# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. M.Schroder' _publ_contact_author_email M.SCHRODER@NOTTINGHAM.AC.UK _publ_section_title ;Synthesis of Pyridazinyl Ligands for Multimetallic Complexes ; loop_ _publ_author_name M.Schroder A.Blake N.Champness F.Thebault C.Wilson data_Compound_L1a _database_code_depnum_ccdc_archive 'CCDC 619843' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H22 N8' _chemical_formula_sum 'C34 H22 N8' _chemical_formula_weight 542.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.0136(17) _cell_length_b 29.216(8) _cell_length_c 7.656(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.536(6) _cell_angle_gamma 90.00 _cell_volume 1344.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1075 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 22.95 _exptl_crystal_description Column _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.262 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.062 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7907 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.1094 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3390 _reflns_number_gt 1382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' ?' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON (Spek,2003)' _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^)+(0.0594P)^2^+0.0957P] 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 3046 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1262 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.888 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.6953(4) 0.34856(7) 0.6340(3) 0.0374(6) Uani 1 1 d . . . N2 N 0.2492(4) 0.31781(7) 0.3391(3) 0.0337(6) Uani 1 1 d . . . N3 N 0.0805(4) 0.33756(7) 0.2483(3) 0.0351(6) Uani 1 1 d . . . N4 N -0.0973(4) 0.44165(7) 0.0871(3) 0.0373(6) Uani 1 1 d . . . C1 C 0.8758(5) 0.33033(10) 0.7111(4) 0.0433(8) Uani 1 1 d . . . H1 H 0.9714 0.3499 0.7777 0.052 Uiso 1 1 calc R . . C2 C 0.9319(5) 0.28482(10) 0.6998(4) 0.0457(8) Uani 1 1 d . . . H2 H 1.0633 0.2734 0.7561 0.055 Uiso 1 1 calc R . . C3 C 0.7940(5) 0.25648(10) 0.6058(4) 0.0471(8) Uani 1 1 d . . . H3 H 0.8288 0.2249 0.5956 0.056 Uiso 1 1 calc R . . C4 C 0.6042(5) 0.27379(9) 0.5258(4) 0.0418(8) Uani 1 1 d . . . H4 H 0.5056 0.2545 0.4609 0.050 Uiso 1 1 calc R . . C5 C 0.5607(4) 0.32025(9) 0.5425(3) 0.0319(7) Uani 1 1 d . . . C6 C 0.3652(4) 0.34258(8) 0.4567(3) 0.0295(6) Uani 1 1 d . . . C7 C 0.3087(4) 0.38782(8) 0.4952(3) 0.0304(6) Uani 1 1 d . . . H7 H 0.3905 0.4043 0.5825 0.037 Uiso 1 1 calc R . . C8 C 0.1347(4) 0.40827(8) 0.4064(3) 0.0270(6) Uani 1 1 d . . . C9 C 0.0278(4) 0.38141(8) 0.2770(3) 0.0292(6) Uani 1 1 d . . . C10 C -0.1462(4) 0.40034(8) 0.1554(3) 0.0300(6) Uani 1 1 d . . . C11 C -0.3406(4) 0.37675(9) 0.1141(4) 0.0348(7) Uani 1 1 d . . . H11 H -0.3659 0.3472 0.1610 0.042 Uiso 1 1 calc R . . C12 C -0.4960(5) 0.39695(10) 0.0042(4) 0.0410(7) Uani 1 1 d . . . H12 H -0.6327 0.3820 -0.0236 0.049 Uiso 1 1 calc R . . C13 C -0.4496(5) 0.43935(10) -0.0651(4) 0.0440(8) Uani 1 1 d . . . H13 H -0.5540 0.4541 -0.1414 0.053 Uiso 1 1 calc R . . C14 C -0.2492(5) 0.46004(10) -0.0217(4) 0.0432(8) Uani 1 1 d . . . H14 H -0.2179 0.4890 -0.0723 0.052 Uiso 1 1 calc R . . C15 C 0.2130(4) 0.49175(8) 0.4447(3) 0.0313(7) Uani 1 1 d . . . H15 H 0.3598 0.4862 0.4069 0.038 Uiso 1 1 calc R . . C16 C 0.0627(4) 0.45575(8) 0.4522(3) 0.0270(6) Uani 1 1 d . . . C17 C -0.1508(4) 0.46426(8) 0.5080(3) 0.0318(6) Uani 1 1 d . . . H17 H -0.2550 0.4399 0.5139 0.038 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 N1 0.0345(14) 0.0373(14) 0.0401(15) 0.0004(11) -0.0043(12) 0.0071(11) N2 0.0359(14) 0.0265(12) 0.0386(15) 0.0007(10) 0.0002(12) 0.0006(10) N3 0.0400(15) 0.0260(12) 0.0393(14) -0.0040(10) 0.0020(12) -0.0029(10) N4 0.0453(15) 0.0327(13) 0.0334(14) 0.0004(11) -0.0072(12) -0.0005(11) C1 0.0369(18) 0.0512(19) 0.0416(18) 0.0046(15) -0.0042(15) 0.0066(15) C2 0.0407(19) 0.051(2) 0.045(2) 0.0158(16) 0.0064(16) 0.0172(16) C3 0.054(2) 0.0341(17) 0.053(2) 0.0085(15) 0.0067(17) 0.0141(15) C4 0.049(2) 0.0289(15) 0.0473(19) 0.0035(13) 0.0044(16) 0.0060(13) C5 0.0331(16) 0.0300(15) 0.0327(16) 0.0052(12) 0.0066(13) 0.0025(12) C6 0.0327(16) 0.0245(14) 0.0316(16) 0.0040(12) 0.0046(13) -0.0011(12) C7 0.0327(16) 0.0261(14) 0.0326(16) -0.0021(12) 0.0016(13) -0.0022(12) C8 0.0259(15) 0.0251(14) 0.0303(15) 0.0007(11) 0.0029(12) -0.0011(11) C9 0.0298(15) 0.0258(14) 0.0321(16) -0.0018(12) 0.0026(12) -0.0052(12) C10 0.0355(17) 0.0279(14) 0.0267(15) -0.0047(12) 0.0013(12) 0.0018(12) C11 0.0331(16) 0.0389(16) 0.0323(16) -0.0039(13) -0.0009(13) -0.0035(13) C12 0.0327(17) 0.0528(19) 0.0374(17) -0.0108(15) -0.0011(14) -0.0038(14) C13 0.0430(19) 0.055(2) 0.0339(17) -0.0059(15) -0.0094(15) 0.0089(15) C14 0.056(2) 0.0386(17) 0.0348(18) 0.0004(14) -0.0094(15) 0.0010(15) C15 0.0254(15) 0.0298(15) 0.0385(16) -0.0040(12) 0.0011(12) 0.0007(12) C16 0.0279(15) 0.0263(14) 0.0263(14) -0.0013(11) -0.0058(12) 0.0003(12) C17 0.0289(15) 0.0255(14) 0.0410(17) -0.0026(12) -0.0008(13) -0.0036(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.333(3) . ? N1 C5 1.341(3) . ? N2 C6 1.337(3) . ? N2 N3 1.344(3) . ? N3 C9 1.339(3) . ? N4 C14 1.333(3) . ? N4 C10 1.351(3) . ? C1 C2 1.375(4) . ? C1 H1 0.9500 . ? C2 C3 1.363(4) . ? C2 H2 0.9500 . ? C3 C4 1.377(4) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 H4 0.9500 . ? C5 C6 1.483(4) . ? C6 C7 1.398(3) . ? C7 C8 1.369(3) . ? C7 H7 0.9500 . ? C8 C9 1.406(3) . ? C8 C16 1.498(3) . ? C9 C10 1.488(4) . ? C10 C11 1.386(4) . ? C11 C12 1.374(4) . ? C11 H11 0.9500 . ? C12 C13 1.379(4) . ? C12 H12 0.9500 . ? C13 C14 1.381(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.389(3) . ? C15 C17 1.389(3) 3_566 ? C15 H15 0.9500 . ? C16 C17 1.386(3) . ? C17 H17 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C5 117.2(2) . . ? C6 N2 N3 119.2(2) . . ? C9 N3 N2 120.3(2) . . ? C14 N4 C10 116.7(2) . . ? N1 C1 C2 123.8(3) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.3(3) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 122.6(3) . . ? N1 C5 C6 114.9(2) . . ? C4 C5 C6 122.5(3) . . ? N2 C6 C7 121.9(2) . . ? N2 C6 C5 117.0(2) . . ? C7 C6 C5 121.1(2) . . ? C8 C7 C6 119.6(2) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 115.8(2) . . ? C7 C8 C16 120.6(2) . . ? C9 C8 C16 123.5(2) . . ? N3 C9 C8 122.9(2) . . ? N3 C9 C10 114.8(2) . . ? C8 C9 C10 122.3(2) . . ? N4 C10 C11 123.2(3) . . ? N4 C10 C9 114.7(2) . . ? C11 C10 C9 122.2(2) . . ? C12 C11 C10 118.8(3) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C13 118.7(3) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C12 C13 C14 119.0(3) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? N4 C14 C13 123.6(3) . . ? N4 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? C16 C15 C17 120.6(2) . 3_566 ? C16 C15 H15 119.7 . . ? C17 C15 H15 119.7 3_566 . ? C17 C16 C15 119.1(2) . . ? C17 C16 C8 120.9(2) . . ? C15 C16 C8 119.9(2) . . ? C16 C17 C15 120.3(2) . 3_566 ? C16 C17 H17 119.9 . . ? C15 C17 H17 119.9 3_566 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.19 _refine_diff_density_min -0.25 _refine_diff_density_rms 0.05 #===END data_Compound_L1b _database_code_depnum_ccdc_archive 'CCDC 619844' _exptl_special_details ; ? ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H22 N8, 4(C H Cl3)' _chemical_formula_sum 'C38 H26 Cl12 N8' _chemical_formula_weight 1020.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 6.2391(4) _cell_length_b 11.6260(8) _cell_length_c 15.4933(11) _cell_angle_alpha 93.237(1) _cell_angle_beta 91.763(1) _cell_angle_gamma 100.927(1) _cell_volume 1100.70(13) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6392 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 30.76 _exptl_crystal_description Column _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.540 _exptl_crystal_size_mid 0.066 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 514 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.708 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.67680 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker ApexII CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12506 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 30.91 _reflns_number_total 6702 _reflns_number_gt 5837 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 version 1.0-27 (Bruker, 2005)' _computing_cell_refinement 'Bruker SAINT version 7.12a (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution Sir-2002 _computing_structure_refinement 'SHELXS97 (Sheldrick, 1998)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0486P)^2^+1.1232P] 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 0.050(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6702 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Cl1 Cl 0.96910(17) 0.61978(7) 0.44801(7) 0.0785(3) Uani 1 1 d . . . Cl2 Cl 1.04527(15) 0.86910(7) 0.43333(6) 0.0706(3) Uani 1 1 d . . . Cl3 Cl 0.61589(12) 0.74552(7) 0.46753(4) 0.0593(2) Uani 1 1 d . . . Cl4 Cl -0.01567(10) 0.35496(8) -0.04487(5) 0.0656(2) Uani 1 1 d . . . Cl5 Cl 0.42969(8) 0.32609(5) -0.05828(4) 0.04782(17) Uani 1 1 d . . . Cl6 Cl 0.18019(11) 0.35928(6) -0.21189(5) 0.05146(18) Uani 1 1 d . . . N1 N 0.4733(3) 0.33373(15) 0.17677(11) 0.0319(3) Uani 1 1 d . . . N2 N 0.8751(2) 0.24427(13) 0.31489(9) 0.0252(3) Uani 1 1 d . . . N3 N 1.0172(2) 0.17209(13) 0.31450(9) 0.0248(3) Uani 1 1 d . . . N4 N 1.1753(3) -0.07229(14) 0.20701(10) 0.0295(3) Uani 1 1 d . . . C1 C 0.3213(3) 0.40103(19) 0.18093(15) 0.0374(4) Uani 1 1 d . . . H1 H 0.2360 0.4057 0.1299 0.045 Uiso 1 1 calc R . . C2 C 0.2814(3) 0.46401(18) 0.25485(16) 0.0391(4) Uani 1 1 d . . . H2 H 0.1712 0.5103 0.2546 0.047 Uiso 1 1 calc R . . C3 C 0.4057(4) 0.45811(18) 0.32939(15) 0.0373(4) Uani 1 1 d . . . H3 H 0.3812 0.4998 0.3815 0.045 Uiso 1 1 calc R . . C4 C 0.5661(3) 0.39065(17) 0.32700(12) 0.0307(4) Uani 1 1 d . . . H4 H 0.6548 0.3858 0.3771 0.037 Uiso 1 1 calc R . . C5 C 0.5943(3) 0.32992(14) 0.24932(11) 0.0245(3) Uani 1 1 d . . . C6 C 0.7576(3) 0.25236(14) 0.24290(10) 0.0226(3) Uani 1 1 d . . . C7 C 0.7853(3) 0.19035(15) 0.16551(10) 0.0230(3) Uani 1 1 d . . . H7 H 0.7023 0.1989 0.1147 0.028 Uiso 1 1 calc R . . C8 C 0.9346(3) 0.11636(14) 0.16353(10) 0.0213(3) Uani 1 1 d . . . C9 C 1.0476(3) 0.10816(14) 0.24292(10) 0.0218(3) Uani 1 1 d . . . C10 C 1.2067(3) 0.02930(15) 0.25568(10) 0.0227(3) Uani 1 1 d . . . C11 C 1.3768(3) 0.06119(16) 0.31802(11) 0.0261(3) Uani 1 1 d . . . H11 H 1.3910 0.1324 0.3528 0.031 Uiso 1 1 calc R . . C12 C 1.5251(3) -0.01266(17) 0.32858(12) 0.0304(4) Uani 1 1 d . . . H12 H 1.6425 0.0072 0.3706 0.036 Uiso 1 1 calc R . . C13 C 1.4985(3) -0.11564(19) 0.27679(13) 0.0347(4) Uani 1 1 d . . . H13 H 1.5993 -0.1671 0.2812 0.042 Uiso 1 1 calc R . . C14 C 1.3206(4) -0.14185(18) 0.21821(13) 0.0354(4) Uani 1 1 d . . . H14 H 1.3007 -0.2137 0.1839 0.042 Uiso 1 1 calc R . . C15 C 1.1768(3) 0.07073(15) 0.04572(10) 0.0247(3) Uani 1 1 d . . . H15 H 1.2976 0.1194 0.0766 0.030 Uiso 1 1 calc R . . C16 C 0.9705(3) 0.05458(14) 0.08023(9) 0.0214(3) Uani 1 1 d . . . C17 C 0.7937(3) -0.01578(15) 0.03388(10) 0.0237(3) Uani 1 1 d . . . H17 H 0.6524 -0.0262 0.0568 0.028 Uiso 1 1 calc R . . C18 C 0.8990(4) 0.7520(2) 0.48497(13) 0.0413(5) Uani 1 1 d . . . H18 H 0.9353 0.7648 0.5485 0.050 Uiso 1 1 calc R . . C19 C 0.1700(3) 0.29858(18) -0.11034(14) 0.0338(4) Uani 1 1 d . . . H19 H 0.1196 0.2117 -0.1194 0.041 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 Cl1 0.0997(7) 0.0484(4) 0.0893(6) -0.0054(4) -0.0338(5) 0.0275(4) Cl2 0.0814(5) 0.0520(4) 0.0753(5) 0.0131(3) 0.0294(4) -0.0017(3) Cl3 0.0572(4) 0.0781(5) 0.0392(3) 0.0056(3) -0.0032(3) 0.0045(3) Cl4 0.0340(3) 0.1007(6) 0.0619(4) -0.0335(4) -0.0039(3) 0.0251(3) Cl5 0.0269(2) 0.0503(3) 0.0664(4) 0.0065(3) -0.0063(2) 0.0081(2) Cl6 0.0478(3) 0.0510(3) 0.0603(4) 0.0236(3) 0.0041(3) 0.0153(2) N1 0.0304(7) 0.0321(7) 0.0338(8) -0.0014(6) -0.0068(6) 0.0102(6) N2 0.0251(6) 0.0307(7) 0.0203(6) -0.0015(5) -0.0013(5) 0.0074(5) N3 0.0244(6) 0.0315(7) 0.0188(6) -0.0013(5) -0.0021(5) 0.0074(5) N4 0.0334(8) 0.0312(7) 0.0250(7) -0.0028(5) -0.0048(6) 0.0111(6) C1 0.0320(9) 0.0368(9) 0.0450(11) 0.0013(8) -0.0070(8) 0.0128(7) C2 0.0309(9) 0.0332(9) 0.0560(13) 0.0013(9) 0.0022(8) 0.0135(7) C3 0.0382(10) 0.0340(9) 0.0419(10) -0.0028(8) 0.0074(8) 0.0129(8) C4 0.0322(9) 0.0306(8) 0.0301(8) -0.0017(6) 0.0029(7) 0.0085(7) C5 0.0236(7) 0.0237(7) 0.0258(7) 0.0005(6) 0.0004(6) 0.0039(6) C6 0.0219(7) 0.0250(7) 0.0206(7) 0.0001(5) 0.0000(5) 0.0039(5) C7 0.0218(7) 0.0280(7) 0.0192(6) 0.0001(5) -0.0016(5) 0.0054(6) C8 0.0210(7) 0.0253(7) 0.0170(6) -0.0003(5) -0.0004(5) 0.0038(5) C9 0.0206(7) 0.0260(7) 0.0183(6) 0.0010(5) -0.0010(5) 0.0033(5) C10 0.0225(7) 0.0273(7) 0.0186(6) 0.0030(5) 0.0000(5) 0.0052(5) C11 0.0236(7) 0.0295(8) 0.0244(7) 0.0028(6) -0.0029(6) 0.0030(6) C12 0.0245(8) 0.0362(9) 0.0310(8) 0.0066(7) -0.0036(6) 0.0068(6) C13 0.0332(9) 0.0405(10) 0.0342(9) 0.0053(7) -0.0004(7) 0.0164(8) C14 0.0408(10) 0.0348(9) 0.0327(9) -0.0034(7) -0.0056(8) 0.0158(8) C15 0.0203(7) 0.0321(8) 0.0200(7) -0.0023(6) -0.0019(5) 0.0024(6) C16 0.0223(7) 0.0265(7) 0.0157(6) 0.0010(5) -0.0012(5) 0.0056(5) C17 0.0196(7) 0.0308(8) 0.0200(6) -0.0006(6) 0.0000(5) 0.0041(6) C18 0.0550(13) 0.0433(11) 0.0219(8) 0.0029(7) -0.0036(8) 0.0003(9) C19 0.0266(8) 0.0342(9) 0.0412(10) -0.0001(7) -0.0006(7) 0.0082(7) 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 Cl1 C18 1.748(3) . ? Cl2 C18 1.739(2) . ? Cl3 C18 1.765(3) . ? Cl4 C19 1.757(2) . ? Cl5 C19 1.753(2) . ? Cl6 C19 1.759(2) . ? N1 C1 1.339(2) . ? N1 C5 1.342(2) . ? N2 N3 1.331(2) . ? N2 C6 1.333(2) . ? N3 C9 1.339(2) . ? N4 C14 1.338(2) . ? N4 C10 1.343(2) . ? C1 C2 1.379(3) . ? C1 H1 0.9500 . ? C2 C3 1.383(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.394(2) . ? C4 