# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Liu, Po-Chun' _publ_contact_author_name 'Dr Po-Chun Liu' _publ_contact_author_email isiahliu@yahoo.com.tw _publ_section_title ; New Trinuclear Metal String Complexes Containing Rigid Hdzp Ligands: Synthesis, Structure, Magnetism and DFT calculation. (Hdzp = 1,9-diazaphenoxazine) ; # Attachment '- compound 1.cif' data_ic14794 _database_code_depnum_ccdc_archive 'CCDC 832185' #TrackingRef '- compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H7 N3 O' _chemical_formula_weight 185.19 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.9523(2) _cell_length_b 16.7982(4) _cell_length_c 7.5968(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.7211(13) _cell_angle_gamma 90.00 _cell_volume 812.25(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5453 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.935 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details ? _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5453 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1845 _reflns_number_gt 1327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0816P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1845 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 O1 O 0.32727(13) 1.03311(5) 0.13550(12) 0.0338(3) Uani 1 1 d . . . N1 N 0.88827(15) 1.07916(5) 0.32103(14) 0.0283(3) Uani 1 1 d . . . N2 N 0.72034(16) 0.96609(6) 0.36397(15) 0.0294(3) Uani 1 1 d . . . H2 H 0.851(3) 0.9515(8) 0.465(2) 0.061(4) Uiso 1 1 d . . . N3 N 0.55523(16) 0.85734(6) 0.43089(14) 0.0304(3) Uani 1 1 d . . . C1 C 0.87755(19) 1.15169(7) 0.24069(17) 0.0307(3) Uani 1 1 d . . . H1 H 1.0050 1.1795 0.2664 0.037 Uiso 1 1 calc R . . C2 C 0.69229(19) 1.18731(7) 0.12384(17) 0.0317(3) Uani 1 1 d . . . H2A H 0.6915 1.2383 0.0693 0.038 Uiso 1 1 calc R . . C3 C 0.50476(19) 1.14642(7) 0.08739(17) 0.0307(3) Uani 1 1 d . . . H3 H 0.3736 1.1692 0.0071 0.037 Uiso 1 1 calc R . . C4 C 0.51292(18) 1.07364(6) 0.16853(17) 0.0268(3) Uani 1 1 d . . . C5 C 0.70932(17) 1.04061(7) 0.28508(16) 0.0259(3) Uani 1 1 d . . . C6 C 0.53720(18) 0.92702(6) 0.34305(16) 0.0263(3) Uani 1 1 d . . . C7 C 0.34225(19) 0.96108(7) 0.22963(16) 0.0270(3) Uani 1 1 d . . . C8 C 0.16137(19) 0.92216(7) 0.20933(18) 0.0314(3) Uani 1 1 d . . . H8 H 0.0276 0.9445 0.1350 0.038 Uiso 1 1 calc R . . C9 C 0.17857(19) 0.84902(7) 0.30042(18) 0.0333(3) Uani 1 1 d . . . H9 H 0.0565 0.8202 0.2887 0.040 Uiso 1 1 calc R . . C10 C 0.3758(2) 0.81923(7) 0.40778(18) 0.0324(3) Uani 1 1 d . . . H10 H 0.3860 0.7691 0.4689 0.039 Uiso 1 1 calc 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 O1 0.0230(5) 0.0315(5) 0.0400(5) 0.0054(4) 0.0054(4) 0.0009(3) N1 0.0266(6) 0.0297(6) 0.0275(5) 0.0006(4) 0.0097(4) -0.0011(4) N2 0.0215(6) 0.0291(6) 0.0326(6) 0.0039(4) 0.0055(4) -0.0001(4) N3 0.0309(6) 0.0293(6) 0.0313(6) 0.0011(4) 0.0129(4) -0.0004(4) C1 0.0315(7) 0.0313(7) 0.0296(7) -0.0022(5) 0.0126(5) -0.0033(5) C2 0.0383(8) 0.0268(6) 0.0300(7) 0.0020(5) 0.0136(6) 0.0011(5) C3 0.0293(7) 0.0309(7) 0.0286(6) 0.0007(5) 0.0082(5) 0.0058(5) C4 0.0228(6) 0.0297(6) 0.0256(6) -0.0027(5) 0.0075(5) 0.0009(4) C5 0.0242(6) 0.0280(6) 0.0234(6) -0.0021(4) 0.0074(5) 0.0017(4) C6 0.0250(6) 0.0282(6) 0.0249(6) -0.0028(5) 0.0091(5) 0.0005(5) C7 0.0260(6) 0.0268(6) 0.0260(6) -0.0027(5) 0.0082(5) 0.0010(5) C8 0.0244(7) 0.0376(7) 0.0307(7) -0.0037(5) 0.0095(5) 0.0004(5) C9 0.0296(7) 0.0367(7) 0.0353(7) -0.0064(5) 0.0147(6) -0.0071(5) C10 0.0358(7) 0.0307(7) 0.0326(7) -0.0005(5) 0.0156(5) -0.0029(5) _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 O1 C7 1.3880(14) . ? O1 C4 1.3899(13) . ? N1 C5 1.3298(14) . ? N1 C1 1.3513(14) . ? N2 C5 1.3767(15) . ? N2 C6 1.3836(14) . ? N3 C6 1.3282(15) . ? N3 C10 1.3495(15) . ? C1 C2 1.3730(17) . ? C2 C3 1.3993(16) . ? C3 C4 1.3600(16) . ? C4 C5 1.4084(16) . ? C6 C7 1.4025(16) . ? C7 C8 1.3699(16) . ? C8 C9 1.3914(17) . ? C9 C10 1.3767(18) . ? 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 C7 O1 C4 117.53(9) . . ? C5 N1 C1 117.98(10) . . ? C5 N2 C6 119.59(10) . . ? C6 N3 C10 117.21(10) . . ? N1 C1 C2 123.50(11) . . ? C1 C2 C3 118.10(11) . . ? C4 C3 C2 119.08(11) . . ? C3 C4 O1 119.48(10) . . ? C3 C4 C5 119.49(11) . . ? O1 C4 C5 121.03(10) . . ? N1 C5 N2 118.02(10) . . ? N1 C5 C4 121.85(11) . . ? N2 C5 C4 120.13(10) . . ? N3 C6 N2 117.64(10) . . ? N3 C6 C7 122.73(10) . . ? N2 C6 C7 119.62(10) . . ? C8 C7 O1 118.87(10) . . ? C8 C7 C6 119.40(11) . . ? O1 C7 C6 121.72(10) . . ? C7 C8 C9 118.30(11) . . ? C10 C9 C8 118.78(11) . . ? N3 C10 C9 123.57(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 N1 0.957(17) 1.954(17) 2.9102(14) 177.8(13) 3_776 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.214 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.048 # Attachment '- compound 2.cif' data_ic14741 _database_code_depnum_ccdc_archive 'CCDC 832186' #TrackingRef '- compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H45 Cl3 N14 Ni3 O6 S2' _chemical_formula_weight 1296.61 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8397(2) _cell_length_b 14.0455(3) _cell_length_c 17.5224(4) _cell_angle_alpha 110.9505(9) _cell_angle_beta 94.3680(12) _cell_angle_gamma 107.3184(12) _cell_volume 2757.57(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 33146 _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour ?dark-greendark-green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.595 _exptl_absorpt_correction_T_max 0.736 _exptl_absorpt_process_details ? _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33146 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12570 _reflns_number_gt 9465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1072P)^2^+6.0499P] 