data_Co(acacen)(Im)2 _audit_update_record ; 2012-10-16 # Formatted by publCIF ; _audit_creation_date 2012-06-05 _audit_creation_method ; Olex2 1.2 (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _publ_contact_author_address ? _publ_contact_author_email tmeade@northwestern.edu _publ_contact_author_name 'Thomas J. Meade' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; trans-bis(imidazole)-(N,N'-ethylene-bis(acetylacetoniminato)) -cobalt(iii) tetraphenylborate ethanol solvate ; _chemical_formula_moiety 'C18 H25 Co N6 O2, C2 H6 O, C24 H20 B' _chemical_formula_sum 'C44 H51 B Co N6 O3' _chemical_formula_weight 781.65 _chemical_melting_point ? 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' 'B' 'B' 0.0013 0.0007 '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' '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' _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_H-M_alt 'P 1 21/m 1' _space_group_name_Hall '-P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' 3 '-x, -y, -z' 4 'x, -y-1/2, z' _cell_length_a 9.6818(5) _cell_length_b 14.5560(8) _cell_length_c 14.3710(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.273(2) _cell_angle_gamma 90.00 _cell_volume 2004.20(19) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3483 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.96 _cell_measurement_theta_min 2.55 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.8436 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; TWINABS-2008/4 (Bruker,2010) was used for absorption correction. For component 1: wR2(int) was 0.0730 before and 0.0471 after correction. The Ratio of minimum to maximum transmission is 0.64. The \l/2 correction factor is Not present For component 2: wR2(int) was 0.0862 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.64. The \l/2 correction factor is Not present ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 826 _exptl_crystal_size_max 0.369 _exptl_crystal_size_mid 0.252 _exptl_crystal_size_min 0.03 _exptl_special_details ? _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_unetI/netI 0.0384 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6066 _diffrn_reflns_theta_full 30.07 _diffrn_reflns_theta_max 30.07 _diffrn_reflns_theta_min 2.00 _diffrn_ambient_temperature 100.09 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 5080 _reflns_number_total 6066 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_collection 'APEX2 V2.1-4 (Bruker, 2007)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.771 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.076 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 339 _refine_ls_number_reflns 6066 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0459 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+1.0256P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1190 _refine_ls_wR_factor_ref 0.1278 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.52092(3) 0.7500 0.65709(2) 0.01564(9) Uani 1 2 d S . . O1 O 0.37575(15) 0.83626(10) 0.65328(10) 0.0321(3) Uani 1 1 d . . . N1 N 0.6645(2) 0.83797(18) 0.66121(13) 0.0484(6) Uani 1 1 d . . . N2 N 0.4950(2) 0.7500 0.52097(14) 0.0169(4) Uani 1 2 d S . . N3 N 0.3875(2) 0.7500 0.37625(15) 0.0268(5) Uani 1 2 d S . . H3 H 0.3197 0.7500 0.3284 0.032 Uiso 1 2 calc SR A . N4 N 0.5418(2) 0.7500 0.79239(14) 0.0196(4) Uani 1 2 d S . . N5 N 0.57624(18) 0.70303(12) 0.94006(11) 0.0262(4) Uani 0.50 1 d P . 1 H5 H 0.5879 0.6670 0.9898 0.031 Uiso 0.50 1 calc PR . 1 C1 C 0.2190(4) 0.9604(3) 0.6374(3) 0.0281(10) Uani 0.495(5) 1 d P A 1 H1A H 0.1526 0.9304 0.5889 0.042 Uiso 0.495(5) 1 calc PR A 1 H1B H 0.2246 1.0259 0.6229 0.042 Uiso 0.495(5) 1 calc PR A 1 H1C H 0.1874 0.9529 0.6988 0.042 Uiso 0.495(5) 1 calc PR A 1 C1A C 0.2927(4) 0.9877(3) 0.6112(3) 0.0280(9) Uani 0.505(5) 1 d P A 2 H1AA H 0.2322 0.9639 0.5559 0.042 Uiso 0.505(5) 1 calc PR A 2 H1AB H 0.3218 1.0504 0.5985 0.042 Uiso 0.505(5) 1 calc PR A 2 H1AC H 0.2416 0.9881 0.6653 0.042 Uiso 0.505(5) 1 calc PR A 2 C2 C 0.3614(6) 0.9170(4) 0.6400(3) 0.0200(9) Uani 0.495(5) 1 d P A 1 C2A C 0.4190(7) 0.9277(3) 0.6323(3) 0.0188(9) Uani 0.505(5) 1 d P A 2 C3 C 0.4743(8) 0.9697(3) 0.6308(3) 0.0235(9) Uani 0.495(5) 1 d P A 1 H3A H 0.4584 1.0333 0.6188 0.028 Uiso 0.495(5) 1 calc PR A 1 C3A C 0.5497(8) 0.9618(3) 0.6288(3) 0.0209(8) Uani 0.505(5) 1 d P A 2 H3AA H 0.5563 1.0236 0.6087 0.025 Uiso 0.505(5) 1 calc PR A 2 C4 C 0.6139(7) 0.9382(3) 0.6377(3) 0.0197(8) Uani 0.495(5) 1 d P A 1 C4A C 0.6762(5) 0.9127(3) 0.6527(3) 0.0200(8) Uani 0.505(5) 1 d P A 2 C5 C 0.7268(5) 1.0076(3) 0.6256(3) 0.0309(10) Uani 0.495(5) 1 d P A 1 H5A H 0.7872 1.0163 0.6858 0.046 Uiso 0.495(5) 1 calc PR A 1 H5B H 0.6835 1.0663 0.6047 0.046 Uiso 0.495(5) 1 calc PR A 1 H5C H 0.7825 0.9851 0.5786 0.046 Uiso 0.495(5) 1 calc PR A 1 C5A C 0.8118(4) 0.9670(3) 0.6650(3) 0.0304(10) Uani 0.505(5) 1 d P A 2 H5AA H 0.8592 0.9598 0.7296 0.046 Uiso 0.505(5) 1 calc PR A 2 H5AB H 0.7914 1.0321 0.6524 0.046 Uiso 0.505(5) 1 calc PR A 2 H5AC H 0.8722 0.9440 0.6210 0.046 Uiso 0.505(5) 1 calc PR A 2 C6 C 0.7961(4) 0.8230(3) 0.6647(3) 0.0235(7) Uani 0.50 1 d P . -1 H6A H 0.8523 0.8670 0.7071 0.028 Uiso 0.50 1 calc PR . -1 H6B H 0.8253 0.8257 0.6016 0.028 Uiso 0.50 1 calc PR . -1 C7 C 0.8063(3) 0.7259(2) 0.7045(3) 0.0214(8) Uani 0.50 1 d P . -1 H7A H 0.8140 0.7287 0.7739 0.026 Uiso 0.50 1 calc PR . -1 H7B H 0.8916 0.6961 0.6883 0.026 Uiso 0.50 1 calc PR . -1 C8 C 0.3717(3) 0.7500 0.46730(17) 0.0201(5) Uani 1 2 d S A . H8 H 0.2844 0.7500 0.4902 0.024 Uiso 1 2 calc SR . . C9 C 0.5280(3) 0.7500 0.37066(19) 0.0306(6) Uani 1 2 d S A . H9 H 0.5704 0.7500 0.3150 0.037 Uiso 1 2 calc SR . . C10 C 0.5940(3) 0.7500 0.46043(18) 0.0234(5) Uani 1 2 d S A . H10 H 0.6923 0.7500 0.4788 0.028 Uiso 1 2 calc SR . . C11 C 0.5548(2) 0.67596(13) 0.84909(13) 0.0265(4) Uani 1 1 d . . . H11 H 0.5497 0.6139 0.8283 0.032 Uiso 1 1 calc R B 1 C12 C 0.57624(18) 0.70303(12) 0.94006(11) 0.0262(4) Uani 0.50 1 d P . 2 O2 O 0.1211(3) 0.7919(3) 0.7178(2) 0.0474(9) Uani 0.50 1 d P C -1 H2 H 0.1607 0.7422 0.7082 0.071 Uiso 0.50 1 calc PR C -1 C40 C 0.1495(5) 0.8143(4) 0.8124(3) 0.0420(11) Uani 0.50 1 d P C -1 H40A H 0.2282 0.8585 0.8195 0.050 Uiso 0.50 1 calc PR C -1 H40B H 0.0673 0.8478 0.8287 0.050 Uiso 0.50 1 calc PR C -1 C41 C 0.1806(5) 0.7500 0.8766(4) 0.0754(15) Uani 0.50 1 d S C -1 H41A H 0.0969 0.7139 0.8825 0.113 Uiso 0.50 1 calc PR C -1 H41B H 0.2152 0.7787 0.9372 0.113 Uiso 0.50 1 calc PR C -1 H41C H 0.2528 0.7096 0.8579 0.113 Uiso 0.50 1 calc PR C -1 C19 C 1.14092(16) 1.16020(11) 0.87164(12) 0.0179(3) Uani 1 1 d . . . C20 C 1.25520(18) 1.12219(12) 0.83503(14) 0.0223(3) Uani 1 1 d . . . H20 H 1.2828 1.1490 0.7803 0.027 Uiso 1 1 calc R . . C21 C 1.3296(2) 1.04694(13) 0.87557(16) 0.0303(4) Uani 1 1 d . . . H21 H 1.4061 1.0235 0.8483 0.036 Uiso 1 1 calc R . . C22 C 1.2927(2) 1.00611(14) 0.95531(16) 0.0333(5) Uani 1 1 d . . . H22 H 1.3421 0.9540 0.9824 0.040 Uiso 1 1 calc R . . C23 C 1.1824(2) 1.04250(14) 0.99510(15) 0.0307(4) Uani 1 1 d . . . H23 H 1.1566 1.0157 1.0503 0.037 Uiso 1 1 calc R . . C24 C 1.10922(18) 1.11847(13) 0.95418(13) 0.0232(3) Uani 1 1 d . . . H24 H 1.0351 1.1429 0.9833 0.028 Uiso 1 1 calc R . . C25 C 0.8917(2) 1.2500 0.83891(16) 0.0190(5) Uani 1 2 d S . . C26 C 0.81534(18) 1.16852(14) 0.84100(13) 0.0244(4) Uani 1 1 d . . . H26 H 0.8617 1.1115 0.8367 0.029 Uiso 1 1 calc R . . C27 C 0.67307(19) 1.16835(17) 0.84914(13) 0.0326(5) Uani 1 1 d . . . H27 H 0.6250 1.1116 0.8510 0.039 Uiso 1 1 calc R . . C28 C 0.6021(3) 1.2500 0.85454(19) 0.0348(7) Uani 1 2 d S . . H28 H 0.5061 1.2500 0.8618 0.042 Uiso 1 2 calc SR . . C31 C 1.0467(2) 1.2500 0.70887(17) 0.0208(5) Uani 1 2 d S . . C32 C 1.03341(18) 1.16858(16) 0.65657(13) 0.0304(4) Uani 1 1 d . . . H32 H 1.0411 1.1115 0.6889 0.037 Uiso 1 1 calc R . . C33 C 1.0092(2) 1.1686(2) 0.55829(15) 0.0460(7) Uani 1 1 d . . . H33 H 1.0017 1.1118 0.5253 0.055 Uiso 1 1 calc R . . C34 C 0.9960(3) 1.2500 0.5087(2) 0.0512(11) Uani 1 2 d S . . H34 H 0.9782 1.2500 0.4420 0.061 Uiso 1 2 calc SR . . B1 B 1.0570(3) 1.2500 0.82359(18) 0.0166(5) Uani 1 2 d S . . 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 0.01297(15) 0.01758(16) 0.01664(16) 0.000 0.00306(10) 0.000 O1 0.0430(8) 0.0333(8) 0.0208(7) 0.0027(6) 0.0073(5) 0.0218(6) N1 0.0435(11) 0.0815(17) 0.0238(9) -0.0223(10) 0.0168(8) -0.0440(11) N2 0.0163(9) 0.0156(9) 0.0197(9) 0.000 0.0053(7) 0.000 N3 0.0240(11) 0.0384(13) 0.0177(10) 0.000 0.0016(8) 0.000 N4 0.0138(9) 0.0253(11) 0.0197(10) 0.000 0.0026(7) 0.000 N5 0.0283(8) 0.0303(9) 0.0195(8) 0.0030(7) 0.0020(6) -0.0031(7) C1 0.024(2) 0.026(2) 0.032(2) -0.0093(16) -0.0035(15) 0.0109(16) C1A 0.026(2) 0.0230(18) 0.035(2) 0.0013(16) 0.0036(15) 0.0104(15) C2 0.023(2) 0.020(2) 0.0165(19) -0.0071(14) -0.0022(17) 0.006(2) C2A 0.019(2) 0.017(2) 0.0206(18) 0.0012(14) 0.0039(17) 0.002(2) C3 0.023(3) 0.018(2) 0.029(2) -0.0018(15) 0.0006(17) 0.003(2) C3A 0.022(3) 0.0139(19) 0.0267(19) 0.0035(14) 0.004(2) 0.000(2) C4 0.020(3) 0.020(2) 0.0185(18) -0.0004(15) 0.0002(18) -0.0019(18) C4A 0.017(2) 0.024(2) 0.0201(18) -0.0037(15) 0.0044(14) -0.0087(16) C5 0.036(2) 0.0207(19) 0.036(2) 0.0028(16) 0.0051(16) -0.0068(16) C5A 0.029(2) 0.0232(19) 0.039(2) -0.0013(16) 0.0072(16) -0.0117(15) C6 0.0184(15) 0.0220(18) 0.0311(19) 0.0005(16) 0.0070(13) -0.0046(13) C7 0.0131(13) 0.026(2) 0.0250(16) 0.0038(13) 0.0042(10) 0.0031(10) C8 0.0206(11) 0.0214(12) 0.0185(11) 0.000 0.0037(8) 0.000 C9 0.0254(13) 0.0472(18) 0.0204(13) 0.000 0.0080(9) 0.000 C10 0.0184(11) 0.0314(14) 0.0213(12) 0.000 0.0064(8) 0.000 C11 0.0358(10) 0.0230(9) 0.0205(8) 0.0020(7) 0.0035(7) -0.0055(7) C12 0.0283(8) 0.0303(9) 0.0195(8) 0.0030(7) 0.0020(6) -0.0031(7) O2 0.0263(15) 0.083(3) 0.0361(16) -0.0148(16) 0.0136(12) -0.0068(14) C40 0.035(2) 0.052(3) 0.037(2) -0.008(2) 0.0012(18) -0.009(2) C41 0.040(2) 0.119(5) 0.064(3) 0.000 -0.0011(19) 0.000 C19 0.0156(7) 0.0160(7) 0.0220(8) -0.0015(6) 0.0021(5) -0.0021(5) C20 0.0204(8) 0.0171(8) 0.0302(9) -0.0004(7) 0.0062(6) -0.0005(6) C21 0.0229(9) 0.0189(9) 0.0500(12) -0.0002(8) 0.0090(8) 0.0037(7) C22 0.0271(9) 0.0189(9) 0.0524(13) 0.0093(9) 0.0004(8) 0.0014(7) C23 0.0289(9) 0.0275(10) 0.0348(10) 0.0122(8) 0.0014(7) -0.0033(7) C24 0.0203(8) 0.0244(8) 0.0249(9) 0.0046(7) 0.0036(6) -0.0016(6) C25 0.0172(10) 0.0250(12) 0.0148(10) 0.000 0.0025(8) 0.000 C26 0.0209(8) 0.0308(10) 0.0212(8) 0.0036(7) 0.0021(6) -0.0042(7) C27 0.0211(9) 0.0534(14) 0.0234(9) 0.0089(9) 0.0034(7) -0.0113(8) C28 0.0158(12) 0.070(2) 0.0193(12) 0.000 0.0046(9) 0.000 C31 0.0133(10) 0.0302(13) 0.0194(11) 0.000 0.0043(8) 0.000 C32 0.0221(8) 0.0457(12) 0.0247(9) -0.0108(8) 0.0077(7) -0.0119(8) C33 0.0237(10) 0.091(2) 0.0243(10) -0.0244(12) 0.0078(7) -0.0202(11) C34 0.0162(12) 0.123(4) 0.0148(12) 0.000 0.0027(9) 0.000 B1 0.0147(11) 0.0174(12) 0.0182(12) 0.000 0.0042(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.8796(13) 4_575 ? Co1 O1 1.8796(13) . ? Co1 N1 1.8848(18) 4_575 ? Co1 N1 1.8848(18) . ? Co1 N2 1.936(2) . ? Co1 N4 1.926(2) . ? O1 C2 1.196(5) . ? O1 C2A 1.440(6) . ? N1 C4 1.560(6) . ? N1 C4A 1.103(5) . ? N1 C6 1.286(4) . ? N1 C7 1.700(4) 4_575 ? N2 C8 1.324(3) . ? N2 C10 1.385(3) . ? N3 H3 0.8800 . ? N3 C8 1.339(3) . ? N3 C9 1.375(4) . ? N4 C11 1.346(2) . ? N4 C11 1.346(2) 4_575 ? N5 N5 1.367(4) 4_575 ? N5 H5 0.8800 . ? N5 C11 1.352(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.513(6) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C1A C2A 1.498(6) . ? C2 C3 1.357(7) . ? C2A C3A 1.367(7) . ? C3 H3A 0.9500 . ? C3 C4 1.418(7) . ? C3A H3AA 0.9500 . ? C3A C4A 1.416(7) . ? C4 C5 1.517(6) . ? C4A C5A 1.520(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5A H5AA 0.9800 . ? C5A H5AB 0.9800 . ? C5A H5AC 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.522(6) . ? C7 N1 1.700(4) 4_575 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C9 C10 1.355(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? O2 H2 0.8400 . ? O2 C40 1.386(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 C41 1.319(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C19 C20 1.405(2) . ? C19 C24 1.405(2) . ? C19 B1 1.638(2) . ? C20 H20 0.9500 . ? C20 C21 1.392(3) . ? C21 H21 0.9500 . ? C21 C22 1.383(3) . ? C22 H22 0.9500 . ? C22 C23 1.387(3) . ? C23 H23 0.9500 . ? C23 C24 1.397(3) . ? C24 H24 0.9500 . ? C25 C26 1.400(2) 4_585 ? C25 C26 1.400(2) . ? C25 B1 1.646(3) . ? C26 H26 0.9500 . ? C26 C27 1.399(3) . ? C27 H27 0.9500 . ? C27 C28 1.381(3) . ? C28 C27 1.381(3) 4_585 ? C28 H28 0.9500 . ? C31 C32 1.399(2) . ? C31 C32 1.399(2) 4_585 ? C31 B1 1.637(3) . ? C32 H32 0.9500 . ? C32 C33 1.398(3) . ? C33 H33 0.9500 . ? C33 C34 1.379(3) . ? C34 C33 1.379(3) 4_585 ? C34 H34 0.9500 . ? B1 C19 1.638(2) 4_585 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 83.83(10) . 4_575 ? O1 Co1 N1 179.11(10) . 4_575 ? O1 Co1 N1 95.29(10) 4_575 4_575 ? O1 Co1 N1 95.29(10) . . ? O1 Co1 N1 179.11(10) 4_575 . ? O1 Co1 N2 89.01(6) . . ? O1 Co1 N2 89.01(6) 4_575 . ? O1 Co1 N4 89.94(6) 4_575 . ? O1 Co1 N4 89.94(6) . . ? N1 Co1 N1 85.59(17) . 4_575 ? N1 Co1 N2 91.13(7) 4_575 . ? N1 Co1 N2 91.13(7) . . ? N1 Co1 N4 89.91(7) 4_575 . ? N1 Co1 N4 89.91(7) . . ? N4 Co1 N2 178.59(8) . . ? C2 O1 Co1 136.9(3) . . ? C2 O1 C2A 24.3(2) . . ? C2A O1 Co1 112.6(2) . . ? C4 N1 Co1 114.9(3) . . ? C4 N1 C7 143.4(3) . 4_575 ? C4A N1 Co1 138.9(3) . . ? C4A N1 C4 24.1(2) . . ? C4A N1 C6 93.1(3) . . ? C4A N1 C7 119.3(3) . 4_575 ? C6 N1 Co1 127.5(3) . . ? C6 N1 C4 116.4(3) . . ? C6 N1 C7 31.8(2) . 4_575 ? C7 N1 Co1 101.12(17) 4_575 . ? C8 N2 Co1 124.30(17) . . ? C8 N2 C10 106.4(2) . . ? C10 N2 Co1 129.34(16) . . ? C8 N3 H3 126.0 . . ? C8 N3 C9 108.1(2) . . ? C9 N3 H3 126.0 . . ? C11 N4 Co1 126.75(11) . . ? C11 N4 Co1 126.75(11) 4_575 . ? C11 N4 C11 106.4(2) 4_575 . ? N5 N5 H5 126.5 4_575 . ? C11 N5 N5 106.94(11) . 4_575 ? C11 N5 H5 126.5 . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? O1 C2 C1 119.9(5) . . ? O1 C2 C3 119.6(4) . . ? C3 C2 C1 120.4(5) . . ? O1 C2A C1A 109.1(4) . . ? C3A C2A O1 129.9(4) . . ? C3A C2A C1A 120.9(5) . . ? C2 C3 H3A 117.1 . . ? C2 C3 C4 125.7(4) . . ? C4 C3 H3A 117.1 . . ? C2A C3A H3AA 117.2 . . ? C2A C3A C4A 125.5(4) . . ? C4A C3A H3AA 117.2 . . ? C3 C4 N1 125.8(4) . . ? C3 C4 C5 118.1(5) . . ? C5 C4 N1 116.0(5) . . ? N1 C4A C3A 115.2(4) . . ? N1 C4A C5A 126.9(5) . . ? C3A C4A C5A 118.0(4) . . ? C4A C5A H5AA 109.5 . . ? C4A C5A H5AB 109.5 . . ? C4A C5A H5AC 109.5 . . ? H5AA C5A H5AB 109.5 . . ? H5AA C5A H5AC 109.5 . . ? H5AB C5A H5AC 109.5 . . ? N1 C6 H6A 111.7 . . ? N1 C6 H6B 111.7 . . ? N1 C6 C7 100.5(3) . . ? H6A C6 H6B 109.4 . . ? C7 C6 H6A 111.7 . . ? C7 C6 H6B 111.7 . . ? N1 C7 H7A 109.3 4_575 . ? N1 C7 H7B 109.3 4_575 . ? C6 C7 N1 111.4(2) . 