# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'A. Durif' _publ_contact_author_email Andre.Durif@ujf-grenoble.fr #------------------------------------------------------------------------------ _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; loop_ _publ_author_name H.Aroraa C.Philouze O.Jarjayes F.Thomas data_Sadabs _database_code_depnum_ccdc_archive 'CCDC 772953' #TrackingRef '- CCDC772953.cif' #------------------------------------------------------------------------------ _audit_creation_date 2010-03-24 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-Enraf-Nonius kappaCCD' _computing_cell_refinement 'Bruker-Enraf-Nonius kappaCCD' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 18.166(4) _cell_length_b 26.129(4) _cell_length_c 6.877(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3264(1) _cell_formula_units_Z 2 _cell_measurement_temperature 200.0 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_Int_Tables_number 60 _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2-y,1/2+z '1/2+x,1/2-y, -z' ' -x, +y,1/2-z' ' -x, -y, -z' 1/2+x,1/2+y,1/2-z '1/2-x,1/2+y, +z' ' +x, -y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1189.13 _chemical_formula_analytical ? _chemical_formula_sum 'C76 H92 Cu N4 O4 ' _chemical_formula_moiety 'C76 H92 Cu N4 O4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1274.00 _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_correction_T_min 0.689 _exptl_special_details ; SADABS relative correction factor 0.717 ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 200.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Bruker-Enraf-Nonius kappaCCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? _diffrn_reflns_number 13221 _reflns_number_total 2950 _reflns_number_gt 1841 _reflns_threshold_expression I>1.00\s(I) _diffrn_reflns_av_R_equivalents 0.03976 _diffrn_reflns_av_sigmaI/netI 0.090 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 152 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 184 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cu 0 2 0.263 1.266 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.0000 0.06150(2) 0.2500 0.0211(1) 1.000 ST Uani d ? O(1) 0.0640(1) 0.11133(8) 0.3483(3) 0.0266(6) 1.000 . Uani d ? N(1) 0.0691(1) 0.00648(9) 0.3061(3) 0.0197(7) 1.000 . Uani d ? C(1) 0.1342(2) 0.1082(1) 0.3869(4) 0.0221(8) 1.000 . Uani d ? C(2) 0.1736(2) 0.1545(1) 0.4300(4) 0.0252(8) 1.000 . Uani d ? C(3) 0.2476(2) 0.1516(1) 0.4683(5) 0.0322(9) 1.000 . Uani d ? C(4) 0.2887(2) 0.1064(1) 0.4627(5) 0.0330(9) 1.000 . Uani d ? C(5) 0.2508(2) 0.0626(1) 0.4241(5) 0.0295(9) 1.000 . Uani d ? C(6) 0.1740(2) 0.0613(1) 0.3924(4) 0.0230(8) 1.000 . Uani d ? C(7) 0.1396(2) 0.0110(1) 0.3705(4) 0.0215(8) 1.000 . Uani d ? C(8) 0.1778(2) -0.0340(1) 0.4182(4) 0.0278(9) 1.000 . Uani d ? C(9) 0.1461(2) -0.0809(1) 0.4014(5) 0.0283(9) 1.000 . Uani d ? C(10) 0.0746(2) -0.0845(1) 0.3355(5) 0.0270(8) 1.000 . Uani d ? C(11) 0.0379(2) -0.0404(1) 0.2877(4) 0.0211(8) 1.000 . Uani d ? C(12) 0.1338(2) 0.2060(1) 0.4268(5) 0.0284(9) 1.000 . Uani d ? C(13) 0.1843(2) 0.2505(1) 0.4815(6) 0.040(1) 1.000 . Uani d ? C(14) 0.0704(2) 0.2068(1) 0.5726(5) 0.035(1) 1.000 . Uani d ? C(15) 0.1049(2) 0.2162(1) 0.2206(5) 0.039(1) 1.000 . Uani d ? C(16) 0.3711(2) 0.1062(1) 0.5083(6) 0.049(1) 1.000 . Uani d ? C(17) 0.3800(2) 0.1154(2) 0.7270(8) 0.097(2) 1.000 . Uani d ? C(18) 0.4098(2) 0.1495(2) 0.4042(8) 0.089(2) 1.000 . Uani d ? C(19) 0.4076(2) 0.0570(2) 0.458(1) 0.106(2) 1.000 . Uani d ? H(1) 0.2726 0.1823 0.5008 0.039 1.000 . Uiso c ? H(2) 0.2774 0.0313 0.4182 0.035 1.000 . Uiso c ? H(3) 0.2271 -0.0316 0.4634 0.033 1.000 . Uiso c ? H(4) 0.1730 -0.1108 0.4347 0.034 1.000 . Uiso c ? H(5) 0.0512 -0.1169 0.3236 0.032 1.000 . Uiso c ? H(6) 0.2254 0.2511 0.3961 0.048 1.000 . Uiso c ? H(7) 0.2009 0.2462 0.6115 0.048 1.000 . Uiso c ? H(8) 0.1580 0.2818 0.4709 0.048 1.000 . Uiso c ? H(9) 0.0894 0.2030 0.7005 0.041 1.000 . Uiso c ? H(10) 0.0449 0.2384 0.5629 0.041 1.000 . Uiso c ? H(11) 0.0376 0.1795 0.5451 0.041 1.000 . Uiso c ? H(12) 0.1451 0.2183 0.1328 0.047 1.000 . Uiso c ? H(13) 0.0783 0.2475 0.2190 0.047 1.000 . Uiso c ? H(14) 0.0732 0.1890 0.1824 0.047 1.000 . Uiso c ? H(15) 0.4309 0.1181 0.7578 0.116 1.000 . Uiso c ? H(16) 0.3557 0.1462 0.7622 0.116 1.000 . Uiso c ? H(17) 0.3591 0.0876 0.7967 0.116 1.000 . Uiso c ? H(18) 0.4597 0.1510 0.4448 0.107 1.000 . Uiso c ? H(19) 0.3862 0.1810 0.4344 0.107 1.000 . Uiso c ? H(20) 0.4078 0.1439 0.2678 0.107 1.000 . Uiso c ? H(21) 0.4575 0.0580 0.4986 0.128 1.000 . Uiso c ? H(22) 0.4055 0.0520 0.3212 0.128 1.000 . Uiso c ? H(23) 0.3829 0.0297 0.5215 0.128 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0196(2) 0.0254(2) 0.0181(3) 0.0000 -0.0005(3) 0.0000 O(1) 0.019(1) 0.029(1) 0.032(1) 0.001(1) -0.003(1) -0.001(1) N(1) 0.021(1) 0.028(1) 0.010(2) 0.001(1) 0.001(1) -0.001(1) C(1) 0.021(2) 0.035(2) 0.010(2) 0.000(1) 0.004(1) 0.000(1) C(2) 0.026(2) 0.035(2) 0.015(2) -0.005(1) 0.002(2) -0.003(2) C(3) 0.027(2) 0.036(2) 0.034(2) -0.006(2) -0.004(2) -0.007(2) C(4) 0.022(2) 0.043(2) 0.033(2) -0.004(2) -0.001(2) -0.008(2) C(5) 0.023(2) 0.039(2) 0.026(2) 