# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Guang-Xiang Liu' _publ_contact_author_address ;School of Biochemical and Environmental Engineering Nanjing Xiaozhuang University Nanjing 211171 China ; _publ_contact_author_email njuliugx@gmail.com _publ_contact_author_phone 86-25-86178260 _publ_contact_author_fax 86-25-86178260 loop_ _publ_author_name _publ_author_address 'Guang-Xiang Liu' ;School of Biochemical and Environmental Engineering Nanjing Xiaozhuang University Nanjing 211171 China ; 'Heng Xu' ;School of Biochemical and Environmental Engineering Nanjing Xiaozhuang University Nanjing 211171 China ; S.Nishihara ;Department of Physical Science Graduate School of Science Osaka Prefecture University Sakai, Osaka 599-8531 Japan ; 'Xiao-Ming Ren' ;School of Biochemical and Environmental Engineering Nanjing Xiaozhuang University Nanjing 211171 China ; _publ_section_title ; Temperature-induced assembly of MOF polymorphs: Syntheses, structures and physical properties ; # Attachment '- 5-CEC1115.cif' #TrackingRef '- 5-CEC1115.cif' data_cec1 _database_code_depnum_ccdc_archive 'CCDC 771953' #TrackingRef '- 5-CEC1115.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H27 Br Co N6 O4, H2 O' _chemical_formula_sum 'C29 H29 Br Co N6 O5' _chemical_formula_weight 680.42 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' 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' _cell_length_a 19.390(4) _cell_length_b 11.906(3) _cell_length_c 12.766(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2947.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4121 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.01 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 1.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6261 _exptl_absorpt_correction_T_max 0.7822 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14154 _diffrn_reflns_av_R_equivalents 0.0869 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4734 _reflns_number_gt 3633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0712P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(14) _refine_ls_number_reflns 4734 _refine_ls_number_parameters 391 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Co1 Co 0.40732(3) 0.87179(5) 0.78400(5) 0.03645(19) Uani 1 1 d . . . N1 N 0.4164(2) 0.7315(4) 0.6842(4) 0.0426(12) Uani 1 1 d . . . N2 N 0.4079(2) 0.5603(4) 0.6209(4) 0.0378(11) Uani 1 1 d . . . N3 N 0.0120(2) 0.5837(3) 0.7736(4) 0.0398(10) Uani 1 1 d . . . N4 N 0.1021(2) 0.4789(4) 0.7359(4) 0.0394(10) Uani 1 1 d . . . N5 N 0.3936(2) 0.0139(4) 0.8841(4) 0.0409(11) Uani 1 1 d . . . N6 N 0.3573(2) 0.1733(4) 0.9494(3) 0.0392(10) Uani 1 1 d . . . O1 O 0.3029(3) 0.7823(4) 0.8590(4) 0.0699(13) Uani 1 1 d . . . O2 O 0.4083(2) 0.7654(4) 0.9169(4) 0.0641(13) Uani 1 1 d . . . O3 O 0.1127(3) 0.5860(7) 1.0600(7) 0.127(3) Uani 1 1 d . . . O4 O 0.1416(2) 0.4537(4) 1.1691(4) 0.0617(12) Uani 1 1 d . . . O1W O 0.9955(4) 0.2721(5) 0.5803(6) 0.0937(18) Uani 1 1 d D . . Br1 Br 0.41377(4) 0.45493(8) 1.22514(9) 0.0903(3) Uani 1 1 d . . . C1 C 0.4385(3) 0.7303(5) 0.5851(5) 0.0517(16) Uani 1 1 d . . . H1 H 0.4548 0.7927 0.5490 0.062 Uiso 1 1 calc R . . C2 C 0.4340(3) 0.6265(6) 0.5448(5) 0.0541(16) Uani 1 1 d . . . H2 H 0.4465 0.6044 0.4775 0.065 Uiso 1 1 calc R . . C3 C 0.3984(3) 0.6260(5) 0.7036(5) 0.0459(14) Uani 1 1 d . . . H3 H 0.3813 0.6011 0.7675 0.055 Uiso 1 1 calc R . . C4 C 0.0716(3) 0.6401(5) 0.7992(5) 0.0500(16) Uani 1 1 d . . . H4 H 0.0734 0.7113 0.8291 0.060 Uiso 1 1 calc R . . C5 C 0.1266(3) 0.5774(5) 0.7748(5) 0.0493(14) Uani 1 1 d . . . H5 H 0.1726 0.5974 0.7829 0.059 Uiso 1 1 calc R . . C6 C 0.0334(3) 0.4870(4) 0.7340(5) 0.0397(12) Uani 1 1 d . . . H6 H 0.0042 0.4316 0.7081 0.048 Uiso 1 1 calc R . . C7 C 0.4307(3) 0.0386(5) 0.9700(5) 0.0497(15) Uani 1 1 d . . . H7 H 0.4663 -0.0053 0.9964 0.060 Uiso 1 1 calc R . . C8 C 0.4087(3) 0.1364(5) 1.0126(5) 0.0467(15) Uani 1 1 d . . . H8 H 0.4253 0.1711 1.0728 0.056 Uiso 1 1 calc R . . C9 C 0.3489(3) 0.0974(5) 0.8732(4) 0.0397(13) Uani 1 1 d . . . H9 H 0.3162 0.1024 0.8200 0.048 Uiso 1 1 calc R . . C10 C 0.3937(3) 0.4393(5) 0.6148(5) 0.0450(14) Uani 1 1 d . . . H10A H 0.4354 0.3980 0.6315 0.054 Uiso 1 1 calc R . . H10B H 0.3803 0.4201 0.5438 0.054 Uiso 1 1 calc R . . C11 C 0.2520(3) 0.4735(5) 0.5556(5) 0.0552(16) Uani 1 1 d . . . H11A H 0.2512 0.4176 0.5015 0.083 Uiso 1 1 calc R . . H11B H 0.2866 0.5286 0.5399 0.083 Uiso 1 1 calc R . . H11C H 0.2077 0.5093 0.5597 0.083 Uiso 1 1 calc R . . C12 C 0.1419(3) 0.3846(5) 0.6897(5) 0.0489(15) Uani 1 1 d . . . H12A H 0.1413 0.3918 0.6140 0.059 Uiso 1 1 calc R . . H12B H 0.1194 0.3145 0.7076 0.059 Uiso 1 1 calc R . . C13 C 0.1744(3) 0.2952(7) 0.8963(6) 0.076(2) Uani 1 1 d . . . H13A H 0.1874 0.2247 0.9271 0.114 Uiso 1 1 calc R . . H13B H 0.1328 0.2856 0.8564 0.114 Uiso 1 1 calc R . . H13C H 0.1667 0.3495 0.9507 0.114 Uiso 1 1 calc R . . C14 C 0.3189(4) 0.2794(5) 0.9612(5) 0.0516(15) Uani 1 1 d . . . H14A H 0.3467 0.3327 1.0002 0.062 Uiso 1 1 calc R . . H14B H 0.2770 0.2657 1.0009 0.062 Uiso 1 1 calc R . . C15 C 0.4282(3) 0.3565(6) 0.8243(6) 0.064(2) Uani 1 1 d . . . H15A H 0.4456 0.2820 0.8129 0.095 Uiso 1 1 calc R . . H15B H 0.4307 0.3742 0.8975 0.095 Uiso 1 1 calc R . . H15C H 0.4555 0.4092 0.7853 0.095 Uiso 1 1 calc R . . C16 C 0.3369(3) 0.4052(4) 0.6896(4) 0.0399(13) Uani 1 1 d . . . C17 C 0.2684(3) 0.4183(4) 0.6594(5) 0.0409(13) Uani 1 1 d . . . C18 C 0.2156(3) 0.3802(4) 0.7263(5) 0.0432(14) Uani 1 1 d . . . C19 C 0.2316(3) 0.3359(5) 0.8249(5) 0.0464(14) Uani 1 1 d . . . C20 C 0.3005(3) 0.3290(4) 0.8563(4) 0.0419(13) Uani 1 1 d . . . C21 C 0.3537(2) 0.3628(4) 0.7880(5) 0.0409(12) Uani 1 1 d . . . C22 C 0.3445(4) 0.7418(5) 0.9203(5) 0.0507(16) Uani 1 1 d . . . C23 C 0.3211(3) 0.6580(5) 1.0025(5) 0.0430(13) Uani 1 1 d . . . C24 C 0.3695(3) 0.6047(5) 1.0652(5) 0.0483(15) Uani 1 1 d . . . H24 H 0.4163 0.6193 1.0565 0.058 Uiso 1 1 calc R . . C25 C 0.3474(3) 0.5295(4) 1.1406(5) 0.0476(15) Uani 1 1 d . . . C26 C 0.2791(3) 0.5042(4) 1.1542(4) 0.0380(13) Uani 1 1 d . . . H26 H 0.2656 0.4518 1.2042 0.046 Uiso 1 1 calc R . . C27 C 0.2303(3) 0.5578(4) 1.0925(4) 0.0408(13) Uani 1 1 d . . . C28 C 0.2520(3) 0.6346(4) 1.0164(4) 0.0429(14) Uani 1 1 d . . . H28 H 0.2194 0.6705 0.9747 0.051 Uiso 1 1 calc R . . C29 C 0.1543(3) 0.5305(5) 1.1087(5) 0.0512(16) Uani 1 1 d . . . H1WA H 0.962(2) 0.318(4) 0.569(5) 0.05(2) Uiso 1 1 d D . . H1WB H 0.995(3) 0.240(5) 0.518(3) 0.06(2) Uiso 1 1 d 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 Co1 0.0343(3) 0.0314(4) 0.0436(4) 0.0065(4) 0.0012(4) -0.0020(3) N1 0.044(3) 0.040(3) 0.044(3) 0.005(2) 0.001(2) -0.005(2) N2 0.038(3) 0.038(3) 0.036(3) 0.000(2) 0.008(2) -0.002(2) N3 0.037(2) 0.032(2) 0.050(3) 0.001(2) 0.004(2) 0.0022(19) N4 0.036(2) 0.036(3) 0.046(3) -0.006(2) -0.002(2) 0.0027(19) N5 0.046(3) 0.037(3) 0.040(3) 0.004(2) 0.003(2) 0.001(2) N6 0.046(3) 0.036(3) 0.035(3) -0.002(2) 0.000(2) 0.000(2) O1 0.094(4) 0.052(3) 0.064(3) 0.019(2) 0.017(3) 0.003(3) O2 0.088(4) 0.052(3) 0.053(3) 0.004(2) 0.020(2) -0.028(2) O3 0.045(3) 0.190(7) 0.148(6) 0.093(6) -0.002(4) 0.009(4) O4 0.061(3) 0.059(3) 0.065(3) 0.011(2) 0.017(2) -0.017(2) O1W 0.091(4) 0.064(4) 0.126(6) 0.009(4) 0.016(4) 0.000(3) Br1 0.0548(4) 0.0951(7) 0.1212(7) 0.0452(6) -0.0150(5) 0.0007(4) C1 0.055(4) 0.047(4) 0.053(4) 0.012(3) 0.006(3) -0.018(3) C2 0.057(4) 0.060(4) 0.045(4) 0.002(3) 0.007(3) -0.005(3) C3 0.058(4) 0.037(3) 0.042(3) 0.001(3) 0.012(3) -0.004(3) C4 0.051(3) 0.038(3) 0.061(4) -0.020(3) -0.005(3) -0.002(3) C5 0.031(3) 0.053(3) 0.064(4) -0.009(3) -0.007(3) 0.000(3) C6 0.034(3) 0.035(3) 0.050(3) -0.002(3) -0.001(3) -0.002(2) C7 0.052(4) 0.042(3) 0.056(4) 0.007(3) -0.005(3) 0.006(3) C8 0.052(4) 0.048(4) 0.041(4) 0.006(3) -0.002(3) -0.003(3) C9 0.038(3) 0.042(3) 0.040(3) 0.003(3) 0.001(2) 0.001(3) C10 0.048(3) 0.033(3) 0.053(4) -0.010(3) 0.011(3) 0.004(3) C11 0.052(4) 0.062(4) 0.051(4) 0.004(3) -0.010(3) 0.002(3) C12 0.038(3) 0.041(3) 0.068(4) -0.012(3) 0.003(3) 0.009(2) C13 0.052(4) 0.085(5) 0.091(6) 0.028(5) 0.015(4) 0.005(4) C14 0.069(4) 0.043(3) 0.043(4) 0.000(3) 0.000(3) 0.015(3) C15 0.051(4) 0.055(4) 0.085(6) 0.013(4) -0.013(3) 0.002(3) C16 0.038(3) 0.027(3) 0.054(4) -0.008(3) -0.001(3) 0.003(2) C17 0.047(3) 0.025(3) 0.051(3) -0.006(3) -0.002(3) 0.008(2) C18 0.043(3) 0.027(3) 0.060(4) -0.011(3) 0.001(3) 0.006(2) C19 0.043(3) 0.034(3) 0.062(4) 0.000(3) 0.005(3) 0.005(3) C20 0.052(3) 0.024(3) 0.050(3) -0.003(3) -0.003(3) 0.006(2) C21 0.040(3) 0.029(3) 0.054(3) -0.009(3) -0.001(3) 0.003(2) C22 0.075(4) 0.033(3) 0.044(4) -0.004(3) 0.024(4) -0.010(3) C23 0.061(3) 0.032(3) 0.037(3) 0.001(2) 0.014(3) -0.005(3) C24 0.042(3) 0.039(3) 0.063(4) -0.003(3) 0.011(3) -0.007(3) C25 0.052(4) 0.034(3) 0.056(4) 0.010(3) -0.001(3) 0.001(3) C26 0.045(3) 0.029(3) 0.041(3) 0.005(2) 0.005(2) -0.005(2) C27 0.051(3) 0.035(3) 0.036(3) 0.001(2) 0.003(3) 0.000(2) C28 0.053(4) 0.036(3) 0.039(3) 0.009(3) 0.008(3) 0.003(3) C29 0.048(4) 0.056(4) 0.050(4) 0.007(3) 0.003(3) -0.002(3) _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 O4 2.000(4) 4_554 ? Co1 N3 2.102(4) 3_565 ? Co1 N1 2.108(5) . ? Co1 O2 2.117(5) . ? Co1 N5 2.138(5) 1_565 ? N1 C3 1.327(7) . ? N1 C1 1.336(8) . ? N2 C3 1.327(7) . ? N2 C2 1.350(8) . ? N2 C10 1.468(7) . ? N3 C6 1.324(7) . ? N3 C4 1.376(7) . ? N3 Co1 2.102(4) 3_465 ? N4 C6 1.337(6) . ? N4 C5 1.359(7) . ? N4 C12 1.483(7) . ? N5 C9 1.326(7) . ? N5 C7 1.344(8) . ? N5 Co1 2.138(5) 1_545 ? N6 C9 1.337(7) . ? N6 C8 1.355(7) . ? N6 C14 1.475(7) . ? O1 C22 1.224(8) . ? O2 C22 1.267(7) . ? O3 C29 1.214(8) . ? O4 C29 1.222(7) . ? O4 Co1 2.000(4) 4_545 ? O1W H1WA 0.87(2) . ? O1W H1WB 0.89(2) . ? Br1 C25 1.900(6) . ? C1 C2 1.341(9) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.337(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.355(9) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C16 1.513(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C17 1.513(8) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C18 1.505(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C19 1.516(9) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C20 1.507(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C21 1.519(8) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.392(8) . ? C16 C21 1.393(8) . ? C17 C18 1.408(8) . ? C18 C19 1.400(9) . ? C19 C20 1.397(8) . ? C20 C21 1.410(8) . ? C22 C23 1.517(8) . ? C23 C28 1.380(8) . ? C23 C24 1.387(9) . ? C24 C25 1.382(8) . ? C24 H24 0.9300 . ? C25 C26 1.370(8) . ? C26 C27 1.386(8) . ? C26 H26 0.9300 . ? C27 C28 1.399(7) . ? C27 C29 1.523(8) . ? C28 H28 0.9300 . ? 