Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name _publ_author_address 'Morten Ghiladi' ; Department of Chemistry University of Southern Denmark Odense Campus 5230 Odense M Denmark ; 'Jonnes T. Gomez' ; Department of Chemistry University of Southern Denmark Odense Campus 5230 Odense M Denmark ; 'Alan Hazell' ; Department of Chemistry Aarhus University Langelandsgade 140 DK-8000 \%Arhus C Denmark ; P.Kofod ; Department od Life Sciences and Chemistry Roskilde University 4000 Roskilde Denmark ; 'Jan Lumtscher' ; Department of Chemistry University of Southern Denmark Odense Campus 5230 Odense M Denmark ; 'Christine J. McKenzie' ; Department of Chemistry University of Southern Denmark Odense Campus 5230 Odense M Denmark ; _publ_contact_author_name 'Dr Pauli Kofod' _publ_contact_author_address ; Department of Life Sciences & Chemistry Roskilde University POB 260 Roskilde DK-4000 DENMARK ; _publ_contact_author_email pkofod@ruc.dk #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; H3O2-, O22- and O2.- bridging ligands in cobalt(III) complexes of an acyclic phenolate-hinged dinucleating ligand. ; data_c8ac _database_code_CSD 195394 #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; insert name here ; _chemical_name_common [Co2(bpbp)(O2)(CH3CO2)](ClO4)2 _chemical_formula_sum 'C38 H42 Cl2 Co2 N6 O13' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety 'C38 H42 Co2 N6 O5, 2(Cl O4)' _chemical_formula_weight 979.600 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z +x,-y,1/2+z -x,-y,-z -x,+y,1/2-z 1/2+x,1/2+y,+z 1/2+x,1/2-y,1/2+z 1/2-x,1/2-y,-z 1/2-x,1/2+y,1/2-z _cell_length_a 36.018(2) _cell_length_b 10.1931(6) _cell_length_c 21.971(1) _cell_angle_alpha 90 _cell_angle_beta 94.602(1) _cell_angle_gamma 90 _cell_volume 8040(1) _cell_formula_units_Z 8 _cell_measurement_temperature 120 _cell_measurement_reflns_used 6819 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 26.8 _exptl_crystal_description lath _exptl_crystal_colour dark_green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'XPREP (Siemens, 1995)' _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.949 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method ; \w rotation scans with narrow frames ; _diffrn_reflns_number 41749 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_theta_max 26.8 _diffrn_reflns_reduction_process 41749 _reflns_number_total 7789 _reflns_number_gt 6008 _reflns_threshold_expression I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; 1/{[\s~cs~(F^2^)+B +(1+A)F^2^]^1/2^-|F|}^2^ A = 0.02, B = 2.0 ; _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6007 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_ref 0.041 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.00004 _refine_diff_density_max 0.78(8) _refine_diff_density_min -0.80(8) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Co1 0.17269(1) 0.12027(4) 0.64206(2) 0.0127(2) Uij Co2 0.15464(1) -0.15492(4) 0.69988(2) 0.0129(2) Uij O1 0.13696(5) -0.0143(2) 0.64899(9) 0.014(1) Uij O2 0.20052(6) 0.0573(2) 0.71175(9) 0.016(1) Uij O3 0.20098(6) 0.0026(2) 0.59586(9) 0.016(1) Uij O4 0.17860(6) -0.0232(2) 0.74774(9) 0.016(1) Uij O5 0.19486(6) -0.1848(2) 0.65016(9) 0.016(1) Uij N11 0.20800(7) 0.2515(2) 0.6220(1) 0.017(1) Uij N21 0.14430(7) 0.2446(2) 0.6849(1) 0.015(1) Uij N31 0.17351(7) -0.2889(2) 0.7562(1) 0.017(1) Uij N41 0.12085(7) -0.2723(2) 0.6457(1) 0.017(1) Uij N51 0.14374(7) 0.1894(2) 0.5659(1) 0.015(1) Uij N61 0.11294(7) -0.1526(2) 0.7525(1) 0.015(1) Uij C1 0.20842(8) -0.1161(3) 0.6090(1) 0.016(2) Uij C2 0.23573(9) -0.1855(3) 0.5723(1) 0.022(2) Uij C12 0.23457(9) 0.3052(3) 0.6601(1) 0.020(2) Uij C13 0.25890(9) 0.3985(3) 0.6409(2) 0.024(2) Uij C14 0.25563(10) 0.4366(3) 0.5800(2) 0.027(2) Uij C15 0.22795(10) 0.3808(3) 0.5404(1) 0.025(2) Uij C16 0.20432(9) 0.2880(3) 0.5622(1) 0.019(2) Uij C17 0.17296(9) 0.2222(3) 0.5244(1) 0.019(2) Uij C22 0.14480(8) 0.2545(3) 0.7464(1) 0.016(2) Uij C23 0.11799(9) 0.3250(3) 0.7741(1) 0.019(2) Uij C24 0.08912(10) 0.3822(3) 0.7383(1) 0.023(2) Uij C25 0.08911(9) 0.3750(3) 0.6750(1) 0.021(2) Uij C26 0.11790(9) 0.3101(3) 0.6498(1) 0.017(2) Uij C27 0.12388(9) 0.3112(3) 0.5830(1) 0.018(2) Uij C32 0.19960(9) -0.3787(3) 0.7466(1) 0.019(2) Uij C33 0.21032(9) -0.4734(3) 0.7897(2) 0.022(2) Uij C34 0.19283(9) -0.4771(3) 0.8435(1) 0.022(2) Uij C35 0.16572(9) -0.3844(3) 0.8537(1) 0.020(2) Uij C36 0.15726(8) -0.2896(3) 0.8099(1) 0.018(2) Uij C37 0.12997(9) -0.1798(3) 0.8154(1) 0.017(2) Uij C42 0.12535(9) -0.3038(3) 0.5873(1) 0.020(2) Uij C43 0.09663(10) -0.3532(3) 0.5485(1) 0.023(2) Uij C44 0.06168(10) -0.3659(3) 0.5696(1) 0.025(2) Uij C45 0.05641(9) -0.3311(3) 0.6295(1) 0.021(2) Uij C46 0.08684(9) -0.2877(3) 0.6665(1) 0.018(2) Uij C47 0.08598(9) -0.2602(3) 0.7334(1) 0.018(2) Uij C52 0.11589(8) 0.0913(3) 0.5382(1) 0.017(2) Uij C53 0.08727(8) 0.0667(3) 0.5830(1) 0.015(2) Uij C54 0.04991(8) 0.1014(3) 0.5729(1) 0.016(2) Uij C55 0.02513(8) 0.0859(3) 0.6177(1) 0.017(2) Uij C56 -0.01669(9) 0.1145(3) 0.6068(1) 0.020(2) Uij C57 -0.02948(9) 0.2060(3) 0.6565(2) 0.027(2) Uij C58 -0.02660(9) 0.1792(4) 0.5448(2) 0.030(2) Uij C59 -0.03766(9) -0.0170(4) 0.6081(2) 0.027(2) Uij C62 0.09298(8) -0.0245(3) 0.7506(1) 0.015(2) Uij C63 0.07675(8) 0.0089(3) 0.6873(1) 0.015(2) Uij C64 0.03939(9) 0.0398(3) 0.6747(1) 0.017(2) Uij C65 0.10005(8) 0.0177(3) 0.6401(1) 0.014(1) Uij Cl1 0.06091(2) 0.40392(8) 0.40596(4) 0.0257(4) Uij Cl2 0.16067(2) 0.81028(9) 0.42705(4) 0.0285(5) Uij O6 0.04441(10) 0.3467(4) 0.3516(1) 0.067(2) Uij O7 0.08854(9) 0.3173(3) 0.4344(1) 0.050(2) Uij O9 0.07972(10) 0.5215(3) 0.3929(2) 0.089(3) Uij O10 0.03326(10) 0.4328(5) 0.4454(2) 0.086(3) Uij O11 0.16595(10) 0.6772(3) 0.4506(2) 0.059(2) Uij O12 0.18200(7) 0.8238(3) 0.3752(1) 0.038(2) Uij O13 0.17447(7) 0.8981(3) 0.4742(1) 0.037(2) Uij O14 0.12229(8) 0.8326(4) 0.4113(2) 0.071(2) Uij H2a 0.24841 -0.2509 0.5967 0.026 Uiso H2b 0.25324 -0.1241 0.5591 0.026 Uiso H2c 0.22290 -0.2257 0.5376 0.026 Uiso H12 0.23679 0.2784 0.7016 0.024 Uiso H13 0.27748 0.4359 0.6688 0.029 Uiso H14 0.27211 0.5002 0.5656 0.033 Uiso H15 0.22530 0.4062 0.4987 0.030 Uiso H17a 0.16316 0.2799 0.4931 0.023 Uiso H17b 0.18170 0.1444 0.5064 0.023 Uiso H22 0.16403 0.2120 0.7711 0.019 Uiso H23 0.11943 0.3340 0.8173 0.023 Uiso H24 0.06954 0.4258 0.7566 0.027 Uiso H25 0.06961 0.4141 0.6496 0.025 Uiso H27a 0.10044 0.3157 0.5599 0.022 Uiso H27b 0.13841 0.3856 0.5742 0.022 Uiso H32 0.21107 -0.3774 0.7091 0.023 Uiso H33 0.22935 -0.5346 0.7825 0.026 Uiso H34 0.19931 -0.5426 0.8733 0.026 Uiso H35 0.15324 -0.3862 0.8902 0.024 Uiso H37a 0.11129 -0.2053 0.8412 0.021 Uiso H37b 0.14244 -0.1040 0.8318 0.021 Uiso H42 0.14910 -0.2917 0.5722 0.024 Uiso H43 0.10084 -0.3782 0.5079 0.028 Uiso H44 0.04143 -0.3980 0.5435 0.029 Uiso H45 0.03249 -0.3371 0.6446 0.026 Uiso H47a 0.06155 -0.2341 0.7416 0.022 Uiso H47b 0.09263 -0.3376 0.7558 0.022 Uiso H52a 0.12821 0.0117 0.5299 0.020 Uiso H52b 0.10413 0.1255 0.5013 0.020 Uiso H54 0.04112 0.1365 0.5343 0.019 Uiso H57a -0.05538 0.2237 0.6498 0.032 Uiso H57b -0.01606 0.2862 0.6558 0.032 Uiso H57c -0.02467 0.1654 0.6952 0.032 Uiso H58a -0.05251 0.1969 0.5381 0.036 Uiso H58b -0.01947 0.1222 0.5136 0.036 Uiso H58c -0.01331 0.2595 0.5432 0.036 Uiso H59a -0.06356 0.0007 0.6013 0.032 Uiso H59b -0.03257 -0.0580 0.6467 0.032 Uiso H59c -0.03001 -0.0731 0.5769 0.032 Uiso H62a 0.11002 0.0424 0.7643 0.018 Uiso H62b 0.07338 -0.0289 0.7770 0.018 Uiso H64 0.02291 0.0291 0.7060 0.021 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0125(2) 0.0134(2) 0.0119(2) 0.0000(2) -0.0014(1) -0.0005(2) Co2 0.0123(2) 0.0125(2) 0.0137(2) 0.0019(2) -0.0007(1) 0.0008(2) O1 0.010(1) 0.014(1) 0.018(1) 0.002(1) -0.001(1) 0.000(1) O2 0.015(1) 0.018(1) 0.014(1) -0.003(1) -0.001(1) 0.002(1) O3 0.015(1) 0.018(1) 0.015(1) -0.001(1) 0.000(1) 0.000(1) O4 0.016(1) 0.017(1) 0.014(1) -0.002(1) 0.000(1) 0.002(1) O5 0.014(1) 0.016(1) 0.018(1) 0.002(1) 0.002(1) -0.001(1) N11 0.017(1) 0.017(1) 0.016(1) 0.002(1) -0.001(1) -0.001(1) N21 0.017(1) 0.012(1) 0.014(1) -0.001(1) -0.001(1) 0.000(1) N31 0.017(1) 0.014(1) 0.018(1) 0.001(1) -0.002(1) 0.000(1) N41 0.019(1) 0.012(1) 0.018(1) 0.001(1) -0.002(1) 0.001(1) N51 0.015(1) 0.015(1) 0.014(1) -0.002(1) 0.000(1) 0.000(1) N61 0.016(1) 0.015(1) 0.013(1) 0.001(1) 0.000(1) 0.003(1) C1 0.011(2) 0.020(2) 0.017(2) -0.001(1) -0.002(1) -0.003(1) C2 0.019(2) 0.023(2) 0.025(2) 0.001(1) 0.005(1) -0.003(1) C12 0.017(2) 0.019(2) 0.022(2) 0.004(1) -0.002(1) -0.004(1) C13 0.018(2) 0.021(2) 0.032(2) -0.003(1) -0.002(1) -0.005(1) C14 0.023(2) 0.025(2) 0.035(2) -0.005(1) 0.003(1) 0.001(1) C15 0.024(2) 0.024(2) 0.025(2) -0.008(1) 0.004(1) 0.003(1) C16 0.019(2) 0.019(2) 0.018(2) 0.000(1) 0.000(1) 0.000(1) C17 0.020(2) 0.022(2) 0.014(2) -0.006(1) 0.001(1) 0.003(1) C22 0.018(2) 0.014(1) 0.016(2) -0.002(1) -0.001(1) 0.000(1) C23 0.026(2) 0.014(2) 0.017(2) -0.004(1) 0.004(1) -0.001(1) C24 0.029(2) 0.014(2) 0.025(2) 0.002(1) 0.008(1) -0.001(1) C25 0.024(2) 0.012(1) 0.026(2) 0.004(1) -0.001(1) 0.002(1) C26 0.021(2) 0.008(1) 