data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Franc Meyer' _publ_contact_author_email FRANC.MEYER@CHEMIE.UNI-GOETTINGEN.DE _publ_section_title ; Structural and Magnetic Variability of Cobalt(II) Complexes with Bridging Pyrazolate Ligands Bearing Appended Imine Groups ; loop_ _publ_author_name 'Franc Meyer' 'Serhiy Demeshko' 'Anna Sachse' # Attachment '_1_.cif' data_as24 _database_code_depnum_ccdc_archive 'CCDC 728434' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H53 Cl3 Co2 N4 O3, 1.5 (C H Cl3)' _chemical_formula_sum 'C35.50 H54.50 Cl7.50 Co2 N4 O3' _chemical_formula_weight 969.07 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Iba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, z+1/2' _cell_length_a 16.3211(11) _cell_length_b 17.7522(11) _cell_length_c 31.585(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9151.2(11) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 37227 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 26.58 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4008 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5469 _exptl_absorpt_correction_T_max 0.8225 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37227 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.58 _reflns_number_total 9530 _reflns_number_gt 9162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2007)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2007)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0505P)^2^+4.5552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(8) _refine_ls_number_reflns 9530 _refine_ls_number_parameters 519 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.005 _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 Co2 Co 0.485153(18) 0.348382(17) 0.337146(10) 0.01534(7) Uani 1 1 d . . . Co1 Co 0.619063(19) 0.402517(18) 0.454879(10) 0.01715(7) Uani 1 1 d . . . Cl3 Cl 0.38284(4) 0.35959(4) 0.388224(19) 0.02256(12) Uani 1 1 d . . . Cl2 Cl 0.58960(3) 0.43026(3) 0.314871(18) 0.02146(11) Uani 1 1 d . . . Cl1 Cl 0.63946(4) 0.50506(3) 0.49978(2) 0.02626(13) Uani 1 1 d . . . O1 O 0.49749(12) 0.39316(12) 0.46513(7) 0.0275(4) Uani 1 1 d . . . O2 O 0.65581(13) 0.46418(12) 0.40386(6) 0.0265(4) Uani 1 1 d . . . O3 O 0.41533(11) 0.39962(12) 0.28933(6) 0.0221(4) Uani 1 1 d . . . N1 N 0.60450(12) 0.30903(11) 0.41417(6) 0.0157(4) Uani 1 1 d . . . N2 N 0.56378(12) 0.29288(11) 0.37927(6) 0.0153(4) Uani 1 1 d . . . N3 N 0.69174(12) 0.32062(11) 0.48306(6) 0.0171(4) Uani 1 1 d . . . N4 N 0.49115(11) 0.24095(11) 0.31156(6) 0.0155(4) Uani 1 1 d . . . C1 C 0.62918(14) 0.18584(14) 0.39938(7) 0.0170(4) Uani 1 1 d . . . C2 C 0.64445(14) 0.24593(13) 0.42721(7) 0.0162(4) Uani 1 1 d . . . C3 C 0.57768(14) 0.21953(13) 0.36917(7) 0.0153(4) Uani 1 1 d . . . C4 C 0.65930(17) 0.10627(15) 0.40124(9) 0.0270(5) Uani 1 1 d . . . H4A H 0.6956 0.1005 0.4249 0.040 Uiso 1 1 calc R . . H4B H 0.6880 0.0945 0.3756 0.040 Uiso 1 1 calc R . . H4C H 0.6135 0.0728 0.4044 0.040 Uiso 1 1 calc R . . C5 C 0.69279(14) 0.25394(14) 0.46598(7) 0.0169(4) Uani 1 1 d . . . C6 C 0.73916(18) 0.18826(15) 0.48311(8) 0.0266(5) Uani 1 1 d . . . H6A H 0.7671 0.2029 0.5086 0.040 Uiso 1 1 calc R . . H6B H 0.7785 0.1717 0.4625 0.040 Uiso 1 1 calc R . . H6C H 0.7018 0.1480 0.4892 0.040 Uiso 1 1 calc R . . C7 C 0.73868(15) 0.33470(13) 0.52091(7) 0.0186(5) Uani 1 1 d . . . C8 C 0.82346(16) 0.34539(15) 0.51787(8) 0.0232(5) Uani 1 1 d . . . C9 C 0.86639(18) 0.35934(17) 0.55536(9) 0.0290(6) Uani 1 1 d . . . H9 H 0.9227 0.3672 0.5543 0.035 Uiso 1 1 calc R . . C10 C 0.8266(2) 0.36167(17) 0.59395(9) 0.0323(6) Uani 1 1 d . . . H10 H 0.8564 0.3693 0.6187 0.039 Uiso 1 1 calc R . . C11 C 0.7426(2) 0.35271(16) 0.59579(8) 0.0298(6) Uani 1 1 d . . . H11 H 0.7163 0.3550 0.6219 0.036 Uiso 1 1 calc R . . C12 C 0.69640(17) 0.34032(14) 0.55940(8) 0.0229(5) Uani 1 1 d . . . C13 C 0.86786(17) 0.34528(17) 0.47532(9) 0.0291(6) Uani 1 1 d . . . H13 H 0.8343 0.3158 0.4556 0.035 Uiso 1 1 calc R . . C14 C 0.8725(3) 0.4248(2) 0.45787(15) 0.0593(11) Uani 1 1 d . . . H14A H 0.9072 0.4549 0.4757 0.089 Uiso 1 1 calc R . . H14B H 0.8186 0.4464 0.4571 0.089 Uiso 1 1 calc R . . H14C H 0.8948 0.4236 0.4297 0.089 Uiso 1 1 calc R . . C15 C 0.9518(2) 0.3084(2) 0.47681(12) 0.0473(9) Uani 1 1 d . . . H15A H 0.9706 0.2992 0.4485 0.071 Uiso 1 1 calc R . . H15B H 0.9481 0.2615 0.4918 0.071 Uiso 1 1 calc R . . H15C H 0.9896 0.3412 0.4911 0.071 Uiso 1 1 calc R . . C16 C 0.60437(17) 0.32930(17) 0.56186(9) 0.0277(6) Uani 1 1 d . . . H16 H 0.5822 0.3378 0.5334 0.033 Uiso 1 1 calc R . . C17 C 0.5628(2) 0.3853(2) 0.59159(12) 0.0438(8) Uani 1 1 d . . . H17A H 0.5044 0.3795 0.5897 0.066 Uiso 1 1 calc R . . H17B H 0.5776 0.4357 0.5836 0.066 Uiso 1 1 calc R . . H17C H 0.5803 0.3760 0.6201 0.066 Uiso 1 1 calc R . . C18 C 0.5834(2) 0.24851(19) 0.57438(10) 0.0377(7) Uani 1 1 d . . . H18A H 0.6094 0.2366 0.6008 0.056 Uiso 1 1 calc R . . H18B H 0.6025 0.2146 0.5529 0.056 Uiso 1 1 calc R . . H18C H 0.5251 0.2436 0.5773 0.056 Uiso 1 1 calc R . . C19 C 0.53704(13) 0.19222(13) 0.33104(7) 0.0175(4) Uani 1 1 d . . . C20 C 0.54952(18) 0.11262(15) 0.31618(9) 0.0285(6) Uani 1 1 d . . . H20A H 0.5215 0.1053 0.2898 0.043 Uiso 1 1 calc R . . H20B H 0.5280 0.0783 0.3369 0.043 Uiso 1 1 calc R . . H20C H 0.6070 0.1033 0.3124 0.043 Uiso 1 1 calc R . . C21 C 0.44474(14) 0.22048(13) 0.27473(7) 0.0175(4) Uani 1 1 d . . . C22 C 0.37020(14) 0.18248(14) 0.27947(8) 0.0201(5) Uani 1 1 d . . . C23 C 0.32333(16) 0.16971(16) 0.24301(9) 0.0274(5) Uani 1 1 d . . . H23 H 0.2736 0.1445 0.2453 0.033 Uiso 1 1 calc R . . C24 C 0.34966(19) 0.19382(18) 0.20377(9) 0.0327(6) Uani 1 1 d . . . H24 H 0.3175 0.1852 0.1800 0.039 Uiso 1 1 calc R . . C25 C 0.42390(18) 0.23082(18) 0.19983(8) 0.0303(6) Uani 1 1 d . . . H25 H 0.4413 0.2465 0.1732 0.036 Uiso 1 1 calc R . . C26 C 0.47319(16) 0.24515(15) 0.23492(8) 0.0226(5) Uani 1 1 d . . . C27 C 0.33880(16) 0.15595(15) 0.32223(9) 0.0254(5) Uani 1 1 d . . . H27 H 0.3816 0.1662 0.3432 0.030 Uiso 1 1 calc R . . C28 C 0.32242(19) 0.07080(17) 0.32241(11) 0.0351(6) Uani 1 1 d . . . H28A H 0.2785 0.0595 0.3032 0.053 Uiso 1 1 calc R . . H28B H 0.3076 0.0551 0.3505 0.053 Uiso 1 1 calc R . . H28C H 0.3710 0.0445 0.3136 0.053 Uiso 1 1 calc R . . C29 C 0.26219(17) 0.19922(17) 0.33561(11) 0.0357(6) Uani 1 1 d . . . H29A H 0.2746 0.2520 0.3373 0.054 Uiso 1 1 calc R . . H29B H 0.2443 0.1816 0.3628 0.054 Uiso 1 1 calc R . . H29C H 0.2196 0.1913 0.3152 0.054 Uiso 1 1 calc R . . C30 C 0.55614(17) 0.28345(17) 0.23003(8) 0.0292(6) Uani 1 1 d . . . H30 H 0.5740 0.2992 0.2583 0.035 Uiso 1 1 calc R . . C31 C 0.6186(2) 0.2260(3) 0.21365(18) 0.0631(12) Uani 1 1 d . . . H31A H 0.6189 0.1828 0.2319 0.095 Uiso 1 1 calc R . . H31B H 0.6721 0.2485 0.2133 0.095 Uiso 1 1 calc R . . H31C H 0.6039 0.2109 0.1855 0.095 Uiso 1 1 calc R . . C32 C 0.5537(3) 0.3530(3) 0.20256(12) 0.0555(11) Uani 1 1 d . . . H32A H 0.5418 0.3388 0.1739 0.083 Uiso 1 1 calc R . . H32B H 0.6058 0.3780 0.2036 0.083 Uiso 1 1 calc R . . H32C H 0.5118 0.3865 0.2127 0.083 Uiso 1 1 calc R . . C33 C 0.32986(17) 0.38969(17) 0.28014(10) 0.0303(6) Uani 1 1 d . . . H33A H 0.2974 0.4124 0.3025 0.036 Uiso 1 1 calc R . . H33B H 0.3172 0.3363 0.2793 0.036 Uiso 1 1 calc R . . C34 C 0.3078(2) 0.4252(2) 0.23840(11) 0.0418(8) Uani 1 1 d . . . H34A H 0.3196 0.4781 0.2394 0.063 Uiso 1 1 calc R . . H34B H 0.2504 0.4179 0.2330 0.063 Uiso 1 1 calc R . . H34C H 0.3392 0.4021 0.2162 0.063 Uiso 1 1 calc R . . C35 C 0.7760(2) 0.06624(19) 0.59596(9) 0.0400(7) Uani 1 1 d . . . H35 H 0.8124 0.0369 0.5776 0.048 Uiso 1 1 calc R . . Cl4 Cl 0.78173(9) 0.02931(5) 0.64715(3) 0.0688(3) Uani 1 1 d . . . Cl5 Cl 0.80897(6) 0.16072(5) 0.59561(3) 0.0496(2) Uani 1 1 d . . . Cl6 Cl 0.67640(8) 0.05983(6) 0.57624(5) 0.0847(4) Uani 1 1 d . . . C36 C 0.9964(4) 0.5364(5) 0.69153(19) 0.066(2) Uani 0.50 1 d PD A -1 H36 H 0.9917 0.5890 0.7006 0.080 Uiso 0.50 1 calc PR A -1 Cl7 Cl 0.9235(2) 0.5011(2) 0.71754(11) 0.0728(10) Uani 0.50 1 d PD A -1 Cl8 Cl 0.9900(2) 0.5479(3) 0.63991(8) 0.1055(12) Uani 0.50 1 d PD A -1 Cl9 Cl 1.0962(2) 0.5201(2) 0.70437(14) 0.0774(11) Uani 0.50 1 d PD A -1 H2A H 0.643(3) 0.451(3) 0.3783(15) 0.049(11) Uiso 1 1 d . . . H1A H 0.469(2) 0.374(2) 0.4473(13) 0.033(9) Uiso 1 1 d . . . H1B H 0.465(3) 0.421(3) 0.4778(16) 0.060(13) Uiso 1 1 d . . . H2B H 0.648(2) 0.508(3) 0.4063(12) 0.037(10) Uiso 1 1 d . . . H3 H 0.422(2) 0.439(2) 0.2914(12) 0.030(10) Uiso 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 Co2 0.01731(14) 0.01333(13) 0.01536(14) -0.00031(12) -0.00229(12) 0.00168(11) Co1 0.01997(15) 0.01483(14) 0.01666(13) -0.00116(12) -0.00377(12) 0.00330(11) Cl3 0.0211(3) 0.0247(3) 0.0218(3) -0.0015(2) 0.0015(2) 0.0029(2) Cl2 0.0210(3) 0.0189(3) 0.0245(3) 0.0035(2) -0.0023(2) -0.0012(2) Cl1 0.0368(3) 0.0179(3) 0.0241(3) -0.0053(2) -0.0126(2) 0.0057(2) O1 0.0224(9) 0.0291(11) 0.0309(11) -0.0121(8) -0.0018(8) 0.0053(8) O2 0.0407(11) 0.0179(10) 0.0208(9) -0.0006(7) -0.0021(8) -0.0013(8) O3 0.0238(9) 0.0172(10) 0.0253(9) 0.0026(7) -0.0075(7) -0.0007(7) N1 0.0178(9) 0.0143(9) 0.0150(8) -0.0008(7) -0.0030(7) 0.0019(7) N2 0.0163(9) 0.0139(9) 0.0156(9) -0.0003(7) -0.0021(7) 0.0006(7) N3 0.0183(9) 0.0186(10) 0.0143(8) 0.0005(7) -0.0022(7) 0.0033(8) N4 0.0160(8) 0.0156(9) 0.0148(9) -0.0015(7) -0.0007(7) -0.0013(7) C1 0.0183(10) 0.0160(11) 0.0166(10) 0.0012(9) -0.0003(8) 0.0006(8) C2 0.0188(10) 0.0152(11) 0.0146(10) 0.0011(8) 0.0006(8) 0.0011(8) C3 0.0165(10) 0.0124(10) 0.0171(10) 0.0013(8) -0.0009(8) 0.0026(8) C4 0.0319(14) 0.0167(12) 0.0323(13) -0.0024(10) -0.0079(11) 0.0059(10) C5 0.0198(10) 0.0172(11) 0.0137(10) 0.0025(8) 0.0005(8) 0.0028(9) C6 0.0396(15) 0.0200(12) 0.0202(11) -0.0005(10) -0.0074(10) 0.0093(11) C7 0.0259(12) 0.0147(11) 0.0153(10) 0.0000(9) -0.0049(9) 0.0046(9) C8 0.0248(12) 0.0235(12) 0.0212(12) 0.0008(10) -0.0048(9) 0.0036(10) C9 0.0258(13) 0.0300(15) 0.0312(14) -0.0014(11) -0.0114(11) 0.0035(11) C10 0.0436(17) 0.0304(15) 0.0230(13) -0.0024(11) -0.0157(12) 0.0054(12) C11 0.0455(17) 0.0281(14) 0.0157(12) -0.0011(10) -0.0019(11) 0.0049(12) C12 0.0335(14) 0.0179(12) 0.0174(11) 0.0011(9) -0.0008(10) 0.0049(10) C13 0.0222(12) 0.0356(16) 0.0294(14) 0.0009(12) -0.0005(10) 0.0012(11) C14 0.070(3) 0.052(2) 0.057(2) 0.026(2) 0.026(2) 0.0164(19) C15 0.0365(17) 0.066(2) 0.0398(17) 0.0004(17) 0.0063(13) 0.0180(16) C16 0.0288(13) 0.0331(15) 0.0213(12) 0.0039(11) 0.0020(10) 0.0007(11) C17 0.0386(18) 0.0410(18) 0.052(2) -0.0062(16) 0.0180(14) -0.0004(14) C18 0.0461(17) 0.0342(16) 