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 12570 _refine_ls_number_parameters 701 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1924 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 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 0.36677(4) 0.27864(4) 0.22581(3) 0.02169(13) Uani 1 1 d . . . Ni2 Ni 0.25877(4) 0.40135(4) 0.23887(3) 0.01937(13) Uani 1 1 d . . . Ni3 Ni 0.14969(4) 0.52345(4) 0.25407(3) 0.02265(14) Uani 1 1 d . . . S1 S 0.57929(10) 0.05236(9) 0.22831(8) 0.0366(3) Uani 1 1 d . . . S2 S -0.03368(12) 0.77530(11) 0.26975(10) 0.0509(4) Uani 1 1 d . . . N1 N 0.2112(3) 0.1591(3) 0.1944(2) 0.0271(7) Uani 1 1 d . . . N2 N 0.1321(3) 0.2927(3) 0.2446(2) 0.0247(7) Uani 1 1 d . . . N3 N 0.0497(3) 0.4222(3) 0.3011(2) 0.0253(7) Uani 1 1 d . . . N4 N 0.5031(3) 0.4214(3) 0.2576(2) 0.0238(7) Uani 1 1 d . . . N5 N 0.3848(3) 0.5103(3) 0.2329(2) 0.0228(7) Uani 1 1 d . . . N6 N 0.2733(3) 0.6052(3) 0.2079(2) 0.0249(7) Uani 1 1 d . . . N7 N 0.3489(3) 0.2605(3) 0.1027(2) 0.0247(7) Uani 1 1 d . . . N8 N 0.2129(3) 0.3417(3) 0.1207(2) 0.0241(7) Uani 1 1 d . . . N9 N 0.0712(3) 0.4153(3) 0.1320(2) 0.0265(7) Uani 1 1 d . . . N10 N 0.3568(3) 0.3130(3) 0.3501(2) 0.0237(7) Uani 1 1 d . . . N11 N 0.3050(3) 0.4612(3) 0.3575(2) 0.0227(7) Uani 1 1 d . . . N12 N 0.2513(3) 0.6103(3) 0.3722(2) 0.0253(7) Uani 1 1 d . . . N13 N 0.4554(3) 0.1821(3) 0.2188(2) 0.0299(8) Uani 1 1 d . . . N14 N 0.0599(3) 0.6196(3) 0.2661(2) 0.0328(8) Uani 1 1 d . . . O1 O -0.0572(3) 0.1327(2) 0.2545(2) 0.0361(7) Uani 1 1 d . . . O2 O 0.5737(3) 0.6741(3) 0.2260(2) 0.0390(8) Uani 1 1 d . . . O3 O 0.1462(3) 0.2568(3) -0.05622(19) 0.0363(7) Uani 1 1 d . . . O4 O 0.3630(3) 0.5425(2) 0.53480(18) 0.0323(7) Uani 1 1 d . . . C1 C 0.2023(4) 0.0529(3) 0.1644(3) 0.0389(11) Uani 1 1 d . . . H1 H 0.2632 0.0340 0.1445 0.047 Uiso 1 1 calc R . . C2 C 0.1090(5) -0.0279(4) 0.1617(4) 0.0530(15) Uani 1 1 d . . . H2 H 0.1041 -0.1018 0.1385 0.064 Uiso 1 1 calc R . . C3 C 0.0222(4) -0.0005(4) 0.1932(4) 0.0476(13) Uani 1 1 d . . . H3 H -0.0419 -0.0548 0.1946 0.057 Uiso 1 1 calc R . . C4 C 0.0291(4) 0.1062(3) 0.2226(3) 0.0326(9) Uani 1 1 d . . . C5 C 0.1243(3) 0.1859(3) 0.2197(3) 0.0255(8) Uani 1 1 d . . . C6 C 0.0462(3) 0.3193(3) 0.2781(3) 0.0246(8) Uani 1 1 d . . . C7 C -0.0444(3) 0.2416(3) 0.2887(3) 0.0289(9) Uani 1 1 d . . . C8 C -0.1210(4) 0.2729(4) 0.3308(3) 0.0350(10) Uani 1 1 d . . . H8 H -0.1806 0.2210 0.3394 0.042 Uiso 1 1 calc R . . C9 C -0.1108(4) 0.3832(4) 0.3617(3) 0.0370(10) Uani 1 1 d . . . H9 H -0.1608 0.4082 0.3940 0.044 Uiso 1 1 calc R . . C10 C -0.0264(4) 0.4535(4) 0.3439(3) 0.0310(9) Uani 1 1 d . . . H10 H -0.0210 0.5275 0.3623 0.037 Uiso 1 1 calc R . . C11 C 0.6077(3) 0.4198(3) 0.2732(3) 0.0276(8) Uani 1 1 d . . . H11 H 0.6163 0.3595 0.2822 0.033 Uiso 1 1 calc R . . C12 C 0.7011(3) 0.5009(4) 0.2766(3) 0.0328(9) Uani 1 1 d . . . H12 H 0.7729 0.4977 0.2892 0.039 Uiso 1 1 calc R . . C13 C 0.6894(3) 0.5884(4) 0.2612(3) 0.0338(10) Uani 1 1 d . . . H13 H 0.7528 0.6454 0.2622 0.041 Uiso 1 1 calc R . . C14 C 0.5850(3) 0.5899(3) 0.2448(3) 0.0278(8) Uani 1 1 d . . . C15 C 0.4899(3) 0.5070(3) 0.2452(2) 0.0232(8) Uani 1 1 d . . . C16 C 0.3749(3) 0.5965(3) 0.2165(2) 0.0237(8) Uani 1 1 d . . . C17 C 0.4675(3) 0.6762(3) 0.2110(3) 0.0296(9) Uani 1 1 d . . . C18 C 0.4551(4) 0.7580(4) 0.1912(3) 0.0387(11) Uani 1 1 d . . . H18 H 0.5179 0.8110 0.1868 0.046 Uiso 1 1 calc R . . C19 C 0.3488(4) 0.7630(4) 0.1776(3) 0.0394(11) Uani 1 1 d . . . H19 H 0.3375 0.8182 0.1623 0.047 Uiso 1 1 calc R . . C20 C 0.2610(4) 0.6866(3) 0.1867(3) 0.0314(9) Uani 1 1 d . . . H20 H 0.1886 0.6903 0.1779 0.038 Uiso 1 1 calc R . . C21 C 0.4060(4) 0.2060(4) 0.0521(3) 0.0311(9) Uani 1 1 d . . . H21 H 0.4664 0.1937 0.0769 0.037 Uiso 1 1 calc R . . C22 C 0.3798(4) 0.1683(4) -0.0330(3) 0.0368(10) Uani 1 1 d . . . H22 H 0.4214 0.1306 -0.0665 0.044 Uiso 1 1 calc R . . C23 C 0.2918(4) 0.1860(4) -0.0699(3) 0.0360(10) Uani 1 1 d . . . H23 H 0.2715 0.1600 -0.1289 0.043 Uiso 1 1 calc R . . C24 C 0.2349(3) 0.2414(3) -0.0195(3) 0.0294(9) Uani 1 1 d . . . C25 C 0.2670(3) 0.2822(3) 0.0687(2) 0.0243(8) Uani 1 1 d . . . C26 C 0.1238(3) 0.3563(3) 0.0834(2) 0.0241(8) Uani 1 1 d . . . C27 C 0.0891(3) 0.3128(3) -0.0040(3) 0.0285(9) Uani 1 1 d . . . C28 C -0.0006(4) 0.3261(3) -0.0400(3) 0.0320(9) Uani 1 1 d . . . H28 H -0.0228 0.2983 -0.0990 0.038 Uiso 1 1 calc R . . C29 C -0.0588(4) 0.3814(4) 0.0121(3) 0.0338(10) Uani 1 1 d . . . H29 H -0.1241 0.3887 -0.0107 0.041 Uiso 1 1 calc R . . C30 C -0.0207(3) 0.4247(3) 0.0959(3) 0.0293(9) Uani 1 1 d . . . H30 H -0.0601 0.4635 0.1310 0.035 Uiso 1 1 calc R . . C31 C 0.3800(3) 0.2490(3) 0.3875(3) 0.0274(8) Uani 1 1 d . . . H31 H 0.3871 0.1823 0.3534 0.033 Uiso 1 1 calc R . . C32 C 0.3934(4) 0.2772(4) 0.4713(3) 0.0329(9) Uani 1 1 d . . . H32 H 0.4062 0.2297 0.4951 0.039 Uiso 1 1 calc R . . C33 C 0.3878(4) 0.3784(4) 0.5221(3) 0.0331(9) Uani 1 1 d . . . H33 H 0.4006 0.4022 0.5811 0.040 Uiso 1 1 calc R . . C34 C 0.3638(3) 0.4413(3) 0.4850(3) 0.0257(8) Uani 1 1 d . . . C35 C 0.3421(3) 0.4048(3) 0.3972(2) 0.0222(7) Uani 1 1 d . . . C36 C 0.2957(3) 0.5580(3) 0.4079(2) 0.0224(8) Uani 1 1 d . . . C37 C 0.3290(3) 0.6015(3) 0.4957(3) 0.0260(8) Uani 1 1 d . . . C38 C 0.3291(4) 0.7019(3) 0.5436(3) 0.0319(9) Uani 1 1 d . . . H38 H 0.3556 0.7325 0.6023 0.038 Uiso 1 1 calc R . . C39 C 0.2895(4) 0.7593(3) 0.5048(3) 0.0348(10) Uani 1 1 d . . . H39 H 0.2899 0.8303 0.5363 0.042 Uiso 1 1 calc R . . C40 C 0.2503(4) 0.7106(3) 0.4203(3) 0.0313(9) Uani 1 1 d . . . H40 H 0.2210 0.7484 0.3940 0.038 Uiso 1 1 calc R . . C41 C 0.5067(3) 0.1273(3) 0.2217(3) 0.0258(8) Uani 1 1 d . . . C42 C 0.0204(3) 0.6848(3) 0.2682(3) 