H4 0.9500 . ? C5 C6 1.485(2) . ? C6 C7 1.396(2) . ? C7 C8 1.383(2) . ? C7 H7 0.9500 . ? C8 C9 1.416(2) . ? C8 C16 1.485(2) . ? C9 C10 1.489(2) . ? C10 C11 1.394(2) . ? C11 C12 1.388(2) . ? C11 H11 0.9500 . ? C12 C13 1.383(3) . ? C12 H12 0.9500 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C17 1.390(2) 2_755 ? C15 C16 1.393(2) . ? C15 H15 0.9500 . ? C16 C17 1.395(2) . ? C17 C15 1.390(2) 2_755 ? C17 H17 0.9500 . ? C18 H18 1.0000 . ? C19 H19 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C5 117.00(17) . . ? N3 N2 C6 119.61(14) . . ? N2 N3 C9 121.52(14) . . ? C14 N4 C10 117.11(16) . . ? N1 C1 C2 123.98(19) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C1 C2 C3 118.36(18) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C2 C3 C4 119.12(19) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 118.40(18) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 123.13(16) . . ? N1 C5 C6 115.53(15) . . ? C4 C5 C6 121.30(15) . . ? N2 C6 C7 121.74(15) . . ? N2 C6 C5 116.63(14) . . ? C7 C6 C5 121.62(14) . . ? C8 C7 C6 119.43(14) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 116.00(14) . . ? C7 C8 C16 119.24(14) . . ? C9 C8 C16 124.74(14) . . ? N3 C9 C8 121.63(15) . . ? N3 C9 C10 113.89(13) . . ? C8 C9 C10 124.49(14) . . ? N4 C10 C11 122.72(15) . . ? N4 C10 C9 117.57(14) . . ? C11 C10 C9 119.69(15) . . ? C12 C11 C10 119.04(16) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 118.70(17) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C14 118.23(17) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? N4 C14 C13 124.14(18) . . ? N4 C14 H14 117.9 . . ? C13 C14 H14 117.9 . . ? C17 C15 C16 120.11(14) 2_755 . ? C17 C15 H15 119.9 2_755 . ? C16 C15 H15 119.9 . . ? C15 C16 C17 119.53(14) . . ? C15 C16 C8 120.76(14) . . ? C17 C16 C8 119.63(14) . . ? C15 C17 C16 120.36(14) 2_755 . ? C15 C17 H17 119.8 2_755 . ? C16 C17 H17 119.8 . . ? Cl2 C18 Cl1 110.83(14) . . ? Cl2 C18 Cl3 109.98(13) . . ? Cl1 C18 Cl3 110.17(13) . . ? Cl2 C18 H18 108.6 . . ? Cl1 C18 H18 108.6 . . ? Cl3 C18 H18 108.6 . . ? Cl5 C19 Cl4 109.95(11) . . ? Cl5 C19 Cl6 110.67(11) . . ? Cl4 C19 Cl6 110.87(11) . . ? Cl5 C19 H19 108.4 . . ? Cl4 C19 H19 108.4 . . ? Cl6 C19 H19 108.4 . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.96 _refine_diff_density_min -0.68 _refine_diff_density_rms 0.06 #===END data_Compound_L2 _database_code_depnum_ccdc_archive 'CCDC 619845' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Carbon atom in chloroform disordered into two positions. Chloroform geometry restrained using SADI instruction. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H24 N8, C H Cl3' _chemical_formula_sum 'C33 H25 Cl3 N8' _chemical_formula_weight 639.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.367(6) _cell_length_b 5.9124(15) _cell_length_c 21.707(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.744(4) _cell_angle_gamma 90.00 _cell_volume 2884.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1472 _cell_measurement_theta_min 3.404 _cell_measurement_theta_max 25.129 _exptl_crystal_description Column _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.672 _exptl_crystal_size_mid 0.035 _exptl_crystal_size_min 0.028 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.359 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17206 _diffrn_reflns_av_R_equivalents 0.1321 _diffrn_reflns_av_sigmaI/netI 0.1418 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3307 _reflns_number_gt 1784 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' ?' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON (Spek,2003)' _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^)+(0.0528P)^2^] 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 3259 _refine_ls_number_parameters 204 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1412 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.893 _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 Cl1 Cl 0.06432(4) 0.88867(16) 0.27593(5) 0.0457(3) Uani 1 1 d D . . Cl2 Cl 0.0000 0.4669(2) 0.2500 0.0616(5) Uani 1 2 d SD . . N1 N 0.29949(11) 0.6834(4) 0.17553(13) 0.0250(6) Uani 1 1 d . . . N2 N 0.14913(11) 0.5808(4) 0.09269(12) 0.0212(6) Uani 1 1 d . . . N3 N 0.10848(10) 0.4420(4) 0.05186(12) 0.0206(6) Uani 1 1 d . . . N4 N 0.08771(11) -0.0374(4) -0.04752(12) 0.0207(6) Uani 1 1 d . . . C1 C 0.33405(15) 0.8257(6) 0.22206(17) 0.0338(8) Uani 1 1 d . . . H1 H 0.3736 0.7788 0.2480 0.041 Uiso 1 1 calc R . . C2 C 0.31674(15) 1.0345(6) 0.23517(16) 0.0304(8) Uani 1 1 d . . . H2 H 0.3435 1.1284 0.2690 0.037 Uiso 1 1 calc R . . C3 C 0.25954(15) 1.1048(5) 0.19817(15) 0.0277(7) Uani 1 1 d . . . H3 H 0.2462 1.2496 0.2053 0.033 Uiso 1 1 calc R . . C4 C 0.22235(14) 0.9617(5) 0.15084(14) 0.0212(7) Uani 1 1 d . . . H4 H 0.1825 1.0054 0.1252 0.025 Uiso 1 1 calc R . . C5 C 0.24319(13) 0.7524(5) 0.14054(14) 0.0183(6) Uani 1 1 d . . . C6 C 0.20307(13) 0.5947(5) 0.08992(14) 0.0186(6) Uani 1 1 d . . . C7 C 0.21806(13) 0.4768(4) 0.04235(14) 0.0162(6) Uani 1 1 d . . . C8 C 0.17447(12) 0.3399(5) -0.00264(14) 0.0155(6) Uani 1 1 d . . . C9 C 0.12052(12) 0.3209(5) 0.00608(14) 0.0170(6) Uani 1 1 d . . . C10 C 0.07144(13) 0.1676(5) -0.03425(14) 0.0178(6) Uani 1 1 d . . . C11 C 0.01227(13) 0.2344(5) -0.05450(14) 0.0211(7) Uani 1 1 d . . . H11 H 0.0023 0.3809 -0.0441 0.025 Uiso 1 1 calc R . . C12 C -0.03181(13) 0.0810(5) -0.09030(14) 0.0230(7) Uani 1 1 d . . . H12 H -0.0727 0.1208 -0.1051 0.028 Uiso 1 1 calc R . . C13 C -0.01515(14) -0.1297(5) -0.10397(14) 0.0244(7) Uani 1 1 d . . . H13 H -0.0444 -0.2381 -0.1280 0.029 Uiso 1 1 calc R . . C14 C 0.04433(13) -0.1808(5) -0.08240(15) 0.0253(7) Uani 1 1 d . . . H14 H 0.0553 -0.3258 -0.0928 0.030 Uiso 1 1 calc R . . C15 C 0.27817(12) 0.4978(5) 0.03797(14) 0.0184(7) Uani 1 1 d . . . H15A H 0.3005 0.6231 0.0672 0.022 Uiso 1 1 calc R . . H15B H 0.2725 0.5362 -0.0085 0.022 Uiso 1 1 calc R . . C16 C 0.18449(12) 0.2238(5) -0.05906(14) 0.0186(6) Uani 1 1 d . . . H16A H 0.2051 0.3299 -0.0782 0.022 Uiso 1 1 calc R . . H16B H 0.1454 0.1873 -0.0945 0.022 Uiso 1 1 calc R . . C17 C -0.0023(2) 0.7489(7) 0.2267(3) 0.0325(16) Uani 0.50 1 d PD . . H17 H -0.0039 0.7490 0.1800 0.039 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0377(5) 0.0453(6) 0.0363(5) -0.0005(5) -0.0054(4) -0.0031(5) Cl2 0.0785(12) 0.0273(7) 0.0839(12) 0.000 0.0368(10) 0.000 N1 0.0200(14) 0.0294(15) 0.0217(14) -0.0070(11) 0.0038(12) -0.0006(12) N2 0.0191(13) 0.0239(14) 0.0179(13) -0.0036(11) 0.0042(11) -0.0007(11) N3 0.0146(13) 0.0254(14) 0.0185(13) -0.0030(11) 0.0028(11) 0.0002(11) N4 0.0196(14) 0.0171(13) 0.0247(14) -0.0001(11) 0.0077(11) -0.0020(11) C1 0.0217(18) 0.044(2) 0.0293(19) -0.0091(17) 0.0027(15) -0.0034(17) C2 0.031(2) 0.036(2) 0.0232(17) -0.0108(15) 0.0096(15) -0.0145(16) C3 0.041(2) 0.0210(16) 0.0226(17) -0.0021(14) 0.0145(15) -0.0033(16) C4 0.0218(17) 0.0242(16) 0.0175(15) 0.0013(13) 0.0075(13) 0.0002(14) C5 0.0166(15) 0.0235(16) 0.0155(15) 0.0018(12) 0.0071(13) 0.0009(13) C6 0.0185(15) 0.0179(15) 0.0166(14) 0.0031(12) 0.0037(12) 0.0057(13) C7 0.0161(15) 0.0127(14) 0.0177(15) 0.0033(12) 0.0042(12) 0.0031(12) C8 0.0138(14) 0.0154(14) 0.0146(14) 0.0041(11) 0.0026(12) 0.0035(12) C9 0.0150(15) 0.0165(14) 0.0168(14) 0.0025(12) 0.0031(12) 0.0032(12) C10 0.0158(15) 0.0216(16) 0.0171(15) 0.0033(12) 0.0076(12) 0.0002(13) C11 0.0186(16) 0.0248(16) 0.0190(15) 0.0011(13) 0.0061(13) 0.0025(13) C12 0.0137(15) 0.0332(18) 0.0181(15) 0.0023(14) 0.0016(12) 0.0001(14) C13 0.0255(17) 0.0283(17) 0.0164(15) -0.0013(14) 0.0047(13) -0.0077(15) C14 0.0262(18) 0.0228(16) 0.0267(17) -0.0015(13) 0.0101(15) -0.0007(15) C15 0.0191(16) 0.0165(15) 0.0182(15) -0.0027(12) 0.0057(13) -0.0049(12) C16 0.0132(15) 0.0228(16) 0.0169(15) -0.0002(12) 0.0027(12) -0.0026(13) C17 0.038(4) 0.032(4) 0.025(4) -0.001(3) 0.009(4) -0.007(3) 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 Cl1 C17 1.704(5) 2 ? Cl1 C17 1.765(5) . ? Cl2 C17 1.737(5) 2 ? Cl2 C17 1.737(5) . ? N1 C1 1.334(4) . ? N1 C5 1.349(4) . ? N2 N3 1.327(3) . ? N2 C6 1.341(4) . ? N3 C9 1.346(4) . ? N4 C14 1.338(4) . ? N4 C10 1.341(4) . ? C1 C2 1.369(5) . ? C1 H1 0.9500 . ? C2 C3 1.376(5) . ? C2 H2 0.9500 . ? C3 C4 1.368(4) . ? C3 H3 0.9500 . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? C5 C6 1.484(4) . ? C6 C7 1.406(4) . ? C7 C8 1.391(4) . ? C7 C15 1.509(4) . ? C8 C9 1.403(4) . ? C8 C16 1.504(4) . ? C9 C10 1.486(4) . ? C10 C11 1.392(4) . ? C11 C12 1.391(4) . ? C11 H11 0.9500 . ? C12 C13 1.378(4) . ? C12 H12 0.9500 . ? C13 C14 1.374(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.559(4) 7 ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C15 1.559(4) 7 ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 Cl1 1.704(5) 2 ? C17 H17 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C5 116.3(3) . . ? N3 N2 C6 120.0(2) . . ? N2 N3 C9 120.2(2) . . ? C14 N4 C10 117.4(3) . . ? N1 C1 C2 124.8(3) . . ? N1 C1 H1 117.6 . . ? C2 C1 H1 117.6 . . ? C1 C2 C3 118.3(3) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 118.6(3) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 122.3(3) . . ? N1 C5 C6 117.6(3) . . ? C4 C5 C6 120.1(3) . . ? N2 C6 C7 122.7(3) . . ? N2 C6 C5 112.5(2) . . ? C7 C6 C5 124.8(3) . . ? C8 C7 C6 117.3(3) . . ? C8 C7 C15 120.0(2) . . ? C6 C7 C15 122.7(3) . . ? C7 C8 C9 116.9(3) . . ? C7 C8 C16 121.1(2) . . ? C9 C8 C16 121.9(3) . . ? N3 C9 C8 122.7(3) . . ? N3 C9 C10 113.8(2) . . ? C8 C9 C10 123.5(3) . . ? N4 C10 C11 123.0(3) . . ? N4 C10 C9 116.1(2) . . ? C11 C10 C9 120.8(3) . . ? C12 C11 C10 118.2(3) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C13 C12 C11 118.8(3) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? N4 C14 C13 123.5(3) . . ? N4 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? C7 C15 C16 112.5(2) . 7 ? C7 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 7 . ? C7 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 7 . ? H15A C15 H15B 107.8 . . ? C8 C16 C15 113.8(2) . 7 ? C8 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 7 . ? C8 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 7 . ? H16A C16 H16B 107.7 . . ? Cl1 C17 Cl2 113.8(3) 2 . ? Cl1 C17 Cl1 112.9(3) 2 . ? Cl2 C17 Cl1 110.8(3) . . ? Cl1 C17 H17 106.2 2 . ? Cl2 C17 H17 106.2 . . ? Cl1 C17 H17 106.2 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.31 _refine_diff_density_min -0.42 _refine_diff_density_rms 0.07 #===END data_Compound_L4 _database_code_depnum_ccdc_archive 'CCDC 619846' _exptl_special_details ; Extinction coefficient refined to 0. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 N8, 2(C2 H6 O S)' _chemical_formula_sum 'C34 H34 N8 O2 S2' _chemical_formula_weight 650.81 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' S S 0.1246 0.1234 '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 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.067(2) _cell_length_b 5.5010(6) _cell_length_c 16.801(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.921(2) _cell_angle_gamma 90.00 _cell_volume 1627.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1955 _cell_measurement_theta_min 2.313 _cell_measurement_theta_max 25.837 _exptl_crystal_description Column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.209 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.433 _exptl_absorpt_correction_T_max 0.654 _exptl_absorpt_process_details '(SHELXTL version 6.12; Bruker, 2001)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3702 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3702 _reflns_number_gt 2717 _reflns_threshold_expression >2s(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' ?' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON (Spek,2003)' _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^)+(0.0689P)^2^] 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 3702 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 S S 0.45772(4) 0.56216(13) 0.12860(4) 0.0366(2) Uani 1 1 d . . . O O 0.53833(11) 0.5689(4) 0.17574(14) 0.0514(6) Uani 1 1 d . . . N1 N 0.07583(11) 0.1512(4) 0.13410(12) 0.0252(5) Uani 1 1 d . . . N2 N 0.23447(11) 0.3763(3) 0.06720(11) 0.0223(4) Uani 1 1 d . . . N3 N 0.26023(11) 0.5466(4) 0.02375(11) 0.0230(4) Uani 1 1 d . . . N4 N 0.19325(11) 1.0302(4) -0.11654(12) 0.0246(5) Uani 1 1 d . . . C1 C 0.06164(14) -0.0200(5) 0.18561(15) 0.0283(6) Uani 1 1 d . . . H1 H 0.0142 -0.0150 0.2010 0.034 Uiso 1 1 calc R . . C2 C 0.11192(14) -0.2034(4) 0.21766(14) 0.0269(6) Uani 1 1 d . . . H2 H 0.0990 -0.3218 0.2534 0.032 Uiso 1 1 calc R . . C3 C 0.18096(14) -0.2094(4) 0.19642(14) 0.0265(6) Uani 1 1 d . . . H3 H 0.2170 -0.3320 0.2178 0.032 Uiso 1 1 calc R . . C4 C 0.19760(14) -0.0361(4) 0.14376(13) 0.0231(5) Uani 1 1 d . . . H4 H 0.2452 -0.0369 0.1285 0.028 Uiso 1 1 calc R . . C5 C 0.14316(13) 0.1406(4) 0.11333(13) 0.0204(5) Uani 1 1 d . . . C6 C 0.16000(13) 0.3321(4) 0.05685(13) 0.0198(5) Uani 1 1 d . . . C7 C 0.10509(13) 0.4569(4) -0.00209(13) 0.0194(5) Uani 1 1 d . . . C8 C 0.13283(13) 0.6367(4) -0.04448(13) 0.0222(5) Uani 1 1 d . . . H8 H 0.0989 0.7321 -0.0835 0.027 Uiso 1 1 calc R . . C9 C 0.21018(13) 0.6781(4) -0.03022(13) 0.0203(5) Uani 1 1 d . . . C10 C 0.24346(13) 0.8695(4) -0.07435(13) 0.0216(5) Uani 1 1 d . . . C11 C 0.32025(14) 0.8802(5) -0.07158(15) 0.0302(6) Uani 1 1 d . . . H11 H 0.3538 0.7623 -0.0419 0.036 Uiso 1 1 calc R . . C12 C 0.34753(15) 1.0653(5) -0.11269(16) 0.0338(6) Uani 1 1 d . . . H12 H 0.4003 1.0776 -0.1111 0.041 Uiso 1 1 calc R . . C13 C 0.29727(15) 1.2318(5) -0.15604(15) 0.0310(6) Uani 1 1 d . . . H13 H 0.3144 1.3607 -0.1850 0.037 Uiso 1 1 calc R . . C14 C 0.22155(15) 1.2057(4) -0.15617(14) 0.0296(6) Uani 1 1 d . . . H14 H 0.1870 1.3202 -0.1864 0.036 Uiso 1 1 calc R . . C15 C 0.02085(12) 0.4097(4) -0.02230(13) 0.0211(5) Uani 1 1 