0.021(2) -0.002(1) -0.001(1) 0.001(1) C27 0.022(2) 0.014(1) 0.019(2) 0.001(1) -0.003(1) 0.003(1) C32 0.014(2) 0.015(2) 0.027(2) 0.002(1) -0.001(1) -0.001(1) C33 0.017(2) 0.016(2) 0.031(2) 0.004(1) -0.003(1) 0.001(1) C34 0.020(2) 0.017(2) 0.028(2) -0.001(1) -0.006(1) 0.008(1) C35 0.019(2) 0.021(2) 0.019(2) 0.001(1) -0.003(1) 0.005(1) C36 0.014(2) 0.019(2) 0.019(2) 0.000(1) -0.003(1) 0.001(1) C37 0.018(2) 0.019(2) 0.014(1) 0.002(1) 0.000(1) 0.003(1) C42 0.027(2) 0.014(2) 0.019(2) 0.002(1) -0.001(1) 0.001(1) C43 0.032(2) 0.017(2) 0.020(2) -0.002(1) -0.006(1) 0.001(1) C44 0.030(2) 0.016(2) 0.026(2) -0.005(1) -0.012(1) 0.006(1) C45 0.020(2) 0.018(2) 0.024(2) -0.002(1) -0.004(1) 0.006(1) C46 0.019(2) 0.011(1) 0.022(2) 0.000(1) -0.001(1) 0.004(1) C47 0.017(2) 0.016(2) 0.022(2) 0.001(1) 0.001(1) 0.003(1) C52 0.016(2) 0.016(2) 0.016(2) -0.002(1) -0.003(1) -0.001(1) C53 0.015(2) 0.013(1) 0.016(2) -0.001(1) -0.001(1) -0.003(1) C54 0.018(2) 0.014(1) 0.015(2) 0.002(1) -0.004(1) 0.000(1) C55 0.014(2) 0.015(2) 0.020(2) 0.004(1) -0.001(1) -0.002(1) C56 0.013(2) 0.028(2) 0.017(2) 0.007(1) -0.002(1) 0.001(1) C57 0.020(2) 0.030(2) 0.029(2) 0.011(1) -0.001(1) -0.001(1) C58 0.017(2) 0.046(2) 0.026(2) 0.009(2) -0.003(1) 0.009(2) C59 0.017(2) 0.035(2) 0.028(2) -0.001(1) 0.001(1) -0.002(1) C62 0.016(2) 0.015(1) 0.014(1) 0.005(1) 0.001(1) 0.002(1) C63 0.016(2) 0.012(1) 0.018(2) 0.003(1) 0.000(1) 0.000(1) C64 0.017(2) 0.017(2) 0.018(2) 0.003(1) 0.003(1) -0.001(1) C65 0.010(1) 0.011(1) 0.020(2) 0.001(1) -0.003(1) -0.002(1) Cl1 0.0274(5) 0.0230(4) 0.0278(4) 0.0010(3) 0.0085(3) -0.0026(3) Cl2 0.0141(4) 0.0443(5) 0.0271(4) -0.0059(4) 0.0027(3) -0.0178(4) O6 0.074(2) 0.089(3) 0.035(2) 0.027(2) -0.011(2) -0.024(2) O7 0.072(2) 0.041(2) 0.037(2) 0.014(2) -0.004(1) 0.014(1) O9 0.057(2) 0.051(2) 0.159(4) -0.011(2) -0.001(2) 0.057(2) O10 0.045(2) 0.147(4) 0.070(2) -0.009(2) 0.029(2) -0.054(3) O11 0.072(2) 0.031(2) 0.078(2) -0.006(2) 0.039(2) -0.011(2) O12 0.033(1) 0.064(2) 0.018(1) 0.002(1) 0.002(1) -0.007(1) O13 0.029(1) 0.047(2) 0.033(1) -0.006(1) 0.000(1) -0.018(1) O14 0.016(2) 0.116(3) 0.079(2) 0.007(2) -0.008(1) -0.045(2) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Co1 Co2 3.168(1) Co1 O1 1.895(2) Co1 O2 1.875(2) Co1 O3 1.916(2) Co1 N11 1.921(3) Co1 N21 1.922(2) Co1 N51 2.026(2) Co2 O1 1.896(2) Co2 O4 1.873(2) Co2 O5 1.908(2) Co2 N31 1.929(2) Co2 N41 2.024(2) Co2 N61 1.968(2) O1 C65 1.368(3) O2 O4 1.422(3) O3 C1 1.268(4) O5 C1 1.272(4) N11 C12 1.337(4) N11 C16 1.361(4) N21 C26 1.352(4) N21 C22 1.352(4) N31 C32 1.340(4) N31 C36 1.359(4) N41 C42 1.345(4) N41 C46 1.350(4) N51 C17 1.486(4) N51 C27 1.495(4) N51 C52 1.509(4) N61 C62 1.490(4) N61 C37 1.493(4) N61 C47 1.502(4) C1 C2 1.499(4) C12 C13 1.382(4) C13 C14 1.389(5) C14 C15 1.391(5) C15 C16 1.383(4) C16 C17 1.506(4) C22 C23 1.384(4) C23 C24 1.382(4) C24 C25 1.392(4) C25 C26 1.383(4) C26 C27 1.501(4) C32 C33 1.386(4) C33 C34 1.384(5) C34 C35 1.390(4) C35 C36 1.381(4) C36 C37 1.500(4) C42 C43 1.382(4) C43 C44 1.383(5) C44 C45 1.389(5) C45 C46 1.384(4) C46 C47 1.500(4) C52 C53 1.503(4) C53 C54 1.392(4) C53 C65 1.393(4) C54 C55 1.390(4) C55 C64 1.398(4) C55 C56 1.534(4) C56 C58 1.529(4) C56 C57 1.536(4) C56 C59 1.539(5) C62 C63 1.504(4) C63 C64 1.388(4) C63 C65 1.389(4) Cl1 O10 1.403(3) Cl1 O6 1.416(3) Cl1 O9 1.418(3) Cl1 O7 1.436(3) Cl2 O14 1.416(3) Cl2 O13 1.428(2) Cl2 O12 1.431(2) Cl2 O11 1.459(3) C2 H2a 0.950 C2 H2b 0.950 C2 H2c 0.950 C12 H12 0.950 C13 H13 0.950 C14 H14 0.950 C15 H15 0.950 C17 H17a 0.950 C17 H17b 0.950 C22 H22 0.950 C23 H23 0.950 C24 H24 0.950 C25 H25 0.950 C27 H27a 0.950 C27 H27b 0.950 C32 H32 0.950 C33 H33 0.950 C34 H34 0.950 C35 H35 0.950 C37 H37a 0.950 C37 H37b 0.950 C42 H42 0.950 C43 H43 0.950 C44 H44 0.950 C45 H45 0.950 C47 H47a 0.950 C47 H47b 0.950 C52 H52a 0.950 C52 H52b 0.950 C54 H54 0.950 C57 H57a 0.950 C57 H57b 0.950 C57 H57c 0.950 C58 H58a 0.950 C58 H58b 0.950 C58 H58c 0.950 C59 H59a 0.950 C59 H59b 0.950 C59 H59c 0.950 C62 H62a 0.950 C62 H62b 0.950 C64 H64 0.950 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Co1 O2 90.49(9) O1 Co1 O3 89.02(9) O1 Co1 N11 171.32(9) O1 Co1 N21 92.7(1) O1 Co1 N51 90.60(9) O2 Co1 O3 86.91(9) O2 Co1 N11 96.05(9) O2 Co1 N21 95.52(9) O2 Co1 N51 178.65(9) O3 Co1 N11 85.7(1) O3 Co1 N21 177.02(9) O3 Co1 N51 92.32(9) N11 Co1 N21 92.4(1) N11 Co1 N51 82.8(1) N21 Co1 N51 85.2(1) O1 Co2 O4 84.66(8) O4 Co2 O5 95.69(9) O4 Co2 N31 91.43(9) O4 Co2 N41 169.2(1) O4 Co2 N61 90.03(9) O1 Co2 O5 91.01(9) O1 Co2 N31 175.9(1) O1 Co2 N41 86.69(9) O1 Co2 N61 95.83(9) O5 Co2 N31 90.5(1) O5 Co2 N41 91.0(1) O5 Co2 N61 171.47(9) N31 Co2 N61 83.0(1) N31 Co2 N41 97.1(1) N41 Co2 N61 84.3(1) Co1 O1 C65 118.3(2) Co2 O1 C65 122.8(2) Co1 O1 Co2 113.4(1) Co1 O2 O4 111.5(1) Co2 O4 O2 110.7(1) Co1 O3 C1 126.1(2) Co2 O5 C1 132.2(2) Co1 N11 C12 126.5(2) Co1 N11 C16 113.4(2) Co1 N21 C22 125.0(2) Co1 N21 C26 115.0(2) Co2 N31 C32 126.7(2) Co2 N31 C36 114.0(2) Co2 N41 C42 126.1(2) Co2 N41 C46 112.9(2) Co1 N51 C17 104.1(2) Co1 N51 C27 107.9(2) Co1 N51 C52 112.6(2) Co2 N61 C37 105.4(2) Co2 N61 C47 109.5(2) Co2 N61 C62 112.5(2) C12 N11 C16 120.1(3) C22 N21 C26 119.0(3) C32 N31 C36 119.3(3) C42 N41 C46 118.5(3) C17 N51 C27 110.1(2) C17 N51 C52 112.4(2) C27 N51 C52 109.6(2) C37 N61 C62 110.5(2) C47 N61 C62 109.4(2) C37 N61 C47 109.4(2) O3 C1 O5 126.9(3) O3 C1 C2 117.7(3) O5 C1 C2 115.4(3) N11 C12 C13 122.0(3) C12 C13 C14 118.7(3) C13 C14 C15 119.3(3) C14 C15 C16 119.5(3) N11 C16 C15 120.4(3) N11 C16 C17 115.0(3) C15 C16 C17 124.6(3) N51 C17 C16 107.3(2) N21 C22 C23 121.7(3) C22 C23 C24 119.2(3) C23 C24 C25 119.1(3) C24 C25 C26 119.0(3) N21 C26 C25 121.5(3) N21 C26 C27 114.4(3) C25 C26 C27 124.0(3) N51 C27 C26 110.3(2) N31 C32 C33 121.9(3) C32 C33 C34 118.9(3) C33 C34 C35 119.5(3) C34 C35 C36 118.9(3) N31 C36 C35 121.5(3) N31 C36 C37 113.4(2) C35 C36 C37 125.1(3) N61 C37 C36 106.6(2) N41 C42 C43 122.3(3) C42 C43 C44 118.9(3) C43 C44 C45 119.5(3) C44 C45 C46 118.4(3) N41 C46 C45 122.4(3) N41 C46 C47 113.6(3) C45 C46 C47 123.9(3) N61 C47 C46 110.3(2) N51 C52 C53 108.4(2) C54 C53 C65 118.7(3) C52 C53 C54 123.9(3) C52 C53 C65 117.1(3) C53 C54 C55 121.7(3) C54 C55 C64 117.6(3) C54 C55 C56 123.1(3) C56 C55 C64 119.3(3) C55 C56 C58 112.2(3) C57 C56 C58 108.0(3) C58 C56 C59 108.2(3) C55 C56 C57 110.6(2) C55 C56 C59 108.0(3) C57 C56 C59 109.9(3) N61 C62 C63 112.1(2) C64 C63 C65 118.0(3) C62 C63 C64 122.3(3) C62 C63 C65 119.5(3) C55 C64 C63 122.4(3) O1 C65 C63 121.1(3) O1 C65 C53 117.5(3) C53 C65 C63 121.3(3) O6 Cl1 O10 109.7(2) O9 Cl1 O10 108.8(3) O7 Cl1 O10 111.2(2) O6 Cl1 O9 110.6(3) O6 Cl1 O7 110.1(2) O7 Cl1 O9 106.4(2) O13 Cl2 O14 110.6(2) O12 Cl2 O14 111.5(2) O11 Cl2 O14 109.5(2) O12 Cl2 O13 109.8(2) O11 Cl2 O13 107.3(2) O11 Cl2 O12 108.0(2) H2a C2 H2b 109.5 H2a C2 H2c 109.4 C1 C2 H2a 109.4 H2b C2 H2c 109.4 C1 C2 H2b 109.4 C1 C2 H2c 109.7 N11 C12 H12 119.0 C13 C12 H12 119.0 C12 C13 H13 120.7 C14 C13 H13 120.7 C13 C14 H14 120.4 C15 C14 H14 120.4 C16 C15 H15 120.2 C14 C15 H15 120.2 H17a C17 H17b 109.5 N51 C17 H17a 110.0 C16 C17 H17a 110.0 N51 C17 H17b 110.0 C16 C17 H17b 110.0 N21 C22 H22 119.2 C23 C22 H22 119.2 C24 C23 H23 120.4 C22 C23 H23 120.4 C23 C24 H24 120.4 C25 C24 H24 120.4 C26 C25 H25 120.5 C24 C25 H25 120.5 H27a C27 H27b 109.5 N51 C27 H27a 109.3 C26 C27 H27a 109.3 N51 C27 H27b 109.3 C26 C27 H27b 109.3 N31 C32 H32 119.1 C33 C32 H32 119.1 C34 C33 H33 120.6 C32 C33 H33 120.6 C33 C34 H34 120.3 C35 C34 H34 120.3 C36 C35 H35 120.6 C34 C35 H35 120.6 H37a C37 H37b 109.5 N61 C37 H37a 110.2 C36 C37 H37a 110.2 N61 C37 H37b 110.2 C36 C37 H37b 110.2 N41 C42 H42 118.9 C43 C42 H42 118.9 C42 C43 H43 120.6 C44 C43 H43 120.6 C43 C44 H44 120.3 C45 C44 H44 120.3 C46 C45 H45 120.8 C44 C45 H45 120.8 H47a C47 H47b 109.5 C46 C47 H47a 109.3 N61 C47 H47a 109.3 C46 C47 H47b 109.3 N61 C47 H47b 109.3 H52a C52 H52b 109.5 C53 C52 H52a 109.7 N51 C52 H52a 109.7 C53 C52 H52b 109.7 N51 C52 H52b 109.7 C55 C54 H54 119.2 C53 C54 H54 119.2 H57a C57 H57b 109.2 H57a C57 H57c 109.2 C56 C57 H57a 110.6 H57b C57 H57c 109.5 C56 C57 H57b 109.2 C56 C57 H57c 109.2 H58a C58 H58b 108.8 H58a C58 H58c 108.8 C56 C58 H58a 112.2 H58b C58 H58c 109.5 C56 C58 H58b 108.8 C56 C58 H58c 108.8 H59a C59 H59b 109.8 H59a C59 H59c 109.8 C56 C59 H59a 108.0 H59b C59 H59c 109.5 C56 C59 H59b 109.8 C56 C59 H59c 109.8 H62a C62 H62b 109.5 N61 C62 H62a 108.8 C63 C62 H62a 108.8 N61 C62 H62b 108.8 C63 C62 H62b 108.8 C63 C64 H64 118.8 C55 C64 H64 118.8 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 Co1 O2 O4 Co2 52.1(2) #============================================================================== data_newmc _database_code_CSD 195395 # compound 3.2H2O #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; insert name here ; _chemical_name_common [Co2(C36H39N6O)(OH)2(H2O)2](ClO4)3.2H2O _chemical_formula_sum 'C36 H49 Cl3 Co2 N6 O19' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety 'C36 H45 Co2 N6 O5,3(Cl O4), 2(H2 O)' _chemical_formula_weight 1094.04 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _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 