# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Song Gao' _publ_contact_author_email GAOSONG@PKU.EDU.CN _publ_section_title ; Transition metal coordination frameworks with bridges of 1,2-bis(4-pyridyl)ethane-N,N'-dioxide incorporating anions of different size ; loop_ _publ_author_name 'Song Gao.' 'Stuart Batten' 'Hao-Ling Sun.' 'Zhe-Ming Wang.' # Attachment 'last-1.cif' data_last-1 _database_code_depnum_ccdc_archive 'CCDC 691371' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Cl2 Mn N6 O14' _chemical_formula_weight 902.55 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.6564(4) _cell_length_b 13.6564(4) _cell_length_c 6.1296(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 990.00(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15800 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 465 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18384 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 27.40 _reflns_number_total 1517 _reflns_number_gt 1132 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland maXus: a computer program for the solution and refinement of crystal structures from diffraction data, University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1240P)^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 1517 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1851 _refine_ls_wR_factor_gt 0.1766 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Mn1 Mn 0.0000 0.0000 0.5000 0.0336(3) Uani 1 6 d S . . Cl1 Cl 0.3333 0.6667 0.7384(4) 0.0884(6) Uani 1 3 d S . . O1 O 0.10531(15) 0.15388(15) 0.3163(3) 0.0479(5) Uani 1 1 d . . . O2 O 0.4329(5) 0.7483(6) 0.6564(14) 0.274(4) Uani 1 1 d . . . O3 O 0.3333 0.6667 0.9518(15) 0.280(7) Uani 1 3 d S . . N1 N 0.07991(17) 0.23494(17) 0.2778(3) 0.0409(5) Uani 1 1 d . . . C1 C -0.0209(3) 0.2099(2) 0.1992(4) 0.0497(7) Uani 1 1 d . . . H1 H -0.0753 0.1346 0.1758 0.060 Uiso 1 1 calc R . . C2 C -0.0458(3) 0.2933(2) 0.1523(5) 0.0551(8) Uani 1 1 d . . . H2 H -0.1172 0.2742 0.1006 0.066 Uiso 1 1 calc R . . C3 C 0.0361(3) 0.4070(2) 0.1819(4) 0.0530(8) Uani 1 1 d . . . C4 C 0.0125(3) 0.5000(3) 0.1210(5) 0.0628(9) Uani 1 1 d . . . H4A H 0.0774 0.5723 0.1593 0.075 Uiso 1 1 calc R . . H4B H -0.0516 0.4913 0.2047 0.075 Uiso 1 1 calc R . . C5 C 0.1381(3) 0.4284(2) 0.2670(5) 0.0619(8) Uani 1 1 d . . . H5 H 0.1945 0.5028 0.2912 0.074 Uiso 1 1 calc R . . C6 C 0.1582(3) 0.3427(2) 0.3166(5) 0.0566(8) Uani 1 1 d . . . H6 H 0.2270 0.3593 0.3782 0.068 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 Mn1 0.0297(4) 0.0297(4) 0.0414(5) 0.000 0.000 0.01483(19) Cl1 0.0743(7) 0.0743(7) 0.1165(14) 0.000 0.000 0.0372(4) O1 0.0481(11) 0.0415(10) 0.0616(12) 0.0168(8) 0.0134(8) 0.0280(9) O2 0.125(4) 0.203(6) 0.391(9) -0.094(6) 0.125(5) 0.005(4) O3 0.377(12) 0.377(12) 0.085(5) 0.000 0.000 0.189(6) N1 0.0462(12) 0.0357(11) 0.0444(12) 0.0078(8) 0.0056(9) 0.0231(10) C1 0.0527(17) 0.0362(13) 0.0580(16) 0.0035(11) -0.0068(12) 0.0206(12) C2 0.0582(17) 0.0448(16) 0.0673(18) 0.0044(13) -0.0107(14) 0.0296(14) C3 0.074(2) 0.0410(15) 0.0507(15) 0.0010(11) -0.0056(13) 0.0342(15) C4 0.092(2) 0.0448(16) 0.0647(18) 0.0006(13) -0.0068(17) 0.0436(17) C5 0.0642(19) 0.0372(15) 0.077(2) 0.0004(13) -0.0124(16) 0.0200(14) C6 0.0497(17) 0.0429(15) 0.0697(18) 0.0069(13) -0.0084(14) 0.0176(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.1748(17) 5_556 ? Mn1 O1 2.1748(17) 2 ? Mn1 O1 2.1748(17) 6_556 ? Mn1 O1 2.1748(17) 4_556 ? Mn1 O1 2.1748(17) . ? Mn1 O1 2.1748(17) 3 ? Cl1 O3 1.308(9) . ? Cl1 O2 1.352(5) 2_665 ? Cl1 O2 1.352(5) . ? Cl1 O2 1.352(5) 3_565 ? O1 N1 1.336(3) . ? N1 C1 1.331(4) . ? N1 C6 1.339(3) . ? C1 C2 1.372(4) . ? C1 H1 0.9300 . ? C2 C3 1.400(4) . ? C2 H2 0.9300 . ? C3 C5 1.376(4) . ? C3 C4 1.505(4) . ? C4 C4 1.522(6) 4_565 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.362(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O1 180.00(6) 5_556 2 ? O1 Mn1 O1 95.62(7) 5_556 6_556 ? O1 Mn1 O1 84.38(7) 2 6_556 ? O1 Mn1 O1 95.62(7) 5_556 4_556 ? O1 Mn1 O1 84.38(7) 2 4_556 ? O1 Mn1 O1 95.62(7) 6_556 4_556 ? O1 Mn1 O1 84.38(7) 5_556 . ? O1 Mn1 O1 95.62(7) 2 . ? O1 Mn1 O1 84.38(7) 6_556 . ? O1 Mn1 O1 180.00(8) 4_556 . ? O1 Mn1 O1 84.38(7) 5_556 3 ? O1 Mn1 O1 95.62(7) 2 3 ? O1 Mn1 O1 180.0 6_556 3 ? O1 Mn1 O1 84.38(7) 4_556 3 ? O1 Mn1 O1 95.62(7) . 3 ? O3 Cl1 O2 111.8(4) . 2_665 ? O3 Cl1 O2 111.8(4) . . ? O2 Cl1 O2 107.0(4) 2_665 . ? O3 Cl1 O2 111.8(4) . 3_565 ? O2 Cl1 O2 107.0(4) 2_665 3_565 ? O2 Cl1 O2 107.0(4) . 3_565 ? N1 O1 Mn1 124.88(14) . . ? C1 N1 O1 120.9(2) . . ? C1 N1 C6 120.1(2) . . ? O1 N1 C6 119.0(2) . . ? N1 C1 C2 121.1(3) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C1 C2 C3 120.1(3) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C5 C3 C2 116.5(2) . . ? C5 C3 C4 122.5(3) . . ? C2 C3 C4 121.0(3) . . ? C3 C4 C4 112.6(3) . 4_565 ? C3 C4 H4A 109.1 . . ? C4 C4 H4A 109.1 4_565 . ? C3 C4 H4B 109.1 . . ? C4 C4 H4B 109.1 4_565 . ? H4A C4 H4B 107.8 . . ? C6 C5 C3 121.3(3) . . ? C6 C5 H5 119.3 . . ? C3 C5 H5 119.3 . . ? N1 C6 C5 120.8(3) . . ? N1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.608 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.067 # Attachment 'last-2.cif' data_last-2 _database_code_depnum_ccdc_archive 'CCDC 691372' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Cl2 Cu N6 O16' _chemical_formula_weight 947.18 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' Cu Cu 0.3201 1.2651 '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 5.8754(2) _cell_length_b 13.3670(3) _cell_length_c 14.6338(4) _cell_angle_alpha 114.664(2) _cell_angle_beta 99.7320(10) _cell_angle_gamma 95.8000(10) _cell_volume 1010.34(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16524 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 489 _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18322 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4581 _reflns_number_gt 3030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland maXus: a computer program for the solution and refinement of crystal structures from diffraction