# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2060 #=============================================================================== data_global #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author #Name and address of author for correspondence ; ? ; _publ_contact_author_phone ? _publ_contact_author_fax ? _publ_contact_author_email ? _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_letter ; ? #Insert text if wanted ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? #Insert chemical title here ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. #=============================================================================== # 4. TEXT _publ_section_abstract ; ? #Insert appropriate text here if wanted. ; _publ_section_comment ; ? #Insert appropriate text here if wanted. ; _publ_section_experimental ; ? #Insert appropriate text here if wanted. ; _publ_section_references ; Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. Flack, H., (1983) Acta Cryst., A39, 876-881. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Larson, A.C., (1970) p.293, Crystallographic Computing, Munksgaard, Copenhagen. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. Rogers, D., (1981) Acta Cryst., A37, 734-741. ? #Insert any other references here ; _publ_section_figure_captions ; ? #Insert figure captions here if wanted ; _publ_section_acknowledgements ; ? #Insert any acknowledgements here. ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_1-2PhCl #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common '1-2PhCl' _chemical_formula_moiety 'Ni C58 N6 Cl2 O6 H26 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Ni C58 N6 Cl2 O6 H26 ' _chemical_formula_weight 1032.49 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni ? 0.285 1.113 'International Tables Vol. IV Table 2.2B' C ? 0.002 0.002 'International Tables Vol. IV Table 2.2B' N ? 0.004 0.003 'International Tables Vol. IV Table 2.2B' Cl ? 0.132 0.159 'International Tables Vol. IV Table 2.2B' O ? 0.008 0.006 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' #=============================================================================== # 6. CRYSTAL DATA _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,z 1/2-x,1/2-y,-z -x,y,1/2-z x,-y,1/2+z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 21.678(3) _cell_length_b 11.4111(10) _cell_length_c 12.9139(16) _cell_angle_alpha 90.0 _cell_angle_beta 103.401(11) _cell_angle_gamma 90.0 _cell_volume 3107.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 20.00 _cell_measurement_theta_max 25.00 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_method ? _exptl_crystal_F_000 2107.04 _exptl_absorpt_coefficient_mu 0.89 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Omega scan b/P/b ' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 2863 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 24.92 _diffrn_reflns_reduction_process ? _reflns_number_total 2739 _reflns_number_observed 2186 _reflns_observed_criterion 'Inet > 3.0\s(Inet)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type atomblock _refine_ls_weighting_scheme 1/(\s^2^(F)+0.0000F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 2186 _refine_ls_number_parameters 215 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_obs 0.054 _refine_ls_wR_factor_all 0.056 _refine_ls_wR_factor_obs 0.056 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 4.35 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean ? _refine_diff_density_max 1.08 _refine_diff_density_min -1.17 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Ni 0.50000 0.81181(7) 0.75000 0.0198(3) Uij ? S Ni Cl101 0.15618(15) 0.1243(3) 0.2082(4) 0.225(4) Uij ? . Cl N1 0.42463(17) 0.8116(4) 0.9277(3) 0.0358(21) Uij ? . N N11 0.50000 1.0007(4) 0.75000 0.026(3) Uij ? S N N12 0.50000 0.6246(4) 0.75000 0.025(3) Uij ? S N N21 0.59531(15) 0.8002(3) 0.8377(3) 0.0250(18) Uij ? . N O1 0.47796(13) 0.8079(3) 0.90007(23) 0.0330(17) Uij ? . O O2 0.39452(19) 0.9018(3) 0.9181(4) 0.079(3) Uij ? . O O3 0.40643(19) 0.7238(4) 0.9640(4) 0.082(3) Uij ? . O C11 0.48682(21) 1.0630(4) 0.8299(4) 0.0297(24) Uij ? . C C12 0.48590(21) 1.1846(4) 0.8332(4) 0.0319(25) Uij ? . C C13 0.50000 1.2485(5) 0.75000 0.027(3) Uij ? S C C14 0.50000 0.3790(5) 0.75000 0.030(4) Uij ? S C C15 0.51702(22) 0.4418(4) 0.8443(4) 0.033(3) Uij ? . C C16 0.51621(21) 0.5629(4) 0.8405(4) 0.0303(24) Uij ? . C C21 0.61605(19) 0.8566(4) 0.9296(4) 0.0304(24) Uij ? . C C22 0.67570(19) 0.8395(4) 0.9953(4) 0.0318(24) Uij ? . C C23 0.71735(18) 0.7609(4) 0.9658(3) 0.0233(22) Uij ? . C C24 0.69623(19) 0.7039(4) 0.8692(4) 0.0314(24) Uij ? . C C25 0.63570(20) 0.7252(4) 0.8083(4) 0.0297(23) Uij ? . C C101 0.2089(3) 0.0324(7) 0.1637(8) 0.116(7) Uij ? . C C102 0.2688(3) 0.0251(6) 0.2307(6) 0.080(5) Uij ? . C C103 0.3090(3) -0.0462(7) 0.1980(8) 0.113(6) Uij ? . C C104 0.3016(5) -0.1132(7) 0.1085(7) 0.113(7) Uij ? . C C105 0.2394(7) -0.0978(9) 0.0445(8) 0.221(15) Uij ? . C C106 0.1918(5) -0.0252(9) 0.0773(8) 0.165(8) Uij ? . C H11 0.477 1.019 0.892 0.0392 Uiso ? . H H12 0.475 1.227 0.895 0.0409 Uiso ? . H H15 0.529 0.400 0.915 0.0412 Uiso ? . H H16 0.527 0.607 0.910 0.0393 Uiso ? . H H21 0.587 0.915 0.953 0.0386 Uiso ? . H H22 0.689 0.884 1.064 0.0398 Uiso ? . H H24 0.725 0.648 0.843 0.0388 Uiso ? . H H25 0.621 0.682 0.739 0.0382 Uiso ? . H H102 0.283 0.070 0.302 0.0853 Uiso ? . H H103 0.352 -0.052 0.247 0.1147 Uiso ? . H H104 0.333 -0.168 0.085 0.1225 Uiso ? . H H105 0.216 -0.125 -0.033 0.1741 Uiso ? . H H106 0.144 -0.012 0.040 0.1196 Uiso ? . H 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 _atom_site_aniso_type_symbol Ni 0.0140(3) 0.0164(3) 0.0243(4) 0.00000 -0.0049(3) 0.00000 Ni Cl101 0.148(3) 0.198(4) 0.368(6) 0.061(3) 0.141(4) 0.119(4) Cl N1 0.0327(20) 0.0383(22) 0.0320(21) -0.0085(19) -0.0014(17) 0.0031(21) N N11 0.021(3) 0.021(3) 0.030(3) 0.00000 -0.0043(23) 0.00000 N N12 0.024(3) 0.0122(25) 0.034(3) 0.00000 -0.0015(24) 0.00000 N N21 0.0177(17) 0.0237(20) 0.0292(20) 0.0011(15) -0.0038(15) -0.0030(17) N O1 0.0265(16) 0.0420(18) 0.0300(17) 0.0056(15) 0.0054(14) -0.0007(17) O O2 0.055(3) 0.055(3) 0.134(4) 0.0188(22) 0.038(3) -0.004(3) O O3 0.061(3) 0.080(3) 0.098(4) -0.0288(24) 0.006(3) 0.050(3) O C11 0.0332(25) 0.0227(22) 0.033(3) 0.0002(20) 0.0061(21) 0.0024(21) C C12 0.0374(25) 0.0237(21) 0.035(3) 0.0028(22) 0.0091(21) -0.0025(24) C C13 0.029(3) 0.019(3) 0.028(4) 0.00000 -0.003(3) 0.00000 C C14 0.028(3) 0.020(3) 0.041(4) 0.00000 0.007(3) 0.00000 C C15 0.042(3) 0.0225(23) 0.031(3) -0.0006(21) 0.0010(22) 0.0024(21) C C16 0.036(3) 0.0224(23) 0.029(3) -0.0004(20) 0.0003(21) -0.0020(20) C C21 0.0183(22) 0.0316(24) 0.037(3) 0.0044(19) -0.0024(20) -0.0098(22) C C22 0.0199(22) 0.038(3) 0.032(3) 0.0036(20) -0.0053(19) -0.0118(22) C C23 0.0160(21) 0.0234(22) 0.0271(24) -0.0010(18) -0.0020(19) -0.0018(19) C C24 0.0202(21) 0.037(3) 0.0327(25) 0.0088(20) -0.0030(19) -0.0045(23) C C25 0.0231(22) 0.0328(25) 0.0282(25) 0.0035(20) -0.0045(19) -0.0083(21) C C101 0.054(4) 0.103(7) 0.193(10) -0.001(4) 0.036(5) 0.089(7) C C102 0.073(5) 0.083(5) 0.084(5) -0.019(4) 0.017(4) 0.041(4) C C103 0.069(5) 0.105(7) 0.167(9) -0.005(4) 0.033(5) 0.073(6) C C104 0.166(9) 0.067(5) 0.128(8) -0.039(5) 0.078(7) -0.009(5) C C105 0.443(23) 0.105(8) 0.114(9) -0.151(11) 0.059(12) -0.027(7) C C106 0.164(9) 0.148(9) 0.135(8) -0.131(8) -0.065(7) 0.042(7) C #=============================================================================== # 10. MOLECULAR GEOMETRY 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 Ni N21 2.118(3) ? ? ? Ni N21a 2.118(3) ? ? ? Ni O1 2.101(3) ? ? ? Ni O1a 2.101(3) ? ? ? Cl101 C101 1.745(9) ? ? ? N1 O1 1.287(5) ? ? ? N1 O2 1.210(6) ? ? ? N1 O3 1.210(5) ? ? ? N11 C11 1.337(5) ? ? ? N11 C11a 1.337(5) ? ? ? N11 Ct 1.420(5) ? ? ? N12 C16 1.340(5) ? ? ? N12 C16a 1.340(5) ? ? ? N12 Ct2 1.397(4) ? ? ? N21 C21 1.333(6) ? ? ? N21 C25 1.342(5) ? ? ? N21 Ct3 1.397(3) ? ? ? C11 C12 1.389(6) ? ? ? C11 H11 1.015(5) ? ? ? C11 Ct 1.337(4) ? ? ? C11 E1 0.695(4) ? ? ? C11 E2a 0.695(4) ? ? ? C12 C13 1.389(5) ? ? ? C12 H12 1.014(4) ? ? ? C12 Ct 1.364(4) ? ? ? C12 E1 0.694(4) ? ? ? C12 E2a 0.694(4) ? ? ? C13 C12a 1.389(5) ? ? ? C13 C14b 1.489(8) ? ? ? C13 Ct 1.407(6) ? ? ? C14 C13c 1.489(8) ? ? ? C14 C15 1.388(6) ? ? ? C14 C15a 1.388(6) ? ? ? C14 Ct2 1.406(6) ? ? ? C14 E3 1.827(5) ? ? ? C14 E3a 1.827(5) ? ? ? C14 E4 1.827(5) ? ? ? C14 E4a 1.827(5) ? ? ? C15 C16 1.382(6) ? ? ? C15 H15 1.009(5) ? ? ? C15 Ct2 1.373(5) ? ? ? C15 E3 0.691(4) ? ? ? C15 E4a 0.691(4) ? ? ? C16 H16 1.012(4) ? ? ? C16 Ct2 1.334(4) ? ? ? C16 E3 0.691(4) ? ? ? C16 E4a 0.691(4) ? ? ? C21 C22 1.387(6) ? ? ? C21 H21 1.009(4) ? ? ? C21 Ct3 1.334(4) ? ? ? C21 E5 0.693(4) ? ? ? C22 C23 1.387(6) ? ? ? C22 H22 1.006(4) ? ? ? C22 Ct3 1.367(4) ? ? ? C22 E5 0.693(4) ? ? ? C23 C23d 1.506(7) ? ? ? C23 C24 1.388(6) ? ? ? C23 Ct3 1.415(4) ? ? ? C24 C25 1.386(6) ? ? ? C24 H24 1.007(4) ? ? ? C24 Ct3 1.367(4) ? ? ? C24 E6 0.693(4) ? ? ? C25 H25 1.005(4) ? ? ? C25 Ct3 1.338(4) ? ? ? C25 E6 0.693(4) ? ? ? C101 C102 1.385(10) ? ? ? C101 C106 1.274(14) ? ? ? C101 Ct4 1.352(8) ? ? ? C101 E7 1.773(7) ? ? ? C101 F 1.738(10) ? ? ? C102 C103 1.330(11) ? ? ? C102 H102 1.037(8) ? ? ? C102 Ct4 1.377(8) ? ? ? C102 E7 0.665(7) ? ? ? C103 C104 1.363(13) ? ? ? C103 H103 0.999(8) ? ? ? C103 Ct4 1.283(8) ? ? ? C103 E7 0.665(9) ? ? ? C103 E8 0.682(10) ? ? ? C103 E9 1.734(10) ? ? ? C104 C105 1.420(18) ? ? ? C104 H104 1.027(9) ? ? ? C104 Ct4 1.470(9) ? ? ? C104 E8 0.682(9) ? ? ? C104 E9 0.710(10) ? ? ? C105 C106 1.460(20) ? ? ? C105 H105 1.054(11) ? ? ? 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 ? ? ? ? ? ? 