11.7233(6) _cell_length_b 13.2960(7) _cell_length_c 16.0808(8) _cell_angle_alpha 108.857(1) _cell_angle_beta 90.455(1) _cell_angle_gamma 112.061(1) _cell_volume 2174.3(1) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8143 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 28.4 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'XPREP (Siemens, 1995)' _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 0.866 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames ' _diffrn_standards_decay_% 0 _diffrn_reflns_number 12051 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_theta_max 28.4 _diffrn_reflns_reduction_process 12051 _reflns_number_total 8241 _reflns_number_gt 6850 _reflns_threshold_expression I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1/{[\s~cs~(F^2^)+B+(1+A)F^2^]^1/2^-|F|}^2^ A = 0.0, B = 1.5 ; _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method ; none ; _refine_ls_number_reflns 6850 _refine_ls_number_parameters 619 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.067 _refine_ls_wR_factor_ref 0.052 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_shift/su_max 0.0037 _refine_ls_shift/su_mean 0.00008 _refine_diff_density_max 1.0(2) _refine_diff_density_min -0.7(2) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type Co1 Co 0.71459(7) 0.42782(6) 0.58826(5) 0.0280(5) Uij Co2 Co 0.89017(7) 0.73228(6) 0.70758(5) 0.0291(5) Uij O1 O 0.7952(3) 0.5683(3) 0.6951(2) 0.027(2) Uij O2 O 0.6414(5) 0.5113(4) 0.5486(3) 0.032(3) Uij O3 O 0.8594(4) 0.4809(3) 0.5344(3) 0.030(3) Uij O4 O 0.7778(4) 0.7154(4) 0.6131(3) 0.033(3) Uij O5 O 0.9912(4) 0.6802(3) 0.6280(3) 0.031(3) Uij N11 N 0.6236(4) 0.2941(4) 0.4865(3) 0.029(3) Uij C12 C 0.6749(5) 0.2448(5) 0.4177(4) 0.035(4) Uij C13 C 0.5968(6) 0.1510(5) 0.3450(4) 0.039(4) Uij C14 C 0.4715(6) 0.1069(5) 0.3440(4) 0.043(4) Uij C15 C 0.4211(5) 0.1569(5) 0.4156(4) 0.036(4) Uij C16 C 0.5003(5) 0.2502(5) 0.4846(4) 0.032(4) Uij C17 C 0.4597(5) 0.3116(5) 0.5684(4) 0.033(4) Uij N21 N 0.7873(4) 0.3492(4) 0.6393(3) 0.028(3) Uij C22 C 0.9059(5) 0.3664(5) 0.6457(4) 0.034(4) Uij C23 C 0.9564(5) 0.3267(5) 0.6989(4) 0.038(4) Uij C24 C 0.8810(6) 0.2677(5) 0.7484(4) 0.041(4) Uij C25 C 0.7571(5) 0.2479(5) 0.7405(4) 0.035(4) Uij C26 C 0.7105(5) 0.2874(4) 0.6842(3) 0.030(4) Uij C27 C 0.5782(5) 0.2640(5) 0.6646(3) 0.034(4) Uij N31 N 0.9943(4) 0.8898(4) 0.7236(3) 0.031(3) Uij C32 C 0.9620(5) 0.9608(5) 0.6965(4) 0.037(4) Uij C33 C 1.0486(6) 1.0707(5) 0.7068(4) 0.039(4) Uij C34 C 1.1661(6) 1.1076(5) 0.7470(4) 0.044(5) Uij C35 C 1.1982(6) 1.0353(5) 0.7784(4) 0.039(4) Uij C36 C 1.1114(5) 0.9266(5) 0.7652(3) 0.032(4) Uij C37 C 1.1322(5) 0.8379(5) 0.7946(4) 0.036(4) Uij N41 N 0.7878(4) 0.7748(4) 0.7938(3) 0.029(3) Uij C42 C 0.6728(5) 0.7604(5) 0.7770(4) 0.036(4) Uij C43 C 0.5981(5) 0.7752(5) 0.8429(4) 0.043(4) Uij C44 C 0.6490(6) 0.8058(5) 0.9292(4) 0.043(5) Uij C45 C 0.7701(6) 0.8217(5) 0.9484(4) 0.038(4) Uij C46 C 0.8398(5) 0.8072(4) 0.8793(4) 0.033(4) Uij C47 C 0.9730(5) 0.8302(5) 0.8923(3) 0.035(4) Uij N51 N 0.5653(4) 0.3603(4) 0.6405(3) 0.027(3) Uij C52 C 0.5536(5) 0.4496(5) 0.7208(3) 0.032(4) Uij C53 C 0.6608(5) 0.4939(4) 0.7913(3) 0.029(4) Uij C54 C 0.6488(5) 0.4754(5) 0.8717(3) 0.031(4) Uij C55 C 0.7503(5) 0.5129(4) 0.9349(3) 0.030(4) Uij C56 C 0.7377(5) 0.5008(5) 1.0270(3) 0.033(4) Uij C57 C 0.8452(6) 0.4859(6) 1.0628(4) 0.049(5) Uij C58 C 0.6160(7) 0.4028(7) 1.0257(5) 0.068(6) Uij C59 C 0.7356(8) 0.6165(7) 1.0904(4) 0.067(7) Uij N61 N 1.0072(4) 0.7642(4) 0.8098(3) 0.032(4) Uij C62 C 1.0090(5) 0.6534(5) 0.8160(3) 0.033(4) Uij C63 C 0.8834(5) 0.5868(4) 0.8349(3) 0.028(4) Uij C64 C 0.8683(5) 0.5680(5) 0.9148(3) 0.031(4) Uij C65 C 0.7817(5) 0.5495(4) 0.7736(3) 0.029(4) Uij Cl1 Cl 0.7123(1) 0.4511(1) 0.3088(1) 0.038(1) Uij O6 O 0.7179(4) 0.5388(5) 0.2755(3) 0.061(4) Uij O7 O 0.8222(4) 0.4903(5) 0.3694(3) 0.058(4) Uij O8 O 0.7038(5) 0.3479(5) 0.2370(3) 0.072(5) Uij O9 O 0.6039(3) 0.4224(4) 0.3538(2) 0.039(3) Uij Cl2 Cl 1.2267(1) 0.9553(1) 0.5204(1) 0.037(1) Uij O10 O 1.2995(4) 1.0607(4) 0.5918(3) 0.059(4) Uij O11 O 1.1504(5) 0.9777(4) 0.4654(3) 0.063(4) Uij O12 O 1.3094(4) 0.9124(4) 0.4709(3) 0.055(4) Uij O13 O 1.1465(4) 0.8703(3) 0.5548(3) 0.047(3) Uij Cl3 Cl 1.2086(2) 0.8911(1) 1.0797(1) 0.058(1) Uij O14 O 1.1275(5) 0.7719(4) 1.0576(3) 0.071(4) Uij O15 O 1.3082(6) 0.9280(6) 1.1452(4) 0.117(6) Uij O16 O 1.2532(5) 0.9155(4) 1.0040(3) 0.065(4) Uij O17 O 1.1306(7) 0.9525(5) 1.1103(4) 0.101(7) Uij O18 O 0.8799(4) 0.8010(4) 0.4822(3) 0.051(4) Uij O19 O 0.5637(6) -0.0172(6) 0.1114(4) 0.101(7) Uij H2 H 0.596(7) 0.511(8) 0.548(5) 0.05(3) Uiso H3a H 0.929(5) 0.578(5) 0.575(3) 0.03(1) Uiso H3b H 0.840(5) 0.480(5) 0.488(4) 0.03(2) Uiso H4a H 0.738(6) 0.641(6) 0.601(4) 0.05(2) Uiso H4b H 0.805(5) 0.739(5) 0.577(3) 0.02(2) Uiso H5 H 1.018(5) 0.710(5) 0.600(4) 0.02(2) Uiso HO18a H 0.9619 0.8142 0.4893 0.059 Uiso HO18b H 0.8824 0.8731 0.4912 0.059 Uiso HO19a H 0.5771 0.0018 0.0616 0.114 Uiso HO19b H 0.4806 -0.0494 0.1082 0.114 Uiso H12 H 0.7626 0.2739 0.4192 0.042 Uiso H13 H 0.6315 0.1177 0.2957 0.047 Uiso H14 H 0.4188 0.0424 0.2946 0.052 Uiso H15 H 0.3339 0.1269 0.4166 0.044 Uiso H17a H 0.3885 0.2582 0.5817 0.039 Uiso H17b H 0.4408 0.3720 0.5611 0.039 Uiso H22 H 0.9580 0.4074 0.6123 0.041 Uiso H23 H 1.0419 0.3395 0.7018 0.046 Uiso H24 H 0.9146 0.2415 0.7870 0.049 Uiso H25 H 0.7037 0.2073 0.7735 0.042 Uiso H27a H 0.5393 0.2586 0.7155 0.041 Uiso H27b H 0.5390 0.1928 0.6163 0.041 Uiso H32 H 0.8790 0.9362 0.6697 0.045 Uiso H33 H 1.0254 1.1203 0.6857 0.046 Uiso H34 H 1.2260 1.1826 0.7535 0.053 Uiso H35 H 1.2794 1.0608 0.8088 0.047 Uiso H37a H 1.1897 0.8746 0.8480 0.043 Uiso H37b H 1.1628 0.7921 0.7499 0.043 Uiso H42 H 0.6383 0.7389 0.7171 0.043 Uiso H43 H 0.5145 0.7645 0.8287 0.051 Uiso H44 H 0.6002 0.8159 0.9757 0.051 Uiso H45 H 0.8058 0.8422 1.0078 0.046 Uiso H47a H 0.9895 0.8071 0.9395 0.042 Uiso H47b H 1.0210 0.9107 0.9067 0.042 Uiso H52a H 0.4787 0.4159 0.7423 0.038 Uiso H52b H 0.5517 0.5121 0.7051 0.038 Uiso H54 H 0.5681 0.4358 0.8836 0.037 Uiso H57a H 0.8374 0.4785 1.1196 0.058 Uiso H57b H 0.9190 0.5515 1.0679 0.058 Uiso H57c H 0.8507 0.4181 1.0227 0.058 Uiso H58a H 0.6082 0.3954 1.0825 0.082 Uiso H58b H 0.6133 0.3321 0.9841 0.082 Uiso H58c H 0.5485 0.4182 1.0082 0.082 Uiso H59a H 0.7279 0.6090 1.1471 0.080 Uiso H59b H 0.6668 0.6282 1.0702 0.080 Uiso H59c H 0.8106 0.6798 1.0932 0.080 Uiso H62a H 1.0716 0.6713 0.8626 0.039 Uiso H62b H 1.0250 0.6092 0.7614 0.039 Uiso H64 H 0.9397 0.5932 0.9568 0.038 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0303(4) 0.0251(4) 0.0285(4) 0.0099(3) 0.0074(3) 0.0107(3) Co2 0.0338(4) 0.0250(4) 0.0282(4) 0.0111(3) 0.0080(3) 0.0099(3) O1 0.030(2) 0.027(2) 0.025(2) 0.009(2) 0.005(1) 0.011(1) O2 0.032(3) 0.029(2) 0.038(2) 0.014(2) 0.006(2) 0.013(2) O3 0.030(2) 0.032(2) 0.027(2) 0.010(2) 0.009(2) 0.012(2) O4 0.040(2) 0.027(2) 0.030(2) 0.009(2) 0.007(2) 0.013(2) O5 0.036(2) 0.027(2) 0.032(2) 0.012(2) 0.014(2) 0.013(2) N11 0.032(3) 0.027(2) 0.030(2) 0.012(2) 0.006(2) 0.012(2) C12 0.034(3) 0.030(3) 0.043(3) 0.011(3) 0.009(3) 0.017(3) C13 0.049(4) 0.030(3) 0.033(3) 0.016(3) 0.008(3) 0.004(2) C14 0.051(4) 0.032(3) 0.039(3) 0.011(3) 0.005(3) 0.010(3) C15 0.037(3) 0.035(3) 0.039(3) 0.014(3) 0.005(3) 0.017(3) C16 0.036(3) 0.033(3) 0.039(3) 0.017(3) 0.010(2) 0.020(3) C17 0.031(3) 0.032(3) 0.036(3) 0.011(2) 0.008(2) 0.014(2) N21 0.031(2) 0.021(2) 0.029(2) 0.008(2) 0.004(2) 0.006(2) C22 0.036(3) 0.030(3) 0.039(3) 0.014(3) 0.012(2) 0.014(2) C23 0.037(3) 0.038(3) 0.041(3) 0.020(3) 0.007(3) 0.010(3) C24 0.053(4) 0.037(3) 0.040(3) 0.023(3) 0.009(3) 0.016(3) C25 0.041(3) 0.031(3) 0.035(3) 0.014(3) 0.007(3) 0.014(2) C26 0.037(3) 0.021(3) 0.031(3) 0.010(2) 0.012(2) 0.008(2) C27 0.041(3) 0.030(3) 0.032(3) 0.012(3) 0.007(2) 0.014(2) N31 0.041(3) 0.024(2) 0.026(2) 0.012(2) 0.014(2) 0.011(2) C32 0.043(3) 0.031(3) 0.035(3) 0.015(3) 0.013(3) 0.010(2) C33 0.051(4) 0.029(3) 0.038(3) 0.018(3) 0.016(3) 0.012(2) C34 0.053(4) 0.027(3) 0.047(4) 0.011(3) 0.022(3) 0.013(3) C35 0.045(4) 0.034(3) 0.032(3) 0.011(3) 0.012(3) 0.009(2) C36 0.035(3) 0.029(3) 0.030(3) 0.011(3) 0.014(2) 0.008(2) C37 0.030(3) 0.030(3) 0.037(3) 0.002(2) 0.006(2) 0.012(2) N41 0.035(3) 0.019(2) 0.033(2) 0.011(2) 0.009(2) 0.008(2) C42 0.039(3) 0.030(3) 0.035(3) 0.010(3) 0.007(3) 0.009(2) C43 0.036(3) 0.034(3) 0.060(4) 0.017(3) 0.016(3) 0.016(3) C44 0.054(4) 0.037(3) 0.037(3) 0.018(3) 0.022(3) 0.011(3) C45 0.046(4) 0.030(3) 0.034(3) 0.011(3) 0.015(3) 0.010(2) C46 0.038(3) 0.021(3) 0.038(3) 0.009(2) 0.014(3) 0.010(2) C47 0.045(3) 0.028(3) 0.026(3) 0.010(3) 0.010(2) 0.009(2) N51 0.027(2) 0.021(2) 0.031(2) 0.008(2) 0.010(2) 0.009(2) C52 0.033(3) 0.031(3) 0.033(3) 0.015(2) 0.011(2) 0.009(2) C53 0.028(3) 0.026(3) 0.035(3) 0.012(2) 0.008(2) 0.011(2) C54 0.032(3) 0.029(3) 0.036(3) 0.014(2) 0.014(2) 0.013(2) C55 0.034(3) 0.026(3) 0.032(3) 0.012(2) 0.011(2) 0.014(2) C56 0.033(3) 0.040(3) 0.031(3) 0.015(3) 0.009(2) 0.018(2) C57 0.055(4) 0.069(5) 0.041(3) 0.032(4) 0.019(3) 0.034(3) C58 