# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_4comethnbz _database_code_depnum_ccdc_archive 'CCDC 791260' #TrackingRef 'cif_791260-791267_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 791260' _audit_creation_method SHELXL-97 _chemical_name_systematic ; carbonatobis(1,10-phenanthroline)cobalt(III) 3-methyl-4-nitrobenzoate.pentahydrate ; _chemical_name_common ; carbonatobis(1,10-phenanthroline)cobalt(iii) 3-methyl-4- nitrobenzoate.pentahydrate ; _chemical_melting_point 'not measured' _chemical_formula_moiety 'C33 H32 Co N5 O12' _chemical_formula_sum 'C33 H32 Co N5 O12' _chemical_formula_weight 749.57 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.395(2) _cell_length_b 12.820(3) _cell_length_c 13.611(3) _cell_angle_alpha 78.43(3) _cell_angle_beta 76.51(3) _cell_angle_gamma 74.00(3) _cell_volume 1677.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 29.90 _exptl_crystal_description block _exptl_crystal_colour 'reddish pink' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.633 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEXII' _diffrn_measurement_method 'combination of \w and \f' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25349 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6588 _reflns_number_gt 5948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 (Bruker, 2007)' _computing_data_reduction 'APEX2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _computing_publication_material SHELXL-97 _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^)+(0.0543P)^2^+0.5329P] 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 6588 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.171542(19) 0.531318(16) 0.203516(15) 0.02880(8) Uani 1 1 d . . . O1 O 0.11969(11) 0.58030(10) 0.07514(8) 0.0374(3) Uani 1 1 d . . . O2 O -0.00423(11) 0.62652(9) 0.21685(8) 0.0360(2) Uani 1 1 d . . . O3 O -0.08655(13) 0.69481(12) 0.07166(11) 0.0531(3) Uani 1 1 d . . . O4 O 0.24362(17) 0.02107(14) 0.33379(13) 0.0688(4) Uani 1 1 d . . . O5 O 0.18542(16) -0.03542(13) 0.49925(13) 0.0658(4) Uani 1 1 d . . . O6 O 0.6261(3) 0.3255(3) 0.4402(3) 0.1477(13) Uani 1 1 d . . . O7 O 0.5619(4) 0.2922(3) 0.5969(2) 0.1494(12) Uani 1 1 d . . . O8 O -0.00012(16) -0.03521(12) 0.33037(11) 0.0594(4) Uani 1 1 d . . . H8B H 0.0705 -0.0207 0.3401 0.071 Uiso 1 1 d R . . H8C H -0.0530 -0.0143 0.3843 0.071 Uiso 1 1 d R . . O9 O 0.3643(3) 0.09920(18) 0.14258(16) 0.1128(8) Uani 1 1 d . . . H9B H 0.3049 0.0846 0.1906 0.135 Uiso 1 1 d R . . H9C H 0.3156 0.1048 0.0950 0.135 Uiso 1 1 d R . . O10 O -0.0773(3) 0.0577(2) 0.14620(18) 0.1232(9) Uani 1 1 d . . . H10B H -0.0604 0.0288 0.2051 0.148 Uiso 1 1 d R . . H10C H -0.1250 0.0211 0.1310 0.148 Uiso 1 1 d R . . O11 O -0.1675(4) 0.8968(3) -0.0278(3) 0.0856(18) Uani 0.571(8) 1 d P . . O11A O 0.1203(7) 0.0751(4) -0.0251(6) 0.102(3) Uani 0.429(8) 1 d P . . O12 O 0.6662(5) 0.0369(4) 0.1044(3) 0.118(2) Uani 0.562(6) 1 d P . . O12A O 0.6004(7) 0.9899(6) 0.0386(5) 0.124(3) Uani 0.438(6) 1 d P . . N1 N 0.08994(13) 0.40848(11) 0.22680(10) 0.0324(3) Uani 1 1 d . . . N2 N 0.18621(12) 0.48865(10) 0.34747(10) 0.0298(3) Uani 1 1 d . . . N3 N 0.35694(13) 0.44812(11) 0.16062(10) 0.0325(3) Uani 1 1 d . . . N4 N 0.25451(13) 0.65270(11) 0.18513(10) 0.0323(3) Uani 1 1 d . . . N5 N 0.5615(2) 0.28041(19) 0.5129(2) 0.0803(7) Uani 1 1 d . . . C1 C 0.00221(16) 0.63854(14) 0.11778(13) 0.0368(3) Uani 1 1 d . . . C2 C 0.04556(18) 0.36940(14) 0.16120(14) 0.0416(4) Uani 1 1 d . . . H2A H 0.0611 0.3983 0.0924 0.050 Uiso 1 1 calc R . . C3 C -0.0239(2) 0.28596(16) 0.19297(16) 0.0500(4) Uani 1 1 d . . . H3A H -0.0529 0.2594 0.1453 0.060 Uiso 1 1 calc R . . C4 C -0.04948(19) 0.24320(14) 0.29379(16) 0.0470(4) Uani 1 1 d . . . H4A H -0.0985 0.1894 0.3152 0.056 Uiso 1 1 calc R . . C5 C -0.00123(16) 0.28109(13) 0.36499(14) 0.0375(4) Uani 1 1 d . . . C6 C 0.06835(14) 0.36419(12) 0.32688(12) 0.0310(3) Uani 1 1 d . . . C7 C 0.12305(14) 0.40615(12) 0.39218(12) 0.0293(3) Uani 1 1 d . . . C8 C 0.11180(15) 0.36273(13) 0.49567(12) 0.0340(3) Uani 1 1 d . . . C9 C 0.03942(17) 0.27799(14) 0.53331(14) 0.0416(4) Uani 1 1 d . . . H9A H 0.0304 0.2485 0.6021 0.050 Uiso 1 1 calc R . . C10 C -0.01582(17) 0.23999(14) 0.47169(15) 0.0436(4) Uani 1 1 d . . . H10A H -0.0641 0.1863 0.4989 0.052 Uiso 1 1 calc R . . C11 C 0.17363(17) 0.40596(14) 0.55454(12) 0.0388(4) Uani 1 1 d . . . H11A H 0.1700 0.3795 0.6237 0.047 Uiso 1 1 calc R . . C12 C 0.23916(17) 0.48736(14) 0.50902(13) 0.0402(4) Uani 1 1 d . . . H12A H 0.2814 0.5158 0.5471 0.048 Uiso 1 1 calc R . . C13 C 0.24275(16) 0.52771(13) 0.40560(13) 0.0357(3) Uani 1 1 d . . . H13A H 0.2863 0.5840 0.3763 0.043 Uiso 1 1 calc R . . C14 C 0.40385(18) 0.34445(14) 0.14450(13) 0.0409(4) Uani 1 1 d . . . H14A H 0.3425 0.3010 0.1533 0.049 Uiso 1 1 calc R . . C15 C 0.5434(2) 0.29866(16) 0.11460(14) 0.0487(4) Uani 1 1 d . . . H15A H 0.5734 0.2259 0.1035 0.058 Uiso 1 1 calc R . . C16 C 0.63478(19) 0.36055(17) 0.10178(14) 0.0503(5) Uani 1 1 d . . . H16A H 0.7275 0.3300 0.0830 0.060 Uiso 1 1 calc R . . C17 C 0.58864(17) 0.47114(16) 0.11707(13) 0.0424(4) Uani 1 1 d . . . C18 C 0.44821(16) 0.51047(14) 0.14607(11) 0.0336(3) Uani 1 1 d . . . C19 C 0.39225(16) 0.62223(13) 0.15847(11) 0.0328(3) Uani 1 1 d . . . C20 C 0.47546(18) 0.69540(16) 0.14038(12) 0.0413(4) Uani 1 1 d . . . C21 C 0.6190(2) 0.65264(19) 0.11443(15) 0.0533(5) Uani 1 1 d . . . H21A H 0.6769 0.6992 0.1046 0.064 Uiso 1 1 calc R . . C22 C 0.67251(18) 0.5465(2) 0.10379(15) 0.0544(5) Uani 1 1 d . . . H22A H 0.7667 0.5213 0.0873 0.065 Uiso 1 1 calc R . . C23 C 0.4104(2) 0.80582(16) 0.14811(14) 0.0495(5) Uani 1 1 d . . . H23A H 0.4614 0.8580 0.1354 0.059 Uiso 1 1 calc R . . C24 C 0.2719(2) 0.83598(16) 0.17444(15) 0.0496(4) Uani 1 1 d . . . H24A H 0.2281 0.9090 0.1799 0.060 Uiso 1 1 calc R . . C25 C 0.19573(19) 0.75761(14) 0.19323(14) 0.0417(4) Uani 1 1 d . . . H25A H 0.1014 0.7792 0.2119 0.050 Uiso 1 1 calc R . . C26 C 0.33341(17) 0.08515(14) 0.44851(15) 0.0430(4) Uani 1 1 d . . . C27 C 0.33472(19) 0.09045(16) 0.54810(16) 0.0479(4) Uani 1 1 d . . . H27A H 0.2844 0.0503 0.5998 0.057 Uiso 1 1 calc R . . C28 C 0.4076(2) 0.15283(17) 0.57549(17) 0.0534(5) Uani 1 1 d . . . C29 C 0.4817(2) 0.20958(17) 0.49528(19) 0.0559(5) Uani 1 1 d . . . C30 C 0.4837(2) 0.20572(19) 0.39494(19) 0.0639(6) Uani 1 1 d . . . H30A H 0.5351 0.2448 0.3431 0.077 Uiso 1 1 calc R . . C31 C 0.4090(2) 0.14343(18) 0.37142(17) 0.0572(5) Uani 1 1 d . . . H31A H 0.4096 0.1408 0.3035 0.069 Uiso 1 1 calc R . . C32 C 0.24710(19) 0.01754(16) 0.42577(17) 0.0487(4) Uani 1 1 d . . . C33 C 0.4008(3) 0.1516(3) 0.6865(2) 0.0883(9) Uani 1 1 d . . . H33A H 0.4894 0.1186 0.7030 0.133 Uiso 1 1 calc R . . H33B H 0.3374 0.1100 0.7261 0.133 Uiso 1 1 calc R . . H33C H 0.3712 0.2254 0.7017 0.133 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02798(12) 0.02825(12) 0.03076(12) -0.00267(8) -0.00301(8) -0.01099(8) O1 0.0374(6) 0.0425(6) 0.0314(5) -0.0025(5) -0.0036(4) -0.0125(5) O2 0.0292(5) 0.0378(6) 0.0378(6) -0.0039(5) -0.0004(4) -0.0092(4) O3 0.0413(7) 0.0573(8) 0.0587(8) 0.0083(6) -0.0205(6) -0.0115(6) O4 0.0751(10) 0.0788(11) 0.0704(10) -0.0222(8) -0.0162(8) -0.0379(9) O5 0.0628(9) 0.0648(10) 0.0788(11) -0.0160(8) -0.0021(8) -0.0358(8) O6 0.168(3) 0.166(3) 0.163(3) -0.043(2) -0.012(2) -0.133(2) O7 0.224(3) 0.159(3) 0.137(2) -0.0239(19) -0.080(2) -0.122(3) O8 0.0663(9) 0.0593(9) 0.0602(9) -0.0048(7) -0.0115(7) -0.0303(7) O9 0.182(3) 0.1025(16) 0.0800(14) -0.0099(12) -0.0214(14) -0.0824(17) O10 0.182(3) 0.129(2) 0.0905(16) 0.0045(14) -0.0487(16) -0.085(2) O11 0.105(3) 0.062(2) 0.077(2) 0.0006(17) -0.026(2) 0.0006(18) O11A 0.137(5) 0.060(3) 0.113(5) -0.012(3) -0.030(4) -0.027(3) O12 0.151(4) 0.094(3) 0.104(3) -0.031(2) -0.026(3) -0.006(3) O12A 0.147(6) 0.141(5) 0.097(4) 0.000(4) -0.020(4) -0.069(4) N1 0.0317(6) 0.0304(7) 0.0366(7) -0.0052(5) -0.0059(5) -0.0103(5) N2 0.0284(6) 0.0270(6) 0.0342(6) -0.0038(5) -0.0036(5) -0.0095(5) N3 0.0322(6) 0.0327(7) 0.0323(6) -0.0032(5) -0.0049(5) -0.0094(5) N4 0.0335(6) 0.0320(7) 0.0318(6) -0.0019(5) -0.0028(5) -0.0132(5) N5 0.0755(14) 0.0655(13) 0.123(2) -0.0266(13) -0.0378(14) -0.0285(11) C1 0.0331(8) 0.0365(8) 0.0422(9) 0.0010(7) -0.0061(7) -0.0165(7) C2 0.0454(9) 0.0404(9) 0.0454(9) -0.0090(7) -0.0137(7) -0.0145(7) C3 0.0526(11) 0.0417(10) 0.0667(12) -0.0139(9) -0.0218(9) -0.0163(8) C4 0.0432(9) 0.0307(9) 0.0725(13) -0.0057(8) -0.0134(9) -0.0167(7) C5 0.0311(8) 0.0257(8) 0.0542(10) -0.0027(7) -0.0056(7) -0.0086(6) C6 0.0265(7) 0.0253(7) 0.0393(8) -0.0042(6) -0.0033(6) -0.0062(6) C7 0.0250(7) 0.0244(7) 0.0363(8) -0.0038(6) -0.0027(6) -0.0051(5) C8 0.0301(7) 0.0286(8) 0.0369(8) -0.0014(6) -0.0017(6) -0.0029(6) C9 0.0390(9) 0.0347(9) 0.0415(9) 0.0055(7) 0.0013(7) -0.0087(7) C10 0.0381(9) 0.0299(8) 0.0566(11) 0.0048(7) -0.0012(8) -0.0127(7) C11 0.0380(8) 0.0405(9) 0.0324(8) -0.0038(6) -0.0050(6) -0.0032(7) C12 0.0408(9) 0.0428(9) 0.0400(9) -0.0107(7) -0.0110(7) -0.0087(7) C13 0.0350(8) 0.0342(8) 0.0410(8) -0.0069(6) -0.0067(6) -0.0127(6) C14 0.0428(9) 0.0362(9) 0.0413(9) -0.0057(7) -0.0058(7) -0.0078(7) C15 0.0495(10) 0.0423(10) 0.0455(10) -0.0085(8) -0.0052(8) 0.0018(8) C16 0.0352(9) 0.0626(12) 0.0436(10) -0.0103(9) -0.0022(7) 0.0011(8) C17 0.0321(8) 0.0598(11) 0.0342(8) -0.0078(7) -0.0034(6) -0.0112(8) C18 0.0316(7) 0.0435(9) 0.0267(7) -0.0048(6) -0.0034(6) -0.0125(7) C19 0.0343(8) 0.0417(9) 0.0253(7) -0.0029(6) -0.0031(6) -0.0174(7) C20 0.0442(9) 0.0544(11) 0.0335(8) -0.0058(7) -0.0038(7) -0.0283(8) C21 0.0430(10) 0.0782(15) 0.0498(11) -0.0142(10) 0.0005(8) -0.0368(10) C22 0.0310(9) 0.0854(16) 0.0503(11) -0.0156(10) 0.0012(8) -0.0228(9) C23 0.0649(12) 0.0490(11) 0.0457(10) -0.0047(8) -0.0068(9) -0.0365(9) C24 0.0628(12) 0.0355(9) 0.0540(11) -0.0060(8) -0.0067(9) -0.0214(8) C25 0.0447(9) 0.0324(8) 0.0474(9) -0.0056(7) -0.0040(7) -0.0122(7) C26 0.0359(8) 0.0357(9) 0.0598(11) -0.0114(8) -0.0123(8) -0.0067(7) C27 0.0385(9) 0.0467(10) 0.0598(11) -0.0107(8) -0.0118(8) -0.0085(8) C28 0.0468(10) 0.0518(11) 0.0672(13) -0.0203(10) -0.0219(9) -0.0032(9) C29 0.0476(10) 0.0435(10) 0.0880(15) -0.0169(10) -0.0264(10) -0.0130(9) C30 0.0686(14) 0.0599(13) 0.0748(15) -0.0054(11) -0.0163(11) -0.0351(11) C31 0.0660(13) 0.0590(13) 0.0567(12) -0.0077(10) -0.0155(10) -0.0287(10) C32 0.0401(9) 0.0417(10) 0.0684(13) -0.0191(9) -0.0114(9) -0.0078(8) C33 0.096(2) 0.111(2) 0.0752(17) -0.0318(16) -0.0309(15) -0.0271(17) _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 1.8844(12) . ? Co1 O2 1.8884(13) . ? Co1 N1 1.9263(14) . ? Co1 N4 1.9264(14) . ? Co1 N3 1.9453(15) . ? Co1 N2 1.9558(14) . ? Co1 C1 2.3089(19) . ? O1 C1 1.314(2) . ? O2 C1 1.314(2) . ? O3 C1 1.220(2) . ? O4 C32 1.252(3) . ? O5 C32 1.241(3) . ? O6 N5 1.199(4) . ? O7 N5 1.183(3) . ? O8 H8B 0.8500 . ? O8 H8C 0.8499 . ? O9 H9B 0.8191 . ? O9 H9C 0.8916 . ? O10 H10B 0.8500 . ? O10 H10C 0.8500 . ? O11 O11A 1.121(6) 2_565 ? O11A O11 1.121(6) 2_565 ? O12 O12A 1.537(7) 1_545 ? O12A O12 1.537(7) 1_565 ? N1 C2 1.327(2) . ? N1 C6 1.359(2) . ? N2 C13 1.327(2) . ? N2 C7 1.3631(19) . ? N3 C14 1.327(2) . ? N3 C18 1.358(2) . ? N4 C25 1.330(2) . ? N4 C19 1.357(2) . ? N5 C29 1.471(3) . ? C2 C3 1.395(3) . ? C2 H2A 0.9300 . ? C3 C4 1.365(3) . ? C3 H3A 0.9300 . ? C4 C5 1.406(3) . ? C4 H4A 0.9300 . ? C5 C6 1.398(2) . ? C5 C10 1.430(3) . ? C6 C7 1.414(2) . ? C7 C8 1.397(2) . ? C8 C11 1.406(2) . ? C8 C9 1.434(2) . ? C9 C10 1.347(3) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.368(3) . ? C11 H11A 0.9300 . ? C12 C13 1.395(2) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.402(3) . ? C14 H14A 0.9300 . ? C15 C16 1.358(3) . ? C15 H15A 0.9300 . ? C16 C17 1.407(3) . ? C16 H16A 0.9300 . ? C17 C18 1.395(2) . ? C17 C22 1.430(3) . ? C18 C19 1.418(2) . ? C19 C20 1.394(2) . ? C20 C23 1.404(3) . ? C20 C21 1.426(3) . ? C21 C22 1.344(3) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.364(3) . ? C23 H23A 0.9300 . ? C24 C25 1.394(3) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.374(3) . ? C26 C31 1.379(3) . ? C26 C32 1.522(2) . ? C27 C28 1.392(3) . ? C27 H27A 0.9300 . ? C28 C29 1.383(3) . ? C28 C33 1.493(3) . ? C29 C30 1.372(3) . ? C30 C31 1.380(3) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 O2 69.37(6) . . ? O1 Co1 N1 91.59(6) . . ? O2 Co1 N1 89.33(6) . . ? O1 Co1 N4 90.46(6) . . ? O2 Co1 N4 91.21(6) . . ? N1 Co1 N4 177.94(5) . . ? O1 Co1 N3 99.55(6) . . ? O2 Co1 N3 168.12(5) . . ? N1 Co1 N3 95.40(6) . . ? N4 Co1 N3 84.44(6) . . ? O1 Co1 N2 168.53(5) . . ? O2 Co1 N2 99.87(6) . . ? N1 Co1 N2 84.14(6) . . ? N4 Co1 N2 93.81(6) . . ? N3 Co1 N2 91.46(6) . . ? O1 Co1 C1 34.68(6) . . ? O2 Co1 C1 34.69(6) . . ? N1 Co1 C1 90.54(6) . . ? N4 Co1 C1 91.04(6) . . ? N3 Co1 C1 134.10(6) . . ? N2 Co1 C1 134.44(6) . . ? C1 O1 Co1 90.63(10) . . ? C1 O2 Co1 90.44(10) . . ? H8B O8 H8C 96.9 . . ? H9B O9 H9C 94.7 . . ? H10B O10 H10C 107.1 . . ? C2 N1 C6 118.51(14) . . ? C2 N1 Co1 128.98(12) . . ? C6 N1 Co1 112.32(10) . . ? C13 N2 C7 117.69(14) . . ? C13 N2 Co1 131.08(11) . . ? C7 N2 Co1 111.22(10) . . ? C14 N3 C18 118.11(14) . . ? C14 N3 Co1 130.40(12) . . ? C18 N3 Co1 111.49(11) . . ? C25 N4 C19 118.53(14) . . ? C25 N4 Co1 129.23(12) . . ? C19 N4 Co1 112.23(11) . . ? O7 N5 O6 121.0(2) . . ? O7 N5 C29 120.6(3) . . ? O6 N5 C29 118.4(3) . . ? O3 C1 O1 124.70(16) . . ? O3 C1 O2 125.73(16) . . ? O1 C1 O2 109.56(14) . . ? O3 C1 Co1 179.40(16) . . ? O1 C1 Co1 54.69(8) . . ? O2 C1 Co1 54.87(8) . . ? N1 C2 C3 121.63(17) . . ? N1 C2 H2A 119.2 . . ? C3 C2 H2A 119.2 . . ? C4 C3 C2 120.25(17) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 119.55(16) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C6 C5 C4 116.63(16) . . ? C6 C5 C10 118.22(16) . . ? C4 C5 C10 125.14(16) . . ? N1 C6 C5 123.40(15) . . ? N1 C6 C7 115.79(13) . . ? C5 C6 C7 120.81(15) . . ? N2 C7 C8 123.77(14) . . ? N2 C7 C6 115.92(14) . . ? C8 C7 C6 120.31(14) . . ? C7 C8 C11 116.77(15) . . ? C7 C8 C9 117.97(16) . . ? C11 C8 C9 125.26(15) . . ? C10 C9 C8 121.74(16) . . ? C10 C9 H9A 119.1 . . ? C8 C9 H9A 119.1 . . ? C9 C10 C5 120.90(15) . . ? C9 C10 H10A 119.6 . . ? C5 C10 H10A 119.6 . . ? C12 C11 C8 119.31(15) . . ? C12 C11 H11A 120.3 . . ? C8 C11 H11A 120.3 . . ? C11 C12 C13 120.11(16) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? N2 C13 C12 122.32(15) . . ? N2 C13 H13A 118.8 . . ? C12 C13 H13A 118.8 . . ? N3 C14 C15 121.79(17) . . ? N3 C14 H14A 119.1 . . ? C15 C14 H14A 119.1 . . ? C16 C15 C14 120.04(18) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 119.75(17) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 116.57(17) . . ? C18 C17 C22 117.61(18) . . ? C16 C17 C22 125.81(17) . . ? N3 C18 C17 123.72(16) . . ? N3 C18 C19 115.87(14) . . ? C17 C18 C19 120.37(15) . . ? N4 C19 C20 123.13(16) . . ? N4 C19 C18 115.81(14) . . ? C20 C19 C18 121.02(15) . . ? C19 C20 C23 117.02(16) . . ? C19 C20 C21 117.64(17) . . ? C23 C20 C21 125.33(17) . . ? C22 C21 C20 121.43(17) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C17 121.82(17) . . ? C21 C22 H22A 119.1 . . ? C17 C22 H22A 119.1 . . ? C24 C23 C20 119.52(16) . . ? C24 C23 H23A 120.2 . . ? C20 C23 H23A 120.2 . . ? C23 C24 C25 120.09(18) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? N4 C25 C24 121.69(17) . . ? N4 C25 H25A 119.2 . . ? C24 C25 H25A 119.2 . . ? C27 C26 C31 118.68(17) . . ? C27 C26 C32 119.66(18) . . ? C31 C26 C32 121.64(18) . . ? C26 C27 C28 123.3(2) . . ? C26 C27 H27A 118.3 . . ? C28 C27 H27A 118.3 . . ? C29 C28 C27 115.67(19) . . ? C29 C28 C33 126.2(2) . . ? C27 C28 C33 118.2(2) . . ? C30 C29 C28 122.69(18) . . ? C30 C29 N5 115.7(2) . . ? C28 C29 N5 121.6(2) . . ? C29 C30 C31 119.6(2) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C26 C31 C30 120.0(2) . . ? C26 C31 H31A 120.0 . . ? C30 C31 H31A 120.0 . . ? O5 C32 O4 125.49(18) . . ? O5 C32 C26 117.77(19) . . ? O4 C32 C26 116.74(19) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 O1 C1 -0.04(8) . . . . ? N1 Co1 O1 C1 88.65(10) . . . . ? N4 Co1 O1 C1 -91.16(10) . . . . ? N3 Co1 O1 C1 -175.60(9) . . . . ? N2 Co1 O1 C1 20.8(3) . . . . ? O1 Co1 O2 C1 0.04(8) . . . . ? N1 Co1 O2 C1 -91.91(10) . . . . ? N4 Co1 O2 C1 90.07(10) . . . . ? N3 Co1 O2 C1 21.8(3) . . . . ? N2 Co1 O2 C1 -175.85(9) . . . . ? O1 Co1 N1 C2 12.62(15) . . . . ? O2 Co1 N1 C2 81.95(15) . . . . ? N4 Co1 N1 C2 -172.7(14) . . . . ? N3 Co1 N1 C2 -87.14(15) . . . . ? N2 Co1 N1 C2 -178.05(15) . . . . ? C1 Co1 N1 C2 47.29(15) . . . . ? O1 Co1 N1 C6 -162.09(11) . . . . ? O2 Co1 N1 C6 -92.75(11) . . . . ? N4 Co1 N1 C6 12.6(15) . . . . ? N3 Co1 N1 C6 98.16(11) . . . . ? N2 Co1 N1 C6 7.24(10) . . . . ? C1 Co1 N1 C6 -127.42(11) . . . . ? O1 Co1 N2 C13 -115.7(3) . . . . ? O2 Co1 N2 C13 -95.92(14) . . . . ? N1 Co1 N2 C13 175.79(14) . . . . ? N4 Co1 N2 C13 -4.02(14) . . . . ? N3 Co1 N2 C13 80.51(14) . . . . ? C1 Co1 N2 C13 -99.23(15) . . . . ? O1 Co1 N2 C7 62.6(3) . . . . ? O2 Co1 N2 C7 82.37(10) . . . . ? N1 Co1 N2 C7 -5.93(10) . . . . ? N4 Co1 N2 C7 174.27(10) . . . . ? N3 Co1 N2 C7 -101.21(10) . . . . ? C1 Co1 N2 C7 79.06(12) . . . . ? O1 Co1 N3 C14 -86.83(15) . . . . ? O2 Co1 N3 C14 -107.4(3) . . . . ? N1 Co1 N3 C14 5.70(15) . . . . ? N4 Co1 N3 C14 -176.37(15) . . . . ? N2 Co1 N3 C14 89.94(15) . . . . ? C1 Co1 N3 C14 -90.32(16) . . . . ? O1 Co1 N3 C18 93.15(11) . . . . ? O2 Co1 N3 C18 72.6(3) . . . . ? N1 Co1 N3 C18 -174.32(10) . . . . ? N4 Co1 N3 C18 3.62(10) . . . . ? N2 Co1 N3 C18 -90.07(11) . . . . ? C1 Co1 N3 C18 89.66(12) . . . . ? O1 Co1 N4 C25 76.10(15) . . . . ? O2 Co1 N4 C25 6.73(15) . . . . ? N1 Co1 N4 C25 -98.6(15) . . . . ? N3 Co1 N4 C25 175.65(15) . . . . ? N2 Co1 N4 C25 -93.25(15) . . . . ? C1 Co1 N4 C25 41.42(15) . . . . ? O1 Co1 N4 C19 -102.60(11) . . . . ? O2 Co1 N4 C19 -171.97(10) . . . . ? N1 Co1 N4 C19 82.7(15) . . . . ? N3 Co1 N4 C19 -3.04(10) . . . . ? N2 Co1 N4 C19 88.06(11) . . . . ? C1 Co1 N4 C19 -137.27(11) . . . . ? Co1 O1 C1 O3 -179.92(16) . . . . ? Co1 O1 C1 O2 0.05(12) . . . . ? Co1 O2 C1 O3 179.92(16) . . . . ? Co1 O2 C1 O1 -0.05(12) . . . . ? O1 Co1 C1 O3 6(13) . . . . ? O2 Co1 C1 O3 -174(100) . . . . ? N1 Co1 C1 O3 -86(13) . . . . ? N4 Co1 C1 O3 95(13) . . . . ? N3 Co1 C1 O3 12(13) . . . . ? N2 Co1 C1 O3 -168(100) . . . . ? O2 Co1 C1 O1 179.94(14) . . . . ? N1 Co1 C1 O1 -92.01(10) . . . . ? N4 Co1 C1 O1 89.31(9) . . . . ? N3 Co1 C1 O1 6.05(12) . . . . ? N2 Co1 C1 O1 -174.32(8) . . . . ? O1 Co1 C1 O2 -179.94(14) . . . . ? N1 Co1 C1 O2 88.05(9) . . . . ? N4 Co1 C1 O2 -90.63(9) . . . . ? N3 Co1 C1 O2 -173.89(8) . . . . ? N2 Co1 C1 O2 5.74(12) . . . . ? C6 N1 