data, University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0852P)^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 SHELXL _refine_ls_extinction_coef 0.009(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4581 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 Cu2 Cu 0.0000 0.0000 0.0000 0.03365(18) Uani 1 2 d S . . Cl1 Cl 0.3877(2) -0.28628(10) 0.33507(7) 0.0812(3) Uani 1 1 d . . . O1 O 0.1445(3) -0.10273(14) 0.04684(13) 0.0378(4) Uani 1 1 d . . . O2 O -0.0686(3) 0.09170(14) 0.13281(12) 0.0390(4) Uani 1 1 d . . . O3 O -0.4761(4) 0.2579(2) 0.25799(19) 0.0806(8) Uani 1 1 d . . . O4 O 0.4098(5) 0.1113(2) 0.0540(2) 0.0574(6) Uani 1 1 d . . . O5 O 0.3614(8) -0.2091(4) 0.2965(4) 0.185(3) Uani 1 1 d . . . O6 O 0.5714(11) -0.3438(7) 0.3062(5) 0.239(3) Uani 1 1 d . . . O7 O 0.1870(9) -0.3664(4) 0.2958(3) 0.1545(19) Uani 1 1 d . . . O8 O 0.4471(9) -0.2359(3) 0.4403(2) 0.1488(18) Uani 1 1 d . . . N1 N 0.0174(4) -0.20132(17) 0.03001(15) 0.0341(5) Uani 1 1 d . . . N2 N -0.0517(4) 0.05685(18) 0.20753(15) 0.0371(5) Uani 1 1 d . . . N3 N -0.2601(5) 0.3034(2) 0.3146(2) 0.0595(7) Uani 1 1 d . . . C1 C -0.1035(5) -0.2753(2) -0.0646(2) 0.0423(6) Uani 1 1 d . . . H1A H -0.1022 -0.2591 -0.1205 0.051 Uiso 1 1 calc R . . C2 C -0.2292(5) -0.3751(2) -0.0795(2) 0.0479(7) Uani 1 1 d . . . H2A H -0.3124 -0.4263 -0.1457 0.057 Uiso 1 1 calc R . . C3 C -0.2345(5) -0.4010(2) 0.0030(2) 0.0448(7) Uani 1 1 d . . . C4 C -0.3802(6) -0.5081(2) -0.0111(3) 0.0529(7) Uani 1 1 d . . . H4A H -0.2975 -0.5347 0.0350 0.063 Uiso 1 1 calc R . . H4B H -0.4000 -0.5649 -0.0815 0.063 Uiso 1 1 calc R . . C5 C -0.1063(6) -0.3223(3) 0.0985(2) 0.0531(8) Uani 1 1 d . . . H5A H -0.1057 -0.3363 0.1557 0.064 Uiso 1 1 calc R . . C6 C 0.0201(5) -0.2243(2) 0.1113(2) 0.0473(7) Uani 1 1 d . . . H6A H 0.1087 -0.1730 0.1765 0.057 Uiso 1 1 calc R . . C7 C -0.2446(6) -0.0007(3) 0.2141(2) 0.0506(7) Uani 1 1 d . . . H7A H -0.3861 -0.0187 0.1660 0.061 Uiso 1 1 calc R . . C8 C -0.2306(7) -0.0322(3) 0.2918(2) 0.0653(10) Uani 1 1 d . . . H8A H -0.3642 -0.0725 0.2956 0.078 Uiso 1 1 calc R . . C9 C -0.0232(8) -0.0059(3) 0.3653(2) 0.0686(11) Uani 1 1 d . . . C10 C -0.0046(12) -0.0399(3) 0.4523(3) 0.121(2) Uani 1 1 d . . . H10A H -0.1386 -0.0989 0.4341 0.145 Uiso 1 1 calc R . . H10B H 0.1354 -0.0721 0.4555 0.145 Uiso 1 1 calc R . . C11 C 0.1682(7) 0.0547(3) 0.3562(2) 0.0630(9) Uani 1 1 d . . . H11A H 0.3107 0.0750 0.4043 0.076 Uiso 1 1 calc R . . C12 C 0.1512(6) 0.0858(2) 0.2764(2) 0.0476(7) Uani 1 1 d . . . H12A H 0.2817 0.1268 0.2711 0.057 Uiso 1 1 calc R . . C13 C -0.1806(6) 0.2837(3) 0.3965(3) 0.0619(9) Uani 1 1 d . . . H13A H -0.2784 0.2355 0.4106 0.074 Uiso 1 1 calc R . . C14 C 0.0360(6) 0.3317(3) 0.4581(3) 0.0604(8) Uani 1 1 d . . . H14A H 0.0849 0.3162 0.5139 0.072 Uiso 1 1 calc R . . C15 C 0.1881(6) 0.4043(3) 0.4396(2) 0.0534(8) Uani 1 1 d . . . C16 C 0.4284(6) 0.4580(3) 0.5117(3) 0.0603(8) Uani 1 1 d . . . H16A H 0.5163 0.3994 0.5083 0.072 Uiso 1 1 calc R . . H16B H 0.4092 0.4957 0.5819 0.072 Uiso 1 1 calc R . . C17 C 0.1037(6) 0.4233(3) 0.3557(3) 0.0652(9) Uani 1 1 d . . . H17A H 0.1995 0.4708 0.3401 0.078 Uiso 1 1 calc R . . C18 C -0.1201(7) 0.3732(3) 0.2942(3) 0.0707(10) Uani 1 1 d . . . H18A H -0.1739 0.3879 0.2384 0.085 Uiso 1 1 calc R . . H1W H 0.452(6) 0.164(3) 0.115(3) 0.052(10) Uiso 1 1 d . . . H2W H 0.521(8) 0.101(4) 0.036(3) 0.082(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu2 0.0473(3) 0.0339(3) 0.0254(2) 0.01801(19) 0.01005(19) 0.0074(2) Cl1 0.0842(7) 0.0970(7) 0.0620(5) 0.0513(6) -0.0086(5) -0.0139(6) O1 0.0430(11) 0.0345(9) 0.0385(9) 0.0222(8) 0.0038(8) 0.0001(8) O2 0.0579(12) 0.0404(10) 0.0280(8) 0.0220(8) 0.0145(8) 0.0107(9) O3 0.0522(15) 0.0948(19) 0.0598(15) 0.0087(14) 0.0097(12) -0.0134(14) O4 0.0460(15) 0.0576(15) 0.0546(15) 0.0143(12) 0.0072(12) 0.0059(12) O5 0.161(4) 0.215(5) 0.193(4) 0.182(4) -0.090(3) -0.099(4) O6 0.179(5) 0.379(10) 0.187(6) 0.115(6) 0.084(4) 0.150(6) O7 0.154(4) 0.129(3) 0.157(4) 0.088(3) -0.042(3) -0.051(3) O8 0.262(5) 0.097(2) 0.0542(18) 0.0310(18) -0.025(2) 0.006(3) N1 0.0387(12) 0.0339(11) 0.0334(11) 0.0192(10) 0.0074(9) 0.0046(9) N2 0.0498(14) 0.0383(12) 0.0249(10) 0.0159(9) 0.0111(10) 0.0035(10) N3 0.0517(17) 0.0574(16) 0.0486(15) 0.0042(13) 0.0183(13) -0.0023(13) C1 0.0537(18) 0.0393(14) 0.0355(14) 0.0183(12) 0.0109(13) 0.0073(13) C2 0.0581(19) 0.0391(16) 0.0400(15) 0.0146(13) 0.0074(14) 0.0014(14) C3 0.0452(17) 0.0389(15) 0.0581(17) 0.0265(14) 0.0178(14) 0.0087(13) C4 0.0557(19) 0.0402(16) 0.069(2) 0.0291(16) 0.0191(16) 0.0053(14) C5 0.069(2) 0.0511(17) 0.0476(17) 0.0335(15) 0.0110(15) -0.0003(15) C6 0.0586(19) 0.0478(16) 0.0359(14) 0.0248(13) 0.0016(13) -0.0009(14) C7 0.0565(19) 0.0540(18) 0.0439(15) 0.0257(14) 0.0151(14) -0.0029(15) C8 0.092(3) 0.061(2) 0.0479(18) 0.0302(16) 0.0279(19) -0.0064(19) C9 0.126(3) 0.0502(18) 0.0338(16) 0.0237(15) 0.0241(19) 0.002(2) C10 0.263(7) 0.071(3) 0.0408(18) 0.039(2) 0.040(3) 0.010(3) C11 0.089(3) 0.060(2) 0.0308(14) 0.0216(15) -0.0060(15) 0.0021(18) C12 0.0571(19) 0.0475(16) 0.0338(14) 0.0182(13) 0.0056(13) -0.0013(14) C13 0.060(2) 0.0436(17) 0.072(2) 0.0160(17) 0.0225(18) -0.0019(16) C14 0.063(2) 0.0468(17) 0.068(2) 0.0225(16) 0.0175(18) 0.0064(16) C15 0.0490(19) 0.0428(16) 0.0571(18) 0.0093(15) 0.0188(15) 0.0073(14) C16 0.057(2) 0.0556(19) 0.070(2) 0.0261(17) 0.0233(17) 0.0113(16) C17 0.061(2) 0.064(2) 0.064(2) 0.0218(18) 0.0256(18) -0.0057(18) C18 0.060(2) 0.091(3) 0.0526(19) 0.0253(19) 0.0183(17) -0.003(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 Cu2 O2 1.9541(16) 2 ? Cu2 O2 1.9541(16) . ? Cu2 O1 1.9751(16) 2 ? Cu2 O1 1.9751(16) . ? Cl1 O8 1.361(3) . ? Cl1 O7 1.367(4) . ? Cl1 O5 1.377(4) . ? Cl1 O6 1.410(6) . ? O1 N1 1.350(3) . ? O2 N2 1.349(2) . ? O3 N3 1.317(4) . ? O4 H1W 0.85(3) . ? O4 H2W 0.75(5) . ? N1 C1 1.335(3) . ? N1 C6 1.345(3) . ? N2 C12 1.327(4) . ? N2 C7 1.344(3) . ? N3 C18 1.340(4) . ? N3 C13 1.350(5) . ? C1 C2 1.370(4) . ? C1 H1A 0.9300 . ? C2 C3 1.391(4) . ? C2 H2A 0.9300 . ? C3 C5 1.373(4) . ? C3 C4 1.507(4) . ? C4 C4 1.513(6) 2_445 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.362(4) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.361(4) . ? C7 H7A 0.9300 . ? C8 C9 1.386(5) . ? C8 H8A 0.9300 . ? C9 C11 1.376(5) . ? C9 C10 1.512(4) . ? C10 C10 1.345(8) 2_556 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.387(4) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.345(5) . ? C13 H13A 0.9300 . ? C14 C15 1.393(4) . ? C14 H14A 0.9300 . ? C15 C17 1.377(5) . ? C15 C16 1.510(5) . ? C16 C16 1.522(6) 2_666 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.381(5) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu2 O2 180.00(10) 2 . ? O2 Cu2 O1 94.81(7) 2 2 ? O2 Cu2 O1 85.19(7) . 