0.071(5) 0.071(5) 0.053(4) -0.002(4) 0.005(4) 0.046(4) C59 0.122(7) 0.065(5) 0.041(4) 0.060(5) 0.037(4) 0.025(4) N61 0.039(3) 0.026(2) 0.028(2) 0.013(2) 0.011(2) 0.007(2) C62 0.033(3) 0.031(3) 0.031(3) 0.010(2) 0.001(2) 0.011(2) C63 0.032(3) 0.023(3) 0.031(3) 0.011(2) 0.011(2) 0.009(2) C64 0.037(3) 0.027(3) 0.030(3) 0.014(2) -0.001(2) 0.008(2) C65 0.037(3) 0.022(3) 0.030(3) 0.013(2) 0.009(2) 0.011(2) Cl1 0.033(1) 0.051(1) 0.035(1) 0.017(1) 0.010(1) 0.020(1) O6 0.055(3) 0.085(4) 0.073(3) 0.038(3) 0.026(3) 0.055(3) O7 0.036(2) 0.092(4) 0.049(3) 0.013(3) 0.009(2) 0.043(3) O8 0.068(4) 0.072(4) 0.066(3) 0.032(3) 0.034(3) 0.006(3) O9 0.033(2) 0.051(3) 0.037(2) 0.019(2) 0.011(2) 0.017(2) Cl2 0.042(1) 0.029(1) 0.040(1) 0.014(1) 0.012(1) 0.013(1) O10 0.061(3) 0.034(2) 0.054(3) 0.000(2) 0.022(2) 0.003(2) O11 0.063(3) 0.065(3) 0.071(3) 0.026(3) 0.012(3) 0.035(3) O12 0.069(3) 0.045(3) 0.068(3) 0.035(3) 0.038(3) 0.027(2) O13 0.050(3) 0.034(2) 0.056(3) 0.014(2) 0.022(2) 0.019(2) Cl3 0.089(1) 0.032(1) 0.037(1) 0.010(1) -0.002(1) 0.010(1) O14 0.092(4) 0.035(3) 0.057(3) 0.000(3) -0.007(3) 0.010(2) O15 0.116(5) 0.096(5) 0.083(4) -0.036(4) -0.052(4) 0.055(4) O16 0.084(4) 0.067(3) 0.044(3) 0.026(3) 0.013(3) 0.025(2) O17 0.154(6) 0.081(4) 0.090(4) 0.058(5) 0.076(4) 0.044(4) O18 0.055(3) 0.051(3) 0.049(3) 0.019(2) 0.014(2) 0.024(2) O19 0.103(5) 0.122(6) 0.072(4) 0.039(5) 0.018(4) 0.034(4) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Co1 Co2 3.601(1) Co1 O1 1.977(3) Co1 O2 1.882(5) Co1 O3 1.910(4) Co1 N11 1.908(4) Co1 N21 1.925(4) Co1 N51 1.976(4) Co2 O1 1.980(4) Co2 O4 1.903(4) Co2 O5 1.894(4) Co2 N31 1.915(4) Co2 N41 1.926(4) Co2 N61 1.960(5) O1 C65 1.364(6) N11 C12 1.362(6) N11 C16 1.336(7) C12 C13 1.394(8) C13 C14 1.360(8) C14 C15 1.389(8) C15 C16 1.364(8) C16 C17 1.518(7) C17 N51 1.479(7) N21 C22 1.319(7) N21 C26 1.358(6) C22 C23 1.370(8) C23 C24 1.388(8) C24 C25 1.373(8) C25 C26 1.382(8) C26 C27 1.472(8) C27 N51 1.509(7) N31 C32 1.325(7) N31 C36 1.357(7) C32 C33 1.385(8) C33 C34 1.352(9) C34 C35 1.380(9) C35 C36 1.365(8) C36 C37 1.500(8) C37 N61 1.500(6) N41 C42 1.301(7) N41 C46 1.362(7) C42 C43 1.393(7) C43 C44 1.373(9) C44 C45 1.372(9) C45 C46 1.391(7) C46 C47 1.473(8) C47 N61 1.487(6) N51 C52 1.493(6) C52 C53 1.484(7) C53 C54 1.391(7) C53 C65 1.411(7) C54 C55 1.380(7) C55 C64 1.398(7) C55 C56 1.543(7) C56 C57 1.486(8) C56 C58 1.524(9) C56 C59 1.556(8) N61 C62 1.515(7) C62 C63 1.500(7) C63 C65 1.364(7) C63 C64 1.385(7) Cl1 O6 1.414(5) Cl1 O7 1.423(4) Cl1 O8 1.449(5) Cl1 O9 1.454(4) Cl2 O10 1.434(4) Cl2 O11 1.424(5) Cl2 O12 1.426(4) Cl2 O13 1.443(4) Cl3 O14 1.428(5) Cl3 O15 1.389(6) Cl3 O16 1.414(4) Cl3 O17 1.433(6) O2 H2 0.52(7) O2 H4a 1.60(7) O3 H3b 0.77(5) O3 H3a 1.19(6) O4 H4b 0.76(5) O4 H4a 0.87(7) O5 H5 0.70(5) O5 H3a 1.26(6) C12 H12 0.950 C13 H13 0.950 C14 H14 0.950 C15 H15 0.950 C17 H17a 0.950 C17 H17b 0.950 C22 H22 0.950 C23 H23 0.950 C24 H24 0.950 C25 H25 0.950 C27 H27a 0.950 C27 H27b 0.950 C32 H32 0.950 C33 H33 0.950 C34 H34 0.950 C35 H35 0.950 C37 H37a 0.950 C37 H37b 0.950 C42 H42 0.950 C43 H43 0.950 C44 H44 0.950 C45 H45 0.950 C47 H47a 0.950 C47 H47b 0.950 C52 H52a 0.950 C52 H52b 0.950 C54 H54 0.950 C57 H57a 0.950 C57 H57b 0.950 C57 H57c 0.950 C58 H58a 0.950 C58 H58b 0.950 C58 H58c 0.950 C59 H59a 0.950 C59 H59b 0.950 C59 H59c 0.950 C62 H62a 0.950 C62 H62b 0.950 C64 H64 0.950 O18 HO18a 0.909 O18 HO18b 0.911 O19 HO19b 0.898 O19 HO19a 0.913 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Co1 O2 87.5(2) O1 Co1 O3 88.4(2) O1 Co1 N11 175.0(2) O1 Co1 N21 88.5(2) O1 Co1 N51 94.9(2) O2 Co1 O3 92.3(2) O2 Co1 N11 89.0(2) O2 Co1 N21 174.9(2) O2 Co1 N51 91.2(2) O3 Co1 N11 95.4(2) O3 Co1 N21 90.7(2) O3 Co1 N51 175.3(2) N11 Co1 N21 94.8(2) N11 Co1 N51 81.6(2) N21 Co1 N51 86.0(2) O1 Co2 O4 90.2(2) O1 Co2 O5 87.4(2) O1 Co2 N31 175.1(2) O1 Co2 N41 88.4(2) O1 Co2 N61 94.1(2) O4 Co2 O5 92.2(2) O4 Co2 N31 94.2(2) O4 Co2 N41 91.5(2) O4 Co2 N61 174.8(2) O5 Co2 N31 90.2(2) O5 Co2 N41 174.5(2) O5 Co2 N61 91.0(2) N31 Co2 N41 93.7(2) N31 Co2 N61 81.7(2) N41 Co2 N61 85.7(2) Co1 O1 C65 114.6(3) Co2 O1 C65 114.5(3) Co1 O1 Co2 131.0(2) Co1 O2 H2 133(10) Co1 O2 H4a 101(2) Co1 O3 H3b 110(4) Co1 O3 H3a 114(2) Co2 O4 H4b 118(4) Co2 O4 H4a 93(4) Co2 O5 H5 119(5) Co2 O5 H3a 110(2) Co1 N11 C12 125.0(4) Co1 N11 C16 115.2(3) Co1 N21 C22 125.3(4) Co1 N21 C26 113.8(3) Co2 N31 C32 126.0(4) Co2 N31 C36 114.2(4) Co2 N41 C42 126.3(4) Co2 N41 C46 113.5(4) Co1 N51 C17 105.1(3) Co1 N51 C27 107.3(3) Co1 N51 C52 111.1(3) Co2 N61 C37 105.4(3) Co2 N61 C47 109.2(3) Co2 N61 C62 111.5(3) C12 N11 C16 119.8(5) N11 C12 C13 119.1(5) C12 C13 C14 120.5(5) C13 C14 C15 119.6(5) C14 C15 C16 118.1(5) N11 C16 C15 122.9(5) N11 C16 C17 112.8(5) C15 C16 C17 124.2(5) C16 C17 N51 106.6(4) C22 N21 C26 119.9(5) N21 C22 C23 122.1(5) C22 C23 C24 119.1(5) C23 C24 C25 118.8(5) C24 C25 C26 119.6(5) N21 C26 C25 120.4(5) N21 C26 C27 114.8(5) C25 C26 C27 124.7(5) C26 C27 N51 110.3(4) C32 N31 C36 119.8(5) N31 C32 C33 120.4(6) C32 C33 C34 120.2(6) C33 C34 C35 119.4(6) C34 C35 C36 118.9(6) N31 C36 C35 121.3(5) N31 C36 C37 113.5(5) C35 C36 C37 125.2(5) C36 C37 N61 105.6(4) C42 N41 C46 119.6(4) N41 C42 C43 123.0(5) C42 C43 C44 117.9(6) C43 C44 C45 120.1(5) C44 C45 C46 118.8(5) N41 C46 C45 120.6(5) N41 C46 C47 115.6(4) C45 C46 C47 123.8(5) C46 C47 N61 110.2(4) C17 N51 C52 112.6(4) C17 N51 C27 109.9(4) C27 N51 C52 110.5(4) N51 C52 C53 110.3(4) C54 C53 C65 118.1(5) C52 C53 C54 123.0(5) C52 C53 C65 118.7(5) C53 C54 C55 122.1(5) C54 C55 C64 117.8(5) C54 C55 C56 122.7(5) C56 C55 C64 119.5(5) C57 C56 C58 110.5(5) C55 C56 C57 112.5(4) C57 C56 C59 107.9(5) C55 C56 C58 111.8(5) C58 C56 C59 107.8(5) C55 C56 C59 106.2(4) C37 N61 C47 109.8(4) C47 N61 C62 110.7(4) C37 N61 C62 110.1(4) N61 C62 C63 107.1(4) C64 C63 C65 119.8(5) C62 C63 C65 118.7(5) C62 C63 C64 121.4(5) C55 C64 C63 121.4(5) O1 C65 C63 120.4(5) O1 C65 C53 118.9(5) C53 C65 C63 120.7(5) O6 Cl1 O7 109.7(3) O6 Cl1 O8 110.4(3) O6 Cl1 O9 109.7(2) O7 Cl1 O8 108.3(3) O7 Cl1 O9 109.7(2) O8 Cl1 O9 109.0(3) O11 Cl2 O12 110.7(3) O10 Cl2 O11 109.5(3) O11 Cl2 O13 108.1(3) O10 Cl2 O12 108.4(3) O12 Cl2 O13 109.8(3) O10 Cl2 O13 110.3(3) O15 Cl3 O16 109.7(4) O14 Cl3 O15 113.3(4) O15 Cl3 O17 110.3(5) O14 Cl3 O16 111.6(3) O16 Cl3 O17 107.3(3) O14 Cl3 O17 104.3(4) H2 O2 H4a 108(10) Co1 O2 H2 133(10) Co1 O2 H4a 101(2) H3a O3 H3b 105(5) H4a O4 H4b 120(5) H3a O5 H5 103(5) Co2 O5 H5 119(5) Co2 O5 H3a 110(2) N11 C12 H12 120.5 C13 C12 H12 120.5 C14 C13 H13 119.7 C12 C13 H13 119.7 C13 C14 H14 120.2 C15 C14 H14 120.2 C16 C15 H15 121.0 C14 C15 H15 120.9 H17a C17 H17b 109.5 N51 C17 H17a 110.2 C16 C17 H17a 110.2 N51 C17 H17b 110.2 C16 C17 H17b 110.2 N21 C22 H22 119.0 C23 C22 H22 119.0 C22 C23 H23 120.4 C24 C23 H23 120.4 C25 C24 H24 120.6 C23 C24 H24 120.6 C24 C25 H25 120.2 C26 C25 H25 120.2 H27a C27 H27b 109.5 C26 C27 H27a 109.3 N51 C27 H27a 109.3 C26 C27 H27b 109.3 N51 C27 H27b 109.3 N31 C32 H32 119.8 C33 C32 H32 119.8 C34 C33 H33 119.9 C32 C33 H33 119.9 C33 C34 H34 120.3 C35 C34 H34 120.3 C36 C35 H35 120.6 C34 C35 H35 120.6 H37a C37 H37b 109.5 N61 C37 H37a 110.4 C36 C37 H37a 110.4 N61 C37 H37b 110.4 C36 C37 H37b 110.4 N41 C42 H42 118.5 C43 C42 H42 118.5 C44 C43 H43 121.1 C42 C43 H43 121.1 C45 C44 H44 119.9 C43 C44 H44 119.9 C44 C45 H45 120.6 C46 C45 H45 120.6 H47a C47 H47b 109.5 C46 C47 H47a 109.3 N61 C47 H47a 109.3 C46 C47 H47b 109.3 N61 C47 H47b 109.3 H52a C52 H52b 109.5 C53 C52 H52a 109.3 N51 C52 H52a 109.3 C53 C52 H52b 109.3 N51 C52 H52b 109.3 C55 C54 H54 118.9 C53 C54 H54 118.9 H57a C57 H57b 108.7 H57a C57 H57c 108.7 C56 C57 H57a 112.5 H57b C57 H57c 109.5 C56 C57 H57b 108.7 C56 C57 H57c 108.7 H58a C58 H58b 108.9 H58a C58 H58c 108.9 C56 C58 H58a 111.8 H58b C58 H58c 109.5 C56 C58 H58b 108.9 C56 C58 H58c 108.9 H59a C59 H59b 110.3 H59a C59 H59c 110.3 C56 C59 H59a 106.2 H59b C59 H59c 109.5 C56 C59 H59b 110.3 C56 C59 H59c 110.3 H62a C62 H62b 109.5 C63 C62 H62a 110.1 N61 C62 H62a 110.1 C63 C62 H62b 110.1 N61 C62 H62b 110.1 C63 C64 H64 119.3 C55 C64 H64 119.3 HO18a O18 HO18b 102.6 HO19a O19 HO19b 105.2 #loop_ #_geom_bond_atom_site_label_D #_geom_bond_atom_site_label_H #_geom_contact_atom_site_label_A #_geom_bond_distance_DH #_geom_contact_distance_HA #_geom_contact_distance_DA #_geom_angle_DHA #O3 H3a O5 1.19(6) 1.26(6) 2.446(5) 170(4) #O4 H4a O2 0.87(7) 1.60(7) 2.427(6) 158(6) #O3 H3b O7 0.77(5) 1.97(5) 2.736(6) 170(6) #O4 H4b O18 0.76(5) 2.01(5) 2.779(6) 179(5) #O5 H5 O13 0.70(5) 2.44(6) 3.097(6) 159(6) #============================================================================== data_kofod _database_code_CSD 195396 #=================================== # 5. CHEMICAL DATA _chemical_name_systematic ; insert name here ; _chemical_name_common [Co2(bpbp)(OH)2(H2O)2](ClO4)3.H2O.CH3CN _chemical_formula_sum 'C38 H50 Cl3 Co2 N7 O18' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety 'C36 H45 Co2 N6 O5, 3(Cl O4),C2 H3 N, H2 O' _chemical_formula_weight 1117.130 _chemical_melting_point ? _chemical_compound_source ? #=================================== # 6. CRYSTAL DATA _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 11.906(1) _cell_length_b 13.329(2) _cell_length_c 16.168(2) _cell_angle_alpha 108.359(2) _cell_angle_beta 90.173(2) _cell_angle_gamma 112.728(2) _cell_volume 2223.