# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1332 data_shelxl _publ_requested_journal 'Chem. Commun.' _publ_contact_author ; Paul H. Walton Department of Chemistry, University of York, Heslington, York, YO1 5DD, UK ; _publ_requested_coeditor_name ? _publ_contact_author_phone '44 1904 432580' _publ_contact_author_fax '44 1904 432516' _publ_contact_author_email 'phw2@york.ac.uk' loop_ _publ_author_name ; Clive J. Boxwell, Paul H. Walton* ; _publ_author_address ; Department of Chemistry, University of York, Heslington, York, YO1 5DD, UK ; _publ_section_title ; Structures of [Co(II)(L)(NO3)(HOCH3)n]BPh4(n=4,5) complexes (L=cis-1,3,5-triaminocyclohexane-based ligand); Structural 'Snapshots' of Anion Binding to a Metal Centre. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H97 B Co N4 O8' _chemical_formula_weight 1240.30 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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P - 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.491(8) _cell_length_b 19.048(11) _cell_length_c 12.838(6) _cell_angle_alpha 98.79(5) _cell_angle_beta 97.26(4) _cell_angle_gamma 114.35(4) _cell_volume 3549(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 8.96 _cell_measurement_theta_max 13.14 _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1330 _exptl_absorpt_coefficient_mu 0.297 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.888 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'AFC6S' _diffrn_measurement_method /w--2/q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 20.599 _diffrn_reflns_number 8918 _diffrn_reflns_av_R_equivalents 0.097 _diffrn_reflns_av_sigmaI/netI 0.2654 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 22.49 _reflns_number_total 8918 _reflns_number_gt 3279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'teXsan' _computing_cell_refinement 'teXsan' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Reflections 0 0 1, 0 -1 1 and -1 0 1 were omitted from the refinement. Hydrogen atoms of the methanol molecules were placed using the HFIX 137 and HFIX 147 commands. The t-butyl group containing C30 to C32 was disordered over two positions and refined isotropically. The occupancy of these positions refined to 0.65 and 0.35. ; _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^)+(0.0702P)^2^+2.9117P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8918 _refine_ls_number_parameters 795 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2402 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.2251 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.32540(9) 0.19117(7) 0.36360(10) 0.0282(4) Uani 1 1 d . . . O1 O 0.3560(4) 0.2482(3) 0.5303(4) 0.0323(16) Uani 1 1 d . . . H1O H 0.4015 0.2999 0.5503 0.039 Uiso 1 1 calc R . . O2 O 0.3447(4) 0.3073(3) 0.3438(5) 0.0320(16) Uani 1 1 d . . . H2O H 0.3934 0.3498 0.3916 0.038 Uiso 1 1 calc R . . O3 O 0.4688(4) 0.2369(3) 0.3740(4) 0.0290(15) Uani 1 1 d . . . H3O H 0.5030 0.2894 0.4109 0.035 Uiso 1 1 calc R . . O4 O 0.5829(4) 0.3774(4) 0.5024(6) 0.0484(19) Uani 1 1 d . . . O5 O 0.5195(5) 0.4293(4) 0.3967(6) 0.0465(18) Uani 1 1 d . . . O6 O 0.6210(5) 0.5035(4) 0.5425(6) 0.059(2) Uani 1 1 d . . . O7 O 0.7502(6) 0.4769(6) 0.7069(8) 0.097(3) Uani 1 1 d . . . H7O H 0.7116 0.4767 0.6597 0.145 Uiso 1 1 calc R . . O8 O 0.4318(4) 0.4035(4) 0.6231(5) 0.0467(18) Uani 1 1 d . . . H8O H 0.4394 0.4442 0.6028 0.070 Uiso 1 1 calc R . . N1 N 0.1816(5) 0.1479(4) 0.3484(6) 0.0288(19) Uani 1 1 d . . . N2 N 0.3156(5) 0.0820(4) 0.3983(7) 0.034(2) Uani 1 1 d . . . N3 N 0.3030(5) 0.1414(4) 0.1948(6) 0.0261(18) Uani 1 1 d . . . N4 N 0.5745(6) 0.4359(6) 0.4805(7) 0.044(2) Uani 1 1 d . . . C1 C 0.1264(6) 0.0655(5) 0.2859(7) 0.034(2) Uani 1 1 d . . . H1 H 0.0623 0.0527 0.2847 0.041 Uiso 1 1 calc R . . C2 C 0.1385(6) 0.0571(5) 0.1685(7) 0.032(2) Uani 1 1 d . . . H2A H 0.1316 0.0993 0.1405 0.039 Uiso 1 1 calc R . . H2B H 0.0905 0.0073 0.1256 0.039 Uiso 1 1 calc R . . C3 C 0.2314(6) 0.0599(5) 0.1551(8) 0.034(2) Uani 1 1 d . . . H3 H 0.2286 0.0437 0.0780 0.041 Uiso 1 1 calc R . . C4 C 0.2505(6) 0.0019(5) 0.2117(8) 0.038(3) Uani 1 1 d . . . H4A H 0.3123 0.0099 0.2100 0.045 Uiso 1 1 calc R . . H4B H 0.2099 -0.0515 0.1712 0.045 Uiso 1 1 calc R . . C5 C 0.2394(6) 0.0086(6) 0.3292(8) 0.039(3) Uani 1 1 d . . . H5 H 0.2421 -0.0369 0.3535 0.047 Uiso 1 1 calc R . . C6 C 0.1480(6) 0.0073(6) 0.3389(8) 0.040(3) Uani 1 1 d . . . H6A H 0.1467 0.0188 0.4148 0.048 Uiso 1 1 calc R . . H6B H 0.1005 -0.0457 0.3068 0.048 Uiso 1 1 calc R . . C7 C 0.1352(7) 0.1828(6) 0.3834(7) 0.038(3) Uani 1 1 d . . . H7 H 0.0722 0.1540 0.3645 0.045 Uiso 1 1 calc R . . C8 C 0.1702(6) 0.2621(6) 0.4493(7) 0.032(2) Uani 1 1 d . . . H8 H 0.2326 0.2939 0.4710 0.038 Uiso 1 1 calc R . . C9 C 0.1104(6) 0.2888(5) 0.4783(7) 0.033(2) Uani 1 1 d . . . H9 H 0.0494 0.2523 0.4579 0.040 Uiso 1 1 calc R . . C10 C 0.1288(6) 0.3679(6) 0.5381(7) 0.034(2) Uani 1 1 d . . . C11 C 0.0587(7) 0.3872(6) 0.5536(8) 0.047(3) Uani 1 1 d . . . H11 H -0.0011 0.3483 0.5316 0.056 Uiso 1 1 calc R . . C12 C 0.0759(7) 0.4631(6) 0.6012(8) 0.043(3) Uani 1 1 d . . . H12 H 0.0269 0.4737 0.6114 0.052 Uiso 1 1 calc R . . C13 C 0.1628(6) 0.5244(6) 0.6344(8) 0.036(2) Uani 1 1 d . . . C14 C 0.2329(7) 0.5036(6) 0.6215(8) 0.044(3) Uani 1 1 d . . . H14 H 0.2925 0.5425 0.6457 0.052 Uiso 1 1 calc R . . C15 C 0.2189(7) 0.4288(6) 0.5749(7) 0.039(3) Uani 1 1 d . . . H15 H 0.2682 0.4179 0.5675 0.047 Uiso 1 1 calc R . . C16 C 0.1826(8) 0.6092(6) 0.6814(10) 0.056(3) Uani 1 1 d . . . C17 C 0.1009(7) 0.6158(6) 0.7167(10) 0.070(4) Uani 1 1 d . . . H17A H 0.0857 0.5884 0.7734 0.105 Uiso 1 1 calc R . . H17B H 0.0500 0.5927 0.6566 0.105 Uiso 1 1 calc R . . H17C H 0.1155 0.6706 0.7423 0.105 Uiso 1 1 calc R . . C18 C 0.2055(8) 0.6551(7) 0.5901(11) 0.081(4) Uani 1 1 d . . . H18A H 0.2575 0.6523 0.5669 0.122 Uiso 1 1 calc R . . H18B H 0.2189 0.7094 0.6169 0.122 Uiso 1 1 calc R . . H18C H 0.1543 0.6317 0.5303 0.122 Uiso 1 1 calc R . . C19 C 0.2642(8) 0.6499(6) 0.7770(10) 0.074(4) Uani 1 1 d . . . H19A H 0.3166 0.6472 0.7553 0.111 Uiso 1 1 calc R . . H19B H 0.2507 0.6237 0.8352 0.111 Uiso 1 1 calc R . . H19C H 0.2764 0.7043 0.8003 0.111 Uiso 1 1 calc R . . C20 C 0.3652(6) 0.0693(5) 0.4724(8) 0.039(3) Uani 1 1 d . . . H20 H 0.3479 0.0173 0.4786 0.047 Uiso 1 1 calc R . . C21 C 0.4466(6) 0.1310(6) 0.5473(8) 0.041(3) Uani 1 1 d . . . H21 H 0.4632 0.1839 0.5464 0.049 Uiso 1 1 calc R . . C22 C 0.4980(7) 0.1120(6) 0.6178(8) 0.041(3) Uani 1 1 d . . . H22 H 0.4752 0.0592 0.6217 0.049 Uiso 1 1 calc R . . C23 C 0.5843(7) 0.1655(6) 0.6875(7) 0.036(2) Uani 1 1 d . . . C24 C 0.6266(7) 0.2452(7) 0.6868(8) 0.049(3) Uani 1 1 d . . . H24 H 0.5968 0.2661 0.6439 0.059 Uiso 1 1 calc R . . C25 C 0.7135(8) 0.2944(7) 0.7498(8) 0.053(3) Uani 1 1 d . . . H25 H 0.7403 0.3474 0.7468 0.063 Uiso 1 1 calc R . . C26 C 0.7608(7) 0.2677(7) 0.8157(8) 0.049(3) Uani 1 1 d . . . C27 C 0.7131(8) 0.1871(8) 0.8199(9) 0.060(3) Uani 1 1 d . . . H27 H 0.7399 0.1669 0.8679 0.072 Uiso 1 1 calc R . . C28 C 0.6293(7) 0.1380(6) 0.7557(8) 0.043(3) Uani 1 1 d . . . H28 H 0.6022 0.0849 0.7584 0.051 Uiso 1 1 calc R . . C29 C 0.8582(9) 0.3211(8) 0.8797(10) 0.076(4) Uani 1 1 d . . . C32A C 0.916(2) 0.2696(18) 0.862(3) 0.066(10) Uiso 0.35 1 d P . . H32A H 0.9251 0.2642 0.7893 0.099 Uiso 0.35 1 calc PR . . H32B H 0.8834 0.2181 0.8755 0.099 Uiso 0.35 1 calc PR . . H32C H 0.9744 0.2964 0.9112 0.099 Uiso 0.35 1 calc PR . . C31A C 0.864(3) 0.341(3) 1.003(4) 0.125(17) Uiso 0.35 1 d P . . H31A H 0.8467 0.3833 1.0199 0.187 Uiso 0.35 1 calc PR . . H31B H 0.9257 0.3582 1.0400 0.187 Uiso 0.35 1 calc PR . . H31C H 0.8243 0.2955 1.0241 0.187 Uiso 0.35 1 calc PR . . C30A C 0.898(4) 0.398(3) 0.845(5) 0.15(2) Uiso 0.35 1 d P . . H30A H 0.8549 0.3980 0.7876 0.227 Uiso 0.35 1 calc PR . . H30B H 0.9526 0.4035 0.8200 0.227 Uiso 0.35 1 calc PR . . H30C H 0.9126 0.4408 0.9048 0.227 Uiso 0.35 1 calc PR . . C30 C 0.9168(14) 0.3533(14) 0.8013(18) 0.096(7) Uiso 0.65 1 d P . . H30D H 0.8862 0.3722 0.7521 0.144 Uiso 0.65 1 calc PR . . H30E H 0.9277 0.3122 0.7618 0.144 Uiso 0.65 1 calc PR . . H30F H 0.9738 0.3961 0.8401 0.144 Uiso 0.65 1 calc PR . . C31 C 0.8544(13) 0.3998(10) 0.9436(16) 0.073(6) Uiso 0.65 1 d P . . H31D H 0.8361 0.4252 0.8925 0.109 Uiso 0.65 1 