# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jyh-Horung Chen' _publ_contact_author_email JYHHCHEN@DRAGON.NCHU.EDU.TW _publ_section_title ; Intermediate (S=1) spin state in five-coordinate cobalt(III): Magnetic properties of N-o-hydroxy-benzamido-meso-tetraphenylporphyrin cobalt(III), Co(N-NCO(o-O)C6H4-tpp) ; loop_ _publ_author_name 'Jyh-Horung Chen.' 'Ting-Yuan Chien.' 'Cheng-Hsiung Cho.' 'Jo-Yu Tung.' ; Shin-Shin Wang ; # Attachment 'CIF_1-3.CIF' data_07ja11lm _database_code_depnum_ccdc_archive 'CCDC 748318' #TrackingRef 'CIF_1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H37 N5 O2' _chemical_formula_weight 749.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.856(2) _cell_length_b 12.509(3) _cell_length_c 14.273(3) _cell_angle_alpha 84.284(3) _cell_angle_beta 80.731(3) _cell_angle_gamma 86.415(3) _cell_volume 1901.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5376 _cell_measurement_theta_min 2.248 _cell_measurement_theta_max 28.201 _exptl_crystal_description LUMP _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.986 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22594 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9467 _reflns_number_gt 7041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 9402 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.25146(9) 0.74339(8) 0.35074(7) 0.0287(2) Uani 1 1 d . . . O2 O 0.42252(9) 0.82109(8) 0.41830(7) 0.0304(2) Uani 1 1 d . . . H2A H 0.3748 0.7762 0.4093 0.046 Uiso 1 1 calc R . . N1 N -0.08238(9) 0.96265(8) 0.31675(8) 0.0204(2) Uani 1 1 d . . . H1A H -0.0305 0.9480 0.2670 0.024 Uiso 0.50 1 calc PR . . N2 N 0.03124(9) 1.08183(8) 0.13890(8) 0.0201(2) Uani 1 1 d . . . H2B H 0.0249 1.0142 0.1559 0.024 Uiso 0.50 1 calc PR . . N3 N 0.16939(9) 0.88875(8) 0.06849(7) 0.0202(2) Uani 1 1 d . . . H3A H 0.1118 0.9027 0.1151 0.024 Uiso 0.50 1 calc PR . . N4 N 0.06627(9) 0.75879(8) 0.25593(7) 0.0188(2) Uani 1 1 d . . . N5 N 0.12992(9) 0.85294(8) 0.25898(7) 0.0189(2) Uani 1 1 d . . . H5A H 0.1106 0.9149 0.2320 0.023 Uiso 0.50 1 calc PR . . C1 C -0.12505(11) 0.88874(10) 0.39088(9) 0.0201(3) Uani 1 1 d . . . C2 C -0.20841(12) 0.94670(10) 0.45893(9) 0.0221(3) Uani 1 1 d . . . H2C H -0.2501 0.9177 0.5171 0.027 Uiso 1 1 calc R . . C3 C -0.21569(12) 1.05122(10) 0.42346(9) 0.0225(3) Uani 1 1 d . . . H3B H -0.2649 1.1060 0.4524 0.027 Uiso 1 1 calc R . . C4 C -0.13435(11) 1.06281(10) 0.33350(9) 0.0201(3) Uani 1 1 d . . . C5 C -0.11076(11) 1.15724(10) 0.27328(9) 0.0197(3) Uani 1 1 d . . . C6 C -0.03028(11) 1.16533(10) 0.18463(9) 0.0204(3) Uani 1 1 d . . . C7 C 0.00454(12) 1.26742(10) 0.13272(10) 0.0247(3) Uani 1 1 d . . . H7A H -0.0255 1.3354 0.1492 0.030 Uiso 1 1 calc R . . C8 C 0.08841(12) 1.24513(10) 0.05643(10) 0.0242(3) Uani 1 1 d . . . H8A H 0.1281 1.2945 0.0101 0.029 Uiso 1 1 calc R . . C9 C 0.10492(11) 1.12824(10) 0.06064(9) 0.0201(3) Uani 1 1 d . . . C10 C 0.19264(11) 1.07460(10) -0.00515(9) 0.0196(3) Uani 1 1 d . . . C11 C 0.21920(11) 0.96323(10) -0.00181(9) 0.0200(3) Uani 1 1 d . . . C12 C 0.30705(12) 0.90612(10) -0.06793(9) 0.0223(3) Uani 1 1 d . . . H12A H 0.3528 0.9359 -0.1242 0.027 Uiso 1 1 calc R . . C13 C 0.31123(12) 0.80129(10) -0.03362(9) 0.0221(3) Uani 1 1 d . . . H13A H 0.3617 0.7468 -0.0619 0.026 Uiso 1 1 calc R . . C14 C 0.22448(11) 0.78824(10) 0.05403(9) 0.0197(3) Uani 1 1 d . . . C15 C 0.19856(11) 0.69282(10) 0.11167(9) 0.0195(3) Uani 1 1 d . . . C16 C 0.11210(11) 0.68054(10) 0.19674(9) 0.0199(3) Uani 1 1 d . . . C17 C 0.04703(11) 0.58621(10) 0.23269(9) 0.0225(3) Uani 1 1 d . . . H17A H 0.0590 0.5202 0.2069 0.027 Uiso 1 1 calc R . . C18 C -0.03589(11) 0.60896(10) 0.31140(9) 0.0223(3) Uani 1 1 d . . . H18A H -0.0902 0.5611 0.3484 0.027 Uiso 1 1 calc R . . C19 C -0.02523(11) 0.71851(10) 0.32747(9) 0.0193(3) Uani 1 1 d . . . C20 C -0.10341(11) 0.77635(10) 0.39509(9) 0.0197(3) Uani 1 1 d . . . C21 C -0.17622(11) 1.25763(10) 0.30845(9) 0.0206(3) Uani 1 1 d . . . C22 C -0.16251(12) 1.28954(10) 0.39684(10) 0.0247(3) Uani 1 1 d . . . H22A H -0.1093 1.2494 0.4333 0.030 Uiso 1 1 calc R . . C23 C -0.22718(13) 1.38059(10) 0.43132(10) 0.0275(3) Uani 1 1 d . . . H23A H -0.2187 1.4000 0.4911 0.033 Uiso 1 1 calc R . . C24 C -0.30428(12) 1.44233(10) 0.37641(10) 0.0279(3) Uani 1 1 d . . . H24A H -0.3468 1.5039 0.3988 0.033 Uiso 1 1 calc R . . C25 C -0.31775(12) 1.41198(11) 0.28797(10) 0.0271(3) Uani 1 1 d . . . H25A H -0.3689 1.4536 0.2508 0.033 Uiso 1 1 calc R . . C26 C -0.25528(12) 1.31990(10) 0.25466(10) 0.0235(3) Uani 1 1 d . . . H26A H -0.2662 1.2994 0.1958 0.028 Uiso 1 1 calc R . . C27 C 0.27320(11) 1.14124(10) -0.08151(9) 0.0203(3) Uani 1 1 d . . . C28 C 0.22385(12) 1.20513(10) -0.15333(9) 0.0229(3) Uani 1 1 d . . . H28A H 0.1386 1.2062 -0.1556 0.027 Uiso 1 1 calc R . . C29 C 0.30144(12) 1.26738(11) -0.22181(9) 0.0247(3) Uani 1 1 d . . . H29A H 0.2677 1.3102 -0.2694 0.030 Uiso 1 1 calc R . . C30 C 0.42923(12) 1.26592(11) -0.21946(9) 0.0253(3) Uani 1 1 d . . . H30A H 0.4808 1.3079 -0.2651 0.030 Uiso 1 1 calc R . . C31 C 0.47912(12) 1.20169(11) -0.14887(10) 0.0259(3) Uani 1 1 d . . . H31A H 0.5646 1.1998 -0.1475 0.031 Uiso 1 1 calc R . . C32 C 0.40186(12) 1.14001(11) -0.08005(9) 0.0236(3) Uani 1 1 d . . . H32A H 0.4360 1.0975 -0.0325 0.028 Uiso 1 1 calc R . . C33 C 0.26307(11) 0.59018(10) 0.08160(9) 0.0213(3) Uani 1 1 d . . . C34 C 0.25250(12) 0.55076(11) -0.00474(10) 0.0257(3) Uani 1 1 d . . . H34A H 0.2052 0.5897 -0.0465 0.031 Uiso 1 1 calc R . . C35 C 0.31236(14) 0.45366(12) -0.02844(11) 0.0329(3) Uani 1 1 d . . . H35A H 0.3057 0.4281 -0.0863 0.039 Uiso 1 1 calc R . . C36 C 0.38181(13) 0.39467(11) 0.03346(11) 0.0328(3) Uani 1 1 d . . . H36A H 0.4220 0.3298 0.0169 0.039 Uiso 1 1 calc R . . C37 C 0.39172(13) 0.43173(11) 0.11976(11) 0.0309(3) Uani 1 1 d . . . H37A H 0.4373 0.3914 0.1619 0.037 Uiso 1 1 calc R . . C38 C 0.33323(12) 0.52960(11) 0.14343(10) 0.0253(3) Uani 1 1 d . . . H38A H 0.3410 0.5550 0.2012 0.030 Uiso 1 1 calc R . . C39 C -0.18602(11) 0.71126(10) 0.47040(9) 0.0199(3) Uani 1 1 d . . . C40 C -0.13810(12) 0.63237(10) 0.53225(9) 0.0238(3) Uani 1 1 d . . . H40A H -0.0521 0.6203 0.5282 0.029 Uiso 1 1 calc R . . C41 C -0.21748(13) 0.57147(11) 0.59995(10) 0.0274(3) Uani 1 1 d . . . H41A H -0.1845 0.5195 0.6415 0.033 Uiso 1 1 calc R . . C42 C -0.34630(12) 0.58789(11) 0.60585(10) 0.0258(3) Uani 1 1 d . . . H42A H -0.3994 0.5466 0.6510 0.031 Uiso 1 1 calc R . . C43 C -0.39544(12) 0.66573(10) 0.54443(9) 0.0236(3) Uani 1 1 d . . . H43A H -0.4815 0.6769 0.5483 0.028 Uiso 1 1 calc R . . C44 C -0.31609(11) 0.72701(10) 0.47705(9) 0.0209(3) Uani 1 1 d . . . H44A H -0.3495 0.7791 0.4358 0.025 Uiso 1 1 calc R . . C45 C 0.22391(11) 0.83366(10) 0.30910(9) 0.0207(3) Uani 1 1 d . . . C46 C 0.30105(11) 0.92739(10) 0.31241(9) 0.0214(3) Uani 1 1 d . . . C47 C 0.28149(13) 1.02684(11) 0.26254(10) 0.0269(3) Uani 1 1 d . . . H47A H 0.2157 1.0367 0.2276 0.032 Uiso 1 1 calc R . . C48 C 0.35735(14) 1.11147(12) 0.26353(11) 0.0342(3) Uani 1 1 d . . . H48A H 0.3427 1.1774 0.2300 0.041 Uiso 1 1 calc R . . C49 C 0.45618(13) 1.09624(13) 0.31574(11) 0.0343(3) Uani 1 1 d . . . H49A H 0.5082 1.1524 0.3165 0.041 Uiso 1 1 calc R . . C50 C 0.47751(12) 0.99919(12) 