5) 0.084(5) 0.088(6) -0.028(5) 0.049(5) -0.025(4) C16 0.060(5) 0.072(6) 0.097(7) -0.021(6) 0.059(6) -0.013(4) C17 0.098(7) 0.064(6) 0.124(8) -0.039(6) 0.084(7) -0.017(5) C18 0.129(8) 0.065(6) 0.133(9) -0.008(7) 0.102(8) 0.003(6) C19 0.109(7) 0.073(6) 0.111(8) -0.021(6) 0.087(7) -0.009(5) C20 0.075(6) 0.060(6) 0.114(8) -0.014(5) 0.077(6) -0.008(4) N21 0.052(4) 0.068(4) 0.088(5) -0.013(4) 0.051(4) -0.006(3) N22 0.056(4) 0.059(4) 0.082(5) -0.006(3) 0.051(4) -0.006(3) C23 0.072(5) 0.066(5) 0.108(7) -0.004(5) 0.072(6) -0.011(4) C24 0.063(5) 0.076(5) 0.084(6) -0.008(5) 0.057(5) -0.012(4) C25 0.069(5) 0.084(5) 0.102(7) 0.001(5) 0.067(6) -0.005(4) C26 0.079(6) 0.090(6) 0.088(7) 0.005(5) 0.066(6) 0.003(5) C27 0.074(6) 0.111(6) 0.074(6) -0.009(5) 0.052(5) -0.009(5) C28 0.064(5) 0.096(6) 0.085(6) 0.002(5) 0.055(5) -0.010(4) C29 0.066(5) 0.065(5) 0.084(6) 0.003(4) 0.058(5) 0.009(4) O30 0.055(3) 0.065(3) 0.077(3) 0.008(2) 0.051(3) 0.000(2) Cl31 0.1148(19) 0.1235(18) 0.130(2) 0.0098(15) 0.1046(19) -0.0010(14) Ni32 0.0502(8) 0.0628(8) 0.0819(10) 0.000 0.0501(8) 0.000 O33 0.048(3) 0.074(3) 0.071(3) -0.004(3) 0.040(3) 0.006(2) C34 0.061(5) 0.058(4) 0.070(5) 0.014(4) 0.049(5) 0.015(4) C35 0.064(5) 0.082(5) 0.083(6) 0.001(5) 0.051(5) 0.007(4) C36 0.084(6) 0.082(6) 0.081(6) -0.018(5) 0.057(6) -0.007(5) C37 0.089(7) 0.079(5) 0.077(6) -0.007(5) 0.060(6) 0.011(5) C38 0.071(6) 0.093(6) 0.095(7) -0.005(5) 0.063(6) 0.013(5) C39 0.058(5) 0.073(5) 0.086(6) -0.002(4) 0.053(5) 0.006(4) Cl40 0.138(2) 0.1028(17) 0.119(2) -0.0093(15) 0.0904(19) 0.0297(15) C41 0.055(5) 0.097(6) 0.096(7) -0.009(5) 0.051(5) 0.000(5) O42 0.057(3) 0.089(4) 0.103(4) -0.022(3) 0.054(3) -0.009(3) O101 0.167(8) 0.202(10) 0.193(9) -0.071(8) 0.098(8) -0.046(7) _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 N12 2.022(7) . ? Ni1 O33 2.032(5) . ? Ni1 O42 2.077(5) . ? Ni1 O30 2.081(4) 2 ? Ni1 N21 2.112(6) . ? Ni1 S2 2.572(2) . ? S2 P3 1.956(3) . ? P3 O8 1.543(5) . ? P3 O4 1.562(6) . ? P3 N12 1.645(6) . ? O4 C5 1.432(11) . ? C5 C6 1.413(19) . ? C5 C7 1.48(2) . ? C5 H5 0.9800 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? O8 C9 1.467(11) . ? C9 C10 1.373(14) . ? C9 C11 1.451(13) . ? C9 H9 0.9800 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? N12 C13 1.345(10) . ? C13 N15 1.366(10) . ? C13 S14 1.679(9) . ? N15 C16 1.380(10) . ? N15 H15 0.8600 . ? C16 N21 1.331(9) . ? C16 C17 1.419(10) . ? C17 C18 1.353(12) . ? C17 H17 0.9300 . ? C18 C19 1.352(12) . ? C18 H18 0.9300 . ? C19 C20 1.377(10) . ? C19 H19 0.9300 . ? C20 N21 1.357(10) . ? C20 N22 1.405(9) . ? N22 C23 1.304(8) . ? N22 Ni32 2.071(5) . ? C23 C24 1.400(10) . ? C23 H23 0.9300 . ? C24 C29 1.428(10) . ? C24 C25 1.430(9) . ? C25 C26 1.341(10) . ? C25 H25 0.9300 . ? C26 C27 1.393(11) . ? C26 Cl31 1.743(7) . ? C27 C28 1.364(10) . ? C27 H27 0.9300 . ? C28 C29 1.406(10) . ? C28 H28 0.9300 . ? C29 O30 1.310(8) . ? O30 Ni32 2.012(5) . ? O30 Ni1 2.081(4) 2 ? Ni32 O30 2.012(5) 2 ? Ni32 O33 2.058(4) . ? Ni32 O33 2.058(4) 2 ? Ni32 N22 2.071(5) 2 ? O33 C34 1.312(8) . ? C34 C35 1.401(10) . ? C34 C39 1.414(9) . ? C35 C36 1.376(10) . ? C35 H35 0.9300 . ? C36 C37 1.381(10) . ? C36 H36 0.9300 . ? C37 C38 1.348(11) . ? C37 Cl40 1.755(8) . ? C38 C39 1.413(10) . ? C38 H38 0.9300 . ? C39 C41 1.421(10) . ? C41 O42 1.253(9) . ? C41 H41 0.9300 . ? O101 H10D 0.8424 . ? O101 H10E 0.8425 . ? 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 N12 Ni1 O33 162.0(2) . . ? N12 Ni1 O42 92.0(2) . . ? O33 Ni1 O42 85.3(2) . . ? N12 Ni1 O30 108.3(2) . 2 ? O33 Ni1 O30 77.24(18) . 2 ? O42 Ni1 O30 158.7(2) . 2 ? N12 Ni1 N21 89.9(3) . . ? O33 Ni1 N21 107.9(2) . . ? O42 Ni1 N21 91.6(2) . . ? O30 Ni1 N21 82.40(19) 2 . ? N12 Ni1 S2 74.89(18) . . ? O33 Ni1 S2 87.40(15) . . ? O42 Ni1 S2 91.45(16) . . ? O30 Ni1 S2 99.72(13) 2 . ? N21 Ni1 S2 164.6(2) . . ? P3 S2 Ni1 78.15(10) . . ? O8 P3 O4 102.3(3) . . ? O8 P3 N12 109.3(3) . . ? O4 P3 N12 113.7(3) . . ? O8 P3 S2 114.3(2) . . ? O4 P3 S2 114.4(3) . . ? N12 P3 S2 103.1(3) . . ? C5 O4 P3 124.9(6) . . ? C6 C5 O4 108.8(13) . . ? C6 C5 C7 113.7(13) . . ? O4 C5 C7 106.8(13) . . ? C6 C5 H5 109.1 . . ? O4 C5 H5 109.1 . . ? C7 C5 H5 109.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 O8 P3 123.2(6) . . ? C10 C9 C11 118.7(12) . . ? C10 C9 O8 111.2(10) . . ? C11 C9 O8 109.6(8) . . ? C10 C9 H9 105.4 . . ? C11 C9 H9 105.4 . . ? O8 C9 H9 105.