C2 C3 1.0(2) . . . . ? Co1 N1 C2 C3 -173.39(13) . . . . ? N1 C2 C3 C4 0.8(3) . . . . ? C2 C3 C4 C5 -2.2(3) . . . . ? C3 C4 C5 C6 1.7(2) . . . . ? C3 C4 C5 C10 -177.15(17) . . . . ? C2 N1 C6 C5 -1.6(2) . . . . ? Co1 N1 C6 C5 173.75(12) . . . . ? C2 N1 C6 C7 177.44(14) . . . . ? Co1 N1 C6 C7 -7.24(16) . . . . ? C4 C5 C6 N1 0.2(2) . . . . ? C10 C5 C6 N1 179.12(14) . . . . ? C4 C5 C6 C7 -178.74(14) . . . . ? C10 C5 C6 C7 0.2(2) . . . . ? C13 N2 C7 C8 1.6(2) . . . . ? Co1 N2 C7 C8 -176.90(11) . . . . ? C13 N2 C7 C6 -177.84(13) . . . . ? Co1 N2 C7 C6 3.62(16) . . . . ? N1 C6 C7 N2 2.37(19) . . . . ? C5 C6 C7 N2 -178.60(13) . . . . ? N1 C6 C7 C8 -177.14(13) . . . . ? C5 C6 C7 C8 1.9(2) . . . . ? N2 C7 C8 C11 -1.9(2) . . . . ? C6 C7 C8 C11 177.51(14) . . . . ? N2 C7 C8 C9 178.35(14) . . . . ? C6 C7 C8 C9 -2.2(2) . . . . ? C7 C8 C9 C10 0.4(2) . . . . ? C11 C8 C9 C10 -179.24(16) . . . . ? C8 C9 C10 C5 1.6(3) . . . . ? C6 C5 C10 C9 -1.9(2) . . . . ? C4 C5 C10 C9 176.87(17) . . . . ? C7 C8 C11 C12 0.7(2) . . . . ? C9 C8 C11 C12 -179.68(15) . . . . ? C8 C11 C12 C13 0.8(2) . . . . ? C7 N2 C13 C12 0.0(2) . . . . ? Co1 N2 C13 C12 178.17(12) . . . . ? C11 C12 C13 N2 -1.2(3) . . . . ? C18 N3 C14 C15 0.8(2) . . . . ? Co1 N3 C14 C15 -179.18(13) . . . . ? N3 C14 C15 C16 0.3(3) . . . . ? C14 C15 C16 C17 -1.0(3) . . . . ? C15 C16 C17 C18 0.6(3) . . . . ? C15 C16 C17 C22 -178.28(18) . . . . ? C14 N3 C18 C17 -1.3(2) . . . . ? Co1 N3 C18 C17 178.72(12) . . . . ? C14 N3 C18 C19 176.44(14) . . . . ? Co1 N3 C18 C19 -3.55(17) . . . . ? C16 C17 C18 N3 0.6(2) . . . . ? C22 C17 C18 N3 179.54(16) . . . . ? C16 C17 C18 C19 -177.04(15) . . . . ? C22 C17 C18 C19 1.9(2) . . . . ? C25 N4 C19 C20 0.9(2) . . . . ? Co1 N4 C19 C20 179.70(12) . . . . ? C25 N4 C19 C18 -176.92(14) . . . . ? Co1 N4 C19 C18 1.92(16) . . . . ? N3 C18 C19 N4 1.1(2) . . . . ? C17 C18 C19 N4 178.94(14) . . . . ? N3 C18 C19 C20 -176.70(14) . . . . ? C17 C18 C19 C20 1.1(2) . . . . ? N4 C19 C20 C23 -1.7(2) . . . . ? C18 C19 C20 C23 175.95(15) . . . . ? N4 C19 C20 C21 179.03(15) . . . . ? C18 C19 C20 C21 -3.3(2) . . . . ? C19 C20 C21 C22 2.5(3) . . . . ? C23 C20 C21 C22 -176.67(19) . . . . ? C20 C21 C22 C17 0.5(3) . . . . ? C18 C17 C22 C21 -2.7(3) . . . . ? C16 C17 C22 C21 176.10(19) . . . . ? C19 C20 C23 C24 1.3(3) . . . . ? C21 C20 C23 C24 -179.49(18) . . . . ? C20 C23 C24 C25 -0.2(3) . . . . ? C19 N4 C25 C24 0.4(3) . . . . ? Co1 N4 C25 C24 -178.21(13) . . . . ? C23 C24 C25 N4 -0.8(3) . . . . ? C31 C26 C27 C28 0.7(3) . . . . ? C32 C26 C27 C28 -178.06(17) . . . . ? C26 C27 C28 C29 -0.8(3) . . . . ? C26 C27 C28 C33 -179.9(2) . . . . ? C27 C28 C29 C30 0.3(3) . . . . ? C33 C28 C29 C30 179.4(2) . . . . ? C27 C28 C29 N5 178.85(19) . . . . ? C33 C28 C29 N5 -2.1(3) . . . . ? O7 N5 C29 C30 177.2(3) . . . . ? O6 N5 C29 C30 -3.0(4) . . . . ? O7 N5 C29 C28 -1.5(4) . . . . ? O6 N5 C29 C28 178.3(3) . . . . ? C28 C29 C30 C31 0.2(4) . . . . ? N5 C29 C30 C31 -178.4(2) . . . . ? C27 C26 C31 C30 -0.2(3) . . . . ? C32 C26 C31 C30 178.6(2) . . . . ? C29 C30 C31 C26 -0.3(4) . . . . ? C27 C26 C32 O5 -3.5(3) . . . . ? C31 C26 C32 O5 177.74(19) . . . . ? C27 C26 C32 O4 175.88(18) . . . . ? C31 C26 C32 O4 -2.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.352 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.052 data_3cocnbz _database_code_depnum_ccdc_archive 'CCDC 791261' #TrackingRef 'cif_791260-791267_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 791261' _audit_creation_method SHELXL-97 _chemical_name_systematic ; carbonatobis(1,10-phenanthroline)cobalt(III) 2-chloro-4-nitrobenzoate.pentahydrate ; _chemical_name_common ; carbonatobis(1,10-phenanthroline)cobalt(iii) 2-chloro-4- nitrobenzoate.pentahydrate ; _chemical_melting_point ? _chemical_formula_moiety C25N4H16O3Co,C7H3N1O4Cl,5(H20) _chemical_formula_sum 'C32 H29 Cl Co N5 O12' _chemical_formula_weight 769.98 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.317(2) _cell_length_b 12.688(3) _cell_length_c 13.277(3) _cell_angle_alpha 76.71(3) _cell_angle_beta 79.98(3) _cell_angle_gamma 88.97(3) _cell_volume 1665.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9347 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'reddish pink' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details '(SADABS; Bruker, 2007' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEXII' _diffrn_measurement_method 'combination of \w and \f' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27523 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6520 _reflns_number_gt 5791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 (Bruker, 2007)' _computing_data_reduction 'APEX2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _computing_publication_material SHELXL-97 _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^)+(0.0931P)^2^+0.6046P] 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 6520 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1298 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Co1 Co 0.69475(3) 0.22032(2) 0.51962(2) 0.03233(12) Uani 1 1 d . . . Cl1 Cl 1.00387(9) 0.74644(7) 0.99352(7) 0.0754(2) Uani 1 1 d . . . N1 N 0.59189(17) 0.23805(14) 0.41007(14) 0.0356(4) Uani 1 1 d . . . N2 N 0.71287(18) 0.37816(14) 0.47667(14) 0.0356(4) Uani 1 1 d . . . N3 N 0.80187(18) 0.20842(14) 0.62547(15) 0.0374(4) Uani 1 1 d . . . N4 N 0.85619(18) 0.18497(14) 0.43488(14) 0.0370(4) Uani 1 1 d . . . N5 N 0.9340(3) 0.5351(3) 0.7265(2) 0.0702(7) Uani 1 1 d . . . O1 O 0.53956(15) 0.21899(12) 0.61709(12) 0.0392(3) Uani 1 1 d . . . O2 O 0.63021(15) 0.07645(12) 0.57776(12) 0.0385(3) Uani 1 1 d . . . O3 O 0.44137(18) 0.05784(15) 0.69494(16) 0.0580(5) Uani 1 1 d . . . O4 O 1.2900(5) 0.5452(4) 1.0708(4) 0.188(3) Uani 1 1 d . . . O5 O 1.3142(3) 0.7122(3) 0.9790(2) 0.1074(10) Uani 1 1 d . . . O6 O 0.9566(3) 0.4567(3) 0.6888(3) 0.1093(10) Uani 1 1 d . . . O7 O 0.8518(3) 0.6021(3) 0.7021(2) 0.1005(9) Uani 1 1 d . . . O8 O 0.7383(3) 0.1004(2) 0.1585(2) 0.0947(8) Uani 1 1 d . . . H8B H 0.7060 0.1559 0.1225 0.114 Uiso 1 1 d R . . H8C H 0.6687 0.0633 0.1917 0.114 Uiso 1 1 d R . . O9 O 0.8666(3) -0.0259(2) 0.0285(3) 0.1039(9) Uani 1 1 d . . . H9B H 0.8316 -0.0175 -0.0236 0.125 Uiso 1 1 d R . . H9C H 0.8462 0.0208 0.0673 0.125 Uiso 1 1 d R . . O10 O 0.7028(4) -0.2041(3) 0.1687(3) 0.1354(13) Uani 1 1 d . . . H10B H 0.7426 -0.1532 0.1273 0.163 Uiso 1 1 d R . . H10C H 0.6879 -0.2346 0.1193 0.163 Uiso 1 1 d R . . O11 O 0.7265(5) -0.0890(7) -0.1274(4) 0.172(3) Uani 0.774(7) 1 d P . . O11A O 0.5261(13) 0.0299(16) -0.0974(11) 0.123(7) Uani 0.226(7) 1 d P . . O12 O 1.3862(7) 0.3292(8) 1.0174(5) 0.164(4) Uani 0.559(8) 1 d P . . O12A O 0.5402(8) 0.1878(13) 0.9158(7) 0.196(7) Uani 0.441(8) 1 d P . . C1 C 0.5303(2) 0.11283(18) 0.63536(18) 0.0394(5) Uani 1 1 d . . . C2 C 0.5373(2) 0.16280(18) 0.37551(19) 0.0425(5) Uani 1 1 d . . . H2A H 0.5522 0.0902 0.4031 0.051 Uiso 1 1 calc R . . C3 C 0.4583(2) 0.1895(2) 0.2992(2) 0.0486(6) Uani 1 1 d . . . H3A H 0.4230 0.1351 0.2749 0.058 Uiso 1 1 calc R . . C4 C 0.4324(2) 0.2947(2) 0.25976(19) 0.0479(6) Uani 1 1 d . . . H4A H 0.3782 0.3124 0.2095 0.058 Uiso 1 1 calc R . . C5 C 0.4877(2) 0.37690(19) 0.29532(17) 0.0406(5) Uani 1 1 d . . . C6 C 0.5683(2) 0.34332(17) 0.36956(16) 0.0344(4) Uani 1 1 d . . . C7 C 0.6324(2) 0.41972(16) 0.40733(16) 0.0339(4) Uani 1 1 d . . . C8 C 0.6129(2) 0.53054(17) 0.37238(17) 0.0391(5) Uani 1 1 d . . . C9 C 0.5284(3) 0.56321(19) 0.29767(19) 0.0475(5) Uani 1 1 d . . . H9A H 0.5137 0.6366 0.2740 0.057 Uiso 1 1 calc R . . C10 C 0.4689(2) 0.4902(2) 0.2602(2) 0.0483(5) Uani 1 1 d . . . H10A H 0.4148 0.5142 0.2108 0.058 Uiso 1 1 calc R . . C11 C 0.6813(3) 0.60080(18) 0.41277(19) 0.0455(5) Uani 1 1 d . . . H11A H 0.6723 0.6753 0.3920 0.055 Uiso 1 1 calc R . . C12 C 0.7611(3) 0.55918(19) 0.4826(2) 0.0488(6) Uani 1 1 d . . . H12A H 0.8064 0.6055 0.5100 0.059 Uiso 1 1 calc R . . C13 C 0.7756(2) 0.44753(18) 0.51347(19) 0.0436(5) Uani 1 1 d . . . H13A H 0.8310 0.4209 0.5613 0.052 Uiso 1 1 calc R . . C14 C 0.7686(3) 0.2204(2) 0.7233(2) 0.0497(6) Uani 1 1 d . . . H14A H 0.6833 0.2404 0.7461 0.060 Uiso 1 1 calc R . . C15 C 0.8565(3) 0.2042(3) 0.7916(2) 0.0630(7) Uani 1 1 d . . . H15A H 0.8298 0.2130 0.8598 0.076 Uiso 1 1 calc R . . C17 C 1.0211(2) 0.16198(19) 0.6588(2) 0.0484(6) Uani 1 1 d . . . C16 C 0.9816(3) 0.1756(3) 0.7613(2) 0.0617(7) Uani 1 1 d . . . H16A H 1.0407 0.1650 0.8080 0.074 Uiso 1 1 calc R . . C18 C 0.9266(2) 0.17953(16) 0.59391(18) 0.0375(5) Uani 1 1 d . . . C19 C 0.9556(2) 0.16506(16) 0.49046(18) 0.0375(5) Uani 1 1 d . . . C20 C 1.0786(2) 0.12813(18) 0.4525(2) 0.0462(5) Uani 1 1 d . . . C21 C 1.1738(2) 0.1107(2) 0.5200(2) 0.0557(7) Uani 1 1 d . . . H21A H 1.2568 0.0874 0.4957 0.067 Uiso 1 1 calc R . . C22 C 1.1472(3) 0.1269(2) 0.6172(3) 0.0582(7) Uani 1 1 d . . . H22A H 1.2123 0.1152 0.6587 0.070 Uiso 1 1 calc R . . C23 C 1.0963(3) 0.1098(2) 0.3514(2) 0.0546(7) Uani 1 1 d . . . H23A H 1.1762 0.0851 0.3221 0.066 Uiso 1 1 calc R . . C24 C 0.9967(3) 0.1282(2) 0.2965(2) 0.0546(6) Uani 1 1 d . . . H24A H 1.0076 0.1151 0.2295 0.065 Uiso 1 1 calc R . . C25 C 0.8772(2) 0.16689(19) 0.33932(19) 0.0459(5) Uani 1 1 d . . . H25A H 0.8105 0.1803 0.2995 0.055 Uiso 1 1 calc R . . C26 C 1.1710(3) 0.5945(3) 0.9353(2) 0.0580(7) Uani 1 1 d . . . C27 C 1.0553(3) 0.6490(2) 0.92416(19) 0.0513(6) Uani 1 1 d . . . C28 C 0.9758(3) 0.6285(2) 0.8593(2) 0.0515(6) Uani 1 1 d . . . H28A H 0.8986 0.6663 0.8526 0.062 Uiso 1 1 calc R . . C29 C 1.0121(3) 0.5505(2) 0.8035(2) 0.0531(6) Uani 1 1 d . . . C30 C 1.1219(3) 0.4911(3) 0.8151(2) 0.0658(8) Uani 1 1 d . . . H30A H 1.1431 0.4366 0.7792 0.079 Uiso 1 1 calc R . . C31 C 1.1995(3) 0.5136(3) 0.8804(3) 0.0689(8) Uani 1 1 d . . . H31A H 1.2747 0.4733 0.8887 0.083 Uiso 1 1 calc R . . C32 C 1.2661(4) 0.6219(4) 1.0017(3) 0.0855(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.03359(18) 0.02920(17) 0.03652(18) -0.00977(12) -0.00989(12) 0.00449(11) Cl1 0.0879(6) 0.0780(5) 0.0696(5) -0.0373(4) -0.0116(4) -0.0030(4) N1 0.0365(9) 0.0328(9) 0.0401(9) -0.0119(7) -0.0094(7) 0.0025(7) N2 0.0395(9) 0.0321(8) 0.0380(9) -0.0104(7) -0.0111(7) 0.0018(7) N3 0.0401(9) 0.0327(9) 0.0424(9) -0.0114(7) -0.0125(8) 0.0059(7) N4 0.0382(9) 0.0325(9) 0.0398(9) -0.0084(7) -0.0051(7) -0.0007(7) N5 0.0760(18) 0.0826(18) 0.0577(14) -0.0275(14) -0.0105(13) -0.0169(15) O1 0.0379(8) 0.0345(8) 0.0470(8) -0.0141(6) -0.0071(6) 0.0082(6) O2 0.0425(8) 0.0298(7) 0.0434(8) -0.0105(6) -0.0055(6) 0.0064(6) O3 0.0497(10) 0.0484(10) 0.0689(12) -0.0124(9) 0.0079(9) -0.0045(8) O4 0.183(4) 0.198(4) 0.172(4) 0.066(3) -0.139(4) -0.081(3) O5 0.109(2) 0.128(3) 0.0931(19) -0.0236(17) -0.0367(17) -0.047(2) O6 0.117(2) 0.129(3) 0.110(2) -0.073(2) -0.0350(18) -0.0093(19) O7 0.110(2) 0.119(2) 0.0896(19) -0.0311(17) -0.0563(17) 0.0123(19) O8 0.0887(18) 0.107(2) 0.0794(16) -0.0192(14) 0.0085(13) -0.0283(15) O9 0.109(2) 0.101(2) 0.105(2) -0.0336(17) -0.0145(17) 0.0153(17) O10 0.123(3) 0.141(3) 0.126(3) -0.014(2) 0.003(2) -0.018(2) O11 0.117(4) 0.317(9) 0.091(3) -0.080(4) 0.007(3) -0.027(4) O11A 0.078(8) 0.212(19) 0.082(9) -0.031(10) -0.024(6) 0.043(10) O12 0.133(6) 0.259(10) 0.097(4) 0.009(5) -0.076(4) 0.009(6) O12A 0.090(5) 0.42(2) 0.093(5) -0.079(8) -0.014(4) -0.107(8) C1 0.0381(11) 0.0372(11) 0.0444(11) -0.0125(9) -0.0080(9) 0.0057(9) C2 0.0448(12) 0.0366(11) 0.0503(12) -0.0145(9) -0.0135(10) 0.0006(9) C3 0.0457(13) 0.0518(14) 0.0565(14) -0.0236(11) -0.0165(11) -0.0018(10) C4 0.0429(12) 0.0612(15) 0.0460(12) -0.0164(11) -0.0195(10) 0.0056(11) C5 0.0368(11) 0.0476(12) 0.0390(11) -0.0111(9) -0.0101(9) 0.0059(9) C6 0.0327(10) 0.0371(10) 0.0342(10) -0.0094(8) -0.0066(8) 0.0040(8) C7 0.0346(10) 0.0333(10) 0.0338(10) -0.0083(8) -0.0058(8) 0.0038(8) C8 0.0411(11) 0.0336(10) 0.0405(11) -0.0079(8) -0.0026(9) 0.0049(8) C9 0.0528(13) 0.0385(11) 0.0491(13) -0.0045(10) -0.0117(11) 0.0119(10) C10 0.0473(13) 0.0521(13) 0.0461(12) -0.0071(10) -0.0168(10) 0.0127(11) C11 0.0544(13) 0.0312(10) 0.0507(13) -0.0114(9) -0.0063(10) 0.0019(9) C12 0.0543(14) 0.0385(12) 0.0582(14) -0.0173(10) -0.0138(11) -0.0034(10) C13 0.0486(12) 0.0387(11) 0.0481(12) -0.0127(10) -0.0169(10) -0.0002(9) C14 0.0553(14) 0.0546(14) 0.0447(12) -0.0195(11) -0.0143(11) 0.0112(11) C15 0.0756(19) 0.0744(18) 0.0498(14) -0.0248(13) -0.0275(13) 0.0124(15) C17 0.0455(13) 0.0403(12) 0.0623(15) -0.0076(11) -0.0234(11) 0.0030(10) C16 0.0676(18) 0.0671(17) 0.0617(16) -0.0194(14) -0.0371(14) 0.0110(14) C18 0.0378(11) 0.0284(9) 0.0474(12) -0.0067(8) -0.0133(9) 0.0025(8) C19 0.0371(11) 0.0272(9) 0.0470(12) -0.0062(8) -0.0072(9) -0.0001(8) C20 0.0367(11) 0.0347(11) 0.0611(14) -0.0061(10) 0.0011(10) -0.0001(9) C21 0.0344(12) 0.0473(13) 0.0812(19) -0.0076(13) -0.0091(12) 0.0062(10) C22 0.0422(13) 0.0537(15) 0.0787(19) -0.0060(13) -0.0235(13) 0.0061(11) C23 0.0443(13) 0.0463(13) 0.0657(16) -0.0143(12) 0.0128(12) 0.0003(10) C24 0.0578(15) 0.0535(14) 0.0481(13) -0.0156(11) 0.0084(12) -0.0050(12) C25 0.0496(13) 0.0459(12) 0.0418(12) -0.0122(10) -0.0035(10) -0.0028(10) C26 0.0527(15) 0.0706(18) 0.0475(13) -0.0084(12) -0.0061(11) -0.0099(13) C27 0.0567(15) 0.0551(14) 0.0418(12) -0.0131(11) -0.0037(11) -0.0097(12) C28 0.0544(14) 0.0541(14) 0.0451(13) -0.0095(11) -0.0084(11) -0.0032(11) C29 0.0544(15) 0.0622(16) 0.0419(12) -0.0130(11) -0.0038(11) -0.0123(12) C30 0.0666(18) 0.0734(19) 0.0572(16) -0.0252(14) 0.0039(14) -0.0053(15) C31 0.0491(15) 0.085(2) 0.0687(18) -0.0162(16) -0.0023(14) 0.0073(14) C32 0.065(2) 0.124(3) 0.066(2) -0.009(2) -0.0212(16) -0.018(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 1.8732(16) . ? Co1 O2 1.8944(16) . ? Co1 N3 1.9122(19) . ? Co1 N1 1.9157(19) . ? Co1 N4 1.9480(19) . ? Co1 N2 1.9551(18) . ? Co1 C1 2.305(2) . ? Cl1 C27 1.729(3) . ? N1 C2 1.323(3) . ? N1 C6 1.355(3) . ? N2 C13 1.327(3) . ? N2 C7 1.357(3) . ? N3 C14 1.327(3) . ? N3 C18 1.354(3) . ? N4 C25 1.321(3) . ? N4 C19 1.352(3) . ? N5 O6 1.215(4) . ? N5 O7 1.220(4) . ? N5 C29 1.455(4) . ? O1 C1 1.315(3) . ? O2 C1 1.316(3) . ? O3 C1 1.213(3) . ? O4 C32 1.228(5) . ? O5 C32 1.208(5) . ? O8 H8B 0.8522 . ? O8 H8C 0.8592 . ? O9 H9B 0.8204 . ? O9 H9C 0.8700 . ? O10 H10B 0.8100 . ? O10 H10C 0.8701 . ? C2 C3 1.388(3) . ? C2 H2A 0.9300 . ? C3 C4 1.358(4) . ? C3 H3A 0.9300 . ? C4 C5 1.406(3) . ? C4 H4A 0.9300 . ? C5 C6 1.387(3) . ? C5 C10 1.427(3) . ? C6 C7 1.411(3) . ? C7 C8 1.398(3) . ? C8 C11 1.398(3) . ? C8 C9 1.420(3) . ? C9 C10 1.349(4) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.356(4) . ? C11 H11A 0.9300 . ? C12 C13 1.394(3) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.372(4) . ? C14 H14A 0.9300 . ? C15 C16 1.352(5) . ? C15 H15A 0.9300 . ? C17 C18 1.393(3) . ? C17 C16 1.400(4) . ? C17 C22 1.427(4) . ? C16 H16A 0.9300 . ? C18 C19 1.407(3) . ? C19 C20 1.396(3) . ? C20 C23 1.394(4) . ? C20 C21 1.423(4) . ? C21 C22 1.334(4) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.348(4) . ? C23 H23A 0.9300 . ? C24 C25 1.394(4) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.381(4) . ? C26 C31 1.390(5) . ? C26 C32 1.521(4) . ? C27 C28 1.356(4) . ? C28 C29 1.377(4) . ? C28 H28A 0.9300 . ? C29 C30 1.360(4) . ? C30 C31 1.355(5) . ? C30 H30A 0.9300 . ? C31 H31A 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 O1 Co1 O2 69.58(7) . . ? O1 Co1 N3 92.19(8) . . ? O2 Co1 N3 90.65(8) . . ? O1 Co1 N1 89.27(7) . . ? O2 Co1 N1 91.87(8) . . ? N3 Co1 N1 177.40(7) . . ? O1 Co1 N4 166.21(7) . . ? O2 Co1 N4 97.19(8) . . ? N3 Co1 N4 83.85(8) . . ? N1 Co1 N4 95.21(8) . . ? O1 Co1 N2 95.17(8) . . ? O2 Co1 N2 164.27(7) . . ? N3 Co1 N2 93.91(8) . . ? N1 Co1 N2 83.82(8) . . ? N4 Co1 N2 98.27(8) . . ? O1 Co1 C1 34.78(7) . . ? O2 Co1 C1 34.81(7) . . ? N3 Co1 C1 91.88(8) . . ? N1 Co1 C1 90.54(8) . . ? N4 Co1 C1 131.90(8) . . ? N2 Co1 C1 129.83(8) . . ? C2 N1 C6 118.35(19) . . ? C2 N1 Co1 128.82(16) . . ? C6 N1 Co1 112.69(14) . . ? C13 N2 C7 117.49(19) . . ? C13 N2 Co1 130.73(16) . . ? C7 N2 Co1 111.16(14) . . ? C14 N3 C18 118.0(2) . . ? C14 N3 Co1 129.00(17) . . ? C18 N3 Co1 112.93(15) . . ? C25 N4 C19 117.5(2) . . ? C25 N4 Co1 130.27(17) . . ? C19 N4 Co1 111.79(15) . . ? O6 N5 O7 123.9(3) . . ? O6 N5 C29 117.5(3) . . ? O7 N5 C29 118.6(3) . . ? C1 O1 Co1 90.86(13) . . ? C1 O2 Co1 89.91(13) . . ? H8B O8 H8C 102.0 . . ? H9B O9 H9C 115.7 . . ? H10B O10 H10C 93.1 . . ? O3 C1 O1 124.6(2) . . ? O3 C1 O2 125.7(2) . . ? O1 C1 O2 109.64(19) . . ? O3 C1 Co1 178.3(2) . . ? O1 C1 Co1 54.36(11) . . ? O2 C1 Co1 55.28(11) . . ? N1 C2 C3 121.6(2) . . ? N1 C2 H2A 119.2 . . ? C3 C2 H2A 119.2 . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 C4 116.3(2) . . ? C6 C5 C10 118.3(2) . . ? C4 C5 C10 125.4(2) . . ? N1 C6 C5 123.8(2) . . ? N1 C6 C7 115.61(18) . . ? C5 C6 C7 120.6(2) . . ? N2 C7 C8 123.9(2) . . ? N2 C7 C6 115.71(18) . . ? C8 C7 C6 120.4(2) . . ? C11 C8 C7 116.7(2) . . ? C11 C8 C9 125.1(2) . . ? C7 C8 C9 118.1(2) . . ? C10 C9 C8 121.5(2) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C9 C10 C5 121.0(2) . . ? C9 C10 H10A 119.5 . . ? C5 C10 H10A 119.5 . . ? C12 C11 C8 119.3(2) . . ? C12 C11 H11A 120.3 . . ? C8 C11 H11A 120.3 . . ? C11 C12 C13 120.5(2) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? N2 C13 C12 122.0(2) . . ? N2 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? N3 C14 C15 121.8(2) . . ? N3 C14 H14A 119.1 . . ? C15 C14 H14A 119.1 . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C18 C17 C16 116.7(2) . . ? C18 C17 C22 117.5(2) . . ? C16 C17 C22 125.7(2) . . ? C15 C16 C17 119.3(2) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? N3 C18 C17 123.3(2) . . ? N3 C18 C19 115.67(19) . . ? C17 C18 C19 121.0(2) . . ? N4 C19 C20 124.0(2) . . ? N4 C19 C18 115.64(19) . . ? C20 C19 C18 120.3(2) . . ? C23 C20 C19 116.5(2) . . ? C23 C20 C21 125.7(2) . . ? C19 C20 C21 117.7(2) . . ? C22 C21 C20 121.8(2) . . ? C22 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? C21 C22 C17 121.5(2) . . ? C21 C22 H22A 119.3 . . ? C17 C22 H22A 119.3 . . ? C24 C23 C20 119.5(2) . . ? C24 C23 H23A 120.3 . . ? C20 C23 H23A 120.3 . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? N4 C25 C24 121.9(2) . . ? N4 C25 H25A 119.0 . . ? C24 C25 H25A 119.0 . . ? C27 C26 C31 116.7(3) . . ? C27 C26 C32 122.8(3) . . ? C31 C26 C32 120.5(3) . . ? C28 C27 C26 122.1(3) . . ? C28 C27 Cl1 116.5(2) . . ? C26 C27 Cl1 121.4(2) . . ? C27 C28 C29 118.5(3) . . ? C27 C28 H28A 120.7 . . ? C29 C28 H28A 120.7 . . ? C30 C29 C28 121.8(3) . . ? C30 C29 N5 119.4(3) . . ? C28 C29 N5 118.8(3) . . ? C31 C30 C29 118.3(3) . . ? C31 C30 H30A 120.8 . . ? C29 C30 H30A 120.8 . . ? C30 C31 C26 122.4(3) . . ? C30 C31 H31A 118.8 . . ? C26 C31 H31A 118.8 . . ? O5 C32 O4 127.2(4) . . ? O5 C32 C26 118.5(3) . . ? O4 C32 C26 114.3(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 O1 Co1 N1 C2 -88.5(2) . . . . ? O2 Co1 N1 C2 -18.9(2) . . . . ? N3 Co1 N1 C2 147.1(15) . . . . ? N4 Co1 N1 C2 78.4(2) . . . . ? N2 Co1 N1 C2 176.2(2) . . . . ? C1 Co1 N1 C2 -53.7(2) . . . . ? O1 Co1 N1 C6 87.19(15) . . . . ? O2 Co1 N1 C6 156.74(15) . . . . ? N3 Co1 N1 C6 -37.2(16) . . . . ? N4 Co1 N1 C6 -105.87(15) . . . . ? N2 Co1 N1 C6 -8.09(14) . . . . ? C1 Co1 N1 C6 121.95(15) . . . . ? O1 Co1 N2 C13 90.9(2) . . . . ? O2 Co1 N2 C13 104.8(3) . . . . ? N3 Co1 N2 C13 -1.7(2) . . . . ? N1 Co1 N2 C13 179.6(2) . . . . ? N4 Co1 N2 C13 -86.0(2) . . . . ? C1 Co1 N2 C13 94.0(2) . . . . ? O1 Co1 N2 C7 -79.60(15) . . . . ? O2 Co1 N2 C7 -65.6(3) . . . . ? N3 Co1 N2 C7 -172.16(14) . . . . ? N1 Co1 N2 C7 9.10(14) . . . . ? N4 Co1 N2 C7 103.49(15) . . . . ? C1 Co1 N2 C7 -76.43(17) . . . . ? O1 Co1 N3 C14 -12.6(2) . . . . ? O2 Co1 N3 C14 -82.2(2) . . . . ? N1 Co1 N3 C14 111.8(16) . . . . ? N4 Co1 N3 C14 -179.3(2) . . . . ? N2 Co1 N3 C14 82.8(2) . . . . ? C1 Co1 N3 C14 -47.4(2) . . . . ? O1 Co1 N3 C18 164.59(15) . . . . ? O2 Co1 N3 C18 95.00(15) . . . . ? N1 Co1 N3 C18 -71.1(16) . . . . ? N4 Co1 N3 C18 -2.16(14) . . . . ? N2 Co1 N3 C18 -100.07(15) . . . . ? C1 Co1 N3 C18 129.79(15) . . . . ? O1 Co1 N4 C25 101.1(3) . . . . ? O2 Co1 N4 C25 85.1(2) . . . . ? N3 Co1 N4 C25 175.0(2) . . . . ? N1 Co1 N4 C25 -7.4(2) . . . . ? N2 Co1 N4 C25 -91.9(2) . . . . ? C1 Co1 N4 C25 88.0(2) . . . . ? O1 Co1 N4 C19 -70.8(3) . . . . ? O2 Co1 N4 C19 -86.74(15) . . . . ? N3 Co1 N4 C19 3.13(14) . . . . ? N1 Co1 N4 C19 -179.30(14) . . . . ? N2 Co1 N4 C19 96.21(15) . . . . ? C1 Co1 N4 C19 -83.87(17) . . . . ? O2 Co1 O1 C1 -0.27(12) . . . . ? N3 Co1 O1 C1 -90.14(13) . . . . ? N1 Co1 O1 C1 92.00(13) . . . . ? N4 Co1 O1 C1 -17.2(4) . . . . ? N2 Co1 O1 C1 175.73(13) . . . . ? O1 Co1 O2 C1 0.27(12) . . . . ? N3 Co1 O2 C1 92.37(13) . . . . ? N1 Co1 O2 C1 -88.26(13) . . . . ? N4 Co1 O2 C1 176.25(13) . . . . ? N2 Co1 O2 C1 -14.6(3) . . . . ? Co1 O1 C1 O3 -178.3(2) . . . . ? Co1 O1 C1 O2 0.39(17) . . . . ? Co1 O2 C1 O3 178.3(2) . . . . ? Co1 O2 C1 O1 -0.38(17) . . . . ? O1 Co1 C1 O3 55(7) . . . . ? O2 Co1 C1 O3 -125(7) . . . . ? N3 Co1 C1 O3 146(7) . . . . ? N1 Co1 C1 O3 -33(7) . . . . ? N4 Co1 C1 O3 -130(7) . . . . ? N2 Co1 C1 O3 49(7) . . . . ? O2 Co1 C1 O1 179.6(2) . . . . ? N3 Co1 C1 O1 91.14(13) . . . . ? N1 Co1 C1 O1 -87.94(13) . . . . ? N4 Co1 C1 O1 174.56(11) . . . . ? N2 Co1 C1 O1 -5.54(17) . . . . ? O1 Co1 C1 O2 -179.6(2) . . . . ? N3 Co1 C1 O2 -88.42(13) . . . . ? N1 Co1 C1 O2 92.50(13) . . . . ? N4 Co1 C1 O2 -5.00(17) . . . . ? N2 Co1 C1 O2 174.90(11) . . . . ? C6 N1 C2 C3 0.5(3) . . . . ? Co1 N1 C2 C3 175.94(18) . . . . ? N1 C2 C3 C4 -1.7(4) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? C3 C4 C5 C10 179.7(2) . . . . ? C2 N1 C6 C5 1.4(3) . . . . ? Co1 N1 C6 C5 -174.75(17) . . . . ? C2 N1 C6 C7 -178.19(19) . . . . ? Co1 N1 C6 C7 5.6(2) . . . . ? C4 C5 C6 N1 -2.0(3) . . . . ? C10 C5 C6 N1 178.9(2) . . . . ? C4 C5 C6 C7 177.6(2) . . . . ? C10 C5 C6 C7 -1.5(3) . . . . ? C13 N2 C7 C8 0.4(3) . . . . ? Co1 N2 C7 C8 172.31(16) . . . . ? C13 N2 C7 C6 179.59(19) . . . . ? Co1 N2 C7 C6 -8.5(2) . . . . ? N1 C6 C7 N2 2.1(3) . . . . ? C5 C6 C7 N2 -177.53(19) . . . . ? N1 C6 C7 C8 -178.71(18) . . . . ? C5 C6 C7 C8 1.7(3) . . . . ? N2 C7 C8 C11 -0.2(3) . . . . ? C6 C7 C8 C11 -179.3(2) . . . . ? N2 C7 C8 C9 178.5(2) . . . . ? C6 C7 C8 C9 -0.6(3) . . . . ? C11 C8 C9 C10 178.0(2) . . . . ? C7 C8 C9 C10 -0.5(4) . . . . ? C8 C9 C10 C5 0.7(4) . . . . ? C6 C5 C10 C9 0.4(4) . . . . ? C4 C5 C10 C9 -178.7(2) . . . . ? C7 C8 C11 C12 -0.3(3) . . . . ? C9 C8 C11 C12 -178.8(2) . . . . ? C8 C11 C12 C13 0.4(4) . . . . ? C7 N2 C13 C12 -0.3(3) . . . . ? Co1 N2 C13 C12 -170.27(18) . . . . ? C11 C12 C13 N2 -0.1(4) . . . . ? C18 N3 C14 C15 -0.1(4) . . . . ? Co1 N3 C14 C15 176.9(2) . . . . ? N3 C14 C15 C16 0.3(5) . . . . ? C14 C15 C16 C17 -0.3(5) . . . . ? C18 C17 C16 C15 0.1(4) . . . . ? C22 C17 C16 C15 -176.7(3) . . . . ? C14 N3 C18 C17 0.0(3) . . . . ? Co1 N3 C18 C17 -177.55(17) . . . . ? C14 N3 C18 C19 178.3(2) . . . . ? Co1 N3 C18 C19 0.8(2) . . . . ? C16 C17 C18 N3 0.0(3) . . . . ? C22 C17 C18 N3 177.2(2) . . . . ? C16 C17 C18 C19 -178.3(2) . . . . ? C22 C17 C18 C19 -1.1(3) . . . . ? C25 N4 C19 C20 0.8(3) . . . . ? Co1 N4 C19 C20 173.85(17) . . . . ? C25 N4 C19 C18 -176.56(19) . . . . ? Co1 N4 C19 C18 -3.5(2) . . . . ? N3 C18 C19 N4 1.9(3) . . . . ? C17 C18 C19 N4 -179.72(19) . . . . ? N3 C18 C19 C20 -175.63(19) . . . . ? C17 C18 C19 C20 2.8(3) . . . . ? N4 C19 C20 C23 -1.0(3) . . . . ? C18 C19 C20 C23 176.2(2) . . . . ? N4 C19 C20 C21 180.0(2) . . . . ? C18 C19 C20 C21 -2.7(3) . . . . ? C23 C20 C21 C22 -177.7(3) . . . . ? C19 C20 C21 C22 1.2(4) . . . . ? C20 C21 C22 C17 0.5(4) . . . . ? C18 C17 C22 C21 -0.5(4) . . . . ? C16 C17 C22 C21 176.4(3) . . . . ? C19 C20 C23 C24 0.1(3) . . . . ? C21 C20 C23 C24 179.0(2) . . . . ? C20 C23 C24 C25 1.0(4) . . . . ? C19 N4 C25 C24 0.3(3) . . . . ? Co1 N4 C25 C24 -171.19(18) . . . . ? C23 C24 C25 N4 -1.2(4) . . . . ? C31 C26 C27 C28 -2.9(4) . . . . ? C32 C26 C27 C28 175.6(3) . . . . ? C31 C26 C27 Cl1 176.5(2) . . . . ? C32 C26 C27 Cl1 -4.9(4) . . . . ? C26 C27 C28 C29 0.3(4) . . . . ? Cl1 C27 C28 C29 -179.2(2) . . . . ? C27 C28 C29 C30 2.7(4) . . . . ? C27 C28 C29 N5 -174.3(2) . . . . ? O6 N5 C29 C30 12.8(4) . . . . ? O7 N5 C29 C30 -165.9(3) . . . . ? O6 N5 C29 C28 -170.2(3) . . . . ? O7 N5 C29 C28 11.1(4) . . . . ? C28 C29 C30 C31 -2.8(4) . . . . ? N5 C29 C30 C31 174.1(3) . . . . ? C29 C30 C31 C26 0.0(5) . . . . ? C27 C26 C31 C30 2.8(4) . . . . ? C32 C26 C31 C30 -175.7(3) . . . . ? C27 C26 C32 O5 -59.9(5) . . . . ? C31 C26 C32 O5 118.5(4) . . . . ? C27 C26 C32 O4 123.6(5) . . . . ? C31 C26 C32 O4 -58.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.541 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.077 data_7cophbz _database_code_depnum_ccdc_archive 'CCDC 791262' #TrackingRef 'cif_791260-791267_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 791262' _audit_creation_method SHELXL-97 _chemical_name_systematic ; carbonatobis(1,10-phenanthroline)cobalt(III) 2-methoxybenzoate.octahydrate ; _chemical_name_common ;carbonatobis(1,10-phenanthroline)cobalt(iii) 2- methoxybenzoate.octahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H41 Co N4 O14' _chemical_formula_weight 836.68 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.227(2) _cell_length_b 12.460(3) _cell_length_c 15.064(3) _cell_angle_alpha 105.26(3) _cell_angle_beta 102.43(3) _cell_angle_gamma 100.50(3) _cell_volume 1920.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5158 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 21.38 _exptl_crystal_description rod _exptl_crystal_colour 'reddish pink' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEXII' _diffrn_measurement_method 'combination of \w and \f' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19602 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6361 _reflns_number_gt 4720 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 (Bruker, 2007)' _computing_data_reduction 'APEX2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _computing_publication_material SHELXL-97 _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. The ISOR restraints are used for the approximately isotropic refinement of many water molecules. ; _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^)+(0.0831P)^2^+0.9432P] 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 6361 _refine_ls_number_parameters 529 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1597 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.116 _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 Co1 Co 0.79954(4) 0.72882(4) 0.23090(3) 0.0453(2) Uani 1 1 d . . . O1 O 0.9541(2) 0.7957(2) 0.21292(18) 0.0589(7) Uani 1 1 d . . . O2 O 0.8583(2) 0.6165(2) 0.15528(18) 0.0584(7) Uani 1 1 d . . . O3 O 1.0331(3) 0.6769(3) 0.1138(2) 0.0920(11) Uani 1 1 d . . . O4 O 1.6793(5) 0.9425(3) 0.8068(3) 0.1333(17) Uani 1 1 d . . . O5 O 1.4826(5) 0.8348(4) 0.7511(2) 0.1045(13) Uani 1 1 d . . . O6 O 1.4819(4) 0.7907(4) 0.5564(3) 0.1361(18) Uani 1 1 d . . . O7 O 1.2743(5) 0.6302(4) 0.6456(3) 0.1340(16) Uani 1 1 d . . . H7B H 1.3477 0.6755 0.6688 0.161 Uiso 1 1 d R . . H7C H 1.2500 0.6439 0.6968 0.161 Uiso 1 1 d R . . O8 O 0.8953(6) 0.3509(5) 0.2326(4) 0.202(3) Uani 1 1 d . . . H8B H 0.9366 0.3762 0.1973 0.243 Uiso 1 1 d R . . H8C H 0.9184 0.2933 0.2370 0.243 Uiso 1 1 d R . . O9 O 1.0467(6) 0.4398(5) 0.1138(6) 0.238(3) Uani 1 1 d U . . H9B H 1.0153 0.3819 0.0635 0.285 Uiso 1 1 d R . . H9C H 1.0089 0.4924 0.1068 0.285 Uiso 1 1 d R . . O10 O 0.6089(8) 1.0340(7) 0.1204(4) 0.259(4) Uani 1 1 d U . . H10B H 0.5456 0.9857 0.0762 0.310 Uiso 1 1 d R . . H10C H 0.5804 1.0754 0.1611 0.310 Uiso 1 1 d R . . O11 O 0.8793(10) 0.1303(7) 0.1795(8) 0.315(5) Uani 1 1 d U . . H11B H 0.8781 0.0930 0.1208 0.378 Uiso 1 1 d R . . H11C H 0.8035 0.0900 0.1738 0.378 Uiso 1 1 d R . . O12 O 1.9914(13) 0.9274(13) 0.9323(10) 0.321(9) Uani 0.742(15) 1 d PU A 1 O12A O 1.087(3) 0.772(2) -0.0087(19) 0.195(15) Uiso 0.258(15) 1 d P . 2 O13 O 1.9252(7) 1.0127(6) 0.8376(5) 0.169(3) Uani 0.800(10) 1 d PU B 1 O13A O 1.079(2) 0.280(2) 0.0643(19) 0.145(12) Uiso 0.200(10) 1 d P . 2 O14 O 1.6583(14) 1.1045(9) 0.9613(8) 0.237(7) Uani 0.662(17) 1 d PU C 1 O14A O 1.776(2) 1.1501(16) 0.9362(14) 0.171(10) Uiso 0.338(17) 1 d P . 2 N1 N 0.7055(3) 0.7510(3) 0.1166(2) 0.0518(8) Uani 1 1 d . . . N2 N 0.6388(3) 0.6302(2) 0.2220(2) 0.0457(7) Uani 1 1 d . . . N3 N 0.7757(3) 0.8653(2) 0.3180(2) 0.0454(7) Uani 1 1 d . . . N4 N 0.8858(3) 0.7079(2) 0.3481(2) 0.0462(7) Uani 1 1 d . . . C1 C 0.9549(4) 0.6946(4) 0.1576(3) 0.0637(11) Uani 1 1 d . . . C2 C 0.7461(5) 0.8120(4) 0.0633(3) 0.0672(11) Uani 1 1 d . . . H2 H 0.8299 0.8537 0.0821 0.081 Uiso 1 1 calc R . . C3 C 0.6646(6) 0.8141(4) -0.0206(3) 0.0805(14) Uani 1 1 d . . . H3A H 0.6949 0.8570 -0.0568 0.097 Uiso 1 1 calc R . . C4 C 0.5432(6) 0.7550(4) -0.0491(3) 0.0799(15) Uani 1 1 d . . . H4A H 0.4901 0.7566 -0.1052 0.096 Uiso 1 1 calc R . . C5 C 0.4963(4) 0.6912(4) 0.0051(3) 0.0639(11) Uani 1 1 d . . . C6 C 0.5834(4) 0.6921(3) 0.0876(3) 0.0510(9) Uani 1 1 d . . . C7 C 0.5466(3) 0.6266(3) 0.1461(3) 0.0478(9) Uani 1 1 d . . . C8 C 0.4229(4) 0.5604(3) 0.1217(3) 0.0598(11) Uani 1 1 d . . . C9 C 0.3360(4) 0.5631(4) 0.0385(4) 0.0775(14) Uani 1 1 d . . . H9A H 0.2527 0.5209 0.0221 0.093 Uiso 1 1 calc R . . C10 C 0.3705(5) 0.6244(4) -0.0169(3) 0.0788(14) Uani 1 1 d . . . H10A H 0.3109 0.6233 -0.0709 0.095 Uiso 1 1 calc R . . C11 C 0.3963(4) 0.4947(4) 0.1808(3) 0.0700(12) Uani 1 1 d . . . H11A H 0.3148 0.4507 0.1690 0.084 Uiso 1 1 calc R . . C12 C 0.4896(4) 0.4953(3) 0.2551(3) 0.0667(11) Uani 1 1 d . . . H12A H 0.4727 0.4497 0.2931 0.080 Uiso 1 1 calc R . . C13 C 0.6104(4) 0.5641(3) 0.2747(3) 0.0561(10) Uani 1 1 d . . . H13A H 0.6732 0.5640 0.3262 0.067 Uiso 1 1 calc R . . C14 C 0.7220(4) 0.9465(3) 0.2987(3) 0.0592(10) Uani 1 1 d . . . H14A H 0.6859 0.9405 0.2353 0.071 Uiso 1 1 calc R . . C16 C 0.7690(4) 1.0508(3) 0.4648(3) 0.0647(11) Uani 1 1 d . . . H16A H 0.7659 1.1136 0.5131 0.078 Uiso 1 1 calc R . . C15 C 0.7191(4) 1.0405(3) 0.3723(4) 0.0688(12) Uani 1 1 d . . . H15A H 0.6822 1.0968 0.3573 0.083 Uiso 1 1 calc R . . C17 C 0.8256(4) 0.9667(3) 0.4881(3) 0.0553(10) Uani 1 1 d . . . C18 C 0.8267(3) 0.8761(3) 0.4109(3) 0.0462(9) Uani 1 1 d . . . C19 C 0.8869(3) 0.7903(3) 0.4278(2) 0.0450(8) Uani 1 1 d . . . C20 C 0.9447(3) 0.7936(3) 0.5211(3) 0.0564(10) Uani 1 1 d . . . C21 C 0.9398(4) 0.8851(4) 0.5992(3) 0.0692(12) Uani 1 1 d . . . H21A H 0.9759 0.8880 0.6617 0.083 Uiso 1 1 calc R . . C22 C 0.8835(4) 0.9668(4) 0.5834(3) 0.0681(12) Uani 1 1 d . . . H22A H 0.8817 1.0256 0.6356 0.082 Uiso 1 1 calc R . . C23 C 1.0051(4) 0.7078(4) 0.5301(3) 0.0666(12) Uani 1 1 d . . . H23A H 1.0460 0.7066 0.5904 0.080 Uiso 1 1 calc R . . C24 C 1.0040(4) 0.6256(4) 0.4503(4) 0.0689(12) Uani 1 1 d . . . H24A H 1.0445 0.5680 0.4561 0.083 Uiso 1 1 calc R . . C25 C 0.9424(4) 0.6263(3) 0.3590(3) 0.0598(10) Uani 1 1 d . . . H25A H 0.9415 0.5683 0.3052 0.072 Uiso 1 1 calc R . . C26 C 1.6346(4) 0.7733(3) 0.6791(3) 0.0602(10) Uani 1 1 d . . . C27 C 1.5740(4) 0.7360(4) 0.5829(3) 0.0739(12) Uani 1 1 d . . . C28 C 1.6045(4) 0.6526(4) 0.5178(3) 0.0787(13) Uani 1 1 d . . . H28A H 1.5617 0.6294 0.4531 0.094 Uiso 1 1 calc R . . C29 C 1.6986(4) 0.6043(4) 0.5498(4) 0.0756(13) Uani 1 1 d . . . H29A H 1.7174 0.5457 0.5068 0.091 Uiso 1 1 calc R . . C30 C 1.7642(4) 0.6411(5) 0.6431(4) 0.0790(13) Uani 1 1 d . . . H30A H 1.8295 0.6093 0.6638 0.095 Uiso 1 1 calc R . . C31 C 1.7342(4) 0.7267(4) 0.7083(3) 0.0735(13) Uani 1 1 d . . . H31A H 1.7813 0.7531 0.7722 0.088 Uiso 1 1 calc R . . C32 C 1.5946(7) 0.8591(4) 0.7499(3) 0.0830(15) Uani 1 1 d . . . C33 C 1.4267(5) 0.7733(5) 0.4616(3) 0.0753(14) Uani 1 1 d . . . C34 C 1.3194(5) 0.6866(4) 0.4121(4) 0.0864(15) Uani 1 1 d . . . H34A H 1.2883 0.6329 0.4396 0.104 Uiso 1 1 calc R . . C35 C 1.2603(5) 0.6817(6) 0.3219(5) 0.0975(18) Uani 1 1 d . . . H35A H 1.1874 0.6237 0.2878 0.117 Uiso 1 1 calc R . . C36 C 1.3026(6) 0.7560(8) 0.2811(5) 0.108(2) Uani 1 1 d . . . H36A H 1.2606 0.7492 0.2188 0.130 Uiso 1 1 calc R . . C37 C 1.4042(7) 0.8401(7) 0.3285(5) 0.119(2) Uani 1 1 d . . . H37A H 1.4327 0.8928 0.2992 0.143 Uiso 1 1 calc R . . C38 C 1.4681(5) 0.8515(6) 0.4190(5) 0.1000(18) Uani 1 1 d . . . H38 H 1.5394 0.9119 0.4518 0.120 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0464(3) 0.0403(3) 0.0423(3) 0.0111(2) 0.0068(2) 0.0035(2) O1 0.0526(16) 0.0580(17) 0.0535(16) 0.0106(13) 0.0114(12) -0.0025(13) O2 0.0554(16) 0.0528(15) 0.0527(16) 0.0025(12) 0.0085(13) 0.0076(13) O3 0.063(2) 0.127(3) 0.071(2) 0.0069(19) 0.0267(17) 0.0159(19) O4 0.216(5) 0.075(2) 0.081(3) 0.004(2) 0.045(3) -0.003(3) O5 0.143(4) 0.119(3) 0.065(2) 0.021(2) 0.039(2) 0.063(3) O6 0.174(4) 0.194(4) 0.060(2) 0.021(3) 0.025(2) 0.131(4) O7 0.163(4) 0.113(3) 0.121(3) 0.027(3) 0.023(3) 0.058(3) O8 0.258(7) 0.162(5) 0.150(5) -0.018(4) 0.023(5) 0.102(5) O9 0.170(5) 0.144(5) 0.338(9) 0.004(5) 0.037(6) 0.033(4) O10 0.438(10) 0.284(7) 0.147(5) 0.068(5) 0.109(6) 0.285(8) O11 0.355(10) 0.198(7) 0.389(11) 0.093(8) 0.105(9) 0.064(7) O12 0.275(13) 0.346(15) 0.290(13) 0.022(10) 0.081(10) 0.064(11) O13 0.173(6) 0.139(5) 0.154(6) 0.054(4) 0.014(4) -0.039(4) O14 0.309(14) 0.159(9) 0.250(11) 0.004(7) 0.141(9) 0.090(9) N1 0.057(2) 0.0488(17) 0.0463(18) 0.0150(15) 0.0114(15) 0.0102(15) N2 0.0468(17) 0.0400(16) 0.0442(17) 0.0117(13) 0.0074(14) 0.0048(13) N3 0.0455(16) 0.0381(16) 0.0493(18) 0.0141(13) 0.0110(14) 0.0047(13) N4 0.0415(16) 0.0404(16) 0.0520(18) 0.0149(14) 0.0085(13) 0.0035(13) C1 0.052(2) 0.079(3) 0.047(2) 0.009(2) 0.005(2) 0.010(2) C2 0.086(3) 0.067(3) 0.054(3) 0.026(2) 0.022(2) 0.017(2) C3 0.124(5) 0.075(3) 0.053(3) 0.032(2) 0.025(3) 0.032(3) C4 0.112(4) 0.081(3) 0.044(2) 0.013(2) 0.005(3) 0.047(3) C5 0.080(3) 0.061(3) 0.042(2) 0.004(2) 0.003(2) 0.031(2) C6 0.059(2) 0.048(2) 0.041(2) 0.0061(17) 0.0067(18) 0.0182(18) C7 0.047(2) 0.0404(19) 0.046(2) 0.0013(16) 0.0061(17) 0.0113(16) C8 0.048(2) 0.050(2) 0.064(3) -0.004(2) 0.009(2) 0.0098(18) C9 0.047(2) 0.079(3) 0.075(3) -0.004(3) -0.007(2) 0.009(2) C10 0.065(3) 0.086(3) 0.058(3) -0.003(3) -0.014(2) 0.029(3) C11 0.053(3) 0.054(3) 0.081(3) -0.002(2) 0.021(2) -0.008(2) C12 0.064(3) 0.053(2) 0.075(3) 0.015(2) 0.022(2) -0.004(2) C13 0.058(2) 0.049(2) 0.054(2) 0.0144(19) 0.0103(19) 0.0022(18) C14 0.059(2) 0.049(2) 0.070(3) 0.023(2) 0.017(2) 0.0114(19) C16 0.057(2) 0.050(2) 0.078(3) 0.003(2) 0.031(2) 0.003(2) C15 0.062(3) 0.045(2) 0.104(4) 0.022(2) 0.031(3) 0.016(2) C17 0.050(2) 0.047(2) 0.060(3) 0.0052(19) 0.0240(19) -0.0051(18) C18 0.0406(19) 0.0409(19) 0.048(2) 0.0096(17) 0.0132(16) -0.0060(16) C19 0.0386(19) 0.044(2) 0.045(2) 0.0161(17) 0.0088(16) -0.0058(16) C20 0.044(2) 0.065(3) 0.051(2) 0.022(2) 0.0082(17) -0.0100(19) C21 0.064(3) 0.086(3) 0.042(2) 0.018(2) 0.010(2) -0.007(2) C22 0.064(3) 0.073(3) 0.044(2) -0.002(2) 0.020(2) -0.014(2) C23 0.053(2) 0.085(3) 0.063(3) 0.043(3) 0.005(2) 0.005(2) C24 0.056(3) 0.074(3) 0.091(3) 0.050(3) 0.018(2) 0.017(2) C25 0.060(2) 0.055(2) 0.069(3) 0.027(2) 0.018(2) 0.014(2) C26 0.077(3) 0.056(2) 0.046(2) 0.0199(19) 0.017(2) 0.007(2) C27 0.071(3) 0.094(3) 0.057(3) 0.018(2) 0.016(2) 0.032(3) C28 0.071(3) 0.095(3) 0.060(3) 0.005(3) 0.019(2) 0.026(3) C29 0.073(3) 0.071(3) 0.088(4) 0.024(3) 0.034(3) 0.020(2) C30 0.064(3) 0.091(4) 0.101(4) 0.052(3) 0.033(3) 0.023(3) C31 0.069(3) 0.079(3) 0.066(3) 0.040(3) 0.008(2) -0.009(2) C32 0.134(5) 0.067(3) 0.045(3) 0.023(2) 0.019(3) 0.018(3) C33 0.074(3) 0.109(4) 0.042(2) 0.010(3) 0.014(2) 0.045(3) C34 0.106(4) 0.062(3) 0.100(4) 0.022(3) 0.047(4) 0.027(3) C35 0.068(3) 0.107(5) 0.086(4) -0.006(3) 0.011(3) 0.014(3) C36 0.081(4) 0.174(7) 0.082(4) 0.043(5) 0.021(3) 0.058(5) C37 0.113(5) 0.152(6) 0.117(5) 0.079(5) 0.045(5) 0.025(5) C38 0.057(3) 0.128(5) 0.099(4) 0.027(4) 0.023(3) -0.004(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 O2 1.874(3) . ? Co1 O1 1.890(3) . ? Co1 N4 1.929(3) . ? Co1 N1 1.931(3) . ? Co1 N2 1.946(3) . ? Co1 N3 1.957(3) . ? O1 C1 1.317(5) . ? O2 C1 1.307(5) . ? O3 C1 1.224(5) . ? O4 C32 1.241(6) . ? O5 C32 1.243(6) . ? O6 C33 1.370(5) . ? O6 C27 1.384(5) . ? O7 H7B 0.8496 . ? O7 H7C 0.8594 . ? O8 H8B 0.8600 . ? O8 H8C 0.8201 . ? O9 H9B 0.8504 . ? O9 H9C 0.8605 . ? O10 H10B 0.8600 . ? O10 H10C 0.8501 . ? O11 H11B 0.8802 . ? O11 H11C 0.8801 . ? O12A O14A 1.64(3) 2_876 ? O12A O13A 1.79(3) 2_765 ? O13A O12A 1.79(3) 2_765 ? O14A O12A 1.64(3) 2_876 ? N1 C2 1.336(5) . ? N1 C6 1.348(5) . ? N2 C13 1.329(5) . ? N2 C7 1.352(4) . ? N3 C14 1.332(5) . ? N3 C18 1.354(4) . ? N4 C25 1.320(5) . ? N4 C19 1.355(5) . ? C2 C3 1.401(6) . ? C2 H2 0.9300 . ? C3 C4 1.342(7) . ? C3 H3A 0.9300 . ? C4 C5 1.397(7) . ? C4 H4A 0.9300 . ? C5 C6 1.402(5) . ? C5 C10 1.423(7) . ? C6 C7 1.423(5) . ? C7 C8 1.395(5) . ? C8 C11 1.400(6) . ? C8 C9 1.426(6) . ? C9 C10 1.341(7) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.356(6) . ? C11 H11A 0.9300 . ? C12 C13 1.391(5) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.396(6) . ? C14 H14A 0.9300 . ? C16 C15 1.347(6) . ? C16 C17 1.401(6) . ? C16 H16A 0.9300 . ? C15 H15A 0.9300 . ? C17 C18 1.396(5) . ? C17 C22 1.443(6) . ? C18 C19 