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 N21 Ni N21a 172.84(14) ? ? ? ? N21 Ni O1 84.69(12) ? ? ? ? N21 Ni O1a 95.15(12) ? ? ? ? N21a Ni O1 95.15(12) ? ? ? ? N21a Ni O1a 84.69(12) ? ? ? ? O1 Ni O1a 177.55(13) ? ? ? ? O1 N1 O2 119.8(4) ? ? ? ? O1 N1 O3 118.3(4) ? ? ? ? O2 N1 O3 121.9(4) ? ? ? ? C11 N11 C11a 115.9(4) ? ? ? ? C11 N11 Ct 57.9(3) ? ? ? ? C11a N11 Ct 57.9(3) ? ? ? ? C16 N12 C16a 116.6(4) ? ? ? ? C16 N12 Ct2 58.30(25) ? ? ? ? C16a N12 Ct2 58.30(25) ? ? ? ? Ni N21 C21 122.1(3) ? ? ? ? Ni N21 C25 120.5(3) ? ? ? ? Ni N21 Ct3 173.41(24) ? ? ? ? C21 N21 C25 116.9(3) ? ? ? ? C21 N21 Ct3 58.48(22) ? ? ? ? C25 N21 Ct3 58.45(22) ? ? ? ? Ni O1 N1 131.76(25) ? ? ? ? N11 C11 C12 124.1(4) ? ? ? ? N11 C11 H11 118.2(4) ? ? ? ? N11 C11 Ct 64.1(3) ? ? ? ? N11 C11 E1 124.1(5) ? ? ? ? N11 C11 E2a 124.1(5) ? ? ? ? C12 C11 H11 117.7(4) ? ? ? ? C12 C11 Ct 60.0(3) ? ? ? ? C12 C11 E1 0.0 ? ? ? ? C12 C11 E2a 0.0 ? ? ? ? H11 C11 Ct 177.7(4) ? ? ? ? H11 C11 E1 117.7(5) ? ? ? ? H11 C11 E2a 117.7(5) ? ? ? ? Ct C11 E1 60.0(3) ? ? ? ? Ct C11 E2a 60.0(3) ? ? ? ? E1 C11 E2a 0.1 ? ? ? ? C11 C12 C13 119.6(4) ? ? ? ? C11 C12 H12 120.3(4) ? ? ? ? C11 C12 Ct 58.1(3) ? ? ? ? C11 C12 E1 0.0 ? ? ? ? C11 C12 E2a 0.0 ? ? ? ? C13 C12 H12 120.1(4) ? ? ? ? C13 C12 Ct 61.5(3) ? ? ? ? C13 C12 E1 119.6(5) ? ? ? ? C13 C12 E2a 119.6(5) ? ? ? ? H12 C12 Ct 178.3(4) ? ? ? ? H12 C12 E1 120.3(5) ? ? ? ? H12 C12 E2a 120.3(5) ? ? ? ? Ct C12 E1 58.1(3) ? ? ? ? Ct C12 E2a 58.1(3) ? ? ? ? E1 C12 E2a 0.1 ? ? ? ? C12 C13 C12a 116.7(5) ? ? ? ? C12 C13 C14b 121.6(3) ? ? ? ? C12 C13 Ct 58.4(3) ? ? ? ? C12a C13 C14b 121.6(3) ? ? ? ? C12a C13 Ct 58.4(3) ? ? ? ? C14b C13 Ct 180.0 ? ? ? ? C13c C14 C15 121.1(3) ? ? ? ? C13c C14 C15a 121.1(3) ? ? ? ? C13c C14 Ct2 180.0 ? ? ? ? C13c C14 E3 140.42(12) ? ? ? ? C13c C14 E3a 140.42(12) ? ? ? ? C13c C14 E4 140.42(12) ? ? ? ? C13c C14 E4a 140.42(12) ? ? ? ? C15 C14 C15a 117.7(5) ? ? ? ? C15 C14 Ct2 58.9(3) ? ? ? ? C15 C14 E3 19.29(20) ? ? ? ? C15 C14 E3a 98.4(4) ? ? ? ? C15 C14 E4 98.4(4) ? ? ? ? C15 C14 E4a 19.29(20) ? ? ? ? C15a C14 Ct2 58.9(3) ? ? ? ? C15a C14 E3 98.4(4) ? ? ? ? C15a C14 E3a 19.29(20) ? ? ? ? C15a C14 E4 19.29(20) ? ? ? ? C15a C14 E4a 98.4(4) ? ? ? ? Ct2 C14 E3 39.58(12) ? ? ? ? Ct2 C14 E3a 39.58(12) ? ? ? ? Ct2 C14 E4 39.58(12) ? ? ? ? Ct2 C14 E4a 39.58(12) ? ? ? ? E3 C14 E3a 79.15(24) ? ? ? ? E3 C14 E4 79.15(24) ? ? ? ? E3 C14 E4a 0.0 ? ? ? ? E3a C14 E4 0.0 ? ? ? ? E3a C14 E4a 79.15(24) ? ? ? ? E4 C14 E4a 79.15(24) ? ? ? ? C14 C15 C16 119.2(4) ? ? ? ? C14 C15 H15 120.4(4) ? ? ? ? C14 C15 Ct2 61.2(3) ? ? ? ? C14 C15 E3 119.2(5) ? ? ? ? C14 C15 E4a 119.2(5) ? ? ? ? C16 C15 H15 120.5(4) ? ? ? ? C16 C15 Ct2 57.9(3) ? ? ? ? C16 C15 E3 0.0 ? ? ? ? C16 C15 E4a 0.0 ? ? ? ? H15 C15 Ct2 178.4(4) ? ? ? ? H15 C15 E3 120.5(6) ? ? ? ? H15 C15 E4a 120.5(6) ? ? ? ? Ct2 C15 E3 57.9(3) ? ? ? ? Ct2 C15 E4a 57.9(3) ? ? ? ? E3 C15 E4a 0.1 ? ? ? ? N12 C16 C15 123.7(4) ? ? ? ? N12 C16 H16 118.1(4) ? ? ? ? N12 C16 Ct2 63.0(3) ? ? ? ? N12 C16 E3 123.7(5) ? ? ? ? N12 C16 E4a 123.7(5) ? ? ? ? C15 C16 H16 118.2(4) ? ? ? ? C15 C16 Ct2 60.7(3) ? ? ? ? C15 C16 E3 0.0 ? ? ? ? C15 C16 E4a 0.0 ? ? ? ? H16 C16 Ct2 178.0(5) ? ? ? ? H16 C16 E3 118.2(5) ? ? ? ? H16 C16 E4a 118.2(5) ? ? ? ? Ct2 C16 E3 60.7(3) ? ? ? ? Ct2 C16 E4a 60.7(3) ? ? ? ? E3 C16 E4a 0.1 ? ? ? ? N21 C21 C22 123.5(4) ? ? ? ? N21 C21 H21 118.4(4) ? ? ? ? N21 C21 Ct3 63.17(24) ? ? ? ? N21 C21 E5 123.5(5) ? ? ? ? C22 C21 H21 118.1(4) ? ? ? ? C22 C21 Ct3 60.3(3) ? ? ? ? C22 C21 E5 0.0 ? ? ? ? H21 C21 Ct3 178.4(4) ? ? ? ? H21 C21 E5 118.1(5) ? ? ? ? Ct3 C21 E5 60.3(3) ? ? ? ? C21 C22 C23 119.8(4) ? ? ? ? C21 C22 H22 120.4(4) ? ? ? ? C21 C22 Ct3 57.96(25) ? ? ? ? C21 C22 E5 0.0 ? ? ? ? C23 C22 H22 119.9(4) ? ? ? ? C23 C22 Ct3 61.84(25) ? ? ? ? C23 C22 E5 119.8(5) ? ? ? ? H22 C22 Ct3 178.3(4) ? ? ? ? H22 C22 E5 120.4(5) ? ? ? ? Ct3 C22 E5 58.0(3) ? ? ? ? C22 C23 C23d 122.0(4) ? ? ? ? C22 C23 C24 116.8(4) ? ? ? ? C22 C23 Ct3 58.41(23) ? ? ? ? C23d C23 C24 121.3(4) ? ? ? ? C23d C23 Ct3 179.6(4) ? ? ? ? C24 C23 Ct3 58.35(23) ? ? ? ? C23 C24 C25 120.0(4) ? ? ? ? C23 C24 H24 120.1(4) ? ? ? ? C23 C24 Ct3 61.84(25) ? ? ? ? C23 C24 E6 120.0(5) ? ? ? ? C25 C24 H24 119.9(4) ? ? ? ? C25 C24 Ct3 58.16(24) ? ? ? ? C25 C24 E6 0.0 ? ? ? ? H24 C24 Ct3 177.6(4) ? ? ? ? H24 C24 E6 119.9(5) ? ? ? ? Ct3 C24 E6 58.2(3) ? ? ? ? N21 C25 C24 123.0(4) ? ? ? ? N21 C25 H25 118.4(4) ? ? ? ? N21 C25 Ct3 62.84(24) ? ? ? ? N21 C25 E6 123.0(5) ? ? ? ? C24 C25 H25 118.6(4) ? ? ? ? C24 C25 Ct3 60.2(3) ? ? ? ? C24 C25 E6 0.0 ? ? ? ? H25 C25 Ct3 178.8(4) ? ? ? ? H25 C25 E6 118.6(5) ? ? ? ? Ct3 C25 E6 60.2(3) ? ? ? ? Cl101 C101 C102 114.9(8) ? ? ? ? Cl101 C101 C106 121.2(7) ? ? ? ? Cl101 C101 Ct4 175.2(7) ? ? ? ? Cl101 C101 E7 134.7(6) ? ? ? ? Cl101 C101 F 143.1(5) ? ? ? ? C102 C101 C106 123.8(9) ? ? ? ? C102 C101 Ct4 60.4(4) ? ? ? ? C102 C101 E7 19.8(3) ? ? ? ? C102 C101 F 102.0(6) ? ? ? ? C106 C101 Ct4 63.5(7) ? ? ? ? C106 C101 E7 104.0(7) ? ? ? ? C106 C101 F 21.8(5) ? ? ? ? Ct4 C101 E7 40.54(19) ? ? ? ? Ct4 C101 F 41.7(3) ? ? ? ? E7 C101 F 82.2(4) ? ? ? ? C101 C102 C103 115.2(8) ? ? ? ? C101 C102 H102 124.5(7) ? ? ? ? C101 C102 Ct4 58.6(5) ? ? ? ? C101 C102 E7 115.2(9) ? ? ? ? C103 C102 H102 120.3(7) ? ? ? ? C103 C102 Ct4 56.6(5) ? ? ? ? C103 C102 E7 0.02(12) ? ? ? ? H102 C102 Ct4 176.9(7) ? ? ? ? H102 C102 E7 120.3(8) ? ? ? ? Ct4 C102 E7 56.6(6) ? ? ? ? C102 C103 C104 130.9(8) ? ? ? ? C102 C103 H103 114.9(9) ? ? ? ? C102 C103 Ct4 63.6(5) ? ? ? ? C102 C103 E7 0.0 ? ? ? ? C102 C103 E8 130.9(9) ? ? ? ? C102 C103 E9 108.2(6) ? ? ? ? C104 C103 H103 114.2(8) ? ? ? ? C104 C103 Ct4 67.4(6) ? ? ? ? C104 C103 E7 130.9(11) ? ? ? ? C104 C103 E8 0.02(14) ? ? ? ? C104 C103 E9 22.7(4) ? ? ? ? H103 C103 Ct4 178.3(9) ? ? ? ? H103 C103 E7 114.9(12) ? ? ? ? H103 C103 E8 114.2(9) ? ? ? ? H103 C103 E9 136.9(8) ? ? ? ? Ct4 C103 E7 63.6(6) ? ? ? ? Ct4 C103 E8 67.4(7) ? ? ? ? Ct4 C103 E9 44.7(3) ? ? ? ? E7 C103 E8 130.9(12) ? ? ? ? E7 C103 E9 108.2(8) ? ? ? ? E8 C103 E9 22.7(4) ? ? ? ? C103 C104 C105 109.5(8) ? ? ? ? C103 C104 H104 129.8(10) ? ? ? ? C103 C104 Ct4 53.7(4) ? ? ? ? C103 C104 E8 0.02(14) ? ? ? ? C103 C104 E9 109.5(9) ? ? ? ? C105 C104 H104 120.7(9) ? ? ? ? C105 C104 Ct4 55.8(6) ? ? ? ? C105 C104 E8 109.5(11) ? ? ? ? C105 C104 E9 0.02(3) ? ? ? ? H104 C104 Ct4 176.4(9) ? ? ? ? H104 C104 E8 129.8(13) ? ? ? ? H104 C104 E9 120.7(10) ? ? ? ? Ct4 C104 E8 53.7(6) ? ? ? ? Ct4 C104 E9 55.8(6) ? ? ? ? E8 C104 E9 109.5(12) ? ? ? ? C104 C105 C106 122.7(8) ? ? ? ? C104 C105 H105 134.1(13) ? ? ? ? C104 C105 Ct4 64.0(6) ? ? ? ? C104 C105 E8 21.3(4) ? ? ? ? C104 C105 E9 0.02(3) ? ? ? ? C104 C105 F 122.7(11) ? ? ? ? C106 C105 H105 103.0(12) ? ? ? ? C106 C105 Ct4 58.8(6) ? ? ? ? C106 C105 E8 101.4(6) ? ? ? ? C106 C105 E9 122.7(11) ? ? ? ? C106 C105 F 0.02(9) ? ? ? ? H105 C105 Ct4 161.0(14) ? ? ? ? H105 C105 E8 155.1(13) ? ? ? ? H105 C105 E9 134.1(17) ? ? ? ? H105 C105 F 103.0(15) ? ? ? ? Ct4 C105 E8 42.7(4) ? ? ? ? Ct4 C105 E9 64.0(7) ? ? ? ? Ct4 C105 F 58.8(7) ? ? ? ? E8 C105 E9 21.3(5) ? ? ? ? E8 C105 F 101.4(9) ? ? ? ? E9 C105 F 122.7(14) ? ? ? ? C101 C106 C105 117.7(8) ? ? ? ? C101 C106 H106 112.7(11) ? ? ? ? C101 C106 Ct4 61.0(5) ? ? ? ? C101 C106 F 117.7(9) ? ? ? ? C105 C106 H106 129.6(10) ? ? ? ? C105 C106 Ct4 56.7(6) ? ? ? ? C105 C106 F 0.02(9) ? ? ? ? H106 C106 Ct4 173.6(12) ? ? ? ? H106 C106 F 129.6(11) ? ? ? ? Ct4 C106 F 56.7(6) ? ? ? ? C11 H11 E1 24.68(24) ? ? ? ? C11 H11 E2a 24.67(24) ? ? ? ? E1 H11 E2a 0.0 ? ? ? ? C12 H12 E1 23.7(3) ? ? ? ? C12 H12 E2a 23.7(3) ? ? ? ? E1 H12 E2a 0.0 ? ? ? ? C15 H15 E3 23.7(3) ? ? ? ? C15 H15 E4a 23.7(3) ? ? ? ? E3 H15 E4a 0.0 ? ? ? ? C16 H16 E3 24.47(25) ? ? ? ? C16 H16 E4a 24.47(25) ? ? ? ? E3 H16 E4a 0.0 ? ? ? ? C21 H21 E5 24.60(24) ? ? ? ? C22 H22 E5 23.80(24) ? ? ? ? C24 H24 E6 23.95(24) ? ? ? ? C25 H25 E6 24.49(24) ? ? ? ? C102 H102 E7 22.7(4) ? ? ? ? C103 H103 E7 25.2(6) ? ? ? ? C103 H103 E8 26.0(6) ? ? ? ? E7 H103 E8 51.209(8) ? ? ? ? C104 H104 E8 19.7(5) ? ? ? ? C104 H104 E9 23.7(5) ? ? ? ? E8 H104 E9 43.406(6) ? ? ? ? C105 H105 E9 18.2(8) ? ? ? ? C105 H105 F 30.3(8) ? ? ? ? E9 H105 F 48.443(7) ? ? ? ? C106 H106 F 20.5(7) ? ? ? ? N11 Ct C11 57.94(19) ? ? ? ? N11 Ct C11a 57.94(19) ? ? ? ? N11 Ct C12 119.84(19) ? ? ? ? N11 Ct C12a 119.84(19) ? ? ? ? N11 Ct C13 180.0 ? ? ? ? N11 Ct E1 89.2 ? ? ? ? N11 Ct E1a 89.2 ? ? ? ? N11 Ct E2 89.2 ? ? ? ? N11 Ct E2a 89.2 ? ? ? ? C11 Ct C11a 115.9(3) ? ? ? ? C11 Ct C12 61.9(3) ? ? ? ? C11 Ct C12a 177.8(3) ? ? ? ? C11 Ct C13 122.06(19) ? ? ? ? C11 Ct E1 31.28(19) ? ? ? ? C11 Ct E1a 147.17(19) ? ? ? ? C11 Ct E2 147.17(19) ? ? ? ? C11 Ct E2a 31.28(19) ? ? ? ? C11a Ct C12 177.8(3) ? ? ? ? C11a Ct C12a 61.9(3) ? ? ? ? C11a Ct C13 122.06(19) ? ? ? ? C11a Ct E1 147.17(19) ? ? ? ? C11a Ct E1a 31.28(19) ? ? ? ? C11a Ct E2 31.28(19) ? ? ? ? C11a Ct E2a 147.17(19) ? ? ? ? C12 Ct C12a 120.3(3) ? ? ? ? C12 Ct C13 60.16(19) ? ? ? ? C12 Ct E1 30.61(19) ? ? ? ? C12 Ct E1a 150.94(19) ? ? ? ? C12 Ct E2 150.94(19) ? ? ? ? C12 Ct E2a 30.61(19) ? ? ? ? C12a Ct C13 60.16(19) ? ? ? ? C12a Ct E1 150.94(19) ? ? ? ? C12a Ct E1a 30.61(19) ? ? ? ? C12a Ct E2 30.61(19) ? ? ? ? C12a Ct E2a 150.94(19) ? ? ? ? C13 Ct E1 90.8 ? ? ? ? C13 Ct E1a 90.8 ? ? ? ? C13 Ct E2 90.8 ? ? ? ? C13 Ct E2a 90.8 ? ? ? ? E1 Ct E1a 178.5 ? ? ? ? E1 Ct E2 178.5 ? ? ? ? E1 Ct E2a 0.0 ? ? ? ? E1a Ct E2 0.0 ? ? ? ? E1a Ct E2a 178.5 ? ? ? ? E2 Ct E2a 178.5 ? ? ? ? N12 Ct2 C14 180.0 ? ? ? ? N12 Ct2 C15 120.10(19) ? ? ? ? N12 Ct2 C15a 120.10(19) ? ? ? ? N12 Ct2 C16 58.71(19) ? ? ? ? N12 Ct2 C16a 58.71(19) ? ? ? ? N12 Ct2 E3 89.9 ? ? ? ? N12 Ct2 E3a 89.9 ? ? ? ? N12 Ct2 E4 89.9 ? ? ? ? N12 Ct2 E4a 89.9 ? ? ? ? C14 Ct2 C15 59.90(19) ? ? ? ? C14 Ct2 C15a 59.90(19) ? ? ? ? C14 Ct2 C16 121.29(19) ? ? ? ? C14 Ct2 C16a 121.29(19) ? ? ? ? C14 Ct2 E3 90.1 ? ? ? ? C14 Ct2 E3a 90.1 ? ? ? ? C14 Ct2 E4 90.1 ? ? ? ? C14 Ct2 E4a 90.1 ? ? ? ? C15 Ct2 C15a 119.8(3) ? ? ? ? C15 Ct2 C16 61.4(3) ? ? ? ? C15 Ct2 C16a 178.8(3) ? ? ? ? C15 Ct2 E3 30.21(19) ? ? ? ? C15 Ct2 E3a 150.02(19) ? ? ? ? C15 Ct2 E4 150.02(19) ? ? ? ? C15 Ct2 E4a 30.21(19) ? ? ? ? C15a Ct2 C16 178.8(3) ? ? ? ? C15a Ct2 C16a 61.4(3) ? ? ? ? C15a Ct2 E3 150.02(19) ? ? ? ? C15a Ct2 E3a 30.21(19) ? ? ? ? C15a Ct2 E4 30.21(19) ? ? ? ? C15a Ct2 E4a 150.02(19) ? ? ? ? C16 Ct2 C16a 117.4(3) ? ? ? ? C16 Ct2 E3 31.17(19) ? ? ? ? C16 Ct2 E3a 148.60(19) ? ? ? ? C16 Ct2 E4 148.60(19) ? ? ? ? C16 Ct2 E4a 31.17(19) ? ? ? ? C16a Ct2 E3 148.60(19) ? ? ? ? C16a Ct2 E3a 31.17(19) ? ? ? ? C16a Ct2 E4 31.17(19) ? ? ? ? C16a Ct2 E4a 148.60(19) ? ? ? ? E3 Ct2 E3a 179.8 ? ? ? ? E3 Ct2 E4 179.8 ? ? ? ? E3 Ct2 E4a 0.0 ? ? ? ? E3a Ct2 E4 0.0 ? ? ? ? E3a Ct2 E4a 179.8 ? ? ? ? E4 Ct2 E4a 179.8 ? ? ? ? N21 Ct3 C21 58.35(23) ? ? ? ? N21 Ct3 C22 120.09(22) ? ? ? ? N21 Ct3 C23 179.42(23) ? ? ? ? N21 Ct3 C24 120.35(22) ? ? ? ? N21 Ct3 C25 58.71(23) ? ? ? ? N21 Ct3 E5 89.64(14) ? ? ? ? N21 Ct3 E6 89.90(14) ? ? ? ? C21 Ct3 C22 61.7(3) ? ? ? ? C21 Ct3 C23 121.5(3) ? ? ? ? C21 Ct3 C24 178.6(3) ? ? ? ? C21 Ct3 C25 117.1(3) ? ? ? ? C21 Ct3 E5 31.29(19) ? ? ? ? C21 Ct3 E6 148.24(19) ? ? ? ? C22 Ct3 C23 59.75(25) ? ? ? ? C22 Ct3 C24 119.56(25) ? ? ? ? C22 Ct3 C25 178.8(3) ? ? ? ? C22 Ct3 E5 30.44(17) ? ? ? ? C22 Ct3 E6 150.02(17) ? ? ? ? C23 Ct3 C24 59.81(25) ? ? ? ? C23 Ct3 C25 121.5(3) ? ? ? ? C23 Ct3 E5 90.20(17) ? ? ? ? C23 Ct3 E6 90.27(17) ? ? ? ? C24 Ct3 C25 61.6(3) ? ? ? ? C24 Ct3 E5 150.00(17) ? ? ? ? C24 Ct3 E6 30.46(17) ? ? ? ? C25 Ct3 E5 148.35(18) ? ? ? ? C25 Ct3 E6 31.19(18) ? ? ? ? E5 Ct3 E6 179.4 ? ? ? ? C101 Ct4 C102 61.0(5) ? ? ? ? C101 Ct4 C103 120.9(6) ? ? ? ? C101 Ct4 C104 179.8(5) ? ? ? ? C101 Ct4 C105 120.0(8) ? ? ? ? C101 Ct4 C106 55.5(6) ? ? ? ? C101 Ct4 E7 89.8(4) ? ? ? ? C101 Ct4 E8 152.5(4) ? ? ? ? C101 Ct4 E9 151.5(4) ? ? ? ? C101 Ct4 F 87.3(4) ? ? ? ? C102 Ct4 C103 59.9(5) ? ? ? ? C102 Ct4 C104 118.8(5) ? ? ? ? C102 Ct4 C105 178.5(6) ? ? ? ? C102 Ct4 C106 116.5(6) ? ? ? ? C102 Ct4 E7 28.8(3) ? ? ? ? C102 Ct4 E8 91.5(3) ? ? ? ? C102 Ct4 E9 147.5(3) ? ? ? ? C102 Ct4 F 148.3(3) ? ? ? ? C103 Ct4 C104 58.9(6) ? ? ? ? C103 Ct4 C105 119.1(8) ? ? ? ? C103 Ct4 C106 176.2(7) ? ? ? ? C103 Ct4 E7 31.1(4) ? ? ? ? C103 Ct4 E8 31.6(4) ? ? ? ? C103 Ct4 E9 87.6(4) ? ? ? ? C103 Ct4 F 151.8(4) ? ? ? ? C104 Ct4 C105 60.2(8) ? ? ? ? C104 Ct4 C106 124.7(6) ? ? ? ? C104 Ct4 E7 90.0(4) ? ? ? ? C104 Ct4 E8 27.3(4) ? ? ? ? C104 Ct4 E9 28.7(4) ? ? ? ? C104 Ct4 F 92.9(4) ? ? ? ? C105 Ct4 C106 64.5(8) ? ? ? ? C105 Ct4 E7 150.2(7) ? ? ? ? C105 Ct4 E8 87.5(7) ? ? ? ? C105 Ct4 E9 31.5(7) ? ? ? ? C105 Ct4 F 32.7(7) ? ? ? ? C106 Ct4 E7 145.3(5) ? ? ? ? C106 Ct4 E8 151.9(5) ? ? ? ? C106 Ct4 E9 96.0(5) ? ? ? ? C106 Ct4 F 31.8(5) ? ? ? ? E7 Ct4 E8 62.747(9) ? ? ? ? E7 Ct4 E9 118.736(8) ? ? ? ? E7 Ct4 F 177.1 ? ? ? ? E8 Ct4 E9 55.994(8) ? ? ? ? E8 Ct4 F 120.149(9) ? ? ? ? E9 Ct4 F 64.160(8) ? ? ? ? C11 E1 C12 180.0 ? ? ? ? C11 E1 H11 37.6(4) ? ? ? ? C11 E1 H12 144.0(4) ? ? ? ? C11 E1 Ct 88.7(4) ? ? ? ? C12 E1 H11 142.4(4) ? ? ? ? C12 E1 H12 36.0(4) ? ? ? ? C12 E1 Ct 91.3(4) ? ? ? ? H11 