2 ? O2 Cu2 O1 85.19(7) 2 . ? O2 Cu2 O1 94.81(7) . . ? O1 Cu2 O1 180.00(8) 2 . ? O8 Cl1 O7 112.4(3) . . ? O8 Cl1 O5 111.4(3) . . ? O7 Cl1 O5 109.4(2) . . ? O8 Cl1 O6 104.5(3) . . ? O7 Cl1 O6 106.1(4) . . ? O5 Cl1 O6 112.8(4) . . ? N1 O1 Cu2 121.00(14) . . ? N2 O2 Cu2 120.63(14) . . ? H1W O4 H2W 105(4) . . ? C1 N1 C6 120.6(2) . . ? C1 N1 O1 121.38(19) . . ? C6 N1 O1 118.0(2) . . ? C12 N2 C7 121.6(2) . . ? C12 N2 O2 119.2(2) . . ? C7 N2 O2 119.1(2) . . ? O3 N3 C18 120.5(3) . . ? O3 N3 C13 120.2(3) . . ? C18 N3 C13 119.3(3) . . ? N1 C1 C2 120.1(2) . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C1 C2 C3 121.0(3) . . ? C1 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 . . ? C5 C3 C2 116.6(3) . . ? C5 C3 C4 121.6(3) . . ? C2 C3 C4 121.8(3) . . ? C3 C4 C4 112.0(3) . 2_445 ? C3 C4 H4A 109.2 . . ? C4 C4 H4A 109.2 2_445 . ? C3 C4 H4B 109.2 . . ? C4 C4 H4B 109.2 2_445 . ? H4A C4 H4B 107.9 . . ? C6 C5 C3 121.4(3) . . ? C6 C5 H5A 119.3 . . ? C3 C5 H5A 119.3 . . ? N1 C6 C5 120.2(3) . . ? N1 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? N2 C7 C8 119.3(3) . . ? N2 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C7 C8 C9 121.9(3) . . ? C7 C8 H8A 119.0 . . ? C9 C8 H8A 119.0 . . ? C11 C9 C8 116.5(3) . . ? C11 C9 C10 120.8(4) . . ? C8 C9 C10 122.7(4) . . ? C10 C10 C9 117.9(5) 2_556 . ? C10 C10 H10A 107.8 2_556 . ? C9 C10 H10A 107.8 . . ? C10 C10 H10B 107.8 2_556 . ? C9 C10 H10B 107.8 . . ? H10A C10 H10B 107.2 . . ? C9 C11 C12 120.8(3) . . ? C9 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? N2 C12 C11 119.8(3) . . ? N2 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C14 C13 N3 121.9(3) . . ? C14 C13 H13A 119.1 . . ? N3 C13 H13A 119.1 . . ? C13 C14 C15 120.9(3) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C17 C15 C14 116.3(3) . . ? C17 C15 C16 124.5(3) . . ? C14 C15 C16 119.2(3) . . ? C15 C16 C16 114.4(4) . 2_666 ? C15 C16 H16A 108.7 . . ? C16 C16 H16A 108.7 2_666 . ? C15 C16 H16B 108.7 . . ? C16 C16 H16B 108.7 2_666 . ? H16A C16 H16B 107.6 . . ? C15 C17 C18 121.5(3) . . ? C15 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? N3 C18 C17 120.2(3) . . ? N3 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.504 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.065 # Attachment 'last-3.cif' data_last-3 _database_code_depnum_ccdc_archive 'CCDC 691373' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H76 B2 Mn N6 O6' _chemical_formula_weight 1342.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mn Mn 0.3368 0.7283 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.99890(10) _cell_length_b 23.9270(3) _cell_length_c 15.1820(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.3545(5) _cell_angle_gamma 90.00 _cell_volume 3631.18(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37990 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1410 _exptl_absorpt_coefficient_mu 0.240 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61562 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8301 _reflns_number_gt 4239 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland maXus: a computer program for the solution and refinement of crystal structures from diffraction data, University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^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 8301 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _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 Mn1 Mn 0.0000 0.5000 0.0000 0.04406(12) Uani 1 2 d S . . O1 O 0.18969(11) 0.52973(6) -0.04445(7) 0.0638(3) Uani 1 1 d . . . O2 O 0.96418(11) 0.57677(5) 0.06432(8) 0.0650(3) Uani 1 1 d . . . O3 O -0.11407(11) 0.52368(5) -0.12113(6) 0.0566(3) Uani 1 1 d . . . N1 N 0.24328(13) 0.57240(7) 0.00137(9) 0.0532(4) Uani 1 1 d . . . N2 N 0.85978(14) 0.61115(6) 0.06694(9) 0.0519(4) Uani 1 1 d . . . N3 N -0.08872(13) 0.51102(5) -0.20439(8) 0.0470(3) Uani 1 1 d . . . B1 B 0.48036(18) 0.64478(9) -0.33259(13) 0.0517(5) Uani 1 1 d . . . C1 C 0.33192(17) 0.56237(8) 0.06609(13) 0.0640(5) Uani 1 1 d . . . H1A H 0.3563 0.5258 0.0796 0.077 Uiso 1 1 calc R . . C2 C 0.38706(19) 0.60563(8) 0.11254(13) 0.0676(5) Uani 1 1 d . . . H2A H 0.4484 0.5978 0.1579 0.081 Uiso 1 1 calc R . . C3 C 0.35557(16) 0.66008(8) 0.09488(11) 0.0534(4) Uani 1 1 d . . . C4 C 0.26242(19) 0.66847(9) 0.02830(14) 0.0709(6) Uani 1 1 d . . . H4A H 0.2363 0.7047 0.0140 0.085 Uiso 1 1 calc R . . C5 C 0.20738(18) 0.62467(9) -0.01743(13) 0.0696(5) Uani 1 1 d . . . H5A H 0.1442 0.6314 -0.0621 0.083 Uiso 1 1 calc R . . C6 C 0.42660(18) 0.70825(8) 0.13936(13) 0.0670(5) Uani 1 1 d . . . H6A H 0.4615 0.6964 0.1965 0.080 Uiso 1 1 calc R . . H6B H 0.3638 0.7385 0.1484 0.080 Uiso 1 1 calc R . . C7 C 0.54206(18) 0.72911(7) 0.08284(13) 0.0645(5) Uani 1 1 d . . . H7A H 0.5074 0.7380 0.0243 0.077 Uiso 1 1 calc R . . H7B H 0.5781 0.7632 0.1085 0.077 Uiso 1 1 calc R . . C8 C 0.65277(17) 0.68706(7) 0.07551(12) 0.0545(4) Uani 1 1 d . . . C9 C 0.66389(18) 0.65131(8) 0.00543(12) 0.0612(5) Uani 1 1 d . . . H9A H 0.6004 0.6527 -0.0403 0.073 Uiso 1 1 calc R . . C10 C 0.76687(18) 0.61362(8) 0.00148(12) 0.0612(5) Uani 1 1 d . . . H10A H 0.7725 0.5897 -0.0466 0.073 Uiso 1 1 calc R . . C11 C 0.74935(19) 0.68244(8) 0.14107(13) 0.0710(6) Uani 1 1 d . . . H11A H 0.7451 0.7058 0.1899 0.085 Uiso 1 1 calc R . . C12 C 0.85089(19) 0.64478(8) 0.13656(13) 0.0694(5) Uani 1 1 d . . . H12A H 0.9143 0.6425 0.1822 0.083 Uiso 1 1 calc R . . C13 C -0.19149(17) 0.50405(7) -0.26152(11) 0.0566(5) Uani 1 1 d . . . H13A H -0.2788 0.5074 -0.2424 0.068 Uiso 1 1 calc