0.0278(8) Uani 1 1 d . . . Cl1 Cl -0.36701(13) 0.08600(14) -0.01971(10) 0.0643(4) Uani 1 1 d . . . Cl2 Cl -0.26591(14) 0.26910(12) 0.13792(10) 0.0632(4) Uani 1 1 d . . . Cl3 Cl -0.14205(14) 0.13077(15) 0.06176(10) 0.0649(4) Uani 1 1 d . . . O5 O 0.0792(6) 0.8780(5) 0.5652(4) 0.0991(18) Uani 1 1 d . . . C43 C -0.2729(5) 0.1370(5) 0.0768(4) 0.0513(13) Uani 1 1 d . . . H43 H -0.3030 0.0898 0.1071 0.062 Uiso 1 1 calc R . . C44 C 0.2252(8) 1.0453(7) 0.6545(7) 0.107(3) Uani 1 1 d . . . H44A H 0.2294 1.1090 0.7038 0.161 Uiso 1 1 calc R . . H44B H 0.2766 1.0683 0.6207 0.161 Uiso 1 1 calc R . . H44C H 0.2458 0.9935 0.6722 0.161 Uiso 1 1 calc R . . C45 C 0.1123(13) 0.9939(9) 0.6053(8) 0.157(6) Uani 1 1 d . . . H45A H 0.0603 1.0126 0.6422 0.189 Uiso 1 1 calc R . . H45B H 0.1065 1.0235 0.5623 0.189 Uiso 1 1 calc R . . C46 C -0.0480(12) 0.8144(9) 0.5302(8) 0.171(7) Uani 1 1 d . . . H46A H -0.0874 0.8213 0.5772 0.205 Uiso 1 1 calc R . . H46B H -0.0770 0.8468 0.4955 0.205 Uiso 1 1 calc R . . C47 C -0.0695(8) 0.7042(7) 0.4821(5) 0.101(3) Uani 1 1 d . . . H47A H -0.1372 0.6753 0.4391 0.152 Uiso 1 1 calc R . . H47B H -0.0797 0.6639 0.5181 0.152 Uiso 1 1 calc R . . H47C H -0.0065 0.6962 0.4554 0.152 Uiso 1 1 calc R . . O6 O 0.3949(10) 1.0130(11) 0.4803(8) 0.109(4) Uiso 0.50 1 d PD A -1 C48 C 0.2547(17) 0.974(2) 0.3901(16) 0.141(8) Uiso 0.50 1 d PD A -1 H48A H 0.2425 0.9996 0.4473 0.211 Uiso 0.50 1 calc PR A -1 H48B H 0.2002 0.9007 0.3574 0.211 Uiso 0.50 1 calc PR A -1 H48C H 0.2460 1.0234 0.3646 0.211 Uiso 0.50 1 calc PR A -1 C49 C 0.3658(13) 0.9699(14) 0.3913(9) 0.084(4) Uiso 0.50 1 d PD A -1 H49A H 0.3665 0.8951 0.3645 0.101 Uiso 0.50 1 calc PR A -1 H49B H 0.4120 1.0176 0.3673 0.101 Uiso 0.50 1 calc PR A -1 C50 C 0.5000 1.0000 0.5000 0.139(6) Uiso 1 2 d SD A -1 H50A H 0.5563 1.0290 0.4708 0.167 Uiso 0.50 1 calc PR A -1 H50B H 0.4914 0.9236 0.4890 0.167 Uiso 0.50 1 calc PR A -1 C51 C 0.525(3) 1.072(2) 0.5935(12) 0.202(14) Uiso 0.50 1 d PD A -1 H51A H 0.5358 1.1469 0.6013 0.303 Uiso 0.50 1 calc PR A -1 H51B H 0.5933 1.0693 0.6209 0.303 Uiso 0.50 1 calc PR A -1 H51C H 0.4628 1.0451 0.6182 0.303 Uiso 0.50 1 calc PR A -1 O7 O 0.4951(10) 0.4763(9) 0.0121(7) 0.079(3) Uiso 0.50 1 d PD . -1 C52 C 0.3382(9) 0.5145(9) -0.0299(7) 0.124(4) Uiso 1 1 d D . . H52A H 0.2998 0.4403 -0.0718 0.187 Uiso 1 1 calc R . . H52B H 0.3200 0.5663 -0.0491 0.187 Uiso 1 1 calc R . . H52C H 0.3142 0.5211 0.0230 0.187 Uiso 1 1 calc R . . C53 C 0.4496(12) 0.5364(13) -0.0184(11) 0.176(7) Uiso 1 1 d D . . H53A H 0.4861 0.6138 0.0200 0.212 Uiso 1 1 calc R . . H53B H 0.4710 0.5288 -0.0728 0.212 Uiso 1 1 calc 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 0.0256(3) 0.0201(2) 0.0209(3) 0.0074(2) 0.00606(19) 0.0106(2) Ni2 0.0211(2) 0.0179(2) 0.0192(3) 0.00738(19) 0.00474(18) 0.00689(19) Ni3 0.0241(3) 0.0211(3) 0.0257(3) 0.0105(2) 0.0060(2) 0.0103(2) S1 0.0427(6) 0.0307(5) 0.0466(7) 0.0180(5) 0.0115(5) 0.0228(5) S2 0.0584(8) 0.0469(7) 0.0779(10) 0.0398(7) 0.0315(7) 0.0376(7) N1 0.0303(17) 0.0194(16) 0.0279(18) 0.0063(14) 0.0079(14) 0.0071(14) N2 0.0256(16) 0.0216(16) 0.0274(18) 0.0091(14) 0.0078(13) 0.0089(13) N3 0.0254(16) 0.0264(17) 0.0277(18) 0.0114(14) 0.0080(13) 0.0126(14) N4 0.0260(16) 0.0253(16) 0.0200(17) 0.0079(14) 0.0051(13) 0.0103(13) N5 0.0221(15) 0.0208(15) 0.0266(18) 0.0102(14) 0.0054(13) 0.0079(13) N6 0.0284(17) 0.0229(16) 0.0254(18) 0.0114(14) 0.0052(13) 0.0095(14) N7 0.0276(17) 0.0252(16) 0.0212(17) 0.0073(14) 0.0067(13) 0.0111(14) N8 0.0261(16) 0.0241(16) 0.0212(17) 0.0074(13) 0.0036(13) 0.0095(13) N9 0.0255(16) 0.0252(17) 0.0282(18) 0.0120(15) 0.0028(14) 0.0071(14) N10 0.0291(17) 0.0218(16) 0.0234(17) 0.0106(14) 0.0077(13) 0.0106(13) N11 0.0276(16) 0.0222(16) 0.0208(17) 0.0099(13) 0.0064(13) 0.0104(13) N12 0.0299(17) 0.0221(16) 0.0262(18) 0.0102(14) 0.0079(14) 0.0111(14) N13 0.0352(19) 0.0281(18) 0.030(2) 0.0117(15) 0.0094(15) 0.0147(15) N14 0.0337(19) 0.0313(19) 0.037(2) 0.0140(17) 0.0080(16) 0.0149(16) O1 0.0333(16) 0.0259(15) 0.049(2) 0.0158(14) 0.0178(14) 0.0067(13) O2 0.0282(15) 0.0336(17) 0.064(2) 0.0307(17) 0.0117(15) 0.0079(13) O3 0.0402(17) 0.0442(18) 0.0223(16) 0.0073(14) -0.0003(13) 0.0209(15) O4 0.0525(19) 0.0280(15) 0.0192(15) 0.0074(12) 0.0074(13) 0.0202(14) C1 0.042(3) 0.022(2) 0.048(3) 0.006(2) 0.017(2) 0.0118(19) C2 0.057(3) 0.020(2) 0.075(4) 0.009(2) 0.029(3) 0.012(2) C3 0.046(3) 0.024(2) 0.064(4) 0.012(2) 0.023(3) 0.006(2) C4 0.031(2) 0.027(2) 0.038(3) 0.0123(19) 0.0112(18) 0.0063(17) C5 0.029(2) 0.0199(18) 0.026(2) 0.0081(16) 0.0065(16) 0.0071(16) C6 0.0242(18) 0.0259(19) 0.025(2) 0.0120(17) 0.0062(15) 0.0086(16) C7 0.029(2) 0.026(2) 0.031(2) 0.0113(18) 0.0061(17) 0.0080(16) C8 0.031(2) 0.038(2) 0.045(3) 0.023(2) 0.0170(19) 0.0126(19) C9 0.035(2) 0.040(2) 0.047(3) 0.024(2) 0.020(2) 0.019(2) C10 0.032(2) 0.033(2) 0.034(2) 0.0146(19) 0.0123(18) 0.0190(18) C11 0.029(2) 0.030(2) 0.023(2) 0.0086(17) 0.0037(16) 0.0123(17) C12 0.025(2) 0.040(2) 0.032(2) 0.012(2) 0.0045(17) 0.0128(18) C13 0.024(2) 0.034(2) 0.037(3) 0.013(2) 0.0074(17) 0.0020(17) C14 0.031(2) 0.026(2) 0.027(2) 0.0114(17) 0.0071(16) 0.0088(17) C15 0.0266(19) 0.0216(18) 0.0198(19) 0.0069(15) 0.0057(15) 0.0073(15) C16 0.0292(19) 0.0228(18) 0.0192(19) 0.0089(15) 0.0059(15) 0.0085(16) C17 0.029(2) 0.029(2) 0.033(2) 0.0157(18) 0.0088(17) 0.0084(17) C18 0.043(3) 0.033(2) 0.048(3) 0.026(2) 0.014(2) 0.010(2) C19 0.048(3) 0.038(2) 0.050(3) 0.032(2) 0.019(2) 0.020(2) C20 0.041(2) 0.030(2) 0.032(2) 0.0182(19) 0.0096(18) 0.0176(19) C21 0.034(2) 0.036(2) 0.029(2) 0.0134(19) 0.0127(18) 0.0182(19) C22 0.041(2) 0.044(3) 0.027(2) 0.009(2) 0.0142(19) 0.022(2) C23 0.041(2) 0.041(3) 0.022(2) 0.0082(19) 0.0071(18) 0.015(2) C24 0.031(2) 