E1 H12 106.459(8) ? ? ? ? H11 E1 Ct 126.3 ? ? ? ? H12 E1 Ct 127.2 ? ? ? ? C11a E2 C12a 180.0 ? ? ? ? C11a E2 H11a 37.6(4) ? ? ? ? C11a E2 H12a 144.0(4) ? ? ? ? C11a E2 Ct 88.7(4) ? ? ? ? C12a E2 H11a 142.4(4) ? ? ? ? C12a E2 H12a 35.9(4) ? ? ? ? C12a E2 Ct 91.3(4) ? ? ? ? H11a E2 H12a 106.451(8) ? ? ? ? H11a E2 Ct 126.3 ? ? ? ? H12a E2 Ct 127.2 ? ? ? ? C14 E3 C15 41.5(4) ? ? ? ? C14 E3 C16 138.5(4) ? ? ? ? C14 E3 H15 77.41(12) ? ? ? ? C14 E3 H16 175.59(11) ? ? ? ? C14 E3 Ct2 50.31(12) ? ? ? ? C15 E3 C16 180.0 ? ? ? ? C15 E3 H15 35.9(4) ? ? ? ? C15 E3 H16 142.7(4) ? ? ? ? C15 E3 Ct2 91.9(4) ? ? ? ? C16 E3 H15 144.1(4) ? ? ? ? C16 E3 H16 37.3(4) ? ? ? ? C16 E3 Ct2 88.1(4) ? ? ? ? H15 E3 H16 106.803(9) ? ? ? ? H15 E3 Ct2 127.7 ? ? ? ? H16 E3 Ct2 125.5 ? ? ? ? C14 E4 C15a 41.5(4) ? ? ? ? C14 E4 C16a 138.5(4) ? ? ? ? C14 E4 H15a 77.41(12) ? ? ? ? C14 E4 H16a 175.60(11) ? ? ? ? C14 E4 Ct2 50.31(12) ? ? ? ? C15a E4 C16a 180.0 ? ? ? ? C15a E4 H15a 35.9(4) ? ? ? ? C15a E4 H16a 142.7(4) ? ? ? ? C15a E4 Ct2 91.9(4) ? ? ? ? C16a E4 H15a 144.1(4) ? ? ? ? C16a E4 H16a 37.3(4) ? ? ? ? C16a E4 Ct2 88.1(4) ? ? ? ? H15a E4 H16a 106.803(9) ? ? ? ? H15a E4 Ct2 127.7 ? ? ? ? H16a E4 Ct2 125.5 ? ? ? ? C21 E5 C22 180.0 ? ? ? ? C21 E5 H21 37.3(4) ? ? ? ? C21 E5 H22 144.2(4) ? ? ? ? C21 E5 Ct3 88.4(4) ? ? ? ? C22 E5 H21 142.7(4) ? ? ? ? C22 E5 H22 35.8(4) ? ? ? ? C22 E5 Ct3 91.6(4) ? ? ? ? H21 E5 H22 106.887(9) ? ? ? ? H21 E5 Ct3 125.672(8) ? ? ? ? H22 E5 Ct3 127.441(7) ? ? ? ? C24 E6 C25 180.0 ? ? ? ? C24 E6 H24 36.1(4) ? ? ? ? C24 E6 H25 143.1(4) ? ? ? ? C24 E6 Ct3 91.4(4) ? ? ? ? C25 E6 H24 143.9(4) ? ? ? ? C25 E6 H25 36.9(4) ? ? ? ? C25 E6 Ct3 88.6(4) ? ? ? ? H24 E6 H25 106.927(10) ? ? ? ? H24 E6 Ct3 127.512(8) ? ? ? ? H25 E6 Ct3 125.553(7) ? ? ? ? C101 E7 C102 45.0(7) ? ? ? ? C101 E7 C103 135.0(9) ? ? ? ? C101 E7 H102 82.0(3) ? ? ? ? C101 E7 H103 174.8(3) ? ? ? ? C101 E7 Ct4 49.7(3) ? ? ? ? C101 E7 E8 110.2(3) ? ? ? ? C102 E7 C103 180.0 ? ? ? ? C102 E7 H102 37.0(6) ? ? ? ? C102 E7 H103 140.2(6) ? ? ? ? C102 E7 Ct4 94.6(6) ? ? ? ? C102 E7 E8 155.1(6) ? ? ? ? C103 E7 H102 143.0(8) ? ? ? ? C103 E7 H103 39.8(8) ? ? ? ? C103 E7 Ct4 85.3(8) ? ? ? ? C103 E7 E8 24.9(8) ? ? ? ? H102 E7 H103 103.175(9) ? ? ? ? H102 E7 Ct4 131.639(7) ? ? ? ? H102 E7 E8 167.9 ? ? ? ? H103 E7 Ct4 125.179(8) ? ? ? ? H103 E7 E8 64.694(8) ? ? ? ? Ct4 E7 E8 60.490(8) ? ? ? ? C103 E8 C104 180.0(3) ? ? ? ? C103 E8 C105 130.8(8) ? ? ? ? C103 E8 H103 39.9(6) ? ? ? ? C103 E8 H104 149.5(6) ? ? ? ? C103 E8 Ct4 81.0(6) ? ? ? ? C103 E8 E7 24.2(6) ? ? ? ? C103 E8 E9 143.9(6) ? ? ? ? C104 E8 C105 49.2(9) ? ? ? ? C104 E8 H103 140.1(8) ? ? ? ? C104 E8 H104 30.5(8) ? ? ? ? C104 E8 Ct4 99.0(8) ? ? ? ? C104 E8 E7 155.8(8) ? ? ? ? C104 E8 E9 36.1(8) ? ? ? ? C105 E8 H103 170.7(4) ? ? ? ? C105 E8 H104 79.7(4) ? ? ? ? C105 E8 Ct4 49.8(4) ? ? ? ? C105 E8 E7 106.6(4) ? ? ? ? C105 E8 E9 13.1(4) ? ? ? ? H103 E8 H104 109.631(9) ? ? ? ? H103 E8 Ct4 120.856(9) ? ? ? ? H103 E8 E7 64.097(8) ? ? ? ? H103 E8 E9 176.2 ? ? ? ? H104 E8 Ct4 129.508(7) ? ? ? ? H104 E8 E7 173.7 ? ? ? ? H104 E8 E9 66.567(8) ? ? ? ? Ct4 E8 E7 56.763(8) ? ? ? ? Ct4 E8 E9 62.947(9) ? ? ? ? E7 E8 E9 119.705(8) ? ? ? ? C103 E9 C104 47.8(7) ? ? ? ? C103 E9 C105 132.2(9) ? ? ? ? C103 E9 H104 83.4(3) ? ? ? ? C103 E9 H105 159.3(3) ? ? ? ? C103 E9 Ct4 47.7(3) ? ? ? ? C103 E9 E8 13.4(3) ? ? ? ? C103 E9 F 103.1(3) ? ? ? ? C104 E9 C105 179.97(8) ? ? ? ? C104 E9 H104 35.6(7) ? ? ? ? C104 E9 H105 152.3(7) ? ? ? ? C104 E9 Ct4 95.5(7) ? ? ? ? C104 E9 E8 34.4(7) ? ? ? ? C104 E9 F 150.9(7) ? ? ? ? C105 E9 H104 144.4(9) ? ? ? ? C105 E9 H105 27.7(9) ? ? ? ? C105 E9 Ct4 84.5(9) ? ? ? ? C105 E9 E8 145.6(9) ? ? ? ? C105 E9 F 29.1(9) ? ? ? ? H104 E9 H105 116.906(9) ? ? ? ? H104 E9 Ct4 131.081(7) ? ? ? ? H104 E9 E8 70.027(9) ? ? ? ? H104 E9 F 173.3 ? ? ? ? H105 E9 Ct4 111.946(8) ? ? ? ? H105 E9 E8 172.1 ? ? ? ? H105 E9 F 56.676(9) ? ? ? ? Ct4 E9 E8 61.059(8) ? ? ? ? Ct4 E9 F 55.462(8) ? ? ? ? E8 E9 F 116.517(9) ? ? ? ? C101 F C105 139.5(9) ? ? ? ? C101 F C106 40.5(7) ? ? ? ? C101 F H105 171.49(24) ? ? ? ? C101 F H106 70.44(24) ? ? ? ? C101 F Ct4 51.00(24) ? ? ? ? C101 F E9 111.38(24) ? ? ? ? C105 F C106 179.95(14) ? ? ? ? C105 F H105 46.7(9) ? ? ? ? C105 F H106 150.1(9) ? ? ? ? C105 F Ct4 88.5(9) ? ? ? ? C105 F E9 28.2(9) ? ? ? ? C106 F H105 133.3(6) ? ? ? ? C106 F H106 30.0(6) ? ? ? ? C106 F Ct4 91.5(6) ? ? ? ? C106 F E9 151.8(6) ? ? ? ? H105 F H106 103.515(10) ? ? ? ? H105 F Ct4 134.952(7) ? ? ? ? H105 F E9 74.881(10) ? ? ? ? H106 F Ct4 121.391(9) ? ? ? ? H106 F E9 177.3 ? ? ? ? Ct4 F E9 60.378(9) ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? #=============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #=============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ data_1-2PhCl2 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common '1-2PhCl2' _chemical_formula_moiety 'Ni Cl4 O6 N6 C32 H24 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Ni Cl4 O6 N6 C32 H24 ' _chemical_formula_weight 789.09 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni ? 0.285 1.113 'International Tables Vol. IV Table 2.2B' Cl ? 0.132 0.159 'International Tables Vol. IV Table 2.2B' O ? 0.008 0.006 'International Tables Vol. IV Table 2.2B' N ? 0.004 0.003 'International Tables Vol. IV Table 2.2B' C ? 0.002 0.002 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' #=============================================================================== # 6. CRYSTAL DATA _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,z 1/2-x,1/2-y,-z -x,y,1/2-z x,-y,1/2+z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 21.5155(17) _cell_length_b 11.4059(9) _cell_length_c 13.3137(10) _cell_angle_alpha 90.0 _cell_angle_beta 103.2940(*) _cell_angle_gamma 90.0 _cell_volume 3179.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 20.00 _cell_measurement_theta_max 25.00 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method ? _exptl_crystal_F_000 1611.90 _exptl_absorpt_coefficient_mu 1.01 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Omega scan b/P/b ' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 4298 _diffrn_reflns_av_R_equivalents 0.088 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 20.77 _diffrn_reflns_reduction_process ? _reflns_number_total 1670 _reflns_number_observed 1336 _reflns_observed_criterion 'Inet > 3.0\s(Inet)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 1/(\s^2^(F)+0.0001F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 1336 _refine_ls_number_parameters 224 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.098 _refine_ls_R_factor_obs 0.098 _refine_ls_wR_factor_all 0.128 _refine_ls_wR_factor_obs 0.128 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 6.61 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean ? _refine_diff_density_max 0.81 _refine_diff_density_min -0.80 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Ni 0.00000 0.31022(22) 0.75000 0.0186(15) Uij ? S Ni Cl1 0.62508(22) 0.4379(4) 0.5946(4) 0.063(3) Uij ? . Cl Cl2 0.7286(3) 0.3682(6) 0.7928(4) 0.098(5) Uij ? . Cl O1 -0.0213(5) 0.3066(9) 0.8970(7) 0.030(6) Uij ? . O O2 -0.0990(5) 0.4032(12) 0.9352(9) 0.051(8) Uij ? . O O3 -0.0952(5) 0.2190(10) 0.9549(9) 0.050(8) Uij ? . O N1 -0.0727(6) 0.3092(12) 0.9301(9) 0.027(8) Uij ? . N N11 0.00000 -0.4970(14) 0.75000 0.025(11) Uij ? S N N12 0.00000 0.1242(14) 0.75000 0.028(11) Uij ? S N N21 0.0955(5) 0.2987(10) 0.8364(8) 0.019(7) Uij ? . N C11 -0.0114(6) -0.4347(13) 0.8274(10) 0.022(9) Uij ? . C C12 -0.0132(6) -0.3180(13) 0.8333(10) 0.023(9) Uij ? . C C13 0.00000 -0.2528(19) 0.75000 0.032(14) Uij ? S C C14 0.00000 -0.1220(18) 0.75000 0.026(14) Uij ? S C C15 0.0197(6) -0.0577(12) 0.8395(10) 0.022(8) Uij ? . C C16 0.0180(6) 0.0624(13) 0.8381(11) 0.024(9) Uij ? . C C21 0.1152(6) 0.3567(12) 0.9262(12) 0.026(9) Uij ? . C C22 0.1753(6) 0.3403(11) 0.9930(11) 0.023(8) Uij ? . C C23 0.2167(6) 0.2614(12) 0.9656(11) 0.019(8) Uij ? . C C24 0.1984(6) 0.2042(12) 0.8701(11) 0.026(9) Uij ? . C C25 0.1375(7) 0.2262(13) 0.8121(10) 0.024(9) Uij ? . C C111 0.7035(7) 0.4977(15) 0.6198(15) 0.042(11) Uij ? . C C112 0.7463(11) 0.4681(16) 0.7081(14) 0.054(13) Uij ? . C C113 0.8080(10) 0.5160(19) 0.7279(15) 0.060(14) Uij ? . C C114 0.8227(10) 0.5902(21) 0.6518(20) 0.084(17) Uij ? . C C115 0.7788(10) 0.6170(16) 0.5656(16) 0.059(13) Uij ? . C C116 0.7185(8) 0.5734(15) 0.5479(13) 0.043(11) Uij ? . C H11 -0.020 -0.481 0.888 0.0329 Uiso ? . H H12 -0.025 -0.278 0.896 0.0325 Uiso ? . H H15 0.036 -0.101 0.908 0.0309 Uiso ? . H H16 0.031 0.106 0.907 0.0365 Uiso ? . H H21 0.085 0.416 0.946 0.0357 Uiso ? . H H22 0.188 0.386 1.061 0.0329 Uiso ? . H H24 0.228 0.148 0.845 0.0341 Uiso ? . H H25 0.123 0.184 0.744 0.0352 Uiso ? . H H113 0.841 0.498 0.795 0.0649 Uiso ? . H H114 0.869 0.625 0.662 0.0900 Uiso ? . H H115 0.792 0.671 0.512 0.0702 Uiso ? . H H116 0.685 0.596 0.483 0.0520 Uiso ? . H 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 _atom_site_aniso_type_symbol Ni 0.0164(15) 0.0132(15) 0.0222(16) 0.00000 -0.0039(12) 0.00000 Ni Cl1 0.056(3) 0.056(4) 0.080(4) -0.006(3) 0.021(3) 0.002(3) Cl Cl2 0.144(6) 0.098(5) 0.067(4) 0.040(4) 0.052(4) 0.040(4) Cl O1 0.022(6) 0.030(6) 0.039(7) 0.002(5) 0.008(5) -0.007(5) O O2 0.030(7) 0.052(9) 0.072(9) -0.003(7) 0.014(6) 0.005(7) O O3 0.035(7) 0.033(8) 0.076(9) -0.007(6) -0.001(6) 0.024(6) O N1 0.031(8) 0.011(8) 0.035(8) 0.000(8) -0.002(7) 0.001(7) N N11 0.025(10) 0.020(10) 0.031(12) 0.00000 0.008(9) 0.00000 N N12 0.047(12) 0.012(10) 0.033(12) 0.00000 0.022(10) 0.00000 N N21 0.014(6) 0.013(7) 0.026(8) -0.004(6) -0.001(6) -0.004(6) N C11 0.019(8) 0.023(10) 0.023(9) -0.006(7) 0.000(7) 0.004(8) C C12 0.032(9) 0.018(9) 0.012(8) -0.006(8) -0.009(6) 0.002(7) C C13 0.038(14) 0.010(12) 0.041(16) 0.00000 -0.006(12) 0.00000 C C14 0.022(12) 0.015(13) 0.038(15) 0.00000 0.005(11) 0.00000 C C15 0.025(8) 0.015(9) 0.022(9) 0.003(7) -0.003(7) -0.001(8) C C16 0.027(9) 0.021(10) 0.022(9) 0.007(7) 0.002(7) -0.001(8) C C21 0.020(9) 0.021(9) 0.038(10) 0.007(7) 0.012(8) -0.003(8) C C22 0.019(8) 0.012(9) 0.035(10) 0.010(7) 0.002(8) -0.007(7) C C23 0.009(7) 0.017(8) 0.029(10) -0.007(7) -0.002(7) 0.003(7) C C24 0.016(8) 0.027(9) 0.030(9) 0.005(8) -0.002(7) -0.006(8) C C25 0.021(9) 0.035(10) 0.018(9) 0.004(8) 0.008(7) -0.008(7) C C111 0.028(10) 0.044(11) 0.057(13) 0.011(9) 0.013(10) -0.018(10) C C112 0.088(16) 0.045(13) 0.028(12) 0.020(12) 0.010(12) -0.008(9) C C113 0.063(15) 0.066(15) 0.034(13) 0.030(12) -0.026(11) -0.027(11) C C114 0.054(15) 0.098(20) 0.090(19) 0.042(15) -0.003(15) -0.057(16) C C115 0.051(14) 0.041(12) 0.080(16) 0.028(11) 0.006(12) 0.013(11) C C116 0.040(11) 0.039(11) 0.047(12) 0.010(9) 0.003(9) 0.014(10) C #=============================================================================== # 10. MOLECULAR GEOMETRY 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 Ni O1 2.111(10) ? ? ? Ni O1a 2.111(10) ? ? ? Ni N12 2.121(17) ? ? ? Ni N21 2.115(10) ? ? ? Ni N21a 2.115(10) ? ? ? Cl1 C111 1.779(17) ? ? ? Cl2 C112 1.706(19) ? ? ? O1 N1 1.281(18) ? ? ? O2 N1 1.221(20) ? ? ? O3 N1 1.215(19) ? ? ? N11 C11 1.320(17) ? ? ? N11 C11a 1.320(17) ? ? ? N12 C16 1.347(16) ? ? ? N12 C16a 1.347(16) ? ? ? N21 C21 1.346(19) ? ? ? N21 C25 1.319(18) ? ? ? C11 C12 1.334(20) ? ? ? C11 H11 1.020(13) ? ? ? C12 C13 1.417(17) ? ? ? C12 H12 1.037(14) ? ? ? C13 C12a 1.417(17) ? ? ? C13 C14 1.49(3) ? ? ? C14 C15 1.380(17) ? ? ? C14 C15a 1.380(17) ? ? ? C15 C16 1.370(20) ? ? ? C15 H15 1.028(13) ? ? ? C16 H16 1.022(14) ? ? ? C21 C22 1.404(19) ? ? ? C21 H21 1.022(13) ? ? ? C22 C23 1.372(19) ? ? ? C22 H22 1.020(14) ? ? ? C23 C23b 1.54(3) ? ? ? C23 C24 1.403(20) ? ? ? C24 C25 1.382(19) ? ? ? C24 H24 1.021(14) ? ? ? C25 H25 1.003(14) ? ? ? C111 C112 1.36(3) ? ? ? C111 C116 1.38(3) ? ? ? C112 C113 1.40(3) ? ? ? C113 C114 1.41(4) ? ? ? C113 H113 1.025(18) ? ? ? C114 C115 1.34(3) ? ? ? C114 H114 1.043(23) ? ? ? C115 C116 1.36(3) ? ? ? C115 H115 1.033(19) ? ? ? C116 H116 1.024(16) ? ? ? 