4_575 ? C6 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N2 C8 N3 110.5(2) . . ? N2 C8 H8 124.8 . . ? N3 C8 H8 124.8 . . ? N3 C9 H9 126.9 . . ? C10 C9 N3 106.2(2) . . ? C10 C9 H9 126.9 . . ? N2 C10 H10 125.5 . . ? C9 C10 N2 108.9(2) . . ? C9 C10 H10 125.5 . . ? N4 C11 N5 109.86(17) . . ? N4 C11 H11 125.1 . . ? N5 C11 H11 125.1 . . ? O2 C40 H40A 107.1 . . ? O2 C40 H40B 107.1 . . ? H40A C40 H40B 106.8 . . ? C41 C40 O2 120.8(5) . . ? C41 C40 H40A 107.1 . . ? C41 C40 H40B 107.1 . . ? C20 C19 C24 115.17(16) . . ? C20 C19 B1 121.72(17) . . ? C24 C19 B1 123.05(17) . . ? C19 C20 H20 118.6 . . ? C21 C20 C19 122.75(18) . . ? C21 C20 H20 118.6 . . ? C20 C21 H21 119.8 . . ? C22 C21 C20 120.36(18) . . ? C22 C21 H21 119.8 . . ? C21 C22 H22 120.5 . . ? C21 C22 C23 118.92(18) . . ? C23 C22 H22 120.5 . . ? C22 C23 H23 119.9 . . ? C22 C23 C24 120.19(19) . . ? C24 C23 H23 119.9 . . ? C19 C24 H24 118.7 . . ? C23 C24 C19 122.57(18) . . ? C23 C24 H24 118.7 . . ? C26 C25 C26 115.8(2) 4_585 . ? C26 C25 B1 121.96(11) . . ? C26 C25 B1 121.96(12) 4_585 . ? C25 C26 H26 118.9 . . ? C27 C26 C25 122.2(2) . . ? C27 C26 H26 118.9 . . ? C26 C27 H27 119.8 . . ? C28 C27 C26 120.5(2) . . ? C28 C27 H27 119.8 . . ? C27 C28 C27 118.8(3) . 4_585 ? C27 C28 H28 120.6 4_585 . ? C27 C28 H28 120.6 . . ? C32 C31 C32 115.8(2) 4_585 . ? C32 C31 B1 121.90(12) . . ? C32 C31 B1 121.90(12) 4_585 . ? C31 C32 H32 118.9 . . ? C33 C32 C31 122.1(2) . . ? C33 C32 H32 118.9 . . ? C32 C33 H33 119.6 . . ? C34 C33 C32 120.7(2) . . ? C34 C33 H33 119.6 . . ? C33 C34 C33 118.5(3) . 4_585 ? C33 C34 H34 120.7 4_585 . ? C33 C34 H34 120.7 . . ? C19 B1 C19 105.84(18) 4_585 . ? C19 B1 C25 112.10(13) 4_585 . ? C19 B1 C25 112.10(13) . . ? C31 B1 C19 112.28(13) . 4_585 ? C31 B1 C19 112.28(13) . . ? C31 B1 C25 102.42(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co1 O1 C2 C1 176.3(2) . . . . ? Co1 O1 C2 C3 -6.2(6) . . . . ? Co1 O1 C2A C1A 168.5(2) . . . . ? Co1 O1 C2A C3A -10.6(5) . . . . ? Co1 N1 C4 C3 12.0(4) . . . . ? Co1 N1 C4 C5 -170.9(2) . . . . ? Co1 N1 C4A C3A -2.4(6) . . . . ? Co1 N1 C4A C5A 176.9(3) . . . . ? Co1 N1 C6 C7 -22.3(4) . . . . ? Co1 N2 C8 N3 180.0 . . . . ? Co1 N2 C10 C9 180.0 . . . . ? Co1 N4 C11 N5 176.12(14) . . . . ? O1 Co1 O1 C2 -166.9(3) 4_575 . . . ? O1 Co1 O1 C2A -166.3(2) 4_575 . . . ? O1 Co1 N1 C4 -13.05(19) . . . . ? O1 Co1 N1 C4 -23(5) 4_575 . . . ? O1 Co1 N1 C4A -20(5) 4_575 . . . ? O1 Co1 N1 C4A -10.2(4) . . . . ? O1 Co1 N1 C6 -180.0(3) . . . . ? O1 Co1 N1 C6 170(32) 4_575 . . . ? O1 Co1 N1 C7 150(5) 4_575 . . 4_575 ? O1 Co1 N1 C7 160.22(15) . . . 4_575 ? O1 Co1 N2 C8 -41.92(5) . . . . ? O1 Co1 N2 C8 41.92(5) 4_575 . . . ? O1 Co1 N2 C10 -138.08(5) 4_575 . . . ? O1 Co1 N2 C10 138.08(5) . . . . ? O1 Co1 N4 C11 50.26(19) 4_575 . . . ? O1 Co1 N4 C11 134.09(19) . . . . ? O1 Co1 N4 C11 -134.09(19) 4_575 . . 4_575 ? O1 Co1 N4 C11 -50.26(19) . . . 4_575 ? O1 C2 C3 C4 -1.5(7) . . . . ? O1 C2A C3A C4A -4.8(7) . . . . ? N1 Co1 O1 C2 13.2(3) . . . . ? N1 Co1 O1 C2 -177(100) 4_575 . . . ? N1 Co1 O1 C2A -176(100) 4_575 . . . ? N1 Co1 O1 C2A 13.9(2) . . . . ? N1 Co1 N1 C4 167.11(16) 4_575 . . . ? N1 Co1 N1 C4A 170.0(3) 4_575 . . . ? N1 Co1 N1 C6 0.2(3) 4_575 . . . ? N1 Co1 N1 C7 -19.63(18) 4_575 . . 4_575 ? N1 Co1 N2 C8 -137.20(8) . . . . ? N1 Co1 N2 C8 137.20(8) 4_575 . . . ? N1 Co1 N2 C10 42.80(8) . . . . ? N1 Co1 N2 C10 -42.80(8) 4_575 . . . ? N1 Co1 N4 C11 -130.6(2) . . . . ? N1 Co1 N4 C11 -45.0(2) 4_575 . . . ? N1 Co1 N4 C11 45.0(2) . . . 4_575 ? N1 Co1 N4 C11 130.6(2) 4_575 . . 4_575 ? N1 C6 C7 N1 36.9(3) . . . 4_575 ? N2 Co1 O1 C2 -77.8(3) . . . . ? N2 Co1 O1 C2A -77.1(2) . . . . ? N2 Co1 N1 C4 76.06(19) . . . . ? N2 Co1 N1 C4A 78.9(4) . . . . ? N2 Co1 N1 C6 -90.8(3) . . . . ? N2 Co1 N1 C7 -110.67(15) . . . 4_575 ? N2 Co1 N4 C11 -92.18(19) . . . 4_575 ? N2 Co1 N4 C11 92.18(19) . . . . ? N3 C9 C10 N2 0.0 . . . . ? N4 Co1 O1 C2 103.1(3) . . . . ? N4 Co1 O1 C2A 103.8(2) . . . . ? N4 Co1 N1 C4 -102.98(18) . . . . ? N4 Co1 N1 C4A -100.1(4) . . . . ? N4 Co1 N1 C6 90.1(3) . . . . ? N4 Co1 N1 C7 70.29(15) . . . 4_575 ? N4 Co1 N2 C8 0.000(8) . . . . ? N4 Co1 N2 C10 180.000(8) . . . . ? N5 N5 C11 N4 0.15(18) 4_575 . . . ? C1 C2 C3 C4 176.0(4) . . . . ? C1A C2A C3A C4A 176.1(4) . . . . ? C2 O1 C2A C1A -12.6(6) . . . . ? C2 O1 C2A C3A 168.3(11) . . . . ? C2 C3 C4 N1 -2.8(6) . . . . ? C2 C3 C4 C5 -179.9(4) . . . . ? C2A O1 C2 C1 174.8(10) . . . . ? C2A O1 C2 C3 -7.7(5) . . . . ? C2A C3A C4A N1 12.3(6) . . . . ? C2A C3A C4A C5A -167.0(4) . . . . ? C4 N1 C4A C3A 4.0(4) . . . . ? C4 N1 C4A C5A -176.7(9) . . . . ? C4 N1 C6 C7 171.0(2) . . . . ? C4A N1 C4 C3 -163.4(8) . . . . ? C4A N1 C4 C5 13.7(6) . . . . ? C4A N1 C6 C7 164.4(3) . . . . ? C6 N1 C4 C3 -179.6(4) . . . . ? C6 N1 C4 C5 -2.5(4) . . . . ? C6 N1 C4A C3A 169.5(4) . . . . ? C6 N1 C4A C5A -11.2(5) . . . . ? C7 N1 C4 C3 -156.9(4) 4_575 . . . ? C7 N1 C4 C5 20.2(5) 4_575 . . . ? C7 N1 C4A C3A -171.6(3) 4_575 . . . ? C7 N1 C4A C5A 7.7(5) 4_575 . . . ? C7 N1 C6 C7 16.9(2) 4_575 . . . ? C8 N2 C10 C9 0.0 . . . . ? C8 N3 C9 C10 0.0 . . . . ? C9 N3 C8 N2 0.0 . . . . ? C10 N2 C8 N3 0.0 . . . . ? C11 N4 C11 N5 -0.2(3) 4_575 . . . ? C19 C20 C21 C22 -0.1(3) . . . . ? C20 C19 C24 C23 -2.3(3) . . . . ? C20 C19 B1 C19 -87.1(2) . . . 4_585 ? C20 C19 B1 C25 150.37(17) . . . . ? C20 C19 B1 C31 35.7(2) . . . . ? C20 C21 C22 C23 -1.3(3) . . . . ? C21 C22 C23 C24 0.8(3) . . . . ? C22 C23 C24 C19 1.1(3) . . . . ? C24 C19 C20 C21 1.8(3) . . . . ? C24 C19 B1 C19 89.7(2) . . . 4_585 ? C24 C19 B1 C25 -32.8(2) . . . . ? C24 C19 B1 C31 -147.48(17) . . . . ? C25 C26 C27 C28 0.7(3) . . . . ? C26 C25 C26 C27 -2.9(3) 4_585 . . . ? C26 C25 B1 C19 33.9(3) 4_585 . . 4_585 ? C26 C25 B1 C19 -152.78(18) . . . 4_585 ? C26 C25 B1 C19 -33.9(3) . . . . ? C26 C25 B1 C19 152.78(18) 4_585 . . . ? C26 C25 B1 C31 -86.66(19) 4_585 . . . ? C26 C25 B1 C31 86.66(19) . . . . ? C26 C27 C28 C27 1.8(4) . . . 4_585 ? C31 C32 C33 C34 -0.6(3) . . . . ? C32 C31 C32 C33 0.3(3) 4_585 . . . ? C32 C31 B1 C19 153.55(18) . . . 4_585 ? C32 C31 B1 C19 -34.4(3) 4_585 . . 4_585 ? C32 C31 B1 C19 -153.55(18) 4_585 . . . ? C32 C31 B1 C19 34.4(3) . . . . ? C32 C31 B1 C25 -86.02(19) . . . . ? C32 C31 B1 C25 86.02(19) 4_585 . . . ? C32 C33 C34 C33 0.9(4) . . . 4_585 ? B1 C19 C20 C21 178.87(17) . . . . ? B1 C19 C24 C23 -179.31(17) . . . . ? B1 C25 C26 C27 -176.64(19) . . . . ? B1 C31 C32 C33 172.81(19) . . . . ? data_Co(acacen)(NH3)2 _audit_creation_date 2012-06-05 _audit_creation_method ; Olex2 1.2 (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _publ_contact_author_address ? _publ_contact_author_email tmeade@northwestern.edu _publ_contact_author_name 'Thomas J. Meade' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; trans-bis(ammine)-(N,N'-ethylene-bis(acetylacetoniminato)) -cobalt(iii) tetraphenylborate ; _chemical_formula_moiety 'C12 H24 Co N4 O2, C24 H20 B' _chemical_formula_sum 'C36 H44 B Co N4 O2' _chemical_formula_weight 634.49 _chemical_absolute_configuration ad _chemical_melting_point ? 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' 'B' 'B' 0.0013 0.0007 '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' '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' _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_H-M_alt 'C 1 c 1' _space_group_name_Hall 'C -2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 'x, -y, z+1/2' 3 'x+1/2, y+1/2, z' 4 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.4323(5) _cell_length_b 17.3432(7) _cell_length_c 15.4529(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.308(2) _cell_angle_gamma 90.00 _cell_volume 3326.3(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9718 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.10 _cell_measurement_theta_min 2.35 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.6677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0627 before and 0.0541 after correction. The Ratio of minimum to maximum transmission is 0.8950. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'plate' _exptl_crystal_F_000 1344 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.211 _exptl_crystal_size_min 0.054 _exptl_special_details ? _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_unetI/netI 0.0584 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 27717 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.02 _diffrn_ambient_temperature 99.97 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 4713 _reflns_number_total 6248 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.279 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.056 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(15) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 403 _refine_ls_number_reflns 6248 _refine_ls_number_restraints 128 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0426 _refine_ls_restrained_S_all 0.801 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1107 _refine_ls_wR_factor_ref 0.1250 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.49368(4) 0.75173(2) -0.00020(4) 0.01612(12) Uani 1 1 d U . . O1 O 0.4937(2) 0.67619(17) 0.08776(16) 0.0209(6) Uani 1 1 d U . . O2 O 0.4918(2) 0.82223(16) 0.09284(16) 0.0194(6) Uani 1 1 d U . . N1 N 0.4996(2) 0.6799(2) -0.0925(2) 0.0205(8) Uani 1 1 d U . . N2 N 0.4938(2) 0.8287(2) -0.0872(2) 0.0205(8) Uani 1 1 d U . . N3 N 0.3372(3) 0.75008(16) -0.0080(3) 0.0241(8) Uani 1 1 d U . . H3A H 0.3131 0.7456 -0.0645 0.029 Uiso 1 1 calc R . . H3B H 0.3118 0.7946 0.0144 0.029 Uiso 1 1 calc R . . H3C H 0.3135 0.7092 0.0226 0.029 Uiso 1 1 calc R . . N4 N 0.6494(3) 0.75280(15) 0.0172(2) 0.0202(8) Uani 1 1 d U . . H4A H 0.6794 0.7545 -0.0351 0.024 Uiso 1 1 calc R . . H4B H 0.6717 0.7094 0.0461 0.024 Uiso 1 1 calc R . . H4C H 0.6703 0.7950 0.0489 0.024 Uiso 1 1 calc R . . C1 C 0.4755(3) 0.5567(2) 0.1548(2) 0.0324(10) Uani 1 1 d U . . H1A H 0.5468 0.5573 0.1854 0.049 Uiso 1 1 calc R . . H1B H 0.4559 0.5035 0.1395 0.049 Uiso 1 1 calc R . . H1C H 0.4222 0.5782 0.1924 0.049 Uiso 1 1 calc R . . C2 C 0.4782(3) 0.6045(2) 0.0732(2) 0.0208(8) Uani 1 1 d U . . C3 C 0.4665(3) 0.5694(2) -0.0062(2) 0.0240(8) Uani 1 1 d U . . H3 H 0.4456 0.5167 -0.0077 0.029 Uiso 1 1 calc R . . C4 C 0.4833(3) 0.6060(3) -0.0860(2) 0.0204(9) Uani 1 1 d U . . C5 C 0.4845(3) 0.5556(2) -0.1650(3) 0.0306(10) Uani 1 1 d U . . H5A H 0.4315 0.5746 -0.2093 0.046 Uiso 1 1 calc R . . H5B H 0.4664 0.5026 -0.1494 0.046 Uiso 1 1 calc R . . H5C H 0.5564 0.5566 -0.1878 0.046 Uiso 1 1 calc R . . C6 C 0.5315(4) 0.7167(2) -0.1711(3) 0.0375(10) Uani 1 1 d U . . H6A H 0.5013 0.6879 -0.2222 0.045 Uiso 1 1 calc R . . H6B H 0.6110 0.7163 -0.1725 0.045 Uiso 1 1 calc R . . C7 C 0.4924(4) 0.7960(2) -0.1744(2) 0.0382(10) Uani 1 1 d U . . H7A H 0.4180 0.7971 -0.2010 0.046 Uiso 1 1 calc R . . H7B H 0.5385 0.8273 -0.2109 0.046 Uiso 1 1 calc R . . C8 C 0.4786(3) 0.9020(2) -0.0753(2) 0.0210(8) Uani 1 1 d U . . C9 C 0.4701(3) 0.9557(2) -0.1515(2) 0.0320(10) Uani 1 1 d U . . H9A H 0.5393 0.9575 -0.1787 0.048 Uiso 1 1 calc R . . H9B H 0.4512 1.0074 -0.1319 0.048 Uiso 1 1 calc R . . H9C H 0.4141 0.9371 -0.1936 0.048 Uiso 1 1 calc R . . C10 C 0.4725(3) 0.9351(2) 0.0084(2) 0.0242(8) Uani 1 1 d U . . H10 H 0.4600 0.9890 0.0116 0.029 Uiso 1 1 calc R . . C11 C 0.4832(3) 0.8956(2) 0.0844(2) 0.0192(8) Uani 1 1 d U . . C12 C 0.4878(3) 0.9389(2) 0.1691(2) 0.0263(9) Uani 1 1 d U . . H12A H 0.4363 0.9162 0.2075 0.039 Uiso 1 1 calc R . . H12B H 0.4694 0.9931 0.1582 0.039 Uiso 1 1 calc R . . H12C H 0.5607 0.9354 0.1965 0.039 Uiso 1 1 calc R . . B1 B 0.9913(5) 0.7498(2) -0.0030(4) 0.0191(6) Uani 1 1 d U . . C13 C 0.9091(3) 0.67751(19) 0.0122(2) 0.0204(7) Uani 1 1 d U . . C14 C 0.8786(3) 0.6546(2) 0.0941(3) 0.0236(8) Uani 1 1 d U . . H14 H 0.9120 0.6784 0.1440 0.028 Uiso 1 1 calc R . . C15 C 0.8006(3) 0.5979(2) 0.1048(3) 0.0278(8) Uani 1 1 d U . . H15 H 0.7831 0.5832 0.1615 0.033 Uiso 1 1 calc R . . C16 C 0.7489(3) 0.5632(2) 0.0339(3) 0.0294(9) Uani 1 1 d U . . H16 H 0.6952 0.5251 0.0412 0.035 Uiso 1 1 calc R . . C17 C 0.7765(3) 0.5846(2) -0.0476(3) 0.0297(8) Uani 1 1 d U . . H17 H 0.7414 0.5613 -0.0972 0.036 Uiso 1 1 calc R . . C18 C 0.8552(3) 0.6399(2) -0.0578(2) 0.0233(8) Uani 1 1 d U . . H18 H 0.8735 0.6529 -0.1149 0.028 Uiso 1 1 calc R . . C19 C 0.9074(3) 0.8231(2) -0.0144(2) 0.0206(7) Uani 1 1 d U . . C20 C 0.8598(3) 0.8456(2) -0.0948(3) 0.0252(8) Uani 1 1 d U . . H20 H 0.8821 0.8213 -0.1459 0.030 Uiso 1 1 calc R . . C21 C 0.7805(3) 0.9029(2) -0.1023(3) 0.0303(9) Uani 1 1 d U . . H21 H 0.7501 0.9169 -0.1579 0.036 Uiso 1 1 calc R . . C22 C 0.7461(3) 0.9390(2) -0.0295(3) 0.0326(9) Uani 1 1 d U . . H22 H 0.6929 0.9784 -0.0343 0.039 Uiso 1 1 calc R . . C23 C 0.7903(3) 0.9171(2) 0.0505(3) 0.0308(9) Uani 1 1 d U . . H23 H 0.7661 0.9405 0.1015 0.037 Uiso 1 1 calc R . . C24 C 0.8694(3) 0.8614(2) 0.0571(3) 0.0257(8) Uani 1 1 d U . . H24 H 0.8995 0.8484 0.1131 0.031 Uiso 1 1 calc R . . C25 C 1.0635(3) 0.7333(2) -0.0860(2) 0.0234(8) Uani 1 1 d U . . C26 C 1.1076(3) 0.6602(2) -0.0995(3) 0.0254(9) Uani 1 1 d U . . H26 H 1.0877 0.6189 -0.0632 0.030 Uiso 1 1 calc R . . C27 C 1.1785(3) 0.6452(2) -0.1630(2) 0.0326(9) Uani 1 1 d U . . H27 H 1.2072 0.5948 -0.1690 0.039 Uiso 1 1 calc R . . C28 C 1.2075(3) 0.7033(3) -0.2178(2) 0.0380(10) Uani 1 1 d U . . H28 H 1.2545 0.6929 -0.2627 0.046 Uiso 1 1 calc R . . C29 C 1.1678(3) 0.7765(3) -0.2068(3) 0.0388(10) Uani 1 1 d U . . H29 H 1.1882 0.8168 -0.2441 0.047 Uiso 1 1 calc R . . C30 C 1.0983(3) 0.7920(2) -0.1417(2) 0.0279(8) Uani 1 1 d U . . H30 H 1.0735 0.8432 -0.1343 0.034 Uiso 1 1 calc R . . C31 C 1.0806(3) 0.7630(2) 0.0775(2) 0.0228(8) Uani 1 1 d U . . C32 C 1.1321(3) 0.7016(2) 0.1218(2) 0.0247(8) Uani 1 1 d U . . H32 H 1.1059 0.6508 0.1115 0.030 Uiso 1 1 calc R . . C33 C 1.2191(3) 0.7121(3) 0.1794(2) 0.0310(9) Uani 1 1 d U . . H33 H 1.2516 0.6685 0.2076 0.037 Uiso 1 1 calc R . . C34 C 1.2603(3) 0.7847(3) 0.1972(2) 0.0317(9) Uani 1 1 d U . . H34 H 1.3209 0.7916 0.2367 0.038 Uiso 1 1 calc R . . C35 C 1.2104(3) 0.8472(2) 0.1554(2) 0.0308(9) Uani 