1.412(5) . ? C19 C20 1.402(5) . ? C20 C23 1.387(6) . ? C20 C21 1.426(6) . ? C21 C22 1.338(6) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.354(6) . ? C23 H23A 0.9300 . ? C24 C25 1.404(6) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.373(6) . ? C26 C31 1.393(6) . ? C26 C32 1.504(7) . ? C27 C28 1.377(6) . ? C28 C29 1.370(6) . ? C28 H28A 0.9300 . ? C29 C30 1.349(7) . ? C29 H29A 0.9300 . ? C30 C31 1.393(7) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C33 C38 1.368(7) . ? C33 C34 1.375(7) . ? C34 C35 1.358(8) . ? C34 H34A 0.9300 . ? C35 C36 1.313(8) . ? C35 H35A 0.9300 . ? C36 C37 1.315(9) . ? C36 H36A 0.9300 . ? C37 C38 1.354(8) . ? C37 H37A 0.9300 . ? C38 H38 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 O2 Co1 O1 69.44(12) . . ? O2 Co1 N4 92.71(12) . . ? O1 Co1 N4 91.38(12) . . ? O2 Co1 N1 89.85(12) . . ? O1 Co1 N1 91.32(13) . . ? N4 Co1 N1 176.80(12) . . ? O2 Co1 N2 97.41(12) . . ? O1 Co1 N2 166.07(12) . . ? N4 Co1 N2 93.93(12) . . ? N1 Co1 N2 83.83(13) . . ? O2 Co1 N3 167.72(12) . . ? O1 Co1 N3 98.90(12) . . ? N4 Co1 N3 83.47(12) . . ? N1 Co1 N3 94.42(12) . . ? N2 Co1 N3 94.50(12) . . ? C1 O1 Co1 89.9(2) . . ? C1 O2 Co1 90.9(2) . . ? C33 O6 C27 120.5(4) . . ? H7B O7 H7C 98.1 . . ? H8B O8 H8C 104.6 . . ? H9B O9 H9C 107.8 . . ? H10B O10 H10C 107.9 . . ? H11B O11 H11C 93.2 . . ? O14A O12A O13A 162(2) 2_876 2_765 ? C2 N1 C6 117.9(3) . . ? C2 N1 Co1 129.1(3) . . ? C6 N1 Co1 113.0(2) . . ? C13 N2 C7 117.8(3) . . ? C13 N2 Co1 130.1(3) . . ? C7 N2 Co1 112.0(2) . . ? C14 N3 C18 118.2(3) . . ? C14 N3 Co1 129.9(3) . . ? C18 N3 Co1 111.8(2) . . ? C25 N4 C19 118.2(3) . . ? C25 N4 Co1 128.5(3) . . ? C19 N4 Co1 113.3(2) . . ? O3 C1 O2 125.2(4) . . ? O3 C1 O1 125.2(4) . . ? O2 C1 O1 109.6(4) . . ? N1 C2 C3 121.1(4) . . ? N1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 120.6(4) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 116.1(4) . . ? C4 C5 C10 126.1(4) . . ? C6 C5 C10 117.8(4) . . ? N1 C6 C5 124.1(4) . . ? N1 C6 C7 115.3(3) . . ? C5 C6 C7 120.6(4) . . ? N2 C7 C8 123.8(4) . . ? N2 C7 C6 115.9(3) . . ? C8 C7 C6 120.2(4) . . ? C7 C8 C11 116.4(4) . . ? C7 C8 C9 117.8(4) . . ? C11 C8 C9 125.7(4) . . ? C10 C9 C8 122.1(4) . . ? C10 C9 H9A 118.9 . . ? C8 C9 H9A 118.9 . . ? C9 C10 C5 121.4(4) . . ? C9 C10 H10A 119.3 . . ? C5 C10 H10A 119.3 . . ? C12 C11 C8 119.8(4) . . ? C12 C11 H11A 120.1 . . ? C8 C11 H11A 120.1 . . ? C11 C12 C13 120.1(4) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? N2 C13 C12 121.9(4) . . ? N2 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? N3 C14 C15 120.8(4) . . ? N3 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C15 C14 121.0(4) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C18 C17 C16 116.0(4) . . ? C18 C17 C22 117.9(4) . . ? C16 C17 C22 126.1(4) . . ? N3 C18 C17 124.0(3) . . ? N3 C18 C19 116.2(3) . . ? C17 C18 C19 119.7(4) . . ? N4 C19 C20 123.6(3) . . ? N4 C19 C18 115.2(3) . . ? C20 C19 C18 121.2(4) . . ? C23 C20 C19 116.9(4) . . ? C23 C20 C21 124.8(4) . . ? C19 C20 C21 118.3(4) . . ? C22 C21 C20 120.6(4) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C21 C22 C17 122.2(4) . . ? C21 C22 H22A 118.9 . . ? C17 C22 H22A 118.9 . . ? C24 C23 C20 119.4(4) . . ? C24 C23 H23A 120.3 . . ? C20 C23 H23A 120.3 . . ? C23 C24 C25 120.8(4) . . ? C23 C24 H24A 119.6 . . ? C25 C24 H24A 119.6 . . ? N4 C25 C24 121.2(4) . . ? N4 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C27 C26 C31 116.7(4) . . ? C27 C26 C32 121.8(4) . . ? C31 C26 C32 121.5(4) . . ? C26 C27 C28 122.6(4) . . ? C26 C27 O6 114.6(4) . . ? C28 C27 O6 122.7(4) . . ? C29 C28 C27 119.0(4) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C30 C29 C28 120.6(5) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C30 C31 C26 120.9(4) . . ? C30 C31 H31A 119.6 . . ? C26 C31 H31A 119.6 . . ? O4 C32 O5 126.3(6) . . ? O4 C32 C26 116.4(6) . . ? O5 C32 C26 117.0(5) . . ? C38 C33 O6 119.9(5) . . ? C38 C33 C34 119.0(5) . . ? O6 C33 C34 120.5(6) . . ? C35 C34 C33 118.0(5) . . ? C35 C34 H34A 121.0 . . ? C33 C34 H34A 121.0 . . ? C36 C35 C34 122.3(6) . . ? C36 C35 H35A 118.8 . . ? C34 C35 H35A 118.8 . . ? C35 C36 C37 120.0(6) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C38 121.3(6) . . ? C36 C37 H37A 119.3 . . ? C38 C37 H37A 119.3 . . ? C37 C38 C33 119.3(5) . . ? C37 C38 H38 120.4 . . ? C33 C38 H38 120.4 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.568 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.057 data_2copnbz _database_code_depnum_ccdc_archive 'CCDC 791263' #TrackingRef 'cif_791260-791267_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 791263' _audit_creation_method SHELXL-97 _chemical_name_systematic ; carbonatobis(1,10-phenanthroline)cobalt(III) 4-nitrobenzoate.pentahydrate ; _chemical_name_common ;carbonatobis(1,10-phenanthroline)cobalt(iii) 4- nitrobenzoate.pentahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 Co N5 O12' _chemical_formula_weight 735.54 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.287(2) _cell_length_b 13.078(3) _cell_length_c 13.134(3) _cell_angle_alpha 70.22(3) _cell_angle_beta 83.92(3) _cell_angle_gamma 72.95(3) _cell_volume 1589.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7402 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 26.11 _exptl_crystal_description block _exptl_crystal_colour 'reddish pink' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEXII' _diffrn_measurement_method 'combination of \w and \f' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21262 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6218 _reflns_number_gt 5012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 (Bruker, 2007)' _computing_data_reduction 'APEX2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _computing_publication_material SHELXL-97 _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^)+(0.0691P)^2^+0.2144P] 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 6218 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Co1 Co 0.16883(3) 1.03380(2) 0.20542(2) 0.03023(11) Uani 1 1 d . . . O1 O 0.10342(15) 1.09332(13) 0.06202(12) 0.0369(3) Uani 1 1 d . . . O2 O -0.00293(14) 1.14028(12) 0.19624(12) 0.0370(4) Uani 1 1 d . . . O3 O -0.10098(17) 1.22153(15) 0.03254(15) 0.0535(4) Uani 1 1 d . . . O4 O -0.6210(3) 0.2177(2) 0.4315(2) 0.1005(9) Uani 1 1 d . . . O5 O -0.5851(3) 0.1746(2) 0.6005(2) 0.0931(8) Uani 1 1 d . . . O6 O -0.1709(2) 0.5416(2) 0.31323(17) 0.0767(7) Uani 1 1 d . . . O7 O -0.1934(2) 0.54810(19) 0.47968(17) 0.0715(6) Uani 1 1 d . . . O8 O 0.2636(2) 0.63386(19) 0.16084(18) 0.0787(6) Uani 1 1 d . . . H8C H 0.2093 0.6691 0.1111 0.094 Uiso 1 1 d R . . H8B H 0.2138 0.6002 0.2050 0.094 Uiso 1 1 d R . . O9 O 0.1210(2) 0.50015(17) 0.30995(17) 0.0726(6) Uani 1 1 d . . . H9B H 0.0347 0.5166 0.3143 0.087 Uiso 1 1 d R . . H9C H 0.1350 0.4920 0.3737 0.087 Uiso 1 1 d R . . O10 O -0.2257(3) 0.5842(3) 0.1005(2) 0.1267(11) Uani 1 1 d . . . H10B H -0.2267 0.5854 0.1619 0.152 Uiso 1 1 d R . . H10C H -0.1613 0.5225 0.1108 0.152 Uiso 1 1 d R . . O11 O 0.5110(3) 1.5304(3) 0.0860(2) 0.1192(10) Uani 1 1 d . . . H11B H 0.5875 1.5460 0.0901 0.143 Uiso 1 1 d R . . H11C H 0.4511 1.5632 0.1230 0.143 Uiso 1 1 d R . . O12 O -0.0489(5) 0.4425(4) 0.0096(5) 0.125(3) Uani 0.564(7) 1 d P . . O12A O 0.7101(10) 1.4012(9) 0.0957(9) 0.193(6) Uani 0.436(7) 1 d P . . N1 N 0.08029(17) 0.91490(14) 0.24208(15) 0.0338(4) Uani 1 1 d . . . N2 N 0.19588(17) 0.98527(14) 0.36187(14) 0.0322(4) Uani 1 1 d . . . N3 N 0.26181(18) 1.14865(15) 0.17889(14) 0.0341(4) Uani 1 1 d . . . N4 N 0.34551(18) 0.94213(15) 0.17582(15) 0.0346(4) Uani 1 1 d . . . N5 N -0.5706(2) 0.2273(2) 0.5063(2) 0.0637(7) Uani 1 1 d . . . C1 C 0.0288(2) 0.87778(19) 0.1776(2) 0.0424(5) Uani 1 1 d . . . H1A H 0.0392 0.9077 0.1032 0.051 Uiso 1 1 calc R . . C2 C -0.0406(2) 0.7953(2) 0.2182(2) 0.0506(6) Uani 1 1 d . . . H2A H -0.0738 0.7699 0.1709 0.061 Uiso 1 1 calc R . . C3 C -0.0601(2) 0.7516(2) 0.3263(2) 0.0502(7) Uani 1 1 d . . . H3A H -0.1096 0.6988 0.3530 0.060 Uiso 1 1 calc R . . C4 C -0.0047(2) 0.78721(18) 0.3981(2) 0.0411(6) Uani 1 1 d . . . C5 C 0.0657(2) 0.86872(17) 0.35097(18) 0.0342(5) Uani 1 1 d . . . C6 C 0.1292(2) 0.90606(17) 0.41638(18) 0.0323(5) Uani 1 1 d . . . C7 C 0.1247(2) 0.86167(18) 0.52917(19) 0.0399(5) Uani 1 1 d . . . C8 C 0.0504(3) 0.7792(2) 0.5758(2) 0.0494(6) Uani 1 1 d . . . H8A H 0.0451 0.7489 0.6507 0.059 Uiso 1 1 calc R . . C9 C -0.0117(2) 0.7449(2) 0.5136(2) 0.0499(7) Uani 1 1 d . . . H9A H -0.0604 0.6923 0.5464 0.060 Uiso 1 1 calc R . . C10 C 0.1935(2) 0.9017(2) 0.58781(19) 0.0465(6) Uani 1 1 d . . . H10A H 0.1937 0.8746 0.6630 0.056 Uiso 1 1 calc R . . C11 C 0.2601(3) 0.9810(2) 0.5330(2) 0.0463(6) Uani 1 1 d . . . H11A H 0.3059 1.0081 0.5710 0.056 Uiso 1 1 calc R . . C12 C 0.2595(2) 1.02112(19) 0.42050(19) 0.0393(5) Uani 1 1 d . . . H12A H 0.3053 1.0751 0.3848 0.047 Uiso 1 1 calc R . . C13 C 0.2129(3) 1.25405(19) 0.18119(19) 0.0431(6) Uani 1 1 d . . . H13A H 0.1205 1.2813 0.1936 0.052 Uiso 1 1 calc R . . C14 C 0.2967(3) 1.3244(2) 0.1655(2) 0.0542(7) Uani 1 1 d . . . H14A H 0.2602 1.3972 0.1689 0.065 Uiso 1 1 calc R . . C15 C 0.4320(3) 1.2874(2) 0.1453(2) 0.0541(7) Uani 1 1 d . . . H15A H 0.4877 1.3348 0.1340 0.065 Uiso 1 1 calc R . . C16 C 0.4860(2) 1.1776(2) 0.14170(19) 0.0459(6) Uani 1 1 d . . . C17 C 0.3966(2) 1.11111(19) 0.15949(17) 0.0354(5) Uani 1 1 d . . . C18 C 0.4418(2) 0.9994(2) 0.15549(18) 0.0373(5) Uani 1 1 d . . . C19 C 0.5765(2) 0.9550(2) 0.1284(2) 0.0472(6) Uani 1 1 d . . . C20 C 0.6660(3) 1.0252(3) 0.1094(2) 0.0627(8) Uani 1 1 d . . . H20A H 0.7562 0.9975 0.0909 0.075 Uiso 1 1 calc R . . C21 C 0.6246(3) 1.1299(3) 0.1172(2) 0.0592(7) Uani 1 1 d . . . H21A H 0.6869 1.1717 0.1066 0.071 Uiso 1 1 calc R . . C22 C 0.6101(3) 0.8466(2) 0.1199(2) 0.0569(7) Uani 1 1 d . . . H22A H 0.6983 0.8130 0.1017 0.068 Uiso 1 1 calc R . . C23 C 0.5136(3) 0.7904(2) 0.1382(2) 0.0552(7) Uani 1 1 d . . . H23A H 0.5358 0.7186 0.1318 0.066 Uiso 1 1 calc R . . C24 C 0.3815(2) 0.8397(2) 0.16664(19) 0.0432(5) Uani 1 1 d . . . H24A H 0.3170 0.7996 0.1795 0.052 Uiso 1 1 calc R . . C25 C -0.0078(2) 1.15744(18) 0.09209(18) 0.0368(5) Uani 1 1 d . . . C26 C -0.4847(2) 0.3051(2) 0.4803(2) 0.0447(6) Uani 1 1 d . . . C27 C -0.4311(2) 0.3206(2) 0.5627(2) 0.0475(6) Uani 1 1 d . . . H27A H -0.4509 0.2844 0.6343 0.057 Uiso 1 1 calc R . . C28 C -0.3471(2) 0.3906(2) 0.5385(2) 0.0450(6) Uani 1 1 d . . . H28A H -0.3112 0.4026 0.5942 0.054 Uiso 1 1 calc R . . C29 C -0.3157(2) 0.44298(19) 0.4327(2) 0.0412(5) Uani 1 1 d . . . C30 C -0.3721(3) 0.4268(2) 0.3507(2) 0.0572(7) Uani 1 1 d . . . H30A H -0.3518 0.4624 0.2790 0.069 Uiso 1 1 calc R . . C31 C -0.4584(3) 0.3585(3) 0.3736(2) 0.0617(8) Uani 1 1 d . . . H31A H -0.4979 0.3488 0.3182 0.074 Uiso 1 1 calc R . . C32 C -0.2180(3) 0.5171(2) 0.4060(2) 0.0528(7) 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 0.03010(17) 0.03174(16) 0.03186(18) -0.01196(12) 0.00466(12) -0.01265(12) O1 0.0364(8) 0.0415(8) 0.0334(8) -0.0136(7) 0.0034(7) -0.0108(7) O2 0.0326(8) 0.0380(8) 0.0397(9) -0.0137(7) 0.0072(7) -0.0101(6) O3 0.0408(9) 0.0568(11) 0.0517(11) -0.0087(9) -0.0052(8) -0.0055(8) O4 0.126(2) 0.112(2) 0.0993(19) -0.0316(16) -0.0148(16) -0.0848(19) O5 0.111(2) 0.0946(18) 0.0829(18) -0.0027(14) 0.0040(15) -0.0733(17) O6 0.0909(16) 0.1048(17) 0.0585(13) -0.0278(12) 0.0207(12) -0.0684(14) O7 0.0855(15) 0.0889(15) 0.0641(13) -0.0280(12) 0.0011(11) -0.0564(13) O8 0.0752(14) 0.0777(14) 0.0789(16) -0.0139(12) -0.0096(12) -0.0250(12) O9 0.0766(14) 0.0732(14) 0.0624(14) -0.0189(11) 0.0061(11) -0.0184(11) O10 0.176(3) 0.112(2) 0.083(2) -0.0362(17) 0.002(2) -0.022(2) O11 0.137(3) 0.111(2) 0.116(2) -0.0389(19) 0.024(2) -0.049(2) O12 0.131(5) 0.097(4) 0.144(6) -0.052(4) 0.019(4) -0.018(3) O12A 0.157(8) 0.205(10) 0.285(14) -0.174(10) 0.080(8) -0.066(8) N1 0.0304(9) 0.0338(9) 0.0390(11) -0.0121(8) 0.0014(8) -0.0115(8) N2 0.0329(9) 0.0308(9) 0.0348(10) -0.0116(8) 0.0048(8) -0.0119(7) N3 0.0383(10) 0.0378(10) 0.0286(10) -0.0092(8) 0.0055(8) -0.0177(8) N4 0.0344(9) 0.0381(10) 0.0325(10) -0.0143(8) 0.0003(8) -0.0086(8) N5 0.0611(15) 0.0550(14) 0.0828(19) -0.0202(14) -0.0010(14) -0.0298(12) C1 0.0401(12) 0.0418(12) 0.0525(15) -0.0198(11) -0.0044(11) -0.0149(10) C2 0.0419(13) 0.0454(13) 0.074(2) -0.0270(13) -0.0063(13) -0.0158(11) C3 0.0347(12) 0.0364(12) 0.084(2) -0.0209(13) 0.0051(13) -0.0167(10) C4 0.0301(11) 0.0298(11) 0.0618(16) -0.0127(10) 0.0090(11) -0.0118(9) C5 0.0279(10) 0.0284(10) 0.0447(13) -0.0116(9) 0.0047(9) -0.0075(8) C6 0.0289(10) 0.0283(10) 0.0380(12) -0.0115(9) 0.0057(9) -0.0067(8) C7 0.0383(12) 0.0355(11) 0.0401(13) -0.0110(10) 0.0113(10) -0.0071(9) C8 0.0489(14) 0.0423(13) 0.0438(15) -0.0035(11) 0.0168(12) -0.0111(11) C9 0.0415(13) 0.0366(12) 0.0639(18) -0.0071(12) 0.0175(13) -0.0165(11) C10 0.0501(14) 0.0520(14) 0.0326(13) -0.0142(11) 0.0056(11) -0.0080(12) C11 0.0514(14) 0.0519(14) 0.0418(14) -0.0217(12) -0.0008(12) -0.0154(12) C12 0.0420(12) 0.0419(12) 0.0397(13) -0.0155(10) 0.0019(10) -0.0182(10) C13 0.0519(14) 0.0373(12) 0.0429(14) -0.0143(10) 0.0087(11) -0.0181(11) C14 0.077(2) 0.0418(13) 0.0517(16) -0.0151(12) 0.0053(14) -0.0299(13) C15 0.0680(18) 0.0579(16) 0.0472(15) -0.0105(12) 0.0035(13) -0.0426(15) C16 0.0472(14) 0.0626(16) 0.0330(13) -0.0088(11) 0.0019(11) -0.0312(12) C17 0.0346(11) 0.0468(12) 0.0272(11) -0.0103(9) 0.0056(9) -0.0188(10) C18 0.0306(11) 0.0511(13) 0.0297(12) -0.0117(10) 0.0018(9) -0.0129(10) C19 0.0339(12) 0.0660(16) 0.0358(13) -0.0140(12) 0.0000(10) -0.0080(11) C20 0.0308(13) 0.092(2) 0.0554(18) -0.0102(16) 0.0052(12) -0.0206(14) C21 0.0445(15) 0.081(2) 0.0538(17) -0.0094(15) 0.0044(13) -0.0358(15) C22 0.0357(13) 0.0731(19) 0.0542(17) -0.0271(14) -0.0001(12) 0.0039(13) C23 0.0529(16) 0.0551(15) 0.0530(16) -0.0264(13) -0.0073(13) 0.0048(13) C24 0.0443(13) 0.0427(13) 0.0428(14) -0.0181(11) -0.0042(11) -0.0056(10) C25 0.0349(12) 0.0373(11) 0.0382(13) -0.0091(10) 0.0036(10) -0.0150(10) C26 0.0407(13) 0.0421(13) 0.0557(16) -0.0162(12) 0.0012(11) -0.0178(11) C27 0.0484(14) 0.0473(14) 0.0431(14) -0.0068(11) 0.0000(11) -0.0168(11) C28 0.0423(13) 0.0489(14) 0.0472(15) -0.0165(12) -0.0040(11) -0.0150(11) C29 0.0358(12) 0.0425(12) 0.0477(14) -0.0160(11) -0.0004(10) -0.0124(10) C30 0.0702(18) 0.0690(18) 0.0432(15) -0.0168(13) 0.0051(13) -0.0388(15) C31 0.0757(19) 0.0773(19) 0.0533(17) -0.0275(15) -0.0043(15) -0.0433(17) C32 0.0523(15) 0.0512(15) 0.0598(18) -0.0146(13) -0.0021(13) -0.0245(12) _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 O2 1.8879(16) . ? Co1 O1 1.8908(17) . ? Co1 N3 1.9261(18) . ? Co1 N1 1.9262(17) . ? Co1 N4 1.9442(19) . ? Co1 N2 1.9588(19) . ? O1 C25 1.317(3) . ? O2 C25 1.313(3) . ? O3 C25 1.215(3) . ? O4 N5 1.217(3) . ? O5 N5 1.213(3) . ? O6 C32 1.234(3) . ? O7 C32 1.242(3) . ? O8 H8C 0.8208 . ? O8 H8B 0.8300 . ? O9 H9B 0.8502 . ? O9 H9C 0.8300 . ? O10 H10B 0.8099 . ? O10 H10C 0.8600 . ? O11 H11B 0.8801 . ? O11 H11C 0.8500 . ? N1 C1 1.326(3) . ? N1 C5 1.362(3) . ? N2 C12 1.331(3) . ? N2 C6 1.366(3) . ? N3 C13 1.331(3) . ? N3 C17 1.356(3) . ? N4 C24 1.325(3) . ? N4 C18 1.363(3) . ? N5 C26 1.470(3) . ? C1 C2 1.393(3) . ? C1 H1A 0.9300 . ? C2 C3 1.357(4) . ? C2 H2A 0.9300 . ? C3 C4 1.413(4) . ? C3 H3A 0.9300 . ? C4 C5 1.399(3) . ? C4 C9 1.429(4) . ? C5 C6 1.412(3) . ? C6 C7 1.398(3) . ? C7 C10 1.405(3) . ? C7 C8 1.434(3) . ? C8 C9 1.344(4) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C11 1.368(3) . ? C10 H10A 0.9300 . ? C11 C12 1.391(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.389(3) . ? C13 H13A 0.9300 . ? C14 C15 1.362(4) . ? C14 H14A 0.9300 . ? C15 C16 1.394(4) . ? C15 H15A 0.9300 . ? C16 C17 1.394(3) . ? C16 C21 1.429(4) . ? C17 C18 1.415(3) . ? C18 C19 1.396(3) . ? C19 C22 1.398(4) . ? C19 C20 1.430(4) . ? C20 C21 1.346(4) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.356(4) . ? C22 H22A 0.9300 . ? C23 C24 1.394(3) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C26 C27 1.363(3) . ? C26 C31 1.376(4) . ? C27 C28 1.376(3) . ? C27 H27A 0.9300 . ? C28 C29 1.377(3) . ? C28 H28A 0.9300 . ? C29 C30 1.379(3) . ? C29 C32 1.530(3) . ? C30 C31 1.379(4) . ? C30 H30A 0.9300 . ? C31 H31A 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 O2 Co1 O1 69.27(7) . . ? O2 Co1 N3 91.84(7) . . ? O1 Co1 N3 91.75(7) . . ? O2 Co1 N1 89.50(7) . . ? O1 Co1 N1 92.20(8) . . ? N3 Co1 N1 176.05(8) . . ? O2 Co1 N4 165.62(7) . . ? O1 Co1 N4 96.96(8) . . ? N3 Co1 N4 84.26(8) . . ? N1 Co1 N4 95.32(8) . . ? O2 Co1 N2 98.93(8) . . ? O1 Co1 N2 167.69(6) . . ? N3 Co1 N2 92.15(8) . . ? N1 Co1 N2 83.96(8) . . ? N4 Co1 N2 95.04(8) . . ? C25 O1 Co1 90.50(13) . . ? C25 O2 Co1 90.74(13) . . ? H8C O8 H8B 98.8 . . ? H9B O9 H9C 97.0 . . ? H10B O10 H10C 95.7 . . ? H11B O11 H11C 108.0 . . ? C1 N1 C5 118.14(19) . . ? C1 N1 Co1 129.46(17) . . ? C5 N1 Co1 112.33(14) . . ? C12 N2 C6 117.46(19) . . ? C12 N2 Co1 130.95(15) . . ? C6 N2 Co1 111.45(14) . . ? C13 N3 C17 118.26(19) . . ? C13 N3 Co1 129.14(16) . . ? C17 N3 Co1 112.55(14) . . ? C24 N4 C18 117.9(2) . . ? C24 N4 Co1 130.39(16) . . ? C18 N4 Co1 111.58(14) . . ? O5 N5 O4 123.6(3) . . ? O5 N5 C26 118.6(3) . . ? O4 N5 C26 117.8(3) . . ? N1 C1 C2 121.9(2) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 120.5(2) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 116.4(2) . . ? C5 C4 C9 118.0(2) . . ? C3 C4 C9 125.6(2) . . ? N1 C5 C4 123.5(2) . . ? N1 C5 C6 116.07(18) . . ? C4 C5 C6 120.4(2) . . ? N2 C6 C7 123.5(2) . . ? N2 C6 C5 115.52(19) . . ? C7 C6 C5 120.96(19) . . ? C6 C7 C10 117.1(2) . . ? C6 C7 C8 117.6(2) . . ? C10 C7 C8 125.2(2) . . ? C9 C8 C7 121.4(2) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C4 121.6(2) . . ? C8 C9 H9A 119.2 . . ? C4 C9 H9A 119.2 . . ? C11 C10 C7 119.3(2) . . ? C11 C10 H10A 120.4 . . ? C7 C10 H10A 120.4 . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? N2 C12 C11 122.6(2) . . ? N2 C12 H12A 118.7 . . ? C11 C12 H12A 118.7 . . ? N3 C13 C14 121.6(2) . . ? N3 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C15 C14 C13 120.4(2) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 119.3(2) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C15 C16 C17 117.3(2) . . ? C15 C16 C21 125.0(2) . . ? C17 C16 C21 117.7(2) . . ? N3 C17 C16 123.1(2) . . ? N3 C17 C18 115.62(18) . . ? C16 C17 C18 121.2(2) . . ? N4 C18 C19 123.6(2) . . ? N4 C18 C17 115.88(19) . . ? C19 C18 C17 120.5(2) . . ? C18 C19 C22 116.5(2) . . ? C18 C19 C20 117.3(3) . . ? C22 C19 C20 126.2(2) . . ? C21 C20 C19 122.4(2) . . ? C21 C20 H20A 118.8 . . ? C19 C20 H20A 118.8 . . ? C20 C21 C16 120.9(2) . . ? C20 C21 H21A 119.6 . . ? C16 C21 H21A 119.6 . . ? C23 C22 C19 119.8(2) . . ? C23 C22 H22A 120.1 . . ? C19 C22 H22A 120.1 . . ? C22 C23 C24 120.4(2) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? N4 C24 C23 121.7(2) . . ? N4 C24 H24A 119.1 . . ? C23 C24 H24A 119.1 . . ? O3 C25 O2 125.5(2) . . ? O3 C25 O1 125.0(2) . . ? O2 C25 O1 109.49(19) . . ? C27 C26 C31 121.7(2) . . ? C27 C26 N5 119.0(2) . . ? C31 C26 N5 119.3(2) . . ? C26 C27 C28 119.1(2) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.4 . . ? C27 C28 C29 120.7(2) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C28 C29 C30 119.2(2) . . ? C28 C29 C32 120.7(2) . . ? C30 C29 C32 120.1(2) . . ? C29 C30 C31 120.8(3) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C26 C31 C30 118.5(2) . . ? C26 C31 H31A 120.8 . . ? C30 C31 H31A 120.8 . . ? O6 C32 O7 125.5(2) . . ? O6 C32 C29 117.5(2) . . ? O7 C32 C29 117.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 O1 C25 0.02(11) . . . . ? N3 Co1 O1 C25 -91.28(12) . . . . ? N1 Co1 O1 C25 88.65(12) . . . . ? N4 Co1 O1 C25 -175.71(12) . . . . ? N2 Co1 O1 C25 17.2(3) . . . . ? O1 Co1 O2 C25 -0.02(11) . . . . ? N3 Co1 O2 C25 91.16(12) . . . . ? N1 Co1 O2 C25 -92.56(13) . . . . ? N4 Co1 O2 C25 17.3(3) . . . . ? N2 Co1 O2 C25 -176.37(11) . . . . ? O2 Co1 N1 C1 85.0(2) . . . . ? O1 Co1 N1 C1 15.7(2) . . . . ? N3 Co1 N1 C1 -165.2(9) . . . . ? N4 Co1 N1 C1 -81.5(2) . . . . ? N2 Co1 N1 C1 -176.0(2) . . . . ? O2 Co1 N1 C5 -91.75(15) . . . . ? O1 Co1 N1 C5 -160.99(14) . . . . ? N3 Co1 N1 C5 18.1(11) . . . . ? N4 Co1 N1 C5 101.81(15) . . . . ? N2 Co1 N1 C5 7.29(14) . . . . ? O2 Co1 N2 C12 -93.8(2) . . . . ? O1 Co1 N2 C12 -110.0(3) . . . . ? N3 Co1 N2 C12 -1.6(2) . . . . ? N1 Co1 N2 C12 177.7(2) . . . . ? N4 Co1 N2 C12 82.8(2) . . . . ? O2 Co1 N2 C6 81.75(14) . . . . ? O1 Co1 N2 C6 65.6(3) . . . . ? N3 Co1 N2 C6 173.95(14) . . . . ? N1 Co1 N2 C6 -6.79(13) . . . . ? N4 Co1 N2 C6 -101.63(14) . . . . ? O2 Co1 N3 C13 13.5(2) . . . . ? O1 Co1 N3 C13 82.8(2) . . . . ? N1 Co1 N3 C13 -96.2(10) . . . . ? N4 Co1 N3 C13 179.6(2) . . . . ? N2 Co1 N3 C13 -85.5(2) . . . . ? O2 Co1 N3 C17 -169.15(15) . . . . ? O1 Co1 N3 C17 -99.84(15) . . . . ? N1 Co1 N3 C17 81.1(10) . . . . ? N4 Co1 N3 C17 -3.02(15) . . . . ? N2 Co1 N3 C17 91.84(16) . . . . ? O2 Co1 N4 C24 -99.1(3) . . . . ? O1 Co1 N4 C24 -82.8(2) . . . . ? N3 Co1 N4 C24 -173.9(2) . . . . ? N1 Co1 N4 C24 10.1(2) . . . . ? N2 Co1 N4 C24 94.5(2) . . . . ? O2 Co1 N4 C18 76.5(3) . . . . ? O1 Co1 N4 C18 92.75(15) . . . . ? N3 Co1 N4 C18 1.68(15) . . . . ? N1 Co1 N4 C18 -174.37(15) . . . . ? N2 Co1 N4 C18 -89.98(15) . . . . ? C5 N1 C1 C2 1.0(3) . . . . ? Co1 N1 C1 C2 -175.52(17) . . . . ? N1 C1 C2 C3 1.4(4) . . . . ? C1 C2 C3 C4 -2.6(4) . . . . ? C2 C3 C4 C5 1.3(3) . . . . ? C2 C3 C4 C9 -176.9(2) . . . . ? C1 N1 C5 C4 -2.3(3) . . . . ? Co1 N1 C5 C4 174.80(16) . . . . ? C1 N1 C5 C6 176.36(19) . . . . ? Co1 N1 C5 C6 -6.5(2) . . . . ? C3 C4 C5 N1 1.2(3) . . . . ? C9 C4 C5 N1 179.54(19) . . . . ? C3 C4 C5 C6 -177.47(19) . . . . ? C9 C4 C5 C6 0.9(3) . . . . ? C12 N2 C6 C7 0.1(3) . . . . ? Co1 N2 C6 C7 -176.15(16) . . . . ? C12 N2 C6 C5 -178.69(19) . . . . ? Co1 N2 C6 C5 5.1(2) . . . . ? N1 C5 C6 N2 0.9(3) . . . . ? C4 C5 C6 N2 179.59(18) . . . . ? N1 C5 C6 C7 -177.92(18) . . . . ? C4 C5 C6 C7 0.8(3) . . . . ? N2 C6 C7 C10 -0.2(3) . . . . ? C5 C6 C7 C10 178.46(19) . . . . ? N2 C6 C7 C8 179.74(19) . . . . ? C5 C6 C7 C8 -1.6(3) . . . . ? C6 C7 C8 C9 0.6(3) . . . . ? C10 C7 C8 C9 -179.4(2) . . . . ? C7 C8 C9 C4 1.1(4) . . . . ? C5 C4 C9 C8 -1.9(3) . . . . ? C3 C4 C9 C8 176.3(2) . . . . ? C6 C7 C10 C11 0.2(3) . . . . ? C8 C7 C10 C11 -179.8(2) . . . . ? C7 C10 C11 C12 -0.1(4) . . . . ? C6 N2 C12 C11 0.1(3) . . . . ? Co1 N2 C12 C11 175.45(17) . . . . ? C10 C11 C12 N2 -0.1(4) . . . . ? C17 N3 C13 C14 -0.7(3) . . . . ? Co1 N3 C13 C14 176.48(18) . . . . ? N3 C13 C14 C15 1.2(4) . . . . ? C13 C14 C15 C16 -0.7(4) . . . . ? C14 C15 C16 C17 -0.1(4) . . . . ? C14 C15 C16 C21 177.5(3) . . . . ? C13 N3 C17 C16 -0.1(3) . . . . ? Co1 N3 C17 C16 -177.78(18) . . . . ? C13 N3 C17 C18 -178.6(2) . . . . ? Co1 N3 C17 C18 3.8(2) . . . . ? C15 C16 C17 N3 0.5(3) . . . . ? C21 C16 C17 N3 -177.2(2) . . . . ? C15 C16 C17 C18 178.9(2) . . . . ? C21 C16 C17 C18 1.2(3) . . . . ? C24 N4 C18 C19 -1.7(3) . . . . ? Co1 N4 C18 C19 -177.86(18) . . . . ? C24 N4 C18 C17 176.1(2) . . . . ? Co1 N4 C18 C17 -0.1(2) . . . . ? N3 C17 C18 N4 -2.5(3) . . . . ? C16 C17 C18 N4 179.1(2) . . . . ? N3 C17 C18 C19 175.4(2) . . . . ? C16 C17 C18 C19 -3.1(3) . . . . ? N4 C18 C19 C22 1.5(4) . . . . ? C17 C18 C19 C22 -176.2(2) . . . . ? N4 C18 C19 C20 -180.0(2) . . . . ? C17 C18 C19 C20 2.3(3) . . . . ? C18 C19 C20 C21 0.2(4) . . . . ? C22 C19 C20 C21 178.6(3) . . . . ? C19 C20 C21 C16 -2.2(5) . . . . ? C15 C16 C21 C20 -176.1(3) . . . . ? C17 C16 C21 C20 1.4(4) . . . . ? C18 C19 C22 C23 -0.3(4) . . . . ? C20 C19 C22 C23 -178.7(3) . . . . ? C19 C22 C23 C24 -0.7(4) . . . . ? C18 N4 C24 C23 0.6(3) . . . . ? Co1 N4 C24 C23 175.94(18) . . . . ? C22 C23 C24 N4 0.5(4) . . . . ? Co1 O2 C25 O3 179.3(2) . . . . ? Co1 O2 C25 O1 0.03(16) . . . . ? Co1 O1 C25 O3 -179.3(2) . . . . ? Co1 O1 C25 O2 -0.03(16) . . . . ? O5 N5 C26 C27 -4.0(4) . . . . ? O4 N5 C26 C27 177.6(3) . . . . ? O5 N5 C26 C31 174.8(3) . . . . ? O4 N5 C26 C31 -3.6(4) . . . . ? C31 C26 C27 C28 -0.8(4) . . . . ? N5 C26 C27 C28 178.0(2) . . . . ? C26 C27 C28 C29 -1.0(4) . . . . ? C27 C28 C29 C30 1.6(4) . . . . ? C27 C28 C29 C32 -177.6(2) . . . . ? C28 C29 C30 C31 -0.4(4) . . . . ? C32 C29 C30 C31 178.8(3) . . . . ? C27 C26 C31 C30 1.9(4) . . . . ? N5 C26 C31 C30 -176.8(3) . . . . ? C29 C30 C31 C26 -1.3(5) . . . . ? C28 C29 C32 O6 164.6(3) . . . . ? C30 C29 C32 O6 -14.6(4) . . . . ? C28 C29 C32 O7 -15.7(4) . . . . ? C30 C29 C32 O7 165.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.614 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.054 data_6coibz _database_code_depnum_ccdc_archive 'CCDC 791264' #TrackingRef 'cif_791260-791267_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 791264' _audit_creation_method SHELXL-97 _chemical_name_systematic ; carbonatobis(1,10-phenanthroline)cobalt(III) 2-iodobenzoate.heptahydrate ; _chemical_name_common ;carbonatobis(1,10-phenanthroline)cobalt(iii) 2- iodobenzoate.heptahydrate ; _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 Co I N4 O12' _chemical_formula_weight 852.46 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.284(2) _cell_length_b 12.636(3) _cell_length_c 14.396(3) _cell_angle_alpha 67.41(3) _cell_angle_beta 77.95(3) _cell_angle_gamma 64.21(3) _cell_volume 1704.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8687 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.31 _exptl_crystal_description block _exptl_crystal_colour 'reddish pink' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 1.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEXII' _diffrn_measurement_method 'combination of \w and \f' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16097 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6595 _reflns_number_gt 5507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 (Bruker, 2007)' _computing_data_reduction 'APEX2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _computing_publication_material SHELXL-97 _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^)+(0.0699P)^2^+0.9546P] 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 6595 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.42605(3) 0.66517(3) 0.71429(3) 0.02699(11) Uani 1 1 d . . . I1 I 0.04551(3) 0.12250(3) 0.03123(3) 0.08194(15) Uani 1 1 d . . . O1 O 0.51235(19) 0.73452(18) 0.59407(14) 0.0343(4) Uani 1 1 d . . . O2 O 0.61042(19) 0.58896(18) 0.72543(15) 0.0347(4) Uani 1 1 d . . . O3 O 0.7331(2) 0.6555(2) 0.59075(18) 0.0469(5) Uani 1 1 d . . . O4 O 0.3038(3) -0.0586(3) 0.2614(2) 0.0753(9) Uani 1 1 d . . . O5 O 0.3615(3) 0.0030(3) 0.0995(2) 0.0611(7) Uani 1 1 d . . . O6 O 0.2017(5) 0.2699(5) 0.7616(4) 0.1335(17) Uani 1 1 d . . . H6B H 0.2558 0.2465 0.8056 0.160 Uiso 1 1 d R . . H6C H 0.1492 0.3369 0.7708 0.160 Uiso 1 1 d R . . O7 O 0.9309(5) 0.4133(4) 0.7110(5) 0.140(2) Uani 1 1 d . . . H7B H 0.8789 0.4800 0.6745 0.168 Uiso 1 1 d R . . H7C H 0.8973 0.3719 0.6997 0.168 Uiso 1 1 d R . . O8 O 0.1735(4) 0.7751(4) 0.2834(3) 0.1068(13) Uani 1 1 d . . . H8B H 0.2290 0.8014 0.2794 0.128 Uiso 1 1 d R . . H8C H 0.0960 0.8314 0.2745 0.128 Uiso 1 1 d R . . O9 O 0.3885(3) 0.1889(3) 0.9141(3) 0.0751(8) Uani 1 1 d . . . H9B H 0.4687 0.1400 0.9107 0.090 Uiso 1 1 d R . . H9C H 0.3708 0.1478 0.9701 0.090 Uiso 1 1 d R . . O10 O 0.3485(5) -0.0535(3) 0.4399(3) 0.1093(15) Uani 1 1 d . . . H10B H 0.4227 -0.1164 0.4625 0.131 Uiso 1 1 d R . . H10C H 0.3507 -0.0548 0.3824 0.131 Uiso 1 1 d R . . O11 O -0.1015(4) 0.8769(4) 0.2901(4) 0.1077(13) Uani 1 1 d . . . H11B H -0.1210 0.8284 0.2709 0.129 Uiso 1 1 d R . . H11C H -0.1474 0.8743 0.3435 0.129 Uiso 1 1 d R . . O12 O 0.2593(4) 0.1163(3) 0.5377(2) 0.0839(10) Uani 1 1 d . . . H12B H 0.2968 0.0716 0.5036 0.101 Uiso 1 1 d R . . H12C H 0.2719 0.1842 0.5023 0.101 Uiso 1 1 d R . . N1 N 0.4290(2) 0.5445(2) 0.66307(17) 0.0309(5) Uani 1 1 d . . . N2 N 0.2468(2) 0.7549(2) 0.67127(17) 0.0309(5) Uani 1 1 d . . . N3 N 0.4131(2) 0.7859(2) 0.77026(17) 0.0298(5) Uani 1 1 d . . . N4 N 0.3750(2) 0.5806(2) 0.85022(17) 0.0283(5) Uani 1 1 d . . . C1 C 0.6267(3) 0.6599(3) 0.6334(2) 0.0336(6) Uani 1 1 d . . . C2 C 0.5253(3) 0.4360(3) 0.6634(2) 0.0418(7) Uani 1 1 d . . . H2A H 0.6059 0.4127 0.6882 0.050 Uiso 1 1 calc R . . C3 C 0.5079(4) 0.3573(3) 0.6276(3) 0.0494(8) Uani 1 1 d . . . H3A H 0.5764 0.2811 0.6297 0.059 Uiso 1 1 calc R . . C4 C 0.3922(4) 0.3892(3) 0.5896(3) 0.0501(8) Uani 1 1 d . . . H4A H 0.3808 0.3350 0.5665 0.060 Uiso 1 1 calc R . . C5 C 0.2898(3) 0.5053(3) 0.5853(2) 0.0414(7) Uani 1 1 d . . . C6 C 0.3140(3) 0.5783(3) 0.6241(2) 0.0330(6) Uani 1 1 d . . . C7 C 0.2156(3) 0.6937(3) 0.6266(2) 0.0320(6) Uani 1 1 d . . . C8 C 0.0944(3) 0.7378(3) 0.5870(2) 0.0413(7) Uani 1 1 d . . . C9 C 0.0718(4) 0.6626(4) 0.5460(3) 0.0563(9) Uani 1 1 d . . . H9A H -0.0086 0.6914 0.5184 0.068 Uiso 1 1 calc R . . C10 C 0.1638(4) 0.5514(4) 0.5462(3) 0.0553(9) Uani 1 1 d . . . H10A H 0.1456 0.5032 0.5205 0.066 Uiso 1 1 calc R . . C11 C 0.0016(3) 0.8539(3) 0.5937(3) 0.0477(8) Uani 1 1 d . . . H11A H -0.0806 0.8891 0.5670 0.057 Uiso 1 1 calc R . . C12 C 0.0320(3) 0.9136(3) 0.6389(3) 0.0463(8) Uani 1 1 d . . . H12A H -0.0297 0.9896 0.6442 0.056 Uiso 1 1 calc R . . C13 C 0.1561(3) 0.8620(3) 0.6780(2) 0.0399(7) Uani 1 1 d . . . H13A H 0.1752 0.9042 0.7096 0.048 Uiso 1 1 calc R . . C14 C 0.4342(3) 0.8897(3) 0.7246(2) 0.0371(6) Uani 1 1 d . . . H14A H 0.4588 0.9117 0.6563 0.045 Uiso 1 1 calc R . . C15 C 0.4197(3) 0.9669(3) 0.7786(3) 0.0430(7) Uani 1 1 d . . . H15A H 0.4346 1.0397 0.7456 0.052 Uiso 1 1 calc R . . C16 C 0.3841(3) 0.9365(3) 0.8781(3) 0.0410(7) Uani 1 1 d . . . H16A H 0.3741 0.9882 0.9134 0.049 Uiso 1 1 calc R . . C17 C 0.3626(3) 0.8267(3) 0.9273(2) 0.0334(6) Uani 1 1 d . . . C18 C 0.3778(3) 0.7553(2) 0.8694(2) 0.0281(5) Uani 1 1 d . . . C19 C 0.3573(2) 0.6432(2) 0.9135(2) 0.0277(5) Uani 1 1 d . . . C20 C 0.3230(3) 0.6026(3) 1.0156(2) 0.0315(6) Uani 1 1 d . . . C21 C 0.3071(3) 0.6773(3) 1.0736(2) 0.0383(7) Uani 1 1 d . . . H21A H 0.2834 0.6516 1.1419 0.046 Uiso 1 1 calc R . . C22 C 0.3257(3) 0.7842(3) 1.0316(2) 0.0386(7) Uani 1 1 d . . . H22A H 0.3142 0.8314 1.0713 0.046 Uiso 1 1 calc R . . C23 C 0.3075(3) 0.4893(3) 1.0533(2) 0.0357(6) Uani 1 1 d . . . H23A H 0.2853 0.4574 1.1213 0.043 Uiso 1 1 calc R . . C24 C 0.3249(3) 0.4262(3) 0.9906(2) 0.0370(6) Uani 1 1 d . . . H24A H 0.3143 0.3510 1.0155 0.044 Uiso 1 1 calc R . . C25 C 0.3587(3) 0.4739(3) 0.8885(2) 0.0333(6) Uani 1 1 d . . . H25A H 0.3700 0.4296 0.8463 0.040 Uiso 1 1 calc R . . C26 C 0.1962(3) 0.1505(3) 0.1668(2) 0.0364(6) Uani 1 1 d . . . C27 C 0.0896(3) 0.2098(3) 0.1083(3) 0.0451(7) Uani 1 1 d . . . C28 C 0.0038(3) 0.3308(3) 0.1033(3) 0.0552(9) Uani 1 1 d . . . H28A H -0.0670 0.3720 0.0618 0.066 Uiso 1 1 calc R . . C29 C 0.0205(4) 0.3894(4) 0.1566(4) 0.0673(12) Uani 1 1 d . . . H29A H -0.0390 0.4698 0.1528 0.081 Uiso 1 1 calc R . . C30 C 0.1246(4) 0.3311(4) 0.2162(3) 0.0548(9) Uani 1 1 d . . . H30A H 0.1368 0.3715 0.2532 0.066 Uiso 1 1 calc R . . C31 C 0.2119(3) 0.2123(3) 0.2217(3) 0.0447(7) Uani 1 1 d . . . H31A H 0.2828 0.1726 0.2629 0.054 Uiso 1 1 calc R . . C32 C 0.2960(3) 0.0199(3) 0.1760(3) 0.0445(7) 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 0.0291(2) 0.02525(19) 0.02501(19) -0.00904(14) -0.00388(14) -0.00761(14) I1 0.05869(19) 0.0948(3) 0.1080(3) -0.0504(2) -0.03370(17) -0.01653(16) O1 0.0370(10) 0.0341(10) 0.0258(9) -0.0065(8) -0.0031(8) -0.0109(8) O2 0.0322(10) 0.0349(10) 0.0325(10) -0.0102(9) -0.0070(8) -0.0078(8) O3 0.0380(12) 0.0538(13) 0.0480(13) -0.0185(11) 0.0060(10) -0.0195(10) O4 0.087(2) 0.0436(15) 0.0706(19) -0.0028(14) -0.0268(16) -0.0076(14) O5 0.0460(14) 0.0657(17) 0.0727(18) -0.0420(14) -0.0038(13) -0.0063(12) O6 0.106(3) 0.115(3) 0.143(4) -0.017(3) -0.017(3) -0.028(3) O7 0.103(3) 0.072(2) 0.225(6) -0.037(3) -0.057(3) -0.007(2) O8 0.094(3) 0.075(2) 0.137(4) -0.030(2) -0.006(2) -0.024(2) O9 0.0647(18) 0.0576(17) 0.111(3) -0.0456(17) -0.0059(17) -0.0151(14) O10 0.158(4) 0.0579(19) 0.070(2) -0.0175(17) -0.051(2) 0.011(2) O11 0.084(3) 0.120(3) 0.132(4) -0.054(3) 0.007(2) -0.046(2) O12 0.104(3) 0.0635(19) 0.074(2) -0.0109(16) -0.0008(18) -0.0351(18) N1 0.0343(12) 0.0304(12) 0.0269(11) -0.0105(9) -0.0029(9) -0.0103(10) N2 0.0315(12) 0.0295(12) 0.0270(11) -0.0065(9) -0.0018(9) -0.0102(10) N3 0.0323(12) 0.0274(11) 0.0305(12) -0.0088(9) -0.0027(9) -0.0126(9) N4 0.0291(11) 0.0261(11) 0.0282(11) -0.0097(9) -0.0040(9) -0.0078(9) C1 0.0361(15) 0.0354(15) 0.0321(14) -0.0145(12) -0.0005(12) -0.0142(12) C2 0.0459(17) 0.0345(16) 0.0404(16) -0.0185(13) -0.0018(13) -0.0069(13) C3 0.061(2) 0.0363(17) 0.0497(19) -0.0218(15) -0.0024(16) -0.0116(15) C4 0.068(2) 0.0472(19) 0.0468(19) -0.0267(16) 0.0011(17) -0.0248(17) C5 0.0522(18) 0.0483(18) 0.0305(15) -0.0148(14) -0.0035(13) -0.0236(15) C6 0.0377(15) 0.0390(15) 0.0224(13) -0.0109(11) 0.0009(11) -0.0156(12) C7 0.0335(14) 0.0361(15) 0.0230(13) -0.0062(11) -0.0002(11) -0.0146(12) C8 0.0364(16) 0.0494(18) 0.0337(15) -0.0083(14) -0.0038(12) -0.0169(14) C9 0.047(2) 0.076(3) 0.052(2) -0.0169(19) -0.0180(16) -0.0269(19) C10 0.059(2) 0.070(2) 0.054(2) -0.0300(19) -0.0086(17) -0.030(2) C11 0.0297(15) 0.0489(19) 0.0465(19) -0.0021(15) -0.0076(13) -0.0090(14) C12 0.0348(16) 0.0367(16) 0.0492(19) -0.0078(14) -0.0018(14) -0.0039(13) C13 0.0362(15) 0.0329(15) 0.0402(16) -0.0094(13) -0.0015(13) -0.0070(12) C14 0.0384(15) 0.0321(15) 0.0395(16) -0.0099(12) -0.0006(13) -0.0150(12) C15 0.0452(17) 0.0300(15) 0.057(2) -0.0148(14) -0.0046(15) -0.0168(13) C16 0.0391(16) 0.0375(16) 0.0548(19) -0.0242(15) -0.0049(14) -0.0137(13) C17 0.0284(13) 0.0344(14) 0.0422(16) -0.0196(13) -0.0057(11) -0.0089(11) C18 0.0258(12) 0.0279(13) 0.0299(14) -0.0114(11) -0.0054(10) -0.0066(10) C19 0.0250(12) 0.0259(13) 0.0306(14) -0.0103(11) -0.0065(10) -0.0055(10) C20 0.0279(13) 0.0349(14) 0.0276(13) -0.0090(11) -0.0048(10) -0.0086(11) C21 0.0375(15) 0.0483(18) 0.0303(15) -0.0174(13) -0.0032(12) -0.0135(13) C22 0.0387(15) 0.0435(17) 0.0393(16) -0.0261(14) -0.0042(12) -0.0095(13) C23 0.0361(15) 0.0396(16) 0.0279(14) -0.0041(12) -0.0055(11) -0.0162(12) C24 0.0413(16) 0.0307(14) 0.0361(15) -0.0033(12) -0.0066(12) -0.0165(13) C25 0.0373(15) 0.0275(13) 0.0363(15) -0.0119(12) -0.0043(12) -0.0116(11) C26 0.0307(14) 0.0375(15) 0.0378(16) -0.0108(13) 0.0011(12) -0.0132(12) C27 0.0356(16) 0.0442(18) 0.0518(19) -0.0144(15) -0.0048(14) -0.0127(14) C28 0.0352(17) 0.051(2) 0.054(2) -0.0074(17) -0.0114(15) 0.0009(15) C29 0.055(2) 0.0394(19) 0.091(3) -0.022(2) 0.010(2) -0.0095(17) C30 0.061(2) 0.054(2) 0.060(2) -0.0289(18) 0.0156(18) -0.0318(18) C31 0.0438(17) 0.0505(19) 0.0434(18) -0.0160(15) 0.0019(14) -0.0233(15) C32 0.0347(16) 0.0432(18) 0.057(2) -0.0182(16) -0.0146(15) -0.0094(13) _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 O2 1.887(2) . ? Co1 O1 1.893(2) . ? Co1 N1 1.918(2) . ? Co1 N3 1.923(2) . ? Co1 N2 1.936(3) . ? Co1 N4 1.939(2) . ? Co1 C1 2.306(3) . ? I1 C27 2.084(4) . ? O1 C1 1.308(4) . ? O2 C1 1.313(3) . ? O3 C1 1.217(4) . ? O4 C32 1.239(4) . ? O5 C32 1.228(4) . ? O6 H6B 0.8501 . ? O6 H6C 0.8380 . ? O7 H7B 0.8300 . ? O7 H7C 0.8400 . ? O8 H8B 0.8099 . ? O8 H8C 0.8500 . ? O9 H9B 0.8497 . ? O9 H9C 0.8127 . ? O10 H10B 0.8801 . ? O10 H10C 0.8296 . ? O11 H11B 0.8800 . ? O11 H11C 0.8300 . ? O12 H12B 0.8101 . ? O12 H12C 0.8701 . ? N1 C2 1.327(4) . ? N1 C6 1.349(4) . ? N2 C13 1.320(4) . ? N2 C7 1.359(4) . ? N3 C14 1.325(4) . ? N3 C18 1.349(3) . ? N4 C25 1.326(4) . ? N4 C19 1.355(3) . ? C2 C3 1.378(5) . ? C2 H2A 0.9300 . ? C3 C4 1.355(5) . ? C3 H3A 0.9300 . ? C4 C5 1.406(5) . ? C4 H4A 0.9300 . ? C5 C6 1.384(4) . ? C5 C10 1.427(5) . ? C6 C7 1.406(4) . ? C7 C8 1.387(4) . ? C8 C11 1.410(5) . ? C8 C9 1.422(5) . ? C9 C10 1.334(6) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.344(5) . ? C11 H11A 0.9300 . ? C12 C13 1.398(5) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.404(4) . ? C14 H14A 0.9300 . ? C15 C16 1.354(5) . ? C15 H15A 0.9300 . ? C16 C17 1.397(4) . ? C16 H16A 0.9300 . ? C17 C18 1.385(4) . ? C17 C22 1.425(4) . ? C18 C19 1.413(4) . ? C19 C20 1.389(4) . ? C20 C23 1.399(4) . ? C20 C21 1.420(4) . ? C21 C22 1.341(5) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.354(4) . ? C23 H23A 0.9300 . ? C24 C25 1.398(4) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.369(5) . ? C26 C31 1.384(5) . ? C26 C32 1.512(4) . ? C27 C28 1.392(5) . ? C28 C29 1.339(6) . ? C28 H28A 0.9300 . ? C29 C30 1.357(6) . ? C29 H29A 0.9300 . ? C30 C31 1.373(5) . ? C30 H30A 0.9300 . ? C31 H31A 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 O2 Co1 O1 69.26(9) . . ? O2 Co1 N1 91.82(10) . . ? O1 Co1 N1 90.90(9) . . ? O2 Co1 N3 90.96(10) . . ? O1 Co1 N3 92.14(9) . . ? N1 Co1 N3 176.46(10) . . ? O2 Co1 N2 167.33(9) . . ? O1 Co1 N2 98.67(10) . . ? N1 Co1 N2 84.32(10) . . ? N3 Co1 N2 93.42(10) . . ? O2 Co1 N4 98.50(10) . . ? O1 Co1 N4 167.22(9) . . ? N1 Co1 N4 93.20(10) . . ? N3 Co1 N4 84.21(10) . . ? N2 Co1 N4 93.78(10) . . ? O2 Co1 C1 34.70(10) . . ? O1 Co1 C1 34.57(10) . . ? N1 Co1 C1 91.59(10) . . ? N3 Co1 C1 91.94(10) . . ? N2 Co1 C1 133.12(10) . . ? N4 Co1 C1 133.10(10) . . ? C1 O1 Co1 90.24(16) . . ? C1 O2 Co1 