R . . C14 C -0.16829(19) 0.49201(8) -0.34844(11) 0.0630(5) Uani 1 1 d . . . H14A H -0.2403 0.4873 -0.3876 0.076 Uiso 1 1 calc R . . C15 C -0.03998(19) 0.48688(8) -0.37808(11) 0.0594(5) Uani 1 1 d . . . C16 C -0.0122(2) 0.47487(9) -0.47401(11) 0.0758(6) Uani 1 1 d . . . H16A H 0.0652 0.4506 -0.4770 0.091 Uiso 1 1 calc R . . H16B H -0.0880 0.4550 -0.4999 0.091 Uiso 1 1 calc R . . C17 C 0.06258(18) 0.49563(8) -0.31799(11) 0.0632(5) Uani 1 1 d . . . H17A H 0.1506 0.4935 -0.3362 0.076 Uiso 1 1 calc R . . C18 C 0.03737(17) 0.50752(7) -0.23146(10) 0.0569(5) Uani 1 1 d . . . H18A H 0.1081 0.5132 -0.1916 0.068 Uiso 1 1 calc R . . C19 C 0.64461(15) 0.64699(7) -0.33499(11) 0.0525(4) Uani 1 1 d . . . C20 C 0.71606(16) 0.64616(7) -0.41266(13) 0.0612(5) Uani 1 1 d . . . H20A H 0.6690 0.6476 -0.4662 0.073 Uiso 1 1 calc R . . C21 C 0.85458(19) 0.64336(8) -0.41334(16) 0.0736(6) Uani 1 1 d . . . H21A H 0.8983 0.6431 -0.4667 0.088 Uiso 1 1 calc R . . C22 C 0.9270(2) 0.64103(8) -0.3363(2) 0.0834(7) Uani 1 1 d . . . H22A H 1.0198 0.6391 -0.3370 0.100 Uiso 1 1 calc R . . C23 C 0.8624(2) 0.64155(8) -0.25787(18) 0.0810(7) Uani 1 1 d . . . H23A H 0.9111 0.6399 -0.2050 0.097 Uiso 1 1 calc R . . C24 C 0.72357(17) 0.64451(8) -0.25753(13) 0.0680(5) Uani 1 1 d . . . H24A H 0.6813 0.6449 -0.2036 0.082 Uiso 1 1 calc R . . C25 C 0.44849(15) 0.57832(7) -0.31264(11) 0.0493(4) Uani 1 1 d . . . C26 C 0.41212(15) 0.55717(8) -0.23121(11) 0.0568(5) Uani 1 1 d . . . H26A H 0.3993 0.5822 -0.1853 0.068 Uiso 1 1 calc R . . C27 C 0.39407(17) 0.50065(9) -0.21517(13) 0.0645(5) Uani 1 1 d . . . H27A H 0.3703 0.4886 -0.1594 0.077 Uiso 1 1 calc R . . C28 C 0.41109(17) 0.46254(9) -0.28123(14) 0.0670(5) Uani 1 1 d . . . H28A H 0.3974 0.4247 -0.2712 0.080 Uiso 1 1 calc R . . C29 C 0.44862(19) 0.48103(9) -0.36239(13) 0.0701(5) Uani 1 1 d . . . H29A H 0.4616 0.4557 -0.4078 0.084 Uiso 1 1 calc R . . C30 C 0.46705(17) 0.53738(9) -0.37644(12) 0.0635(5) Uani 1 1 d . . . H30A H 0.4935 0.5488 -0.4319 0.076 Uiso 1 1 calc R . . C31 C 0.41432(16) 0.66591(8) -0.42708(11) 0.0530(4) Uani 1 1 d . . . C32 C 0.31336(19) 0.63935(9) -0.47396(13) 0.0772(6) Uani 1 1 d . . . H32A H 0.2802 0.6059 -0.4521 0.093 Uiso 1 1 calc R . . C33 C 0.2588(2) 0.65993(12) -0.55191(16) 0.1053(8) Uani 1 1 d . . . H33A H 0.1903 0.6405 -0.5810 0.126 Uiso 1 1 calc R . . C34 C 0.3056(3) 0.70890(13) -0.58624(15) 0.0987(8) Uani 1 1 d . . . H34A H 0.2711 0.7224 -0.6395 0.118 Uiso 1 1 calc R . . C35 C 0.4030(2) 0.73752(10) -0.54155(15) 0.0807(6) Uani 1 1 d . . . H35A H 0.4343 0.7713 -0.5634 0.097 Uiso 1 1 calc R . . C36 C 0.45550(18) 0.71624(8) -0.46331(13) 0.0655(5) Uani 1 1 d . . . H36A H 0.5216 0.7366 -0.4335 0.079 Uiso 1 1 calc R . . C37 C 0.41632(16) 0.68630(7) -0.25930(11) 0.0526(4) Uani 1 1 d . . . C38 C 0.48291(19) 0.73152(9) -0.21982(12) 0.0676(5) Uani 1 1 d . . . H38A H 0.5730 0.7368 -0.2311 0.081 Uiso 1 1 calc R . . C39 C 0.4195(2) 0.76892(9) -0.16430(14) 0.0817(6) Uani 1 1 d . . . H39A H 0.4677 0.7982 -0.1388 0.098 Uiso 1 1 calc R . . C40 C 0.2866(3) 0.76269(10) -0.14713(13) 0.0823(7) Uani 1 1 d . . . H40A H 0.2440 0.7876 -0.1100 0.099 Uiso 1 1 calc R . . C41 C 0.2169(2) 0.71928(10) -0.18546(13) 0.0733(6) Uani 1 1 d . . . H41A H 0.1261 0.7150 -0.1752 0.088 Uiso 1 1 calc R . . C42 C 0.28121(17) 0.68214(8) -0.23904(12) 0.0594(5) Uani 1 1 d . . . H42A H 0.2321 0.6526 -0.2631 0.071 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 Mn1 0.0496(2) 0.0526(2) 0.03025(19) -0.00478(16) 0.00553(14) -0.00130(16) O1 0.0646(7) 0.0853(9) 0.0420(7) -0.0116(7) 0.0114(6) -0.0196(7) O2 0.0595(7) 0.0658(8) 0.0696(9) -0.0245(7) -0.0027(6) 0.0114(6) O3 0.0652(7) 0.0771(8) 0.0278(6) -0.0070(6) 0.0063(5) 0.0142(6) N1 0.0518(8) 0.0671(11) 0.0411(8) 0.0051(8) 0.0073(7) -0.0090(8) N2 0.0567(9) 0.0483(9) 0.0509(9) -0.0117(7) 0.0038(7) 0.0003(7) N3 0.0561(8) 0.0580(10) 0.0269(7) -0.0019(6) 0.0029(6) 0.0067(7) B1 0.0463(11) 0.0657(14) 0.0429(12) 0.0062(10) -0.0008(9) -0.0011(10) C1 0.0630(11) 0.0583(12) 0.0699(13) 0.0090(11) -0.0152(10) 0.0013(10) C2 0.0711(12) 0.0623(14) 0.0680(13) 0.0034(11) -0.0253(10) -0.0018(10) C3 0.0537(10) 0.0541(12) 0.0526(11) 0.0038(9) 0.0033(9) 0.0033(9) C4 0.0723(13) 0.0559(13) 0.0843(15) 0.0197(12) -0.0065(12) 0.0020(10) C5 0.0682(12) 0.0733(16) 0.0663(13) 0.0251(12) -0.0163(10) -0.0052(11) C6 0.0721(12) 0.0575(12) 0.0718(13) -0.0104(10) 0.0088(10) 0.0041(10) C7 0.0668(12) 0.0451(11) 0.0815(14) -0.0112(10) 0.0022(10) 0.0021(9) C8 0.0609(11) 0.0427(11) 0.0600(12) -0.0075(9) 0.0042(9) -0.0033(8) C9 0.0642(11) 0.0646(13) 0.0547(12) -0.0106(10) -0.0026(9) 0.0059(10) C10 0.0681(12) 0.0661(13) 0.0492(11) -0.0194(9) -0.0019(9) 0.0029(10) C11 0.0765(13) 0.0688(14) 0.0675(14) -0.0324(11) -0.0021(11) 0.0121(11) C12 0.0810(13) 0.0702(13) 0.0567(12) -0.0257(10) -0.0085(10) 0.0092(11) C13 0.0535(10) 0.0782(13) 0.0380(10) -0.0038(9) 0.0017(8) -0.0018(9) C14 0.0688(12) 0.0857(15) 0.0343(10) -0.0060(9) -0.0044(9) -0.0100(10) C15 0.0840(14) 0.0627(13) 0.0320(9) -0.0034(8) 0.0091(9) -0.0012(10) C16 0.1070(16) 0.0858(15) 0.0351(11) -0.0109(9) 0.0132(10) -0.0046(13) C17 0.0619(11) 0.0940(15) 0.0341(10) 0.0000(10) 0.0104(8) 0.0135(10) C18 0.0523(10) 0.0847(14) 0.0339(9) 0.0005(9) 0.0019(8) 0.0103(9) C19 0.0477(9) 0.0539(11) 0.0558(12) 0.0085(8) -0.0013(9) -0.0012(8) C20 0.0525(11) 0.0580(12) 0.0733(13) 0.0033(10) 0.0062(9) 0.0020(9) C21 0.0564(12) 0.0559(13) 0.1094(18) 0.0095(12) 0.0220(12) 0.0034(10) C22 0.0447(11) 0.0554(13) 0.150(2) 0.0211(14) -0.0020(15) -0.0013(10) C23 0.0624(13) 0.0669(14) 0.1120(19) 0.0189(13) -0.0299(13) -0.0063(11) C24 0.0581(12) 0.0740(14) 0.0714(14) 0.0105(10) -0.0092(10) 0.0007(10) C25 0.0402(9) 0.0666(12) 0.0413(10) 0.0061(9) 0.0009(7) 0.0022(8) C26 0.0541(10) 0.0688(13) 0.0478(11) 0.0059(9) 0.0045(8) 0.0114(9) C27 0.0636(11) 0.0728(14) 0.0574(12) 0.0201(12) 0.0065(9) 0.0115(10) C28 0.0650(12) 0.0624(13) 0.0734(14) 0.0132(12) -0.0030(10) 0.0023(10) C29 0.0805(14) 0.0694(14) 0.0606(13) -0.0042(10) 0.0014(10) 0.0018(11) C30 0.0689(12) 0.0744(15) 0.0476(11) 0.0069(10) 0.0090(9) -0.0031(10) C31 0.0447(9) 0.0674(12) 0.0470(10) 0.0072(9) 