1 1 d U . . H35 H 1.2361 0.8979 0.1671 0.037 Uiso 1 1 calc R . . C36 C 1.1232(3) 0.8359(2) 0.0969(2) 0.0270(9) Uani 1 1 d U . . H36 H 1.0910 0.8796 0.0688 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0161(2) 0.0198(2) 0.01274(19) -0.0007(2) 0.00265(14) -0.00069(19) O1 0.0269(16) 0.0198(15) 0.0162(14) -0.0008(11) 0.0031(11) -0.0049(11) O2 0.0237(15) 0.0191(14) 0.0149(14) 0.0016(11) -0.0032(11) 0.0043(11) N1 0.0180(17) 0.028(2) 0.0159(17) -0.0031(14) 0.0078(13) -0.0054(13) N2 0.0204(18) 0.027(2) 0.0142(16) 0.0005(13) 0.0033(13) 0.0028(13) N3 0.0179(17) 0.041(2) 0.0143(18) -0.0015(12) 0.0049(14) -0.0024(12) N4 0.0176(17) 0.0190(19) 0.023(2) 0.0010(11) -0.0019(15) 0.0003(10) C1 0.046(3) 0.028(2) 0.023(2) 0.0037(17) 0.0025(18) -0.0093(18) C2 0.0171(18) 0.022(2) 0.0231(19) 0.0009(15) 0.0014(14) -0.0052(15) C3 0.025(2) 0.0219(19) 0.0260(18) -0.0017(15) 0.0049(17) -0.0083(14) C4 0.0164(18) 0.026(2) 0.0189(18) -0.0047(15) 0.0012(14) -0.0033(15) C5 0.042(2) 0.025(2) 0.025(2) -0.0107(17) 0.0051(18) -0.0016(18) C6 0.058(3) 0.031(2) 0.025(2) -0.0025(18) 0.0190(19) -0.005(2) C7 0.064(3) 0.033(2) 0.0184(19) 0.0005(17) 0.0087(18) -0.004(2) C8 0.0183(18) 0.025(2) 0.0200(18) 0.0053(15) 0.0016(14) 0.0004(15) C9 0.040(2) 0.031(2) 0.025(2) 0.0059(17) 0.0021(18) 0.0033(18) C10 0.029(2) 0.0213(18) 0.0228(18) 0.0009(15) 0.0040(16) 0.0043(14) C11 0.0132(17) 0.020(2) 0.0245(19) -0.0038(15) 0.0008(14) 0.0042(14) C12 0.031(2) 0.027(2) 0.0203(19) -0.0040(16) -0.0016(16) 0.0047(16) B1 0.0167(15) 0.0234(16) 0.0176(16) -0.0001(16) 0.0044(12) -0.0033(15) C13 0.0166(17) 0.0204(19) 0.0248(18) 0.0005(14) 0.0052(14) 0.0051(13) C14 0.0229(19) 0.025(2) 0.0227(19) 0.0044(16) 0.0012(15) 0.0010(15) C15 0.0191(18) 0.035(2) 0.030(2) 0.0096(17) 0.0077(15) 0.0043(14) C16 0.0232(19) 0.0175(19) 0.048(2) 0.0061(17) 0.0086(16) 0.0006(15) C17 0.0216(18) 0.031(2) 0.036(2) -0.0060(17) -0.0008(15) -0.0001(15) C18 0.0215(18) 0.025(2) 0.0239(19) -0.0032(15) 0.0011(15) 0.0017(14) C19 0.0124(17) 0.0237(19) 0.0262(19) -0.0004(14) 0.0050(13) -0.0048(13) C20 0.0203(19) 0.025(2) 0.031(2) 0.0029(16) 0.0023(16) -0.0035(14) C21 0.026(2) 0.030(2) 0.034(2) 0.0068(17) -0.0048(16) -0.0016(15) C22 0.0205(19) 0.024(2) 0.053(2) 0.0019(18) -0.0021(17) -0.0030(15) C23 0.0225(19) 0.026(2) 0.044(2) -0.0079(17) 0.0084(17) -0.0020(15) C24 0.0162(17) 0.029(2) 0.032(2) -0.0018(16) 0.0016(15) -0.0062(14) C25 0.0148(17) 0.039(2) 0.0161(17) -0.0011(15) -0.0019(13) -0.0027(14) C26 0.019(2) 0.031(2) 0.027(2) -0.0030(17) 0.0026(15) -0.0023(15) C27 0.0207(18) 0.047(3) 0.030(2) -0.0138(18) 0.0045(15) 0.0004(17) C28 0.030(2) 0.063(3) 0.021(2) -0.0117(19) 0.0039(16) -0.005(2) C29 0.036(2) 0.055(3) 0.026(2) 0.014(2) 0.0043(18) -0.002(2) C30 0.027(2) 0.035(2) 0.0221(19) 0.0094(16) 0.0048(15) 0.0012(17) C31 0.0166(18) 0.036(2) 0.0165(17) -0.0021(14) 0.0057(13) -0.0031(14) C32 0.0177(17) 0.041(2) 0.0154(17) 0.0028(16) 0.0036(13) -0.0016(15) C33 0.0234(19) 0.050(3) 0.0203(19) 0.0057(18) 0.0059(14) 0.0010(18) C34 0.0224(19) 0.060(3) 0.0135(17) -0.0031(18) 0.0044(14) -0.0085(18) C35 0.029(2) 0.042(2) 0.0229(19) -0.0109(17) 0.0079(15) -0.0059(17) C36 0.023(2) 0.038(2) 0.021(2) -0.0034(17) 0.0081(16) -0.0004(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.888(3) . ? Co1 O2 1.888(3) . ? Co1 N1 1.898(4) . ? Co1 N2 1.894(4) . ? Co1 N3 1.942(4) . ? Co1 N4 1.940(3) . ? O1 C2 1.276(5) . ? O2 C11 1.282(4) . ? N1 C4 1.303(5) . ? N1 C6 1.448(5) . ? N2 C7 1.462(5) . ? N2 C8 1.301(5) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.512(5) . ? C2 C3 1.369(5) . ? C3 H3 0.9500 . ? C3 C4 1.413(5) . ? C4 C5 1.502(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.458(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.499(5) . ? C8 C10 1.422(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10 0.9500 . ? C10 C11 1.359(5) . ? C11 C12 1.507(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? B1 C13 1.643(6) . ? B1 C19 1.648(6) . ? B1 C25 1.634(7) . ? B1 C31 1.636(7) . ? C13 C14 1.398(5) . ? C13 C18 1.400(5) . ? C14 H14 0.9500 . ? C14 C15 1.397(5) . ? C15 H15 0.9500 . ? C15 C16 1.375(5) . ? C16 H16 0.9500 . ? C16 C17 1.376(5) . ? C17 H17 0.9500 . ? C17 C18 1.386(5) . ? C18 H18 0.9500 . ? C19 C20 1.400(5) . ? C19 C24 1.395(5) . ? C20 H20 0.9500 . ? C20 C21 1.400(5) . ? C21 H21 0.9500 . ? C21 C22 1.378(5) . ? C22 H22 0.9500 . ? C22 C23 1.377(5) . ? C23 H23 0.9500 . ? C23 C24 1.377(5) . ? C24 H24 0.9500 . ? C25 C26 1.402(5) . ? C25 C30 1.416(5) . ? C26 H26 0.9500 . ? C26 C27 1.381(5) . ? C27 H27 0.9500 . ? C27 C28 1.377(5) . ? C28 H28 0.9500 . ? C28 C29 1.376(6) . ? C29 H29 0.9500 . ? C29 C30 1.390(5) . ? C30 H30 0.9500 . ? C31 C32 1.400(5) . ? C31 C36 1.397(5) . ? C32 H32 0.9500 . ? C32 C33 1.373(5) . ? C33 H33 0.9500 . ? C33 C34 1.381(6) . ? C34 H34 0.9500 . ? C34 C35 1.390(6) . ? C35 H35 0.9500 . ? C35 C36 1.384(5) . ? C36 H36 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 84.30(14) . . ? O1 Co1 N1 95.00(10) . . ? O1 Co1 N2 179.16(16) . . ? O1 Co1 N3 89.60(13) . . ? O1 Co1 N4 87.01(12) . . ? O2 Co1 N1 178.34(15) . . ? O2 Co1 N2 94.86(10) . . ? O2 Co1 N3 90.01(13) . . ? O2 Co1 N4 86.80(12) . . ? N1 Co1 N3 91.50(14) . . ? N1 Co1 N4 91.66(14) . . ? N2 Co1 N1 85.83(18) . . ? N2 Co1 N3 90.47(13) . . ? N2 Co1 N4 92.88(14) . . ? N4 Co1 N3 175.56(19) . . ? C2 O1 Co1 123.7(2) . . ? C11 O2 Co1 124.7(2) . . ? C4 N1 Co1 125.1(3) . . ? C4 N1 C6 123.3(4) . . ? C6 N1 Co1 111.5(3) . . ? C7 N2 Co1 112.4(3) . . ? C8 N2 Co1 125.7(3) . . ? C8 N2 C7 121.0(3) . . ? Co1 N3 H3A 109.5 . . ? Co1 N3 H3B 109.5 . . ? Co1 N3 H3C 109.5 . . ? H3A N3 H3B 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Co1 N4 H4A 109.5 . . ? Co1 N4 H4B 109.5 . . ? Co1 N4 H4C 109.5 . . ? H4A N4 H4B 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? O1 C2 C1 113.4(3) . . ? O1 C2 C3 126.8(4) . . ? C3 C2 C1 119.8(3) . . ? C2 C3 H3 117.7 . . ? C2 C3 C4 124.7(3) . . ? C4 C3 H3 117.7 . . ? N1 C4 C3 122.7(4) . . ? N1 C4 C5 120.1(3) . . ? C3 C4 C5 117.2(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 H6A 109.7 . . ? N1 C6 H6B 109.7 . . ? N1 C6 C7 109.8(3) . . ? H6A C6 H6B 108.2 . . ? C7 C6 H6A 109.7 . . ? C7 C6 H6B 109.7 . . ? N2 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C6 C7 N2 110.3(3) . . ? C6 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N2 C8 C9 120.1(3) . . ? N2 C8 C10 122.6(3) . . ? C10 C8 C9 117.4(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10 117.4 . . ? C11 C10 C8 125.1(3) . . ? C11 C10 H10 117.4 . . ? O2 C11 C10 126.3(3) . . ? O2 C11 C12 114.0(3) . . ? C10 C11 C12 119.7(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C13 B1 C19 102.1(4) . . ? C25 B1 C13 110.7(3) . . ? C25 B1 C19 115.1(4) . . ? C25 B1 C31 104.0(4) . . ? C31 B1 C13 113.5(4) . . ? C31 B1 C19 111.8(3) . . ? C14 C13 B1 123.3(4) . . ? C14 C13 C18 115.1(3) . . ? C18 C13 B1 121.2(4) . . ? C13 C14 H14 118.9 . . ? C15 C14 C13 122.2(4) . . ? C15 C14 H14 118.9 . . ? C14 C15 H15 119.7 . . ? C16 C15 C14 120.6(3) . . ? C16 C15 H15 119.7 . . ? C15 C16 H16 120.6 . . ? C15 C16 C17 118.7(3) . . ? C17 C16 H16 120.6 . . ? C16 C17 H17 119.8 . . ? C16 C17 C18 120.4(3) . . ? C18 C17 H17 119.8 . . ? C13 C18 H18 118.6 . . ? C17 C18 C13 122.9(3) . . ? C17 C18 H18 118.6 . . ? C20 C19 B1 122.9(4) . . ? C24 C19 B1 121.6(4) . . ? C24 C19 C20 115.2(3) . . ? C19 C20 H20 119.0 . . ? C19 C20 C21 122.0(4) . . ? C21 C20 H20 119.0 . . ? C20 C21 H21 119.8 . . ? C22 C21 C20 120.4(3) . . ? C22 C21 H21 119.8 . . ? C21 C22 H22 120.6 . . ? C23 C22 C21 118.7(3) . . ? C23 C22 H22 120.6 . . ? C22 C23 H23 119.8 . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H23 119.8 . . ? C19 C24 H24 118.4 . . ? C23 C24 C19 123.2(4) . . ? C23 C24 H24 118.4 . . ? C26 C25 B1 120.8(3) . . ? C26 C25 C30 115.1(3) . . ? C30 C25 B1 123.5(3) . . ? C25 C26 H26 118.4 . . ? C27 C26 C25 123.1(4) . . ? C27 C26 H26 118.4 . . ? C26 C27 H27 120.0 . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H27 120.0 . . ? C27 C28 H28 120.3 . . ? C29 C28 C27 119.4(4) . . ? C29 C28 H28 120.3 . . ? C28 C29 H29 119.7 . . ? C28 C29 C30 120.7(4) . . ? C30 C29 H29 119.7 . . ? C25 C30 H30 119.2 . . ? C29 C30 C25 121.7(4) . . ? C29 C30 H30 119.2 . . ? C32 C31 B1 122.4(3) . . ? C36 C31 B1 121.5(3) . . ? C36 C31 C32 115.3(3) . . ? C31 C32 H32 118.8 . . ? C33 C32 C31 122.5(4) . . ? C33 C32 H32 118.8 . . ? C32 C33 H33 119.4 . . ? C32 C33 C34 121.3(4) . . ? C34 C33 H33 119.4 . . ? C33 C34 H34 121.0 . . ? C33 C34 C35 117.9(4) . . ? C35 C34 H34 121.0 . . ? C34 C35 H35 119.8 . . ? C36 C35 C34 120.3(4) . . ? C36 C35 H35 119.8 . . ? C31 C36 H36 118.7 . . ? C35 C36 C31 122.7(4) . . ? C35 C36 H36 118.7 . . ? data_Co(acacen)(Py)2 _audit_creation_date 2012-06-05 _audit_creation_method ; Olex2 1.2 (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _publ_contact_author_address ? _publ_contact_author_email tmeade@northwestern.edu _publ_contact_author_name 'Thomas J. Meade' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; trans-bis(pyridine)-(N,N'-ethylene-bis(acetylacetoniminato)) -cobalt(iii) bromide ethanol solvate ; _chemical_formula_moiety 'Br, C22 H28 Co N4 O2, 2(C H4 O)' _chemical_formula_sum 'C24 H36 Br Co N4 O4' _chemical_formula_weight 583.41 _chemical_absolute_configuration ad _chemical_melting_point ? 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' 'Br' 'Br' -0.2901 2.4595 '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' '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' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, z+1/2' 3 'x+1/2, -y+1/2, z' 4 '-x+1/2, y+1/2, z+1/2' _cell_length_a 23.538(5) _cell_length_b 14.372(3) _cell_length_c 15.616(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5282.6(18) _cell_formula_units_Z 8 _cell_measurement_reflns_used ? _cell_measurement_temperature 100(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _exptl_absorpt_coefficient_mu 2.198 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.597253 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; TWINABS-2008/4 (Bruker,2010) was used for absorption correction. For component 1: wR2(int) was 0.0692 before and 0.0471 after correction. The Ratio of minimum to maximum transmission not present. The \l/2 correction factor is Not present For component 2: wR2(int) was 0.1002 before and 0.0519 after correction. The Ratio of minimum to maximum transmission is 0.80. The \l/2 correction factor is Not present ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block' _exptl_crystal_F_000 2416 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.245 _exptl_crystal_size_min 0.188 _exptl_special_details ? _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_unetI/netI 0.0124 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6300 _diffrn_reflns_theta_full 27.56 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_theta_min 1.66 _diffrn_ambient_temperature 100.14 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker Kappa APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 6153 _reflns_number_total 6300 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_collection 'APEX2 V2.1-4 (Bruker, 2007)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.265 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.086 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.109(11) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 629 _refine_ls_number_reflns 6300 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0362 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+15.7602P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.0871 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Br01 Br 0.73095(3) 0.26755(4) 0.46298(4) 0.02444(13) Uani 1 1 d . . . Br02 Br 0.48115(3) 0.24372(4) 0.72633(4) 0.02326(13) Uani 1 1 d . . . Co2 Co 0.61234(3) 0.76982(5) 0.69681(4) 0.01413(14) Uani 1 1 d . . . Co1 Co 0.36281(3) 0.71747(5) 0.49645(5) 0.01423(14) Uani 1 1 d . . . O1 O 0.31007(15) 0.8159(2) 0.5145(2) 0.0166(8) Uani 1 1 d . . . N7 N 0.6272(2) 0.7637(3) 0.5753(3) 0.0182(10) Uani 1 1 d . . . N8 N 0.59018(19) 0.7744(3) 0.8192(3) 0.0154(9) Uani 1 1 d . . . N1 N 0.42600(18) 0.7978(3) 0.4776(3) 0.0181(9) Uani 1 1 d . . . O4 O 0.55998(15) 0.6693(2) 0.6854(2) 0.0165(7) Uani 1 1 d . . . C7 C 0.4804(3) 0.7507(3) 0.4876(6) 0.0296(17) Uani 1 1 d . . . H7A H 0.5068 0.7724 0.4424 0.035 Uiso 1 1 calc R . . H7B H 0.4970 0.7675 0.5438 0.035 Uiso 1 1 calc R . . O3 O 0.54898(15) 0.8481(2) 0.6735(2) 0.0158(7) Uani 1 1 d . . . C16 C 0.2668(2) 0.7129(4) 0.2717(4) 0.0223(12) Uani 1 1 d . . . H16 H 0.2273 0.7101 0.2593 0.027 Uiso 1 1 calc R . . C43 C 0.6108(3) 0.7829(4) 0.9690(4) 0.0240(12) Uani 1 1 d . . . H43 H 0.6384 0.7833 1.0134 0.029 Uiso 1 1 calc R . . N5 N 0.67555(19) 0.6935(3) 0.7201(3) 0.0197(9) Uani 1 1 d . . . C13 C 0.3795(2) 0.7178(4) 0.3119(4) 0.0182(11) Uani 1 1 d . . . H13 H 0.4188 0.7191 0.3257 0.022 Uiso 1 1 calc R . . O2 O 0.30044(16) 0.6365(2) 0.5187(3) 0.0170(8) Uani 1 1 d . . . C17 C 0.2856(2) 0.7167(3) 0.3558(4) 0.0172(10) Uani 1 1 d . . . H17 H 0.2584 0.7184 0.4007 0.021 Uiso 1 1 calc R . . C40 C 0.5343(2) 0.7755(4) 0.8385(4) 0.0184(11) Uani 1 1 d . . . H40 H 0.5073 0.7716 0.7934 0.022 Uiso 1 1 calc R . . N6 N 0.66433(19) 0.8709(3) 0.7147(3) 0.0188(10) Uani 1 1 d . . . C41 C 0.5154(2) 0.7820(4) 0.9217(4) 0.0204(11) Uani 1 1 d . . . H41 H 0.4758 0.7827 0.9333 0.024 Uiso 1 1 calc R . . C20 C 0.3846(3) 0.7149(5) 0.7973(4) 0.0258(13) Uani 1 1 d . . . H20 H 0.3874 0.7145 0.8579 0.031 Uiso 1 1 calc R . . C38 C 0.6338(2) 0.6715(4) 0.4476(4) 0.0246(12) Uani 1 1 d . . . H38 H 0.6370 0.6120 0.4215 0.030 Uiso 1 1 calc R . . C22 C 0.3771(2) 0.6348(4) 0.6639(4) 0.0195(11) Uani 1 1 d . . . H22 H 0.3747 0.5781 0.6329 0.023 Uiso 1 1 calc R . . C42 C 0.5538(2) 0.7875(4) 0.9885(4) 0.0234(11) Uani 1 1 d . . . H42 H 0.5412 0.7941 1.0460 0.028 Uiso 1 1 calc R . . C21 C 0.3805(2) 0.6319(4) 0.7526(4) 0.0218(11) Uani 1 1 d . . . H21 H 0.3801 0.5741 0.7822 0.026 Uiso 1 1 calc R . . N2 N 0.41575(19) 0.6193(3) 0.4792(3) 0.0179(10) Uani 1 1 d . . . C19 C 0.3844(2) 0.7976(4) 0.7536(4) 0.0220(12) Uani 1 1 d . . . H19 H 0.3863 0.8550 0.7836 0.026 Uiso 1 1 calc R . . C11 C 0.3191(2) 0.8998(3) 0.4883(4) 0.0202(11) Uani 1 1 d . . . C1 C 0.2427(2) 0.5048(4) 0.5037(4) 0.0255(12) Uani 1 1 d . . . H1A H 0.2248 0.5229 0.5578 0.038 Uiso 1 1 calc R . . H1B H 0.2470 0.4370 0.5019 0.038 Uiso 1 1 calc R . . H1C H 0.2189 0.5251 0.4557 0.038 