0.0326(15) -0.0019(13) 0.0017(13) -0.0075(13) C19 0.0172(10) 0.0158(11) 0.0195(11) -0.0019(9) 0.0014(9) 0.0008(8) C20 0.0325(14) 0.0226(13) 0.0304(14) -0.0087(11) -0.0083(11) 0.0071(10) C21 0.0201(11) 0.0159(11) 0.0164(11) -0.0044(8) -0.0026(8) 0.0020(8) C22 0.0182(11) 0.0185(12) 0.0237(12) -0.0046(9) -0.0011(9) -0.0006(9) C23 0.0226(12) 0.0256(13) 0.0339(14) -0.0051(11) -0.0065(11) -0.0008(10) C24 0.0378(15) 0.0344(16) 0.0260(13) -0.0056(11) -0.0133(11) -0.0023(12) C25 0.0374(15) 0.0364(16) 0.0170(11) -0.0010(10) -0.0069(11) -0.0055(12) C26 0.0264(12) 0.0228(12) 0.0187(11) -0.0026(10) -0.0021(9) -0.0004(10) C27 0.0222(12) 0.0261(13) 0.0278(12) -0.0009(10) 0.0007(10) -0.0044(10) C28 0.0347(15) 0.0242(14) 0.0465(17) 0.0071(12) 0.0056(12) 0.0002(11) C29 0.0314(14) 0.0285(14) 0.0471(16) -0.0079(13) 0.0151(13) -0.0081(11) C30 0.0332(14) 0.0364(16) 0.0181(11) -0.0040(11) 0.0017(10) -0.0102(12) C31 0.0315(17) 0.060(3) 0.098(3) -0.021(2) 0.0206(19) -0.0121(17) C32 0.057(2) 0.066(3) 0.044(2) 0.0202(18) 0.0007(17) -0.0288(19) C33 0.0220(13) 0.0297(14) 0.0392(15) 0.0072(12) -0.0099(11) -0.0013(10) C34 0.0390(16) 0.0443(18) 0.0420(18) 0.0065(14) -0.0240(14) -0.0021(14) C35 0.063(2) 0.0335(16) 0.0236(14) -0.0006(12) -0.0029(14) 0.0157(15) Cl4 0.1451(11) 0.0357(4) 0.0255(4) 0.0017(3) -0.0113(5) -0.0027(6) Cl5 0.0605(5) 0.0501(5) 0.0381(4) 0.0123(4) -0.0107(4) -0.0079(4) Cl6 0.0762(8) 0.0436(5) 0.1344(12) 0.0248(7) -0.0436(8) -0.0106(5) C36 0.083(6) 0.046(5) 0.070(5) 0.011(4) -0.027(5) -0.014(4) Cl7 0.087(2) 0.070(2) 0.0605(18) 0.0141(15) 0.0254(15) 0.0450(18) Cl8 0.096(2) 0.176(3) 0.0443(12) 0.0327(16) -0.0026(12) -0.035(2) Cl9 0.086(2) 0.065(2) 0.081(3) 0.0009(15) -0.0190(17) -0.0266(15) _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 Co2 4.4191(5) . ? Co2 N4 2.074(2) . ? Co2 N2 2.0947(19) . ? Co2 O3 2.0991(18) . ? Co2 Cl3 2.3304(7) . ? Co2 Cl2 2.3482(6) . ? Co1 O1 2.017(2) . ? Co1 O2 2.038(2) . ? Co1 N3 2.077(2) . ? Co1 N1 2.113(2) . ? Co1 Cl1 2.3315(7) . ? O3 C33 1.436(3) . ? N1 N2 1.319(3) . ? N1 C2 1.360(3) . ? N2 C3 1.360(3) . ? N3 C5 1.301(3) . ? N3 C7 1.442(3) . ? N4 C19 1.299(3) . ? N4 C21 1.435(3) . ? C1 C2 1.404(3) . ? C1 C3 1.405(3) . ? C1 C4 1.497(3) . ? C2 C5 1.464(3) . ? C3 C19 1.458(3) . ? C5 C6 1.492(3) . ? C7 C8 1.400(4) . ? C7 C12 1.401(4) . ? C8 C9 1.398(4) . ? C8 C13 1.527(4) . ? C9 C10 1.382(4) . ? C10 C11 1.382(5) . ? C11 C12 1.392(4) . ? C12 C16 1.517(4) . ? C13 C14 1.518(5) . ? C13 C15 1.518(4) . ? C16 C18 1.527(4) . ? C16 C17 1.527(4) . ? C19 C20 1.503(3) . ? C21 C22 1.399(3) . ? C21 C26 1.410(3) . ? C22 C23 1.401(4) . ? C22 C27 1.519(4) . ? C23 C24 1.380(4) . ? C24 C25 1.384(4) . ? C25 C26 1.393(4) . ? C26 C30 1.523(4) . ? C27 C29 1.527(4) . ? C27 C28 1.535(4) . ? C30 C32 1.510(5) . ? C30 C31 1.532(5) . ? C33 C34 1.505(4) . ? C35 Cl6 1.745(4) . ? C35 Cl4 1.747(3) . ? C35 Cl5 1.761(4) . ? C36 Cl7 1.576(6) . ? C36 Cl8 1.647(6) . ? C36 Cl9 1.703(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 N4 Co2 N2 77.64(8) . . ? N4 Co2 O3 98.27(8) . . ? N2 Co2 O3 173.38(8) . . ? N4 Co2 Cl3 112.46(6) . . ? N2 Co2 Cl3 92.26(6) . . ? O3 Co2 Cl3 94.13(6) . . ? N4 Co2 Cl2 114.73(6) . . ? N2 Co2 Cl2 92.10(6) . . ? O3 Co2 Cl2 84.86(6) . . ? Cl3 Co2 Cl2 132.43(3) . . ? O1 Co1 O2 117.42(9) . . ? O1 Co1 N3 115.81(8) . . ? O2 Co1 N3 123.14(8) . . ? O1 Co1 N1 85.55(8) . . ? O2 Co1 N1 88.49(8) . . ? N3 Co1 N1 77.01(8) . . ? O1 Co1 Cl1 96.15(6) . . ? O2 Co1 Cl1 91.13(6) . . ? N3 Co1 Cl1 101.79(6) . . ? N1 Co1 Cl1 178.24(6) . . ? C33 O3 Co2 128.30(16) . . ? N2 N1 C2 108.41(19) . . ? N2 N1 Co1 137.40(15) . . ? C2 N1 Co1 114.12(15) . . ? N1 N2 C3 108.67(18) . . ? N1 N2 Co2 137.51(16) . . ? C3 N2 Co2 113.81(15) . . ? C5 N3 C7 119.64(19) . . ? C5 N3 Co1 117.83(15) . . ? C7 N3 Co1 122.52(15) . . ? C19 N4 C21 121.3(2) . . ? C19 N4 Co2 117.08(15) . . ? C21 N4 Co2 121.59(15) . . ? C2 C1 C3 102.0(2) . . ? C2 C1 C4 129.3(2) . . ? C3 C1 C4 128.7(2) . . ? N1 C2 C1 110.5(2) . . ? N1 C2 C5 115.6(2) . . ? C1 C2 C5 133.9(2) . . ? N2 C3 C1 110.4(2) . . ? N2 C3 C19 115.87(19) . . ? C1 C3 C19 133.8(2) . . ? N3 C5 C2 115.4(2) . . ? N3 C5 C6 124.6(2) . . ? C2 C5 C6 120.1(2) . . ? C8 C7 C12 122.5(2) . . ? C8 C7 N3 119.5(2) . . ? C12 C7 N3 118.0(2) . . ? C9 C8 C7 117.5(2) . . ? C9 C8 C13 120.5(2) . . ? C7 C8 C13 122.0(2) . . ? C10 C9 C8 121.1(3) . . ? C9 C10 C11 120.0(2) . . ? C10 C11 C12 121.4(3) . . ? C11 C12 C7 117.5(3) . . ? C11 C12 C16 120.9(2) . . ? C7 C12 C16 121.5(2) . . ? C14 C13 C15 111.5(3) . . ? C14 C13 C8 110.0(3) . . ? C15 C13 C8 113.7(3) . . ? C12 C16 C18 110.9(2) . . ? C12 C16 C17 112.8(3) . . ? C18 C16 C17 110.7(2) . . ? N4 C19 C3 115.6(2) . . ? N4 C19 C20 123.8(2) . . ? C3 C19 C20 120.6(2) . . ? C22 C21 C26 122.1(2) . . ? C22 C21 N4 119.6(2) . . ? C26 C21 N4 118.1(2) . . ? C21 C22 C23 117.7(2) . . ? C21 C22 C27 122.5(2) . . ? C23 C22 C27 119.8(2) . . ? C24 C23 C22 121.2(2) . . ? C23 C24 C25 120.0(2) . . ? C24 C25 C26 121.4(3) . . ? C25 C26 C21 117.6(2) . . ? C25 C26 C30 121.0(2) . . ? C21 C26 C30 121.5(2) . . ? C22 C27 C29 111.5(2) . . ? C22 C27 C28 111.5(2) . . ? C29 C27 C28 110.6(2) . . ? C32 C30 C26 113.6(3) . . ? C32 C30 C31 111.6(3) . . ? C26 C30 C31 109.2(3) . . ? O3 C33 C34 111.0(2) . . ? Cl6 C35 Cl4 110.8(2) . . ? Cl6 C35 Cl5 110.14(17) . . ? Cl4 C35 Cl5 110.30(18) . . ? Cl7 C36 Cl8 121.2(4) . . ? Cl7 C36 Cl9 122.0(4) . . ? Cl8 C36 Cl9 108.5(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A Cl3 0.81(4) 2.35(4) 3.123(2) 161(4) . O2 H2A Cl2 0.87(5) 2.22(5) 3.071(2) 169(4) . O3 H3 Cl2 0.71(4) 2.44(4) 3.127(2) 162(4) 2_665 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.58 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.582 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.052 # Attachment '_2_.cif' data_as49 _database_code_depnum_ccdc_archive 'CCDC 728435' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C105 H123 N12 Co4 Cl5, 0.5 (C4 H8 O), C2 H3 N' _chemical_formula_sum 'C109 H130 Cl5 Co4 N13 O0.50' _chemical_formula_weight 2043.23 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.5141(4) _cell_length_b 22.4226(4) _cell_length_c 31.4461(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.388(2) _cell_angle_gamma 90.00 _cell_volume 11373.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 86436 _cell_measurement_theta_min 1.12 _cell_measurement_theta_max 25.74 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4288 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4799 _exptl_absorpt_correction_T_max 0.8394 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86436 _diffrn_reflns_av_R_equivalents 0.1459 _diffrn_reflns_av_sigmaI/netI 0.0899 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 25.74 _reflns_number_total 21492 _reflns_number_gt 16904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2007)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2007)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1377P)^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 21492 _refine_ls_number_parameters 1210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.2050 _refine_ls_wR_factor_gt 0.1914 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.63179(3) 0.82220(2) 0.923275(15) 0.02754(13) Uani 1 1 d . . . Co2 Co 0.48613(3) 0.73808(2) 0.812230(14) 0.02688(12) Uani 1 1 d . . . Co3 Co 0.60840(3) 0.61810(2) 0.767673(15) 0.03081(13) Uani 1 1 d . . . Co4 Co 0.65360(3) 0.65786(2) 0.902828(14) 0.02827(13) Uani 1 1 d . . . Cl1 Cl 0.67048(6) 0.73423(4) 0.95834(3) 0.03234(19) Uani 1 1 d . . . Cl2 Cl 0.50445(5) 0.66591(4) 0.87364(3) 0.03254(19) Uani 1 1 d . . . Cl3 Cl 0.48510(6) 0.66751(4) 0.75352(3) 0.0344(2) Uani 1 1 d . . . Cl4 Cl 0.73319(6) 0.87034(4) 0.90320(3) 0.0428(2) Uani 1 1 d . . . Cl5 Cl 0.70055(8) 0.65951(5) 0.73652(4) 0.0540(3) Uani 1 1 d . . . N1 N 0.51096(19) 0.82068(13) 0.89326(9) 0.0284(6) Uani 1 1 d . . . N2 N 0.46269(18) 0.79406(12) 0.85946(9) 0.0267(6) Uani 1 1 d . . . N3 N 0.58335(18) 0.87361(13) 0.96733(9) 0.0279(6) Uani 1 1 d . . . N4 N 0.35093(19) 0.73419(13) 0.80283(9) 0.0305(6) Uani 1 1 d . . . N11 N 0.62985(18) 0.57104(13) 0.82358(9) 0.0283(6) Uani 1 1 d . . . N12 N 0.64151(19) 0.58178(13) 0.86566(9) 0.0295(6) Uani 1 1 d . . . N13 N 0.58959(19) 0.53203(14) 0.74204(9) 0.0311(6) Uani 1 1 d . . . N14 N 0.6367(2) 0.58823(13) 0.94986(9) 0.0318(6) Uani 1 1 d . . . N21 N 0.61172(18) 0.74464(12) 0.82599(9) 0.0270(6) Uani 1 1 d . . . N22 N 0.66889(18) 0.71517(13) 0.85509(9) 0.0273(6) Uani 1 1 d . . . N23 N 0.52037(19) 0.81687(13) 0.76693(9) 0.0289(6) Uani 1 1 d . . . N24 N 0.80293(19) 0.66394(13) 0.90523(10) 0.0308(6) Uani 1 1 d . . . C1 C 0.3795(2) 0.82407(15) 0.90383(11) 0.0290(7) Uani 1 1 d . . . C2 C 0.4615(2) 0.83966(15) 0.92055(11) 0.0279(7) Uani 1 1 d . . . C3 C 0.3835(2) 0.79450(15) 0.86490(11) 0.0281(7) Uani 1 1 d . . . C4 C 0.3079(2) 0.83349(16) 0.92381(12) 0.0325(8) Uani 1 1 d . . . C5 C 0.3141(3) 0.82006(18) 0.96756(14) 0.0413(9) Uani 1 1 d . . . H5 H 0.3635 0.8050 0.9839 0.050 Uiso 1 1 calc R . . C6 C 0.2475(3) 0.8288(2) 0.98715(17) 0.0557(13) Uani 1 1 d . . . H6 H 0.2518 0.8189 1.0163 0.067 Uiso 1 1 calc R . . C7 C 0.1743(3) 0.8524(2) 0.96289(19) 0.0614(15) Uani 1 1 d . . . H7 H 0.1297 0.8594 0.9760 0.074 Uiso 1 1 calc R . . C8 C 0.1675(3) 0.8655(2) 0.91988(19) 0.0575(13) Uani 1 1 d . . . H8 H 0.1181 0.8810 0.9038 0.069 Uiso 1 1 calc R . . C9 C 0.2335(3) 0.85596(19) 0.89971(14) 0.0419(9) Uani 1 1 d . . . H9 H 0.2280 0.8645 0.8703 0.050 Uiso 1 1 calc R . . C10 C 0.5039(2) 0.87221(15) 0.95882(11) 0.0289(7) Uani 1 1 d . . . H10 H 0.4741 0.8916 0.9767 0.035 Uiso 1 1 calc R . . C11 C 0.6245(2) 0.91034(16) 1.00317(11) 0.0295(7) Uani 1 1 d . . . C12 C 0.6460(2) 0.88528(16) 1.04467(12) 0.0330(8) Uani 1 1 d . . . C13 C 0.6816(2) 0.92335(18) 1.07879(12) 0.0382(8) Uani 1 1 d . . . H13 H 0.6962 0.9083 1.1070 0.046 Uiso 1 1 calc R . . C14 C 0.6954(3) 0.98269(19) 1.07152(13) 0.0427(9) Uani 1 1 d . . . H14 H 0.7170 1.0076 1.0948 0.051 Uiso 1 1 calc R . . C15 C 0.6774(3) 1.00538(18) 1.02954(13) 0.0393(9) Uani 1 1 d . . . H15 H 0.6893 1.0451 1.0249 0.047 Uiso 1 1 calc R . . C16 C 0.6419(2) 0.96986(16) 0.99440(11) 0.0310(7) Uani 1 1 d . . . C17 C 0.6328(3) 0.81908(18) 1.05254(13) 0.0411(9) Uani 1 1 d . . . H17 H 0.6184 0.7994 1.0241 0.049 Uiso 1 1 calc R . . C18 C 0.5606(3) 0.8102(2) 1.07498(17) 0.0552(12) Uani 1 1 d . . . H18A H 0.5120 0.8292 1.0582 0.083 Uiso 1 1 calc R . . H18B H 0.5741 0.8275 1.1036 0.083 Uiso 1 1 calc R . . H18C H 0.5501 0.7683 1.0773 0.083 Uiso 1 1 calc R . . C19 C 