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 O4 Co1 N3 106.77(19) 4_554 3_565 ? O4 Co1 N1 89.01(18) 4_554 . ? N3 Co1 N1 94.63(17) 3_565 . ? O4 Co1 O2 152.02(19) 4_554 . ? N3 Co1 O2 101.15(18) 3_565 . ? N1 Co1 O2 90.55(19) . . ? O4 Co1 N5 89.62(18) 4_554 1_565 ? N3 Co1 N5 87.63(17) 3_565 1_565 ? N1 Co1 N5 177.62(17) . 1_565 ? O2 Co1 N5 89.74(18) . 1_565 ? C3 N1 C1 104.5(5) . . ? C3 N1 Co1 128.0(4) . . ? C1 N1 Co1 127.5(4) . . ? C3 N2 C2 106.3(5) . . ? C3 N2 C10 126.5(5) . . ? C2 N2 C10 127.2(5) . . ? C6 N3 C4 104.6(4) . . ? C6 N3 Co1 123.1(3) . 3_465 ? C4 N3 Co1 132.3(4) . 3_465 ? C6 N4 C5 107.0(4) . . ? C6 N4 C12 124.4(4) . . ? C5 N4 C12 128.1(4) . . ? C9 N5 C7 105.8(5) . . ? C9 N5 Co1 127.7(4) . 1_545 ? C7 N5 Co1 126.4(4) . 1_545 ? C9 N6 C8 107.7(5) . . ? C9 N6 C14 126.3(5) . . ? C8 N6 C14 126.0(5) . . ? C22 O2 Co1 98.7(4) . . ? C29 O4 Co1 157.5(4) . 4_545 ? H1WA O1W H1WB 96(7) . . ? N1 C1 C2 110.7(5) . . ? N1 C1 H1 124.7 . . ? C2 C1 H1 124.7 . . ? C1 C2 N2 106.6(6) . . ? C1 C2 H2 126.7 . . ? N2 C2 H2 126.7 . . ? N2 C3 N1 111.9(5) . . ? N2 C3 H3 124.0 . . ? N1 C3 H3 124.0 . . ? C5 C4 N3 110.0(5) . . ? C5 C4 H4 125.0 . . ? N3 C4 H4 125.0 . . ? C4 C5 N4 106.8(5) . . ? C4 C5 H5 126.6 . . ? N4 C5 H5 126.6 . . ? N3 C6 N4 111.6(5) . . ? N3 C6 H6 124.2 . . ? N4 C6 H6 124.2 . . ? N5 C7 C8 110.3(5) . . ? N5 C7 H7 124.9 . . ? C8 C7 H7 124.9 . . ? C7 C8 N6 105.7(6) . . ? C7 C8 H8 127.2 . . ? N6 C8 H8 127.2 . . ? N5 C9 N6 110.5(5) . . ? N5 C9 H9 124.8 . . ? N6 C9 H9 124.8 . . ? N2 C10 C16 111.5(4) . . ? N2 C10 H10A 109.3 . . ? C16 C10 H10A 109.3 . . ? N2 C10 H10B 109.3 . . ? C16 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C17 C11 H11A 109.5 . . ? C17 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C17 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C18 113.4(5) . . ? N4 C12 H12A 108.9 . . ? C18 C12 H12A 108.9 . . ? N4 C12 H12B 108.9 . . ? C18 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C19 C13 H13A 109.5 . . ? C19 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C19 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N6 C14 C20 111.3(5) . . ? N6 C14 H14A 109.4 . . ? C20 C14 H14A 109.4 . . ? N6 C14 H14B 109.4 . . ? C20 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C21 C15 H15A 109.5 . . ? C21 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C21 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 120.9(5) . . ? C17 C16 C10 119.3(5) . . ? C21 C16 C10 119.8(5) . . ? C16 C17 C18 119.3(5) . . ? C16 C17 C11 119.4(5) . . ? C18 C17 C11 121.2(5) . . ? C19 C18 C17 120.4(5) . . ? C19 C18 C12 120.2(6) . . ? C17 C18 C12 119.4(6) . . ? C20 C19 C18 119.5(5) . . ? C20 C19 C13 120.6(6) . . ? C18 C19 C13 120.0(5) . . ? C19 C20 C21 120.4(5) . . ? C19 C20 C14 120.3(6) . . ? C21 C20 C14 119.2(5) . . ? C16 C21 C20 119.3(5) . . ? C16 C21 C15 121.0(5) . . ? C20 C21 C15 119.6(6) . . ? O1 C22 O2 122.3(6) . . ? O1 C22 C23 120.3(6) . . ? O2 C22 C23 117.4(6) . . ? C28 C23 C24 119.3(5) . . ? C28 C23 C22 120.8(6) . . ? C24 C23 C22 119.8(5) . . ? C25 C24 C23 119.2(6) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C26 C25 C24 122.1(6) . . ? C26 C25 Br1 118.7(4) . . ? C24 C25 Br1 119.2(5) . . ? C25 C26 C27 119.1(5) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C26 C27 C28 119.4(5) . . ? C26 C27 C29 119.0(5) . . ? C28 C27 C29 121.6(5) . . ? C23 C28 C27 120.9(5) . . ? C23 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? O3 C29 O4 126.6(6) . . ? O3 C29 C27 117.3(6) . . ? O4 C29 C27 116.1(6) . . ? 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 O4 Co1 N1 C3 -127.9(5) 4_554 . . . ? N3 Co1 N1 C3 125.4(5) 3_565 . . . ? O2 Co1 N1 C3 24.1(5) . . . . ? N5 Co1 N1 C3 -73(5) 1_565 . . . ? O4 Co1 N1 C1 48.4(5) 4_554 . . . ? N3 Co1 N1 C1 -58.3(5) 3_565 . . . ? O2 Co1 N1 C1 -159.5(5) . . . . ? N5 Co1 N1 C1 103(4) 1_565 . . . ? O4 Co1 O2 C22 3.2(6) 4_554 . . . ? N3 Co1 O2 C22 179.5(4) 3_565 . . . ? N1 Co1 O2 C22 -85.7(4) . . . . ? N5 Co1 O2 C22 91.9(4) 1_565 . . . ? C3 N1 C1 C2 0.1(7) . . . . ? Co1 N1 C1 C2 -176.9(4) . . . . ? N1 C1 C2 N2 0.4(8) . . . . ? C3 N2 C2 C1 -0.7(7) . . . . ? C10 N2 C2 C1 -179.6(5) . . . . ? C2 N2 C3 N1 0.8(7) . . . . ? C10 N2 C3 N1 179.7(5) . . . . ? C1 N1 C3 N2 -0.5(7) . . . . ? Co1 N1 C3 N2 176.5(3) . . . . ? C6 N3 C4 C5 0.1(7) . . . . ? Co1 N3 C4 C5 -178.0(4) 3_465 . . . ? N3 C4 C5 N4 -1.6(8) . . . . ? C6 N4 C5 C4 2.5(7) . . . . ? C12 N4 C5 C4 174.6(6) . . . . ? C4 N3 C6 N4 1.5(7) . . . . ? Co1 N3 C6 N4 179.8(4) 3_465 . . . ? C5 N4 C6 N3 -2.6(7) . . . . ? C12 N4 C6 N3 -175.1(5) . . . . ? C9 N5 C7 C8 0.5(7) . . . . ? Co1 N5 C7 C8 178.5(4) 1_545 . . . ? N5 C7 C8 N6 -1.1(7) . . . . ? C9 N6 C8 C7 1.2(6) . . . . ? C14 N6 C8 C7 -177.4(5) . . . . ? C7 N5 C9 N6 0.3(6) . . . . ? Co1 N5 C9 N6 -177.7(3) 1_545 . . . ? C8 N6 C9 N5 -0.9(6) . . . . ? C14 N6 C9 N5 177.7(5) . . . . ? C3 N2 C10 C16 27.8(8) . . . . ? C2 N2 C10 C16 -153.5(6) . . . . ? C6 N4 C12 C18 -164.9(6) . . . . ? C5 N4 C12 C18 24.2(9) . . . . ? C9 N6 C14 C20 -33.5(8) . . . . ? C8 N6 C14 C20 144.9(5) . . . . ? N2 C10 C16 C17 83.1(6) . . . . ? N2 C10 C16 C21 -95.8(6) . . . . ? C21 C16 C17 C18 -4.9(8) . . . . ? C10 C16 C17 C18 176.1(5) . . . . ? C21 C16 C17 C11 175.0(5) . . . . ? C10 C16 C17 C11 -4.0(8) . . . . ? C16 C17 C18 C19 4.0(8) . . . . ? C11 C17 C18 C19 -175.9(5) . . . . ? C16 C17 C18 C12 -174.4(5) . . . . ? C11 C17 C18 C12 5.7(8) . . . . ? N4 C12 C18 C19 78.6(6) . . . . ? N4 C12 C18 C17 -103.0(6) . . . . ? C17 C18 C19 C20 -0.5(8) . . . . ? C12 C18 C19 C20 177.9(5) . . . . ? C17 C18 C19 C13 179.9(6) . . . . ? C12 C18 C19 C13 -1.7(8) . . . . ? C18 C19 C20 C21 -2.1(8) . . . . ? C13 C19 C20 C21 177.5(6) . . . . ? C18 C19 C20 C14 -178.8(5) . . . . ? C13 C19 C20 C14 0.8(9) . . . . ? N6 C14 C20 C19 113.5(6) . . . . ? N6 C14 C20 C21 -63.2(7) . . . . ? C17 C16 C21 C20 2.4(7) . . . . ? C10 C16 C21 C20 -178.7(5) . . . . ? C17 C16 C21 C15 -175.4(5) . . . . ? C10 C16 C21 C15 3.6(7) . . . . ? C19 C20 C21 C16 1.2(8) . . . . ? C14 C20 C21 C16 177.9(5) . . . . ? C19 C20 C21 C15 179.0(5) . . . . ? C14 C20 C21 C15 -4.3(8) . . . . ? Co1 O2 C22 O1 -2.5(7) . . . . ? Co1 O2 C22 C23 175.9(4) . . . . ? O1 C22 C23 C28 -6.6(9) . . . . ? O2 C22 C23 C28 175.0(5) . . . . ? O1 C22 C23 C24 173.9(6) . . . . ? O2 C22 C23 C24 -4.5(8) . . . . ? C28 C23 C24 C25 -0.3(9) . . . . ? C22 C23 C24 C25 179.2(5) . . . . ? C23 C24 C25 C26 1.3(9) . . . . ? C23 C24 C25 Br1 179.2(4) . . . . ? C24 C25 C26 C27 -1.8(9) . . . . ? Br1 C25 C26 C27 -179.7(4) . . . . ? C25 C26 C27 C28 1.2(8) . . . . ? C25 C26 C27 C29 -179.3(5) . . . . ? C24 C23 C28 C27 -0.2(8) . . . . ? C22 C23 C28 C27 -179.7(5) . . . . ? C26 C27 C28 C23 -0.3(8) . . . . ? C29 C27 C28 C23 -179.7(5) . . . . ? Co1 O4 C29 O3 -42.8(17) 4_545 . . . ? Co1 O4 C29 C27 137.9(9) 4_545 . . . ? C26 C27 C29 O3 173.6(7) . . . . ? C28 C27 C29 O3 -7.0(10) . . . . ? C26 C27 C29 O4 -7.0(8) . . . . ? C28 C27 C29 O4 172.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.434 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.090 #====================================# data_cec2 _database_code_depnum_ccdc_archive 'CCDC 771954' #TrackingRef '- 5-CEC1115.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H57 Br3 Co3 N12 O12, 0.73(H2 O)' _chemical_formula_sum 'C66 H58.46 Br3 Co3 N12 O12.73' _chemical_formula_weight 1639.85 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3734(13) _cell_length_b 16.6806(16) _cell_length_c 16.8150(15) _cell_angle_alpha 111.6570(10) _cell_angle_beta 97.4360(10) _cell_angle_gamma 102.7300(10) _cell_volume 3307.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5043 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.47 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1649 _exptl_absorpt_coefficient_mu 2.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5711 _exptl_absorpt_correction_T_max 0.6215 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16523 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11426 _reflns_number_gt 7993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0674P)^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 11426 _refine_ls_number_parameters 881 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _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 Co1 Co 0.20523(4) 0.98206(4) 0.78885(4) 0.03739(15) Uani 1 1 d . . . Co2 Co -0.26179(5) 0.53931(4) 0.92128(4) 0.04349(17) Uani 1 1 d . . . Co3 Co 0.64235(4) 1.29295(4) 0.46587(4) 0.03732(16) Uani 1 1 d . . . N1 N -0.3202(3) 0.4048(2) 0.8573(2) 0.0441(9) Uani 1 1 d . . . N2 N -0.3284(3) 0.2627(2) 0.7851(2) 0.0420(9) Uani 1 1 d . . . N3 N 0.0420(3) 0.1435(2) 0.9350(2) 0.0422(9) Uani 1 1 d . . . N4 N 0.1486(3) 0.0752(2) 0.8663(2) 0.0427(9) Uani 1 1 d . . . N5 N -0.4965(3) -0.0309(3) 0.8569(3) 0.0503(10) Uani 1 1 d . . . N6 N -0.6527(3) -0.0101(3) 0.8550(2) 0.0454(9) Uani 1 1 d . . . N7 N 0.7796(3) 1.2738(2) 0.5134(2) 0.0438(9) Uani 1 1 d . . . N8 N 0.9248(3) 1.2327(2) 0.5273(2) 0.0412(9) Uani 1 1 d . . . N9 N 1.2842(3) 1.3879(3) 0.8195(2) 0.0471(9) Uani 1 1 d . . . N10 N 1.2437(3) 1.4331(3) 0.9490(2) 0.0477(9) Uani 1 1 d . . . N11 N 1.3228(3) 1.4306(3) 0.4384(3) 0.0496(10) Uani 1 1 d . . . N12 N 1.3350(3) 1.5721(2) 0.4636(2) 0.0452(9) Uani 1 1 d . . . O1 O 0.1322(3) 0.8541(2) 0.7493(2) 0.0598(9) Uani 1 1 d . . . O2 O 0.0175(3) 0.8625(2) 0.8346(2) 0.0722(11) Uani 1 1 d . . . O3 O -0.1358(3) 0.5920(2) 0.8883(2) 0.0647(10) Uani 1 1 d . . . O4 O -0.0671(3) 