Uiso 1 1 calc R . . C45 C 0.6044(3) 0.4219(5) 0.5237(5) 0.0377(16) Uani 1 1 d . . . H45A H 0.5936 0.3561 0.5230 0.057 Uiso 1 1 calc R . . H45B H 0.5701 0.4605 0.5203 0.057 Uiso 1 1 calc R . . H45C H 0.6247 0.4357 0.5770 0.057 Uiso 1 1 calc R . . C35 C 0.6261(2) 0.8407(4) 0.5264(4) 0.0180(11) Uani 1 1 d . . . H35 H 0.6238 0.8997 0.5536 0.022 Uiso 1 1 calc R . . C30 C 0.6929(3) 1.0304(4) 0.7517(4) 0.0272(13) Uani 1 1 d . . . H30A H 0.7160 1.0079 0.7997 0.041 Uiso 1 1 calc R . . H30B H 0.6737 1.0882 0.7683 0.041 Uiso 1 1 calc R . . H30C H 0.7174 1.0421 0.7022 0.041 Uiso 1 1 calc R . . C31 C 0.6488(2) 0.9574(4) 0.7286(4) 0.0205(10) Uani 1 1 d . . . C4 C 0.4033(2) 0.5326(4) 0.4667(4) 0.0184(10) Uani 1 1 d . . . C29 C 0.7238(2) 0.8434(5) 0.7252(4) 0.0299(13) Uani 1 1 d . . . H29A H 0.7358 0.8535 0.7853 0.036 Uiso 1 1 calc R . . H29B H 0.7483 0.8818 0.6877 0.036 Uiso 1 1 calc R . . C32 C 0.5920(2) 0.9887(4) 0.7209(4) 0.0231(11) Uani 1 1 d . . . H32 H 0.5841 1.0513 0.7366 0.028 Uiso 1 1 calc R . . C25 C 0.6220(3) 0.5556(4) 0.7468(4) 0.0246(12) Uani 1 1 d . . . H25 H 0.6230 0.4957 0.7724 0.029 Uiso 1 1 calc R . . C2 C 0.3000(2) 0.5497(3) 0.4971(4) 0.0188(10) Uani 1 1 d . . . C24 C 0.5701(2) 0.5867(3) 0.7156(4) 0.0205(11) Uani 1 1 d . . . C8 C 0.4749(2) 0.9396(4) 0.4314(4) 0.0257(12) Uani 1 1 d . . . H8A H 0.5026 0.9381 0.4783 0.039 Uiso 1 1 calc R . . H8B H 0.4646 1.0043 0.4191 0.039 Uiso 1 1 calc R . . H8C H 0.4916 0.9113 0.3802 0.039 Uiso 1 1 calc R . . C23 C 0.5199(2) 0.5229(4) 0.7142(4) 0.0270(13) Uani 1 1 d . . . H23A H 0.4914 0.5448 0.7553 0.041 Uiso 1 1 calc R . . H23B H 0.5320 0.4599 0.7298 0.041 Uiso 1 1 calc R . . H23C H 0.5034 0.5222 0.6566 0.041 Uiso 1 1 calc R . . O5 O 0.6399(2) 0.4411(3) 0.4533(3) 0.0390(11) Uani 1 1 d . . . H5 H 0.6608 0.3950 0.4437 0.058 Uiso 1 1 calc R . . O8 O 0.1333(3) 0.6102(5) 0.2392(4) 0.0581(16) Uani 1 1 d . . . H8 H 0.1320 0.6686 0.2380 0.087 Uiso 1 1 calc R . . O7 O 0.6210(2) 0.1289(4) 0.4486(3) 0.0427(12) Uani 1 1 d . . . H7 H 0.6545 0.1494 0.4477 0.064 Uiso 1 1 calc R . . C46 C 0.6049(3) 0.1118(5) 0.5328(4) 0.0304(14) Uani 1 1 d . . . H46A H 0.5737 0.0667 0.5336 0.046 Uiso 1 1 calc R . . H46B H 0.5924 0.1700 0.5594 0.046 Uiso 1 1 calc R . . H46C H 0.6373 0.0867 0.5647 0.046 Uiso 1 1 calc R . . C9 C 0.4219(2) 0.8854(4) 0.4574(4) 0.0199(11) Uani 1 1 d . . . N3 N 0.34156(19) 0.7182(3) 0.3760(3) 0.0156(9) Uani 1 1 d . . . N4 N 0.3771(2) 0.7162(3) 0.6208(3) 0.0159(9) Uani 1 1 d . . . C18 C 0.3816(2) 0.7963(4) 0.6641(4) 0.0197(11) Uani 1 1 d . . . H18 H 0.3828 0.8533 0.6334 0.024 Uiso 1 1 calc R . . C39 C 0.6319(2) 0.6798(4) 0.5355(4) 0.0217(12) Uani 1 1 d . . . H39 H 0.6339 0.6251 0.5694 0.026 Uiso 1 1 calc R . . C3 C 0.3460(2) 0.4997(4) 0.4697(4) 0.0216(11) Uani 1 1 d . . . H3 H 0.3393 0.4378 0.4510 0.026 Uiso 1 1 calc R . . C10 C 0.3699(2) 0.9346(3) 0.4584(4) 0.0209(11) Uani 1 1 d . . . H10 H 0.3701 0.9964 0.4368 0.025 Uiso 1 1 calc R . . C33 C 0.5475(2) 0.9355(4) 0.6927(4) 0.0193(10) Uani 1 1 d . . . C27 C 0.7278(3) 0.5551(5) 0.7674(5) 0.0327(14) Uani 1 1 d . . . H27A H 0.7534 0.5532 0.7180 0.049 Uiso 1 1 calc R . . H27B H 0.7183 0.4915 0.7849 0.049 Uiso 1 1 calc R . . H27C H 0.7466 0.5874 0.8149 0.049 Uiso 1 1 calc R . . C26 C 0.6739(2) 0.6067(4) 0.7434(4) 0.0227(12) Uani 1 1 d . . . C12 C 0.2674(2) 0.9619(4) 0.4929(4) 0.0265(12) Uani 1 1 d . . . H12A H 0.2400 0.9433 0.4488 0.040 Uiso 1 1 calc R . . H12B H 0.2787 1.0267 0.4834 0.040 Uiso 1 1 calc R . . H12C H 0.2497 0.9561 0.5495 0.040 Uiso 1 1 calc R . . C14 C 0.3640(2) 0.7154(4) 0.2269(4) 0.0213(12) Uani 1 1 d . . . H14 H 0.3922 0.7153 0.1833 0.026 Uiso 1 1 calc R . . C36 C 0.6282(2) 0.8372(4) 0.4377(4) 0.0240(12) Uani 1 1 d . . . H36 H 0.6277 0.8929 0.4049 0.029 Uiso 1 1 calc R . . C34 C 0.4898(2) 0.9802(4) 0.6817(4) 0.0271(13) Uani 1 1 d . . . H34A H 0.4738 0.9620 0.6262 0.041 Uiso 1 1 calc R . . H34B H 0.4938 1.0480 0.6839 0.041 Uiso 1 1 calc R . . H34C H 0.4645 0.9595 0.7277 0.041 Uiso 1 1 calc R . . C48 C 0.1478(3) 0.5771(5) 0.1597(4) 0.0304(14) Uani 1 1 d . . . H48A H 0.1141 0.5768 0.1227 0.046 Uiso 1 1 calc R . . H48B H 0.1626 0.5136 0.1650 0.046 Uiso 1 1 calc R . . H48C H 0.1770 0.6173 0.1345 0.046 Uiso 1 1 calc R . . C5 C 0.4487(2) 0.4603(4) 0.4517(4) 0.0257(12) Uani 1 1 d . . . H5A H 0.4787 0.4866 0.4154 0.039 Uiso 1 1 calc R . . H5B H 0.4320 0.4061 0.4231 0.039 Uiso 1 1 calc R . . H5C H 0.4650 0.4412 0.5067 0.039 Uiso 1 1 calc R . . C44 C 0.6276(3) 0.7778(4) 0.8836(4) 0.0204(11) Uani 1 1 d . . . H44 H 0.6670 0.7766 0.8706 0.025 Uiso 1 1 calc R . . C37 C 0.6310(3) 0.7513(5) 0.3978(4) 0.0249(13) Uani 1 1 d . . . H37 H 0.6310 0.7471 0.3371 0.030 Uiso 1 1 calc R . . C15 C 0.3066(3) 0.7132(4) 0.2055(4) 0.0256(12) Uani 1 1 d . . . H15 H 0.2949 0.7119 0.1473 0.031 Uiso 1 1 calc R . . O6 O 0.1023(2) 0.9165(4) 0.1733(6) 0.075(2) Uani 1 1 d . . . H6 H 0.0799 0.8834 0.2021 0.112 Uiso 1 1 calc R . . C47 C 0.1557(3) 0.8776(6) 0.1750(6) 0.049(2) Uani 1 1 d . . . H47A H 0.1811 0.9135 0.1377 0.073 Uiso 1 1 calc R . . H47B H 0.1537 0.8132 0.1546 0.073 Uiso 1 1 calc R . . H47C H 0.1703 0.8785 0.2337 0.073 Uiso 1 1 calc R . . C28 C 0.7299(2) 0.7414(5) 0.7020(5) 0.0296(16) Uani 1 1 d . . . H28A H 0.7396 0.7352 0.6405 0.035 Uiso 1 1 calc R . . H28B H 0.7609 0.7129 0.7360 0.035 Uiso 1 1 calc R . . C6 C 0.4748(3) 0.6509(4) 0.4822(7) 0.050(2) Uani 1 1 d . . . H6A H 0.4937 0.6224 0.5325 0.060 Uiso 1 1 calc R . . H6B H 0.4947 0.6287 0.4302 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br01 0.0216(3) 0.0250(3) 0.0268(3) 0.0006(2) 0.0056(3) -0.0002(2) Br02 0.0207(3) 0.0213(2) 0.0278(3) -0.0025(2) -0.0057(3) 0.00079(19) Co2 0.0106(3) 0.0184(3) 0.0134(3) 0.0011(3) 0.0002(3) 0.0000(3) Co1 0.0135(3) 0.0144(3) 0.0148(3) 0.0003(3) -0.0002(3) -0.0004(3) O1 0.0180(17) 0.0120(15) 0.0200(19) 0.0026(13) -0.0011(15) 0.0037(13) N7 0.014(2) 0.022(2) 0.018(3) 0.0017(18) -0.0048(19) -0.0006(17) N8 0.015(2) 0.0130(19) 0.018(2) 0.0015(16) 0.0000(18) -0.0023(16) N1 0.014(2) 0.023(2) 0.017(2) 0.0001(17) 0.0003(17) -0.0013(16) O4 0.0179(17) 0.0143(16) 0.0173(18) -0.0014(14) 0.0020(15) 0.0042(13) C7 0.024(3) 0.012(2) 0.052(5) -0.003(3) -0.006(4) 0.0002(19) O3 0.0123(17) 0.0144(16) 0.0206(19) 0.0005(14) 0.0006(15) 0.0007(13) C16 0.022(3) 0.009(2) 0.036(3) -0.003(2) -0.003(2) 0.0023(19) C43 0.032(3) 0.020(3) 0.020(3) 0.001(2) -0.004(2) -0.002(2) N5 0.018(2) 0.026(2) 0.016(2) 0.0000(19) 0.0036(18) 0.0052(17) C13 0.017(3) 0.020(3) 0.018(3) -0.001(2) 0.002(2) 0.002(2) O2 0.0183(18) 0.0155(16) 0.0170(19) 0.0007(14) 0.0003(14) -0.0006(14) C17 0.016(2) 0.012(2) 0.023(3) -0.0003(19) 0.000(2) 0.0011(19) C40 0.016(3) 0.019(2) 0.021(3) 0.000(2) 0.000(2) 0.0009(19) N6 0.015(2) 0.025(2) 0.016(2) 0.0029(18) 0.0027(17) -0.0025(16) C41 0.019(3) 0.023(3) 0.019(3) 0.002(2) 0.006(2) -0.005(2) C20 0.018(3) 0.040(3) 0.019(3) 0.002(3) 0.001(2) 0.005(3) C38 0.017(3) 0.037(3) 0.020(3) -0.005(2) 0.000(2) 0.002(2) C22 0.021(3) 0.016(2) 0.022(3) 0.001(2) -0.001(2) 0.001(2) C42 0.032(3) 0.019(2) 0.019(3) 0.001(2) 0.005(2) -0.001(2) C21 0.019(3) 0.025(3) 0.021(3) 0.004(2) -0.001(2) 0.004(2) N2 0.015(2) 0.017(2) 0.022(3) 0.0005(17) 0.0010(17) 0.0029(16) C19 0.020(3) 0.025(3) 0.022(3) -0.007(2) -0.003(2) -0.004(2) C11 0.021(3) 0.017(2) 0.024(3) -0.007(2) -0.006(2) 0.0009(19) C1 0.022(3) 0.017(2) 0.037(3) 0.000(2) 0.000(3) -0.003(2) C45 0.037(4) 0.036(3) 0.041(4) -0.003(3) 0.006(3) 0.005(3) C35 0.011(2) 0.023(3) 0.020(3) 0.003(2) 0.001(2) -0.0021(19) C30 0.027(3) 0.029(3) 0.026(3) -0.002(2) 0.002(2) -0.014(2) C31 0.028(3) 0.020(2) 0.014(2) 0.000(2) 0.000(2) -0.012(2) C4 0.014(2) 0.023(2) 0.018(2) 0.000(2) 0.000(2) 0.0036(19) C29 0.014(2) 0.054(4) 0.022(3) 0.011(3) -0.004(2) -0.004(2) C32 0.027(3) 0.017(2) 0.025(3) -0.003(2) 0.007(2) -0.004(2) C25 0.029(3) 0.020(2) 0.024(3) 0.006(2) 0.002(2) 0.005(2) C2 0.023(3) 0.014(2) 0.019(2) 0.001(2) -0.002(2) -0.0028(18) C24 0.028(3) 0.016(2) 0.017(3) -0.002(2) 0.006(2) 0.004(2) C8 0.025(3) 0.021(3) 0.031(3) 0.001(2) 0.002(2) -0.009(2) C23 0.028(3) 0.017(2) 0.036(3) 0.003(2) 0.000(3) -0.004(2) O5 0.041(3) 0.033(2) 0.042(3) 0.000(2) 0.001(2) 0.009(2) O8 0.044(3) 0.080(4) 0.050(3) -0.023(3) -0.008(3) 0.021(3) O7 0.029(2) 0.070(3) 0.030(3) 0.014(2) -0.002(2) -0.018(2) C46 0.020(3) 0.037(3) 0.034(3) 0.007(3) -0.002(3) 0.001(2) C9 0.021(3) 0.021(2) 0.018(3) -0.002(2) -0.005(2) -0.005(2) N3 0.015(2) 0.0134(19) 0.018(2) 0.0006(17) -0.0006(18) -0.0010(16) N4 0.010(2) 0.017(2) 0.021(2) 0.0003(17) -0.0025(19) -0.0004(17) C18 0.017(3) 0.017(2) 0.025(3) 0.001(2) 0.002(2) 0.004(2) C39 0.016(3) 0.031(3) 0.018(3) 0.000(2) 0.002(2) 0.007(2) C3 0.021(2) 0.016(2) 0.028(3) -0.002(2) -0.001(2) -0.0022(19) C10 0.025(3) 0.011(2) 0.026(3) 0.004(2) -0.004(2) -0.0041(19) C33 0.021(3) 0.018(2) 0.019(3) -0.001(2) 0.005(2) -0.0040(19) C27 0.024(3) 0.037(3) 0.037(4) 0.005(3) -0.001(3) 0.013(3) C26 0.024(3) 0.027(3) 0.018(3) -0.003(2) 0.001(2) 0.009(2) C12 0.028(3) 0.020(2) 0.031(3) -0.001(2) -0.005(3) 0.004(2) C14 0.020(3) 0.023(2) 0.020(3) 0.001(2) 0.002(2) -0.0025(19) C36 0.019(3) 0.033(3) 0.021(3) 0.007(2) 0.001(2) -0.002(2) C34 0.023(3) 0.018(3) 0.040(4) -0.001(2) 0.002(3) 0.005(2) C48 0.030(3) 0.032(3) 0.029(3) -0.004(3) -0.002(3) 0.004(3) C5 0.021(3) 0.020(2) 0.036(3) -0.001(2) -0.001(2) 0.006(2) C44 0.016(3) 0.022(3) 0.023(3) 0.002(2) 0.000(2) 0.002(2) C37 0.015(3) 0.044(4) 0.015(3) -0.002(2) 0.001(2) 0.001(2) C15 0.028(3) 0.030(3) 0.019(3) 0.002(2) -0.006(2) 0.001(2) O6 0.039(3) 0.029(3) 0.157(7) 0.022(4) 0.024(4) 0.001(2) C47 0.030(4) 0.048(4) 0.069(6) 0.025(4) -0.001(4) -0.003(3) C28 0.003(3) 0.060(4) 0.025(4) 0.001(3) -0.001(3) 0.002(2) C6 0.018(3) 0.013(3) 0.120(8) 0.007(4) -0.009(4) 0.001(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 Co2 N7 1.932(5) . ? Co2 N8 1.982(5) . ? Co2 O4 1.907(4) . ? Co2 O3 1.903(4) . ? Co2 N5 1.884(4) . ? Co2 N6 1.920(5) . ? Co1 O1 1.903(4) . ? Co1 N1 1.906(4) . ? Co1 O2 1.905(4) . ? Co1 N2 1.901(4) . ? Co1 N3 1.946(5) . ? Co1 N4 1.971(5) . ? O1 C11 1.292(6) . ? N7 C35 1.345(7) . ? N7 C39 1.361(8) . ? N8 C40 1.349(7) . ? N8 C44 1.338(8) . ? N1 C7 1.456(7) . ? N1 C9 1.302(7) . ? O4 C24 1.299(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C6 1.444(7) . ? O3 C33 1.292(6) . ? C16 H16 0.9500 . ? C16 C17 1.388(9) . ? C16 C15 1.395(9) . ? C43 H43 0.9500 . ? C43 C42 1.378(8) . ? C43 C44 1.393(9) . ? N5 C26 1.300(7) . ? N5 C28 1.480(7) . ? C13 H13 0.9500 . ? C13 N3 1.342(7) . ? C13 C14 1.377(8) . ? O2 C2 1.293(6) . ? C17 H17 0.9500 . ? C17 N3 1.354(7) . ? C40 H40 0.9500 . ? C40 C41 1.377(8) . ? N6 C31 1.314(7) . ? N6 C29 1.463(7) . ? C41 H41 0.9500 . ? C41 C42 1.382(8) . ? C20 H20 0.9500 . ? C20 C21 1.384(9) . ? C20 C19 1.371(9) . ? C38 H38 0.9500 . ? C38 C39 1.378(8) . ? C38 C37 1.388(9) . ? C22 H22 0.9500 . ? C22 C21 1.388(8) . ? C22 N4 1.349(7) . ? C42 H42 0.9500 . ? C21 H21 0.9500 . ? N2 C4 1.295(7) . ? N2 C6 1.463(7) . ? C19 H19 0.9500 . ? C19 C18 1.400(8) . ? C11 C10 1.379(8) . ? C11 C12 1.511(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.500(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C45 O5 1.408(8) . ? C35 H35 0.9500 . ? C35 C36 1.386(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30 C31 1.519(7) . ? C31 C32 1.416(8) . ? C4 C3 1.430(7) . ? C4 C5 1.510(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C28 1.518(9) . ? C32 H32 0.9500 . ? C32 C33 1.370(7) . ? C25 H25 0.9500 . ? C25 C24 1.390(8) . ? C25 C26 1.425(8) . ? C2 C3 1.367(8) . ? C24 C23 1.497(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8 C9 1.526(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O5 H5 0.8400 . ? O8 H8 0.8400 . ? O8 C48 1.373(9) . ? O7 H7 0.8400 . ? O7 C46 1.391(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C9 C10 1.412(8) . ? N4 C18 1.339(7) . ? C18 H18 0.9500 . ? C39 H39 0.9500 . ? C3 H3 0.9500 . ? C10 H10 0.9500 . ? C33 C34 1.512(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 C26 1.518(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 H14 0.9500 . ? C14 C15 1.391(8) . ? C36 H36 0.9500 . ? C36 C37 1.385(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C44 H44 0.9500 . ? C37 H37 0.9500 . ? C15 H15 0.9500 . ? O6 H6 0.8400 . ? O6 C47 1.376(9) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 N7 Co2 N8 175.1(2) . . ? O4 Co2 N7 89.44(19) . . ? O4 Co2 N8 86.88(17) . . ? O4 Co2 N6 177.00(19) . . ? O3 Co2 N7 88.87(19) . . ? O3 Co2 N8 87.63(18) . . ? O3 Co2 O4 85.59(16) . . ? O3 Co2 N6 94.61(18) . . ? N5 Co2 N7 91.2(2) . . ? N5 Co2 N8 92.37(19) . . ? N5 Co2 O4 95.02(18) . . ? N5 Co2 O3 179.38(18) . . ? N5 Co2 N6 84.78(19) . . ? N6 Co2 N7 93.6(2) . . ? N6 Co2 N8 90.13(19) . . ? O1 Co1 N1 94.70(17) . . ? O1 Co1 O2 85.65(16) . . ? O1 Co1 N3 88.35(18) . . ? O1 Co1 N4 88.44(18) . . ? N1 Co1 N3 92.73(19) . . ? N1 Co1 N4 91.43(19) . . ? O2 Co1 N1 178.28(18) . . ? O2 Co1 N3 88.97(18) . . ? O2 Co1 N4 86.89(18) . . ? N2 Co1 O1 179.6(2) . . ? N2 Co1 N1 85.17(19) . . ? N2 Co1 O2 94.47(18) . . ? N2 Co1 N3 92.06(19) . . ? N2 Co1 N4 91.2(2) . . ? N3 Co1 N4 174.9(2) . . ? C11 O1 Co1 122.7(3) . . ? C35 N7 Co2 121.1(4) . . ? C35 N7 C39 118.1(5) . . ? C39 N7 Co2 120.2(4) . . ? C40 N8 Co2 118.2(4) . . ? C44 N8 Co2 123.6(4) . . ? C44 N8 C40 118.3(5) . . ? C7 N1 Co1 112.8(3) . . ? C9 N1 Co1 124.4(4) . . ? C9 N1 C7 122.7(5) . . ? C24 O4 Co2 122.6(4) . . ? N1 C7 H7A 109.2 . . ? N1 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C6 C7 N1 112.1(5) . . ? C6 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C33 O3 Co2 123.5(4) . . ? C17 C16 H16 120.4 . . ? C17 C16 C15 119.1(5) . . ? C15 C16 H16 120.4 . . ? C42 C43 H43 120.3 . . ? C42 C43 C44 119.4(6) . . ? C44 C43 H43 120.3 . . ? C26 N5 Co2 126.1(4) . . ? C26 N5 C28 121.7(5) . . ? C28 N5 Co2 112.0(4) . . ? N3 C13 H13 118.6 . . ? N3 C13 C14 122.9(5) . . ? C14 C13 H13 118.6 . . ? C2 O2 Co1 123.2(4) . . ? C16 C17 H17 119.0 . . ? N3 C17 C16 122.1(5) . . ? N3 C17 H17 119.0 . . ? N8 C40 H40 119.1 . . ? N8 C40 C41 121.8(5) . . ? C41 C40 H40 119.1 . . ? C31 N6 Co2 124.2(4) . . ? C31 N6 C29 120.2(5) . . ? C29 N6 Co2 115.0(4) . . ? C40 C41 H41 119.9 . . ? C40 C41 C42 120.3(5) . . ? C42 C41 H41 119.9 . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C19 C20 C21 119.8(6) . . ? C39 C38 H38 120.5 . . ? C39 C38 C37 119.0(6) . . ? C37 C38 H38 120.5 . . ? C21 C22 H22 119.2 . . ? N4 C22 H22 119.2 . . ? N4 C22 C21 121.6(5) . . ? C43 C42 C41 117.9(6) . . ? C43 C42 H42 121.1 . . ? C41 C42 H42 121.1 . . ? C20 C21 C22 118.7(6) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C4 N2 Co1 125.9(4) . . ? C4 N2 C6 121.2(4) . . ? C6 N2 Co1 112.9(3) . . ? C20 C19 H19 120.5 . . ? C20 C19 C18 119.0(6) . . ? C18 C19 H19 120.5 . . ? O1 C11 C10 126.0(5) . . ? O1 C11 C12 113.9(5) . . ? C10 C11 C12 120.1(5) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O5 C45 H45A 109.5 . . ? O5 C45 H45B 109.5 . . ? O5 C45 H45C 109.5 . . ? N7 C35 H35 118.8 . . ? N7 C35 C36 122.5(6) . . ? C36 C35 H35 118.8 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? N6 C31 C30 120.1(5) . . ? N6 C31 C32 123.4(5) . . ? C32 C31 C30 116.5(5) . . ? N2 C4 C3 121.8(5) . . ? N2 C4 C5 121.7(5) . . ? C3 C4 C5 116.4(5) . . ? N6 C29 H29A 109.9 . . ? N6 C29 H29B 109.9 . . ? N6 C29 C28 109.0(5) . . ? H29A C29 H29B 108.3 . . ? C28 C29 H29A 109.9 . . ? C28 C29 H29B 109.9 . . ? C31 C32 H32 117.6 . . ? C33 C32 C31 124.8(5) . . ? C33 C32 H32 117.6 . . ? C24 C25 H25 117.5 . . ? C24 C25 C26 125.0(5) . . ? C26 C25 H25 117.5 . . ? O2 C2 C1 113.8(5) . . ? O2 C2 C3 125.7(5) . . ? C3 C2 C1 120.5(5) . . ? O4 C24 C25 125.7(5) . . ? O4 C24 C23 114.2(5) . . ? C25 C24 C23 120.2(5) . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C45 O5 H5 109.5 . . ? C48 O8 H8 109.5 . . ? C46 O7 H7 109.5 . . ? O7 C46 H46A 109.5 . . ? O7 C46 H46B 109.5 . . ? O7 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N1 C9 C8 119.8(5) . . ? N1 C9 C10 123.0(5) . . ? C10 C9 C8 117.1(5) . . ? C13 N3 Co1 123.4(4) . . ? C13 N3 C17 118.3(5) . . ? C17 N3 Co1 118.3(4) . . ? C22 N4 Co1 120.0(4) . . ? C18 N4 Co1 120.2(4) . . ? C18 N4 C22 119.5(5) . . ? C19 C18 H18 119.3 . . ? N4 C18 C19 121.3(5) . . ? N4 C18 H18 119.3 . . ? N7 C39 C38 122.3(6) . . ? N7 C39 H39 118.9 . . ? C38 C39 H39 118.9 . . ? C4 C3 H3 117.2 . . ? C2 C3 C4 125.6(5) . . ? C2 C3 H3 117.2 . . ? C11 C10 C9 125.1(5) . . ? C11 C10 H10 117.5 . . ? C9 C10 H10 117.5 . . ? O3 C33 C32 126.7(5) . . ? O3 C33 C34 114.3(5) . . ? C32 C33 C34 119.1(5) . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? N5 C26 C25 122.1(5) . . ? N5 C26 C27 120.8(5) . . ? C25 C26 C27 117.1(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C13 C14 H14 120.3 . . ? C13 C14 C15 119.3(6) . . ? C15 C14 H14 120.3 . . ? C35 C36 H36 120.5 . . ? C37 C36 C35 118.9(6) . . ? C37 C36 H36 120.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O8 C48 H48A 109.5 . . ? O8 C48 H48B 109.5 . . ? O8 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N8 C44 C43 122.3(5) . . ? N8 C44 H44 118.8 . . ? C43 C44 H44 118.8 . . ? C38 C37 H37 120.4 . . ? C36 C37 C38 119.2(6) . . ? C36 C37 H37 120.4 . . ? C16 C15 H15 120.9 . . ? C14 C15 C16 118.3(6) . . ? C14 C15 H15 120.9 . . ? C47 O6 H6 109.5 . . ? O6 C47 H47A 109.5 . . ? O6 C47 H47B 109.5 . . ? O6 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N5 C28 C29 108.7(5) . . ? N5 C28 H28A 109.9 . . ? N5 C28 H28B 109.9 . . ? C29 C28 H28A 109.9 . . ? C29 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? C7 C6 N2 113.3(5) . . ? C7 C6 H6A 108.9 . . ? C7 C6 H6B 108.9 . . ? N2 C6 H6A 108.9 . . ? N2 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? data_Co(acacen)(NMeIm)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 Co N6 O2, C24 H20 B, 2(C2 H6 O) ' _chemical_formula_sum 'C48 H62 B Co N6 O4' _chemical_formula_weight 856.78 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.9254(5) _cell_length_b 18.0542(6) _cell_length_c 17.8151(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.6470(18) _cell_angle_gamma 90.00 _cell_volume 4439.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9722 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 29.96 _exptl_crystal_description tabular _exptl_crystal_colour orange _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.437 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8904 _exptl_absorpt_correction_T_max 0.9631 _exptl_absorpt_process_details 'face-indexed' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76376 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 30.03 _reflns_number_total 12872 _reflns_number_gt 9315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Rigid bond restraints (esd 0.01) were imposed on the displacement parameters as well as restraints on similar amplitudes (esd 0.05) separated by less than 1.7 Ang. on the disordered ethanol solvent molecule. Chemically equivalent, but not symmetry equivalent disordered ethanol molecules atoms were restrained so that bond distances and angles were similar to the non-disordered ethanol. ; _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^)+(0.0660P)^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 12872 _refine_ls_number_parameters 581 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.302 _refine_ls_restrained_S_all 1.321 _refine_ls_shift/su_max 0.009 _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 0.175505(16) 0.994700(13) 0.292767(12) 0.01528(8) Uani 1 1 d . . . O1 O 0.03944(9) 0.97962(7) 0.27386(7) 0.0187(3) Uani 1 1 d . . . O2 O 0.14398(9) 1.08950(7) 0.25044(6) 0.0183(3) Uani 1 1 d . . . N1 N 0.20339(11) 0.89799(8) 0.33138(8) 0.0181(3) Uani 1 1 d . . . N2 N 0.31097(10) 1.01291(8) 0.31304(8) 0.0171(3) Uani 1 1 d . . . N3 N 0.16133(10) 1.03186(8) 0.39293(8) 0.0167(3) Uani 1 1 d . . . N4 N 0.15514(11) 1.10830(8) 0.48795(8) 0.0183(3) Uani 1 1 d . . . N5 N 0.18933(11) 0.95634(8) 0.19305(8) 0.0194(3) Uani 1 1 d . . . N6 N 0.24351(11) 0.93484(9) 0.08482(8) 0.0220(3) Uani 1 1 d . . . C1 C -0.00548(13) 0.92217(10) 0.29589(9) 0.0194(4) Uani 1 1 d . . . C2 C 0.03859(14) 0.85975(10) 0.32885(10) 0.0226(4) Uani 1 1 d . . . H2 H -0.0024 0.8221 0.3440 0.027 Uiso 1 1 calc R . . C3 C 0.14009(14) 0.84670(10) 0.34220(10) 0.0216(4) Uani 1 1 d . . . C4 C 0.30664(13) 0.88196(10) 0.33587(10) 0.0213(4) Uani 1 1 d . . . H4A H 0.3217 0.8634 0.2865 0.026 Uiso 1 1 calc R . . H4B H 0.3252 0.8434 0.3746 0.026 Uiso 1 1 calc R . . C5 C 0.36230(13) 0.95243(10) 0.35677(10) 0.0209(4) Uani 1 1 d . . . H5A H 0.3653 0.9622 0.4117 0.025 Uiso 1 1 calc R . . H5B H 0.4293 0.9481 0.3443 0.025 Uiso 1 1 calc R . . C6 C 0.35527(13) 1.07439(10) 0.29890(9) 0.0186(4) Uani 1 1 d . . . C7 C 0.30513(13) 1.13482(10) 0.26026(9) 0.0201(4) Uani 1 1 d . . . H7 H 0.3432 1.1759 0.2486 0.024 Uiso 1 1 calc R . . C8 C 0.20741(13) 1.13945(10) 0.23832(9) 0.0183(4) Uani 1 1 d . . . C9 C -0.11372(13) 0.92677(11) 0.28028(10) 0.0249(4) Uani 1 1 d . . . H9A H -0.1355 0.9736 0.3001 0.037 Uiso 1 1 calc R . . H9B H -0.1423 0.8853 0.3050 0.037 Uiso 1 1 calc R . . H9C H -0.1341 0.9244 0.2255 0.037 Uiso 1 1 calc R . . C10 C 0.17357(16) 0.77114(11) 0.37024(14) 0.0350(5) Uani 1 1 d . . . H10A H 0.2111 0.7481 0.3337 0.052 Uiso 1 1 calc R . . H10B H 0.1171 0.7402 0.3759 0.052 Uiso 1 1 calc R . . H10C H 0.2142 0.7759 0.4193 0.052 Uiso 1 1 calc R . . C11 C 0.46256(14) 1.08308(11) 0.32164(11) 0.0258(4) Uani 1 1 d . . . H11A H 0.4802 1.0644 0.3733 0.039 Uiso 1 1 calc R . . H11B H 0.4800 1.1356 0.3197 0.039 Uiso 1 1 calc R . . H11C H 0.4974 1.0549 0.2868 0.039 Uiso 1 1 calc R . . C12 C 0.16412(15) 1.20727(10) 0.19785(10) 0.0251(4) Uani 1 1 d . . . H12A H 0.1342 1.1936 0.1468 0.038 Uiso 1 1 calc R . . H12B H 0.2152 1.2440 0.1943 0.038 Uiso 1 1 calc R . . H12C H 0.1149 1.2284 0.2261 0.038 Uiso 1 1 calc R . . C13 C 0.17690(12) 1.10077(10) 0.41724(9) 0.0176(4) Uani 1 1 d . . . H13 H 0.2003 1.1395 0.3885 0.021 Uiso 1 1 calc R . . C14 C 0.12498(14) 1.04094(11) 0.51065(10) 0.0239(4) Uani 1 1 d . . . H14 H 0.1054 1.0293 0.5584 0.029 Uiso 1 1 calc R . . C15 C 0.12852(14) 0.99393(10) 0.45178(10) 0.0231(4) Uani 1 1 d . . . H15 H 0.1112 0.9430 0.4511 0.028 Uiso 1 1 calc R . . C16 C 0.16547(14) 1.17555(10) 0.53367(10) 0.0228(4) Uani 1 1 d . . . H16A H 0.2180 1.1690 0.5756 0.034 Uiso 1 1 calc R . . H16B H 0.1047 1.1855 0.5540 0.034 Uiso 1 1 calc R . . H16C H 0.1806 1.2173 0.5021 0.034 Uiso 1 1 calc R . . C17 C 0.25196(13) 0.97692(11) 0.14734(9) 0.0198(4) Uani 1 1 d . . . H17 H 0.2970 1.0163 0.1575 0.024 Uiso 1 1 calc R . . C18 C 0.17324(15) 0.88346(11) 0.09186(11) 0.0273(4) Uani 1 1 d . . . H18 H 0.1519 0.8454 0.0567 0.033 Uiso 1 1 calc R . . C19 C 0.13967(14) 0.89701(11) 0.15854(10) 0.0248(4) Uani 1 1 d . . . H19 H 0.0900 0.8700 0.1782 0.030 Uiso 1 1 calc R . . C20 C 0.30182(15) 0.94094(12) 0.02236(10) 0.0290(4) Uani 1 1 d . . . H20A H 0.2683 0.9727 -0.0174 0.043 Uiso 1 1 calc R . . H20B H 0.3112 0.8916 0.0016 0.043 Uiso 1 1 calc R . . H20C H 0.3650 0.9626 0.0411 0.043 Uiso 1 1 calc R . . C21 C 0.34834(13) 0.30589(10) 0.49305(9) 0.0191(4) Uani 1 1 d . . . C22 C 0.30512(14) 0.28904(11) 0.41907(10) 0.0230(4) Uani 1 1 d . . . H22 H 0.3406 0.2600 0.3878 0.028 Uiso 1 1 calc R . . C23 C 0.21311(15) 0.31295(11) 0.38985(11) 0.0297(5) Uani 1 1 d . . . H23 H 0.1872 0.3006 0.3394 0.036 Uiso 1 1 calc R . . C24 C 0.15867(15) 0.35502(12) 0.43414(11) 0.0301(5) Uani 1 1 d . . . H24 H 0.0959 0.3721 0.4142 0.036 Uiso 1 1 calc R . . C25 C 0.19761(14) 0.37151(11) 0.50794(11) 0.0255(4) Uani 1 1 d . . . H25 H 0.1611 0.3996 0.5392 0.031 Uiso 1 1 calc R . . C26 C 0.28953(13) 0.34713(10) 0.53616(10) 0.0216(4) Uani 1 1 d . . . H26 H 0.3142 0.3588 0.5871 0.026 Uiso 1 1 calc R . . C27 C 0.43123(13) 0.19935(10) 0.57518(10) 0.0190(4) Uani 1 1 d . . . C28 C 0.40737(13) 0.13342(11) 0.53507(10) 0.0216(4) Uani 1 1 d . . . H28 H 0.4134 0.1320 0.4826 0.026 Uiso 1 1 calc R . . C29 C 0.37547(13) 0.07033(11) 0.56860(11) 0.0242(4) Uani 1 1 d . . . H29 H 0.3603 0.0271 0.5390 0.029 Uiso 1 1 calc R . . C30 C 0.36560(14) 0.07002(11) 0.64489(11) 0.0253(4) Uani 1 1 d . . . H30 H 0.3431 0.0271 0.6679 0.030 Uiso 1 1 calc R . . C31 C 0.38917(14) 0.13347(11) 0.68700(10) 0.0250(4) Uani 1 1 d . . . H31 H 0.3831 0.1343 0.7395 0.030 Uiso 1 1 calc R . . C32 C 0.42178(13) 0.19624(10) 0.65239(10) 0.0217(4) Uani 1 1 d . . . H32 H 0.4383 0.2389 0.6826 0.026 Uiso 1 1 calc R . . C33 C 0.52550(13) 0.25896(11) 0.46540(9) 0.0209(4) Uani 1 1 d . . . C34 C 0.59301(14) 0.20186(12) 0.46979(11) 0.0275(4) Uani 1 1 d . . . H34 H 0.5945 0.1672 0.5101 0.033 Uiso 1 1 calc R . . C35 C 0.65896(15) 0.19316(13) 0.41739(12) 0.0350(5) Uani 1 1 d . . . H35 H 0.7041 0.1534 0.4229 0.042 Uiso 1 1 calc R . . C36 C 0.65847(16) 0.24215(14) 0.35789(12) 0.0382(6) Uani 1 1 d . . . H36 H 0.7037 0.2371 0.3227 0.046 Uiso 1 1 calc R . . C37 C 0.59139(17) 0.29847(13) 0.35045(12) 0.0378(5) Uani 1 1 d . . . H37 H 0.5888 0.3317 0.3089 0.045 Uiso 1 1 calc R . . C38 C 0.52719(15) 0.30701(12) 0.40350(11) 0.0292(4) Uani 1 1 d . . . H38 H 0.4826 0.3471 0.3976 0.035 Uiso 1 1 calc R . . C39 C 0.51321(13) 0.33850(10) 0.58523(9) 0.0188(4) Uani 1 1 d . . . C40 C 0.58814(13) 0.32146(10) 0.64375(10) 0.0222(4) Uani 1 1 d . . . H40 H 0.6005 0.2709 0.6562 0.027 Uiso 1 1 calc R . . C41 C 0.64480(14) 0.37498(11) 0.68420(10) 0.0256(4) Uani 1 1 d . . . H41 H 0.6949 0.3606 0.7230 0.031 Uiso 1 1 calc R . . C42 C 0.62861(14) 0.44942(11) 0.66825(10) 0.0240(4) Uani 1 1 d . . . H42 H 0.6672 0.4864 0.6957 0.029 Uiso 1 1 calc R . . C43 C 0.55539(14) 0.46886(11) 0.61174(10) 0.0242(4) Uani 1 1 d . . . H43 H 0.5430 0.5196 0.6003 0.029 Uiso 1 1 calc R . . C44 C 0.49964(13) 0.41431(11) 0.57142(10) 0.0223(4) Uani 1 1 d . . . H44 H 0.4499 0.4293 0.5326 0.027 Uiso 1 1 calc R . . O3 O 0.94976(15) 0.12082(11) 0.19375(11) 0.0679(6) Uani 1 1 d D . . H3 H 0.9988 0.0980 0.2145 0.102 Uiso 1 1 calc R . . C45 C 0.89976(17) 0.07600(13) 0.13568(12) 0.0375(5) Uani 1 1 d D . . H45A H 0.8436 0.1038 0.1099 0.045 Uiso 1 1 calc R . . H45B H 0.8748 0.0312 0.1587 0.045 Uiso 1 1 calc R . . C46 C 0.96313(18) 0.05324(15) 0.07879(13) 0.0462(6) Uani 1 1 d D . . H46A H 0.9882 0.0974 0.0560 0.069 Uiso 1 1 calc R . . H46B H 0.9256 0.0235 0.0392 0.069 Uiso 1 1 calc R . . H46C H 1.0174 0.0238 0.1037 0.069 Uiso 1 1 calc R . . O4A O 0.8430(2) 0.11058(19) 0.32583(18) 0.0434(10) Uani 0.515(4) 1 d PDU A 1 H4OA H 0.8631 0.1099 0.2834 0.065 Uiso 0.515(4) 1 calc PR A 1 C47A C 0.9190(9) 0.1395(6) 0.3830(7) 0.048(3) Uani 0.515(4) 1 d PDU A 1 H47A H 0.8950 0.1396 0.4329 0.058 Uiso 0.515(4) 1 calc PR A 1 H47B H 0.9759 0.1062 0.3865 0.058 Uiso 0.515(4) 1 calc PR A 1 C48A C 0.9474(7) 0.2100(4) 0.3671(3) 0.0410(16) Uani 0.515(4) 1 d PDU A 1 H48A H 0.9793 0.2092 0.3213 0.062 Uiso 0.515(4) 1 calc PR A 1 H48B H 0.9926 0.2287 0.4097 0.062 Uiso 0.515(4) 1 calc PR A 1 H48C H 0.8904 0.2423 0.3590 0.062 Uiso 0.515(4) 1 calc PR A 1 O4B O 0.8900(4) 0.2131(3) 0.2943(2) 0.0806(17) Uani 0.485(4) 1 d PDU A 2 H4OB H 0.9026 0.1785 0.2656 0.121 Uiso 0.485(4) 1 calc PR A 2 C47B C 0.9421(12) 0.1971(7) 0.3794(8) 0.157(6) Uani 0.485(4) 1 d PDU A 2 H47C H 1.0130 0.2051 0.3848 0.189 Uiso 0.485(4) 1 calc PR A 2 H47D H 0.9135 0.2264 0.4178 0.189 Uiso 0.485(4) 1 calc PR A 2 C48B C 0.9177(10) 0.1221(6) 0.3811(6) 0.040(3) Uani 0.485(4) 1 d PDU A 2 H48D H 0.8482 0.1161 0.3642 0.059 Uiso 0.485(4) 1 calc PR A 2 H48E H 0.9330 0.1033 0.4330 0.059 Uiso 0.485(4) 1 calc PR A 2 H48F H 0.9547 0.0943 0.3475 0.059 Uiso 0.485(4) 1 calc PR A 2 B1 B 0.45508(15) 0.27500(12) 0.53043(10) 0.0188(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01516(14) 0.01746(14) 0.01345(12) -0.00026(8) 0.00279(9) -0.00020(9) O1 0.0160(6) 0.0228(7) 0.0174(6) -0.0004(5) 0.0030(5) -0.0016(5) O2 0.0180(6) 0.0199(7) 0.0172(6) 0.0014(5) 0.0026(5) 0.0003(5) N1 0.0177(8) 0.0186(8) 0.0181(7) 0.0001(5) 0.0023(6) 0.0004(6) N2 0.0143(7) 0.0206(8) 0.0164(7) 0.0000(5) 0.0023(5) 0.0015(6) N3 0.0148(7) 0.0201(8) 0.0154(7) 0.0006(5) 0.0028(5) -0.0007(6) N4 0.0189(8) 0.0210(8) 0.0154(7) -0.0030(5) 0.0036(5) -0.0026(6) N5 0.0179(8) 0.0223(8) 0.0180(7) -0.0024(6) 0.0023(6) -0.0013(6) N6 0.0258(9) 0.0236(8) 0.0177(7) -0.0022(6) 0.0069(6) -0.0008(7) C1 0.0186(9) 0.0237(10) 0.0165(8) -0.0061(7) 0.0048(6) -0.0049(8) C2 0.0229(10) 0.0216(10) 0.0244(9) -0.0022(7) 0.0069(7) -0.0068(8) C3 0.0250(10) 0.0182(9) 0.0220(9) 0.0006(7) 0.0039(7) -0.0029(8) C4 0.0204(10) 0.0205(9) 0.0230(9) 0.0015(7) 0.0034(7) 0.0039(7) C5 0.0185(9) 0.0215(10) 0.0220(9) 0.0030(7) -0.0005(7) 0.0009(7) C6 0.0183(9) 0.0224(9) 0.0158(8) -0.0024(6) 0.0052(6) -0.0019(7) C7 0.0230(10) 0.0187(9) 0.0200(8) 0.0015(7) 0.0084(7) -0.0031(7) C8 0.0245(10) 0.0178(9) 0.0133(7) -0.0001(6) 0.0057(6) 0.0003(7) C9 0.0213(10) 0.0295(11) 0.0242(9) -0.0031(7) 0.0043(7) -0.0047(8) C10 0.0309(12) 0.0193(10) 0.0543(14) 0.0082(9) 0.0041(10) -0.0021(9) C11 0.0197(10) 0.0281(11) 0.0305(10) -0.0020(8) 0.0062(7) -0.0041(8) C12 0.0316(11) 0.0218(10) 0.0220(9) 