0.030(2) 0.026(2) 0.0115(17) 0.0034(16) 0.0082(17) C25 0.0253(19) 0.0231(18) 0.0210(19) 0.0076(16) 0.0029(15) 0.0055(15) C26 0.0230(18) 0.0229(18) 0.025(2) 0.0095(16) 0.0030(15) 0.0061(15) C27 0.028(2) 0.028(2) 0.026(2) 0.0094(17) 0.0026(16) 0.0083(17) C28 0.033(2) 0.029(2) 0.028(2) 0.0111(18) -0.0043(17) 0.0059(17) C29 0.029(2) 0.032(2) 0.039(3) 0.017(2) -0.0031(18) 0.0091(18) C30 0.0250(19) 0.027(2) 0.036(2) 0.0138(18) 0.0014(17) 0.0084(16) C31 0.034(2) 0.0243(19) 0.030(2) 0.0136(17) 0.0111(17) 0.0136(17) C32 0.043(2) 0.032(2) 0.034(2) 0.0194(19) 0.0108(19) 0.0189(19) C33 0.047(3) 0.036(2) 0.023(2) 0.0146(19) 0.0101(18) 0.018(2) C34 0.030(2) 0.0254(19) 0.023(2) 0.0093(16) 0.0081(16) 0.0109(16) C35 0.0240(18) 0.0224(18) 0.0202(19) 0.0092(15) 0.0066(14) 0.0069(15) C36 0.0239(18) 0.0220(18) 0.023(2) 0.0097(16) 0.0093(15) 0.0082(15) C37 0.0282(19) 0.0242(19) 0.024(2) 0.0084(16) 0.0068(16) 0.0086(16) C38 0.038(2) 0.029(2) 0.024(2) 0.0042(17) 0.0099(18) 0.0120(18) C39 0.045(3) 0.023(2) 0.033(2) 0.0053(18) 0.009(2) 0.0143(19) C40 0.038(2) 0.024(2) 0.034(2) 0.0114(18) 0.0085(18) 0.0136(18) C41 0.032(2) 0.0210(18) 0.025(2) 0.0084(16) 0.0085(16) 0.0099(16) C42 0.027(2) 0.028(2) 0.031(2) 0.0124(18) 0.0106(17) 0.0111(17) Cl1 0.0603(9) 0.0676(10) 0.0596(9) 0.0117(8) 0.0097(7) 0.0323(8) Cl2 0.0714(10) 0.0484(8) 0.0626(10) 0.0120(7) 0.0255(8) 0.0207(7) Cl3 0.0639(9) 0.0841(11) 0.0592(9) 0.0277(8) 0.0202(7) 0.0425(8) O5 0.120(5) 0.078(4) 0.104(5) 0.028(3) 0.018(4) 0.052(4) C43 0.064(3) 0.046(3) 0.049(3) 0.017(3) 0.021(3) 0.026(3) C44 0.094(6) 0.059(5) 0.132(8) 0.000(5) -0.005(6) 0.030(4) C45 0.261(17) 0.088(7) 0.127(10) 0.023(7) -0.008(10) 0.102(10) C46 0.221(14) 0.098(7) 0.142(10) -0.001(7) -0.105(10) 0.079(9) C47 0.116(7) 0.093(6) 0.062(5) -0.004(4) -0.002(5) 0.039(5) _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 N13 1.992(4) . ? Ni1 N7 2.066(3) . ? Ni1 N1 2.071(3) . ? Ni1 N10 2.078(3) . ? Ni1 N4 2.088(3) . ? Ni1 Ni2 2.4770(6) . ? Ni2 N8 1.901(3) . ? Ni2 N5 1.907(3) . ? Ni2 N2 1.908(3) . ? Ni2 N11 1.910(3) . ? Ni2 Ni3 2.4766(6) . ? Ni3 N14 1.989(4) . ? Ni3 N3 2.065(3) . ? Ni3 N6 2.066(3) . ? Ni3 N12 2.076(3) . ? Ni3 N9 2.083(3) . ? S1 C41 1.626(4) . ? S2 C42 1.612(4) . ? N1 C5 1.338(5) . ? N1 C1 1.358(5) . ? N2 C6 1.374(5) . ? N2 C5 1.374(5) . ? N3 C6 1.340(5) . ? N3 C10 1.357(5) . ? N4 C15 1.350(5) . ? N4 C11 1.359(5) . ? N5 C15 1.368(5) . ? N5 C16 1.378(5) . ? N6 C16 1.349(5) . ? N6 C20 1.368(5) . ? N7 C25 1.333(5) . ? N7 C21 1.363(5) . ? N8 C26 1.379(5) . ? N8 C25 1.380(5) . ? N9 C26 1.335(5) . ? N9 C30 1.360(5) . ? N10 C35 1.337(5) . ? N10 C31 1.370(5) . ? N11 C36 1.378(5) . ? N11 C35 1.379(5) . ? N12 C36 1.334(5) . ? N12 C40 1.363(5) . ? N13 C41 1.164(5) . ? N14 C42 1.164(5) . ? O1 C4 1.369(5) . ? O1 C7 1.380(5) . ? O2 C14 1.378(5) . ? O2 C17 1.379(5) . ? O3 C24 1.376(5) . ? O3 C27 1.386(5) . ? O4 C34 1.380(5) . ? O4 C37 1.387(5) . ? C1 C2 1.368(7) . ? C2 C3 1.375(7) . ? C3 C4 1.371(6) . ? C4 C5 1.408(6) . ? C6 C7 1.415(6) . ? C7 C8 1.357(6) . ? C8 C9 1.407(6) . ? C9 C10 1.372(6) . ? C11 C12 1.365(6) . ? C12 C13 1.396(6) . ? C13 C14 1.358(6) . ? C14 C15 1.417(6) . ? C16 C17 1.407(6) . ? C17 C18 1.361(6) . ? C18 C19 1.393(7) . ? C19 C20 1.370(6) . ? C21 C22 1.367(6) . ? C22 C23 1.388(7) . ? C23 C24 1.366(6) . ? C24 C25 1.421(6) . ? C26 C27 1.408(6) . ? C27 C28 1.364(6) . ? C28 C29 1.391(7) . ? C29 C30 1.357(6) . ? C31 C32 1.360(6) . ? C32 C33 1.408(6) . ? C33 C34 1.357(6) . ? C34 C35 1.412(6) . ? C36 C37 1.413(6) . ? C37 C38 1.358(6) . ? C38 C39 1.397(6) . ? C39 C40 1.367(6) . ? Cl1 C43 1.773(6) . ? Cl2 C43 1.750(6) . ? Cl3 C43 1.743(6) . ? O5 C45 1.432(11) . ? O5 C46 1.558(14) . ? C44 C45 1.451(15) . ? C46 C47 1.400(12) . ? O6 C49 1.427(14) . ? O6 C50 1.447(11) . ? C48 C49 1.442(16) . ? C50 C51 1.533(18) . ? O7 C53 0.791(17) 2_665 ? O7 C53 1.382(13) . ? C52 C53 1.353(12) . ? C53 O7 0.791(17) 2_665 ? 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 N13 Ni1 N7 97.38(14) . . ? N13 Ni1 N1 96.68(14) . . ? N7 Ni1 N1 88.35(14) . . ? N13 Ni1 N10 95.52(14) . . ? N7 Ni1 N10 166.79(13) . . ? N1 Ni1 N10 87.32(13) . . ? N13 Ni1 N4 96.09(14) . . ? N7 Ni1 N4 89.33(13) . . ? N1 Ni1 N4 167.22(13) . . ? N10 Ni1 N4 92.14(13) . . ? N13 Ni1 Ni2 178.37(11) . . ? N7 Ni1 Ni2 84.10(9) . . ? N1 Ni1 Ni2 84.01(9) . . ? N10 Ni1 Ni2 83.03(9) . . ? N4 Ni1 Ni2 83.25(9) . . ? N8 Ni2 N5 89.92(14) . . ? N8 Ni2 N2 89.93(14) . . ? N5 Ni2 N2 179.64(14) . . ? N8 Ni2 N11 179.90(15) . . ? N5 Ni2 N11 90.06(14) . . ? N2 Ni2 N11 90.09(14) . . ? N8 Ni2 Ni3 90.89(10) . . ? N5 Ni2 Ni3 89.79(10) . . ? N2 Ni2 Ni3 89.88(10) . . ? N11 Ni2 Ni3 89.21(10) . . ? N8 Ni2 Ni1 89.88(10) . . ? N5 Ni2 Ni1 90.87(10) . . ? N2 Ni2 Ni1 89.46(10) . . ? N11 Ni2 Ni1 90.03(10) . . ? Ni3 Ni2 Ni1 178.99(3) . . ? N14 Ni3 N3 96.06(14) . . ? N14 Ni3 N6 96.80(14) . . ? N3 Ni3 N6 167.01(13) . . ? N14 Ni3 N12 96.33(14) . . ? N3 Ni3 N12 88.28(13) . . ? N6 Ni3 N12 88.57(13) . . ? N14 Ni3 N9 96.68(15) . . ? N3 Ni3 N9 91.39(13) . . ? N6 Ni3 N9 88.85(13) . . ? N12 Ni3 N9 166.95(13) . . ? N14 Ni3 Ni2 179.07(11) . . ? N3 Ni3 Ni2 83.10(9) . . ? N6 Ni3 Ni2 84.05(9) . . ? N12 Ni3 Ni2 84.07(9) . . ? N9 Ni3 Ni2 82.94(9) . . ? C5 N1 C1 119.1(4) . . ? C5 N1 Ni1 119.9(3) . . ? C1 N1 Ni1 119.5(3) . . ? C6 N2 C5 116.7(3) . . ? C6 N2 Ni2 121.0(3) . . ? C5 N2 Ni2 122.3(3) . . ? C6 N3 C10 119.2(4) . . ? C6 N3 Ni3 120.2(3) . . ? C10 N3 Ni3 119.7(3) . . ? C15 N4 C11 119.0(3) . . ? C15 N4 Ni1 120.3(3) . . ? C11 N4 Ni1 119.2(3) . . ? C15 N5 C16 116.6(3) . . ? C15 N5 Ni2 121.5(3) . . ? C16 N5 Ni2 121.9(3) . . ? C16 N6 C20 118.9(3) . . ? C16 N6 Ni3 119.7(3) . . ? C20 N6 Ni3 119.6(3) . . ? C25 N7 C21 119.2(4) . . ? C25 N7 Ni1 120.2(3) . . ? C21 