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 29.5 _exptl_crystal_description plate _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.074 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'XPREP, Siemens, 1995' _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.934 #=================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method ; \w rotation scans with narrow frames ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 17416 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_theta_max 29.5 _diffrn_reflns_reduction_process 17416 _reflns_number_total 10910 _reflns_number_gt 7507 _reflns_threshold_expression I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997 ), KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #=================================== # 8. REFINEMENT DATA _refine_special_details ; ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w= 1/{[\s~cs~(F^2^)+B +(1+A)F^2^]^1/2^- |F|}^2^ A = 0.03, B = 0.3 ; _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method ; B-C type 1 Lorentzian isotropic Becker and Coppens (1974) ; _refine_ls_extinction_coef 79(10) _refine_ls_number_reflns 7504 _refine_ls_number_parameters 638 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.048 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_shift/su_max 0.0009 _refine_ls_shift/su_mean 0.00005 _refine_diff_density_max 2.1(1) _refine_diff_density_min -0.7(1) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Co1 0.71513(4) 0.42882(4) 0.59010(3) 0.0151(3) Uij Co2 0.88672(4) 0.73394(4) 0.70518(3) 0.0160(3) Uij O1 0.7947(2) 0.5696(2) 0.6943(1) 0.017(1) Uij O2 0.6387(2) 0.5095(2) 0.5502(2) 0.018(2) Uij O3 0.8564(2) 0.4839(2) 0.5352(2) 0.019(2) Uij O4 0.7752(2) 0.7145(2) 0.6110(2) 0.019(2) Uij O5 0.9875(2) 0.6838(2) 0.6277(2) 0.019(2) Uij N11 0.6268(2) 0.2940(2) 0.4904(2) 0.018(2) Uij C12 0.6754(3) 0.2446(3) 0.4234(2) 0.022(2) Uij C13 0.6027(4) 0.1496(3) 0.3526(2) 0.029(3) Uij C14 0.4757(4) 0.1047(3) 0.3501(2) 0.030(3) Uij C15 0.4263(3) 0.1550(3) 0.4202(2) 0.024(2) Uij C16 0.5032(3) 0.2490(3) 0.4899(2) 0.019(2) Uij C17 0.4635(3) 0.3083(3) 0.5718(2) 0.020(2) Uij N21 0.7884(2) 0.3523(2) 0.6412(2) 0.017(2) Uij C22 0.9084(3) 0.3722(3) 0.6462(2) 0.021(2) Uij C23 0.9596(3) 0.3321(3) 0.6989(2) 0.025(2) Uij C24 0.8862(3) 0.2730(3) 0.7491(2) 0.026(2) Uij C25 0.7622(3) 0.2507(3) 0.7428(2) 0.023(2) Uij C26 0.7163(3) 0.2904(3) 0.6872(2) 0.018(2) Uij C27 0.5832(3) 0.2641(3) 0.6682(2) 0.019(2) Uij N31 0.9859(3) 0.8918(2) 0.7192(2) 0.021(2) Uij C32 0.9512(3) 0.9601(3) 0.6896(2) 0.024(2) Uij C33 1.0332(4) 1.0709(3) 0.6969(3) 0.030(3) Uij C34 1.1522(4) 1.1116(3) 0.7369(3) 0.032(3) Uij C35 1.1871(3) 1.0427(3) 0.7713(2) 0.029(2) Uij C36 1.1024(3) 0.9321(3) 0.7601(2) 0.022(2) Uij C37 1.1256(3) 0.8459(3) 0.7917(2) 0.023(2) Uij N41 0.7851(2) 0.7728(2) 0.7906(2) 0.019(2) Uij C42 0.6656(3) 0.7508(3) 0.7727(2) 0.025(2) Uij C43 0.5930(3) 0.7590(3) 0.8384(3) 0.032(3) Uij C44 0.6433(4) 0.7909(3) 0.9250(3) 0.035(3) Uij C45 0.7661(3) 0.8148(3) 0.9438(2) 0.028(2) Uij C46 0.8347(3) 0.8054(3) 0.8754(2) 0.021(2) Uij C47 0.9689(3) 0.8339(3) 0.8881(2) 0.022(2) Uij N51 0.5702(2) 0.3596(2) 0.6431(2) 0.017(2) Uij C52 0.5565(3) 0.4472(3) 0.7222(2) 0.018(2) Uij C53 0.6645(3) 0.4938(3) 0.7924(2) 0.017(2) Uij C54 0.6527(3) 0.4764(3) 0.8731(2) 0.019(2) Uij C55 0.7545(3) 0.5164(3) 0.9362(2) 0.019(2) Uij C56 0.7421(3) 0.5065(3) 1.0282(2) 0.022(2) Uij C57 0.8440(4) 0.4789(4) 1.0590(3) 0.036(3) Uij C58 0.6189(4) 0.4148(4) 1.0307(3) 0.040(3) Uij C59 0.7557(5) 0.6244(4) 1.0924(3) 0.042(3) Uij N61 1.0037(2) 0.7685(2) 0.8063(2) 0.018(2) Uij C62 1.0074(3) 0.6606(3) 0.8149(2) 0.020(2) Uij C63 0.8847(3) 0.5908(3) 0.8345(2) 0.019(2) Uij C64 0.8702(3) 0.5737(3) 0.9153(2) 0.020(2) Uij C65 0.7813(3) 0.5510(3) 0.7736(2) 0.017(2) Uij Cl1 0.70992(8) 0.44808(8) 0.30958(6) 0.0251(6) Uij O6 0.7117(3) 0.5312(3) 0.2711(2) 0.040(2) Uij O7 0.8204(2) 0.4957(3) 0.3719(2) 0.041(2) Uij O8 0.7057(3) 0.3453(3) 0.2425(2) 0.048(2) Uij O9 0.6039(2) 0.4194(2) 0.3552(2) 0.026(2) Uij Cl2 1.22682(8) 0.95415(7) 0.52151(6) 0.0229(5) Uij O10 1.3048(3) 1.0531(2) 0.5939(2) 0.039(2) Uij O11 1.1554(3) 0.9889(3) 0.4727(2) 0.044(2) Uij O12 1.2994(3) 0.9074(2) 0.4656(2) 0.036(2) Uij O13 1.1429(2) 0.8682(2) 0.5542(2) 0.033(2) Uij Cl3 1.17159(10) 0.89735(8) 1.08827(6) 0.0386(7) Uij O14 1.1203(3) 0.7751(2) 1.0670(2) 0.051(2) Uij O15 1.0704(4) 0.9354(3) 1.1000(2) 0.060(3) Uij O16 1.2292(3) 0.9258(3) 1.0155(2) 0.044(2) Uij O17 1.2544(4) 0.9553(3) 1.1678(2) 0.077(3) Uij O18 0.8812(3) 0.7984(2) 0.4798(2) 0.036(2) Uij C1 0.5356(7) 0.0465(7) 0.1073(6) 0.101(8) Uij C2 0.5301(6) -0.0462(5) 0.1283(3) 0.057(4) Uij N3 0.5151(5) -0.1292(6) 0.1513(4) 0.101(6) Uij H2a 0.700(5) 0.602(5) 0.571(4) 0.08(2) Uiso H2b 0.626(4) 0.485(4) 0.501(3) 0.04(1) Uiso H3a 0.923(6) 0.575(6) 0.576(4) 0.10(2) Uiso H3b 0.842(3) 0.487(3) 0.498(2) 0.01(1) Uiso H4 0.812(4) 0.736(4) 0.578(3) 0.04(1) Uiso H5 1.009(5) 0.716(4) 0.608(3) 0.04(2) Uiso H18a 0.8653 0.8535 0.4846 0.050 Uiso H18b 0.9506 0.8050 0.4744 0.050 Uiso H12 0.7622 0.2758 0.4246 0.026 Uiso H13 0.6389 0.1151 0.3061 0.035 Uiso H14 0.4238 0.0406 0.3011 0.036 Uiso H15 0.3398 0.1248 0.4203 0.029 Uiso H17a 0.3940 0.2541 0.5860 0.024 Uiso H17b 0.4433 0.3675 0.5641 0.024 Uiso H22 0.9590 0.4146 0.6128 0.025 Uiso H23 1.0440 0.3450 0.7006 0.029 Uiso H24 0.9206 0.2479 0.7876 0.031 Uiso H25 0.7100 0.2091 0.7759 0.028 Uiso H27a 0.5451 0.2586 0.7191 0.023 Uiso H27b 0.5446 0.1927 0.6210 0.023 Uiso H32 0.8687 0.9321 0.6630 0.028 Uiso H33 1.0077 1.1180 0.6747 0.036 Uiso H34 1.2102 1.1864 0.7410 0.038 Uiso H35 1.2675 1.0713 0.8018 0.035 Uiso H37a 1.1812 0.8846 0.8451 0.028 Uiso H37b 1.1586 0.8022 0.7485 0.028 Uiso H42 0.6308 0.7292 0.7135 0.030 Uiso H43 0.5089 0.7428 0.8245 0.038 Uiso H44 0.5939 0.7962 0.9709 0.042 Uiso H45 0.8027 0.8373 1.0027 0.033 Uiso H47a 0.9876 0.8132 0.9358 0.027 Uiso H47b 1.0139 0.9147 0.9008 0.027 Uiso H52a 0.4828 0.4118 0.7440 0.021 Uiso H52b 0.5530 0.5089 0.7064 0.021 Uiso H54 0.5730 0.4361 0.8854 0.023 Uiso H57a 0.8363 0.4728 1.1159 0.043 Uiso H57b 0.9213 0.5389 1.0610 0.043 Uiso H57c 0.8393 0.4075 1.0186 0.043 Uiso H58a 0.6113 0.4087 1.0876 0.048 Uiso H58b 0.6104 0.3422 0.9900 0.048 Uiso H58c 0.5555 0.4343 1.0143 0.048 Uiso H59a 0.7480 0.6182 1.1492 0.051 Uiso H59b 0.6930 0.6442 1.0750 0.051 Uiso H59c 0.8340 0.6820 1.0930 0.051 Uiso H62a 1.0697 0.6809 0.8614 0.024 Uiso H62b 1.0242 0.6168 0.7614 0.024 Uiso H64 0.9410 0.6018 0.9572 0.024 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0145(2) 0.0129(2) 0.0162(2) 0.0022(2) 0.0009(2) 0.0073(2) Co2 0.0160(2) 0.0133(2) 0.0164(2) 0.0021(2) 0.0015(2) 0.0070(2) O1 0.019(1) 0.014(1) 0.017(1) 0.004(1) 0.001(1) 0.009(1) O2 0.019(1) 0.015(1) 0.018(1) 0.003(1) -0.001(1) 0.007(1) O3 0.020(1) 0.019(1) 0.016(1) 0.004(1) 0.002(1) 0.009(1) O4 0.022(1) 0.016(1) 0.018(1) 0.004(1) 0.001(1) 0.008(1) O5 0.018(1) 0.017(1) 0.022(1) 0.002(1) 0.004(1) 0.010(1) N11 0.017(1) 0.015(1) 0.022(1) 0.003(1) 0.002(1) 0.010(1) C12 0.025(2) 0.017(2) 0.023(2) 0.007(1) 0.002(1) 0.008(1) C13 0.032(2) 0.022(2) 0.026(2) 0.008(2) 0.005(2) 0.004(2) C14 0.032(2) 0.022(2) 0.026(2) 0.002(2) -0.002(2) 0.006(2) C15 0.022(2) 0.020(2) 0.026(2) 0.002(1) -0.001(1) 0.010(1) C16 0.018(2) 0.017(2) 0.023(2) 0.003(1) 0.001(1) 0.012(1) C17 0.015(2) 0.019(2) 0.021(2) 0.001(1) -0.002(1) 0.008(1) N21 0.016(1) 0.014(1) 0.018(1) 0.002(1) 0.002(1) 0.007(1) C22 0.019(2) 0.020(2) 0.024(2) 0.006(1) 0.004(1) 0.009(1) C23 0.020(2) 0.025(2) 0.030(2) 0.008(1) 0.002(1) 0.011(2) C24 0.030(2) 0.027(2) 0.027(2) 0.014(2) 0.002(2) 0.013(2) C25 0.028(2) 0.019(2) 0.025(2) 0.007(1) 0.004(1) 0.012(1) C26 0.021(2) 0.013(2) 0.019(2) 0.004(1) 0.003(1) 0.006(1) C27 0.020(2) 0.015(2) 0.022(2) 0.003(1) 0.002(1) 0.010(1) N31 0.024(1) 0.017(1) 0.019(1) 0.005(1) 0.005(1) 0.006(1) C32 0.030(2) 0.017(2) 0.023(2) 0.009(1) 0.007(1) 0.007(1) C33 0.040(2) 0.017(2) 0.031(2) 0.008(2) 0.011(2) 0.010(2) C34 0.038(2) 0.015(2) 0.030(2) 0.000(2) 0.012(2) 0.004(2) C35 0.026(2) 0.021(2) 0.027(2) 0.000(2) 0.007(2) 0.005(2) C36 0.019(2) 0.019(2) 0.020(2) 0.001(1) 0.005(1) 0.006(1) C37 0.015(2) 0.023(2) 0.023(2) -0.001(1) 0.001(1) 0.008(1) N41 0.018(1) 0.014(1) 0.022(1) 0.002(1) 0.003(1) 0.007(1) C42 0.021(2) 0.017(2) 0.031(2) 0.003(1) 0.000(1) 0.006(1) C43 0.018(2) 0.027(2) 0.039(2) 0.005(2) 0.008(2) 0.003(2) C44 0.029(2) 0.028(2) 0.035(2) 0.004(2) 0.015(2) 0.005(2) C45 0.029(2) 0.022(2) 0.025(2) 0.004(2) 0.009(2) 0.006(2) C46 0.022(2) 0.012(2) 0.022(2) 0.001(1) 0.002(1) 0.004(1) C47 0.023(2) 0.020(2) 0.017(2) 0.002(1) 0.002(1) 0.005(1) N51 0.015(1) 0.015(1) 0.019(1) 0.002(1) 0.001(1) 0.008(1) C52 0.017(2) 0.017(2) 0.018(2) 0.004(1) 0.003(1) 0.007(1) C53 0.016(2) 0.016(2) 0.019(2) 0.004(1) 0.002(1) 0.007(1) C54 0.020(2) 0.015(2) 0.021(2) 0.005(1) 0.006(1) 0.009(1) C55 