0.0057(8) 0.0033(9) C32 0.0712(13) 0.0877(15) 0.0715(14) 0.0173(12) -0.0204(11) -0.0050(11) C33 0.1096(19) 0.115(2) 0.0886(19) 0.0175(17) -0.0470(15) 0.0018(16) C34 0.1024(19) 0.129(2) 0.0638(15) 0.0278(16) -0.0148(14) 0.0357(17) C35 0.0744(14) 0.0917(17) 0.0767(16) 0.0326(13) 0.0158(12) 0.0238(13) C36 0.0605(11) 0.0724(14) 0.0637(13) 0.0131(11) 0.0050(10) 0.0065(10) C37 0.0498(10) 0.0640(12) 0.0437(10) 0.0104(9) -0.0043(8) 0.0034(9) C38 0.0640(12) 0.0819(15) 0.0564(12) -0.0031(11) -0.0081(10) 0.0022(11) C39 0.1029(18) 0.0796(16) 0.0618(14) -0.0110(12) -0.0158(13) 0.0083(13) C40 0.112(2) 0.0825(17) 0.0528(13) 0.0023(12) 0.0107(13) 0.0288(15) C41 0.0787(13) 0.0802(16) 0.0619(14) 0.0184(12) 0.0196(11) 0.0197(13) C42 0.0601(11) 0.0624(12) 0.0558(12) 0.0131(9) 0.0069(9) 0.0062(9) _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 Mn1 O2 2.1147(11) 3_665 ? Mn1 O2 2.1147(11) 1_455 ? Mn1 O1 2.1493(11) . ? Mn1 O1 2.1493(11) 3_565 ? Mn1 O3 2.2146(10) . ? Mn1 O3 2.2146(10) 3_565 ? O1 N1 1.3400(17) . ? O2 N2 1.3304(16) . ? O2 Mn1 2.1147(11) 1_655 ? O3 N3 1.3301(15) . ? N1 C1 1.329(2) . ? N1 C5 1.330(2) . ? N2 C12 1.333(2) . ? N2 C10 1.345(2) . ? N3 C18 1.338(2) . ? N3 C13 1.339(2) . ? B1 C37 1.634(3) . ? B1 C19 1.644(2) . ? B1 C31 1.645(2) . ? B1 C25 1.651(3) . ? C1 C2 1.362(2) . ? C1 H1A 0.9300 . ? C2 C3 1.366(2) . ? C2 H2A 0.9300 . ? C3 C4 1.373(2) . ? C3 C6 1.505(2) . ? C4 C5 1.366(3) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.538(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.502(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.372(2) . ? C8 C11 1.375(2) . ? C9 C10 1.371(2) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.360(2) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.376(2) . ? C13 H13A 0.9300 . ? C14 C15 1.375(2) . ? C14 H14A 0.9300 . ? C15 C17 1.372(2) . ? C15 C16 1.517(2) . ? C16 C16 1.462(4) 3_564 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.373(2) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.393(2) . ? C19 C24 1.402(2) . ? C20 C21 1.387(2) . ? C20 H20A 0.9300 . ? C21 C22 1.362(3) . ? C21 H21A 0.9300 . ? C22 C23 1.368(3) . ? C22 H22A 0.9300 . ? C23 C24 1.390(3) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.392(2) . ? C25 C30 1.393(2) . ? C26 C27 1.387(2) . ? C26 H26A 0.9300 . ? C27 C28 1.369(3) . ? C27 H27A 0.9300 . ? C28 C29 1.370(3) . ? C28 H28A 0.9300 . ? C29 C30 1.378(3) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.377(2) . ? C31 C36 1.390(2) . ? C32 C33 1.382(3) . ? C32 H32A 0.9300 . ? C33 C34 1.369(3) . ? C33 H33A 0.9300 . ? C34 C35 1.359(3) . ? C34 H34A 0.9300 . ? C35 C36 1.384(3) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C42 1.396(2) . ? C37 C38 1.398(2) . ? C38 C39 1.392(3) . ? C38 H38A 0.9300 . ? C39 C40 1.369(3) . ? C39 H39A 0.9300 . ? C40 C41 1.372(3) . ? C40 H40A 0.9300 . ? C41 C42 1.375(3) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O2 180.00(3) 3_665 1_455 ? O2 Mn1 O1 88.98(5) 3_665 . ? O2 Mn1 O1 91.02(5) 1_455 . ? O2 Mn1 O1 91.02(5) 3_665 3_565 ? O2 Mn1 O1 88.98(5) 1_455 3_565 ? O1 Mn1 O1 180.0 . 3_565 ? O2 Mn1 O3 85.89(4) 3_665 . ? O2 Mn1 O3 94.11(4) 1_455 . ? O1 Mn1 O3 95.49(4) . . ? O1 Mn1 O3 84.51(4) 3_565 . ? O2 Mn1 O3 94.11(4) 3_665 3_565 ? O2 Mn1 O3 85.89(4) 1_455 3_565 ? O1 Mn1 O3 84.51(4) . 3_565 ? O1 Mn1 O3 95.49(4) 3_565 3_565 ? O3 Mn1 O3 180.00(6) . 3_565 ? N1 O1 Mn1 115.73(8) . . ? N2 O2 Mn1 133.82(9) . 1_655 ? N3 O3 Mn1 128.68(9) . . ? C1 N1 C5 120.01(16) . . ? C1 N1 O1 119.84(16) . . ? C5 N1 O1 120.15(15) . . ? O2 N2 C12 117.65(15) . . ? O2 N2 C10 122.26(14) . . ? C12 N2 C10 120.08(15) . . ? O3 N3 C18 120.55(13) . . ? O3 N3 C13 118.90(13) . . ? C18 N3 C13 120.50(14) . . ? C37 B1 C19 113.78(14) . . ? C37 B1 C31 104.56(13) . . ? C19 B1 C31 110.58(13) . . ? C37 B1 C25 112.35(14) . . ? C19 B1 C25 103.42(13) . . ? C31 B1 C25 112.38(14) . . ? N1 C1 C2 120.02(18) . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C1 C2 C3 122.34(17) . . ? C1 C2 H2A 118.8 . . ? C3 C2 H2A 118.8 . . ? C2 C3 C4 115.68(17) . . ? C2 C3 C6 122.57(17) . . ? C4 C3 C6 121.53(17) . . ? C5 C4 C3 121.35(18) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? N1 C5 C4 120.60(17) . . ? N1 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C3 C6 C7 110.53(15) . . ? C3 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 112.84(15) . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C11 116.30(16) . . ? C9 C8 C7 123.27(17) . . ? C11 C8 C7 120.43(16) . . ? C10 C9 C8 121.25(17) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? N2 C10 C9 120.18(16) . . ? N2 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C12 C11 C8 121.94(17) . . ? C12 C11 H11A 119.0 . . ? C8 C11 H11A 119.0 . . ? N2 C12 C11 120.24(18) . . ? N2 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? N3 C13 C14 120.20(16) . . ? N3 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C15 C14 C13 120.82(17) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C17 C15 C14 117.21(15) . . ? C17 C15 C16 121.09(17) . . ? C14 C15 C16 121.63(17) . . ? C16 C16 C15 113.5(2) 3_564 . ? C16 C16 H16A 108.9 3_564 . ? C15 C16 H16A 108.9 . . ? C16 C16 H16B 108.9 3_564 . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C15 C17 C18 121.08(16) . . ? C15 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? N3 C18 C17 120.16(16) . . ? N3 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C20 C19 C24 114.80(15) . . ? C20 C19 B1 123.41(15) . . ? C24 C19 B1 121.53(15) . . ? C21 C20 C19 122.62(18) . . ? C21 C20 H20A 118.7 . . ? C19 C20 H20A 118.7 . . ? C22 C21 C20 120.4(2) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C21 C22 C23 119.66(19) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C22 C23 C24 119.7(2) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C23 C24 C19 122.8(2) . . ? C23 C24 H24A 118.6 . . ? C19 C24 H24A 118.6 . . ? C26 C25 C30 113.80(16) . . ? C26 C25 B1 124.66(16) . . ? C30 C25 B1 121.34(15) . . ? C27 C26 C25 123.26(17) . . ? C27 C26 H26A 118.4 . . ? C25 C26 H26A 118.4 . . ? C28 C27 C26 120.13(18) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 119.02(19) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? C28 