0.36602(10) 0.0309(3) Uani 1 1 d . . . H50A H 0.5438 0.9901 0.4005 0.037 Uiso 1 1 calc R . . C51 C 0.40042(12) 0.91432(11) 0.36570(9) 0.0244(3) 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 O1 0.0295(5) 0.0253(5) 0.0319(5) 0.0031(4) -0.0101(4) 0.0002(4) O2 0.0262(5) 0.0362(6) 0.0303(5) -0.0072(4) -0.0095(4) 0.0062(4) N1 0.0207(5) 0.0177(5) 0.0210(5) -0.0013(4) 0.0015(4) -0.0005(4) N2 0.0190(5) 0.0194(5) 0.0213(5) -0.0010(4) -0.0020(4) -0.0008(4) N3 0.0200(5) 0.0198(5) 0.0200(5) -0.0018(4) -0.0006(4) -0.0001(4) N4 0.0170(5) 0.0184(5) 0.0203(5) -0.0025(4) 0.0004(4) -0.0019(4) N5 0.0180(5) 0.0173(5) 0.0212(5) -0.0013(4) -0.0017(4) -0.0027(4) C1 0.0170(6) 0.0217(6) 0.0209(6) -0.0023(5) -0.0008(5) -0.0015(5) C2 0.0223(6) 0.0222(6) 0.0208(6) -0.0045(5) 0.0019(5) -0.0026(5) C3 0.0216(6) 0.0204(6) 0.0248(7) -0.0048(5) 0.0012(5) -0.0027(5) C4 0.0181(6) 0.0193(6) 0.0227(6) -0.0042(5) -0.0016(5) -0.0004(5) C5 0.0176(6) 0.0197(6) 0.0219(6) -0.0028(5) -0.0024(5) -0.0012(5) C6 0.0178(6) 0.0209(6) 0.0225(6) -0.0018(5) -0.0031(5) -0.0004(5) C7 0.0225(6) 0.0207(6) 0.0287(7) -0.0009(5) 0.0016(5) -0.0005(5) C8 0.0226(6) 0.0218(6) 0.0262(7) 0.0004(5) 0.0009(5) -0.0013(5) C9 0.0172(6) 0.0215(6) 0.0212(6) -0.0002(5) -0.0030(5) -0.0019(5) C10 0.0178(6) 0.0229(6) 0.0183(6) -0.0011(5) -0.0033(5) -0.0018(5) C11 0.0194(6) 0.0230(6) 0.0176(6) -0.0017(5) -0.0031(5) -0.0016(5) C12 0.0228(6) 0.0248(7) 0.0183(6) -0.0023(5) 0.0004(5) -0.0022(5) C13 0.0223(6) 0.0234(6) 0.0203(6) -0.0057(5) -0.0002(5) -0.0009(5) C14 0.0185(6) 0.0208(6) 0.0201(6) -0.0036(5) -0.0033(5) 0.0001(5) C15 0.0180(6) 0.0202(6) 0.0206(6) -0.0033(5) -0.0029(5) -0.0006(5) C16 0.0175(6) 0.0191(6) 0.0231(6) -0.0020(5) -0.0035(5) 0.0011(5) C17 0.0215(6) 0.0188(6) 0.0261(7) -0.0021(5) -0.0013(5) 0.0002(5) C18 0.0191(6) 0.0204(6) 0.0261(7) -0.0001(5) -0.0010(5) -0.0014(5) C19 0.0158(5) 0.0194(6) 0.0218(6) 0.0003(5) -0.0021(5) -0.0005(4) C20 0.0173(5) 0.0205(6) 0.0207(6) -0.0012(5) -0.0011(5) -0.0022(5) C21 0.0186(6) 0.0186(6) 0.0236(6) -0.0020(5) 0.0012(5) -0.0027(5) C22 0.0267(6) 0.0208(6) 0.0270(7) -0.0026(5) -0.0044(5) -0.0038(5) C23 0.0324(7) 0.0238(7) 0.0261(7) -0.0081(6) 0.0031(5) -0.0088(5) C24 0.0251(7) 0.0194(6) 0.0354(8) -0.0062(6) 0.0095(6) -0.0032(5) C25 0.0222(6) 0.0225(7) 0.0336(8) 0.0010(6) 0.0020(5) -0.0002(5) C26 0.0231(6) 0.0230(6) 0.0231(7) -0.0017(5) 0.0006(5) -0.0019(5) C27 0.0204(6) 0.0197(6) 0.0202(6) -0.0038(5) -0.0003(5) -0.0015(5) C28 0.0193(6) 0.0262(7) 0.0230(6) -0.0026(5) -0.0024(5) -0.0017(5) C29 0.0286(7) 0.0243(7) 0.0202(6) -0.0020(5) -0.0011(5) -0.0018(5) C30 0.0266(7) 0.0263(7) 0.0214(6) -0.0065(5) 0.0054(5) -0.0063(5) C31 0.0179(6) 0.0318(7) 0.0281(7) -0.0093(6) 0.0012(5) -0.0026(5) C32 0.0216(6) 0.0255(7) 0.0239(7) -0.0041(5) -0.0031(5) -0.0002(5) C33 0.0190(6) 0.0187(6) 0.0247(6) -0.0029(5) 0.0027(5) -0.0031(5) C34 0.0280(7) 0.0253(7) 0.0231(7) -0.0026(5) 0.0002(5) -0.0049(5) C35 0.0380(8) 0.0293(8) 0.0298(8) -0.0128(6) 0.0089(6) -0.0102(6) C36 0.0294(7) 0.0212(7) 0.0446(9) -0.0096(6) 0.0078(6) -0.0018(5) C37 0.0258(7) 0.0243(7) 0.0403(8) -0.0032(6) 0.0003(6) 0.0030(5) C38 0.0245(6) 0.0240(7) 0.0264(7) -0.0049(5) 0.0003(5) -0.0001(5) C39 0.0204(6) 0.0194(6) 0.0197(6) -0.0035(5) -0.0005(5) -0.0020(5) C40 0.0193(6) 0.0259(7) 0.0258(7) -0.0020(5) -0.0029(5) 0.0006(5) C41 0.0288(7) 0.0276(7) 0.0246(7) 0.0030(6) -0.0043(5) -0.0002(5) C42 0.0253(6) 0.0278(7) 0.0218(7) 0.0024(5) 0.0027(5) -0.0044(5) C43 0.0194(6) 0.0243(7) 0.0255(7) -0.0037(5) 0.0017(5) -0.0011(5) C44 0.0200(6) 0.0206(6) 0.0211(6) -0.0017(5) -0.0007(5) 0.0005(5) C45 0.0203(6) 0.0241(6) 0.0164(6) -0.0019(5) 0.0005(5) 0.0009(5) C46 0.0179(6) 0.0266(7) 0.0195(6) -0.0052(5) -0.0008(5) -0.0015(5) C47 0.0259(7) 0.0289(7) 0.0271(7) -0.0024(6) -0.0062(5) -0.0050(5) C48 0.0358(8) 0.0317(8) 0.0358(8) -0.0020(6) -0.0052(6) -0.0099(6) C49 0.0269(7) 0.0402(8) 0.0369(8) -0.0135(7) 0.0016(6) -0.0122(6) C50 0.0191(6) 0.0442(9) 0.0320(8) -0.0153(7) -0.0043(5) -0.0021(6) C51 0.0203(6) 0.0323(7) 0.0203(6) -0.0084(5) -0.0010(5) 0.0037(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C45 1.2645(15) . ? O2 C51 1.3527(16) . ? O2 H2A 0.8200 . ? N1 C4 1.3686(15) . ? N1 C1 1.3747(16) . ? N1 H1A 0.8600 . ? N2 C9 1.3660(15) . ? N2 C6 1.3679(16) . ? N2 H2B 0.8600 . ? N3 C11 1.3672(16) . ? N3 C14 1.3780(15) . ? N3 H3A 0.8600 . ? N4 C16 1.3739(16) . ? N4 C19 1.3844(15) . ? N4 N5 1.4100(14) . ? N5 C45 1.3346(16) . ? N5 H5A 0.8600 . ? C1 C20 1.4077(17) . ? C1 C2 1.4363(17) . ? C2 C3 1.3566(18) . ? C2 H2C 0.9300 . ? C3 C4 1.4363(17) . ? C3 H3B 0.9300 . ? C4 C5 1.4017(17) . ? C5 C6 1.4157(17) . ? C5 C21 1.4942(16) . ? C6 C7 1.4506(18) . ? C7 C8 1.3423(18) . ? C7 H7A 0.9300 . ? C8 C9 1.4583(18) . ? C8 H8A 0.9300 . ? C9 C10 1.4129(17) . ? C10 C11 1.4025(17) . ? C10 C27 1.5002(17) . ? C11 C12 1.4387(17) . ? C12 C13 1.3540(18) . ? C12 H12A 0.9300 . ? C13 C14 1.4414(17) . ? C13 H13A 0.9300 . ? C14 C15 1.3974(17) . ? C15 C16 1.4117(17) . ? C15 C33 1.4911(16) . ? C16 C17 1.4219(17) . ? C17 C18 1.3635(18) . ? C17 H17A 0.9300 . ? C18 C19 1.4266(18) . ? C18 H18A 0.9300 . ? C19 C20 1.4049(17) . ? C20 C39 1.4930(17) . ? C21 C26 1.3937(18) . ? C21 C22 1.3934(19) . ? C22 C23 1.3902(18) . ? C22 H22A 0.9300 . ? C23 C24 1.386(2) . ? C23 H23A 0.9300 . ? C24 C25 1.386(2) . ? C24 H24A 0.9300 . ? C25 C26 1.3857(18) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.3917(18) . ? C27 C32 1.3994(17) . ? C28 C29 1.3916(18) . ? C28 H28A 0.9300 . ? C29 C30 1.3920(19) . ? C29 H29A 0.9300 . ? C30 C31 1.384(2) . ? C30 H30A 0.9300 . ? C31 C32 1.3886(18) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C38 1.3944(18) . ? C33 C34 1.3960(19) . ? C34 C35 1.3873(19) . ? C34 H34A 0.9300 . ? C35 C36 1.382(2) . ? C35 H35A 0.9300 . ? C36 C37 1.381(2) . ? C36 H36A 0.9300 . ? C37 C38 1.3900(18) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C40 1.3908(17) . ? C39 C44 1.4027(17) . ? C40 C41 1.3870(18) . ? C40 H40A 0.9300 . ? C41 C42 1.3908(19) . ? C41 H41A 0.9300 . ? C42 C43 1.3845(18) . ? C42 H42A 0.9300 . ? C43 C44 1.3869(17) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 C46 1.4915(18) . ? C46 C47 1.3925(18) . ? C46 C51 1.4094(17) . ? C47 C48 1.384(2) . ? C47 H47A 0.9300 . ? C48 C49 1.395(2) . ? C48 H48A 0.9300 . ? C49 C50 1.374(2) . ? C49 H49A 0.9300 . ? C50 C51 1.393(2) . ? C50 H50A 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 C51 O2 H2A 109.5 . . ? C4 N1 C1 110.27(10) . . ? C4 N1 H1A 124.9 . . ? C1 N1 H1A 124.9 . . ? C9 N2 C6 105.62(10) . . ? C9 N2 H2B 127.2 . . ? C6 N2 H2B 127.2 . . ? C11 N3 C14 110.40(10) . . ? C11 N3 H3A 124.8 . . ? C14 N3 H3A 124.8 . . ? C16 N4 C19 110.26(10) . . ? C16 N4 N5 122.66(10) . . ? C19 N4 N5 124.51(10) . . ? C45 N5 N4 111.40(10) . . ? C45 N5 H5A 124.3 . . ? N4 N5 H5A 124.3 . . ? N1 C1 C20 126.96(11) . . ? N1 C1 C2 106.72(11) . . ? C20 C1 C2 125.95(12) . . ? C3 C2 C1 107.99(11) . . ? C3 C2 H2C 126.0 . . ? C1 C2 H2C 126.0 . . ? C2 C3 C4 108.27(11) . . ? C2 C3 H3B 125.9 . . ? C4 C3 H3B 125.9 . . ? N1 C4 C5 125.62(11) . . ? N1 C4 C3 106.72(10) . . ? C5 C4 C3 127.65(11) . . ? C4 C5 C6 126.00(11) . . ? C4 C5 C21 115.70(11) . . ? C6 C5 C21 118.29(11) . . ? N2 C6 C5 126.36(12) . . ? N2 