0.7113(3) 0.7898(2) 1.07833(16) 0.0574(12) Uani 1 1 d . . . H19A H 0.7008 0.7483 1.0826 0.086 Uiso 1 1 calc R . . H19B H 0.7278 0.8090 1.1061 0.086 Uiso 1 1 calc R . . H19C H 0.7547 0.7934 1.0625 0.086 Uiso 1 1 calc R . . C20 C 0.6208(3) 0.99517(17) 0.94858(12) 0.0377(8) Uani 1 1 d . . . H20 H 0.6119 0.9611 0.9286 0.045 Uiso 1 1 calc R . . C21 C 0.6909(4) 1.0318(2) 0.93758(16) 0.0643(15) Uani 1 1 d . . . H21A H 0.7409 1.0085 0.9429 0.096 Uiso 1 1 calc R . . H21B H 0.6994 1.0670 0.9554 0.096 Uiso 1 1 calc R . . H21C H 0.6769 1.0432 0.9074 0.096 Uiso 1 1 calc R . . C22 C 0.5414(4) 1.0300(3) 0.94034(16) 0.0687(16) Uani 1 1 d . . . H22A H 0.5301 1.0452 0.9111 0.103 Uiso 1 1 calc R . . H22B H 0.5465 1.0626 0.9605 0.103 Uiso 1 1 calc R . . H22C H 0.4968 1.0044 0.9441 0.103 Uiso 1 1 calc R . . C23 C 0.3238(2) 0.76148(16) 0.83301(11) 0.0313(7) Uani 1 1 d . . . H23 H 0.2681 0.7601 0.8343 0.038 Uiso 1 1 calc R . . C24 C 0.2902(2) 0.70237(18) 0.77032(12) 0.0347(8) Uani 1 1 d . . . C25 C 0.2804(2) 0.64057(18) 0.77476(13) 0.0386(8) Uani 1 1 d . . . C26 C 0.2235(3) 0.6113(2) 0.74184(15) 0.0483(10) Uani 1 1 d . . . H26 H 0.2154 0.5705 0.7439 0.058 Uiso 1 1 calc R . . C27 C 0.1795(3) 0.6419(2) 0.70657(15) 0.0532(12) Uani 1 1 d . . . H27 H 0.1428 0.6215 0.6849 0.064 Uiso 1 1 calc R . . C28 C 0.1890(3) 0.7028(2) 0.70294(14) 0.0479(10) Uani 1 1 d . . . H28 H 0.1573 0.7231 0.6794 0.057 Uiso 1 1 calc R . . C29 C 0.2464(2) 0.73441(19) 0.73446(12) 0.0386(9) Uani 1 1 d . . . C30 C 0.3247(3) 0.6062(2) 0.81422(15) 0.0472(10) Uani 1 1 d . . . H30 H 0.3711 0.6308 0.8293 0.057 Uiso 1 1 calc R . . C31 C 0.2678(4) 0.5962(3) 0.84545(18) 0.0821(19) Uani 1 1 d . . . H31A H 0.2968 0.5743 0.8703 0.123 Uiso 1 1 calc R . . H31B H 0.2201 0.5739 0.8311 0.123 Uiso 1 1 calc R . . H31C H 0.2504 0.6340 0.8547 0.123 Uiso 1 1 calc R . . C32 C 0.3605(4) 0.5473(2) 0.8029(2) 0.0672(14) Uani 1 1 d . . . H32A H 0.3880 0.5276 0.8291 0.101 Uiso 1 1 calc R . . H32B H 0.3996 0.5547 0.7848 0.101 Uiso 1 1 calc R . . H32C H 0.3166 0.5224 0.7874 0.101 Uiso 1 1 calc R . . C33 C 0.2538(3) 0.8018(2) 0.73042(14) 0.0472(10) Uani 1 1 d . . . H33 H 0.3077 0.8136 0.7482 0.057 Uiso 1 1 calc R . . C34 C 0.2511(4) 0.8222(3) 0.68421(16) 0.0612(13) Uani 1 1 d . . . H34A H 0.2565 0.8648 0.6837 0.092 Uiso 1 1 calc R . . H34B H 0.1993 0.8106 0.6659 0.092 Uiso 1 1 calc R . . H34C H 0.2959 0.8042 0.6738 0.092 Uiso 1 1 calc R . . C35 C 0.1868(4) 0.8338(2) 0.74857(17) 0.0610(13) Uani 1 1 d . . . H35A H 0.1931 0.8762 0.7459 0.091 Uiso 1 1 calc R . . H35B H 0.1923 0.8236 0.7787 0.091 Uiso 1 1 calc R . . H35C H 0.1331 0.8219 0.7325 0.091 Uiso 1 1 calc R . . C101 C 0.6093(2) 0.48387(16) 0.85604(11) 0.0304(7) Uani 1 1 d . . . C102 C 0.6104(2) 0.51196(16) 0.81657(11) 0.0296(7) Uani 1 1 d . . . C103 C 0.6277(2) 0.53089(15) 0.88629(11) 0.0308(7) Uani 1 1 d . . . C104 C 0.5966(2) 0.42043(16) 0.86512(11) 0.0336(8) Uani 1 1 d . . . C105 C 0.5280(3) 0.38909(17) 0.84291(13) 0.0371(8) Uani 1 1 d . . . H105 H 0.4880 0.4085 0.8222 0.045 Uiso 1 1 calc R . . C106 C 0.5186(3) 0.32861(18) 0.85135(14) 0.0448(10) Uani 1 1 d . . . H106 H 0.4721 0.3081 0.8365 0.054 Uiso 1 1 calc R . . C107 C 0.5782(3) 0.29916(19) 0.88166(16) 0.0504(11) Uani 1 1 d . . . H107 H 0.5723 0.2587 0.8868 0.061 Uiso 1 1 calc R . . C108 C 0.6468(3) 0.3300(2) 0.90442(16) 0.0533(11) Uani 1 1 d . . . H108 H 0.6870 0.3105 0.9249 0.064 Uiso 1 1 calc R . . C109 C 0.6549(3) 0.39051(18) 0.89620(14) 0.0447(10) Uani 1 1 d . . . H109 H 0.7003 0.4113 0.9119 0.054 Uiso 1 1 calc R . . C110 C 0.5958(2) 0.49215(16) 0.77181(11) 0.0312(7) Uani 1 1 d . . . H110 H 0.5910 0.4518 0.7648 0.037 Uiso 1 1 calc R . . C111 C 0.5820(2) 0.51341(16) 0.69768(11) 0.0330(8) Uani 1 1 d . . . C112 C 0.6537(3) 0.49888(17) 0.68349(13) 0.0393(9) Uani 1 1 d . . . C113 C 0.6439(3) 0.4779(2) 0.64073(14) 0.0497(11) Uani 1 1 d . . . H113 H 0.6903 0.4660 0.6306 0.060 Uiso 1 1 calc R . . C114 C 0.5667(4) 0.4746(2) 0.61350(14) 0.0530(12) Uani 1 1 d . . . H114 H 0.5615 0.4602 0.5853 0.064 Uiso 1 1 calc R . . C115 C 0.4967(3) 0.49260(19) 0.62775(13) 0.0487(10) Uani 1 1 d . . . H115 H 0.4453 0.4914 0.6086 0.058 Uiso 1 1 calc R . . C116 C 0.5024(3) 0.51257(17) 0.67050(12) 0.0388(8) Uani 1 1 d . . . C117 C 0.7388(3) 0.50491(18) 0.71263(14) 0.0423(9) Uani 1 1 d . . . H117 H 0.7335 0.5291 0.7378 0.051 Uiso 1 1 calc R . . C118 C 0.7730(3) 0.44374(19) 0.72948(16) 0.0501(10) Uani 1 1 d . . . H11A H 0.8270 0.4485 0.7479 0.075 Uiso 1 1 calc R . . H11B H 0.7769 0.4186 0.7053 0.075 Uiso 1 1 calc R . . H11C H 0.7365 0.4258 0.7458 0.075 Uiso 1 1 calc R . . C119 C 0.7999(3) 0.5364(2) 0.6898(2) 0.0621(13) Uani 1 1 d . . . H11D H 0.8529 0.5394 0.7094 0.093 Uiso 1 1 calc R . . H11E H 0.7796 0.5756 0.6811 0.093 Uiso 1 1 calc R . . H11F H 0.8053 0.5139 0.6646 0.093 Uiso 1 1 calc R . . C120 C 0.4269(3) 0.5327(2) 0.68581(13) 0.0434(9) Uani 1 1 d . . . H120 H 0.4455 0.5479 0.7155 0.052 Uiso 1 1 calc R . . C121 C 0.3679(3) 0.4809(3) 0.68761(19) 0.0659(14) Uani 1 1 d . . . H12A H 0.3205 0.4951 0.6977 0.099 Uiso 1 1 calc R . . H12B H 0.3958 0.4509 0.7072 0.099 Uiso 1 1 calc R . . H12C H 0.3502 0.4641 0.6591 0.099 Uiso 1 1 calc R . . C122 C 0.3821(3) 0.5839(2) 0.65781(16) 0.0578(12) Uani 1 1 d . . . H12D H 0.3344 0.5957 0.6687 0.087 Uiso 1 1 calc R . . H12E H 0.3648 0.5708 0.6282 0.087 Uiso 1 1 calc R . . H12F H 0.4191 0.6172 0.6591 0.087 Uiso 1 1 calc R . . C123 C 0.6242(2) 0.53621(16) 0.93153(11) 0.0322(7) Uani 1 1 d . . . H123 H 0.6132 0.5031 0.9472 0.039 Uiso 1 1 calc R . . C124 C 0.6310(3) 0.59156(16) 0.99502(11) 0.0360(8) Uani 1 1 d . . . C125 C 0.7035(3) 0.5818(2) 1.02699(13) 0.0452(10) Uani 1 1 d . . . C126 C 0.6968(4) 0.5840(2) 1.06983(15) 0.0586(12) Uani 1 1 d . . . H126 H 0.7438 0.5769 1.0914 0.070 Uiso 1 1 calc R . . C127 C 0.6239(4) 0.5961(2) 1.08188(14) 0.0593(13) Uani 1 1 d . . . H127 H 0.6220 0.5973 1.1112 0.071 Uiso 1 1 calc R . . C128 C 0.5522(3) 0.6067(2) 1.05023(14) 0.0521(11) Uani 1 1 d . . . H128 H 0.5024 0.6149 1.0584 0.063 Uiso 1 1 calc R . . C129 C 0.5553(3) 0.60486(17) 1.00595(13) 0.0399(9) Uani 1 1 d . . . C130 C 0.7841(3) 0.5678(3) 1.01436(15) 0.0584(12) Uani 1 1 d . . . H130 H 0.7825 0.5857 0.9858 0.070 Uiso 1 1 calc R . . C131 C 0.7958(4) 0.4997(3) 1.0101(2) 0.089(2) Uani 1 1 d . . . H13A H 0.8478 0.4921 1.0021 0.133 Uiso 1 1 calc R . . H13B H 0.7514 0.4841 0.9881 0.133 Uiso 1 1 calc R . . H13C H 0.7954 0.4808 1.0375 0.133 Uiso 1 1 calc R . . C132 C 0.8602(4) 0.5913(4) 1.04534(19) 0.087(2) Uani 1 1 d . . . H13D H 0.9088 0.5805 1.0350 0.131 Uiso 1 1 calc R . . H13E H 0.8633 0.5744 1.0737 0.131 Uiso 1 1 calc R . . H13F H 0.8568 0.6340 1.0470 0.131 Uiso 1 1 calc R . . C133 C 0.4765(3) 0.61746(19) 0.97243(14) 0.0454(10) Uani 1 1 d . . . H133 H 0.4889 0.6119 0.9436 0.055 Uiso 1 1 calc R . . C134 C 0.4065(3) 0.5750(2) 0.97598(17) 0.0590(12) Uani 1 1 d . . . H13G H 0.3583 0.5847 0.9541 0.088 Uiso 1 1 calc R . . H13H H 0.3939 0.5788 1.0043 0.088 Uiso 1 1 calc R . . H13I H 0.4232 0.5348 0.9719 0.088 Uiso 1 1 calc R . . C135 C 0.4485(4) 0.6820(2) 0.97536(18) 0.0587(13) Uani 1 1 d . . . H13J H 0.3988 0.6889 0.9537 0.088 Uiso 1 1 calc R . . H13K H 0.4913 0.7084 0.9704 0.088 Uiso 1 1 calc R . . H13L H 0.4380 0.6892 1.0038 0.088 Uiso 1 1 calc R . . C201 C 0.7371(2) 0.77117(15) 0.81467(11) 0.0285(7) Uani 1 1 d . . . C202 C 0.6511(2) 0.77883(15) 0.80136(11) 0.0283(7) Uani 1 1 d . . . C203 C 0.7441(2) 0.73057(15) 0.84880(11) 0.0271(7) Uani 1 1 d . . . C204 C 0.8049(2) 0.79739(16) 0.79719(12) 0.0307(7) Uani 1 1 d . . . C205 C 0.8046(3) 0.79472(17) 0.75296(13) 0.0361(8) Uani 1 1 d . . . H205 H 0.7595 0.7782 0.7337 0.043 Uiso 1 1 calc R . . C206 C 0.8715(3) 0.81672(18) 0.73762(15) 0.0434(9) Uani 1 1 d . . . H206 H 0.8710 0.8150 0.7080 0.052 Uiso 1 1 calc R . . C207 C 0.9392(3) 0.84122(18) 0.76606(15) 0.0431(9) Uani 1 1 d . . . H207 H 0.9844 0.8550 0.7557 0.052 Uiso 1 1 calc R . . C208 C 0.9392(3) 0.84508(18) 0.80987(15) 0.0424(9) Uani 1 1 d . . . H208 H 0.9841 0.8623 0.8289 0.051 Uiso 1 1 calc R . . C209 C 0.8731(2) 0.82355(17) 0.82571(13) 0.0362(8) Uani 1 1 d . . . H209 H 0.8736 0.8263 0.8553 0.043 Uiso 1 1 calc R . . C210 C 0.5995(2) 0.81696(15) 0.77052(11) 0.0294(7) Uani 1 1 d . . . H210 H 0.6233 0.8420 0.7530 0.035 Uiso 1 1 calc R . . C211 C 0.4769(2) 0.85839(17) 0.73482(12) 0.0344(8) Uani 1 1 d . . . C212 C 0.4380(2) 0.90740(17) 0.74982(12) 0.0351(8) Uani 1 1 d . . . C213 C 0.4027(3) 0.95037(18) 0.71911(14) 0.0456(10) Uani 1 1 d . . . H213 H 0.3770 0.9835 0.7281 0.055 Uiso 1 1 calc R . . C214 C 0.4053(3) 0.9445(2) 0.67576(14) 0.0566(12) Uani 1 1 d . . . H214 H 0.3823 0.9738 0.6559 0.068 Uiso 1 1 calc R . . C215 C 0.4420(3) 0.8950(2) 0.66192(14) 0.0552(12) Uani 1 1 d . . . H215 H 0.4428 0.8912 0.6326 0.066 Uiso 1 1 calc R . . C216 C 0.4781(3) 0.85052(19) 0.69101(13) 0.0440(9) Uani 1 1 d . . . C217 C 0.4394(2) 0.91562(17) 0.79767(13) 0.0369(8) Uani 1 1 d . . . H217 H 0.4417 0.8757 0.8105 0.044 Uiso 1 1 calc R . . C218 C 0.5170(3) 0.9479(3) 0.82032(15) 0.0563(12) Uani 1 1 d . . . H21D H 0.5166 0.9525 0.8506 0.085 Uiso 1 1 calc R . . H21E H 0.5189 0.9865 0.8074 0.085 Uiso 1 1 calc R . . H21F H 0.5649 0.9253 0.8174 0.085 Uiso 1 1 calc R . . C219 C 0.3627(3) 0.9460(2) 0.80695(17) 0.0562(12) Uani 1 1 d . . . H21G H 0.3680 0.9496 0.8378 0.084 Uiso 1 1 calc R . . H21H H 0.3146 0.9226 0.7949 0.084 Uiso 1 1 calc R . . H21I H 0.3572 0.9849 0.7940 0.084 Uiso 1 1 calc R . . C220 C 0.5169(3) 0.7970(2) 0.67340(14) 0.0522(11) Uani 1 1 d . . . H220 H 0.5404 0.7713 0.6982 0.063 Uiso 1 1 calc R . . C221 C 0.5879(5) 0.8153(3) 0.6517(2) 0.0760(18) Uani 1 1 d . . . H22D H 0.6111 0.7804 0.6411 0.114 Uiso 1 1 calc R . . H22E H 0.6301 0.8354 0.6725 0.114 Uiso 1 1 calc R . . H22F H 0.5670 0.8416 0.6277 0.114 Uiso 1 1 calc R . . C222 C 0.4503(4) 0.7604(3) 0.64208(17) 0.0755(18) Uani 1 1 d . . . H22G H 0.4759 0.7269 0.6313 0.113 Uiso 1 1 calc R . . H22H H 0.4241 0.7851 0.6181 0.113 Uiso 1 1 calc R . . H22I H 0.4094 0.7465 0.6574 0.113 Uiso 1 1 calc R . . C223 C 0.8142(2) 0.70175(16) 0.87631(11) 0.0308(7) Uani 1 1 d . . . H223 H 0.8677 0.7105 0.8731 0.037 Uiso 1 1 calc R . . C224 C 0.8793(2) 0.64295(19) 0.93223(13) 0.0393(9) Uani 1 1 d . . . C225 C 0.9051(3) 0.5845(2) 0.92611(15) 0.0480(10) Uani 1 1 d . . . C226 C 0.9801(3) 0.5656(2) 0.95242(19) 0.0616(13) Uani 1 1 d . . . H226 H 0.9985 0.5268 0.9498 0.074 Uiso 1 1 calc R . . C227 C 1.0275(3) 0.6043(3) 0.9826(2) 0.0713(16) Uani 1 1 d . . . H227 H 1.0774 0.5911 0.9996 0.086 Uiso 1 1 calc R . . C228 