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 N12 P3 125.6(6) . . ? C13 N12 Ni1 130.5(6) . . ? P3 N12 Ni1 103.8(3) . . ? N12 C13 N15 117.0(8) . . ? N12 C13 S14 126.1(7) . . ? N15 C13 S14 116.9(7) . . ? C13 N15 C16 136.0(7) . . ? C13 N15 H15 112.0 . . ? C16 N15 H15 112.0 . . ? N21 C16 N15 122.8(7) . . ? N21 C16 C17 122.1(9) . . ? N15 C16 C17 115.1(8) . . ? C18 C17 C16 118.4(8) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C17 C18 C19 120.7(8) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 118.3(9) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N21 C20 C19 123.6(8) . . ? N21 C20 N22 116.9(7) . . ? C19 C20 N22 119.5(9) . . ? C16 N21 C20 116.9(7) . . ? C16 N21 Ni1 123.2(6) . . ? C20 N21 Ni1 119.7(5) . . ? C23 N22 C20 116.2(6) . . ? C23 N22 Ni32 122.2(5) . . ? C20 N22 Ni32 121.6(5) . . ? N22 C23 C24 129.6(7) . . ? N22 C23 H23 115.2 . . ? C24 C23 H23 115.2 . . ? C23 C24 C29 124.4(6) . . ? C23 C24 C25 116.7(7) . . ? C29 C24 C25 118.7(7) . . ? C26 C25 C24 121.4(7) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 120.7(7) . . ? C25 C26 Cl31 120.5(6) . . ? C27 C26 Cl31 118.8(7) . . ? C28 C27 C26 119.1(8) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 123.5(7) . . ? C27 C28 H28 118.2 . . ? C29 C28 H28 118.2 . . ? O30 C29 C28 121.2(7) . . ? O30 C29 C24 122.4(7) . . ? C28 C29 C24 116.4(7) . . ? C29 O30 Ni32 128.8(5) . . ? C29 O30 Ni1 133.2(5) . 2 ? Ni32 O30 Ni1 96.53(18) . 2 ? O30 Ni32 O30 171.9(2) 2 . ? O30 Ni32 O33 78.22(18) 2 . ? O30 Ni32 O33 96.84(18) . . ? O30 Ni32 O33 96.84(18) 2 2 ? O30 Ni32 O33 78.22(18) . 2 ? O33 Ni32 O33 105.4(3) . 2 ? O30 Ni32 N22 95.6(2) 2 . ? O30 Ni32 N22 89.8(2) . . ? O33 Ni32 N22 81.0(2) . . ? O33 Ni32 N22 166.9(2) 2 . ? O30 Ni32 N22 89.8(2) 2 2 ? O30 Ni32 N22 95.6(2) . 2 ? O33 Ni32 N22 166.9(2) . 2 ? O33 Ni32 N22 81.0(2) 2 2 ? N22 Ni32 N22 95.1(3) . 2 ? C34 O33 Ni1 123.3(4) . . ? C34 O33 Ni32 139.5(4) . . ? Ni1 O33 Ni32 96.64(19) . . ? O33 C34 C35 120.1(6) . . ? O33 C34 C39 121.2(7) . . ? C35 C34 C39 118.6(6) . . ? C36 C35 C34 121.1(7) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 119.3(8) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 121.7(7) . . ? C38 C37 Cl40 119.3(7) . . ? C36 C37 Cl40 118.9(7) . . ? C37 C38 C39 120.5(7) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C34 C39 C38 118.6(7) . . ? C34 C39 C41 123.1(7) . . ? C38 C39 C41 118.3(7) . . ? O42 C41 C39 128.1(7) . . ? O42 C41 H41 115.9 . . ? C39 C41 H41 115.9 . . ? C41 O42 Ni1 121.8(5) . . ? H10D O101 H10E 104.0 . . ? 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 N12 Ni1 S2 P3 -1.83(18) . . . . ? O33 Ni1 S2 P3 175.11(14) . . . . ? O42 Ni1 S2 P3 89.88(18) . . . . ? O30 Ni1 S2 P3 -108.31(16) 2 . . . ? N21 Ni1 S2 P3 -11.6(6) . . . . ? Ni1 S2 P3 O8 120.8(3) . . . . ? Ni1 S2 P3 O4 -121.7(3) . . . . ? Ni1 S2 P3 N12 2.2(2) . . . . ? O8 P3 O4 C5 -175.0(10) . . . . ? N12 P3 O4 C5 -57.2(11) . . . . ? S2 P3 O4 C5 60.9(10) . . . . ? P3 O4 C5 C6 -103.9(12) . . . . ? P3 O4 C5 C7 132.9(9) . . . . ? O4 P3 O8 C9 -82.6(7) . . . . ? N12 P3 O8 C9 156.6(7) . . . . ? S2 P3 O8 C9 41.6(7) . . . . ? P3 O8 C9 C10 92.9(13) . . . . ? P3 O8 C9 C11 -133.8(8) . . . . ? O8 P3 N12 C13 58.5(7) . . . . ? O4 P3 N12 C13 -55.1(7) . . . . ? S2 P3 N12 C13 -179.5(6) . . . . ? O8 P3 N12 Ni1 -124.9(3) . . . . ? O4 P3 N12 Ni1 121.6(3) . . . . ? S2 P3 N12 Ni1 -2.9(3) . . . . ? O33 Ni1 N12 C13 168.6(6) . . . . ? O42 Ni1 N12 C13 87.6(7) . . . . ? O30 Ni1 N12 C13 -86.0(7) 2 . . . ? N21 Ni1 N12 C13 -4.0(7) . . . . ? S2 Ni1 N12 C13 178.6(7) . . . . ? O33 Ni1 N12 P3 -7.8(8) . . . . ? O42 Ni1 N12 P3 -88.8(3) . . . . ? O30 Ni1 N12 P3 97.6(3) 2 . . . ? N21 Ni1 N12 P3 179.6(3) . . . . ? S2 Ni1 N12 P3 2.2(2) . . . . ? P3 N12 C13 N15 178.0(5) . . . . ? Ni1 N12 C13 N15 2.3(11) . . . . ? P3 N12 C13 S14 -1.0(11) . . . . ? Ni1 N12 C13 S14 -176.7(4) . . . . ? N12 C13 N15 C16 5.9(14) . . . . ? S14 C13 N15 C16 -175.0(7) . . . . ? C13 N15 C16 N21 -10.4(13) . . . . ? C13 N15 C16 C17 171.0(9) . . . . ? N21 C16 C17 C18 1.9(11) . . . . ? N15 C16 C17 C18 -179.5(7) . . . . ? C16 C17 C18 C19 -0.3(13) . . . . ? C17 C18 C19 C20 -1.5(13) . . . . ? C18 C19 C20 N21 1.8(11) . . . . ? C18 C19 C20 N22 -179.9(7) . . . . ? N15 C16 N21 C20 179.9(6) . . . . ? C17 C16 N21 C20 -1.6(9) . . . . ? N15 C16 N21 Ni1 5.7(9) . . . . ? C17 C16 N21 Ni1 -175.8(5) . . . . ? C19 C20 N21 C16 -0.3(10) . . . . ? N22 C20 N21 C16 -178.6(5) . . . . ? C19 C20 N21 Ni1 174.1(5) . . . . ? N22 C20 N21 Ni1 -4.1(7) . . . . ? N12 Ni1 N21 C16 -0.1(5) . . . . ? O33 Ni1 N21 C16 -177.7(5) . . . . ? O42 Ni1 N21 C16 -92.1(5) . . . . ? O30 Ni1 N21 C16 108.4(5) 2 . . . ? S2 Ni1 N21 C16 9.4(9) . . . . ? N12 Ni1 N21 C20 -174.2(5) . . . . ? O33 Ni1 N21 C20 8.2(5) . . . . ? O42 Ni1 N21 C20 93.8(5) . . . . ? O30 Ni1 N21 C20 -65.7(5) 2 . . . ? S2 Ni1 N21 C20 -164.7(4) . . . . ? N21 C20 N22 C23 -125.4(7) . . . . ? C19 C20 N22 C23 56.3(9) . . . . ? N21 C20 N22 Ni32 54.9(7) . . . . ? C19 C20 N22 Ni32 -123.5(6) . . . . ? C20 N22 C23 C24 -177.3(7) . . . . ? Ni32 N22 C23 C24 2.5(11) . . . . ? N22 C23 C24 C29 10.1(13) . . . . ? N22 C23 C24 C25 -174.2(7) . . . . ? C23 C24 C25 C26 -176.1(7) . . . . ? C29 C24 C25 C26 -0.2(11) . . . . ? C24 C25 C26 C27 2.5(12) . . . . ? C24 C25 C26 Cl31 -177.2(6) . . . . ? C25 C26 C27 C28 -2.7(13) . . . . ? Cl31 C26 C27 C28 177.0(6) . . . . ? C26 C27 C28 C29 0.7(13) . . . . ? C27 C28 C29 O30 -179.4(7) . . . . ? C27 C28 C29 C24 1.4(11) . . . . ? C23 C24 C29 O30 -5.2(11) . . . . ? C25 C24 C29 O30 179.2(6) . . . . ? C23 C24 C29 C28 173.9(7) . . . . ? C25 C24 C29 C28 -1.7(10) . . . . ? C28 C29 O30 Ni32 169.0(5) . . . . ? C24 C29 O30 Ni32 -11.9(9) . . . . ? C28 C29 O30 Ni1 -28.2(9) . . . 