90.41(17) . . ? H6B O6 H6C 97.9 . . ? H7B O7 H7C 92.1 . . ? H8B O8 H8C 113.6 . . ? H9B O9 H9C 96.4 . . ? H10B O10 H10C 101.3 . . ? H11B O11 H11C 99.4 . . ? H12B O12 H12C 103.2 . . ? C2 N1 C6 118.5(3) . . ? C2 N1 Co1 129.0(2) . . ? C6 N1 Co1 112.51(19) . . ? C13 N2 C7 118.0(3) . . ? C13 N2 Co1 130.5(2) . . ? C7 N2 Co1 111.45(18) . . ? C14 N3 C18 118.9(2) . . ? C14 N3 Co1 128.7(2) . . ? C18 N3 Co1 112.35(18) . . ? C25 N4 C19 117.8(2) . . ? C25 N4 Co1 130.39(19) . . ? C19 N4 Co1 111.82(18) . . ? O3 C1 O1 125.2(3) . . ? O3 C1 O2 124.7(3) . . ? O1 C1 O2 110.1(2) . . ? O3 C1 Co1 179.1(2) . . ? O1 C1 Co1 55.19(13) . . ? O2 C1 Co1 54.90(13) . . ? N1 C2 C3 121.2(3) . . ? N1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C6 C5 C4 116.5(3) . . ? C6 C5 C10 118.3(3) . . ? C4 C5 C10 125.2(3) . . ? N1 C6 C5 123.7(3) . . ? N1 C6 C7 115.8(3) . . ? C5 C6 C7 120.5(3) . . ? N2 C7 C8 123.8(3) . . ? N2 C7 C6 115.9(3) . . ? C8 C7 C6 120.3(3) . . ? C7 C8 C11 116.2(3) . . ? C7 C8 C9 118.5(3) . . ? C11 C8 C9 125.3(3) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C9 C10 C5 121.1(3) . . ? C9 C10 H10A 119.5 . . ? C5 C10 H10A 119.5 . . ? C12 C11 C8 119.9(3) . . ? C12 C11 H11A 120.0 . . ? C8 C11 H11A 120.0 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? N2 C13 C12 121.7(3) . . ? N2 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? N3 C14 C15 120.5(3) . . ? N3 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 117.0(3) . . ? C18 C17 C22 118.3(3) . . ? C16 C17 C22 124.7(3) . . ? N3 C18 C17 123.5(3) . . ? N3 C18 C19 116.0(2) . . ? C17 C18 C19 120.4(2) . . ? N4 C19 C20 124.0(2) . . ? N4 C19 C18 115.6(2) . . ? C20 C19 C18 120.4(2) . . ? C19 C20 C23 116.6(3) . . ? C19 C20 C21 118.5(3) . . ? C23 C20 C21 125.0(3) . . ? C22 C21 C20 121.2(3) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C21 C22 C17 121.3(3) . . ? C21 C22 H22A 119.4 . . ? C17 C22 H22A 119.4 . . ? C24 C23 C20 119.8(3) . . ? C24 C23 H23A 120.1 . . ? C20 C23 H23A 120.1 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? N4 C25 C24 121.7(3) . . ? N4 C25 H25A 119.1 . . ? C24 C25 H25A 119.1 . . ? C27 C26 C31 118.3(3) . . ? C27 C26 C32 123.1(3) . . ? C31 C26 C32 118.6(3) . . ? C26 C27 C28 119.1(3) . . ? C26 C27 I1 122.4(2) . . ? C28 C27 I1 118.4(3) . . ? C29 C28 C27 121.8(4) . . ? C29 C28 H28A 119.1 . . ? C27 C28 H28A 119.1 . . ? C28 C29 C30 119.7(4) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C29 C30 C31 119.8(4) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C30 C31 C26 121.2(3) . . ? C30 C31 H31A 119.4 . . ? C26 C31 H31A 119.4 . . ? O5 C32 O4 127.0(3) . . ? O5 C32 C26 117.4(3) . . ? O4 C32 C26 115.6(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 O2 Co1 O1 C1 0.11(15) . . . . ? N1 Co1 O1 C1 -91.49(17) . . . . ? N3 Co1 O1 C1 90.33(17) . . . . ? N2 Co1 O1 C1 -175.89(16) . . . . ? N4 Co1 O1 C1 17.3(5) . . . . ? O1 Co1 O2 C1 -0.11(15) . . . . ? N1 Co1 O2 C1 90.17(17) . . . . ? N3 Co1 O2 C1 -92.03(16) . . . . ? N2 Co1 O2 C1 18.2(5) . . . . ? N4 Co1 O2 C1 -176.32(16) . . . . ? O2 Co1 N1 C2 14.0(3) . . . . ? O1 Co1 N1 C2 83.3(3) . . . . ? N3 Co1 N1 C2 -127.6(16) . . . . ? N2 Co1 N1 C2 -178.1(3) . . . . ? N4 Co1 N1 C2 -84.6(3) . . . . ? C1 Co1 N1 C2 48.7(3) . . . . ? O2 Co1 N1 C6 -167.46(19) . . . . ? O1 Co1 N1 C6 -98.18(19) . . . . ? N3 Co1 N1 C6 50.9(17) . . . . ? N2 Co1 N1 C6 0.44(19) . . . . ? N4 Co1 N1 C6 93.9(2) . . . . ? C1 Co1 N1 C6 -132.7(2) . . . . ? O2 Co1 N2 C13 -108.2(5) . . . . ? O1 Co1 N2 C13 -90.9(3) . . . . ? N1 Co1 N2 C13 179.1(3) . . . . ? N3 Co1 N2 C13 1.8(3) . . . . ? N4 Co1 N2 C13 86.2(3) . . . . ? C1 Co1 N2 C13 -94.1(3) . . . . ? O2 Co1 N2 C7 71.1(5) . . . . ? O1 Co1 N2 C7 88.42(18) . . . . ? N1 Co1 N2 C7 -1.63(18) . . . . ? N3 Co1 N2 C7 -178.90(18) . . . . ? N4 Co1 N2 C7 -94.48(18) . . . . ? C1 Co1 N2 C7 85.2(2) . . . . ? O2 Co1 N3 C14 81.6(3) . . . . ? O1 Co1 N3 C14 12.3(3) . . . . ? N1 Co1 N3 C14 -136.8(15) . . . . ? N2 Co1 N3 C14 -86.5(3) . . . . ? N4 Co1 N3 C14 -180.0(3) . . . . ? C1 Co1 N3 C14 46.9(3) . . . . ? O2 Co1 N3 C18 -98.29(19) . . . . ? O1 Co1 N3 C18 -167.57(19) . . . . ? N1 Co1 N3 C18 43.4(17) . . . . ? N2 Co1 N3 C18 93.61(19) . . . . ? N4 Co1 N3 C18 0.16(19) . . . . ? C1 Co1 N3 C18 -132.98(19) . . . . ? O2 Co1 N4 C25 -88.6(3) . . . . ? O1 Co1 N4 C25 -104.8(4) . . . . ? N1 Co1 N4 C25 3.7(3) . . . . ? N3 Co1 N4 C25 -178.7(3) . . . . ? N2 Co1 N4 C25 88.3(3) . . . . ? C1 Co1 N4 C25 -91.4(3) . . . . ? O2 Co1 N4 C19 89.77(18) . . . . ? O1 Co1 N4 C19 73.5(4) . . . . ? N1 Co1 N4 C19 -177.91(18) . . . . ? N3 Co1 N4 C19 -0.34(18) . . . . ? N2 Co1 N4 C19 -93.40(19) . . . . ? C1 Co1 N4 C19 86.9(2) . . . . ? Co1 O1 C1 O3 179.0(3) . . . . ? Co1 O1 C1 O2 -0.2(2) . . . . ? Co1 O2 C1 O3 -179.0(3) . . . . ? Co1 O2 C1 O1 0.2(2) . . . . ? O2 Co1 C1 O3 63(16) . . . . ? O1 Co1 C1 O3 -117(17) . . . . ? N1 Co1 C1 O3 -28(16) . . . . ? N3 Co1 C1 O3 152(16) . . . . ? N2 Co1 C1 O3 -111(16) . . . . ? N4 Co1 C1 O3 68(16) . . . . ? O2 Co1 C1 O1 -179.8(3) . . . . ? N1 Co1 C1 O1 89.28(17) . . . . ? N3 Co1 C1 O1 -90.94(16) . . . . ? N2 Co1 C1 O1 5.6(2) . . . . ? N4 Co1 C1 O1 -174.83(14) . . . . ? O1 Co1 C1 O2 179.8(3) . . . . ? N1 Co1 C1 O2 -90.90(16) . . . . ? N3 Co1 C1 O2 88.88(16) . . . . ? N2 Co1 C1 O2 -174.61(15) . . . . ? N4 Co1 C1 O2 5.0(2) . . . . ? C6 N1 C2 C3 -1.9(4) . . . . ? Co1 N1 C2 C3 176.6(2) . . . . ? N1 C2 C3 C4 1.0(5) . . . . ? C2 C3 C4 C5 1.0(5) . . . . ? C3 C4 C5 C6 -2.0(5) . . . . ? C3 C4 C5 C10 179.3(3) . . . . ? C2 N1 C6 C5 0.8(4) . . . . ? Co1 N1 C6 C5 -177.9(2) . . . . ? C2 N1 C6 C7 179.5(3) . . . . ? Co1 N1 C6 C7 0.8(3) . . . . ? C4 C5 C6 N1 1.1(4) . . . . ? C10 C5 C6 N1 180.0(3) . . . . ? C4 C5 C6 C7 -177.6(3) . . . . ? C10 C5 C6 C7 1.3(4) . . . . ? C13 N2 C7 C8 0.6(4) . . . . ? Co1 N2 C7 C8 -178.8(2) . . . . ? C13 N2 C7 C6 -178.1(2) . . . . ? Co1 N2 C7 C6 2.5(3) . . . . ? N1 C6 C7 N2 -2.3(4) . . . . ? C5 C6 C7 N2 176.5(3) . . . . ? N1 C6 C7 C8 179.0(2) . . . . ? C5 C6 C7 C8 -2.2(4) . . . . ? N2 C7 C8 C11 0.9(4) . . . . ? C6 C7 C8 C11 179.5(3) . . . . ? N2 C7 C8 C9 -177.4(3) . . . . ? C6 C7 C8 C9 1.2(4) . . . . ? C7 C8 C9 C10 0.8(5) . . . . ? C11 C8 C9 C10 -177.3(3) . . . . ? C8 C9 C10 C5 -1.7(6) . . . . ? C6 C5 C10 C9 0.7(5) . . . . ? C4 C5 C10 C9 179.4(4) . . . . ? C7 C8 C11 C12 -1.6(5) . . . . ? C9 C8 C11 C12 176.6(3) . . . . ? C8 C11 C12 C13 0.9(5) . . . . ? C7 N2 C13 C12 -1.3(4) . . . . ? Co1 N2 C13 C12 177.9(2) . . . . ? C11 C12 C13 N2 0.6(5) . . . . ? C18 N3 C14 C15 -0.2(4) . . . . ? Co1 N3 C14 C15 180.0(2) . . . . ? N3 C14 C15 C16 0.1(5) . . . . ? C14 C15 C16 C17 0.4(5) . . . . ? C15 C16 C17 C18 -0.8(4) . . . . ? C15 C16 C17 C22 179.6(3) . . . . ? C14 N3 C18 C17 -0.3(4) . . . . ? Co1 N3 C18 C17 179.6(2) . . . . ? C14 N3 C18 C19 -179.8(2) . . . . ? Co1 N3 C18 C19 0.1(3) . . . . ? C16 C17 C18 N3 0.7(4) . . . . ? C22 C17 C18 N3 -179.6(3) . . . . ? C16 C17 C18 C19 -179.7(3) . . . . ? C22 C17 C18 C19 -0.1(4) . . . . ? C25 N4 C19 C20 -0.1(4) . . . . ? Co1 N4 C19 C20 -178.7(2) . . . . ? C25 N4 C19 C18 179.0(2) . . . . ? Co1 N4 C19 C18 0.5(3) . . . . ? N3 C18 C19 N4 -0.3(3) . . . . ? C17 C18 C19 N4 -179.9(2) . . . . ? N3 C18 C19 C20 178.8(2) . . . . ? C17 C18 C19 C20 -0.7(4) . . . . ? N4 C19 C20 C23 0.5(4) . . . . ? C18 C19 C20 C23 -178.6(2) . . . . ? N4 C19 C20 C21 -179.8(3) . . . . ? C18 C19 C20 C21 1.1(4) . . . . ? C19 C20 C21 C22 -0.6(4) . . . . ? C23 C20 C21 C22 179.1(3) . . . . ? C20 C21 C22 C17 -0.3(5) . . . . ? C18 C17 C22 C21 0.6(4) . . . . ? C16 C17 C22 C21 -179.8(3) . . . . ? C19 C20 C23 C24 -0.5(4) . . . . ? C21 C20 C23 C24 179.8(3) . . . . ? C20 C23 C24 C25 0.2(5) . . . . ? C19 N4 C25 C24 -0.2(4) . . . . ? Co1 N4 C25 C24 178.0(2) . . . . ? C23 C24 C25 N4 0.2(5) . . . . ? C31 C26 C27 C28 2.1(5) . . . . ? C32 C26 C27 C28 -179.1(3) . . . . ? C31 C26 C27 I1 -174.9(2) . . . . ? C32 C26 C27 I1 3.9(4) . . . . ? C26 C27 C28 C29 -2.1(6) . . . . ? I1 C27 C28 C29 175.1(3) . . . . ? C27 C28 C29 C30 1.0(6) . . . . ? C28 C29 C30 C31 -0.2(6) . . . . ? C29 C30 C31 C26 0.4(5) . . . . ? C27 C26 C31 C30 -1.4(5) . . . . ? C32 C26 C31 C30 179.8(3) . . . . ? C27 C26 C32 O5 63.8(4) . . . . ? C31 C26 C32 O5 -117.4(3) . . . . ? C27 C26 C32 O4 -117.3(4) . . . . ? C31 C26 C32 O4 61.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.986 _refine_diff_density_min -1.218 _refine_diff_density_rms 0.084 data_1comnbz _database_code_depnum_ccdc_archive 'CCDC 791265' #TrackingRef 'cif_791260-791267_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 791265' _audit_creation_method SHELXL-97 _chemical_name_systematic ; carbonatobis(1,10-phenanthroline)cobalt(III) 3-nitrobenzoate.tetrahydrate ; _chemical_name_common ;carbonatobis(1,10-phenanthroline)cobalt(iii) 3- nitrobenzoate.tetrahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 Co N5 O11' _chemical_formula_weight 717.52 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3056(14) _cell_length_b 12.0933(14) _cell_length_c 12.9967(17) _cell_angle_alpha 79.683(5) _cell_angle_beta 87.857(5) _cell_angle_gamma 79.362(5) _cell_volume 1566.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2598 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 21.55 _exptl_crystal_description block _exptl_crystal_colour 'reddish pink' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.613 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEXII' _diffrn_measurement_method 'combination of \w and \f' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12053 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.1048 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5289 _reflns_number_gt 3319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 (Bruker, 2007)' _computing_data_reduction 'APEX2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _computing_publication_material SHELXL-97 _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^)+(0.0518P)^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 5289 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.31808(5) 0.48470(5) 0.28164(4) 0.0390(2) Uani 1 1 d . . . O1 O 0.3823(3) 0.4303(2) 0.41965(19) 0.0435(7) Uani 1 1 d . . . O2 O 0.4741(2) 0.3752(2) 0.28185(19) 0.0421(7) Uani 1 1 d . . . O3 O 0.5707(3) 0.3004(3) 0.4385(2) 0.0590(9) Uani 1 1 d . . . O4 O 0.6312(4) -0.0195(4) -0.1404(3) 0.0987(14) Uani 1 1 d . . . O5 O 0.7484(4) 0.0872(3) -0.2460(3) 0.0787(11) Uani 1 1 d . . . O6 O 1.0748(5) 0.2614(5) 0.0628(4) 0.145(2) Uani 1 1 d . . . O7 O 1.0526(5) 0.2803(5) -0.1002(4) 0.130(2) Uani 1 1 d . . . O8 O 0.4696(4) -0.0440(4) -0.2888(4) 0.1443(19) Uani 1 1 d . . . H8C H 0.5235 -0.0203 -0.3450 0.173 Uiso 1 1 d R . . H8B H 0.5174 -0.0346 -0.2374 0.173 Uiso 1 1 d R . . O9 O 0.6816(8) 0.0823(5) -0.4400(4) 0.260(4) Uani 1 1 d . . . H9B H 0.6500 0.1477 -0.4766 0.312 Uiso 1 1 d R . . H9C H 0.7104 0.0852 -0.3792 0.312 Uiso 1 1 d R . . O10 O 0.6369(10) 0.8800(7) 0.4801(8) 0.124(5) Uani 0.617(18) 1 d P . . O10A O 0.759(4) 0.941(3) 0.4060(15) 0.28(3) Uani 0.383(18) 1 d P . . O11 O 0.890(2) 0.9982(13) 0.4390(15) 0.216(9) Uani 0.452(9) 1 d P . . O11A O 0.7241(6) 1.1600(7) 0.3171(6) 0.101(3) Uani 0.548(9) 1 d P . . N1 N 0.4220(3) 0.6039(3) 0.2592(2) 0.0411(8) Uani 1 1 d . . . N2 N 0.2935(3) 0.5244(3) 0.1295(2) 0.0368(8) Uani 1 1 d . . . N3 N 0.1586(3) 0.5831(3) 0.3175(2) 0.0459(9) Uani 1 1 d . . . N4 N 0.2082(3) 0.3723(3) 0.2989(2) 0.0419(9) Uani 1 1 d . . . N5 N 1.0261(5) 0.2396(4) -0.0124(5) 0.0846(15) Uani 1 1 d . . . C1 C 0.4828(4) 0.3639(4) 0.3839(3) 0.0457(11) Uani 1 1 d . . . C2 C 0.4813(4) 0.6457(4) 0.3293(3) 0.0470(11) Uani 1 1 d . . . H2A H 0.4694 0.6194 0.4001 0.056 Uiso 1 1 calc R . . C3 C 0.5599(4) 0.7270(4) 0.2994(4) 0.0556(12) Uani 1 1 d . . . H3A H 0.5982 0.7558 0.3501 0.067 Uiso 1 1 calc R . . C4 C 0.5815(4) 0.7647(4) 0.1977(4) 0.0578(13) Uani 1 1 d . . . H4A H 0.6365 0.8179 0.1785 0.069 Uiso 1 1 calc R . . C5 C 0.5204(4) 0.7235(4) 0.1192(3) 0.0460(11) Uani 1 1 d . . . C6 C 0.4404(4) 0.6442(3) 0.1561(3) 0.0346(9) Uani 1 1 d . . . C7 C 0.3702(4) 0.6001(4) 0.0846(3) 0.0382(10) Uani 1 1 d . . . C8 C 0.3803(4) 0.6379(4) -0.0224(3) 0.0451(11) Uani 1 1 d . . . C9 C 0.4629(4) 0.7170(4) -0.0580(4) 0.0546(12) Uani 1 1 d . . . H9A H 0.4715 0.7416 -0.1296 0.066 Uiso 1 1 calc R . . C10 C 0.5309(4) 0.7587(4) 0.0096(4) 0.0589(13) Uani 1 1 d . . . H10A H 0.5850 0.8110 -0.0164 0.071 Uiso 1 1 calc R . . C11 C 0.3061(4) 0.5904(4) -0.0866(3) 0.0539(12) Uani 1 1 d . . . H11A H 0.3094 0.6113 -0.1589 0.065 Uiso 1 1 calc R . . C12 C 0.2300(4) 0.5141(4) -0.0424(3) 0.0582(13) Uani 1 1 d . . . H12A H 0.1806 0.4830 -0.0846 0.070 Uiso 1 1 calc R . . C13 C 0.2256(4) 0.4823(4) 0.0654(3) 0.0496(11) Uani 1 1 d . . . H13A H 0.1733 0.4294 0.0940 0.060 Uiso 1 1 calc R . . C14 C 0.1383(4) 0.6913(4) 0.3312(3) 0.0551(12) Uani 1 1 d . . . H14A H 0.2070 0.7320 0.3167 0.066 Uiso 1 1 calc R . . C15 C 0.0182(5) 0.7464(4) 0.3665(4) 0.0669(14) Uani 1 1 d . . . H15A H 0.0075 0.8224 0.3747 0.080 Uiso 1 1 calc R . . C16 C -0.0830(5) 0.6880(5) 0.3889(4) 0.0640(14) Uani 1 1 d . . . H16A H -0.1633 0.7242 0.4125 0.077 Uiso 1 1 calc R . . C17 C -0.0671(4) 0.5739(5) 0.3766(3) 0.0588(13) Uani 1 1 d . . . C18 C 0.0567(4) 0.5248(4) 0.3407(3) 0.0408(10) Uani 1 1 d . . . C19 C 0.0843(4) 0.4092(4) 0.3284(3) 0.0429(11) Uani 1 1 d . . . C20 C -0.0121(4) 0.3403(5) 0.3511(3) 0.0501(12) Uani 1 1 d . . . C21 C -0.1390(5) 0.3943(6) 0.3859(4) 0.0733(17) Uani 1 1 d . . . H21A H -0.2056 0.3512 0.4003 0.088 Uiso 1 1 calc R . . C22 C -0.1644(4) 0.5033(6) 0.3981(4) 0.0669(15) Uani 1 1 d . . . H22A H -0.2476 0.5339 0.4212 0.080 Uiso 1 1 calc R . . C23 C 0.0247(5) 0.2274(5) 0.3400(4) 0.0673(15) Uani 1 1 d . . . H23A H -0.0363 0.1787 0.3534 0.081 Uiso 1 1 calc R . . C24 C 0.1504(5) 0.1867(4) 0.3094(4) 0.0603(13) Uani 1 1 d . . . H24A H 0.1749 0.1104 0.3022 0.072 Uiso 1 1 calc R . . C25 C 0.2420(4) 0.2605(4) 0.2890(3) 0.0519(12) Uani 1 1 d . . . H25A H 0.3273 0.2325 0.2683 0.062 Uiso 1 1 calc R . . C26 C 0.7812(4) 0.0692(4) -0.0663(4) 0.0542(12) Uani 1 1 d . . . C27 C 0.8738(4) 0.1381(4) -0.0808(4) 0.0540(12) Uani 1 1 d . . . H27A H 0.8978 0.1688 -0.1480 0.065 Uiso 1 1 calc R . . C28 C 0.9316(5) 0.1618(4) 0.0051(4) 0.0584(13) Uani 1 1 d . . . C29 C 0.8999(6) 0.1180(5) 0.1045(4) 0.0825(17) Uani 1 1 d . . . H29A H 0.9393 0.1355 0.1613 0.099 Uiso 1 1 calc R . . C30 C 0.8089(6) 0.0476(6) 0.1192(4) 0.0873(18) Uani 1 1 d . . . H30A H 0.7878 0.0144 0.1864 0.105 Uiso 1 1 calc R . . C31 C 0.7485(5) 0.0259(5) 0.0341(5) 0.0798(16) Uani 1 1 d . . . H31A H 0.6837 -0.0193 0.0450 0.096 Uiso 1 1 calc R . . C32 C 0.7139(5) 0.0432(4) -0.1581(4) 0.0625(14) 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 0.0345(3) 0.0496(4) 0.0348(3) -0.0152(3) 0.0022(2) -0.0054(3) O1 0.0422(17) 0.0553(19) 0.0323(15) -0.0154(14) 0.0059(12) -0.0007(14) O2 0.0371(16) 0.0528(19) 0.0365(17) -0.0171(14) 0.0028(12) -0.0001(13) O3 0.0533(19) 0.068(2) 0.0488(19) -0.0110(16) -0.0100(15) 0.0087(17) O4 0.115(3) 0.094(3) 0.100(3) -0.001(2) -0.024(2) -0.062(3) O5 0.099(3) 0.073(3) 0.073(3) -0.014(2) -0.016(2) -0.033(2) O6 0.175(5) 0.161(5) 0.126(4) -0.019(3) -0.066(3) -0.093(4) O7 0.157(5) 0.149(5) 0.108(4) -0.004(3) -0.026(3) -0.103(4) O8 0.143(4) 0.148(5) 0.165(5) -0.043(4) -0.046(3) -0.061(4) O9 0.473(12) 0.127(5) 0.144(5) -0.065(4) -0.157(6) 0.108(6) O10 0.162(9) 0.126(7) 0.102(8) -0.054(5) -0.023(6) -0.038(6) O10A 0.39(5) 0.26(3) 0.132(17) -0.11(2) -0.05(2) 0.21(3) O11 0.35(2) 0.105(10) 0.211(19) -0.037(11) 0.043(15) -0.082(13) O11A 0.060(5) 0.120(7) 0.146(7) -0.079(5) 0.015(4) -0.022(4) N1 0.038(2) 0.051(2) 0.037(2) -0.0164(17) 0.0007(15) -0.0064(17) N2 0.0363(19) 0.043(2) 0.0338(19) -0.0170(16) -0.0024(15) -0.0033(16) N3 0.042(2) 0.048(2) 0.043(2) -0.0074(18) 0.0017(16) 0.0023(19) N4 0.0303(19) 0.066(3) 0.0245(18) -0.0066(17) -0.0003(14) 0.0034(18) N5 0.084(4) 0.082(4) 0.094(4) -0.020(3) -0.033(3) -0.020(3) C1 0.043(3) 0.063(3) 0.033(3) -0.008(2) -0.001(2) -0.016(2) C2 0.049(3) 0.055(3) 0.040(3) -0.017(2) -0.006(2) -0.007(2) C3 0.059(3) 0.055(3) 0.059(3) -0.021(3) -0.016(2) -0.012(3) C4 0.051(3) 0.047(3) 0.079(4) -0.010(3) -0.005(3) -0.017(2) C5 0.041(3) 0.045(3) 0.053(3) -0.013(2) 0.001(2) -0.006(2) C6 0.033(2) 0.035(2) 0.036(2) -0.0104(19) 0.0052(18) -0.0027(19) C7 0.030(2) 0.048(3) 0.037(2) -0.016(2) 0.0022(18) 0.001(2) C8 0.044(3) 0.050(3) 0.037(3) -0.007(2) 0.004(2) 0.003(2) C9 0.067(3) 0.050(3) 0.044(3) -0.011(2) 0.013(2) -0.003(3) C10 0.062(3) 0.055(3) 0.062(3) -0.007(3) 0.016(3) -0.022(3) C11 0.060(3) 0.066(3) 0.035(3) -0.015(2) 0.003(2) -0.004(3) C12 0.062(3) 0.076(4) 0.041(3) -0.024(3) -0.008(2) -0.011(3) C13 0.047(3) 0.060(3) 0.045(3) -0.014(2) -0.003(2) -0.012(2) C14 0.054(3) 0.054(3) 0.050(3) -0.011(2) -0.002(2) 0.008(2) C15 0.066(3) 0.059(3) 0.065(3) -0.017(3) -0.005(3) 0.022(3) C16 0.052(3) 0.075(4) 0.052(3) -0.014(3) -0.001(2) 0.024(3) C17 0.041(3) 0.084(4) 0.040(3) 0.000(3) 0.003(2) 0.006(3) C18 0.032(2) 0.054(3) 0.031(2) -0.009(2) -0.0004(18) 0.006(2) C19 0.039(2) 0.058(3) 0.031(2) -0.005(2) -0.0034(19) -0.009(2) C20 0.044(3) 0.070(4) 0.039(3) -0.010(2) -0.004(2) -0.017(3) C21 0.039(3) 0.126(6) 0.051(3) 0.000(3) 0.000(2) -0.023(3) C22 0.032(3) 0.105(5) 0.054(3) -0.008(3) 0.005(2) 0.008(3) C23 0.063(3) 0.096(5) 0.055(3) -0.015(3) -0.007(3) -0.040(3) C24 0.066(3) 0.062(3) 0.058(3) -0.014(3) -0.005(3) -0.019(3) C25 0.048(3) 0.059(3) 0.049(3) -0.016(2) 0.003(2) -0.008(3) C26 0.057(3) 0.043(3) 0.063(3) -0.012(2) -0.005(2) -0.007(2) C27 0.060(3) 0.045(3) 0.055(3) -0.008(2) -0.010(2) -0.001(2) C28 0.058(3) 0.056(3) 0.062(3) -0.012(3) -0.014(3) -0.009(3) C29 0.083(4) 0.102(5) 0.064(4) -0.024(4) -0.017(3) -0.009(4) C30 0.102(5) 0.104(5) 0.061(4) -0.020(3) 0.000(3) -0.026(4) C31 0.079(4) 0.084(4) 0.079(4) -0.012(3) 0.003(3) -0.027(3) C32 0.077(4) 0.043(3) 0.068(4) -0.010(3) -0.003(3) -0.011(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 O2 1.885(3) . ? Co1 O1 1.896(3) . ? Co1 N4 1.902(4) . ? Co1 N1 1.925(3) . ? Co1 N3 1.938(3) . ? Co1 N2 1.964(3) . ? O1 C1 1.312(5) . ? O2 C1 1.314(4) . ? O3 C1 1.229(5) . ? O4 C32 1.231(6) . ? O5 C32 1.240(5) . ? O6 N5 1.205(6) . ? O7 N5 1.202(6) . ? O8 H8C 0.9367 . ? O8 H8B 0.8808 . ? O9 H9B 0.8600 . ? O9 H9C 0.8634 . ? O10 O10A 1.75(4) . ? O10A O11 1.72(4) . ? N1 C2 1.334(5) . ? N1 C6 1.360(4) . ? N2 C13 1.330(5) . ? N2 C7 1.358(5) . ? N3 C14 1.330(5) . ? N3 C18 1.365(5) . ? N4 C19 1.339(5) . ? N4 C25 1.361(5) . ? N5 C28 1.459(6) . ? C2 C3 1.381(6) . ? C2 H2A 0.9300 . ? C3 C4 1.343(6) . ? C3 H3A 0.9300 . ? C4 C5 1.425(6) . ? C4 H4A 0.9300 . ? C5 C6 1.389(5) . ? C5 C10 1.417(6) . ? C6 C7 