0.023(2) 0.018(2) 0.019(2) 0.008(1) 0.004(1) 0.010(1) C56 0.025(2) 0.023(2) 0.019(2) 0.009(1) 0.005(1) 0.011(1) C57 0.038(2) 0.051(3) 0.030(2) 0.020(2) 0.008(2) 0.027(2) C58 0.037(2) 0.046(3) 0.029(2) 0.000(2) 0.004(2) 0.024(2) C59 0.074(3) 0.035(2) 0.027(2) 0.028(2) 0.018(2) 0.016(2) N61 0.016(1) 0.015(1) 0.018(1) 0.000(1) 0.001(1) 0.008(1) C62 0.017(2) 0.021(2) 0.020(2) 0.003(1) 0.000(1) 0.010(1) C63 0.018(2) 0.018(2) 0.021(2) 0.005(1) 0.003(1) 0.011(1) C64 0.020(2) 0.020(2) 0.020(2) 0.005(1) 0.001(1) 0.010(1) C65 0.020(2) 0.013(1) 0.017(2) 0.005(1) 0.003(1) 0.008(1) Cl1 0.0190(4) 0.0391(5) 0.0193(4) 0.0099(4) 0.0028(3) 0.0151(4) O6 0.035(2) 0.061(2) 0.044(2) 0.021(1) 0.012(1) 0.039(2) O7 0.018(1) 0.070(2) 0.030(1) 0.001(1) -0.004(1) 0.031(2) O8 0.045(2) 0.053(2) 0.041(2) 0.025(2) 0.016(2) 0.004(2) O9 0.020(1) 0.035(1) 0.023(1) 0.007(1) 0.006(1) 0.014(1) Cl2 0.0266(4) 0.0168(4) 0.0255(4) 0.0066(3) 0.0075(3) 0.0101(3) O10 0.036(2) 0.026(1) 0.033(2) -0.003(1) 0.006(1) 0.000(1) O11 0.046(2) 0.050(2) 0.053(2) 0.025(2) 0.008(2) 0.034(2) O12 0.047(2) 0.028(1) 0.038(2) 0.018(1) 0.022(1) 0.013(1) O13 0.030(1) 0.022(1) 0.046(2) 0.003(1) 0.013(1) 0.020(1) Cl3 0.0506(6) 0.0228(5) 0.0251(5) -0.0035(4) -0.0128(4) 0.0093(4) O14 0.071(2) 0.020(1) 0.045(2) 0.001(1) -0.001(2) 0.009(1) O15 0.081(3) 0.064(2) 0.046(2) 0.044(2) 0.017(2) 0.015(2) O16 0.040(2) 0.051(2) 0.039(2) 0.010(1) 0.002(1) 0.026(2) O17 0.091(3) 0.050(2) 0.049(2) -0.015(2) -0.041(2) 0.020(2) O18 0.038(2) 0.035(2) 0.038(2) 0.011(1) 0.008(1) 0.019(1) C1 0.078(5) 0.112(6) 0.129(7) 0.040(5) 0.021(5) 0.057(6) C2 0.077(4) 0.054(3) 0.047(3) 0.042(3) -0.005(3) 0.007(3) N3 0.075(4) 0.105(5) 0.102(5) 0.032(4) -0.010(3) 0.014(4) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Co1 Co2 3.601(1) Co1 O1 1.970(2) Co1 O2 1.896(2) Co1 O3 1.903(2) Co1 N11 1.908(3) Co1 N21 1.923(3) Co1 N51 1.959(3) Co2 O1 1.983(2) Co2 O4 1.903(2) Co2 O5 1.886(3) Co2 N31 1.910(3) Co2 N41 1.920(3) Co2 N61 1.960(3) O1 C65 1.379(4) N11 C12 1.338(4) N11 C16 1.357(4) C12 C13 1.377(5) C13 C14 1.390(5) C14 C15 1.381(5) C15 C16 1.378(5) C16 C17 1.495(5) C17 N51 1.495(4) N21 C22 1.346(4) N21 C26 1.348(4) C22 C23 1.386(5) C23 C24 1.386(5) C24 C25 1.385(5) C25 C26 1.380(4) C26 C27 1.493(5) C27 N51 1.512(4) N31 C32 1.339(4) N31 C36 1.357(4) C32 C33 1.387(5) C33 C34 1.378(6) C34 C35 1.392(6) C35 C36 1.381(5) C36 C37 1.508(5) C37 N61 1.491(4) N41 C42 1.347(4) N41 C46 1.356(4) C42 C43 1.375(5) C43 C44 1.387(6) C44 C45 1.382(6) C45 C46 1.380(5) C46 C47 1.489(5) C47 N61 1.496(4) N51 C52 1.495(4) C52 C53 1.503(4) C53 C65 1.391(4) C53 C54 1.393(4) C54 C55 1.395(5) C55 C64 1.396(5) C55 C56 1.537(4) C56 C58 1.514(5) C56 C57 1.520(5) C56 C59 1.532(5) N61 C62 1.505(4) C62 C63 1.497(5) C63 C65 1.388(4) C63 C64 1.396(4) Cl1 O6 1.426(3) Cl1 O8 1.437(3) Cl1 O7 1.447(3) Cl1 O9 1.447(2) Cl2 O12 1.421(3) Cl2 O10 1.430(3) Cl2 O11 1.445(3) Cl2 O13 1.446(2) Cl3 O17 1.414(3) Cl3 O14 1.423(3) Cl3 O16 1.444(3) Cl3 O15 1.468(4) C1 C2 1.359(9) C2 N3 1.226(8) O2 H2a 1.10(6) O2 H2b 0.75(5) O3 H3b 0.65(4) O3 H3a 1.14(7) O4 H4 0.75(4) O4 H2a 1.35(6) O5 H5 0.60(5) O5 H3a 1.32(7) C12 H12 0.950 C13 H13 0.950 C14 H14 0.950 C15 H15 0.950 C17 H17a 0.950 C17 H17b 0.950 C22 H22 0.950 C23 H23 0.950 C24 H24 0.950 C25 H25 0.950 C27 H27b 0.950 C27 H27a 0.950 C32 H32 0.950 C33 H33 0.950 C34 H34 0.950 C35 H35 0.950 C37 H37a 0.950 C37 H37b 0.950 C42 H42 0.950 C43 H43 0.950 C44 H44 0.950 C45 H45 0.950 C47 H47b 0.950 C47 H47a 0.950 C52 H52a 0.950 C52 H52b 0.950 C54 H54 0.950 C57 H57c 0.950 C57 H57a 0.950 C57 H57b 0.950 C58 H58a 0.950 C58 H58b 0.950 C58 H58c 0.950 C59 H59c 0.950 C59 H59a 0.950 C59 H59b 0.950 C62 H62a 0.950 C62 H62b 0.950 C64 H64 0.950 O18 H18b 0.804 O18 H18a 0.808 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Co1 O2 87.7(1) O1 Co1 O3 88.2(1) O1 Co1 N11 175.7(1) O1 Co1 N21 88.6(1) O1 Co1 N51 95.1(1) O2 Co1 O3 92.5(1) O2 Co1 N11 89.3(1) O2 Co1 N21 174.7(1) O2 Co1 N51 90.9(1) O3 Co1 N11 94.9(1) O3 Co1 N21 91.2(1) O3 Co1 N51 175.3(1) N11 Co1 N21 94.2(1) N11 Co1 N51 81.9(1) N21 Co1 N51 85.6(1) O1 Co2 O4 90.2(1) O1 Co2 O5 87.0(1) O1 Co2 N31 175.8(1) O1 Co2 N41 88.1(1) O1 Co2 N61 94.3(1) O4 Co2 O5 92.5(1) O4 Co2 N31 93.6(1) O4 Co2 N41 91.9(1) O4 Co2 N61 174.9(1) O5 Co2 N31 91.0(1) O5 Co2 N41 173.3(1) O5 Co2 N61 90.2(1) N31 Co2 N41 93.7(1) N31 Co2 N61 82.0(1) N41 Co2 N61 85.7(1) Co1 O1 C65 114.4(2) Co2 O1 C65 114.4(2) Co1 O1 Co2 131.2(1) Co1 O2 H2b 108(3) Co1 O2 H2a 110(3) Co1 O3 H3b 112(4) Co1 O3 H3a 112(3) Co2 O4 H4 108(4) Co2 O4 H2a 111(2) Co2 O5 H5 110(5) Co2 O5 H3a 109(3) Co1 N11 C12 126.2(2) Co1 N11 C16 114.1(2) Co1 N21 C22 124.6(2) Co1 N21 C26 115.1(2) Co2 N31 C32 125.7(3) Co2 N31 C36 114.3(2) Co2 N41 C42 125.3(2) Co2 N41 C46 114.4(2) Co1 N51 C52 111.7(2) Co1 N51 C17 105.3(2) Co1 N51 C27 108.2(2) Co2 N61 C37 105.8(2) Co2 N61 C47 108.8(2) Co2 N61 C62 112.1(2) C12 N11 C16 119.7(3) N11 C12 C13 121.6(3) C12 C13 C14 119.3(4) C13 C14 C15 118.8(4) C14 C15 C16 119.6(3) N11 C16 C15 121.0(3) N11 C16 C17 113.5(3) C15 C16 C17 125.5(3) C16 C17 N51 106.3(3) C22 N21 C26 119.3(3) N21 C22 C23 121.3(3) C22 C23 C24 119.1(3) C23 C24 C25 119.5(3) C24 C25 C26 118.4(3) N21 C26 C25 122.3(3) N21 C26 C27 113.6(3) C25 C26 C27 124.0(3) C26 C27 N51 109.6(3) C32 N31 C36 119.9(3) N31 C32 C33 121.4(4) C32 C33 C34 118.9(3) C33 C34 C35 119.8(3) C34 C35 C36 118.6(4) N31 C36 C35 121.2(3) N31 C36 C37 113.4(3) C35 C36 C37 125.4(3) C36 C37 N61 106.1(3) C42 N41 C46 119.1(3) N41 C42 C43 121.3(3) C42 C43 C44 119.7(4) C43 C44 C45 119.2(4) C44 C45 C46 118.7(4) N41 C46 C45 122.0(3) N41 C46 C47 114.5(3) C45 C46 C47 123.4(3) C46 C47 N61 109.9(3) C17 N51 C52 111.8(2) C27 N51 C52 110.2(2) C17 N51 C27 109.4(2) N51 C52 C53 109.6(3) C54 C53 C65 119.2(3) C52 C53 C65 118.2(3) C52 C53 C54 122.6(3) C53 C54 C55 121.9(3) C54 C55 C64 117.5(3) C54 C55 C56 122.4(3) C56 C55 C64 119.9(3) C57 C56 C58 108.9(3) C58 C56 C59 109.3(3) C55 C56 C58 112.0(3) C57 C56 C59 107.8(3) C55 C56 C57 111.0(3) C55 C56 C59 107.7(3) C37 N61 C47 108.5(3) C37 N61 C62 111.3(3) C47 N61 C62 110.0(2) N61 C62 C63 108.3(3) C64 C63 C65 119.3(3) C62 C63 C65 118.7(3) C62 C63 C64 121.8(3) C55 C64 C63 121.7(3) O1 C65 C63 119.6(3) O1 C65 C53 119.9(3) C53 C65 C63 120.5(3) O6 Cl1 O8 110.1(2) O6 Cl1 O7 109.5(2) O6 Cl1 O9 109.8(2) O7 Cl1 O8 108.6(2) O8 Cl1 O9 109.8(2) O7 Cl1 O9 109.0(2) O10 Cl2 O12 109.8(2) O11 Cl2 O12 109.7(2) O12 Cl2 O13 110.3(2) O10 Cl2 O11 109.0(2) O10 Cl2 O13 109.7(2) O11 Cl2 O13 108.4(2) O14 Cl3 O17 112.0(2) O16 Cl3 O17 111.8(2) O15 Cl3 O17 107.7(3) O14 Cl3 O16 109.2(2) O14 Cl3 O15 107.9(2) O15 Cl3 O16 108.0(2) C1 C2 N3 173.5(7) H2a O2 H2b 110(4) H3a O3 H3b 105(5) H2a O4 H4 108(4) H3a O5 H5 113(6) N11 C12 H12 119.2 C13 C12 H12 119.2 C12 C13 H13 120.3 C14 C13 H13 120.3 C15 C14 H14 120.6 C13 C14 H14 120.6 C16 C15 H15 120.2 C14 C15 H15 120.2 H17a C17 H17b 109.5 C16 C17 H17a 110.3 N51 C17 H17a 110.3 C16 C17 H17b 110.3 N51 C17 H17b 110.3 N21 C22 H22 119.3 C23 C22 H22 119.3 C24 C23 H23 120.4 C22 C23 H23 120.4 C25 C24 H24 120.2 C23 C24 H24 120.2 C26 C25 H25 120.8 C24 C25 H25 120.8 H27a C27 H27b 109.5 C26 C27 H27b 109.4 N51 C27 H27b 109.4 C26 C27 H27a 109.4 N51 C27 H27a 109.4 N31 C32 H32 119.3 C33 C32 H32 119.3 C34 C33 H33 120.5 C32 C33 H33 120.5 C33 C34 H34 120.1 C35 C34 H34 120.1 C36 C35 H35 120.7 C34 C35 H35 120.7 H37a C37 H37b 109.5 N61 C37 H37a 110.3 C36 C37 H37a 110.3 N61 C37 H37b 110.3 C36 C37 H37b 110.3 N41 C42 H42 119.4 C43 C42 H42 119.4 C42 C43 H43 120.1 C44 C43 H43 120.1 C45 C44 H44 120.4 C43 C44 H44 120.4 C46 C45 H45 120.6 C44 C45 H45 120.6 H47a C47 H47b 109.5 C46 C47 H47b 109.4 N61 C47 H47b 109.4 C46 C47 H47a 109.4 N61 C47 H47a 109.4 H52a C52 H52b 109.5 N51 C52 H52a 109.4 C53 C52 H52a 109.4 N51 C52 H52b 109.4 C53 C52 H52b 109.4 C53 C54 H54 119.1 C55 C54 H54 119.1 H57a C57 H57c 109.1 H57b C57 H57c 109.5 C56 C57 H57c 109.1 H57a C57 H57b 109.1 C56 C57 H57a 111.0 C56 C57 H57b 109.1 H58a C58 H58b 108.8 H58a C58 H58c 108.8 C56 C58 H58a 112.0 H58b C58 H58c 109.5 C56 C58 H58b 108.8 C56 C58 H58c 108.8 H59a C59 H59c 109.9 H59b C59 H59c 109.5 C56 C59 H59c 109.9 H59a C59 H59b 109.9 C56 C59 H59a 107.7 C56 C59 H59b 109.9 H62a C62 H62b 109.5 C63 C62 H62a 109.8 N61 C62 H62a 109.8 C63 C62 H62b 109.8 N61 C62 H62b 109.8 C63 C64 H64 119.1 C55 C64 H64 119.1 H18a O18 H18b 118.4 #loop_ #_geom_bond_atom_site_label_D #_geom_bond_atom_site_label_H #_geom_contact_atom_site_label_A #_geom_bond_distance_DH #_geom_contact_distance_HA #_geom_contact_distance_DA #_geom_angle_DHA #O2 H2a O4 1.10(6) 1.35(6) 2.437(3) 170(5) #O3 H3a O5 1.14(7) 1.32(7) 2.456(4) 172(6) #O2 H2b O9 0.75(5) 2.22(5) 2.963(4) 176(5) #O3 H3b O7 0.65(4) 2.09(4) 2.736(4) 172(4) #O4 H4 O18 0.75(4) 2.05(5) 2.787(4) 168(5) #O5 H5 O13 0.60(5) 2.45(5) 3.036(4) 165(6) #============================================================================== data_newjtg77 _database_code_CSD 195397 #================================== # 5. CHEMICAL DATA _chemical_name_systematic ; insert name here ; _chemical_name_common [Co2(bpbp)(NH2NHCO2)2](ClO4).3.875H2O _chemical_formula_sum 'C38 H48.75 