C6 C7 110.49(11) . . ? C5 C6 C7 123.03(11) . . ? C8 C7 C6 106.96(12) . . ? C8 C7 H7A 126.5 . . ? C6 C7 H7A 126.5 . . ? C7 C8 C9 106.42(11) . . ? C7 C8 H8A 126.8 . . ? C9 C8 H8A 126.8 . . ? N2 C9 C10 126.57(11) . . ? N2 C9 C8 110.50(11) . . ? C10 C9 C8 122.79(12) . . ? C11 C10 C9 125.84(12) . . ? C11 C10 C27 115.65(10) . . ? C9 C10 C27 118.31(11) . . ? N3 C11 C10 125.70(11) . . ? N3 C11 C12 107.03(11) . . ? C10 C11 C12 127.21(12) . . ? C13 C12 C11 107.77(11) . . ? C13 C12 H12A 126.1 . . ? C11 C12 H12A 126.1 . . ? C12 C13 C14 108.66(11) . . ? C12 C13 H13A 125.7 . . ? C14 C13 H13A 125.7 . . ? N3 C14 C15 126.68(11) . . ? N3 C14 C13 106.07(10) . . ? C15 C14 C13 127.23(11) . . ? C14 C15 C16 126.84(11) . . ? C14 C15 C33 119.02(11) . . ? C16 C15 C33 114.10(11) . . ? N4 C16 C15 127.11(11) . . ? N4 C16 C17 106.75(11) . . ? C15 C16 C17 125.90(12) . . ? C18 C17 C16 108.36(11) . . ? C18 C17 H17A 125.8 . . ? C16 C17 H17A 125.8 . . ? C17 C18 C19 108.46(11) . . ? C17 C18 H18A 125.8 . . ? C19 C18 H18A 125.8 . . ? N4 C19 C20 127.24(11) . . ? N4 C19 C18 106.17(10) . . ? C20 C19 C18 126.14(11) . . ? C19 C20 C1 126.48(12) . . ? C19 C20 C39 116.16(11) . . ? C1 C20 C39 116.63(10) . . ? C26 C21 C22 118.44(12) . . ? C26 C21 C5 120.66(12) . . ? C22 C21 C5 120.87(11) . . ? C23 C22 C21 120.95(13) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C24 C23 C22 119.85(13) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C25 C24 C23 119.72(12) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 120.30(13) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C21 120.71(13) . . ? C25 C26 H26A 119.6 . . ? C21 C26 H26A 119.6 . . ? C28 C27 C32 118.88(12) . . ? C28 C27 C10 122.07(11) . . ? C32 C27 C10 119.04(11) . . ? C29 C28 C27 120.30(12) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C28 C29 C30 120.34(12) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C31 C30 C29 119.66(12) . . ? C31 C30 H30A 120.2 . . ? C29 C30 H30A 120.2 . . ? C30 C31 C32 120.15(12) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C31 C32 C27 120.65(12) . . ? C31 C32 H32A 119.7 . . ? C27 C32 H32A 119.7 . . ? C38 C33 C34 118.78(12) . . ? C38 C33 C15 118.74(12) . . ? C34 C33 C15 122.44(12) . . ? C35 C34 C33 120.16(13) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C36 C35 C34 120.38(14) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C37 C36 C35 120.20(13) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C36 C37 C38 119.70(14) . . ? C36 C37 H37A 120.1 . . ? C38 C37 H37A 120.1 . . ? C37 C38 C33 120.77(13) . . ? C37 C38 H38A 119.6 . . ? C33 C38 H38A 119.6 . . ? C40 C39 C44 118.68(12) . . ? C40 C39 C20 122.00(11) . . ? C44 C39 C20 119.27(11) . . ? C41 C40 C39 120.59(12) . . ? C41 C40 H40A 119.7 . . ? C39 C40 H40A 119.7 . . ? C40 C41 C42 120.17(12) . . ? C40 C41 H41A 119.9 . . ? C42 C41 H41A 119.9 . . ? C43 C42 C41 119.93(12) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 119.92(12) . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C43 C44 C39 120.71(12) . . ? C43 C44 H44A 119.6 . . ? C39 C44 H44A 119.6 . . ? O1 C45 N5 124.81(12) . . ? O1 C45 C46 119.76(11) . . ? N5 C45 C46 115.41(11) . . ? C47 C46 C51 118.34(12) . . ? C47 C46 C45 122.70(11) . . ? C51 C46 C45 118.93(12) . . ? C48 C47 C46 121.75(13) . . ? C48 C47 H47A 119.1 . . ? C46 C47 H47A 119.1 . . ? C47 C48 C49 118.91(14) . . ? C47 C48 H48A 120.5 . . ? C49 C48 H48A 120.5 . . ? C50 C49 C48 120.69(14) . . ? C50 C49 H49A 119.7 . . ? C48 C49 H49A 119.7 . . ? C49 C50 C51 120.37(13) . . ? C49 C50 H50A 119.8 . . ? C51 C50 H50A 119.8 . . ? O2 C51 C50 118.48(12) . . ? O2 C51 C46 121.59(12) . . ? C50 C51 C46 119.92(13) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.490 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.054 #=== END data_coooh _database_code_depnum_ccdc_archive 'CCDC 748319' #TrackingRef 'CIF_1-3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H32 Co N5 O2' _chemical_formula_sum 'C51 H32 Co N5 O2' _chemical_formula_weight 805.75 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' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0697(3) _cell_length_b 13.3945(4) _cell_length_c 14.9320(5) _cell_angle_alpha 81.118(3) _cell_angle_beta 84.516(3) _cell_angle_gamma 83.579(3) _cell_volume 2166.82(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11484 _cell_measurement_theta_min 2.7624 _cell_measurement_theta_max 29.1543 _exptl_crystal_description parallelepiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76613 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19912 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 29.21 _reflns_number_total 9855 _reflns_number_gt 7351 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+6.1676P] 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 constro _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9855 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.2187 _refine_ls_wR_factor_gt 0.2095 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.006 _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 Co Co 0.38440(6) 0.18826(5) 0.38670(5) 0.01026(17) Uani 0.80 1 d P A 1 Co' Co 0.3877(3) 0.1887(2) 0.3413(3) 0.0189(6) Uani 0.20 1 d P A 2 O1 O 0.2533(3) 0.2805(2) 0.42177(19) 0.0266(6) Uani 1 1 d . . . O2 O 0.2491(3) 0.2692(3) 0.1379(2) 0.0352(8) Uani 1 1 d . . . N1 N 0.3081(3) 0.0590(2) 0.38817(19) 0.0131(6) Uani 1 1 d . . . N2 N 0.4235(3) 0.1529(3) 0.5096(2) 0.0210(7) Uani 1 1 d . . . N3 N 0.5348(3) 0.2612(2) 0.3500(2) 0.0141(6) Uani 1 1 d . . . N4 N 0.4348(3) 0.1564(3) 0.2176(2) 0.0190(7) Uani 1 1 d . . . N5 N 0.3495(3) 0.2201(3) 0.2662(2) 0.0229(7) Uani 1 1 d . A . C1 C 0.2580(3) 0.0193(3) 0.3202(2) 0.0146(7) Uani 1 1 d . A . C2 C 0.1575(3) -0.0352(3) 0.3592(2) 0.0160(7) Uani 1 1 d . . . H2A H 0.1065 -0.0673 0.3271 0.019 Uiso 1 1 calc R A . C3 C 0.1476(3) -0.0333(3) 0.4497(2) 0.0166(7) Uani 1 1 d . A . H3A H 0.0885 -0.0632 0.4928 0.020 Uiso 1 1 calc R . . C4 C 0.2436(3) 0.0225(3) 0.4682(2) 0.0140(7) Uani 1 1 d . A . C5 C 0.2732(3) 0.0309(3) 0.5569(2) 0.0146(7) Uani 1 1 d . . . C6 C 0.3660(3) 0.0869(3) 0.5738(2) 0.0155(7) Uani 1 1 d . A . C7 C 0.4169(3) 0.0852(3) 0.6591(2) 0.0161(7) Uani 1 1 d . . . H7A H 0.3968 0.0430 0.7145 0.019 Uiso 1 1 calc R A . C8 C 0.4987(3) 0.1548(3) 0.6457(2) 0.0163(7) Uani 1 1 d . A . H8A H 0.5458 0.1713 0.6903 0.020 Uiso 1 1 calc R . . C9 C 0.5013(3) 0.1991(3) 0.5523(2) 0.0178(7) Uani 1 1 d . A . C10 C 0.5684(3) 0.2771(3) 0.5097(2) 0.0175(7) Uani 1 1 d . . . C11 C 0.5790(3) 0.3081(3) 0.4148(2) 0.0162(7) Uani 1 1 d . A . C12 C 0.6443(3) 0.3911(3) 0.3728(2) 0.0182(8) Uani 1 1 d . . . H12A H 0.6800 0.4366 0.4029 0.022 Uiso 1 1 calc R A . C13 C 0.6460(3) 0.3930(3) 0.2816(2) 0.0176(7) Uani 1 1 d . A . H13A H 0.6830 0.4403 0.2361 0.021 Uiso 1 1 calc R . . C14 C 0.5818(3) 0.3104(3) 0.2662(2) 0.0150(7) Uani 1 1 d . A . C15 C 0.5850(3) 0.2794(3) 0.1797(2) 0.0158(7) Uani 1 1 d . . . C16 C 0.5298(3) 0.1959(3) 0.1621(2) 0.0168(7) Uani 1 1 d . A . C17 C 0.5570(4) 0.1336(3) 0.0938(3) 0.0220(8) Uani 1 1 d . . . H17A H 0.6193 0.1415 0.0457 0.026 Uiso 1 1 calc R A . C18 C 0.4788(4) 0.0600(3) 0.1085(3) 0.0214(8) Uani 1 1 d . A . H18A H 0.4773 0.0076 0.0724 0.026 Uiso 1 1 calc R . . C19 C 0.4000(3) 