d . . . H15A H 0.0111 0.2417 -0.0062 0.025 Uiso 1 1 calc R . . H15B H 0.0010 0.4250 -0.0820 0.025 Uiso 1 1 calc R . . C16 C 0.43792(18) 0.2550(6) 0.0980(2) 0.0534(9) Uani 1 1 d . . . H16A H 0.4655 0.2124 0.0560 0.080 Uiso 1 1 calc R . . H16B H 0.3833 0.2355 0.0760 0.080 Uiso 1 1 calc R . . H16C H 0.4541 0.1478 0.1453 0.080 Uiso 1 1 calc R . . C17 C 0.40029(16) 0.5706(6) 0.20150(17) 0.0421(7) Uani 1 1 d . . . H17A H 0.4034 0.7324 0.2265 0.063 Uiso 1 1 calc R . . H17B H 0.4183 0.4485 0.2439 0.063 Uiso 1 1 calc R . . H17C H 0.3475 0.5358 0.1744 0.063 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 S 0.0397(4) 0.0309(4) 0.0385(4) 0.0074(3) 0.0070(3) -0.0033(3) O 0.0336(12) 0.0517(14) 0.0684(14) 0.0019(11) 0.0103(10) -0.0141(10) N1 0.0233(11) 0.0237(11) 0.0286(10) 0.0023(9) 0.0057(9) -0.0018(8) N2 0.0213(11) 0.0214(11) 0.0232(10) 0.0015(8) 0.0032(8) 0.0007(8) N3 0.0216(10) 0.0229(11) 0.0243(10) 0.0025(9) 0.0044(8) -0.0006(8) N4 0.0298(11) 0.0207(11) 0.0227(9) 0.0001(8) 0.0043(8) 0.0000(9) C1 0.0267(13) 0.0273(14) 0.0322(13) 0.0034(11) 0.0090(11) -0.0039(11) C2 0.0363(15) 0.0200(13) 0.0236(11) 0.0020(10) 0.0051(11) -0.0080(11) C3 0.0343(15) 0.0196(13) 0.0231(11) -0.0005(10) 0.0010(10) 0.0018(10) C4 0.0257(13) 0.0217(12) 0.0211(11) -0.0035(10) 0.0037(9) 0.0013(10) C5 0.0243(12) 0.0165(12) 0.0184(10) -0.0034(9) 0.0004(9) -0.0019(9) C6 0.0203(12) 0.0176(12) 0.0205(11) -0.0032(9) 0.0027(9) 0.0019(9) C7 0.0203(12) 0.0178(11) 0.0189(10) -0.0038(9) 0.0017(9) 0.0008(9) C8 0.0227(13) 0.0235(13) 0.0188(10) 0.0005(10) 0.0015(9) 0.0021(10) C9 0.0236(12) 0.0192(12) 0.0178(10) -0.0016(9) 0.0041(9) 0.0037(9) C10 0.0265(13) 0.0207(12) 0.0171(10) -0.0028(9) 0.0039(9) -0.0003(10) C11 0.0275(14) 0.0290(14) 0.0320(13) 0.0068(11) 0.0027(11) 0.0005(11) C12 0.0293(14) 0.0399(16) 0.0333(13) 0.0047(12) 0.0092(11) -0.0081(12) C13 0.0419(16) 0.0241(14) 0.0277(12) 0.0006(11) 0.0091(12) -0.0087(12) C14 0.0405(16) 0.0203(13) 0.0270(12) 0.0016(10) 0.0054(11) 0.0037(11) C15 0.0188(12) 0.0199(12) 0.0224(11) -0.0021(9) 0.0003(9) -0.0021(9) C16 0.0421(18) 0.043(2) 0.066(2) -0.0206(16) -0.0066(16) 0.0066(15) C17 0.0297(15) 0.056(2) 0.0363(15) -0.0064(14) -0.0025(12) -0.0040(14) 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 S O 1.495(2) . ? S C17 1.774(3) . ? S C16 1.779(3) . ? N1 C5 1.340(3) . ? N1 C1 1.342(3) . ? N2 N3 1.334(3) . ? N2 C6 1.340(3) . ? N3 C9 1.340(3) . ? N4 C14 1.338(3) . ? N4 C10 1.349(3) . ? C1 C2 1.383(3) . ? C1 H1 0.9500 . ? C2 C3 1.372(3) . ? C2 H2 0.9500 . ? C3 C4 1.379(3) . ? C3 H3 0.9500 . ? C4 C5 1.396(3) . ? C4 H4 0.9500 . ? C5 C6 1.494(3) . ? C6 C7 1.413(3) . ? C7 C8 1.377(3) . ? C7 C15 1.506(3) . ? C8 C9 1.383(3) . ? C8 H8 0.9500 . ? C9 C10 1.490(3) . ? C10 C11 1.379(3) . ? C11 C12 1.382(3) . ? C11 H11 0.9500 . ? C12 C13 1.378(4) . ? C12 H12 0.9500 . ? C13 C14 1.375(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C15 1.539(4) 3_565 ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O S C17 106.54(13) . . ? O S C16 106.59(14) . . ? C17 S C16 96.51(16) . . ? C5 N1 C1 117.0(2) . . ? N3 N2 C6 121.30(19) . . ? N2 N3 C9 118.96(19) . . ? C14 N4 C10 116.6(2) . . ? N1 C1 C2 124.0(2) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C1 118.2(2) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 118.7(2) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 122.8(2) . . ? N1 C5 C6 117.4(2) . . ? C4 C5 C6 119.8(2) . . ? N2 C6 C7 122.0(2) . . ? N2 C6 C5 112.75(19) . . ? C7 C6 C5 125.2(2) . . ? C8 C7 C6 115.6(2) . . ? C8 C7 C15 118.3(2) . . ? C6 C7 C15 126.2(2) . . ? C7 C8 C9 120.0(2) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? N3 C9 C8 122.1(2) . . ? N3 C9 C10 115.6(2) . . ? C8 C9 C10 122.3(2) . . ? N4 C10 C11 122.9(2) . . ? N4 C10 C9 115.2(2) . . ? C11 C10 C9 121.9(2) . . ? C10 C11 C12 118.9(2) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C13 C12 C11 119.2(2) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 118.0(2) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? N4 C14 C13 124.4(2) . . ? N4 C14 H14 117.8 . . ? C13 C14 H14 117.8 . . ? C7 C15 C15 111.0(2) . 3_565 ? C7 C15 H15A 109.4 . . ? C15 C15 H15A 109.4 3_565 . ? C7 C15 H15B 109.4 . . ? C15 C15 H15B 109.4 3_565 . ? H15A C15 H15B 108.0 . . ? S C16 H16A 109.5 . . ? S C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S C17 H17A 109.5 . . ? S C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.80 _refine_diff_density_min -0.28 _refine_diff_density_rms 0.06 #===END data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 619847' _exptl_special_details ; Chloroform molecules refined with partial occupency of 0.75 and 0.5. Methanol meolcule refined with partial occupency of 0.5. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H28 Cu4 N14 O22, 0.75(C H Cl3), 0.5(C H Cl3), 0.5(C H4 O)' _chemical_formula_sum 'C39.75 H37.25 Cl3.75 Cu4 N14 O22.50' _chemical_formula_weight 1458.18 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' Cu Cu 0.3201 1.2651 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.403(2) _cell_length_b 16.763(3) _cell_length_c 17.194(3) _cell_angle_alpha 80.373(3) _cell_angle_beta 82.560(3) _cell_angle_gamma 82.475(3) _cell_volume 2912.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5268 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 29.0 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1467 _exptl_absorpt_coefficient_mu 1.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.569 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.67680 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker ApexII CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 33424 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11774 _reflns_number_gt 7094 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 version 1.0-27 (Bruker, 2005)' _computing_cell_refinement 'Bruker SAINT version 7.12a (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXS97 (Sheldrick, 1998)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1219P)^2^+2.0290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed, except Me and OH of MeOH and Me H of bridging MeO' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11774 _refine_ls_number_parameters 798 _refine_ls_number_restraints 287 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.2130 _refine_ls_wR_factor_gt 0.1837 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.027 _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 Cu1 Cu 0.92851(8) 1.30054(4) 0.49668(4) 0.0351(2) Uani 1 1 d U . . Cu2 Cu 0.89126(7) 1.13788(4) 0.41775(4) 0.0321(2) Uani 1 1 d U . . Cu3 Cu 0.11792(8) 0.86306(5) 1.05454(4) 0.0378(2) Uani 1 1 d U . . Cu4 Cu 0.07393(8) 0.69484(5) 0.98666(4) 0.0384(2) Uani 1 1 d U . . Cl1 Cl 0.8100(2) 0.62625(17) 0.31923(16) 0.0579(7) Uani 0.75 1 d PDU . . Cl2 Cl 0.6699(3) 0.78645(15) 0.29743(16) 0.0593(7) Uani 0.75 1 d PDU . . Cl3 Cl 0.5325(3) 0.64420(19) 0.32391(17) 0.0660(8) Uani 0.75 1 d PDU . . Cl4 Cl 0.4861(3) 0.6152(2) 0.8788(2) 0.0500(8) Uani 0.50 1 d PDU . . Cl5 Cl 0.5288(4) 0.5587(4) 0.7268(3) 0.0883(17) Uani 0.50 1 d PDU . . Cl6 Cl 0.6049(4) 0.7146(3) 0.7423(3) 0.0873(16) Uani 0.50 1 d PDU . . O1 O 0.9685(4) 1.2364(2) 0.4122(2) 0.0363(10) Uani 1 1 d U . . O2 O 0.7366(5) 1.3598(3) 0.4473(3) 0.0469(11) Uani 1 1 d U . . O3 O 1.2319(6) 1.4153(3) 0.4648(4) 0.0701(17) Uani 1 1 d U . . O4 O 1.0367(5) 1.3905(3) 0.4508(3) 0.0435(11) Uani 1 1 d U . . O5 O 1.1657(5) 1.2995(3) 0.5206(3) 0.0501(12) Uani 1 1 d U . . O6 O 1.0893(5) 1.0653(3) 0.3145(3) 0.0522(12) Uani 1 1 d U . . O7 O 1.0305(5) 1.1125(3) 0.1988(3) 0.0569(14) Uani 1 1 d U . . O8 O 0.9038(4) 1.1379(3) 0.3033(2) 0.0390(10) Uani 1 1 d U . . O9 O 0.5431(8) 1.2358(5) 0.4995(5) 0.118(3) Uani 1 1 d U . . O10 O 0.6794(5) 1.2080(3) 0.4008(3) 0.0533(13) Uani 1 1 d U . . O11 O 0.5442(6) 1.1229(4) 0.4624(4) 0.0786(18) Uani 1 1 d U . . O12 O 0.0475(5) 0.7622(3) 1.0674(3) 0.0432(11) Uani 1 1 d U . . O13 O -0.1359(5) 0.6991(3) 0.9733(4) 0.0626(14) Uani 1 1 d U . . O14 O 0.4782(6) 0.7719(5) 1.1438(4) 0.083(2) Uani 1 1 d U . . O15 O 0.4297(6) 0.8075(4) 1.0235(3) 0.0799(19) Uani 1 1 d U . . O16 O 0.2838(6) 0.8265(3) 1.1251(3) 0.0613(14) Uani 1 1 d U . . O17 O 0.0506(7) 0.8790(5) 1.2348(4) 0.094(2) Uani 1 1 d U . . O18 O -0.0249(5) 0.9207(3) 1.1222(3) 0.0560(13) Uani 1 1 d U . . O19 O -0.1321(6) 0.9512(4) 1.2286(3) 0.0724(17) Uani 1 1 d U . . O20 O 0.2661(6) 0.5965(4) 1.0518(4) 0.0679(16) Uani 1 1 d U . . O21 O 0.0598(5) 0.5875(3) 1.0573(3) 0.0449(11) Uani 1 1 d U . . O22 O 0.1822(6) 0.4941(3) 1.1247(4) 0.0693(17) Uani 1 1 d U . . O23 O 0.6767(8) 0.6601(5) 1.0877(6) 0.042(2) Uani 0.50 1 d PU . . H23A H 0.6794 0.6907 1.0437 0.062 Uiso 0.50 1 calc PR . . N1 N 0.8753(5) 1.3442(3) 0.5990(3) 0.0362(11) Uani 1 1 d U . . N2 N 0.8461(5) 1.2067(3) 0.5615(3) 0.0308(11) Uani 1 1 d U . . N3 N 0.8376(5) 1.1400(3) 0.5332(3) 0.0303(10) Uani 1 1 d U . . N4 N 0.8401(5) 1.0259(3) 0.4527(3) 0.0319(11) Uani 1 1 d U . . N5 N 0.1912(5) 0.9676(3) 1.0134(3) 0.0378(12) Uani 1 1 d U . . N6 N 0.1857(5) 0.8480(3) 0.9427(3) 0.0301(10) Uani 1 1 d U . . N7 N 0.1681(5) 0.7806(3) 0.9174(3) 0.0322(11) Uani 1 1 d U . . N8 N 0.1236(6) 0.6442(3) 0.8876(3) 0.0430(13) Uani 1 1 d U . . N9 N 1.1481(6) 1.3681(3) 0.4796(4) 0.0471(14) Uani 1 1 d U . . N10 N 1.0119(5) 1.1035(3) 0.2718(3) 0.0392(12) Uani 1 1 d U . . N11 N 0.5856(6) 1.1890(4) 0.4490(4) 0.0549(16) Uani 1 1 d U . . N12 N 0.3967(7) 0.8021(4) 1.0940(4) 0.0580(17) Uani 1 1 d U . . N13 N -0.0312(6) 0.9146(4) 1.1973(3) 0.0516(16) Uani 1 1 d U . . N14 N 0.1736(7) 0.5589(4) 1.0778(4) 0.0503(14) Uani 1 1 d U . . C1 C 0.8930(7) 1.4179(4) 0.6135(4) 0.0429(15) Uani 1 1 d U . . H1 H 0.9378 1.4533 0.5731 0.051 Uiso 1 1 calc R . . C2 C 0.8486(7) 1.4441(4) 0.6852(4) 0.0482(17) Uani 1 1 d U . . H2 H 0.8629 1.4965 0.6942 0.058 Uiso 1 1 calc R . . C3 C 0.7821(8) 1.3921(4) 0.7443(4) 0.0502(18) Uani 1 1 d U . . H3 H 0.7494 1.4092 0.7938 0.060 Uiso 1 1 calc R . . C4 C 0.7643(7) 1.3157(4) 0.7303(4) 0.0428(16) Uani 1 1 d U . . H4 H 0.7214 1.2787 0.7700 0.051 Uiso 1 1 calc R . . C5 C 0.8106(6) 1.2952(4) 0.6569(4) 0.0341(13) Uani 1 1 d U . . C6 C 0.7904(6) 1.2162(4) 0.6337(3) 0.0318(13) Uani 1 1 d U . . C7 C 0.7171(6) 1.1578(4) 0.6799(4) 0.0348(13) Uani 1 1 d U . . H7 H 0.6790 1.1646 0.7319 0.042 Uiso 1 1 calc R . . C8 C 0.7012(6) 1.0894(4) 0.6477(3) 0.0311(12) Uani 1 1 d U . . C9 C 0.7688(6) 1.0806(4) 0.5728(3) 0.0306(12) Uani 1 1 d U . . C10 C 0.7805(6) 1.0109(4) 0.5288(3) 0.0324(13) Uani 1 1 d U . . C11 C 0.7394(6) 0.9358(4) 0.5586(4) 0.0381(14) Uani 1 1 d U . . H11 H 0.6984 0.9254 0.6114 0.046 Uiso 1 1 calc R . . C12 C 0.7590(7) 0.8748(4) 0.5099(4) 0.0417(15) Uani 1 1 d U . . H12 H 0.7309 0.8228 0.5293 0.050 Uiso 1 1 calc R . . C13 C 0.8180(6) 0.8911(4) 0.4354(4) 0.0383(14) Uani 1 1 d U . . H13 H 0.8318 0.8503 0.4019 0.046 Uiso 1 1 calc R . . C14 C 0.8588(6) 0.9674(4) 0.4073(4) 0.0357(14) Uani 1 1 d U . . H14 H 0.9008 0.9780 0.3547 0.043 Uiso 1 1 calc R . . C15 C 0.6095(6) 1.0333(3) 0.6927(3) 0.0305(12) Uani 1 1 d U . . C16 C 0.5001(6) 1.0207(4) 0.6598(4) 0.0348(13) Uani 1 1 d U . . H16 H 0.4866 1.0453 0.6071 0.042 Uiso 1 1 calc R . . C17 C 0.4114(6) 0.9723(4) 0.7042(3) 0.0345(13) Uani 1 1 d U . . H17 H 0.3364 0.9637 0.6819 0.041 Uiso 1 1 calc R . . C18 C 0.4301(6) 0.9357(4) 0.7814(3) 0.0330(13) Uani 1 1 d U . . C19 C 0.5400(6) 0.9471(4) 0.8136(4) 0.0354(14) Uani 1 1 d U . . H19 H 0.5537 0.9220 0.8661 0.042 Uiso 1 1 calc R . . C20 C 0.6293(6) 0.9948(4) 0.7697(3) 0.0358(14) Uani 1 1 d U . . H20 H 0.7054 1.0017 0.7918 0.043 Uiso 1 1 calc R . . C21 C 0.1740(7) 1.0310(4) 1.0545(4) 0.0472(17) Uani 1 1 d U . . H21 H 0.1254 1.0259 1.1055 0.057 Uiso 1 1 calc R . . C22 C 0.2254(8) 1.1025(4) 1.0242(5) 0.0523(18) Uani 1 1 d U . . H22 H 0.2126 1.1464 1.0540 0.063 Uiso 1 1 calc R . . C23 C 0.2959(7) 1.1102(4) 0.9499(4) 0.0480(17) Uani 1 1 d U . . H23 H 0.3330 1.1591 0.9286 0.058 Uiso 1 1 calc R . . C24 C 0.3124(7) 1.0453(4) 0.9061(4) 0.0411(15) Uani 1 1 d U . . H24 H 0.3586 1.0497 0.8544 0.049 Uiso 1 1 calc R . . C25 C 0.2593(6) 0.9749(4) 0.9406(3) 0.0334(13) Uani 1 1 d U . . C26 C 0.2620(6) 0.9010(4) 0.9010(3) 0.0319(13) Uani 1 1 d U . . C27 C 0.3311(6) 0.8854(4) 0.8278(3) 0.0317(13) Uani 1 1 d U . . C28 C 0.3033(6) 0.8176(4) 0.7991(3) 0.0325(13) Uani 1 1 d U . . H28 H 0.3403 0.8066 0.7480 0.039 Uiso 1 1 calc R . . C29 C 0.2205(6) 0.7661(4) 0.8464(3) 0.0329(13) Uani 1 1 d U . . C30 C 0.1878(7) 0.6885(4) 0.8266(4) 0.0393(15) Uani 1 1 d U . . C31 C 0.2181(7) 0.6637(4) 0.7538(4) 0.0454(17) Uani 1 1 d U . . H31 H 0.2615 0.6969 0.7108 0.055 Uiso 1 1 calc R . . C32 C 0.1839(9) 0.5896(4) 0.7445(4) 0.057(2) Uani 1 1 d U . . H32 H 0.2051 0.5705 0.6949 0.068 Uiso 1 1 calc R . . C33 C 0.1199(8) 0.5440(4) 0.8064(4) 0.056(2) Uani 1 1 d U . . H33 H 0.0965 0.4927 0.8003 0.067 Uiso 1 1 calc R . . C34 C 0.0891(8) 0.5719(4) 0.8774(4) 0.056(2) Uani 1 1 d U . . H34 H 0.0429 0.5401 0.9203 0.067 Uiso 1 1 calc R . . C35 C 0.6654(5) 0.6861(3) 0.3476(5) 0.0373(18) Uani 0.75 1 d PDU . . H35 H 0.6570 0.6864 0.4061 0.045 Uiso 0.75 1 calc PR . . C36 C 0.5873(10) 0.6150(5) 0.7884(4) 0.053(3) Uani 0.50 1 d PDU . . H36 H 0.6756 0.5881 0.8008 0.064 Uiso 0.50 1 calc PR . . C37 C 0.6172(15) 0.5954(9) 1.0835(9) 0.055(4) Uani 0.50 1 d PU . . H37A H 0.6144 0.5595 1.1347 0.082 Uiso 0.50 1 calc PR . . H37B H 0.6653 0.5658 1.0423 0.082 Uiso 0.50 1 calc PR . . H37C H 0.5280 0.6134 1.0703 0.082 Uiso 0.50 1 calc PR . . C38 C 1.0600(8) 1.2598(5) 0.3456(4) 0.0524(19) Uani 1 1 d U . . H38A H 1.0308 1.2476 0.2973 0.079 Uiso 1 1 calc R . . H38B H 1.1457 1.2296 0.3535 0.079 Uiso 1 1 calc R . . H38C H 1.0663 1.3184 0.3401 0.079 Uiso 1 1 calc R . . C39 C 0.6505(10) 1.4239(6) 0.4704(5) 0.076(3) Uani 1 1 d U . . H39A H 0.5784 1.4347 0.4373 0.114 Uiso 1 1 calc R . . H39B H 0.6961 1.4726 