0.008(1) -0.002(2) -0.009(2) C(6) 0.024(2) 0.033(2) 0.012(2) -0.001(1) 0.000(1) -0.002(1) C(7) 0.023(2) 0.032(2) 0.010(2) 0.001(1) 0.003(1) -0.002(1) C(8) 0.025(2) 0.042(2) 0.016(2) 0.005(2) 0.002(2) -0.001(2) C(9) 0.031(2) 0.031(2) 0.023(2) 0.010(2) 0.006(2) 0.003(2) C(10) 0.031(2) 0.028(2) 0.022(2) 0.002(2) 0.003(2) -0.002(2) C(11) 0.027(2) 0.026(1) 0.010(2) 0.003(1) 0.005(1) -0.001(2) C(12) 0.029(2) 0.031(2) 0.025(2) -0.001(1) -0.001(2) 0.005(2) C(13) 0.040(2) 0.037(2) 0.045(2) -0.007(2) 0.003(2) -0.002(2) C(14) 0.036(2) 0.029(2) 0.039(2) 0.000(2) 0.003(2) 0.001(2) C(15) 0.039(2) 0.036(2) 0.043(2) -0.006(1) -0.007(2) 0.009(2) C(16) 0.017(2) 0.059(2) 0.071(3) 0.000(2) -0.005(2) -0.019(2) C(17) 0.042(2) 0.152(5) 0.097(4) 0.009(3) -0.033(3) -0.020(4) C(18) 0.022(2) 0.101(4) 0.144(5) -0.010(2) 0.004(3) 0.001(4) C(19) 0.026(2) 0.084(3) 0.210(6) 0.011(2) -0.020(3) -0.057(4) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1841 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_all 0.0512 _refine_ls_wR_factor_ref 0.0512 _refine_ls_goodness_of_fit_all 1.474 _refine_ls_goodness_of_fit_ref 1.474 _refine_ls_shift/su_max 0.0117 _refine_ls_shift/su_mean 0.0005 _refine_diff_density_min -0.27 _refine_diff_density_max 0.47 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CU1 O1 1.871(2) . . yes CU1 O1 1.871(2) . 4 yes CU1 N1 1.947(2) . . yes CU1 N1 1.947(2) . 4 yes O1 C1 1.306(4) . . yes N1 C7 1.360(4) . . yes N1 C11 1.356(4) . . yes C1 C2 1.436(4) . . yes C1 C6 1.423(4) . . yes C2 C3 1.373(4) . . yes C2 C12 1.529(4) . . yes C3 C4 1.395(4) . . yes C3 H1 0.95 . . no C4 C5 1.363(4) . . yes C4 C16 1.530(4) . . yes C5 C6 1.412(4) . . yes C5 H2 0.95 . . no C6 C7 1.465(4) . . yes C7 C8 1.404(4) . . yes C8 C9 1.358(4) . . yes C8 H3 0.95 . . no C9 C10 1.380(4) . . yes C9 H4 0.95 . . no C10 C11 1.372(4) . . yes C10 H5 0.95 . . no C11 C11 1.472(6) . 4 yes C12 C13 1.527(4) . . yes C12 C14 1.527(4) . . yes C12 C15 1.536(5) . . yes C13 H6 0.95 . . no C13 H7 0.95 . . no C13 H8 0.95 . . no C14 H9 0.95 . . no C14 H10 0.95 . . no C14 H11 0.95 . . no C15 H12 0.95 . . no C15 H13 0.95 . . no C15 H14 0.95 . . no C16 C17 1.531(7) . . yes C16 C18 1.513(6) . . yes C16 C19 1.488(6) . . yes C17 H15 0.95 . . no C17 H16 0.95 . . no C17 H17 0.95 . . no C18 H18 0.95 . . no C18 H19 0.95 . . no C18 H20 0.95 . . no C19 H21 0.95 . . no C19 H22 0.95 . . no C19 H23 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 CU1 O1 91.8(1) . . 4 yes O1 CU1 N1 92.39(9) . . . yes O1 CU1 N1 170.22(9) . . 4 yes O1 CU1 N1 170.22(9) 4 . . yes O1 CU1 N1 92.39(9) 4 . 4 yes N1 CU1 N1 84.8(1) . . 4 yes CU1 O1 C1 129.5(2) . . . yes CU1 N1 C7 127.4(2) . . . yes CU1 N1 C11 112.3(2) . . . yes C7 N1 C11 120.1(2) . . . yes O1 C1 C2 118.4(3) . . . yes O1 C1 C6 123.8(3) . . . yes C2 C1 C6 117.8(3) . . . yes C1 C2 C3 118.8(3) . . . yes C1 C2 C12 120.3(3) . . . yes C3 C2 C12 120.9(3) . . . yes C2 C3 C4 124.4(3) . . . yes C2 C3 H1 117.8 . . . no C4 C3 H1 117.8 . . . no C3 C4 C5 116.5(3) . . . yes C3 C4 C16 121.3(3) . . . yes C5 C4 C16 122.1(3) . . . yes C4 C5 C6 123.2(3) . . . yes C4 C5 H2 118.4 . . . no C6 C5 H2 118.4 . . . no C1 C6 C5 119.1(3) . . . yes C1 C6 C7 123.6(3) . . . yes C5 C6 C7 117.3(3) . . . yes N1 C7 C6 120.9(3) . . . yes N1 C7 C8 118.0(3) . . . yes C6 C7 C8 121.1(3) . . . yes C7 C8 C9 121.7(3) . . . yes C7 C8 H3 119.2 . . . no C9 C8 H3 119.2 . . . no C8 C9 C10 119.3(3) . . . yes C8 C9 H4 120.3 . . . no C10 C9 H4 120.3 . . . no C9 C10 C11 118.5(3) . . . yes C9 C10 H5 120.7 . . . no C11 C10 H5 120.7 . . . no N1 C11 C10 122.3(3) . . . yes N1 C11 C11 115.1(2) . . 4 yes C10 C11 C11 122.6(2) . . 4 yes C2 C12 C13 112.5(3) . . . yes C2 C12 C14 111.0(3) . . . yes C2 C12 C15 109.1(3) . . . yes C13 C12 C14 106.3(3) . . . yes C13 C12 C15 107.6(3) . . . yes C14 C12 C15 110.2(3) . . . yes C12 C13 H6 109.5 . . . no C12 C13 H7 109.5 . . . no C12 C13 H8 109.5 . . . no H6 C13 H7 109.5 . . . no H6 C13 H8 109.5 . . . no H7 C13 H8 109.5 . . . no C12 C14 H9 109.5 . . . no C12 C14 H10 109.5 . . . no C12 C14 H11 109.5 . . . no H9 C14 H10 109.5 . . . no H9 C14 H11 109.5 . . . no H10 C14 H11 109.5 . . . no C12 C15 H12 109.5 . . . no C12 C15 H13 109.5 . . . no C12 C15 H14 109.5 . . . no H12 C15 H13 109.5 . . . no H12 C15 H14 109.5 . . . no H13 C15 H14 109.5 . . . no C4 C16 C17 107.7(3) . . . yes C4 C16 C18 110.8(3) . . . yes C4 C16 C19 113.0(3) . . . yes C17 C16 C18 107.4(4) . . . yes C17 C16 C19 108.5(4) . . . yes C18 C16 C19 109.2(4) . . . yes C16 C17 H15 109.5 . . . no C16 C17 H16 109.5 . . . no C16 C17 H17 109.5 . . . no H15 C17 H16 109.5 . . . no H15 C17 H17 109.5 . . . no H16 C17 H17 109.5 . . . no C16 C18 H18 109.5 . . . no C16 C18 H19 109.5 . . . no C16 C18 H20 109.5 . . . no H18 C18 H19 109.5 . . . no H18 C18 H20 109.5 . . . no H19 C18 H20 109.5 . . . no C16 C19 H21 109.5 . . . no C16 C19 H22 109.5 . . . no C16 C19 H23 109.5 . . . no H21 C19 H22 109.5 . . . no H21 C19 H23 109.5 . . . no H22 C19 H23 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag CU1 C10 3.213(3) . 5_556 no CU1 C10 3.213(3) . 8_554 no CU1 C11 3.300(3) . 5_556 no CU1 C11 3.300(3) . 8_554 no O1 C10 3.399(4) . 5_556 no O1 C10 3.428(4) . 