calc PR . . H31E H 0.9135 0.4356 0.9867 0.109 Uiso 0.65 1 calc PR . . H31F H 0.8112 0.3852 0.9894 0.109 Uiso 0.65 1 calc PR . . C32 C 0.8874(16) 0.2894(14) 0.959(2) 0.110(8) Uiso 0.65 1 d P . . H32D H 0.9486 0.3254 0.9960 0.165 Uiso 0.65 1 calc PR . . H32E H 0.8856 0.2398 0.9264 0.165 Uiso 0.65 1 calc PR . . H32F H 0.8481 0.2810 1.0098 0.165 Uiso 0.65 1 calc PR . . C33 C 0.3435(6) 0.1725(5) 0.1204(8) 0.030(2) Uani 1 1 d . . . H33 H 0.3239 0.1409 0.0509 0.036 Uiso 1 1 calc R . . C34 C 0.4154(6) 0.2512(5) 0.1363(8) 0.034(2) Uani 1 1 d . . . H34 H 0.4364 0.2853 0.2042 0.041 Uiso 1 1 calc R . . C35 C 0.4517(6) 0.2751(5) 0.0543(8) 0.035(2) Uani 1 1 d . . . H35 H 0.4272 0.2387 -0.0118 0.042 Uiso 1 1 calc R . . C36 C 0.5255(6) 0.3517(6) 0.0552(7) 0.033(2) Uani 1 1 d . . . C37 C 0.5677(7) 0.3614(6) -0.0330(7) 0.042(3) Uani 1 1 d . . . H37 H 0.5487 0.3189 -0.0917 0.051 Uiso 1 1 calc R . . C38 C 0.6374(7) 0.4334(6) -0.0338(8) 0.047(3) Uani 1 1 d . . . H38 H 0.6641 0.4384 -0.0936 0.057 Uiso 1 1 calc R . . C39 C 0.6686(7) 0.4980(6) 0.0515(9) 0.049(3) Uani 1 1 d . . . C40 C 0.6261(6) 0.4891(6) 0.1397(8) 0.043(3) Uani 1 1 d . . . H40 H 0.6454 0.5315 0.1984 0.051 Uiso 1 1 calc R . . C41 C 0.5561(7) 0.4178(6) 0.1395(8) 0.044(3) Uani 1 1 d . . . H41 H 0.5279 0.4135 0.1981 0.053 Uiso 1 1 calc R . . C42 C 0.7453(8) 0.5795(7) 0.0524(10) 0.072(4) Uani 1 1 d . . . C43 C 0.8094(8) 0.6192(7) 0.1547(10) 0.093(5) Uani 1 1 d . . . H43A H 0.7768 0.6213 0.2111 0.139 Uiso 1 1 calc R . . H43B H 0.8497 0.6720 0.1517 0.139 Uiso 1 1 calc R . . H43C H 0.8441 0.5906 0.1692 0.139 Uiso 1 1 calc R . . C44 C 0.6995(11) 0.6292(8) 0.0173(16) 0.186(11) Uani 1 1 d . . . H44A H 0.6580 0.6016 -0.0509 0.279 Uiso 1 1 calc R . . H44B H 0.7449 0.6789 0.0104 0.279 Uiso 1 1 calc R . . H44C H 0.6667 0.6385 0.0702 0.279 Uiso 1 1 calc R . . C45 C 0.7986(14) 0.5741(11) -0.0368(17) 0.259(16) Uani 1 1 d . . . H45A H 0.7567 0.5482 -0.1050 0.389 Uiso 1 1 calc R . . H45B H 0.8316 0.5444 -0.0210 0.389 Uiso 1 1 calc R . . H45C H 0.8404 0.6264 -0.0397 0.389 Uiso 1 1 calc R . . C46 C 0.7972(6) 0.0812(5) 0.3528(7) 0.028(2) Uani 1 1 d . . . C47 C 0.8682(6) 0.1253(5) 0.4434(7) 0.032(2) Uani 1 1 d . . . H47 H 0.9249 0.1267 0.4404 0.039 Uiso 1 1 calc R . . C48 C 0.8603(8) 0.1665(5) 0.5362(8) 0.043(3) Uani 1 1 d . . . H48 H 0.9098 0.1932 0.5941 0.052 Uiso 1 1 calc R . . C49 C 0.7776(8) 0.1678(6) 0.5425(9) 0.046(3) Uani 1 1 d . . . H49 H 0.7704 0.1945 0.6049 0.055 Uiso 1 1 calc R . . C50 C 0.7067(7) 0.1289(6) 0.4553(8) 0.039(3) Uani 1 1 d . . . H50 H 0.6515 0.1308 0.4578 0.047 Uiso 1 1 calc R . . C51 C 0.7161(6) 0.0863(5) 0.3617(7) 0.032(2) Uani 1 1 d . . . H51 H 0.6666 0.0605 0.3038 0.039 Uiso 1 1 calc R . . C52 C 0.7169(6) -0.0036(5) 0.1528(7) 0.031(2) Uani 1 1 d . . . C53 C 0.6449(7) -0.0707(6) 0.1669(8) 0.046(3) Uani 1 1 d . . . H53 H 0.6543 -0.0937 0.2233 0.055 Uiso 1 1 calc R . . C54 C 0.5584(7) -0.1044(6) 0.0979(9) 0.048(3) Uani 1 1 d . . . H54 H 0.5117 -0.1488 0.1099 0.058 Uiso 1 1 calc R . . C55 C 0.5424(8) -0.0731(7) 0.0144(9) 0.056(3) Uani 1 1 d . . . H55 H 0.4854 -0.0959 -0.0316 0.068 Uiso 1 1 calc R . . C56 C 0.6128(8) -0.0059(7) -0.0014(8) 0.049(3) Uani 1 1 d . . . H56 H 0.6023 0.0170 -0.0575 0.058 Uiso 1 1 calc R . . C57 C 0.6987(6) 0.0273(6) 0.0661(7) 0.036(2) Uani 1 1 d . . . H57 H 0.7451 0.0713 0.0528 0.043 Uiso 1 1 calc R . . C58 C 0.8936(6) 0.1032(5) 0.1959(7) 0.029(2) Uani 1 1 d . . . C59 C 0.9249(6) 0.1837(5) 0.2281(7) 0.035(2) Uani 1 1 d . . . H59 H 0.9009 0.2025 0.2814 0.042 Uiso 1 1 calc R . . C60 C 0.9901(6) 0.2389(6) 0.1864(8) 0.047(3) Uani 1 1 d . . . H60 H 1.0113 0.2927 0.2152 0.057 Uiso 1 1 calc R . . C61 C 1.0232(7) 0.2141(6) 0.1032(9) 0.052(3) Uani 1 1 d . . . H61 H 1.0651 0.2508 0.0732 0.062 Uiso 1 1 calc R . . C62 C 0.9935(6) 0.1335(6) 0.0636(8) 0.042(3) Uani 1 1 d . . . H62 H 1.0154 0.1158 0.0070 0.051 Uiso 1 1 calc R . . C63 C 0.9317(6) 0.0805(5) 0.1088(7) 0.036(2) Uani 1 1 d . . . H63 H 0.9133 0.0268 0.0820 0.043 Uiso 1 1 calc R . . C64 C 0.8465(6) -0.0327(5) 0.2624(7) 0.028(2) Uani 1 1 d . . . C65 C 0.8361(6) -0.0920(5) 0.1770(8) 0.042(3) Uani 1 1 d . . . H65 H 0.8078 -0.0934 0.1088 0.050 Uiso 1 1 calc R . . C66 C 0.8658(7) -0.1495(6) 0.1879(9) 0.048(3) Uani 1 1 d . . . H66 H 0.8578 -0.1878 0.1280 0.058 Uiso 1 1 calc R . . C67 C 0.9069(7) -0.1492(6) 0.2881(9) 0.045(3) Uani 1 1 d . . . H67 H 0.9270 -0.1874 0.2972 0.054 Uiso 1 1 calc R . . C68 C 0.9176(6) -0.0930(6) 0.3723(8) 0.042(3) Uani 1 1 d . . . H68 H 0.9458 -0.0924 0.4401 0.050 Uiso 1 1 calc R . . C69 C 0.8882(6) -0.0359(5) 0.3620(8) 0.031(2) Uani 1 1 d . . . H69 H 0.8964 0.0015 0.4231 0.038 Uiso 1 1 calc R . . B1 B 0.8136(7) 0.0389(6) 0.2419(8) 0.026(3) Uani 1 1 d . . . C70 C 0.5207(6) 0.1973(6) 0.3315(8) 0.047(3) Uani 1 1 d . . . H70A H 0.5842 0.2335 0.3495 0.071 Uiso 1 1 calc R . . H70B H 0.5008 0.1800 0.2545 0.071 Uiso 1 1 calc R . . H70C H 0.5111 0.1524 0.3623 0.071 Uiso 1 1 calc R . . C71 C 0.3147(7) 0.2161(6) 0.6154(8) 0.048(3) Uani 1 1 d . . . H71A H 0.3422 0.2552 0.6820 0.072 Uiso 1 1 calc R . . H71B H 0.3237 0.1702 0.6222 0.072 Uiso 1 1 calc R . . H71C H 0.2506 0.2016 0.5985 0.072 Uiso 1 1 calc R . . C72 C 0.2917(7) 0.3271(6) 0.2656(7) 0.042(3) Uani 1 1 d . . . H72A H 0.3163 0.3836 0.2764 0.063 Uiso 1 1 calc R . . H72B H 0.2297 0.3062 0.2743 0.063 Uiso 1 1 calc R . . H72C H 0.2937 0.3048 0.1942 0.063 Uiso 1 1 calc R . . C73 C 0.8372(8) 0.5252(8) 0.6930(11) 0.094(5) Uani 1 1 d . . . H73A H 0.8555 0.5787 0.7306 0.142 Uiso 1 1 calc R . . H73B H 0.8359 0.5232 0.6176 0.142 Uiso 1 1 calc R . . H73C H 0.8796 0.5068 0.7213 0.142 Uiso 1 1 calc R . . C74 C 0.4995(7) 0.4221(6) 0.7183(8) 0.058(3) Uani 1 1 d . . . H74A H 0.5587 0.4537 0.7061 0.088 Uiso 1 1 calc R . . H74B H 0.4976 0.3740 0.7347 0.088 Uiso 1 1 calc R . . H74C H 0.4876 0.4510 0.7777 0.088 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 0.0251(8) 0.0306(8) 0.0301(8) 0.0107(6) 0.0087(6) 0.0113(6) O1 0.029(4) 0.032(4) 0.027(4) 0.008(3) 0.007(3) 0.004(3) O2 0.031(4) 0.028(4) 0.034(4) 0.007(3) 0.000(3) 0.012(3) O3 0.024(4) 0.025(4) 0.035(4) 0.004(3) 0.003(3) 0.009(3) O4 0.047(5) 0.042(5) 0.061(5) 0.017(4) 0.010(4) 0.024(4) O5 0.042(5) 0.055(5) 0.041(5) 0.017(4) 0.006(4) 0.018(4) O6 0.040(5) 0.045(5) 0.071(6) -0.007(4) 0.020(4) 0.003(4) O7 0.079(7) 0.109(7) 0.099(8) 0.055(6) 0.011(6) 0.030(6) O8 0.046(4) 0.049(4) 0.047(5) 0.015(4) 0.004(4) 0.024(4) N1 0.026(5) 0.029(5) 0.027(5) 0.005(4) 0.009(4) 0.008(4) N2 0.030(5) 0.036(5) 0.052(6) 0.028(4) 0.022(4) 0.019(4) N3 0.029(5) 0.024(5) 0.027(5) 0.006(4) 0.008(4) 0.013(4) N4 0.033(6) 0.052(7) 0.044(6) 0.008(6) 0.019(5) 0.013(5) C1 0.017(5) 0.031(6) 0.041(6) 0.000(5) 0.015(5) -0.002(5) C2 0.023(6) 0.025(5) 0.040(6) 0.006(5) 0.006(5) 0.003(4) C3 0.025(6) 0.030(6) 0.044(6) 0.003(5) 0.010(5) 0.009(5) C4 0.033(6) 0.034(6) 0.048(7) 0.007(5) 0.017(5) 0.015(5) C5 0.034(6) 0.040(7) 0.045(7) 0.016(5) 0.007(5) 0.016(5) C6 0.034(6) 0.049(7) 0.035(6) 0.013(5) 0.014(5) 0.014(5) C7 0.044(7) 0.035(7) 0.033(6) 0.007(5) 0.013(5) 0.017(6) C8 0.024(6) 0.051(7) 0.032(6) 0.012(5) 0.009(5) 0.025(5) C9 0.034(6) 0.030(6) 0.031(6) 0.010(5) 0.007(5) 0.008(5) C10 0.026(6) 0.044(7) 0.039(6) 0.018(5) 0.010(5) 0.018(5) C11 0.023(6) 0.046(7) 0.075(8) 0.012(6) 0.012(6) 0.018(5) C12 0.039(7) 0.054(7) 0.056(7) 0.015(6) 0.015(6) 0.036(6) C13 0.023(6) 0.038(6) 0.052(7) 0.010(5) 0.015(5) 0.015(5) C14 0.034(7) 0.037(7) 0.053(7) 0.008(6) 0.016(5) 0.007(5) C15 0.040(7) 0.055(7) 0.036(6) 0.014(6) 0.010(5) 0.032(6) C16 0.058(8) 0.038(7) 0.079(9) 0.017(6) 0.019(7) 0.026(6) C17 0.064(9) 0.064(8) 0.095(10) 0.015(7) 0.025(8) 0.039(7) C18 0.072(9) 0.061(8) 0.132(12) 0.056(9) 0.046(9) 0.031(7) C19 0.060(9) 0.044(7) 0.108(11) -0.004(7) 0.001(8) 0.025(7) C20 0.035(7) 0.024(6) 0.062(8) 0.026(6) 0.018(6) 0.010(5) C21 0.042(7) 0.041(6) 0.049(7) 0.027(6) 0.019(6) 0.017(6) C22 0.048(7) 0.051(7) 0.038(7) 0.037(6) 0.013(6) 0.027(6) C23 0.040(7) 0.054(7) 0.028(6) 0.014(6) 0.018(5) 0.030(6) C24 0.039(7) 0.069(8) 0.054(8) 0.021(7) 0.009(6) 0.036(7) C25 0.063(9) 0.058(8) 0.047(7) 0.007(6) 0.010(7) 0.039(7) C26 0.034(7) 0.072(9) 0.036(7) -0.010(6) -0.005(5) 0.029(7) C27 0.057(9) 0.097(11) 0.043(8) 0.020(7) 0.003(7) 0.049(8) C28 0.040(7) 0.060(7) 0.044(7) 0.030(6) 0.011(6) 0.031(6) C29 0.080(10) 0.087(10) 0.044(8) 