N7 Ni1 119.2(3) . . ? C26 N8 C25 117.2(3) . . ? C26 N8 Ni2 121.1(3) . . ? C25 N8 Ni2 121.8(3) . . ? C26 N9 C30 118.9(4) . . ? C26 N9 Ni3 120.4(3) . . ? C30 N9 Ni3 118.8(3) . . ? C35 N10 C31 118.9(3) . . ? C35 N10 Ni1 120.6(3) . . ? C31 N10 Ni1 120.0(3) . . ? C36 N11 C35 116.8(3) . . ? C36 N11 Ni2 122.1(3) . . ? C35 N11 Ni2 121.0(3) . . ? C36 N12 C40 119.1(4) . . ? C36 N12 Ni3 118.9(3) . . ? C40 N12 Ni3 120.0(3) . . ? C41 N13 Ni1 174.1(3) . . ? C42 N14 Ni3 169.0(4) . . ? C4 O1 C7 117.3(3) . . ? C14 O2 C17 117.5(3) . . ? C24 O3 C27 117.6(3) . . ? C34 O4 C37 117.7(3) . . ? N1 C1 C2 122.4(4) . . ? C1 C2 C3 118.9(4) . . ? C4 C3 C2 119.3(4) . . ? O1 C4 C3 118.8(4) . . ? O1 C4 C5 121.5(4) . . ? C3 C4 C5 119.8(4) . . ? N1 C5 N2 118.3(3) . . ? N1 C5 C4 120.1(4) . . ? N2 C5 C4 121.6(4) . . ? N3 C6 N2 118.3(3) . . ? N3 C6 C7 119.8(4) . . ? N2 C6 C7 121.9(4) . . ? C8 C7 O1 119.2(4) . . ? C8 C7 C6 120.5(4) . . ? O1 C7 C6 120.3(4) . . ? C7 C8 C9 119.0(4) . . ? C10 C9 C8 118.0(4) . . ? N3 C10 C9 123.0(4) . . ? N4 C11 C12 123.1(4) . . ? C11 C12 C13 119.0(4) . . ? C14 C13 C12 118.1(4) . . ? C13 C14 O2 117.8(4) . . ? C13 C14 C15 121.6(4) . . ? O2 C14 C15 120.6(4) . . ? N4 C15 N5 118.7(3) . . ? N4 C15 C14 119.1(4) . . ? N5 C15 C14 122.2(3) . . ? N6 C16 N5 118.3(3) . . ? N6 C16 C17 119.6(3) . . ? N5 C16 C17 122.1(4) . . ? C18 C17 O2 118.0(4) . . ? C18 C17 C16 121.0(4) . . ? O2 C17 C16 120.9(4) . . ? C17 C18 C19 119.0(4) . . ? C20 C19 C18 118.6(4) . . ? N6 C20 C19 122.7(4) . . ? N7 C21 C22 122.6(4) . . ? C21 C22 C23 119.1(4) . . ? C24 C23 C22 118.5(4) . . ? C23 C24 O3 118.5(4) . . ? C23 C24 C25 120.6(4) . . ? O3 C24 C25 120.9(4) . . ? N7 C25 N8 118.8(3) . . ? N7 C25 C24 119.7(4) . . ? N8 C25 C24 121.4(4) . . ? N9 C26 N8 118.6(4) . . ? N9 C26 C27 119.8(4) . . ? N8 C26 C27 121.6(4) . . ? C28 C27 O3 117.9(4) . . ? C28 C27 C26 120.9(4) . . ? O3 C27 C26 121.1(4) . . ? C27 C28 C29 118.2(4) . . ? C30 C29 C28 118.9(4) . . ? C29 C30 N9 123.0(4) . . ? C32 C31 N10 122.7(4) . . ? C31 C32 C33 118.6(4) . . ? C34 C33 C32 118.6(4) . . ? C33 C34 O4 118.7(4) . . ? C33 C34 C35 120.7(4) . . ? O4 C34 C35 120.7(3) . . ? N10 C35 N11 118.2(3) . . ? N10 C35 C34 120.0(3) . . ? N11 C35 C34 121.8(3) . . ? N12 C36 N11 118.5(3) . . ? N12 C36 C37 119.5(3) . . ? N11 C36 C37 122.0(3) . . ? C38 C37 O4 118.6(4) . . ? C38 C37 C36 120.9(4) . . ? O4 C37 C36 120.4(3) . . ? C37 C38 C39 118.8(4) . . ? C40 C39 C38 118.3(4) . . ? N12 C40 C39 122.9(4) . . ? N13 C41 S1 178.6(4) . . ? N14 C42 S2 179.1(4) . . ? C45 O5 C46 116.2(8) . . ? Cl3 C43 Cl2 112.1(3) . . ? Cl3 C43 Cl1 111.3(3) . . ? Cl2 C43 Cl1 109.9(3) . . ? O5 C45 C44 113.1(9) . . ? C47 C46 O5 111.4(10) . . ? C49 O6 C50 105.9(10) . . ? O6 C49 C48 93.9(14) . . ? O6 C50 C51 96.2(14) . . ? C53 O7 C53 142.5(14) 2_665 . ? O7 C53 C52 155(2) 2_665 . ? O7 C53 O7 37.5(14) 2_665 . ? C52 C53 O7 119.6(12) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.298 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.166 # Attachment '- compound 3.cif' data_ic14755 _database_code_depnum_ccdc_archive 'CCDC 832187' #TrackingRef '- compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48.50 H38 Cl7 Co3 N14 O4 S2' _chemical_formula_weight 1369.99 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2548(2) _cell_length_b 13.6957(2) _cell_length_c 16.9851(3) _cell_angle_alpha 109.9557(9) _cell_angle_beta 93.5481(8) _cell_angle_gamma 106.9729(9) _cell_volume 2726.89(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35563 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1382 _exptl_absorpt_coefficient_mu 1.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.814 _exptl_absorpt_process_details ? _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35563 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12459 _reflns_number_gt 7861 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1572P)^2^+4.1623P] 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 12459 _refine_ls_number_parameters 703 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1234 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2652 _refine_ls_wR_factor_gt 0.2328 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 Co1 Co 0.87301(6) 0.77266(6) 0.22743(4) 0.0296(2) Uani 1 1 d . . . Co2 Co 0.76584(5) 0.88903(5) 0.23646(4) 0.0275(2) Uani 1 1 d . . . Co3 Co 0.65766(6) 1.00431(6) 0.24713(5) 0.0314(2) Uani 1 1 d . . . S1 S 1.09593(14) 0.55687(13) 0.24621(11) 0.0465(4) Uani 1 1 d . . . S2 S 0.46116(14) 1.25655(15) 0.28528(11) 0.0492(4) Uani 1 1 d . . . N1 N 0.8723(4) 0.8089(4) 0.3514(3) 0.0306(10) Uani 1 1 d . . . N2 N 0.8047(3) 0.9488(3) 0.3568(3) 0.0281(9) Uani 1 1 d . . . N3 N 0.7351(4) 1.0886(4) 0.3661(3) 0.0322(10) Uani 1 1 d . . . N4 N 0.8576(4) 0.7432(4) 0.1036(3) 0.0360(11) Uani 1 1 d . . . N5 N 0.7275(4) 0.8297(4) 0.1157(3) 0.0326(10) Uani 1 1 d . . . N6 N 0.5940(4) 0.9094(4) 0.1267(3) 0.0366(11) Uani 1 1 d . . . N7 N 0.7374(4) 0.6490(4) 0.2050(3) 0.0341(10) Uani 1 1 d . . . N8 N 0.6453(4) 0.7750(4) 0.2415(3) 0.0323(10) Uani 1 1 d . . . N9 N 0.5534(4) 0.8992(4) 0.2840(3) 0.0347(10) Uani 1 1 d . . . N10 N 0.9995(4) 0.9092(4) 0.2499(3) 0.0312(10) Uani 1 1 d . . . N11 N 0.8843(4) 1.0031(4) 0.2310(3) 0.0314(10) Uani 1 1 d . . . N12 N 0.7728(4) 1.0995(4) 0.2103(3) 0.0348(10) Uani 1 1 d . . . N13 N 0.9683(4) 0.6773(4) 0.2228(3) 0.0390(11) Uani 1 1 d . . . N14 N 0.5641(4) 1.1012(4) 0.2557(3) 0.0427(12) Uani 1 1 d . . . O1 O 0.8630(3) 1.0367(3) 0.5361(2) 0.0377(9) Uani 1 1 d . . . O2 O 0.6717(4) 0.7434(4) -0.0632(3) 0.0510(11) Uani 1 1 d . . . O3 O 0.4658(3) 0.6077(3) 0.2478(3) 0.0432(10) Uani 1 1 d . . . O4 O 1.0624(3) 1.1735(3) 0.2257(3) 0.0461(10) Uani 1 1 d . . . C1 C 0.9009(5) 0.7476(5) 