C 1.0019(3) 0.6612(2) 0.98742(17) 0.0583(12) Uani 1 1 d . . . H228 H 1.0349 0.6864 1.0075 0.070 Uiso 1 1 calc R . . C229 C 0.9266(3) 0.6824(2) 0.96270(14) 0.0443(9) Uani 1 1 d . . . C230 C 0.8547(3) 0.54481(19) 0.89110(17) 0.0507(11) Uani 1 1 d . . . H230 H 0.7961 0.5545 0.8891 0.061 Uiso 1 1 calc R . . C231 C 0.8741(4) 0.5576(3) 0.84706(19) 0.0669(14) Uani 1 1 d . . . H23A H 0.8414 0.5320 0.8256 0.100 Uiso 1 1 calc R . . H23B H 0.9319 0.5505 0.8483 0.100 Uiso 1 1 calc R . . H23C H 0.8613 0.5985 0.8394 0.100 Uiso 1 1 calc R . . C232 C 0.8649(4) 0.4779(2) 0.9003(2) 0.0761(17) Uani 1 1 d . . . H23D H 0.8311 0.4560 0.8767 0.114 Uiso 1 1 calc R . . H23E H 0.8480 0.4687 0.9269 0.114 Uiso 1 1 calc R . . H23F H 0.9219 0.4669 0.9029 0.114 Uiso 1 1 calc R . . C233 C 0.9013(3) 0.7465(2) 0.96880(14) 0.0463(10) Uani 1 1 d . . . H233 H 0.8462 0.7528 0.9502 0.056 Uiso 1 1 calc R . . C234 C 0.9611(3) 0.7898(2) 0.95387(17) 0.0582(12) Uani 1 1 d . . . H23G H 0.9443 0.8300 0.9578 0.087 Uiso 1 1 calc R . . H23H H 0.9604 0.7831 0.9236 0.087 Uiso 1 1 calc R . . H23I H 1.0161 0.7834 0.9708 0.087 Uiso 1 1 calc R . . C235 C 0.8956(4) 0.7595(3) 1.01532(17) 0.0691(15) Uani 1 1 d . . . H23J H 0.8796 0.8003 1.0177 0.104 Uiso 1 1 calc R . . H23K H 0.9485 0.7526 1.0343 0.104 Uiso 1 1 calc R . . H23L H 0.8550 0.7337 1.0234 0.104 Uiso 1 1 calc R . . O1 O 1.1319(3) 0.7388(3) 0.8358(2) 0.0475(15) Uani 0.50 1 d P . . C301 C 1.0787(5) 0.7080(4) 0.7995(3) 0.0432(19) Uani 0.50 1 d P . . H30A H 1.0511 0.7365 0.7780 0.052 Uiso 0.50 1 calc PR . . H30B H 1.1113 0.6812 0.7857 0.052 Uiso 0.50 1 calc PR . . C302 C 1.0181(6) 0.6746(5) 0.8172(4) 0.059(3) Uani 0.50 1 d P . . H30C H 1.0079 0.6359 0.8032 0.071 Uiso 0.50 1 calc PR . . H30D H 0.9661 0.6962 0.8130 0.071 Uiso 0.50 1 calc PR . . C303 C 1.0566(6) 0.6677(4) 0.8652(3) 0.053(2) Uani 0.50 1 d P . . H30E H 1.0147 0.6671 0.8826 0.064 Uiso 0.50 1 calc PR . . H30F H 1.0900 0.6319 0.8708 0.064 Uiso 0.50 1 calc PR . . C304 C 1.1070(6) 0.7208(4) 0.8733(3) 0.055(2) Uani 0.50 1 d P . . H30G H 1.0756 0.7526 0.8831 0.065 Uiso 0.50 1 calc PR . . H30H H 1.1555 0.7129 0.8961 0.065 Uiso 0.50 1 calc PR . . N31 N 1.0237(7) 0.9271(5) 1.0146(3) 0.0726(19) Uani 0.50 1 d P . . C305 C 0.9546(7) 0.9342(5) 1.0143(3) 0.0573(12) Uani 0.50 1 d P . . C306 C 0.8724(7) 0.9428(5) 1.0112(3) 0.0573(12) Uani 0.50 1 d P . . H30I H 0.8595 0.9843 1.0059 0.086 Uiso 0.50 1 calc PR . . H30J H 0.8578 0.9309 1.0379 0.086 Uiso 0.50 1 calc PR . . H30K H 0.8417 0.9195 0.9876 0.086 Uiso 0.50 1 calc PR . . N32 N 0.1425(7) 0.7786(5) 1.0645(3) 0.0726(19) Uani 0.50 1 d P . . C307 C 0.1467(7) 0.8163(4) 1.0888(3) 0.0573(12) Uani 0.50 1 d P . . C308 C 0.1157(7) 0.8630(4) 1.1118(3) 0.0573(12) Uani 0.50 1 d P . . H30L H 0.1609 0.8814 1.1319 0.086 Uiso 0.50 1 calc PR . . H30M H 0.0770 0.8468 1.1276 0.086 Uiso 0.50 1 calc PR . . H30N H 0.0882 0.8923 1.0915 0.086 Uiso 0.50 1 calc PR . . 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 0.0265(2) 0.0246(2) 0.0302(2) -0.00142(17) 0.00311(18) -0.00182(18) Co2 0.0255(2) 0.0260(2) 0.0276(2) -0.00258(17) 0.00228(18) 0.00018(18) Co3 0.0368(3) 0.0244(2) 0.0299(2) 0.00002(18) 0.00429(19) 0.0020(2) Co4 0.0341(3) 0.0224(2) 0.0263(2) 0.00101(17) 0.00206(19) -0.00155(19) Cl1 0.0385(5) 0.0263(4) 0.0300(4) -0.0007(3) 0.0024(3) 0.0006(3) Cl2 0.0306(4) 0.0316(4) 0.0335(4) 0.0053(3) 0.0026(3) -0.0029(3) Cl3 0.0362(5) 0.0314(4) 0.0330(4) -0.0056(3) 0.0013(3) 0.0038(4) Cl4 0.0416(5) 0.0344(5) 0.0571(6) -0.0048(4) 0.0209(4) -0.0097(4) Cl5 0.0687(8) 0.0356(5) 0.0681(7) -0.0093(5) 0.0381(6) -0.0120(5) N1 0.0314(15) 0.0257(14) 0.0268(14) -0.0038(11) 0.0037(11) 0.0000(12) N2 0.0245(14) 0.0244(14) 0.0289(14) -0.0029(11) 0.0007(11) -0.0023(11) N3 0.0291(15) 0.0263(14) 0.0266(14) -0.0015(11) 0.0025(11) -0.0045(12) N4 0.0294(15) 0.0292(15) 0.0306(15) -0.0045(12) 0.0010(12) -0.0005(12) N11 0.0314(15) 0.0235(14) 0.0291(14) -0.0006(11) 0.0046(11) -0.0015(12) N12 0.0343(16) 0.0249(14) 0.0280(14) 0.0005(11) 0.0037(12) -0.0002(12) N13 0.0314(16) 0.0305(15) 0.0313(15) -0.0034(12) 0.0066(12) -0.0001(13) N14 0.0369(17) 0.0264(15) 0.0294(15) 0.0015(11) 0.0009(12) 0.0009(13) N21 0.0289(15) 0.0240(14) 0.0262(13) 0.0019(11) 0.0021(11) 0.0026(12) N22 0.0247(14) 0.0254(14) 0.0302(14) 0.0043(11) 0.0021(11) 0.0045(11) N23 0.0304(15) 0.0241(14) 0.0293(14) -0.0013(11) -0.0001(11) 0.0022(12) N24 0.0265(15) 0.0280(15) 0.0351(16) 0.0028(12) 0.0002(12) 0.0051(12) C1 0.0280(17) 0.0254(16) 0.0334(17) -0.0027(13) 0.0058(14) 0.0002(14) C2 0.0285(17) 0.0251(16) 0.0276(16) -0.0026(13) 0.0008(13) -0.0016(14) C3 0.0230(16) 0.0270(16) 0.0326(17) -0.0010(13) 0.0024(13) -0.0024(14) C4 0.0308(19) 0.0252(17) 0.043(2) -0.0092(14) 0.0118(15) -0.0055(14) C5 0.046(2) 0.034(2) 0.046(2) -0.0085(16) 0.0144(18) -0.0088(18) C6 0.067(3) 0.052(3) 0.058(3) -0.017(2) 0.035(3) -0.021(2) C7 0.049(3) 0.058(3) 0.089(4) -0.031(3) 0.041(3) -0.020(2) C8 0.031(2) 0.056(3) 0.086(4) -0.022(3) 0.014(2) -0.008(2) C9 0.034(2) 0.039(2) 0.052(2) -0.0113(17) 0.0086(17) -0.0046(17) C10 0.0326(18) 0.0254(16) 0.0278(16) -0.0028(13) 0.0043(13) -0.0031(14) C11 0.0284(17) 0.0295(17) 0.0291(17) -0.0068(13) 0.0029(13) -0.0033(14) C12 0.0347(19) 0.0307(18) 0.0328(18) -0.0024(14) 0.0050(14) 0.0015(15) C13 0.038(2) 0.043(2) 0.0306(18) -0.0017(15) 0.0006(15) -0.0029(17) C14 0.045(2) 0.045(2) 0.0350(19) -0.0137(17) 0.0016(16) -0.0078(19) C15 0.042(2) 0.035(2) 0.041(2) -0.0068(16) 0.0065(16) -0.0081(17) C16 0.0332(19) 0.0265(17) 0.0326(18) -0.0044(13) 0.0053(14) -0.0013(15) C17 0.057(3) 0.033(2) 0.0314(19) 0.0015(15) 0.0066(17) -0.0004(18) C18 0.059(3) 0.046(3) 0.061(3) 0.010(2) 0.013(2) -0.008(2) C19 0.066(3) 0.051(3) 0.055(3) 0.012(2) 0.013(2) 0.016(2) C20 0.052(2) 0.0307(18) 0.0312(18) -0.0022(14) 0.0108(16) -0.0009(17) C21 0.088(4) 0.059(3) 0.048(3) -0.003(2) 0.020(3) -0.035(3) C22 0.086(4) 0.075(4) 0.046(3) 0.016(2) 0.016(3) 0.040(3) C23 0.0275(18) 0.0295(18) 0.0357(18) -0.0061(14) 0.0042(14) -0.0035(14) C24 0.0288(18) 0.040(2) 0.0352(18) -0.0128(15) 0.0065(15) -0.0053(16) C25 0.0315(19) 0.036(2) 0.048(2) -0.0116(17) 0.0075(16) -0.0064(16) C26 0.046(2) 0.044(2) 0.053(2) -0.0149(19) 0.0067(19) -0.012(2) C27 0.042(2) 0.062(3) 0.051(3) -0.024(2) 0.0016(19) -0.017(2) C28 0.038(2) 0.062(3) 0.038(2) -0.0089(19) -0.0030(17) -0.008(2) C29 0.032(2) 0.047(2) 0.0333(19) -0.0078(16) 0.0012(15) -0.0041(17) C30 0.043(2) 0.038(2) 0.056(3) -0.0077(18) -0.0002(19) -0.0102(19) C31 0.092(5) 0.102(5) 0.051(3) 0.009(3) 0.013(3) 0.032(4) C32 0.079(4) 0.045(3) 0.083(4) 0.011(3) 0.028(3) 0.012(3) C33 0.043(2) 0.051(2) 0.042(2) -0.0033(18) -0.0059(17) -0.006(2) C34 0.060(3) 0.063(3) 0.052(3) 0.007(2) -0.006(2) -0.004(3) C35 0.067(3) 0.055(3) 0.056(3) -0.009(2) 0.001(2) 0.007(3) C101 0.0346(18) 0.0248(17) 0.0309(17) -0.0016(13) 0.0050(14) -0.0020(14) C102 0.0308(18) 0.0254(17) 0.0318(17) -0.0038(13) 0.0048(14) -0.0006(14) C103 0.0345(19) 0.0236(16) 0.0326(18) 0.0012(13) 0.0032(14) -0.0018(14) C104 0.043(2) 0.0260(18) 0.0318(18) -0.0001(14) 0.0092(15) 0.0003(16) C105 0.041(2) 0.0319(19) 0.039(2) -0.0022(15) 0.0102(16) -0.0035(16) C106 0.053(3) 0.033(2) 0.052(2) -0.0063(17) 0.020(2) -0.0115(19) C107 0.067(3) 0.0251(19) 0.063(3) 0.0066(18) 0.024(2) -0.004(2) C108 0.061(3) 0.035(2) 0.062(3) 0.0152(19) 0.009(2) 0.005(2) C109 0.049(2) 0.030(2) 0.052(2) 0.0055(17) 0.0028(19) -0.0014(18) C110 0.0317(18) 0.0271(17) 0.0350(18) -0.0049(14) 0.0075(14) -0.0007(15) C111 0.043(2) 0.0259(17) 0.0299(17) -0.0025(13) 0.0069(15) -0.0024(15) C112 0.053(2) 0.0270(18) 0.041(2) -0.0016(15) 0.0163(18) 0.0051(17) C113 0.073(3) 0.038(2) 0.044(2) -0.0041(18) 0.026(2) 0.004(2) C114 0.085(4) 0.043(2) 0.033(2) -0.0055(17) 0.017(2) 0.001(2) C115 0.067(3) 0.040(2) 0.035(2) -0.0031(17) -0.0004(19) -0.001(2) C116 0.048(2) 0.0328(19) 0.0332(19) -0.0018(15) 0.0029(16) 0.0016(17) C117 0.045(2) 0.033(2) 0.052(2) -0.0011(17) 0.0178(19) 0.0042(18) C118 0.051(3) 0.035(2) 0.064(3) 0.0023(19) 0.009(2) 0.0040(19) C119 0.053(3) 0.050(3) 0.090(4) 0.015(3) 0.032(3) 0.008(2) C120 0.042(2) 0.045(2) 0.039(2) -0.0049(17) -0.0003(17) -0.0027(19) C121 0.055(3) 0.066(3) 0.078(4) -0.012(3) 0.018(3) -0.020(3) C122 0.051(3) 0.061(3) 0.055(3) -0.002(2) -0.004(2) 0.014(2) C123 0.039(2) 0.0257(17) 0.0302(17) 0.0022(13) 0.0047(14) -0.0012(15) C124 0.053(2) 0.0260(17) 0.0278(17) -0.0014(13) 0.0054(16) -0.0032(17) C125 0.054(3) 0.043(2) 0.034(2) 0.0000(16) -0.0017(17) -0.006(2) C126 0.069(3) 0.067(3) 0.035(2) -0.003(2) 0.000(2) 0.001(3) C127 0.084(4) 0.062(3) 0.031(2) -0.003(2) 0.010(2) -0.001(3) C128 0.073(3) 0.046(2) 0.041(2) 0.0025(19) 0.020(2) 0.008(2) C129 0.057(3) 0.0276(18) 0.0362(19) 0.0049(15) 0.0124(18) 0.0042(18) C130 0.052(3) 0.077(3) 0.040(2) 0.002(2) -0.002(2) -0.005(3) C131 0.058(4) 0.103(5) 0.099(5) -0.019(4) 0.002(3) 0.020(4) C132 0.062(4) 0.140(7) 0.053(3) 0.004(4) -0.002(3) -0.032(4) C133 0.057(3) 0.039(2) 0.044(2) 0.0106(17) 0.0184(19) 0.006(2) C134 0.063(3) 0.053(3) 0.059(3) 0.011(2) 0.009(2) 0.000(2) C135 0.066(3) 0.043(3) 0.071(3) 0.011(2) 0.024(3) 0.013(2) C201 0.0266(17) 0.0254(16) 0.0334(17) 0.0017(13) 0.0063(14) 0.0016(14) C202 0.0289(17) 0.0274(17) 0.0279(16) 0.0019(13) 0.0049(13) 0.0021(14) C203 0.0257(17) 0.0233(16) 0.0306(16) 0.0009(13) 0.0023(13) 0.0006(13) C204 0.0271(17) 0.0260(17) 0.0395(19) 0.0040(14) 0.0081(14) 0.0010(14) C205 0.038(2) 0.0304(18) 0.041(2) 0.0025(15) 0.0106(16) 0.0003(16) C206 0.049(2) 0.035(2) 0.053(2) 0.0058(17) 0.024(2) 0.0023(18) C207 0.034(2) 0.034(2) 0.065(3) 0.0122(18) 0.0189(19) 0.0019(17) C208 0.0285(19) 0.036(2) 0.061(3) 0.0120(18) 0.0055(17) -0.0020(16) C209 0.035(2) 0.0300(18) 0.043(2) 0.0043(15) 0.0062(16) -0.0010(16) C210 0.0336(19) 0.0241(16) 0.0291(17) 0.0012(13) 0.0038(14) 0.0024(14) C211 0.0314(19) 0.0302(18) 0.0375(19) 0.0040(15) -0.0021(15) 0.0045(15) C212 0.0318(19) 0.0323(19) 0.0383(19) 0.0030(15) 0.0007(15) 0.0060(16) C213 0.050(2) 0.031(2) 0.049(2) 0.0054(17) -0.0028(18) 0.0133(19) C214 0.078(3) 0.042(2) 0.041(2) 0.0097(18) -0.008(2) 0.020(2) C215 0.075(3) 0.050(3) 0.034(2) 0.0064(18) -0.003(2) 0.016(2) C216 0.052(3) 0.037(2) 0.038(2) 0.0021(16) -0.0027(18) 0.0092(19) C217 0.036(2) 0.0305(18) 0.042(2) 0.0034(15) 0.0034(16) 0.0066(16) C218 0.050(3) 0.072(3) 0.045(2) -0.018(2) 0.006(2) -0.008(2) C219 0.046(3) 0.060(3) 0.063(3) -0.007(2) 0.011(2) 0.013(2) C220 0.075(3) 0.045(2) 0.032(2) -0.0018(18) 0.003(2) 0.016(2) C221 0.105(5) 0.063(3) 0.070(4) 0.007(3) 0.039(3) 0.023(3) C222 0.103(5) 0.059(3) 0.051(3) -0.017(2) -0.015(3) 0.018(3) C223 