Cl1 Co2 N10 O12.875' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety 'C38 H49 Co2 N10 O9, Cl O4,3.875(H2 O)' _chemical_formula_weight 1006.99 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _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 10.823(2) _cell_length_b 12.824(2) _cell_length_c 16.787(2) _cell_angle_alpha 85.545(3) _cell_angle_beta 84.364(3) _cell_angle_gamma 78.741(3) _cell_formula_units_Z 2 _cell_volume 2270.0(5) _cell_measurement_temperature 295 _cell_measurement_reflns_used 6668 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1045.50 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'XPREP (Siemens, 1995)' _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_T_max 0.951 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method ; \w rotation scans with narrow frames ; _diffrn_standards_decay_% 0 _diffrn_reflns_number 28542 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_reduction_process 11537 _reflns_number_total 10436 _reflns_number_gt 6233 _reflns_threshold_expression I>1.5\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997) KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1/{[\s~cs~(F^2^)+B +(1+A)F^2^]^1/2^-|F|}^2^ A = 0.03, B = 0.5 ; _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6231 _refine_ls_number_parameters 603 _refine_ls_number_restraints 0 _refine_ls_number_constraints 2 _refine_ls_R_factor_gt 0.056 _refine_ls_wR_factor_ref 0.052 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_shift/su_max 0.0005 _refine_ls_shift/su_mean 0.00003 _refine_diff_density_max 0.80(9) _refine_diff_density_min -0.67(9) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type _atom_site_occupancy Co1 Co 0.67610(6) 0.23022(5) 0.66869(4) 0.0383(4) Uij 1. Co2 Co 0.31631(6) 0.34362(5) 0.68745(3) 0.0368(4) Uij 1. O1 O 0.4957(3) 0.2763(2) 0.7303(2) 0.038(2) Uij 1. N1 N 0.5925(4) 0.1519(4) 0.5860(2) 0.042(3) Uij 1. N2 N 0.6281(4) 0.1970(3) 0.5092(2) 0.052(3) Uij 1. C1 C 0.6655(5) 0.2942(4) 0.5041(3) 0.046(3) Uij 1. O2 O 0.6915(4) 0.3320(3) 0.4351(2) 0.066(3) Uij 1. O3 O 0.6700(3) 0.3374(2) 0.5694(2) 0.046(2) Uij 1. N3 N 0.3988(5) 0.4432(4) 0.5962(3) 0.049(3) Uij 1. N4 N 0.3730(4) 0.4092(4) 0.5228(2) 0.057(3) Uij 1. C2 C 0.3369(5) 0.3139(4) 0.5215(3) 0.050(3) Uij 1. O4 O 0.3244(3) 0.2592(2) 0.5880(2) 0.046(2) Uij 1. O5 O 0.3195(3) 0.2833(3) 0.4549(2) 0.069(3) Uij 1. N11 N 0.8599(4) 0.1443(3) 0.6179(2) 0.047(3) Uij 1. N21 N 0.7510(3) 0.3116(3) 0.7509(2) 0.043(3) Uij 1. N31 N 0.1355(4) 0.4485(3) 0.6599(2) 0.049(3) Uij 1. N41 N 0.2285(3) 0.2427(3) 0.7686(2) 0.038(2) Uij 1. N51 N 0.7307(4) 0.1013(3) 0.7565(2) 0.042(2) Uij 1. N61 N 0.2669(3) 0.4448(3) 0.7863(2) 0.037(2) Uij 1. C12 C 0.9413(5) 0.1831(4) 0.5633(3) 0.057(4) Uij 1. C13 C 1.0591(6) 0.1259(5) 0.5412(4) 0.073(4) Uij 1. C14 C 1.0967(6) 0.0264(6) 0.5764(4) 0.083(5) Uij 1. C15 C 1.0132(6) -0.0150(5) 0.6320(3) 0.071(4) Uij 1. C16 C 0.8964(5) 0.0465(4) 0.6513(3) 0.051(3) Uij 1. C17 C 0.8008(5) 0.0096(4) 0.7128(3) 0.049(3) Uij 1. C22 C 0.7349(5) 0.4173(4) 0.7520(3) 0.055(4) Uij 1. C23 C 0.7595(6) 0.4677(5) 0.8158(4) 0.071(5) Uij 1. C24 C 0.7991(6) 0.4064(6) 0.8837(4) 0.077(5) Uij 1. C25 C 0.8149(5) 0.2982(5) 0.8837(3) 0.062(4) Uij 1. C26 C 0.7911(4) 0.2524(4) 0.8164(3) 0.045(3) Uij 1. C27 C 0.8152(5) 0.1332(4) 0.8106(3) 0.050(3) Uij 1. C32 C 0.0517(5) 0.4313(5) 0.6111(3) 0.060(4) Uij 1. C33 C -0.0579(6) 0.5040(6) 0.5985(3) 0.078(5) Uij 1. C34 C -0.0802(6) 0.5974(6) 0.6367(4) 0.084(5) Uij 1. C35 C 0.0036(6) 0.6152(5) 0.6881(4) 0.072(4) Uij 1. C36 C 0.1114(5) 0.5389(4) 0.6983(3) 0.050(3) Uij 1. C37 C 0.2073(5) 0.5505(4) 0.7535(3) 0.050(3) Uij 1. C42 C 0.2297(5) 0.1408(4) 0.7594(3) 0.046(3) Uij 1. C43 C 0.1871(5) 0.0741(4) 0.8194(3) 0.056(4) Uij 1. C44 C 0.1455(5) 0.1138(5) 0.8927(3) 0.064(4) Uij 1. C45 C 0.1455(5) 0.2193(4) 0.9035(3) 0.053(3) Uij 1. C46 C 0.1864(4) 0.2822(4) 0.8397(3) 0.039(3) Uij 1. C47 C 0.1763(4) 0.4000(4) 0.8445(3) 0.043(3) Uij 1. C52 C 0.6140(5) 0.0750(4) 0.8009(3) 0.043(3) Uij 1. C53 C 0.5475(4) 0.1659(4) 0.8495(3) 0.038(3) Uij 1. C54 C 0.5469(4) 0.1539(4) 0.9326(3) 0.040(3) Uij 1. C55 C 0.4969(4) 0.2365(4) 0.9812(3) 0.041(3) Uij 1. C56 C 0.4925(5) 0.2255(4) 1.0723(3) 0.047(3) Uij 1. C57 C 0.5431(6) 0.3182(5) 1.1031(3) 0.070(4) Uij 1. C58 C 0.5728(5) 0.1217(4) 1.1023(3) 0.060(4) Uij 1. C59 C 0.3552(6) 0.2308(5) 1.1069(3) 0.068(4) Uij 1. C62 C 0.3833(4) 0.4523(4) 0.8227(3) 0.043(3) Uij 1. C63 C 0.4435(4) 0.3469(4) 0.8599(3) 0.039(3) Uij 1. C64 C 0.4455(4) 0.3327(4) 0.9424(3) 0.041(3) Uij 1. C65 C 0.4956(4) 0.2627(4) 0.8109(2) 0.035(3) Uij 1. Cl1 Cl 0.9630(2) 0.1945(1) 1.1193(1) 0.064(1) Uij 1. O8 O 0.8992(6) 0.1825(4) 1.1938(3) 0.138(5) Uij 1. O9 O 0.9657(9) 0.2928(4) 1.0910(4) 0.224(9) Uij 1. O10 O 0.9087(9) 0.1472(7) 1.0640(4) 0.209(9) Uij 1. O11 O 1.0770(7) 0.1291(7) 1.1128(5) 0.228(9) Uij 1. O12 O 0.6864(5) 0.2035(4) 1.3109(2) 0.099(4) Uij 1. O13 O 0.4481(5) 0.3712(4) 1.3238(3) 0.119(4) Uij 1. O14 O 0.6449(5) -0.0764(4) 0.5395(3) 0.100(5) Uij 0.875(9) O15 O 0.4123(6) -0.0326(4) 0.6176(3) 0.110(5) Uij 0.875 O16 O 0.5456(19) -0.0862(15) 0.6132(13) 0.028(13) Uij 0.125 HN1a H 0.499(5) 0.169(4) 0.592(3) 0.07(2) Uiso 1. HN1b H 0.612(4) 0.083(3) 0.587(2) 0.03(1) Uiso 1. HN3a H 0.477(5) 0.431(4) 0.601(3) 0.06(2) Uiso 1. HN3b H 0.374(5) 0.516(5) 0.594(3) 0.09(2) Uiso 1. HN2 H 0.6260 0.1609 0.4622 0.062 Uiso 1. HN4 H 0.3807 0.4526 0.4748 0.068 Uiso 1. H12 H 0.9164 0.2525 0.5390 0.068 Uiso 1. H13 H 1.1140 0.1551 0.5018 0.087 Uiso 1. H14 H 1.1786 -0.0137 0.5629 0.099 Uiso 1. H15 H 1.0361 -0.0845 0.6565 0.085 Uiso 1. H17a H 0.7435 -0.0209 0.6867 0.059 Uiso 1. H17b H 0.8431 -0.0422 0.7494 0.059 Uiso 1. H22 H 0.7049 0.4595 0.7063 0.066 Uiso 1. H23 H 0.7496 0.5430 0.8138 0.085 Uiso 1. H24 H 0.8151 0.4392 0.9294 0.093 Uiso 1. H25 H 0.8419 0.2548 0.9295 0.075 Uiso 1. H27a H 0.9005 0.1099 0.7905 0.060 Uiso 1. H27b H 0.8011 0.1005 0.8626 0.060 Uiso 1. H32 H 0.0681 0.3668 0.5842 0.072 Uiso 1. H33 H -0.1165 0.4897 0.5642 0.093 Uiso 1. H34 H -0.1534 0.6497 0.6275 0.101 Uiso 1. H35 H -0.0121 0.6787 0.7162 0.087 Uiso 1. H37a H 0.2702 0.5843 0.7248 0.061 Uiso 1. H37b H 0.1671 0.5926 0.7962 0.061 Uiso 1. H42 H 0.2614 0.1126 0.7092 0.056 Uiso 1. H43 H 0.1866 0.0020 0.8103 0.067 Uiso 1. H44 H 0.1170 0.0692 0.9356 0.076 Uiso 1. H45 H 0.1178 0.2482 0.9540 0.064 Uiso 1. H47a H 0.0930 0.4345 0.8342 0.052 Uiso 1. H47b H 0.1922 0.4133 0.8971 0.052 Uiso 1. H52a H 0.6359 0.0135 0.8357 0.052 Uiso 1. H52b H 0.5592 0.0612 0.7637 0.052 Uiso 1. H54 H 0.5820 0.0866 0.9568 0.048 Uiso 1. H57a H 0.5404 0.3114 1.1600 0.084 Uiso 1. H57b H 0.4922 0.3840 1.0869 0.084 Uiso 1. H57c H 0.6279 0.3164 1.0814 0.084 Uiso 1. H58a H 0.5701 0.1149 1.1592 0.072 Uiso 1. H58b H 0.6579 0.1196 1.0812 0.072 Uiso 1. H58c H 0.5424 0.0639 1.0841 0.072 Uiso 1. H59a H 0.3525 0.2240 1.1638 0.081 Uiso 1. H59b H 0.3226 0.1746 1.0880 0.081 Uiso 1. H59c H 0.3057 0.2972 1.0905 0.081 Uiso 1. H62a H 0.3628 0.5025 0.8630 0.051 Uiso 1. H62b H 0.4415 0.4756 0.7824 0.051 Uiso 1. H64 H 0.4101 0.3914 0.9739 0.049 Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0387(4) 0.0377(4) 0.0363(3) -0.0038(3) -0.0028(3) 0.0021(3) Co2 0.0380(4) 0.0367(4) 0.0340(3) -0.0059(3) -0.0004(3) 0.0021(3) O1 0.040(2) 0.040(2) 0.033(2) -0.006(1) -0.003(1) 0.000(1) N1 0.052(3) 0.031(3) 0.041(2) -0.006(2) 0.000(2) 0.000(2) N2 0.068(3) 0.054(3) 0.032(2) -0.011(2) -0.001(2) 0.000(2) C1 0.046(3) 0.039(3) 0.046(3) 0.005(2) 0.002(2) 0.006(2) O2 0.092(3) 0.054(2) 0.043(2) -0.006(2) 0.009(2) 0.013(2) O3 0.052(2) 0.042(2) 0.042(2) -0.009(2) 0.001(2) 0.004(2) N3 0.041(3) 0.047(3) 0.055(3) -0.007(2) -0.002(2) 0.012(2) N4 0.068(3) 0.056(3) 0.040(2) -0.004(2) 0.001(2) 0.013(2) C2 0.037(3) 0.065(4) 0.040(3) 0.005(3) -0.005(2) 0.004(3) O4 0.051(2) 0.049(2) 0.035(2) -0.006(2) -0.003(1) 0.001(1) O5 0.063(3) 0.106(3) 0.038(2) -0.015(2) -0.012(2) -0.003(2) N11 0.042(2) 0.047(3) 0.048(2) -0.002(2) -0.002(2) -0.003(2) N21 0.036(2) 0.045(3) 0.047(2) -0.008(2) -0.002(2) -0.002(2) N31 0.045(3) 0.058(3) 0.041(2) -0.008(2) -0.006(2) 0.006(2) N41 0.040(2) 0.037(2) 0.039(2) -0.011(2) -0.002(2) -0.002(2) N51 0.047(3) 0.037(2) 0.040(2) -0.003(2) -0.006(2) -0.001(2) N61 0.039(2) 0.029(2) 0.041(2) -0.004(2) -0.003(2) 0.002(2) C12 0.048(3) 0.062(4) 0.061(3) -0.009(3) -0.001(3) -0.003(3) C13 0.055(4) 0.086(5) 0.072(4) -0.004(4) 0.008(3) -0.006(3) C14 0.051(4) 0.098(5) 0.086(5) 0.016(4) 0.006(3) -0.015(4) C15 0.066(4) 0.067(4) 0.068(4) 0.013(3) -0.001(3) -0.004(3) C16 0.047(3) 0.053(3) 0.048(3) 0.006(3) -0.006(2) -0.010(3) C17 0.058(3) 0.038(3) 0.047(3) 0.004(3) -0.003(2) -0.004(2) C22 0.052(3) 0.048(4) 0.065(4) -0.015(3) 0.003(3) -0.006(3) C23 0.074(4) 0.052(4) 0.089(5) -0.020(3) 0.007(4) -0.020(3) C24 0.082(5) 0.082(5) 0.077(4) -0.029(4) -0.003(4) -0.033(4) C25 0.054(4) 0.079(5) 0.056(3) -0.011(3) -0.012(3) -0.014(3) C26 0.033(3) 0.051(3) 0.053(3) -0.008(2) -0.005(2) -0.008(2) C27 0.045(3) 0.055(4) 0.047(3) 0.000(3) -0.010(2) -0.001(2) C32 0.050(4) 0.084(4) 0.047(3) -0.016(3) -0.005(3) 0.002(3) C33 0.043(4) 0.125(6) 