0.4775(3) 0.8435(3) 0.0869(13) Uani 1 1 d . . . O5 O 0.2087(2) 0.9896(2) 0.6756(2) 0.0505(8) Uani 1 1 d . . . O6 O 0.3323(3) 1.1183(2) 0.7590(2) 0.0556(8) Uani 1 1 d . . . O7 O 0.5119(2) 1.2042(2) 0.4546(2) 0.0540(8) Uani 1 1 d . . . O8 O 0.5676(3) 1.2533(2) 0.5984(2) 0.0611(9) Uani 1 1 d . . . O9 O 0.6545(2) 1.2659(2) 0.34059(19) 0.0467(7) Uani 1 1 d . . . O10 O 0.5162(3) 1.3163(2) 0.3552(2) 0.0648(10) Uani 1 1 d . . . O11 O 0.3421(3) 1.3882(3) 0.1152(3) 0.0742(11) Uani 1 1 d . . . O12 O 0.4636(3) 1.4599(3) 0.0687(3) 0.0887(13) Uani 1 1 d . . . O1W O 0.7666(7) 0.7713(6) 0.8167(6) 0.171(6) Uani 0.728(16) 1 d P . . H1WA H 0.8302 0.7778 0.8124 0.256 Uiso 0.728(16) 1 d PR . . H1WB H 0.7495 0.7294 0.8340 0.256 Uiso 0.728(16) 1 d PR . . Br1 Br 0.14778(7) 0.51048(5) 0.60760(6) 0.1250(4) Uani 1 1 d . . . Br2 Br 0.10722(4) 0.99838(4) 0.35651(3) 0.06701(18) Uani 1 1 d . . . Br3 Br 0.74910(4) 1.26576(4) 0.03508(4) 0.07218(19) Uani 1 1 d . . . C1 C 0.0670(4) 0.8210(3) 0.7854(3) 0.0493(12) Uani 1 1 d . . . C2 C 0.0506(3) 0.7223(3) 0.7640(3) 0.0397(10) Uani 1 1 d . . . C3 C 0.0973(4) 0.6706(3) 0.7033(3) 0.0502(12) Uani 1 1 d . . . H3 H 0.1371 0.6956 0.6723 0.060 Uiso 1 1 calc R . . C4 C 0.0840(4) 0.5823(3) 0.6898(4) 0.0629(14) Uani 1 1 d . . . C5 C 0.0286(4) 0.5444(3) 0.7367(4) 0.0644(15) Uani 1 1 d . . . H5 H 0.0235 0.4852 0.7284 0.077 Uiso 1 1 calc R . . C6 C -0.0191(3) 0.5944(3) 0.7959(3) 0.0442(11) Uani 1 1 d . . . C7 C -0.0095(3) 0.6823(3) 0.8078(3) 0.0397(10) Uani 1 1 d . . . H7 H -0.0443 0.7155 0.8461 0.048 Uiso 1 1 calc R . . C8 C -0.0786(4) 0.5501(3) 0.8458(3) 0.0546(12) Uani 1 1 d . . . C9 C 0.2786(4) 1.0613(3) 0.6862(3) 0.0429(11) Uani 1 1 d . . . C10 C 0.2921(3) 1.0760(3) 0.6047(3) 0.0382(10) Uani 1 1 d . . . C11 C 0.2112(3) 1.0344(3) 0.5304(3) 0.0432(11) Uani 1 1 d . . . H11 H 0.1491 0.9955 0.5296 0.052 Uiso 1 1 calc R . . C12 C 0.2230(3) 1.0510(3) 0.4572(3) 0.0443(11) Uani 1 1 d . . . C13 C 0.3156(3) 1.1049(3) 0.4543(3) 0.0414(10) Uani 1 1 d . . . H13 H 0.3228 1.1135 0.4036 0.050 Uiso 1 1 calc R . . C14 C 0.3984(3) 1.1462(3) 0.5293(3) 0.0371(10) Uani 1 1 d . . . C15 C 0.3858(3) 1.1332(3) 0.6048(3) 0.0394(10) Uani 1 1 d . . . H15 H 0.4398 1.1625 0.6555 0.047 Uiso 1 1 calc R . . C16 C 0.5006(3) 1.2053(3) 0.5294(3) 0.0400(10) Uani 1 1 d . . . C17 C 0.5808(4) 1.2931(3) 0.3124(3) 0.0447(11) Uani 1 1 d . . . C18 C 0.5766(3) 1.3019(3) 0.2263(3) 0.0397(10) Uani 1 1 d . . . C19 C 0.6503(3) 1.2794(3) 0.1771(3) 0.0423(10) Uani 1 1 d . . . H19 H 0.6990 1.2530 0.1937 0.051 Uiso 1 1 calc R . . C20 C 0.6492(4) 1.2970(3) 0.1037(3) 0.0468(11) Uani 1 1 d . . . C21 C 0.5813(4) 1.3379(3) 0.0784(3) 0.0526(12) Uani 1 1 d . . . H21 H 0.5856 1.3524 0.0304 0.063 Uiso 1 1 calc R . . C22 C 0.5058(4) 1.3575(3) 0.1257(3) 0.0475(11) Uani 1 1 d . . . C23 C 0.5029(3) 1.3378(3) 0.1983(3) 0.0438(11) Uani 1 1 d . . . H23 H 0.4506 1.3489 0.2287 0.053 Uiso 1 1 calc R . . C24 C 0.4325(4) 1.4046(4) 0.1004(3) 0.0600(13) Uani 1 1 d . . . C25 C -0.2744(3) 0.3492(3) 0.8087(3) 0.0434(11) Uani 1 1 d . . . H25 H -0.2123 0.3674 0.7925 0.052 Uiso 1 1 calc R . . C26 C -0.4090(3) 0.3508(3) 0.8652(3) 0.0433(11) Uani 1 1 d . . . H26 H -0.4575 0.3714 0.8962 0.052 Uiso 1 1 calc R . . C27 C -0.4146(3) 0.2639(3) 0.8210(3) 0.0460(11) Uani 1 1 d . . . H27 H -0.4671 0.2140 0.8158 0.055 Uiso 1 1 calc R . . C28 C 0.0515(3) 0.0664(3) 0.8798(3) 0.0398(10) Uani 1 1 d . . . H28 H -0.0030 0.0127 0.8537 0.048 Uiso 1 1 calc R . . C29 C 0.2023(4) 0.1639(3) 0.9178(4) 0.0721(17) Uani 1 1 d . . . H29 H 0.2725 0.1909 0.9218 0.086 Uiso 1 1 calc R . . C30 C 0.1393(4) 0.2058(3) 0.9613(4) 0.0761(18) Uani 1 1 d . . . H30 H 0.1576 0.2656 1.0016 0.091 Uiso 1 1 calc R . . C31 C -0.5984(3) -0.0640(3) 0.8160(3) 0.0495(12) Uani 1 1 d . . . H31 H -0.6274 -0.1180 0.7665 0.059 Uiso 1 1 calc R . . C32 C -0.5807(4) 0.0608(3) 0.9254(3) 0.0543(12) Uani 1 1 d . . . H32 H -0.5960 0.1097 0.9655 0.065 Uiso 1 1 calc R . . C33 C -0.4843(4) 0.0481(3) 0.9270(3) 0.0557(13) Uani 1 1 d . . . H33 H -0.4219 0.0858 0.9678 0.067 Uiso 1 1 calc R . . C34 C -0.2984(4) 0.1841(3) 0.7298(3) 0.0505(12) Uani 1 1 d . . . H34A H -0.2386 0.2046 0.7080 0.061 Uiso 1 1 calc R . . H34B H -0.3565 0.1455 0.6796 0.061 Uiso 1 1 calc R . . C35 C -0.0916(4) 0.2468(3) 0.8501(4) 0.0619(14) Uani 1 1 d . . . H35A H -0.1009 0.2989 0.8945 0.093 Uiso 1 1 calc R . . H35B H -0.0997 0.2525 0.7950 0.093 Uiso 1 1 calc R . . H35C H -0.0223 0.2423 0.8666 0.093 Uiso 1 1 calc R . . C36 C -0.0514(3) 0.1612(3) 0.9668(3) 0.0479(11) Uani 1 1 d . . . H36A H -0.0400 0.2258 0.9943 0.058 Uiso 1 1 calc R . . H36B H -0.0603 0.1381 1.0114 0.058 Uiso 1 1 calc R . . C37 C -0.2013(4) -0.0053(4) 0.9472(4) 0.0700(16) Uani 1 1 d . . . H37A H -0.1265 0.0059 0.9636 0.105 Uiso 1 1 calc R . . H37B H -0.2347 -0.0690 0.9168 0.105 Uiso 1 1 calc R . . H37C H -0.2273 0.0183 0.9991 0.105 Uiso 1 1 calc R . . C38 C -0.4091(3) -0.0674(3) 0.8248(4) 0.0602(14) Uani 1 1 d . . . H38A H -0.4356 -0.1140 0.7654 0.072 Uiso 1 1 calc R . . H38B H -0.3820 -0.0938 0.8624 0.072 Uiso 1 1 calc R . . C39 C -0.4496(4) 0.0142(3) 0.7035(3) 0.0563(13) Uani 1 1 d . . . H39A H -0.4997 0.0427 0.7288 0.084 Uiso 1 1 calc R . . H39B H -0.4755 -0.0496 0.6860 0.084 Uiso 1 1 calc R . . H39C H -0.4394 0.0261 0.6529 0.084 Uiso 1 1 calc R . . C40 C -0.2701(3) 0.1303(3) 0.7805(3) 0.0409(10) Uani 1 1 d . . . C41 C -0.1733(3) 0.1630(3) 0.8408(3) 0.0394(10) Uani 1 1 d . . . C42 C -0.1517(3) 0.1188(3) 0.8945(3) 0.0393(10) Uani 1 1 d . . . C43 C -0.2259(3) 0.0409(3) 0.8871(3) 0.0423(10) Uani 1 1 d . . . C44 C -0.3223(3) 0.0091(3) 0.8265(3) 0.0450(11) Uani 1 1 d . . . C45 C -0.3442(3) 0.0518(3) 0.7716(3) 0.0434(11) Uani 1 1 d . . . C46 C 0.8362(3) 1.2229(3) 0.4736(3) 0.0430(11) Uani 1 1 d . . . H46 H 0.8164 1.1843 0.4142 0.052 Uiso 1 1 calc R . . C47 C 0.8356(5) 1.3182(4) 0.5997(4) 0.0801(19) Uani 1 1 d . . . H47 H 0.8150 1.3585 0.6449 0.096 Uiso 1 1 calc R . . C48 C 0.9253(5) 1.2939(4) 0.6086(3) 0.0802(19) Uani 1 1 d . . . H48 H 0.9773 1.3149 0.6599 0.096 Uiso 1 1 calc R . . C49 C 1.2958(4) 1.3851(3) 0.8980(3) 0.0521(12) Uani 1 1 d . . . H49 H 1.3361 1.3530 0.9154 0.063 Uiso 1 1 calc R . . C50 C 1.1967(5) 1.4683(4) 0.8989(4) 0.0785(18) Uani 1 1 d . . . H50 H 1.1533 1.5050 0.9164 0.094 Uiso 1 1 calc R . . C51 C 1.2221(5) 1.4422(4) 0.8201(4) 0.0816(19) Uani 1 1 d . . . H51 H 1.2011 1.4584 0.7747 0.098 Uiso 1 1 calc R . . C52 C 1.3450(4) 1.5144(3) 0.4988(3) 0.0478(12) Uani 1 1 d . . . H52 H 1.3652 1.5306 0.5589 0.057 Uiso 1 1 calc R . . C53 C 1.3066(4) 1.5210(3) 0.3741(3) 0.0559(12) Uani 1 1 d . . . H53 H 1.2943 1.5429 0.3314 0.067 Uiso 1 1 calc R . . C54 C 1.2996(4) 1.4342(4) 0.3579(4) 0.0610(14) Uani 1 1 d . . . H54 H 1.2823 1.3862 0.3030 0.073 Uiso 1 1 calc R . . C55 C 1.0036(3) 1.1838(3) 0.5069(3) 0.0457(11) Uani 1 1 d . . . H55A H 0.9909 1.1520 0.4436 0.055 Uiso 1 1 calc R . . H55B H 0.9945 1.1390 0.5314 0.055 Uiso 1 1 calc R . . C56 C 1.1250(4) 1.2177(3) 0.6818(3) 0.0560(13) Uani 1 1 d . . . H56A H 1.1804 1.2129 0.7206 0.084 Uiso 1 1 calc R . . H56B H 1.0787 1.1586 0.6446 0.084 Uiso 1 1 calc R . . H56C H 1.0861 1.2537 0.7158 0.084 Uiso 1 1 calc R . . C57 C 1.3347(4) 1.3415(4) 0.7501(3) 0.0588(13) Uani 1 1 d . . . H57A H 1.3405 1.2861 0.7541 0.071 Uiso 1 1 calc R . . H57B H 1.4055 1.3795 0.7603 0.071 Uiso 1 1 calc R . . C58 C 1.4383(4) 1.4162(3) 0.6407(4) 0.0677(15) Uani 1 1 d . . . H58A H 1.4422 1.4658 0.6945 0.102 Uiso 1 1 calc R . . H58B H 1.4587 1.4388 0.5985 0.102 Uiso 1 1 calc R . . H58C H 1.4850 1.3834 0.6519 0.102 Uiso 1 1 calc R . . C59 C 1.3313(4) 1.3497(3) 0.4530(3) 0.0529(12) Uani 1 1 d . . . H59A H 1.4053 1.3566 0.4730 0.063 Uiso 1 1 calc R . . H59B H 1.3051 1.2977 0.3970 0.063 Uiso 1 1 calc R . . C60 C 1.1064(4) 1.2614(4) 0.3980(3) 0.0699(16) Uani 1 1 d . . . H60A H 1.1071 1.2041 0.3560 0.105 Uiso 1 1 calc R . . H60B H 1.1391 1.3081 0.3814 0.105 Uiso 1 1 calc R . . H60C H 1.0348 1.2613 0.3996 0.105 Uiso 1 1 calc R . . C61 C 1.1168(3) 1.2438(3) 0.5421(3) 0.0364(10) Uani 1 1 d . . . C62 C 1.1718(3) 1.2612(3) 0.6260(3) 0.0392(10) Uani 1 1 d . . . C63 C 1.2748(3) 1.3193(3) 0.6583(3) 0.0424(10) Uani 1 1 d . . . C64 C 1.3255(3) 1.3538(3) 0.6046(3) 0.0413(10) Uani 1 1 d . . . C65 C 1.2730(3) 1.3301(3) 0.5187(3) 0.0388(10) Uani 1 1 d . . . C66 C 1.1664(3) 1.2782(3) 0.4883(3) 0.0417(10) 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 Co1 0.0328(3) 0.0385(3) 0.0517(3) 0.0250(3) 0.0195(3) 0.0142(2) Co2 0.0456(4) 0.0413(3) 0.0548(4) 0.0258(3) 0.0231(3) 0.0169(3) Co3 0.0344(3) 0.0412(3) 0.0461(3) 0.0248(3) 0.0173(3) 0.0131(3) N1 0.045(2) 0.042(2) 0.053(2) 0.0251(18) 0.0139(18) 0.0155(18) N2 0.045(2) 0.043(2) 0.042(2) 0.0202(17) 0.0124(17) 0.0162(17) N3 0.034(2) 0.036(2) 0.054(2) 0.0122(18) 0.0158(17) 0.0113(16) N4 0.034(2) 0.037(2) 0.061(2) 0.0200(18) 0.0195(17) 0.0131(16) N5 0.030(2) 0.044(2) 0.081(3) 0.030(2) 0.0133(19) 0.0112(17) N6 0.038(2) 0.051(2) 0.061(2) 0.032(2) 0.0192(19) 0.0192(19) N7 0.039(2) 0.052(2) 0.047(2) 0.0219(19) 0.0141(18) 0.0195(18) N8 0.0335(19) 0.0327(19) 0.051(2) 0.0098(17) 0.0099(17) 0.0102(16) N9 0.045(2) 0.052(2) 0.045(2) 0.0157(19) 0.0065(18) 0.0236(19) N10 0.047(2) 0.050(2) 0.053(2) 0.024(2) 0.0146(19) 0.0206(19) N11 0.053(2) 0.045(2) 0.066(3) 0.030(2) 0.034(2) 0.0209(19) N12 0.047(2) 0.045(2) 0.057(2) 0.028(2) 0.0258(19) 0.0174(18) O1 0.060(2) 0.0442(19) 0.079(2) 0.0321(18) 0.0219(18) 0.0064(16) O2 0.107(3) 0.047(2) 0.077(2) 0.0306(19) 0.045(2) 0.028(2) O3 0.061(2) 0.060(2) 0.092(3) 0.041(2) 0.044(2) 0.0204(18) O4 0.073(3) 0.069(3) 0.157(4) 0.075(3) 0.053(3) 0.030(2) O5 0.056(2) 0.0482(18) 0.0608(19) 0.0352(16) 0.0249(16) 0.0124(16) O6 0.056(2) 0.062(2) 0.053(2) 0.0308(18) 0.0170(17) 0.0110(17) O7 0.0447(18) 0.067(2) 0.0531(19) 0.0352(17) 0.0169(15) -0.0007(16) O8 0.047(2) 0.068(2) 0.057(2) 0.0248(18) 0.0115(17) -0.0027(17) O9 0.0516(19) 0.059(2) 0.0489(18) 0.0344(16) 0.0212(15) 0.0258(16) O10 0.070(2) 0.087(3) 0.069(2) 0.046(2) 0.045(2) 0.042(2) O11 0.061(2) 0.079(3) 0.097(3) 0.038(2) 0.021(2) 0.044(2) O12 