0.000(7) -0.003(7) 0.031(8) C33 0.029(6) 0.037(6) 0.035(6) 0.010(5) 0.008(5) 0.024(5) C34 0.028(6) 0.030(6) 0.041(7) 0.007(5) 0.008(5) 0.009(5) C35 0.035(6) 0.026(6) 0.038(6) 0.006(5) 0.013(5) 0.006(5) C36 0.040(6) 0.049(7) 0.022(6) 0.018(5) 0.016(5) 0.024(5) C37 0.050(7) 0.036(6) 0.029(6) -0.001(5) 0.008(5) 0.011(6) C38 0.050(7) 0.047(7) 0.032(7) 0.011(6) 0.012(5) 0.007(6) C39 0.037(7) 0.048(7) 0.057(8) 0.023(6) -0.004(6) 0.014(6) C40 0.038(7) 0.034(6) 0.045(7) 0.005(5) 0.008(5) 0.007(5) C41 0.044(7) 0.052(7) 0.035(7) 0.007(6) 0.014(5) 0.019(6) C42 0.071(9) 0.045(7) 0.068(9) 0.027(7) 0.001(8) -0.006(7) C43 0.058(9) 0.096(11) 0.081(10) 0.048(9) -0.016(8) -0.008(8) C44 0.107(14) 0.081(12) 0.29(3) 0.121(15) -0.081(15) -0.032(10) C45 0.21(2) 0.163(19) 0.24(2) -0.031(17) 0.19(2) -0.088(17) C46 0.044(7) 0.017(5) 0.022(6) 0.008(4) 0.011(5) 0.009(5) C47 0.032(6) 0.038(6) 0.026(6) 0.007(5) 0.012(5) 0.013(5) C48 0.061(8) 0.032(6) 0.032(7) 0.003(5) 0.016(6) 0.017(6) C49 0.075(9) 0.034(6) 0.042(7) 0.021(6) 0.029(7) 0.030(6) C50 0.047(7) 0.051(7) 0.045(7) 0.023(6) 0.025(6) 0.036(6) C51 0.037(6) 0.029(6) 0.038(6) 0.012(5) 0.013(5) 0.019(5) C52 0.026(6) 0.031(6) 0.039(6) 0.011(5) 0.017(5) 0.013(5) C53 0.035(7) 0.052(7) 0.056(7) 0.005(6) 0.010(6) 0.028(6) C54 0.030(7) 0.045(7) 0.063(8) -0.008(6) 0.016(6) 0.015(6) C55 0.059(9) 0.074(9) 0.040(8) -0.007(7) -0.003(6) 0.043(8) C56 0.055(8) 0.070(8) 0.039(7) 0.010(6) 0.010(6) 0.047(7) C57 0.034(7) 0.044(6) 0.037(6) 0.009(5) 0.014(5) 0.024(5) C58 0.031(6) 0.028(6) 0.033(6) 0.011(5) 0.009(5) 0.016(5) C59 0.029(6) 0.031(6) 0.044(7) 0.009(5) 0.012(5) 0.011(5) C60 0.042(7) 0.035(6) 0.055(8) 0.010(6) 0.014(6) 0.007(6) C61 0.042(7) 0.055(8) 0.060(8) 0.030(7) 0.018(6) 0.015(6) C62 0.036(6) 0.049(7) 0.043(7) 0.016(6) 0.022(5) 0.015(6) C63 0.035(6) 0.037(6) 0.036(6) 0.012(5) 0.010(5) 0.014(5) C64 0.025(5) 0.032(6) 0.030(6) 0.014(5) 0.018(5) 0.009(5) C65 0.051(7) 0.033(6) 0.032(6) -0.001(5) 0.001(5) 0.014(6) C66 0.048(7) 0.051(7) 0.059(8) 0.001(6) 0.013(6) 0.037(6) C67 0.048(7) 0.039(7) 0.054(8) 0.014(6) 0.012(6) 0.024(6) C68 0.043(7) 0.040(7) 0.042(7) 0.024(6) 0.001(5) 0.014(5) C69 0.029(6) 0.030(6) 0.033(6) 0.011(5) 0.006(5) 0.009(5) B1 0.029(7) 0.028(6) 0.025(7) 0.007(5) 0.005(5) 0.015(5) C70 0.035(6) 0.058(7) 0.062(8) 0.024(6) 0.020(6) 0.027(6) C71 0.048(7) 0.040(6) 0.040(7) 0.009(5) 0.020(6) 0.000(5) C72 0.051(7) 0.050(7) 0.034(6) 0.011(5) 0.006(5) 0.031(6) C73 0.042(8) 0.119(12) 0.100(11) 0.058(10) 0.008(8) 0.005(8) C74 0.053(8) 0.073(9) 0.043(8) 0.008(6) 0.004(6) 0.026(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.134(6) . ? Co1 N1 2.137(7) . ? Co1 N2 2.138(7) . ? Co1 O1 2.140(6) . ? Co1 N3 2.148(7) . ? Co1 O2 2.161(6) . ? O1 C71 1.442(9) . ? O2 C72 1.443(10) . ? O3 C70 1.456(10) . ? O4 N4 1.245(10) . ? O5 N4 1.271(10) . ? O6 N4 1.264(9) . ? O7 C73 1.401(12) . ? O8 C74 1.436(11) . ? N1 C7 1.283(11) . ? N1 C1 1.479(10) . ? N2 C20 1.293(11) . ? N2 C5 1.487(11) . ? N3 C33 1.310(10) . ? N3 C3 1.470(10) . ? C1 C6 1.521(12) . ? C1 C2 1.538(11) . ? C2 C3 1.543(12) . ? C3 C4 1.525(12) . ? C4 C5 1.535(12) . ? C5 C6 1.519(12) . ? C7 C8 1.448(12) . ? C8 C9 1.349(11) . ? C9 C10 1.470(12) . ? C10 C11 1.377(12) . ? C10 C15 1.417(12) . ? C11 C12 1.376(13) . ? C12 C13 1.383(13) . ? C13 C14 1.387(12) . ? C13 C16 1.518(13) . ? C14 C15 1.369(12) . ? C16 C17 1.520(14) . ? C16 C19 1.532(14) . ? C16 C18 1.560(14) . ? C20 C21 1.460(13) . ? C21 C22 1.353(12) . ? C22 C23 1.438(13) . ? C23 C28 1.374(12) . ? C23 C24 1.387(13) . ? C24 C25 1.398(14) . ? C25 C26 1.369(14) . ? C26 C27 1.421(14) . ? C26 C29 1.534(15) . ? C27 C28 1.370(14) . ? C29 C32 1.39(2) . ? C29 C30A 1.50(5) . ? C29 C30 1.51(2) . ? C29 C31A 1.55(4) . ? C29 C31 1.63(2) . ? C29 C32A 1.64(3) . ? C33 C34 1.441(12) . ? C34 C35 1.324(11) . ? C35 C36 1.463(12) . ? C36 C41 1.391(12) . ? C36 C37 1.399(12) . ? C37 C38 1.382(12) . ? C38 C39 1.380(13) . ? C39 C40 1.401(13) . ? C39 C42 1.543(14) . ? C40 C41 1.371(12) . ? C42 C43 1.450(14) . ? C42 C44 1.517(18) . ? C42 C45 1.544(19) . ? C46 C51 1.398(12) . ? C46 C47 1.406(12) . ? C46 B1 1.635(13) . ? C47 C48 1.375(12) . ? C48 C49 1.386(13) . ? C49 C50 1.368(13) . ? C50 C51 1.407(12) . ? C52 C57 1.392(12) . ? C52 C53 1.396(12) . ? C52 B1 1.641(13) . ? C53 C54 1.408(13) . ? C54 C55 1.353(14) . ? C55 C56 1.393(14) . ? C56 C57 1.394(13) . ? C58 C59 1.374(11) . ? C58 C63 1.445(12) . ? C58 B1 1.636(12) . ? C59 C60 1.391(12) . ? C60 C61 1.366(13) . ? C61 C62 1.391(13) . ? C62 C63 1.369(12) . ? C64 C65 1.386(12) . ? C64 C69 1.396(11) . ? C64 B1 1.707(13) . ? C65 C66 1.388(12) . ? C66 C67 1.376(13) . ? C67 C68 1.338(13) . ? C68 C69 1.376(12) . ? 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 O3 Co1 N1 177.8(3) . . ? O3 Co1 N2 92.4(3) . . ? N1 Co1 N2 89.4(3) . . ? O3 Co1 O1 87.1(2) . . ? N1 Co1 O1 94.0(3) . . ? N2 Co1 O1 93.3(3) . . ? O3 Co1 N3 89.6(2) . . ? N1 Co1 N3 89.2(3) . . ? N2 Co1 N3 89.5(3) . . ? O1 Co1 N3 175.8(3) . . ? O3 Co1 O2 84.6(2) . . ? N1 Co1 O2 93.6(3) . . ? N2 Co1 O2 174.3(3) . . ? O1 Co1 O2 81.7(2) . . ? N3 Co1 O2 95.3(2) . . ? C71 O1 Co1 127.9(5) . . ? C72 O2 Co1 128.2(5) . . ? C70 O3 Co1 129.1(5) . . ? C7 N1 C1 114.6(7) . . ? C7 N1 Co1 130.0(7) . . ? C1 N1 Co1 115.4(5) . . ? C20 N2 C5 113.7(7) . . ? C20 N2 Co1 129.9(7) . . ? C5 N2 Co1 116.4(6) . . ? C33 N3 C3 114.1(7) . . ? C33 N3 Co1 130.0(6) . . ? C3 N3 Co1 115.9(5) . . ? O4 N4 O6 120.0(9) . . ? O4 N4 O5 121.4(9) . . ? O6 N4 O5 118.6(9) . . ? N1 C1 C6 111.5(8) . . ? N1 C1 C2 110.9(7) . . ? C6 C1 C2 111.4(7) . . ? C1 C2 C3 113.8(8) . . ? N3 C3 C4 112.3(7) . . ? N3 C3 C2 109.7(7) . . ? C4 C3 C2 110.5(7) . . ? C3 C4 C5 115.1(8) . . ? N2 C5 C6 111.0(8) . . ? N2 C5 C4 109.6(7) . . ? C6 C5 C4 110.9(8) . . ? C5 C6 C1 114.6(7) . . ? N1 C7 C8 127.1(9) . . ? C9 C8 C7 118.5(9) . . ? C8 C9 C10 128.6(9) . . ? C11 C10 C15 117.4(9) . . ? C11 C10 C9 121.0(9) . . ? C15 C10 C9 121.4(8) . . ? C12 C11 C10 121.0(10) . . ? C11 C12 C13 122.8(9) . . ? C12 C13 C14 115.5(9) . . ? C12 C13 C16 123.4(9) . . ? C14 C13 C16 121.0(9) . . ? C15 C14 C13 123.5(9) . . ? C14 C15 C10 119.6(9) . . ? C13 C16 C17 112.4(9) . . ? C13 C16 C19 112.8(9) . . ? C17 C16 C19 108.7(10) . . ? C13 C16 C18 106.8(9) . . ? C17 C16 C18 107.8(9) . . ? C19 C16 C18 108.1(10) . . ? N2 C20 C21 124.5(9) . . ? C22 C21 C20 120.6(9) . . ? C21 C22 C23 126.4(9) . . ? C28 C23 C24 117.5(10) . . ? C28 C23 C22 120.2(10) . . ? C24 C23 C22 122.2(9) . . ? C23 C24 C25 120.8(10) . . ? C26 C25 C24 122.7(11) . . ? C25 C26 C27 115.0(10) . . ? C25 C26 C29 122.2(12) . . ? C27 C26 C29 122.7(11) . . ? C28 C27 C26 122.4(10) . . ? C27 C28 C23 121.4(10) . . ? C32 C29 C30A 135(3) . . ? C32 C29 C30 120.5(17) . . ? C30A C29 C30 43(2) . . ? C32 C29 C26 113.6(15) . . ? C30A C29 C26 111(2) . . ? C30 C29 C26 108.2(12) . . ? C32 C29 C31A 51.3(18) . . ? C30A C29 C31A 107(3) . . ? C30 C29 C31A 137(2) . . ? C26 C29 C31A 113(2) . . ? C32 C29 C31 105.7(14) . . ? C30A C29 C31 59(2) . . ? C30 C29 C31 101.8(14) . . ? C26 C29 C31 105.2(11) . . ? C31A C29 C31 55.9(19) . . ? C32 C29 C32A 56.0(15) . . ? C30A C29 C32A 113(3) . . ? C30 C29 C32A 73.1(15) . . ? C26 C29 C32A 106.4(14) . . ? C31A C29 C32A 106(2) . . ? C31 C29 C32A 148.0(16) . . ? N3 C33 C34 126.0(9) . . ? C35 C34 C33 120.0(9) . . ? C34 C35 C36 127.8(9) . . ? C41 C36 C37 116.8(9) . . ? C41 C36 C35 123.3(8) . . ? C37 C36 C35 119.8(9) . . ? C38 C37 C36 120.7(9) . . ? C39 C38 C37 121.9(9) . . ? C38 C39 C40 117.7(9) . . ? C38 C39 C42 123.1(10) . . ? C40 C39 C42 119.1(10) . . ? C41 C40 C39 120.1(10) . . ? C40 C41 C36 122.7(9) . . ? C43 C42 C44 111.4(12) . . ? C43 C42 C39 114.6(10) . . ? C44 C42 C39 106.8(10) . . ? C43 C42 C45 108.8(14) . . ? C44 C42 C45 102.8(15) . . ? C39 C42 C45 111.8(11) . . ? C51 C46 C47 113.6(8) . . ? C51 C46 B1 123.6(8) . . ? C47 C46 B1 122.2(8) . . ? C48 C47 C46 125.0(9) . . ? C47 C48 C49 119.2(10) . . ? C50 C49 C48 118.9(10) . . ? C49 C50 C51 120.9(9) . . ? C46 C51 C50 122.3(9) . . ? C57 C52 C53 116.3(9) . . ? C57 C52 B1 123.4(8) . . ? C53 C52 B1 120.1(8) . . ? C52 C53 C54 121.7(10) . . ? C55 C54 C53 120.8(10) . . ? C54 C55 C56 118.8(10) . . ? C55 C56 C57 120.6(10) . . ? C52 C57 C56 121.8(9) . . ? C59 C58 C63 113.1(8) . . ? C59 C58 B1 123.8(8) . . ? C63 C58 B1 122.8(8) . . ? C58 C59 C60 124.4(9) . . ? C61 C60 C59 