0.060(4) -0.009(4) -0.010(3) 0.014(4) C34 0.054(4) 0.104(6) 0.079(5) 0.017(4) -0.011(3) 0.022(4) C35 0.060(4) 0.073(4) 0.073(4) 0.009(3) -0.008(3) 0.009(3) C36 0.044(3) 0.047(3) 0.052(3) 0.000(3) -0.002(2) 0.013(3) C37 0.049(3) 0.038(3) 0.059(3) 0.002(2) -0.003(2) 0.000(2) C42 0.051(3) 0.042(3) 0.048(3) -0.014(2) -0.003(2) -0.004(2) C43 0.058(4) 0.041(3) 0.071(4) -0.017(3) -0.005(3) 0.004(3) C44 0.067(4) 0.058(4) 0.062(4) -0.017(3) 0.006(3) 0.019(3) C45 0.059(4) 0.056(4) 0.043(3) -0.009(3) 0.008(2) 0.001(2) C46 0.036(3) 0.041(3) 0.039(3) -0.006(2) -0.001(2) 0.002(2) C47 0.040(3) 0.046(3) 0.041(3) -0.004(2) 0.002(2) -0.007(2) C52 0.052(3) 0.034(3) 0.040(3) -0.006(2) -0.004(2) 0.006(2) C53 0.041(3) 0.035(3) 0.040(3) -0.009(2) -0.004(2) -0.001(2) C54 0.044(3) 0.038(3) 0.040(3) -0.012(2) -0.007(2) 0.004(2) C55 0.043(3) 0.043(3) 0.039(3) -0.013(2) -0.007(2) 0.001(2) C56 0.059(3) 0.049(3) 0.035(3) -0.015(3) -0.004(2) -0.003(2) C57 0.093(5) 0.074(4) 0.051(3) -0.028(4) -0.020(3) -0.005(3) C58 0.077(4) 0.069(4) 0.038(3) -0.019(3) -0.014(3) 0.005(3) C59 0.068(4) 0.078(4) 0.054(3) -0.014(3) 0.010(3) 0.000(3) C62 0.043(3) 0.039(3) 0.048(3) -0.011(2) -0.005(2) -0.005(2) C63 0.037(3) 0.037(3) 0.044(3) -0.009(2) -0.006(2) -0.001(2) C64 0.045(3) 0.041(3) 0.041(3) -0.013(2) -0.004(2) -0.010(2) C65 0.033(3) 0.041(3) 0.035(2) -0.014(2) -0.006(2) 0.001(2) Cl1 0.065(1) 0.068(1) 0.053(1) -0.015(1) 0.010(1) 0.005(1) O8 0.217(6) 0.101(4) 0.086(3) -0.045(4) 0.084(4) -0.019(3) O9 0.394(12) 0.069(4) 0.176(6) -0.052(5) 0.165(7) -0.019(4) O10 0.277(10) 0.286(10) 0.104(5) -0.154(9) -0.019(5) -0.001(5) O11 0.113(6) 0.314(11) 0.194(7) 0.044(6) 0.031(5) 0.108(7) O12 0.118(4) 0.099(3) 0.073(3) -0.018(3) 0.022(3) 0.003(2) O13 0.130(5) 0.121(4) 0.086(3) 0.002(3) 0.008(3) 0.031(3) O14 0.097(4) 0.085(4) 0.118(5) -0.018(3) 0.017(3) -0.037(3) O15 0.123(6) 0.091(4) 0.115(5) -0.027(4) 0.025(4) -0.016(3) O16 0.013(12) 0.014(11) 0.058(15) -0.010(9) 0.002(10) -0.007(10) #================================= # 10. MOLECULAR GEOMETRY #2_666 1.000000 -1 0 0 1.000000 0 -1 0 1.000000 0 0 -1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Co1 Co2 3.873(1) Co1 O1 2.116(3) Co1 O3 2.074(3) Co1 N1 2.138(4) Co1 N11 2.204(4) Co1 N21 2.104(4) Co1 N51 2.160(4) Co2 O1 2.134(3) Co2 O4 2.045(3) Co2 N3 2.156(4) Co2 N31 2.215(4) Co2 N41 2.094(3) Co2 N61 2.148(4) O1 C65 1.352(5) N1 N2 1.421(5) N2 C1 1.378(6) C1 O2 1.249(5) C1 O3 1.275(5) N3 N4 1.408(6) N4 C2 1.356(6) C2 O4 1.281(5) C2 O5 1.256(5) N11 C16 1.337(6) N11 C12 1.343(6) N21 C22 1.334(6) N21 C26 1.344(6) N31 C36 1.338(6) N31 C32 1.341(6) N41 C42 1.326(5) N41 C46 1.337(5) N51 C17 1.474(5) N51 C27 1.482(6) N51 C52 1.486(6) N61 C37 1.472(6) N61 C62 1.476(5) N61 C47 1.480(5) C12 C13 1.373(7) C13 C14 1.368(8) C14 C15 1.383(8) C15 C16 1.376(7) C16 C17 1.505(7) C22 C23 1.366(7) C23 C24 1.387(8) C24 C25 1.365(8) C25 C26 1.381(7) C26 C27 1.508(7) C32 C33 1.381(8) C33 C34 1.371(9) C34 C35 1.373(9) C35 C36 1.384(7) C36 C37 1.493(7) C42 C43 1.374(6) C43 C44 1.369(7) C44 C45 1.379(7) C45 C46 1.379(6) C46 C47 1.500(6) C52 C53 1.499(6) C53 C54 1.392(6) C53 C65 1.396(6) C54 C55 1.379(6) C55 C64 1.391(6) C55 C56 1.523(6) C56 C58 1.520(7) C56 C59 1.533(7) C56 C57 1.545(7) C62 C63 1.498(6) C63 C64 1.384(6) C63 C65 1.403(6) Cl1 O8 1.381(4) Cl1 O9 1.316(5) Cl1 O10 1.382(7) Cl1 O11 1.350(7) O14 O16 1.572(20) O15 O16 1.469(21) N1 HN1b 0.87(4) N1 HN1a 0.99(5) N3 HN3a 0.84(5) N3 HN3b 0.92(6) N2 HN2 0.950 N4 HN4 0.950 C12 H12 0.950 C13 H13 0.950 C14 H14 0.950 C15 H15 0.950 C17 H17a 0.950 C17 H17b 0.950 C22 H22 0.950 C23 H23 0.950 C24 H24 0.950 C25 H25 0.950 C27 H27a 0.950 C27 H27b 0.950 C32 H32 0.950 C33 H33 0.950 C34 H34 0.950 C35 H35 0.950 C37 H37a 0.950 C37 H37b 0.950 C42 H42 0.950 C43 H43 0.950 C44 H44 0.950 C45 H45 0.950 C47 H47a 0.950 C47 H47b 0.950 C52 H52a 0.950 C52 H52b 0.950 C54 H54 0.950 C57 H57a 0.950 C57 H57b 0.950 C57 H57c 0.950 C58 H58a 0.950 C58 H58b 0.950 C58 H58c 0.950 C59 H59a 0.950 C59 H59b 0.950 C59 H59c 0.950 C62 H62a 0.950 C62 H62b 0.950 C64 H64 0.950 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Co1 O3 102.7(1) O1 Co1 N1 89.4(1) O1 Co1 N11 166.3(1) O1 Co1 N21 88.4(1) O1 Co1 N51 92.5(1) O3 Co1 N1 78.3(1) O3 Co1 N21 101.2(1) O3 Co1 N51 164.8(1) O3 Co1 N11 89.3(1) N1 Co1 N11 86.5(2) N1 Co1 N21 177.6(2) N1 Co1 N51 101.1(2) N11 Co1 N21 95.8(1) N11 Co1 N51 75.5(1) N21 Co1 N51 80.1(1) O1 Co2 O4 100.3(1) O1 Co2 N3 92.4(2) O1 Co2 N31 165.3(1) O1 Co2 N41 90.7(1) O1 Co2 N61 91.8(1) O4 Co2 N3 78.4(2) O4 Co2 N31 93.0(1) O4 Co2 N41 97.4(1) O4 Co2 N61 167.8(1) N3 Co2 N31 84.3(2) N3 Co2 N41 175.2(2) N3 Co2 N61 102.9(2) N31 Co2 N41 93.6(1) N31 Co2 N61 75.1(1) N41 Co2 N61 80.7(1) Co1 O1 C65 113.8(2) Co2 O1 C65 114.9(2) Co1 O1 Co2 131.3(1) Co1 N1 N2 104.9(3) Co1 O3 C1 113.0(3) Co2 N3 N4 105.2(3) Co2 o4 C2 114.1(3) Co1 N11 C12 127.0(3) Co1 N11 C16 114.7(3) Co1 N21 C22 124.8(3) Co1 N21 C26 115.0(3) Co2 N31 C32 127.9(4) Co2 N31 C36 113.4(3) Co2 N41 C42 125.3(3) Co2 N41 C46 115.1(3) Co1 N51 C17 107.5(3) Co1 N51 C27 109.5(3) Co1 N51 C52 108.3(3) Co2 N61 C37 107.1(3) Co2 N61 C47 108.8(3) Co2 N61 C62 108.8(3) N1 N2 C1 118.8(4) O2 C1 O3 126.0(5) N2 C1 O2 116.2(5) N2 C1 O3 117.8(4) N3 N4 C2 119.3(4) O5 C2 O4 123.5(5) N4 C2 O5 118.1(5) N4 C2 O4 118.4(5) C12 N11 C16 118.0(4) C22 N21 C26 118.3(4) C32 N31 C36 118.8(5) C42 N41 C46 118.7(4) C17 N51 C27 108.9(4) C17 N51 C52 110.7(4) C27 N51 C52 111.9(3) C37 N61 C62 110.0(3) C37 N61 C47 110.3(3) C47 N61 C62 111.8(3) N11 C12 C13 122.3(5) C12 C13 C14 119.4(5) C13 C14 C15 118.8(6) C14 C15 C16 118.8(5) N11 C16 C15 122.6(5) N11 C16 C17 114.8(4) C15 C16 C17 122.6(5) N51 C17 C16 109.4(4) N21 C22 C23 123.0(5) C22 C23 C24 118.6(5) C23 C24 C25 119.0(5) C24 C25 C26 119.4(5) N21 C26 C25 121.7(5) N21 C26 C27 116.3(4) C25 C26 C27 121.8(5) N51 C27 C26 111.6(4) N31 C32 C33 122.2(6) C32 C33 C34 118.6(6) C33 C34 C35 119.8(6) C34 C35 C36 118.7(6) N31 C36 C35 121.9(5) N31 C36 C37 115.5(4) C35 C36 C37 122.6(5) N61 C37 C36 109.8(4) N41 C42 C43 122.9(4) C42 C43 C44 118.5(5) C43 C44 C45 119.2(4) C44 C45 C46 119.0(4) N41 C46 C45 121.6(4) N41 C46 C47 116.4(4) C45 C46 C47 121.9(4) N61 C47 C46 113.0(3) N51 C52 C53 110.4(4) C54 C53 C65 121.3(4) C52 C53 C54 118.7(4) C52 C53 C65 119.9(4) C53 C54 C55 122.2(4) C54 C55 C64 116.2(4) C54 C55 C56 123.5(4) C56 C55 C64 120.2(4) C55 C56 C58 112.1(4) C58 C56 C59 109.4(4) C57 C56 C58 107.9(4) C55 C56 C59 109.1(4) C55 C56 C57 109.6(4) C57 C56 C59 108.7(4) N61 C62 C63 111.5(4) C64 C63 C65 120.4(4) C62 C63 C64 119.8(4) C62 C63 C65 119.8(4) C55 C64 C63 123.0(4) O1 C65 C53 122.3(4) O1 C65 C63 120.8(4) C53 C65 C63 116.9(4) O14 O16 O15 125.1(15) O8 Cl1 O9 116.7(3) O8 Cl1 O10 108.9(4) O8 Cl1 O11 112.2(4) O9 Cl1 O10 107.0(5) O9 Cl1 O11 113.5(5) O10 Cl1 O11 96.3(6) Co1 N1 HN1b 118(3) Co1 N1 HN1a 113(3) Co1 O3 HN3a 97(1) Co2 N3 HN3a 107(3) Co2 N3 HN3b 122(4) Co2 O4 HN1a 100(1) HN1a N1 HN1b 106(4) N2 N1 HN1b 110(3) N2 N1 HN1a 105(3) C1 N2 HN2 120.6 N1 N2 HN2 120.6 HN3a N3 HN3b 106(5) N4 N3 HN3a 112(4) N4 N3 HN3b 106(4) C2 N4 HN4 120.3 N3 N4 HN4 120.3 N11 C12 H12 118.8 C13 C12 H12 118.8 C14 C13 H13 120.3 C12 C13 H13 120.3 C13 C14 H14 120.6 C15 C14 H14 120.6 C16 C15 H15 120.6 C14 C15 H15 120.6 H17a C17 H17b 109.5 N51 C17 H17a 109.5 C16 C17 H17a 109.5 N51 C17 H17b 109.5 C16 C17 H17b 109.5 N21 C22 H22 118.5 C23 C22 H22 118.5 C22 C23 H23 120.7 C24 C23 H23 120.7 C25 C24 H24 120.5 C23 C24 H24 120.5 C24 C25 H25 120.3 C26 C25 H25 120.3 H27a C27 H27b 109.5 N51 C27 H27a 108.9 C26 C27 H27a 108.9 N51 C27 H27b 108.9 C26 C27 H27b 108.9 N31 C32 H32 118.9 C33 C32 H32 118.9 C34 C33 H33 120.7 C32 C33 H33 120.7 C33 C34 H34 120.1 C35 C34 H34 120.1 C34 C35 H35 120.6 C36 C35 H35 120.6 H37a C37 H37b 109.5 N61 C37 H37a 109.4 C36 C37 H37a 109.4 N61 C37 H37b 109.4 C36 C37 H37b 109.4 N41 C42 H42 118.6 C43 C42 H42 118.6 C44 C43 H43 120.7 C42 C43 H43 120.7 C43 C44 H44 120.4 C45 C44 H44 120.4 C44 C45 H45 120.5 C46 C45 H45 120.5 H47a C47 H47b 109.5 N61 C47 H47a 108.6 C46 C47 H47a 108.6 N61 C47 H47b 108.6 C46 C47 H47b 108.6 H52a C52 H52b 109.5 N51 C52 H52a 109.2 C53 C52 H52a 109.2 N51 C52 H52b 109.2 C53 C52 H52b 109.2 C55 C54 H54 118.9 C53 C54 H54 118.9 H57a C57 H57b 109.4 H57a C57 H57c 109.4 C56 C57 H57a 109.6 H57b C57 H57c 109.5 C56 C57 H57b 109.4 C56 C57 H57c 109.4 H58a C58 H58b 108.8 H58a C58 H58c 108.8 C56 C58 H58a 112.1 H58b C58 H58c 109.5 C56 C58 H58b 108.8 C56 C58 H58c 108.8 H59a C59 H59b 109.6 H59a C59 H59c 109.6 C56 C59 H59a 109.1 H59b C59 H59c 109.5 C56 C59 H59b 109.6 C56 C59 H59c 109.6 H62a C62 H62b 109.5 N61 C62 H62a 109.0 C63 C62 H62a 109.0 N61 C62 H62b 109.0 C63 C62 H62b 109.0 C63 C64 H64 118.5 C55 C64 H64 118.5 #loop_ #_geom_bond_atom_site_label_D #_geom_bond_atom_site_label_H #_geom_contact_atom_site_label_A #_geom_bond_distance_DH #_geom_contact_distance_HA #_geom_contact_distance_DA #_geom_angle_DHA #_geom_contact_site_symmetry_A #N1 HN1a O4 0.99(5) 2.01(5) 2.957(6) 158(4) . #N3 HN3a O3 0.84(5) 2.24(5) 2.989(6) 149(5) . #N1 HN1b O14 0.87(4) 2.20(4) 3.021(6) 157(4) . #N3 HN3b O2 0.92(6) 1.98(6) 2.882(6) 168(5) 2_666