2 ? C24 C29 O30 Ni1 150.9(6) . . . 2 ? C29 O30 Ni32 O33 -63.1(5) . . . . ? Ni1 O30 Ni32 O33 129.44(17) 2 . . . ? C29 O30 Ni32 O33 -167.5(5) . . . 2 ? Ni1 O30 Ni32 O33 25.04(17) 2 . . 2 ? C29 O30 Ni32 N22 17.8(5) . . . . ? Ni1 O30 Ni32 N22 -149.7(2) 2 . . . ? C29 O30 Ni32 N22 113.0(5) . . . 2 ? Ni1 O30 Ni32 N22 -54.5(2) 2 . . 2 ? C23 N22 Ni32 O30 161.4(5) . . . 2 ? C20 N22 Ni32 O30 -18.8(6) . . . 2 ? C23 N22 Ni32 O30 -12.6(6) . . . . ? C20 N22 Ni32 O30 167.1(6) . . . . ? C23 N22 Ni32 O33 84.3(6) . . . . ? C20 N22 Ni32 O33 -95.9(6) . . . . ? C23 N22 Ni32 O33 -36.2(12) . . . 2 ? C20 N22 Ni32 O33 143.6(8) . . . 2 ? C23 N22 Ni32 N22 -108.3(6) . . . 2 ? C20 N22 Ni32 N22 71.5(5) . . . 2 ? N12 Ni1 O33 C34 -38.0(9) . . . . ? O42 Ni1 O33 C34 44.0(5) . . . . ? O30 Ni1 O33 C34 -148.2(5) 2 . . . ? N21 Ni1 O33 C34 134.3(5) . . . . ? S2 Ni1 O33 C34 -47.6(5) . . . . ? N12 Ni1 O33 Ni32 135.1(6) . . . . ? O42 Ni1 O33 Ni32 -142.9(2) . . . . ? O30 Ni1 O33 Ni32 24.88(17) 2 . . . ? N21 Ni1 O33 Ni32 -52.7(2) . . . . ? S2 Ni1 O33 Ni32 125.46(15) . . . . ? O30 Ni32 O33 C34 145.4(7) 2 . . . ? O30 Ni32 O33 C34 -28.2(7) . . . . ? O33 Ni32 O33 C34 51.5(6) 2 . . . ? N22 Ni32 O33 C34 -116.9(7) . . . . ? N22 Ni32 O33 C34 169.5(8) 2 . . . ? O30 Ni32 O33 Ni1 -25.69(18) 2 . . . ? O30 Ni32 O33 Ni1 160.75(18) . . . . ? O33 Ni32 O33 Ni1 -119.6(2) 2 . . . ? N22 Ni32 O33 Ni1 72.1(2) . . . . ? N22 Ni32 O33 Ni1 -1.6(10) 2 . . . ? Ni1 O33 C34 C35 146.4(5) . . . . ? Ni32 O33 C34 C35 -23.0(10) . . . . ? Ni1 O33 C34 C39 -34.0(8) . . . . ? Ni32 O33 C34 C39 156.6(5) . . . . ? O33 C34 C35 C36 -177.1(7) . . . . ? C39 C34 C35 C36 3.4(11) . . . . ? C34 C35 C36 C37 -1.3(12) . . . . ? C35 C36 C37 C38 -2.3(13) . . . . ? C35 C36 C37 Cl40 -178.3(6) . . . . ? C36 C37 C38 C39 3.7(13) . . . . ? Cl40 C37 C38 C39 179.7(6) . . . . ? O33 C34 C39 C38 178.5(6) . . . . ? C35 C34 C39 C38 -1.9(11) . . . . ? O33 C34 C39 C41 -2.0(11) . . . . ? C35 C34 C39 C41 177.6(7) . . . . ? C37 C38 C39 C34 -1.5(12) . . . . ? C37 C38 C39 C41 178.9(8) . . . . ? C34 C39 C41 O42 12.7(13) . . . . ? C38 C39 C41 O42 -167.8(8) . . . . ? C39 C41 O42 Ni1 13.8(12) . . . . ? N12 Ni1 O42 C41 128.9(6) . . . . ? O33 Ni1 O42 C41 -33.3(6) . . . . ? O30 Ni1 O42 C41 -68.0(9) 2 . . . ? N21 Ni1 O42 C41 -141.1(6) . . . . ? S2 Ni1 O42 C41 54.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 21.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.442 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 905821' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_safin144 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H52 Br4 N8 Ni3 O10 P2 S4' _chemical_formula_sum 'C52 H52 Br4 N8 Ni3 O10 P2 S4' _chemical_formula_weight 1634.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.853(19) _cell_length_b 10.6228(11) _cell_length_c 23.605(13) _cell_angle_alpha 90.00 _cell_angle_beta 130.11(9) _cell_angle_gamma 90.00 _cell_volume 6493(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 1259 _cell_measurement_theta_min 3.0349 _cell_measurement_theta_max 17.5207 _exptl_crystal_description plate _exptl_crystal_colour 'yellow translucent' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 3.559 _exptl_absorpt_correction_T_min 0.34844 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _iucr_refine_instructions_details ; TITL SAFIN144 in C2/c CELL 0.71073 33.852955 10.622819 23.605335 90.0000 130.1074 90.0000 ZERR 4.00 0.018805 0.001115 0.013261 0.0000 0.0917 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O P S Br Ni UNIT 208 208 32 40 8 16 16 12 L.S. 50 ACTA BOND $H FMAP 2 PLAN 20 SHEL 999 1.33 DFIX 1.334 0.02 N21 C20 N21 C16 DFIX 1.373 0.02 C16 C17 C19 C20 DFIX 1.374 0.02 C17 C18 C18 C19 HTAB CONF DFIX 1.441 0.01 O4 C5 O8 C9 DFIX 1.487 0.01 C5 C6 C5 C7 C9 C10 C9 C11 DFIX 2.482 0.01 C6 C7 C10 C11 FLAT 0.02 C23 > Br31 FLAT 0.02 C33 > Br41 FLAT 0.02 N15 > N22 TEMP -113 DELU DAMP 800 ISOR 0.05 $C $N ISOR 0.03 C29 C37 C39 C34 REM WGHT 0.090100 158.395325 REM WGHT 0.097000 168.901993 WGHT 0.086400 122.199295 FVAR 5.47337 NI1 8 0.105508 0.782874 0.401314 11.00000 0.13949 0.06976 = 0.15488 0.01181 0.13095 0.00263 S2 6 0.110343 1.011547 0.441154 11.00000 0.15292 0.07275 = 0.14672 0.00569 0.12675 -0.00436 P3 5 0.156145 0.925466 0.536218 11.00000 0.14235 0.08026 = 0.15172 0.00847 0.12816 -0.00476 