C29 C30 119.72(19) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C29 C30 C25 124.05(17) . . ? C29 C30 H30A 118.0 . . ? C25 C30 H30A 118.0 . . ? C32 C31 C36 114.57(17) . . ? C32 C31 B1 125.69(16) . . ? C36 C31 B1 119.65(16) . . ? C31 C32 C33 123.2(2) . . ? C31 C32 H32A 118.4 . . ? C33 C32 H32A 118.4 . . ? C34 C33 C32 120.0(2) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C35 C34 C33 119.2(2) . . ? C35 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? C34 C35 C36 119.7(2) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C35 C36 C31 123.25(19) . . ? C35 C36 H36A 118.4 . . ? C31 C36 H36A 118.4 . . ? C42 C37 C38 114.48(16) . . ? C42 C37 B1 120.23(16) . . ? C38 C37 B1 124.91(15) . . ? C39 C38 C37 122.55(19) . . ? C39 C38 H38A 118.7 . . ? C37 C38 H38A 118.7 . . ? C40 C39 C38 120.2(2) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C39 C40 C41 119.2(2) . . ? C39 C40 H40A 120.4 . . ? C41 C40 H40A 120.4 . . ? C40 C41 C42 120.0(2) . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 C37 123.57(19) . . ? C41 C42 H42A 118.2 . . ? C37 C42 H42A 118.2 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.183 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.034 # Attachment 'last-4.cif' data_last-4 _database_code_depnum_ccdc_archive 'CCDC 691374' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H76 B2 Co N6 O6' _chemical_formula_weight 1346.06 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.72030(10) _cell_length_b 25.4382(4) _cell_length_c 14.5710(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.7020(10) _cell_angle_gamma 90.00 _cell_volume 3595.41(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36481 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1414 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52358 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8249 _reflns_number_gt 4824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _publ_section_references ; collect: "Collect" data collection software, Nonius B.V., Delft, The Netherlands, 1998. HKL Scalepack & HKL Denzo: Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R.M. Sweet, Eds., Academic Press. absorption correction: R.H. Blessing (1995) Acta Cryst. A51, 33-37. R.H. Blessing (1997) J.Appl. Cryst. 30, 421-426. maXus: S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland maXus: a computer program for the solution and refinement of crystal structures from diffraction data, University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998). Sheldrick, G. M. (1998). SHELXTL Version 5.1. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELX-97. PC Version. University of Goettingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^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 8249 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 0.0000 0.0000 0.5000 0.03917(10) Uani 1 2 d S . . B1 B 0.4939(2) 0.14585(8) 0.14476(13) 0.0469(5) Uani 1 1 d . . . N1 N 0.16112(15) 0.09790(5) 0.57097(8) 0.0462(3) Uani 1 1 d . . . N2 N 0.76466(14) 0.07212(5) 0.55498(8) 0.0424(3) Uani 1 1 d . . . N3 N 0.01825(14) 0.03633(5) 0.30937(8) 0.0409(3) Uani 1 1 d . . . O1 O 0.07339(13) 0.05951(4) 0.58902(7) 0.0550(3) Uani 1 1 d . . . O2 O 0.80481(12) 0.02337(4) 0.53645(7) 0.0520(3) Uani 1 1 d . . . O3 O 0.00698(12) 0.05427(4) 0.39482(6) 0.0499(3) Uani 1 1 d . . . C1 C 0.26472(18) 0.09020(7) 0.51613(10) 0.0501(4) Uani 1 1 d . . . H1A H 0.2760 0.0576 0.4888 0.060 Uiso 1 1 calc R . . C2 C 0.35417(18) 0.13039(7) 0.50028(11) 0.0523(4) Uani 1 1 d . . . H2A H 0.4243 0.1247 0.4610 0.063 Uiso 1 1 calc R . . C3 C 0.34303(18) 0.17921(6) 0.54114(11) 0.0487(4) Uani 1 1 d . . . C4 C 0.2350(2) 0.18521(7) 0.59621(12) 0.0622(5) Uani 1 1 d . . . H4A H 0.2224 0.2174 0.6249 0.075 Uiso 1 1 calc R . . C5 C 0.1449(2) 0.14489(7) 0.61003(12) 0.0635(5) Uani 1 1 d . . . H5A H 0.0717 0.1503 0.6470 0.076 Uiso 1 1 calc R . . C6 C 0.44529(19) 0.22251(6) 0.52843(12) 0.0579(5) Uani 1 1 d . . . H6A H 0.3999 0.2561 0.5354 0.069 Uiso 1 1 calc R . . H6B H 0.4755 0.2208 0.4664 0.069 Uiso 1 1 calc R . . C7 C 0.57228(19) 0.21969(6) 0.59694(12) 0.0582(5) Uani 1 1 d . . . H7A H 0.6323 0.2493 0.5868 0.070 Uiso 1 1 calc R . . H7B H 0.5428 0.2222 0.6591 0.070 Uiso 1 1 calc R . . C8 C 0.65088(17) 0.16951(6) 0.58685(11) 0.0467(4) Uani 1 1 d . . . C9 C 0.7257(2) 0.15977(7) 0.51168(12) 0.0612(5) Uani 1 1 d . . . H9A H 0.7384 0.1868 0.4701 0.073 Uiso 1 1 calc R . . C10 C 0.78181(19) 0.11158(7) 0.49620(11) 0.0582(5) Uani 1 1 d . . . H10A H 0.8319 0.1062 0.4448 0.070 Uiso 1 1 calc R . . C11 C 0.6442(2) 0.12873(7) 0.64827(11) 0.0563(5) Uani 1 1 d . . . H11A H 0.6003 0.1339 0.7024 0.068 Uiso 1 1 calc R . . C12 C 0.70084(19) 0.08066(7) 0.63163(11) 0.0553(5) Uani 1 1 d . . . H12A H 0.6946 0.0537 0.6743 0.066 Uiso 1 1 calc R . . C13 C -0.09376(19) 0.02043(8) 0.26015(11) 0.0627(5) Uani 1 1 d . . . H13A H -0.1787 0.0208 0.2860 0.075 Uiso 1 1 calc R . . C14 C -0.0849(2) 0.00357(8) 0.17166(12) 0.0682(6) Uani 1 1 d . . . H14A H -0.1641 -0.0078 0.1382 0.082 Uiso 1 1 calc R . . C15 C 0.03919(19) 0.00314(6) 0.13112(10) 0.0505(4) Uani 1 1 d . . . C16 C 0.0509(2) -0.01238(8) 0.03257(11) 0.0700(6) Uani 1 1 d . . . H16A H 0.1425 -0.0034 0.0149 0.084 Uiso 1 1 calc R . . H16B H 0.0411 -0.0502 0.0276 0.084 Uiso 1 1 calc R . . C17 C 0.15221(18) 0.01986(7) 0.18460(10) 0.0489(4) Uani 1 1 d . . . H17A H 0.2382 0.0202 0.1601 0.059 Uiso 1 1 calc R . . C18 C 0.14049(17) 0.03599(6) 0.27273(10) 0.0447(4) Uani 1 1 d . . . H18A H 0.2186 0.0469 0.3078 0.054 Uiso 1 1 calc R . . C19 C 0.56397(18) 0.18997(7) 0.21501(10) 0.0487(4) Uani 1 1 d . . . C20 C 0.4991(2) 0.23560(7) 0.24346(11) 0.0594(5) Uani 1 1 d . . . H20A H 0.4067 0.2409 0.2251 0.071 Uiso 1 1 calc R . . C21 C 0.5675(3) 0.27333(8) 0.29812(13) 0.0717(6) Uani 1 1 d . . . H21A H 0.5201 0.3028 0.3167 0.086 Uiso 1 1 calc R . . C22 C 0.7047(3) 0.26730(9) 0.32484(13) 0.0780(7) Uani 1 1 d . . . H22A H 0.7506 0.2925 0.3615 0.094 Uiso 1 1 calc R . . C23 C 0.7728(2) 0.22369(9) 0.29674(12) 0.0740(6) Uani 1 1 d . . . H23A H 0.8662 0.2195 0.3134 0.089 Uiso 1 1 calc R . . C24 C 0.70364(19) 