0.0251(17) 0.0283(17) 0.0374(18) 0.0000(14) 0.0028(14) 0.0009(14) C224 0.034(2) 0.039(2) 0.042(2) 0.0097(16) 0.0028(16) 0.0026(17) C225 0.041(2) 0.039(2) 0.062(3) 0.0129(19) 0.0048(19) 0.0070(19) C226 0.042(3) 0.047(3) 0.087(4) 0.014(2) -0.005(2) 0.014(2) C227 0.049(3) 0.070(4) 0.081(4) 0.015(3) -0.016(3) 0.015(3) C228 0.044(3) 0.064(3) 0.058(3) 0.007(2) -0.011(2) 0.003(2) C229 0.036(2) 0.048(2) 0.045(2) 0.0058(18) 0.0000(17) -0.0024(18) C230 0.043(2) 0.032(2) 0.075(3) 0.003(2) 0.009(2) 0.0045(19) C231 0.068(3) 0.052(3) 0.080(4) -0.009(3) 0.015(3) -0.003(3) C232 0.072(4) 0.036(3) 0.114(5) 0.006(3) 0.007(3) 0.004(3) C233 0.039(2) 0.049(2) 0.047(2) -0.0056(18) 0.0012(18) -0.0022(19) C234 0.053(3) 0.052(3) 0.065(3) -0.003(2) 0.004(2) -0.011(2) C235 0.070(4) 0.079(4) 0.057(3) -0.011(3) 0.012(3) 0.005(3) O1 0.029(3) 0.052(4) 0.067(4) -0.018(3) 0.022(3) -0.020(3) C301 0.030(4) 0.036(4) 0.069(5) -0.006(4) 0.023(4) 0.003(3) C302 0.048(5) 0.054(6) 0.084(7) -0.017(5) 0.031(5) -0.031(5) C303 0.046(5) 0.043(5) 0.082(7) -0.012(4) 0.038(5) -0.005(4) C304 0.039(5) 0.054(5) 0.079(6) -0.016(5) 0.031(5) -0.013(4) N31 0.081(5) 0.079(5) 0.062(4) -0.016(3) 0.026(4) -0.009(4) C305 0.075(3) 0.047(3) 0.054(3) -0.002(2) 0.023(2) -0.004(2) C306 0.075(3) 0.047(3) 0.054(3) -0.002(2) 0.023(2) -0.004(2) N32 0.081(5) 0.079(5) 0.062(4) -0.016(3) 0.026(4) -0.009(4) C307 0.075(3) 0.047(3) 0.054(3) -0.002(2) 0.023(2) -0.004(2) C308 0.075(3) 0.047(3) 0.054(3) -0.002(2) 0.023(2) -0.004(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 Co2 4.2348(6) . ? Co1 Co3 6.6501(7) . ? Co1 Co4 3.7711(6) . ? Co2 Co3 3.8068(7) . ? Co2 Co4 3.9522(7) . ? Co3 Co4 4.2490(7) . ? Co1 N1 2.016(3) . ? Co1 N3 2.089(3) . ? Co1 Cl4 2.1958(10) . ? Co1 Cl1 2.2831(9) . ? Co2 N21 2.031(3) . ? Co2 N2 2.044(3) . ? Co2 N4 2.190(3) . ? Co2 N23 2.412(3) . ? Co2 Cl3 2.4288(9) . ? Co2 Cl2 2.4877(9) . ? Co3 N11 2.015(3) . ? Co3 N13 2.089(3) . ? Co3 Cl5 2.1857(12) . ? Co3 Cl3 2.2765(10) . ? Co4 N22 2.032(3) . ? Co4 N12 2.053(3) . ? Co4 N14 2.209(3) . ? Co4 Cl1 2.4182(9) . ? Co4 Cl2 2.4437(10) . ? N1 N2 1.326(4) . ? N1 C2 1.373(4) . ? N2 C3 1.355(4) . ? N3 C10 1.283(5) . ? N3 C11 1.443(4) . ? N4 C23 1.288(5) . ? N4 C24 1.456(5) . ? N11 N12 1.318(4) . ? N11 C102 1.370(4) . ? N12 C103 1.356(4) . ? N13 C110 1.283(5) . ? N13 C111 1.436(4) . ? N14 C123 1.298(5) . ? N14 C124 1.445(4) . ? N21 N22 1.340(4) . ? N21 C202 1.351(4) . ? N22 C203 1.344(4) . ? N23 C210 1.288(5) . ? N23 C211 1.446(4) . ? N24 C223 1.286(5) . ? N24 C224 1.440(5) . ? C1 C2 1.387(5) . ? C1 C3 1.406(5) . ? C1 C4 1.469(5) . ? C2 C10 1.453(5) . ? C3 C23 1.449(5) . ? C4 C5 1.390(6) . ? C4 C9 1.393(6) . ? C5 C6 1.384(6) . ? C6 C7 1.390(8) . ? C7 C8 1.365(8) . ? C8 C9 1.390(6) . ? C11 C12 1.395(5) . ? C11 C16 1.405(5) . ? C12 C13 1.398(5) . ? C12 C17 1.528(5) . ? C13 C14 1.377(6) . ? C14 C15 1.386(6) . ? C15 C16 1.386(5) . ? C16 C20 1.518(5) . ? C17 C18 1.523(6) . ? C17 C19 1.523(6) . ? C20 C22 1.499(7) . ? C20 C21 1.520(6) . ? C24 C29 1.401(6) . ? C24 C25 1.406(6) . ? C25 C26 1.403(6) . ? C25 C30 1.510(6) . ? C26 C27 1.373(7) . ? C27 C28 1.381(7) . ? C28 C29 1.406(5) . ? C29 C33 1.523(6) . ? C30 C31 1.515(8) . ? C30 C32 1.521(7) . ? C33 C34 1.515(6) . ? C33 C35 1.529(7) . ? C101 C102 1.395(5) . ? C101 C103 1.409(5) . ? C101 C104 1.475(5) . ? C102 C110 1.446(5) . ? C103 C123 1.441(5) . ? C104 C105 1.387(6) . ? C104 C109 1.389(6) . ? C105 C106 1.397(5) . ? C106 C107 1.382(7) . ? C107 C108 1.389(7) . ? C108 C109 1.392(6) . ? C111 C112 1.390(6) . ? C111 C116 1.406(6) . ? C112 C113 1.401(6) . ? C112 C117 1.511(6) . ? C113 C114 1.376(7) . ? C114 C115 1.386(7) . ? C115 C116 1.401(6) . ? C116 C120 1.498(6) . ? C117 C119 1.529(6) . ? C117 C118 1.534(6) . ? C120 C121 1.525(7) . ? C120 C122 1.538(6) . ? C124 C129 1.397(6) . ? C124 C125 1.406(6) . ? C125 C126 1.376(6) . ? C125 C130 1.503(7) . ? C126 C127 1.365(8) . ? C127 C128 1.394(7) . ? C128 C129 1.405(6) . ? C129 C133 1.516(6) . ? C130 C132 1.510(7) . ? C130 C131 1.547(9) . ? C133 C134 1.519(7) . ? C133 C135 1.528(6) . ? C201 C203 1.393(5) . ? C201 C202 1.403(5) . ? C201 C204 1.472(5) . ? C202 C210 1.429(5) . ? C203 C223 1.442(5) . ? C204 C205 1.391(5) . ? C204 C209 1.408(5) . ? C205 C206 1.388(6) . ? C206 C207 1.386(7) . ? C207 C208 1.380(6) . ? C208 C209 1.381(6) . ? C211 C216 1.393(6) . ? C211 C212 1.404(5) . ? C212 C213 1.400(5) . ? C212 C217 1.511(5) . ? C213 C214 1.379(6) . ? C214 C215 1.378(7) . ? C215 C216 1.398(6) . ? C216 C220 1.520(6) . ? C217 C218 1.511(6) . ? C217 C219 1.521(6) . ? C220 C221 1.535(8) . ? C220 C222 1.545(8) . ? C224 C225 1.405(6) . ? C224 C229 1.411(6) . ? C225 C226 1.399(6) . ? C225 C230 1.517(7) . ? C226 C227 1.395(8) . ? C227 C228 1.364(8) . ? C228 C229 1.400(6) . ? C229 C233 1.520(6) . ? C230 C231 1.515(7) . ? C230 C232 1.531(6) . ? C233 C235 1.514(7) . ? C233 C234 1.528(7) . ? O1 C304 1.388(11) . ? O1 C301 1.457(11) . ? C301 C302 1.451(11) . ? C302 C303 1.515(15) . ? C303 C304 1.444(13) . ? N31 C305 1.151(15) . ? C305 C306 1.353(16) . ? N32 C307 1.132(13) . ? C307 C308 1.430(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N3 80.70(11) . . ? N1 Co1 Cl4 127.80(9) . . ? N3 Co1 Cl4 110.09(9) . . ? N1 Co1 Cl1 110.96(9) . . ? N3 Co1 Cl1 105.30(8) . . ? Cl4 Co1 Cl1 114.32(4) . . ? N21 Co2 N2 98.31(11) . . ? N21 Co2 N4 175.17(11) . . ? N2 Co2 N4 77.06(11) . . ? N21 Co2 N23 73.42(11) . . ? N2 Co2 N23 94.83(11) . . ? N4 Co2 N23 108.12(11) . . ? N21 Co2 Cl3 92.84(8) . . ? N2 Co2 Cl3 168.78(9) . . ? N4 Co2 Cl3 91.76(8) . . ? N23 Co2 Cl3 89.58(7) . . ? N21 Co2 Cl2 86.17(8) . . ? N2 Co2 Cl2 81.14(8) . . ? N4 Co2 Cl2 91.69(8) . . ? N23 Co2 Cl2 158.46(8) . . ? Cl3 Co2 Cl2 98.40(3) . . ? N11 Co3 N13 80.60(12) . . ? N11 Co3 Cl5 127.18(10) . . ? N13 Co3 Cl5 106.25(9) . . ? N11 Co3 Cl3 114.06(9) . . ? N13 Co3 Cl3 108.75(9) . . ? Cl5 Co3 Cl3 112.65(5) . . ? N22 Co4 N12 96.73(11) . . ? N22 Co4 N14 174.20(11) . . ? N12 Co4 N14 77.47(11) . . ? N22 Co4 Cl1 94.13(9) . . ? N12 Co4 Cl1 168.89(8) . . ? N14 Co4 Cl1 91.65(8) . . ? N22 Co4 Cl2 87.18(8) . . ? N12 Co4 Cl2 83.13(9) . . ? N14 Co4 Cl2 92.39(9) . . ? Cl1 Co4 Cl2 99.77(3) . . ? Co1 Cl1 Co4 106.63(4) . . ? Co4 Cl2 Co2 106.53(3) . . ? Co3 Cl3 Co2 107.96(4) . . ? N2 N1 C2 107.7(3) . . ? N2 N1 Co1 138.4(2) . . ? C2 N1 Co1 111.4(2) . . ? N1 N2 C3 109.0(3) . . ? N1 N2 Co2 133.2(2) . . ? C3 N2 Co2 115.8(2) . . ? C10 N3 C11 117.8(3) . . ? C10 N3 Co1 111.6(2) . . ? C11 N3 Co1 130.5(2) . . ? C23 N4 C24 117.0(3) . . ? C23 N4 Co2 112.8(2) . . ? C24 N4 Co2 130.0(2) . . ? N12 N11 C102 108.5(3) . . ? N12 N11 Co3 137.8(2) . . ? C102 N11 Co3 112.0(2) . . ? N11 N12 C103 108.9(3) . . ? N11 N12 Co4 134.3(2) . . ? C103 N12 Co4 115.6(2) . . ? C110 N13 C111 118.9(3) . . ? C110 N13 Co3 112.4(2) . . ? C111 N13 Co3 128.2(2) . . ? C123 N14 C124 116.4(3) . . ? C123 N14 Co4 111.7(2) . . ? C124 N14 Co4 131.7(2) . . ? N22 N21 C202 108.4(3) . . ? N22 N21 Co2 130.4(2) . . ? C202 N21 Co2 120.9(2) . . ? N21 N22 C203 108.1(3) . . ? N21 N22 Co4 129.4(2) . . ? C203 N22 Co4 122.4(2) . . ? C210 N23 C211 113.7(3) . . ? C210 N23 Co2 108.2(2) . . ? C211 N23 Co2 137.7(2) . . ? C223 N24 C224 113.0(3) . . ? C2 C1 C3 103.0(3) . . ? C2 C1 C4 127.7(3) . . ? C3 C1 C4 129.2(3) . . ? N1 C2 C1 110.4(3) . . ? N1 C2 C10 115.3(3) . . ? C1 C2 C10 134.3(3) . . ? N2 C3 C1 109.9(3) . . ? N2 C3 C23 116.1(3) . . ? C1 C3 C23 133.7(3) . . ? C5 C4 C9 119.0(4) . . ? C5 C4 C1 119.8(4) . . ? C9 C4 C1 121.1(3) . . ? C6 C5 C4 120.9(4) . . ? C5 C6 C7 119.4(5) . . ? C8 C7 C6 120.1(4) . . ? C7 C8 C9 120.9(5) . . ? C8 C9 C4 119.6(4) . . ? N3 C10 C2 118.4(3) . . ? C12 C11 C16 123.0(3) . . ? C12 C11 N3 118.9(3) . . ? C16 C11 N3 118.1(3) . . ? C11 C12 C13 116.9(3) . . ? C11 C12 C17 121.8(3) . . ? C13 C12 C17 121.3(3) . . ? C14 C13 C12 121.3(4) . . ? C13 C14 C15 120.2(4) . . ? C14 C15 C16 121.1(4) . . ? C15 C16 C11 117.3(3) . . ? C15 C16 C20 120.9(3) . . ? C11 C16 C20 121.8(3) . . ? C18 C17 C19 111.0(4) . . ? C18 C17 C12 110.8(4) . . ? C19 C17 C12 111.8(4) . . ? C22 C20 C16 111.9(3) . . ? C22 C20 C21 111.1(4) . . ? C16 C20 C21 112.8(4) . . ? N4 C23 C3 117.4(3) . . ? C29 C24 C25 122.3(3) . . ? C29 C24 N4 118.2(3) . . ? C25 C24 N4 119.3(3) . . ? C26 C25 C24 117.4(4) . . ? C26 C25 C30 119.8(4) . . ? C24 C25 C30 122.6(3) . . ? C27 C26 C25 121.1(4) . . ? C26 C27 C28 120.7(4) . . ? C27 C28 C29 120.7(4) . . ? C24 C29 C28 117.6(4) . . ? C24 C29 C33 122.6(3) . . ? C28 C29 C33 119.7(4) . . ? C25 C30 C31 110.5(4) . . ? C25 C30 C32 113.2(4) . . ? C31 C30 C32 110.5(4) . . ? C34 C33 C29 113.2(4) . . ? C34 C33 C35 109.9(4) . . ? C29 C33 C35 110.9(4) . . ? C102 C101 C103 102.8(3) . . ? C102 C101 C104 129.6(3) . . ? C103 C101 C104 127.6(3) . . ? N11 C102 C101 109.9(3) . . ? N11 C102 C110 116.0(3) . . ? C101 C102 C110 134.1(3) . . ? N12 C103 C101 109.9(3) . . ? N12 C103 C123 116.7(3) . . ? C101 C103 C123 132.9(3) . . ? C105 C104 C109 118.5(4) . . ? C105 C104 C101 121.7(3) . . ? C109 C104 C101 119.7(4) . . ? C104 C105 C106 120.6(4) . . ? C107 C106 C105 120.2(4) . . ? C106 C107 C108 119.9(4) . . ? C107 C108 C109 119.3(4) . . ? C104 C109 C108 121.5(4) . . ? N13 C110 C102 117.8(3) . . ? C112 C111 C116 123.5(3) . . ? C112 C111 N13 118.5(3) . . ? C116 C111 N13 118.0(3) . . ? C111 C112 C113 117.1(4) . . ? C111 C112 C117 122.0(3) . . ? C113 C112 C117 120.9(4) . . ? C114 C113 C112 121.1(4) . . ? C113 C114 C115 120.5(4) . . ? C114 C115 C116 121.0(4) . . ? C115 C116 C111 116.6(4) . . ? C115 C116 C120 121.1(4) . . ? C111 C116 C120 122.3(3) . . ? C112 C117 C119 112.2(4) . . ? C112 C117 C118 110.8(4) . . ? C119 C117 C118 110.1(4) . . ? C116 C120 C121 111.4(4) . . ? C116 C120 C122 111.9(4) . . ? C121 C120 C122 110.9(4) . . ? N14 C123 C103 118.4(3) . . ? C129 C124 C125 121.8(4) . . ? C129 C124 N14 120.2(3) . . ? C125 C124 N14 118.0(4) . . ? C126 C125 C124 117.4(4) . . ? C126 C125 C130 121.9(4) . . ? C124 C125 C130 120.7(4) . . ? C127 C126 C125 122.7(5) . . ? C126 C127 C128 120.0(4) . . ? C127 C128 C129 119.7(5) . . ? C124 C129 C128 118.4(4) . . ? C124 C129 C133 123.3(3) . . ? C128 C129 C133 118.3(4) . . ? C125 C130 C132 114.7(5) . . ? C125 C130 C131 111.3(5) . . ? C132 C130 C131 107.4(5) . . ? C129 C133 C134 112.7(4) . . ? C129 C133 C135 111.1(4) . . ? C134 C133 C135 110.1(4) . . ? C203 C201 C202 102.8(3) . . ? C203 C201 C204 127.2(3) . . ? C202 C201 C204 130.0(3) . . ? N21 C202 C201 109.9(3) . . ? N21 C202 C210 116.0(3) . . ? C201 C202 C210 133.9(3) . . ? N22 C203 C201 110.8(3) . . ? N22 C203 C223 116.5(3) . . ? C201 C203 C223 132.7(3) . . ? C205 