O4 4 0.139904 0.932647 0.584779 11.00000 0.14164 0.08119 = 0.14069 0.01406 0.12112 0.01278 C5 1 0.124812 1.052858 0.594058 11.00000 0.15551 0.10285 = 0.16632 -0.01632 0.12763 0.00513 AFIX 13 H5 2 0.120807 1.115053 0.558862 11.00000 -1.20000 AFIX 0 C6 1 0.074198 1.036001 0.576326 11.00000 0.14983 0.12379 = 0.18985 0.04132 0.13149 0.05524 AFIX 137 H6A 2 0.078894 0.983569 0.614433 11.00000 -1.50000 H6B 2 0.049836 0.994942 0.527970 11.00000 -1.50000 H6C 2 0.060566 1.118401 0.574909 11.00000 -1.50000 AFIX 0 C7 1 0.166470 1.095668 0.671224 11.00000 0.20906 0.18960 = 0.18970 -0.06863 0.16181 -0.05744 AFIX 137 H7A 2 0.157733 1.178855 0.678328 11.00000 -1.50000 H7B 2 0.199097 1.100767 0.680448 11.00000 -1.50000 H7C 2 0.170081 1.035643 0.705837 11.00000 -1.50000 AFIX 0 O8 4 0.215057 0.976735 0.591674 11.00000 0.14142 0.09013 = 0.14794 -0.01808 0.12279 -0.00864 C9 1 0.247848 0.972010 0.572224 11.00000 0.13830 0.14174 = 0.17376 -0.01345 0.13112 -0.01526 AFIX 13 H9 2 0.235645 0.905344 0.534202 11.00000 -1.20000 AFIX 0 C10 1 0.297752 0.935682 0.644098 11.00000 0.12962 0.14131 = 0.24090 -0.00210 0.11694 0.00117 AFIX 137 H10A 2 0.324229 0.997414 0.658149 11.00000 -1.50000 H10B 2 0.307917 0.852303 0.639655 11.00000 -1.50000 H10C 2 0.294169 0.933263 0.682102 11.00000 -1.50000 AFIX 0 C11 1 0.248953 1.096142 0.544817 11.00000 0.18315 0.21218 = 0.28268 0.06528 0.18684 -0.00279 AFIX 137 H11A 2 0.259144 1.161010 0.581554 11.00000 -1.50000 H11B 2 0.214551 1.115581 0.498096 11.00000 -1.50000 H11C 2 0.273897 1.094039 0.536652 11.00000 -1.50000 AFIX 0 N12 3 0.151950 0.773773 0.515761 11.00000 0.13732 0.07389 = 0.14889 0.00992 0.13214 -0.00126 C13 1 0.175499 0.674400 0.555357 11.00000 0.12858 0.09107 = 0.16225 0.02142 0.10497 0.00702 S14 6 0.220773 0.689106 0.652572 11.00000 0.16377 0.11398 = 0.16514 0.02353 0.10932 0.02940 N15 3 0.169978 0.559187 0.530580 11.00000 0.07567 0.07686 = 0.14547 0.03835 0.07498 0.00547 AFIX 43 H15 2 0.189667 0.502122 0.565016 11.00000 -1.20000 AFIX 0 C16 1 0.137358 0.513325 0.457347 11.00000 0.10227 0.08630 = 0.14978 0.02777 0.09853 0.00869 C17 1 0.138274 0.382964 0.456925 11.00000 0.12254 0.08756 = 0.15435 0.02955 0.10772 -0.00827 AFIX 43 H17 2 0.158746 0.335579 0.501543 11.00000 -1.20000 AFIX 0 C18 1 0.107865 0.325292 0.388229 11.00000 0.11118 0.10506 = 0.16417 0.00926 0.11164 0.01119 AFIX 43 H18 2 0.107589 0.236059 0.385317 11.00000 -1.20000 AFIX 0 C19 1 0.078170 0.394712 0.324388 11.00000 0.13148 0.09147 = 0.15155 -0.00643 0.11880 0.01251 AFIX 43 H19 2 0.056606 0.357122 0.276643 11.00000 -1.20000 AFIX 0 C20 1 0.081912 0.523189 0.334591 11.00000 0.10892 0.09312 = 0.14302 -0.00596 0.11708 0.00813 N21 3 0.109927 0.588182 0.398389 11.00000 0.11810 0.08062 = 0.13284 0.00997 0.11162 0.01676 N22 3 0.053354 0.598331 0.272011 11.00000 0.10665 0.08655 = 0.13158 -0.01193 0.10511 -0.00651 C23 1 0.061371 0.586828 0.224526 11.00000 0.07496 0.09392 = 0.09500 -0.02917 0.06514 -0.01489 AFIX 43 H23 2 0.090524 0.536201 0.242625 11.00000 -1.20000 AFIX 66 C24 1 0.035687 0.634040 0.151990 11.00000 0.08656 0.13339 = 0.11122 -0.01066 0.08481 -0.01093 C25 1 0.057632 0.603811 0.120275 11.00000 0.15774 0.06317 = 0.16773 0.02799 0.14975 0.00772 AFIX 43 H25 2 0.088213 0.554502 0.147075 11.00000 -1.20000 AFIX 65 C26 1 0.034833 0.645728 0.049349 11.00000 0.12724 0.06201 = 0.12558 -0.01339 0.11017 -0.02009 C27 1 -0.009912 0.717874 0.010137 11.00000 0.12808 0.09769 = 0.10627 -0.02743 0.09424 -0.00517 AFIX 43 H27 2 -0.025494 0.746521 -0.038338 11.00000 -1.20000 AFIX 65 C28 1 -0.031858 0.748104 0.041851 11.00000 0.10307 0.09194 = 0.10907 -0.01081 0.08804 -0.02494 AFIX 43 H28 2 -0.062439 0.797414 0.015051 11.00000 -1.20000 AFIX 65 C29 1 -0.009059 0.706188 0.112777 11.00000 0.07874 0.08388 = 0.11286 -0.00051 0.08400 -0.03192 AFIX 0 O30 4 -0.029711 0.737587 0.144307 11.00000 0.12384 0.06902 = 0.15152 0.00323 0.12624 -0.01390 BR31 7 0.062309 0.611819 0.002365 11.00000 0.18946 0.09380 = 0.18650 -0.01431 0.17298 -0.00458 O32 4 0.169652 0.811975 0.409003 11.00000 0.13507 0.10214 = 0.14637 0.03527 0.12606 0.01961 C33 1 0.168206 0.895652 0.371424 11.00000 0.11520 0.09540 = 0.10569 0.00655 0.09676 -0.00183 AFIX 43 H33 2 0.201192 0.913245 0.386155 11.00000 -1.20000 AFIX 66 C34 1 0.129465 0.969836 0.312643 11.00000 0.11057 0.11405 = 0.09464 0.01404 0.08981 -0.00843 C35 1 0.077824 0.943304 0.275723 11.00000 0.11108 0.06762 = 0.09962 -0.01194 0.08871 -0.00802 C36 1 0.039371 1.018597 0.216952 11.00000 0.11033 0.09496 = 0.10683 0.00513 0.09918 0.00742 AFIX 43 H36 2 0.004077 1.000464 0.191720 11.00000 -1.20000 AFIX 65 C37 1 0.052558 1.120423 0.195100 11.00000 0.12628 0.09189 = 0.08571 0.00366 0.09725 0.01033 AFIX 43 H37 2 0.026276 1.171883 0.154932 11.00000 -1.20000 AFIX 65 C38 1 0.104198 1.146956 