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 ? ? ? ? ? ? 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 Ni O1a 177.7(4) ? ? ? ? O1 Ni N12 88.9(3) ? ? ? ? O1 Ni N21 83.4(4) ? ? ? ? O1 Ni N21a 96.5(4) ? ? ? ? O1a Ni N12 88.9(3) ? ? ? ? O1a Ni N21 96.5(4) ? ? ? ? O1a Ni N21a 83.4(4) ? ? ? ? N12 Ni N21 86.4(3) ? ? ? ? N12 Ni N21a 86.4(3) ? ? ? ? N21 Ni N21a 172.9(4) ? ? ? ? Ni O1 N1 135.0(8) ? ? ? ? O1 N1 O2 119.2(13) ? ? ? ? O1 N1 O3 120.2(13) ? ? ? ? O2 N1 O3 120.6(14) ? ? ? ? C11 N11 C11a 114.9(15) ? ? ? ? Ni N12 C16 121.6(8) ? ? ? ? Ni N12 C16a 121.6(8) ? ? ? ? C16 N12 C16a 116.8(15) ? ? ? ? Ni N21 C21 121.4(9) ? ? ? ? Ni N21 C25 122.7(9) ? ? ? ? C21 N21 C25 115.6(11) ? ? ? ? N11 C11 C12 126.6(13) ? ? ? ? N11 C11 H11 116.3(14) ? ? ? ? C12 C11 H11 117.1(13) ? ? ? ? C11 C12 C13 117.7(13) ? ? ? ? C11 C12 H12 120.3(13) ? ? ? ? C13 C12 H12 122.0(14) ? ? ? ? C12 C13 C12a 116.6(17) ? ? ? ? C12 C13 C14 121.7(9) ? ? ? ? C12a C13 C14 121.7(9) ? ? ? ? C13 C14 C15 122.1(9) ? ? ? ? C13 C14 C15a 122.1(9) ? ? ? ? C15 C14 C15a 115.8(16) ? ? ? ? C14 C15 C16 121.2(13) ? ? ? ? C14 C15 H15 119.1(14) ? ? ? ? C16 C15 H15 119.7(13) ? ? ? ? N12 C16 C15 122.5(13) ? ? ? ? N12 C16 H16 119.1(14) ? ? ? ? C15 C16 H16 118.5(13) ? ? ? ? N21 C21 C22 123.6(12) ? ? ? ? N21 C21 H21 117.7(13) ? ? ? ? C22 C21 H21 118.7(14) ? ? ? ? C21 C22 C23 118.6(12) ? ? ? ? C21 C22 H22 120.6(12) ? ? ? ? C23 C22 H22 120.8(13) ? ? ? ? C22 C23 C23b 121.7(12) ? ? ? ? C22 C23 C24 118.8(12) ? ? ? ? C23b C23 C24 119.4(12) ? ? ? ? C23 C24 C25 117.0(12) ? ? ? ? C23 C24 H24 121.7(12) ? ? ? ? C25 C24 H24 121.2(13) ? ? ? ? N21 C25 C24 126.3(13) ? ? ? ? N21 C25 H25 115.9(13) ? ? ? ? C24 C25 H25 117.8(14) ? ? ? ? Cl1 C111 C112 119.5(15) ? ? ? ? Cl1 C111 C116 118.1(14) ? ? ? ? C112 C111 C116 122.4(16) ? ? ? ? Cl2 C112 C111 121.9(17) ? ? ? ? Cl2 C112 C113 118.7(16) ? ? ? ? C111 C112 C113 119.3(18) ? ? ? ? C112 C113 C114 117.2(17) ? ? ? ? C112 C113 H113 121.7(24) ? ? ? ? C114 C113 H113 121.1(23) ? ? ? ? C113 C114 C115 121.3(20) ? ? ? ? C113 C114 H114 119.6(23) ? ? ? ? C115 C114 H114 119(3) ? ? ? ? C114 C115 C116 121.4(20) ? ? ? ? C114 C115 H115 118.6(21) ? ? ? ? C116 C115 H115 120.0(19) ? ? ? ? C111 C116 C115 118.3(16) ? ? ? ? C111 C116 H116 121.2(17) ? ? ? ? C115 C116 H116 120.5(18) ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? #=============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #=============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ data_1-2PhH _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '1-2PhH' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H28 N6 Ni O6' _chemical_formula_weight 651.31 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 21.164(2) _cell_length_b 11.4128(9) _cell_length_c 12.6597(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.2060(10) _cell_angle_gamma 90.00 _cell_volume 2999.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method ? _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4492 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.93 _reflns_number_total 3067 _reflns_number_observed 2321 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.2833P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3067 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_obs 0.0449 _refine_ls_wR_factor_all 0.1179 _refine_ls_wR_factor_obs 0.1085 _refine_ls_goodness_of_fit_all 1.038 _refine_ls_goodness_of_fit_obs 1.108 _refine_ls_restrained_S_all 1.038 _refine_ls_restrained_S_obs 1.108 _refine_ls_shift/esd_max -0.008 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.5000 0.18458(4) 0.2500 0.01626(15) Uani 1 d S . O1 O 0.52260(9) 0.1859(2) 0.09506(15) 0.0280(4) Uani 1 d . . O2 O 0.60651(14) 0.1041(2) 0.0553(3) 0.0807(11) Uani 1 d . . O3 O 0.59265(13) 0.2863(3) 0.0347(3) 0.0781(11) Uani 1 d . . N1 N 0.57537(12) 0.1907(2) 0.0608(2) 0.0287(5) Uani 1 d . . N11 N 0.59556(10) 0.1955(2) 0.3346(2) 0.0188(5) Uani 1 d . . N21 N 0.5000 -0.0043(3) 0.2500 0.0182(7) Uani 1 d S . N22 N 0.5000 0.3716(3) 0.2500 0.0202(7) Uani 1 d S . C11 C 0.63693(13) 0.2738(2) 0.3076(2) 0.0237(6) Uani 1 d . . H11 H 0.62446(13) 0.3148(2) 0.2434(2) 0.028 Uiso 1 d R . C12 C 0.69666(13) 0.2973(2) 0.3690(2) 0.0236(6) Uani 1 d . . H12 H 0.72297(13) 0.3531(2) 0.3459(2) 0.028 Uiso 1 d R . C13 C 0.71798(12) 0.2383(2) 0.4654(2) 0.0170(5) Uani 1 d . . C14 C 0.67521(12) 0.1555(2) 0.4929(2) 0.0231(6) Uani 1 d . . H14 H 0.68668(12) 0.1128(2) 0.5563(2) 0.028 Uiso 1 d R . C15 C 0.61631(12) 0.1368(2) 0.4271(2) 0.0225(6) Uani 1 d . . H15 H 0.58934(12) 0.0804(2) 0.4475(2) 0.027 Uiso 1 d R . C21 C 0.52109(14) -0.0674(2) 0.1737(2) 0.0274(6) Uani 1 d . . H21 H 0.53583(14) -0.0271(2) 0.1195(2) 0.033 Uiso 1 d R . C22 C 0.52211(14) -0.1886(2) 0.1714(2) 0.0290(6) Uani 1 d . . H22 H 0.53763(14) -0.2272(2) 0.1170(2) 0.035 Uiso 1 d R . C23 C 0.5000 -0.2529(3) 0.2500 0.0224(8) Uani 1 d S . C24 C 0.5000 -0.3829(3) 0.2500 0.0242(9) Uani 1 d S . C25 C 0.48364(14) -0.4457(2) 0.1546(2) 0.0272(6) Uani 1 d . . H25 H 0.47246(14) -0.4068(2) 0.0891(2) 0.033 Uiso 1 d R . C26 C 0.48414(14) -0.5666(2) 0.1582(2) 0.0238(6) Uani 1 d . . H26 H 0.47292(14) -0.6075(2) 0.0938(2) 0.029 Uiso 1 d R . C31 C 0.7968(3) -0.0398(4) 0.4078(3) 0.137(3) Uani 1 d G . H31 H 0.8129(3) -0.0808(4) 0.4708(3) 0.164 Uiso 1 calc R . C32 C 0.7328(2) -0.0537(3) 0.3571(4) 0.123(3) Uani 1 d G . H32 H 0.7061(4) -0.1040(4) 0.3861(6) 0.147 Uiso 1 calc R . C33 C 0.70878(14) 0.0076(4) 0.2629(4) 0.094(2) Uani 1 d G . H33 H 0.66598(15) -0.0017(5) 0.2290(5) 0.113 Uiso 1 calc R . C34 C 0.7487(2) 0.0827(3) 0.2195(3) 0.104(2) Uani 1 d G . H34 H 0.7326(3) 0.1237(5) 0.1565(3) 0.124 Uiso 1 calc R . C35 C 0.8127(2) 0.0966(3) 0.2702(4) 0.125(3) Uani 1 d G . H35 H 0.8394(3) 0.1469(4) 0.2412(6) 0.150 Uiso 1 calc R . C36 C 0.8367(2) 0.0353(5) 0.3644(4) 0.137(3) Uani 1 d G . H36 H 0.8795(2) 0.0446(6) 0.3983(6) 0.165 Uiso 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 Ni1 0.0148(2) 0.0134(2) 0.0181(3) 0.000 -0.0029(2) 0.000 O1 0.0256(10) 0.0344(11) 0.0235(10) 0.0005(9) 0.0034(8) 0.0041(9) O2 0.052(2) 0.043(2) 0.159(3) -0.025(2) 0.052(2) 0.0061(13) O3 0.048(2) 0.070(2) 0.110(3) 0.057(2) 0.000(2) -0.0188(14) N1 0.0295(13) 0.0280(13) 0.0274(13) 0.0026(11) 0.0021(10) -0.0073(11) N11 0.0178(11) 0.0164(11) 0.0200(11) 0.0007(9) -0.0014(9) -0.0009(8) N21 0.018(2) 0.014(2) 0.020(2) 0.000 -0.0034(13) 0.000 N22 0.021(2) 0.016(2) 0.021(2) 0.000 -0.0020(14) 0.000 C11 0.0226(14) 0.0230(14) 0.0225(15) 0.0081(11) -0.0031(12) -0.0038(11) C12 0.0205(14) 0.023(2) 0.0251(15) 0.0061(11) -0.0017(12) -0.0070(10) C13 0.0151(12) 0.0159(12) 0.0185(14) -0.0011(10) -0.0004(10) 0.0009(10) C14 0.0206(14) 0.024(2) 0.0219(15) 0.0093(11) -0.0025(11) -0.0026(10) C15 0.0166(13) 0.0213(14) 0.027(2) 0.0070(11) -0.0018(12) -0.0035(10) C21 0.036(2) 0.0184(14) 0.028(2) 0.0024(12) 0.0082(13) -0.0022(12) C22 0.042(2) 0.0188(14) 0.028(2) -0.0043(12) 0.0110(13) 0.0006(13) C23 0.028(2) 0.015(2) 0.022(2) 0.000 -0.002(2) 0.000 C24 0.028(2) 0.017(2) 0.027(2) 0.000 0.004(2) 0.000 C25 0.039(2) 0.0183(15) 0.022(2) 0.0026(11) -0.0008(13) 0.0002(12) C26 0.032(2) 0.0190(14) 0.0172(14) -0.0017(11) -0.0024(12) 0.0011(11) C31 0.104(5) 0.156(7) 0.144(6) -0.060(5) 0.009(5) 0.079(5) C32 0.100(5) 0.131(6) 0.138(6) -0.063(5) 0.027(4) 0.051(4) C33 0.062(3) 0.103(4) 0.114(5) -0.077(4) 0.011(3) 0.018(3) C34 0.069(3) 0.103(4) 0.135(5) -0.075(4) 0.011(4) 0.023(3) C35 0.064(4) 0.115(5) 0.187(8) -0.090(5) 0.004(4) 0.018(3) C36 0.068(4) 0.155(7) 0.172(8) -0.098(6) -0.018(5) 0.052(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N11 2.100(2) . ? Ni1 N11 2.100(2) 2_655 ? Ni1 O1 2.107(2) . ? Ni1 O1 2.107(2) 2_655 ? Ni1 N22 2.135(3) . ? Ni1 N21 2.155(3) . ? O1 N1 1.275(3) . ? O2 N1 1.197(3) . ? O3 N1 1.217(3) . ? N11 C11 1.341(3) . ? N11 C15 1.346(3) . ? N21 C21 1.348(3) . ? N21 C21 1.348(3) 2_655 ? N22 C26 1.344(3) 2_665 ? N22 C26 1.344(3) 1_565 ? C11 C12 1.376(4) . ? C12 C13 1.390(4) . ? C13 C14 1.399(3) . ? C13 C13 1.488(5) 7_656 ? C14 C15 1.375(4) . ? C21 C22 1.384(4) . ? C22 C23 1.388(3) . ? C23 C22 1.388(3) 2_655 ? C23 C24 1.484(5) . ? C24 C25 1.390(3) 2_655 ? C24 C25 1.390(3) . ? C25 C26 1.381(4) . ? C26 N22 1.344(3) 1_545 ? C31 C32 1.39 . ? C31 C36 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? C34 C35 1.39 . ? C35 C36 1.39 . ? 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 N11 Ni1 N11 173.20(12) . 2_655 ? N11 Ni1 O1 95.97(8) . . ? N11 Ni1 O1 83.98(8) 2_655 . ? N11 Ni1 O1 83.98(8) . 2_655 ? N11 Ni1 O1 95.97(8) 2_655 2_655 ? O1 Ni1 O1 179.19(11) . 2_655 ? N11 Ni1 N22 86.60(6) . . ? N11 Ni1 N22 86.60(6) 2_655 . ? O1 Ni1 N22 89.59(6) . . ? O1 Ni1 N22 89.59(6) 2_655 . ? N11 Ni1 N21 93.40(6) . . ? N11 Ni1 N21 93.40(6) 2_655 . ? O1 Ni1 N21 90.41(6) . . ? O1 Ni1 N21 90.41(6) 2_655 . ? N22 Ni1 N21 180.0 . . ? N1 O1 Ni1 133.5(2) . . ? O2 N1 O3 121.8(3) . . ? O2 N1 O1 120.8(3) . . ? O3 N1 O1 117.4(3) . . ? C11 N11 C15 115.7(2) . . ? C11 N11 Ni1 121.4(2) . . ? C15 N11 Ni1 122.2(2) . . ? C21 N21 C21 115.4(3) . 2_655 ? C21 N21 Ni1 122.3(2) . . ? C21 N21 Ni1 122.3(2) 2_655 . ? C26 N22 C26 116.8(3) 2_665 1_565 ? C26 N22 Ni1 121.6(2) 2_665 . ? C26 N22 Ni1 121.6(2) 1_565 . ? N11 C11 C12 124.0(2) . . ? C11 C12 C13 120.5(2) . . ? C12 C13 C14 115.5(2) . . ? C12 C13 C13 122.2(3) . 7_656 ? C14 C13 C13 122.3(3) . 7_656 ? C15 C14 C13 120.6(2) . . ? N11 C15 C14 123.6(2) . . ? N21 C21 C22 123.9(3) . . ? C21 C22 C23 120.2(3) . . ? C22 C23 C22 116.3(3) . 2_655 ? C22 C23 C24 121.9(2) . . ? C22 C23 C24 121.9(2) 2_655 . ? C25 C24 C25 117.9(3) 2_655 . ? C25 C24 C23 121.1(2) 2_655 . ? C25 C24 C23 121.1(2) . . ? C26 C25 C24 119.2(3) . . ? N22 C26 C25 123.5(3) 1_545 . ? C32 C31 C36 120.0 . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? _refine_diff_density_max 0.539 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.071 data_2-2PhNO2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '2-2PhNO2' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H26 N8 Ni O10' _chemical_formula_weight 741.32 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 21.5968(13) _cell_length_b 11.4000(7) _cell_length_c 12.9303(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.1040(10) _cell_angle_gamma 90.00 _cell_volume 3100.