0.0042(7) 0.0044(8) 0.0033(8) C13 0.0168(9) 0.0203(9) 0.0164(8) 0.0007(6) 0.0045(6) 0.0002(7) C14 0.0290(11) 0.0274(11) 0.0167(8) 0.0000(7) 0.0077(7) -0.0084(8) C15 0.0299(11) 0.0217(10) 0.0186(8) -0.0004(7) 0.0065(7) -0.0084(8) C16 0.0258(10) 0.0236(10) 0.0198(8) -0.0056(7) 0.0062(7) -0.0024(8) C17 0.0199(9) 0.0229(9) 0.0166(8) -0.0002(7) 0.0030(7) -0.0013(8) C18 0.0338(11) 0.0263(10) 0.0228(9) -0.0075(7) 0.0076(8) -0.0052(9) C19 0.0269(11) 0.0258(10) 0.0223(9) -0.0040(7) 0.0056(7) -0.0053(8) C20 0.0335(12) 0.0357(12) 0.0201(9) -0.0052(8) 0.0124(8) -0.0023(9) C21 0.0224(10) 0.0198(9) 0.0156(8) 0.0022(6) 0.0047(6) -0.0030(7) C22 0.0267(10) 0.0245(10) 0.0180(8) 0.0012(7) 0.0034(7) -0.0020(8) C23 0.0363(12) 0.0295(11) 0.0207(9) 0.0050(8) -0.0056(8) -0.0033(9) C24 0.0242(11) 0.0297(11) 0.0339(11) 0.0072(8) -0.0059(8) 0.0021(9) C25 0.0228(10) 0.0223(10) 0.0318(10) 0.0013(8) 0.0048(8) 0.0006(8) C26 0.0234(10) 0.0221(10) 0.0195(8) -0.0009(7) 0.0035(7) -0.0010(8) C27 0.0151(9) 0.0225(9) 0.0195(8) 0.0004(7) 0.0024(6) 0.0024(7) C28 0.0198(9) 0.0263(10) 0.0191(8) -0.0001(7) 0.0037(7) 0.0011(8) C29 0.0199(10) 0.0217(10) 0.0303(10) -0.0006(7) 0.0008(7) 0.0016(8) C30 0.0213(10) 0.0245(10) 0.0305(10) 0.0086(8) 0.0041(7) 0.0012(8) C31 0.0234(10) 0.0318(11) 0.0207(9) 0.0049(7) 0.0057(7) 0.0031(8) C32 0.0217(10) 0.0246(10) 0.0190(8) -0.0009(7) 0.0040(7) 0.0029(8) C33 0.0195(9) 0.0259(10) 0.0177(8) -0.0060(7) 0.0046(7) -0.0048(8) C34 0.0204(10) 0.0388(12) 0.0230(9) -0.0065(8) 0.0014(7) -0.0007(9) C35 0.0192(11) 0.0498(14) 0.0364(11) -0.0174(10) 0.0053(8) 0.0003(10) C36 0.0289(12) 0.0587(16) 0.0305(11) -0.0219(10) 0.0170(9) -0.0160(11) C37 0.0426(14) 0.0477(14) 0.0264(10) -0.0075(9) 0.0173(9) -0.0171(11) C38 0.0350(12) 0.0296(11) 0.0254(10) -0.0009(8) 0.0127(8) -0.0058(9) C39 0.0171(9) 0.0249(10) 0.0154(8) -0.0008(7) 0.0058(6) 0.0007(7) C40 0.0232(10) 0.0204(9) 0.0228(9) 0.0001(7) 0.0019(7) 0.0022(8) C41 0.0259(10) 0.0287(11) 0.0210(9) -0.0016(7) -0.0014(7) -0.0005(8) C42 0.0265(10) 0.0277(11) 0.0186(8) -0.0048(7) 0.0057(7) -0.0039(8) C43 0.0287(11) 0.0194(10) 0.0253(9) 0.0005(7) 0.0069(8) -0.0012(8) C44 0.0223(10) 0.0259(10) 0.0190(8) 0.0025(7) 0.0029(7) 0.0000(8) O3 0.0644(14) 0.0646(13) 0.0633(13) -0.0293(10) -0.0333(10) 0.0367(10) C45 0.0386(13) 0.0404(13) 0.0321(11) 0.0002(9) 0.0000(9) 0.0029(11) C46 0.0361(14) 0.0655(18) 0.0362(13) -0.0018(11) 0.0018(10) 0.0085(12) O4A 0.0299(18) 0.053(2) 0.046(2) -0.0117(16) -0.0008(14) 0.0015(15) C47A 0.025(4) 0.035(5) 0.083(6) -0.015(3) 0.000(3) 0.006(3) C48A 0.063(4) 0.037(3) 0.024(2) 0.0063(19) 0.013(2) 0.009(3) O4B 0.097(4) 0.096(4) 0.052(3) -0.007(2) 0.020(2) 0.024(3) C47B 0.117(11) 0.049(6) 0.275(12) 0.004(8) -0.088(10) 0.018(6) C48B 0.048(5) 0.042(5) 0.030(3) -0.003(3) 0.010(3) -0.009(4) B1 0.0185(10) 0.0242(11) 0.0141(8) 0.0003(7) 0.0039(7) -0.0005(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 Co1 N1 1.8978(15) . ? Co1 O2 1.8981(12) . ? Co1 O1 1.8994(12) . ? Co1 N2 1.9015(15) . ? Co1 N5 1.9400(14) . ? Co1 N3 1.9408(14) . ? O1 C1 1.299(2) . ? O2 C8 1.300(2) . ? N1 C3 1.310(2) . ? N1 C4 1.458(2) . ? N2 C6 1.311(2) . ? N2 C5 1.470(2) . ? N3 C13 1.326(2) . ? N3 C15 1.380(2) . ? N4 C13 1.341(2) . ? N4 C14 1.365(2) . ? N4 C16 1.458(2) . ? N5 C17 1.323(2) . ? N5 C19 1.375(2) . ? N6 C17 1.340(2) . ? N6 C18 1.366(3) . ? N6 C20 1.466(2) . ? C1 C2 1.377(3) . ? C1 C9 1.498(3) . ? C2 C3 1.421(3) . ? C2 H2 0.9500 . ? C3 C10 1.505(3) . ? C4 C5 1.510(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.423(3) . ? C6 C11 1.503(3) . ? C7 C8 1.367(3) . ? C7 H7 0.9500 . ? C8 C12 1.506(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13 0.9500 . ? C14 C15 1.355(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17 0.9500 . ? C18 C19 1.356(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.407(2) . ? C21 C26 1.408(2) . ? C21 B1 1.643(3) . ? C22 C23 1.386(3) . ? C22 H22 0.9500 . ? C23 C24 1.390(3) . ? C23 H23 0.9500 . ? C24 C25 1.386(3) . ? C24 H24 0.9500 . ? C25 C26 1.383(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.400(2) . ? C27 C28 1.405(3) . ? C27 B1 1.638(3) . ? C28 C29 1.386(3) . ? C28 H28 0.9500 . ? C29 C30 1.384(3) . ? C29 H29 0.9500 . ? C30 C31 1.385(3) . ? C30 H30 0.9500 . ? C31 C32 1.395(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.390(3) . ? C33 C38 1.406(3) . ? C33 B1 1.640(3) . ? C34 C35 1.403(3) . ? C34 H34 0.9500 . ? C35 C36 1.380(3) . ? C35 H35 0.9500 . ? C36 C37 1.375(3) . ? C36 H36 0.9500 . ? C37 C38 1.393(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.399(3) . ? C39 C40 1.407(2) . ? C39 B1 1.647(3) . ? C40 C41 1.387(3) . ? C40 H40 0.9500 . ? C41 C42 1.386(3) . ? C41 H41 0.9500 . ? C42 C43 1.379(3) . ? C42 H42 0.9500 . ? C43 C44 1.393(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? O3 C45 1.421(3) . ? O3 H3 0.8400 . ? C45 C46 1.488(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? O4A C47A 1.464(11) . ? O4A H4OA 0.8400 . ? C47A C48A 1.372(9) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? O4B C47B 1.618(12) . ? O4B H4OB 0.8400 . ? C47B C48B 1.398(11) . ? C47B H47C 0.9900 . ? C47B H47D 0.9900 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? 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 177.43(6) . . ? N1 Co1 O1 94.79(6) . . ? O2 Co1 O1 83.47(5) . . ? N1 Co1 N2 86.58(6) . . ? O2 Co1 N2 95.20(6) . . ? O1 Co1 N2 178.11(6) . . ? N1 Co1 N5 87.88(6) . . ? O2 Co1 N5 90.23(6) . . ? O1 Co1 N5 90.27(6) . . ? N2 Co1 N5 91.08(6) . . ? N1 Co1 N3 91.48(6) . . ? O2 Co1 N3 90.41(6) . . ? O1 Co1 N3 89.51(6) . . ? N2 Co1 N3 89.15(6) . . ? N5 Co1 N3 179.30(6) . . ? C1 O1 Co1 124.76(12) . . ? C8 O2 Co1 124.40(11) . . ? C3 N1 C4 121.96(15) . . ? C3 N1 Co1 126.47(13) . . ? C4 N1 Co1 110.80(11) . . ? C6 N2 C5 121.51(15) . . ? C6 N2 Co1 126.19(12) . . ? C5 N2 Co1 111.86(11) . . ? C13 N3 C15 105.88(14) . . ? C13 N3 Co1 126.34(12) . . ? C15 N3 Co1 127.69(12) . . ? C13 N4 C14 107.74(14) . . ? C13 N4 C16 126.24(15) . . ? C14 N4 C16 125.98(14) . . ? C17 N5 C19 106.09(15) . . ? C17 N5 Co1 128.11(13) . . ? C19 N5 Co1 125.61(12) . . ? C17 N6 C18 107.05(15) . . ? C17 N6 C20 126.28(16) . . ? C18 N6 C20 126.61(15) . . ? O1 C1 C2 125.27(17) . . ? O1 C1 C9 114.38(16) . . ? C2 C1 C9 120.32(16) . . ? C1 C2 C3 125.73(17) . . ? C1 C2 H2 117.1 . . ? C3 C2 H2 117.1 . . ? N1 C3 C2 122.12(17) . . ? N1 C3 C10 120.30(17) . . ? C2 C3 C10 117.58(17) . . ? N1 C4 C5 108.43(14) . . ? N1 C4 H4A 110.0 . . ? C5 C4 H4A 110.0 . . ? N1 C4 H4B 110.0 . . ? C5 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? N2 C5 C4 107.32(14) . . ? N2 C5 H5A 110.3 . . ? C4 C5 H5A 110.3 . . ? N2 C5 H5B 110.3 . . ? C4 C5 H5B 110.3 . . ? H5A C5 H5B 108.5 . . ? N2 C6 C7 121.96(16) . . ? N2 C6 C11 120.86(16) . . ? C7 C6 C11 117.17(16) . . ? C8 C7 C6 126.22(17) . . ? C8 C7 H7 116.9 . . ? C6 C7 H7 116.9 . . ? O2 C8 C7 125.61(16) . . ? O2 C8 C12 113.95(15) . . ? C7 C8 C12 120.42(16) . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3 C10 H10A 109.5 . . ? C3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 N4 110.76(15) . . ? N3 C13 H13 124.6 . . ? N4 C13 H13 124.6 . . ? C15 C14 N4 106.52(15) . . ? C15 C14 H14 126.7 . . ? N4 C14 H14 126.7 . . ? C14 C15 N3 109.09(16) . . ? C14 C15 H15 125.5 . . ? N3 C15 H15 125.5 . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 N6 111.11(16) . . ? N5 C17 H17 124.4 . . ? N6 C17 H17 124.4 . . ? C19 C18 N6 107.02(16) . . ? C19 C18 H18 126.5 . . ? N6 C18 H18 126.5 . . ? C18 C19 N5 108.71(17) . . ? C18 C19 H19 125.6 . . ? N5 C19 H19 125.6 . . ? N6 C20 H20A 109.5 . . ? N6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 114.70(17) . . ? C22 C21 B1 123.86(16) . . ? C26 C21 B1 121.25(15) . . ? C23 C22 C21 122.89(18) . . ? C23 C22 H22 118.6 . . ? C21 C22 H22 118.6 . . ? C22 C23 C24 120.24(18) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 118.78(18) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C26 C25 C24 120.18(18) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C21 123.18(17) . . ? C25 C26 H26 118.4 . . ? C21 C26 H26 118.4 . . ? C32 C27 C28 114.76(16) . . ? C32 C27 B1 124.28(16) . . ? C28 C27 B1 120.57(15) . . ? C29 C28 C27 122.99(17) . . ? C29 C28 H28 118.5 . . ? C27 C28 H28 118.5 . . ? C30 C29 C28 120.38(18) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 118.77(17) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C30 C31 C32 120.02(17) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C27 123.07(17) . . ? C31 C32 H32 118.5 . . ? C27 C32 H32 118.5 . . ? C34 C33 C38 114.83(17) . . ? C34 C33 B1 123.68(16) . . ? C38 C33 B1 121.28(17) . . ? C33 C34 C35 122.9(2) . . ? C33 C34 H34 118.5 . . ? C35 C34 H34 118.5 . . ? C36 C35 C34 120.2(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 118.81(19) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C36 C37 C38 120.4(2) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C33 122.9(2) . . ? C37 C38 H38 118.6 . . ? C33 C38 H38 118.6 . . ? C44 C39 C40 114.42(16) . . ? C44 C39 B1 122.18(16) . . ? C40 C39 B1 122.99(16) . . ? C41 C40 C39 123.16(18) . . ? C41 C40 H40 118.4 . . ? C39 C40 H40 118.4 . . ? C42 C41 C40 120.21(18) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 118.73(18) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C42 C43 C44 120.23(18) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 123.24(17) . . ? C43 C44 H44 118.4 . . ? C39 C44 H44 118.4 . . ? C45 O3 H3 109.5 . . ? O3 C45 C46 112.1(2) . . ? O3 C45 H45A 109.2 . . ? C46 C45 H45A 109.2 . . ? O3 C45 H45B 109.2 . . ? C46 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48A C47A O4A 112.9(9) . . ? C48A C47A H47A 109.0 . . ? O4A C47A H47A 109.0 . . ? C48A C47A H47B 109.0 . . ? O4A C47A H47B 109.0 . . ? H47A C47A H47B 107.8 . . ? C47B O4B H4OB 109.5 . . ? C48B C47B O4B 96.5(9) . . ? C48B C47B H47C 112.4 . . ? O4B C47B H47C 112.4 . . ? C48B C47B H47D 112.4 . . ? O4B C47B H47D 112.4 . . ? H47C C47B H47D 110.0 . . ? C47B C48B H48D 109.5 . . ? C47B C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C47B C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C27 B1 C33 112.06(15) . . ? C27 B1 C21 104.43(14) . . ? C33 B1 C21 111.55(14) . . ? C27 B1 C39 114.06(14) . . ? C33 B1 C39 104.40(14) . . ? C21 B1 C39 110.53(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 O1 C1 9.05(13) . . . . ? O2 Co1 O1 C1 -172.86(13) . . . . ? N2 Co1 O1 C1 -127.4(17) . . . . ? N5 Co1 O1 C1 96.94(13) . . . . ? N3 Co1 O1 C1 -82.39(13) . . . . ? N1 Co1 O2 C8 -128.6(12) . . . . ? O1 Co1 O2 C8 -176.14(13) . . . . ? N2 Co1 O2 C8 5.21(13) . . . . ? N5 Co1 O2 C8 -85.89(13) . . . . ? N3 Co1 O2 C8 94.40(13) . . . . ? O2 Co1 N1 C3 -51.2(13) . . . . ? O1 Co1 N1 C3 -3.84(15) . . . . ? N2 Co1 N1 C3 174.85(15) . . . . ? N5 Co1 N1 C3 -93.94(15) . . . . ? N3 Co1 N1 C3 85.79(15) . . . . ? O2 Co1 N1 C4 118.8(12) . . . . ? O1 Co1 N1 C4 166.17(11) . . . . ? N2 Co1 N1 C4 -15.13(11) . . . . ? N5 Co1 N1 C4 76.08(11) . . . . ? N3 Co1 N1 C4 -104.19(11) . . . . ? N1 Co1 N2 C6 178.42(15) . . . . ? O2 Co1 N2 C6 0.28(15) . . . . ? O1 Co1 N2 C6 -45.0(18) . . . . ? N5 Co1 N2 C6 90.61(15) . . . . ? N3 Co1 N2 C6 -90.05(15) . . . . ? N1 Co1 N2 C5 -9.15(11) . . . . ? O2 Co1 N2 C5 172.71(11) . . . . ? O1 Co1 N2 C5 127.4(17) . . . . ? N5 Co1 N2 C5 -96.96(12) . . . . ? N3 Co1 N2 C5 82.38(12) . . . . ? N1 Co1 N3 C13 152.32(15) . . . . ? O2 Co1 N3 C13 -29.43(15) . . . . ? O1 Co1 N3 C13 -112.90(15) . . . . ? N2 Co1 N3 C13 65.76(15) . . . . ? N5 Co1 N3 C13 175(100) . . . . ? N1 Co1 N3 C15 -31.40(16) . . . . ? O2 Co1 N3 C15 146.85(16) . . . . ? O1 Co1 N3 C15 63.38(16) . . . . ? N2 Co1 N3 C15 -117.95(16) . . . . ? N5 Co1 N3 C15 -8(5) . . . . ? N1 Co1 N5 C17 -119.27(16) . . . . ? O2 Co1 N5 C17 62.48(16) . . . . ? O1 Co1 N5 C17 145.95(16) . . . . ? N2 Co1 N5 C17 -32.73(16) . . . . ? N3 Co1 N5 C17 -142(5) . . . . ? N1 Co1 N5 C19 54.94(15) . . . . ? O2 Co1 N5 C19 -123.32(15) . . . . ? O1 Co1 N5 C19 -39.85(15) . . . . ? N2 Co1 N5 C19 141.47(15) . . . . ? N3 Co1 N5 C19 32(5) . . . . ? Co1 O1 C1 C2 -7.5(2) . . . . ? Co1 O1 C1 C9 174.50(11) . . . . ? O1 C1 C2 C3 -2.0(3) . . . . ? C9 C1 C2 C3 175.84(17) . . . . ? C4 N1 C3 C2 -172.13(16) . . . . ? Co1 N1 C3 C2 -3.1(2) . . . . ? C4 N1 C3 C10 8.4(3) . . . . ? Co1 N1 C3 C10 177.36(14) . . . . ? C1 C2 C3 N1 7.8(3) . . . . ? C1 C2 C3 C10 -172.74(18) . . . . ? C3 N1 C4 C5 -154.23(16) . . . . ? Co1 N1 C4 C5 35.23(16) . . . . ? C6 N2 C5 C4 -157.11(16) . . . . ? Co1 N2 C5 C4 30.06(17) . . . . ? N1 C4 C5 N2 -41.64(18) . . . . ? C5 N2 C6 C7 -176.49(15) . . . . ? Co1 N2 C6 C7 -4.7(2) . . . . ? C5 N2 C6 C11 4.9(2) . . . . ? Co1 N2 C6 C11 176.66(12) . . . . ? N2 C6 C7 C8 4.9(3) . . . . ? C11 C6 C7 C8 -176.46(16) . . . . ? Co1 O2 C8 C7 -6.5(2) . . . . ? Co1 O2 C8 C12 174.79(11) . . . . ? C6 C7 C8 O2 1.2(3) . . . . ? C6 C7 C8 C12 179.80(16) . . . . ? C15 N3 C13 N4 -0.36(19) . . . . ? Co1 N3 C13 N4 176.58(11) . . . . ? C14 N4 C13 N3 0.6(2) . . . . ? C16 N4 C13 N3 178.34(16) . . . . ? C13 N4 C14 C15 -0.6(2) . . . . ? C16 N4 C14 C15 -178.33(17) . . . . ? N4 C14 C15 N3 0.4(2) . . . . ? C13 N3 C15 C14 0.0(2) . . . . ? Co1 N3 C15 C14 -176.90(13) . . . . ? C19 N5 C17 N6 1.3(2) . . . . ? Co1 N5 C17 N6 176.37(12) . . . . ? C18 N6 C17 N5 -1.5(2) . . . . ? C20 N6 C17 N5 -179.07(17) . . . . ? C17 N6 C18 C19 1.1(2) . . . . ? C20 N6 C18 C19 178.66(18) . . . . ? N6 C18 C19 N5 -0.4(2) . . . . ? C17 N5 C19 C18 -0.5(2) . . . . ? Co1 N5 C19 C18 -175.80(13) . . . . ? C26 C21 C22 C23 1.9(3) . . . . ? B1 C21 C22 C23 176.99(18) . . . . ? C21 C22 C23 C24 -0.6(3) . . . . ? C22 C23 C24 C25 -0.9(3) . . . . ? C23 C24 C25 C26 0.8(3) . . . . ? C24 C25 C26 C21 0.7(3) . . . . ? C22 C21 C26 C25 -2.0(3) . . . . ? B1 C21 C26 C25 -177.19(17) . . . . ? C32 C27 C28 C29 1.0(3) . . . . ? B1 C27 C28 C29 -172.14(17) . . . . ? C27 C28 C29 C30 0.1(3) . . . . ? C28 C29 C30 C31 -0.7(3) . . . . ? C29 C30 C31 C32 0.3(3) . . . . ? C30 C31 C32 C27 0.9(3) . . . . ? C28 C27 C32 C31 -1.4(3) . . . . ? B1 C27 C32 C31 171.39(17) . . . . ? C38 C33 C34 C35 0.9(3) . . . . ? B1 C33 C34 C35 -173.76(18) . . . . ? C33 C34 C35 C36 -0.4(3) . . . . ? C34 C35 C36 C37 -1.1(3) . . . . ? C35 C36 C37 C38 1.9(3) . . . . ? C36 C37 C38 C33 -1.4(3) . . . . ? C34 C33 C38 C37 -0.1(3) . . . . ? B1 C33 C38 C37 174.79(18) . . . . ? C44 C39 C40 C41 -0.6(3) . . . . ? B1 C39 C40 C41 172.24(17) . . . . ? C39 C40 C41 C42 0.5(3) . . . . ? C40 C41 C42 C43 0.1(3) . . . . ? C41 C42 C43 C44 -0.5(3) . . . . ? C42 C43 C44 C39 0.3(3) . . . . ? C40 C39 C44 C43 0.2(3) . . . . ? B1 C39 C44 C43 -172.72(17) . . . . ? C32 C27 B1 C33 143.86(17) . . . . ? C28 C27 B1 C33 -43.7(2) . . . . ? C32 C27 B1 C21 -95.24(19) . . . . ? C28 C27 B1 C21 77.16(19) . . . . ? C32 C27 B1 C39 25.5(2) . . . . ? C28 C27 B1 C39 -162.08(16) . . . . ? C34 C33 B1 C27 -29.0(2) . . . . ? C38 C33 B1 C27 156.65(17) . . . . ? C34 C33 B1 C21 -145.66(18) . . . . ? C38 C33 B1 C21 40.0(2) . . . . ? C34 C33 B1 C39 95.0(2) . . . . ? C38 C33 B1 C39 -79.4(2) . . . . ? C22 C21 B1 C27 -93.39(19) . . . . ? C26 C21 B1 C27 81.4(2) . . . . ? C22 C21 B1 C33 27.8(2) . . . . ? C26 C21 B1 C33 -157.38(16) . . . . ? C22 C21 B1 C39 143.53(17) . . . . ? C26 C21 B1 C39 -41.7(2) . . . . ? C44 C39 B1 C27 -147.67(17) . . . . ? C40 C39 B1 C27 40.0(2) . . . . ? C44 C39 B1 C33 89.69(19) . . . . ? C40 C39 B1 C33 -82.6(2) . . . . ? C44 C39 B1 C21 -30.4(2) . . . . ? C40 C39 B1 C21 157.34(16) . . . . ? 