8 no O1 C9 3.508(4) . 8_554 no O1 C11 3.576(4) . 8 no N1 C7 3.289(4) . 8_554 no N1 C8 3.395(4) . 8_554 no N1 N1 3.455(3) . 8 no N1 N1 3.455(3) . 8_554 no N1 C11 3.475(4) . 8 no N1 C11 3.518(4) . 5_556 no C1 C10 3.328(4) . 8 no C1 C9 3.421(4) . 8_554 no C6 C8 3.339(4) . 8_554 no C6 C9 3.453(4) . 8_554 no C6 C9 3.573(4) . 8 no C6 C10 3.594(4) . 8 no C7 C8 3.243(4) . 8_554 no C7 C7 3.486(4) . 8 no C7 C7 3.486(4) . 8_554 no C7 C11 3.497(4) . 8 no C14 C14 3.536(7) . 4_556 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ # Attachment '- CCDC772954.cif' data_Radical_? _database_code_depnum_ccdc_archive 'CCDC 772954' #TrackingRef '- CCDC772954.cif' #------------------------------------------------------------------------------ _audit_creation_date 2010-04-06 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-Enraf-Nonius kappaCCD' _computing_cell_refinement 'Bruker-Enraf-Nonius kappaCCD' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 30.036(4) _cell_length_b 9.288(4) _cell_length_c 27.611(4) _cell_angle_alpha 90 _cell_angle_beta 98.65(1) _cell_angle_gamma 90 _cell_volume 7615(3) _cell_formula_units_Z 8 _cell_measurement_temperature 200.0 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, -y, -z' ' +x, -y,1/2+z' '1/2+x,1/2+y, +z' 1/2-x,1/2+y,1/2-z '1/2-x,1/2-y, -z' 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 700.83 _chemical_formula_analytical ? _chemical_formula_sum 'C43 H51 Co N3 O2 ' _chemical_formula_moiety 'C43 H51 Co N3 O2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2984.00 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 200.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device_type 'Bruker-Enraf-Nonius kappaCCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? _diffrn_reflns_number 46772 _reflns_number_total 8740 _reflns_number_gt 5818 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.08026 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co 0 8 0.299 0.973 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 344 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 24 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 408 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Co(1) 0.96639(1) 0.07634(4) 0.58968(1) 0.02991(8) 1.000 . Uani d ? O(1) 1.01216(6) 0.2144(2) 0.61157(6) 0.0354(5) 1.000 . Uani d ? O(2) 0.91972(6) 0.2176(2) 0.58437(6) 0.0328(5) 1.000 . Uani d ? N(1) 1.01318(7) -0.0596(2) 0.57216(7) 0.0254(5) 1.000 . Uani d ? N(2) 0.92669(7) -0.0557(2) 0.54533(7) 0.0282(5) 1.000 . Uani d ? N(3) 0.95630(8) -0.0105(3) 0.65753(8) 0.0352(6) 1.000 . Uani d ? C(1) 1.05371(9) 0.1883(3) 0.63149(8) 0.0284(6) 1.000 . Uani d ? C(2) 1.07946(9) 0.2995(3) 0.65844(9) 0.0358(7) 1.000 . Uani d ? C(3) 1.1217(1) 0.2648(4) 0.6833(1) 0.0479(8) 1.000 . Uani d ? C(4) 1.1410(1) 0.1293(4) 0.6832(1) 0.0490(9) 1.000 . Uani d ? C(5) 1.1182(1) 0.0286(3) 0.6536(1) 0.0388(8) 1.000 . Uani d ? C(6) 1.07548(9) 0.0553(3) 0.62619(8) 0.0286(6) 1.000 . Uani d ? C(7) 1.05777(8) -0.0509(3) 0.58856(8) 0.0263(6) 1.000 . Uani d ? C(8) 1.08771(9) -0.1376(3) 0.56745(9) 0.0321(7) 1.000 . Uani d ? C(9) 1.0721(1) -0.2315(3) 0.53013(9) 0.0357(7) 1.000 . Uani d ? C(10) 1.0265(1) -0.2397(3) 0.51389(9) 0.0335(7) 1.000 . Uani d ? C(11) 0.99782(9) -0.1534(3) 0.53549(8) 0.0285(6) 1.000 . Uani d ? C(12) 0.94899(9) -0.1511(3) 0.52037(8) 0.0291(6) 1.000 . Uani d ? C(13) 0.9269(1) -0.2340(3) 0.48278(9) 0.0371(7) 1.000 . Uani d ? C(14) 0.8817(1) -0.2175(3) 0.4696(1) 0.0461(8) 1.000 . Uani d ? C(15) 0.8587(1) -0.1229(3) 0.4948(1) 0.0423(8) 1.000 . Uani d ? C(16) 0.88161(9) -0.0415(3) 0.53375(9) 0.0338(7) 1.000 . Uani d ? C(17) 0.85679(9) 0.0614(3) 0.5596(1) 0.0370(7) 1.000 . Uani d ? C(18) 0.8110(1) 0.0341(4) 0.5610(1) 0.0457(8) 1.000 . Uani d ? C(19) 0.7833(1) 0.1310(4) 0.5784(1) 0.0520(9) 1.000 . Uani d ? C(20) 0.8019(1) 0.2629(4) 0.5939(1) 0.0518(9) 1.000 . Uani d ? C(21) 0.84694(9) 0.2982(3) 0.5948(1) 0.0398(8) 1.000 . Uani d ? C(22) 0.87630(9) 0.1914(3) 0.58023(9) 0.0326(7) 1.000 . Uani d ? C(23) 1.0607(1) 0.4517(3) 0.6621(1) 0.0438(8) 1.000 . Uani d ? C(24) 1.0966(1) 0.5579(4) 0.6846(2) 0.082(1) 1.000 . Uani d ? C(25) 1.0244(1) 0.4490(3) 0.6947(1) 0.0511(9) 1.000 . Uani d ? C(26) 1.0409(2) 0.5097(4) 0.6117(1) 0.091(1) 1.000 . Uani d ? C(27) 1.1872(1) 0.0972(6) 0.7132(2) 0.082(1) 1.000 . Uani d ? C(28) 1.2212(2) 0.098(2) 0.6821(3) 0.299(6) 1.000 . Uani d ? C(29) 1.1986(2) 0.199(1) 0.7533(3) 0.235(3) 1.000 . Uani d ? C(30) 1.1872(2) -0.048(1) 0.7358(3) 0.210(3) 1.000 . Uani d ? C(31) 0.8643(1) 0.4479(3) 0.6107(1) 0.0494(9) 1.000 . Uani d ? C(32) 0.8271(2) 0.5511(5) 0.6206(2) 0.094(2) 1.000 . Uani d ? C(33) 0.8880(1) 0.5160(4) 0.5713(1) 0.071(1) 1.000 . Uani d ? C(34) 0.8974(1) 0.4365(4) 0.6585(1) 0.064(1) 1.000 . Uani d ? C(35) 0.7335(1) 0.0959(5) 0.5806(1) 0.073(1) 1.000 . Uani d ? C(36) 0.7263(2) 0.060(2) 0.6239(3) 0.475(6) 1.000 . Uani d ? C(37) 0.7149(2) -0.001(1) 0.5440(3) 0.227(3) 1.000 . Uani d ? C(38) 0.7062(2) 0.220(1) 0.5670(8) 0.458(8) 1.000 . Uani d ? C(39) 0.9508(1) 0.0807(3) 0.6930(1) 0.0515(9) 1.000 . Uani d ? C(40) 0.9418(1) 0.0414(3) 0.7381(1) 0.0533(9) 1.000 . Uani d ? C(41) 0.9387(1) -0.0993(4) 