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method ? _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9438 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.95 _reflns_number_total 3627 _reflns_number_observed 2920 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+1.0514P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3627 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_obs 0.0301 _refine_ls_wR_factor_all 0.0733 _refine_ls_wR_factor_obs 0.0690 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_goodness_of_fit_obs 1.071 _refine_ls_restrained_S_all 1.013 _refine_ls_restrained_S_obs 1.071 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni Ni 0.5000 0.18519(2) 0.7500 0.01347(8) Uani 1 d S . O1 O 0.47578(5) 0.19033(9) 0.89934(9) 0.0206(2) Uani 1 d . . O2 O 0.40067(6) 0.27309(12) 0.95884(12) 0.0447(4) Uani 1 d . . O3 O 0.38948(6) 0.09478(12) 0.90594(13) 0.0449(4) Uani 1 d . . N1 N 0.42032(6) 0.18584(12) 0.92132(11) 0.0220(3) Uani 1 d . . N11 N 0.59462(6) 0.19771(10) 0.83882(10) 0.0168(3) Uani 1 d . . N21 N 0.5000 0.3726(2) 0.7500 0.0173(4) Uani 1 d S . N22 N 0.5000 -0.00292(15) 0.7500 0.0160(4) Uani 1 d S . C21 C 0.51643(7) 0.43430(13) 0.84093(13) 0.0201(3) Uani 1 d . . H21 H 0.52772(7) 0.39335(13) 0.90464(13) 0.024 Uiso 1 calc R . C22 C 0.51733(8) 0.55535(13) 0.84425(13) 0.0209(3) Uani 1 d . . H22 H 0.52942(8) 0.59414(13) 0.90896(13) 0.025 Uiso 1 calc R . C23 C 0.5000 0.6192(2) 0.7500 0.0183(5) Uani 1 d S . C24 C 0.5000 -0.2508(2) 0.7500 0.0174(4) Uani 1 d S . C25 C 0.48895(7) -0.18675(13) 0.83603(12) 0.0203(3) Uani 1 d . . H25 H 0.48106(7) -0.22529(13) 0.89513(12) 0.024 Uiso 1 calc R . C26 C 0.48981(7) -0.06554(13) 0.83273(13) 0.0195(3) Uani 1 d . . H26 H 0.48290(7) -0.02476(13) 0.89138(13) 0.023 Uiso 1 calc R . C11 C 0.63544(7) 0.27272(14) 0.80902(13) 0.0213(3) Uani 1 d . . H11 H 0.62221(7) 0.31210(14) 0.74481(13) 0.026 Uiso 1 calc R . C12 C 0.69579(7) 0.29425(14) 0.86860(13) 0.0219(3) Uani 1 d . . H12 H 0.72223(7) 0.34612(14) 0.84353(13) 0.026 Uiso 1 calc R . C13 C 0.71758(6) 0.23874(13) 0.96642(12) 0.0167(3) Uani 1 d . . C14 C 0.67535(7) 0.16073(13) 0.99684(13) 0.0203(3) Uani 1 d . . H14 H 0.68716(7) 0.12077(13) 1.06100(13) 0.024 Uiso 1 calc R . C15 C 0.61564(7) 0.14263(14) 0.93142(13) 0.0201(3) Uani 1 d . . H15 H 0.58871(7) 0.08910(14) 0.95325(13) 0.024 Uiso 1 calc R . O31 O 0.66156(10) 0.3658(2) 1.2476(2) 0.1008(8) Uani 1 d . . O32 O 0.61116(8) 0.3903(2) 1.0860(2) 0.0725(6) Uani 1 d . . N31 N 0.65696(9) 0.4069(2) 1.1596(2) 0.0505(5) Uani 1 d . . C31 C 0.70925(8) 0.4797(2) 1.1404(2) 0.0327(4) Uani 1 d . . C32 C 0.70109(10) 0.5374(2) 1.0443(2) 0.0418(5) Uani 1 d . . H32 H 0.66327(10) 0.5312(2) 0.9931(2) 0.050 Uiso 1 calc R . C33 C 0.75081(12) 0.6046(2) 1.0268(2) 0.0497(6) Uani 1 d . . H33 H 0.74691(12) 0.6435(2) 0.9625(2) 0.060 Uiso 1 calc R . C34 C 0.80628(12) 0.6143(2) 1.1040(2) 0.0489(6) Uani 1 d . . H34 H 0.83919(12) 0.6609(2) 1.0916(2) 0.059 Uiso 1 calc R . C35 C 0.81356(9) 0.5558(2) 1.1994(2) 0.0408(5) Uani 1 d . . H35 H 0.85128(9) 0.5629(2) 1.2507(2) 0.049 Uiso 1 calc R . C36 C 0.76493(9) 0.4865(2) 1.2189(2) 0.0337(4) Uani 1 d . . H36 H 0.76935(9) 0.4458(2) 1.2825(2) 0.040 Uiso 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 Ni 0.01284(13) 0.00974(13) 0.01601(15) 0.000 -0.00056(10) 0.000 O1 0.0184(5) 0.0233(6) 0.0202(6) -0.0009(5) 0.0046(4) -0.0019(4) O2 0.0392(8) 0.0403(8) 0.0549(10) -0.0209(7) 0.0113(7) 0.0143(6) O3 0.0329(7) 0.0335(7) 0.0725(11) -0.0078(7) 0.0211(7) -0.0127(6) N1 0.0222(7) 0.0230(7) 0.0204(7) -0.0004(6) 0.0039(5) 0.0034(6) N11 0.0142(6) 0.0141(6) 0.0205(7) -0.0003(5) 0.0007(5) 0.0000(5) N21 0.0180(9) 0.0128(9) 0.0193(10) 0.000 0.0003(7) 0.000 N22 0.0136(8) 0.0118(8) 0.0212(10) 0.000 0.0008(7) 0.000 C21 0.0236(8) 0.0150(7) 0.0192(8) 0.0019(6) -0.0001(6) 0.0009(6) C22 0.0271(8) 0.0151(7) 0.0191(8) -0.0022(6) 0.0021(7) -0.0003(6) C23 0.0191(11) 0.0125(10) 0.0230(12) 0.000 0.0038(9) 0.000 C24 0.0183(10) 0.0113(10) 0.0203(12) 0.000 -0.0005(9) 0.000 C25 0.0265(8) 0.0151(7) 0.0192(8) 0.0029(7) 0.0047(6) -0.0005(6) C26 0.0231(8) 0.0139(7) 0.0210(8) -0.0021(6) 0.0038(6) 0.0006(6) C11 0.0207(8) 0.0211(7) 0.0199(8) 0.0037(7) -0.0003(6) -0.0014(6) C12 0.0181(8) 0.0228(8) 0.0232(8) 0.0044(7) 0.0010(6) -0.0055(6) C13 0.0138(7) 0.0160(7) 0.0186(8) -0.0020(6) 0.0004(6) 0.0008(5) C14 0.0187(8) 0.0211(8) 0.0190(8) 0.0057(6) -0.0001(6) -0.0005(6) C15 0.0162(7) 0.0184(7) 0.0240(9) 0.0038(7) 0.0014(6) -0.0018(6) O31 0.0709(14) 0.134(2) 0.099(2) 0.044(2) 0.0231(13) -0.0269(13) O32 0.0392(9) 0.0882(14) 0.0878(14) -0.0350(12) 0.0094(10) -0.0135(9) N31 0.0373(10) 0.0513(12) 0.0647(14) -0.0101(11) 0.0153(10) 0.0009(8) C31 0.0299(9) 0.0279(9) 0.0414(11) -0.0073(8) 0.0103(8) 0.0060(7) C32 0.0471(12) 0.0345(11) 0.0392(12) -0.0067(9) 0.0002(10) 0.0196(9) C33 0.079(2) 0.0299(11) 0.0433(13) 0.0059(10) 0.0211(13) 0.0171(11) C34 0.0563(14) 0.0324(11) 0.067(2) -0.0055(11) 0.0321(13) -0.0009(10) C35 0.0321(10) 0.0420(11) 0.0474(13) -0.0144(10) 0.0069(9) 0.0041(9) C36 0.0366(10) 0.0344(10) 0.0308(10) -0.0046(8) 0.0091(8) 0.0084(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N11 2.1097(12) . ? Ni N11 2.1097(12) 2_656 ? Ni O1 2.1128(11) . ? Ni O1 2.1128(11) 2_656 ? Ni N21 2.136(2) . ? Ni N22 2.144(2) . ? O1 N1 1.293(2) . ? O2 N1 1.224(2) . ? O3 N1 1.225(2) . ? N11 C15 1.337(2) . ? N11 C11 1.346(2) . ? N21 C21 1.347(2) . ? N21 C21 1.347(2) 2_656 ? N22 C26 1.345(2) 2_656 ? N22 C26 1.345(2) . ? C21 C22 1.381(2) . ? C22 C23 1.396(2) . ? C23 C22 1.396(2) 2_656 ? C23 C24 1.481(3) 1_565 ? C24 C25 1.396(2) . ? C24 C25 1.396(2) 2_656 ? C24 C23 1.481(3) 1_545 ? C25 C26 1.383(2) . ? C11 C12 1.377(2) . ? C12 C13 1.397(2) . ? C13 C14 1.393(2) . ? C13 C13 1.493(3) 7_657 ? C14 C15 1.388(2) . ? O31 N31 1.214(3) . ? O32 N31 1.222(2) . ? N31 C31 1.467(3) . ? C31 C32 1.381(3) . ? C31 C36 1.389(3) . ? C32 C33 1.379(3) . ? C33 C34 1.379(3) . ? C34 C35 1.380(3) . ? C35 C36 1.382(3) . ? 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 N11 Ni N11 172.24(7) . 2_656 ? N11 Ni O1 84.87(4) . . ? N11 Ni O1 94.92(4) 2_656 . ? N11 Ni O1 94.92(4) . 2_656 ? N11 Ni O1 84.87(4) 2_656 2_656 ? O1 Ni O1 176.82(6) . 2_656 ? N11 Ni N21 86.12(3) . . ? N11 Ni N21 86.12(3) 2_656 . ? O1 Ni N21 88.41(3) . . ? O1 Ni N21 88.41(3) 2_656 . ? N11 Ni N22 93.88(3) . . ? N11 Ni N22 93.88(3) 2_656 . ? O1 Ni N22 91.59(3) . . ? O1 Ni N22 91.59(3) 2_656 . ? N21 Ni N22 180.0 . . ? N1 O1 Ni 129.30(9) . . ? O3 N1 O2 121.89(15) . . ? O3 N1 O1 119.64(13) . . ? O2 N1 O1 118.46(14) . . ? C15 N11 C11 116.31(13) . . ? C15 N11 Ni 123.10(10) . . ? C11 N11 Ni 120.24(10) . . ? C21 N21 C21 117.0(2) . 2_656 ? C21 N21 Ni 121.50(9) . . ? C21 N21 Ni 121.50(9) 2_656 . ? C26 N22 C26 115.9(2) 2_656 . ? C26 N22 Ni 122.06(9) 2_656 . ? C26 N22 Ni 122.06(9) . . ? N21 C21 C22 123.3(2) . . ? C21 C22 C23 119.7(2) . . ? C22 C23 C22 117.1(2) 2_656 . ? C22 C23 C24 121.45(10) 2_656 1_565 ? C22 C23 C24 121.45(10) . 1_565 ? C25 C24 C25 116.9(2) . 2_656 ? C25 C24 C23 121.55(9) . 1_545 ? C25 C24 C23 121.55(9) 2_656 1_545 ? C26 C25 C24 119.49(15) . . ? N22 C26 C25 124.11(15) . . ? N11 C11 C12 123.46(15) . . ? C11 C12 C13 120.50(14) . . ? C14 C13 C12 115.92(13) . . ? C14 C13 C13 122.2(2) . 7_657 ? C12 C13 C13 121.8(2) . 7_657 ? C15 C14 C13 120.01(15) . . ? N11 C15 C14 123.78(14) . . ? O31 N31 O32 123.4(2) . . ? O31 N31 C31 118.3(2) . . ? O32 N31 C31 118.3(2) . . ? C32 C31 C36 122.9(2) . . ? C32 C31 N31 118.4(2) . . ? C36 C31 N31 118.7(2) . . ? C33 C32 C31 117.8(2) . . ? C32 C33 C34 120.4(2) . . ? C35 C34 C33 120.8(2) . . ? C34 C35 C36 120.1(2) . . ? C35 C36 C31 117.8(2) . . ? _refine_diff_density_max 0.291 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.051 data_2-2PhMe _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '2-2PhMe' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C68 H32 Co2 N12 O12' _chemical_formula_weight 1326.92 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 21.7636(13) _cell_length_b 11.5176(7) _cell_length_c 12.8555(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.7410(10) _cell_angle_gamma 90.00 _cell_volume 3143.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method ? _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9565 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.02 _reflns_number_total 3676 _reflns_number_observed 2937 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.6194P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3676 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_obs 0.0379 _refine_ls_wR_factor_all 0.1097 _refine_ls_wR_factor_obs 0.1030 _refine_ls_goodness_of_fit_all 1.064 _refine_ls_goodness_of_fit_obs 1.128 _refine_ls_restrained_S_all 1.064 _refine_ls_restrained_S_obs 1.128 _refine_ls_shift/esd_max -0.345 _refine_ls_shift/esd_mean 0.038 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co Co 0.5000 0.18384(3) 0.7500 0.01487(12) Uani 1 d S . O1 O 0.48141(6) 0.18623(12) 0.90273(10) 0.0233(3) Uani 1 d . . O2 O 0.41022(8) 0.2842(2) 0.9589(2) 0.0503(5) Uani 1 d . . O3 O 0.39850(9) 0.1007(2) 0.9340(2) 0.0531(5) Uani 1 d . . N1 N 0.42801(8) 0.19038(14) 0.93179(13) 0.0247(4) Uani 1 d . . N11 N 0.5000 0.3742(2) 0.7500 0.0192(5) Uani 1 d S . N12 N 0.5000 -0.0077(2) 0.7500 0.0185(4) Uani 1 d S . N21 N 0.59721(7) 0.19652(13) 0.83609(12) 0.0184(3) Uani 1 d . . C11 C 0.51681(9) 0.4350(2) 0.84078(15) 0.0229(4) Uani 1 d . . H11 H 0.52850(9) 0.3944(2) 0.90464(15) 0.028 Uiso 1 calc R . C12 C 0.51762(9) 0.5549(2) 0.8442(2) 0.0245(4) Uani 1 d . . H12 H 0.52987(9) 0.5933(2) 0.9092(2) 0.029 Uiso 1 calc R . C13 C 0.5000 0.6181(2) 0.7500 0.0212(5) Uani 1 d S . C14 C 0.5000 -0.2529(2) 0.7500 0.0197(5) Uani 1 d S . C15 C 0.48407(9) -0.1895(2) 0.8326(2) 0.0234(4) Uani 1 d . . H15 H 0.47291(9) -0.2277(2) 0.8894(2) 0.028 Uiso 1 calc R . C16 C 0.48491(9) -0.0694(2) 0.82965(15) 0.0223(4) Uani 1 d . . H16 H 0.47445(9) -0.0290(2) 0.88597(15) 0.027 Uiso 1 calc R . C21 C 0.63697(9) 0.2749(2) 0.8093(2) 0.0225(4) Uani 1 d . . H21 H 0.62366(9) 0.3160(2) 0.7461(2) 0.027 Uiso 1 calc R . C22 C 0.69628(9) 0.2979(2) 0.8702(2) 0.0237(4) Uani 1 d . . H22 H 0.72164(9) 0.3531(2) 0.8475(2) 0.028 Uiso 1 calc R . C23 C 0.71830(8) 0.2384(2) 0.96568(14) 0.0188(4) Uani 1 d . . C24 C 0.67726(9) 0.1565(2) 0.9930(2) 0.0262(4) Uani 1 d . . H24 H 0.68933(9) 0.1142(2) 1.0557(2) 0.031 Uiso 1 calc R . C25 C 0.61869(9) 0.1382(2) 0.9269(2) 0.0243(4) Uani 1 d . . H25 H 0.59273(9) 0.0821(2) 0.9467(2) 0.029 Uiso 1 calc R . C31 C 0.3056(7) -0.0178(15) 0.7306(9) 0.100(7) Uani 0.50 d P . C32 C 0.3190(5) -0.1270(10) 0.6336(8) 0.071(3) Uani 0.50 d P . C33 C 0.3158(10) -0.0726(31) 0.6713(36) 0.353(29) Uani 0.50 d P . C34 C 0.1947(7) -0.0341(14) 0.5992(9) 0.083(4) Uani 0.50 d P . C35 C 0.2217(23) 0.0273(15) 0.6753(38) 0.391(32) Uani 0.50 d P . C36 C 0.1580(7) 0.0431(16) 0.6316(11) 0.101(6) Uani 0.50 d P . C37 C 0.1820(9) 0.1065(13) 0.7292(12) 0.109(6) Uani 0.50 d P . C38 C 0.2162(6) -0.0699(9) 0.5482(7) 0.079(4) Uani 0.50 d P . C39 C 0.1577(15) 0.0957(37) 0.6785(34) 0.287(25) Uani 0.50 d P . C310 C 0.2496(5) 0.0913(8) 0.7771(7) 0.083(3) Uani 0.50 d P . C311 C 0.2737(5) -0.1166(6) 0.5636(10) 0.090(3) Uani 0.50 d P . C312 C 0.2697(5) -0.0563(8) 0.6624(7) 0.084(2) Uani 0.50 d P . C313 C 0.2717(4) 0.0207(6) 0.7343(6) 0.0348(14) Uani 0.50 d P . C314 C 0.2110(5) -0.0085(29) 0.6267(26) 0.227(22) Uani 0.50 d P . 