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 O3 H3 O2 0.84 2.04 2.816(2) 152.6 1_645 O3 H3 O1 0.84 2.42 3.102(2) 139.0 1_645 O4A H4OA O3 0.84 2.14 2.952(4) 163.9 . O4B H4OB O3 0.84 1.84 2.659(5) 165.4 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.032 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.071 data_Co(acacen)(2MeIm)2 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C20 H28 N6 O2 Co), 2Cl, 1.75(H2 O), 0.6(C2 H6 O)' _chemical_formula_sum 'C41.20 H63.10 Cl2 Co2 N12 O6.35' _chemical_formula_weight 1016.90 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.8162(9) _cell_length_b 11.6873(4) _cell_length_c 16.9470(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.328(2) _cell_angle_gamma 90.00 _cell_volume 4835.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4635 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 24.91 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2132 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7070 _exptl_absorpt_correction_T_max 0.9699 _exptl_absorpt_process_details 'face-indexed' _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41559 _diffrn_reflns_av_R_equivalents 0.1431 _diffrn_reflns_av_sigmaI/netI 0.1293 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.83 _diffrn_reflns_theta_max 27.58 _reflns_number_total 10981 _reflns_number_gt 5642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2.1-4 (Bruker, 2007)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There are several disordered solvent molecules and anions in the lattice. The two independent chloride anions are disordered over 2 and 3 unique positions. Additionally, there are three partially occupied water molecules and one partially occupied ethanol molecule in the lattice. Hydrogen atoms for the water molecules could not be found from residual electron density and were not included in the refinement. ; _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^)+(0.0667P)^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 10981 _refine_ls_number_parameters 645 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _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 0.41699(2) 0.56279(4) 0.24335(3) 0.02631(15) Uani 1 1 d . . . O1 O 0.40284(12) 0.4347(2) 0.30610(15) 0.0279(6) Uani 1 1 d . . . O2 O 0.44578(11) 0.4534(2) 0.17883(15) 0.0276(6) Uani 1 1 d . . . N1 N 0.38778(15) 0.6732(3) 0.3076(2) 0.0325(9) Uani 1 1 d . . . N2 N 0.43126(14) 0.6884(3) 0.18017(19) 0.0291(8) Uani 1 1 d . . . N3 N 0.48881(14) 0.5790(3) 0.31292(18) 0.0277(8) Uani 1 1 d . . . N4 N 0.57666(15) 0.5831(3) 0.3670(2) 0.0313(9) Uani 1 1 d . . . N5 N 0.34461(14) 0.5442(3) 0.17498(18) 0.0282(8) Uani 1 1 d . . . N6 N 0.27184(17) 0.4767(3) 0.0951(2) 0.0449(11) Uani 1 1 d . . . C1 C 0.37277(17) 0.4397(4) 0.3613(2) 0.0300(10) Uani 1 1 d . . . C2 C 0.35175(17) 0.5370(4) 0.3893(2) 0.0327(10) Uani 1 1 d . . . H2A H 0.3300 0.5274 0.4296 0.039 Uiso 1 1 calc R . . C3 C 0.35931(18) 0.6499(4) 0.3640(3) 0.0338(11) Uani 1 1 d . . . C4 C 0.36156(19) 0.3242(4) 0.3953(2) 0.0373(11) Uani 1 1 d . . . H4A H 0.3964 0.2861 0.4162 0.056 Uiso 1 1 calc R . . H4B H 0.3403 0.2771 0.3529 0.056 Uiso 1 1 calc R . . H4C H 0.3408 0.3346 0.4387 0.056 Uiso 1 1 calc R . . C5 C 0.3332(2) 0.7463(4) 0.4036(3) 0.0466(13) Uani 1 1 d . . . H5A H 0.3617 0.7996 0.4287 0.070 Uiso 1 1 calc R . . H5B H 0.3141 0.7148 0.4446 0.070 Uiso 1 1 calc R . . H5C H 0.3070 0.7869 0.3631 0.070 Uiso 1 1 calc R . . C6 C 0.3954(2) 0.7933(4) 0.2839(3) 0.0422(12) Uani 1 1 d . . . H6A H 0.4100 0.8395 0.3320 0.051 Uiso 1 1 calc R . . H6B H 0.3597 0.8263 0.2585 0.051 Uiso 1 1 calc R . . C7 C 0.43501(19) 0.7967(3) 0.2253(3) 0.0367(11) Uani 1 1 d . . . H7A H 0.4258 0.8616 0.1877 0.044 Uiso 1 1 calc R . . H7B H 0.4728 0.8077 0.2548 0.044 Uiso 1 1 calc R . . C8 C 0.43804(18) 0.6820(3) 0.1061(2) 0.0310(10) Uani 1 1 d . . . C9 C 0.43893(19) 0.5758(3) 0.0657(2) 0.0334(10) Uani 1 1 d . . . H9A H 0.4353 0.5771 0.0089 0.040 Uiso 1 1 calc R . . C10 C 0.44475(18) 0.4708(3) 0.1034(2) 0.0296(10) Uani 1 1 d . . . C11 C 0.4473(2) 0.7892(4) 0.0606(3) 0.0443(12) Uani 1 1 d . . . H11A H 0.4794 0.8300 0.0895 0.066 Uiso 1 1 calc R . . H11B H 0.4150 0.8387 0.0560 0.066 Uiso 1 1 calc R . . H11C H 0.4535 0.7686 0.0069 0.066 Uiso 1 1 calc R . . C12 C 0.4519(2) 0.3636(4) 0.0568(2) 0.0393(11) Uani 1 1 d . . . H12A H 0.4848 0.3228 0.0831 0.059 Uiso 1 1 calc R . . H12B H 0.4559 0.3841 0.0021 0.059 Uiso 1 1 calc R . . H12C H 0.4198 0.3143 0.0550 0.059 Uiso 1 1 calc R . . C13 C 0.49377(18) 0.5689(3) 0.3949(2) 0.0288(9) Uani 1 1 d . . . H13A H 0.4643 0.5616 0.4234 0.035 Uiso 1 1 calc R . . C14 C 0.54762(19) 0.5712(3) 0.4282(2) 0.0323(10) Uani 1 1 d . . . H14A H 0.5625 0.5656 0.4838 0.039 Uiso 1 1 calc R . . C15 C 0.53968(18) 0.5877(3) 0.2974(2) 0.0287(10) Uani 1 1 d . . . C16 C 0.55761(19) 0.6057(4) 0.2199(2) 0.0369(11) Uani 1 1 d . . . H16A H 0.5348 0.5597 0.1784 0.055 Uiso 1 1 calc R . . H16B H 0.5960 0.5824 0.2246 0.055 Uiso 1 1 calc R . . H16C H 0.5540 0.6868 0.2053 0.055 Uiso 1 1 calc R . . C17 C 0.31141(18) 0.6347(4) 0.1424(2) 0.0351(11) Uani 1 1 d . . . H17A H 0.3192 0.7134 0.1529 0.042 Uiso 1 1 calc R . . C18 C 0.2666(2) 0.5938(4) 0.0939(3) 0.0454(13) Uani 1 1 d . . . H18A H 0.2373 0.6372 0.0647 0.054 Uiso 1 1 calc R . . C19 C 0.31879(18) 0.4497(3) 0.1449(2) 0.0327(10) Uani 1 1 d . . . C20 C 0.33499(19) 0.3270(3) 0.1604(3) 0.0365(11) Uani 1 1 d . . . H20A H 0.3746 0.3223 0.1793 0.055 Uiso 1 1 calc R . . H20B H 0.3251 0.2830 0.1107 0.055 Uiso 1 1 calc R . . H20C H 0.3158 0.2956 0.2013 0.055 Uiso 1 1 calc R . . Co2 Co 0.09771(2) 0.59565(5) 0.33958(3) 0.02940(16) Uani 1 1 d . . . O3 O 0.07597(11) 0.6141(3) 0.22663(16) 0.0320(7) Uani 1 1 d . . . O4 O 0.03123(12) 0.6718(2) 0.34510(16) 0.0333(7) Uani 1 1 d . . . N7 N 0.16332(14) 0.5194(3) 0.3328(2) 0.0313(8) Uani 1 1 d . . . N8 N 0.11923(15) 0.5804(3) 0.4514(2) 0.0349(9) Uani 1 1 d . . . N9 N 0.13361(15) 0.7457(3) 0.3499(2) 0.0387(10) Uani 1 1 d . . . N10 N 0.18567(17) 0.8973(3) 0.3436(2) 0.0425(10) Uani 1 1 d . . . N11 N 0.06107(14) 0.4450(3) 0.33621(18) 0.0288(8) Uani 1 1 d . . . N12 N 0.00750(14) 0.2961(3) 0.30946(19) 0.0307(8) Uani 1 1 d . . . C21 C 0.09390(18) 0.5474(4) 0.1752(2) 0.0325(10) Uani 1 1 d . . . C22 C 0.13725(18) 0.4729(4) 0.1935(3) 0.0369(11) Uani 1 1 d . . . H22A H 0.1440 0.4222 0.1525 0.044 Uiso 1 1 calc R . . C23 C 0.17313(19) 0.4663(4) 0.2702(3) 0.0385(11) Uani 1 1 d . . . C24 C 0.0647(2) 0.5588(4) 0.0901(2) 0.0409(11) Uani 1 1 d . . . H24A H 0.0634 0.6396 0.0745 0.061 Uiso 1 1 calc R . . H24B H 0.0274 0.5290 0.0854 0.061 Uiso 1 1 calc R . . H24C H 0.0844 0.5152 0.0549 0.061 Uiso 1 1 calc R . . C25 C 0.2247(2) 0.3976(5) 0.2727(3) 0.0597(16) Uani 1 1 d . . . H25A H 0.2279 0.3412 0.3160 0.089 Uiso 1 1 calc R . . H25B H 0.2565 0.4489 0.2823 0.089 Uiso 1 1 calc R . . H25C H 0.2234 0.3582 0.2214 0.089 Uiso 1 1 calc R . . C26 C 0.20262(19) 0.5202(4) 0.4091(3) 0.0452(13) Uani 1 1 d . . . H26A H 0.2192 0.4433 0.4188 0.054 Uiso 1 1 calc R . . H26B H 0.2323 0.5753 0.4053 0.054 Uiso 1 1 calc R . . C27 C 0.1762(2) 0.5517(6) 0.4765(3) 0.0698(19) Uani 1 1 d . . . H27A H 0.1793 0.4870 0.5148 0.084 Uiso 1 1 calc R . . H27B H 0.1957 0.6180 0.5048 0.084 Uiso 1 1 calc R . . C28 C 0.0871(2) 0.5943(4) 0.5041(3) 0.0389(11) Uani 1 1 d . . . C29 C 0.0320(2) 0.6319(4) 0.4823(2) 0.0378(11) Uani 1 1 d . . . H29A H 0.0097 0.6295 0.5224 0.045 Uiso 1 1 calc R . . C30 C 0.00854(19) 0.6712(4) 0.4080(3) 0.0351(11) Uani 1 1 d . . . C31 C 0.1079(3) 0.5731(6) 0.5920(3) 0.0680(18) Uani 1 1 d . . . H31A H 0.1276 0.5000 0.5987 0.102 Uiso 1 1 calc R . . H31B H 0.0769 0.5705 0.6205 0.102 Uiso 1 1 calc R . . H31C H 0.1328 0.6350 0.6138 0.102 Uiso 1 1 calc R . . C32 C -0.0482(2) 0.7211(5) 0.3941(3) 0.0480(13) Uani 1 1 d . . . H32A H -0.0468 0.8009 0.3769 0.072 Uiso 1 1 calc R . . H32B H -0.0630 0.7178 0.4439 0.072 Uiso 1 1 calc R . . H32C H -0.0719 0.6771 0.3524 0.072 Uiso 1 1 calc R . . C33 C 0.1237(2) 0.8270(4) 0.4087(3) 0.0376(11) Uani 1 1 d . . . H33A H 0.0988 0.8171 0.4447 0.045 Uiso 1 1 calc R . . C34 C 0.1546(2) 0.9175(4) 0.4052(3) 0.0498(14) Uani 1 1 d . . . H34A H 0.1559 0.9841 0.4376 0.060 Uiso 1 1 calc R . . C35 C 0.1710(2) 0.7934(4) 0.3150(3) 0.0440(13) Uani 1 1 d . . . C36 C 0.1970(2) 0.7435(5) 0.2508(3) 0.0504(13) Uani 1 1 d . . . H36A H 0.1693 0.7038 0.2120 0.076 Uiso 1 1 calc R . . H36B H 0.2254 0.6890 0.2743 0.076 Uiso 1 1 calc R . . H36C H 0.2136 0.8046 0.2236 0.076 Uiso 1 1 calc R . . C37 C 0.08539(18) 0.3512(4) 0.3790(2) 0.0304(10) Uani 1 1 d . . . H37A H 0.1198 0.3520 0.4142 0.036 Uiso 1 1 calc R . . C38 C 0.05295(18) 0.2601(4) 0.3631(2) 0.0326(10) Uani 1 1 d . . . H38A H 0.0597 0.1852 0.3844 0.039 Uiso 1 1 calc R . . C39 C 0.01364(17) 0.4081(4) 0.2943(2) 0.0277(9) Uani 1 1 d . . . C40 C -0.02801(18) 0.4731(4) 0.2378(2) 0.0346(11) Uani 1 1 d . . . H40A H -0.0647 0.4463 0.2426 0.052 Uiso 1 1 calc R . . H40B H -0.0221 0.4610 0.1828 0.052 Uiso 1 1 calc R . . H40C H -0.0247 0.5548 0.2508 0.052 Uiso 1 1 calc R . . Cl1 Cl 0.3112(5) 0.5351(8) 0.6041(6) 0.049(2) Uani 0.50 1 d P A 1 Cl2 Cl 0.17580(10) 0.3054(2) 0.02913(15) 0.0634(7) Uani 0.60 1 d P B 1 Cl3 Cl 0.3042(7) 0.5122(12) 0.6193(10) 0.055(3) Uani 0.40 1 d P C 2 Cl3' Cl 0.3005(9) 0.461(2) 0.5752(12) 0.080(7) Uani 0.10 1 d P D 3 Cl4 Cl 0.20053(16) 0.3073(3) -0.02573(18) 0.0535(10) Uani 0.40 1 d P E 2 O1W O 0.2062(3) 0.3512(6) -0.3661(4) 0.0767(19) Uani 0.70 1 d P F 1 O1O O 0.2269(6) 0.3871(10) -0.3281(6) 0.045(4) Uani 0.30 1 d P G 2 O2W O 0.1585(3) 0.3485(7) -0.2373(4) 0.065(2) Uani 0.50 1 d P . . O3W O 0.3416(6) 0.4508(12) -0.0758(8) 0.059(4) Uani 0.25 1 d P . . O1S O 0.2433(4) 0.3255(8) -0.1086(7) 0.128(4) Uani 0.60 1 d P H 1 H1SO H 0.2124 0.3322 -0.0954 0.154 Uiso 0.60 1 calc PR H 1 C1S C 0.2508(5) 0.4215(8) -0.1706(5) 0.080(4) Uani 0.60 1 d P H 1 H1SA H 0.2396 0.3761 -0.2202 0.096 Uiso 0.60 1 calc PR H 1 H1SB H 0.2177 0.4668 -0.1665 0.096 Uiso 0.60 1 calc PR H 1 C2S C 0.2818(4) 0.5134(8) -0.2055(6) 0.061(3) Uani 0.60 1 d P H 1 H2SA H 0.2699 0.5886 -0.1897 0.091 Uiso 0.60 1 calc PR H 1 H2SB H 0.2746 0.5072 -0.2641 0.091 Uiso 0.60 1 calc PR H 1 H2SC H 0.3211 0.5042 -0.1854 0.091 Uiso 0.60 1 calc PR H 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0274(3) 0.0140(3) 0.0327(3) -0.0022(2) -0.0074(2) 0.0009(2) O1 0.0278(16) 0.0202(15) 0.0325(14) -0.0011(12) -0.0030(12) -0.0013(12) O2 0.0319(17) 0.0170(14) 0.0305(14) 0.0004(11) -0.0036(12) 0.0013(12) N1 0.034(2) 0.0176(18) 0.040(2) -0.0076(15) -0.0117(17) 0.0055(16) N2 0.031(2) 0.0140(17) 0.0370(19) -0.0015(14) -0.0094(16) -0.0010(15) N3 0.030(2) 0.0158(18) 0.0330(17) -0.0024(13) -0.0069(15) 0.0017(15) N4 0.032(2) 0.0168(18) 0.0390(19) 0.0014(14) -0.0095(16) -0.0040(15) N5 0.029(2) 0.0187(18) 0.0332(17) -0.0022(14) -0.0054(15) 0.0000(15) N6 0.043(2) 0.026(2) 0.054(2) 0.0041(17) -0.0214(19) -0.0026(18) C1 0.025(2) 0.030(2) 0.030(2) -0.0019(18) -0.0075(18) -0.0004(19) C2 0.022(2) 0.038(3) 0.035(2) -0.0045(19) -0.0033(18) 0.000(2) C3 0.026(2) 0.032(2) 0.038(2) -0.010(2) -0.009(2) 0.003(2) C4 0.037(3) 0.037(3) 0.035(2) 0.0012(19) -0.003(2) -0.004(2) C5 0.033(3) 0.042(3) 0.062(3) -0.018(2) 0.000(2) 0.007(2) C6 0.048(3) 0.019(2) 0.053(3) -0.009(2) -0.008(2) 0.003(2) C7 0.042(3) 0.012(2) 0.050(3) -0.0050(18) -0.011(2) -0.0003(19) C8 0.029(2) 0.018(2) 0.041(2) 0.0053(18) -0.0068(19) -0.0021(18) C9 0.040(3) 0.023(2) 0.033(2) 0.0039(17) -0.0046(19) -0.005(2) C10 0.032(2) 0.019(2) 0.034(2) -0.0026(17) -0.0037(18) -0.0025(18) C11 0.054(3) 0.024(2) 0.052(3) 0.008(2) 0.000(2) -0.003(2) C12 0.054(3) 0.024(2) 0.039(2) -0.0059(19) 0.006(2) -0.003(2) C13 0.034(2) 0.016(2) 0.033(2) -0.0014(16) -0.0044(18) -0.0021(18) C14 0.040(3) 0.016(2) 0.035(2) 0.0016(17) -0.010(2) -0.0037(19) C15 0.030(2) 0.015(2) 0.038(2) -0.0021(16) -0.0024(18) -0.0005(18) C16 0.033(3) 0.031(2) 0.044(2) -0.003(2) 0.000(2) -0.002(2) C17 0.032(3) 0.020(2) 0.049(2) 0.0001(19) -0.006(2) 0.0020(19) C18 0.037(3) 0.026(2) 0.061(3) 0.004(2) -0.023(2) 0.002(2) C19 0.036(3) 0.019(2) 0.038(2) -0.0017(18) -0.0092(19) -0.0027(19) C20 0.038(3) 0.021(2) 0.044(2) -0.0014(19) -0.008(2) -0.001(2) Co2 0.0223(3) 0.0258(3) 0.0358(3) 0.0081(2) -0.0065(2) -0.0047(2) O3 0.0240(16) 0.0352(17) 0.0351(15) 0.0097(13) 0.0004(12) 0.0025(13) O4 0.0283(17) 0.0298(17) 0.0374(16) 0.0032(13) -0.0061(13) -0.0015(13) N7 0.025(2) 0.0283(19) 0.0371(19) 0.0098(16) -0.0040(16) -0.0019(16) N8 0.030(2) 0.029(2) 0.040(2) 0.0053(16) -0.0105(17) -0.0023(17) N9 0.031(2) 0.032(2) 0.048(2) 0.0126(18) -0.0088(18) -0.0013(18) N10 0.040(2) 0.029(2) 0.053(2) 0.0064(18) -0.0052(19) -0.0052(19) N11 0.0257(19) 0.0254(18) 0.0323(17) 0.0046(15) -0.0025(15) -0.0044(16) N12 0.028(2) 0.027(2) 0.0363(18) -0.0013(15) 0.0021(15) -0.0046(16) C21 0.026(2) 0.031(2) 0.038(2) 0.0115(19) 0.0008(19) -0.005(2) C22 0.030(3) 0.031(3) 0.048(3) 0.004(2) 0.000(2) -0.003(2) C23 0.030(3) 0.023(2) 0.059(3) 0.010(2) -0.002(2) -0.003(2) C24 0.041(3) 0.044(3) 0.038(2) 0.007(2) 0.008(2) 0.005(2) C25 0.052(4) 0.045(3) 0.072(3) -0.009(3) -0.013(3) 0.019(3) C26 0.030(3) 0.043(3) 0.054(3) 0.007(2) -0.016(2) 0.000(2) C27 0.036(3) 0.122(6) 0.044(3) 0.001(3) -0.013(2) 0.011(3) C28 0.045(3) 0.032(3) 0.036(2) 0.002(2) -0.001(2) -0.005(2) C29 0.043(3) 0.032(3) 0.036(2) 0.0013(19) 0.002(2) -0.005(2) C30 0.036(3) 0.026(2) 0.041(2) -0.0052(19) 0.002(2) -0.010(2) C31 0.072(4) 0.092(5) 0.037(3) 0.011(3) 0.000(3) 0.012(4) C32 0.039(3) 0.050(3) 0.053(3) -0.006(2) 0.002(2) 