0.7482(1) 0.063(1) 1.000 . Uani d ? C(42) 0.9455(2) -0.1969(4) 0.7126(1) 0.082(1) 1.000 . Uani d ? C(43) 0.9539(1) -0.1483(4) 0.6679(1) 0.063(1) 1.000 . Uani d ? H(1) 1.1385 0.3387 0.7015 0.057 1.000 . Uiso c ? H(2) 1.1315 -0.0633 0.6511 0.047 1.000 . Uiso c ? H(3) 1.1191 -0.1318 0.5789 0.039 1.000 . Uiso c ? H(4) 1.0925 -0.2900 0.5157 0.043 1.000 . Uiso c ? H(5) 1.0150 -0.3038 0.4882 0.040 1.000 . Uiso c ? H(6) 0.9431 -0.3016 0.4663 0.045 1.000 . Uiso c ? H(7) 0.8661 -0.2715 0.4431 0.055 1.000 . Uiso c ? H(8) 0.8271 -0.1120 0.4858 0.051 1.000 . Uiso c ? H(9) 0.7988 -0.0560 0.5493 0.055 1.000 . Uiso c ? H(10) 0.7826 0.3335 0.6045 0.062 1.000 . Uiso c ? H(11) 1.1085 0.5275 0.7168 0.099 1.000 . Uiso c ? H(12) 1.1201 0.5617 0.6651 0.099 1.000 . Uiso c ? H(13) 1.0835 0.6508 0.6859 0.099 1.000 . Uiso c ? H(14) 1.0372 0.4201 0.7268 0.061 1.000 . Uiso c ? H(15) 1.0015 0.3827 0.6819 0.061 1.000 . Uiso c ? H(16) 1.0117 0.5423 0.6959 0.061 1.000 . Uiso c ? H(17) 1.0642 0.5184 0.5920 0.110 1.000 . Uiso c ? H(18) 1.0185 0.4453 0.5964 0.110 1.000 . Uiso c ? H(19) 1.0278 0.6015 0.6152 0.110 1.000 . Uiso c ? H(20) 1.2492 0.0700 0.7004 0.359 1.000 . Uiso c ? H(21) 1.2132 0.0318 0.6559 0.359 1.000 . Uiso c ? H(22) 1.2237 0.1917 0.6692 0.359 1.000 . Uiso c ? H(23) 1.2271 0.1743 0.7713 0.282 1.000 . Uiso c ? H(24) 1.1763 0.1947 0.7743 0.282 1.000 . Uiso c ? H(25) 1.1998 0.2933 0.7405 0.282 1.000 . Uiso c ? H(26) 1.2162 -0.0677 0.7535 0.252 1.000 . Uiso c ? H(27) 1.1799 -0.1182 0.7109 0.252 1.000 . Uiso c ? H(28) 1.1655 -0.0506 0.7575 0.252 1.000 . Uiso c ? H(29) 0.8399 0.6416 0.6308 0.113 1.000 . Uiso c ? H(30) 0.8120 0.5125 0.6455 0.113 1.000 . Uiso c ? H(31) 0.8062 0.5634 0.5914 0.113 1.000 . Uiso c ? H(32) 0.9118 0.4550 0.5648 0.085 1.000 . Uiso c ? H(33) 0.8671 0.5284 0.5422 0.085 1.000 . Uiso c ? H(34) 0.9000 0.6069 0.5824 0.085 1.000 . Uiso c ? H(35) 0.9091 0.5292 0.6677 0.076 1.000 . Uiso c ? H(36) 0.9214 0.3739 0.6538 0.076 1.000 . Uiso c ? H(37) 0.8823 0.3992 0.6836 0.076 1.000 . Uiso c ? H(38) 0.7439 -0.0226 0.6346 0.570 1.000 . Uiso c ? H(39) 0.6953 0.0375 0.6230 0.570 1.000 . Uiso c ? H(40) 0.7343 0.1370 0.6459 0.570 1.000 . Uiso c ? H(41) 0.7184 0.0365 0.5127 0.272 1.000 . Uiso c ? H(42) 0.7299 -0.0909 0.5488 0.272 1.000 . Uiso c ? H(43) 0.6838 -0.0136 0.5456 0.272 1.000 . Uiso c ? H(44) 0.7094 0.2485 0.5347 0.550 1.000 . Uiso c ? H(45) 0.6755 0.1973 0.5683 0.550 1.000 . Uiso c ? H(46) 0.7154 0.2965 0.5891 0.550 1.000 . Uiso c ? H(47) 0.9533 0.1806 0.6865 0.062 1.000 . Uiso c ? H(48) 0.9378 0.1122 0.7619 0.064 1.000 . Uiso c ? H(49) 0.9321 -0.1306 0.7791 0.075 1.000 . Uiso c ? H(50) 0.9444 -0.2972 0.7189 0.099 1.000 . Uiso c ? H(51) 0.9580 -0.2168 0.6434 0.075 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0292(2) 0.0294(2) 0.0309(2) 0.0002(2) 0.0039(1) 0.0070(2) O(1) 0.046(1) 0.0227(9) 0.0347(9) 0.0050(8) -0.0028(8) -0.0025(8) O(2) 0.0303(9) 0.034(1) 0.0346(9) -0.0025(8) 0.0053(7) -0.0017(8) N(1) 0.037(1) 0.021(1) 0.0193(9) -0.0008(9) 0.0068(8) 0.0011(8) N(2) 0.037(1) 0.026(1) 0.0217(9) -0.0051(9) 0.0020(8) 0.0017(9) N(3) 0.045(1) 0.031(1) 0.030(1) -0.003(1) 0.007(1) 0.004(1) C(1) 0.039(1) 0.028(1) 0.019(1) -0.003(1) 0.006(1) 0.001(1) C(2) 0.047(2) 0.033(1) 0.031(1) -0.011(1) 0.020(1) -0.008(1) C(3) 0.041(2) 0.063(2) 0.041(1) -0.020(2) 0.010(1) -0.022(1) C(4) 0.034(2) 0.071(2) 0.041(2) -0.001(2) 0.003(1) -0.015(2) C(5) 0.037(1) 0.046(2) 0.034(1) 0.005(1) 0.008(1) -0.005(1) C(6) 0.034(1) 0.030(1) 0.022(1) 0.000(1) 0.0049(9) 0.001(1) C(7) 0.036(1) 0.020(1) 0.023(1) 0.001(1) 0.006(1) 0.004(1) C(8) 0.037(1) 0.032(1) 0.028(1) 0.006(1) 0.007(1) 0.006(1) C(9) 0.051(2) 0.029(1) 0.029(1) 0.009(1) 0.012(1) 0.002(1) C(10) 0.054(2) 0.025(1) 0.023(1) 0.002(1) 0.010(1) -0.002(1) C(11) 0.044(1) 0.021(1) 0.023(1) -0.002(1) 0.009(1) 0.004(1) C(12) 0.045(1) 0.025(1) 0.018(1) -0.007(1) 0.006(1) 0.002(1) C(13) 0.053(2) 0.032(1) 0.028(1) -0.010(1) 0.010(1) -0.003(1) C(14) 0.060(2) 0.046(2) 0.031(1) -0.022(2) 0.000(1) -0.008(1) C(15) 0.041(2) 0.049(2) 0.034(1) -0.015(1) -0.003(1) 0.001(1) C(16) 0.041(1) 0.032(1) 0.027(1) -0.009(1) 0.002(1) 0.004(1) C(17) 0.031(1) 0.045(2) 0.033(1) 0.000(1) 0.000(1) 0.005(1) C(18) 0.033(1) 0.058(2) 0.044(2) -0.008(1) -0.001(1) 0.003(1) C(19) 0.027(1) 0.079(2) 0.048(2) -0.001(2) -0.001(1) 0.001(2) C(20) 0.035(2) 0.070(2) 0.049(2) 0.015(2) 0.002(1) -0.003(2) C(21) 0.037(1) 0.049(2) 0.033(1) 0.007(1) 0.000(1) 0.003(1) C(22) 0.031(1) 0.040(2) 0.025(1) 0.002(1) 0.001(1) 0.006(1) C(23) 0.072(2) 0.028(2) 0.035(1) -0.012(1) 0.022(1) -0.010(1) C(24) 0.093(3) 0.049(2) 0.116(3) -0.032(2) 0.050(2) -0.041(2) C(25) 0.058(2) 0.039(2) 0.060(2) 0.003(2) 0.022(1) -0.004(2) C(26) 0.208(5) 0.023(2) 0.048(2) 0.008(2) 0.033(2) 0.003(2) C(27) 0.043(2) 0.120(4) 0.075(2) 0.011(2) -0.016(2) -0.036(2) C(28) 0.033(3) 0.70(3) 0.165(7) 0.074(6) 0.014(3) -0.02(1) C(29) 0.160(5) 0.279(8) 0.211(5) 0.098(5) -0.146(4) -0.159(5) C(30) 0.124(4) 0.191(8) 0.263(7) 0.011(5) -0.142(4) 0.037(6) C(31) 0.048(2) 0.041(2) 0.058(2) 0.011(1) 0.007(1) -0.006(1) C(32) 0.071(3) 0.070(3) 0.139(4) 0.025(2) 0.010(3) -0.033(3) C(33) 0.094(3) 0.042(2) 0.077(2) 0.002(2) 