0.3918(4) 0.0359(12) Uani 1 1 d . . . H1 H 0.9116 0.6812 0.3584 0.043 Uiso 1 1 calc R . . C2 C 0.9149(5) 0.7776(5) 0.4778(4) 0.0401(13) Uani 1 1 d . . . H2 H 0.9325 0.7316 0.5035 0.048 Uiso 1 1 calc R . . C3 C 0.9031(5) 0.8762(5) 0.5275(4) 0.0427(14) Uani 1 1 d . . . H3 H 0.9162 0.9010 0.5879 0.051 Uiso 1 1 calc R . . C4 C 0.8722(4) 0.9364(5) 0.4877(3) 0.0328(12) Uani 1 1 d . . . C5 C 0.8497(4) 0.8980(4) 0.3989(3) 0.0291(11) Uani 1 1 d . . . C6 C 0.7863(4) 1.0422(4) 0.4054(3) 0.0305(11) Uani 1 1 d . . . C7 C 0.8213(4) 1.0914(4) 0.4952(3) 0.0320(12) Uani 1 1 d . . . C8 C 0.8150(5) 1.1910(5) 0.5402(4) 0.0381(13) Uani 1 1 d . . . H8 H 0.8404 1.2246 0.6000 0.046 Uiso 1 1 calc R . . C9 C 0.7705(5) 1.2440(5) 0.4978(4) 0.0419(14) Uani 1 1 d . . . H9 H 0.7689 1.3160 0.5276 0.050 Uiso 1 1 calc R . . C10 C 0.7290(5) 1.1901(5) 0.4120(4) 0.0390(13) Uani 1 1 d . . . H10 H 0.6951 1.2244 0.3838 0.047 Uiso 1 1 calc R . . C11 C 0.9130(5) 0.6858(5) 0.0533(4) 0.0435(14) Uani 1 1 d . . . H11 H 0.9691 0.6716 0.0803 0.052 Uiso 1 1 calc R . . C12 C 0.8935(6) 0.6477(5) -0.0322(4) 0.0531(17) Uani 1 1 d . . . H12 H 0.9355 0.6090 -0.0645 0.064 Uiso 1 1 calc R . . C13 C 0.8100(6) 0.6665(6) -0.0723(4) 0.0570(19) Uani 1 1 d . . . H13 H 0.7923 0.6381 -0.1327 0.068 Uiso 1 1 calc R . . C14 C 0.7546(6) 0.7256(5) -0.0243(4) 0.0440(15) Uani 1 1 d . . . C15 C 0.7813(5) 0.7670(5) 0.0658(4) 0.0372(13) Uani 1 1 d . . . C16 C 0.6441(5) 0.8452(5) 0.0768(3) 0.0377(13) Uani 1 1 d . . . C17 C 0.6139(5) 0.7998(5) -0.0120(4) 0.0456(15) Uani 1 1 d . . . C18 C 0.5251(6) 0.8117(6) -0.0509(4) 0.0541(18) Uani 1 1 d . . . H18 H 0.5042 0.7822 -0.1110 0.065 Uiso 1 1 calc R . . C19 C 0.4681(6) 0.8690(6) 0.0023(5) 0.0564(18) Uani 1 1 d . . . H19 H 0.4037 0.8741 -0.0211 0.068 Uiso 1 1 calc R . . C20 C 0.5049(5) 0.9174(5) 0.0878(4) 0.0489(16) Uani 1 1 d . . . H20 H 0.4667 0.9590 0.1223 0.059 Uiso 1 1 calc R . . C21 C 0.7374(5) 0.5432(5) 0.1824(4) 0.0443(15) Uani 1 1 d . . . H21 H 0.8006 0.5277 0.1677 0.053 Uiso 1 1 calc R . . C22 C 0.6510(6) 0.4600(5) 0.1801(5) 0.0571(19) Uani 1 1 d . . . H22 H 0.6536 0.3873 0.1629 0.069 Uiso 1 1 calc R . . C23 C 0.5574(5) 0.4807(5) 0.2029(4) 0.0494(16) Uani 1 1 d . . . H23 H 0.4967 0.4229 0.2030 0.059 Uiso 1 1 calc R . . C24 C 0.5554(5) 0.5852(5) 0.2248(4) 0.0404(13) Uani 1 1 d . . . C25 C 0.6470(4) 0.6700(4) 0.2231(3) 0.0315(12) Uani 1 1 d . . . C26 C 0.5563(4) 0.7967(5) 0.2665(3) 0.0350(12) Uani 1 1 d . . . C27 C 0.4682(5) 0.7158(5) 0.2748(4) 0.0391(13) Uani 1 1 d . . . C28 C 0.3838(5) 0.7412(6) 0.3071(5) 0.0509(16) Uani 1 1 d . . . H28 H 0.3248 0.6864 0.3129 0.061 Uiso 1 1 calc R . . C29 C 0.3864(5) 0.8492(6) 0.3313(5) 0.0552(18) Uani 1 1 d . . . H29 H 0.3304 0.8707 0.3564 0.066 Uiso 1 1 calc R . . C30 C 0.4708(5) 0.9248(5) 0.3184(4) 0.0476(15) Uani 1 1 d . . . H30 H 0.4713 0.9986 0.3345 0.057 Uiso 1 1 calc R . . C31 C 1.1017(4) 0.9080(5) 0.2635(3) 0.0365(12) Uani 1 1 d . . . H31 H 1.1117 0.8455 0.2710 0.044 Uiso 1 1 calc R . . C32 C 1.1897(5) 0.9916(5) 0.2669(4) 0.0440(14) Uani 1 1 d . . . H32 H 1.2594 0.9881 0.2781 0.053 Uiso 1 1 calc R . . C33 C 1.1771(5) 1.0827(5) 0.2540(4) 0.0414(14) Uani 1 1 d . . . H33 H 1.2373 1.1415 0.2547 0.050 Uiso 1 1 calc R . . C34 C 1.0759(5) 1.0849(5) 0.2402(4) 0.0372(13) Uani 1 1 d . . . C35 C 0.9864(4) 0.9989(4) 0.2401(3) 0.0325(12) Uani 1 1 d . . . C36 C 0.8721(5) 1.0923(4) 0.2178(3) 0.0340(12) Uani 1 1 d . . . C37 C 0.9598(5) 1.1760(5) 0.2128(4) 0.0396(13) Uani 1 1 d . . . C38 C 0.9460(6) 1.2635(5) 0.1964(4) 0.0499(16) Uani 1 1 d . . . H38 H 1.0055 1.3209 0.1944 0.060 Uiso 1 1 calc R . . C39 C 0.8418(6) 1.2650(5) 0.1830(4) 0.0521(17) Uani 1 1 d . . . H39 H 0.8285 1.3213 0.1678 0.063 Uiso 1 1 calc R . . C40 C 0.7586(6) 1.1844(5) 0.1919(4) 0.0455(15) Uani 1 1 d . . . H40 H 0.6882 1.1879 0.1850 0.055 Uiso 1 1 calc R . . C41 C 1.0220(5) 0.6259(5) 0.2311(3) 0.0361(13) Uani 1 1 d . . . C42 C 0.5197(4) 1.1648(5) 0.2675(4) 0.0360(13) Uani 1 1 d . . . C43 C 0.407(2) 0.2216(13) 0.4854(11) 0.271(15) Uani 1 1 d D . . H43A H 0.3576 0.2005 0.4316 0.326 Uiso 1 1 calc R . . H43B H 0.4797 0.2585 0.4780 0.326 Uiso 1 1 calc R . . Cl1 Cl 0.4066(2) 0.1069(2) 0.49761(17) 0.0970(8) Uani 1 1 d D . . Cl2 Cl 0.3719(2) 0.3162(2) 0.56289(17) 0.0937(8) Uani 1 1 d D . . C44 C 0.3670(14) 0.4718(14) 0.4055(10) 0.235(12) Uani 1 1 d D . . H44A H 0.4215 0.5160 0.3825 0.282 Uiso 1 1 calc R . . H44B H 0.3916 0.4113 0.4084 0.282 Uiso 1 1 calc R . . Cl3 Cl 0.3695(4) 0.5534(4) 0.5069(3) 0.1637(18) Uani 1 1 d D . . Cl4 Cl 0.2591(5) 0.4168(6) 0.3368(3) 0.225(3) Uani 1 1 d D . . C45 C 0.2848(10) 0.6654(17) 0.0883(9) 0.192(9) Uani 1 1 d D . . H45A H 0.2542 0.6377 0.1314 0.230 Uiso 1 1 calc R . . H45B H 0.3203 0.7461 0.1169 0.230 Uiso 1 1 calc R . . Cl5 Cl 0.3852(4) 0.6039(4) 0.0523(2) 0.1441(14) Uani 1 1 d D . . Cl6 Cl 0.1819(4) 0.6410(4) 0.0108(3) 0.1689(18) Uani 1 1 d D . . C46 C 0.961(2) 0.435(3) 0.3954(12) 0.172(13) Uiso 0.50 1 d PD A 1 H46A H 0.9461 0.3545 0.3774 0.207 Uiso 0.50 1 calc PR A 1 H46B H 1.0133 0.4651 0.3636 0.207 Uiso 0.50 1 calc PR A 1 Cl7 Cl 0.8470(12) 0.4655(12) 0.3854(9) 0.241(3) Uiso 0.50 1 d PD A 1 Cl8 Cl 1.0000 0.5000 0.5000 0.241(3) Uiso 1 2 d SD . 