0.232018 11.00000 0.13683 0.07559 = 0.11852 0.00628 0.10195 -0.01141 C39 1 0.142652 1.071664 0.290790 11.00000 0.12294 0.10507 = 0.09405 0.00435 0.09410 -0.01277 AFIX 43 H39 2 0.177945 1.089798 0.316022 11.00000 -1.20000 AFIX 0 O40 4 0.063963 0.848706 0.294941 11.00000 0.13013 0.07914 = 0.14209 0.00329 0.12366 -0.00103 BR41 7 0.123466 1.282036 0.203754 11.00000 0.21046 0.08688 = 0.18054 0.00772 0.16702 -0.01912 NI42 8 0.000000 0.731489 0.250000 10.50000 0.13825 0.06860 = 0.15125 0.00000 0.13199 0.00000 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 REM SAFIN144 in C2/c REM R1 = 0.0713 for 1000 Fo > 4sig(Fo) and 0.1019 for all 1429 data REM 355 parameters refined using 365 restraints END WGHT 0.0852 118.1927 REM Highest difference peak 0.426, deepest hole -0.444, 1-sigma level 0.085 Q1 1 0.0503 0.7585 -0.0193 11.00000 0.05 0.43 ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku UltraX 18 rotating anode' _diffrn_radiation_monochromator 'Zr filter' _diffrn_measurement_device_type 'MAR345 image plate' _diffrn_measurement_method '80 images, \D\F 2.5\% ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5550 _diffrn_reflns_av_R_equivalents 0.0958 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 15.50 _reflns_number_total 1429 _reflns_number_gt 1000 _reflns_threshold_expression >2sigma(I) _computing_data_collection MAR _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0864P)^2^+122.1993P] 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_number_reflns 1429 _refine_ls_number_parameters 355 _refine_ls_number_restraints 365 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.1808 _refine_ls_wR_factor_gt 0.1637 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.000 _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 0.10551(7) 0.7829(2) 0.40131(11) 0.0948(8) Uani 1 1 d U . . S2 S 0.11034(15) 1.0115(4) 0.4412(2) 0.1019(15) Uani 1 1 d U . . P3 P 0.15615(16) 0.9255(5) 0.5362(3) 0.1002(15) Uani 1 1 d U . . O4 O 0.1399(3) 0.9326(7) 0.5848(5) 0.099(3) Uani 1 1 d DU . . C5 C 0.1248(2) 1.0529(10) 0.5941(5) 0.124(5) Uani 1 1 d DU . . H5 H 0.1208 1.1151 0.5589 0.149 Uiso 1 1 calc R . . C6 C 0.0742(3) 1.0360(15) 0.5763(7) 0.138(7) Uani 1 1 d DU . . H6A H 0.0789 0.9836 0.6144 0.207 Uiso 1 1 calc R . . H6B H 0.0498 0.9949 0.5280 0.207 Uiso 1 1 calc R . . H6C H 0.0606 1.1184 0.5749 0.207 Uiso 1 1 calc R . . C7 C 0.1665(4) 1.0957(17) 0.6712(6) 0.172(7) Uani 1 1 d DU . . H7A H 0.1577 1.1789 0.6783 0.257 Uiso 1 1 calc R . . H7B H 0.1991 1.1008 0.6804 0.257 Uiso 1 1 calc R . . H7C H 0.1701 1.0356 0.7058 0.257 Uiso 1 1 calc R . . O8 O 0.2151(2) 0.9767(10) 0.5917(4) 0.105(3) Uani 1 1 d DU . . C9 C 0.2478(3) 0.9720(9) 0.5722(5) 0.129(5) Uani 1 1 d DU . . H9 H 0.2356 0.9053 0.5342 0.155 Uiso 1 1 calc R . . C10 C 0.2978(5) 0.9357(11) 0.6441(6) 0.172(8) Uani 1 1 d DU . . H10A H 0.3242 0.9974 0.6581 0.259 Uiso 1 1 calc R . . H10B H 0.3079 0.8523 0.6397 0.259 Uiso 1 1 calc R . . H10C H 0.2942 0.9333 0.6821 0.259 Uiso 1 1 calc R . . C11 C 0.2490(5) 1.0961(10) 0.5448(7) 0.199(7) Uani 1 1 d DU . . H11A H 0.2591 1.1610 0.5816 0.298 Uiso 1 1 calc R . . H11B H 0.2146 1.1156 0.4981 0.298 Uiso 1 1 calc R . . H11C H 0.2739 1.0940 0.5367 0.298 Uiso 1 1 calc R . . N12 N 0.1519(4) 0.7738(12) 0.5158(6) 0.091(3) Uani 1 1 d U . . C13 C 0.1755(6) 0.6744(18) 0.5554(10) 0.119(6) Uani 1 1 d U . . S14 S 0.2208(2) 0.6891(5) 0.6526(3) 0.145(2) Uani 1 1 d U . . N15 N 0.16998(9) 0.5592(12) 0.5306(3) 0.097(4) Uani 1 1 d DU . . H15 H 0.1897 0.5021 0.5650 0.116 Uiso 1 1 calc R . . C16 C 0.13736(8) 0.5133(11) 0.4573(2) 0.100(5) Uani 1 1 d DU . . C17 C 0.13827(18) 0.3830(12) 0.4569(4) 0.108(5) Uani 1 1 d DU . . H17 H 0.1587 0.3356 0.5015 0.129 Uiso 1 1 calc R . . C18 C 0.1079(3) 0.3253(14) 0.3882(5) 0.110(5) Uani 1 1 d DU . . H18 H 0.1076 0.2361 0.3853 0.132 Uiso 1 1 calc R . . C19 C 0.0782(3) 0.3947(11) 0.3244(6) 0.105(5) Uani 1 1 d DU . . H19 H 0.0566 0.3571 0.2766 0.125 Uiso 1 1 calc R . . C20 C 0.0819(3) 0.5232(12) 0.3346(5) 0.089(4) Uani 1 1 d DU . . N21 N 0.1099(2) 0.5882(10) 0.3984(5) 0.088(3) Uani 1 1 d DU . . N22 N 0.0534(3) 0.5983(12) 0.2720(6) 0.087(3) Uani 1 1 d DU . . C23 C 0.0614(2) 0.5868(5) 0.2245(6) 0.080(4) Uani 1 1 d DU . . H23 H 0.0905 0.5362 0.2426 0.096 Uiso 1 1 calc R . . C24 C 0.0357(2) 0.6340(4) 0.1520(4) 0.095(4) Uani 1 1 d GDU . . C25 C 0.0576(2) 0.6038(5) 0.1203(5) 0.097(4) Uani 1 1 d GDU . . H25 H 0.0882 0.5545 0.1471 0.116 Uiso 1 1 calc R . . C26 C 0.0348(3) 0.6457(6) 0.0493(5) 0.084(4) Uani 1 1 d GDU . . C27 C -0.0099(3) 0.7179(7) 0.0101(4) 0.097(5) Uani 1 1 d GDU . . H27 H -0.0255 0.7465 -0.0383 0.116 Uiso 1 1 calc R . . C28 C -0.0319(3) 0.7481(6) 0.0419(4) 0.087(4) Uani 1 1 d GDU . . H28 H -0.0624 0.7974 0.0151 0.104 Uiso 1 1 calc R . . C29 C -0.0091(2) 