0.015(2) 0.010(2) C(34) 0.070(2) 0.057(2) 0.060(2) -0.002(2) -0.001(2) -0.017(2) C(35) 0.024(1) 0.116(3) 0.077(2) -0.003(2) 0.003(2) -0.005(2) C(36) 0.052(3) 1.24(3) 0.131(5) -0.168(7) 0.002(3) 0.221(9) C(37) 0.065(3) 0.39(1) 0.238(7) -0.128(4) 0.061(3) -0.150(7) C(38) 0.021(3) 0.173(7) 1.16(4) 0.002(4) 0.027(8) -0.22(1) C(39) 0.085(2) 0.027(1) 0.047(2) 0.002(2) 0.026(1) 0.004(1) C(40) 0.087(2) 0.037(2) 0.040(2) 0.002(2) 0.025(2) -0.003(1) C(41) 0.110(3) 0.049(2) 0.033(1) -0.015(2) 0.025(2) 0.005(1) C(42) 0.173(4) 0.032(2) 0.047(2) -0.023(2) 0.034(2) 0.006(2) C(43) 0.123(3) 0.036(2) 0.031(2) -0.009(2) 0.018(2) -0.004(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00038|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5818 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_all 0.0694 _refine_ls_wR_factor_ref 0.0694 _refine_ls_goodness_of_fit_all 1.906 _refine_ls_goodness_of_fit_ref 1.906 _refine_ls_shift/su_max 0.0090 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -0.82 _refine_diff_density_max 0.89 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag CO1 O1 1.910(2) . . yes CO1 O2 1.910(2) . . yes CO1 N1 2.002(2) . . yes CO1 N2 1.996(2) . . yes CO1 N3 2.103(2) . . yes O1 C1 1.308(3) . . yes O2 C22 1.315(3) . . yes N1 C7 1.350(3) . . yes N1 C11 1.363(3) . . yes N2 C12 1.359(3) . . yes N2 C16 1.350(3) . . yes N3 C39 1.323(4) . . yes N3 C43 1.316(4) . . yes C1 C2 1.431(4) . . yes C1 C6 1.415(4) . . yes C2 C3 1.386(4) . . yes C2 C23 1.531(4) . . yes C3 C4 1.386(5) . . yes C3 H1 0.95 . . no C4 C5 1.359(4) . . yes C4 C27 1.535(5) . . yes C5 C6 1.409(4) . . yes C5 H2 0.95 . . no C6 C7 1.473(3) . . yes C7 C8 1.398(4) . . yes C8 C9 1.377(4) . . yes C8 H3 0.95 . . no C9 C10 1.377(4) . . yes C9 H4 0.95 . . no C10 C11 1.376(4) . . yes C10 H5 0.95 . . no C11 C12 1.464(4) . . yes C12 C13 1.379(4) . . yes C13 C14 1.362(4) . . yes C13 H6 0.95 . . no C14 C15 1.368(4) . . yes C14 H7 0.95 . . no C15 C16 1.407(4) . . yes C15 H8 0.95 . . no C16 C17 1.464(4) . . yes C17 C18 1.406(4) . . yes C17 C22 1.423(4) . . yes C18 C19 1.361(5) . . yes C18 H9 0.95 . . no C19 C20 1.388(5) . . yes C19 C35 1.539(4) . . yes C20 C21 1.388(4) . . yes C20 H10 0.95 . . no C21 C22 1.424(4) . . yes C21 C31 1.527(4) . . yes C23 C24 1.524(5) . . yes C23 C25 1.517(4) . . yes C23 C26 1.526(5) . . yes C24 H11 0.95 . . no C24 H12 0.95 . . no C24 H13 0.95 . . no C25 H14 0.95 . . no C25 H15 0.95 . . no C25 H16 0.95 . . no C26 H17 0.95 . . no C26 H18 0.95 . . no C26 H19 0.95 . . no C27 C28 1.429(8) . . yes C27 C29 1.456(8) . . yes C27 C30 1.49(1) . . yes C28 H20 0.95 . . no C28 H21 0.95 . . no C28 H22 0.95 . . no C29 H23 0.95 . . no C29 H24 0.95 . . no C29 H25 0.95 . . no C30 H26 0.95 . . no C30 H27 0.95 . . no C30 H28 0.95 . . no C31 C32 1.528(5) . . yes C31 C33 1.524(5) . . yes C31 C34 1.531(5) . . yes C32 H29 0.95 . . no C32 H30 0.95 . . no C32 H31 0.95 . . no C33 H32 0.95 . . no C33 H33 0.95 . . no C33 H34 0.95 . . no C34 H35 0.95 . . no C34 H36 0.95 . . no C34 H37 0.95 . . no C35 C36 1.292(8) . . yes C35 C37 1.405(8) . . yes C35 C38 1.43(1) . . yes C36 H38 0.95 . . no C36 H39 0.95 . . no C36 H40 0.95 . . no C37 H41 0.95 . . no C37 H42 0.95 . . no C37 H43 0.95 . . no C38 H44 0.95 . . no C38 H45 0.95 . . no C38 H46 0.95 . . no C39 C40 1.363(4) . . yes C39 H47 0.95 . . no C40 C41 1.342(5) . . yes C40 H48 0.95 . . no C41 C42 1.375(5) . . yes C41 H49 0.95 . . no C42 C43 1.373(5) . . yes C42 H50 0.95 . . no C43 H51 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 CO1 O2 92.77(8) . . . yes O1 CO1 N1 90.08(8) . . . yes O1 CO1 N2 160.27(8) . . . yes O1 CO1 N3 99.71(8) . . . yes O2 CO1 N1 161.57(8) . . . yes O2 CO1 N2 90.64(8) . . . yes O2 CO1 N3 97.44(8) . . . yes N1 CO1 N2 80.84(8) . . . yes N1 CO1 N3 100.02(8) . . . yes N2 CO1 N3 99.11(8) . . . yes CO1 O1 C1 127.2(2) . . . yes CO1 O2 C22 125.9(2) . . . yes CO1 N1 C7 125.3(2) . . . yes CO1 N1 C11 114.3(2) . . . yes C7 N1 C11 119.7(2) . . . yes CO1 N2 C12 114.6(2) . . . yes CO1 N2 C16 124.8(2) . . . yes C12 N2 C16 119.8(2) . . . yes CO1 N3 C39 117.7(2) . . . yes CO1 N3 C43 125.9(2) . . . yes C39 N3 C43 116.4(2) . . . yes O1 C1 C2 119.5(2) . . . yes O1 C1 C6 123.0(2) . . . yes C2 C1 C6 117.5(2) . . . yes C1 C2 C3 118.2(3) . . . yes C1 C2 C23 121.7(2) . . . yes C3 C2 C23 120.1(3) . . . yes C2 C3 C4 124.3(3) . . . yes C2 C3 H1 117.9 . . . no C4 C3 H1 117.9 . . . no C3 C4 C5 116.9(3) . . . yes C3 C4 C27 121.4(3) . . . yes C5 C4 C27 121.6(3) . . . yes C4 C5 C6 122.6(3) . . . yes C4 C5 H2 118.7 . . . no C6 C5 H2 118.7 . . . no C1 C6 C5 119.7(2) . . . yes C1 C6 C7 122.3(2) . . . yes C5 C6 C7 117.6(2) . . . yes N1 C7 C6 120.8(2) . . . yes N1 C7 C8 119.6(2) . . . yes C6 C7 C8 119.6(2) . . . yes C7 C8 C9 120.5(2) . . . yes C7 C8 H3 119.7 . . . no C9 C8 H3 119.7 . . . no C8 C9 C10 119.3(2) . . . yes C8 C9 H4 120.3 . . . no C10 C9 H4 120.3 . . . no C9 C10 C11 118.9(2) . . . yes C9 C10 H5 120.6 . . . no C11 C10 H5 120.6 . . . no N1 C11 C10 122.1(2) . . . yes N1 C11 C12 114.5(2) . . . yes C10 C11 C12 123.4(2) . . . yes N2 C12 C11 114.5(2) . . . yes N2 C12 C13 121.9(2) . . . yes C11 C12 C13 123.6(2) . . . yes C12 C13 C14 