0.18605(8) 0.24396(11) 0.0596(5) Uani 1 1 d . . . H24A H 0.7521 0.1565 0.2267 0.071 Uiso 1 1 calc R . . C25 C 0.52289(17) 0.08601(7) 0.18402(12) 0.0498(4) Uani 1 1 d . . . C26 C 0.51199(19) 0.04141(8) 0.12815(14) 0.0629(5) Uani 1 1 d . . . H26A H 0.4934 0.0458 0.0652 0.076 Uiso 1 1 calc R . . C27 C 0.5278(2) -0.00948(8) 0.16269(19) 0.0799(7) Uani 1 1 d . . . H27A H 0.5217 -0.0382 0.1230 0.096 Uiso 1 1 calc R . . C28 C 0.5524(2) -0.01700(9) 0.2555(2) 0.0896(8) Uani 1 1 d . . . H28A H 0.5642 -0.0508 0.2791 0.108 Uiso 1 1 calc R . . C29 C 0.5594(2) 0.02526(10) 0.31305(16) 0.0805(6) Uani 1 1 d . . . H29A H 0.5731 0.0202 0.3762 0.097 Uiso 1 1 calc R . . C30 C 0.54627(19) 0.07539(8) 0.27796(12) 0.0615(5) Uani 1 1 d . . . H30A H 0.5533 0.1036 0.3187 0.074 Uiso 1 1 calc R . . C31 C 0.32574(18) 0.14957(6) 0.13334(12) 0.0483(4) Uani 1 1 d . . . C32 C 0.25049(19) 0.14262(7) 0.04958(13) 0.0593(5) Uani 1 1 d . . . H32A H 0.2981 0.1383 -0.0032 0.071 Uiso 1 1 calc R . . C33 C 0.1079(2) 0.14193(7) 0.04165(16) 0.0704(6) Uani 1 1 d . . . H33A H 0.0622 0.1377 -0.0159 0.084 Uiso 1 1 calc R . . C34 C 0.0337(2) 0.14734(7) 0.11745(19) 0.0752(6) Uani 1 1 d . . . H34A H -0.0621 0.1466 0.1120 0.090 Uiso 1 1 calc R . . C35 C 0.1025(2) 0.15390(7) 0.20176(17) 0.0698(6) Uani 1 1 d . . . H35A H 0.0534 0.1577 0.2541 0.084 Uiso 1 1 calc R . . C36 C 0.24565(19) 0.15491(6) 0.20891(13) 0.0583(5) Uani 1 1 d . . . H36A H 0.2902 0.1594 0.2668 0.070 Uiso 1 1 calc R . . C37 C 0.56422(17) 0.15823(7) 0.04676(11) 0.0485(4) Uani 1 1 d . . . C38 C 0.66368(19) 0.12779(8) 0.00665(12) 0.0612(5) Uani 1 1 d . . . H38A H 0.6894 0.0959 0.0340 0.073 Uiso 1 1 calc R . . C39 C 0.7256(2) 0.14287(9) -0.07185(14) 0.0773(6) Uani 1 1 d . . . H39A H 0.7908 0.1211 -0.0962 0.093 Uiso 1 1 calc R . . C40 C 0.6922(2) 0.18920(11) -0.11378(13) 0.0804(7) Uani 1 1 d . . . H40A H 0.7337 0.1992 -0.1668 0.097 Uiso 1 1 calc R . . C41 C 0.5963(2) 0.22119(9) -0.07682(13) 0.0768(6) Uani 1 1 d . . . H41A H 0.5736 0.2533 -0.1042 0.092 Uiso 1 1 calc R . . C42 C 0.5334(2) 0.20542(8) 0.00150(12) 0.0646(5) Uani 1 1 d . . . H42A H 0.4676 0.2274 0.0248 0.077 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 0.0491(2) 0.03627(17) 0.03253(16) -0.00271(12) 0.00579(13) 0.00092(14) B1 0.0379(12) 0.0490(12) 0.0536(11) 0.0036(9) 0.0027(9) 0.0017(9) N1 0.0553(10) 0.0437(8) 0.0398(7) -0.0078(6) 0.0048(6) -0.0054(7) N2 0.0463(9) 0.0335(7) 0.0478(8) -0.0020(6) 0.0076(6) 0.0026(6) N3 0.0449(9) 0.0458(8) 0.0327(7) 0.0035(6) 0.0074(6) 0.0027(6) O1 0.0703(9) 0.0514(7) 0.0443(6) -0.0103(5) 0.0122(6) -0.0187(6) O2 0.0550(8) 0.0319(6) 0.0706(7) -0.0049(5) 0.0148(6) 0.0037(6) O3 0.0720(9) 0.0458(7) 0.0330(6) -0.0006(5) 0.0120(5) 0.0068(6) C1 0.0544(12) 0.0453(10) 0.0512(10) -0.0145(8) 0.0076(8) -0.0016(9) C2 0.0547(12) 0.0494(11) 0.0538(10) -0.0105(8) 0.0110(8) -0.0018(9) C3 0.0534(12) 0.0392(10) 0.0529(10) -0.0007(8) 0.0000(8) 0.0020(8) C4 0.0704(14) 0.0434(11) 0.0744(12) -0.0191(9) 0.0178(10) -0.0009(10) C5 0.0717(14) 0.0523(12) 0.0685(12) -0.0238(9) 0.0216(10) -0.0053(10) C6 0.0620(13) 0.0350(10) 0.0769(12) 0.0061(8) 0.0067(10) 0.0022(9) C7 0.0626(13) 0.0331(9) 0.0792(12) -0.0080(8) 0.0065(10) 0.0005(9) C8 0.0496(11) 0.0349(9) 0.0556(10) -0.0057(8) 0.0029(8) -0.0033(8) C9 0.0764(15) 0.0403(10) 0.0693(12) 0.0134(9) 0.0233(10) 0.0075(10) C10 0.0726(14) 0.0478(11) 0.0567(11) 0.0066(9) 0.0229(9) 0.0096(10) C11 0.0753(14) 0.0471(11) 0.0482(10) -0.0062(8) 0.0162(9) 0.0080(9) C12 0.0714(14) 0.0447(10) 0.0515(10) 0.0081(8) 0.0159(9) 0.0075(9) C13 0.0397(12) 0.1013(15) 0.0481(11) 0.0011(10) 0.0095(9) -0.0053(11) C14 0.0532(13) 0.1097(17) 0.0414(10) -0.0082(10) -0.0002(9) -0.0168(11) C15 0.0608(13) 0.0549(11) 0.0363(9) 0.0015(8) 0.0064(8) 0.0084(9) C16 0.0864(16) 0.0842(15) 0.0396(10) -0.0072(9) 0.0053(9) 0.0237(11) C17 0.0473(12) 0.0588(11) 0.0419(10) 0.0090(8) 0.0123(8) 0.0087(9) C18 0.0433(11) 0.0483(10) 0.0424(9) 0.0074(7) 0.0028(8) -0.0031(8) C19 0.0475(12) 0.0569(11) 0.0426(9) 0.0059(8) 0.0093(8) -0.0027(9) C20 0.0585(13) 0.0597(12) 0.0611(11) -0.0013(9) 0.0126(9) -0.0080(10) C21 0.0871(18) 0.0637(13) 0.0670(13) -0.0081(10) 0.0257(12) -0.0111(12) C22 0.0914(19) 0.0884(17) 0.0547(12) -0.0100(11) 0.0078(12) -0.0358(14) C23 0.0659(15) 0.0930(17) 0.0621(13) -0.0015(12) -0.0038(10) -0.0175(13) C24 0.0524(13) 0.0678(13) 0.0584(11) 0.0000(9) 0.0015(9) -0.0052(10) C25 0.0321(10) 0.0538(11) 0.0641(11) 0.0050(9) 0.0081(8) 0.0000(8) C26 0.0490(12) 0.0578(13) 0.0828(13) 0.0010(10) 0.0105(10) -0.0042(9) C27 0.0563(15) 0.0535(14) 0.132(2) -0.0007(13) 0.0202(14) -0.0044(10) C28 0.0556(15) 0.0671(16) 0.149(2) 0.0437(16) 0.0244(15) 0.0026(12) C29 0.0654(16) 0.0824(17) 0.0953(16) 0.0367(14) 0.0164(12) 0.0062(13) C30 0.0533(13) 0.0654(13) 0.0668(12) 0.0159(10) 0.0119(9) 0.0059(10) C31 0.0441(11) 0.0392(9) 0.0616(11) 0.0081(8) 0.0039(9) 0.0003(8) C32 0.0454(12) 0.0512(11) 0.0803(13) 0.0110(9) -0.0033(10) -0.0051(9) C33 0.0519(14) 0.0538(12) 0.1029(16) 0.0157(11) -0.0152(12) -0.0065(10) C34 0.0412(13) 0.0467(12) 0.137(2) 0.0249(12) 0.0011(14) -0.0017(9) C35 0.0498(14) 0.0469(12) 0.1156(18) 0.0185(11) 0.0264(12) 0.0049(10) C36 0.0490(13) 0.0473(11) 0.0795(13) 0.0098(9) 0.0115(10) 0.0026(9) C37 0.0386(11) 0.0566(11) 0.0494(9) 0.0019(8) -0.0033(8) -0.0042(8) C38 0.0514(13) 0.0732(13) 0.0593(11) 0.0057(9) 0.0066(9) -0.0014(10) C39 0.0607(15) 0.1066(19) 0.0665(13) 0.0023(12) 0.0175(11) 0.0000(13) C40 0.0568(15) 0.130(2) 0.0547(12) 0.0159(13) 0.0046(10) -0.0202(14) C41 0.0664(16) 0.0922(17) 0.0706(14) 0.0325(12) -0.0064(11) -0.0123(13) C42 0.0571(13) 0.0694(13) 0.0673(12) 0.0139(10) 0.0046(10) -0.0016(10) _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 2.0671(10) . ? Co1 O3 2.0671(10) 3_556 ? Co1 O1 2.0889(10) . ? Co1 O1 2.0889(10) 3_556 ? Co1 O2 2.0893(11) 3_656 ? Co1 O2 2.0893(11) 1_455 ? B1 C31 1.635(3) . ? B1 C19 1.638(3) . ? B1 C25 1.644(2) . ? B1 C37 1.653(2) . ? N1 O1 1.3338(16) . ? N1 C5 1.338(2) . ? N1 C1 1.340(2) . ? N2 C12 1.3301(19) . ? N2 O2 1.3331(15) . ? N2 C10 1.3368(19) . ? N3 C13 1.328(2) . ? N3 C18 1.3337(19) . ? N3 O3 1.3372(14) . ? O2 Co1 2.0893(11) 1_655 ? C1 C2 1.371(2) . ? C1 H1A 0.9300 . ? C2 C3 1.384(2) . ? C2 H2A 0.9300 . ? C3 C4 1.371(2) . ? C3 C6 1.503(2) . ? C4 C5 1.372(2) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.538(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.500(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C11 1.374(2) . ? C8 C9 1.376(2) . ? C9 C10 1.366(2) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.369(2) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.367(2) . ? C13 H13A 0.9300 . ? C14 C15 1.377(2) . ? C14 H14A 0.9300 . ? C15 C17 1.373(2) . ? C15 C16 1.501(2) . ? C16 C16 1.468(4) 3 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.360(2) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.397(2) . ? C19 C24 1.399(2) . ? C20 C21 1.389(3) . ? C20 H20A 0.9300 . ? C21 C22 1.373(3) . ? C21 H21A 0.9300 . ? C22 C23 1.368(3) . ? C22 H22A 0.9300 . ? C23 C24 1.376(3) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.396(2) . ? C25 C30 1.399(2) . ? C26 C27 1.394(3) . ? C26 H26A 0.9300 . ? C27 C28 1.371(3) . ? C27 H27A 0.9300 . ? C28 C29 1.362(3) . ? C28 H28A 0.9300 . ? C29 C30 1.377(3) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.393(2) . ? C31 C36 1.396(2) . ? C32 C33 1.383(3) . ? C32 H32A 0.9300 . ? C33 C34 1.365(3) . ? C33 H33A 0.9300 . ? C34 C35 1.370(3) . ? C34 H34A 0.9300 . ? C35 C36 1.389(2) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C42 1.393(2) . ? C37 C38 1.396(2) . ? C38 C39 1.381(2) . ? C38 H38A 0.9300 . ? C39 C40 1.357(3) . ? C39 H39A 0.9300 . ? C40 C41 1.373(3) . ? C40 H40A 0.9300 . ? C41 C42 1.388(2) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O3 180.00(4) . 3_556 ? O3 Co1 O1 87.14(4) . . ? O3 Co1 O1 92.86(4) 3_556 . ? O3 Co1 O1 92.86(4) . 3_556 ? O3 Co1 O1 87.14(4) 3_556 3_556 ? O1 Co1 O1 180.00(4) . 3_556 ? O3 Co1 O2 85.86(4) . 3_656 ? O3 Co1 O2 94.14(4) 3_556 3_656 ? O1 Co1 O2 94.86(4) . 3_656 ? O1 Co1 O2 85.14(4) 3_556 3_656 ? O3 Co1 O2 94.14(4) . 1_455 ? O3 Co1 O2 85.86(4) 3_556 1_455 ? O1 Co1 O2 85.14(4) . 1_455 ? O1 Co1 O2 94.86(4) 3_556 1_455 ? O2 Co1 O2 180.0 3_656 1_455 ? C31 B1 C19 113.38(14) . . ? C31 B1 C25 103.71(13) . . ? C19 B1 C25 111.22(14) . . ? C31 B1 C37 111.57(14) . . ? C19 B1 C37 103.34(13) . . ? C25 B1 C37 113.93(14) . . ? O1 N1 C5 118.43(14) . . ? O1 N1 C1 121.69(13) . . ? C5 N1 C1 119.88(15) . . ? C12 N2 O2 118.72(12) . . ? C12 N2 C10 119.97(14) . . ? O2 N2 C10 121.24(12) . . ? C13 N3 C18 120.17(14) . . ? C13 N3 O3 119.55(13) . . ? C18 N3 O3 120.24(13) . . ? N1 O1 Co1 127.25(8) . . ? N2 O2 Co1 126.78(9) . 1_655 ? N3 O3 Co1 118.09(8) . . ? N1 C1 C2 120.05(15) . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C1 C2 C3 121.89(16) . . ? C1 C2 H2A 119.1 . . ? C3 C2 H2A 119.1 . . ? C4 C3 C2 115.84(16) . . ? C4 C3 C6 121.88(15) . . ? C2 C3 C6 122.26(16) . . ? C3 C4 C5 121.53(16) . . ? C3 C4 H4A 119.2 . . ? C5 C4 H4A 119.2 . . ? N1 C5 C4 120.79(17) . . ? N1 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C3 C6 C7 113.27(14) . . ? C3 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? C3 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C8 C7 C6 111.64(14) . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C11 C8 C9 115.59(15) . . ? C11 C8 C7 122.20(15) . . ? C9 C8 C7 122.02(15) . . ? C10 C9 C8 122.02(16) . . ? C10 C9 H9A 119.0 . . ? C8 C9 H9A 119.0 . . ? N2 C10 C9 120.02(15) . . ? N2 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C12 C11 C8 121.51(15) . . ? C12 C11 H11A 119.2 . . ? C8 C11 H11A 119.2 . . ? N2 C12 C11 120.61(15) . . ? N2 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? N3 C13 C14 120.38(17) . . ? N3 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C13 C14 C15 121.16(17) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C17 C15 C14 116.44(15) . . ? C17 C15 C16 121.16(17) . . ? C14 C15 C16 122.35(17) . . ? C16 C16 C15 114.62(19) 3 . ? C16 C16 H16A 108.6 3 . ? C15 C16 H16A 108.6 . . ? C16 C16 H16B 108.6 3 . ? C15 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? C18 C17 C15 121.11(16) . . ? C18 C17 H17A 119.4 . . ? C15 C17 H17A 119.4 . . ? N3 C18 C17 120.73(15) . . ? N3 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C20 C19 C24 114.69(17) . . ? C20 C19 B1 125.27(16) . . ? C24 C19 B1 119.75(15) . . ? C21 C20 C19 122.41(19) . . ? C21 C20 H20A 118.8 . . ? C19 C20 H20A 118.8 . . ? C22 C21 C20 120.4(2) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C23 C22 C21 119.1(2) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C22 C23 C24 120.2(2) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C23 C24 C19 123.28(19) . . ? C23 C24 H24A 118.4 . . ? C19 C24 H24A 118.4 . . ? C26 C25 C30 114.51(17) . . ? C26 C25 B1 123.00(15) . . ? C30 C25 B1 122.17(16) . . ? C27 C26 C25 122.8(2) . . ? C27 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? C28 C27 C26 119.6(2) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C29 C28 C27 119.7(2) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C30 120.2(2) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C29 C30 C25 123.2(2) . . ? C29 C30 H30A 118.4 . . ? C25 C30 H30A 118.4 . . ? C32 C31 C36 114.55(17) . . ? C32 C31 B1 123.15(15) . . ? C36 C31 B1 122.02(15) . . ? C33 C32 C31 122.78(19) . . ? C33 C32 H32A 118.6 . . ? C31 C32 H32A 118.6 . . ? C34 C33 C32 120.7(2) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C33 C34 C35 119.0(2) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C34 C35 C36 119.9(2) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C35 C36 C31 123.11(19) . . ? C35 C36 H36A 118.4 . . ? C31 C36 H36A 118.4 . . ? C42 C37 C38 114.41(16) . . ? C42 C37 B1 119.01(16) . . ? C38 C37 B1 126.33(15) . . ? C39 C38 C37 122.91(19) . . ? C39 C38 H38A 118.5 . . ? C37 C38 H38A 118.5 . . ? C40 C39 C38 120.7(2) . . ? C40 C39 H39A 119.7 . . ? C38 C39 H39A 119.7 . . ? C39 C40 C41 119.13(19) . . ? C39 C40 H40A 120.4 . . ? C41 C40 H40A 120.4 . . ? C40 C41 C42 119.8(2) . . ? C40 C41 H41A 120.1 . . ? C42 C41 H41A 120.1 . . ? C41 C42 C37 123.1(2) . . ? C41 C42 H42A 118.5 . . ? C37 C42 H42A 118.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.224 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.035