1.428(5) . ? C7 C8 1.391(5) . ? C8 C9 1.402(6) . ? C8 C11 1.412(6) . ? C9 C10 1.361(6) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.357(6) . ? C11 H11A 0.9300 . ? C12 C13 1.386(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.396(6) . ? C14 H14A 0.9300 . ? C15 C16 1.359(7) . ? C15 H15A 0.9300 . ? C16 C17 1.397(7) . ? C16 H16A 0.9300 . ? C17 C18 1.404(5) . ? C17 C22 1.422(7) . ? C18 C19 1.411(6) . ? C19 C20 1.400(6) . ? C20 C23 1.380(6) . ? C20 C21 1.445(7) . ? C21 C22 1.333(7) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.369(6) . ? C23 H23A 0.9300 . ? C24 C25 1.402(6) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.366(6) . ? C26 C31 1.370(6) . ? C26 C32 1.509(7) . ? C27 C28 1.382(6) . ? C27 H27A 0.9300 . ? C28 C29 1.357(6) . ? C29 C30 1.364(7) . ? C29 H29A 0.9300 . ? C30 C31 1.377(7) . ? C30 H30A 0.9300 . ? C31 H31A 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 O2 Co1 O1 69.26(11) . . ? O2 Co1 N4 92.99(13) . . ? O1 Co1 N4 90.25(12) . . ? O2 Co1 N1 89.53(12) . . ? O1 Co1 N1 92.41(13) . . ? N4 Co1 N1 176.86(14) . . ? O2 Co1 N3 166.08(12) . . ? O1 Co1 N3 97.20(12) . . ? N4 Co1 N3 83.56(15) . . ? N1 Co1 N3 94.43(15) . . ? O2 Co1 N2 97.67(12) . . ? O1 Co1 N2 166.46(12) . . ? N4 Co1 N2 94.06(13) . . ? N1 Co1 N2 83.73(13) . . ? N3 Co1 N2 96.03(13) . . ? C1 O1 Co1 90.3(2) . . ? C1 O2 Co1 90.7(2) . . ? H8C O8 H8B 98.6 . . ? H9B O9 H9C 114.6 . . ? O11 O10A O10 132.8(12) . . ? C2 N1 C6 118.0(4) . . ? C2 N1 Co1 129.1(3) . . ? C6 N1 Co1 112.8(2) . . ? C13 N2 C7 117.0(3) . . ? C13 N2 Co1 130.9(3) . . ? C7 N2 Co1 111.8(2) . . ? C14 N3 C18 117.4(4) . . ? C14 N3 Co1 130.5(3) . . ? C18 N3 Co1 111.7(3) . . ? C19 N4 C25 117.5(4) . . ? C19 N4 Co1 114.4(3) . . ? C25 N4 Co1 128.1(3) . . ? O7 N5 O6 122.0(6) . . ? O7 N5 C28 119.7(5) . . ? O6 N5 C28 118.3(6) . . ? O3 C1 O1 124.7(4) . . ? O3 C1 O2 125.5(4) . . ? O1 C1 O2 109.8(4) . . ? N1 C2 C3 121.7(4) . . ? N1 C2 H2A 119.1 . . ? C3 C2 H2A 119.1 . . ? C4 C3 C2 120.5(4) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 120.3(4) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C10 118.4(4) . . ? C6 C5 C4 115.3(4) . . ? C10 C5 C4 126.2(4) . . ? N1 C6 C5 124.1(4) . . ? N1 C6 C7 115.6(3) . . ? C5 C6 C7 120.3(4) . . ? N2 C7 C8 124.8(4) . . ? N2 C7 C6 115.2(3) . . ? C8 C7 C6 120.0(4) . . ? C7 C8 C9 118.8(4) . . ? C7 C8 C11 115.8(4) . . ? C9 C8 C11 125.5(4) . . ? C10 C9 C8 121.5(4) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C9 C10 C5 121.0(4) . . ? C9 C10 H10A 119.5 . . ? C5 C10 H10A 119.5 . . ? C12 C11 C8 119.8(4) . . ? C12 C11 H11A 120.1 . . ? C8 C11 H11A 120.1 . . ? C11 C12 C13 120.1(4) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? N2 C13 C12 122.5(4) . . ? N2 C13 H13A 118.7 . . ? C12 C13 H13A 118.7 . . ? N3 C14 C15 122.8(5) . . ? N3 C14 H14A 118.6 . . ? C15 C14 H14A 118.6 . . ? C16 C15 C14 119.5(5) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C15 C16 C17 120.3(4) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C16 C17 C18 116.7(5) . . ? C16 C17 C22 125.8(5) . . ? C18 C17 C22 117.5(5) . . ? N3 C18 C17 123.3(4) . . ? N3 C18 C19 115.4(4) . . ? C17 C18 C19 121.3(4) . . ? N4 C19 C20 124.6(4) . . ? N4 C19 C18 114.8(4) . . ? C20 C19 C18 120.6(4) . . ? C23 C20 C19 116.7(4) . . ? C23 C20 C21 126.7(5) . . ? C19 C20 C21 116.6(5) . . ? C22 C21 C20 122.6(5) . . ? C22 C21 H21A 118.7 . . ? C20 C21 H21A 118.7 . . ? C21 C22 C17 121.4(5) . . ? C21 C22 H22A 119.3 . . ? C17 C22 H22A 119.3 . . ? C24 C23 C20 120.5(4) . . ? C24 C23 H23A 119.8 . . ? C20 C23 H23A 119.8 . . ? C23 C24 C25 119.6(5) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? N4 C25 C24 121.1(4) . . ? N4 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C27 C26 C31 118.2(5) . . ? C27 C26 C32 121.2(5) . . ? C31 C26 C32 120.6(5) . . ? C26 C27 C28 119.6(5) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C29 C28 C27 122.0(5) . . ? C29 C28 N5 119.4(5) . . ? C27 C28 N5 118.5(5) . . ? C28 C29 C30 118.5(5) . . ? C28 C29 H29A 120.7 . . ? C30 C29 H29A 120.7 . . ? C29 C30 C31 119.8(6) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C26 C31 C30 121.8(5) . . ? C26 C31 H31A 119.1 . . ? C30 C31 H31A 119.1 . . ? O4 C32 O5 125.5(5) . . ? O4 C32 C26 118.3(5) . . ? O5 C32 C26 116.1(5) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.854 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.067 data_8conapac _database_code_depnum_ccdc_archive 'CCDC 791266' #TrackingRef 'cif_791260-791267_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 791266' _audit_creation_method SHELXL-97 _chemical_name_systematic ; carbonatobis(1,10-phenanthroline)cobalt(III) 2-napthaleneacetate.heptahydrate ; _chemical_name_common ;carbonatobis(1,10-phenanthroline)cobalt(iii) 2- napthaleneacetate.heptahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H39 Co N4 O12' _chemical_formula_weight 790.65 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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' _cell_length_a 16.3601(3) _cell_length_b 16.1545(3) _cell_length_c 14.0117(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.0270(10) _cell_angle_gamma 90.00 _cell_volume 3607.84(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5195 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 24.10 _exptl_crystal_description block _exptl_crystal_colour 'reddish pink' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.605 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEXII' _diffrn_measurement_method 'combination of \w and \f' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24792 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7081 _reflns_number_gt 5091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 (Bruker, 2007)' _computing_data_reduction 'APEX2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _computing_publication_material SHELXL-97 _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^)+(0.0429P)^2^+0.3404P] 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 7081 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Co1 Co 0.119169(17) 0.172276(17) 0.690634(18) 0.02701(9) Uani 1 1 d . . . O1 O 0.02608(9) 0.13064(9) 0.73494(9) 0.0327(3) Uani 1 1 d . . . O2 O 0.13081(9) 0.19551(9) 0.82543(9) 0.0348(4) Uani 1 1 d . . . O3 O 0.02786(10) 0.14899(10) 0.89536(11) 0.0457(4) Uani 1 1 d . . . O4 O 0.56334(16) -0.02304(15) 0.21117(15) 0.0952(8) Uani 1 1 d . . . O5 O 0.46217(15) -0.10737(15) 0.21834(13) 0.0820(7) Uani 1 1 d . . . O6 O 0.61662(12) 0.09369(12) 0.96831(12) 0.0644(5) Uani 1 1 d . . . H6B H 0.6165 0.0441 0.9690 0.077 Uiso 1 1 d R . . H6C H 0.5861 0.0967 0.9097 0.077 Uiso 1 1 d R . . O7 O 0.54361(13) 0.13612(15) 1.12597(16) 0.0851(7) Uani 1 1 d . . . H7B H 0.5694 0.1258 1.0831 0.102 Uiso 1 1 d R . . H7C H 0.5538 0.0919 1.1545 0.102 Uiso 1 1 d R . . O8 O -0.13811(13) 0.20591(15) 0.85159(15) 0.0880(7) Uani 1 1 d . . . H8B H -0.0917 0.1789 0.8605 0.106 Uiso 1 1 d R . . H8C H -0.1483 0.2110 0.7903 0.106 Uiso 1 1 d R . . O9 O 0.21834(13) -0.21703(14) 0.34575(14) 0.0819(6) Uani 1 1 d . . . H9B H 0.2648 -0.1959 0.3516 0.098 Uiso 1 1 d R . . H9C H 0.2294 -0.2465 0.3973 0.098 Uiso 1 1 d R . . O10 O 0.36556(15) -0.22218(16) 0.28710(19) 0.1048(8) Uani 1 1 d . . . H10B H 0.3956 -0.1894 0.2647 0.126 Uiso 1 1 d R . . H10C H 0.4024 -0.2482 0.3248 0.126 Uiso 1 1 d R . . O11 O 0.59935(12) -0.06800(12) 0.03810(13) 0.0659(5) Uani 1 1 d . . . H11B H 0.5848 -0.0573 0.0937 0.079 Uiso 1 1 d R . . H11C H 0.5685 -0.0977 0.0008 0.079 Uiso 1 1 d R . . O12 O 0.77035(12) 0.17768(13) 0.99317(14) 0.0742(6) Uani 1 1 d . . . H12B H 0.7253 0.1566 0.9703 0.089 Uiso 1 1 d R . . H12C H 0.7828 0.1830 0.9400 0.089 Uiso 1 1 d R . . N1 N 0.17478(10) 0.06676(10) 0.71920(11) 0.0301(4) Uani 1 1 d . . . N2 N 0.08831(10) 0.12987(10) 0.55692(11) 0.0278(4) Uani 1 1 d . . . N3 N 0.06515(10) 0.27779(11) 0.65546(11) 0.0293(4) Uani 1 1 d . . . N4 N 0.21974(11) 0.22949(11) 0.67243(11) 0.0316(4) Uani 1 1 d . . . C1 C -0.01498(14) 0.29801(14) 0.64489(15) 0.0357(5) Uani 1 1 d . . . H1A H -0.0533 0.2574 0.6526 0.043 Uiso 1 1 calc R . . C2 C -0.04295(15) 0.37855(15) 0.62256(16) 0.0423(6) Uani 1 1 d . . . H2A H -0.0995 0.3911 0.6153 0.051 Uiso 1 1 calc R . . C3 C 0.01213(16) 0.43921(15) 0.61130(15) 0.0444(6) Uani 1 1 d . . . H3A H -0.0064 0.4933 0.5980 0.053 Uiso 1 1 calc R . . C4 C 0.09690(15) 0.41940(14) 0.61996(15) 0.0387(6) Uani 1 1 d . . . C5 C 0.12030(14) 0.33727(13) 0.64180(14) 0.0314(5) Uani 1 1 d . . . C6 C 0.16091(19) 0.47614(16) 0.60733(18) 0.0560(7) Uani 1 1 d . . . H6A H 0.1472 0.5313 0.5930 0.067 Uiso 1 1 calc R . . C7 C 0.24059(19) 0.45091(17) 0.6159(2) 0.0595(8) Uani 1 1 d . . . H7A H 0.2806 0.4893 0.6070 0.071 Uiso 1 1 calc R . . C8 C 0.26595(15) 0.36702(16) 0.63829(16) 0.0436(6) Uani 1 1 d . . . C9 C 0.20384(14) 0.31081(14) 0.65057(14) 0.0334(5) Uani 1 1 d . . . C10 C 0.34726(17) 0.33612(19) 0.65120(18) 0.0550(7) Uani 1 1 d . . . H10A H 0.3908 0.3712 0.6450 0.066 Uiso 1 1 calc R . . C11 C 0.36301(15) 0.25512(18) 0.67268(18) 0.0522(7) Uani 1 1 d . . . H11A H 0.4172 0.2345 0.6805 0.063 Uiso 1 1 calc R . . C12 C 0.29797(14) 0.20272(16) 0.68299(16) 0.0424(6) Uani 1 1 d . . . H12A H 0.3097 0.1472 0.6977 0.051 Uiso 1 1 calc R . . C13 C 0.21695(14) 0.03706(15) 0.80438(16) 0.0402(6) Uani 1 1 d . . . H13A H 0.2247 0.0703 0.8599 0.048 Uiso 1 1 calc R . . C14 C 0.24992(15) -0.04306(16) 0.81242(18) 0.0478(6) Uani 1 1 d . . . H14A H 0.2786 -0.0627 0.8732 0.057 Uiso 1 1 calc R . . C15 C 0.24032(14) -0.09293(16) 0.73177(18) 0.0466(6) Uani 1 1 d . . . H15A H 0.2630 -0.1460 0.7373 0.056 Uiso 1 1 calc R . . C16 C 0.19590(13) -0.06331(14) 0.64062(17) 0.0365(5) Uani 1 1 d . . . C17 C 0.16388(12) 0.01683(13) 0.63887(15) 0.0301(5) Uani 1 1 d . . . C18 C 0.18011(15) -0.10876(15) 0.55054(19) 0.0465(6) Uani 1 1 d . . . H18A H 0.2021 -0.1618 0.5497 0.056 Uiso 1 1 calc R . . C19 C 0.13404(15) -0.07629(15) 0.46700(18) 0.0433(6) Uani 1 1 d . . . H19A H 0.1247 -0.1076 0.4098 0.052 Uiso 1 1 calc R . . C20 C 0.09930(13) 0.00465(14) 0.46404(15) 0.0340(5) Uani 1 1 d . . . C21 C 0.11678(12) 0.05159(12) 0.55068(14) 0.0275(4) Uani 1 1 d . . . C22 C 0.04928(14) 0.04240(15) 0.38128(15) 0.0400(6) Uani 1 1 d . . . H22A H 0.0352 0.0139 0.3221 0.048 Uiso 1 1 calc R . . C23 C 0.02137(15) 0.12101(15) 0.38797(15) 0.0408(6) Uani 1 1 d . . . H23A H -0.0120 0.1462 0.3332 0.049 Uiso 1 1 calc R . . C24 C 0.04234(14) 0.16402(14) 0.47626(14) 0.0348(5) Uani 1 1 d . . . H24A H 0.0236 0.2182 0.4788 0.042 Uiso 1 1 calc R . . C25 C 0.05954(14) 0.15796(13) 0.82433(15) 0.0330(5) Uani 1 1 d . . . C26 C 0.51726(17) -0.05814(16) 0.25644(17) 0.0476(6) Uani 1 1 d . . . C27 C 0.53059(16) -0.04160(16) 0.36513(16) 0.0495(6) Uani 1 1 d . . . H27A H 0.4947 -0.0782 0.3924 0.059 Uiso 1 1 calc R . . H27B H 0.5883 -0.0542 0.3967 0.059 Uiso 1 1 calc R . . C28 C 0.51189(15) 0.04668(16) 0.38718(15) 0.0420(6) Uani 1 1 d . . . C29 C 0.57519(18) 0.1038(2) 0.4072(2) 0.0625(8) Uani 1 1 d . . . H29A H 0.6297 0.0870 0.4080 0.075 Uiso 1 1 calc R . . C30 C 0.5603(2) 0.1865(2) 0.4265(2) 0.0771(10) Uani 1 1 d . . . H30A H 0.6046 0.2238 0.4392 0.092 Uiso 1 1 calc R . . C31 C 0.4821(2) 0.2127(2) 0.4269(2) 0.0713(9) Uani 1 1 d . . . H31A H 0.4730 0.2680 0.4395 0.086 Uiso 1 1 calc R . . C32 C 0.41452(17) 0.15742(17) 0.40846(17) 0.0496(7) Uani 1 1 d . . . C33 C 0.3320(2) 0.1832(2) 0.40967(19) 0.0658(9) Uani 1 1 d . . . H33A H 0.3224 0.2382 0.4232 0.079 Uiso 1 1 calc R . . C34 C 0.2671(2) 0.1296(3) 0.3915(2) 0.0763(10) Uani 1 1 d . . . H34A H 0.2134 0.1474 0.3931 0.092 Uiso 1 1 calc R . . C35 C 0.28141(19) 0.0474(2) 0.3704(2) 0.0683(9) Uani 1 1 d . . . H35A H 0.2365 0.0106 0.3575 0.082 Uiso 1 1 calc R . . C36 C 0.35918(16) 0.01955(17) 0.36821(17) 0.0510(6) Uani 1 1 d . . . H36A H 0.3667 -0.0358 0.3540 0.061 Uiso 1 1 calc R . . C37 C 0.42882(15) 0.07348(15) 0.38719(15) 0.0393(6) 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 0.02945(16) 0.02472(16) 0.02701(14) -0.00033(12) 0.00667(11) 0.00036(12) O1 0.0344(8) 0.0311(9) 0.0331(7) -0.0012(6) 0.0087(6) -0.0059(6) O2 0.0398(9) 0.0353(9) 0.0288(7) -0.0056(6) 0.0069(6) -0.0069(7) O3 0.0593(11) 0.0455(11) 0.0385(9) -0.0001(7) 0.0244(8) -0.0040(8) O4 0.133(2) 0.105(2) 0.0680(13) -0.0253(12) 0.0645(14) -0.0513(16) O5 0.1067(18) 0.0933(18) 0.0458(11) -0.0040(11) 0.0168(11) -0.0438(15) O6 0.0720(14) 0.0632(14) 0.0532(11) -0.0006(9) 0.0039(9) -0.0068(10) O7 0.0725(15) 0.0974(18) 0.0950(16) 0.0194(13) 0.0393(12) 0.0236(13) O8 0.0710(15) 0.121(2) 0.0770(14) -0.0087(13) 0.0273(11) 0.0182(14) O9 0.0803(15) 0.0955(18) 0.0716(13) 0.0011(12) 0.0203(11) 0.0256(13) O10 0.0866(18) 0.098(2) 0.145(2) 0.0181(16) 0.0584(16) -0.0126(14) O11 0.0692(13) 0.0765(15) 0.0563(11) -0.0133(10) 0.0232(10) -0.0115(10) O12 0.0664(14) 0.0875(17) 0.0699(13) -0.0019(11) 0.0178(10) -0.0099(11) N1 0.0300(10) 0.0278(10) 0.0311(9) 0.0020(7) 0.0040(7) 0.0007(7) N2 0.0305(10) 0.0259(10) 0.0277(8) 0.0020(7) 0.0083(7) 0.0014(7) N3 0.0330(10) 0.0260(10) 0.0292(9) -0.0033(7) 0.0078(7) 0.0009(8) N4 0.0323(10) 0.0317(11) 0.0311(9) 0.0008(8) 0.0076(7) 0.0001(8) C1 0.0366(13) 0.0360(13) 0.0357(11) -0.0028(10) 0.0109(10) 0.0032(10) C2 0.0440(15) 0.0443(16) 0.0382(12) -0.0006(11) 0.0085(10) 0.0134(12) C3 0.0663(18) 0.0313(14) 0.0350(12) 0.0019(10) 0.0099(12) 0.0156(12) C4 0.0541(16) 0.0276(13) 0.0329(11) 0.0038(9) 0.0068(10) -0.0002(11) C5 0.0415(13) 0.0272(12) 0.0262(10) -0.0005(9) 0.0089(9) -0.0021(10) C6 0.079(2) 0.0311(15) 0.0577(16) 0.0122(12) 0.0143(14) -0.0068(13) C7 0.065(2) 0.0472(18) 0.0685(18) 0.0156(14) 0.0195(15) -0.0210(14) C8 0.0471(16) 0.0450(16) 0.0415(13) 0.0059(11) 0.0155(11) -0.0106(12) C9 0.0370(13) 0.0354(14) 0.0287(10) 0.0020(9) 0.0095(9) -0.0045(10) C10 0.0443(16) 0.070(2) 0.0537(15) 0.0049(14) 0.0171(12) -0.0217(14) C11 0.0317(14) 0.071(2) 0.0567(15) 0.0014(14) 0.0151(12) -0.0017(13) C12 0.0346(14) 0.0455(15) 0.0482(13) 0.0009(11) 0.0120(11) 0.0025(11) C13 0.0370(13) 0.0449(15) 0.0354(12) 0.0053(10) 0.0011(10) 0.0003(11) C14 0.0402(15) 0.0475(16) 0.0508(14) 0.0208(12) -0.0003(11) 0.0060(12) C15 0.0368(14) 0.0330(14) 0.0685(17) 0.0127(12) 0.0089(12) 0.0059(10) C16 0.0275(12) 0.0290(13) 0.0538(14) 0.0036(10) 0.0109(10) 0.0023(9) C17 0.0257(12) 0.0286(13) 0.0380(11) 0.0016(9) 0.0114(9) -0.0005(9) C18 0.0461(15) 0.0254(13) 0.0727(17) -0.0072(12) 0.0235(13) 0.0031(11) C19 0.0507(15) 0.0328(14) 0.0504(14) -0.0131(11) 0.0197(12) -0.0048(11) C20 0.0359(13) 0.0334(13) 0.0374(11) -0.0068(10) 0.0181(10) -0.0087(10) C21 0.0273(11) 0.0248(12) 0.0317(10) 0.0001(9) 0.0099(9) -0.0013(9) C22 0.0478(15) 0.0473(16) 0.0273(11) -0.0069(10) 0.0133(10) -0.0120(11) C23 0.0472(15) 0.0459(16) 0.0287(11) 0.0050(10) 0.0071(10) -0.0001(11) C24 0.0412(13) 0.0312(13) 0.0321(11) 0.0057(9) 0.0083(9) 0.0039(10) C25 0.0413(14) 0.0247(12) 0.0333(11) -0.0004(9) 0.0086(10) 0.0008(10) C26 0.0583(18) 0.0450(16) 0.0440(14) 0.0029(12) 0.0212(13) 0.0031(13) C27 0.0501(16) 0.0589(18) 0.0402(13) 0.0022(12) 0.0117(11) 0.0109(13) C28 0.0461(15) 0.0501(16) 0.0313(11) -0.0011(10) 0.0120(10) 0.0011(12) C29 0.0482(17) 0.078(2) 0.0630(17) -0.0084(16) 0.0160(14) -0.0108(15) C30 0.080(2) 0.067(2) 0.084(2) -0.0135(17) 0.0160(18) -0.0307(18) C31 0.096(3) 0.048(2) 0.069(2) -0.0099(15) 0.0156(18) -0.0042(18) C32 0.0658(19) 0.0465(17) 0.0373(12) 0.0022(11) 0.0135(12) 0.0062(13) C33 0.087(2) 0.064(2) 0.0499(16) 0.0077(14) 0.0240(16) 0.0332(18) C34 0.059(2) 0.110(3) 0.0663(19) 0.0137(19) 0.0265(16) 0.027(2) C35 0.0479(18) 0.094(3) 0.0663(19) 0.0067(17) 0.0201(14) -0.0052(17) C36 0.0514(17) 0.0547(18) 0.0485(14) 0.0030(12) 0.0147(12) -0.0022(13) C37 0.0466(15) 0.0437(15) 0.0287(11) 0.0024(10) 0.0108(10) -0.0008(11) _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 O2 1.8927(13) . ? Co1 O1 1.8930(14) . ? Co1 N1 1.9311(17) . ? Co1 N3 1.9320(17) . ? Co1 N2 1.9514(16) . ? Co1 N4 1.9534(17) . ? Co1 C25 2.310(2) . ? O1 C25 1.324(2) . ? O2 C25 1.311(3) . ? O3 C25 1.230(2) . ? O4 C26 1.228(3) . ? O5 C26 1.230(3) . ? O6 H6B 0.8012 . ? O6 H6C 0.8613 . ? O7 H7B 0.8255 . ? O7 H7C 0.8164 . ? O8 H8B 0.8599 . ? O8 H8C 0.8414 . ? O9 H9B 0.8202 . ? O9 H9C 0.8498 . ? O10 H10B 0.8301 . ? O10 H10C 0.8221 . ? O11 H11B 0.8819 . ? O11 H11C 0.8000 . ? O12 H12B 0.8099 . ? O12 H12C 0.8200 . ? N1 C13 1.327(3) . ? N1 C17 1.363(3) . ? N2 C24 1.328(2) . ? N2 C21 1.357(3) . ? N3 C1 1.327(3) . ? N3 C5 1.361(3) . ? N4 C12 1.327(3) . ? N4 C9 1.361(3) . ? C1 C2 1.391(3) . ? C1 H1A 0.9300 . ? C2 C3 1.364(3) . ? C2 H2A 0.9300 . ? C3 C4 1.402(3) . ? C3 H3A 0.9300 . ? C4 C5 1.396(3) . ? C4 C6 1.432(3) . ? C5 C9 1.411(3) . ? C6 C7 1.345(4) . ? C6 H6A 0.9300 . ? C7 C8 1.431(4) . ? C7 H7A 0.9300 . ? C8 C10 1.394(4) . ? C8 C9 1.402(3) . ? C10 C11 1.354(4) . ? C10 H10A 0.9300 . ? C11 C12 1.393(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.397(3) . ? C13 H13A 0.9300 . ? C14 C15 1.368(3) . ? C14 H14A 0.9300 . ? C15 C16 1.404(3) . ? C15 H15A 0.9300 . ? C16 C17 1.395(3) . ? C16 C18 1.432(3) . ? C17 C21 1.417(3) . ? C18 C19 1.347(3) . ? C18 H18A 0.9300 . ? C19 C20 1.423(3) . ? C19 H19A 0.9300 . ? C20 C22 1.399(3) . ? C20 C21 1.405(3) . ? C22 C23 1.360(3) . ? C22 H22A 0.9300 . ? C23 C24 1.393(3) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C26 C27 1.513(3) . ? C27 C28 1.505(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.368(4) . ? C28 C37 1.426(3) . ? C29 C30 1.395(4) . ? C29 H29A 0.9300 . ? C30 C31 1.349(4) . ? C30 H30A 0.9300 . ? C31 C32 1.399(4) . ? C31 H31A 0.9300 . ? C32 C33 1.417(4) . ? C32 C37 1.419(3) . ? C33 C34 1.349(4) . ? C33 H33A 0.9300 . ? C34 C35 1.392(4) . ? C34 H34A 0.9300 . ? C35 C36 1.356(4) . ? C35 H35A 0.9300 . ? C36 C37 1.411(3) . ? C36 H36A 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 O2 Co1 O1 69.55(6) . . ? O2 Co1 N1 91.81(6) . . ? O1 Co1 N1 89.69(7) . . ? O2 Co1 N3 90.97(6) . . ? O1 Co1 N3 92.38(7) . . ? N1 Co1 N3 176.98(7) . . ? O2 Co1 N2 166.85(7) . . ? O1 Co1 N2 97.87(6) . . ? N1 Co1 N2 84.09(7) . . ? N3 Co1 N2 93.46(7) . . ? O2 Co1 N4 97.94(6) . . ? O1 Co1 N4 167.04(6) . . ? N1 Co1 N4 94.21(7) . . ? N3 Co1 N4 84.23(7) . . ? N2 Co1 N4 94.82(7) . . ? O2 Co1 C25 34.58(7) . . ? O1 Co1 C25 34.98(6) . . ? N1 Co1 C25 90.51(7) . . ? N3 Co1 C25 92.45(7) . . ? N2 Co1 C25 132.70(7) . . ? N4 Co1 C25 132.47(7) . . ? C25 O1 Co1 90.01(12) . . ? C25 O2 Co1 90.42(11) . . ? H6B O6 H6C 93.8 . . ? H7B O7 H7C 95.7 . . ? H8B O8 H8C 99.4 . . ? H9B O9 H9C 97.6 . . ? H10B O10 H10C 99.2 . . ? H11B O11 H11C 116.0 . . ? H12B O12 H12C 94.3 . . ? C13 N1 C17 118.26(19) . . ? C13 N1 Co1 129.12(16) . . ? C17 N1 Co1 112.54(13) . . ? C24 N2 C21 117.96(17) . . ? C24 N2 Co1 130.21(15) . . ? C21 N2 Co1 111.75(12) . . ? C1 N3 C5 118.71(19) . . ? C1 N3 Co1 129.01(15) . . ? C5 N3 Co1 112.28(14) . . ? C12 N4 C9 118.05(19) . . ? C12 N4 Co1 130.59(16) . . ? C9 N4 Co1 111.25(14) . . ? N3 C1 C2 121.5(2) . . ? N3 C1 H1A 119.3 . . ? C2 C1 H1A 119.3 . . ? C3 C2 C1 120.4(2) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 117.0(2) . . ? C5 C4 C6 117.6(2) . . ? C3 C4 C6 125.4(2) . . ? N3 C5 C4 123.0(2) . . ? N3 C5 C9 115.71(19) . . ? C4 C5 C9 121.3(2) . . ? C7 C6 C4 121.1(2) . . ? C7 C6 H6A 119.5 . . ? C4 C6 H6A 119.5 . . ? C6 C7 C8 122.3(2) . . ? C6 C7 H7A 118.9 . . ? C8 C7 H7A 118.9 . . ? C10 C8 C9 116.7(2) . . ? C10 C8 C7 126.1(2) . . ? C9 C8 C7 117.2(2) . . ? N4 C9 C8 123.1(2) . . ? N4 C9 C5 116.38(18) . . ? C8 C9 C5 120.5(2) . . ? C11 C10 C8 120.2(2) . . ? C11 C10 H10A 119.9 . . ? C8 C10 H10A 119.9 . . ? C10 C11 C12 119.9(2) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? N4 C12 C11 122.0(2) . . ? N4 C12 H12A 119.0 . . ? C11 C12 H12A 119.0 . . ? N1 C13 C14 121.4(2) . . ? N1 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C15 C14 C13 120.6(2) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 119.4(2) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C17 C16 C15 116.6(2) . . ? C17 C16 C18 117.9(2) . . ? C15 C16 C18 125.5(2) . . ? N1 C17 C16 123.78(19) . . ? N1 C17 C21 115.46(18) . . ? C16 C17 C21 120.76(19) . . ? C19 C18 C16 121.4(2) . . ? C19 C18 H18A 119.3 . . ? C16 C18 H18A 119.3 . . ? C18 C19 C20 121.7(2) . . ? C18 C19 H19A 119.2 . . ? C20 C19 H19A 119.2 . . ? C22 C20 C21 116.6(2) . . ? C22 C20 C19 125.4(2) . . ? C21 C20 C19 117.9(2) . . ? N2 C21 C20 123.54(18) . . ? N2 C21 C17 116.12(17) . . ? C20 C21 C17 120.3(2) . . ? C23 C22 C20 119.5(2) . . ? C23 C22 H22A 120.2 . . ? C20 C22 H22A 120.2 . . ? C22 C23 C24 120.5(2) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? N2 C24 C23 121.8(2) . . ? N2 C24 H24A 119.1 . . ? C23 C24 H24A 119.1 . . ? O3 C25 O2 125.50(19) . . ? O3 C25 O1 124.5(2) . . ? O2 C25 O1 110.01(17) . . ? O3 C25 Co1 178.98(17) . . ? O2 C25 Co1 55.00(9) . . ? O1 C25 Co1 55.02(10) . . ? O4 C26 O5 123.3(2) . . ? O4 C26 C27 118.2(3) . . ? O5 C26 C27 118.5(2) . . ? C28 C27 C26 112.6(2) . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C29 C28 C37 118.2(2) . . ? C29 C28 C27 120.1(2) . . ? C37 C28 C27 121.7(2) . . ? C28 C29 C30 121.9(3) . . ? C28 C29 H29A 119.1 . . ? C30 C29 H29A 119.1 . . ? C31 C30 C29 120.6(3) . . ? C31 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C30 C31 C32 120.6(3) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C31 C32 C33 121.7(3) . . ? C31 C32 C37 119.2(3) . . ? C33 C32 C37 119.1(3) . . ? C34 C33 C32 121.4(3) . . ? C34 C33 H33A 119.3 . . ? C32 C33 H33A 119.3 . . ? C33 C34 C35 119.3(3) . . ? C33 C34 H34A 120.3 . . ? C35 C34 H34A 120.3 . . ? C36 C35 C34 121.6(3) . . ? C36 C35 H35A 119.2 . . ? C34 C35 H35A 119.2 . . ? C35 C36 C37 120.9(3) . . ? C35 C36 H36A 119.6 . . ? C37 C36 H36A 119.6 . . ? C36 C37 C32 117.7(2) . . ? C36 C37 C28 122.8(2) . . ? C32 C37 C28 119.5(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.387 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.049 # ===== END ===== # data_5cocbz _database_code_depnum_ccdc_archive 'CCDC 791267' #TrackingRef 'cif_791260-791267_rev.cif' _database_code_depnum_ccdc_archive 'CCDC 791267' _audit_creation_method SHELXL-97 _chemical_name_systematic ; carbonatobis(1,10-phenanthroline)cobalt(III) 2-chlorobenzoate.heptahydrate ; _chemical_name_common ;carbonatobis(1,10-phenanthroline)cobalt(iii) 2- chlorobenzoate.heptahydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 Cl Co N4 O12' _chemical_formula_weight 761.01 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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' _cell_length_a 13.2762(3) _cell_length_b 19.9687(5) _cell_length_c 14.0664(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.8510(10) _cell_angle_gamma 90.00 _cell_volume 3355.95(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8871 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 24.30 _exptl_crystal_description block _exptl_crystal_colour 'reddish pink' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.575 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEXII' _diffrn_measurement_method 'combination of \w and \f' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17482 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.06 _reflns_number_total 5887 _reflns_number_gt 4031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 (Bruker, 2007)' _computing_data_reduction 'APEX2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens)' _computing_publication_material SHELXL-97 _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^)+(0.1080P)^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 5887 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1681 _refine_ls_wR_factor_gt 0.1500 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Co1 Co 0.26137(4) 0.64787(2) 0.82847(3) 0.04748(19) Uani 1 1 d . . . Cl1 Cl 0.12314(12) 0.56181(7) 0.09053(11) 0.1068(4) Uani 1 1 d . . . O1 O 0.22953(19) 0.66182(12) 0.68510(16) 0.0551(6) Uani 1 1 d . . . O2 O 0.39460(19) 0.66237(11) 0.81380(17) 0.0505(5) Uani 1 1 d . . . O3 O 0.3769(2) 0.67922(14) 0.6493(2) 0.0707(7) Uani 1 1 d . . . O4 O -0.2914(3) 0.7861(2) -0.0725(4) 0.1392(15) Uani 1 1 d . . . O5 O -0.1481(3) 0.85455(19) -0.0002(3) 0.1045(11) Uani 1 1 d . . . O6 O -0.3868(3) 0.6992(2) 0.7483(3) 0.1221(13) Uani 1 1 d . . . H6B H -0.3816 0.7264 0.7994 0.147 Uiso 1 1 d R . . H6C H -0.4611 0.6947 0.7267 0.147 Uiso 1 1 d R . . O7 O 0.3986(4) 0.26531(19) 0.9343(4) 0.1401(15) Uani 1 1 d . . . H7B H 0.3522 0.2513 0.9543 0.168 Uiso 1 1 d R . . H7C H 0.3976 0.2394 0.8897 0.168 Uiso 1 1 d R . . O8 O 0.5725(4) 0.4585(2) 1.3957(3) 0.168(2) Uani 1 1 d . . . H8B H 0.6220 0.4820 1.4404 0.201 Uiso 1 1 d R . . H8C H 0.6099 0.4230 1.3971 0.201 Uiso 1 1 d R . . O9 O 0.5572(6) 0.8690(4) 0.9325(5) 0.243(4) Uani 1 1 d . . . H9B H 0.6066 0.8436 0.9305 0.292 Uiso 1 1 d R . . H9C H 0.5985 0.9008 0.9638 0.292 Uiso 1 1 d R . . O10 O -0.3586(7) 0.5604(3) 0.6772(6) 0.239(3) Uani 1 1 d . . . H10B H -0.3633 0.6003 0.6706 0.287 Uiso 1 1 d R . . H10C H -0.4208 0.5432 0.6486 0.287 Uiso 1 1 d R . . O11 O 0.0388(7) 0.5794(5) 0.5202(7) 0.233(6) Uani 0.763(15) 1 d P . . O11A O 0.025(2) 0.4764(15) 0.4316(19) 0.154(11) Uiso 0.237(15) 1 d P . . O12 O 0.7352(12) 0.5373(5) 1.5420(6) 0.161(7) Uani 0.579(19) 1 d P . . O12A O 0.860(3) 0.5089(7) 1.5480(15) 0.262(19) Uani 0.421(19) 1 d P . . N1 N 0.1055(3) 0.64188(17) 0.8079(2) 0.0578(8) Uani 1 1 d . . . N2 N 0.2440(3) 0.74198(15) 0.8457(2) 0.0591(8) Uani 1 1 d . . . N3 N 0.3286(2) 0.62946(14) 0.9796(2) 0.0486(7) Uani 1 1 d . . . N4 N 0.2750(2) 0.55219(14) 0.81540(19) 0.0481(6) Uani 1 1 d . . . C1 C 0.3363(3) 0.66885(16) 0.7114(3) 0.0509(8) Uani 1 1 d . . . C2 C 0.0392(3) 0.5900(2) 0.7905(3) 0.0732(11) Uani 1 1 d . . . H2A H 0.0691 0.5474 0.7942 0.088 Uiso 1 1 calc R . . C3 C -0.0754(4) 0.5958(3) 0.7664(3) 0.0901(14) Uani 1 1 d . . . H3A H -0.1196 0.5577 0.7545 0.108 Uiso 1 1 calc R . . C4 C -0.1191(4) 0.6561(4) 0.7610(3) 0.0915(16) Uani 1 1 d . . . H4A H -0.1947 0.6602 0.7445 0.110 Uiso 1 1 calc R . . C5 C -0.0533(4) 0.7136(3) 0.7798(3) 0.0814(14) Uani 1 1 d . . . C6 C 0.0611(3) 0.7030(2) 0.8043(3) 0.0643(10) Uani 1 1 d . . . C7 C 0.1358(4) 0.7571(2) 0.8260(2) 0.0663(11) Uani 1 1 d . . . C8 C 0.1000(5) 0.8221(3) 0.8273(3) 0.0862(15) Uani 1 1 d . . . C9 C -0.0183(5) 0.8327(3) 0.8010(4) 0.1003(19) Uani 1 1 d . . . H9A H -0.0452 0.8758 0.8002 0.120 Uiso 1 1 calc R . . C10 C -0.0890(5) 0.7796(4) 0.7779(4) 0.1039(19) Uani 1 1 d . . . H10A H -0.1641 0.7874 0.7601 0.125 Uiso 1 1 calc R . . C11 C 0.1803(6) 0.8721(3) 0.8513(4) 0.0964(17) Uani 1 1 d . . . H11A H 0.1596 0.9165 0.8526 0.116 Uiso 1 1 calc R . . C12 C 0.2891(6) 0.8579(2) 0.8732(4) 0.0930(16) Uani 1 1 d . . . H12A H 0.3421 0.8918 0.8900 0.112 Uiso 1 1 calc R . . C13 C 0.3189(4) 0.78986(19) 0.8694(3) 0.0682(10) Uani 1 1 d . . . H13A H 0.3923 0.7791 0.8839 0.082 Uiso 1 1 calc R . . C14 C 0.3601(3) 0.67085(18) 1.0617(3) 0.0554(8) Uani 1 1 d . . . H14A H 0.3469 0.7165 1.0496 0.067 Uiso 1 1 calc R . . C15 C 0.4129(3) 0.6473(2) 1.1660(3) 0.0628(10) Uani 1 1 d . . . H15A H 0.4340 0.6774 1.2218 0.075 Uiso 1 1 calc R . . C16 C 0.4335(3) 0.5809(2) 1.1859(3) 0.0607(9) Uani 1 1 d . . . H16A H 0.4674 0.5654 1.2552 0.073 Uiso 1 1 calc R . . C17 C 0.4033(3) 0.53605(17) 1.1018(2) 0.0486(8) Uani 1 1 d . . . C18 C 0.3511(2) 0.56330(16) 1.0006(2) 0.0435(7) Uani 1 1 d . . . C19 C 0.3219(2) 0.52064(16) 0.9105(2) 0.0446(7) Uani 1 1 d . . . C20 C 0.3444(3) 0.45218(16) 0.9223(3) 0.0496(8) Uani 1 1 d . . . C21 C 0.3980(3) 0.42516(18) 1.0264(3) 0.0566(9) Uani 1 1 d . . . H21A H 0.4141 0.3796 1.0358 0.068 Uiso 1 1 calc R . . C22 C 0.4258(3) 0.46560(19) 1.1119(3) 0.0616(10) Uani 1 1 d . . . H22A H 0.4605 0.4469 1.1791 0.074 Uiso 1 1 calc R . . C23 C 0.3155(3) 0.41509(18) 0.8298(3) 0.0599(9) Uani 1 1 d . . . H23A H 0.3290 0.3692 0.8334 0.072 Uiso 1 1 calc R . . C24 C 0.2670(3) 0.4467(2) 0.7336(3) 0.0667(10) Uani 1 1 d . . . H24A H 0.2466 0.4223 0.6715 0.080 Uiso 1 1 calc R . . C25 C 0.2488(3) 0.51507(19) 0.7297(3) 0.0585(9) Uani 1 1 d . . . H25A H 0.2167 0.5359 0.6641 0.070 Uiso 1 1 calc R . . C26 C -0.1105(3) 0.7385(2) 0.0062(3) 0.0634(10) Uani 1 1 d . . . C27 C -0.1509(4) 0.6744(3) -0.0038(3) 0.0749(11) Uani 1 1 d . . . H27A H -0.2277 0.6678 -0.0299 0.090 Uiso 1 1 calc R . . C28 C -0.0806(4) 0.6195(2) 0.0238(3) 0.0752(11) Uani 1 1 d . . . H28A H -0.1093 0.5764 0.0186 0.090 Uiso 1 1 calc R . . C29 C 0.0330(4) 0.6295(2) 0.0592(3) 0.0707(11) Uani 1 1 d . . . C30 C 0.0759(3) 0.6930(2) 0.0703(3) 0.0706(11) Uani 1 1 d . . . H30A H 0.1526 0.6993 0.0947 0.085 Uiso 1 1 calc R . . C31 C 0.0051(4) 0.7474(2) 0.0451(3) 0.0679(11) Uani 1 1 d . . . H31A H 0.0345 0.7905 0.0541 0.081 Uiso 1 1 calc R . . C32 C -0.1874(4) 0.7978(3) -0.0241(3) 0.0792(12) 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 0.0548(3) 0.0466(3) 0.0418(3) 0.00577(18) 0.0217(2) 0.0114(2) Cl1 0.1063(10) 0.0963(10) 0.1043(9) -0.0085(7) 0.0334(7) 0.0169(7) O1 0.0565(16) 0.0622(16) 0.0443(12) 0.0122(10) 0.0199(11) 0.0170(11) O2 0.0555(13) 0.0479(14) 0.0487(13) 0.0042(10) 0.0234(11) 0.0054(10) O3 0.0860(18) 0.0750(18) 0.0647(15) 0.0084(13) 0.0455(15) 0.0018(15) O4 0.089(3) 0.131(4) 0.170(4) -0.010(3) 0.031(3) 0.020(3) O5 0.128(3) 0.083(3) 0.095(3) -0.0008(19) 0.043(2) 0.011(2) O6 0.074(2) 0.180(4) 0.108(3) -0.012(2) 0.0356(19) 0.003(2) O7 0.188(4) 0.085(3) 0.185(4) -0.006(3) 0.115(4) -0.006(3) O8 0.221(5) 0.125(4) 0.124(3) -0.013(3) 0.044(3) 0.036(3) O9 0.213(7) 0.375(11) 0.168(6) 0.068(6) 0.108(5) 0.099(6) O10 0.275(8) 0.232(7) 0.291(8) -0.041(6) 0.198(7) -0.069(6) O11 0.184(8) 0.236(11) 0.206(9) 0.051(7) 0.016(6) 0.099(7) O12 0.237(14) 0.124(7) 0.106(6) -0.018(5) 0.059(6) -0.067(7) O12A 0.58(5) 0.092(9) 0.245(17) -0.033(10) 0.31(3) -0.076(17) N1 0.0588(18) 0.073(2) 0.0451(15) 0.0098(14) 0.0258(14) 0.0157(16) N2 0.087(2) 0.0486(18) 0.0477(16) 0.0106(13) 0.0347(16) 0.0194(16) N3 0.0573(17) 0.0457(16) 0.0471(15) 0.0013(12) 0.0266(13) 0.0036(13) N4 0.0502(16) 0.0491(17) 0.0434(14) -0.0005(12) 0.0189(12) 0.0012(12) C1 0.069(2) 0.0376(18) 0.0502(19) 0.0077(14) 0.0294(18) 0.0076(16) C2 0.065(3) 0.094(3) 0.063(2) 0.004(2) 0.031(2) 0.001(2) C3 0.067(3) 0.131(5) 0.077(3) -0.001(3) 0.036(2) -0.004(3) C4 0.069(3) 0.151(6) 0.058(3) 0.014(3) 0.032(2) 0.019(3) C5 0.087(3) 0.123(4) 0.042(2) 0.027(2) 0.036(2) 0.050(3) C6 0.075(3) 0.084(3) 0.0411(18) 0.0211(18) 0.0317(18) 0.026(2) C7 0.093(3) 0.075(3) 0.0406(17) 0.0219(17) 0.0377(19) 0.048(2) C8 0.139(4) 0.068(3) 0.069(3) 0.027(2) 0.061(3) 0.045(3) C9 0.129(5) 0.109(4) 0.078(3) 0.039(3) 0.059(3) 0.084(4) C10 0.104(4) 0.140(5) 0.074(3) 0.039(3) 0.044(3) 0.065(4) C11 0.163(5) 0.063(3) 0.075(3) 0.018(2) 0.063(3) 0.054(3) C12 0.158(5) 0.057(3) 0.078(3) 0.011(2) 0.065(3) 0.012(3) C13 0.101(3) 0.049(2) 0.065(2) 0.0055(18) 0.046(2) 0.010(2) C14 0.068(2) 0.051(2) 0.0507(19) -0.0024(16) 0.0288(17) 0.0035(17) C15 0.075(3) 0.071(3) 0.0454(19) -0.0028(17) 0.0291(18) 0.000(2) C16 0.063(2) 0.073(3) 0.0469(19) 0.0143(18) 0.0249(17) 0.0049(19) C17 0.0467(18) 0.058(2) 0.0441(17) 0.0101(15) 0.0224(14) 0.0021(15) C18 0.0431(17) 0.0427(19) 0.0461(16) 0.0039(14) 0.0207(14) 0.0034(14) C19 0.0388(17) 0.047(2) 0.0498(18) 0.0054(14) 0.0209(14) 0.0036(14) C20 0.0421(18) 0.0420(19) 0.067(2) 0.0028(16) 0.0259(16) -0.0024(14) C21 0.050(2) 0.046(2) 0.071(2) 0.0132(17) 0.0236(18) 0.0023(16) C22 0.054(2) 0.065(3) 0.064(2) 0.0267(19) 0.0242(18) 0.0116(18) C23 0.059(2) 0.042(2) 0.082(3) -0.0083(18) 0.0335(19) -0.0075(17) C24 0.075(3) 0.058(2) 0.070(2) -0.0180(19) 0.035(2) -0.015(2) C25 0.068(2) 0.059(2) 0.0459(19) -0.0023(16) 0.0224(17) -0.0051(18) C26 0.072(3) 0.074(3) 0.0450(18) -0.0045(17) 0.0272(18) -0.010(2) C27 0.069(3) 0.092(3) 0.069(3) -0.005(2) 0.035(2) -0.013(3) C28 0.089(3) 0.067(3) 0.071(2) -0.013(2) 0.036(2) -0.020(2) C29 0.077(3) 0.076(3) 0.056(2) -0.0124(19) 0.026(2) -0.005(2) C30 0.062(2) 0.092(3) 0.052(2) 0.000(2) 0.0196(18) -0.008(2) C31 0.078(3) 0.075(3) 0.0452(19) -0.0023(18) 0.0223(19) -0.019(2) C32 0.082(3) 0.095(4) 0.061(2) -0.002(2) 0.031(2) 0.006(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 O2 1.890(2) . ? Co1 O1 1.892(2) . ? Co1 N2 1.922(3) . ? Co1 N4 1.935(3) . ? Co1 N3 1.949(3) . ? Co1 N1 1.965(3) . ? Cl1 C29 1.731(5) . ? O1 C1 1.307(4) . ? O2 C1 1.310(4) . ? O3 C1 1.229(4) . ? O4 C32 1.266(6) . ? O5 C32 1.231(6) . ? O6 H6B 0.8796 . ? O6 H6C 0.9000 . ? O7 H7B 0.8300 . ? O7 H7C 0.8099 . ? O8 H8B 0.8300 . ? O8 H8C 0.8599 . ? O9 H9B 0.8398 . ? O9 H9C 0.8300 . ? O10 H10B 0.8001 . ? O10 H10C 0.8199 . ? O11 O11A 1.71(3) 3_566 ? O11A O12A 1.45(4) 3_667 ? O11A O11 1.71(3) 3_566 ? O12 O12A 1.71(3) . ? O12A O11A 1.45(4) 3_667 ? N1 C2 1.312(5) . ? N1 C6 1.346(5) . ? N2 C13 1.314(5) . ? N2 C7 1.373(5) . ? N3 C14 1.330(4) . ? N3 C18 1.358(4) . ? N4 C25 1.326(4) . ? N4 C19 1.360(4) . ? C2 C3 1.412(6) . ? C2 H2A 0.9300 . ? C3 C4 1.325(7) . ? C3 H3A 0.9300 . ? C4 C5 1.397(7) . ? C4 H4A 0.9300 . ? C5 C10 1.396(8) . ? C5 C6 1.418(6) . ? C6 C7 1.408(6) . ? C7 C8 1.385(6) . ? C8 C11 1.390(8) . ? C8 C9 1.464(7) . ? C9 C10 1.358(8) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.369(7) . ? C11 H11A 0.9300 . ? C12 C13 1.422(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.403(5) . ? C14 H14A 0.9300 . ? C15 C16 1.358(5) . ? C15 H15A 0.9300 . ? C16 C17 1.397(5) . ? C16 H16A 0.9300 . ? C17 C18 1.394(4) . ? C17 C22 1.432(5) . ? C18 C19 1.433(4) . ? C19 C20 1.394(4) . ? C20 C23 1.398(5) . ? C20 C21 1.425(5) . ? C21 C22 1.359(5) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.372(5) . ? C23 H23A 0.9300 . ? C24 C25 1.384(5) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.372(6) . ? C26 C31 1.398(5) . ? C26 C32 1.499(6) . ? C27 C28 1.382(6) . ? C27 H27A 0.9300 . ? C28 C29 1.382(6) . ? C28 H28A 0.9300 . ? C29 C30 1.370(6) . ? C30 C31 1.378(6) . ? C30 H30A 0.9300 . ? C31 H31A 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 O2 Co1 O1 69.27(10) . . ? O2 Co1 N2 91.93(12) . . ? O1 Co1 N2 90.40(11) . . ? O2 Co1 N4 90.58(10) . . ? O1 Co1 N4 91.77(10) . . ? N2 Co1 N4 177.14(11) . . ? O2 Co1 N3 98.22(10) . . ? O1 Co1 N3 166.89(10) . . ? N2 Co1 N3 94.01(11) . . ? N4 Co1 N3 84.27(11) . . ? O2 Co1 N1 165.72(10) . . ? O1 Co1 N1 96.93(11) . . ? N2 Co1 N1 84.32(14) . . ? N4 Co1 N1 93.57(12) . . ? N3 Co1 N1 95.79(11) . . ? C1 O1 Co1 90.17(18) . . ? C1 O2 Co1 90.1(2) . . ? H6B O6 H6C 91.2 . . ? H7B O7 H7C 106.5 . . ? H8B O8 H8C 101.0 . . ? H9B O9 H9C 97.7 . . ? H10B O10 H10C 110.5 . . ? O12A O11A O11 136(2) 3_667 3_566 ? O11A O12A O12 148.2(14) 3_667 . ? C2 N1 C6 117.5(4) . . ? C2 N1 Co1 130.8(3) . . ? C6 N1 Co1 111.5(3) . . ? C13 N2 C7 120.0(3) . . ? C13 N2 Co1 128.6(3) . . ? C7 N2 Co1 111.3(3) . . ? C14 N3 C18 117.4(3) . . ? C14 N3 Co1 130.6(2) . . ? C18 N3 Co1 111.9(2) . . ? C25 N4 C19 117.5(3) . . ? C25 N4 Co1 129.8(2) . . ? C19 N4 Co1 112.7(2) . . ? O3 C1 O1 125.1(3) . . ? O3 C1 O2 124.5(3) . . ? O1 C1 O2 110.4(3) . . ? N1 C2 C3 123.0(5) . . ? N1 C2 H2A 118.5 . . ? C3 C2 H2A 118.5 . . ? C4 C3 C2 119.2(5) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 120.9(5) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C10 C5 C4 126.3(5) . . ? C10 C5 C6 117.7(6) . . ? C4 C5 C6 116.0(5) . . ? N1 C6 C7 115.6(3) . . ? N1 C6 C5 123.3(5) . . ? C7 C6 C5 121.1(4) . . ? N2 C7 C8 122.6(5) . . ? N2 C7 C6 116.8(3) . . ? C8 C7 C6 120.6(4) . . ? C7 C8 C11 116.4(5) . . ? C7 C8 C9 117.9(5) . . ? C11 C8 C9 125.7(5) . . ? C10 C9 C8 120.1(5) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C5 122.6(5) . . ? C9 C10 H10A 118.7 . . ? C5 C10 H10A 118.7 . . ? C12 C11 C8 121.8(4) . . ? C12 C11 H11A 119.1 . . ? C8 C11 H11A 119.1 . . ? C11 C12 C13 118.3(5) . . ? C11 C12 H12A 120.9 . . ? C13 C12 H12A 120.9 . . ? N2 C13 C12 120.8(4) . . ? N2 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? N3 C14 C15 121.6(3) . . ? N3 C14 H14A 119.2 . . ? C15 C14 H14A 119.2 . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C17 119.6(3) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 116.5(3) . . ? C18 C17 C22 118.3(3) . . ? C16 C17 C22 125.2(3) . . ? N3 C18 C17 124.5(3) . . ? N3 C18 C19 115.9(3) . . ? C17 C18 C19 119.6(3) . . ? N4 C19 C20 123.6(3) . . ? N4 C19 C18 115.2(3) . . ? C20 C19 C18 121.1(3) . . ? C19 C20 C23 116.8(3) . . ? C19 C20 C21 118.6(3) . . ? C23 C20 C21 124.5(3) . . ? C22 C21 C20 120.3(3) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C21 C22 C17 122.1(3) . . ? C21 C22 H22A 118.9 . . ? C17 C22 H22A 118.9 . . ? C24 C23 C20 119.7(3) . . ? C24 C23 H23A 120.2 . . ? C20 C23 H23A 120.2 . . ? C23 C24 C25 119.4(3) . . ? C23 C24 H24A 120.3 . . ? C25 C24 H24A 120.3 . . ? N4 C25 C24 123.0(3) . . ? N4 C25 H25A 118.5 . . ? C24 C25 H25A 118.5 . . ? C27 C26 C31 118.2(4) . . ? C27 C26 C32 121.4(4) . . ? C31 C26 C32 120.5(4) . . ? C26 C27 C28 121.8(4) . . ? C26 C27 H27A 119.1 . . ? C28 C27 H27A 119.1 . . ? C29 C28 C27 118.9(4) . . ? C29 C28 H28A 120.6 . . ? C27 C28 H28A 120.6 . . ? C30 C29 C28 120.7(4) . . ? C30 C29 Cl1 119.1(3) . . ? C28 C29 Cl1 120.2(4) . . ? C29 C30 C31 119.8(4) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C30 C31 C26 120.7(4) . . ? C30 C31 H31A 119.6 . . ? C26 C31 H31A 119.6 . . ? O5 C32 O4 123.4(5) . . ? O5 C32 C26 119.6(5) . . ? O4 C32 C26 117.0(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.427 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.065