119.0(3) . . . yes C12 C13 H6 120.5 . . . no C14 C13 H6 120.5 . . . no C13 C14 C15 119.7(3) . . . yes C13 C14 H7 120.1 . . . no C15 C14 H7 120.1 . . . no C14 C15 C16 120.5(3) . . . yes C14 C15 H8 119.8 . . . no C16 C15 H8 119.8 . . . no N2 C16 C15 119.1(3) . . . yes N2 C16 C17 120.9(2) . . . yes C15 C16 C17 119.9(3) . . . yes C16 C17 C18 117.9(3) . . . yes C16 C17 C22 122.7(2) . . . yes C18 C17 C22 119.3(3) . . . yes C17 C18 C19 122.9(3) . . . yes C17 C18 H9 118.6 . . . no C19 C18 H9 118.6 . . . no C18 C19 C20 117.0(3) . . . yes C18 C19 C35 121.5(3) . . . yes C20 C19 C35 121.6(3) . . . yes C19 C20 C21 124.1(3) . . . yes C19 C20 H10 118.0 . . . no C21 C20 H10 118.0 . . . no C20 C21 C22 118.3(3) . . . yes C20 C21 C31 120.7(3) . . . yes C22 C21 C31 121.1(3) . . . yes O2 C22 C17 122.4(2) . . . yes O2 C22 C21 119.7(2) . . . yes C17 C22 C21 117.9(2) . . . yes C2 C23 C24 112.3(3) . . . yes C2 C23 C25 109.2(2) . . . yes C2 C23 C26 111.3(2) . . . yes C24 C23 C25 107.2(3) . . . yes C24 C23 C26 107.3(3) . . . yes C25 C23 C26 109.5(3) . . . yes C23 C24 H11 109.5 . . . no C23 C24 H12 109.5 . . . no C23 C24 H13 109.5 . . . no H11 C24 H12 109.5 . . . no H11 C24 H13 109.5 . . . no H12 C24 H13 109.5 . . . no C23 C25 H14 109.5 . . . no C23 C25 H15 109.5 . . . no C23 C25 H16 109.5 . . . no H14 C25 H15 109.5 . . . no H14 C25 H16 109.5 . . . no H15 C25 H16 109.5 . . . no C23 C26 H17 109.5 . . . no C23 C26 H18 109.5 . . . no C23 C26 H19 109.5 . . . no H17 C26 H18 109.5 . . . no H17 C26 H19 109.5 . . . no H18 C26 H19 109.5 . . . no C4 C27 C28 110.2(4) . . . yes C4 C27 C29 111.9(4) . . . yes C4 C27 C30 110.2(4) . . . yes C28 C27 C29 110.4(7) . . . yes C28 C27 C30 107.6(8) . . . yes C29 C27 C30 106.4(6) . . . yes C27 C28 H20 109.5 . . . no C27 C28 H21 109.5 . . . no C27 C28 H22 109.5 . . . no H20 C28 H21 109.5 . . . no H20 C28 H22 109.5 . . . no H21 C28 H22 109.5 . . . no C27 C29 H23 109.5 . . . no C27 C29 H24 109.5 . . . no C27 C29 H25 109.5 . . . no H23 C29 H24 109.5 . . . no H23 C29 H25 109.5 . . . no H24 C29 H25 109.5 . . . no C27 C30 H26 109.5 . . . no C27 C30 H27 109.5 . . . no C27 C30 H28 109.5 . . . no H26 C30 H27 109.5 . . . no H26 C30 H28 109.5 . . . no H27 C30 H28 109.5 . . . no C21 C31 C32 113.3(3) . . . yes C21 C31 C33 110.4(3) . . . yes C21 C31 C34 109.5(3) . . . yes C32 C31 C33 107.5(3) . . . yes C32 C31 C34 106.7(3) . . . yes C33 C31 C34 109.3(3) . . . yes C31 C32 H29 109.5 . . . no C31 C32 H30 109.5 . . . no C31 C32 H31 109.5 . . . no H29 C32 H30 109.5 . . . no H29 C32 H31 109.5 . . . no H30 C32 H31 109.5 . . . no C31 C33 H32 109.5 . . . no C31 C33 H33 109.5 . . . no C31 C33 H34 109.5 . . . no H32 C33 H33 109.5 . . . no H32 C33 H34 109.5 . . . no H33 C33 H34 109.5 . . . no C31 C34 H35 109.5 . . . no C31 C34 H36 109.5 . . . no C31 C34 H37 109.5 . . . no H35 C34 H36 109.5 . . . no H35 C34 H37 109.5 . . . no H36 C34 H37 109.5 . . . no C19 C35 C36 113.1(4) . . . yes C19 C35 C37 113.0(4) . . . yes C19 C35 C38 109.9(5) . . . yes C36 C35 C37 113.3(9) . . . yes C36 C35 C38 106(1) . . . yes C37 C35 C38 100.1(8) . . . yes C35 C36 H38 109.5 . . . no C35 C36 H39 109.5 . . . no C35 C36 H40 109.5 . . . no H38 C36 H39 109.5 . . . no H38 C36 H40 109.5 . . . no H39 C36 H40 109.5 . . . no C35 C37 H41 109.5 . . . no C35 C37 H42 109.5 . . . no C35 C37 H43 109.5 . . . no H41 C37 H42 109.5 . . . no H41 C37 H43 109.5 . . . no H42 C37 H43 109.5 . . . no C35 C38 H44 109.5 . . . no C35 C38 H45 109.5 . . . no C35 C38 H46 109.5 . . . no H44 C38 H45 109.5 . . . no H44 C38 H46 109.5 . . . no H45 C38 H46 109.5 . . . no N3 C39 C40 124.7(3) . . . yes N3 C39 H47 117.7 . . . no C40 C39 H47 117.7 . . . no C39 C40 C41 118.7(3) . . . yes C39 C40 H48 120.6 . . . no C41 C40 H48 120.6 . . . no C40 C41 C42 118.0(3) . . . yes C40 C41 H49 121.0 . . . no C42 C41 H49 121.0 . . . no C41 C42 C43 119.6(3) . . . yes C41 C42 H50 120.2 . . . no C43 C42 H50 120.2 . . . no N3 C43 C42 122.6(3) . . . yes N3 C43 H51 118.7 . . . no C42 C43 H51 118.7 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag CO1 C10 3.273(2) . 3_756 no O1 C13 3.406(3) . 3_756 no O1 C10 3.492(3) . 3_756 no O2 C9 3.211(3) . 3_756 no O2 C10 3.366(3) . 3_756 no N1 C12 3.538(3) . 3_756 no N1 C11 3.544(3) . 3_756 no N2 C9 3.388(3) . 3_756 no N2 C8 3.564(3) . 3_756 no N2 C10 3.588(3) . 3_756 no C1 C13 3.320(3) . 3_756 no C6 C13 3.427(4) . 3_756 no C6 C14 3.457(4) . 3_756 no C7 C13 3.371(4) . 3_756 no C7 C12 3.525(3) . 3_756 no C8 C16 3.493(4) . 3_756 no C8 C15 3.497(4) . 3_756 no C9 C16 3.495(4) . 3_756 no C9 C26 3.515(5) . 1_545 no C10 C26 3.541(4) . 1_545 no C11 C11 3.473(5) . 3_756 no C25 C25 3.577(6) . 2_756 no C39 C40 3.509(5) . 2_756 no C40 C40 3.458(8) . 2_756 no C41 C42 3.599(7) . 2_756 no C42 C42 3.60(1) . 2_756 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------ # Attachment '- CCDC772955.cif' data_sadabs_772955 _database_code_depnum_ccdc_archive 'CCDC 772955' #TrackingRef '- CCDC772955.cif' #------------------------------------------------------------------------------ _audit_creation_date 2010-04-08 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-Enraf-Nonius kappaCCD' _computing_cell_refinement 'Bruker-Enraf-Nonius kappaCCD' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 18.044(2) _cell_length_b 26.673(9) _cell_length_c 6.846(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3294.