C204 C209 119.1(3) . . ? C205 C204 C201 121.1(3) . . ? C209 C204 C201 119.8(3) . . ? C206 C205 C204 120.0(4) . . ? C207 C206 C205 120.5(4) . . ? C208 C207 C206 119.8(4) . . ? C207 C208 C209 120.5(4) . . ? C208 C209 C204 120.1(4) . . ? N23 C210 C202 120.3(3) . . ? C216 C211 C212 122.4(3) . . ? C216 C211 N23 119.9(3) . . ? C212 C211 N23 117.6(3) . . ? C213 C212 C211 117.4(4) . . ? C213 C212 C217 121.2(3) . . ? C211 C212 C217 121.3(3) . . ? C214 C213 C212 121.3(4) . . ? C215 C214 C213 119.9(4) . . ? C214 C215 C216 121.5(4) . . ? C211 C216 C215 117.5(4) . . ? C211 C216 C220 123.8(4) . . ? C215 C216 C220 118.6(4) . . ? C218 C217 C212 111.0(3) . . ? C218 C217 C219 110.6(4) . . ? C212 C217 C219 114.2(3) . . ? C216 C220 C221 111.9(4) . . ? C216 C220 C222 110.7(4) . . ? C221 C220 C222 111.5(5) . . ? N24 C223 C203 120.0(3) . . ? C225 C224 C229 122.6(4) . . ? C225 C224 N24 118.5(4) . . ? C229 C224 N24 118.9(4) . . ? C226 C225 C224 117.2(4) . . ? C226 C225 C230 122.0(4) . . ? C224 C225 C230 120.7(4) . . ? C227 C226 C225 120.6(5) . . ? C228 C227 C226 121.1(5) . . ? C227 C228 C229 121.0(5) . . ? C228 C229 C224 117.4(4) . . ? C228 C229 C233 119.1(4) . . ? C224 C229 C233 123.5(4) . . ? C231 C230 C225 111.2(4) . . ? C231 C230 C232 108.8(5) . . ? C225 C230 C232 114.7(4) . . ? C235 C233 C229 112.3(4) . . ? C235 C233 C234 110.7(4) . . ? C229 C233 C234 110.4(4) . . ? C304 O1 C301 106.8(6) . . ? C302 C301 O1 107.1(7) . . ? C301 C302 C303 104.9(8) . . ? C304 C303 C302 101.2(8) . . ? O1 C304 C303 110.7(8) . . ? N31 C305 C306 176.3(12) . . ? N32 C307 C308 155.8(13) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.74 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.488 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.123 # Attachment '_3_.cif' data_as40 _database_code_depnum_ccdc_archive 'CCDC 728436' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H98 N8 Cl6 Co4 O5, 2 (C H Cl3)' _chemical_formula_sum 'C96 H100 Cl12 Co4 N8 O5' _chemical_formula_weight 2106.96 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.2650(7) _cell_length_b 15.1857(9) _cell_length_c 17.6502(10) _cell_angle_alpha 112.618(4) _cell_angle_beta 90.388(5) _cell_angle_gamma 106.495(4) _cell_volume 2649.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 22714 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 27.03 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 0.969 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7942 _exptl_absorpt_correction_T_max 0.9121 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22714 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.03 _reflns_number_total 11412 _reflns_number_gt 8282 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2007)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2007)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. platon sqeeze was used ; _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^)+(0.0913P)^2^+4.2284P] 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 11412 _refine_ls_number_parameters 587 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1775 _refine_ls_wR_factor_gt 0.1654 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.54433(6) 0.38783(4) 0.57714(4) 0.01771(15) Uani 1 1 d . . . Co2 Co 0.61323(6) 0.67967(4) 0.61935(3) 0.01647(14) Uani 1 1 d . . . O1 O 0.7170(4) 0.4072(3) 0.5223(2) 0.0426(10) Uani 1 1 d . A . Cl4 Cl 0.55002(10) 0.76032(6) 0.54326(6) 0.0183(2) Uani 1 1 d . . . Cl5 Cl 0.5000 0.5000 0.5000 0.0335(4) Uani 1 2 d S . . Cl7 Cl 0.7186(6) 0.3299(5) 0.1328(3) 0.194(3) Uani 1 1 d . . . Cl8 Cl 0.5843(3) 0.4587(3) 0.1270(3) 0.1277(12) Uani 1 1 d . . . Cl6 Cl 0.8360(3) 0.5371(6) 0.1982(4) 0.225(3) Uani 1 1 d . . . N1 N 0.6389(3) 0.5163(2) 0.6740(2) 0.0156(7) Uani 1 1 d . A . N2 N 0.6542(3) 0.6114(2) 0.6894(2) 0.0147(7) Uani 1 1 d . A . N3 N 0.6005(3) 0.3366(2) 0.6660(2) 0.0137(6) Uani 1 1 d . A . N4 N 0.7046(3) 0.8036(2) 0.7355(2) 0.0142(7) Uani 1 1 d . A . C1 C 0.7290(4) 0.6075(3) 0.8069(2) 0.0137(7) Uani 1 1 d . A . C2 C 0.6826(4) 0.5103(3) 0.7424(3) 0.0143(7) Uani 1 1 d . . . C3 C 0.7059(4) 0.6686(3) 0.7691(2) 0.0140(7) Uani 1 1 d . . . C4 C 0.7901(4) 0.6399(3) 0.8918(3) 0.0161(8) Uani 1 1 d . . . C5 C 0.9086(4) 0.7117(3) 0.9191(3) 0.0253(10) Uani 1 1 d . A . H5 H 0.9506 0.7364 0.8827 0.030 Uiso 1 1 calc R . . C6 C 0.9643(5) 0.7466(4) 1.0006(3) 0.0339(12) Uani 1 1 d . . . H6 H 1.0432 0.7940 1.0181 0.041 Uiso 1 1 calc R A . C7 C 0.9017(6) 0.7106(4) 1.0551(3) 0.0418(14) Uani 1 1 d . A . H7 H 0.9378 0.7350 1.1097 0.050 Uiso 1 1 calc R . . C8 C 0.7854(6) 0.6383(4) 1.0283(3) 0.0359(12) Uani 1 1 d . . . H8 H 0.7445 0.6129 1.0646 0.043 Uiso 1 1 calc R A . C9 C 0.7300(5) 0.6038(3) 0.9478(3) 0.0257(10) Uani 1 1 d . A . H9 H 0.6516 0.5557 0.9306 0.031 Uiso 1 1 calc R . . C10 C 0.6655(4) 0.4064(3) 0.7336(2) 0.0128(7) Uani 1 1 d . A . C11 C 0.7210(4) 0.3905(3) 0.8021(3) 0.0176(8) Uani 1 1 d . . . C12 C 0.6435(5) 0.3434(3) 0.8464(3) 0.0240(9) Uani 1 1 d . A . H12 H 0.5578 0.3172 0.8298 0.029 Uiso 1 1 calc R . . C13 C 0.6934(5) 0.3356(3) 0.9140(3) 0.0315(11) Uani 1 1 d . . . H13 H 0.6412 0.3048 0.9432 0.038 Uiso 1 1 calc R A . C14 C 0.8212(6) 0.3737(4) 0.9388(3) 0.0344(12) Uani 1 1 d . A . H14 H 0.8545 0.3685 0.9847 0.041 Uiso 1 1 calc R . . C15 C 0.8990(5) 0.4193(4) 0.8955(3) 0.0312(11) Uani 1 1 d . . . H15 H 0.9849 0.4435 0.9114 0.037 Uiso 1 1 calc R A . C16 C 0.8487(4) 0.4291(3) 0.8279(3) 0.0224(9) Uani 1 1 d . A . H16 H 0.9010 0.4618 0.7999 0.027 Uiso 1 1 calc R . . C17 C 0.5825(4) 0.2318(3) 0.6484(2) 0.0161(8) Uani 1 1 d . . . C18 C 0.6758(4) 0.1883(3) 0.6144(3) 0.0219(9) Uani 1 1 d . A . C19 C 0.6514(5) 0.0865(3) 0.5943(3) 0.0340(12) Uani 1 1 d . . . H19 H 0.7122 0.0569 0.5725 0.041 Uiso 1 1 calc R A . C20 C 0.5417(6) 0.0280(3) 0.6053(3) 0.0388(14) Uani 1 1 d . A . H20 H 0.5288 -0.0399 0.5915 0.047 Uiso 1 1 calc R . . C21 C 0.4498(6) 0.0708(3) 0.6371(3) 0.0367(13) Uani 1 1 d . . . H21 H 0.3749 0.0309 0.6444 0.044 Uiso 1 1 calc R A . C22 C 0.4674(5) 0.1729(3) 0.6587(3) 0.0249(10) Uani 1 1 d . A . C23 C 0.7972(5) 0.2473(4) 0.5950(3) 0.0289(10) Uani 1 1 d . . . H23 H 0.8011 0.3180 0.6158 0.035 Uiso 1 1 calc R A . C24 C 0.9125(6) 0.2398(5) 0.6359(4) 0.0502(11) Uani 1 1 d . A . H24A H 0.9868 0.2782 0.6228 0.075 Uiso 1 1 calc R . . H24B H 0.9102 0.1709 0.6157 0.075 Uiso 1 1 calc R . . H24C H 0.9127 0.2658 0.6949 0.075 Uiso 1 1 calc R . . C25 C 0.7961(6) 0.2069(5) 0.5003(4) 0.0455(14) Uani 1 1 d . A . H25A H 0.8716 0.2439 0.4873 0.068 Uiso 1 1 calc R . . H25B H 0.7255 0.2145 0.4756 0.068 Uiso 1 1 calc R . . H25C H 0.7904 0.1372 0.4790 0.068 Uiso 1 1 calc R . . C26 C 0.3604(5) 0.2142(4) 0.6878(3) 0.0355(12) Uani 1 1 d . . . H26 H 0.3913 0.2872 0.7060 0.043 Uiso 1 1 calc R A . C27 C 0.3079(6) 0.1908(5) 0.7608(4) 0.0502(11) Uani 1 1 d . A . H27A H 0.2411 0.2190 0.7770 0.075 Uiso 1 1 calc R . . H27B H 0.3729 0.2195 0.8066 0.075 Uiso 1 1 calc R . . H27C H 0.2769 0.1194 0.7441 0.075 Uiso 1 1 calc R . . C28 C 0.2547(5) 0.1718(5) 0.6158(4) 0.0432(14) Uani 1 1 d . A . H28A H 0.2869 0.1869 0.5705 0.065 Uiso 1 1 calc R . . H28B H 0.1898 0.2016 0.6338 0.065 Uiso 1 1 calc R . . H28C H 0.2215 0.1004 0.5982 0.065 Uiso 1 1 calc R . . C29 C 0.7218(3) 0.7770(3) 0.7951(2) 0.0119(7) Uani 1 1 d . A . C30 C 0.7431(4) 0.8426(3) 0.8856(2) 0.0145(7) Uani 1 1 d . . . C31 C 0.6684(4) 0.8050(3) 0.9361(3) 0.0183(8) Uani 1 1 d . A . H31 H 0.6097 0.7415 0.9128 0.022 Uiso 1 1 calc R . . C32 C 0.6810(4) 0.8613(3) 1.0209(3) 0.0244(9) Uani 1 1 d . . . H32 H 0.6307 0.8361 1.0541 0.029 Uiso 1 1 calc R A . C33 C 0.7698(5) 0.9562(4) 1.0557(3) 0.0280(10) Uani 1 1 d . A . H33 H 0.7796 0.9942 1.1124 0.034 Uiso 1 1 calc R . . C34 C 0.8434(5) 0.9937(3) 1.0058(3) 0.0266(10) Uani 1 1 d . . . H34 H 0.9022 1.0571 1.0295 0.032 Uiso 1 1 calc R A . C35 C 0.8310(4) 0.9383(3) 0.9211(3) 0.0191(8) Uani 1 1 d . A . H35 H 0.8806 0.9645 0.8882 0.023 Uiso 1 1 calc R . . C36 C 0.7224(4) 0.9085(3) 0.7525(2) 0.0137(7) Uani 1 1 d . . . C37 C 0.6332(4) 0.9550(3) 0.7878(2) 0.0157(8) Uani 1 1 d . A . C38 C 0.6602(4) 1.0574(3) 0.8045(3) 0.0218(9) Uani 1 1 d . . . H38 H 0.6034 1.0905 0.8285 0.026 Uiso 1 1 calc R A . C39 C 0.7691(5) 1.1095(3) 0.7858(3) 0.0265(10) Uani 1 1 d . A . H39 H 0.7864 1.1778 0.7993 0.032 Uiso 1 1 calc R . . C40 C 0.8528(4) 1.0615(3) 0.7475(3) 0.0244(9) Uani 1 1 d . . . H40 H 0.9253 1.0972 0.7343 0.029 Uiso 1 1 calc R A . C41 C 0.8293(4) 0.9596(3) 0.7285(3) 0.0176(8) Uani 1 1 d . A . C42 C 0.5109(4) 0.8999(3) 0.8068(3) 0.0192(8) Uani 1 1 d . . . H42 H 0.5107 0.8312 0.7950 0.023 Uiso 1 1 calc R A . C43 C 0.4002(4) 0.8943(4) 0.7519(3) 0.0274(10) Uani 1 1 d . A . H43A H 0.3236 0.8586 0.7647 0.041 Uiso 1 1 calc R . . H43B H 0.4082 0.8598 0.6947 0.041 Uiso 1 1 calc R . . H43C H 0.3998 0.9610 0.7619 0.041 Uiso 1 1 calc R . . C44 C 0.4953(5) 0.9498(4) 0.8983(3) 0.0286(10) Uani 1 1 d . A . H44A H 0.4171 0.9132 0.9086 0.043 Uiso 1 1 calc R . . H44B H 0.4968 1.0176 0.9113 0.043 Uiso 1 1 calc R . . H44C H 0.5624 0.9500 0.9322 0.043 Uiso 1 1 calc R . . C45 C 0.9217(4) 0.9077(3) 0.6833(3) 0.0230(9) Uani 1 1 d . . . H45 H 0.8842 0.8355 0.6676 0.028 Uiso 1 1 calc R A . C46 C 0.9445(6) 0.9242(5) 0.6040(4) 0.0431(13) Uani 1 1 d . A . H46A H 1.0021 0.8905 0.5765 0.065 Uiso 1 1 calc R . . H46B H 0.9788 0.9947 0.6174 0.065 Uiso 1 1 calc R . . H46C H 0.8670 0.8978 0.5683 0.065 Uiso 1 1 calc R . . C47 C 1.0444(5) 0.9419(5) 0.7398(4) 0.0443(14) Uani 1 1 d . A . H47A H 1.0270 0.9303 0.7890 0.067 Uiso 1 1 calc R . . H47B H 1.0847 1.0122 0.7547 0.067 Uiso 1 1 calc R . . H47C H 1.0981 0.9046 0.7112 0.067 Uiso 1 1 calc R . . C48 C 0.7010(11) 0.4455(8) 0.1778(7) 0.096(3) Uani 1 1 d . . . H48 H 0.6750 0.4509 0.2319 0.115 Uiso 1 1 calc R . . Cl1 Cl 0.3447(6) 0.4081(6) 0.6324(4) 0.0220(9) Uani 0.50 1 d P A 1 O2 O 0.3752(14) 0.4083(13) 0.6178(11) 0.019(3) Uani 0.50 1 d P A 2 Cl2 Cl 0.7975(3) 0.6514(2) 0.54808(17) 0.0269(5) Uani 0.50 1 d P A 3 O3 O 0.7608(7) 0.6800(6) 0.5577(5) 0.0262(18) Uani 0.50 1 d P A 4 Cl3 Cl 0.3993(5) 0.6424(4) 0.6655(3) 0.0231(8) Uani 0.50 1 d P A 5 O4 O 0.4376(13) 0.6530(15) 0.6720(13) 0.045(5) Uani 0.50 1 d P A 6 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 0.0230(3) 0.0093(2) 0.0171(3) 0.0025(2) -0.0079(2) 0.0038(2) Co2 0.0274(3) 0.0100(2) 0.0104(3) 0.0037(2) -0.0009(2) 0.0040(2) O1 0.043(2) 0.046(2) 0.0176(18) -0.0041(16) -0.0049(16) 0.0055(18) Cl4 0.0257(5) 0.0083(4) 0.0199(5) 0.0043(3) -0.0006(4) 0.0056(3) Cl5 0.0461(10) 0.0209(7) 0.0240(8) 0.0155(6) -0.0169(7) -0.0124(7) Cl7 0.323(7) 0.267(6) 0.100(3) 