0.0750(3) 0.1867(2) 0.0156(7) Uani 1 1 d . A . C20 C 0.3032(3) 0.0208(3) 0.2287(2) 0.0139(7) Uani 1 1 d . . . C21 C 0.2014(3) -0.0213(3) 0.6364(2) 0.0139(7) Uani 1 1 d . A . C22 C 0.1821(3) -0.1232(3) 0.6430(3) 0.0190(8) Uani 1 1 d . . . H22A H 0.2195 -0.1620 0.5979 0.023 Uiso 1 1 calc R A . C23 C 0.1090(4) -0.1682(3) 0.7145(3) 0.0229(8) Uani 1 1 d . A . H23A H 0.0952 -0.2374 0.7174 0.027 Uiso 1 1 calc R . . C24 C 0.0554(4) -0.1137(3) 0.7821(3) 0.0251(9) Uani 1 1 d . . . H24A H 0.0041 -0.1447 0.8307 0.030 Uiso 1 1 calc R A . C25 C 0.0778(3) -0.0132(3) 0.7776(2) 0.0203(8) Uani 1 1 d . A . H25A H 0.0441 0.0241 0.8248 0.024 Uiso 1 1 calc R . . C26 C 0.1485(3) 0.0332(3) 0.7056(2) 0.0163(7) Uani 1 1 d . . . H26A H 0.1614 0.1026 0.7029 0.020 Uiso 1 1 calc R A . C27 C 0.6366(3) 0.3294(3) 0.5679(2) 0.0167(7) Uani 1 1 d . A . C28 C 0.5734(4) 0.3905(3) 0.6269(3) 0.0257(9) Uani 1 1 d . . . H28A H 0.4869 0.4002 0.6293 0.031 Uiso 1 1 calc R A . C29 C 0.6352(4) 0.4381(4) 0.6828(3) 0.0284(9) Uani 1 1 d . A . H29A H 0.5908 0.4806 0.7225 0.034 Uiso 1 1 calc R . . C30 C 0.7608(4) 0.4236(3) 0.6805(3) 0.0231(8) Uani 1 1 d . . . H30A H 0.8032 0.4555 0.7189 0.028 Uiso 1 1 calc R A . C31 C 0.8248(4) 0.3620(3) 0.6218(3) 0.0247(9) Uani 1 1 d . A . H31A H 0.9113 0.3517 0.6201 0.030 Uiso 1 1 calc R . . C32 C 0.7633(4) 0.3156(3) 0.5657(3) 0.0222(8) Uani 1 1 d . . . H32A H 0.8079 0.2740 0.5253 0.027 Uiso 1 1 calc R A . C33 C 0.6541(5) 0.3351(4) 0.1008(3) 0.0382(5) Uani 1 1 d . A . C34 C 0.7768(5) 0.3476(4) 0.0995(3) 0.0382(5) Uani 1 1 d . . . H34A H 0.8204 0.3203 0.1510 0.046 Uiso 1 1 calc R A . C35 C 0.8372(5) 0.3999(4) 0.0229(3) 0.0382(5) Uani 1 1 d . A . H35A H 0.9211 0.4091 0.0227 0.046 Uiso 1 1 calc R . . C36 C 0.7749(5) 0.4379(4) -0.0517(3) 0.0382(5) Uani 1 1 d . . . H36A H 0.8159 0.4733 -0.1038 0.046 Uiso 1 1 calc R A . C37 C 0.6554(5) 0.4254(4) -0.0518(3) 0.0382(5) Uani 1 1 d . A . H37A H 0.6130 0.4524 -0.1040 0.046 Uiso 1 1 calc R . . C38 C 0.5935(5) 0.3733(4) 0.0240(3) 0.0382(5) Uani 1 1 d . . . H38A H 0.5098 0.3642 0.0228 0.046 Uiso 1 1 calc R A . C39 C 0.2489(3) -0.0400(3) 0.1698(2) 0.0171(7) Uani 1 1 d . A . C40 C 0.2091(3) 0.0093(3) 0.0870(2) 0.0193(8) Uani 1 1 d . . . H40A H 0.2178 0.0795 0.0695 0.023 Uiso 1 1 calc R A . C41 C 0.1568(4) -0.0432(4) 0.0297(3) 0.0254(9) Uani 1 1 d . A . H41A H 0.1301 -0.0087 -0.0266 0.030 Uiso 1 1 calc R . . C42 C 0.1435(4) -0.1449(4) 0.0541(3) 0.0292(10) Uani 1 1 d . . . H42A H 0.1074 -0.1807 0.0151 0.035 Uiso 1 1 calc R A . C43 C 0.1830(4) -0.1950(3) 0.1360(3) 0.0269(9) Uani 1 1 d . A . H43A H 0.1743 -0.2653 0.1526 0.032 Uiso 1 1 calc R . . C44 C 0.2353(4) -0.1435(3) 0.1943(3) 0.0237(8) Uani 1 1 d . . . H44A H 0.2617 -0.1785 0.2505 0.028 Uiso 1 1 calc R A . C45 C 0.1631(4) 0.3272(3) 0.3724(3) 0.0249(9) Uani 1 1 d . A . C46 C 0.0631(4) 0.3822(3) 0.4161(3) 0.0259(9) Uani 1 1 d . . . H46A H 0.0593 0.3809 0.4800 0.031 Uiso 1 1 calc R A . C47 C -0.0278(4) 0.4368(3) 0.3681(3) 0.0253(9) Uani 1 1 d . A . H47A H -0.0927 0.4743 0.3986 0.030 Uiso 1 1 calc R . . C48 C -0.0249(4) 0.4373(3) 0.2749(3) 0.0240(8) Uani 1 1 d . . . H48A H -0.0873 0.4755 0.2410 0.029 Uiso 1 1 calc R A . C49 C 0.0694(4) 0.3819(3) 0.2322(3) 0.0233(8) Uani 1 1 d . A . H49A H 0.0699 0.3813 0.1686 0.028 Uiso 1 1 calc R . . C50 C 0.1637(4) 0.3270(3) 0.2786(3) 0.0242(9) Uani 1 1 d . . . C51 C 0.2569(4) 0.2701(3) 0.2224(3) 0.0275(9) Uani 1 1 d . A . 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 Co 0.0110(3) 0.0145(3) 0.0058(3) -0.0034(3) 0.0005(3) -0.0016(2) Co' 0.0136(14) 0.0148(14) 0.0276(18) -0.0048(15) 0.0054(14) -0.0017(10) O1 0.0279(16) 0.0285(16) 0.0237(14) -0.0051(12) -0.0016(12) -0.0026(13) O2 0.0391(19) 0.043(2) 0.0229(15) -0.0063(14) -0.0034(13) 0.0028(15) N1 0.0107(14) 0.0150(15) 0.0145(14) -0.0060(12) -0.0004(11) -0.0006(11) N2 0.0230(17) 0.0273(18) 0.0146(15) -0.0017(13) -0.0020(12) -0.0127(14) N3 0.0118(14) 0.0147(15) 0.0162(14) -0.0040(12) 0.0013(11) -0.0027(12) N4 0.0202(16) 0.0243(17) 0.0140(14) -0.0100(13) 0.0087(12) -0.0072(13) N5 0.0243(18) 0.0288(19) 0.0162(16) -0.0056(14) -0.0027(13) -0.0006(15) C1 0.0124(16) 0.0172(18) 0.0140(16) -0.0020(14) -0.0025(12) -0.0001(14) C2 0.0124(17) 0.0199(18) 0.0169(16) -0.0046(14) -0.0023(13) -0.0026(14) C3 0.0130(17) 0.0197(19) 0.0172(17) -0.0035(14) 0.0025(13) -0.0049(14) C4 0.0107(16) 0.0157(17) 0.0165(16) -0.0069(14) 0.0004(12) 0.0000(13) C5 0.0158(17) 0.0148(17) 0.0128(16) -0.0017(13) 0.0017(13) -0.0023(14) C6 0.0184(18) 0.0177(18) 0.0115(15) -0.0040(13) -0.0018(13) -0.0036(14) C7 0.0151(17) 0.0187(18) 0.0147(16) -0.0019(14) -0.0033(13) -0.0008(14) C8 0.0148(17) 0.0181(18) 0.0173(17) -0.0049(14) -0.0038(13) -0.0011(14) C9 0.0162(18) 0.024(2) 0.0156(17) -0.0073(15) -0.0036(13) -0.0048(15) C10 0.0150(17) 0.0224(19) 0.0170(17) -0.0085(15) 0.0019(13) -0.0055(15) C11 0.0141(17) 0.0175(18) 0.0183(17) -0.0072(14) 0.0006(13) -0.0031(14) C12 0.0164(18) 0.0197(19) 0.0201(18) -0.0059(15) 0.0015(14) -0.0068(15) C13 0.0173(18) 0.0167(18) 0.0186(17) -0.0012(14) 0.0019(13) -0.0055(14) C14 0.0129(17) 0.0159(18) 0.0159(16) -0.0024(14) 0.0003(13) -0.0010(14) C15 0.0152(17) 0.0189(18) 0.0124(16) -0.0002(14) -0.0001(13) -0.0019(14) C16 0.0144(17) 0.0213(19) 0.0140(16) -0.0025(14) 0.0037(13) -0.0027(14) C17 0.0202(19) 0.024(2) 0.0210(18) -0.0055(16) 0.0068(15) -0.0036(16) C18 0.022(2) 0.027(2) 0.0172(17) -0.0126(16) 0.0050(14) -0.0050(16) C19 0.0149(17) 0.0200(18) 0.0129(16) -0.0058(14) -0.0008(13) -0.0022(14) C20 0.0137(17) 0.0183(18) 0.0111(15) -0.0049(13) -0.0009(12) -0.0034(14) C21 0.0108(16) 0.0183(18) 0.0128(15) -0.0011(14) -0.0011(12) -0.0036(14) C22 0.0204(19) 0.0177(19) 0.0190(17) -0.0025(15) -0.0017(14) -0.0022(15) C23 0.025(2) 0.019(2) 0.0236(19) 0.0034(16) -0.0023(15) -0.0060(16) C24 0.023(2) 0.033(2) 0.0170(18) 0.0051(16) 0.0015(15) -0.0063(17) C25 0.0176(18) 0.030(2) 0.0122(16) -0.0023(15) -0.0001(13) 0.0006(16) C26 0.0155(17) 0.0212(19) 0.0134(16) -0.0048(14) -0.0013(13) -0.0036(14) C27 0.0174(18) 0.0187(18) 0.0152(16) -0.0029(14) 0.0010(13) -0.0084(15) C28 0.0174(19) 0.034(2) 0.029(2) -0.0155(18) -0.0002(16) -0.0040(17) C29 0.029(2) 0.034(2) 0.026(2) -0.0189(19) -0.0009(17) -0.0021(19) C30 0.029(2) 0.024(2) 0.0201(18) -0.0053(16) -0.0041(15) -0.0130(17) C31 0.0169(19) 0.032(2) 0.028(2) -0.0100(18) -0.0003(15) -0.0103(17) C32 0.0198(19) 0.025(2) 0.0236(19) -0.0095(16) 0.0022(15) -0.0059(16) C33 0.0575(13) 0.0344(11) 0.0243(9) -0.0010(8) 0.0046(9) -0.0224(10) C34 0.0575(13) 0.0344(11) 0.0243(9) -0.0010(8) 0.0046(9) -0.0224(10) C35 0.0575(13) 0.0344(11) 0.0243(9) -0.0010(8) 0.0046(9) -0.0224(10) C36 0.0575(13) 0.0344(11) 0.0243(9) -0.0010(8) 0.0046(9) -0.0224(10) C37 0.0575(13) 0.0344(11) 0.0243(9) -0.0010(8) 0.0046(9) -0.0224(10) C38 0.0575(13) 0.0344(11) 0.0243(9) -0.0010(8) 0.0046(9) -0.0224(10) C39 0.0123(17) 0.026(2) 0.0147(16) -0.0083(15) -0.0008(13) -0.0035(15) C40 0.0147(18) 0.029(2) 0.0155(17) -0.0055(15) 0.0022(13) -0.0051(15) C41 0.0191(19) 0.046(3) 0.0126(17) -0.0072(17) 0.0007(14) -0.0056(18) C42 0.025(2) 0.042(3) 0.027(2) -0.020(2) -0.0026(16) -0.0108(19) C43 0.025(2) 0.028(2) 0.030(2) -0.0112(18) 0.0008(17) -0.0091(18) C44 0.021(2) 0.026(2) 