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 200.0 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_Int_Tables_number 60 _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2-y,1/2+z '1/2+x,1/2-y, -z' ' -x, +y,1/2-z' ' -x, -y, -z' 1/2+x,1/2+y,1/2-z '1/2-x,1/2+y, +z' ' +x, -y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1184.29 _chemical_formula_analytical ? _chemical_formula_sum 'C76 H92 N4 Ni O4 ' _chemical_formula_moiety 'C76 H92 N4 Ni O4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1328.00 _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_correction_T_min 0.428 _exptl_special_details ; SADABS relative correction factor 0.453 ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 200.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Enraf-Nonius kappaCCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? _diffrn_reflns_number 25920 _reflns_number_total 4790 _reflns_number_gt 2875 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.06947 _diffrn_reflns_av_sigmaI/netI 0.150 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 30.01 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 152 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 184 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ni 0 4 0.285 1.113 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni(1) 1.0000 0.05909(3) 0.7500 0.0278(2) 1.000 ST Uani d ? O(1) 1.0631(2) 0.1095(1) 0.6741(6) 0.0346(8) 1.000 . Uani d ? N(1) 1.0681(2) 0.0077(1) 0.6941(6) 0.0293(9) 1.000 . Uani d ? C(1) 1.1327(2) 0.1075(2) 0.6295(7) 0.033(1) 1.000 . Uani d ? C(2) 1.1710(3) 0.1540(2) 0.5826(8) 0.040(1) 1.000 . Uani d ? C(3) 1.2472(3) 0.1510(2) 0.5368(9) 0.047(1) 1.000 . Uani d ? C(4) 1.2882(3) 0.1070(3) 0.5413(9) 0.052(2) 1.000 . Uani d ? C(5) 1.2519(3) 0.0643(2) 0.5801(8) 0.041(1) 1.000 . Uani d ? C(6) 1.1754(3) 0.0622(2) 0.6183(8) 0.035(1) 1.000 . Uani d ? C(7) 1.1399(2) 0.0125(2) 0.6371(7) 0.030(1) 1.000 . Uani d ? C(8) 1.1797(2) -0.0316(2) 0.5974(8) 0.039(1) 1.000 . Uani d ? C(9) 1.1496(2) -0.0785(2) 0.6124(8) 0.035(1) 1.000 . Uani d ? C(10) 1.0771(3) -0.0825(2) 0.6760(8) 0.036(1) 1.000 . Uani d ? C(11) 1.0382(2) -0.0394(2) 0.7140(6) 0.026(1) 1.000 . Uani d ? C(12) 1.1300(3) 0.2044(2) 0.5816(9) 0.044(1) 1.000 . Uani d ? C(13) 1.1815(4) 0.2483(2) 0.521(1) 0.067(2) 1.000 . Uani d ? C(14) 1.0669(3) 0.2032(2) 0.4347(9) 0.049(2) 1.000 . Uani d ? C(15) 1.1023(4) 0.2156(2) 0.7904(9) 0.055(2) 1.000 . Uani d ? C(16) 1.3715(3) 0.1079(3) 0.488(1) 0.074(2) 1.000 . Uani d ? C(17) 1.3786(5) 0.1181(4) 0.276(2) 0.103(3) 1.000 . Uani d ? C(18) 1.4089(4) 0.1506(4) 0.600(2) 0.109(3) 1.000 . Uani d ? C(19) 1.4100(4) 0.0602(3) 0.535(2) 0.118(4) 1.000 . Uani d ? H(1) 1.2719 0.1811 0.5007 0.056 1.000 . Uiso c ? H(2) 1.2793 0.0339 0.5820 0.049 1.000 . Uiso c ? H(3) 1.2300 -0.0287 0.5582 0.046 1.000 . Uiso c ? H(4) 1.1777 -0.1075 0.5802 0.042 1.000 . Uiso c ? H(5) 1.0546 -0.1144 0.6930 0.043 1.000 . Uiso c ? H(6) 1.2210 0.2510 0.6125 0.080 1.000 . Uiso c ? H(7) 1.2010 0.2421 0.3948 0.080 1.000 . Uiso c ? H(8) 1.1540 0.2786 0.5201 0.080 1.000 . Uiso c ? H(9) 1.0424 0.2347 0.4344 0.059 1.000 . Uiso c ? H(10) 1.0862 0.1966 0.3082 0.059 1.000 . Uiso c ? H(11) 1.0328 0.1777 0.4697 0.059 1.000 . Uiso c ? H(12) 1.1433 0.2167 0.8772 0.066 1.000 . Uiso c ? H(13) 1.0775 0.2470 0.7919 0.066 1.000 . Uiso c ? H(14) 1.0690 0.1900 0.8307 0.066 1.000 . Uiso c ? H(15) 1.4295 0.1188 0.2413 0.124 1.000 . Uiso c ? H(16) 1.3565 0.1496 0.2469 0.124 1.000 . Uiso c ? H(17) 1.3541 0.0925 0.2047 0.124 1.000 . Uiso c ? H(18) 1.4602 0.1515 0.5684 0.131 1.000 . Uiso c ? H(19) 1.3866 0.1816 0.5650 0.131 1.000 . Uiso c ? H(20) 1.4032 0.1453 0.7365 0.131 1.000 . Uiso c ? H(21) 1.4610 0.0629 0.5015 0.141 1.000 . Uiso c ? H(22) 1.4056 0.0535 0.6710 0.141 1.000 . Uiso c ? H(23) 1.3882 0.0336 0.4631 0.141 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0227(3) 0.0283(3) 0.0324(4) 0.0000 -0.0004(4) 0.0000 O(1) 0.021(1) 0.035(2) 0.047(2) -0.004(1) 0.005(1) 0.002(2) N(1) 0.028(2) 0.035(2) 0.025(2) -0.001(2) -0.005(2) 0.002(2) C(1) 0.026(2) 0.047(3) 0.027(3) -0.005(2) -0.007(2) 0.004(2) C(2) 0.034(2) 0.048(3) 0.038(3) -0.012(2) 0.007(2) 0.004(2) C(3) 0.035(2) 0.050(3) 0.056(4) -0.021(2) -0.004(3) 0.008(3) C(4) 0.022(2) 0.076(4) 0.057(4) -0.020(2) 0.008(2) 0.014(3) C(5) 0.019(2) 0.060(3) 0.045(3) 0.002(2) -0.007(2) 0.009(3) C(6) 0.029(2) 0.047(3) 0.029(3) 0.001(2) 0.000(2) 0.003(2) C(7) 0.015(2) 0.047(3) 0.028(3) 0.000(2) 0.000(2) 0.003(2) C(8) 0.020(2) 0.058(3) 0.037(3) 0.009(2) -0.003(2) 0.003(3) C(9) 0.021(2) 0.046(3) 0.039(3) 0.010(2) -0.011(2) -0.002(2) C(10) 0.031(2) 0.030(2) 0.046(3) 0.004(2) -0.003(2) -0.001(2) C(11) 0.022(2) 0.038(2) 0.017(2) 0.001(2) -0.005(2) 0.003(2) C(12) 0.054(3) 0.032(2) 0.047(3) -0.007(2) 0.001(3) 0.000(2) C(13) 0.093(5) 0.038(3) 0.070(4) -0.030(3) 0.003(4) 0.008(3) C(14) 0.063(3) 0.029(2) 0.054(4) 0.008(2) -0.004(3) 0.001(3) C(15) 0.073(4) 0.048(3) 0.043(4) -0.018(3) 