1 C47 C 0.2204(9) 0.9619(9) 0.0403(6) 0.107(4) Uani 1 1 d D . . H47A H 0.2462 0.9652 -0.0119 0.161 Uiso 1 1 calc R . . H47B H 0.2413 0.9068 0.0556 0.161 Uiso 1 1 calc R . . H47C H 0.2519 1.0342 0.0866 0.161 Uiso 1 1 calc R . . C48 C 0.0993(10) 0.9302(7) 0.0257(5) 0.120(5) Uani 1 1 d D . . H48A H 0.0681 0.8585 -0.0226 0.144 Uiso 1 1 calc R . . H48B H 0.0733 0.9208 0.0770 0.144 Uiso 1 1 calc R . . C49 C 0.0604(8) 1.0139(7) 0.0071(6) 0.102(4) Uani 1 1 d D . . H49A H 0.0865 1.0228 -0.0442 0.122 Uiso 1 1 calc R . . H49B H 0.0928 1.0857 0.0552 0.122 Uiso 1 1 calc 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 Co1 0.0342(4) 0.0266(4) 0.0249(4) 0.0080(3) 0.0065(3) 0.0073(3) Co2 0.0320(4) 0.0256(4) 0.0215(4) 0.0083(3) 0.0038(3) 0.0056(3) Co3 0.0338(4) 0.0293(4) 0.0296(4) 0.0121(3) 0.0020(3) 0.0078(3) S1 0.0504(9) 0.0336(8) 0.0505(9) 0.0079(7) 0.0051(7) 0.0172(7) S2 0.0530(10) 0.0550(10) 0.0563(10) 0.0300(8) 0.0200(8) 0.0292(8) N1 0.035(2) 0.029(2) 0.026(2) 0.0091(18) 0.0036(19) 0.010(2) N2 0.033(2) 0.030(2) 0.022(2) 0.0094(18) 0.0050(18) 0.0117(19) N3 0.035(2) 0.031(2) 0.030(2) 0.0125(19) 0.0058(19) 0.009(2) N4 0.043(3) 0.030(2) 0.030(2) 0.0093(19) 0.010(2) 0.008(2) N5 0.041(3) 0.027(2) 0.024(2) 0.0075(18) 0.0022(19) 0.006(2) N6 0.040(3) 0.034(3) 0.032(2) 0.016(2) -0.001(2) 0.005(2) N7 0.040(3) 0.028(2) 0.029(2) 0.0085(19) 0.004(2) 0.008(2) N8 0.032(2) 0.028(2) 0.031(2) 0.0115(19) 0.0030(19) 0.0041(19) N9 0.031(2) 0.039(3) 0.037(3) 0.018(2) 0.005(2) 0.010(2) N10 0.035(2) 0.029(2) 0.026(2) 0.0092(18) 0.0078(19) 0.007(2) N11 0.035(2) 0.030(2) 0.030(2) 0.0130(19) 0.0070(19) 0.009(2) N12 0.046(3) 0.030(2) 0.029(2) 0.0134(19) 0.004(2) 0.010(2) N13 0.042(3) 0.033(3) 0.038(3) 0.010(2) 0.011(2) 0.010(2) N14 0.045(3) 0.036(3) 0.048(3) 0.018(2) 0.002(2) 0.013(2) O1 0.051(2) 0.035(2) 0.0230(19) 0.0073(16) 0.0048(17) 0.0129(19) O2 0.069(3) 0.051(3) 0.025(2) 0.0109(19) 0.001(2) 0.014(2) O3 0.034(2) 0.036(2) 0.053(3) 0.0170(19) 0.0098(19) 0.0011(18) O4 0.042(2) 0.035(2) 0.061(3) 0.023(2) 0.015(2) 0.0064(19) C1 0.041(3) 0.034(3) 0.036(3) 0.016(2) 0.006(2) 0.014(3) C2 0.047(3) 0.044(3) 0.034(3) 0.022(3) 0.005(3) 0.014(3) C3 0.045(3) 0.053(4) 0.027(3) 0.011(3) 0.002(3) 0.017(3) C4 0.034(3) 0.034(3) 0.028(3) 0.011(2) 0.004(2) 0.007(2) C5 0.027(3) 0.027(3) 0.030(3) 0.011(2) 0.005(2) 0.004(2) C6 0.032(3) 0.028(3) 0.027(3) 0.007(2) 0.005(2) 0.008(2) C7 0.034(3) 0.033(3) 0.027(3) 0.009(2) 0.007(2) 0.010(2) C8 0.037(3) 0.037(3) 0.031(3) 0.006(2) 0.006(2) 0.007(3) C9 0.045(3) 0.030(3) 0.040(3) 0.002(2) 0.005(3) 0.011(3) C10 0.043(3) 0.029(3) 0.043(3) 0.010(2) 0.008(3) 0.015(3) C11 0.056(4) 0.037(3) 0.035(3) 0.010(3) 0.019(3) 0.014(3) C12 0.077(5) 0.042(4) 0.038(3) 0.010(3) 0.019(3) 0.020(4) C13 0.087(5) 0.046(4) 0.027(3) 0.007(3) 0.023(3) 0.012(4) C14 0.066(4) 0.031(3) 0.023(3) 0.006(2) 0.009(3) 0.003(3) C15 0.045(3) 0.030(3) 0.028(3) 0.011(2) 0.009(2) 0.000(3) C16 0.046(3) 0.033(3) 0.027(3) 0.013(2) -0.004(2) 0.003(3) C17 0.059(4) 0.035(3) 0.032(3) 0.015(3) -0.001(3) 0.000(3) C18 0.068(5) 0.045(4) 0.036(3) 0.018(3) -0.014(3) 0.002(3) C19 0.058(4) 0.055(4) 0.052(4) 0.021(3) -0.012(3) 0.016(4) C20 0.050(4) 0.039(4) 0.051(4) 0.018(3) -0.008(3) 0.008(3) C21 0.045(3) 0.024(3) 0.054(4) 0.007(3) 0.008(3) 0.009(3) C22 0.053(4) 0.028(3) 0.085(5) 0.017(3) 0.016(4) 0.011(3) C23 0.052(4) 0.028(3) 0.061(4) 0.019(3) 0.006(3) 0.000(3) C24 0.036(3) 0.040(3) 0.043(3) 0.018(3) 0.010(3) 0.007(3) C25 0.038(3) 0.025(3) 0.026(3) 0.011(2) 0.003(2) 0.003(2) C26 0.033(3) 0.039(3) 0.030(3) 0.012(2) 0.001(2) 0.010(2) C27 0.032(3) 0.038(3) 0.045(3) 0.019(3) 0.003(3) 0.006(3) C28 0.039(3) 0.049(4) 0.066(5) 0.028(3) 0.015(3) 0.007(3) C29 0.039(3) 0.061(5) 0.073(5) 0.031(4) 0.023(3) 0.018(3) C30 0.045(4) 0.045(4) 0.061(4) 0.024(3) 0.013(3) 0.020(3) C31 0.037(3) 0.038(3) 0.032(3) 0.012(2) 0.007(2) 0.011(3) C32 0.029(3) 0.051(4) 0.045(4) 0.013(3) 0.007(3) 0.009(3) C33 0.036(3) 0.043(3) 0.037(3) 0.013(3) 0.008(3) 0.003(3) C34 0.041(3) 0.032(3) 0.032(3) 0.009(2) 0.010(2) 0.006(3) C35 0.034(3) 0.032(3) 0.022(2) 0.005(2) 0.005(2) 0.002(2) C36 0.041(3) 0.029(3) 0.027(3) 0.010(2) 0.007(2) 0.006(2) C37 0.048(3) 0.029(3) 0.035(3) 0.013(2) 0.010(3) 0.001(3) C38 0.061(4) 0.037(3) 0.051(4) 0.020(3) 0.018(3) 0.009(3) C39 0.072(5) 0.040(4) 0.057(4) 0.030(3) 0.023(4) 0.019(3) C40 0.055(4) 0.036(3) 0.046(4) 0.019(3) 0.004(3) 0.012(3) C41 0.039(3) 0.033(3) 0.029(3) 0.007(2) 0.007(2) 0.006(3) C42 0.031(3) 0.038(3) 0.034(3) 0.016(2) 0.003(2) 0.004(3) C43 0.54(4) 0.159(15) 0.173(16) 0.094(13) 0.26(2) 0.13(2) Cl1 0.0949(18) 0.0983(19) 0.0761(16) 0.0175(14) 0.0242(13) 0.0175(15) Cl2 0.0984(18) 0.0904(18) 0.0799(16) 0.0336(14) 0.0015(13) 0.0147(14) C44 0.23(2) 0.149(14) 0.22(2) -0.085(13) -0.096(16) 0.125(14) Cl3 0.196(4) 0.158(4) 0.124(3) 0.005(2) -0.005(3) 0.105(3) Cl4 0.203(5) 0.323(7) 0.128(4) 0.014(4) -0.030(3) 0.155(5) C45 0.087(9) 0.37(3) 0.117(12) 0.103(15) 0.001(8) 0.061(13) Cl5 0.168(3) 0.160(3) 0.111(3) 0.071(2) 0.010(2) 0.043(3) Cl6 0.238(5) 0.165(4) 0.179(4) 0.099(3) 0.098(4) 0.123(4) C47 0.128(9) 0.084(7) 0.070(6) 0.012(5) 0.050(6) -0.008(7) C48 0.213(14) 0.049(5) 0.046(5) 0.001(4) 0.052(7) -0.015(7) C49 0.164(10) 0.043(5) 0.053(5) 0.004(4) 0.043(6) -0.017(6) _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 Co1 N7 1.985(5) . ? Co1 N4 1.988(5) . ? Co1 N1 1.993(4) . ? Co1 N10 2.014(4) . ? Co1 N13 2.053(5) . ? Co1 Co2 2.4007(10) . ? Co2 N2 1.897(4) . ? Co2 N11 1.897(4) . ? Co2 N5 1.902(4) . ? Co2 N8 1.910(4) . ? Co2 Co3 2.3959(10) . ? Co3 N6 1.980(5) . ? Co3 N3 1.982(4) . ? Co3 N12 1.983(5) . ? Co3 N9 1.984(5) . ? Co3 N14 2.042(5) . ? S1 C41 1.611(6) . ? S2 C42 1.616(6) . ? N1 C5 1.341(7) . ? N1 C1 1.367(7) . ? N2 C6 1.364(7) . ? N2 C5 1.372(6) . ? N3 C6 1.340(7) . ? N3 C10 1.371(7) . ? N4 C15 1.340(8) . ? N4 C11 1.358(7) . ? N5 C16 1.359(7) . ? N5 C15 1.378(7) . ? N6 C16 1.354(8) . ? N6 C20 1.369(8) . ? N7 C25 1.342(7) . ? N7 C21 1.367(7) . ? N8 C26 1.357(7) . ? N8 C25 1.371(7) . ? N9 C26 1.344(7) . ? N9 C30 1.352(8) . ? N10 C35 1.352(7) . ? N10 C31 1.366(7) . ? N11 C36 1.365(7) . ? N11 C35 1.373(7) . ? N12 C36 1.349(7) . ? N12 C40 1.362(7) . ? N13 C41 1.171(8) . ? N14 C42 1.159(8) . ? O1 C7 1.378(6) . ? O1 