120.0(10) . . ? C60 C61 C62 119.3(9) . . ? C63 C62 C61 119.4(9) . . ? C62 C63 C58 123.6(9) . . ? C65 C64 C69 114.4(9) . . ? C65 C64 B1 120.9(8) . . ? C69 C64 B1 124.6(8) . . ? C64 C65 C66 123.5(10) . . ? C67 C66 C65 119.3(10) . . ? C68 C67 C66 118.6(10) . . ? C67 C68 C69 122.2(10) . . ? C68 C69 C64 121.9(9) . . ? C46 B1 C58 111.1(7) . . ? C46 B1 C52 108.4(7) . . ? C58 B1 C52 111.0(7) . . ? C46 B1 C64 111.6(7) . . ? C58 B1 C64 107.0(7) . . ? C52 B1 C64 107.7(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 O3 Co1 O1 C71 -134.5(7) . . . . ? N1 Co1 O1 C71 47.4(7) . . . . ? N2 Co1 O1 C71 -42.2(7) . . . . ? N3 Co1 O1 C71 -173(3) . . . . ? O2 Co1 O1 C71 140.5(7) . . . . ? O3 Co1 O2 C72 133.8(6) . . . . ? N1 Co1 O2 C72 -44.8(7) . . . . ? N2 Co1 O2 C72 -167(2) . . . . ? O1 Co1 O2 C72 -138.4(7) . . . . ? N3 Co1 O2 C72 44.7(7) . . . . ? N1 Co1 O3 C70 -103(7) . . . . ? N2 Co1 O3 C70 42.9(7) . . . . ? O1 Co1 O3 C70 136.1(7) . . . . ? N3 Co1 O3 C70 -46.6(7) . . . . ? O2 Co1 O3 C70 -142.0(7) . . . . ? O3 Co1 N1 C7 -77(8) . . . . ? N2 Co1 N1 C7 137.0(8) . . . . ? O1 Co1 N1 C7 43.8(8) . . . . ? N3 Co1 N1 C7 -133.4(8) . . . . ? O2 Co1 N1 C7 -38.1(8) . . . . ? O3 Co1 N1 C1 102(7) . . . . ? N2 Co1 N1 C1 -44.4(6) . . . . ? O1 Co1 N1 C1 -137.6(6) . . . . ? N3 Co1 N1 C1 45.1(6) . . . . ? O2 Co1 N1 C1 140.4(6) . . . . ? O3 Co1 N2 C20 46.7(8) . . . . ? N1 Co1 N2 C20 -134.5(8) . . . . ? O1 Co1 N2 C20 -40.5(8) . . . . ? N3 Co1 N2 C20 136.3(8) . . . . ? O2 Co1 N2 C20 -12(3) . . . . ? O3 Co1 N2 C5 -134.7(6) . . . . ? N1 Co1 N2 C5 44.0(6) . . . . ? O1 Co1 N2 C5 138.0(6) . . . . ? N3 Co1 N2 C5 -45.1(6) . . . . ? O2 Co1 N2 C5 166(2) . . . . ? O3 Co1 N3 C33 -44.6(7) . . . . ? N1 Co1 N3 C33 133.5(7) . . . . ? N2 Co1 N3 C33 -137.1(7) . . . . ? O1 Co1 N3 C33 -6(4) . . . . ? O2 Co1 N3 C33 39.9(7) . . . . ? O3 Co1 N3 C3 135.6(6) . . . . ? N1 Co1 N3 C3 -46.3(6) . . . . ? N2 Co1 N3 C3 43.1(6) . . . . ? O1 Co1 N3 C3 174(3) . . . . ? O2 Co1 N3 C3 -139.9(6) . . . . ? C7 N1 C1 C6 -119.0(8) . . . . ? Co1 N1 C1 C6 62.2(8) . . . . ? C7 N1 C1 C2 116.3(8) . . . . ? Co1 N1 C1 C2 -62.5(8) . . . . ? N1 C1 C2 C3 73.4(9) . . . . ? C6 C1 C2 C3 -51.4(9) . . . . ? C33 N3 C3 C4 120.3(8) . . . . ? Co1 N3 C3 C4 -59.8(8) . . . . ? C33 N3 C3 C2 -116.4(8) . . . . ? Co1 N3 C3 C2 63.4(8) . . . . ? C1 C2 C3 N3 -73.5(9) . . . . ? C1 C2 C3 C4 50.9(10) . . . . ? N3 C3 C4 C5 71.9(10) . . . . ? C2 C3 C4 C5 -50.9(10) . . . . ? C20 N2 C5 C6 118.2(9) . . . . ? Co1 N2 C5 C6 -60.6(8) . . . . ? C20 N2 C5 C4 -118.9(9) . . . . ? Co1 N2 C5 C4 62.2(8) . . . . ? C3 C4 C5 N2 -72.1(10) . . . . ? C3 C4 C5 C6 50.8(11) . . . . ? N2 C5 C6 C1 71.4(10) . . . . ? C4 C5 C6 C1 -50.7(11) . . . . ? N1 C1 C6 C5 -72.9(10) . . . . ? C2 C1 C6 C5 51.6(10) . . . . ? C1 N1 C7 C8 177.9(8) . . . . ? Co1 N1 C7 C8 -3.5(14) . . . . ? N1 C7 C8 C9 179.9(9) . . . . ? C7 C8 C9 C10 -175.6(8) . . . . ? C8 C9 C10 C11 174.7(9) . . . . ? C8 C9 C10 C15 -0.7(14) . . . . ? C15 C10 C11 C12 1.3(14) . . . . ? C9 C10 C11 C12 -174.3(9) . . . . ? C10 C11 C12 C13 1.1(16) . . . . ? C11 C12 C13 C14 -3.0(15) . . . . ? C11 C12 C13 C16 176.6(10) . . . . ? C12 C13 C14 C15 2.8(14) . . . . ? C16 C13 C14 C15 -176.9(10) . . . . ? C13 C14 C15 C10 -0.6(15) . . . . ? C11 C10 C15 C14 -1.5(13) . . . . ? C9 C10 C15 C14 174.0(9) . . . . ? C12 C13 C16 C17 15.9(15) . . . . ? C14 C13 C16 C17 -164.5(10) . . . . ? C12 C13 C16 C19 139.2(10) . . . . ? C14 C13 C16 C19 -41.2(14) . . . . ? C12 C13 C16 C18 -102.2(11) . . . . ? C14 C13 C16 C18 77.5(12) . . . . ? C5 N2 C20 C21 176.9(8) . . . . ? Co1 N2 C20 C21 -4.5(14) . . . . ? N2 C20 C21 C22 -175.6(9) . . . . ? C20 C21 C22 C23 172.9(9) . . . . ? C21 C22 C23 C28 179.9(9) . . . . ? C21 C22 C23 C24 -2.0(15) . . . . ? C28 C23 C24 C25 2.8(14) . . . . ? C22 C23 C24 C25 -175.3(9) . . . . ? C23 C24 C25 C26 -0.8(16) . . . . ? C24 C25 C26 C27 -3.1(15) . . . . ? C24 C25 C26 C29 176.6(10) . . . . ? C25 C26 C27 C28 5.3(15) . . . . ? C29 C26 C27 C28 -174.4(10) . . . . ? C26 C27 C28 C23 -3.6(16) . . . . ? C24 C23 C28 C27 -0.7(14) . . . . ? C22 C23 C28 C27 177.5(9) . . . . ? C25 C26 C29 C32 166.7(15) . . . . ? C27 C26 C29 C32 -14(2) . . . . ? C25 C26 C29 C30A -10(3) . . . . ? C27 C26 C29 C30A 169(3) . . . . ? C25 C26 C29 C30 -56.7(16) . . . . ? C27 C26 C29 C30 123.0(15) . . . . ? C25 C26 C29 C31A 110(2) . . . . ? C27 C26 C29 C31A -70(3) . . . . ? C25 C26 C29 C31 51.6(15) . . . . ? C27 C26 C29 C31 -128.8(12) . . . . ? C25 C26 C29 C32A -133.8(15) . . . . ? C27 C26 C29 C32A 45.9(18) . . . . ? C3 N3 C33 C34 179.6(8) . . . . ? Co1 N3 C33 C34 -0.2(13) . . . . ? N3 C33 C34 C35 178.9(8) . . . . ? C33 C34 C35 C36 -179.0(8) . . . . ? C34 C35 C36 C41 -14.3(16) . . . . ? C34 C35 C36 C37 167.0(10) . . . . ? C41 C36 C37 C38 1.0(14) . . . . ? C35 C36 C37 C38 179.8(9) . . . . ? C36 C37 C38 C39 0.5(16) . . . . ? C37 C38 C39 C40 -1.0(15) . . . . ? C37 C38 C39 C42 -179.1(10) . . . . ? C38 C39 C40 C41 0.1(15) . . . . ? C42 C39 C40 C41 178.2(10) . . . . ? C39 C40 C41 C36 1.5(15) . . . . ? C37 C36 C41 C40 -2.0(15) . . . . ? C35 C36 C41 C40 179.3(9) . . . . ? C38 C39 C42 C43 -139.4(12) . . . . ? C40 C39 C42 C43 42.6(16) . . . . ? C38 C39 C42 C44 96.7(15) . . . . ? C40 C39 C42 C44 -81.3(14) . . . . ? C38 C39 C42 C45 -15.0(19) . . . . ? C40 C39 C42 C45 167.0(15) . . . . ? C51 C46 C47 C48 3.7(13) . . . . ? B1 C46 C47 C48 175.5(8) . . . . ? C46 C47 C48 C49 -2.0(14) . . . . ? C47 C48 C49 C50 -1.1(14) . . . . ? C48 C49 C50 C51 2.0(14) . . . . ? C47 C46 C51 C50 -2.7(12) . . . . ? B1 C46 C51 C50 -174.3(8) . . . . ? C49 C50 C51 C46 0.0(13) . . . . ? C57 C52 C53 C54 -0.9(13) . . . . ? B1 C52 C53 C54 173.9(8) . . . . ? C52 C53 C54 C55 0.7(15) . . . . ? C53 C54 C55 C56 -0.9(15) . . . . ? C54 C55 C56 C57 1.4(15) . . . . ? C53 C52 C57 C56 1.4(13) . . . . ? B1 C52 C57 C56 -173.2(8) . . . . ? C55 C56 C57 C52 -1.7(14) . . . . ? C63 C58 C59 C60 -3.2(13) . . . . ? B1 C58 C59 C60 -177.2(9) . . . . ? C58 C59 C60 C61 4.3(16) . . . . ? C59 C60 C61 C62 -2.4(16) . . . . ? C60 C61 C62 C63 0.0(15) . . . . ? C61 C62 C63 C58 0.9(15) . . . . ? C59 C58 C63 C62 0.6(13) . . . . ? B1 C58 C63 C62 174.6(9) . . . . ? C69 C64 C65 C66 -1.0(13) . . . . ? B1 C64 C65 C66 176.7(8) . . . . ? C64 C65 C66 C67 0.7(15) . . . . ? C65 C66 C67 C68 -0.4(15) . . . . ? C66 C67 C68 C69 0.5(15) . . . . ? C67 C68 C69 C64 -0.9(14) . . . . ? C65 C64 C69 C68 1.1(12) . . . . ? B1 C64 C69 C68 -176.5(8) . . . . ? C51 C46 B1 C58 115.6(9) . . . . ? C47 C46 B1 C58 -55.3(11) . . . . ? C51 C46 B1 C52 -6.7(11) . . . . ? C47 C46 B1 C52 -177.6(7) . . . . ? C51 C46 B1 C64 -125.0(8) . . . . ? C47 C46 B1 C64 64.1(10) . . . . ? C59 C58 B1 C46 -16.4(12) . . . . ? C63 C58 B1 C46 170.2(8) . . . . ? C59 C58 B1 C52 104.3(10) . . . . ? C63 C58 B1 C52 -69.1(10) . . . . ? C59 C58 B1 C64 -138.5(9) . . . . ? C63 C58 B1 C64 48.2(11) . . . . ? C57 C52 B1 C46 104.3(9) . . . . ? C53 C52 B1 C46 -70.1(10) . . . . ? C57 C52 B1 C58 -18.0(12) . . . . ? C53 C52 B1 C58 167.6(8) . . . . ? C57 C52 B1 C64 -134.9(8) . . . . ? C53 C52 B1 C64 50.7(10) . . . . ? C65 C64 B1 C46 159.2(8) . . . . ? C69 C64 B1 C46 -23.4(11) . . . . ? C65 C64 B1 C58 -79.0(10) . . . . ? C69 C64 B1 C58 98.4(9) . . . . ? C65 C64 B1 C52 40.4(10) . . . . ? C69 C64 B1 C52 -142.2(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O O8 0.93 1.88 2.690(9) 144.7 . O2 H2O O5 0.93 1.99 2.769(9) 140.2 . O3 H3O O4 0.93 1.76 2.672(9) 164.2 . O7 H7O O6 0.82 2.25 3.055(12) 168.2 . O8 H8O O5 0.82 2.22 3.005(9) 161.5 2_666 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.421 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.076 data_shelxl2 _publ_requested_journal 'Chem. Commun.' _publ_contact_author ; Paul H. Walton Department of Chemistry, University of York, Heslington, York, YO1 5DD, UK ; _publ_requested_coeditor_name ? _publ_contact_author_phone '44 1904 432580' _publ_contact_author_fax '44 1904 432516' _publ_contact_author_email 'phw2@york.ac.uk' loop_ _publ_author_name ; Clive J. Boxwell and Paul H. Walton* ; _publ_author_address ; Department of Chemistry, University of York, Heslington, York, YO1 5DD, UK ; _publ_section_title ; Structures of [Co(II)(L)(NO3)(HOCH3)n]BPh4(n=4,5) complexes (L=cis-1,3,5-triaminocyclohexane-based ligand); Structural 'Snapshots' of Anion Binding to a Metal Centre. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H97 B Cl4 Co N4 O7' _chemical_formula_weight 1378.11 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.393(4) _cell_length_b 16.811(5) _cell_length_c 21.737(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.21(2) _cell_angle_gamma 90.00 _cell_volume 3768(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 9.22 _cell_measurement_theta_max 11.09 _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1462 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'AFC6S' _diffrn_measurement_method /w--2/q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -1.257 _diffrn_reflns_number 5138 _diffrn_reflns_av_R_equivalents 0.088 _diffrn_reflns_av_sigmaI/netI 0.1710 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 22.51 _reflns_number_total 5138 _reflns_number_gt 2322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'teXsan' _computing_cell_refinement 'teXsan' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms of the methanol molecules were placed using the HFIX 137 and HFIX 147 commands. The thermal parameters of C42 were restrained using the ISOR, SIMU, and DELU commands. Reflection 0 1 1 was omitted from the refinement. The phenyl ring comprising C64 to C69 was restrained using the ISOR and SIMU commands. The t-butyl group containing C17 to C19 was disordered over two positions. The occupancy of these positions refined to 0.56 and 0.44. C17, C18 and C19 were refined isotropically. Cl4 of a dichloromethane molecule was disordered over two positions (Cl4 and Cl4a), the occupancy of each position refined to 0.5. ; _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^)+(0.1072P)^2^+5.3182P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(6) _refine_ls_number_reflns 5138 _refine_ls_number_parameters 833 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.1932 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.2319 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.25168(19) 0.00412(15) 0.22409(9) 0.0373(6) Uani 1 1 d . . . O1 O 0.2940(10) 0.0631(7) 0.3118(5) 0.049(3) Uani 1 1 d . . . O2 O 0.1069(9) 0.0098(9) 0.2923(4) 0.045(3) Uani 1 1 d . . . O3 O 0.1702(11) 0.0517(8) 0.3864(5) 0.067(4) Uani 1 1 d . . . O4 O 0.3222(10) -0.1004(7) 0.2748(5) 0.046(3) Uani 1 1 d . . . H4 H 0.3725 -0.1314 0.2517 0.055 Uiso 1 1 calc R . . N1 N 0.4312(10) 0.0096(11) 0.1899(5) 0.041(3) Uani 1 1 d . . . N2 N 0.1887(15) 0.1014(9) 0.1665(6) 0.038(4) Uani 1 1 d . . . N3 N 0.1741(14) -0.0717(8) 0.1528(6) 0.036(4) Uani 1 1 d . . . N4 N 0.1872(14) 0.0407(8) 0.3329(6) 0.044(4) Uani 1 1 d . . . C70 C 0.3135(18) -0.1354(12) 0.3338(8) 0.068(6) Uani 1 1 d . . . H70A H 0.3619 -0.1842 0.3374 0.101 Uiso 1 1 calc R . . H70B H 0.2243 -0.1462 0.3380 0.101 Uiso 1 1 calc R . . H70C H 0.3484 -0.0994 0.3660 0.101 Uiso 1 1 calc R . . C71 C 0.483(2) 0.2171(13) 0.3144(9) 0.075(6) Uani 1 1 d . . . H71A H 0.4636 0.1610 0.3174 0.090 Uiso 1 1 calc R . . H71B H 0.5659 0.2267 0.3395 0.090 Uiso 1 1 calc R . . Cl1 Cl 0.4986(8) 0.2403(4) 0.2363(3) 0.109(2) Uani 1 1 d . . . Cl2 Cl 0.3637(7) 0.2723(4) 0.3441(3) 0.111(2) Uani 1 1 d . . . C1 C 0.4297(12) 0.0120(14) 0.1236(6) 0.042(4) Uani 1 1 d . . . H1 H 0.5197 0.0111 0.1144 0.051 Uiso 1 1 calc R . . C2 C 0.3595(18) -0.0593(12) 0.0918(8) 0.050(6) Uani 1 1 d . . . H2A H 0.3929 -0.1075 0.1125 0.060 Uiso 1 1 calc R . . H2B H 0.3782 -0.0617 0.0493 0.060 Uiso 1 1 calc R . . C3 C 0.2099(19) -0.0566(11) 0.0920(9) 0.047(5) Uani 1 1 d . . . H3 H 0.1725 -0.0992 0.0647 0.056 Uiso 1 1 calc R . . C4 C 0.1543(13) 0.0213(11) 0.0654(7) 0.046(5) Uani 1 1 d . . . H4A H 0.0621 0.0230 0.0686 0.055 Uiso 1 1 calc R . . H4B H 0.1654 0.0242 0.0218 0.055 Uiso 1 1 calc R . . C5 C 0.2220(16) 0.0943(11) 0.1001(8) 0.041(5) Uani 1 1 d . . . H5 H 0.1903 0.1423 0.0777 0.049 Uiso 1 1 calc R . . C6 C 0.3679(16) 0.0899(11) 0.0988(9) 0.044(5) Uani 1 1 d . . . H6A H 0.4086 0.1336 0.1231 0.053 Uiso 1 1 calc R . . H6B H 0.3856 0.0971 0.0563 0.053 Uiso 1 1 calc R . . C7 C 0.5424(14) 0.0139(12) 0.2226(6) 0.041(4) Uani 1 1 d . . . H7 H 0.6141 0.0169 0.2011 0.049 Uiso 1 1 calc R . . C8 C 0.5677(14) 0.0147(12) 0.2888(6) 0.043(4) Uani 1 1 d . . . H8 H 0.4985 0.0066 0.3114 0.052 Uiso 1 1 calc R . . C9 C 0.6867(14) 0.0266(10) 0.3204(6) 0.040(5) Uani 1 1 d . . . H9 H 0.7539 0.0358 0.2968 0.048 Uiso 1 1 calc R . . C10 C 0.7203(13) 0.0265(10) 0.3858(6) 0.039(5) Uani 1 1 d . . . C11 C 0.8488(16) 0.0285(10) 0.4143(8) 0.051(5) Uani 1 1 d . . . H11 H 0.9144 0.0298 0.3889 0.061 Uiso 1 1 calc R . . C12 C 0.8855(16) 0.0287(10) 0.4791(7) 0.050(5) Uani 1 1 d . . . H12 H 0.9730 0.0298 0.4947 0.060 Uiso 1 1 calc R . . C13 C 0.7931(16) 0.0274(11) 0.5195(7) 0.048(5) Uani 1 1 d . . . C14 C 0.6647(16) 0.0259(13) 0.4922(7) 0.060(6) Uani 1 1 d . . . H14 H 0.5993 0.0234 0.5177 0.072 Uiso 1 1 calc R . . C15 C 0.6310(15) 0.0278(11) 0.4296(8) 0.054(5) Uani 1 1 d . . . H15 H 0.5432 0.0301 0.4147 0.065 Uiso 1 1 calc R . . C16 C 0.8311(16) 0.0257(13) 0.5887(8) 0.065(6) Uani 1 1 d . . . C17 C 0.959(5) 0.054(4) 0.611(2) 0.081(15) Uiso 0.44 1 d P . . H17A H 0.9978 0.0757 0.5765 0.121 Uiso 0.44 1 calc PR . . H17B H 1.0105 0.0112 0.6290 0.121 Uiso 0.44 1 calc PR . . H17C H 0.9528 0.0951 0.6410 0.121 Uiso 0.44 1 calc PR . . C17A C 0.975(3) -0.001(3) 0.6070(15) 0.062(9) Uiso 0.56 1 d P . . H17D H 1.0303 0.0282 0.5828 0.093 Uiso 0.56 1 calc PR . . H17E H 0.9828 -0.0568 0.5992 0.093 Uiso 0.56 1 calc PR . . H17F H 1.0005 0.0096 0.6502 0.093 Uiso 0.56 1 calc PR . . C18 C 0.808(4) -0.054(2) 0.6150(18) 0.046(11) Uiso 0.44 1 d P . . H18A H 0.8761 -0.0895 0.6068 0.070 Uiso 0.44 1 calc PR . . H18B H 0.7261 -0.0741 0.5962 0.070 Uiso 0.44 1 calc PR . . H18C H 0.8073 -0.0493 0.6589 0.070 Uiso 0.44 1 calc PR . . C18A C 0.722(4) -0.011(3) 0.6221(18) 0.097(14) Uiso 0.56 1 d P . . H18D H 0.7237 -0.0681 0.6180 0.146 Uiso 0.56 1 calc PR . . H18E H 0.6395 0.0086 0.6037 0.146 Uiso 0.56 1 calc PR . . H18F H 0.7356 0.0028 0.6652 0.146 Uiso 0.56 1 calc PR . . C19 C 0.758(4) 0.086(3) 0.6185(19) 0.055(12) Uiso 0.44 1 d P . . H19A H 0.7922 0.1374 0.6112 0.082 Uiso 0.44 1 calc PR . . H19B H 0.7665 0.0756 0.6623 0.082 Uiso 0.44 1 calc PR . . H19C H 0.6687 0.0832 0.6015 0.082 Uiso 0.44 1 calc PR . . C19A C 0.840(4) 0.119(2) 0.6113(18) 0.076(11) Uiso 0.56 1 d P . . H19D H 0.9066 0.1459 0.5923 0.114 Uiso 0.56 1 calc PR . . H19E H 0.8603 0.1214 0.6556 0.114 Uiso 0.56 1 calc PR . . H19F H 0.7582 0.1449 0.5992 0.114 Uiso 0.56 1 calc PR . . C20 C 0.0971(17) -0.1315(11) 0.1598(8) 0.039(5) Uani 1 1 d . . . H20 H 0.0762 -0.1641 0.1254 0.047 Uiso 1 1 calc R . . C21 C 0.0407(18) -0.1528(12) 0.2149(10) 0.056(6) Uani 1 1 d . . . H21 H 0.0602 -0.1195 0.2489 0.067 Uiso 1 1 calc R . . C22 C -0.0321(18) -0.2115(10) 0.2225(9) 0.046(5) Uani 1 1 d . . . H22 H -0.0487 -0.2462 0.1891 0.055 Uiso 1 1 calc R . . C23 C -0.0942(16) -0.2313(12) 0.2787(8) 0.041(5) Uani 1 1 d . . . C24 C -0.1045(17) -0.1748(11) 0.3230(8) 0.050(5) Uani 1 1 d . . . H24 H -0.0735 -0.1236 0.3181 0.060 Uiso 1 1 calc R . . C25 C -0.1621(17) -0.1944(12) 0.3760(8) 0.055(5) Uani 1 1 d . . . H25 H -0.1619 -0.1561 0.4069 0.066 Uiso 1 1 calc R . . C26 C -0.2180(16) -0.2658(11) 0.3852(8) 0.040(5) Uani 1 1 d . . . C27 C -0.2109(19) -0.3208(10) 0.3359(9) 0.045(5) Uani 1 1 d . . . H27 H -0.2510 -0.3700 0.3383 0.054 Uiso 1 1 calc R . . C28 C -0.148(2) -0.3057(12) 0.2851(9) 0.051(5) Uani 1 1 d . . . H28 H -0.1420 -0.3449 0.2554 0.061 Uiso 1 1 calc R . . C29 C -0.296(2) -0.2864(13) 0.4396(11) 0.069(6) Uani 1 1 d . . . C30 C -0.324(3) -0.2126(18) 0.4721(13) 0.135(13) Uani 1 1 d . . . H30A H -0.3743 -0.1776 0.4436 0.203 Uiso 1 1 calc R . . H30B H -0.2438 -0.1869 0.4878 0.203 Uiso 1 1 calc R . . H30C H -0.3715 -0.2251 0.5058 0.203 Uiso 1 1 calc R . . C31 C -0.427(2) -0.322(2) 0.4157(13) 0.140(12) Uani 1 1 d . . . H31A H -0.4152 -0.3711 0.3944 0.210 Uiso 1 1 calc R . . H31B H -0.4752 -0.2855 0.3877 0.210 Uiso 1 1 calc R . . H31C H -0.4750 -0.3325 0.4500 0.210 Uiso 1 1 calc R . . C32 C -0.221(4) -0.344(3) 0.4781(18) 0.26(3) Uani 1 1 d . . . H32A H -0.2099 -0.3910 0.4543 0.388 Uiso 1 1 calc R . . H32B H -0.2660 -0.3573 0.5127 0.388 Uiso 1 1 calc R . . H32C H -0.1377 -0.3220 0.4929 0.388 Uiso 1 1 calc R . . C33 C 0.1181(18) 0.1621(13) 0.1737(8) 0.043(5) Uani 1 1 d . . . H33 H 0.0964 0.1956 0.1400 0.052 Uiso 1 1 calc R . . C34 C 0.0712(17) 