0.4641 0.114 Uiso 1 1 calc R . . H39C H 0.6161 1.4098 0.5261 0.114 Uiso 1 1 calc R . . C40 C -0.0391(8) 0.7379(5) 1.1366(4) 0.0503(19) Uani 1 1 d U . . H40A H 0.0095 0.7251 1.1830 0.075 Uiso 1 1 calc R . . H40B H -0.0778 0.6896 1.1297 0.075 Uiso 1 1 calc R . . H40C H -0.1085 0.7823 1.1443 0.075 Uiso 1 1 calc R . . C41 C -0.1897(10) 0.7082(6) 0.8973(7) 0.088(3) Uani 1 1 d U . . H41A H -0.2847 0.7086 0.9068 0.133 Uiso 1 1 calc R . . H41B H -0.1524 0.6625 0.8696 0.133 Uiso 1 1 calc R . . H41C H -0.1680 0.7594 0.8647 0.133 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 Cu1 0.0442(5) 0.0275(4) 0.0337(4) -0.0049(3) 0.0018(3) -0.0101(3) Cu2 0.0409(5) 0.0297(4) 0.0257(4) -0.0051(3) 0.0022(3) -0.0084(3) Cu3 0.0441(5) 0.0411(5) 0.0291(4) -0.0101(3) 0.0062(3) -0.0122(4) Cu4 0.0506(5) 0.0347(4) 0.0298(4) -0.0049(3) 0.0061(3) -0.0153(4) Cl1 0.0525(15) 0.0673(17) 0.0550(15) -0.0259(13) -0.0022(11) 0.0069(12) Cl2 0.086(2) 0.0408(13) 0.0550(15) -0.0077(11) -0.0184(13) -0.0113(12) Cl3 0.0579(16) 0.085(2) 0.0625(16) -0.0021(14) -0.0196(13) -0.0338(15) Cl4 0.0395(19) 0.054(2) 0.057(2) -0.0076(16) -0.0157(16) 0.0033(15) Cl5 0.049(2) 0.137(5) 0.090(3) -0.067(3) -0.021(2) 0.025(3) Cl6 0.046(2) 0.094(3) 0.100(4) 0.024(3) 0.014(2) 0.005(2) O1 0.043(2) 0.032(2) 0.033(2) -0.0059(17) 0.0060(18) -0.0118(18) O2 0.054(3) 0.040(3) 0.045(3) -0.008(2) -0.005(2) 0.002(2) O3 0.064(4) 0.050(3) 0.100(5) -0.008(3) -0.004(3) -0.029(3) O4 0.053(3) 0.026(2) 0.052(3) -0.0038(19) -0.003(2) -0.011(2) O5 0.062(3) 0.035(3) 0.054(3) -0.007(2) -0.007(2) -0.005(2) O6 0.044(3) 0.062(3) 0.049(3) -0.006(2) -0.004(2) 0.000(2) O7 0.068(3) 0.068(4) 0.031(2) -0.014(2) 0.012(2) -0.003(3) O8 0.050(3) 0.037(2) 0.029(2) -0.0071(18) 0.0007(19) -0.003(2) O9 0.114(6) 0.127(7) 0.116(6) -0.064(5) 0.030(5) -0.012(5) O10 0.039(3) 0.068(3) 0.042(3) 0.013(2) 0.004(2) -0.002(2) O11 0.069(4) 0.066(4) 0.101(5) -0.010(3) 0.002(4) -0.024(3) O12 0.056(3) 0.042(2) 0.032(2) -0.0063(19) 0.008(2) -0.019(2) O13 0.050(3) 0.060(3) 0.081(4) -0.013(3) -0.013(3) -0.010(3) O14 0.054(3) 0.127(6) 0.058(4) 0.019(4) -0.009(3) -0.016(4) O15 0.074(4) 0.113(6) 0.048(3) -0.009(3) -0.010(3) 0.004(4) O16 0.062(3) 0.060(3) 0.059(3) 0.002(3) -0.010(3) -0.006(3) O17 0.095(5) 0.097(5) 0.090(5) -0.016(4) -0.046(4) 0.022(4) O18 0.061(3) 0.061(3) 0.046(3) -0.009(2) -0.002(2) -0.008(3) O19 0.074(4) 0.093(5) 0.052(3) -0.029(3) 0.000(3) 0.004(3) O20 0.057(3) 0.074(4) 0.073(4) -0.005(3) -0.006(3) -0.015(3) O21 0.058(3) 0.037(2) 0.038(2) -0.0008(19) 0.003(2) -0.012(2) O22 0.104(5) 0.036(3) 0.073(4) -0.005(3) -0.034(3) -0.004(3) O23 0.015(4) 0.040(5) 0.065(6) 0.003(4) 0.007(4) -0.013(4) N1 0.044(3) 0.029(3) 0.037(3) -0.005(2) -0.007(2) -0.008(2) N2 0.041(3) 0.026(2) 0.028(2) -0.0070(19) -0.003(2) -0.007(2) N3 0.039(3) 0.026(2) 0.026(2) -0.0029(18) -0.002(2) -0.005(2) N4 0.041(3) 0.030(2) 0.027(2) -0.0066(19) -0.002(2) -0.009(2) N5 0.046(3) 0.035(3) 0.033(3) -0.009(2) 0.000(2) -0.010(2) N6 0.034(3) 0.027(2) 0.030(2) -0.0033(19) 0.001(2) -0.009(2) N7 0.040(3) 0.030(3) 0.027(2) -0.0056(19) 0.000(2) -0.008(2) N8 0.063(4) 0.034(3) 0.035(3) -0.007(2) 0.000(3) -0.018(3) N9 0.050(3) 0.035(3) 0.057(4) -0.012(3) 0.005(3) -0.013(3) N10 0.041(3) 0.041(3) 0.036(3) -0.009(2) 0.004(2) -0.009(2) N11 0.041(3) 0.046(4) 0.074(4) -0.006(3) 0.001(3) -0.005(3) N12 0.052(4) 0.064(4) 0.050(4) 0.015(3) -0.006(3) -0.005(3) N13 0.058(4) 0.063(4) 0.037(3) -0.024(3) 0.016(3) -0.021(3) N14 0.068(4) 0.039(3) 0.047(3) -0.011(3) -0.008(3) -0.010(3) C1 0.051(4) 0.031(3) 0.049(4) -0.008(3) -0.004(3) -0.008(3) C2 0.061(5) 0.032(4) 0.057(4) -0.019(3) -0.007(3) -0.010(3) C3 0.071(5) 0.043(4) 0.040(4) -0.019(3) -0.002(3) -0.008(3) C4 0.058(4) 0.037(3) 0.036(3) -0.007(3) -0.004(3) -0.013(3) C5 0.042(4) 0.026(3) 0.036(3) -0.007(2) -0.008(3) -0.002(3) C6 0.037(3) 0.032(3) 0.029(3) -0.006(2) -0.005(2) -0.007(2) C7 0.041(4) 0.035(3) 0.029(3) -0.006(2) 0.001(3) -0.006(3) C8 0.035(3) 0.032(3) 0.026(3) -0.001(2) -0.004(2) -0.004(2) C9 0.034(3) 0.034(3) 0.026(3) -0.006(2) -0.005(2) -0.008(3) C10 0.035(3) 0.031(3) 0.031(3) -0.006(2) 0.000(2) -0.007(3) C11 0.046(4) 0.036(3) 0.032(3) -0.007(2) 0.004(3) -0.009(3) C12 0.049(4) 0.025(3) 0.050(4) -0.005(3) 0.001(3) -0.009(3) C13 0.050(4) 0.033(3) 0.035(3) -0.014(3) -0.008(3) -0.003(3) C14 0.041(4) 0.038(3) 0.031(3) -0.012(2) -0.003(3) -0.003(3) C15 0.036(3) 0.026(3) 0.029(3) -0.007(2) 0.001(2) -0.003(2) C16 0.045(4) 0.031(3) 0.026(3) 0.000(2) -0.004(2) -0.003(3) C17 0.037(3) 0.037(3) 0.031(3) -0.004(2) -0.007(2) -0.010(3) C18 0.043(3) 0.027(3) 0.029(3) -0.003(2) 0.002(2) -0.007(3) C19 0.039(3) 0.039(4) 0.028(3) 0.000(2) -0.003(2) -0.010(3) C20 0.037(3) 0.043(4) 0.028(3) -0.005(2) -0.001(2) -0.011(3) C21 0.057(4) 0.041(4) 0.046(4) -0.021(3) 0.000(3) -0.005(3) C22 0.066(5) 0.038(4) 0.059(4) -0.023(3) -0.011(4) -0.006(3) C23 0.053(4) 0.035(4) 0.057(4) -0.011(3) -0.003(3) -0.007(3) C24 0.047(4) 0.035(3) 0.043(4) -0.007(3) -0.005(3) -0.010(3) C25 0.041(4) 0.030(3) 0.030(3) -0.007(2) -0.004(2) -0.003(3) C26 0.039(3) 0.032(3) 0.025(3) -0.002(2) -0.003(2) -0.006(3) C27 0.033(3) 0.031(3) 0.031(3) -0.004(2) -0.001(2) -0.004(2) C28 0.040(3) 0.030(3) 0.026(3) -0.003(2) 0.002(2) -0.004(2) C29 0.039(3) 0.031(3) 0.028(3) -0.005(2) 0.000(2) -0.008(3) C30 0.051(4) 0.031(3) 0.035(3) -0.007(2) 0.007(3) -0.011(3) C31 0.063(5) 0.033(3) 0.040(3) -0.010(3) 0.007(3) -0.015(3) C32 0.091(6) 0.044(4) 0.039(4) -0.017(3) 0.003(4) -0.023(4) C33 0.086(6) 0.037(4) 0.049(4) -0.017(3) 0.004(4) -0.027(4) C34 0.087(6) 0.035(4) 0.048(4) -0.008(3) 0.009(4) -0.028(4) C35 0.037(4) 0.048(5) 0.030(4) -0.011(3) -0.005(3) -0.008(4) C36 0.014(6) 0.064(7) 0.086(9) -0.026(7) -0.017(5) 0.012(6) C37 0.055(9) 0.051(9) 0.060(9) -0.008(7) -0.002(7) -0.015(7) C38 0.061(5) 0.048(4) 0.047(4) -0.007(3) 0.013(3) -0.023(4) C39 0.084(6) 0.076(6) 0.062(5) -0.015(5) -0.003(5) 0.019(5) C40 0.060(5) 0.058(5) 0.031(3) -0.007(3) 0.013(3) -0.021(4) C41 0.097(7) 0.057(6) 0.125(8) -0.038(6) -0.048(7) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.921(4) . ? Cu1 N2 1.992(5) . ? Cu1 O4 1.995(4) . ? Cu1 N1 2.001(5) . ? Cu1 O2 2.309(5) . ? Cu2 O1 1.912(4) . ? Cu2 O8 1.955(4) . ? Cu2 N4 1.992(5) . ? Cu2 N3 1.996(5) . ? Cu2 O10 2.387(5) . ? Cu3 O12 1.898(4) . ? Cu3 N5 1.987(5) . ? Cu3 N6 2.006(5) . ? Cu3 O18 2.012(5) . ? Cu3 O16 2.200(6) . ? Cu4 O12 1.902(4) . ? Cu4 N7 1.984(5) . ? Cu4 O21 2.006(4) . ? Cu4 N8 2.007(5) . ? Cu4 O13 2.215(5) . ? Cl1 C35 1.757(6) . ? Cl2 C35 1.761(6) . ? Cl3 C35 1.750(6) . ? Cl4 C36 1.760(7) . ? Cl5 C36 1.742(7) . ? Cl6 C36 1.747(7) . ? O1 C38 1.428(7) . ? O2 C39 1.383(9) . ? O3 N9 1.227(7) . ? O4 N9 1.304(8) . ? O5 N9 1.249(7) . ? O6 N10 1.208(7) . ? O7 N10 1.231(7) . ? O8 N10 1.292(7) . ? O9 N11 1.267(9) . ? O10 N11 1.235(7) . ? O11 N11 1.217(8) . ? O12 C40 1.432(7) . ? O13 C41 1.464(11) . ? O14 N12 1.281(8) . ? O15 N12 1.207(8) . ? O16 N12 1.271(8) . ? O17 N13 1.173(8) . ? O18 N13 1.272(8) . ? O19 N13 1.250(8) . ? O20 N14 1.215(8) . ? O21 N14 1.288(8) . ? O22 N14 1.239(8) . ? O23 C37 1.333(16) . ? O23 H23A 0.8400 . ? N1 C1 1.341(8) . ? N1 C5 1.348(8) . ? N2 N3 1.310(6) . ? N2 C6 1.327(7) . ? N3 C9 1.341(7) . ? N4 C14 1.333(7) . ? N4 C10 1.372(7) . ? N5 C25 1.351(8) . ? N5 C21 1.353(8) . ? N6 N7 1.318(7) . ? N6 C26 1.326(7) . ? N7 C29 1.319(7) . ? N8 C30 1.337(8) . ? N8 C34 1.352(8) . ? C1 C2 1.382(10) . ? C1 H1 0.9500 . ? C2 C3 1.396(10) . ? C2 H2 0.9500 . ? C3 C4 1.382(9) . ? C3 H3 0.9500 . ? C4 C5 1.374(9) . ? C4 H4 0.9500 . ? C5 C6 1.492(8) . ? C6 C7 1.396(8) . ? C7 C8 1.389(8) . ? C7 H7 0.9500 . ? C8 C9 1.407(8) . ? C8 C15 1.481(8) . ? C9 C10 1.478(8) . ? C10 C11 1.377(8) . ? C11 C12 1.405(9) . ? C11 H11 0.9500 . ? C12 C13 1.349(9) . ? C12 H12 0.9500 . ? C13 C14 1.390(9) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.389(9) . ? C15 C20 1.401(8) . ? C16 C17 1.379(8) . ? C16 H16 0.9500 . ? C17 C18 1.393(8) . ? C17 H17 0.9500 . ? C18 C19 1.380(9) . ? C18 C27 1.482(8) . ? C19 C20 1.372(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.371(10) . ? C21 H21 0.9500 . ? C22 C23 1.384(10) . ? C22 H22 0.9500 . ? C23 C24 1.404(9) . ? C23 H23 0.9500 . ? C24 C25 1.379(9) . ? C24 H24 0.9500 . ? C25 C26 1.506(8) . ? C26 C27 1.413(8) . ? C27 C28 1.390(8) . ? C28 C29 1.387(8) . ? C28 H28 0.9500 . ? C29 C30 1.490(8) . ? C30 C31 1.370(9) . ? C31 C32 1.375(9) . ? C31 H31 0.9500 . ? C32 C33 1.356(10) . ? C32 H32 0.9500 . ? C33 C34 1.365(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 H35 1.0000 . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 87.67(18) . . ? O1 Cu1 O4 98.47(18) . . ? N2 Cu1 O4 167.4(2) . . ? O1 Cu1 N1 167.20(19) . . ? N2 Cu1 N1 79.7(2) . . ? O4 Cu1 N1 93.6(2) . . ? O1 Cu1 O2 91.16(18) . . ? N2 Cu1 O2 93.52(19) . . ? O4 Cu1 O2 97.38(19) . . ? N1 Cu1 O2 91.6(2) . . ? O1 Cu2 O8 96.58(18) . . ? O1 Cu2 N4 162.4(2) . . ? O8 Cu2 N4 97.68(19) . . ? O1 Cu2 N3 89.05(18) . . ? O8 Cu2 N3 167.7(2) . . ? N4 Cu2 N3 78.99(19) . . ? O1 Cu2 O10 93.24(19) . . ? O8 Cu2 O10 84.13(18) . . ? N4 Cu2 O10 98.3(2) . . ? N3 Cu2 O10 84.71(19) . . ? O12 Cu3 N5 166.1(2) . . ? O12 Cu3 N6 88.61(18) . . ? N5 Cu3 N6 78.4(2) . . ? O12 Cu3 O18 97.5(2) . . ? N5 Cu3 O18 90.4(2) . . ? N6 Cu3 O18 144.2(2) . . ? O12 Cu3 O16 99.9(2) . . ? N5 Cu3 O16 88.6(2) . . ? N6 Cu3 O16 106.4(2) . . ? O18 Cu3 O16 107.1(2) . . ? O12 Cu4 N7 88.16(19) . . ? O12 Cu4 O21 97.82(19) . . ? N7 Cu4 O21 155.0(2) . . ? O12 Cu4 N8 167.1(2) . . ? N7 Cu4 N8 78.9(2) . . ? O21 Cu4 N8 93.8(2) . . ? O12 Cu4 O13 95.1(2) . . ? N7 Cu4 O13 116.0(2) . . ? O21 Cu4 O13 87.8(2) . . ? N8 Cu4 O13 90.9(2) . . ? C38 O1 Cu2 118.9(4) . . ? C38 O1 Cu1 120.5(4) . . ? Cu2 O1 Cu1 120.6(2) . . ? C39 O2 Cu1 129.5(5) . . ? N9 O4 Cu1 104.5(4) . . ? N10 O8 Cu2 115.7(4) . . ? N11 O10 Cu2 119.6(4) . . ? C40 O12 Cu3 120.0(4) . . ? C40 O12 Cu4 117.3(4) . . ? Cu3 O12 Cu4 122.5(2) . . ? C41 O13 Cu4 124.7(6) . . ? N12 O16 Cu3 121.9(5) . . ? N13 O18 Cu3 124.3(5) . . ? N14 O21 Cu4 108.6(4) . . ? C37 O23 H23A 109.5 . . ? C1 N1 C5 117.9(6) . . ? C1 N1 Cu1 126.3(4) . . ? C5 N1 Cu1 115.8(4) . . ? N3 N2 C6 120.1(5) . . ? N3 N2 Cu1 122.4(4) . . ? C6 N2 Cu1 117.3(4) . . ? N2 N3 C9 122.9(5) . . ? N2 N3 Cu2 118.2(4) . . ? C9 N3 Cu2 117.2(4) . . ? C14 N4 C10 119.8(5) . . ? C14 N4 Cu2 124.5(4) . . ? C10 N4 Cu2 115.7(4) . . ? C25 N5 C21 119.5(6) . . ? C25 N5 Cu3 117.6(4) . . ? C21 N5 Cu3 122.9(5) . . ? N7 N6 C26 122.3(5) . . ? N7 N6 Cu3 119.0(3) . . ? C26 N6 Cu3 118.0(4) . . ? N6 N7 C29 120.2(5) . . ? N6 N7 Cu4 121.6(4) . . ? C29 N7 Cu4 118.0(4) . . ? C30 N8 C34 118.8(6) . . ? C30 N8 Cu4 116.5(4) . . ? C34 N8 Cu4 124.5(5) . . ? O3 N9 O5 122.6(7) . . ? O3 N9 O4 118.5(6) . . ? O5 N9 O4 118.9(5) . . ? O6 N10 O7 123.6(6) . . ? O6 N10 O8 119.1(5) . . ? O7 N10 O8 117.3(6) . . ? O11 N11 O10 126.0(7) . . ? O11 N11 O9 115.0(7) . . ? O10 N11 O9 117.6(7) . . ? O15 N12 O16 124.8(7) . . ? O15 N12 O14 120.5(7) . . ? O16 N12 O14 114.7(6) . . ? O17 N13 O19 122.1(7) . . ? O17 N13 O18 123.7(7) . . ? O19 N13 O18 114.2(7) . . ? O20 N14 O22 123.3(7) . . ? O20 N14 O21 119.2(6) . . ? O22 N14 O21 117.5(6) . . ? N1 C1 C2 122.3(6) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 118.7(6) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 119.6(6) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 117.7(6) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? N1 C5 C4 123.9(6) . . ? N1 C5 C6 113.8(5) . . ? C4 C5 C6 122.3(6) . . ? N2 C6 C7 121.4(5) . . ? N2 C6 C5 113.1(5) . . ? C7 C6 C5 125.4(5) . . ? C8 C7 C6 118.4(5) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 C9 117.5(5) . . ? C7 C8 C15 117.9(5) . . ? C9 C8 C15 124.6(5) . . ? N3 C9 C8 119.6(5) . . ? N3 C9 C10 111.6(5) . . ? C8 C9 C10 128.8(5) . . ? N4 C10 C11 120.5(5) . . ? N4 C10 C9 113.9(5) . . ? C11 C10 C9 125.6(5) . . ? C10 C11 C12 119.1(6) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 119.3(6) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 120.1(6) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? N4 C14 C13 121.2(6) . . ? N4 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C20 119.3(5) . . ? C16 C15 C8 120.1(5) . . ? C20 C15 C8 120.6(5) . . ? C17 C16 C15 119.4(6) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 121.0(6) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 119.6(5) . . ? C19 C18 C27 121.1(5) . . ? C17 C18 C27 119.3(6) . . ? C20 C19 C18 119.9(6) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C15 120.8(6) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? N5 C21 C22 121.4(7) . . ? N5 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C21 C22 C23 119.4(6) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 119.8(7) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 117.7(6) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.2 . . ? N5 C25 C24 122.3(6) . . ? N5 C25 C26 112.7(5) . . ? C24 C25 C26 124.9(6) . . ? N6 C26 C27 120.3(5) . . ? N6 C26 C25 111.8(5) . . ? C27 C26 C25 127.8(5) . . ? C28 C27 C26 116.4(5) . . ? C28 C27 C18 119.1(5) . . ? C26 C27 C18 124.5(5) . . ? C29 C28 C27 118.9(5) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? N7 C29 C28 121.3(5) . . ? N7 C29 C30 113.1(5) . . ? C28 C29 C30 125.4(5) . . ? N8 C30 C31 122.2(6) . . ? N8 C30 C29 113.1(5) . . ? C31 C30 C29 124.7(6) . . ? C30 C31 C32 118.3(6) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? C33 C32 C31 119.7(7) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.0(7) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? N8 C34 C33 120.9(6) . . ? N8 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? Cl3 C35 Cl1 109.0(4) . . ? Cl3 C35 Cl2 110.2(4) . . ? Cl1 C35 Cl2 109.5(4) . . ? Cl3 C35 H35 109.4 . . ? Cl1 C35 H35 109.4 . . ? Cl2 C35 H35 109.4 . . ? Cl5 C36 Cl6 111.9(5) . . ? Cl5 C36 Cl4 111.1(5) . . ? Cl6 C36 Cl4 110.4(5) . . ? Cl5 C36 H36 107.8 . . ? Cl6 C36 H36 107.8 . . ? Cl4 C36 H36 107.8 . . ? O23 C37 H37A 109.5 . . ? O23 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O23 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O1 C38 H38A 109.5 . . ? O1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O2 C39 H39A 109.5 . . ? O2 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O12 C40 H40A 109.5 . . ? O12 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O12 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O13 C41 H41A 109.5 . . ? O13 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O13 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.41 _refine_diff_density_min -0.74 _refine_diff_density_rms 0.12 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 619848' _exptl_special_details ; One nitrate anion is disordered over three positions, with atom O5 modeled over three positions. Atoms O5A, O5B and O5C were refined as isotropic with occupancies of 0.40, 0.40 and 0.20, respectively. A distance similarity restraint (SADI instruction) was retained for this nitrate. After refinement, the occupancy of the chloroform solvent molecule was fixed at 0.60. The main residual electron density features lie near the copper positions. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Cu4 N14 O22, 1.20(C H Cl3)' _chemical_formula_sum 'C41.2 H41.2 Cl3.6 Cu4 N14 O22' _chemical_formula_weight 1467.46 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' Cu Cu 0.3201 1.2651 '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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.430(2) _cell_length_b 10.588(3) _cell_length_c 16.580(4) _cell_angle_alpha 85.393(4) _cell_angle_beta 81.475(4) _cell_angle_gamma 84.808(4) _cell_volume 1454.2(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3077 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 27.16 _exptl_crystal_description 'Thin plate' _exptl_crystal_colour Green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.323 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6906 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16426 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_av_sigmaI/netI 0.107 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 29.66 _reflns_number_total 8643 _reflns_number_gt 4308 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2 version 1.0-27 (Bruker, 2005)' _computing_cell_refinement 'Bruker SAINT version 7.12a (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXS97 (Sheldrick, 1998)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^)+(0.1436P)^2^] 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 8643 _refine_ls_number_parameters 400 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.158 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.261 _refine_ls_wR_factor_gt 0.214 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.008 _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 Cu1 Cu -0.13827(8) 0.38367(7) 0.13486(4) 0.0386(2) Uani 1 1 d . . . Cu2 Cu 0.01386(9) 0.43485(8) 0.30103(4) 0.0429(2) Uani 1 1 d . . . Cl1 Cl 0.6231(6) 0.2879(4) 0.6202(3) 0.0932(13) Uani 0.60 1 d P . . Cl2 Cl 0.5962(6) 0.1640(5) 0.7795(3) 0.0991(14) Uani 0.60 1 d P . . Cl3 Cl 0.6220(7) 0.0194(5) 0.6392(4) 0.1217(19) Uani 0.60 1 d P . . O1 O -0.5824(6) 0.5156(6) 0.1175(4) 0.0717(16) Uani 1 1 d . . . O2 O -0.3716(5) 0.3937(4) 0.1301(3) 0.0485(11) Uani 1 1 d . . . O3 O -0.3534(7) 0.5758(5) 0.0600(3) 0.0657(14) Uani 1 1 d . . . O4 O -0.1960(6) 0.1911(5) 0.2069(3) 0.0536(11) Uani 1 1 d . A . O5A O -0.0700(13) 0.0551(10) 0.1182(6) 0.042(2) Uiso 0.40 1 d PD A 1 O5B O -0.0215(13) 0.0548(11) 0.1543(9) 0.052(3) Uiso 0.40 1 d PD A 2 O5C O -0.015(2) 0.048(2) 0.2003(17) 0.056(6) Uiso 0.20 1 d PD A 3 O6 O -0.2765(9) 0.0162(7) 0.1864(6) 0.113(3) Uani 1 1 d . A . O7 O -0.0544(12) 0.7310(6) 0.4245(4) 0.112(3) Uani 1 1 d . . . O8 O 0.0550(9) 0.6720(6) 0.3058(4) 0.0835(19) Uani 1 1 d . . . O9 O -0.0808(6) 0.5428(5) 0.3903(3) 0.0546(12) Uani 1 1 d . . . O10 O -0.1517(5) 0.4682(4) 0.2331(3) 0.0440(10) Uani 1 1 d . . . O11 O -0.1027(6) 0.2546(5) 0.3540(3) 0.0568(12) Uani 1 1 d . . . H11' H -0.1289 0.2317 0.3108 0.085 Uiso 1 1 calc R . . N1 N -0.0635(6) 0.3215(5) 0.0255(3) 0.0429(11) Uani 1 1 d . . . N2 N 0.0936(6) 0.3309(5) 0.1429(3) 0.0371(10) Uani 1 1 d . . . N3 N 0.1495(6) 0.3453(5) 0.2095(3) 0.0404(11) Uani 1 1 d . . . N4 N 0.2157(6) 0.3864(5) 0.3504(3) 0.0461(12) Uani 1 1 d . . . N5 N -0.4380(7) 0.4987(5) 0.1008(3) 0.0484(13) Uani 1 1 d . . . N6 N -0.1607(9) 0.0883(6) 0.1812(4) 0.0660(17) Uani 1 1 d D . . N7 N -0.0267(10) 0.6532(6) 0.3724(4) 0.0663(18) Uani 1 1 d . . . C1 C -0.1498(8) 0.3393(6) -0.0370(4) 0.0462(14) Uani 1 1 d . . . H1 H -0.2541 0.3825 -0.0283 0.055 Uiso 1 1 calc R . . C2 C -0.0935(8) 0.2978(6) -0.1125(4) 0.0489(15) Uani 1 1 d . . . H2 H -0.1576 0.3117 -0.1554 0.059 Uiso 1 1 calc R . . C3 C 0.0590(8) 0.2349(7) -0.1257(4) 0.0490(15) Uani 1 1 d . . . H3 H 0.1001 0.2042 -0.1776 0.059 Uiso 1 1 calc R . . C4 C 0.1505(7) 0.2175(6) -0.0622(4) 0.0442(14) Uani 1 1 d . . . H4 H 0.2557 0.1760 -0.0702 0.053 Uiso 1 1 calc R . . C5 C 0.0861(7) 0.2616(5) 0.0131(3) 0.0369(12) Uani 1 1 d . . . C6 C 0.1714(7) 0.2566(5) 0.0859(3) 0.0366(12) Uani 1 1 d . . . C7 C 0.3186(7) 0.1886(6) 0.0992(4) 0.0391(12) Uani 1 1 d . . . C8 C 0.3791(7) 0.2111(6) 0.1686(4) 0.0401(13) Uani 1 1 d . . . H8 H 0.4816 0.1728 0.1783 0.048 Uiso 1 1 calc R . . C9 C 0.2895(7) 0.2904(6) 0.2249(4) 0.0403(13) Uani 1 1 d . . . C10 C 0.3344(7) 0.3188(6) 0.3034(4) 0.0436(14) Uani 1 1 d . . . C11 C 0.4775(8) 0.2816(8) 0.3290(4) 0.0560(18) Uani 1 1 d . . . H11 H 0.5592 0.2351 0.2950 0.067 Uiso 1 1 calc R . . C12 C 0.5033(9) 0.3124(8) 0.4058(4) 0.0604(19) Uani 1 1 d . . . H12 H 0.6039 0.2894 0.4245 0.073 Uiso 1 1 calc R . . C13 C 0.3811(9) 0.3765(8) 0.4538(4) 0.0601(19) Uani 1 1 d . . . H13 H 0.3942 0.3947 0.5075 0.072 Uiso 1 1 calc R . . C14 C 0.2400(8) 0.4142(7) 0.4241(4) 0.0505(16) Uani 1 1 d . . . H14 H 0.1572 0.4614 0.4571 0.061 Uiso 1 1 calc R . . C15 C 0.4087(6) 0.0928(5) 0.0453(3) 0.0356(12) Uani 1 1 d . . . C16 C 0.3383(7) -0.0124(6) 0.0283(4) 0.0427(13) Uani 1 1 d . . . H16 H 0.2277 -0.0216 0.0473 0.051 Uiso 1 1 calc R . . C17 C 0.5705(7) 0.1048(6) 0.0169(4) 0.0419(13) Uani 1 1 d . . . H17 H 0.6193 0.1775 0.0285 0.050 Uiso 1 1 calc R . . C18 C -0.2915(9) 0.5492(7) 0.2599(5) 0.0565(18) Uani 1 1 d . . . H18A H -0.3646 0.5567 0.2187 0.085 Uiso 1 1 calc R . . H18B H -0.2595 0.6335 0.2678 0.085 Uiso 1 1 calc R . . H18C H -0.3464 0.5129 0.3117 0.085 Uiso 1 1 calc R . . C19 C -0.0419(15) 0.1497(10) 0.3982(8) 0.097(3) Uani 1 1 d . . . H19A H -0.0192 0.1774 0.4507 0.117 Uiso 1 1 calc R . . H19B H 0.0618 0.1176 0.3676 0.117 Uiso 1 1 calc R . . C20 C -0.1447(18) 0.0458(11) 0.4157(9) 0.129(5) Uani 1 1 d . . . H20A H -0.0912 -0.0237 0.4470 0.194 Uiso 1 1 calc R . . H20B H -0.1658 0.0154 0.3643 0.194 Uiso 1 1 calc R . . H20C H -0.2466 0.0752 0.4478 0.194 Uiso 1 1 calc R . . C21 C 0.674(2) 0.1484(12) 0.6773(9) 0.073(4) Uani 0.60 1 d P . . H21 H 0.7937 0.1401 0.6738 0.087 Uiso 0.60 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0281(3) 0.0409(4) 0.0438(4) -0.0094(3) 0.0025(3) 0.0071(3) Cu2 0.0331(4) 0.0502(5) 0.0426(4) -0.0160(3) 0.0052(3) 0.0067(3) Cl1 0.088(3) 0.096(3) 0.093(3) 0.007(2) -0.023(2) 0.010(2) Cl2 0.086(3) 0.137(4) 0.075(3) 0.003(2) -0.015(2) -0.019(3) Cl3 0.098(4) 0.094(3) 0.177(5) -0.045(3) -0.008(4) -0.014(3) O1 0.033(3) 0.081(4) 0.095(4) 0.001(3) -0.006(2) 0.019(3) O2 0.028(2) 0.048(3) 0.064(3) -0.001(2) 0.0022(18) 0.0081(18) O3 0.070(4) 0.049(3) 0.071(3) -0.005(2) 0.014(3) -0.006(3) O4 0.047(3) 0.047(3) 0.061(3) -0.010(2) 0.008(2) 0.005(2) O6 0.068(5) 0.085(5) 0.188(8) -0.044(5) -0.012(5) 0.000(4) O7 0.175(9) 0.069(4) 0.088(5) -0.042(4) 0.028(5) -0.021(5) O8 0.114(6) 0.074(4) 0.058(3) -0.010(3) 0.014(3) -0.022(4) O9 0.057(3) 0.056(3) 0.047(2) -0.016(2) 0.005(2) 0.010(2) O10 0.034(2) 0.048(2) 0.047(2) -0.0152(18) 0.0033(17) 0.0134(18) O11 0.054(3) 0.058(3) 0.056(3) -0.003(2) -0.003(2) -0.001(2) N1 0.034(3) 0.039(3) 0.054(3) -0.008(2) -0.001(2) 0.004(2) N2 0.028(2) 0.042(3) 0.039(2) -0.012(2) 0.0072(18) 0.0008(19) N3 0.030(2) 0.045(3) 0.044(3) -0.011(2) 0.0036(19) 0.004(2) N4 0.039(3) 0.055(3) 0.042(3) -0.019(2) 0.009(2) 0.003(2) N5 0.040(3) 0.052(3) 0.051(3) -0.008(2) -0.006(2) 0.010(3) N6 0.075(5) 0.053(4) 0.067(4) -0.010(3) 0.004(3) -0.004(4) N7 0.088(5) 0.056(4) 0.051(4) -0.010(3) 0.003(3) 0.000(4) C1 0.040(3) 0.044(3) 0.052(4) -0.003(3) -0.002(3) 0.006(3) C2 0.049(4) 0.049(4) 0.047(3) -0.005(3) -0.005(3) 0.003(3) C3 0.050(4) 0.054(4) 0.039(3) -0.005(3) 0.002(3) 0.003(3) C4 0.035(3) 0.049(4) 0.045(3) -0.015(3) 0.004(2) 0.006(3) C5 0.033(3) 0.034(3) 0.041(3) -0.005(2) 0.004(2) 0.000(2) C6 0.028(3) 0.037(3) 0.042(3) -0.011(2) 0.006(2) 0.002(2) C7 0.028(3) 0.039(3) 0.047(3) -0.012(2) 0.007(2) 0.002(2) C8 0.027(3) 0.045(3) 0.045(3) -0.012(3) 0.004(2) 0.002(2) C9 0.030(3) 0.043(3) 0.045(3) -0.013(2) 0.006(2) 0.001(2) C10 0.033(3) 0.053(4) 0.043(3) -0.014(3) 0.007(2) -0.002(3) C11 0.036(3) 0.079(5) 0.052(4) -0.022(3) 0.002(3) 0.006(3) C12 0.040(4) 0.089(6) 0.054(4) -0.019(4) -0.011(3) 0.005(4) C13 0.051(4) 0.086(6) 0.046(4) -0.024(4) -0.004(3) -0.005(4) C14 0.041(3) 0.065(4) 0.042(3) -0.015(3) 0.002(3) 0.007(3) C15 0.025(2) 0.041(3) 0.038(3) -0.011(2) 0.0054(19) 0.004(2) C16 0.027(3) 0.043(3) 0.054(3) -0.014(3) 0.010(2) -0.001(2) C17 0.029(3) 0.043(3) 0.050(3) -0.015(3) 0.009(2) -0.003(2) C18 0.045(4) 0.059(4) 0.063(4) -0.023(3) -0.003(3) 0.017(3) C19 0.095(8) 0.082(7) 0.119(9) 0.008(6) -0.042(7) 0.002(6) C20 0.143(13) 0.072(7) 0.169(13) 0.041(8) -0.036(11) -0.014(8) C21 0.080(10) 0.050(7) 0.091(10) -0.014(7) -0.020(8) 0.003(7) 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 Cu1 N1 1.975(5) . ? Cu1 N2 2.004(5) . ? Cu1 O2 1.973(4) . ? Cu1 O4 2.332(5) . ? Cu1 O10 1.904(4) . ? Cu2 N3 2.008(5) . ? Cu2 N4 2.005(6) . ? Cu2 O9 1.972(4) . ? Cu2 O10 1.912(4) . ? Cu2 O11 2.279(5) . ? Cl1 C21 1.743(14) . ? Cl2 C21 1.739(16) . ? Cl3 C21 1.669(15) . ? O1 N5 1.208(7) . ? O2 N5 1.291(7) . ? O3 N5 1.227(8) . ? O4 N6 1.198(8) . ? O5A N6 1.254(11) . ? O5B N6 1.223(12) . ? O5C N6 1.336(16) . ? O6 N6 1.281(10) . ? O7 N7 1.224(9) . ? O8 N7 1.224(8) . ? O9 N7 1.290(8) . ? O10 C18 1.431(7) . ? O11 C19 1.382(10) . ? O11 H11' 0.8400 . ? N1 C1 1.344(8) . ? N1 C5 1.355(7) . ? N2 N3 1.288(7) . ? N2 C6 1.336(7) . ? N3 C9 1.318(7) . ? N4 C14 1.328(8) . ? N4 C10 1.360(7) . ? C1 C2 1.363(9) . ? C1 H1 0.9500 . ? C2 C3 1.390(9) . ? C2 H2 0.9500 . ? C3 C4 1.386(9) . ? C3 H3 0.9500 . ? C4 C5 1.384(8) . ? C4 H4 0.9500 . ? C5 C6 1.489(8) . ? C6 C7 1.414(8) . ? C7 C8 1.371(8) . ? C7 C15 1.487(7) . ? C8 C9 1.397(8) . ? C8 H8 0.9500 . ? C9 C10 1.469(9) . ? C10 C11 1.352(9) . ? C11 C12 1.392(10) . ? C11 H11 0.9500 . ? C12 C13 1.369(10) . ? C12 H12 0.9500 . ? C13 C14 1.369(10) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.375(8) . ? C15 C17 1.389(8) . ? C16 C17 1.386(8) 2_655 ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.447(15) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21 1.0000 . ? 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 O10 Cu1 O2 96.66(18) . . ? O10 Cu1 N1 162.7(2) . . ? O2 Cu1 N1 97.9(2) . . ? O10 Cu1 N2 89.01(18) . . ? O2 Cu1 N2 166.98(19) . . ? N1 Cu1 N2 78.8(2) . . ? O10 Cu1 O4 92.07(19) . . ? O2 Cu1 O4 81.43(18) . . ? N1 Cu1 O4 99.28(19) . . ? N2 Cu1 O4 86.67(19) . . ? O10 Cu2 O9 98.46(19) . . ? O10 Cu2 N4 167.68(18) . . ? O9 Cu2 N4 93.3(2) . . ? O10 Cu2 N3 88.49(18) . . ? O9 Cu2 N3 168.3(2) . . ? N4 Cu2 N3 79.3(2) . . ? O10 Cu2 O11 88.71(19) . . ? O9 Cu2 O11 96.7(2) . . ? N4 Cu2 O11 93.6(2) . . ? N3 Cu2 O11 92.8(2) . . ? N5 O2 Cu1 117.9(4) . . ? N6 O4 Cu1 125.1(5) . . ? N7 O9 Cu2 107.0(4) . . ? C18 O10 Cu1 120.3(4) . . ? C18 O10 Cu2 119.3(4) . . ? Cu1 O10 Cu2 120.2(2) . . ? C19 O11 Cu2 130.3(6) . . ? C19 O11 H11' 109.5 . . ? Cu2 O11 H11' 98.4 . . ? C1 N1 C5 119.1(5) . . ? C1 N1 Cu1 123.8(4) . . ? C5 N1 Cu1 117.1(4) . . ? N3 N2 C6 122.2(5) . . ? N3 N2 Cu1 119.4(3) . . ? C6 N2 Cu1 116.6(4) . . ? N2 N3 C9 122.2(5) . . ? N2 N3 Cu2 120.9(4) . . ? C9 N3 Cu2 116.5(4) . . ? C14 N4 C10 119.0(6) . . ? C14 N4 Cu2 125.2(4) . . ? C10 N4 Cu2 115.7(4) . . ? O1 N5 O3 124.0(6) . . ? O1 N5 O2 116.5(6) . . ? O3 N5 O2 119.5(6) . . ? O4 N6 O5B 121.1(9) . . ? O4 N6 O5A 130.7(8) . . ? O4 N6 O6 115.6(7) . . ? O5B N6 O6 123.3(9) . . ? O5A N6 O6 103.3(8) . . ? O4 N6 O5C 107.7(13) . . ? O6 N6 O5C 123.3(12) . . ? O8 N7 O7 124.0(8) . . ? O8 N7 O9 118.0(6) . . ? O7 N7 O9 118.0(7) . . ? N1 C1 C2 122.5(6) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 119.0(6) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 119.2(6) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C5 C4 C3 119.0(6) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 121.2(6) . . ? N1 C5 C6 113.0(5) . . ? C4 C5 C6 125.6(5) . . ? N2 C6 C7 119.5(5) . . ? N2 C6 C5 111.7(5) . . ? C7 C6 C5 128.8(5) . . ? C8 C7 C6 116.8(5) . . ? C8 C7 C15 118.1(5) . . ? C6 C7 C15 125.0(5) . . ? C7 C8 C9 119.7(5) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? N3 C9 C8 119.4(6) . . ? N3 C9 C10 114.6(5) . . ? C8 C9 C10 126.0(5) . . ? C11 C10 N4 121.7(6) . . ? C11 C10 C9 124.9(6) . . ? N4 C10 C9 113.4(5) . . ? C10 C11 C12 119.1(6) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C13 C12 C11 118.7(6) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 119.7(6) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? N4 C14 C13 121.7(6) . . ? N4 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C16 C15 C17 119.5(5) . . ? C16 C15 C7 121.2(5) . . ? C17 C15 C7 119.2(5) . . ? C15 C16 C17 119.6(5) . 