0.0247(19) -0.0057(17) -0.0010(15) -0.0040(16) C45 0.0179(19) 0.0155(19) 0.042(2) 0.0033(17) -0.0117(17) -0.0047(15) C46 0.028(2) 0.026(2) 0.025(2) -0.0041(17) -0.0024(16) -0.0058(17) C47 0.0169(19) 0.022(2) 0.038(2) -0.0089(18) 0.0041(16) -0.0028(16) C48 0.0186(19) 0.0166(19) 0.038(2) -0.0016(17) -0.0086(16) -0.0024(15) C49 0.025(2) 0.0172(19) 0.028(2) -0.0006(16) 0.0002(16) -0.0088(16) C50 0.0187(19) 0.0136(18) 0.039(2) -0.0018(17) 0.0071(16) -0.0058(15) C51 0.020(2) 0.026(2) 0.036(2) -0.0013(18) -0.0018(17) -0.0035(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 Co N5 1.851(3) . ? Co O1 1.887(3) . ? Co N2 1.902(3) . ? Co N1 2.006(3) . ? Co N3 2.013(3) . ? Co' N5 1.232(5) . ? Co' N4 1.971(5) . ? Co' N3 2.011(4) . ? Co' N1 2.034(4) . ? Co' O1 2.208(4) . ? Co' C51 2.445(6) . ? O1 C45 1.338(5) . ? O2 C51 1.275(5) . ? N1 C4 1.383(4) . ? N1 C1 1.400(4) . ? N2 C6 1.361(5) . ? N2 C9 1.371(5) . ? N3 C11 1.384(5) . ? N3 C14 1.403(5) . ? N4 C19 1.354(5) . ? N4 C16 1.376(5) . ? N4 N5 1.424(4) . ? N5 C51 1.329(5) . ? C1 C20 1.407(5) . ? C1 C2 1.427(5) . ? C2 C3 1.349(5) . ? C2 H2A 0.9500 . ? C3 C4 1.437(5) . ? C3 H3A 0.9500 . ? C4 C5 1.418(5) . ? C5 C6 1.400(5) . ? C5 C21 1.489(5) . ? C6 C7 1.437(5) . ? C7 C8 1.352(5) . ? C7 H7A 0.9500 . ? C8 C9 1.427(5) . ? C8 H8A 0.9500 . ? C9 C10 1.388(5) . ? C10 C11 1.411(5) . ? C10 C27 1.499(5) . ? C11 C12 1.426(5) . ? C12 C13 1.356(5) . ? C12 H12A 0.9500 . ? C13 C14 1.438(5) . ? C13 H13A 0.9500 . ? C14 C15 1.413(5) . ? C15 C16 1.403(5) . ? C15 C33 1.487(6) . ? C16 C17 1.405(5) . ? C17 C18 1.364(6) . ? C17 H17A 0.9500 . ? C18 C19 1.416(5) . ? C18 H18A 0.9500 . ? C19 C20 1.404(5) . ? C20 C39 1.493(5) . ? C21 C22 1.392(5) . ? C21 C26 1.402(5) . ? C22 C23 1.380(5) . ? C22 H22A 0.9500 . ? C23 C24 1.386(6) . ? C23 H23A 0.9500 . ? C24 C25 1.386(6) . ? C24 H24A 0.9500 . ? C25 C26 1.376(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.382(5) . ? C27 C32 1.391(5) . ? C28 C29 1.394(6) . ? C28 H28A 0.9500 . ? C29 C30 1.381(6) . ? C29 H29A 0.9500 . ? C30 C31 1.387(6) . ? C30 H30A 0.9500 . ? C31 C32 1.385(5) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.384(7) . ? C33 C34 1.385(8) . ? C34 C35 1.400(6) . ? C34 H34A 0.9500 . ? C35 C36 1.366(7) . ? C35 H35A 0.9500 . ? C36 C37 1.353(7) . ? C36 H36A 0.9500 . ? C37 C38 1.397(6) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.395(5) . ? C39 C44 1.400(6) . ? C40 C41 1.390(5) . ? C40 H40A 0.9500 . ? C41 C42 1.376(7) . ? C41 H41A 0.9500 . ? C42 C43 1.385(6) . ? C42 H42A 0.9500 . ? C43 C44 1.393(6) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C50 1.401(6) . ? C45 C46 1.421(6) . ? C46 C47 1.368(6) . ? C46 H46A 0.9500 . ? C47 C48 1.388(6) . ? C47 H47A 0.9500 . ? C48 C49 1.376(6) . ? C48 H48A 0.9500 . ? C49 C50 1.386(6) . ? C49 H49A 0.9500 . ? C50 C51 1.485(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Co O1 90.91(14) . . ? N5 Co N2 178.51(16) . . ? O1 Co N2 90.57(14) . . ? N5 Co N1 86.78(14) . . ? O1 Co N1 104.04(13) . . ? N2 Co N1 92.76(13) . . ? N5 Co N3 86.58(14) . . ? O1 Co N3 109.87(13) . . ? N2 Co N3 93.02(13) . . ? N1 Co N3 145.50(12) . . ? N5 Co' N4 46.0(2) . . ? N5 Co' N3 107.2(3) . . ? N4 Co' N3 95.81(18) . . ? N5 Co' N1 106.0(3) . . ? N4 Co' N1 96.00(19) . . ? N3 Co' N1 143.2(2) . . ? N5 Co' O1 97.4(2) . . ? N4 Co' O1 143.4(2) . . ? N3 Co' O1 98.25(18) . . ? N1 Co' O1 92.63(17) . . ? N5 Co' C51 18.0(2) . . ? N4 Co' C51 63.34(18) . . ? N3 Co' C51 114.3(2) . . ? N1 Co' C51 102.07(19) . . ? O1 Co' C51 80.04(16) . . ? C45 O1 Co 128.2(3) . . ? C45 O1 Co' 111.8(3) . . ? Co O1 Co' 16.70(10) . . ? C4 N1 C1 105.0(3) . . ? C4 N1 Co 116.5(2) . . ? C1 N1 Co 131.9(2) . . ? C4 N1 Co' 134.7(3) . . ? C1 N1 Co' 113.3(3) . . ? Co N1 Co' 19.20(11) . . ? C6 N2 C9 107.8(3) . . ? C6 N2 Co 125.4(3) . . ? C9 N2 Co 126.2(3) . . ? C11 N3 C14 105.0(3) . . ? C11 N3 Co 117.6(2) . . ? C14 N3 Co 132.4(2) . . ? C11 N3 Co' 136.3(3) . . ? C14 N3 Co' 113.8(3) . . ? Co N3 Co' 19.29(11) . . ? C19 N4 C16 111.0(3) . . ? C19 N4 N5 120.9(3) . . ? C16 N4 N5 120.7(3) . . ? C19 N4 Co' 123.3(3) . . ? C16 N4 Co' 123.7(3) . . ? N5 N4 Co' 38.47(18) . . ? Co' N5 C51 145.3(4) . . ? Co' N5 N4 95.5(3) . . ? C51 N5 N4 117.4(3) . . ? Co' N5 Co 10.18(16) . . ? C51 N5 Co 135.4(3) . . ? N4 N5 Co 105.7(2) . . ? N1 C1 C20 127.5(3) . . ? N1 C1 C2 109.6(3) . . ? C20 C1 C2 122.6(3) . . ? C3 C2 C1 108.0(3) . . ? C3 C2 H2A 126.0 . . ? C1 C2 H2A 126.0 . . ? C2 C3 C4 106.9(3) . . ? C2 C3 H3A 126.6 . . ? C4 C3 H3A 126.6 . . ? N1 C4 C5 125.4(3) . . ? N1 C4 C3 110.3(3) . . ? C5 C4 C3 124.1(3) . . ? C6 C5 C4 123.3(3) . . ? C6 C5 C21 118.1(3) . . ? C4 C5 C21 118.7(3) . . ? N2 C6 C5 124.4(3) . . ? N2 C6 C7 108.6(3) . . ? C5 C6 C7 127.1(3) . . ? C8 C7 C6 107.3(3) . . ? C8 C7 H7A 126.4 . . ? C6 C7 H7A 126.4 . . ? C7 C8 C9 107.5(3) . . ? C7 C8 H8A 126.2 . . ? C9 C8 H8A 126.2 . . ? N2 C9 C10 124.1(3) . . ? N2 C9 C8 108.6(3) . . ? C10 C9 C8 127.2(3) . . ? C9 C10 C11 123.9(3) . . ? C9 C10 C27 117.8(3) . . ? C11 C10 C27 118.2(3) . . ? N3 C11 C10 126.2(3) . . ? N3 C11 C12 110.7(3) . . ? C10 C11 C12 123.0(3) . . ? C13 C12 C11 107.1(3) . . ? C13 C12 H12A 126.4 . . ? C11 C12 H12A 126.4 . . ? C12 C13 C14 107.6(3) . . ? C12 C13 H13A 126.2 . . ? C14 C13 H13A 126.2 . . ? N3 C14 C15 128.0(3) . . ? N3 C14 C13 109.2(3) . . ? C15 C14 C13 122.1(3) . . ? C16 C15 C14 124.4(3) . . ? C16 C15 C33 116.1(3) . . ? C14 C15 C33 119.5(4) . . ? N4 C16 C15 122.7(3) . . ? N4 C16 C17 106.1(3) . . ? C15 C16 C17 131.2(3) . . ? C18 C17 C16 108.4(3) . . ? C18 C17 H17A 125.8 . . ? C16 C17 H17A 125.8 . . ? C17 C18 C19 108.2(3) . . ? C17 C18 H18A 125.9 . . ? C19 C18 H18A 125.9 . . ? N4 C19 C20 123.4(3) . . ? N4 C19 C18 106.3(3) . . ? C20 C19 C18 130.2(3) . . ? C19 C20 C1 124.7(3) . . ? C19 C20 C39 115.5(3) . . ? C1 C20 C39 119.8(3) . . ? C22 C21 C26 118.5(3) . . ? C22 C21 C5 121.6(3) . . ? C26 C21 C5 119.9(3) . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 120.8(4) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C25 C24 C23 118.9(4) . . ? C25 C24 H24A 120.6 . . ? C23 C24 H24A 120.6 . . ? C26 C25 C24 120.9(4) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C25 C26 C21 120.4(4) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? C28 C27 C32 118.8(3) . . ? C28 C27 C10 120.0(3) . . ? C32 C27 C10 121.2(3) . . ? C27 C28 C29 120.8(4) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? C30 C29 C28 120.0(4) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C31 119.5(4) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C31 C32 C27 120.5(4) . . ? C31 C32 H32A 119.7 . . ? C27 C32 H32A 119.7 . . ? C38 C33 C34 118.6(4) . . ? C38 C33 C15 118.2(5) . . ? C34 C33 C15 123.1(4) . . ? C33 C34 C35 120.5(5) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C36 C35 C34 119.7(5) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C37 C36 C35 120.4(4) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C36 C37 C38 120.8(5) . . ? C36 C37 H37A 119.6 . . ? C38 C37 H37A 119.6 . . ? C33 C38 C37 120.0(5) . . ? C33 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C40 C39 C44 118.8(3) . . ? C40 C39 C20 118.3(3) . . ? C44 C39 C20 123.0(3) . . ? C41 C40 C39 120.9(4) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C42 C41 C40 120.2(4) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C41 C42 C43 119.6(4) . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C42 C43 C44 120.9(4) . . ? C42 C43 H43A 119.5 . . ? C44 C43 H43A 119.5 . . ? C43 C44 C39 119.7(4) . . ? C43 C44 H44A 120.2 . . ? C39 C44 H44A 120.2 . . ? O1 C45 C50 123.1(4) . . ? O1 C45 C46 119.0(4) . . ? C50 C45 C46 117.9(4) . . ? C47 C46 C45 121.6(4) . . ? C47 C46 H46A 119.2 . . ? C45 C46 H46A 119.2 . . ? C46 C47 C48 119.8(4) . . ? C46 C47 H47A 120.1 . . ? C48 C47 H47A 120.1 . . ? C49 C48 C47 119.2(4) . . ? C49 C48 H48A 120.4 . . ? C47 C48 H48A 120.4 . . ? C48 C49 C50 122.4(4) . . ? C48 C49 H49A 118.8 . . ? C50 C49 H49A 118.8 . . ? C49 C50 C45 119.1(4) . . ? C49 C50 C51 115.4(4) . . ? C45 C50 C51 125.6(4) . . ? O2 C51 N5 122.1(4) . . ? O2 C51 C50 122.5(4) . . ? N5 C51 C50 115.4(4) . . ? O2 C51 Co' 138.2(3) . . ? N5 C51 Co' 16.65(19) . . ? C50 C51 Co' 99.2(3) . . ? _diffrn_measured_fraction_theta_max 0.836 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.783 _refine_diff_density_min -1.183 _refine_diff_density_rms 0.108 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.232 0.293 0.799 253 64 ' ' 2 -0.232 0.707 0.201 252 63 ' ' _platon_squeeze_details ; ; #=== END data_jhc374m _database_code_depnum_ccdc_archive 'CCDC 748320' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H33 Cl3 Ga N5 O3' _chemical_formula_weight 963.91 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' Ga Ga 0.2307 1.6083 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1417(10) _cell_length_b 13.6899(12) _cell_length_c 14.9925(14) _cell_angle_alpha 81.500(2) _cell_angle_beta 84.290(2) _cell_angle_gamma 84.643(2) _cell_volume 2243.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12860 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.04 _reflns_number_total 8728 _reflns_number_gt 6116 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8728 _refine_ls_number_parameters 624 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2526 _refine_ls_wR_factor_gt 0.2362 _refine_ls_goodness_of_fit_ref 1.535 _refine_ls_restrained_S_all 1.535 _refine_ls_shift/su_max 0.011 _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 N1 N 0.4663(4) 0.7375(3) 0.6510(3) 0.0368(10) Uani 1 1 d . . . N2 N 0.5783(4) 0.8465(3) 0.4913(3) 0.0424(11) Uani 1 1 d . . . N3 N 0.6913(4) 0.9424(3) 0.6118(3) 0.0342(9) Uani 1 1 d . . . N4 N 0.5715(4) 0.8391(3) 0.7861(3) 0.0414(11) Uani 1 1 d . . . O1 O 0.7559(5) 0.7305(4) 0.8644(3) 0.0815(15) Uani 1 1 d . B . O2 O 0.7542(4) 0.7166(3) 0.5784(3) 0.0570(11) Uani 1 1 d . . . C1 C 0.4205(5) 0.6895(4) 0.7343(3) 0.0389(12) Uani 1 1 d . B . C2 C 0.3555(5) 0.6083(4) 0.7183(4) 0.0469(13) Uani 1 1 d . . . H2A H 0.3192 0.5626 0.7625 0.056 Uiso 1 1 calc R B . C3 C 0.3566(5) 0.6101(4) 0.6280(4) 0.0472(14) Uani 1 1 d . B . H3A H 0.3209 0.5663 0.5989 0.057 Uiso 1 1 calc R . . C4 C 0.4223(4) 0.6916(4) 0.5850(3) 0.0381(12) Uani 1 1 d . B . C5 C 0.4341(5) 0.7226(4) 0.4927(3) 0.0404(12) Uani 1 1 d . . . C6 C 0.5007(5) 0.7995(4) 0.4491(3) 0.0406(12) Uani 1 1 d . B . C7 C 0.5038(5) 0.8438(4) 0.3566(4) 0.0437(13) Uani 1 1 d . . . H7A H 0.4582 0.8276 0.3130 0.052 Uiso 1 1 calc R B . C8 C 0.5837(5) 0.9127(4) 0.3434(3) 0.0416(12) Uani 1 1 d . B . H8A H 0.6030 0.9529 0.2892 0.050 Uiso 1 1 calc R . . C9 C 0.6342(5) 0.9138(4) 0.4274(3) 0.0374(11) Uani 1 1 d . B . C10 C 0.7249(5) 0.9703(4) 0.4443(3) 0.0374(11) Uani 1 1 d . . . C11 C 0.7546(4) 0.9803(4) 0.5320(3) 0.0362(11) Uani 1 1 d . B . C12 C 0.8501(5) 1.0358(4) 0.5508(3) 0.0392(12) Uani 1 1 d . . . H12A H 0.9075 1.0658 0.5089 0.047 Uiso 1 1 calc R B . C13 C 0.8408(5) 1.0361(4) 0.6400(4) 0.0417(12) Uani 1 1 d . B . H13A H 0.8910 1.0672 0.6710 0.050 Uiso 1 1 calc R . . C14 C 0.7416(4) 0.9810(4) 0.6809(3) 0.0364(11) Uani 1 1 d . B . C15 C 0.6977(5) 0.9780(4) 0.7721(3) 0.0383(12) Uani 1 1 d . . . C16 C 0.6031(5) 0.9222(4) 0.8150(3) 0.0390(12) Uani 1 1 d . B . C17 C 0.5204(5) 0.9376(4) 0.8909(4) 0.0500(14) Uani 1 1 d . . . H17A H 0.5186 0.9892 0.9251 0.060 Uiso 1 1 calc R B . C18 C 0.4439(5) 0.8635(5) 0.9050(4) 0.0521(15) Uani 1 1 d . B . H18A H 0.3815 0.8560 0.9510 0.062 Uiso 1 1 calc R . . C19 C 0.4746(5) 0.8005(4) 0.8390(3) 0.0419(12) Uani 1 1 d . B . C20 C 0.4180(5) 0.7188(4) 0.8200(3) 0.0403(12) Uani 1 1 d . . . C21 C 0.3670(5) 0.6709(4) 0.4329(4) 0.0452(13) Uani 1 1 d . B . C22 C 0.2410(5) 0.6854(5) 0.4335(4) 0.0589(16) Uani 1 1 d . . . H22A H 0.1976 0.7264 0.4716 0.071 Uiso 1 1 calc R B . C23 C 0.1808(6) 0.6388(5) 0.3772(5) 0.0649(18) Uani 1 1 d . B . H23A H 0.0972 0.6496 0.3773 0.078 Uiso 1 1 calc R . . C24 C 0.2430(6) 0.5767(5) 0.3212(4) 0.0629(18) Uani 1 1 d . . . H24A H 0.2023 0.5457 0.2834 0.075 Uiso 1 1 calc R B . C25 C 0.3663(8) 0.5614(6) 0.3223(5) 0.086(2) Uani 1 1 d . B . H25A H 0.4090 0.5184 0.2856 0.103 Uiso 1 1 calc R . . C26 C 0.4288(6) 0.6086(6) 0.3769(5) 0.071(2) Uani 1 1 d . . . H26A H 0.5126 0.5981 0.3756 0.085 Uiso 1 1 calc R B . C27 C 0.7965(5) 1.0224(4) 0.3646(3) 0.0388(12) Uani 1 1 d . B . C28 C 0.8500(5) 0.9699(5) 0.2962(4) 0.0454(13) Uani 1 1 d . . . H28A H 0.8388 0.9030 0.2988 0.054 Uiso 1 1 calc R B . C29 C 0.9205(5) 1.0179(5) 0.2241(4) 0.0578(17) Uani 1 1 d . B . H29A H 0.9546 0.9828 0.1779 0.069 Uiso 1 1 calc R . . C30 C 0.9405(6) 1.1157(6) 0.2195(5) 0.0658(18) Uani 1 1 d . . . H30A H 0.9900 1.1465 0.1721 0.079 Uiso 1 1 calc R B . C31 C 0.8857(6) 1.1678(5) 0.2869(5) 0.0647(18) Uani 1 1 d . B . H31A H 0.8980 1.2345 0.2843 0.078 Uiso 1 1 calc R . . C32 C 0.8130(5) 1.1227(4) 0.3579(4) 0.0490(14) Uani 1 1 d . . . H32A H 0.7749 1.1595 0.4016 0.059 Uiso 1 1 calc R B . C33 C 0.7508(5) 1.0385(4) 0.8307(3) 0.0412(12) Uani 1 1 d . B . C34 C 0.7610(5) 1.1395(5) 0.8080(4) 0.0535(15) Uani 1 1 d . . . H34A H 0.7337 1.1728 0.7542 0.064 Uiso 1 1 calc R B . C35 C 0.8124(6) 1.1908(5) 0.8662(5) 0.0687(19) Uani 1 1 d . B . H35A H 0.8200 1.2584 0.8502 0.082 Uiso 1 1 calc R . . C36 C 0.8516(6) 1.1450(6) 0.9452(5) 0.0662(19) Uani 1 1 d . . . H36A H 0.8858 1.1804 0.9832 0.079 Uiso 1 1 calc R B . C37 C 0.8402(6) 1.0458(6) 0.9686(4) 0.0641(19) Uani 1 1 d . B . H37A H 0.8659 1.0142 1.0235 0.077 Uiso 1 1 calc R . . C38 C 0.7914(5) 0.9914(5) 0.9125(4) 0.0489(14) Uani 1 1 d . . . H38A H 0.7856 0.9237 0.9291 0.059 Uiso 1 1 calc R B . C39 C 0.3486(5) 0.6652(4) 0.8991(4) 0.0452(13) Uani 1 1 d . B . C40 C 0.4059(7) 0.6266(5) 0.9743(4) 0.0661(18) Uani 1 1 d . . . H40A H 0.4880 0.6334 0.9756 0.079 Uiso 1 1 calc R B . C41 C 0.3420(10) 0.5772(6) 1.0487(5) 0.095(3) Uani 1 1 d . B . H41A H 0.3818 0.5505 1.0995 0.114 Uiso 1 1 calc R . . C42 C 0.2204(10) 0.5671(6) 1.0484(5) 0.091(3) Uani 1 1 d . . . H42A H 0.1784 0.5337 1.0988 0.110 Uiso 1 1 calc R B . C43 C 0.1639(8) 0.6045(6) 0.9773(5) 0.083(2) Uani 1 1 d . B . H43A H 0.0815 0.5980 0.9777 0.099 Uiso 1 1 calc R . . C44 C 0.2260(6) 0.6543(5) 0.9005(4) 0.0627(17) Uani 1 1 d . . . H44A H 0.1846 0.6801 0.8503 0.075 Uiso 1 1 calc R B . C45 C 0.7466(5) 0.7285(5) 0.7799(5) 0.0554(16) Uani 1 1 d . . . C46 C 0.8382(5) 0.6720(4) 0.7230(4) 0.0458(13) Uani 1 1 d . B . C47 C 0.9299(5) 0.6180(4) 0.7695(4) 0.0522(15) Uani 1 1 d . . . H47A H 0.9286 0.6184 0.8316 0.063 Uiso 1 1 calc R B . C48 C 1.0222(5) 0.5639(5) 0.7271(5) 