0.095(3) 0.075(4) 0.218(6) Cl8 0.0703(17) 0.127(2) 0.176(4) 0.061(2) 0.009(2) 0.0164(16) Cl6 0.0608(18) 0.414(9) 0.200(5) 0.211(6) -0.031(2) -0.047(3) N1 0.0203(17) 0.0084(14) 0.0159(17) 0.0027(13) -0.0035(14) 0.0045(12) N2 0.0187(17) 0.0096(14) 0.0148(17) 0.0036(13) -0.0014(13) 0.0051(12) N3 0.0182(17) 0.0068(14) 0.0146(16) 0.0023(12) 0.0002(13) 0.0045(12) N4 0.0162(16) 0.0081(14) 0.0153(17) 0.0026(12) -0.0008(13) 0.0024(12) C1 0.0144(18) 0.0148(17) 0.0114(18) 0.0033(15) 0.0007(15) 0.0065(14) C2 0.0159(19) 0.0120(17) 0.0156(19) 0.0057(15) -0.0016(15) 0.0049(14) C3 0.0121(18) 0.0141(17) 0.0134(19) 0.0045(15) -0.0049(15) 0.0021(14) C4 0.023(2) 0.0129(17) 0.0144(19) 0.0042(15) -0.0048(16) 0.0101(15) C5 0.025(2) 0.022(2) 0.027(2) 0.0070(18) -0.0074(19) 0.0079(17) C6 0.037(3) 0.027(2) 0.032(3) 0.004(2) -0.016(2) 0.013(2) C7 0.068(4) 0.036(3) 0.020(2) 0.002(2) -0.016(3) 0.028(3) C8 0.063(4) 0.032(3) 0.019(2) 0.012(2) 0.004(2) 0.022(2) C9 0.036(3) 0.0165(19) 0.020(2) 0.0038(17) 0.0021(19) 0.0077(18) C10 0.0112(17) 0.0119(16) 0.0150(19) 0.0043(14) -0.0001(15) 0.0046(13) C11 0.028(2) 0.0110(17) 0.016(2) 0.0038(15) 0.0002(17) 0.0107(15) C12 0.034(3) 0.0171(19) 0.021(2) 0.0095(17) 0.0014(19) 0.0045(17) C13 0.052(3) 0.024(2) 0.019(2) 0.0106(19) 0.001(2) 0.011(2) C14 0.062(4) 0.026(2) 0.018(2) 0.0066(19) -0.006(2) 0.022(2) C15 0.036(3) 0.028(2) 0.025(2) 0.0019(19) -0.012(2) 0.016(2) C16 0.024(2) 0.021(2) 0.023(2) 0.0089(17) -0.0009(18) 0.0088(17) C17 0.026(2) 0.0094(16) 0.0120(18) 0.0056(14) -0.0053(16) 0.0032(15) C18 0.029(2) 0.021(2) 0.019(2) 0.0076(17) -0.0024(18) 0.0117(17) C19 0.050(3) 0.017(2) 0.033(3) 0.0032(19) -0.011(2) 0.018(2) C20 0.065(4) 0.0115(19) 0.034(3) 0.0058(19) -0.019(3) 0.008(2) C21 0.054(3) 0.018(2) 0.030(3) 0.016(2) -0.012(2) -0.008(2) C22 0.032(2) 0.0178(19) 0.018(2) 0.0081(17) -0.0062(19) -0.0035(17) C23 0.031(3) 0.032(2) 0.028(3) 0.008(2) 0.007(2) 0.020(2) C24 0.039(2) 0.059(3) 0.044(3) 0.017(2) 0.006(2) 0.007(2) C25 0.040(3) 0.069(4) 0.030(3) 0.015(3) 0.012(3) 0.029(3) C26 0.026(2) 0.037(3) 0.032(3) 0.011(2) 0.008(2) -0.003(2) C27 0.039(2) 0.059(3) 0.044(3) 0.017(2) 0.006(2) 0.007(2) C28 0.023(3) 0.049(3) 0.041(3) 0.009(3) 0.004(2) -0.001(2) C29 0.0080(17) 0.0149(17) 0.0128(18) 0.0043(14) 0.0000(14) 0.0057(13) C30 0.0144(18) 0.0156(17) 0.0124(18) 0.0017(15) -0.0044(15) 0.0086(14) C31 0.023(2) 0.0175(18) 0.016(2) 0.0058(16) 0.0021(17) 0.0106(16) C32 0.030(2) 0.033(2) 0.016(2) 0.0071(18) 0.0054(18) 0.0201(19) C33 0.030(2) 0.037(2) 0.013(2) -0.0017(18) -0.0047(18) 0.019(2) C34 0.029(2) 0.021(2) 0.019(2) -0.0021(17) -0.0060(19) 0.0084(18) C35 0.018(2) 0.0177(19) 0.018(2) 0.0035(16) -0.0046(16) 0.0060(16) C36 0.0201(19) 0.0101(16) 0.0092(17) 0.0015(14) -0.0036(15) 0.0057(14) C37 0.019(2) 0.0158(18) 0.0098(18) 0.0013(14) 0.0001(15) 0.0076(15) C38 0.030(2) 0.0139(18) 0.021(2) 0.0016(16) -0.0011(18) 0.0142(17) C39 0.037(3) 0.0099(18) 0.028(2) 0.0031(17) -0.005(2) 0.0069(17) C40 0.024(2) 0.0151(19) 0.028(2) 0.0066(17) -0.0053(19) 0.0007(16) C41 0.018(2) 0.0147(18) 0.017(2) 0.0046(15) -0.0028(16) 0.0029(15) C42 0.019(2) 0.0214(19) 0.020(2) 0.0074(17) 0.0058(17) 0.0119(16) C43 0.020(2) 0.035(2) 0.030(3) 0.016(2) 0.0039(19) 0.0102(19) C44 0.033(3) 0.038(3) 0.022(2) 0.012(2) 0.011(2) 0.023(2) C45 0.019(2) 0.021(2) 0.026(2) 0.0080(18) 0.0039(18) 0.0050(16) C46 0.047(3) 0.050(3) 0.039(3) 0.019(3) 0.021(3) 0.022(3) C47 0.021(3) 0.047(3) 0.060(4) 0.017(3) -0.004(3) 0.011(2) C48 0.106(8) 0.087(7) 0.077(7) 0.044(5) 0.001(6) -0.011(6) Cl1 0.022(2) 0.0287(15) 0.0188(18) 0.0103(12) 0.0070(14) 0.0120(17) O2 0.019(8) 0.011(3) 0.021(8) 0.003(5) -0.004(4) 0.001(5) Cl2 0.0268(15) 0.0233(13) 0.0225(12) 0.0049(10) 0.0004(11) 0.0020(10) O3 0.021(4) 0.031(4) 0.027(4) 0.006(3) 0.005(3) 0.017(3) Cl3 0.027(2) 0.0219(14) 0.0202(14) 0.0073(11) 0.0053(14) 0.0083(15) O4 0.042(11) 0.035(7) 0.056(8) 0.011(6) 0.011(7) 0.018(7) _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 Co2 4.0370(7) . ? Co1 N1 2.024(3) . ? Co1 O2 2.103(13) . ? Co1 N3 2.161(3) . ? Co1 O1 2.175(4) . ? Co1 Cl4 2.3752(11) 2_666 ? Co1 Cl1 2.509(5) . ? Co1 Cl5 2.6949(5) . ? Co2 O3 1.993(8) . ? Co2 N2 2.016(3) . ? Co2 N4 2.169(3) . ? Co2 O4 2.191(17) . ? Co2 Cl4 2.3576(11) . ? Co2 Cl2 2.491(3) . ? Co2 Cl3 2.529(5) . ? Co2 Cl5 2.6599(6) . ? Cl4 Co1 2.3752(11) 2_666 ? Cl5 Co2 2.6599(6) 2_666 ? Cl5 Co1 2.6949(5) 2_666 ? Cl7 C48 1.696(12) . ? Cl8 C48 1.687(12) . ? Cl6 C48 1.669(10) . ? N1 N2 1.321(4) . ? N1 C2 1.345(5) . ? N2 C3 1.354(5) . ? N3 C10 1.288(5) . ? N3 C17 1.452(4) . ? N4 C29 1.295(5) . ? N4 C36 1.455(4) . ? C1 C3 1.407(5) . ? C1 C2 1.418(5) . ? C1 C4 1.480(5) . ? C2 C10 1.480(5) . ? C3 C29 1.485(5) . ? C4 C9 1.396(6) . ? C4 C5 1.402(6) . ? C5 C6 1.398(7) . ? C6 C7 1.385(9) . ? C7 C8 1.387(9) . ? C8 C9 1.383(7) . ? C10 C11 1.487(5) . ? C11 C16 1.387(6) . ? C11 C12 1.402(6) . ? C12 C13 1.375(7) . ? C13 C14 1.387(8) . ? C14 C15 1.380(8) . ? C15 C16 1.393(6) . ? C17 C22 1.408(6) . ? C17 C18 1.414(6) . ? C18 C19 1.387(6) . ? C18 C23 1.529(7) . ? C19 C20 1.366(9) . ? C20 C21 1.385(9) . ? C21 C22 1.400(6) . ? C22 C26 1.516(7) . ? C23 C24 1.535(8) . ? C23 C25 1.541(7) . ? C26 C28 1.536(8) . ? C26 C27 1.542(8) . ? C29 C30 1.496(5) . ? C30 C31 1.399(6) . ? C30 C35 1.400(6) . ? C31 C32 1.391(6) . ? C32 C33 1.395(7) . ? C33 C34 1.383(7) . ? C34 C35 1.388(6) . ? C36 C41 1.401(6) . ? C36 C37 1.404(5) . ? C37 C38 1.405(5) . ? C37 C42 1.509(6) . ? C38 C39 1.376(7) . ? C39 C40 1.377(7) . ? C40 C41 1.394(6) . ? C41 C45 1.528(6) . ? C42 C44 1.533(6) . ? C42 C43 1.537(6) . ? C45 C46 1.524(7) . ? C45 C47 1.534(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 O2 89.5(5) . . ? N1 Co1 N3 76.25(13) . . ? O2 Co1 N3 99.5(5) . . ? N1 Co1 O1 85.56(14) . . ? O2 Co1 O1 160.4(5) . . ? N3 Co1 O1 97.63(15) . . ? N1 Co1 Cl4 174.60(11) . 2_666 ? O2 Co1 Cl4 95.4(5) . 2_666 ? N3 Co1 Cl4 105.19(9) . 2_666 ? O1 Co1 Cl4 89.08(10) . 2_666 ? N1 Co1 Cl1 88.7(2) . . ? O2 Co1 Cl1 3.6(6) . . ? N3 Co1 Cl1 95.89(19) . . ? O1 Co1 Cl1 163.6(2) . . ? Cl4 Co1 Cl1 96.25(19) 2_666 . ? N1 Co1 Cl5 88.50(9) . . ? O2 Co1 Cl5 78.3(5) . . ? N3 Co1 Cl5 164.66(8) . . ? O1 Co1 Cl5 82.63(12) . . ? Cl4 Co1 Cl5 90.14(3) 2_666 . ? Cl1 Co1 Cl5 81.89(16) . . ? O3 Co2 N2 97.8(3) . . ? O3 Co2 N4 98.4(3) . . ? N2 Co2 N4 76.50(13) . . ? O3 Co2 O4 170.3(6) . . ? N2 Co2 O4 80.8(5) . . ? N4 Co2 O4 90.6(5) . . ? O3 Co2 Cl4 87.2(2) . . ? N2 Co2 Cl4 175.08(11) . . ? N4 Co2 Cl4 102.78(9) . . ? O4 Co2 Cl4 94.3(5) . . ? O3 Co2 Cl2 11.2(2) . . ? N2 Co2 Cl2 87.67(12) . . ? N4 Co2 Cl2 100.72(11) . . ? O4 Co2 Cl2 161.6(5) . . ? Cl4 Co2 Cl2 97.24(8) . . ? O3 Co2 Cl3 166.0(3) . . ? N2 Co2 Cl3 84.84(16) . . ? N4 Co2 Cl3 95.62(16) . . ? O4 Co2 Cl3 5.8(6) . . ? Cl4 Co2 Cl3 90.41(13) . . ? Cl2 Co2 Cl3 159.90(15) . . ? O3 Co2 Cl5 86.5(2) . . ? N2 Co2 Cl5 89.01(9) . . ? N4 Co2 Cl5 165.17(9) . . ? O4 Co2 Cl5 83.9(5) . . ? Cl4 Co2 Cl5 91.38(3) . . ? Cl2 Co2 Cl5 81.52(6) . . ? Cl3 Co2 Cl5 79.73(13) . . ? Co2 Cl4 Co1 96.04(4) . 2_666 ? Co2 Cl5 Co2 180.00(2) . 2_666 ? Co2 Cl5 Co1 82.142(17) . 2_666 ? Co2 Cl5 Co1 97.858(17) 2_666 2_666 ? Co2 Cl5 Co1 97.858(17) . . ? Co2 Cl5 Co1 82.142(17) 2_666 . ? Co1 Cl5 Co1 180.0 2_666 . ? N2 N1 C2 109.1(3) . . ? N2 N1 Co1 131.6(3) . . ? C2 N1 Co1 118.6(2) . . ? N1 N2 C3 108.9(3) . . ? N1 N2 Co2 132.6(3) . . ? C3 N2 Co2 118.6(2) . . ? C10 N3 C17 120.7(3) . . ? C10 N3 Co1 115.3(2) . . ? C17 N3 Co1 123.5(2) . . ? C29 N4 C36 120.4(3) . . ? C29 N4 Co2 114.3(2) . . ? C36 N4 Co2 124.1(2) . . ? C3 C1 C2 102.2(3) . . ? C3 C1 C4 127.6(3) . . ? C2 C1 C4 130.1(3) . . ? N1 C2 C1 109.9(3) . . ? N1 C2 C10 114.0(3) . . ? C1 C2 C10 136.1(4) . . ? N2 C3 C1 109.9(3) . . ? N2 C3 C29 113.9(3) . . ? C1 C3 C29 136.2(4) . . ? C9 C4 C5 118.3(4) . . ? C9 C4 C1 121.5(4) . . ? C5 C4 C1 120.1(4) . . ? C6 C5 C4 120.5(5) . . ? C7 C6 C5 119.9(5) . . ? C6 C7 C8 120.0(5) . . ? C9 C8 C7 120.2(5) . . ? C8 C9 C4 121.0(5) . . ? N3 C10 C2 115.5(3) . . ? N3 C10 C11 125.6(3) . . ? C2 C10 C11 118.9(3) . . ? C16 C11 C12 118.8(4) . . ? C16 C11 C10 120.9(4) . . ? C12 C11 C10 120.1(4) . . ? C13 C12 C11 120.5(5) . . ? C12 C13 C14 120.2(5) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C16 119.9(5) . . ? C11 C16 C15 120.5(4) . . ? C22 C17 C18 120.9(4) . . ? C22 C17 N3 119.1(4) . . ? C18 C17 N3 119.7(4) . . ? C19 C18 C17 117.6(4) . . ? C19 C18 C23 119.6(4) . . ? C17 C18 C23 122.7(4) . . ? C20 C19 C18 122.7(5) . . ? C19 C20 C21 119.3(4) . . ? C20 C21 C22 121.3(5) . . ? C21 C22 C17 118.1(5) . . ? C21 C22 C26 118.9(5) . . ? C17 C22 C26 122.9(4) . . ? C18 C23 C24 111.8(4) . . ? C18 C23 C25 108.8(4) . . ? C24 C23 C25 110.2(4) . . ? C22 C26 C28 110.0(4) . . ? C22 C26 C27 112.9(5) . . ? C28 C26 C27 109.2(4) . . ? N4 C29 C3 115.1(3) . . ? N4 C29 C30 126.0(3) . . ? C3 C29 C30 118.6(3) . . ? C31 C30 C35 119.4(4) . . ? C31 C30 C29 116.9(3) . . ? C35 C30 C29 123.7(4) . . ? C32 C31 C30 120.8(4) . . ? C31 C32 C33 119.3(4) . . ? C34 C33 C32 120.0(4) . . ? C33 C34 C35 121.1(4) . . ? C34 C35 C30 119.4(4) . . ? C41 C36 C37 121.4(3) . . ? C41 C36 N4 117.1(3) . . ? C37 C36 N4 121.4(4) . . ? C36 C37 C38 117.4(4) . . ? C36 C37 C42 123.1(3) . . ? C38 C37 C42 119.6(4) . . ? C39 C38 C37 121.2(4) . . ? C38 C39 C40 120.6(4) . . ? C39 C40 C41 120.3(4) . . ? C40 C41 C36 118.8(4) . . ? C40 C41 C45 119.1(4) . . ? C36 C41 C45 122.2(3) . . ? C37 C42 C44 111.3(4) . . ? C37 C42 C43 110.9(4) . . ? C44 C42 C43 109.8(4) . . ? C46 C45 C41 111.0(4) . . ? C46 C45 C47 111.4(5) . . ? C41 C45 C47 111.2(4) . . ? Cl6 C48 Cl8 114.0(6) . . ? Cl6 C48 Cl7 112.3(8) . . ? Cl8 C48 Cl7 112.9(6) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.113 _refine_diff_density_min -1.454 _refine_diff_density_rms 0.105 # Attachment '_HL2_.cif' data_as36a _database_code_depnum_ccdc_archive 'CCDC 728437' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H42 N4' _chemical_formula_sum 'C35 H42 N4' _chemical_formula_weight 518.73 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.7190(14) _cell_length_b 8.8990(3) _cell_length_c 25.4394(14) _cell_angle_alpha 90.00 _cell_angle_beta 100.727(4) _cell_angle_gamma 90.00 _cell_volume 6165.5(5) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 26988 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 26.78 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26988 _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.78 _reflns_number_total 6546 _reflns_number_gt 4224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2007)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2007)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0606P)^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 