0.000(3) -0.005(3) C(16) 0.023(2) 0.104(5) 0.094(6) -0.016(3) -0.003(3) 0.025(5) C(17) 0.051(4) 0.148(9) 0.110(8) -0.008(5) 0.021(4) 0.005(6) C(18) 0.040(3) 0.137(7) 0.149(9) -0.047(4) -0.018(5) 0.016(7) C(19) 0.028(3) 0.109(7) 0.22(1) -0.003(4) 0.028(5) 0.051(7) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00250|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2875 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0955 _refine_ls_wR_factor_all 0.1498 _refine_ls_wR_factor_ref 0.1498 _refine_ls_goodness_of_fit_all 1.954 _refine_ls_goodness_of_fit_ref 1.954 _refine_ls_shift/su_max 0.0147 _refine_ls_shift/su_mean 0.0012 _refine_diff_density_min -0.87 _refine_diff_density_max 0.60 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag NI1 O1 1.837(3) . . yes NI1 O1 1.837(3) . 4_756 yes NI1 N1 1.880(4) . . yes NI1 N1 1.880(4) . 4_756 yes O1 C1 1.294(5) . . yes N1 C7 1.360(5) . . yes N1 C11 1.373(6) . . yes C1 C2 1.456(7) . . yes C1 C6 1.434(7) . . yes C2 C3 1.412(7) . . yes C2 C12 1.534(7) . . yes C3 C4 1.389(9) . . yes C3 H1 0.95 . . no C4 C5 1.339(8) . . yes C4 C16 1.547(7) . . yes C5 C6 1.406(7) . . yes C5 H2 0.95 . . no C6 C7 1.478(7) . . yes C7 C8 1.403(7) . . yes C8 C9 1.368(8) . . yes C8 H3 0.95 . . no C9 C10 1.384(7) . . yes C9 H4 0.95 . . no C10 C11 1.372(7) . . yes C10 H5 0.95 . . no C11 C11 1.465(8) . 4_756 yes C12 C13 1.551(8) . . yes C12 C14 1.519(9) . . yes C12 C15 1.544(9) . . yes C13 H6 0.95 . . no C13 H7 0.95 . . no C13 H8 0.95 . . no C14 H9 0.95 . . no C14 H10 0.95 . . no C14 H11 0.95 . . no C15 H12 0.95 . . no C15 H13 0.95 . . no C15 H14 0.95 . . no C16 C17 1.48(1) . . yes C16 C18 1.53(1) . . yes C16 C19 1.49(1) . . yes C17 H15 0.95 . . no C17 H16 0.95 . . no C17 H17 0.95 . . no C18 H18 0.95 . . no C18 H19 0.95 . . no C18 H20 0.95 . . no C19 H21 0.95 . . no C19 H22 0.95 . . no C19 H23 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 NI1 O1 85.9(2) . . 4_756 yes O1 NI1 N1 94.1(2) . . . yes O1 NI1 N1 175.1(2) . . 4_756 yes O1 NI1 N1 175.1(2) 4_756 . . yes O1 NI1 N1 94.1(2) 4_756 . 4_756 yes N1 NI1 N1 86.4(2) . . 4_756 yes NI1 O1 C1 129.6(3) . . . yes NI1 N1 C7 127.8(3) . . . yes NI1 N1 C11 113.0(3) . . . yes C7 N1 C11 119.2(4) . . . yes O1 C1 C2 118.5(5) . . . yes O1 C1 C6 124.7(5) . . . yes C2 C1 C6 116.9(4) . . . yes C1 C2 C3 117.6(5) . . . yes C1 C2 C12 121.2(4) . . . yes C3 C2 C12 121.2(5) . . . yes C2 C3 C4 124.2(5) . . . yes C2 C3 H1 117.9 . . . no C4 C3 H1 117.9 . . . no C3 C4 C5 117.5(4) . . . yes C3 C4 C16 120.0(6) . . . yes C5 C4 C16 122.4(6) . . . yes C4 C5 C6 123.5(5) . . . yes C4 C5 H2 118.3 . . . no C6 C5 H2 118.3 . . . no C1 C6 C5 120.1(5) . . . yes C1 C6 C7 121.3(4) . . . yes C5 C6 C7 118.5(4) . . . yes N1 C7 C6 121.4(4) . . . yes N1 C7 C8 117.7(4) . . . yes C6 C7 C8 120.9(4) . . . yes C7 C8 C9 123.3(4) . . . yes C7 C8 H3 118.3 . . . no C9 C8 H3 118.3 . . . no C8 C9 C10 117.9(5) . . . yes C8 C9 H4 121.0 . . . no C10 C9 H4 121.0 . . . no C9 C10 C11 118.6(4) . . . yes C9 C10 H5 120.7 . . . no C11 C10 H5 120.7 . . . no N1 C11 C10 123.2(4) . . . yes N1 C11 C11 113.8(2) . . 4_756 yes C10 C11 C11 123.0(3) . . 4_756 yes C2 C12 C13 111.9(5) . . . yes C2 C12 C14 110.3(4) . . . yes C2 C12 C15 108.8(5) . . . yes C13 C12 C14 106.8(5) . . . yes C13 C12 C15 107.0(5) . . . yes C14 C12 C15 112.0(5) . . . yes C12 C13 H6 109.5 . . . no C12 C13 H7 109.5 . . . no C12 C13 H8 109.5 . . . no H6 C13 H7 109.5 . . . no H6 C13 H8 109.5 . . . no H7 C13 H8 109.5 . . . no C12 C14 H9 109.5 . . . no C12 C14 H10 109.5 . . . no C12 C14 H11 109.5 . . . no H9 C14 H10 109.5 . . . no H9 C14 H11 109.5 . . . no H10 C14 H11 109.5 . . . no C12 C15 H12 109.5 . . . no C12 C15 H13 109.5 . . . no C12 C15 H14 109.5 . . . no H12 C15 H13 109.5 . . . no H12 C15 H14 109.5 . . . no H13 C15 H14 109.5 . . . no C4 C16 C17 108.5(6) . . . yes C4 C16 C18 108.8(7) . . . yes C4 C16 C19 113.0(6) . . . yes C17 C16 C18 108.4(8) . . . yes C17 C16 C19 109.2(9) . . . yes C18 C16 C19 108.9(7) . . . yes C16 C17 H15 109.5 . . . no C16 C17 H16 109.5 . . . no C16 C17 H17 109.5 . . . no H15 C17 H16 109.5 . . . no H15 C17 H17 109.5 . . . no H16 C17 H17 109.5 . . . no C16 C18 H18 109.5 . . . no C16 C18 H19 109.5 . . . no C16 C18 H20 109.5 . . . no H18 C18 H19 109.5 . . . no H18 C18 H20 109.5 . . . no H19 C18 H20 109.5 . . . no C16 C19 H21 109.5 . . . no C16 C19 H22 109.5 . . . no C16 C19 H23 109.5 . . . no H21 C19 H22 109.5 . . . no H21 C19 H23 109.5 . . . no H22 C19 H23 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 C9 3.482(6) . 8 no O1 C10 3.495(7) . 8_554 no O1 C10 3.520(7) . 8 no O1 C10 3.558(6) . 5_756 no N1 C7 3.342(6) . 8 no N1 C11 3.436(6) . 8_554 no N1 N1 3.448(6) . 8 no N1 N1 3.448(6) . 8_554 no N1 C8 3.476(6) . 8 no N1 C11 3.493(5) . 5_756 no C1 C10 3.331(7) . 8_554 no C1 C9 3.409(7) . 8 no C6 C8 3.381(8) . 8 no C6 C9 3.442(8) . 8 no C6 C9 3.522(7) . 8_554 no C6 C10 3.551(7) . 8_554 no C7 C8 3.272(7) . 8 no C7 C7 3.487(2) . 8 no C7 C7 3.487(2) . 8_554 no C7 C11 3.504(6) . 8_554 no C14 C14 3.50(1) . 4_755 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #------------------------------------------------------------------------------