0.1810(11) 0.2305(9) 0.046(5) Uani 1 1 d . . . H34 H 0.0980 0.1501 0.2652 0.055 Uiso 1 1 calc R . . C35 C -0.0137(18) 0.2442(12) 0.2361(9) 0.050(5) Uani 1 1 d . . . H35 H -0.0363 0.2769 0.2019 0.060 Uiso 1 1 calc R . . C36 C -0.0712(18) 0.2623(11) 0.2959(9) 0.048(5) Uani 1 1 d . . . C37 C -0.046(2) 0.2214(13) 0.3497(9) 0.070(7) Uani 1 1 d . . . H37 H 0.0068 0.1767 0.3518 0.084 Uiso 1 1 calc R . . C38 C -0.100(2) 0.2461(16) 0.4015(11) 0.088(8) Uani 1 1 d . . . H38 H -0.0757 0.2199 0.4388 0.106 Uiso 1 1 calc R . . C39 C -0.188(2) 0.3083(11) 0.4001(9) 0.051(5) Uani 1 1 d . . . C40 C -0.2133(18) 0.3490(13) 0.3460(10) 0.057(6) Uani 1 1 d . . . H40 H -0.2681 0.3928 0.3442 0.068 Uiso 1 1 calc R . . C41 C -0.158(2) 0.3260(14) 0.2922(11) 0.069(7) Uani 1 1 d . . . H41 H -0.1800 0.3529 0.2549 0.082 Uiso 1 1 calc R . . C42 C -0.2380(19) 0.3309(13) 0.4627(9) 0.057(5) Uani 1 1 d U . . C43 C -0.131(2) 0.3541(16) 0.5105(9) 0.094(8) Uani 1 1 d . . . H43A H -0.0717 0.3105 0.5182 0.141 Uiso 1 1 calc R . . H43B H -0.1658 0.3675 0.5481 0.141 Uiso 1 1 calc R . . H43C H -0.0867 0.3993 0.4964 0.141 Uiso 1 1 calc R . . C44 C -0.328(2) 0.4050(15) 0.4530(10) 0.091(8) Uani 1 1 d . . . H44A H -0.4006 0.3931 0.4223 0.137 Uiso 1 1 calc R . . H44B H -0.2808 0.4491 0.4393 0.137 Uiso 1 1 calc R . . H44C H -0.3597 0.4184 0.4914 0.137 Uiso 1 1 calc R . . C45 C -0.314(2) 0.2608(17) 0.4826(10) 0.097(9) Uani 1 1 d . . . H45A H -0.3829 0.2482 0.4506 0.145 Uiso 1 1 calc R . . H45B H -0.3491 0.2739 0.5201 0.145 Uiso 1 1 calc R . . H45C H -0.2571 0.2157 0.4899 0.145 Uiso 1 1 calc R . . C46 C 0.1861(16) 0.4187(11) 0.0889(9) 0.059(6) Uani 1 1 d . . . C47 C 0.0696(19) 0.4587(14) 0.0842(9) 0.081(7) Uani 1 1 d . . . H47 H 0.0311 0.4756 0.0455 0.097 Uiso 1 1 calc R . . C48 C 0.0065(19) 0.4749(17) 0.1376(13) 0.113(11) Uani 1 1 d . . . H48 H -0.0689 0.5052 0.1336 0.135 Uiso 1 1 calc R . . C49 C 0.0548(19) 0.4467(16) 0.1931(12) 0.093(8) Uani 1 1 d . . . H49 H 0.0118 0.4568 0.2273 0.112 Uiso 1 1 calc R . . C50 C 0.168(2) 0.4030(14) 0.2002(11) 0.078(7) Uani 1 1 d . . . H50 H 0.2004 0.3828 0.2388 0.094 Uiso 1 1 calc R . . C51 C 0.231(2) 0.3898(14) 0.1496(10) 0.078(8) Uani 1 1 d . . . H51 H 0.3071 0.3603 0.1550 0.094 Uiso 1 1 calc R . . C52 C 0.4171(18) 0.3853(12) 0.0480(8) 0.058(5) Uani 1 1 d . . . C53 C 0.5051(18) 0.4475(14) 0.0488(8) 0.064(6) Uani 1 1 d . . . H53 H 0.4756 0.4974 0.0348 0.077 Uiso 1 1 calc R . . C54 C 0.629(3) 0.438(3) 0.0688(11) 0.132(15) Uani 1 1 d . . . H54 H 0.6845 0.4814 0.0680 0.159 Uiso 1 1 calc R . . C55 C 0.682(3) 0.365(4) 0.0913(13) 0.16(2) Uani 1 1 d . . . H55 H 0.7711 0.3592 0.1023 0.191 Uiso 1 1 calc R . . C56 C 0.606(3) 0.307(2) 0.0963(11) 0.133(16) Uani 1 1 d . . . H56 H 0.6414 0.2603 0.1147 0.159 Uiso 1 1 calc R . . C57 C 0.463(2) 0.3084(15) 0.0743(10) 0.087(7) Uani 1 1 d . . . H57 H 0.4082 0.2649 0.0772 0.105 Uiso 1 1 calc R . . C58 C 0.232(2) 0.4618(13) -0.0264(10) 0.058(6) Uani 1 1 d . . . C59 C 0.1966(17) 0.4419(14) -0.0895(10) 0.066(7) Uani 1 1 d . . . H59 H 0.1868 0.3887 -0.1010 0.079 Uiso 1 1 calc R . . C60 C 0.1756(15) 0.503(2) -0.1361(10) 0.081(8) Uani 1 1 d . . . H60 H 0.1485 0.4903 -0.1773 0.098 Uiso 1 1 calc R . . C61 C 0.197(3) 0.5803(19) -0.1173(15) 0.094(10) Uani 1 1 d . . . H61 H 0.1910 0.6198 -0.1475 0.113 Uiso 1 1 calc R . . C62 C 0.226(3) 0.6011(15) -0.0600(12) 0.107(10) Uani 1 1 d . . . H62 H 0.2346 0.6544 -0.0487 0.128 Uiso 1 1 calc R . . C63 C 0.243(2) 0.5396(14) -0.0150(11) 0.075(8) Uani 1 1 d . . . H63 H 0.2630 0.5550 0.0261 0.090 Uiso 1 1 calc R . . C64 C 0.188(2) 0.3109(15) -0.0007(9) 0.079(7) Uani 1 1 d U . . C65 C 0.057(2) 0.2927(16) 0.0100(12) 0.118(10) Uani 1 1 d U . . H65 H 0.0112 0.3237 0.0352 0.142 Uiso 1 1 calc R . . C66 C 0.003(3) 0.222(2) -0.0215(15) 0.134(12) Uani 1 1 d U . . H66 H -0.0826 0.2090 -0.0171 0.161 Uiso 1 1 calc R . . C67 C 0.069(4) 0.174(2) -0.0575(17) 0.140(12) Uani 1 1 d U . . H67 H 0.0292 0.1290 -0.0755 0.168 Uiso 1 1 calc R . . C68 C 0.186(4) 0.1914(19) -0.0666(15) 0.135(10) Uani 1 1 d U . . H68 H 0.2279 0.1592 -0.0924 0.162 Uiso 1 1 calc R . . C69 C 0.255(3) 0.2620(15) -0.0363(11) 0.102(8) Uani 1 1 d U . . H69 H 0.3405 0.2726 -0.0415 0.123 Uiso 1 1 calc R . . B1 B 0.258(2) 0.3935(13) 0.0270(11) 0.055(6) Uani 1 1 d . . . Cl3 Cl 0.5088(7) -0.0207(6) 0.7159(3) 0.135(4) Uani 1 1 d . . . Cl4 Cl 0.2984(16) 0.0223(13) 0.7808(7) 0.093(5) Uani 0.50 1 d P . . Cl4A Cl 0.344(5) 0.052(4) 0.803(2) 0.42(5) Uani 0.50 1 d P . . C75 C 0.455(2) -0.0181(15) 0.7884(10) 0.096(9) Uani 1 1 d . . . H75A H 0.4182 -0.0698 0.7956 0.115 Uiso 1 1 calc R . . H75B H 0.5305 -0.0116 0.8190 0.115 Uiso 1 1 calc R . . O5 O 0.4447(14) -0.2029(10) 0.2139(7) 0.085(5) Uani 1 1 d . . . H5 H 0.4153 -0.2413 0.1935 0.127 Uiso 1 1 calc R . . C76 C 0.580(2) -0.2028(17) 0.2172(13) 0.120(11) Uani 1 1 d . . . H76A H 0.6047 -0.1856 0.1782 0.180 Uiso 1 1 calc R . . H76B H 0.6123 -0.2555 0.2263 0.180 Uiso 1 1 calc R . . H76C H 0.6158 -0.1671 0.2493 0.180 Uiso 1 1 calc R . . O7 O 0.260(3) -0.4036(14) 0.1571(11) 0.153(9) Uani 1 1 d . . . H7A H 0.2683 -0.4515 0.1636 0.230 Uiso 1 1 calc R . . C79 C 0.215(3) -0.3656(12) 0.2100(11) 0.19(2) Uani 1 1 d . . . H79A H 0.2161 -0.4034 0.2432 0.279 Uiso 1 1 calc R . . H79B H 0.1286 -0.3464 0.1987 0.279 Uiso 1 1 calc R . . H79C H 0.2714 -0.3219 0.2233 0.279 Uiso 1 1 calc R . . O6 O 0.344(2) -0.2799(12) 0.1083(9) 0.228(15) Uani 1 1 d R . . H6 H 0.3585 -0.3198 0.1297 0.342 Uiso 1 1 calc R . . C77 C 0.418(2) -0.2807(13) 0.0623(9) 0.24(3) Uani 1 1 d R . . H77A H 0.3849 -0.2426 0.0314 0.357 Uiso 1 1 calc R . . H77B H 0.4157 -0.3328 0.0442 0.357 Uiso 1 1 calc R . . H77C H 0.5051 -0.2673 0.0784 0.357 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 0.0351(12) 0.0481(14) 0.0303(11) -0.0031(14) 0.0108(9) -0.0055(15) O1 0.045(7) 0.060(8) 0.044(7) -0.009(6) 0.020(6) -0.009(6) O2 0.044(6) 0.054(7) 0.039(6) -0.009(8) 0.008(5) 0.001(8) O3 0.061(8) 0.110(11) 0.033(7) -0.013(7) 0.021(6) 0.001(7) O4 0.053(7) 0.049(8) 0.039(7) 0.005(6) 0.017(6) -0.002(6) N1 0.032(7) 0.065(9) 0.026(7) 0.012(9) -0.002(5) -0.007(10) N2 0.045(10) 0.031(9) 0.040(9) -0.006(7) 0.011(7) 0.002(8) N3 0.039(9) 0.048(10) 0.023(8) -0.006(7) 0.013(7) -0.005(8) N4 0.047(10) 0.055(10) 0.030(9) 0.003(7) 0.008(7) -0.001(8) C70 0.068(13) 0.085(16) 0.051(12) 0.025(11) 0.014(10) 0.016(12) C71 0.071(15) 0.072(16) 0.079(15) -0.011(13) -0.004(12) 0.001(12) Cl1 0.142(7) 0.095(5) 0.084(5) -0.019(4) -0.014(4) 0.011(5) Cl2 0.132(6) 0.105(6) 0.095(5) -0.008(4) 0.012(4) 0.022(4) C1 0.022(7) 0.071(12) 0.035(9) -0.007(12) 0.011(6) -0.006(12) C2 0.053(14) 0.071(15) 0.028(10) 0.004(10) 0.006(10) 0.007(11) C3 0.059(14) 0.033(12) 0.048(12) -0.001(9) 0.006(10) 0.003(9) C4 0.023(8) 0.061(14) 0.056(10) -0.002(10) 0.011(7) -0.012(10) C5 0.029(10) 0.052(12) 0.043(11) 0.020(9) 0.007(8) 0.006(9) C6 0.031(11) 0.044(12) 0.056(12) 0.017(10) 0.000(9) -0.007(9) C7 0.046(10) 0.043(10) 0.037(9) 0.020(10) 0.021(7) -0.016(10) C8 0.051(10) 0.050(11) 0.033(9) 0.024(10) 0.020(7) -0.012(11) C9 0.039(10) 0.057(14) 0.025(9) 0.012(8) 0.009(7) -0.015(9) C10 0.029(9) 0.059(14) 0.030(9) -0.015(9) 0.001(7) -0.009(9) C11 0.048(11) 0.047(14) 0.062(12) 0.014(9) 0.025(9) -0.005(9) C12 0.050(10) 0.062(15) 0.036(10) 0.019(9) 0.002(8) -0.010(10) C13 0.056(11) 0.063(16) 0.024(9) 0.012(9) 0.000(8) -0.006(10) C14 0.041(10) 0.10(2) 0.034(10) 0.010(11) 0.000(8) 0.002(12) C15 0.034(10) 0.056(15) 0.070(13) 0.007(10) -0.004(9) 0.010(9) C16 0.043(10) 0.084(19) 0.068(13) 0.013(12) 0.005(9) -0.008(12) C20 0.044(12) 0.044(12) 0.029(10) -0.016(8) 0.004(9) -0.024(10) C21 0.051(13) 0.042(13) 0.073(15) -0.002(11) 0.004(11) -0.016(11) C22 0.057(13) 0.015(10) 0.066(13) 0.000(9) 0.007(10) -0.005(10) C23 0.027(11) 0.053(13) 0.040(11) 0.008(10) -0.007(8) -0.014(9) C24 0.072(14) 0.038(12) 0.041(11) 0.012(10) 0.010(10) -0.033(10) C25 0.056(12) 0.053(14) 0.057(13) -0.018(11) 0.012(10) -0.009(11) C26 0.036(11) 0.030(11) 0.058(12) 0.023(10) 0.016(9) 0.007(9) C27 0.072(15) 0.019(10) 0.048(12) 0.002(9) 0.022(11) -0.022(9) C28 0.062(14) 0.049(14) 0.044(13) -0.004(10) 0.011(11) -0.012(11) C29 0.061(15) 0.052(14) 0.095(18) 0.007(13) 0.016(13) -0.002(11) C30 0.18(3) 0.12(2) 0.13(2) -0.03(2) 0.12(2) -0.06(2) C31 0.070(17) 0.20(3) 0.17(3) -0.02(2) 0.080(18) -0.06(2) C32 0.20(4) 0.42(7) 