0.000(2) C33 0.036(3) 0.034(3) 0.040(2) 0.002(2) 0.000(2) -0.001(2) C34 0.048(3) 0.038(3) 0.055(3) 0.001(2) -0.015(3) 0.001(2) C35 0.035(3) 0.041(3) 0.051(3) 0.018(2) -0.008(2) -0.004(2) C36 0.056(4) 0.051(3) 0.043(3) 0.005(2) 0.006(2) -0.003(3) C37 0.028(2) 0.027(2) 0.033(2) 0.0090(18) -0.0027(18) -0.0043(19) C38 0.031(2) 0.025(2) 0.039(2) 0.0058(18) 0.0001(19) -0.0024(19) C39 0.026(2) 0.027(2) 0.0282(19) 0.0003(17) 0.0006(17) -0.0042(18) C40 0.029(2) 0.034(3) 0.036(2) 0.0027(19) -0.0049(19) -0.005(2) Cl1 0.026(3) 0.044(4) 0.071(4) -0.018(4) -0.009(3) 0.004(3) Cl2 0.0597(16) 0.0612(16) 0.0669(15) -0.0290(12) 0.0046(12) -0.0299(13) Cl3 0.028(4) 0.040(4) 0.093(6) 0.014(3) -0.003(4) 0.001(3) Cl3' 0.052(11) 0.11(2) 0.073(13) 0.032(11) 0.008(10) 0.023(13) Cl4 0.082(3) 0.0292(16) 0.0375(16) 0.0035(13) -0.0209(17) -0.0212(16) O1W 0.072(5) 0.054(4) 0.107(6) 0.006(4) 0.023(4) 0.003(4) O1O 0.074(10) 0.029(6) 0.021(5) -0.013(4) -0.019(5) 0.017(6) O2W 0.069(6) 0.050(5) 0.083(5) 0.006(4) 0.030(4) 0.015(4) O3W 0.055(9) 0.041(8) 0.066(9) -0.011(7) -0.029(7) 0.013(7) O1S 0.077(6) 0.115(8) 0.212(10) -0.091(8) 0.079(7) -0.043(6) C1S 0.154(12) 0.051(6) 0.031(4) -0.004(4) 0.007(5) 0.075(7) C2S 0.066(7) 0.041(5) 0.086(6) -0.041(5) 0.045(5) -0.023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.888(3) . ? Co1 O2 1.903(3) . ? Co1 O1 1.905(3) . ? Co1 N1 1.913(4) . ? Co1 N3 1.962(3) . ? Co1 N5 1.967(3) . ? O1 C1 1.298(5) . ? O2 C10 1.291(5) . ? N1 C3 1.314(6) . ? N1 C6 1.482(5) . ? N2 C8 1.299(5) . ? N2 C7 1.472(5) . ? N3 C15 1.338(5) . ? N3 C13 1.378(5) . ? N4 C15 1.360(5) . ? N4 C14 1.372(6) . ? N5 C19 1.332(5) . ? N5 C17 1.393(5) . ? N6 C19 1.347(5) . ? N6 C18 1.374(6) . ? C1 C2 1.371(6) . ? C1 C4 1.513(6) . ? C2 C3 1.411(6) . ? C2 H2A 0.9500 . ? C3 C5 1.515(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.519(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.420(6) . ? C8 C11 1.509(6) . ? C9 C10 1.379(5) . ? C9 H9A 0.9500 . ? C10 C12 1.508(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.354(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.475(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.346(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.499(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? Co2 N7 1.878(4) . ? Co2 N8 1.884(3) . ? Co2 O4 1.891(3) . ? Co2 O3 1.906(3) . ? Co2 N9 1.960(4) . ? Co2 N11 1.978(3) . ? O3 C21 1.305(5) . ? O4 C30 1.292(5) . ? N7 C23 1.289(6) . ? N7 C26 1.474(5) . ? N8 C28 1.308(6) . ? N8 C27 1.442(6) . ? N9 C35 1.311(6) . ? N9 C33 1.431(6) . ? N10 C35 1.334(6) . ? N10 C34 1.424(7) . ? N11 C39 1.333(5) . ? N11 C37 1.391(5) . ? N12 C39 1.349(5) . ? N12 C38 1.381(5) . ? C21 C22 1.376(6) . ? C21 C24 1.499(6) . ? C22 C23 1.441(6) . ? C22 H22A 0.9500 . ? C23 C25 1.506(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.462(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.422(7) . ? C28 C31 1.506(6) . ? C29 C30 1.368(6) . ? C29 H29A 0.9500 . ? C30 C32 1.504(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.314(7) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.480(7) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.334(6) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.485(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? O1S C1S 1.572(14) . ? O1S H1SO 0.8400 . ? C1S C2S 1.502(15) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? 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 Co1 O2 93.95(14) . . ? N2 Co1 O1 179.27(15) . . ? O2 Co1 O1 85.33(12) . . ? N2 Co1 N1 85.82(16) . . ? O2 Co1 N1 179.64(13) . . ? O1 Co1 N1 94.90(14) . . ? N2 Co1 N3 91.31(14) . . ? O2 Co1 N3 90.92(13) . . ? O1 Co1 N3 88.80(12) . . ? N1 Co1 N3 89.36(14) . . ? N2 Co1 N5 89.79(14) . . ? O2 Co1 N5 89.11(13) . . ? O1 Co1 N5 90.10(13) . . ? N1 Co1 N5 90.62(14) . . ? N3 Co1 N5 178.90(15) . . ? C1 O1 Co1 123.7(3) . . ? C10 O2 Co1 121.4(2) . . ? C3 N1 C6 120.3(4) . . ? C3 N1 Co1 125.6(3) . . ? C6 N1 Co1 113.9(3) . . ? C8 N2 C7 123.0(4) . . ? C8 N2 Co1 125.0(3) . . ? C7 N2 Co1 112.0(3) . . ? C15 N3 C13 106.7(3) . . ? C15 N3 Co1 132.6(3) . . ? C13 N3 Co1 120.3(3) . . ? C15 N4 C14 107.2(4) . . ? C19 N5 C17 105.6(3) . . ? C19 N5 Co1 130.0(3) . . ? C17 N5 Co1 124.2(3) . . ? C19 N6 C18 108.1(3) . . ? O1 C1 C2 126.2(4) . . ? O1 C1 C4 113.8(4) . . ? C2 C1 C4 120.0(4) . . ? C1 C2 C3 126.2(4) . . ? C1 C2 H2A 116.9 . . ? C3 C2 H2A 116.9 . . ? N1 C3 C2 122.2(4) . . ? N1 C3 C5 119.7(4) . . ? C2 C3 C5 118.1(4) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C7 109.3(4) . . ? N1 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? N1 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N2 C7 C6 109.2(4) . . ? N2 C7 H7A 109.8 . . ? C6 C7 H7A 109.8 . . ? N2 C7 H7B 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? N2 C8 C9 122.2(4) . . ? N2 C8 C11 120.2(4) . . ? C9 C8 C11 117.6(4) . . ? C10 C9 C8 124.3(4) . . ? C10 C9 H9A 117.8 . . ? C8 C9 H9A 117.8 . . ? O2 C10 C9 125.5(4) . . ? O2 C10 C12 113.8(3) . . ? C9 C10 C12 120.6(4) . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N3 108.8(4) . . ? C14 C13 H13A 125.6 . . ? N3 C13 H13A 125.6 . . ? C13 C14 N4 107.5(3) . . ? C13 C14 H14A 126.3 . . ? N4 C14 H14A 126.3 . . ? N3 C15 N4 109.9(4) . . ? N3 C15 C16 129.1(3) . . ? N4 C15 C16 120.9(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N5 109.7(4) . . ? C18 C17 H17A 125.2 . . ? N5 C17 H17A 125.2 . . ? C17 C18 N6 106.2(4) . . ? C17 C18 H18A 126.9 . . ? N6 C18 H18A 126.9 . . ? N5 C19 N6 110.4(4) . . ? N5 C19 C20 129.1(4) . . ? N6 C19 C20 120.6(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N7 Co2 N8 85.66(16) . . ? N7 Co2 O4 179.27(14) . . ? N8 Co2 O4 95.00(15) . . ? N7 Co2 O3 94.86(14) . . ? N8 Co2 O3 178.92(14) . . ? O4 Co2 O3 84.49(12) . . ? N7 Co2 N9 92.56(16) . . ? N8 Co2 N9 87.31(15) . . ? O4 Co2 N9 87.79(15) . . ? O3 Co2 N9 91.72(14) . . ? N7 Co2 N11 88.57(15) . . ? N8 Co2 N11 89.46(14) . . ? O4 Co2 N11 91.13(14) . . ? O3 Co2 N11 91.50(13) . . ? N9 Co2 N11 176.49(15) . . ? C21 O3 Co2 122.2(2) . . ? C30 O4 Co2 123.4(3) . . ? C23 N7 C26 122.2(4) . . ? C23 N7 Co2 124.9(3) . . ? C26 N7 Co2 112.8(3) . . ? C28 N8 C27 120.9(4) . . ? C28 N8 Co2 125.3(3) . . ? C27 N8 Co2 113.9(3) . . ? C35 N9 C33 104.8(4) . . ? C35 N9 Co2 133.5(4) . . ? C33 N9 Co2 121.6(3) . . ? C35 N10 C34 105.7(4) . . ? C39 N11 C37 106.4(3) . . ? C39 N11 Co2 131.4(3) . . ? C37 N11 Co2 122.2(3) . . ? C39 N12 C38 108.3(3) . . ? O3 C21 C22 125.1(4) . . ? O3 C21 C24 115.2(4) . . ? C22 C21 C24 119.7(4) . . ? C21 C22 C23 124.6(4) . . ? C21 C22 H22A 117.7 . . ? C23 C22 H22A 117.7 . . ? N7 C23 C22 122.7(4) . . ? N7 C23 C25 121.2(4) . . ? C22 C23 C25 116.0(4) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 N7 111.6(4) . . ? C27 C26 H26A 109.3 . . ? N7 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? N7 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? N8 C27 C26 112.4(4) . . ? N8 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? N8 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? N8 C28 C29 122.5(4) . . ? N8 C28 C31 120.8(4) . . ? C29 C28 C31 116.8(5) . . ? C30 C29 C28 125.0(5) . . ? C30 C29 H29A 117.5 . . ? C28 C29 H29A 117.5 . . ? O4 C30 C29 125.8(4) . . ? O4 C30 C32 113.7(4) . . ? C29 C30 C32 120.4(4) . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 N9 109.2(5) . . ? C34 C33 H33A 125.4 . . ? N9 C33 H33A 125.4 . . ? C33 C34 N10 107.2(5) . . ? C33 C34 H34A 126.4 . . ? N10 C34 H34A 126.4 . . ? N9 C35 N10 113.1(5) . . ? N9 C35 C36 126.9(5) . . ? N10 C35 C36 120.0(5) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 N11 109.5(4) . . ? C38 C37 H37A 125.2 . . ? N11 C37 H37A 125.2 . . ? C37 C38 N12 106.4(4) . . ? C37 C38 H38A 126.8 . . ? N12 C38 H38A 126.8 . . ? N11 C39 N12 109.4(3) . . ? N11 C39 C40 128.6(4) . . ? N12 C39 C40 122.0(4) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C2S C1S O1S 154.6(10) . . ? C2S C1S H1SA 97.8 . . ? O1S C1S H1SA 97.8 . . ? C2S C1S H1SB 97.8 . . ? O1S C1S H1SB 97.8 . . ? H1SA C1S H1SB 103.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Co1 O1 C1 -160(34) . . . . ? O2 Co1 O1 C1 -168.4(3) . . . . ? N1 Co1 O1 C1 11.3(3) . . . . ? N3 Co1 O1 C1 100.5(3) . . . . ? N5 Co1 O1 C1 -79.4(3) . . . . ? N2 Co1 O2 C10 -28.6(3) . . . . ? O1 Co1 O2 C10 151.3(3) . . . . ? N1 Co1 O2 C10 22(28) . . . . ? N3 Co1 O2 C10 -120.0(3) . . . . ? N5 Co1 O2 C10 61.2(3) . . . . ? N2 Co1 N1 C3 168.8(3) . . . . ? O2 Co1 N1 C3 119(28) . . . . ? O1 Co1 N1 C3 -11.1(3) . . . . ? N3 Co1 N1 C3 -99.8(3) . . . . ? N5 Co1 N1 C3 79.1(3) . . . . ? N2 Co1 N1 C6 -5.8(3) . . . . ? O2 Co1 N1 C6 -56(28) . . . . ? O1 Co1 N1 C6 174.3(3) . . . . ? N3 Co1 N1 C6 85.6(3) . . . . ? N5 Co1 N1 C6 -95.5(3) . . . . ? O2 Co1 N2 C8 21.4(4) . . . . ? O1 Co1 N2 C8 13(11) . . . . ? N1 Co1 N2 C8 -158.3(4) . . . . ? N3 Co1 N2 C8 112.4(4) . . . . ? N5 Co1 N2 C8 -67.7(4) . . . . ? O2 Co1 N2 C7 -157.5(3) . . . . ? O1 Co1 N2 C7 -166(33) . . . . ? N1 Co1 N2 C7 22.8(3) . . . . ? N3 Co1 N2 C7 -66.5(3) . . . . ? N5 Co1 N2 C7 113.4(3) . . . . ? N2 Co1 N3 C15 -50.8(4) . . . . ? O2 Co1 N3 C15 43.2(4) . . . . ? O1 Co1 N3 C15 128.5(4) . . . . ? N1 Co1 N3 C15 -136.6(4) . . . . ? N5 Co1 N3 C15 135(8) . . . . ? N2 Co1 N3 C13 137.4(3) . . . . ? O2 Co1 N3 C13 -128.6(3) . . . . ? O1 Co1 N3 C13 -43.3(3) . . . . ? N1 Co1 N3 C13 51.6(3) . . . . ? N5 Co1 N3 C13 -37(8) . . . . ? N2 Co1 N5 C19 136.6(4) . . . . ? O2 Co1 N5 C19 42.7(4) . . . . ? O1 Co1 N5 C19 -42.7(4) . . . . ? N1 Co1 N5 C19 -137.6(4) . . . . ? N3 Co1 N5 C19 -49(8) . . . . ? N2 Co1 N5 C17 -37.5(4) . . . . ? O2 Co1 N5 C17 -131.5(3) . . . . ? O1 Co1 N5 C17 143.2(3) . . . . ? N1 Co1 N5 C17 48.3(4) . . . . ? N3 Co1 N5 C17 137(8) . . . . ? Co1 O1 C1 C2 -7.6(5) . . . . ? Co1 O1 C1 C4 172.5(2) . . . . ? O1 C1 C2 C3 -0.7(6) . . . . ? C4 C1 C2 C3 179.2(4) . . . . ? C6 N1 C3 C2 -179.0(4) . . . . ? Co1 N1 C3 C2 6.7(5) . . . . ? C6 N1 C3 C5 1.3(6) . . . . ? Co1 N1 C3 C5 -173.0(3) . . . . ? C1 C2 C3 N1 1.2(6) . . . . ? C1 C2 C3 C5 -179.1(4) . . . . ? C3 N1 C6 C7 173.4(3) . . . . ? Co1 N1 C6 C7 -11.7(4) . . . . ? C8 N2 C7 C6 146.9(4) . . . . ? Co1 N2 C7 C6 -34.2(4) . . . . ? N1 C6 C7 N2 28.7(4) . . . . ? C7 N2 C8 C9 174.5(4) . . . . ? Co1 N2 C8 C9 -4.3(6) . . . . ? C7 N2 C8 C11 -3.4(6) . . . . ? Co1 N2 C8 C11 177.8(3) . . . . ? N2 C8 C9 C10 -14.7(7) . . . . ? C11 C8 C9 C10 163.2(4) . . . . ? Co1 O2 C10 C9 19.9(6) . . . . ? Co1 O2 C10 C12 -161.4(3) . . . . ? C8 C9 C10 O2 5.8(7) . . . . ? C8 C9 C10 C12 -172.7(4) . . . . ? C15 N3 C13 C14 -0.2(4) . . . . ? Co1 N3 C13 C14 173.5(3) . . . . ? N3 C13 C14 N4 0.1(4) . . . . ? C15 N4 C14 C13 0.0(4) . . . . ? C13 N3 C15 N4 0.2(4) . . . . ? Co1 N3 C15 N4 -172.4(3) . . . . ? C13 N3 C15 C16 -176.8(4) . . . . ? Co1 N3 C15 C16 10.5(6) . . . . ? C14 N4 C15 N3 -0.1(4) . . . . ? C14 N4 C15 C16 177.2(4) . . . . ? C19 N5 C17 C18 0.1(5) . . . . ? Co1 N5 C17 C18 175.5(3) . . . . ? N5 C17 C18 N6 -0.6(6) . . . . ? C19 N6 C18 C17 0.9(6) . . . . ? C17 N5 C19 N6 0.5(5) . . . . ? Co1 N5 C19 N6 -174.5(3) . . . . ? C17 N5 C19 C20 -178.6(5) . . . . ? Co1 N5 C19 C20 6.4(7) . . . . ? C18 N6 C19 N5 -0.9(6) . . . . ? C18 N6 C19 C20 178.3(4) . . . . ? N7 Co2 O3 C21 23.5(3) . . . . ? N8 Co2 O3 C21 142(8) . . . . ? O4 Co2 O3 C21 -156.2(3) . . . . ? N9 Co2 O3 C21 116.2(3) . . . . ? N11 Co2 O3 C21 -65.2(3) . . . . ? N7 Co2 O4 C30 137(12) . . . . ? N8 Co2 O4 C30 -17.6(3) . . . . ? O3 Co2 O4 C30 163.4(3) . . . . ? N9 Co2 O4 C30 -104.7(3) . . . . ? N11 Co2 O4 C30 72.0(3) . . . . ? N8 Co2 N7 C23 159.3(4) . . . . ? O4 Co2 N7 C23 4(12) . . . . ? O3 Co2 N7 C23 -21.7(4) . . . . ? N9 Co2 N7 C23 -113.6(4) . . . . ? N11 Co2 N7 C23 69.7(4) . . . . ? N8 Co2 N7 C26 -17.4(3) . . . . ? O4 Co2 N7 C26 -172(75) . . . . ? O3 Co2 N7 C26 161.6(3) . . . . ? N9 Co2 N7 C26 69.7(3) . . . . ? N11 Co2 N7 C26 -107.0(3) . . . . ? N7 Co2 N8 C28 -164.6(4) . . . . ? O4 Co2 N8 C28 15.1(4) . . . . ? O3 Co2 N8 C28 77(8) . . . . ? N9 Co2 N8 C28 102.6(4) . . . . ? N11 Co2 N8 C28 -76.0(4) . . . . ? N7 Co2 N8 C27 15.8(4) . . . . ? O4 Co2 N8 C27 -164.6(4) . . . . ? O3 Co2 N8 C27 -103(8) . . . . ? N9 Co2 N8 C27 -77.0(4) . . . . ? N11 Co2 N8 C27 104.4(4) . . . . ? N7 Co2 N9 C35 40.9(4) . . . . ? N8 Co2 N9 C35 126.4(4) . . . . ? O4 Co2 N9 C35 -138.5(4) . . . . ? O3 Co2 N9 C35 -54.1(4) . . . . ? N11 Co2 N9 C35 149(2) . . . . ? N7 Co2 N9 C33 -134.3(3) . . . . ? N8 Co2 N9 C33 -48.7(3) . . . . ? O4 Co2 N9 C33 46.4(3) . . . . ? O3 Co2 N9 C33 130.8(3) . . . . ? N11 Co2 N9 C33 -26(3) . . . . ? N7 Co2 N11 C39 -134.2(4) . . . . ? N8 Co2 N11 C39 140.2(4) . . . . ? O4 Co2 N11 C39 45.2(4) . . . . ? O3 Co2 N11 C39 -39.4(4) . . . . ? N9 Co2 N11 C39 117(2) . . . . ? N7 Co2 N11 C37 42.1(3) . . . . ? N8 Co2 N11 C37 -43.6(3) . . . . ? O4 Co2 N11 C37 -138.6(3) . . . . ? O3 Co2 N11 C37 136.9(3) . . . . ? N9 Co2 N11 C37 -67(3) . . . . ? Co2 O3 C21 C22 -13.4(6) . . . . ? Co2 O3 C21 C24 168.6(3) . . . . ? O3 C21 C22 C23 -7.1(7) . . . . ? C24 C21 C22 C23 170.8(4) . . . . ? C26 N7 C23 C22 -174.5(4) . . . . ? Co2 N7 C23 C22 9.1(6) . . . . ? C26 N7 C23 C25 2.5(7) . . . . ? Co2 N7 C23 C25 -173.9(4) . . . . ? C21 C22 C23 N7 9.8(7) . . . . ? C21 C22 C23 C25 -167.4(5) . . . . ? C23 N7 C26 C27 -161.1(5) . . . . ? Co2 N7 C26 C27 15.6(5) . . . . ? C28 N8 C27 C26 169.9(5) . . . . ? Co2 N8 C27 C26 -10.5(7) . . . . ? N7 C26 C27 N8 -3.3(7) . . . . ? C27 N8 C28 C29 174.6(5) . . . . ? Co2 N8 C28 C29 -5.0(6) . . . . ? C27 N8 C28 C31 -4.1(7) . . . . ? Co2 N8 C28 C31 176.4(4) . . . . ? N8 C28 C29 C30 -8.8(7) . . . . ? C31 C28 C29 C30 170.0(5) . . . . ? Co2 O4 C30 C29 10.4(6) . . . . ? Co2 O4 C30 C32 -170.6(3) . . . . ? C28 C29 C30 O4 5.8(7) . . . . ? C28 C29 C30 C32 -173.1(4) . . . . ? C35 N9 C33 C34 0.8(5) . . . . ? Co2 N9 C33 C34 177.2(3) . . . . ? N9 C33 C34 N10 -0.2(5) . . . . ? C35 N10 C34 C33 -0.5(5) . . . . ? C33 N9 C35 N10 -1.2(5) . . . . ? Co2 N9 C35 N10 -176.9(3) . . . . ? C33 N9 C35 C36 178.2(4) . . . . ? Co2 N9 C35 C36 2.5(7) . . . . ? C34 N10 C35 N9 1.1(5) . . . . ? C34 N10 C35 C36 -178.4(4) . . . . ? C39 N11 C37 C38 -0.2(5) . . . . ? Co2 N11 C37 C38 -177.2(3) . . . . ? N11 C37 C38 N12 0.1(5) . . . . ? C39 N12 C38 C37 0.0(5) . . . . ? C37 N11 C39 N12 0.2(5) . . . . ? Co2 N11 C39 N12 176.9(3) . . . . ? C37 N11 C39 C40 -179.1(4) . . . . ? Co2 N11 C39 C40 -2.4(7) . . . . ? C38 N12 C39 N11 -0.2(5) . . . . ? C38 N12 C39 C40 179.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.809 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.124