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 Co 0.0145(2) 0.0106(2) 0.0171(2) 0.000 -0.00164(12) 0.000 O1 0.0223(7) 0.0263(7) 0.0207(7) -0.0007(5) 0.0034(5) -0.0018(5) O2 0.0436(10) 0.0411(10) 0.0616(12) -0.0242(9) 0.0013(9) 0.0186(8) O3 0.0426(10) 0.0367(10) 0.088(2) 0.0017(9) 0.0321(10) -0.0109(8) N1 0.0258(8) 0.0243(8) 0.0224(8) -0.0002(7) 0.0021(7) 0.0043(7) N11 0.0196(10) 0.0136(10) 0.0210(11) 0.000 -0.0024(9) 0.000 N12 0.0159(10) 0.0150(10) 0.0222(11) 0.000 -0.0007(8) 0.000 N21 0.0156(7) 0.0160(7) 0.0212(8) 0.0010(6) -0.0015(6) -0.0013(6) C11 0.0295(10) 0.0151(9) 0.0209(10) 0.0018(7) -0.0014(8) 0.0000(8) C12 0.0338(11) 0.0161(9) 0.0206(10) -0.0018(7) -0.0008(8) -0.0013(8) C13 0.0234(13) 0.0139(12) 0.0252(14) 0.000 0.0029(11) 0.000 C14 0.0206(12) 0.0144(12) 0.0211(13) 0.000 -0.0022(10) 0.000 C15 0.0309(10) 0.0155(9) 0.0230(10) 0.0021(7) 0.0044(8) -0.0006(8) C16 0.0276(10) 0.0160(9) 0.0226(10) -0.0013(7) 0.0039(8) 0.0021(7) C21 0.0204(9) 0.0231(9) 0.0210(9) 0.0064(7) -0.0019(7) -0.0026(7) C22 0.0191(9) 0.0261(10) 0.0234(10) 0.0067(8) -0.0005(8) -0.0068(7) C23 0.0155(8) 0.0193(9) 0.0196(9) 0.0003(7) -0.0003(7) -0.0005(7) C24 0.0208(9) 0.0283(10) 0.0251(10) 0.0112(8) -0.0047(8) -0.0044(8) C25 0.0171(9) 0.0223(9) 0.0302(11) 0.0088(8) -0.0019(8) -0.0042(7) C31 0.067(8) 0.135(13) 0.073(6) 0.071(7) -0.038(7) -0.083(9) C32 0.066(6) 0.083(6) 0.063(5) -0.012(5) 0.013(4) 0.012(5) C33 0.070(10) 0.354(36) 0.671(64) 0.445(43) 0.157(24) 0.095(16) C34 0.051(7) 0.138(10) 0.057(5) -0.002(6) 0.001(5) -0.075(7) C35 0.691(67) 0.059(9) 0.635(66) 0.152(22) 0.604(61) 0.117(23) C36 0.094(9) 0.142(12) 0.077(6) -0.003(7) 0.043(6) -0.075(11) C37 0.142(13) 0.081(7) 0.096(8) 0.034(6) 0.011(8) -0.052(9) C38 0.105(9) 0.073(5) 0.062(5) -0.001(5) 0.021(5) -0.049(5) C39 0.227(28) 0.390(41) 0.314(43) 0.273(34) 0.213(31) 0.191(26) C310 0.092(6) 0.088(6) 0.067(5) 0.010(4) 0.012(5) -0.049(5) C311 0.091(6) 0.037(3) 0.165(11) 0.007(5) 0.077(7) -0.008(4) C312 0.094(7) 0.069(5) 0.094(6) 0.036(5) 0.035(6) -0.028(5) C313 0.044(4) 0.027(3) 0.039(3) 0.005(2) 0.021(3) -0.005(3) C314 0.014(5) 0.345(36) 0.280(32) 0.266(31) -0.059(10) -0.080(11) _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 Co O1 2.0905(13) 2_656 ? Co O1 2.0905(13) . ? Co N21 2.1655(15) . ? Co N21 2.1655(15) 2_656 ? Co N11 2.193(2) . ? Co N12 2.206(2) . ? O1 N1 1.298(2) . ? O2 N1 1.224(2) . ? O3 N1 1.220(2) . ? N11 C11 1.341(2) . ? N11 C11 1.341(2) 2_656 ? N12 C16 1.345(2) 2_656 ? N12 C16 1.345(2) . ? N21 C25 1.339(2) . ? N21 C21 1.347(2) . ? C11 C12 1.382(3) . ? C12 C13 1.392(2) . ? C13 C12 1.392(2) 2_656 ? C13 C14 1.485(4) 1_565 ? C14 C15 1.394(2) 2_656 ? C14 C15 1.394(2) . ? C14 C13 1.485(4) 1_545 ? C15 C16 1.384(3) . ? C21 C22 1.380(3) . ? C22 C23 1.395(3) . ? C23 C24 1.396(3) . ? C23 C23 1.489(3) 7_657 ? C24 C25 1.383(3) . ? C31 C313 0.87(2) . ? C31 C33 1.05(5) . ? C31 C312 1.128(12) . ? C31 C32 1.84(2) . ? C31 C35 1.88(5) . ? C31 C310 1.93(2) . ? C32 C33 0.80(5) . ? C32 C311 1.18(2) . ? C32 C312 1.457(15) . ? C33 C312 1.00(2) . ? C33 C311 1.57(5) . ? C33 C313 1.75(4) . ? C34 C314 0.53(3) . ? C34 C38 0.98(2) . ? C34 C35 1.24(5) . ? C34 C36 1.32(2) . ? C34 C312 1.68(2) . ? C34 C39 2.07(4) . ? C35 C314 0.74(6) . ? C35 C313 1.18(6) . ? C35 C36 1.39(5) . ? C35 C312 1.46(3) . ? C35 C310 1.51(5) . ? C35 C37 1.52(3) . ? C35 C39 1.61(4) . ? C35 C38 1.96(4) . ? C36 C39 0.86(5) . ? C36 C314 1.31(4) . ? C36 C37 1.45(2) . ? C37 C39 0.75(5) . ? C37 C310 1.48(2) . ? C37 C314 2.06(4) . ? C38 C314 1.26(4) . ? C38 C311 1.34(2) . ? C38 C312 1.667(14) . ? C39 C314 1.89(6) . ? C310 C313 1.146(13) . ? C311 C312 1.467(13) . ? C312 C313 1.275(12) . ? C312 C314 1.37(2) . ? C313 C314 1.72(2) . ? 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 Co O1 178.49(8) 2_656 . ? O1 Co N21 96.29(6) 2_656 . ? O1 Co N21 83.61(6) . . ? O1 Co N21 83.61(6) 2_656 2_656 ? O1 Co N21 96.29(6) . 2_656 ? N21 Co N21 172.26(8) . 2_656 ? O1 Co N11 89.24(4) 2_656 . ? O1 Co N11 89.24(4) . . ? N21 Co N11 86.13(4) . . ? N21 Co N11 86.13(4) 2_656 . ? O1 Co N12 90.76(4) 2_656 . ? O1 Co N12 90.76(4) . . ? N21 Co N12 93.87(4) . . ? N21 Co N12 93.87(4) 2_656 . ? N11 Co N12 180.0 . . ? N1 O1 Co 129.94(11) . . ? O3 N1 O2 122.7(2) . . ? O3 N1 O1 119.0(2) . . ? O2 N1 O1 118.3(2) . . ? C11 N11 C11 117.0(2) . 2_656 ? C11 N11 Co 121.48(11) . . ? C11 N11 Co 121.48(11) 2_656 . ? C16 N12 C16 116.2(2) 2_656 . ? C16 N12 Co 121.88(11) 2_656 . ? C16 N12 Co 121.88(11) . . ? C25 N21 C21 116.0(2) . . ? C25 N21 Co 121.71(12) . . ? C21 N21 Co 121.66(12) . . ? N11 C11 C12 123.3(2) . . ? C11 C12 C13 119.7(2) . . ? C12 C13 C12 117.0(2) 2_656 . ? C12 C13 C14 121.51(12) 2_656 1_565 ? C12 C13 C14 121.51(12) . 1_565 ? C15 C14 C15 116.8(2) 2_656 . ? C15 C14 C13 121.62(12) 2_656 1_545 ? C15 C14 C13 121.62(12) . 1_545 ? C16 C15 C14 119.8(2) . . ? N12 C16 C15 123.7(2) . . ? N21 C21 C22 123.8(2) . . ? C21 C22 C23 120.1(2) . . ? C22 C23 C24 116.0(2) . . ? C22 C23 C23 121.8(2) . 7_657 ? C24 C23 C23 122.2(2) . 7_657 ? C25 C24 C23 120.2(2) . . ? N21 C25 C24 123.8(2) . . ? C313 C31 C33 131.6(19) . . ? C313 C31 C312 78.1(10) . . ? C33 C31 C312 54.6(15) . . ? C313 C31 C32 130.5(11) . . ? C33 C31 C32 6.6(13) . . ? C312 C31 C32 52.4(12) . . ? C313 C31 C35 28.0(13) . . ? C33 C31 C35 103.6(20) . . ? C312 C31 C35 50.8(14) . . ? C32 C31 C35 102.6(14) . . ? C313 C31 C310 18.8(10) . . ? C33 C31 C310 149.7(19) . . ? C312 C31 C310 97.0(14) . . ? C32 C31 C310 149.2(6) . . ? C35 C31 C310 46.5(15) . . ? C33 C32 C311 102.2(26) . . ? C33 C32 C312 41.1(20) . . ? C311 C32 C312 66.5(8) . . ? C33 C32 C31 8.6(15) . . ? C311 C32 C31 102.5(9) . . ? C312 C32 C31 37.8(6) . . ? C32 C33 C312 107.1(47) . . ? C32 C33 C31 164.8(27) . . ? C312 C33 C31 66.6(21) . . ? C32 C33 C311 47.7(29) . . ? C312 C33 C311 65.4(23) . . ? C31 C33 C311 131.3(18) . . ? C32 C33 C313 152.1(31) . . ? C312 C33 C313 45.7(20) . . ? C31 C33 C313 21.8(8) . . ? C311 C33 C313 109.5(11) . . ? C314 C34 C38 109.4(52) . . ? C314 C34 C35 14.4(46) . . ? C38 C34 C35 123.6(20) . . ? C314 C34 C36 77.1(51) . . ? C38 C34 C36 155.1(16) . . ? C35 C34 C36 65.4(19) . . ? C314 C34 C312 47.7(45) . . ? C38 C34 C312 72.6(13) . . ? C35 C34 C312 57.6(17) . . ? C36 C34 C312 122.8(10) . . ? C314 C34 C39 63.0(47) . . ? C38 C34 C39 158.6(14) . . ? C35 C34 C39 51.0(23) . . ? C36 C34 C39 14.4(15) . . ? C312 C34 C39 108.4(14) . . ? C314 C35 C313 125.3(38) . . ? C314 C35 C34 10.3(25) . . ? C313 C35 C34 132.5(18) . . ? C314 C35 C36 68.3(51) . . ? C313 C35 C36 164.3(27) . . ? C34 C35 C36 60.0(31) . . ? C314 C35 C312 68.8(27) . . ? C313 C35 C312 56.6(16) . . ? C34 C35 C312 76.2(14) . . ? C36 C35 C312 135.9(39) . . ? C314 C35 C310 173.8(51) . . ? C313 C35 C310 48.6(24) . . ? C34 C35 C310 171.9(16) . . ? C36 C35 C310 117.5(14) . . ? C312 C35 C310 105.1(38) . . ? C314 C35 C37 127.6(60) . . ? C313 C35 C37 106.3(34) . . ? C34 C35 C37 118.7(39) . . ? C36 C35 C37 59.3(13) . . ? C312 C35 C37 160.1(40) . . ? C310 C35 C37 58.2(13) . . ? C314 C35 C39 100.3(65) . . ? C313 C35 C39 134.0(39) . . ? C34 C35 C39 92.1(44) . . ? C36 C35 C39 32.1(21) . . ? C312 C35 C39 166.7(45) . . ? C310 C35 C39 85.7(22) . . ? C37 C35 C39 27.7(18) . . ? C314 C35 C31 105.3(34) . . ? C313 C35 C31 20.2(9) . . ? C34 C35 C31 113.0(14) . . ? C36 C35 C31 171.5(23) . . ? C312 C35 C31 36.8(13) . . ? C310 C35 C31 68.6(27) . . ? C37 C35 C31 126.5(37) . . ? C39 C35 C31 154.2(41) . . ? C314 C35 C38 14.5(27) . . ? C313 C35 C38 112.0(15) . . ? C34 C35 C38 24.5(9) . . ? C36 C35 C38 82.3(30) . . ? C312 C35 C38 56.0(12) . . ? C310 C35 C38 160.1(30) . . ? C37 C35 C38 141.6(38) . . ? C39 C35 C38 113.9(43) . . ? C31 C35 C38 91.9(11) . . ? C39 C36 C314 119.9(31) . . ? C39 C36 C34 142.9(32) . . ? C314 C36 C34 23.3(16) . . ? C39 C36 C35 88.3(30) . . ? C314 C36 C35 31.7(22) . . ? C34 C36 C35 54.6(18) . . ? C39 C36 C37 24.3(25) . . ? C314 C36 C37 96.8(16) . . ? C34 C36 C37 119.0(15) . . ? C35 C36 C37 65.0(18) . . ? C39 C37 C36 27.8(33) . . ? C39 C37 C310 141.8(44) . . ? C36 C37 C310 116.0(19) . . ? C39 C37 C35 82.4(42) . . ? C36 C37 C35 55.6(23) . . ? C310 C37 C35 60.3(24) . . ? C39 C37 C314 66.2(37) . . ? C36 C37 C314 39.1(10) . . ? C310 C37 C314 76.9(12) . . ? C35 C37 C314 16.6(23) . . ? C34 C38 C314 23.5(6) . . ? C34 C38 C311 130.0(13) . . ? C314 C38 C311 110.8(11) . . ? C34 C38 C312 73.4(10) . . ? C314 C38 C312 53.9(8) . . ? C311 C38 C312 57.2(7) . . ? C34 C38 C35 31.9(15) . . ? C314 C38 C35 8.5(15) . . ? C311 C38 C35 102.9(16) . . ? C312 C38 C35 46.5(14) . . ? C36 C39 C37 127.8(48) . . ? C36 C39 C35 59.6(27) . . ? C37 C39 C35 69.9(36) . . ? C36 C39 C314 37.0(19) . . ? C37 C39 C314 92.4(33) . . ? C35 C39 C314 22.7(22) . . ? C36 C39 C34 22.7(19) . . ? C37 C39 C34 105.7(36) . . ? C35 C39 C34 36.9(24) . . ? C314 C39 C34 14.5(8) . . ? C313 C310 C37 111.7(11) . . ? C313 C310 C35 50.8(14) . . ? C37 C310 C35 61.5(17) . . ? C313 C310 C31 14.2(5) . . ? C37 C310 C31 125.9(9) . . ? C35 C310 C31 64.8(15) . . ? C32 C311 C38 138.4(11) . . ? C32 C311 C312 65.7(9) . . ? C38 C311 C312 72.8(7) . . ? C32 C311 C33 30.1(13) . . ? C38 C311 C33 110.3(14) . . ? C312 C311 C33 38.4(11) . . ? C33 C312 C31 58.8(29) . . ? C33 C312 C313 100.0(32) . . ? C31 C312 C313 41.9(10) . . ? C33 C312 C314 161.3(14) . . ? C31 C312 C314 122.3(24) . . ? C313 C312 C314 81.0(20) . . ? C33 C312 C32 31.8(32) . . ? C31 C312 C32 89.7(15) . . ? C313 C312 C32 131.5(10) . . ? C314 C312 C32 145.2(20) . . ? C33 C312 C35 146.7(32) . . ? C31 C312 C35 92.4(25) . . ? C313 C312 C35 50.8(23) . . ? C314 C312 C35 30.2(28) . . ? C32 C312 C35 169.9(11) . . ? C33 C312 C311 76.2(31) . . ? C31 C312 C311 134.1(15) . . ? C313 C312 C311 163.4(6) . . ? C314 C312 C311 97.5(19) . . ? C32 C312 C311 47.8(7) . . ? C35 C312 C311 126.4(23) . . ? C33 C312 C34 158.2(29) . . ? C31 C312 C34 138.6(16) . . ? C313 C312 C34 96.8(10) . . ? C314 C312 C34 16.6(20) . . ? C32 C312 C34 131.0(9) . . ? C35 C312 C34 46.2(23) . . ? C311 C312 C34 83.7(9) . . ? C33 C312 C38 124.8(31) . . ? C31 C312 C38 161.8(10) . . ? C313 C312 C38 127.5(10) . . ? C314 C312 C38 47.7(18) . . ? C32 C312 C38 97.7(8) . . ? C35 C312 C38 77.5(24) . . ? C311 C312 C38 50.0(7) . . ? C34 C312 C38 34.0(6) . . ? C31 C313 C310 147.0(15) . . ? C31 C313 C35 131.9(17) . . ? C310 C313 C35 80.6(15) . . ? C31 C313 C312 60.0(10) . . ? C310 C313 C312 153.0(11) . . ? C35 C313 C312 72.6(14) . . ? C31 C313 C314 111.4(17) . . ? C310 C313 C314 101.2(16) . . ? C35 C313 C314 20.6(20) . . ? C312 C313 C314 52.0(15) . . ? C31 C313 C33 26.6(14) . . ? C310 C313 C33 170.9(14) . . ? C35 C313 C33 105.2(19) . . ? C312 C313 C33 34.2(13) . . ? C314 C313 C33 84.9(19) . . ? C34 C314 C35 155.3(70) . . ? C34 C314 C36 79.6(37) . . ? C35 C314 C36 79.9(52) . . ? C34 C314 C38 47.1(49) . . ? C35 C314 C38 157.0(40) . . ? C36 C314 C38 122.0(19) . . ? C34 C314 C312 115.7(65) . . ? C35 C314 C312 81.0(32) . . ? C36 C314 C312 158.3(32) . . ? C38 C314 C312 78.4(22) . . ? C34 C314 C313 157.4(44) . . ? C35 C314 C313 34.1(32) . . ? C36 C314 C313 113.6(30) . . ? C38 C314 C313 124.3(18) . . ? C312 C314 C313 47.0(7) . . ? C34 C314 C39 102.5(42) . . ? C35 C314 C39 57.0(52) . . ? C36 C314 C39 23.1(16) . . ? C38 C314 C39 144.2(20) . . ? C312 C314 C39 137.3(33) . . ? C313 C314 C39 90.9(29) . . ? C34 C314 C37 121.9(48) . . ? C35 C314 C37 35.9(41) . . ? C36 C314 C37 44.1(15) . . ? C38 C314 C37 165.5(12) . . ? C312 C314 C37 115.9(22) . . ? C313 C314 C37 69.6(17) . . ? C39 C314 C37 21.4(16) . . ? _refine_diff_density_max 0.521 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.071 data_2-2PhCl #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common '2-2PhCl' _chemical_formula_moiety 'Co Cl2 O6 N6 C38 H26 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Co Cl2 O6 N6 C38 H26 ' _chemical_formula_weight 792.49 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co ? 