0.19(4) 0.22(5) 0.15(3) 0.16(5) C33 0.040(12) 0.064(14) 0.026(10) 0.003(9) 0.007(9) -0.009(11) C34 0.036(11) 0.051(13) 0.052(12) 0.020(10) 0.010(9) -0.001(10) C35 0.047(12) 0.051(13) 0.053(12) -0.013(10) 0.010(10) -0.009(11) C36 0.043(12) 0.037(12) 0.067(14) 0.006(10) 0.022(10) 0.004(10) C37 0.102(17) 0.070(16) 0.044(12) 0.018(12) 0.036(12) 0.039(13) C38 0.088(18) 0.10(2) 0.075(16) -0.017(15) 0.012(13) 0.040(17) C39 0.069(14) 0.035(12) 0.051(13) 0.000(10) 0.017(10) -0.021(10) C40 0.031(12) 0.076(16) 0.063(15) -0.021(12) 0.007(10) 0.014(11) C41 0.053(14) 0.076(17) 0.077(17) -0.021(14) 0.010(12) 0.009(13) C42 0.052(9) 0.067(9) 0.057(9) 0.007(8) 0.031(8) -0.004(8) C43 0.095(17) 0.15(2) 0.045(13) -0.043(14) 0.023(12) -0.038(17) C44 0.100(19) 0.109(19) 0.075(16) 0.009(15) 0.047(14) 0.026(16) C45 0.11(2) 0.15(3) 0.042(13) 0.002(15) 0.029(13) -0.021(19) C46 0.038(11) 0.048(12) 0.087(15) 0.035(11) -0.005(10) -0.022(10) C47 0.056(13) 0.13(2) 0.056(13) 0.047(13) 0.001(10) 0.037(13) C48 0.037(13) 0.16(3) 0.14(2) 0.06(2) 0.008(14) 0.022(14) C49 0.025(12) 0.14(2) 0.12(2) 0.056(18) 0.002(12) 0.011(13) C50 0.076(18) 0.092(18) 0.064(15) 0.049(14) -0.001(13) -0.026(14) C51 0.067(15) 0.097(19) 0.063(15) 0.040(14) -0.024(13) -0.006(13) C52 0.050(12) 0.064(15) 0.055(12) -0.007(11) -0.009(9) 0.000(11) C53 0.038(12) 0.119(19) 0.035(11) -0.021(11) 0.009(9) -0.008(12) C54 0.06(2) 0.31(5) 0.034(15) -0.04(2) 0.001(13) -0.06(2) C55 0.031(17) 0.41(8) 0.035(17) -0.01(3) 0.013(13) 0.02(3) C56 0.10(2) 0.25(4) 0.045(15) -0.04(2) 0.002(17) 0.13(3) C57 0.091(18) 0.084(19) 0.083(17) 0.016(15) -0.004(14) 0.022(15) C58 0.059(14) 0.052(16) 0.061(15) -0.009(12) -0.002(11) 0.002(12) C59 0.027(11) 0.093(17) 0.080(17) 0.050(15) 0.018(11) -0.007(11) C60 0.025(10) 0.15(2) 0.070(14) 0.06(2) 0.009(8) 0.004(16) C61 0.077(18) 0.09(2) 0.13(3) 0.06(2) 0.074(18) 0.037(16) C62 0.20(3) 0.062(18) 0.062(16) 0.006(15) 0.040(18) 0.056(18) C63 0.12(2) 0.055(16) 0.066(15) 0.017(12) 0.064(14) 0.033(14) C64 0.106(17) 0.073(15) 0.046(12) 0.022(11) -0.034(11) -0.020(13) C65 0.100(17) 0.122(18) 0.111(16) 0.096(14) -0.074(14) -0.091(15) C66 0.12(2) 0.13(2) 0.13(2) 0.098(18) -0.064(18) -0.059(18) C67 0.17(3) 0.09(2) 0.14(2) 0.074(18) -0.04(2) -0.04(2) C68 0.17(2) 0.11(2) 0.113(19) 0.030(16) -0.05(2) -0.02(2) C69 0.15(2) 0.070(16) 0.066(15) 0.007(13) -0.059(14) -0.013(16) B1 0.046(13) 0.036(14) 0.079(16) 0.015(12) -0.007(11) 0.005(11) Cl3 0.128(6) 0.209(11) 0.071(4) -0.008(5) 0.026(4) -0.013(6) Cl4 0.103(9) 0.113(13) 0.065(7) 0.022(8) 0.017(6) 0.090(10) Cl4A 0.47(7) 0.44(8) 0.40(6) 0.30(6) 0.25(6) 0.32(7) C75 0.082(15) 0.13(3) 0.088(16) 0.034(15) 0.044(13) 0.042(15) O5 0.088(11) 0.089(13) 0.079(12) 0.001(9) 0.016(9) 0.039(9) C76 0.036(14) 0.15(3) 0.17(3) -0.04(2) -0.004(15) 0.033(16) O7 0.16(2) 0.150(19) 0.163(19) 0.047(17) 0.085(16) 0.005(18) C79 0.12(3) 0.34(6) 0.12(3) -0.08(3) 0.08(2) 0.04(3) O6 0.27(3) 0.25(3) 0.19(2) -0.12(2) 0.12(2) -0.15(3) C77 0.31(6) 0.21(5) 0.23(5) 0.00(4) 0.19(5) -0.11(4) _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 N3 2.090(14) . ? Co1 N1 2.095(10) . ? Co1 N2 2.112(15) . ? Co1 O1 2.145(11) . ? Co1 O4 2.153(11) . ? Co1 O2 2.244(9) . ? O1 N4 1.307(15) . ? O2 N4 1.249(15) . ? O3 N4 1.214(15) . ? O4 C70 1.425(19) . ? N1 C7 1.281(16) . ? N1 C1 1.441(16) . ? N2 C33 1.28(2) . ? N2 C5 1.53(2) . ? N3 C20 1.31(2) . ? N3 C3 1.44(2) . ? C71 Cl2 1.74(2) . ? C71 Cl1 1.77(2) . ? C1 C2 1.52(3) . ? C1 C6 1.53(3) . ? C2 C3 1.56(2) . ? C3 C4 1.52(2) . ? C4 C5 1.56(2) . ? C5 C6 1.52(2) . ? C7 C8 1.430(18) . ? C8 C9 1.352(19) . ? C9 C10 1.419(19) . ? C10 C11 1.40(2) . ? C10 C15 1.41(2) . ? C11 C12 1.41(2) . ? C12 C13 1.38(2) . ? C13 C14 1.39(2) . ? C13 C16 1.51(2) . ? C14 C15 1.36(2) . ? C16 C17 1.43(5) . ? C16 C19 1.46(4) . ? C16 C18 1.49(4) . ? C16 C18A 1.55(4) . ? C16 C17A 1.56(4) . ? C16 C19A 1.65(4) . ? C17A C18 1.98(5) . ? C20 C21 1.44(3) . ? C21 C22 1.27(2) . ? C22 C23 1.49(3) . ? C23 C24 1.37(2) . ? C23 C28 1.39(3) . ? C24 C25 1.40(2) . ? C25 C26 1.36(2) . ? C26 C27 1.42(2) . ? C26 C29 1.55(3) . ? C27 C28 1.38(3) . ? C29 C32 1.44(4) . ? C29 C30 1.47(3) . ? C29 C31 1.53(3) . ? C33 C34 1.42(2) . ? C34 C35 1.40(3) . ? C35 C36 1.53(3) . ? C36 C37 1.35(2) . ? C36 C41 1.40(3) . ? C37 C38 1.38(3) . ? C38 C39 1.39(3) . ? C39 C40 1.36(3) . ? C39 C42 1.57(3) . ? C40 C41 1.42(3) . ? C42 C43 1.47(3) . ? C42 C45 1.51(3) . ? C42 C44 1.56(3) . ? C46 C47 1.38(2) . ? C46 C51 1.43(3) . ? C46 B1 1.67(3) . ? C47 C48 1.43(3) . ? C48 C49 1.33(3) . ? C49 C50 1.38(3) . ? C50 C51 1.37(3) . ? C52 C53 1.39(3) . ? C52 C57 1.47(3) . ? C52 B1 1.67(3) . ? C53 C54 1.32(3) . ? C54 C55 1.41(6) . ? C55 C56 1.27(5) . ? C56 C57 1.51(4) . ? C58 C63 1.33(3) . ? C58 C59 1.41(3) . ? C58 B1 1.63(3) . ? C59 C60 1.44(3) . ? C60 C61 1.37(4) . ? C61 C62 1.29(4) . ? C62 C63 1.42(3) . ? C64 C69 1.37(3) . ? C64 C65 1.45(3) . ? C64 B1 1.64(3) . ? C65 C66 1.44(4) . ? C66 C67 1.37(5) . ? C67 C68 1.28(4) . ? C68 C69 1.50(4) . ? Cl3 C75 1.739(19) . ? Cl4 Cl4A 0.81(8) . ? Cl4A C75 1.71(4) . ? O5 C76 1.40(2) . ? O7 C79 1.44(3) . ? O6 C77 1.3335(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 N1 92.4(6) . . ? N3 Co1 N2 88.3(5) . . ? N1 Co1 N2 88.8(6) . . ? N3 Co1 O1 163.4(5) . . ? N1 Co1 O1 101.7(5) . . ? N2 Co1 O1 100.5(5) . . ? N3 Co1 O4 87.5(5) . . ? N1 Co1 O4 87.5(5) . . ? N2 Co1 O4 174.3(5) . . ? O1 Co1 O4 84.4(5) . . ? N3 Co1 O2 106.7(5) . . ? N1 Co1 O2 159.0(4) . . ? N2 Co1 O2 100.1(5) . . ? O1 Co1 O2 58.2(4) . . ? O4 Co1 O2 84.8(4) . . ? N4 O1 Co1 95.2(9) . . ? N4 O2 Co1 92.3(8) . . ? C70 O4 Co1 137.9(11) . . ? C7 N1 C1 116.7(10) . . ? C7 N1 Co1 126.0(9) . . ? C1 N1 Co1 117.3(8) . . ? C33 N2 C5 112.3(15) . . ? C33 N2 Co1 133.3(13) . . ? C5 N2 Co1 114.1(11) . . ? C20 N3 C3 118.5(15) . . ? C20 N3 Co1 124.6(12) . . ? C3 N3 Co1 116.9(11) . . ? O3 N4 O2 125.1(13) . . ? O3 N4 O1 121.6(14) . . ? O2 N4 O1 113.3(12) . . ? Cl2 C71 Cl1 113.1(12) . . ? N1 C1 C2 112.1(16) . . ? N1 C1 C6 109.2(16) . . ? C2 C1 C6 111.0(12) . . ? C1 C2 C3 113.5(15) . . ? N3 C3 C4 111.9(15) . . ? N3 C3 C2 111.7(15) . . ? C4 C3 C2 110.9(15) . . ? C3 C4 C5 111.5(12) . . ? C6 C5 N2 111.5(14) . . ? C6 C5 C4 110.0(14) . . ? N2 C5 C4 112.1(13) . . ? C5 C6 C1 114.2(14) . . ? N1 C7 C8 126.7(12) . . ? C9 C8 C7 123.7(12) . . ? C8 C9 C10 127.1(13) . . ? C11 C10 C15 111.8(13) . . ? C11 C10 C9 123.0(13) . . ? C15 C10 C9 125.1(14) . . ? C10 C11 C12 124.4(14) . . ? C13 C12 C11 120.8(15) . . ? C12 C13 C14 115.8(14) . . ? C12 C13 C16 121.3(14) . . ? C14 C13 C16 122.9(14) . . ? C15 C14 C13 122.5(15) . . ? C14 C15 C10 124.5(15) . . ? C17 C16 C19 97(3) . . ? C17 C16 C18 111(3) . . ? C19 C16 C18 109(2) . . ? C17 C16 C13 116(2) . . ? C19 C16 C13 110(2) . . ? C18 C16 C13 111(2) . . ? C17 C16 C18A 133(3) . . ? C19 C16 C18A 68(3) . . ? C18 C16 C18A 45(2) . . ? C13 C16 C18A 111(2) . . ? C17 C16 C17A 37(2) . . ? C19 C16 C17A 128(3) . . ? C18 C16 C17A 81(2) . . ? C13 C16 C17A 112.4(18) . . ? C18A C16 C17A 120(2) . . ? C17 C16 C19A 64(3) . . ? C19 C16 C19A 38.8(19) . . ? C18 C16 C19A 139(2) . . ? C13 C16 C19A 106.2(19) . . ? C18A C16 C19A 105(3) . . ? C17A C16 C19A 100(2) . . ? C16 C17A C18 47.9(16) . . ? C16 C18 C17A 51.4(18) . . ? N3 C20 C21 127.3(16) . . ? C22 C21 C20 128(2) . . ? C21 C22 C23 127.4(19) . . ? C24 C23 C28 119.3(17) . . ? C24 C23 C22 120.3(16) . . ? C28 C23 C22 120.4(18) . . ? C23 C24 C25 119.7(16) . . ? C26 C25 C24 124.2(17) . . ? C25 C26 C27 113.6(15) . . ? C25 C26 C29 125.5(17) . . ? C27 C26 C29 120.7(16) . . ? C28 C27 C26 124.0(16) . . ? C27 C28 C23 119.0(19) . . ? C32 C29 C30 114(3) . . ? C32 C29 C31 109(3) . . ? C30 C29 C31 106(2) . . ? C32 C29 C26 107.5(19) . . ? C30 C29 C26 109.2(17) . . ? C31 C29 C26 111.0(19) . . ? N2 C33 C34 123.4(18) . . ? C35 C34 C33 122.5(18) . . ? C34 C35 C36 123.1(18) . . ? C37 C36 C41 119.4(19) . . ? C37 C36 C35 125.5(18) . . ? C41 C36 C35 115.0(19) . . ? C36 C37 C38 119.9(19) . . ? C37 C38 C39 123(2) . . ? C40 C39 C38 117.1(19) . . ? C40 C39 C42 125.4(19) . . ? C38 C39 C42 117.2(19) . . ? C39 C40 C41 121(2) . . ? C36 C41 C40 119(2) . . ? C43 C42 C45 112.1(18) . . ? C43 C42 C44 105.8(19) . . ? C45 C42 C44 109.6(18) . . ? C43 C42 C39 111.8(16) . . ? C45 C42 C39 107.7(17) . . ? C44 C42 C39 109.8(16) . . ? C47 C46 C51 114.5(19) . . ? C47 C46 B1 122.8(16) . . ? C51 C46 B1 122.1(18) . . ? C46 C47 C48 121.5(18) . . ? C49 C48 C47 121(2) . . ? C48 C49 C50 121(2) . . ? C51 C50 C49 119(2) . . ? C50 C51 C46 124(2) . . ? C53 C52 C57 118.7(18) . . ? C53 C52 B1 124.8(18) . . ? C57 C52 B1 116.1(18) . . ? C54 C53 C52 122(3) . . ? C53 C54 C55 123(3) . . ? C56 C55 C54 119(3) . . ? C55 C56 C57 124(4) . . ? C52 C57 C56 113(2) . . ? C63 C58 C59 115(2) . . ? C63 C58 B1 124(2) . . ? C59 C58 B1 121.5(19) . . ? C58 C59 C60 121(2) . . ? C61 C60 C59 118(2) . . ? C62 C61 C60 124(3) . . ? C61 C62 C63 117(3) . . ? C58 C63 C62 126(3) . . ? C69 C64 C65 121(2) . . ? C69 C64 B1 119(2) . . ? C65 C64 B1 120(2) . . ? C66 C65 C64 115(3) . . ? C67 C66 C65 124(4) . . ? C68 C67 C66 121(4) . . ? C67 C68 C69 121(4) . . ? C64 C69 C68 118(3) . . ? C58 B1 C64 108.0(16) . . ? C58 B1 C52 108.7(16) . . ? C64 B1 C52 113.9(16) . . ? C58 B1 C46 110.1(16) . . ? C64 B1 C46 106.8(16) . . ? C52 B1 C46 109.2(15) . . ? Cl4 Cl4A C75 79(4) . . ? Cl4A C75 Cl3 119.5(19) . . ? 