0.087(3) 0.105(3) 0.107(3) 0.068(3) 0.021(3) 0.049(3) O1W 0.159(9) 0.119(7) 0.185(9) 0.004(6) 0.006(7) 0.067(6) Br1 0.1605(8) 0.0814(5) 0.1705(8) 0.0460(5) 0.1308(7) 0.0633(5) Br2 0.0495(3) 0.0799(4) 0.0534(3) 0.0183(3) 0.0050(2) 0.0040(3) Br3 0.0706(4) 0.1062(5) 0.0618(3) 0.0367(3) 0.0409(3) 0.0493(3) C1 0.055(3) 0.049(3) 0.047(3) 0.026(2) 0.005(2) 0.015(2) C2 0.036(2) 0.038(2) 0.045(2) 0.020(2) 0.0040(19) 0.0085(19) C3 0.049(3) 0.055(3) 0.059(3) 0.030(2) 0.027(2) 0.019(2) C4 0.073(4) 0.044(3) 0.086(4) 0.024(3) 0.051(3) 0.028(3) C5 0.066(3) 0.039(3) 0.097(4) 0.027(3) 0.042(3) 0.019(3) C6 0.036(2) 0.039(3) 0.059(3) 0.021(2) 0.016(2) 0.008(2) C7 0.032(2) 0.045(3) 0.040(2) 0.014(2) 0.0114(19) 0.0129(19) C8 0.047(3) 0.052(3) 0.071(3) 0.030(3) 0.024(3) 0.014(2) C9 0.044(3) 0.046(3) 0.056(3) 0.032(2) 0.022(2) 0.020(2) C10 0.042(2) 0.037(2) 0.048(2) 0.025(2) 0.019(2) 0.016(2) C11 0.039(2) 0.036(2) 0.056(3) 0.019(2) 0.023(2) 0.006(2) C12 0.036(2) 0.047(3) 0.046(3) 0.015(2) 0.011(2) 0.011(2) C13 0.045(3) 0.046(3) 0.045(3) 0.024(2) 0.022(2) 0.019(2) C14 0.038(2) 0.035(2) 0.047(2) 0.021(2) 0.017(2) 0.0147(19) C15 0.036(2) 0.038(2) 0.051(3) 0.023(2) 0.016(2) 0.0125(19) C16 0.035(2) 0.041(3) 0.053(3) 0.025(2) 0.016(2) 0.014(2) C17 0.052(3) 0.041(3) 0.045(3) 0.022(2) 0.021(2) 0.010(2) C18 0.043(2) 0.040(2) 0.041(2) 0.018(2) 0.016(2) 0.016(2) C19 0.049(3) 0.045(3) 0.046(2) 0.023(2) 0.020(2) 0.024(2) C20 0.051(3) 0.056(3) 0.040(2) 0.018(2) 0.021(2) 0.026(2) C21 0.060(3) 0.070(3) 0.043(3) 0.030(2) 0.021(2) 0.033(3) C22 0.049(3) 0.053(3) 0.046(3) 0.020(2) 0.010(2) 0.024(2) C23 0.041(2) 0.046(3) 0.050(3) 0.017(2) 0.021(2) 0.020(2) C24 0.063(4) 0.060(3) 0.059(3) 0.023(3) 0.009(3) 0.028(3) C25 0.044(3) 0.040(3) 0.053(3) 0.023(2) 0.018(2) 0.013(2) C26 0.039(2) 0.051(3) 0.046(3) 0.024(2) 0.012(2) 0.016(2) C27 0.040(3) 0.051(3) 0.051(3) 0.026(2) 0.012(2) 0.010(2) C28 0.032(2) 0.039(2) 0.045(2) 0.015(2) 0.0070(19) 0.0073(19) C29 0.035(3) 0.042(3) 0.124(5) 0.016(3) 0.031(3) 0.006(2) C30 0.046(3) 0.038(3) 0.120(5) 0.007(3) 0.027(3) 0.006(2) C31 0.038(3) 0.039(3) 0.072(3) 0.026(2) 0.011(2) 0.009(2) C32 0.050(3) 0.061(3) 0.056(3) 0.024(3) 0.018(2) 0.021(3) C33 0.041(3) 0.053(3) 0.066(3) 0.022(3) 0.007(2) 0.007(2) C34 0.064(3) 0.044(3) 0.047(3) 0.019(2) 0.018(2) 0.018(2) C35 0.051(3) 0.061(3) 0.075(3) 0.034(3) 0.013(3) 0.010(3) C36 0.037(2) 0.056(3) 0.050(3) 0.016(2) 0.020(2) 0.017(2) C37 0.048(3) 0.083(4) 0.098(4) 0.062(4) 0.011(3) 0.015(3) C38 0.037(3) 0.049(3) 0.108(4) 0.041(3) 0.023(3) 0.020(2) C39 0.045(3) 0.054(3) 0.063(3) 0.018(3) 0.006(2) 0.017(2) C40 0.043(3) 0.041(3) 0.045(2) 0.015(2) 0.020(2) 0.021(2) C41 0.038(2) 0.036(2) 0.045(2) 0.012(2) 0.021(2) 0.0137(19) C42 0.036(2) 0.042(2) 0.044(2) 0.012(2) 0.020(2) 0.022(2) C43 0.036(2) 0.042(3) 0.060(3) 0.024(2) 0.022(2) 0.020(2) C44 0.036(2) 0.036(2) 0.067(3) 0.020(2) 0.020(2) 0.017(2) C45 0.036(2) 0.040(3) 0.056(3) 0.015(2) 0.015(2) 0.019(2) C46 0.035(2) 0.043(3) 0.043(2) 0.011(2) 0.009(2) 0.008(2) C47 0.080(4) 0.108(5) 0.052(3) 0.013(3) 0.007(3) 0.064(4) C48 0.084(4) 0.093(4) 0.049(3) 0.003(3) -0.004(3) 0.056(4) C49 0.053(3) 0.059(3) 0.055(3) 0.027(3) 0.014(2) 0.030(2) C50 0.107(5) 0.085(4) 0.058(3) 0.024(3) 0.015(3) 0.070(4) C51 0.123(5) 0.092(4) 0.051(3) 0.030(3) 0.019(3) 0.073(4) C52 0.057(3) 0.043(3) 0.054(3) 0.022(2) 0.032(2) 0.020(2) C53 0.056(3) 0.051(3) 0.061(3) 0.024(3) 0.010(2) 0.018(2) C54 0.064(3) 0.058(3) 0.062(3) 0.022(3) 0.019(3) 0.021(3) C55 0.031(2) 0.036(2) 0.062(3) 0.013(2) 0.010(2) 0.0103(19) C56 0.055(3) 0.062(3) 0.065(3) 0.037(3) 0.021(3) 0.021(3) C57 0.042(3) 0.082(4) 0.049(3) 0.017(3) 0.006(2) 0.029(3) C58 0.034(3) 0.055(3) 0.103(4) 0.025(3) 0.013(3) 0.006(2) C59 0.062(3) 0.043(3) 0.075(3) 0.034(3) 0.040(3) 0.026(2) C60 0.071(4) 0.076(4) 0.053(3) 0.026(3) 0.000(3) 0.010(3) C61 0.029(2) 0.030(2) 0.050(3) 0.0140(19) 0.0096(19) 0.0120(17) C62 0.038(2) 0.039(2) 0.046(2) 0.016(2) 0.018(2) 0.019(2) C63 0.032(2) 0.048(3) 0.049(3) 0.015(2) 0.013(2) 0.021(2) C64 0.031(2) 0.032(2) 0.056(3) 0.009(2) 0.010(2) 0.0165(18) C65 0.041(2) 0.034(2) 0.050(3) 0.018(2) 0.022(2) 0.0190(19) C66 0.046(3) 0.032(2) 0.045(2) 0.014(2) 0.010(2) 0.012(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 Co1 O1 1.954(3) . ? Co1 O5 1.960(3) . ? Co1 N4 1.991(3) 1_565 ? Co1 N6 2.025(4) 1_665 ? Co2 O3 1.966(3) . ? Co2 O11 1.985(4) 2_576 ? Co2 N1 2.007(4) . ? Co2 N10 2.026(4) 2_677 ? Co3 O7 1.960(3) . ? Co3 O9 2.022(3) . ? Co3 N7 2.044(4) . ? Co3 N12 2.050(4) 2_786 ? N1 C25 1.313(5) . ? N1 C26 1.377(5) . ? N2 C25 1.344(5) . ? N2 C27 1.370(5) . ? N2 C34 1.473(6) . ? N3 C28 1.323(5) . ? N3 C30 1.372(6) . ? N3 C36 1.467(5) . ? N4 C28 1.334(5) . ? N4 C29 1.371(6) . ? N4 Co1 1.991(3) 1_545 ? N5 C31 1.335(5) . ? N5 C33 1.364(6) . ? N5 C38 1.503(6) . ? N6 C31 1.320(6) . ? N6 C32 1.378(6) . ? N6 Co1 2.025(4) 1_445 ? N7 C46 1.317(5) . ? N7 C47 1.377(6) . ? N8 C46 1.332(5) . ? N8 C48 1.370(6) . ? N8 C55 1.471(5) . ? N9 C49 1.328(6) . ? N9 C51 1.356(6) . ? N9 C57 1.479(6) . ? N10 C49 1.324(6) . ? N10 C50 1.356(6) . ? N10 Co2 2.026(4) 2_677 ? N11 C52 1.328(6) . ? N11 C54 1.375(6) . ? N11 C59 1.483(6) . ? N12 C52 1.324(6) . ? N12 C53 1.378(6) . ? N12 Co3 2.050(4) 2_786 ? O1 C1 1.267(5) . ? O2 C1 1.234(6) . ? O3 C8 1.262(6) . ? O4 C8 1.241(6) . ? O5 C9 1.281(5) . ? O6 C9 1.237(5) . ? O7 C16 1.281(5) . ? O8 C16 1.232(5) . ? O9 C17 1.278(5) . ? O10 C17 1.232(5) . ? O11 C24 1.258(6) . ? O11 Co2 1.985(4) 2_576 ? O12 C24 1.248(6) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? Br1 C4 1.899(5) . ? Br2 C12 1.913(4) . ? Br3 C20 1.910(4) . ? C1 C2 1.508(6) . ? C2 C7 1.383(6) . ? C2 C3 1.388(6) . ? C3 C4 1.372(7) . ? C3 H3 0.9300 . ? C4 C5 1.372(7) . ? C5 C6 1.372(6) . ? C5 H5 0.9300 . ? C6 C7 1.380(6) . ? C6 C8 1.501(6) . ? C7 H7 0.9300 . ? C9 C10 1.506(6) . ? C10 C11 1.375(6) . ? C10 C15 1.396(5) . ? C11 C12 1.377(6) . ? C11 H11 0.9300 . ? C12 C13 1.379(6) . ? C13 C14 1.397(6) . ? C13 H13 0.9300 . ? C14 C15 1.389(6) . ? C14 C16 1.499(6) . ? C15 H15 0.9300 . ? C17 C18 1.503(6) . ? C18 C23 1.378(6) . ? C18 C19 1.393(6) . ? C19 C20 1.370(6) . ? C19 H19 0.9300 . ? C20 C21 1.363(6) . ? C21 C22 1.386(6) . ? C21 H21 0.9300 . ? C22 C23 1.379(6) . ? C22 C24 1.496(7) . ? C23 H23 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.342(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.332(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.350(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C40 1.519(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C41 1.515(6) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C42 1.518(6) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C43 1.525(6) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C44 1.514(6) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C45 1.534(6) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.394(6) . ? C40 C45 1.401(6) . ? C41 C42 1.400(6) . ? C42 C43 1.403(6) . ? C43 C44 1.393(6) . ? C44 C45 1.397(6) . ? C46 H46 0.9300 . ? C47 C48 1.356(7) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C51 1.349(7) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.349(7) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C61 1.519(5) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C62 1.502(6) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C63 1.513(6) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C64 1.527(6) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C65 1.520(6) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C66 1.516(6) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C62 1.396(6) . ? C61 C66 1.399(6) . ? C62 C63 1.400(6) . ? C63 C64 1.406(6) . ? C64 C65 1.389(6) . ? C65 C66 1.409(6) . ? 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 O1 Co1 O5 100.60(14) . . ? O1 Co1 N4 120.25(14) . 1_565 ? O5 Co1 N4 112.26(14) . 1_565 ? O1 Co1 N6 100.77(15) . 1_665 ? O5 Co1 N6 113.22(14) . 1_665 ? N4 Co1 N6 109.22(15) 1_565 1_665 ? O3 Co2 O11 92.12(16) . 2_576 ? O3 Co2 N1 114.53(15) . . ? O11 Co2 N1 116.48(16) 2_576 . ? O3 Co2 N10 115.03(16) . 2_677 ? O11 Co2 N10 112.57(16) 2_576 2_677 ? N1 Co2 N10 106.09(15) . 2_677 ? O7 Co3 O9 104.47(12) . . ? O7 Co3 N7 116.15(14) . . ? O9 Co3 N7 99.47(13) . . ? O7 Co3 N12 120.53(14) . 2_786 ? O9 Co3 N12 111.38(13) . 2_786 ? N7 Co3 N12 103.00(15) . 2_786 ? C25 N1 C26 105.5(4) . . ? C25 N1 Co2 127.0(3) . . ? C26 N1 Co2 127.0(3) . . ? C25 N2 C27 106.5(4) . . ? C25 N2 C34 125.0(4) . . ? C27 N2 C34 128.5(4) . . ? C28 N3 C30 106.9(4) . . ? C28 N3 C36 128.2(4) . . ? C30 N3 C36 124.9(4) . . ? C28 N4 C29 104.5(4) . . ? C28 N4 Co1 128.5(3) . 1_545 ? C29 N4 Co1 127.0(3) . 1_545 ? C31 N5 C33 107.5(4) . . ? C31 N5 C38 126.0(4) . . ? C33 N5 C38 126.0(4) . . ? C31 N6 C32 105.6(4) . . ? C31 N6 Co1 120.3(3) . 1_445 ? C32 N6 Co1 130.3(3) . 1_445 ? C46 N7 C47 104.6(4) . . ? C46 N7 Co3 131.2(3) . . ? C47 N7 Co3 124.2(3) . . ? C46 N8 C48 106.2(4) . . ? C46 N8 C55 128.0(4) . . ? C48 N8 C55 125.7(4) . . ? C49 N9 C51 106.0(4) . . ? C49 N9 C57 124.2(4) . . ? C51 N9 C57 129.8(4) . . ? C49 N10 C50 104.3(4) . . ? C49 N10 Co2 123.4(3) . 2_677 ? C50 N10 Co2 131.2(3) . 2_677 ? C52 N11 C54 106.6(4) . . ? C52 N11 C59 127.3(4) . . ? C54 N11 C59 125.8(4) . . ? C52 N12 C53 104.9(4) . . ? C52 N12 Co3 124.6(3) . 2_786 ? C53 N12 Co3 130.5(3) . 2_786 ? C1 O1 Co1 125.6(3) . . ? C8 O3 Co2 126.7(3) . . ? C9 O5 Co1 110.4(3) . . ? C16 O7 Co3 111.6(3) . . ? C17 O9 Co3 102.0(3) . . ? C24 O11 Co2 109.6(4) . 