6546 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 N1 N 0.03937(6) 1.0283(2) 0.20707(6) 0.0195(4) Uani 1 1 d . . . N2 N 0.04327(6) 1.1115(2) 0.16413(6) 0.0220(4) Uani 1 1 d . . . N3 N 0.05526(5) 0.8733(2) 0.31124(6) 0.0199(3) Uani 1 1 d . . . N4 N 0.14515(6) 1.3315(2) 0.14307(6) 0.0224(4) Uani 1 1 d . . . C1 C 0.11685(6) 1.1011(2) 0.22162(7) 0.0196(4) Uani 1 1 d . . . C2 C 0.08264(6) 1.0181(2) 0.24249(7) 0.0192(4) Uani 1 1 d . . . C3 C 0.09034(6) 1.1586(2) 0.17296(8) 0.0203(4) Uani 1 1 d . . . C5 C 0.18457(9) 1.1783(3) 0.29556(10) 0.0397(6) Uani 1 1 d . . . H5 H 0.1614 1.2191 0.3136 0.048 Uiso 1 1 calc R . . C6 C 0.23449(11) 1.1829(4) 0.31891(12) 0.0620(9) Uani 1 1 d . . . H6 H 0.2446 1.2277 0.3522 0.074 Uiso 1 1 calc R . . C7 C 0.26870(9) 1.1200(4) 0.29206(13) 0.0612(10) Uani 1 1 d . . . H7 H 0.3019 1.1232 0.3072 0.073 Uiso 1 1 calc R . . C8 C 0.25403(9) 1.0540(4) 0.24394(14) 0.0581(9) Uani 1 1 d . . . H8 H 0.2772 1.0109 0.2264 0.070 Uiso 1 1 calc R . . C9 C 0.20458(8) 1.0500(3) 0.22030(11) 0.0411(6) Uani 1 1 d . . . H9 H 0.1949 1.0043 0.1871 0.049 Uiso 1 1 calc R . . C10 C 0.09004(7) 0.9314(2) 0.29117(7) 0.0196(4) Uani 1 1 d . . . H10 H 0.1221 0.9166 0.3091 0.024 Uiso 1 1 calc R . . C11 C 0.07011(6) 0.7901(3) 0.36022(8) 0.0216(4) Uani 1 1 d . . . C12 C 0.07820(7) 0.8670(3) 0.40912(8) 0.0256(5) Uani 1 1 d . . . C13 C 0.09320(8) 0.7822(3) 0.45565(9) 0.0334(5) Uani 1 1 d . . . H13 H 0.0988 0.8302 0.4887 0.040 Uiso 1 1 calc R . . C14 C 0.09984(8) 0.6304(3) 0.45357(9) 0.0362(6) Uani 1 1 d . . . H14 H 0.1104 0.5766 0.4850 0.043 Uiso 1 1 calc R . . C15 C 0.09094(8) 0.5567(3) 0.40517(9) 0.0334(5) Uani 1 1 d . . . H15 H 0.0953 0.4531 0.4044 0.040 Uiso 1 1 calc R . . C16 C 0.07552(7) 0.6338(3) 0.35720(8) 0.0256(5) Uani 1 1 d . . . C17 C 0.07410(8) 1.0361(3) 0.41304(9) 0.0307(5) Uani 1 1 d . . . H17 H 0.0589 1.0739 0.3776 0.037 Uiso 1 1 calc R . . C19 C 0.12555(9) 1.1049(3) 0.42758(10) 0.0397(6) Uani 1 1 d . . . H19A H 0.1229 1.2122 0.4298 0.059 Uiso 1 1 calc R . . H19B H 0.1442 1.0795 0.4006 0.059 Uiso 1 1 calc R . . H19C H 0.1418 1.0662 0.4615 0.059 Uiso 1 1 calc R . . C18 C 0.04188(10) 1.0844(4) 0.45265(10) 0.0488(7) Uani 1 1 d . . . H18A H 0.0402 1.1921 0.4536 0.073 Uiso 1 1 calc R . . H18B H 0.0557 1.0472 0.4876 0.073 Uiso 1 1 calc R . . H18C H 0.0094 1.0441 0.4416 0.073 Uiso 1 1 calc R . . C20 C 0.06737(8) 0.5528(3) 0.30369(9) 0.0321(5) Uani 1 1 d . . . H20 H 0.0422 0.6084 0.2790 0.039 Uiso 1 1 calc R . . C22 C 0.11441(9) 0.5517(3) 0.27983(10) 0.0406(6) Uani 1 1 d . . . H22A H 0.1083 0.4999 0.2461 0.061 Uiso 1 1 calc R . . H22B H 0.1401 0.5014 0.3039 0.061 Uiso 1 1 calc R . . H22C H 0.1242 0.6532 0.2745 0.061 Uiso 1 1 calc R . . C21 C 0.04915(10) 0.3918(3) 0.30680(13) 0.0492(7) Uani 1 1 d . . . H21A H 0.0446 0.3465 0.2720 0.074 Uiso 1 1 calc R . . H21B H 0.0185 0.3924 0.3191 0.074 Uiso 1 1 calc R . . H21C H 0.0729 0.3351 0.3312 0.074 Uiso 1 1 calc R . . C25 C 0.13080(7) 1.5637(2) 0.08910(8) 0.0234(4) Uani 1 1 d . . . C26 C 0.14835(8) 1.6617(3) 0.05445(9) 0.0305(5) Uani 1 1 d . . . H26 H 0.1312 1.7500 0.0442 0.037 Uiso 1 1 calc R . . C27 C 0.19056(8) 1.6311(3) 0.03484(9) 0.0365(6) Uani 1 1 d . . . H27 H 0.2012 1.6974 0.0112 0.044 Uiso 1 1 calc R . . C29 C 0.21690(8) 1.5015(3) 0.05056(9) 0.0335(5) Uani 1 1 d . . . H29 H 0.2454 1.4817 0.0373 0.040 Uiso 1 1 calc R . . C30 C 0.20165(7) 1.4005(3) 0.08568(8) 0.0268(5) Uani 1 1 d . . . C31 C 0.08393(8) 1.6022(3) 0.10946(9) 0.0318(5) Uani 1 1 d . . . H31 H 0.0812 1.5326 0.1386 0.038 Uiso 1 1 calc R . . C32 C 0.03876(9) 1.5810(3) 0.06567(11) 0.0445(7) Uani 1 1 d . . . H32A H 0.0098 1.6053 0.0795 0.067 Uiso 1 1 calc R . . H32B H 0.0370 1.4785 0.0538 0.067 Uiso 1 1 calc R . . H32C H 0.0410 1.6461 0.0361 0.067 Uiso 1 1 calc R . . C33 C 0.08497(13) 1.7618(4) 0.13178(14) 0.0605(8) Uani 1 1 d . . . H33A H 0.0549 1.7814 0.1442 0.091 Uiso 1 1 calc R . . H33B H 0.0884 1.8323 0.1042 0.091 Uiso 1 1 calc R . . H33C H 0.1122 1.7720 0.1610 0.091 Uiso 1 1 calc R . . C34 C 0.23028(7) 1.2593(3) 0.10471(10) 0.0341(5) Uani 1 1 d . . . H34 H 0.2261 1.2411 0.1416 0.041 Uiso 1 1 calc R . . C36 C 0.28534(9) 1.2750(5) 0.10576(15) 0.0696(11) Uani 1 1 d . . . H36A H 0.3015 1.1826 0.1179 0.104 Uiso 1 1 calc R . . H36B H 0.2983 1.3549 0.1296 0.104 Uiso 1 1 calc R . . H36C H 0.2908 1.2974 0.0704 0.104 Uiso 1 1 calc R . . C35 C 0.20910(11) 1.1234(3) 0.07171(11) 0.0509(7) Uani 1 1 d . . . H35A H 0.2279 1.0356 0.0842 0.076 Uiso 1 1 calc R . . H35B H 0.2105 1.1403 0.0347 0.076 Uiso 1 1 calc R . . H35C H 0.1756 1.1088 0.0754 0.076 Uiso 1 1 calc R . . C4 C 0.16967(7) 1.1139(3) 0.24608(8) 0.0252(4) Uani 1 1 d . . . C24 C 0.15758(7) 1.4311(2) 0.10414(7) 0.0213(4) Uani 1 1 d . . . C23 C 0.10527(7) 1.2582(2) 0.13335(8) 0.0206(4) Uani 1 1 d . . . H23 H 0.0850 1.2682 0.1000 0.025 Uiso 1 1 calc R . . H1 H 0.0128(9) 0.971(3) 0.2060(9) 0.024(6) Uiso 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 N1 0.0158(7) 0.0236(10) 0.0191(8) 0.0025(7) 0.0037(6) -0.0014(7) N2 0.0181(7) 0.0257(9) 0.0223(8) 0.0036(7) 0.0039(6) -0.0016(7) N3 0.0192(7) 0.0203(9) 0.0209(8) 0.0021(7) 0.0052(6) 0.0029(7) N4 0.0188(7) 0.0260(10) 0.0226(8) 0.0034(7) 0.0040(6) 0.0002(7) C1 0.0165(8) 0.0203(10) 0.0222(9) 0.0006(8) 0.0042(7) -0.0002(7) C2 0.0151(8) 0.0226(11) 0.0195(9) -0.0008(8) 0.0024(7) 0.0002(7) C3 0.0165(8) 0.0218(11) 0.0228(9) 0.0009(8) 0.0044(7) -0.0002(7) C5 0.0349(12) 0.0466(16) 0.0343(12) 0.0046(11) -0.0017(10) -0.0132(11) C6 0.0521(17) 0.076(2) 0.0459(16) 0.0153(16) -0.0206(13) -0.0285(17) C7 0.0210(11) 0.080(2) 0.075(2) 0.0416(19) -0.0107(13) -0.0107(14) C8 0.0190(11) 0.074(2) 0.080(2) 0.0256(18) 0.0066(13) 0.0087(13) C9 0.0231(10) 0.0490(16) 0.0516(15) 0.0075(13) 0.0080(10) 0.0068(11) C10 0.0149(8) 0.0209(11) 0.0228(9) -0.0004(8) 0.0027(7) 0.0014(7) C11 0.0122(8) 0.0297(12) 0.0231(9) 0.0068(9) 0.0041(7) 0.0002(8) C12 0.0201(9) 0.0321(13) 0.0247(10) 0.0031(9) 0.0046(7) 0.0034(9) C13 0.0293(11) 0.0472(16) 0.0232(10) 0.0059(10) 0.0040(8) -0.0001(10) C14 0.0311(11) 0.0452(16) 0.0318(12) 0.0191(11) 0.0044(9) 0.0024(11) C15 0.0270(10) 0.0300(13) 0.0435(13) 0.0134(11) 0.0072(9) 0.0015(9) C16 0.0154(8) 0.0270(12) 0.0345(11) 0.0056(9) 0.0048(8) 0.0002(8) C17 0.0326(11) 0.0350(14) 0.0230(10) -0.0019(10) 0.0012(8) 0.0083(10) C19 0.0470(13) 0.0318(14) 0.0373(12) -0.0045(11) 0.0002(11) -0.0020(11) C18 0.0487(14) 0.065(2) 0.0324(13) -0.0085(13) 0.0055(11) 0.0188(14) C20 0.0281(10) 0.0243(12) 0.0417(13) 0.0014(10) 0.0007(9) 0.0025(9) C22 0.0462(13) 0.0343(14) 0.0443(14) -0.0061(12) 0.0161(11) 0.0001(11) C21 0.0425(13) 0.0335(15) 0.0697(18) -0.0031(14) 0.0058(13) -0.0048(12) C25 0.0256(9) 0.0243(11) 0.0193(9) -0.0014(8) 0.0014(7) -0.0032(8) C26 0.0320(11) 0.0275(13) 0.0299(11) 0.0039(9) 0.0007(9) -0.0018(9) C27 0.0324(11) 0.0401(15) 0.0367(12) 0.0118(11) 0.0054(9) -0.0113(11) C29 0.0209(9) 0.0487(16) 0.0313(11) 0.0080(11) 0.0062(8) -0.0043(9) C30 0.0171(9) 0.0354(13) 0.0274(10) 0.0016(9) 0.0026(8) -0.0024(9) C31 0.0368(11) 0.0327(13) 0.0281(11) 0.0039(10) 0.0119(9) 0.0096(10) C32 0.0296(11) 0.0558(19) 0.0493(15) 0.0103(13) 0.0101(11) 0.0103(11) C33 0.078(2) 0.0418(18) 0.0658(19) -0.0129(15) 0.0240(17) 0.0175(16) C34 0.0202(10) 0.0444(15) 0.0391(12) 0.0118(11) 0.0096(9) 0.0068(9) C36 0.0239(12) 0.089(3) 0.098(3) 0.039(2) 0.0161(14) 0.0164(14) C35 0.0571(16) 0.0441(17) 0.0530(16) 0.0006(14) 0.0138(13) 0.0194(14) C4 0.0166(9) 0.0285(12) 0.0293(10) 0.0114(9) 0.0010(8) -0.0033(8) C24 0.0207(9) 0.0248(11) 0.0182(9) 0.0010(8) 0.0027(7) -0.0034(8) C23 0.0192(9) 0.0240(11) 0.0182(9) 0.0011(8) 0.0020(7) 0.0012(8) _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 N2 1.340(2) . ? N1 C2 1.363(2) . ? N2 C3 1.349(2) . ? N3 C10 1.281(2) . ? N3 C11 1.442(2) . ? N4 C23 1.268(3) . ? N4 C24 1.419(3) . ? C1 C2 1.383(3) . ? C1 C3 1.413(3) . ? C1 C4 1.485(2) . ? C2 C10 1.441(3) . ? C3 C23 1.459(3) . ? C5 C4 1.375(3) . ? C5 C6 1.401(4) . ? C6 C7 1.386(5) . ? C7 C8 1.350(5) . ? C8 C9 1.391(3) . ? C9 C4 1.388(3) . ? C11 C12 1.401(3) . ? C11 C16 1.402(3) . ? C12 C13 1.400(3) . ? C12 C17 1.514(3) . ? C13 C14 1.366(4) . ? C14 C15 1.376(4) . ? C15 C16 1.396(3) . ? C16 C20 1.519(3) . ? C17 C18 1.527(3) . ? C17 C19 1.533(3) . ? C20 C21 1.527(4) . ? C20 C22 1.537(3) . ? C25 C26 1.390(3) . ? C25 C24 1.408(3) . ? C25 C31 1.525(3) . ? C26 C27 1.382(3) . ? C27 C29 1.384(4) . ? C29 C30 1.387(3) . ? C30 C24 1.414(3) . ? C30 C34 1.517(3) . ? C31 C32 1.525(3) . ? C31 C33 1.528(4) . ? C34 C35 1.526(4) . ? C34 C36 1.528(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 N2 N1 C2 112.40(15) . . ? N1 N2 C3 104.98(15) . . ? C10 N3 C11 115.90(15) . . ? C23 N4 C24 120.11(17) . . ? C2 C1 C3 104.35(15) . . ? C2 C1 C4 124.94(17) . . ? C3 C1 C4 130.63(17) . . ? N1 C2 C1 107.01(16) . . ? N1 C2 C10 124.80(17) . . ? C1 C2 C10 128.16(16) . . ? N2 C3 C1 111.25(17) . . ? N2 C3 C23 117.65(17) . . ? C1 C3 C23 131.09(17) . . ? C4 C5 C6 120.3(3) . . ? C7 C6 C5 119.5(3) . . ? C8 C7 C6 120.3(2) . . ? C7 C8 C9 120.6(3) . . ? C4 C9 C8 120.2(3) . . ? N3 C10 C2 124.16(17) . . ? C12 C11 C16 122.15(19) . . ? C12 C11 N3 119.3(2) . . ? C16 C11 N3 118.55(18) . . ? C13 C12 C11 117.4(2) . . ? C13 C12 C17 119.6(2) . . ? C11 C12 C17 122.86(19) . . ? C14 C13 C12 121.4(2) . . ? C13 C14 C15 120.2(2) . . ? C14 C15 C16 121.5(2) . . ? C15 C16 C11 117.3(2) . . ? C15 C16 C20 121.3(2) . . ? C11 C16 C20 121.32(19) . . ? C12 C17 C18 112.5(2) . . ? C12 C17 C19 109.60(18) . . ? C18 C17 C19 111.1(2) . . ? C16 C20 C21 113.2(2) . . ? C16 C20 C22 111.18(18) . . ? C21 C20 C22 109.1(2) . . ? C26 C25 C24 117.94(19) . . ? C26 C25 C31 119.7(2) . . ? C24 C25 C31 122.38(19) . . ? C27 C26 C25 121.7(2) . . ? C26 C27 C29 119.8(2) . . ? C27 C29 C30 121.2(2) . . ? C29 C30 C24 118.3(2) . . ? C29 C30 C34 122.54(18) . . ? C24 C30 C34 119.11(19) . . ? C25 C31 C32 111.09(18) . . ? C25 C31 C33 112.1(2) . . ? C32 C31 C33 110.0(2) . . ? C30 C34 C35 110.87(19) . . ? C30 C34 C36 113.0(2) . . ? C35 C34 C36 111.3(2) . . ? C5 C4 C9 119.1(2) . . ? C5 C4 C1 121.4(2) . . ? C9 C4 C1 119.4(2) . . ? C25 C24 C30 121.02(19) . . ? C25 C24 N4 121.92(17) . . ? C30 C24 N4 116.65(18) . . ? N4 C23 C3 121.80(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 N3 0.89(2) 2.05(2) 2.923(2) 166(2) 2 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.78 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.212 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.047