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 N3 Co1 O1 N4 -20(2) . . . . ? N1 Co1 O1 N4 -167.2(9) . . . . ? N2 Co1 O1 N4 101.8(9) . . . . ? O4 Co1 O1 N4 -81.0(8) . . . . ? O2 Co1 O1 N4 6.4(8) . . . . ? N3 Co1 O2 N4 165.9(9) . . . . ? N1 Co1 O2 N4 11(2) . . . . ? N2 Co1 O2 N4 -102.9(10) . . . . ? O1 Co1 O2 N4 -6.6(8) . . . . ? O4 Co1 O2 N4 80.0(9) . . . . ? N3 Co1 O4 C70 -125.2(16) . . . . ? N1 Co1 O4 C70 142.3(16) . . . . ? N2 Co1 O4 C70 -168(5) . . . . ? O1 Co1 O4 C70 40.3(16) . . . . ? O2 Co1 O4 C70 -18.1(16) . . . . ? N3 Co1 N1 C7 -144.7(18) . . . . ? N2 Co1 N1 C7 127.0(18) . . . . ? O1 Co1 N1 C7 26.5(19) . . . . ? O4 Co1 N1 C7 -57.3(18) . . . . ? O2 Co1 N1 C7 11(3) . . . . ? N3 Co1 N1 C1 38.1(16) . . . . ? N2 Co1 N1 C1 -50.2(16) . . . . ? O1 Co1 N1 C1 -150.7(15) . . . . ? O4 Co1 N1 C1 125.5(16) . . . . ? O2 Co1 N1 C1 -166.0(15) . . . . ? N3 Co1 N2 C33 125.7(18) . . . . ? N1 Co1 N2 C33 -141.9(17) . . . . ? O1 Co1 N2 C33 -40.2(17) . . . . ? O4 Co1 N2 C33 169(4) . . . . ? O2 Co1 N2 C33 19.0(18) . . . . ? N3 Co1 N2 C5 -46.9(10) . . . . ? N1 Co1 N2 C5 45.5(11) . . . . ? O1 Co1 N2 C5 147.2(11) . . . . ? O4 Co1 N2 C5 -4(6) . . . . ? O2 Co1 N2 C5 -153.6(11) . . . . ? N1 Co1 N3 C20 140.8(14) . . . . ? N2 Co1 N3 C20 -130.4(16) . . . . ? O1 Co1 N3 C20 -8(3) . . . . ? O4 Co1 N3 C20 53.5(14) . . . . ? O2 Co1 N3 C20 -30.4(15) . . . . ? N1 Co1 N3 C3 -38.6(13) . . . . ? N2 Co1 N3 C3 50.2(12) . . . . ? O1 Co1 N3 C3 173.0(15) . . . . ? O4 Co1 N3 C3 -126.0(12) . . . . ? O2 Co1 N3 C3 150.2(12) . . . . ? Co1 O2 N4 O3 -171.6(14) . . . . ? Co1 O2 N4 O1 10.1(12) . . . . ? Co1 O1 N4 O3 171.0(13) . . . . ? Co1 O1 N4 O2 -10.6(13) . . . . ? C7 N1 C1 C2 125.1(18) . . . . ? Co1 N1 C1 C2 -57(2) . . . . ? C7 N1 C1 C6 -111.5(18) . . . . ? Co1 N1 C1 C6 66.0(18) . . . . ? N1 C1 C2 C3 71.8(19) . . . . ? C6 C1 C2 C3 -50.6(16) . . . . ? C20 N3 C3 C4 113.2(17) . . . . ? Co1 N3 C3 C4 -67.3(17) . . . . ? C20 N3 C3 C2 -121.7(18) . . . . ? Co1 N3 C3 C2 57.8(17) . . . . ? C1 C2 C3 N3 -72.3(19) . . . . ? C1 C2 C3 C4 53(2) . . . . ? N3 C3 C4 C5 70.4(17) . . . . ? C2 C3 C4 C5 -55.1(17) . . . . ? C33 N2 C5 C6 124.7(16) . . . . ? Co1 N2 C5 C6 -61.1(16) . . . . ? C33 N2 C5 C4 -111.5(17) . . . . ? Co1 N2 C5 C4 62.7(15) . . . . ? C3 C4 C5 C6 55.7(16) . . . . ? C3 C4 C5 N2 -68.9(16) . . . . ? N2 C5 C6 C1 70.6(19) . . . . ? C4 C5 C6 C1 -54(2) . . . . ? N1 C1 C6 C5 -71.9(18) . . . . ? C2 C1 C6 C5 52.2(17) . . . . ? C1 N1 C7 C8 178(2) . . . . ? Co1 N1 C7 C8 1(3) . . . . ? N1 C7 C8 C9 -174(2) . . . . ? C7 C8 C9 C10 -178.5(19) . . . . ? C8 C9 C10 C11 171.0(18) . . . . ? C8 C9 C10 C15 -12(3) . . . . ? C15 C10 C11 C12 2(2) . . . . ? C9 C10 C11 C12 179.9(16) . . . . ? C10 C11 C12 C13 0(3) . . . . ? C11 C12 C13 C14 0(3) . . . . ? C11 C12 C13 C16 178.6(17) . . . . ? C12 C13 C14 C15 -2(3) . . . . ? C16 C13 C14 C15 179.6(19) . . . . ? C13 C14 C15 C10 4(3) . . . . ? C11 C10 C15 C14 -4(3) . . . . ? C9 C10 C15 C14 178.4(18) . . . . ? C12 C13 C16 C17 22(4) . . . . ? C14 C13 C16 C17 -159(3) . . . . ? C12 C13 C16 C19 132(3) . . . . ? C14 C13 C16 C19 -50(3) . . . . ? C12 C13 C16 C18 -107(2) . . . . ? C14 C13 C16 C18 72(3) . . . . ? C12 C13 C16 C18A -155(2) . . . . ? C14 C13 C16 C18A 23(3) . . . . ? C12 C13 C16 C17A -18(3) . . . . ? C14 C13 C16 C17A 161(2) . . . . ? C12 C13 C16 C19A 91(2) . . . . ? C14 C13 C16 C19A -91(2) . . . . ? C17 C16 C17A C18 146(5) . . . . ? C19 C16 C17A C18 108(3) . . . . ? C13 C16 C17A C18 -109(2) . . . . ? C18A C16 C17A C18 24(3) . . . . ? C19A C16 C17A C18 138(2) . . . . ? C17 C16 C18 C17A -21(3) . . . . ? C19 C16 C18 C17A -127(3) . . . . ? C13 C16 C18 C17A 111(2) . . . . ? C18A C16 C18 C17A -151(3) . . . . ? C19A C16 C18 C17A -95(4) . . . . ? C3 N3 C20 C21 -174.2(18) . . . . ? Co1 N3 C20 C21 6(3) . . . . ? N3 C20 C21 C22 -178.6(19) . . . . ? C20 C21 C22 C23 -177.3(18) . . . . ? C21 C22 C23 C24 17(3) . . . . ? C21 C22 C23 C28 -166(2) . . . . ? C28 C23 C24 C25 4(3) . . . . ? C22 C23 C24 C25 -179.4(16) . . . . ? C23 C24 C25 C26 -5(3) . . . . ? C24 C25 C26 C27 1(3) . . . . ? C24 C25 C26 C29 -172.9(18) . . . . ? C25 C26 C27 C28 3(3) . . . . ? C29 C26 C27 C28 177.5(19) . . . . ? C26 C27 C28 C23 -4(3) . . . . ? C24 C23 C28 C27 0(3) . . . . ? C22 C23 C28 C27 -176.6(18) . . . . ? C25 C26 C29 C32 -112(3) . . . . ? C27 C26 C29 C32 74(3) . . . . ? C25 C26 C29 C30 12(3) . . . . ? C27 C26 C29 C30 -161(2) . . . . ? C25 C26 C29 C31 128(2) . . . . ? C27 C26 C29 C31 -45(3) . . . . ? C5 N2 C33 C34 178.4(16) . . . . ? Co1 N2 C33 C34 6(3) . . . . ? N2 C33 C34 C35 -175.1(17) . . . . ? C33 C34 C35 C36 176.3(17) . . . . ? C34 C35 C36 C37 1(3) . . . . ? C34 C35 C36 C41 -177.5(18) . . . . ? C41 C36 C37 C38 -5(3) . . . . ? C35 C36 C37 C38 177(2) . . . . ? C36 C37 C38 C39 5(4) . . . . ? C37 C38 C39 C40 -5(3) . . . . ? C37 C38 C39 C42 -179(2) . . . . ? C38 C39 C40 C41 3(3) . . . . ? C42 C39 C40 C41 177.1(19) . . . . ? C37 C36 C41 C40 3(3) . . . . ? C35 C36 C41 C40 -177.8(18) . . . . ? C39 C40 C41 C36 -3(3) . . . . ? C40 C39 C42 C43 -114(2) . . . . ? C38 C39 C42 C43 59(3) . . . . ? C40 C39 C42 C45 122(2) . . . . ? C38 C39 C42 C45 -64(3) . . . . ? C40 C39 C42 C44 3(3) . . . . ? C38 C39 C42 C44 176(2) . . . . ? C51 C46 C47 C48 5(3) . . . . ? B1 C46 C47 C48 176(2) . . . . ? C46 C47 C48 C49 -5(4) . . . . ? C47 C48 C49 C50 1(4) . . . . ? C48 C49 C50 C51 1(4) . . . . ? C49 C50 C51 C46 0(4) . . . . ? C47 C46 C51 C50 -3(3) . . . . ? B1 C46 C51 C50 -174(2) . . . . ? C57 C52 C53 C54 4(3) . . . . ? B1 C52 C53 C54 176.6(18) . . . . ? C52 C53 C54 C55 -1(4) . . . . ? C53 C54 C55 C56 -5(5) . . . . ? C54 C55 C56 C57 6(5) . . . . ? C53 C52 C57 C56 -3(3) . . . . ? B1 C52 C57 C56 -176.1(17) . . . . ? C55 C56 C57 C52 -2(4) . . . . ? C63 C58 C59 C60 0(3) . . . . ? B1 C58 C59 C60 -179.4(17) . . . . ? C58 C59 C60 C61 3(3) . . . . ? C59 C60 C61 C62 -5(4) . . . . ? C60 C61 C62 C63 4(4) . . . . ? C59 C58 C63 C62 -2(4) . . . . ? B1 C58 C63 C62 178(2) . . . . ? C61 C62 C63 C58 0(5) . . . . ? C69 C64 C65 C66 -2(3) . . . . ? B1 C64 C65 C66 174.4(16) . . . . ? C64 C65 C66 C67 2(3) . . . . ? C65 C66 C67 C68 -2(5) . . . . ? C66 C67 C68 C69 2(5) . . . . ? C65 C64 C69 C68 3(3) . . . . ? B1 C64 C69 C68 -173.9(18) . . . . ? C67 C68 C69 C64 -3(4) . . . . ? C63 C58 B1 C64 161(2) . . . . ? C59 C58 B1 C64 -19(3) . . . . ? C63 C58 B1 C52 -75(3) . . . . ? C59 C58 B1 C52 105(2) . . . . ? C63 C58 B1 C46 45(3) . . . . ? C59 C58 B1 C46 -135.6(19) . . . . ? C69 C64 B1 C58 84(2) . . . . ? C65 C64 B1 C58 -92(2) . . . . ? C69 C64 B1 C52 -36(3) . . . . ? C65 C64 B1 C52 146.6(17) . . . . ? C69 C64 B1 C46 -157.1(17) . . . . ? C65 C64 B1 C46 26(2) . . . . ? C53 C52 B1 C58 32(3) . . . . ? C57 C52 B1 C58 -155.3(18) . . . . ? C53 C52 B1 C64 152.9(18) . . . . ? C57 C52 B1 C64 -35(2) . . . . ? C53 C52 B1 C46 -88(2) . . . . ? C57 C52 B1 C46 85(2) . . . . ? C47 C46 B1 C58 35(2) . . . . ? C51 C46 B1 C58 -154.8(18) . . . . ? C47 C46 B1 C64 -82(2) . . . . ? C51 C46 B1 C64 88(2) . . . . ? C47 C46 B1 C52 154.4(18) . . . . ? C51 C46 B1 C52 -35(2) . . . . ? Cl4 Cl4A C75 Cl3 73(5) . . . . ? 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 O4 H4 O5 0.93 1.68 2.602(18) 168.3 . O5 H5 O6 0.82 2.01 2.73(2) 145.1 . O6 H6 O7 0.82 1.88 2.54(3) 136.2 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.369 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.085