0.7062(5) 0.1128(4) 0.075(4) Uani 1 1 d GDU . . O30 O -0.0297(3) 0.7376(7) 0.1443(5) 0.087(3) Uani 1 1 d DU . . Br31 Br 0.06231(6) 0.61182(19) 0.00236(9) 0.1185(7) Uani 1 1 d DU . . O32 O 0.1697(3) 0.8120(10) 0.4090(5) 0.102(3) Uani 1 1 d U . . C33 C 0.16821(16) 0.8957(6) 0.3714(3) 0.087(4) Uani 1 1 d DU . . H33 H 0.2012 0.9132 0.3862 0.104 Uiso 1 1 calc R . . C34 C 0.1295(2) 0.9698(6) 0.3126(2) 0.089(4) Uani 1 1 d GDU . . C35 C 0.0778(2) 0.9433(7) 0.2757(3) 0.077(4) Uani 1 1 d GDU . . C36 C 0.0394(2) 1.0186(9) 0.2170(4) 0.083(4) Uani 1 1 d GDU . . H36 H 0.0041 1.0005 0.1917 0.099 Uiso 1 1 calc R . . C37 C 0.0526(3) 1.1204(8) 0.1951(3) 0.080(4) Uani 1 1 d GDU . . H37 H 0.0263 1.1719 0.1549 0.096 Uiso 1 1 calc R . . C38 C 0.1042(4) 1.1470(6) 0.2320(4) 0.096(5) Uani 1 1 d GDU . . C39 C 0.1427(3) 1.0717(6) 0.2908(3) 0.090(4) Uani 1 1 d GDU . . H39 H 0.1779 1.0898 0.3160 0.108 Uiso 1 1 calc R . . O40 O 0.0640(3) 0.8487(8) 0.2949(4) 0.091(3) Uani 1 1 d DU . . Br41 Br 0.12347(7) 1.2820(2) 0.20375(10) 0.1291(8) Uani 1 1 d DU . . Ni42 Ni 0.0000 0.7315(3) 0.2500 0.0909(10) Uani 1 2 d SU . . 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 0.1395(11) 0.0698(16) 0.1549(12) 0.0118(11) 0.1309(9) 0.0026(13) S2 0.153(2) 0.073(3) 0.147(2) 0.006(2) 0.1267(19) -0.004(3) P3 0.142(2) 0.080(3) 0.152(2) 0.008(2) 0.1282(18) -0.005(3) O4 0.142(3) 0.081(6) 0.141(4) 0.014(4) 0.121(3) 0.013(5) C5 0.156(5) 0.103(10) 0.166(7) -0.016(7) 0.128(5) 0.005(7) C6 0.150(5) 0.124(15) 0.190(11) 0.041(10) 0.131(6) 0.055(8) C7 0.209(8) 0.190(14) 0.190(9) -0.069(8) 0.162(7) -0.057(11) O8 0.141(3) 0.090(7) 0.148(5) -0.018(5) 0.123(3) -0.009(5) C9 0.138(4) 0.142(10) 0.174(8) -0.013(8) 0.131(4) -0.015(9) C10 0.130(6) 0.141(14) 0.241(12) -0.002(9) 0.117(7) 0.001(11) C11 0.183(9) 0.212(13) 0.283(12) 0.065(9) 0.187(7) -0.003(11) N12 0.137(5) 0.074(4) 0.149(3) 0.010(3) 0.132(3) -0.001(5) C13 0.129(10) 0.091(5) 0.162(5) 0.021(5) 0.105(7) 0.007(9) S14 0.164(4) 0.114(5) 0.165(3) 0.024(3) 0.109(3) 0.029(4) N15 0.076(7) 0.077(5) 0.145(5) 0.038(5) 0.075(5) 0.005(7) C16 0.102(8) 0.086(5) 0.150(5) 0.028(4) 0.099(6) 0.009(9) C17 0.123(9) 0.088(5) 0.154(6) 0.030(5) 0.108(6) -0.008(9) C18 0.111(9) 0.105(7) 0.164(7) 0.009(5) 0.112(7) 0.011(9) C19 0.131(9) 0.091(5) 0.152(6) -0.006(5) 0.119(6) 0.013(9) C20 0.109(6) 0.093(5) 0.143(4) -0.006(4) 0.117(4) 0.008(6) N21 0.118(6) 0.081(4) 0.133(4) 0.010(3) 0.112(4) 0.017(5) N22 0.107(5) 0.087(5) 0.132(4) -0.012(5) 0.105(3) -0.007(5) C23 0.075(5) 0.094(11) 0.095(4) -0.029(5) 0.065(3) -0.015(6) C24 0.087(4) 0.133(13) 0.111(4) -0.011(6) 0.085(3) -0.011(6) C25 0.158(4) 0.063(11) 0.168(4) 0.028(6) 0.150(3) 0.008(6) C26 0.127(4) 0.062(11) 0.126(4) -0.013(6) 0.110(3) -0.020(6) C27 0.128(4) 0.098(12) 0.106(5) -0.027(7) 0.094(3) -0.005(6) C28 0.103(5) 0.092(12) 0.109(4) -0.011(6) 0.088(4) -0.025(7) C29 0.079(4) 0.084(10) 0.113(4) -0.001(6) 0.084(3) -0.032(5) O30 0.124(4) 0.069(7) 0.152(3) 0.003(5) 0.126(3) -0.014(5) Br31 0.1895(10) 0.0938(16) 0.1865(11) -0.0143(11) 0.1730(8) -0.0046(12) O32 0.135(3) 0.102(7) 0.146(4) 0.035(4) 0.126(3) 0.020(4) C33 0.115(5) 0.095(9) 0.106(7) 0.007(5) 0.097(4) -0.002(6) C34 0.111(4) 0.114(8) 0.095(6) 0.014(5) 0.090(4) -0.008(5) C35 0.111(4) 0.068(8) 0.100(6) -0.012(4) 0.089(4) -0.008(5) C36 0.110(5) 0.095(8) 0.107(7) 0.005(5) 0.099(4) 0.007(5) C37 0.126(4) 0.092(8) 0.086(6) 0.004(5) 0.097(4) 0.010(5) C38 0.137(5) 0.076(9) 0.119(8) 0.006(5) 0.102(5) -0.011(6) C39 0.123(5) 0.105(8) 0.094(7) 0.004(5) 0.094(5) -0.013(5) O40 0.130(4) 0.079(5) 0.142(3) 0.003(3) 0.124(3) -0.001(4) Br41 0.2105(12) 0.0869(16) 0.1805(12) 0.0077(11) 0.1670(10) -0.0191(13) Ni42 0.1382(15) 0.069(2) 0.1513(16) 0.000 0.1320(12) 0.000 _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 O40 2.055(9) . ? Ni1 N12 2.075(11) . ? Ni1 N21 2.078(11) . ? Ni1 O32 2.082(10) . ? Ni1 O30 2.101(9) 2 ? Ni1 S2 2.572(5) . ? S2 P3 1.948(6) . ? P3 O4 1.560(11) . ? P3 O8 1.620(8) . ? P3 N12 1.662(13) . ? O4 C5 1.444(8) . ? C5 C7 1.485(9) . ? C5 C6 1.490(9) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O8 C9 1.450(9) . ? C9 C10 1.479(8) . ? C9 C11 1.480(9) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N12 C13 1.290(19) . ? C13 N15 1.32(2) . ? C13 S14 1.763(18) . ? N15 C16 1.409(8) . ? N15 H15 0.8800 . ? C16 N21 1.329(10) . ? C16 C17 1.385(13) . ? C17 C18 1.383(12) . ? C17 H17 0.9500 . ? C18 C19 1.369(13) . ? C18 H18 0.9500 . ? C19 C20 1.377(13) . ? C19 H19 0.9500 . ? C20 N21 1.343(11) . ? C20 N22 1.383(15) . ? N22 C23 1.318(17) . ? N22 Ni42 2.079(11) . ? C23 C24 1.422(14) . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 C29 1.3900 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 C27 1.3900 . ? C26 Br31 1.885(8) . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.3900 . ? C28 H28 0.9500 . ? C29 O30 1.351(12) . ? O30 Ni42 2.002(9) . ? O30 Ni1 2.101(9) 2 ? O32 C33 1.234(12) . ? C33 C34 1.386(7) . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 O40 1.308(11) . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C36 H36 0.9500 . ? C37 C38 1.3900 . ? C37 H37 0.9500 . ? C38 C39 1.3900 . ? C38 Br41 1.868(8) . ? C39 H39 0.9500 . ? O40 Ni42 2.099(9) . ? Ni42 O30 2.002(9) 2 ? Ni42 N22 2.079(11) 2 ? Ni42 O40 2.099(9) 2 ? 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 O40 Ni1 N12 162.7(4) . . ? O40 Ni1 N21 107.8(4) . . ? N12 Ni1 N21 89.2(4) . . ? O40 Ni1 O32 84.9(4) . . ? N12 Ni1 O32 91.2(4) . . ? N21 Ni1 O32 93.3(4) . . ? O40 Ni1 O30 78.6(4) . 2 ? N12 Ni1 O30 107.9(4) . 2 ? N21 Ni1 O30 81.1(3) . 2 ? O32 Ni1 O30 159.9(4) . 2 ? O40 Ni1 S2 87.6(3) . . ? N12 Ni1 S2 75.6(4) . . ? N21 Ni1 S2 164.4(3) . . ? O32 Ni1 S2 90.6(3) . . ? O30 Ni1 S2 99.9(3) 2 . ? P3 S2 Ni1 78.1(2) . . ? O4 P3 O8 102.9(5) . . ? O4 P3 N12 104.9(6) . . ? O8 P3 N12 113.0(6) . . ? O4 P3 S2 115.3(4) . . ? O8 P3 S2 115.2(5) . . ? N12 P3 S2 105.4(5) . . ? C5 O4 P3 118.8(8) . . ? O4 C5 C7 107.9(9) . . ? O4 C5 C6 107.8(10) . . ? C7 C5 C6 113.1(8) . . ? O4 C5 H5 109.3 . . ? C7 C5 H5 109.3 . . ? C6 C5 H5 109.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 O8 P3 121.8(7) . . ? O8 C9 C10 100.8(10) . . ? O8 C9 C11 110.3(11) . . ? C10 C9 C11 113.7(7) . . ? O8 C9 H9 110.5 . . ? C10 C9 H9 110.5 . . ? C11 C9 H9 110.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 N12 P3 133.3(12) . . ? C13 N12 Ni1 125.3(12) . . ? P3 N12 Ni1 100.6(6) . . ? N12 C13 N15 126.5(16) . . ? N12 C13 S14 118.9(14) . . ? N15 C13 S14 114.6(12) . . ? C13 N15 C16 129.9(11) . . ? C13 N15 H15 115.1 . . ? C16 N15 H15 115.1 . . ? N21 C16 C17 126.5(7) . . ? N21 C16 N15 123.0(11) . . ? C17 C16 N15 110.5(8) . . ? C18 C17 C16 116.6(9) . . ? C18 C17 H17 121.7 . . ? C16 C17 H17 121.7 . . ? C19 C18 C17 121.1(13) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 114.9(11) . . ? C18 C19 H19 122.5 . . ? C20 C19 H19 122.5 . . ? N21 C20 C19 128.6(11) . . ? N21 C20 N22 113.8(11) . . ? C19 C20 N22 117.6(10) . . ? C16 N21 C20 112.3(10) . . ? C16 N21 Ni1 125.3(7) . . ? C20 N21 Ni1 122.3(8) . . ? C23 N22 C20 118.0(9) . . ? C23 N22 Ni42 118.2(8) . . ? C20 N22 Ni42 123.8(8) . . ? N22 C23 C24 133.7(8) . . ? N22 C23 H23 113.2 . . ? C24 C23 H23 113.2 . . ? C25 C24 C29 120.0 . . ? C25 C24 C23 116.3(6) . . ? C29 C24 C23 123.7(6) . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 Br31 123.1(5) . . ? C27 C26 Br31 116.9(5) . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? O30 C29 C28 120.1(5) . . ? O30 C29 C24 119.9(5) . . ? C28 C29 C24 120.0 . . ? C29 O30 Ni42 131.0(6) . . ? C29 O30 Ni1 132.0(6) . 2 ? Ni42 O30 Ni1 96.5(4) . 2 ? C33 O32 Ni1 119.2(6) . . ? O32 C33 C34 134.6(6) . . ? O32 C33 H33 112.7 . . ? C34 C33 H33 112.7 . . ? C33 C34 C35 120.6(5) . . ? C33 C34 C39 119.4(5) . . ? C35 C34 C39 120.0 . . ? O40 C35 C34 121.7(5) . . ? O40 C35 C36 118.3(5) . . ? C34 C35 C36 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.0 . . ? C37 C38 Br41 121.3(5) . . ? C39 C38 Br41 118.7(5) . . ? C38 C39 C34 120.0 . . ? C38 C39 H39 120.0 . . ? C34 C39 H39 120.0 . . ? C35 O40 Ni1 124.7(5) . . ? C35 O40 Ni42 139.9(6) . . ? Ni1 O40 Ni42 95.0(4) . . ? O30 Ni42 O30 176.3(5) 2 . ? O30 Ni42 N22 93.0(4) 2 . ? O30 Ni42 N22 89.5(4) . . ? O30 Ni42 N22 89.5(4) 2 2 ? O30 Ni42 N22 93.0(4) . 2 ? N22 Ni42 N22 94.3(6) . 2 ? O30 Ni42 O40 79.9(4) 2 . ? O30 Ni42 O40 97.9(3) . . ? N22 Ni42 O40 80.2(4) . . ? N22 Ni42 O40 167.7(4) 2 . ? O30 Ni42 O40 97.9(3) 2 2 ? O30 Ni42 O40 79.9(4) . 2 ? N22 Ni42 O40 167.7(4) . 2 ? N22 Ni42 O40 80.2(4) 2 2 ? O40 Ni42 O40 107.2(5) . 2 ? 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 O40 Ni1 S2 P3 -172.5(3) . . . . ? N12 Ni1 S2 P3 3.4(4) . . . . ? N21 Ni1 S2 P3 16.9(10) . . . . ? O32 Ni1 S2 P3 -87.7(3) . . . . ? O30 Ni1 S2 P3 109.5(3) 2 . . . ? Ni1 S2 P3 O4 -119.4(4) . . . . ? Ni1 S2 P3 O8 121.0(5) . . . . ? Ni1 S2 P3 N12 -4.3(5) . . . . ? O8 P3 O4 C5 79.5(7) . . . . ? N12 P3 O4 C5 -162.1(6) . . . . ? S2 P3 O4 C5 -46.7(7) . . . . ? P3 O4 C5 C7 -108.3(10) . . . . ? P3 O4 C5 C6 129.1(8) . . . . ? O4 P3 O8 C9 172.4(8) . . . . ? N12 P3 O8 C9 59.9(11) . . . . ? S2 P3 O8 C9 -61.3(10) . . . . ? P3 O8 C9 C10 -140.3(8) . . . . ? P3 O8 C9 C11 99.2(10) . . . . ? O4 P3 N12 C13 -62.7(18) . . . . ? O8 P3 N12 C13 49(2) . . . . ? S2 P3 N12 C13 175.1(17) . . . . ? O4 P3 N12 Ni1 127.4(5) . . . . ? O8 P3 N12 Ni1 -121.3(5) . . . . ? S2 P3 N12 Ni1 5.3(6) . . . . ? O40 Ni1 N12 C13 -161.0(14) . . . . ? N21 Ni1 N12 C13 8.7(14) . . . . ? O32 Ni1 N12 C13 -84.6(15) . . . . ? O30 Ni1 N12 C13 89.0(14) 2 . . . ? S2 Ni1 N12 C13 -175.0(15) . . . . ? O40 Ni1 N12 P3 10.0(17) . . . . ? N21 Ni1 N12 P3 179.6(5) . . . . ? O32 Ni1 N12 