0.0594(17) Uani 1 1 d . B . H48A H 1.0811 0.5270 0.7605 0.071 Uiso 1 1 calc R . . C49 C 1.0275(5) 0.5644(5) 0.6337(5) 0.0573(16) Uani 1 1 d . . . H49A H 1.0907 0.5293 0.6039 0.069 Uiso 1 1 calc R B . C50 C 0.9397(5) 0.6167(5) 0.5875(5) 0.0567(16) Uani 1 1 d . B . H50A H 0.9435 0.6174 0.5251 0.068 Uiso 1 1 calc R . . C51 C 0.8403(5) 0.6714(4) 0.6310(4) 0.0452(13) Uani 1 1 d . B . N5 N 0.6566(4) 0.7780(4) 0.7363(3) 0.0466(11) Uani 1 1 d . B . O3 O 0.7342(7) 0.6080(6) 0.4313(5) 0.125(2) Uani 1 1 d . . . C53 C 0.7841(14) 0.6745(11) 0.3591(13) 0.217(10) Uani 1 1 d . . . C52 C 1.2833(10) 1.2705(7) 0.9284(6) 0.037(2) Uani 0.50 1 d P . . H52A H 1.2799 1.2660 0.9945 0.044 Uiso 0.50 1 calc PR A 1 Ga1 Ga 0.62542(6) 0.80604(5) 0.61283(13) 0.0317(4) Uani 0.852(6) 1 d P B 1 Cl1 Cl 1.192(2) 1.1977(13) 0.8887(8) 0.149(12) Uani 0.228(10) 1 d P C 1 Cl2 Cl 1.4166(15) 1.2198(18) 0.8763(8) 0.133(9) Uani 0.228(10) 1 d P C 1 Cl3 Cl 1.3571(15) 1.3704(13) 0.8670(9) 0.095(5) Uani 0.228(10) 1 d P C 1 Ga1' Ga 0.6227(4) 0.8051(3) 0.6681(7) 0.036(2) Uani 0.148(6) 1 d P B 2 Cl1' Cl 1.1294(7) 1.284(2) 0.9126(8) 0.177(10) Uani 0.272(10) 1 d P C 2 Cl2' Cl 1.324(2) 1.1681(6) 0.8826(6) 0.120(8) Uani 0.272(10) 1 d P C 2 Cl3' Cl 1.280(2) 1.3883(5) 0.9031(9) 0.119(6) Uani 0.272(10) 1 d P C 2 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 N1 0.034(2) 0.045(3) 0.033(2) -0.0097(18) 0.0018(17) -0.0105(19) N2 0.048(3) 0.051(3) 0.031(2) -0.0065(19) -0.0061(19) -0.017(2) N3 0.034(2) 0.039(2) 0.031(2) -0.0095(17) 0.0006(17) -0.0063(18) N4 0.045(2) 0.049(3) 0.033(2) -0.0186(19) 0.0127(19) -0.013(2) O1 0.095(4) 0.108(4) 0.040(3) -0.015(2) -0.015(2) 0.015(3) O2 0.060(3) 0.061(3) 0.052(2) -0.016(2) -0.004(2) 0.000(2) C1 0.038(3) 0.042(3) 0.036(3) -0.007(2) 0.001(2) -0.008(2) C2 0.047(3) 0.046(3) 0.048(3) -0.006(2) 0.002(3) -0.014(3) C3 0.047(3) 0.052(3) 0.048(3) -0.015(3) -0.001(3) -0.017(3) C4 0.034(3) 0.047(3) 0.037(3) -0.014(2) -0.002(2) -0.009(2) C5 0.038(3) 0.047(3) 0.040(3) -0.017(2) -0.001(2) -0.010(2) C6 0.038(3) 0.051(3) 0.036(3) -0.014(2) -0.005(2) -0.009(2) C7 0.039(3) 0.058(4) 0.037(3) -0.011(2) -0.010(2) -0.002(3) C8 0.044(3) 0.049(3) 0.032(3) -0.005(2) -0.005(2) -0.006(3) C9 0.038(3) 0.043(3) 0.032(3) -0.009(2) -0.001(2) -0.007(2) C10 0.041(3) 0.041(3) 0.031(3) -0.009(2) 0.002(2) -0.003(2) C11 0.035(3) 0.041(3) 0.033(3) -0.009(2) -0.001(2) 0.001(2) C12 0.036(3) 0.046(3) 0.036(3) -0.004(2) 0.001(2) -0.010(2) C13 0.035(3) 0.049(3) 0.044(3) -0.011(2) -0.004(2) -0.010(2) C14 0.036(3) 0.042(3) 0.033(3) -0.007(2) -0.006(2) -0.007(2) C15 0.040(3) 0.043(3) 0.034(3) -0.012(2) -0.003(2) -0.003(2) C16 0.042(3) 0.045(3) 0.032(3) -0.014(2) 0.001(2) -0.009(2) C17 0.055(3) 0.058(4) 0.042(3) -0.025(3) 0.009(3) -0.009(3) C18 0.050(3) 0.067(4) 0.041(3) -0.021(3) 0.015(3) -0.014(3) C19 0.042(3) 0.052(3) 0.031(3) -0.008(2) 0.006(2) -0.008(3) C20 0.042(3) 0.047(3) 0.033(3) -0.007(2) 0.000(2) -0.006(2) C21 0.045(3) 0.053(3) 0.041(3) -0.012(2) -0.004(2) -0.016(3) C22 0.046(3) 0.070(4) 0.067(4) -0.027(3) -0.002(3) -0.011(3) C23 0.054(4) 0.079(5) 0.069(4) -0.017(4) -0.013(3) -0.027(4) C24 0.073(5) 0.068(4) 0.058(4) -0.024(3) -0.012(3) -0.029(4) C25 0.092(6) 0.096(6) 0.083(5) -0.062(5) -0.004(4) -0.008(5) C26 0.048(4) 0.096(5) 0.082(5) -0.055(4) -0.010(3) -0.001(4) C27 0.042(3) 0.043(3) 0.032(3) -0.005(2) -0.001(2) -0.008(2) C28 0.043(3) 0.057(4) 0.037(3) -0.009(2) -0.001(2) -0.004(3) C29 0.048(3) 0.087(5) 0.035(3) -0.006(3) 0.003(3) -0.001(3) C30 0.058(4) 0.076(5) 0.056(4) 0.012(3) 0.007(3) -0.011(4) C31 0.069(4) 0.055(4) 0.065(4) 0.015(3) -0.008(3) -0.017(3) C32 0.058(4) 0.044(3) 0.044(3) -0.003(2) -0.003(3) -0.006(3) C33 0.038(3) 0.050(3) 0.040(3) -0.018(2) 0.001(2) -0.007(2) C34 0.048(3) 0.064(4) 0.053(4) -0.018(3) -0.007(3) -0.009(3) C35 0.072(5) 0.062(4) 0.082(5) -0.037(4) -0.005(4) -0.016(4) C36 0.063(4) 0.088(5) 0.060(4) -0.038(4) -0.004(3) -0.023(4) C37 0.054(4) 0.110(6) 0.034(3) -0.025(3) -0.002(3) -0.015(4) C38 0.048(3) 0.066(4) 0.036(3) -0.013(3) 0.000(2) -0.011(3) C39 0.049(3) 0.046(3) 0.039(3) -0.005(2) 0.007(2) -0.012(3) C40 0.085(5) 0.068(4) 0.045(4) 0.000(3) -0.005(3) -0.014(4) C41 0.150(9) 0.091(6) 0.041(4) 0.010(4) -0.009(5) -0.030(6) C42 0.140(8) 0.080(6) 0.054(5) 0.002(4) 0.018(5) -0.052(6) C43 0.103(6) 0.077(5) 0.067(5) -0.015(4) 0.035(4) -0.044(5) C44 0.068(4) 0.064(4) 0.056(4) -0.004(3) 0.012(3) -0.025(3) C45 0.045(3) 0.049(4) 0.069(4) 0.003(3) -0.002(3) -0.004(3) C46 0.040(3) 0.039(3) 0.058(4) -0.004(2) 0.002(3) -0.012(2) C47 0.044(3) 0.047(3) 0.066(4) 0.000(3) -0.012(3) -0.009(3) C48 0.043(3) 0.047(4) 0.089(5) -0.004(3) -0.017(3) -0.001(3) C49 0.035(3) 0.052(4) 0.084(5) -0.011(3) -0.005(3) 0.003(3) C50 0.048(4) 0.058(4) 0.064(4) -0.014(3) 0.001(3) -0.002(3) C51 0.032(3) 0.033(3) 0.070(4) -0.002(3) -0.008(3) -0.005(2) N5 0.046(3) 0.056(3) 0.038(3) -0.012(2) 0.003(2) -0.006(2) O3 0.128(6) 0.131(6) 0.129(6) -0.057(5) -0.024(5) 0.001(5) C53 0.168(13) 0.134(11) 0.274(19) 0.100(13) 0.079(13) 0.063(10) C52 0.065(7) 0.032(5) 0.016(4) -0.009(4) 0.003(4) -0.009(5) Ga1 0.0309(4) 0.0373(4) 0.0278(10) -0.0083(3) -0.0009(3) -0.0033(3) Cl1 0.27(3) 0.145(15) 0.057(7) 0.031(8) -0.067(11) -0.166(18) Cl2 0.136(12) 0.21(2) 0.049(6) -0.056(9) -0.007(6) 0.083(12) Cl3 0.131(10) 0.103(9) 0.058(6) 0.021(6) -0.023(6) -0.081(8) Ga1' 0.040(2) 0.045(3) 0.024(6) -0.0084(19) 0.0010(19) -0.0055(17) Cl1' 0.036(4) 0.41(3) 0.090(7) -0.026(11) -0.003(4) -0.026(8) Cl2' 0.26(2) 0.039(4) 0.053(4) -0.009(3) 0.008(8) 0.035(7) Cl3' 0.259(19) 0.017(3) 0.088(8) 0.001(4) -0.074(10) -0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.395(6) . ? N1 C4 1.396(6) . ? N1 Ga1 2.074(4) . ? N1 Ga1' 2.102(6) . ? N2 C9 1.372(6) . ? N2 C6 1.377(6) . ? N2 Ga1 1.933(4) . ? N3 C11 1.384(6) . ? N3 C14 1.414(6) . ? N3 Ga1 2.066(4) . ? N3 Ga1' 2.122(6) . ? N4 C16 1.363(7) . ? N4 C19 1.373(6) . ? N4 N5 1.433(6) . ? N4 Ga1' 1.914(11) . ? O1 C45 1.286(8) . ? O2 C51 1.349(7) . ? O2 Ga1 1.880(4) . ? O2 Ga1' 2.276(8) . ? C1 C20 1.399(7) . ? C1 C2 1.442(7) . ? C2 C3 1.349(8) . ? C2 H2A 0.9300 . ? C3 C4 1.430(7) . ? C3 H3A 0.9300 . ? C4 C5 1.383(7) . ? C5 C6 1.390(7) . ? C5 C21 1.511(7) . ? C6 C7 1.428(7) . ? C7 C8 1.336(7) . ? C7 H7A 0.9300 . ? C8 C9 1.432(7) . ? C8 H8A 0.9300 . ? C9 C10 1.392(7) . ? C10 C11 1.416(7) . ? C10 C27 1.495(7) . ? C11 C12 1.438(7) . ? C12 C13 1.331(7) . ? C12 H12A 0.9300 . ? C13 C14 1.432(7) . ? C13 H13A 0.9300 . ? C14 C15 1.401(7) . ? C15 C16 1.406(7) . ? C15 C33 1.489(7) . ? C16 C17 1.420(7) . ? C17 C18 1.364(8) . ? C17 H17A 0.9300 . ? C18 C19 1.404(7) . ? C18 H18A 0.9300 . ? C19 C20 1.411(7) . ? C20 C39 1.487(7) . ? C21 C26 1.375(8) . ? C21 C22 1.399(8) . ? C22 C23 1.386(8) . ? C22 H22A 0.9300 . ? C23 C24 1.376(10) . ? C23 H23A 0.9300 . ? C24 C25 1.372(10) . ? C24 H24A 0.9300 . ? C25 C26 1.388(9) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C32 1.391(7) . ? C27 C28 1.393(7) . ? C28 C29 1.391(8) . ? C28 H28A 0.9300 . ? C29 C30 1.369(10) . ? C29 H29A 0.9300 . ? C30 C31 1.383(10) . ? C30 H30A 0.9300 . ? C31 C32 1.378(8) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.387(8) . ? C33 C38 1.395(8) . ? C34 C35 1.392(8) . ? C34 H34A 0.9300 . ? C35 C36 1.348(10) . ? C35 H35A 0.9300 . ? C36 C37 1.366(10) . ? C36 H36A 0.9300 . ? C37 C38 1.382(8) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C40 1.365(9) . ? C39 C44 1.386(9) . ? C40 C41 1.385(10) . ? C40 H40A 0.9300 . ? C41 C42 1.376(12) . ? C41 H41A 0.9300 . ? C42 C43 1.306(11) . ? C42 H42A 0.9300 . ? C43 C44 1.402(9) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 N5 1.328(8) . ? C45 C46 1.497(9) . ? C45 Ga1' 2.342(10) . ? C46 C51 1.378(8) . ? C46 C47 1.388(8) . ? C47 C48 1.370(9) . ? C47 H47A 0.9300 . ? C48 C49 1.395(9) . ? C48 H48A 0.9300 . ? C49 C50 1.344(8) . ? C49 H49A 0.9300 . ? C50 C51 1.435(8) . ? C50 H50A 0.9300 . ? N5 Ga1' 1.125(12) . ? N5 Ga1 1.894(6) . ? O3 C53 1.411(14) . ? C52 Cl3' 1.599(12) . ? C52 Cl2' 1.657(12) . ? C52 Cl1 1.693(13) . ? C52 Cl2 1.742(15) . ? C52 Cl1' 1.744(14) . ? C52 Cl3 1.754(13) . ? C52 H52A 0.9800 . ? Cl2 Cl3 2.09(3) . ? Cl1' Cl3' 2.29(3) . ? 