2_655 ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 2_655 . ? C16 C17 C15 120.9(6) 2_655 . ? C16 C17 H17 119.5 2_655 . ? C15 C17 H17 119.5 . . ? O10 C18 H18A 109.5 . . ? O10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O11 C19 C20 115.6(9) . . ? O11 C19 H19A 108.4 . . ? C20 C19 H19A 108.4 . . ? O11 C19 H19B 108.4 . . ? C20 C19 H19B 108.4 . . ? H19A C19 H19B 107.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Cl3 C21 Cl2 113.9(10) . . ? Cl3 C21 Cl1 112.4(9) . . ? Cl2 C21 Cl1 109.3(8) . . ? Cl3 C21 H21 106.9 . . ? Cl2 C21 H21 106.9 . . ? Cl1 C21 H21 106.9 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.74 _refine_diff_density_min -1.31 _refine_diff_density_rms 0.17 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 619849' _exptl_special_details ; one ethanol molecule is disordered over two positions: o1 c38 c37 and o1 c38' c37' with occupancies 0.724(9) and 0.276(9). ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H42 Cd2 N12 O15' _chemical_formula_sum 'C38 H42 Cd2 N12 O15' _chemical_formula_weight 1131.64 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' Cd Cd -0.8075 1.2024 '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 9.4936(19) _cell_length_b 10.691(2) _cell_length_c 22.746(5) _cell_angle_alpha 85.21(3) _cell_angle_beta 85.11(3) _cell_angle_gamma 74.06(3) _cell_volume 2207.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5382 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 28.8 _exptl_crystal_description Lath _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.182 _exptl_crystal_size_mid 0.037 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8088 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6749 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker ApexII CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17495 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.85 _reflns_number_total 12307 _reflns_number_gt 10190 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 version 1.0-27 (Bruker, 2005)' _computing_cell_refinement 'Bruker SAINT version 7.12a (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SAINT' _computing_structure_refinement 'SHELXS97 (Sheldrick, 1998)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0429P)^2^+0.9071P] 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 5382 _refine_ls_number_reflns 12307 _refine_ls_number_parameters 623 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Cd1 Cd 0.329156(18) -0.180135(17) 0.344782(7) 0.02549(5) Uani 1 1 d . A . Cd2 Cd 0.265528(17) 0.350375(16) 0.144692(7) 0.02214(5) Uani 1 1 d . . . O1 O 0.3581(3) 0.0250(2) 0.31604(9) 0.0464(5) Uani 1 1 d D . . H1A H 0.3498 0.0597 0.2815 0.070 Uiso 0.276(9) 1 calc PR A 1 H1'A H 0.3104 0.0340 0.2858 0.070 Uiso 0.724(9) 1 d PR A 2 O2 O 0.50249(19) -0.22905(18) 0.26630(8) 0.0314(4) Uani 1 1 d . . . H2A H 0.4992 -0.1746 0.2372 0.047 Uiso 1 1 calc R A . O3 O 0.2963(2) -0.38920(19) 0.35075(9) 0.0422(5) Uani 1 1 d . . . H3A H 0.2334 -0.3965 0.3284 0.063 Uiso 1 1 calc R A . O4 O 0.5594(2) -0.2770(3) 0.39139(9) 0.0526(6) Uani 1 1 d . . . O5 O 0.3648(3) -0.2067(3) 0.44573(10) 0.0636(8) Uani 1 1 d . . . O6 O 0.5654(3) -0.3124(3) 0.48633(10) 0.0633(7) Uani 1 1 d . . . O7 O 0.4315(2) 0.14066(19) 0.11337(8) 0.0347(4) Uani 1 1 d . . . O8 O 0.3305(2) 0.13841(18) 0.20164(8) 0.0322(4) Uani 1 1 d . . . O9 O 0.4874(2) -0.03689(17) 0.17006(8) 0.0322(4) Uani 1 1 d . . . O10 O 0.6203(2) 0.4729(2) 0.08474(10) 0.0468(5) Uani 1 1 d . . . O11 O 0.5125(2) 0.3735(2) 0.15387(10) 0.0456(5) Uani 1 1 d . . . O12 O 0.3984(2) 0.4594(2) 0.07655(9) 0.0392(4) Uani 1 1 d . . . O13 O 0.1139(3) 0.5739(2) 0.17663(9) 0.0511(6) Uani 1 1 d . . . O14 O 0.2488(2) 0.4366(2) 0.23835(11) 0.0500(6) Uani 1 1 d . . . O15 O 0.0883(3) 0.6063(2) 0.27062(9) 0.0426(5) Uani 1 1 d . . . N1 N 0.1564(3) -0.0088(2) 0.08055(9) 0.0303(4) Uani 1 1 d . . . N2 N 0.2105(2) -0.14691(19) 0.21863(8) 0.0224(4) Uani 1 1 d . A . N3 N 0.1579(2) -0.14679(19) 0.27449(8) 0.0227(4) Uani 1 1 d . . . N4 N 0.0769(2) -0.1057(2) 0.38939(9) 0.0284(4) Uani 1 1 d . . . N5 N -0.2140(3) 0.2063(2) 0.34498(9) 0.0357(5) Uani 1 1 d . . . N6 N -0.0123(2) 0.32736(19) 0.22877(8) 0.0235(4) Uani 1 1 d . . . N7 N 0.0297(2) 0.32685(19) 0.17169(8) 0.0221(4) Uani 1 1 d . . . N8 N 0.1489(2) 0.32423(19) 0.06130(8) 0.0232(4) Uani 1 1 d . . . N9 N 0.4997(3) -0.2663(3) 0.44166(11) 0.0421(6) Uani 1 1 d . A . N10 N 0.5134(2) 0.4355(2) 0.10468(10) 0.0306(4) Uani 1 1 d . . . N11 N 0.1492(3) 0.5400(2) 0.22893(10) 0.0368(5) Uani 1 1 d . . . N12 N 0.4178(2) 0.07772(19) 0.16133(9) 0.0237(4) Uani 1 1 d . . . C1 C 0.2379(3) -0.0074(3) 0.02962(11) 0.0354(6) Uani 1 1 d . . . H1 H 0.2146 0.0692 0.0040 0.042 Uiso 1 1 calc R . . C2 C 0.3532(3) -0.1092(3) 0.01187(11) 0.0322(5) Uani 1 1 d . . . H2 H 0.4097 -0.1018 -0.0242 0.039 Uiso 1 1 calc R . . C3 C 0.3845(3) -0.2225(3) 0.04793(12) 0.0360(6) Uani 1 1 d . . . H3 H 0.4600 -0.2965 0.0362 0.043 Uiso 1 1 calc R . . C4 C 0.3040(3) -0.2263(3) 0.10155(11) 0.0314(5) Uani 1 1 d . . . H4 H 0.3243 -0.3024 0.1276 0.038 Uiso 1 1 calc R . . C5 C 0.1933(2) -0.1170(2) 0.11623(9) 0.0214(4) Uani 1 1 d . A . C6 C 0.1160(2) -0.1117(2) 0.17613(9) 0.0207(4) Uani 1 1 d . . . C7 C -0.0374(2) -0.0688(2) 0.18791(9) 0.0201(4) Uani 1 1 d . A . C8 C -0.0901(2) -0.0614(2) 0.24694(9) 0.0208(4) Uani 1 1 d . . . C9 C 0.0144(2) -0.1089(2) 0.28965(9) 0.0217(4) Uani 1 1 d . A . C10 C -0.0210(3) -0.1255(2) 0.35455(10) 0.0242(4) Uani 1 1 d . A . C11 C -0.1420(3) -0.1685(3) 0.37695(11) 0.0304(5) Uani 1 1 d . . . H11 H -0.2066 -0.1867 0.3512 0.036 Uiso 1 1 calc R A . C12 C -0.1655(3) -0.1841(3) 0.43773(12) 0.0401(7) Uani 1 1 d . A . H12 H -0.2466 -0.2138 0.4543 0.048 Uiso 1 1 calc R . . C13 C -0.0709(3) -0.1563(3) 0.47384(12) 0.0431(7) Uani 1 1 d . . . H13 H -0.0880 -0.1624 0.5156 0.052 Uiso 1 1 calc R A . C14 C 0.0503(3) -0.1190(3) 0.44805(11) 0.0366(6) Uani 1 1 d . A . H14 H 0.1173 -0.1023 0.4731 0.044 Uiso 1 1 calc R . . C15 C 0.1960(3) 0.3535(2) 0.00589(10) 0.0289(5) Uani 1 1 d . . . H15 H 0.2893 0.3708 -0.0003 0.035 Uiso 1 1 calc R . . C16 C 0.1151(3) 0.3597(3) -0.04258(10) 0.0304(5) Uani 1 1 d . . . H16 H 0.1535 0.3771 -0.0814 0.036 Uiso 1 1 calc R . . C17 C -0.0231(3) 0.3399(2) -0.03300(10) 0.0290(5) Uani 1 1 d . . . H17 H -0.0827 0.3460 -0.0652 0.035 Uiso 1 1 calc R . . C18 C -0.0738(3) 0.3112(2) 0.02412(10) 0.0245(4) Uani 1 1 d . . . H18 H -0.1694 0.2993 0.0316 0.029 Uiso 1 1 calc R . . C19 C 0.0166(2) 0.2999(2) 0.07038(9) 0.0209(4) Uani 1 1 d . . . C20 C -0.0320(2) 0.2732(2) 0.13333(9) 0.0196(4) Uani 1 1 d . . . C21 C -0.1323(2) 0.2009(2) 0.15289(9) 0.0195(4) Uani 1 1 d . . . C22 C -0.1851(2) 0.2081(2) 0.21233(9) 0.0199(4) Uani 1 1 d . A . C23 C -0.1225(2) 0.2762(2) 0.24870(9) 0.0212(4) Uani 1 1 d . . . C24 C -0.1660(2) 0.2983(2) 0.31218(10) 0.0245(4) Uani 1 1 d . . . C25 C -0.1536(3) 0.4113(3) 0.33500(10) 0.0305(5) Uani 1 1 d . . . H25 H -0.1171 0.4735 0.3106 0.037 Uiso 1 1 calc R . . C26 C -0.1957(3) 0.4313(3) 0.39397(11) 0.0358(6) Uani 1 1 d . . . H26 H -0.1889 0.5078 0.4107 0.043 Uiso 1 1 calc R . . C27 C -0.2474(3) 0.3386(3) 0.42800(11) 0.0413(7) Uani 1 1 d . . . H27 H -0.2788 0.3508 0.4684 0.050 Uiso 1 1 calc R . . C28 C -0.2529(4) 0.2283(3) 0.40246(11) 0.0442(7) Uani 1 1 d . . . H28 H -0.2860 0.1638 0.4266 0.053 Uiso 1 1 calc R . . C29 C -0.1416(2) -0.0321(2) 0.13911(10) 0.0230(4) Uani 1 1 d . . . H29A H -0.2357 -0.0497 0.1542 0.028 Uiso 1 1 calc R A . H29B H -0.1007 -0.0896 0.1063 0.028 Uiso 1 1 calc R . . C30 C -0.1741(3) 0.1123(2) 0.11366(9) 0.0230(4) Uani 1 1 d . A . H30A H -0.1199 0.1151 0.0746 0.028 Uiso 1 1 calc R . . H30B H -0.2802 0.1453 0.1075 0.028 Uiso 1 1 calc R . . C31 C -0.2492(2) 0.0035(2) 0.26358(10) 0.0231(4) Uani 1 1 d . A . H31A H -0.2626 0.0083 0.3071 0.028 Uiso 1 1 calc R . . H31B H -0.3103 -0.0508 0.2520 0.028 Uiso 1 1 calc R . . C32 C -0.3040(2) 0.1431(2) 0.23400(10) 0.0222(4) Uani 1 1 d . . . H32A H -0.3608 0.1388 0.2001 0.027 Uiso 1 1 calc R A . H32B H -0.3718 0.1987 0.2628 0.027 Uiso 1 1 calc R . . C33 C 0.6854(4) -0.3654(4) 0.20160(15) 0.0574(10) Uani 1 1 d . . . H33A H 0.7223 -0.4547 0.1890 0.086 Uiso 1 1 calc R A . H33B H 0.7639 -0.3408 0.2192 0.086 Uiso 1 1 calc R . . H33C H 0.6530 -0.3057 0.1673 0.086 Uiso 1 1 calc R . . C34 C 0.5583(3) -0.3580(3) 0.24659(13) 0.0393(6) Uani 1 1 d . A . H34A H 0.4794 -0.3836 0.2289 0.047 Uiso 1 1 calc R . . H34B H 0.5906 -0.4199 0.2808 0.047 Uiso 1 1 calc R . . C35 C 0.3223(4) -0.4961(3) 0.39441(15) 0.0468(8) Uani 1 1 d . A . H35A H 0.3869 -0.4819 0.4237 0.056 Uiso 1 1 calc R . . H35B H 0.3729 -0.5776 0.3752 0.056 Uiso 1 1 calc R . . C36 C 0.1816(4) -0.5092(4) 0.42523(18) 0.0672(11) Uani 1 1 d . . . H36A H 0.2020 -0.5822 0.4552 0.101 Uiso 1 1 calc R A . H36B H 0.1186 -0.5255 0.3964 0.101 Uiso 1 1 calc R . . H36C H 0.1316 -0.4286 0.4444 0.101 Uiso 1 1 calc R . . C37 C 0.1973(13) 0.2048(12) 0.3563(6) 0.052(4) Uani 0.276(9) 1 d PD A 1 H37A H 0.1837 0.2771 0.3819 0.078 Uiso 0.276(9) 1 calc PR A 1 H37B H 0.1317 0.1510 0.3711 0.078 Uiso 0.276(9) 1 calc PR A 1 H37C H 0.1746 0.2395 0.3159 0.078 Uiso 0.276(9) 1 calc PR A 1 C38 C 0.3554(17) 0.122(2) 0.3563(11) 0.049(5) Uani 0.276(9) 1 d PD A 1 H38A H 0.4245 0.1743 0.3421 0.074 Uiso 0.276(9) 1 calc PR A 1 H38B H 0.3800 0.0822 0.3963 0.074 Uiso 0.276(9) 1 calc PR A 1 C37' C 0.3960(7) 0.1119(6) 0.4020(2) 0.073(2) Uani 0.724(9) 1 d PD A 2 H37D H 0.3646 0.1852 0.4276 0.110 Uiso 0.724(9) 1 calc PR A 2 H37E H 0.4992 0.1005 0.3882 0.110 Uiso 0.724(9) 1 calc PR A 2 H37F H 0.3850 0.0322 0.4242 0.110 Uiso 0.724(9) 1 calc PR A 2 C38' C 0.3031(10) 0.1394(7) 0.3498(3) 0.056(2) Uani 0.724(9) 1 d PD A 2 H38C H 0.1982 0.1515 0.3626 0.084 Uiso 0.724(9) 1 calc PR A 2 H38D H 0.3142 0.2185 0.3261 0.084 Uiso 0.724(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02220(9) 0.03341(10) 0.02142(8) 0.00226(6) -0.00355(6) -0.00896(7) Cd2 0.01996(8) 0.02564(9) 0.02085(8) 0.00066(6) -0.00073(6) -0.00699(6) O1 0.0786(16) 0.0356(11) 0.0296(10) -0.0067(8) 0.0066(10) -0.0247(11) O2 0.0282(9) 0.0351(9) 0.0271(8) 0.0006(7) 0.0012(7) -0.0036(8) O3 0.0535(13) 0.0365(10) 0.0432(11) 0.0100(9) -0.0203(9) -0.0219(10) O4 0.0418(13) 0.0789(17) 0.0345(11) -0.0002(11) -0.0092(9) -0.0109(12) O5 0.0346(12) 0.120(2) 0.0308(10) 0.0042(13) -0.0043(9) -0.0129(14) O6 0.0471(13) 0.111(2) 0.0371(11) 0.0274(13) -0.0211(10) -0.0341(14) O7 0.0348(10) 0.0381(10) 0.0266(8) 0.0041(7) 0.0014(7) -0.0049(8) O8 0.0321(10) 0.0332(9) 0.0265(8) -0.0035(7) 0.0057(7) -0.0026(8) O9 0.0265(9) 0.0253(8) 0.0426(10) 0.0010(7) -0.0010(7) -0.0044(7) O10 0.0290(10) 0.0552(13) 0.0572(13) 0.0030(11) 0.0107(9) -0.0190(10) O11 0.0354(11) 0.0530(13) 0.0491(12) 0.0186(10) -0.0084(9) -0.0178(10) O12 0.0335(10) 0.0479(12) 0.0393(10) 0.0063(9) -0.0052(8) -0.0181(9) O13 0.0928(18) 0.0440(12) 0.0285(10) -0.0033(9) 0.0001(11) -0.0394(13) O14 0.0329(11) 0.0648(15) 0.0568(13) -0.0289(12) -0.0059(10) -0.0124(11) O15 0.0591(14) 0.0401(11) 0.0335(10) -0.0176(9) 0.0067(9) -0.0201(10) N1 0.0381(12) 0.0295(10) 0.0198(9) -0.0028(8) 0.0033(8) -0.0044(9) N2 0.0210(9) 0.0265(9) 0.0194(8) 0.0000(7) -0.0005(7) -0.0064(8) N3 0.0219(9) 0.0265(9) 0.0193(8) 0.0007(7) -0.0011(7) -0.0063(8) N4 0.0253(10) 0.0396(12) 0.0203(9) -0.0051(8) -0.0001(7) -0.0081(9) N5 0.0482(14) 0.0454(13) 0.0207(9) -0.0014(9) 0.0013(9) -0.0258(11) N6 0.0255(10) 0.0298(10) 0.0177(8) -0.0044(7) 0.0026(7) -0.0121(8) N7 0.0221(9) 0.0274(9) 0.0182(8) -0.0028(7) 0.0009(7) -0.0092(8) N8 0.0202(9) 0.0283(10) 0.0196(8) -0.0016(7) 0.0020(7) -0.0046(8) N9 0.0327(13) 0.0633(17) 0.0356(12) 0.0128(11) -0.0108(10) -0.0239(12) N10 0.0239(10) 0.0280(10) 0.0386(11) -0.0024(9) 0.0057(8) -0.0072(8) N11 0.0480(14) 0.0429(13) 0.0311(11) -0.0128(10) 0.0072(10) -0.0313(12) N12 0.0189(9) 0.0264(10) 0.0274(9) -0.0017(8) -0.0029(7) -0.0086(8) C1 0.0473(16) 0.0372(14) 0.0196(10) -0.0026(10) 0.0050(10) -0.0099(12) C2 0.0298(13) 0.0489(16) 0.0202(10) -0.0093(10) 0.0034(9) -0.0140(12) C3 0.0260(13) 0.0443(15) 0.0328(13) -0.0089(11) 0.0066(10) -0.0021(11) C4 0.0249(12) 0.0336(13) 0.0302(12) 0.0006(10) 0.0030(9) -0.0008(10) C5 0.0197(10) 0.0278(11) 0.0190(9) -0.0050(8) -0.0018(7) -0.0092(9) C6 0.0226(11) 0.0219(10) 0.0190(9) -0.0030(8) -0.0003(8) -0.0083(8) C7 0.0210(10) 0.0199(10) 0.0211(9) -0.0014(8) -0.0029(8) -0.0077(8) C8 0.0202(10) 0.0227(10) 0.0218(9) -0.0007(8) -0.0015(8) -0.0097(8) C9 0.0242(11) 0.0222(10) 0.0204(9) -0.0003(8) -0.0005(8) -0.0099(9) C10 0.0219(11) 0.0276(11) 0.0216(10) 0.0009(8) 0.0002(8) -0.0052(9) C11 0.0263(12) 0.0394(14) 0.0263(11) 0.0060(10) -0.0008(9) -0.0129(11) C12 0.0321(14) 0.0573(18) 0.0300(13) 0.0092(12) 0.0031(10) -0.0154(13) C13 0.0381(16) 0.066(2) 0.0220(11) 0.0015(12) 0.0039(10) -0.0117(14) C14 0.0318(14) 0.0558(17) 0.0210(11) -0.0062(11) -0.0013(9) -0.0090(13) C15 0.0273(12) 0.0337(13) 0.0230(10) -0.0014(9) 0.0051(9) -0.0061(10) C16 0.0384(14) 0.0336(13) 0.0161(9) -0.0002(9) 0.0031(9) -0.0065(11) C17 0.0360(13) 0.0290(12) 0.0200(10) -0.0011(9) -0.0048(9) -0.0045(10) C18 0.0260(11) 0.0269(11) 0.0193(9) -0.0008(8) -0.0032(8) -0.0044(9) C19 0.0217(11) 0.0211(10) 0.0179(9) -0.0021(8) 0.0004(7) -0.0026(8) C20 0.0179(10) 0.0218(10) 0.0173(9) -0.0005(8) -0.0020(7) -0.0026(8) C21 0.0155(10) 0.0222(10) 0.0198(9) -0.0005(8) -0.0035(7) -0.0031(8) C22 0.0148(9) 0.0233(10) 0.0206(9) 0.0013(8) -0.0032(7) -0.0038(8) C23 0.0207(10) 0.0239(10) 0.0181(9) -0.0022(8) -0.0013(7) -0.0045(8) C24 0.0199(11) 0.0342(12) 0.0194(9) -0.0022(9) 0.0002(8) -0.0075(9) C25 0.0354(14) 0.0349(13) 0.0230(11) -0.0049(9) 0.0009(9) -0.0124(11) C26 0.0393(15) 0.0446(15) 0.0247(11) -0.0136(11) 0.0004(10) -0.0107(12) C27 0.0416(16) 0.067(2) 0.0177(10) -0.0082(12) 0.0063(10) -0.0196(15) C28 0.0567(19) 0.066(2) 0.0197(11) -0.0012(12) 0.0032(11) -0.0354(17) C29 0.0214(11) 0.0282(11) 0.0218(10) -0.0035(8) -0.0046(8) -0.0091(9) C30 0.0230(11) 0.0285(11) 0.0194(9) -0.0032(8) -0.0055(8) -0.0087(9) C31 0.0182(10) 0.0279(11) 0.0245(10) -0.0010(9) 0.0005(8) -0.0091(9) C32 0.0170(10) 0.0266(11) 0.0236(10) -0.0001(8) -0.0021(8) -0.0072(8) C33 0.058(2) 0.0500(19) 0.0447(17) -0.0027(15) 0.0141(16) 0.0124(16) C34 0.0409(16) 0.0356(14) 0.0357(14) -0.0019(11) -0.0014(12) -0.0010(12) C35 0.0462(18) 0.0352(15) 0.0600(19) 0.0156(14) -0.0185(15) -0.0136(13) C36 0.055(2) 0.075(3) 0.070(2) 0.027(2) -0.0086(19) -0.021(2) C37 0.059(9) 0.045(7) 0.050(7) -0.012(5) 0.004(6) -0.012(6) C38 0.039(9) 0.041(9) 0.067(11) -0.021(8) -0.007(7) -0.003(7) C37' 0.091(5) 0.088(4) 0.053(3) -0.037(3) -0.007(3) -0.033(4) C38' 0.086(7) 0.035(3) 0.041(3) -0.009(2) 0.009(4) -0.007(4) 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 Cd1 O2 2.3131(19) . ? Cd1 N3 2.315(2) . ? Cd1 O1 2.319(2) . ? Cd1 O3 2.3316(19) . ? Cd1 O5 2.332(2) . ? Cd1 O4 2.437(2) . ? Cd1 N4 2.464(2) . ? Cd2 N7 2.3453(19) . ? Cd2 N8 2.349(2) . ? Cd2 O12 2.350(2) . ? Cd2 O14 2.367(2) . ? Cd2 O11 2.452(2) . ? Cd2 O8 2.464(2) . ? Cd2 O7 2.481(2) . ? Cd2 O13 2.556(3) . ? O1 C38 1.435(9) . ? O1 C38' 1.447(6) . ? O1 H1A 0.8400 . ? O1 H1'A 0.8399 . ? O2 C34 1.430(3) . ? O2 H2A 0.8400 . ? O3 C35 1.432(3) . ? O3 H3A 0.8400 . ? O4 N9 1.232(3) . ? O5 N9 1.263(3) . ? O6 N9 1.233(3) . ? O7 N12 1.249(2) . ? O8 N12 1.274(3) . ? O9 N12 1.231(3) . ? O10 N10 1.229(3) . ? O11 N10 1.253(3) . ? O12 N10 1.267(3) . ? O13 N11 1.260(3) . ? O14 N11 1.259(3) . ? O15 N11 1.237(3) . ? N1 C5 1.338(3) . ? N1 C1 1.339(3) . ? N2 N3 1.325(2) . ? N2 C6 1.335(3) . ? N3 C9 1.334(3) . ? N4 C14 1.340(3) . ? N4 C10 1.341(3) . ? N5 C24 1.340(3) . ? N5 C28 1.350(3) . ? N6 N7 1.325(2) . ? N6 C23 1.338(3) . ? N7 C20 1.338(3) . ? N8 C15 1.342(3) . ? N8 C19 1.346(3) . ? C1 C2 1.375(4) . ? C1 H1 0.9500 . ? C2 C3 1.380(4) . ? C2 H2 0.9500 . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C5 1.383(3) . ? C4 H4 0.9500 . ? C5 C6 1.489(3) . ? C6 C7 1.410(3) . ? C7 C8 1.393(3) . ? C7 C29 1.506(3) . ? C8 C9 1.411(3) . ? C8 C31 1.509(3) . ? C9 C10 1.492(3) . ? C10 C11 1.394(3) . ? C11 C12 1.385(3) . ? C11 H11 0.9500 . ? C12 C13 1.372(4) . ? C12 H12 0.9500 . ? C13 C14 1.387(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.384(4) . ? C15 H15 0.9500 . ? C16 C17 1.382(4) . ? C16 H16 0.9500 . ? C17 C18 1.386(3) . ? C17 H17 0.9500 . ? C18 C19 1.391(3) . ? C18 H18 0.9500 . ? C19 C20 1.496(3) . ? C20 C21 1.406(3) . ? C21 C22 1.402(3) . ? C21 C30 1.503(3) . ? C22 C23 1.411(3) . ? C22 C32 1.509(3) . ? C23 C24 1.488(3) . ? C24 C25 1.392(3) . ? C25 C26 1.384(3) . ? C25 H25 0.9500 . ? C26 C27 1.378(4) . ? C26 H26 0.9500 . ? C27 C28 1.373(4) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.560(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.555(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.503(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.491(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.518(9) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C37' C38' 1.501(7) . ? C37' H37D 0.9800 . ? C37' H37E 0.9800 . ? C37' H37F 0.9800 . ? C38' H38C 0.9900 . ? C38' H38D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 N3 85.44(7) . . ? O2 Cd1 O1 79.34(8) . . ? N3 Cd1 O1 88.20(8) . . ? O2 Cd1 O3 91.68(8) . . ? N3 Cd1 O3 81.62(7) . . ? O1 Cd1 O3 166.96(7) . . ? O2 Cd1 O5 128.49(8) . . ? N3 Cd1 O5 144.99(8) . . ? O1 Cd1 O5 104.75(10) . . ? O3 Cd1 O5 88.24(10) . . ? O2 Cd1 O4 75.74(7) . . ? N3 Cd1 O4 157.62(8) . . ? O1 Cd1 O4 99.89(9) . . ? O3 Cd1 O4 86.86(8) . . ? O5 Cd1 O4 52.81(8) . . ? O2 Cd1 N4 153.96(7) . . ? N3 Cd1 N4 68.66(7) . . ? O1 Cd1 N4 96.62(8) . . ? O3 Cd1 N4 87.28(8) . . ? O5 Cd1 N4 77.51(8) . . ? O4 Cd1 N4 130.10(7) . . ? N7 Cd2 N8 69.14(7) . . ? N7 Cd2 O12 143.28(7) . . ? N8 Cd2 O12 84.18(7) . . ? N7 Cd2 O14 85.21(8) . . ? N8 Cd2 O14 148.91(7) . . ? O12 Cd2 O14 109.12(8) . . ? N7 Cd2 O11 160.04(7) . . ? N8 Cd2 O11 130.74(7) . . ? O12 Cd2 O11 53.11(7) . . ? O14 Cd2 O11 76.38(8) . . ? N7 Cd2 O8 80.27(7) . . ? N8 Cd2 O8 107.68(7) . . ? O12 Cd2 O8 133.42(7) . . ? O14 Cd2 O8 83.91(8) . . ? O11 Cd2 O8 90.04(7) . . ? N7 Cd2 O7 110.26(7) . . ? N8 Cd2 O7 80.34(7) . . ? O12 Cd2 O7 88.58(7) . . ? O14 Cd2 O7 126.53(8) . . ? O11 Cd2 O7 75.84(8) . . ? O8 Cd2 O7 51.58(6) . . ? N7 Cd2 O13 74.62(8) . . ? N8 Cd2 O13 102.50(8) . . ? O12 Cd2 O13 87.70(8) . . ? O14 Cd2 O13 52.06(8) . . ? O11 Cd2 O13 99.31(8) . . ? O8 Cd2 O13 130.16(6) . . ? O7 Cd2 O13 175.06(7) . . ? C38 O1 Cd1 124.2(13) . . ? C38' O1 Cd1 125.2(4) . . ? C38 O1 H1A 109.5 . . ? C38' O1 H1A 100.1 . . ? Cd1 O1 H1A 124.6 . . ? C38 O1 H1'A 127.6 . . ? C38' O1 H1'A 109.4 . . ? Cd1 O1 H1'A 94.3 . . ? C34 O2 Cd1 122.49(16) . . ? C34 O2 H2A 109.5 . . ? Cd1 O2 H2A 119.1 . . ? C35 O3 Cd1 134.41(18) . . ? C35 O3 H3A 109.5 . . ? Cd1 O3 H3A 113.0 . . ? N9 O4 Cd1 93.01(17) . . ? N9 O5 Cd1 97.22(17) . . ? N12 O7 Cd2 95.65(14) . . ? N12 O8 Cd2 95.76(13) . . ? N10 O11 Cd2 92.66(15) . . ? N10 O12 Cd2 97.12(14) . . ? N11 O13 Cd2 89.44(18) . . ? N11 O14 Cd2 98.43(17) . . ? C5 N1 C1 116.5(2) . . ? N3 N2 C6 118.65(19) . . ? N2 N3 C9 122.27(19) . . ? N2 N3 Cd1 115.89(14) . . ? C9 N3 Cd1 120.96(15) . . ? C14 N4 C10 118.0(2) . . ? C14 N4 Cd1 120.31(17) . . ? C10 N4 Cd1 111.30(15) . . ? C24 N5 C28 116.8(2) . . ? N7 N6 C23 119.43(19) . . ? N6 N7 C20 121.92(18) . . ? N6 N7 Cd2 117.16(14) . . ? C20 N7 Cd2 117.29(14) . . ? C15 N8 C19 118.7(2) . . ? C15 N8 Cd2 122.71(16) . . ? C19 N8 Cd2 117.63(14) . . ? O4 N9 O6 122.8(3) . . ? O4 N9 O5 116.6(2) . . ? O6 N9 O5 120.6(3) . . ? O10 N10 O11 121.6(2) . . ? O10 N10 O12 121.3(2) . . ? O11 N10 O12 117.1(2) . . ? O15 N11 O14 119.9(3) . . ? O15 N11 O13 121.3(3) . . ? O14 N11 O13 118.7(2) . . ? O9 N12 O7 121.9(2) . . ? O9 N12 O8 121.1(2) . . ? O7 N12 O8 117.0(2) . . ? N1 C1 C2 124.5(2) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C3 118.0(2) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 118.5(2) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 123.4(2) . . ? N1 C5 C6 116.3(2) . . ? C4 C5 C6 120.1(2) . . ? N2 C6 C7 123.05(19) . . ? N2 C6 C5 111.63(19) . . ? C7 C6 C5 125.24(19) . . ? C8 C7 C6 117.4(2) . . ? C8 C7 C29 120.6(2) . . ? C6 C7 C29 121.93(19) . . ? C7 C8 C9 116.6(2) . . ? C7 C8 C31 121.0(2) . . ? C9 C8 C31 122.2(2) . . ? N3 C9 C8 121.62(19) . . ? N3 C9 C10 113.30(19) . . ? C8 C9 C10 125.1(2) . . ? N4 C10 C11 122.5(2) . . ? N4 C10 C9 115.58(19) . . ? C11 C10 C9 121.7(2) . . ? C12 C11 C10 118.2(2) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C13 C12 C11 119.6(2) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 118.6(2) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? N4 C14 C13 122.8(3) . . ? N4 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? N8 C15 C16 123.1(2) . . ? N8 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C17 C16 C15 118.2(2) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C16 C17 C18 119.2(2) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C17 C18 C19 119.4(2) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? N8 C19 C18 121.24(19) . . ? N8 C19 C20 116.04(19) . . ? C18 C19 C20 122.5(2) . . ? N7 C20 C21 121.10(19) . . ? N7 C20 C19 112.98(18) . . ? C21 C20 C19 125.92(19) . . ? C22 C21 C20 116.9(2) . . ? C22 C21 C30 120.77(19) . . ? C20 C21 C30 122.16(19) . . ? C21 C22 C23 117.37(19) . . ? C21 C22 C32 118.96(19) . . ? C23 C22 C32 123.66(19) . . ? N6 C23 C22 122.15(19) . . ? N6 C23 C24 112.15(19) . . ? C22 C23 C24 125.70(19) . . ? N5 C24 C25 123.1(2) . . ? N5 C24 C23 117.8(2) . . ? C25 C24 C23 119.1(2) . . ? C26 C25 C24 118.6(2) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C27 C26 C25 119.0(3) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C28 C27 C26 118.8(2) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? N5 C28 C27 123.7(3) . . ? N5 C28 H28 118.2 . . ? C27 C28 H28 118.2 . . ? C7 C29 C30 115.63(18) . . ? C7 C29 H29A 108.4 . . ? C30 C29 H29A 108.4 . . ? C7 C29 H29B 108.4 . . ? C30 C29 H29B 108.4 . . ? H29A C29 H29B 107.4 . . ? C21 C30 C29 113.59(17) . . ? C21 C30 H30A 108.8 . . ? C29 C30 H30A 108.8 . . ? C21 C30 H30B 108.8 . . ? C29 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C8 C31 C32 113.28(17) . . ? C8 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? C8 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? C22 C32 C31 115.27(18) . . ? C22 C32 H32A 108.5 . . ? C31 C32 H32A 108.5 . . ? C22 C32 H32B 108.5 . . ? C31 C32 H32B 108.5 . . ? H32A C32 H32B 107.5 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O2 C34 C33 110.9(3) . . ? O2 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.0 . . ? O3 C35 C36 110.9(3) . . ? O3 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? O3 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O1 C38 C37 102.5(9) . . ? O1 C38 H38A 111.3 . . ? C37 C38 H38A 111.3 . . ? O1 C38 H38B 111.3 . . ? C37 C38 H38B 111.3 . . ? H38A C38 H38B 109.2 . . ? C38' C37' H37D 109.5 . . ? C38' C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? C38' C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? O1 C38' C37' 104.3(5) . . ? O1 C38' H38C 110.9 . . ? C37' C38' H38C 110.9 . . ? O1 C38' H38D 110.9 . . ? C37' C38' H38D 110.9 . . ? H38C C38' H38D 108.9 . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.23 _refine_diff_density_min -0.81 _refine_diff_density_rms 0.08 #===END data_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 619850' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H54 Cd2 N28 O12' _chemical_formula_sum 'C90 H54 Cd2 N28 O12' _chemical_formula_weight 1944.41 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' Cd Cd -0.8075 1.2024 '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 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7406(4) _cell_length_b 21.5613(10) _cell_length_c 16.7294(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.066(3) _cell_angle_gamma 90.00 _cell_volume 3825.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8776 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 27.5 _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_max 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1964 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.627 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS version 2.10; Sheldrick, 2003)' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39190 _diffrn_reflns_av_R_equivalents 0.141 _diffrn_reflns_av_sigmaI/netI 0.149 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.56 _reflns_number_total 9012 _reflns_number_gt 4969 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO; COLLECT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004; PLATON (Spek, 2003)' _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^)+20.73P] 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 8770 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.168 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.144 _refine_ls_wR_factor_gt 0.117 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _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 Cd Cd 0.26382(4) 0.75167(2) 0.50258(3) 0.01765(12) Uani 1 1 d . . . O1 O 0.5375(5) 0.8809(2) 0.5587(3) 0.0379(13) Uani 1 1 d . . . O2 O 0.3930(4) 0.8379(2) 0.4698(3) 0.0307(12) Uani 1 1 d . . . O3 O 0.4096(5) 0.8107(2) 0.5954(3) 0.0357(13) Uani 1 1 d . . . O4 O 0.1109(5) 0.8485(2) 0.5171(3) 0.0309(12) Uani 1 1 d . . . O5 O -0.0384(4) 0.8645(2) 0.4149(3) 0.0290(12) Uani 1 1 d . . . O6 O 0.1082(4) 0.7958(2) 0.4071(3) 0.0240(11) Uani 1 1 d . . . N1 N 0.1217(5) 0.4778(2) 0.3102(3) 0.0191(12) Uani 1 1 d . . . N2 N 0.1356(4) 0.6239(2) 0.4058(3) 0.0176(12) Uani 1 1 d . . . N3 N 0.1255(5) 0.6570(2) 0.4742(3) 0.0186(12) Uani 1 1 d . . . N4 N 0.1611(4) 0.7272(2) 0.6096(3) 0.0158(12) Uani 1 1 d . . . N5 N 0.2761(4) 0.3407(2) 0.4517(3) 0.0192(12) Uani 1 1 d . . . N6 N 0.1890(5) 0.3408(2) 0.6456(3) 0.0203(12) Uani 1 1 d . . . N7 N 0.1798(5) 0.3747(2) 0.7135(3) 0.0188(12) Uani 1 1 d . . . N8 N 0.2029(5) 0.5239(2) 0.8016(3) 0.0207(13) Uani 1 1 d . . . N9 N 0.3566(4) 0.7146(2) 0.3953(3) 0.0160(12) Uani 1 1 d . . . N10 N 0.4112(5) 0.6604(2) 0.5414(3) 0.0178(13) Uani 1 1 d . . . N11 N 0.4264(5) 0.6360(2) 0.6184(3) 0.0170(12) Uani 1 1 d . . . N12 N 0.4693(5) 0.5027(3) 0.7363(3) 0.0240(14) Uani 1 1 d . . . N13 N 0.4495(6) 0.8441(3) 0.5424(4) 0.0278(15) Uani 1 1 d . . . N14 N 0.0578(5) 0.8372(3) 0.4464(4) 0.0243(13) Uani 1 1 d . . . C1 C 0.1296(6) 0.4565(3) 0.2355(4) 0.0207(15) Uani 1 1 d . . . H1 H 0.1040 0.4150 0.2231 0.025 Uiso 1 1 calc R . . C2 C 0.1722(6) 0.4908(3) 0.1760(4) 0.0202(15) Uani 1 1 d . . . H2 H 0.1750 0.4735 0.1242 0.024 Uiso 1 1 calc R . . C3 C 0.2106(6) 0.5508(3) 0.1933(4) 0.0217(15) Uani 1 1 d . . . H3 H 0.2415 0.5756 0.1537 0.026 Uiso 1 1 calc R . . C4 C 0.2036(5) 0.5743(3) 0.2690(4) 0.0177(14) Uani 1 1 d . . . H4 H 0.2297 0.6156 0.2825 0.021 Uiso 1 1 calc R . . C5 C 0.1577(5) 0.5367(3) 0.3259(4) 0.0143(13) Uani 1 1 d . . . C6 C 0.1468(5) 0.5626(3) 0.4073(4) 0.0133(13) Uani 1 1 d . . . C7 C 0.1520(5) 0.5277(3) 0.4818(4) 0.0132(13) Uani 1 1 d . . . C8 C 0.1377(5) 0.5625(3) 0.5524(4) 0.0145(13) Uani 1 1 d . . . C9 C 0.1219(5) 0.6287(3) 0.5429(4) 0.0140(14) Uani 1 1 d . . . C10 C 0.1030(5) 0.6719(3) 0.6097(4) 0.0148(14) Uani 1 1 d . . . C11 C 0.0220(6) 0.6587(3) 0.6643(4) 0.0177(14) Uani 1 1 d . . . H11 H -0.0205 0.6200 0.6623 0.021 Uiso 1 1 calc R . . C12 C 0.0035(6) 0.7031(3) 0.7220(4) 0.0178(14) Uani 1 1 d . . . H12 H -0.0495 0.6945 0.7610 0.021 Uiso 1 1 calc R . . C13 C 0.0639(5) 0.7596(3) 0.7214(4) 0.0220(15) Uani 1 1 d . . . H13 H 0.0519 0.7910 0.7594 0.026 Uiso 1 1 calc R . . C14 C 0.1417(6) 0.7696(3) 0.6647(4) 0.0186(15) Uani 1 1 d . . . H14 H 0.1835 0.8084 0.6646 0.022 Uiso 1 1 calc R . . C15 C 0.1738(5) 0.4635(3) 0.4889(4) 0.0151(13) Uani 1 1 d . . . H15 H 0.1843 0.4399 0.4424 0.018 Uiso 1 1 calc R . . C16 C 0.1496(5) 0.5328(3) 0.6278(4) 0.0152(14) Uani 1 1 d . . . H16 H 0.1451 0.5566 0.6750 0.018 