P3 86.4(6) . . . . ? O30 Ni1 N12 P3 -100.0(5) 2 . . . ? S2 Ni1 N12 P3 -4.0(4) . . . . ? P3 N12 C13 N15 -175.9(11) . . . . ? Ni1 N12 C13 N15 -8(3) . . . . ? P3 N12 C13 S14 3(3) . . . . ? Ni1 N12 C13 S14 170.8(8) . . . . ? N12 C13 N15 C16 -2(3) . . . . ? S14 C13 N15 C16 179.3(5) . . . . ? C13 N15 C16 N21 8.6(13) . . . . ? C13 N15 C16 C17 -171.0(13) . . . . ? N21 C16 C17 C18 0.5(6) . . . . ? N15 C16 C17 C18 -179.9(4) . . . . ? C16 C17 C18 C19 -0.6(9) . . . . ? C17 C18 C19 C20 1.0(12) . . . . ? C18 C19 C20 N21 -1.3(14) . . . . ? C18 C19 C20 N22 179.0(8) . . . . ? C17 C16 N21 C20 -0.7(8) . . . . ? N15 C16 N21 C20 179.8(5) . . . . ? C17 C16 N21 Ni1 175.3(5) . . . . ? N15 C16 N21 Ni1 -4.2(7) . . . . ? C19 C20 N21 C16 1.1(12) . . . . ? N22 C20 N21 C16 -179.2(6) . . . . ? C19 C20 N21 Ni1 -175.0(7) . . . . ? N22 C20 N21 Ni1 4.7(11) . . . . ? O40 Ni1 N21 C16 174.1(6) . . . . ? N12 Ni1 N21 C16 -2.6(7) . . . . ? O32 Ni1 N21 C16 88.5(6) . . . . ? O30 Ni1 N21 C16 -110.9(7) 2 . . . ? S2 Ni1 N21 C16 -15.8(14) . . . . ? O40 Ni1 N21 C20 -10.3(8) . . . . ? N12 Ni1 N21 C20 173.0(8) . . . . ? O32 Ni1 N21 C20 -95.9(7) . . . . ? O30 Ni1 N21 C20 64.7(7) 2 . . . ? S2 Ni1 N21 C20 159.8(7) . . . . ? N21 C20 N22 C23 122.0(10) . . . . ? C19 C20 N22 C23 -58.3(12) . . . . ? N21 C20 N22 Ni42 -56.3(10) . . . . ? C19 C20 N22 Ni42 123.4(9) . . . . ? C20 N22 C23 C24 170.5(6) . . . . ? Ni42 N22 C23 C24 -11.1(12) . . . . ? N22 C23 C24 C25 177.7(8) . . . . ? N22 C23 C24 C29 -2.6(8) . . . . ? C29 C24 C25 C26 0.0 . . . . ? C23 C24 C25 C26 179.71(16) . . . . ? C24 C25 C26 C27 0.0 . . . . ? C24 C25 C26 Br31 179.0(3) . . . . ? C25 C26 C27 C28 0.0 . . . . ? Br31 C26 C27 C28 -179.0(3) . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 O30 178.6(4) . . . . ? C27 C28 C29 C24 0.0 . . . . ? C25 C24 C29 O30 -178.6(4) . . . . ? C23 C24 C29 O30 1.7(5) . . . . ? C25 C24 C29 C28 0.0 . . . . ? C23 C24 C29 C28 -179.68(17) . . . . ? C28 C29 O30 Ni42 -163.4(4) . . . . ? C24 C29 O30 Ni42 15.2(8) . . . . ? C28 C29 O30 Ni1 26.9(7) . . . 2 ? C24 C29 O30 Ni1 -154.4(5) . . . 2 ? O40 Ni1 O32 C33 29.2(8) . . . . ? N12 Ni1 O32 C33 -133.9(8) . . . . ? N21 Ni1 O32 C33 136.8(8) . . . . ? O30 Ni1 O32 C33 63.9(15) 2 . . . ? S2 Ni1 O32 C33 -58.3(8) . . . . ? Ni1 O32 C33 C34 -12.3(12) . . . . ? O32 C33 C34 C35 -10.8(9) . . . . ? O32 C33 C34 C39 169.1(8) . . . . ? C33 C34 C35 O40 0.2(5) . . . . ? C39 C34 C35 O40 -179.7(5) . . . . ? C33 C34 C35 C36 179.89(15) . . . . ? C39 C34 C35 C36 0.0 . . . . ? O40 C35 C36 C37 179.7(5) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C36 C37 C38 Br41 179.4(4) . . . . ? C37 C38 C39 C34 0.0 . . . . ? Br41 C38 C39 C34 -179.4(4) . . . . ? C33 C34 C39 C38 -179.89(15) . . . . ? C35 C34 C39 C38 0.0 . . . . ? C34 C35 O40 Ni1 32.3(8) . . . . ? C36 C35 O40 Ni1 -147.3(4) . . . . ? C34 C35 O40 Ni42 -157.5(6) . . . . ? C36 C35 O40 Ni42 22.8(10) . . . . ? N12 Ni1 O40 C35 36.5(17) . . . . ? N21 Ni1 O40 C35 -132.6(6) . . . . ? O32 Ni1 O40 C35 -40.8(7) . . . . ? O30 Ni1 O40 C35 150.7(7) 2 . . . ? S2 Ni1 O40 C35 50.1(6) . . . . ? N12 Ni1 O40 Ni42 -137.1(13) . . . . ? N21 Ni1 O40 Ni42 53.8(4) . . . . ? O32 Ni1 O40 Ni42 145.6(4) . . . . ? O30 Ni1 O40 Ni42 -22.9(3) 2 . . . ? S2 Ni1 O40 Ni42 -123.6(3) . . . . ? C29 O30 Ni42 N22 -22.1(7) . . . . ? Ni1 O30 Ni42 N22 150.2(4) 2 . . . ? C29 O30 Ni42 N22 -116.4(7) . . . 2 ? Ni1 O30 Ni42 N22 55.9(4) 2 . . 2 ? C29 O30 Ni42 O40 58.0(7) . . . . ? Ni1 O30 Ni42 O40 -129.7(3) 2 . . . ? C29 O30 Ni42 O40 164.2(7) . . . 2 ? Ni1 O30 Ni42 O40 -23.6(3) 2 . . 2 ? C23 N22 Ni42 O30 -159.6(7) . . . 2 ? C20 N22 Ni42 O30 18.8(9) . . . 2 ? C23 N22 Ni42 O30 17.7(8) . . . . ? C20 N22 Ni42 O30 -164.0(9) . . . . ? C23 N22 Ni42 N22 110.7(8) . . . 2 ? C20 N22 Ni42 N22 -71.0(9) . . . 2 ? C23 N22 Ni42 O40 -80.4(8) . . . . ? C20 N22 Ni42 O40 98.0(9) . . . . ? C23 N22 Ni42 O40 48(2) . . . 2 ? C20 N22 Ni42 O40 -133.7(17) . . . 2 ? C35 O40 Ni42 O30 -147.8(9) . . . 2 ? Ni1 O40 Ni42 O30 24.1(3) . . . 2 ? C35 O40 Ni42 O30 29.2(9) . . . . ? Ni1 O40 Ni42 O30 -158.9(3) . . . . ? C35 O40 Ni42 N22 117.3(9) . . . . ? Ni1 O40 Ni42 N22 -70.8(4) . . . . ? C35 O40 Ni42 N22 -178.6(17) . . . 2 ? Ni1 O40 Ni42 N22 -7(2) . . . 2 ? C35 O40 Ni42 O40 -52.6(8) . . . 2 ? Ni1 O40 Ni42 O40 119.2(4) . . . 2 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 15.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.426 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.085 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.279 0.135 0.314 60 12 ' ' 2 0.279 -0.135 0.814 60 12 ' ' 3 0.721 0.135 0.186 60 12 ' ' 4 0.721 -0.135 0.686 60 12 ' ' 5 0.221 0.365 0.686 60 12 ' ' 6 0.779 0.365 0.814 60 12 ' ' 7 0.221 0.635 0.186 60 12 ' ' 8 0.779 0.635 0.314 60 12 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 905822'