2_576 ? H1WA O1W H1WB 107.7 . . ? O2 C1 O1 125.5(4) . . ? O2 C1 C2 119.4(4) . . ? O1 C1 C2 115.1(4) . . ? C7 C2 C3 118.8(4) . . ? C7 C2 C1 119.5(4) . . ? C3 C2 C1 121.7(4) . . ? C4 C3 C2 119.1(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 121.8(4) . . ? C5 C4 Br1 118.3(4) . . ? C3 C4 Br1 119.9(4) . . ? C4 C5 C6 119.5(5) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C7 119.2(4) . . ? C5 C6 C8 117.7(4) . . ? C7 C6 C8 123.1(4) . . ? C6 C7 C2 121.4(4) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? O4 C8 O3 125.5(5) . . ? O4 C8 C6 118.7(4) . . ? O3 C8 C6 115.8(4) . . ? O6 C9 O5 123.5(4) . . ? O6 C9 C10 119.7(4) . . ? O5 C9 C10 116.8(4) . . ? C11 C10 C15 119.9(4) . . ? C11 C10 C9 119.9(4) . . ? C15 C10 C9 120.1(4) . . ? C10 C11 C12 119.4(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C11 C12 C13 122.0(4) . . ? C11 C12 Br2 119.2(3) . . ? C13 C12 Br2 118.8(3) . . ? C12 C13 C14 118.6(4) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 119.9(4) . . ? C15 C14 C16 119.6(4) . . ? C13 C14 C16 120.6(4) . . ? C14 C15 C10 120.1(4) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? O8 C16 O7 123.0(4) . . ? O8 C16 C14 121.0(4) . . ? O7 C16 C14 115.9(4) . . ? O10 C17 O9 122.3(4) . . ? O10 C17 C18 118.7(4) . . ? O9 C17 C18 118.8(4) . . ? C23 C18 C19 119.5(4) . . ? C23 C18 C17 119.6(4) . . ? C19 C18 C17 120.8(4) . . ? C20 C19 C18 118.4(4) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C21 C20 C19 122.7(4) . . ? C21 C20 Br3 118.4(3) . . ? C19 C20 Br3 118.9(4) . . ? C20 C21 C22 118.7(4) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C23 C22 C21 119.6(4) . . ? C23 C22 C24 120.9(4) . . ? C21 C22 C24 119.4(4) . . ? C18 C23 C22 120.8(4) . . ? C18 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? O12 C24 O11 122.9(5) . . ? O12 C24 C22 119.8(5) . . ? O11 C24 C22 117.3(5) . . ? N1 C25 N2 111.7(4) . . ? N1 C25 H25 124.1 . . ? N2 C25 H25 124.1 . . ? C27 C26 N1 109.4(4) . . ? C27 C26 H26 125.3 . . ? N1 C26 H26 125.3 . . ? C26 C27 N2 106.9(4) . . ? C26 C27 H27 126.5 . . ? N2 C27 H27 126.5 . . ? N3 C28 N4 111.7(4) . . ? N3 C28 H28 124.1 . . ? N4 C28 H28 124.1 . . ? C30 C29 N4 110.2(4) . . ? C30 C29 H29 124.9 . . ? N4 C29 H29 124.9 . . ? C29 C30 N3 106.7(4) . . ? C29 C30 H30 126.7 . . ? N3 C30 H30 126.7 . . ? N6 C31 N5 111.2(4) . . ? N6 C31 H31 124.4 . . ? N5 C31 H31 124.4 . . ? C33 C32 N6 109.2(4) . . ? C33 C32 H32 125.4 . . ? N6 C32 H32 125.4 . . ? C32 C33 N5 106.5(4) . . ? C32 C33 H33 126.7 . . ? N5 C33 H33 126.7 . . ? N2 C34 C40 111.8(3) . . ? N2 C34 H34A 109.3 . . ? C40 C34 H34A 109.3 . . ? N2 C34 H34B 109.3 . . ? C40 C34 H34B 109.3 . . ? H34A C34 H34B 107.9 . . ? C41 C35 H35A 109.5 . . ? C41 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C41 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 C42 113.2(3) . . ? N3 C36 H36A 108.9 . . ? C42 C36 H36A 108.9 . . ? N3 C36 H36B 108.9 . . ? C42 C36 H36B 108.9 . . ? H36A C36 H36B 107.8 . . ? C43 C37 H37A 109.5 . . ? C43 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C43 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C38 C44 108.6(4) . . ? N5 C38 H38A 110.0 . . ? C44 C38 H38A 110.0 . . ? N5 C38 H38B 110.0 . . ? C44 C38 H38B 110.0 . . ? H38A C38 H38B 108.3 . . ? C45 C39 H39A 109.5 . . ? C45 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C45 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 120.2(4) . . ? C41 C40 C34 119.6(4) . . ? C45 C40 C34 120.0(4) . . ? C40 C41 C42 119.7(4) . . ? C40 C41 C35 120.8(4) . . ? C42 C41 C35 119.5(4) . . ? C41 C42 C43 120.6(4) . . ? C41 C42 C36 119.0(4) . . ? C43 C42 C36 120.1(4) . . ? C44 C43 C42 119.0(4) . . ? C44 C43 C37 121.4(4) . . ? C42 C43 C37 119.6(4) . . ? C43 C44 C45 121.0(4) . . ? C43 C44 C38 120.2(4) . . ? C45 C44 C38 118.6(4) . . ? C44 C45 C40 119.5(4) . . ? C44 C45 C39 120.3(4) . . ? C40 C45 C39 120.2(4) . . ? N7 C46 N8 113.0(4) . . ? N7 C46 H46 123.5 . . ? N8 C46 H46 123.5 . . ? C48 C47 N7 109.5(5) . . ? C48 C47 H47 125.3 . . ? N7 C47 H47 125.3 . . ? C47 C48 N8 106.7(5) . . ? C47 C48 H48 126.7 . . ? N8 C48 H48 126.7 . . ? N10 C49 N9 112.7(4) . . ? N10 C49 H49 123.6 . . ? N9 C49 H49 123.6 . . ? C51 C50 N10 109.9(5) . . ? C51 C50 H50 125.0 . . ? N10 C50 H50 125.0 . . ? C50 C51 N9 107.0(5) . . ? C50 C51 H51 126.5 . . ? N9 C51 H51 126.5 . . ? N12 C52 N11 112.3(4) . . ? N12 C52 H52 123.8 . . ? N11 C52 H52 123.8 . . ? C54 C53 N12 109.5(5) . . ? C54 C53 H53 125.3 . . ? N12 C53 H53 125.3 . . ? C53 C54 N11 106.7(5) . . ? C53 C54 H54 126.7 . . ? N11 C54 H54 126.7 . . ? N8 C55 C61 113.9(3) . . ? N8 C55 H55A 108.8 . . ? C61 C55 H55A 108.8 . . ? N8 C55 H55B 108.8 . . ? C61 C55 H55B 108.8 . . ? H55A C55 H55B 107.7 . . ? C62 C56 H56A 109.5 . . ? C62 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C62 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N9 C57 C63 113.1(4) . . ? N9 C57 H57A 109.0 . . ? C63 C57 H57A 109.0 . . ? N9 C57 H57B 109.0 . . ? C63 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? C64 C58 H58A 109.5 . . ? C64 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C64 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N11 C59 C65 116.1(4) . . ? N11 C59 H59A 108.3 . . ? C65 C59 H59A 108.3 . . ? N11 C59 H59B 108.3 . . ? C65 C59 H59B 108.3 . . ? H59A C59 H59B 107.4 . . ? C66 C60 H60A 109.5 . . ? C66 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C66 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C66 120.5(4) . . ? C62 C61 C55 120.1(4) . . ? C66 C61 C55 119.3(4) . . ? C61 C62 C63 119.1(4) . . ? C61 C62 C56 122.0(4) . . ? C63 C62 C56 118.8(4) . . ? C62 C63 C64 120.6(4) . . ? C62 C63 C57 120.0(4) . . ? C64 C63 C57 119.3(4) . . ? C65 C64 C63 119.7(4) . . ? C65 C64 C58 120.5(4) . . ? C63 C64 C58 119.8(4) . . ? C64 C65 C66 119.9(4) . . ? C64 C65 C59 121.2(4) . . ? C66 C65 C59 118.5(4) . . ? C61 C66 C65 119.7(4) . . ? C61 C66 C60 120.8(4) . . ? C65 C66 C60 119.5(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 O3 Co2 N1 C25 12.0(4) . . . . ? O11 Co2 N1 C25 117.9(4) 2_576 . . . ? N10 Co2 N1 C25 -116.0(4) 2_677 . . . ? O3 Co2 N1 C26 -177.8(3) . . . . ? O11 Co2 N1 C26 -72.0(4) 2_576 . . . ? N10 Co2 N1 C26 54.1(4) 2_677 . . . ? O7 Co3 N7 C46 84.2(4) . . . . ? O9 Co3 N7 C46 -27.1(4) . . . . ? N12 Co3 N7 C46 -141.8(4) 2_786 . . . ? O7 Co3 N7 C47 -98.3(4) . . . . ? O9 Co3 N7 C47 150.4(4) . . . . ? N12 Co3 N7 C47 35.7(5) 2_786 . . . ? O5 Co1 O1 C1 -143.9(4) . . . . ? N4 Co1 O1 C1 -20.2(4) 1_565 . . . ? N6 Co1 O1 C1 99.7(4) 1_665 . . . ? O11 Co2 O3 C8 -135.0(4) 2_576 . . . ? N1 Co2 O3 C8 -14.5(5) . . . . ? N10 Co2 O3 C8 108.8(4) 2_677 . . . ? O1 Co1 O5 C9 -161.6(3) . . . . ? N4 Co1 O5 C9 69.3(3) 1_565 . . . ? N6 Co1 O5 C9 -54.9(3) 1_665 . . . ? O9 Co3 O7 C16 171.5(3) . . . . ? N7 Co3 O7 C16 63.1(3) . . . . ? N12 Co3 O7 C16 -62.4(3) 2_786 . . . ? O7 Co3 O9 C17 71.3(3) . . . . ? N7 Co3 O9 C17 -168.4(3) . . . . ? N12 Co3 O9 C17 -60.4(3) 2_786 . . . ? Co1 O1 C1 O2 20.9(7) . . . . ? Co1 O1 C1 C2 -159.5(3) . . . . ? O2 C1 C2 C7 -7.7(6) . . . . ? O1 C1 C2 C7 172.7(4) . . . . ? O2 C1 C2 C3 174.4(5) . . . . ? O1 C1 C2 C3 -5.2(6) . . . . ? C7 C2 C3 C4 -1.2(7) . . . . ? C1 C2 C3 C4 176.7(5) . . . . ? C2 C3 C4 C5 -2.1(8) . . . . ? C2 C3 C4 Br1 -179.6(4) . . . . ? C3 C4 C5 C6 3.1(9) . . . . ? Br1 C4 C5 C6 -179.4(4) . . . . ? C4 C5 C6 C7 -0.6(8) . . . . ? C4 C5 C6 C8 -179.9(5) . . . . ? C5 C6 C7 C2 -2.7(7) . . . . ? C8 C6 C7 C2 176.5(4) . . . . ? C3 C2 C7 C6 3.6(6) . . . . ? C1 C2 C7 C6 -174.3(4) . . . . ? Co2 O3 C8 O4 -26.7(8) . . . . ? Co2 O3 C8 C6 154.4(3) . . . . ? C5 C6 C8 O4 12.5(7) . . . . ? C7 C6 C8 O4 -166.7(5) . . . . ? C5 C6 C8 O3 -168.5(5) . . . . ? C7 C6 C8 O3 12.3(7) . . . . ? Co1 O5 C9 O6 -2.6(5) . . . . ? Co1 O5 C9 C10 179.1(3) . . . . ? O6 C9 C10 C11 -155.9(4) . . . . ? O5 C9 C10 C11 22.5(6) . . . . ? O6 C9 C10 C15 23.0(6) . . . . ? O5 C9 C10 C15 -158.7(4) . . . . ? C15 C10 C11 C12 -1.2(6) . . . . ? C9 C10 C11 C12 177.7(4) . . . . ? C10 C11 C12 C13 3.2(7) . . . . ? C10 C11 C12 Br2 -176.5(3) . . . . ? C11 C12 C13 C14 -2.3(7) . . . . ? Br2 C12 C13 C14 177.4(3) . . . . ? C12 C13 C14 C15 -0.6(6) . . . . ? C12 C13 C14 C16 180.0(4) . . . . ? C13 C14 C15 C10 2.6(6) . . . . ? C16 C14 C15 C10 -178.0(4) . . . . ? C11 C10 C15 C14 -1.7(6) . . . . ? C9 C10 C15 C14 179.5(4) . . . . ? Co3 O7 C16 O8 -3.8(6) . . . . ? Co3 O7 C16 C14 174.4(3) . . . . ? C15 C14 C16 O8 -11.2(6) . . . . ? C13 C14 C16 O8 168.2(4) . . . . ? C15 C14 C16 O7 170.6(4) . . . . ? C13 C14 C16 O7 -10.0(6) . . . . ? Co3 O9 C17 O10 -8.5(5) . . . . ? Co3 O9 C17 C18 167.9(3) . . . . ? O10 C17 C18 C23 1.7(6) . . . . ? O9 C17 C18 C23 -174.9(4) . . . . ? O10 C17 C18 C19 177.8(4) . . . . ? O9 C17 C18 C19 1.2(6) . . . . ? C23 C18 C19 C20 2.4(6) . . . . ? C17 C18 C19 C20 -173.7(4) . . . . ? C18 C19 C20 C21 2.0(7) . . . . ? C18 C19 C20 Br3 -179.6(3) . . . . ? C19 C20 C21 C22 -4.2(7) . . . . ? Br3 C20 C21 C22 177.4(4) . . . . ? C20 C21 C22 C23 1.9(7) . . . . ? C20 C21 C22 C24 178.4(4) . . . . ? C19 C18 C23 C22 -4.6(6) . . . . ? C17 C18 C23 C22 171.6(4) . . . . ? C21 C22 C23 C18 2.4(7) . . . . ? C24 C22 C23 C18 -174.0(4) . . . . ? Co2 O11 C24 O12 1.0(7) 2_576 . . . ? Co2 O11 C24 C22 178.6(3) 2_576 . . . ? C23 C22 C24 O12 144.3(5) . . . . ? C21 C22 C24 O12 -32.2(7) . . . . ? C23 C22 C24 O11 -33.4(7) . . . . ? C21 C22 C24 O11 150.2(5) . . . . ? C26 N1 C25 N2 -0.2(5) . . . . ? Co2 N1 C25 N2 171.6(3) . . . . ? C27 N2 C25 N1 0.4(5) . . . . ? C34 N2 C25 N1 179.3(4) . . . . ? C25 N1 C26 C27 0.0(5) . . . . ? Co2 N1 C26 C27 -171.8(3) . . . . ? N1 C26 C27 N2 0.3(5) . . . . ? C25 N2 C27 C26 -0.4(5) . . . . ? C34 N2 C27 C26 -179.3(4) . . . . ? C30 N3 C28 N4 -1.9(5) . . . . ? C36 N3 C28 N4 -179.4(4) . . . . ? C29 N4 C28 N3 0.7(5) . . . . ? Co1 N4 C28 N3 -179.1(3) 1_545 . . . ? C28 N4 C29 C30 0.9(7) . . . . ? Co1 N4 C29 C30 -179.4(4) 1_545 . . . ? N4 C29 C30 N3 -2.0(8) . . . . ? C28 N3 C30 C29 2.3(7) . . . . ? C36 N3 C30 C29 180.0(5) . . . . ? C32 N6 C31 N5 -0.7(5) . . . . ? Co1 N6 C31 N5 159.6(3) 1_445 . . . ? C33 N5 C31 N6 0.9(5) . . . . ? C38 N5 C31 N6 -171.7(4) . . . . ? C31 N6 C32 C33 0.3(5) . . . . ? Co1 N6 C32 C33 -157.2(3) 1_445 . . . ? N6 C32 C33 N5 0.3(6) . . . . ? C31 N5 C33 C32 -0.7(5) . . . . ? C38 N5 C33 C32 171.9(4) . . . . ? C25 N2 C34 C40 114.8(5) . . . . ? C27 N2 C34 C40 -66.6(6) . . . . ? C28 N3 C36 C42 -44.4(6) . . . . ? C30 N3 C36 C42 138.4(5) . . . . ? C31 N5 C38 C44 128.5(5) . . . . ? C33 N5 C38 C44 -42.7(7) . . . . ? N2 C34 C40 C41 -75.7(5) . . . . ? N2 C34 C40 C45 99.3(5) . . . . ? C45 C40 C41 C42 -2.0(6) . . . . ? C34 C40 C41 C42 173.0(4) . . . . ? C45 C40 C41 C35 179.0(4) . . . . ? C34 C40 C41 C35 -6.0(6) . . . . ? C40 C41 C42 C43 1.1(6) . . . . ? C35 C41 C42 C43 -179.9(4) . . . . ? C40 C41 C42 C36 -173.1(3) . . . . ? C35 C41 C42 C36 6.0(6) . . . . ? N3 C36 C42 C41 -81.4(5) . . . . ? N3 C36 C42 C43 104.5(5) . . . . ? C41 C42 C43 C44 -1.1(6) . . . . ? C36 C42 C43 C44 172.9(4) . . . . ? C41 C42 C43 C37 -179.1(4) . . . . ? C36 C42 C43 C37 -5.0(6) . . . . ? C42 C43 C44 C45 2.1(6) . . . . ? C37 C43 C44 C45 -180.0(4) . . . . ? C42 C43 C44 C38 -172.3(4) . . . . ? C37 C43 C44 C38 5.6(7) . . . . ? N5 C38 C44 C43 110.6(5) . . . . ? N5 C38 C44 C45 -63.9(6) . . . . ? C43 C44 C45 C40 -3.0(6) . . . . ? C38 C44 C45 C40 171.5(4) . . . . ? C43 C44 C45 C39 178.2(4) . . . . ? C38 C44 C45 C39 -7.3(6) . . . . ? C41 C40 C45 C44 3.0(6) . . . . ? C34 C40 C45 C44 -172.0(4) . . . . ? C41 C40 C45 C39 -178.3(4) . . . . ? C34 C40 C45 C39 6.7(6) . . . . ? C47 N7 C46 N8 -1.2(5) . . . . ? Co3 N7 C46 N8 176.6(3) . . . . ? C48 N8 C46 N7 0.7(5) . . . . ? C55 N8 C46 N7 176.6(4) . . . . ? C46 N7 C47 C48 1.3(7) . . . . ? Co3 N7 C47 C48 -176.7(4) . . . . ? N7 C47 C48 N8 -0.9(8) . . . . ? C46 N8 C48 C47 0.2(7) . . . . ? C55 N8 C48 C47 -175.8(5) . . . . ? C50 N10 C49 N9 -0.2(6) . . . . ? Co2 N10 C49 N9 -169.8(3) 2_677 . . . ? C51 N9 C49 N10 1.1(6) . . . . ? C57 N9 C49 N10 179.2(4) . . . . ? C49 N10 C50 C51 -0.8(7) . . . . ? Co2 N10 C50 C51 167.7(4) 2_677 . . . ? N10 C50 C51 N9 1.4(7) . . . . ? C49 N9 C51 C50 -1.5(7) . . . . ? C57 N9 C51 C50 -179.4(5) . . . . ? C53 N12 C52 N11 -1.3(5) . . . . ? Co3 N12 C52 N11 178.1(3) 2_786 . . . ? C54 N11 C52 N12 1.7(5) . . . . ? C59 N11 C52 N12 176.2(4) . . . . ? C52 N12 C53 C54 0.4(5) . . . . ? Co3 N12 C53 C54 -178.9(3) 2_786 . . . ? N12 C53 C54 N11 0.6(6) . . . . ? C52 N11 C54 C53 -1.4(5) . . . . ? C59 N11 C54 C53 -176.0(4) . . . . ? C46 N8 C55 C61 135.1(4) . . . . ? C48 N8 C55 C61 -49.8(6) . . . . ? C49 N9 C57 C63 154.1(4) . . . . ? C51 N9 C57 C63 -28.3(8) . . . . ? C52 N11 C59 C65 54.2(6) . . . . ? C54 N11 C59 C65 -132.4(5) . . . . ? N8 C55 C61 C62 90.2(5) . . . . ? N8 C55 C61 C66 -92.5(5) . . . . ? C66 C61 C62 C63 5.0(6) . . . . ? C55 C61 C62 C63 -177.8(4) . . . . ? C66 C61 C62 C56 -173.4(4) . . . . ? C55 C61 C62 C56 3.8(6) . . . . ? C61 C62 C63 C64 -5.3(6) . . . . ? C56 C62 C63 C64 173.2(4) . . . . ? C61 C62 C63 C57 178.1(4) . . . . ? C56 C62 C63 C57 -3.5(6) . . . . ? N9 C57 C63 C62 -61.9(6) . . . . ? N9 C57 C63 C64 121.4(5) . . . . ? C62 C63 C64 C65 0.0(6) . . . . ? C57 C63 C64 C65 176.7(4) . . . . ? C62 C63 C64 C58 -179.3(4) . . . . ? C57 C63 C64 C58 -2.6(6) . . . . ? C63 C64 C65 C66 5.6(6) . . . . ? C58 C64 C65 C66 -175.1(4) . . . . ? C63 C64 C65 C59 -167.4(4) . . . . ? C58 C64 C65 C59 11.9(6) . . . . ? N11 C59 C65 C64 -99.8(5) . . . . ? N11 C59 C65 C66 87.1(5) . . . . ? C62 C61 C66 C65 0.5(6) . . . . ? C55 C61 C66 C65 -176.7(4) . . . . ? C62 C61 C66 C60 -178.6(4) . . . . ? C55 C61 C66 C60 4.2(6) . . . . ? C64 C65 C66 C61 -5.9(6) . . . . ? C59 C65 C66 C61 167.3(4) . . . . ? C64 C65 C66 C60 173.2(4) . . . . ? C59 C65 C66 C60 -13.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.449 _refine_diff_density_min -1.278 _refine_diff_density_rms 0.075 #======================================# data_cec3 _database_code_depnum_ccdc_archive 'CCDC 803646' #TrackingRef '- 5-CEC1115.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 N4 Ni O6 S' _chemical_formula_sum 'C28 H26 N4 Ni O8 S' _chemical_formula_weight 637.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C m c a' _symmetry_space_group_name_Hall '-C 2bc 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y, z-1/2' _cell_length_a 24.2834(9) _cell_length_b 20.5803(9) _cell_length_c 12.6997(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6346.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2075 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 19.62 _exptl_crystal_description Pillar _exptl_crystal_colour green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8332 _exptl_absorpt_correction_T_max 0.9049 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20083 _diffrn_reflns_av_R_equivalents 0.0993 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2929 _reflns_number_gt 1506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0308P)^2^+1.3791P] 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 2929 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.2500 0.03837(3) 0.2500 0.0500(2) Uani 1 2 d S . 1 N1 N 0.30186(13) -0.02743(14) 0.1883(2) 0.0524(8) Uani 1 1 d . A 1 N2 N 0.33193(14) -0.10255(15) 0.0787(2) 0.0513(8) Uani 1 1 d . A 1 O1 O 0.20788(10) 0.05607(12) 0.10838(17) 0.0556(7) Uani 1 1 d . B 1 O2 O 0.18841(10) 0.11300(11) 0.24907(19) 0.0587(7) Uani 1 1 d . B 1 O3 O 0.0000 0.3108(2) -0.0400(4) 0.126(2) Uani 1 2 d S C 1 O4 O 0.0000 0.2247(3) -0.1827(4) 0.121(2) Uani 1 2 d S D 1 S1 S 0.0000 0.24270(11) -0.07212(17) 0.0909(7) Uani 1 2 d S . 1 C1 C 0.18079(16) 0.1005(2) 0.1534(3) 0.0512(10) Uani 1 1 d . B 1 C2 C 0.13859(15) 0.13808(18) 0.0934(3) 0.0498(10) Uani 1 1 d . B 1 C3 C 0.12569(17) 0.1221(2) -0.0086(3) 0.0742(13) Uani 1 1 d . B 1 H3 H 0.1450 0.0891 -0.0425 0.089 Uiso 1 1 calc R B 1 C4 C 0.08415(18) 0.1548(3) -0.0614(3) 0.0803(15) Uani 1 1 d . B 1 H4 H 0.0751 0.1434 -0.1302 0.096 Uiso 1 1 calc R B 1 C5 C 0.05657(16) 0.2037(2) -0.0115(3) 0.0623(12) Uani 1 1 d . B 1 C6 C 0.06982(17) 0.2209(2) 0.0905(4) 0.0728(13) Uani 1 1 d . B 1 H6 H 0.0513 0.2547 0.1240 0.087 Uiso 1 1 calc R B 1 C7 C 0.11051(17) 0.1876(2) 0.1414(3) 0.0665(12) Uani 1 1 d . B 1 H7 H 0.1194 0.1988 0.2103 0.080 Uiso 1 1 calc R B 1 C8 C 0.3515(2) -0.0497(2) 0.2209(3) 0.0810(15) Uani 1 1 d . A 1 H8 H 0.3698 -0.0352 0.2807 0.097 Uiso 1 1 calc R A 1 C9 C 0.37078(19) -0.0959(2) 0.1549(3) 0.0848(15) Uani 1 1 d . A 1 H9 H 0.4039 -0.1184 0.1604 0.102 Uiso 1 1 calc R A 1 C10 C 0.29155(16) -0.06088(19) 0.1010(3) 0.0544(11) Uani 1 1 d . A 1 H10 H 0.2600 -0.0558 0.0604 0.065 Uiso 1 1 calc R A 1 C11 C 0.33282(17) -0.14815(18) -0.0105(3) 0.0585(11) Uani 1 1 d . A 1 H11A H 0.3687 -0.1687 -0.0138 0.070 Uiso 1 1 calc R A 1 H11B H 0.3276 -0.1240 -0.0754 0.070 Uiso 1 1 calc R A 1 C12 C 0.26644(17) -0.22017(19) 0.0906(3) 0.0596(12) Uani 1 1 d . . 1 H12 H 0.2775 -0.2005 0.1530 0.071 Uiso 1 1 calc R . 1 C13 C 0.28906(16) -0.20022(18) -0.0031(3) 0.0489(10) Uani 1 1 d . A 1 C14 C 0.27228(17) -0.23134(19) -0.0933(3) 0.0594(12) Uani 1 1 d . . 1 H14 H 0.2875 -0.2193 -0.1576 0.071 Uiso 1 1 calc R . 1 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 0.0568(5) 0.0540(4) 0.0391(4) 0.000 -0.0074(4) 0.000 N1 0.052(2) 0.056(2) 0.0485(19) -0.0007(17) -0.0174(18) 0.0035(18) N2 0.057(2) 0.054(2) 0.0431(19) 0.0034(17) -0.0054(18) 0.0035(19) O1 0.0590(18) 0.0656(18) 0.0423(15) -0.0049(13) -0.0072(13) 0.0171(15) O2 0.0697(17) 0.0673(17) 0.0390(14) -0.0090(16) -0.0093(15) 0.0066(14) O3 0.089(4) 0.080(3) 0.211(6) 0.079(4) 0.000 0.000 O4 0.068(3) 0.215(6) 0.081(3) 0.081(4) 0.000 0.000 S1 0.0461(11) 0.1245(18) 0.1022(15) 0.0672(14) 0.000 0.000 C1 0.049(3) 0.055(3) 0.050(3) 0.003(2) -0.002(2) 0.002(2) C2 0.045(3) 0.057(3) 0.048(2) 0.000(2) 0.004(2) 0.005(2) C3 0.074(3) 0.111(4) 0.038(2) -0.008(2) -0.006(2) 0.033(3) C4 0.071(3) 0.124(4) 0.045(3) 0.012(3) -0.005(2) 0.021(3) C5 0.039(3) 0.081(3) 0.067(3) 0.032(3) 0.000(2) 0.003(3) C6 0.052(3) 0.071(3) 0.096(4) -0.005(3) -0.010(3) 0.008(2) C7 0.056(3) 0.075(3) 0.069(3) -0.008(3) -0.016(2) 0.009(3) C8 0.084(4) 0.103(4) 0.056(3) -0.023(3) -0.027(3) 0.017(3) C9 0.071(3) 0.111(4) 0.073(3) -0.019(3) -0.029(3) 0.032(3) C10 0.049(3) 0.060(3) 0.053(3) 0.002(2) -0.015(2) 0.005(2) C11 0.071(3) 0.064(3) 0.040(2) -0.004(2) 0.000(2) 0.007(3) C12 0.083(3) 0.064(3) 0.032(2) -0.005(2) 0.000(2) -0.006(3) C13 0.064(3) 0.046(3) 0.037(2) 0.0056(19) 0.007(2) 0.009(2) C14 0.086(3) 0.061(3) 0.031(2) -0.001(2) 0.010(2) 0.000(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 N1 2.009(3) . ? Ni1 N1 2.009(3) 8_545 ? Ni1 O1 2.101(2) . ? Ni1 O1 2.101(2) 8_545 ? Ni1 O2 2.144(2) . ? Ni1 O2 2.144(2) 8_545 ? Ni1 C1 2.443(4) 8_545 ? N1 C10 1.329(4) . ? N1 C8 1.355(5) . ? N2 C10 1.333(4) . ? N2 C9 1.358(4) . ? N2 C11 1.471(4) . ? O1 C1 1.264(4) . ? O2 C1 1.255(4) . ? O3 S1 1.459(5) . ? O4 S1 1.453(5) . ? S1 C5 1.767(4) . ? S1 C5 1.767(4) 11 ? C1 C2 1.493(5) . ? C2 C7 1.370(5) . ? C2 C3 1.373(5) . ? C3 C4 1.386(5) . ? C3 H3 0.9300 . ? C4 C5 1.366(5) . ? C4 H4 0.9300 . ? C5 C6 1.381(5) . ? C6 C7 1.365(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.350(5) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C13 1.512(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C14 1.372(5) 13_545 ? C12 C13 1.373(5) . ? C12 H12 0.9300 . ? C13 C14 1.374(5) . ? C14 C12 1.371(5) 13_545 ? C14 H14 0.9300 . ? 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 N1 Ni1 N1 95.21(17) . 8_545 ? N1 Ni1 O1 95.05(11) . . ? N1 Ni1 O1 98.38(11) 8_545 . ? N1 Ni1 O1 98.38(11) . 8_545 ? N1 Ni1 O1 95.05(11) 8_545 8_545 ? O1 Ni1 O1 160.03(14) . 8_545 ? N1 Ni1 O2 156.68(11) . . ? N1 Ni1 O2 92.74(11) 8_545 . ? O1 Ni1 O2 62.06(9) . . ? O1 Ni1 O2 102.72(10) 8_545 . ? N1 Ni1 O2 92.74(11) . 8_545 ? N1 Ni1 O2 156.68(11) 8_545 8_545 ? O1 Ni1 O2 102.72(10) . 8_545 ? O1 Ni1 O2 62.05(9) 8_545 8_545 ? O2 Ni1 O2 88.48(13) . 8_545 ? N1 Ni1 C1 96.76(12) . 8_545 ? N1 Ni1 C1 126.06(13) 8_545 8_545 ? O1 Ni1 C1 132.38(13) . 8_545 ? O1 Ni1 C1 31.16(10) 8_545 8_545 ? O2 Ni1 C1 96.17(11) . 8_545 ? O2 Ni1 C1 30.89(10) 8_545 8_545 ? C10 N1 C8 104.3(3) . . ? C10 N1 Ni1 123.8(3) . . ? C8 N1 Ni1 131.8(3) . . ? C10 N2 C9 107.1(3) . . ? C10 N2 C11 125.8(3) . . ? C9 N2 C11 127.1(4) . . ? C1 O1 Ni1 89.5(2) . . ? C1 O2 Ni1 87.8(2) . . ? O4 S1 O3 121.0(3) . . ? O4 S1 C5 107.8(2) . . ? O3 S1 C5 108.3(2) . . ? O4 S1 C5 107.8(2) . 11 ? O3 S1 C5 108.3(2) . 11 ? C5 S1 C5 102.0(3) . 11 ? O2 C1 O1 120.6(4) . . ? O2 C1 C2 119.3(4) . . ? O1 C1 C2 120.1(3) . . ? C7 C2 C3 119.0(4) . . ? C7 C2 C1 120.0(4) . . ? C3 C2 C1 120.9(4) . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.6(4) . . ? C4 C5 S1 120.9(4) . . ? C6 C5 S1 118.3(4) . . ? C7 C6 C5 118.9(4) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C2 121.6(4) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? C9 C8 N1 110.9(4) . . ? C9 C8 H8 124.5 . . ? N1 C8 H8 124.5 . . ? C8 C9 N2 105.8(4) . . ? C8 C9 H9 127.1 . . ? N2 C9 H9 127.1 . . ? N1 C10 N2 111.8(3) . . ? N1 C10 H10 124.1 . . ? N2 C10 H10 124.1 . . ? N2 C11 C13 113.2(3) . . ? N2 C11 H11A 108.9 . . ? C13 C11 H11A 108.9 . . ? N2 C11 H11B 108.9 . . ? C13 C11 H11B 108.9 . . ? H11A C11 H11B 107.8 . . ? C14 C12 C13 120.9(3) 13_545 . ? C14 C12 H12 119.5 13_545 . ? C13 C12 H12 119.5 . . ? C12 C13 C14 117.7(4) . . ? C12 C13 C11 123.2(4) . . ? C14 C13 C11 119.1(3) . . ? C12 C14 C13 121.4(3) 13_545 . ? C12 C14 H14 119.3 13_545 . ? C13 C14 H14 119.3 . . ? 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 N1 Ni1 N1 C10 76.5(3) 8_545 . . . ? O1 Ni1 N1 C10 -22.4(3) . . . . ? O1 Ni1 N1 C10 172.5(3) 8_545 . . . ? O2 Ni1 N1 C10 -32.9(5) . . . . ? O2 Ni1 N1 C10 -125.4(3) 8_545 . . . ? C1 Ni1 N1 C10 -156.1(3) 8_545 . . . ? N1 Ni1 N1 C8 -101.6(4) 8_545 . . . ? O1 Ni1 N1 C8 159.5(4) . . . . ? O1 Ni1 N1 C8 -5.7(4) 8_545 . . . ? O2 Ni1 N1 C8 148.9(3) . . . . ? O2 Ni1 N1 C8 56.4(4) 8_545 . . . ? C1 Ni1 N1 C8 25.7(4) 8_545 . . . ? N1 Ni1 O1 C1 -174.7(2) . . . . ? N1 Ni1 O1 C1 89.2(2) 8_545 . . . ? O1 Ni1 O1 C1 -42.5(2) 8_545 . . . ? O2 Ni1 O1 C1 0.6(2) . . . . ? O2 Ni1 O1 C1 -80.8(2) 8_545 . . . ? C1 Ni1 O1 C1 -70.8(3) 8_545 . . . ? N1 Ni1 O2 C1 11.3(4) . . . . ? N1 Ni1 O2 C1 -98.6(2) 8_545 . . . ? O1 Ni1 O2 C1 -0.6(2) . . . . ? O1 Ni1 O2 C1 165.6(2) 8_545 . . . ? O2 Ni1 O2 C1 104.7(2) 8_545 . . . ? C1 Ni1 O2 C1 134.7(2) 8_545 . . . ? Ni1 O2 C1 O1 1.0(4) . . . . ? Ni1 O2 C1 C2 179.9(3) . . . . ? Ni1 O1 C1 O2 -1.0(4) . . . . ? Ni1 O1 C1 C2 -180.0(3) . . . . ? O2 C1 C2 C7 3.1(5) . . . . ? O1 C1 C2 C7 -177.9(4) . . . . ? O2 C1 C2 C3 -174.2(4) . . . . ? O1 C1 C2 C3 4.8(6) . . . . ? C7 C2 C3 C4 -1.2(6) . . . . ? C1 C2 C3 C4 176.1(4) . . . . ? C2 C3 C4 C5 0.9(7) . . . . ? C3 C4 C5 C6 0.2(6) . . . . ? C3 C4 C5 S1 -175.3(3) . . . . ? O4 S1 C5 C4 -13.7(4) . . . . ? O3 S1 C5 C4 -146.2(4) . . . . ? C5 S1 C5 C4 99.7(4) 11 . . . ? O4 S1 C5 C6 170.8(4) . . . . ? O3 S1 C5 C6 38.2(4) . . . . ? C5 S1 C5 C6 -75.9(5) 11 . . . ? C4 C5 C6 C7 -0.8(6) . . . . ? S1 C5 C6 C7 174.7(3) . . . . ? C5 C6 C7 C2 0.5(6) . . . . ? C3 C2 C7 C6 0.5(6) . . . . ? C1 C2 C7 C6 -176.8(4) . . . . ? C10 N1 C8 C9 -0.2(5) . . . . ? Ni1 N1 C8 C9 178.3(3) . . . . ? N1 C8 C9 N2 0.0(5) . . . . ? C10 N2 C9 C8 0.2(5) . . . . ? C11 N2 C9 C8 -178.3(3) . . . . ? C8 N1 C10 N2 0.3(4) . . . . ? Ni1 N1 C10 N2 -178.3(2) . . . . ? C9 N2 C10 N1 -0.3(4) . . . . ? C11 N2 C10 N1 178.2(3) . . . . ? C10 N2 C11 C13 -65.9(4) . . . . ? C9 N2 C11 C13 112.3(4) . . . . ? C14 C12 C13 C14 -1.2(6) 13_545 . . . ? C14 C12 C13 C11 -178.5(3) 13_545 . . . ? N2 C11 C13 C12 -25.0(5) . . . . ? N2 C11 C13 C14 157.8(3) . . . . ? C12 C13 C14 C12 1.2(6) . . . 13_545 ? C11 C13 C14 C12 178.6(3) . . . 13_545 ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.419 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.052 # 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 0.000 0.000 -0.009 339 13 ' ' 2 0.500 0.000 -0.008 339 13 ' ' 3 0.000 0.500 -0.007 339 13 ' ' 4 0.500 0.500 -0.013 339 13 ' ' _platon_squeeze_details ; ; #============================# data_CEC4 _database_code_depnum_ccdc_archive 'CCDC 803647' #TrackingRef '- 5-CEC1115.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 N4 Ni O7 S, 0.38(H2 O)' _chemical_formula_sum 'C28 H27.76 N4 Ni O7.38 S' _chemical_formula_weight 629.14 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1202(16) _cell_length_b 10.8830(17) _cell_length_c 13.409(2) _cell_angle_alpha 70.501(2) _cell_angle_beta 87.561(3) _cell_angle_gamma 76.947(3) _cell_volume 1355.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3159 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.77 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8092 _exptl_absorpt_correction_T_max 0.8484 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6835 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4728 _reflns_number_gt 3929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0430P)^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 4728 _refine_ls_number_parameters 382 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.04977(3) 0.57295(3) 0.66657(2) 0.03389(11) Uani 1 1 d . . . O1 O 0.21490(16) 0.41478(17) 0.76817(13) 0.0413(4) Uani 1 1 d . . . O2 O 0.10154(16) 0.38570(16) 0.64513(13) 0.0391(4) Uani 1 1 d . . . O3 O 0.25801(18) -0.5262(2) 1.31468(14) 0.0570(5) Uani 1 1 d . . . O4 O 0.07573(17) -0.49711(18) 1.21573(13) 0.0434(4) Uani 1 1 d . . . O5 O 0.46339(18) -0.28366(18) 0.75944(13) 0.0491(5) Uani 1 1 d . . . O6 O 0.62630(17) -0.24663(18) 0.87309(15) 0.0511(5) Uani 1 1 d . . . N1 N 0.0114(2) 0.7440(2) 0.70662(16) 0.0428(5) Uani 1 1 d . . . N2 N -0.0885(2) 0.8945(3) 0.7773(2) 0.0576(7) Uani 1 1 d . . . N3 N 0.1941(2) 0.6366(2) 0.56228(15) 0.0387(5) Uani 1 1 d . . . N4 N 0.3881(2) 0.6898(2) 0.50760(16) 0.0410(5) Uani 1 1 d . . . O1W O -0.10269(19) 0.65150(19) 0.55116(15) 0.0422(4) Uani 1 1 d D . . H1WA H -0.101(3) 0.639(3) 0.4931(17) 0.066(10) Uiso 1 1 d D . . H1WB H -0.160(3) 0.611(3) 0.585(2) 0.087(13) Uiso 1 1 d D . . C1 C 0.1915(2) 0.3420(2) 0.71884(18) 0.0344(5) Uani 1 1 d . . . C2 C 0.2690(2) 0.2003(2) 0.74791(18) 0.0352(6) Uani 1 1 d . . . C3 C 0.3638(3) 0.1452(3) 0.8305(2) 0.0570(8) Uani 1 1 d . . . H3 H 0.3816 0.1981 0.8680 0.068 Uiso 1 1 calc R . . C4 C 0.4325(3) 0.0141(3) 0.8585(2) 0.0566(8) Uani 1 1 d . . . H4 H 0.4973 -0.0212 0.9138 0.068 Uiso 1 1 calc R . . C5 C 0.4048(2) -0.0647(2) 0.80425(18) 0.0343(5) Uani 1 1 d . . . C6 C 0.3133(3) -0.0126(3) 0.7211(2) 0.0459(7) Uani 1 1 d . . . H6 H 0.2966 -0.0659 0.6835 0.055 Uiso 1 1 calc R . . C7 C 0.2455(3) 0.1197(3) 0.6928(2) 0.0453(7) Uani 1 1 d . . . H7 H 0.1830 0.1553 0.6359 0.054 Uiso 1 1 calc R . . C8 C 0.1955(3) -0.4885(2) 1.2287(2) 0.0381(6) Uani 1 1 d . . . C9 C 0.2682(2) -0.4261(2) 1.13102(19) 0.0354(6) Uani 1 1 d . . . C10 C 0.3969(3) -0.4071(3) 1.1413(2) 0.0408(6) Uani 1 1 d . . . H10 H 0.4374 -0.4328 1.2083 0.049 Uiso 1 1 calc R . . C11 C 0.4655(3) -0.3505(3) 1.0534(2) 0.0415(6) Uani 1 1 d . . . H11 H 0.5523 -0.3385 1.0608 0.050 Uiso 1 1 calc R . . C12 C 0.4049(2) -0.3119(2) 0.95459(18) 0.0351(6) Uani 1 1 d . . . C13 C 0.2775(3) -0.3317(3) 0.9431(2) 0.0516(7) Uani 1 1 d . . . H13 H 0.2373 -0.3064 0.8760 0.062 Uiso 1 1 calc R . . C14 C 0.2104(3) -0.3891(3) 1.0313(2) 0.0496(7) Uani 1 1 d . . . H14 H 0.1247 -0.4032 1.0236 0.060 Uiso 1 1 calc R . . C15 C -0.0595(3) 0.7641(3) 0.7870(2) 0.0508(7) Uani 1 1 d . . . H15 H -0.0859 0.6972 0.8427 0.061 Uiso 1 1 calc R . . C16 C 0.0261(3) 0.8677(3) 0.6437(3) 0.0669(6) Uani 1 1 d . . . H16 H 0.0717 0.8853 0.5805 0.080 Uiso 1 1 calc R . . C17 C -0.0348(3) 0.9597(3) 0.6865(3) 0.0669(6) Uani 1 1 d . . . H17 H -0.0392 1.0512 0.6590 0.080 Uiso 1 1 calc R . . C18 C -0.1671(3) 0.9521(4) 0.8524(3) 0.0830(12) Uani 1 1 d . . . H18A H -0.2227 0.8917 0.8924 0.100 Uiso 1 1 calc R . . H18B H -0.2276 1.0360 0.8130 0.100 Uiso 1 1 calc R . . C19 C -0.0453(4) 0.8856(4) 1.0260(3) 0.0804(12) Uani 1 1 d . . . H19 H -0.0765 0.8070 1.0451 0.096 Uiso 1 1 calc R . . C20 C -0.0794(3) 0.9770(4) 0.9288(3) 0.0668(10) Uani 1 1 d . . . C21 C -0.0348(4) 1.0946(4) 0.9019(3) 0.0796(11) Uani 1 1 d . . . H21 H -0.0583 1.1599 0.8360 0.095 Uiso 1 1 calc R . . C22 C 0.3085(3) 0.6576(3) 0.5900(2) 0.0435(6) Uani 1 1 d . . . H22 H 0.3310 0.6508 0.6585 0.052 Uiso 1 1 calc R . . C23 C 0.2025(3) 0.6558(3) 0.4567(2) 0.0488(7) Uani 1 1 d . . . H23 H 0.1367 0.6471 0.4148 0.059 Uiso 1 1 calc R . . C24 C 0.3201(3) 0.6892(3) 0.4226(2) 0.0564(8) Uani 1 1 d . . . H24 H 0.3496 0.7083 0.3536 0.068 Uiso 1 1 calc R . . C25 C 0.5182(3) 0.7260(3) 0.5101(2) 0.0485(7) Uani 1 1 d . . . H25A H 0.5702 0.7117 0.4509 0.058 Uiso 1 1 calc R . . H25B H 0.5685 0.6668 0.5747 0.058 Uiso 1 1 calc R . . C26 C 0.6052(3) 0.8988(3) 0.5536(2) 0.0462(7) Uani 1 1 d . . . H26 H 0.6771 0.8308 0.5905 0.055 Uiso 1 1 calc R . . C27 C 0.5056(2) 0.8684(3) 0.5050(2) 0.0409(6) Uani 1 1 d . . . C28 C 0.4004(3) 0.9720(3) 0.4518(2) 0.0474(7) Uani 1 1 d . . . H28 H 0.3317 0.9539 0.4187 0.057 Uiso 1 1 calc R . . S1 S 0.48940(6) -0.23511(6) 0.84192(5) 0.03839(17) Uani 1 1 d . . . O2W O 0.8650(7) 0.6138(7) 0.0244(5) 0.091(3) Uani 0.383(6) 1 d P . . 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 0.03634(19) 0.0324(2) 0.03405(19) -0.01225(14) 0.00269(13) -0.00829(14) O1 0.0453(10) 0.0380(10) 0.0437(10) -0.0183(9) -0.0016(8) -0.0075(8) O2 0.0406(10) 0.0351(10) 0.0410(10) -0.0143(8) -0.0029(8) -0.0037(8) O3 0.0463(11) 0.0863(16) 0.0348(11) -0.0142(10) 0.0023(9) -0.0171(10) O4 0.0397(10) 0.0484(11) 0.0381(10) -0.0077(9) 0.0031(8) -0.0128(8) O5 0.0660(12) 0.0376(11) 0.0459(11) -0.0188(9) 0.0096(9) -0.0094(9) O6 0.0354(10) 0.0437(11) 0.0667(13) -0.0100(10) 0.0037(9) -0.0070(8) N1 0.0446(13) 0.0436(14) 0.0457(13) -0.0225(11) 0.0026(10) -0.0094(10) N2 0.0443(14) 0.0633(17) 0.0867(19) -0.0552(16) 0.0061(13) -0.0095(12) N3 0.0433(12) 0.0393(13) 0.0389(12) -0.0164(10) 0.0064(9) -0.0156(10) N4 0.0396(12) 0.0411(13) 0.0439(12) -0.0140(10) 0.0083(10) -0.0137(10) O1W 0.0464(11) 0.0412(11) 0.0337(11) -0.0099(9) -0.0018(9) -0.0029(9) C1 0.0339(13) 0.0357(14) 0.0342(13) -0.0110(12) 0.0040(11) -0.0103(11) C2 0.0364(14) 0.0339(14) 0.0351(14) -0.0106(11) 0.0029(11) -0.0091(11) C3 0.070(2) 0.0433(17) 0.0633(19) -0.0272(16) -0.0259(15) -0.0032(15) C4 0.0633(19) 0.0459(18) 0.0588(19) -0.0204(15) -0.0259(15) 0.0014(15) C5 0.0369(13) 0.0297(13) 0.0361(13) -0.0103(11) 0.0054(10) -0.0090(11) C6 0.0583(17) 0.0363(16) 0.0447(16) -0.0162(13) -0.0067(13) -0.0083(13) C7 0.0540(17) 0.0400(16) 0.0400(15) -0.0129(13) -0.0112(12) -0.0050(13) C8 0.0398(15) 0.0323(14) 0.0411(15) -0.0145(12) 0.0050(12) -0.0031(11) C9 0.0358(14) 0.0291(13) 0.0389(14) -0.0099(11) 0.0026(11) -0.0052(11) C10 0.0455(15) 0.0411(15) 0.0367(14) -0.0134(12) -0.0018(11) -0.0103(12) C11 0.0389(14) 0.0397(15) 0.0496(16) -0.0165(13) 