C4 1.385(7) . ? O2 C14 1.371(8) . ? O2 C17 1.382(8) . ? O3 C24 1.359(7) . ? O3 C27 1.382(7) . ? O4 C34 1.374(7) . ? O4 C37 1.377(8) . ? C1 C2 1.360(8) . ? C2 C3 1.386(8) . ? C3 C4 1.360(8) . ? C4 C5 1.397(7) . ? C6 C7 1.423(7) . ? C7 C8 1.347(8) . ? C8 C9 1.396(8) . ? C9 C10 1.379(8) . ? C11 C12 1.344(9) . ? C12 C13 1.396(10) . ? C13 C14 1.353(9) . ? C14 C15 1.417(8) . ? C16 C17 1.401(8) . ? C17 C18 1.391(9) . ? C18 C19 1.397(11) . ? C19 C20 1.361(9) . ? C21 C22 1.346(9) . ? C22 C23 1.399(10) . ? C23 C24 1.360(9) . ? C24 C25 1.424(8) . ? C26 C27 1.408(8) . ? C27 C28 1.359(9) . ? C28 C29 1.382(10) . ? C29 C30 1.371(9) . ? C31 C32 1.358(8) . ? C32 C33 1.393(9) . ? C33 C34 1.358(8) . ? C34 C35 1.406(8) . ? C36 C37 1.405(8) . ? C37 C38 1.376(9) . ? C38 C39 1.393(10) . ? C39 C40 1.372(9) . ? C43 Cl1 1.652(13) . ? C43 Cl2 1.698(11) . ? C44 Cl4 1.593(12) . ? C44 Cl3 1.695(13) . ? C45 Cl6 1.708(11) . ? C45 Cl5 1.806(13) . ? C46 Cl8 1.660(18) . ? C46 Cl7 1.693(18) . ? Cl8 C46 1.660(18) 2_766 ? C47 C48 1.515(13) . ? C48 C49 1.501(13) . ? C49 C49 1.52(2) 2_575 ? 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 N7 Co1 N4 89.54(19) . . ? N7 Co1 N1 87.88(18) . . ? N4 Co1 N1 172.58(19) . . ? N7 Co1 N10 173.16(19) . . ? N4 Co1 N10 89.61(18) . . ? N1 Co1 N10 92.12(18) . . ? N7 Co1 N13 93.99(19) . . ? N4 Co1 N13 94.0(2) . . ? N1 Co1 N13 93.16(18) . . ? N10 Co1 N13 92.84(19) . . ? N7 Co1 Co2 87.49(14) . . ? N4 Co1 Co2 87.17(14) . . ? N1 Co1 Co2 85.77(13) . . ? N10 Co1 Co2 85.69(13) . . ? N13 Co1 Co2 178.14(14) . . ? N2 Co2 N11 89.55(19) . . ? N2 Co2 N5 179.7(2) . . ? N11 Co2 N5 90.14(19) . . ? N2 Co2 N8 90.67(19) . . ? N11 Co2 N8 179.25(19) . . ? N5 Co2 N8 89.63(19) . . ? N2 Co2 Co3 89.31(13) . . ? N11 Co2 Co3 89.28(14) . . ? N5 Co2 Co3 90.66(14) . . ? N8 Co2 Co3 90.01(14) . . ? N2 Co2 Co1 90.10(13) . . ? N11 Co2 Co1 91.37(14) . . ? N5 Co2 Co1 89.93(14) . . ? N8 Co2 Co1 89.34(14) . . ? Co3 Co2 Co1 179.12(4) . . ? N6 Co3 N3 172.42(19) . . ? N6 Co3 N12 90.11(19) . . ? N3 Co3 N12 88.56(19) . . ? N6 Co3 N9 89.91(19) . . ? N3 Co3 N9 90.56(19) . . ? N12 Co3 N9 173.46(19) . . ? N6 Co3 N14 93.9(2) . . ? N3 Co3 N14 93.6(2) . . ? N12 Co3 N14 93.1(2) . . ? N9 Co3 N14 93.5(2) . . ? N6 Co3 Co2 85.67(14) . . ? N3 Co3 Co2 86.81(13) . . ? N12 Co3 Co2 87.36(14) . . ? N9 Co3 Co2 86.12(14) . . ? N14 Co3 Co2 179.42(15) . . ? C5 N1 C1 117.7(5) . . ? C5 N1 Co1 121.1(3) . . ? C1 N1 Co1 121.1(4) . . ? C6 N2 C5 117.2(4) . . ? C6 N2 Co2 121.6(3) . . ? C5 N2 Co2 121.2(3) . . ? C6 N3 C10 118.8(5) . . ? C6 N3 Co3 119.8(4) . . ? C10 N3 Co3 121.1(4) . . ? C15 N4 C11 118.0(5) . . ? C15 N4 Co1 120.0(4) . . ? C11 N4 Co1 121.4(4) . . ? C16 N5 C15 118.4(5) . . ? C16 N5 Co2 120.7(4) . . ? C15 N5 Co2 120.9(4) . . ? C16 N6 C20 117.2(5) . . ? C16 N6 Co3 121.5(4) . . ? C20 N6 Co3 120.7(4) . . ? C25 N7 C21 118.7(5) . . ? C25 N7 Co1 120.0(4) . . ? C21 N7 Co1 120.8(4) . . ? C26 N8 C25 117.8(5) . . ? C26 N8 Co2 120.7(4) . . ? C25 N8 Co2 121.5(4) . . ? C26 N9 C30 118.5(5) . . ? C26 N9 Co3 120.6(4) . . ? C30 N9 Co3 120.4(4) . . ? C35 N10 C31 117.8(5) . . ? C35 N10 Co1 121.0(4) . . ? C31 N10 Co1 120.5(4) . . ? C36 N11 C35 117.2(5) . . ? C36 N11 Co2 121.9(4) . . ? C35 N11 Co2 120.9(4) . . ? C36 N12 C40 118.9(5) . . ? C36 N12 Co3 119.2(4) . . ? C40 N12 Co3 120.9(4) . . ? C41 N13 Co1 171.3(5) . . ? C42 N14 Co3 172.7(5) . . ? C7 O1 C4 118.5(4) . . ? C14 O2 C17 118.0(5) . . ? C24 O3 C27 118.5(4) . . ? C34 O4 C37 118.2(5) . . ? C2 C1 N1 122.9(5) . . ? C1 C2 C3 119.1(5) . . ? C4 C3 C2 118.4(5) . . ? C3 C4 O1 119.3(5) . . ? C3 C4 C5 120.6(5) . . ? O1 C4 C5 120.0(5) . . ? N1 C5 N2 117.4(5) . . ? N1 C5 C4 120.5(5) . . ? N2 C5 C4 122.1(5) . . ? N3 C6 N2 118.2(5) . . ? N3 C6 C7 119.9(5) . . ? N2 C6 C7 121.9(5) . . ? C8 C7 O1 119.9(5) . . ? C8 C7 C6 120.7(5) . . ? O1 C7 C6 119.4(5) . . ? C7 C8 C9 119.0(5) . . ? C10 C9 C8 118.9(5) . . ? N3 C10 C9 122.1(5) . . ? C12 C11 N4 124.1(7) . . ? C11 C12 C13 118.3(6) . . ? C14 C13 C12 119.3(6) . . ? C13 C14 O2 119.6(6) . . ? C13 C14 C15 119.9(7) . . ? O2 C14 C15 120.4(6) . . ? N4 C15 N5 119.0(5) . . ? N4 C15 C14 120.3(6) . . ? N5 C15 C14 120.7(6) . . ? N6 C16 N5 117.6(5) . . ? N6 C16 C17 121.2(5) . . ? N5 C16 C17 121.1(6) . . ? O2 C17 C18 118.4(6) . . ? O2 C17 C16 121.1(6) . . ? C18 C17 C16 120.5(6) . . ? C17 C18 C19 117.2(6) . . ? C20 C19 C18 119.8(6) . . ? C19 C20 N6 123.5(7) . . ? C22 C21 N7 122.4(6) . . ? C21 C22 C23 120.1(6) . . ? C24 C23 C22 118.5(6) . . ? O3 C24 C23 119.7(5) . . ? O3 C24 C25 120.6(5) . . ? C23 C24 C25 119.7(6) . . ? N7 C25 N8 118.7(5) . . ? N7 C25 C24 120.5(5) . . ? N8 C25 C24 120.8(5) . . ? N9 C26 N8 118.3(5) . . ? N9 C26 C27 119.6(5) . . ? N8 C26 C27 122.1(5) . . ? C28 C27 O3 119.0(5) . . ? C28 C27 C26 121.3(6) . . ? O3 C27 C26 119.7(5) . . ? C27 C28 C29 118.0(6) . . ? C30 C29 C28 119.2(6) . . ? N9 C30 C29 122.9(6) . . ? C32 C31 N10 123.2(6) . . ? C31 C32 C33 119.5(6) . . ? C34 C33 C32 117.9(6) . . ? C33 C34 O4 118.4(5) . . ? C33 C34 C35 121.4(6) . . ? O4 C34 C35 120.2(5) . . ? N10 C35 N11 118.0(5) . . ? N10 C35 C34 120.1(5) . . ? N11 C35 C34 121.8(5) . . ? N12 C36 N11 118.4(5) . . ? N12 C36 C37 119.8(5) . . ? N11 C36 C37 121.8(5) . . ? C38 C37 O4 118.2(5) . . ? C38 C37 C36 121.2(6) . . ? O4 C37 C36 120.5(5) . . ? C37 C38 C39 117.8(6) . . ? C40 C39 C38 119.4(6) . . ? N12 C40 C39 122.6(6) . . ? N13 C41 S1 177.9(5) . . ? N14 C42 S2 178.2(6) . . ? Cl1 C43 Cl2 118.8(7) . . ? Cl4 C44 Cl3 120.7(10) . . ? Cl6 C45 Cl5 115.4(8) . . ? Cl8 C46 Cl7 98.5(12) . . ? C46 Cl8 C46 180.0(7) . 2_766 ? C49 C48 C47 113.0(8) . . ? C48 C49 C49 114.9(9) . 2_575 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.894 _refine_diff_density_min -1.460 _refine_diff_density_rms 0.165