0.299 0.973 'International Tables Vol. IV Table 2.2B' Cl ? 0.132 0.159 'International Tables Vol. IV Table 2.2B' O ? 0.008 0.006 'International Tables Vol. IV Table 2.2B' N ? 0.004 0.003 'International Tables Vol. IV Table 2.2B' C ? 0.002 0.002 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' #=============================================================================== # 6. CRYSTAL DATA _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,z 1/2-x,1/2-y,-z -x,y,1/2-z x,-y,1/2+z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 21.8140(12) _cell_length_b 11.52810(20) _cell_length_c 12.8767(7) _cell_angle_alpha 90.0 _cell_angle_beta 102.6740(10) _cell_angle_gamma 90.0 _cell_volume 3159.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 20.00 _cell_measurement_theta_max 25.00 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method ? _exptl_crystal_F_000 1622.92 _exptl_absorpt_coefficient_mu 0.77 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Omega scan b/P/b ' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 7457 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_reduction_process ? _reflns_number_total 3442 _reflns_number_observed 2783 _reflns_observed_criterion 'Inet > 4.0\s(Inet)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type atomblock _refine_ls_weighting_scheme 1/(\s^2^(F)+0.0000F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 2783 _refine_ls_number_parameters 215 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.057 _refine_ls_R_factor_obs 0.057 _refine_ls_wR_factor_all 0.074 _refine_ls_wR_factor_obs 0.074 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 5.53 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean ? _refine_diff_density_max 1.26 _refine_diff_density_min -1.29 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Co 0.50000 0.18630(6) 0.25000 0.0213(3) Uij ? S Co Cl31 0.15760(16) 1.1266(3) 0.2129(4) 0.230(4) Uij ? . Cl O1 0.52157(12) 0.18912(22) 0.09872(19) 0.0332(14) Uij ? . O O2 0.59310(17) 0.2779(3) 0.0375(3) 0.0761(24) Uij ? . O O3 0.60480(16) 0.0991(3) 0.0776(3) 0.075(3) Uij ? . O N1 0.57498(15) 0.1888(3) 0.07091(24) 0.0346(17) Uij ? . N N11 0.50000 0.3766(3) 0.25000 0.0276(23) Uij ? S N N12 0.50000 0.9943(3) 0.25000 0.0244(21) Uij ? S N N21 0.40336(13) 0.19969(25) 0.16141(22) 0.0260(15) Uij ? . N C11 0.48392(18) 0.4382(3) 0.1596(3) 0.0304(21) Uij ? . C C12 0.48299(19) 0.5569(3) 0.1557(3) 0.0328(22) Uij ? . C C13 0.50000 0.6204(4) 0.25000 0.028(3) Uij ? S C C14 0.50000 0.7493(4) 0.25000 0.026(3) Uij ? S C C15 0.51450(19) 0.8126(3) 0.1671(3) 0.0323(21) Uij ? . C C16 0.51375(18) 0.9326(3) 0.1700(3) 0.0305(21) Uij ? . C C21 0.38236(17) 0.1436(3) 0.0688(3) 0.0325(19) Uij ? . C C22 0.32343(17) 0.1611(3) 0.0043(3) 0.0337(19) Uij ? . C C23 0.28187(15) 0.2393(3) 0.0335(3) 0.0245(18) Uij ? . C C24 0.30340(17) 0.2961(3) 0.1298(3) 0.0329(19) Uij ? . C C25 0.36282(18) 0.2748(3) 0.1905(3) 0.0323(19) Uij ? . C C31 0.2097(3) 1.0317(6) 0.1667(7) 0.127(6) Uij ? . C C32 0.1917(5) 0.9752(9) 0.0832(7) 0.214(9) Uij ? . C C33 0.2375(8) 0.9042(9) 0.0491(7) 0.252(15) Uij ? . C C34 0.3015(4) 0.8887(6) 0.1118(7) 0.125(7) Uij ? . C C35 0.3104(3) 0.9568(6) 0.2035(6) 0.108(5) Uij ? . C C36 0.2697(3) 1.0272(5) 0.2343(5) 0.081(4) Uij ? . C H11 0.472 0.394 0.090 0.0390 Uiso ? . H H12 0.471 0.599 0.086 0.0406 Uiso ? . H H15 0.527 0.771 0.105 0.0411 Uiso ? . H H16 0.523 0.976 0.107 0.0400 Uiso ? . H H21 0.411 0.086 0.045 0.0403 Uiso ? . H H22 0.311 0.115 -0.064 0.0408 Uiso ? . H H24 0.275 0.352 0.156 0.0404 Uiso ? . H H25 0.377 0.318 0.259 0.0405 Uiso ? . H H32 0.146 0.983 0.047 0.1484 Uiso ? . H H33 0.220 0.869 -0.026 0.2014 Uiso ? . H H34 0.333 0.833 0.085 0.1321 Uiso ? . H H35 0.354 0.948 0.251 0.1222 Uiso ? . H H36 0.283 1.075 0.304 0.0929 Uiso ? . H 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 _atom_site_aniso_type_symbol Co 0.0200(3) 0.0154(3) 0.0250(3) 0.00000 -0.0025(3) 0.00000 Co Cl31 0.167(3) 0.195(3) 0.370(5) 0.0674(24) 0.152(3) 0.120(3) Cl O1 0.0312(14) 0.0373(15) 0.0301(13) 0.0032(12) 0.0046(11) -0.0015(12) O O2 0.0625(24) 0.067(3) 0.095(3) -0.0266(19) 0.0072(20) 0.0421(21) O O3 0.0545(23) 0.0528(23) 0.128(3) 0.0159(17) 0.0397(23) -0.0022(21) O N1 0.0345(18) 0.0339(18) 0.0333(17) -0.0067(15) 0.0025(14) 0.0014(15) N N11 0.0305(24) 0.0173(22) 0.0304(24) 0.00000 -0.0031(19) 0.00000 N N12 0.0260(23) 0.0170(21) 0.0266(22) 0.00000 -0.0019(18) 0.00000 N N21 0.0209(15) 0.0249(17) 0.0287(16) 0.0015(12) -0.0024(12) -0.0016(13) N C11 0.0417(23) 0.0210(20) 0.0251(19) 0.0004(16) -0.0003(16) -0.0005(15) C C12 0.0471(25) 0.0202(20) 0.0278(20) 0.0010(17) 0.0013(17) 0.0016(16) C C13 0.033(3) 0.016(3) 0.035(3) 0.00000 0.0032(24) 0.00000 C C14 0.032(3) 0.017(3) 0.027(3) 0.00000 -0.0015(22) 0.00000 C C15 0.0472(23) 0.0191(19) 0.0312(20) -0.0011(17) 0.0099(17) -0.0027(17) C C16 0.0377(22) 0.0189(19) 0.0350(20) 0.0003(16) 0.0082(17) 0.0015(16) C C21 0.0227(19) 0.0326(21) 0.0381(22) 0.0045(16) -0.0020(16) -0.0112(17) C C22 0.0277(20) 0.0374(24) 0.0310(20) 0.0044(16) -0.0042(16) -0.0127(17) C C23 0.0192(18) 0.0242(19) 0.0272(19) 0.0000(14) -0.0007(15) 0.0000(15) C C24 0.0247(20) 0.0362(24) 0.0336(20) 0.0098(16) -0.0025(16) -0.0095(17) C C25 0.0285(21) 0.0319(21) 0.0316(20) 0.0051(16) -0.0044(16) -0.0096(17) C C31 0.061(4) 0.113(6) 0.211(8) 0.003(4) 0.041(5) 0.105(6) C C32 0.243(11) 0.209(10) 0.128(7) -0.199(10) -0.097(7) 0.063(7) C C33 0.521(25) 0.126(8) 0.125(8) -0.195(12) 0.106(11) -0.053(6) C C34 0.184(9) 0.063(5) 0.154(7) -0.041(5) 0.089(6) -0.005(4) C C35 0.074(5) 0.096(5) 0.158(7) -0.006(4) 0.035(4) 0.064(5) C C36 0.088(5) 0.076(4) 0.082(4) -0.020(3) 0.023(3) 0.032(3) C #=============================================================================== # 10. MOLECULAR GEOMETRY 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 Co O1 2.1022(25) ? ? ? Co O1a 2.1022(25) ? ? ? Cl31 C31 1.772(9) ? ? ? O1 N1 1.292(4) ? ? ? O2 N1 1.213(4) ? ? ? O3 N1 1.215(5) ? ? ? N11 C11 1.343(4) ? ? ? N11 C11a 1.343(4) ? ? ? N11 Ct 1.399(4) ? ? ? N12 C16 1.339(4) ? ? ? N12 C16a 1.339(4) ? ? ? N12 Ct2b 1.406(4) ? ? ? N21 C21 1.346(5) ? ? ? N21 C25 1.348(5) ? ? ? N21 Ct4 1.409(3) ? ? ? C11 C12 1.369(5) ? ? ? C11 H11 1.011(3) ? ? ? C11 Ct 1.331(3) ? ? ? C12 C13 1.397(4) ? ? ? C12 H12 1.005(4) ? ? ? C12 Ct 1.371(4) ? ? ? C13 C12a 1.397(4) ? ? ? C13 C14 1.486(7) ? ? ? C13 Ct 1.413(5) ? ? ? C14 C15 1.385(4) ? ? ? C14 C15a 1.385(4) ? ? ? C14 Ct2b 1.418(5) ? ? ? C15 C16 1.384(5) ? ? ? C15 H15 1.015(4) ? ? ? C15 Ct2b 1.364(4) ? ? ? C16 H16 1.017(4) ? ? ? C16 Ct2b 1.330(4) ? ? ? C21 C22 1.384(5) ? ? ? C21 H21 1.004(4) ? ? ? C21 Ct4 1.336(4) ? ? ? C22 C23 1.388(5) ? ? ? C22 H22 1.012(4) ? ? ? C22 Ct4 1.364(3) ? ? ? C23 C23c 1.487(6) ? ? ? C23 C24 1.390(5) ? ? ? C23 Ct4 1.425(3) ? ? ? C24 C25 1.381(5) ? ? ? C24 H24 1.006(4) ? ? ? C24 Ct4 1.361(4) ? ? ? C25 H25 1.008(4) ? ? ? C25 Ct4 1.339(4) ? ? ? C31 C32 1.246(13) ? ? ? C31 C36 1.405(10) ? ? ? C31 Ct3 1.327(8) ? ? ? C32 C33 1.434(21) ? ? ? C32 H32 1.013(10) ? ? ? C32 Ct3 1.397(9) ? ? ? C33 C34 1.462(19) ? ? ? C33 H33 1.040(9) ? ? ? C33 Ct3 1.352(8) ? ? ? C34 C35 1.395(12) ? ? ? C34 H34 1.050(8) ? ? ? C34 Ct3 1.475(9) ? ? ? C35 C36 1.326(10) ? ? ? C35 H35 1.010(7) ? ? ? C35 Ct3 1.325(7) ? ? ? C36 H36 1.036(6) ? ? ? C36 Ct3 1.379(6) ? ? ? Ct C11a 1.331(3) ? ? ? Ct C12a 1.371(4) ? ? ? Ct2 N12d 1.406(4) ? ? ? Ct2 C14d 1.418(5) ? ? ? Ct2 C15d 1.364(4) ? ? ? Ct2 C15e 1.364(4) ? ? ? Ct2 C16d 1.330(4) ? ? ? Ct2 C16e 1.330(4) ? ? ? 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 ? ? ? ? ? ? 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 Co O1a 178.23(11) ? ? ? ? Co O1 N1 130.97(21) ? ? ? ? O1 N1 O2 118.7(3) ? ? ? ? O1 N1 O3 119.0(3) ? ? ? ? O2 N1 O3 122.3(4) ? ? ? ? C11 N11 C11a 116.1(4) ? ? ? ? C11 N11 Ct 58.03(21) ? ? ? ? C11a N11 Ct 58.03(21) ? ? ? ? C16 N12 C16a 115.8(4) ? ? ? ? C16 N12 Ct2b 57.89(21) ? ? ? ? C16a N12 Ct2b 57.89(21) ? ? ? ? C21 N21 C25 116.0(3) ? ? ? ? C21 N21 Ct4 57.96(19) ? ? ? ? C25 N21 Ct4 58.04(19) ? ? ? ? N11 C11 C12 124.1(3) ? ? ? ? N11 C11 H11 117.9(3) ? ? ? ? N11 C11 Ct 63.08(21) ? ? ? ? C12 C11 H11 118.0(3) ? ? ? ? C12 C11 Ct 61.00(21) ? ? ? ? H11 C11 Ct 178.7(4) ? ? ? ? C11 C12 C13 119.5(3) ? ? ? ? C11 C12 H12 121.0(3) ? ? ? ? C11 C12 Ct 58.12(21) ? ? ? ? C13 C12 H12 119.5(4) ? ? ? ? C13 C12 Ct 61.38(23) ? ? ? ? H12 C12 Ct 178.8(4) ? ? ? ? C12 C13 C12a 116.8(4) ? ? ? ? C12 C13 C14 121.60(22) ? ? ? ? C12 C13 Ct 58.40(22) ? ? ? ? C12a C13 C14 121.60(22) ? ? ? ? C12a C13 Ct 58.40(22) ? ? ? ? C14 C13 Ct 180.0 ? ? ? ? C13 C14 C15 121.76(22) ? ? ? ? C13 C14 C15a 121.76(22) ? ? ? ? C13 C14 Ct2b 180.0 ? ? ? ? C15 C14 C15a 116.5(4) ? ? ? ? C15 C14 Ct2b 58.24(22) ? ? ? ? C15a C14 Ct2b 58.24(22) ? ? ? ? C14 C15 C16 120.0(3) ? ? ? ? C14 C15 H15 120.0(4) ? ? ? ? C14 C15 Ct2b 62.09(23) ? ? ? ? C16 C15 H15 120.0(3) ? ? ? ? C16 C15 Ct2b 57.86(21) ? ? ? ? H15 C15 Ct2b 177.5(4) ? ? ? ? N12 C16 C15 123.9(3) ? ? ? ? N12 C16 H16 118.3(3) ? ? ? ? N12 C16 Ct2b 63.61(22) ? ? ? ? C15 C16 H16 117.8(3) ? ? ? ? C15 C16 Ct2b 60.32(21) ? ? ? ? H16 C16 Ct2b 177.7(4) ? ? ? ? N21 C21 C22 123.6(3) ? ? ? ? N21 C21 H21 117.8(3) ? ? ? ? N21 C21 Ct4 63.39(20) ? ? ? ? C22 C21 H21 118.6(3) ? ? ? ? C22 C21 Ct4 60.17(21) ? ? ? ? H21 C21 Ct4 178.8(4) ? ? ? ? C21 C22 C23 120.5(3) ? ? ? ? C21 C22 H22 119.3(4) ? ? ? ? C21 C22 Ct4 58.17(21) ? ? ? ? C23 C22 H22 120.2(3) ? ? ? ? C23 C22 Ct4 62.37(21) ? ? ? ? H22 C22 Ct4 177.3(4) ? ? ? ? C22 C23 C23c 122.2(3) ? ? ? ? C22 C23 C24 115.8(3) ? ? ? ? C22 C23 Ct4 58.00(19) ? ? ? ? C23c C23 C24 122.0(3) ? ? ? ? C23c C23 Ct4 179.8(3) ? ? ? ? C24 C23 Ct4 57.79(19) ? ? ? ? C23 C24 C25 120.8(3) ? ? ? ? C23 C24 H24 119.6(3) ? ? ? ? C23 C24 Ct4 62.39(21) ? ? ? ? C25 C24 H24 119.5(3) ? ? ? ? C25 C24 Ct4 58.45(21) ? ? ? ? H24 C24 Ct4 177.6(4) ? ? ? ? N21 C25 C24 123.3(3) ? ? ? ? N21 C25 H25 118.4(3) ? ? ? ? N21 C25 Ct4 63.25(20) ? ? ? ? C24 C25 H25 118.3(3) ? ? ? ? C24 C25 Ct4 60.03(21) ? ? ? ? H25 C25 Ct4 178.3(4) ? ? ? ? Cl31 C31 C32 120.6(8) ? ? ? ? Cl31 C31 C36 113.2(7) ? ? ? ? Cl31 C31 Ct3 173.8(7) ? ? ? ? C32 C31 C36 126.2(9) ? ? ? ? C32 C31 Ct3 65.7(8) ? ? ? ? C36 C31 Ct3 60.5(4) ? ? ? ? C31 C32 C33 117.0(9) ? ? ? ? C31 C32 H32 116.3(13) ? ? ? ? C31 C32 Ct3 60.0(4) ? ? ? ? C33 C32 H32 126.7(9) ? ? ? ? C33 C32 Ct3 57.0(7) ? ? ? ? H32 C32 Ct3 175.1(11) ? ? ? ? C32 C33 C34 123.1(7) ? ? ? ? C32 C33 H33 111.1(13) ? ? ? ? C32 C33 Ct3 60.1(5) ? ? ? ? C34 C33 H33 125.8(13) ? ? ? ? C34 C33 Ct3 63.1(6) ? ? ? ? H33 C33 Ct3 170.4(16) ? ? ? ? C33 C34 C35 109.7(8) ? ? ? ? C33 C34 H34 120.5(8) ? ? ? ? C33 C34 Ct3 54.8(5) ? ? ? ? C35 C34 H34 129.8(9) ? ? ? ? C35 C34 Ct3 54.9(4) ? ? ? ? H34 C34 Ct3 175.3(8) ? ? ? ? C34 C35 C36 128.3(7) ? ? ? ? C34 C35 H35 112.9(7) ? ? ? ? C34 C35 Ct3 65.6(5) ? ? ? ? C36 C35 H35 118.8(8) ? ? ? ? C36 C35 Ct3 62.7(4) ? ? ? ? H35 C35 Ct3 177.5(7) ? ? ? ? C31 C36 C35 115.6(7) ? ? ? ? C31 C36 H36 124.1(7) ? ? ? ? C31 C36 Ct3 56.9(5) ? ? ? ? C35 C36 H36 120.3(6) ? ? ? ? C35 C36 Ct3 58.6(5) ? ? ? ? H36 C36 Ct3 178.5(6) ? ? ? ? N11 Ct C11 58.89(15) ? ? ? ? N11 Ct C11a 58.89(15) ? ? ? ? N11 Ct C12 119.77(15) ? ? ? ? N11 Ct C12a 119.77(15) ? ? ? ? N11 Ct C13 180.0 ? ? ? ? C11 Ct C11a 117.78(22) ? ? ? ? C11 Ct C12 60.88(22) ? ? ? ? C11 Ct C12a 178.65(22) ? ? ? ? C11 Ct C13 121.11(15) ? ? ? ? C11a Ct C12 178.65(22) ? ? ? ? C11a Ct C12a 60.88(22) ? ? ? ? C11a Ct C13 