Uiso 1 1 calc R . . C17 C 0.2958(6) 0.2977(3) 0.3974(4) 0.0259(16) Uani 1 1 d . . . H17 H 0.3413 0.3097 0.3557 0.031 Uiso 1 1 calc R . . C18 C 0.2548(6) 0.2371(3) 0.3978(4) 0.0258(17) Uani 1 1 d . . . H18 H 0.2717 0.2086 0.3576 0.031 Uiso 1 1 calc R . . C19 C 0.1885(7) 0.2191(3) 0.4583(4) 0.0321(18) Uani 1 1 d . . . H19 H 0.1592 0.1777 0.4610 0.039 Uiso 1 1 calc R . . C20 C 0.1657(6) 0.2627(3) 0.5148(4) 0.0280(17) Uani 1 1 d . . . H20 H 0.1190 0.2518 0.5564 0.034 Uiso 1 1 calc R . . C21 C 0.2118(6) 0.3224(3) 0.5101(4) 0.0184(14) Uani 1 1 d . . . C22 C 0.1930(5) 0.3673(3) 0.5746(4) 0.0169(14) Uani 1 1 d . . . C23 C 0.1801(5) 0.4341(3) 0.5635(4) 0.0152(14) Uani 1 1 d . . . C24 C 0.1677(5) 0.4690(3) 0.6347(4) 0.0132(13) Uani 1 1 d . . . C25 C 0.1715(5) 0.4356(3) 0.7099(4) 0.0164(14) Uani 1 1 d . . . C26 C 0.1640(6) 0.4649(3) 0.7900(4) 0.0184(15) Uani 1 1 d . . . C27 C 0.1207(6) 0.4307(3) 0.8497(4) 0.0211(15) Uani 1 1 d . . . H27 H 0.0903 0.3897 0.8389 0.025 Uiso 1 1 calc R . . C28 C 0.1217(6) 0.4565(3) 0.9250(4) 0.0271(17) Uani 1 1 d . . . H28 H 0.0932 0.4337 0.9671 0.033 Uiso 1 1 calc R . . C29 C 0.1650(6) 0.5162(3) 0.9377(4) 0.0229(15) Uani 1 1 d . . . H29 H 0.1682 0.5353 0.9892 0.027 Uiso 1 1 calc R . . C30 C 0.2036(6) 0.5478(3) 0.8747(4) 0.0230(15) Uani 1 1 d . . . H30 H 0.2324 0.5892 0.8840 0.028 Uiso 1 1 calc R . . C31 C 0.3560(5) 0.7496(3) 0.3300(3) 0.0199(13) Uani 1 1 d . . . H31 H 0.3038 0.7854 0.3245 0.024 Uiso 1 1 calc R . . C32 C 0.4266(6) 0.7373(3) 0.2693(4) 0.0181(15) Uani 1 1 d . . . H32 H 0.4215 0.7632 0.2230 0.022 Uiso 1 1 calc R . . C33 C 0.5041(6) 0.6865(3) 0.2781(4) 0.0205(15) Uani 1 1 d . . . H33 H 0.5553 0.6772 0.2383 0.025 Uiso 1 1 calc R . . C34 C 0.5070(5) 0.6491(3) 0.3455(4) 0.0172(14) Uani 1 1 d . . . H34 H 0.5601 0.6136 0.3522 0.021 Uiso 1 1 calc R . . C35 C 0.4321(5) 0.6635(3) 0.4031(4) 0.0162(14) Uani 1 1 d . . . C36 C 0.4343(5) 0.6272(3) 0.4796(4) 0.0159(14) Uani 1 1 d . . . C37 C 0.4657(5) 0.5625(3) 0.4870(4) 0.0152(13) Uani 1 1 d . . . C38 C 0.4919(5) 0.5388(3) 0.5665(4) 0.0147(13) Uani 1 1 d . . . C39 C 0.4710(5) 0.5796(3) 0.6314(4) 0.0168(14) Uani 1 1 d . . . C40 C 0.4955(6) 0.5615(3) 0.7195(4) 0.0194(14) Uani 1 1 d . . . C41 C 0.5386(6) 0.6049(3) 0.7784(4) 0.0241(16) Uani 1 1 d . . . H41 H 0.5561 0.6462 0.7639 0.029 Uiso 1 1 calc R . . C42 C 0.5557(6) 0.5870(4) 0.8588(4) 0.0319(18) Uani 1 1 d . . . H42 H 0.5853 0.6157 0.9005 0.038 Uiso 1 1 calc R . . C43 C 0.5292(6) 0.5268(4) 0.8769(5) 0.0324(18) Uani 1 1 d . . . H43 H 0.5402 0.5134 0.9317 0.039 Uiso 1 1 calc R . . C44 C 0.4867(6) 0.4862(4) 0.8154(4) 0.0311(18) Uani 1 1 d . . . H44 H 0.4687 0.4447 0.8290 0.037 Uiso 1 1 calc R . . C45 C 0.5292(5) 0.4765(3) 0.5793(4) 0.0159(14) Uani 1 1 d . . . H45 H 0.5508 0.4610 0.6328 0.019 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 Cd 0.0256(2) 0.0126(2) 0.0155(2) 0.0006(3) 0.00552(16) -0.0002(2) O1 0.047(3) 0.033(3) 0.034(3) -0.009(3) 0.007(3) -0.022(3) O2 0.040(3) 0.036(3) 0.016(3) 0.003(2) 0.003(2) -0.014(2) O3 0.053(3) 0.034(3) 0.021(3) 0.006(2) 0.007(2) -0.018(3) O4 0.050(3) 0.022(3) 0.020(3) 0.001(2) 0.002(2) 0.003(2) O5 0.035(3) 0.026(3) 0.026(3) 0.008(2) 0.005(2) 0.012(2) O6 0.028(2) 0.016(2) 0.028(3) -0.002(2) 0.003(2) 0.004(2) N1 0.026(3) 0.017(3) 0.013(3) -0.002(2) 0.001(2) -0.003(2) N2 0.021(3) 0.014(3) 0.019(3) -0.003(2) 0.005(2) -0.002(2) N3 0.026(3) 0.012(3) 0.017(3) 0.001(2) 0.003(2) 0.003(2) N4 0.021(3) 0.013(3) 0.014(3) 0.005(2) 0.003(2) 0.001(2) N5 0.019(3) 0.020(3) 0.020(3) -0.003(2) 0.008(2) 0.000(2) N6 0.030(3) 0.014(3) 0.016(3) -0.003(2) 0.002(2) 0.000(2) N7 0.028(3) 0.016(3) 0.013(3) -0.001(2) 0.005(2) 0.003(2) N8 0.027(3) 0.022(3) 0.014(3) -0.002(2) 0.006(2) -0.001(3) N9 0.021(3) 0.014(3) 0.013(3) 0.002(2) -0.001(2) 0.001(2) N10 0.023(3) 0.016(3) 0.014(3) 0.001(2) 0.001(2) 0.001(2) N11 0.028(3) 0.014(3) 0.009(3) 0.000(2) 0.002(2) 0.004(2) N12 0.026(3) 0.029(3) 0.018(4) 0.004(3) 0.006(3) 0.009(3) N13 0.034(3) 0.022(3) 0.026(4) -0.009(3) 0.001(3) -0.003(3) N14 0.037(3) 0.017(3) 0.021(4) 0.007(3) 0.010(3) 0.002(3) C1 0.030(4) 0.021(4) 0.012(4) -0.005(3) 0.006(3) 0.001(3) C2 0.024(3) 0.026(4) 0.010(3) -0.002(3) 0.003(3) 0.004(3) C3 0.032(4) 0.023(4) 0.011(3) -0.002(3) 0.008(3) 0.000(3) C4 0.024(3) 0.018(3) 0.011(3) -0.001(3) 0.002(3) -0.002(3) C5 0.014(3) 0.018(3) 0.011(3) 0.001(3) 0.003(2) -0.001(3) C6 0.009(3) 0.011(3) 0.020(4) -0.005(3) 0.004(3) -0.004(2) C7 0.013(3) 0.016(3) 0.010(3) 0.002(3) 0.000(2) -0.003(3) C8 0.012(3) 0.016(3) 0.017(3) 0.002(3) 0.004(2) -0.002(3) C9 0.009(3) 0.008(3) 0.025(4) 0.006(3) 0.002(3) -0.005(2) C10 0.015(3) 0.009(3) 0.020(4) -0.004(3) 0.003(3) 0.005(3) C11 0.025(3) 0.013(3) 0.016(4) 0.005(3) 0.003(3) 0.001(3) C12 0.026(3) 0.011(3) 0.017(4) 0.000(3) 0.006(3) -0.001(3) C13 0.027(3) 0.019(4) 0.021(4) 0.000(3) 0.007(3) 0.002(3) C14 0.025(3) 0.017(3) 0.013(4) -0.003(3) 0.001(3) -0.003(3) C15 0.018(3) 0.012(3) 0.016(4) -0.002(3) 0.004(3) -0.004(3) C16 0.013(3) 0.015(3) 0.016(3) -0.008(3) -0.002(3) -0.001(3) C17 0.026(4) 0.029(4) 0.024(4) -0.005(3) 0.007(3) -0.002(3) C18 0.030(4) 0.025(4) 0.025(4) -0.006(3) 0.010(3) 0.003(3) C19 0.051(5) 0.017(4) 0.030(5) -0.002(3) 0.011(4) -0.007(3) C20 0.049(4) 0.013(4) 0.024(4) -0.003(3) 0.011(3) -0.008(3) C21 0.022(3) 0.017(3) 0.016(4) -0.006(3) 0.002(3) 0.003(3) C22 0.021(3) 0.010(3) 0.019(4) -0.006(3) 0.001(3) -0.003(3) C23 0.012(3) 0.015(3) 0.019(4) 0.003(3) 0.004(3) 0.000(3) C24 0.014(3) 0.009(3) 0.017(4) 0.000(3) 0.002(3) -0.003(2) C25 0.016(3) 0.017(3) 0.017(4) -0.001(3) 0.002(3) -0.005(3) C26 0.019(3) 0.021(4) 0.015(4) -0.005(3) 0.001(3) 0.005(3) C27 0.032(4) 0.013(3) 0.018(4) 0.000(3) 0.005(3) 0.003(3) C28 0.040(4) 0.020(4) 0.025(4) 0.006(3) 0.015(3) 0.005(3) C29 0.033(4) 0.021(4) 0.015(4) -0.008(3) 0.003(3) -0.001(3) C30 0.036(4) 0.020(4) 0.013(4) -0.004(3) 0.003(3) 0.000(3) C31 0.026(3) 0.020(3) 0.015(3) 0.001(4) 0.005(2) 0.000(3) C32 0.032(3) 0.011(4) 0.012(3) 0.003(3) 0.005(3) -0.007(3) C33 0.025(3) 0.020(4) 0.015(4) 0.001(3) -0.002(3) -0.003(3) C34 0.016(3) 0.018(3) 0.017(4) -0.005(3) 0.001(3) 0.005(3) C35 0.020(3) 0.014(3) 0.014(4) -0.004(3) 0.000(3) 0.006(3) C36 0.014(3) 0.017(3) 0.016(4) -0.003(3) 0.000(3) 0.002(3) C37 0.013(3) 0.023(4) 0.011(3) 0.001(3) 0.005(2) 0.001(3) C38 0.013(3) 0.015(3) 0.017(4) -0.003(3) 0.006(3) 0.002(3) C39 0.017(3) 0.018(3) 0.016(4) 0.000(3) 0.005(3) -0.002(3) C40 0.026(3) 0.015(3) 0.017(4) 0.002(3) 0.005(3) 0.006(3) C41 0.033(4) 0.023(4) 0.016(4) -0.002(3) 0.001(3) 0.015(3) C42 0.040(4) 0.039(5) 0.016(4) -0.009(3) -0.001(3) 0.018(4) C43 0.029(4) 0.052(5) 0.019(4) 0.008(4) 0.010(3) 0.014(4) C44 0.036(4) 0.036(4) 0.025(4) 0.007(4) 0.015(3) 0.010(4) C45 0.012(3) 0.020(3) 0.017(3) 0.004(3) 0.005(3) 0.002(3) _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 Cd N3 2.526(5) . ? Cd N4 2.307(5) . ? Cd N9 2.327(5) . ? Cd N10 2.545(5) . ? Cd O2 2.434(5) . ? Cd O3 2.390(5) . ? Cd O6 2.325(4) . ? O1 N13 1.231(7) . ? O2 N13 1.277(7) . ? O3 N13 1.268(7) . ? O4 N14 1.254(7) . ? O5 N14 1.234(7) . ? O6 N14 1.278(7) . ? N1 C5 1.342(8) . ? N1 C1 1.347(8) . ? N2 C6 1.327(7) . ? N2 N3 1.368(7) . ? N3 C9 1.306(8) . ? N4 C14 1.338(8) . ? N4 C10 1.345(7) . ? N5 C17 1.339(8) . ? N5 C21 1.341(8) . ? N6 C22 1.325(8) . ? N6 N7 1.368(7) . ? N7 C25 1.317(8) . ? N8 C30 1.326(8) . ? N8 C26 1.345(8) . ? N9 C31 1.327(8) . ? N9 C35 1.362(7) . ? N10 C36 1.313(8) . ? N10 N11 1.378(7) . ? N11 C39 1.313(8) . ? N12 C40 1.338(8) . ? N12 C44 1.356(8) . ? C1 C2 1.375(9) . ? C1 H1 0.9500 . ? C2 C3 1.374(9) . ? C2 H2 0.9500 . ? C3 C4 1.378(8) . ? C3 H3 0.9500 . ? C4 C5 1.397(8) . ? C4 H4 0.9500 . ? C5 C6 1.493(8) . ? C6 C7 1.450(8) . ? C7 C15 1.406(8) . ? C7 C8 1.428(8) . ? C8 C16 1.403(8) . ? C8 C9 1.443(8) . ? C9 C10 1.493(9) . ? C10 C11 1.386(9) . ? C11 C12 1.395(9) . ? C11 H11 0.9500 . ? C12 C13 1.382(9) . ? C12 H12 0.9500 . ? C13 C14 1.377(9) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C23 1.392(8) . ? C15 H15 0.9500 . ? C16 C24 1.390(8) . ? C16 H16 0.9500 . ? C17 C18 1.378(9) . ? C17 H17 0.9500 . ? C18 C19 1.382(9) . ? C18 H18 0.9500 . ? C19 C20 1.381(9) . ? C19 H19 0.9500 . ? C20 C21 1.386(9) . ? C20 H20 0.9500 . ? C21 C22 1.487(8) . ? C22 C23 1.456(8) . ? C23 C24 1.433(8) . ? C24 C25 1.445(8) . ? C25 C26 1.494(9) . ? C26 C27 1.380(9) . ? C27 C28 1.375(9) . ? C27 H27 0.9500 . ? C28 C29 1.373(9) . ? C28 H28 0.9500 . ? C29 C30 1.373(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.386(8) . ? C31 H31 0.9500 . ? C32 C33 1.368(9) . ? C32 H32 0.9500 . ? C33 C34 1.383(9) . ? C33 H33 0.9500 . ? C34 C35 1.385(8) . ? C34 H34 0.9500 . ? C35 C36 1.495(9) . ? C36 C37 1.437(9) . ? C37 C45 1.400(8) 3_666 ? C37 C38 1.410(8) . ? C38 C45 1.408(8) . ? C38 C39 1.442(8) . ? C39 C40 1.508(9) . ? C40 C41 1.385(9) . ? C41 C42 1.383(9) . ? C41 H41 0.9500 . ? C42 C43 1.372(10) . ? C42 H42 0.9500 . ? C43 C44 1.374(10) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C37 1.400(8) 3_666 ? C45 H45 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cd O6 104.26(16) . . ? N4 Cd N9 146.62(17) . . ? O6 Cd N9 87.68(16) . . ? N4 Cd O3 87.85(17) . . ? O6 Cd O3 123.70(16) . . ? N9 Cd O3 111.55(17) . . ? N4 Cd O2 135.18(17) . . ? O6 Cd O2 84.64(15) . . ? N9 Cd O2 76.09(17) . . ? O3 Cd O2 53.24(16) . . ? N4 Cd N3 67.75(18) . . ? O6 Cd N3 82.17(16) . . ? N9 Cd N3 83.59(17) . . ? O3 Cd N3 149.07(17) . . ? O2 Cd N3 156.15(17) . . ? N4 Cd N10 88.82(17) . . ? O6 Cd N10 147.39(16) . . ? N9 Cd N10 66.84(17) . . ? O3 Cd N10 85.90(17) . . ? O2 Cd N10 107.12(17) . . ? N3 Cd N10 75.31(16) . . ? N13 O2 Cd 93.9(4) . . ? N13 O3 Cd 96.2(4) . . ? N14 O6 Cd 104.5(4) . . ? C5 N1 C1 116.4(6) . . ? C6 N2 N3 121.5(5) . . ? C9 N3 N2 120.7(5) . . ? C9 N3 Cd 108.0(4) . . ? N2 N3 Cd 117.2(4) . . ? C14 N4 C10 118.8(5) . . ? C14 N4 Cd 121.6(4) . . ? C10 N4 Cd 118.9(4) . . ? C17 N5 C21 116.3(6) . . ? C22 N6 N7 122.0(5) . . ? C25 N7 N6 120.6(5) . . ? C30 N8 C26 117.2(6) . . ? C31 N9 C35 117.7(6) . . ? C31 N9 Cd 119.5(4) . . ? C35 N9 Cd 121.6(4) . . ? C36 N10 N11 121.3(5) . . ? C36 N10 Cd 114.0(4) . . ? N11 N10 Cd 120.8(4) . . ? C39 N11 N10 119.6(5) . . ? C40 N12 C44 116.9(6) . . ? O1 N13 O3 122.9(6) . . ? O1 N13 O2 120.8(6) . . ? O3 N13 O2 116.3(6) . . ? O5 N14 O4 122.4(6) . . ? O5 N14 O6 120.6(6) . . ? O4 N14 O6 117.0(5) . . ? N1 C1 C2 124.4(6) . . ? N1 C1 H1 117.8 . . ? C2 C1 H1 117.8 . . ? C3 C2 C1 118.6(6) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 118.7(6) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 119.3(6) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 122.6(6) . . ? N1 C5 C6 118.0(5) . . ? C4 C5 C6 119.4(5) . . ? N2 C6 C7 121.6(6) . . ? N2 C6 C5 112.0(5) . . ? C7 C6 C5 126.3(5) . . ? C15 C7 C8 119.1(6) . . ? C15 C7 C6 124.5(6) . . ? C8 C7 C6 116.3(5) . . ? C16 C8 C7 119.7(5) . . ? C16 C8 C9 122.9(6) . . ? C7 C8 C9 117.1(6) . . ? N3 C9 C8 122.6(6) . . ? N3 C9 C10 113.2(5) . . ? C8 C9 C10 124.2(6) . . ? N4 C10 C11 121.5(6) . . ? N4 C10 C9 115.7(6) . . ? C11 C10 C9 122.6(5) . . ? C10 C11 C12 119.2(6) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 118.8(6) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 C12 118.6(6) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? N4 C14 C13 123.0(6) . . ? N4 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? C23 C15 C7 120.5(6) . . ? C23 C15 H15 119.8 . . ? C7 C15 H15 119.8 . . ? C24 C16 C8 121.2(6) . . ? C24 C16 H16 119.4 . . ? C8 C16 H16 119.4 . . ? N5 C17 C18 124.7(7) . . ? N5 C17 H17 117.7 . . ? C18 C17 H17 117.7 . . ? C17 C18 C19 118.1(6) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C20 C19 C18 118.5(6) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C21 119.3(7) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N5 C21 C20 123.0(6) . . ? N5 C21 C22 118.7(6) . . ? C20 C21 C22 118.2(6) . . ? N6 C22 C23 121.7(6) . . ? N6 C22 C21 113.4(5) . . ? C23 C22 C21 124.9(6) . . ? C15 C23 C24 120.6(6) . . ? C15 C23 C22 123.7(6) . . ? C24 C23 C22 115.7(6) . . ? C16 C24 C23 118.7(6) . . ? C16 C24 C25 123.3(6) . . ? C23 C24 C25 117.9(5) . . ? N7 C25 C24 122.0(6) . . ? N7 C25 C26 113.2(6) . . ? C24 C25 C26 124.9(6) . . ? N8 C26 C27 122.2(6) . . ? N8 C26 C25 118.1(6) . . ? C27 C26 C25 119.7(6) . . ? C28 C27 C26 119.5(6) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 118.4(7) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C28 C29 C30 118.8(6) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? N8 C30 C29 123.8(6) . . ? N8 C30 H30 118.1 . . ? C29 C30 H30 118.1 . . ? N9 C31 C32 124.2(6) . . ? N9 C31 H31 117.9 . . ? C32 C31 H31 117.9 . . ? C33 C32 C31 117.9(6) . . ? C33 C32 H32 121.0 . . ? C31 C32 H32 121.0 . . ? C32 C33 C34 119.4(6) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C33 C34 C35 119.7(6) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? N9 C35 C34 121.1(6) . . ? N9 C35 C36 115.8(6) . . ? C34 C35 C36 123.0(5) . . ? N10 C36 C37 122.1(6) . . ? N10 C36 C35 114.2(5) . . ? C37 C36 C35 123.6(6) . . ? C45 C37 C38 120.1(6) 3_666 . ? C45 C37 C36 123.6(6) 3_666 . ? C38 C37 C36 116.3(6) . . ? C45 C38 C37 119.9(6) . . ? C45 C38 C39 122.7(6) . . ? C37 C38 C39 117.2(5) . . ? N11 C39 C38 122.5(6) . . ? N11 C39 C40 113.8(5) . . ? C38 C39 C40 123.7(5) . . ? N12 C40 C41 123.3(6) . . ? N12 C40 C39 116.1(6) . . ? C41 C40 C39 120.6(6) . . ? C42 C41 C40 118.8(7) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C43 C42 C41 118.6(7) . . ? C43 C42 H42 120.7 . . ? C41 C42 H42 120.7 . . ? C42 C43 C44 119.6(7) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? N12 C44 C43 122.8(7) . . ? N12 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? C37 C45 C38 119.8(6) 3_666 . ? C37 C45 H45 120.1 3_666 . ? C38 C45 H45 120.1 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.69 _refine_diff_density_min -0.82 _refine_diff_density_rms 0.14 #===END