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 C1 N1 C4 106.2(4) . . ? C1 N1 Ga1 131.3(3) . . ? C4 N1 Ga1 116.0(3) . . ? C1 N1 Ga1' 109.5(4) . . ? C4 N1 Ga1' 137.8(4) . . ? Ga1 N1 Ga1' 22.7(2) . . ? C9 N2 C6 108.1(4) . . ? C9 N2 Ga1 125.2(3) . . ? C6 N2 Ga1 125.6(4) . . ? C11 N3 C14 105.3(4) . . ? C11 N3 Ga1 115.8(3) . . ? C14 N3 Ga1 130.0(3) . . ? C11 N3 Ga1' 136.7(4) . . ? C14 N3 Ga1' 108.2(4) . . ? Ga1 N3 Ga1' 22.7(2) . . ? C16 N4 C19 111.6(4) . . ? C16 N4 N5 121.9(4) . . ? C19 N4 N5 121.3(4) . . ? C16 N4 Ga1' 122.8(4) . . ? C19 N4 Ga1' 123.1(4) . . ? N5 N4 Ga1' 35.7(3) . . ? C51 O2 Ga1 126.3(4) . . ? C51 O2 Ga1' 106.5(4) . . ? Ga1 O2 Ga1' 20.13(18) . . ? N1 C1 C20 128.6(5) . . ? N1 C1 C2 108.5(4) . . ? C20 C1 C2 122.3(5) . . ? C3 C2 C1 108.1(5) . . ? C3 C2 H2A 126.0 . . ? C1 C2 H2A 126.0 . . ? C2 C3 C4 107.7(5) . . ? C2 C3 H3A 126.1 . . ? C4 C3 H3A 126.1 . . ? C5 C4 N1 125.9(5) . . ? C5 C4 C3 124.7(5) . . ? N1 C4 C3 109.3(4) . . ? C4 C5 C6 125.7(5) . . ? C4 C5 C21 118.1(5) . . ? C6 C5 C21 116.1(5) . . ? N2 C6 C5 123.7(5) . . ? N2 C6 C7 107.7(5) . . ? C5 C6 C7 128.6(5) . . ? C8 C7 C6 108.2(5) . . ? C8 C7 H7A 125.9 . . ? C6 C7 H7A 125.9 . . ? C7 C8 C9 108.1(5) . . ? C7 C8 H8A 126.0 . . ? C9 C8 H8A 126.0 . . ? N2 C9 C10 124.3(4) . . ? N2 C9 C8 107.7(4) . . ? C10 C9 C8 128.0(5) . . ? C9 C10 C11 124.1(5) . . ? C9 C10 C27 117.8(4) . . ? C11 C10 C27 118.2(4) . . ? N3 C11 C10 124.7(4) . . ? N3 C11 C12 110.2(4) . . ? C10 C11 C12 125.0(5) . . ? C13 C12 C11 106.8(5) . . ? C13 C12 H12A 126.6 . . ? C11 C12 H12A 126.6 . . ? C12 C13 C14 109.5(5) . . ? C12 C13 H13A 125.2 . . ? C14 C13 H13A 125.2 . . ? C15 C14 N3 128.0(4) . . ? C15 C14 C13 123.7(5) . . ? N3 C14 C13 108.0(4) . . ? C14 C15 C16 125.1(5) . . ? C14 C15 C33 119.8(5) . . ? C16 C15 C33 115.1(4) . . ? N4 C16 C15 123.7(4) . . ? N4 C16 C17 105.6(4) . . ? C15 C16 C17 130.7(5) . . ? C18 C17 C16 108.2(5) . . ? C18 C17 H17A 125.9 . . ? C16 C17 H17A 125.9 . . ? C17 C18 C19 108.9(5) . . ? C17 C18 H18A 125.5 . . ? C19 C18 H18A 125.5 . . ? N4 C19 C18 105.6(5) . . ? N4 C19 C20 123.2(5) . . ? C18 C19 C20 131.0(5) . . ? C1 C20 C19 124.9(5) . . ? C1 C20 C39 120.4(5) . . ? C19 C20 C39 114.7(5) . . ? C26 C21 C22 118.8(5) . . ? C26 C21 C5 120.6(5) . . ? C22 C21 C5 120.6(5) . . ? C23 C22 C21 120.0(6) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 121.0(6) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C25 C24 C23 118.6(6) . . ? C25 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? C24 C25 C26 121.4(6) . . ? C24 C25 H25A 119.3 . . ? C26 C25 H25A 119.3 . . ? C21 C26 C25 120.2(6) . . ? C21 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C32 C27 C28 118.8(5) . . ? C32 C27 C10 121.2(5) . . ? C28 C27 C10 120.0(5) . . ? C29 C28 C27 119.7(6) . . ? C29 C28 H28A 120.2 . . ? C27 C28 H28A 120.2 . . ? C30 C29 C28 121.4(6) . . ? C30 C29 H29A 119.3 . . ? C28 C29 H29A 119.3 . . ? C29 C30 C31 118.7(6) . . ? C29 C30 H30A 120.7 . . ? C31 C30 H30A 120.7 . . ? C32 C31 C30 121.1(6) . . ? C32 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C31 C32 C27 120.3(6) . . ? C31 C32 H32A 119.8 . . ? C27 C32 H32A 119.8 . . ? C34 C33 C38 118.5(5) . . ? C34 C33 C15 123.1(5) . . ? C38 C33 C15 118.4(5) . . ? C33 C34 C35 119.6(6) . . ? C33 C34 H34A 120.2 . . ? C35 C34 H34A 120.2 . . ? C36 C35 C34 121.7(7) . . ? C36 C35 H35A 119.2 . . ? C34 C35 H35A 119.2 . . ? C35 C36 C37 119.1(6) . . ? C35 C36 H36A 120.5 . . ? C37 C36 H36A 120.5 . . ? C36 C37 C38 121.4(6) . . ? C36 C37 H37A 119.3 . . ? C38 C37 H37A 119.3 . . ? C37 C38 C33 119.7(6) . . ? C37 C38 H38A 120.1 . . ? C33 C38 H38A 120.1 . . ? C40 C39 C44 118.1(6) . . ? C40 C39 C20 119.5(5) . . ? C44 C39 C20 122.4(5) . . ? C39 C40 C41 120.0(7) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C42 C41 C40 120.8(7) . . ? C42 C41 H41A 119.6 . . ? C40 C41 H41A 119.6 . . ? C43 C42 C41 119.9(7) . . ? C43 C42 H42A 120.1 . . ? C41 C42 H42A 120.1 . . ? C42 C43 C44 120.9(8) . . ? C42 C43 H43A 119.6 . . ? C44 C43 H43A 119.6 . . ? C39 C44 C43 120.3(7) . . ? C39 C44 H44A 119.8 . . ? C43 C44 H44A 119.8 . . ? O1 C45 N5 122.5(6) . . ? O1 C45 C46 122.4(5) . . ? N5 C45 C46 115.1(6) . . ? O1 C45 Ga1' 137.8(5) . . ? N5 C45 Ga1' 15.9(3) . . ? C46 C45 Ga1' 99.5(5) . . ? C51 C46 C47 118.8(5) . . ? C51 C46 C45 126.3(5) . . ? C47 C46 C45 114.8(6) . . ? C48 C47 C46 122.2(6) . . ? C48 C47 H47A 118.9 . . ? C46 C47 H47A 118.9 . . ? C47 C48 C49 119.8(6) . . ? C47 C48 H48A 120.1 . . ? C49 C48 H48A 120.1 . . ? C50 C49 C48 118.8(6) . . ? C50 C49 H49A 120.6 . . ? C48 C49 H49A 120.6 . . ? C49 C50 C51 122.3(6) . . ? C49 C50 H50A 118.8 . . ? C51 C50 H50A 118.8 . . ? O2 C51 C46 125.0(5) . . ? O2 C51 C50 117.0(6) . . ? C46 C51 C50 118.0(5) . . ? Ga1' N5 C45 145.3(6) . . ? Ga1' N5 N4 96.2(5) . . ? C45 N5 N4 117.3(5) . . ? Ga1' N5 Ga1 11.6(3) . . ? C45 N5 Ga1 133.9(4) . . ? N4 N5 Ga1 107.8(4) . . ? Cl3' C52 Cl2' 140.4(10) . . ? Cl3' C52 Cl1 124.7(11) . . ? Cl2' C52 Cl1 52.5(9) . . ? Cl3' C52 Cl2 107.8(16) . . ? Cl2' C52 Cl2 44.6(8) . . ? Cl1 C52 Cl2 95.0(11) . . ? Cl3' C52 Cl1' 86.3(14) . . ? Cl2' C52 Cl1' 99.8(11) . . ? Cl1 C52 Cl1' 47.5(10) . . ? Cl2 C52 Cl1' 137.7(9) . . ? Cl3' C52 Cl3 34.2(6) . . ? Cl2' C52 Cl3 110.3(11) . . ? Cl1 C52 Cl3 127.2(8) . . ? Cl2 C52 Cl3 73.6(14) . . ? Cl1' C52 Cl3 110.8(12) . . ? Cl3' C52 H52A 98.9 . . ? Cl2' C52 H52A 117.9 . . ? Cl1 C52 H52A 115.6 . . ? Cl2 C52 H52A 115.6 . . ? Cl1' C52 H52A 100.5 . . ? Cl3 C52 H52A 115.6 . . ? O2 Ga1 N5 92.2(2) . . ? O2 Ga1 N2 94.8(2) . . ? N5 Ga1 N2 173.0(2) . . ? O2 Ga1 N3 108.55(17) . . ? N5 Ga1 N3 87.22(18) . . ? N2 Ga1 N3 90.19(18) . . ? O2 Ga1 N1 112.21(18) . . ? N5 Ga1 N1 86.50(19) . . ? N2 Ga1 N1 91.23(17) . . ? N3 Ga1 N1 138.94(17) . . ? C52 Cl2 Cl3 53.5(7) . . ? C52 Cl3 Cl2 52.9(9) . . ? N5 Ga1' N4 48.1(4) . . ? N5 Ga1' N1 111.4(5) . . ? N4 Ga1' N1 96.7(3) . . ? N5 Ga1' N3 111.0(5) . . ? N4 Ga1' N3 97.1(3) . . ? N1 Ga1' N3 133.3(4) . . ? N5 Ga1' O2 100.7(4) . . ? N4 Ga1' O2 148.8(4) . . ? N1 Ga1' O2 97.1(3) . . ? N3 Ga1' O2 93.5(3) . . ? N5 Ga1' C45 18.8(3) . . ? N4 Ga1' C45 66.4(4) . . ? N1 Ga1' C45 118.3(3) . . ? N3 Ga1' C45 108.2(3) . . ? O2 Ga1' C45 82.4(2) . . ? C52 Cl1' Cl3' 44.2(7) . . ? C52 Cl3' Cl1' 49.5(9) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.347 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.148