0.0021(12) -0.0137(12) C12 0.0377(14) 0.0290(13) 0.0365(14) -0.0085(11) 0.0012(11) -0.0069(11) C13 0.0418(16) 0.067(2) 0.0365(15) -0.0021(14) -0.0045(12) -0.0161(14) C14 0.0370(15) 0.062(2) 0.0441(16) -0.0061(14) -0.0011(12) -0.0178(14) C15 0.0497(17) 0.059(2) 0.0548(17) -0.0321(16) 0.0056(13) -0.0145(14) C16 0.0759(17) 0.0458(14) 0.0861(18) -0.0301(13) 0.0132(14) -0.0170(12) C17 0.0759(17) 0.0458(14) 0.0861(18) -0.0301(13) 0.0132(14) -0.0170(12) C18 0.0503(19) 0.110(3) 0.130(3) -0.097(3) 0.017(2) -0.0163(19) C19 0.079(2) 0.084(3) 0.116(3) -0.070(3) 0.030(2) -0.042(2) C20 0.0502(19) 0.082(3) 0.098(3) -0.067(2) 0.0213(19) -0.0194(18) C21 0.087(3) 0.078(3) 0.100(3) -0.058(2) 0.015(2) -0.029(2) C22 0.0472(16) 0.0459(17) 0.0402(15) -0.0158(13) 0.0063(12) -0.0148(13) C23 0.0547(17) 0.0560(19) 0.0445(16) -0.0222(14) 0.0030(13) -0.0218(15) C24 0.0658(19) 0.072(2) 0.0429(16) -0.0241(16) 0.0168(14) -0.0323(17) C25 0.0372(15) 0.0444(17) 0.0633(18) -0.0166(14) 0.0097(13) -0.0113(12) C26 0.0378(15) 0.0409(17) 0.0517(17) -0.0062(13) -0.0011(12) -0.0058(12) C27 0.0339(14) 0.0423(16) 0.0445(15) -0.0104(13) 0.0078(11) -0.0119(12) C28 0.0375(15) 0.0490(18) 0.0553(17) -0.0140(14) -0.0026(12) -0.0133(13) S1 0.0381(4) 0.0318(4) 0.0426(4) -0.0098(3) 0.0064(3) -0.0074(3) O2W 0.112(6) 0.112(6) 0.060(4) -0.026(4) 0.004(4) -0.048(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 N3 2.0510(19) . ? Ni1 O4 2.0540(16) 2_557 ? Ni1 O1W 2.0568(18) . ? Ni1 N1 2.056(2) . ? Ni1 O2 2.0990(16) . ? Ni1 O1 2.2228(17) . ? O1 C1 1.253(3) . ? O2 C1 1.264(3) . ? O3 C8 1.235(3) . ? O4 C8 1.260(3) . ? O4 Ni1 2.0539(16) 2_557 ? O5 S1 1.4315(17) . ? O6 S1 1.4303(18) . ? N1 C15 1.321(3) . ? N1 C16 1.367(4) . ? N2 C15 1.345(4) . ? N2 C17 1.350(4) . ? N2 C18 1.473(3) . ? N3 C22 1.320(3) . ? N3 C23 1.362(3) . ? N4 C22 1.336(3) . ? N4 C24 1.360(3) . ? N4 C25 1.461(3) . ? O1W H1WA 0.836(17) . ? O1W H1WB 0.837(18) . ? C1 C2 1.491(3) . ? C2 C3 1.376(3) . ? C2 C7 1.383(3) . ? C3 C4 1.369(4) . ? C3 H3 0.9300 . ? C4 C5 1.374(3) . ? C4 H4 0.9300 . ? C5 C6 1.361(3) . ? C5 S1 1.767(2) . ? C6 C7 1.378(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.506(3) . ? C9 C14 1.376(3) . ? C9 C10 1.384(3) . ? C10 C11 1.374(3) . ? C10 H10 0.9300 . ? C11 C12 1.375(3) . ? C11 H11 0.9300 . ? C12 C13 1.378(3) . ? C12 S1 1.756(2) . ? C13 C14 1.370(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.336(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C20 1.511(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.350(5) . ? C19 C21 1.387(4) 2_577 ? C19 H19 0.9300 . ? C20 C21 1.383(5) . ? C21 C19 1.387(4) 2_577 ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.339(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C27 1.504(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C28 1.372(4) 2_676 ? C26 C27 1.378(3) . ? C26 H26 0.9300 . ? C27 C28 1.378(4) . ? C28 C26 1.372(4) 2_676 ? C28 H28 0.9300 . ? 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 N3 Ni1 O4 173.06(8) . 2_557 ? N3 Ni1 O1W 92.96(8) . . ? O4 Ni1 O1W 93.93(8) 2_557 . ? N3 Ni1 N1 92.20(8) . . ? O4 Ni1 N1 88.37(8) 2_557 . ? O1W Ni1 N1 92.48(8) . . ? N3 Ni1 O2 90.00(7) . . ? O4 Ni1 O2 88.59(7) 2_557 . ? O1W Ni1 O2 94.51(7) . . ? N1 Ni1 O2 172.56(7) . . ? N3 Ni1 O1 88.23(7) . . ? O4 Ni1 O1 85.14(7) 2_557 . ? O1W Ni1 O1 155.42(7) . . ? N1 Ni1 O1 112.03(7) . . ? O2 Ni1 O1 60.92(6) . . ? C1 O1 Ni1 86.26(14) . . ? C1 O2 Ni1 91.55(14) . . ? C8 O4 Ni1 125.98(16) . 2_557 ? C15 N1 C16 105.3(2) . . ? C15 N1 Ni1 126.5(2) . . ? C16 N1 Ni1 126.58(19) . . ? C15 N2 C17 107.3(2) . . ? C15 N2 C18 125.0(3) . . ? C17 N2 C18 127.7(3) . . ? C22 N3 C23 105.2(2) . . ? C22 N3 Ni1 124.15(17) . . ? C23 N3 Ni1 130.47(17) . . ? C22 N4 C24 106.3(2) . . ? C22 N4 C25 125.5(2) . . ? C24 N4 C25 128.1(2) . . ? Ni1 O1W H1WA 126(2) . . ? Ni1 O1W H1WB 97(2) . . ? H1WA O1W H1WB 104(3) . . ? O1 C1 O2 121.2(2) . . ? O1 C1 C2 119.9(2) . . ? O2 C1 C2 118.9(2) . . ? C3 C2 C7 118.1(2) . . ? C3 C2 C1 121.6(2) . . ? C7 C2 C1 120.3(2) . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 120.6(2) . . ? C6 C5 S1 119.53(19) . . ? C4 C5 S1 119.9(2) . . ? C5 C6 C7 119.6(2) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 120.9(2) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? O3 C8 O4 125.6(2) . . ? O3 C8 C9 117.3(2) . . ? O4 C8 C9 117.1(2) . . ? C14 C9 C10 119.0(2) . . ? C14 C9 C8 121.5(2) . . ? C10 C9 C8 119.5(2) . . ? C11 C10 C9 120.6(2) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.5(2) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.5(2) . . ? C11 C12 S1 119.93(18) . . ? C13 C12 S1 119.53(19) . . ? C14 C13 C12 119.5(2) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C9 120.9(2) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? N1 C15 N2 110.6(3) . . ? N1 C15 H15 124.7 . . ? N2 C15 H15 124.7 . . ? C17 C16 N1 109.8(3) . . ? C17 C16 H16 125.1 . . ? N1 C16 H16 125.1 . . ? C16 C17 N2 106.9(3) . . ? C16 C17 H17 126.5 . . ? N2 C17 H17 126.5 . . ? N2 C18 C20 113.3(2) . . ? N2 C18 H18A 108.9 . . ? C20 C18 H18A 108.9 . . ? N2 C18 H18B 108.9 . . ? C20 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C20 C19 C21 122.0(3) . 2_577 ? C20 C19 H19 119.0 . . ? C21 C19 H19 119.0 2_577 . ? C19 C20 C21 118.6(3) . . ? C19 C20 C18 120.5(3) . . ? C21 C20 C18 120.9(4) . . ? C20 C21 C19 119.4(4) . 2_577 ? C20 C21 H21 120.3 . . ? C19 C21 H21 120.3 2_577 . ? N3 C22 N4 111.7(2) . . ? N3 C22 H22 124.1 . . ? N4 C22 H22 124.1 . . ? C24 C23 N3 109.6(2) . . ? C24 C23 H23 125.2 . . ? N3 C23 H23 125.2 . . ? C23 C24 N4 107.2(2) . . ? C23 C24 H24 126.4 . . ? N4 C24 H24 126.4 . . ? N4 C25 C27 114.0(2) . . ? N4 C25 H25A 108.7 . . ? C27 C25 H25A 108.7 . . ? N4 C25 H25B 108.7 . . ? C27 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C28 C26 C27 120.9(2) 2_676 . ? C28 C26 H26 119.6 2_676 . ? C27 C26 H26 119.6 . . ? C26 C27 C28 117.7(2) . . ? C26 C27 C25 119.0(2) . . ? C28 C27 C25 123.3(2) . . ? C26 C28 C27 121.5(2) 2_676 . ? C26 C28 H28 119.3 2_676 . ? C27 C28 H28 119.3 . . ? O6 S1 O5 119.75(11) . . ? O6 S1 C12 108.37(11) . . ? O5 S1 C12 108.25(11) . . ? O6 S1 C5 108.22(11) . . ? O5 S1 C5 107.34(11) . . ? C12 S1 C5 103.77(11) . . ? 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 N3 Ni1 O1 C1 -91.67(14) . . . . ? O4 Ni1 O1 C1 90.41(14) 2_557 . . . ? O1W Ni1 O1 C1 1.6(2) . . . . ? N1 Ni1 O1 C1 176.67(13) . . . . ? O2 Ni1 O1 C1 -0.69(12) . . . . ? N3 Ni1 O2 C1 88.66(14) . . . . ? O4 Ni1 O2 C1 -84.54(13) 2_557 . . . ? O1W Ni1 O2 C1 -178.37(13) . . . . ? N1 Ni1 O2 C1 -18.6(6) . . . . ? O1 Ni1 O2 C1 0.68(12) . . . . ? N3 Ni1 N1 C15 -167.8(2) . . . . ? O4 Ni1 N1 C15 5.3(2) 2_557 . . . ? O1W Ni1 N1 C15 99.1(2) . . . . ? O2 Ni1 N1 C15 -60.7(6) . . . . ? O1 Ni1 N1 C15 -78.8(2) . . . . ? N3 Ni1 N1 C16 28.5(2) . . . . ? O4 Ni1 N1 C16 -158.4(2) 2_557 . . . ? O1W Ni1 N1 C16 -64.6(2) . . . . ? O2 Ni1 N1 C16 135.6(5) . . . . ? O1 Ni1 N1 C16 117.5(2) . . . . ? O4 Ni1 N3 C22 -30.9(7) 2_557 . . . ? O1W Ni1 N3 C22 156.4(2) . . . . ? N1 Ni1 N3 C22 63.8(2) . . . . ? O2 Ni1 N3 C22 -109.1(2) . . . . ? O1 Ni1 N3 C22 -48.2(2) . . . . ? O4 Ni1 N3 C23 143.2(5) 2_557 . . . ? O1W Ni1 N3 C23 -29.6(2) . . . . ? N1 Ni1 N3 C23 -122.2(2) . . . . ? O2 Ni1 N3 C23 64.9(2) . . . . ? O1 Ni1 N3 C23 125.8(2) . . . . ? Ni1 O1 C1 O2 1.2(2) . . . . ? Ni1 O1 C1 C2 -178.0(2) . . . . ? Ni1 O2 C1 O1 -1.2(2) . . . . ? Ni1 O2 C1 C2 177.90(19) . . . . ? O1 C1 C2 C3 2.1(4) . . . . ? O2 C1 C2 C3 -177.1(2) . . . . ? O1 C1 C2 C7 -178.9(2) . . . . ? O2 C1 C2 C7 1.9(3) . . . . ? C7 C2 C3 C4 -0.6(4) . . . . ? C1 C2 C3 C4 178.4(3) . . . . ? C2 C3 C4 C5 -1.0(5) . . . . ? C3 C4 C5 C6 2.1(4) . . . . ? C3 C4 C5 S1 -178.3(2) . . . . ? C4 C5 C6 C7 -1.6(4) . . . . ? S1 C5 C6 C7 178.8(2) . . . . ? C5 C6 C7 C2 0.0(4) . . . . ? C3 C2 C7 C6 1.1(4) . . . . ? C1 C2 C7 C6 -177.9(2) . . . . ? Ni1 O4 C8 O3 1.1(4) 2_557 . . . ? Ni1 O4 C8 C9 -178.48(15) 2_557 . . . ? O3 C8 C9 C14 175.7(3) . . . . ? O4 C8 C9 C14 -4.7(4) . . . . ? O3 C8 C9 C10 -3.3(3) . . . . ? O4 C8 C9 C10 176.3(2) . . . . ? C14 C9 C10 C11 0.8(4) . . . . ? C8 C9 C10 C11 179.9(2) . . . . ? C9 C10 C11 C12 0.4(4) . . . . ? C10 C11 C12 C13 -1.2(4) . . . . ? C10 C11 C12 S1 178.15(19) . . . . ? C11 C12 C13 C14 0.8(4) . . . . ? S1 C12 C13 C14 -178.6(2) . . . . ? C12 C13 C14 C9 0.5(4) . . . . ? C10 C9 C14 C13 -1.3(4) . . . . ? C8 C9 C14 C13 179.7(2) . . . . ? C16 N1 C15 N2 -0.5(3) . . . . ? Ni1 N1 C15 N2 -167.05(16) . . . . ? C17 N2 C15 N1 0.6(3) . . . . ? C18 N2 C15 N1 179.5(2) . . . . ? C15 N1 C16 C17 0.3(3) . . . . ? Ni1 N1 C16 C17 166.8(2) . . . . ? N1 C16 C17 N2 0.1(4) . . . . ? C15 N2 C17 C16 -0.4(3) . . . . ? C18 N2 C17 C16 -179.2(3) . . . . ? C15 N2 C18 C20 99.5(4) . . . . ? C17 N2 C18 C20 -81.9(4) . . . . ? C21 C19 C20 C21 -1.2(6) 2_577 . . . ? C21 C19 C20 C18 -179.9(3) 2_577 . . . ? N2 C18 C20 C19 -95.5(4) . . . . ? N2 C18 C20 C21 85.9(4) . . . . ? C19 C20 C21 C19 1.2(5) . . . 2_577 ? C18 C20 C21 C19 179.9(3) . . . 2_577 ? C23 N3 C22 N4 0.4(3) . . . . ? Ni1 N3 C22 N4 175.73(16) . . . . ? C24 N4 C22 N3 0.0(3) . . . . ? C25 N4 C22 N3 176.6(2) . . . . ? C22 N3 C23 C24 -0.7(3) . . . . ? Ni1 N3 C23 C24 -175.6(2) . . . . ? N3 C23 C24 N4 0.7(3) . . . . ? C22 N4 C24 C23 -0.4(3) . . . . ? C25 N4 C24 C23 -176.9(2) . . . . ? C22 N4 C25 C27 -79.8(3) . . . . ? C24 N4 C25 C27 96.0(3) . . . . ? C28 C26 C27 C28 -0.4(4) 2_676 . . . ? C28 C26 C27 C25 178.1(2) 2_676 . . . ? N4 C25 C27 C26 150.2(2) . . . . ? N4 C25 C27 C28 -31.4(4) . . . . ? C26 C27 C28 C26 0.4(4) . . . 2_676 ? C25 C27 C28 C26 -178.0(2) . . . 2_676 ? C11 C12 S1 O6 10.2(2) . . . . ? C13 C12 S1 O6 -170.4(2) . . . . ? C11 C12 S1 O5 141.5(2) . . . . ? C13 C12 S1 O5 -39.1(2) . . . . ? C11 C12 S1 C5 -104.7(2) . . . . ? C13 C12 S1 C5 74.7(2) . . . . ? C6 C5 S1 O6 142.3(2) . . . . ? C4 C5 S1 O6 -37.2(2) . . . . ? C6 C5 S1 O5 11.8(2) . . . . ? C4 C5 S1 O5 -167.8(2) . . . . ? C6 C5 S1 C12 -102.7(2) . . . . ? C4 C5 S1 C12 77.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.354 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.057 #=======================END