121.11(15) ? ? ? ? C12 Ct C12a 120.46(22) ? ? ? ? C12 Ct C13 60.23(15) ? ? ? ? C12a Ct C13 60.23(15) ? ? ? ? N12d Ct2 C14d 180.0 ? ? ? ? N12d Ct2 C15d 120.33(15) ? ? ? ? N12d Ct2 C15e 120.33(15) ? ? ? ? N12d Ct2 C16d 58.51(16) ? ? ? ? N12d Ct2 C16e 58.51(16) ? ? ? ? C14d Ct2 C15d 59.67(15) ? ? ? ? C14d Ct2 C15e 59.67(15) ? ? ? ? C14d Ct2 C16d 121.49(16) ? ? ? ? C14d Ct2 C16e 121.49(16) ? ? ? ? C15d Ct2 C15e 119.35(22) ? ? ? ? C15d Ct2 C16d 61.82(22) ? ? ? ? C15d Ct2 C16e 178.81(22) ? ? ? ? C15e Ct2 C16d 178.81(22) ? ? ? ? C15e Ct2 C16e 61.82(22) ? ? ? ? C16d Ct2 C16e 117.01(22) ? ? ? ? C31 Ct3 C32 54.4(7) ? ? ? ? C31 Ct3 C33 117.1(8) ? ? ? ? C31 Ct3 C34 179.2(5) ? ? ? ? C31 Ct3 C35 121.2(5) ? ? ? ? C31 Ct3 C36 62.5(5) ? ? ? ? C32 Ct3 C33 62.8(9) ? ? ? ? C32 Ct3 C34 124.9(6) ? ? ? ? C32 Ct3 C35 175.3(6) ? ? ? ? C32 Ct3 C36 116.9(6) ? ? ? ? C33 Ct3 C34 62.1(8) ? ? ? ? C33 Ct3 C35 121.6(8) ? ? ? ? C33 Ct3 C36 178.7(5) ? ? ? ? C34 Ct3 C35 59.5(5) ? ? ? ? C34 Ct3 C36 118.2(4) ? ? ? ? C35 Ct3 C36 58.7(5) ? ? ? ? N21 Ct4 C21 58.65(19) ? ? ? ? N21 Ct4 C22 120.32(19) ? ? ? ? N21 Ct4 C23 179.59(19) ? ? ? ? N21 Ct4 C24 120.23(19) ? ? ? ? N21 Ct4 C25 58.71(20) ? ? ? ? C21 Ct4 C22 61.66(22) ? ? ? ? C21 Ct4 C23 121.30(21) ? ? ? ? C21 Ct4 C24 178.86(21) ? ? ? ? C21 Ct4 C25 117.36(22) ? ? ? ? C22 Ct4 C23 59.63(21) ? ? ? ? C22 Ct4 C24 119.45(21) ? ? ? ? C22 Ct4 C25 179.01(22) ? ? ? ? C23 Ct4 C24 59.82(20) ? ? ? ? C23 Ct4 C25 121.34(21) ? ? ? ? C24 Ct4 C25 61.52(22) ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? #=============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #=============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ data_2-2PhCl2 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common '2-2PhCl2' _chemical_formula_moiety 'Co Cl4 N6 O6 C54 H24 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Co Cl4 N6 O6 C54 H24 ' _chemical_formula_weight 1053.55 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co ? 0.299 0.973 'International Tables Vol. IV Table 2.2B' Cl ? 0.132 0.159 'International Tables Vol. IV Table 2.2B' N ? 0.004 0.003 'International Tables Vol. IV Table 2.2B' O ? 0.008 0.006 'International Tables Vol. IV Table 2.2B' C ? 0.002 0.002 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' #=============================================================================== # 6. CRYSTAL DATA _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,z 1/2-x,1/2-y,-z -x,y,1/2-z x,-y,1/2+z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 21.6458(13) _cell_length_b 11.5193(7) _cell_length_c 13.3717(8) _cell_angle_alpha 90.0 _cell_angle_beta 102.6680(*) _cell_angle_gamma 90.0 _cell_volume 3253.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 20.00 _cell_measurement_theta_max 25.00 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_method ? _exptl_crystal_F_000 2136.11 _exptl_absorpt_coefficient_mu 0.94 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Omega scan b/P/b ' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 8972 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_reduction_process ? _reflns_number_total 3547 _reflns_number_observed 3036 _reflns_observed_criterion 'Inet > 3.0\s(Inet)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type atomblock _refine_ls_weighting_scheme 1/(\s^2^(F)+0.0002F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 3037 _refine_ls_number_parameters 224 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.062 _refine_ls_R_factor_obs 0.062 _refine_ls_wR_factor_all 0.089 _refine_ls_wR_factor_obs 0.089 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.94 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean ? _refine_diff_density_max 0.89 _refine_diff_density_min -0.88 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Co 0.50000 0.19016(4) 0.25000 0.0262(3) Uij ? S Co Cl1 0.87574(8) 0.05856(14) 0.40568(16) 0.1134(13) Uij ? . Cl Cl2 0.77554(16) 0.12838(22) 0.20873(16) 0.1869(24) Uij ? . Cl O1 0.52268(12) 0.19234(19) 0.10362(18) 0.0430(13) Uij ? . O O2 0.59497(18) 0.2782(3) 0.0443(3) 0.097(3) Uij ? . O O3 0.59968(17) 0.0966(3) 0.0656(3) 0.0877(25) Uij ? . O N1 0.57394(14) 0.18931(22) 0.07131(21) 0.0390(15) Uij ? . N N11 0.50000 0.3796(3) 0.25000 0.0326(19) Uij ? S N N12 0.50000 -0.0029(3) 0.25000 0.0302(18) Uij ? S N N21 0.40266(12) 0.20227(20) 0.16163(21) 0.0306(13) Uij ? . N C11 0.48119(17) 0.4410(3) 0.16274(24) 0.0379(18) Uij ? . C C12 0.48054(18) 0.5601(3) 0.15989(25) 0.0391(19) Uij ? . C C13 0.50000 0.6240(4) 0.25000 0.0327(24) Uij ? S C C14 0.50000 -0.2476(4) 0.25000 0.0330(23) Uij ? S C C15 0.51297(17) -0.1836(3) 0.1680(3) 0.0381(20) Uij ? . C C16 0.51238(16) -0.0640(3) 0.17129(25) 0.0364(18) Uij ? . C C21 0.38360(16) 0.1470(3) 0.0718(3) 0.0400(18) Uij ? . C C22 0.32542(16) 0.1627(3) 0.0063(3) 0.0393(17) Uij ? . C C23 0.28189(14) 0.2397(3) 0.03389(23) 0.0293(16) Uij ? . C C24 0.30137(16) 0.2958(3) 0.1275(3) 0.0367(17) Uij ? . C C25 0.36086(16) 0.2751(3) 0.18729(25) 0.0371(17) Uij ? . C C111 0.80008(22) 0.0019(4) 0.3821(3) 0.061(3) Uij ? . C C112 0.7558(3) 0.0315(4) 0.2936(4) 0.083(4) Uij ? . C C113 0.6956(3) -0.0144(5) 0.2765(4) 0.093(4) Uij ? . C C114 0.6808(3) -0.0898(5) 0.3495(5) 0.100(4) Uij ? . C C115 0.7214(3) -0.1155(4) 0.4327(5) 0.090(4) Uij ? . C C116 0.78215(24) -0.0708(4) 0.4490(4) 0.073(3) Uij ? . C H11 0.467 0.398 0.096 0.0457 Uiso ? . H H12 0.466 0.602 0.092 0.0472 Uiso ? . H H15 0.523 -0.225 0.108 0.0474 Uiso ? . H H16 0.521 -0.019 0.112 0.0450 Uiso ? . H H21 0.413 0.089 0.052 0.0471 Uiso ? . H H22 0.314 0.119 -0.060 0.0465 Uiso ? . H H24 0.272 0.349 0.153 0.0440 Uiso ? . H H25 0.373 0.318 0.254 0.0456 Uiso ? . H H113 0.663 0.007 0.212 0.0979 Uiso ? . H H114 0.636 -0.122 0.333 0.1125 Uiso ? . H H115 0.709 -0.169 0.483 0.1092 Uiso ? . H H116 0.814 -0.095 0.514 0.0846 Uiso ? . H 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 _atom_site_aniso_type_symbol Co 0.0232(3) 0.0164(3) 0.0345(3) 0.00000 -0.00335(24) 0.00000 Co Cl1 0.0876(12) 0.0994(11) 0.1637(16) -0.0141(9) 0.0506(11) -0.0142(11) Cl Cl2 0.317(4) 0.1592(19) 0.1200(15) 0.0898(22) 0.1249(21) 0.0685(15) Cl O1 0.0370(14) 0.0459(15) 0.0440(14) 0.0048(10) 0.0042(12) 0.0003(11) O O2 0.083(3) 0.0748(23) 0.132(3) -0.0295(19) 0.0205(24) 0.0421(22) O O3 0.0745(25) 0.0631(20) 0.139(3) 0.0200(16) 0.0539(24) 0.0075(20) O N1 0.0388(17) 0.0383(16) 0.0366(15) -0.0065(12) 0.0011(13) 0.0030(12) N N11 0.0339(21) 0.0181(17) 0.0414(21) 0.00000 -0.0012(17) 0.00000 N N12 0.0319(20) 0.0184(17) 0.0356(19) 0.00000 -0.0029(16) 0.00000 N N21 0.0255(14) 0.0247(13) 0.0371(14) 0.0018(10) -0.0025(11) -0.0013(10) N C11 0.0449(21) 0.0232(16) 0.0391(18) -0.0010(14) -0.0047(16) 0.0006(13) C C12 0.0503(22) 0.0239(16) 0.0386(18) 0.0000(14) 0.0002(16) 0.0047(14) C C13 0.0320(25) 0.0199(21) 0.044(3) 0.00000 0.0039(21) 0.00000 C C14 0.035(3) 0.0194(22) 0.042(3) 0.00000 0.0015(21) 0.00000 C C15 0.0483(22) 0.0228(16) 0.0428(19) 0.0009(14) 0.0095(16) -0.0031(13) C C16 0.0406(20) 0.0210(16) 0.0461(19) 0.0000(13) 0.0062(16) 0.0040(14) C C21 0.0278(17) 0.0349(18) 0.0513(21) 0.0032(14) -0.0043(16) -0.0130(16) C C22 0.0300(18) 0.0402(19) 0.0417(19) 0.0069(14) -0.0048(15) -0.0125(15) C C23 0.0240(16) 0.0275(16) 0.0336(16) -0.0005(12) 0.0004(13) 0.0014(13) C C24 0.0286(17) 0.0384(20) 0.0396(18) 0.0067(13) 0.0000(15) -0.0097(14) C C25 0.0301(18) 0.0381(18) 0.0377(18) 0.0042(14) -0.0043(15) -0.0088(14) C C111 0.069(3) 0.0483(24) 0.072(3) 0.0091(20) 0.0272(24) -0.0073(21) C C112 0.139(5) 0.056(3) 0.065(3) 0.029(3) 0.045(3) -0.0018(23) C C113 0.084(4) 0.110(4) 0.071(3) 0.049(3) -0.014(3) -0.034(3) C C114 0.076(4) 0.080(4) 0.137(5) 0.016(3) 0.009(4) -0.034(4) C C115 0.073(4) 0.051(3) 0.151(5) 0.0114(25) 0.039(4) 0.011(3) C C116 0.064(3) 0.066(3) 0.092(3) 0.0235(23) 0.021(3) 0.012(3) C #=============================================================================== # 10. MOLECULAR GEOMETRY 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 Co O1 2.1200(25) ? ? ? Co O1a 2.1200(25) ? ? ? Cl1 C111 1.727(5) ? ? ? Cl2 C112 1.711(5) ? ? ? Cl2 E7 2.143(3) ? ? ? O1 N1 1.276(4) ? ? ? O2 N1 1.207(4) ? ? ? O3 N1 1.215(4) ? ? ? N11 C11 1.349(4) ? ? ? N11 C11a 1.349(4) ? ? ? N11 Ct 1.398(3) ? ? ? N12 C16 1.341(4) ? ? ? N12 C16a 1.341(4) ? ? ? N12 Ct3 1.398(3) ? ? ? N21 C21 1.342(4) ? ? ? N21 C25 1.333(4) ? ? ? N21 Ct2 1.404(3) ? ? ? C11 C12 1.373(4) ? ? ? C11 H11 1.001(3) ? ? ? C11 Ct 1.340(3) ? ? ? C11 E1a 0.687(3) ? ? ? C11 E2 0.687(3) ? ? ? C12 C13 1.396(4) ? ? ? C12 H12 1.008(3) ? ? ? C12 Ct 1.368(3) ? ? ? C12 E1a 0.687(3) ? ? ? C12 E2 0.687(3) ? ? ? C13 C12a 1.396(4) ? ? ? C13 C14b 1.479(6) ? ? ? C13 Ct 1.417(4) ? ? ? C14 C13c 1.479(6) ? ? ? C14 C15 1.401(4) ? ? ? C14 C15a 1.401(4) ? ? ? C14 Ct3 1.421(4) ? ? ? C15 C16 1.379(4) ? ? ? C15 H15 1.006(3) ? ? ? C15 Ct3 1.373(3) ? ? ? C15 E5 0.689(3) ? ? ? C15 E6a 0.689(3) ? ? ? C16 H16 1.000(3) ? ? ? C16 Ct3 1.336(3) ? ? ? C16 E5 0.689(3) ? ? ? C16 E6a 0.689(3) ? ? ? C21 C22 1.379(5) ? ? ? C21 H21 1.004(3) ? ? ? C21 Ct2 1.327(3) ? ? ? C21 E3 0.690(3) ? ? ? C22 C23 1.401(4) ? ? ? C22 H22 1.005(3) ? ? ? C22 Ct2 1.374(3) ? ? ? C22 E3 0.690(3) ? ? ? C23 C23d 1.495(6) ? ? ? C23 C24 1.390(4) ? ? ? C23 Ct2 1.421(3) ? ? ? C24 C25 1.380(5) ? ? ? C24 H24 0.999(3) ? ? ? C24 Ct2 1.364(3) ? ? ? C24 E4 0.690(3) ? ? ? C25 H25 1.006(3) ? ? ? C25 Ct2 1.330(3) ? ? ? C25 E4 0.690(3) ? ? ? C111 C112 1.392(7) ? ? ? C111 C116 1.344(7) ? ? ? C111 Ct4 1.384(5) ? ? ? C111 E8 1.808(5) ? ? ? C112 C113 1.379(9) ? ? ? C112 Ct4 1.376(5) ? ? ? C112 E7 0.689(6) ? ? ? C113 C114 1.396(10) ? ? ? C113 H113 1.014(5) ? ? ? C113 Ct4 1.373(5) ? ? ? C113 E7 0.689(7) ? ? ? C114 C115 1.292(9) ? ? ? C114 H114 1.013(6) ? ? ? C114 Ct4 1.352(6) ? ? ? C114 E7 1.828(7) ? ? ? C114 E8 1.741(6) ? ? ? C115 C116 1.385(8) ? ? ? C115 H115 0.997(6) ? ? ? C115 Ct4 1.362(6) ? ? ? C115 E8 0.693(6) ? ? ? C116 H116 1.019(5) ? ? ? C116 Ct4 1.341(5) ? ? ? C116 E8 0.692(5) ? ? ? H11 E1a 1.45527(6) ? ? ? H11 E2 1.45536(6) ? ? ? H12 E1a 1.47506(6) ? ? ? H12 E2 1.47516(6) ? ? ? H15 E5 1.47988(6) ? ? ? H15 E6a 1.47986(6) ? ? ? H16 E5 1.46485(7) ? ? ? H16 E6a 1.46483(7) ? ? ? H21 E3 1.46066(7) ? ? ? H22 E3 1.47835(7) ? ? ? H24 E4 1.47060(7) ? ? ? H25 E4 1.46175(6) ? ? ? H113 E7 1.48306(7) ? ? ? H115 E8 1.47656(5) ? ? ? H116 E8 1.48101(7) ? ? ? Ct C11a 1.340(3) ? ? ? Ct C12a 1.368(3) ? ? ? Ct E1 1.16731(7) ? ? ? Ct E1a 1.16731(7) ? ? ? Ct E2 1.16716(7) ? ? ? Ct E2a 1.16716(7) ? ? ? Ct2 E3 1.16114(5) ? ? ? Ct2 E4 1.15736(5) ? ? ? Ct3 C15a 1.373(3) ? ? ? Ct3 C16a 1.336(3) ? ? ? Ct3 E5 1.16605(6) ? ? ? Ct3 E5a 1.16606(6) ? ? ? Ct3 E6 1.16609(6) ? ? ? Ct3 E6a 1.16609(6) ? ? ? Ct4 E7 1.18892(6) ? ? ? Ct4 E8 1.16024(5) ? ? ? E1 C11a 0.687(3) ? ? ? E1 C12a 0.687(3) ? ? ? E1 H11a 1.45527(6) ? ? ? E1 H12a 1.47506(6) ? ? ? E6 C15a 0.689(3) ? ? ? E6 C16a 0.689(3) ? ? ? E6 H15a 1.47986(6) ? ? ? E6 H16a 1.46483(7) ? ? ? 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 ? ? ? ? ? ? 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 Co O1a 178.64(9) ? ? ? ? C112 Cl2 E7 16.13(22) ? ? ? ? Co O1 N1 134.96(20) ? ? ? ? O1 N1 O2 119.4(3) ? ? ? ? O1 N1 O3 119.3(3) ? ? ? ? O2 N1 O3 121.2(4) ? ? ? ? C11 N11 C11a 116.7(3) ? ? ? ? C11 N11 Ct 58.37(18) ? ? ? ? C11a N11 Ct 58.37(18) ? ? ? ? C16 N12 C16a 116.7(3) ? ? ? ? C16 N12 Ct3 58.37(18) ? ? ? ? C16a N12 Ct3 58.37(18) ? ? ? ? C21 N21 C25 115.9(3) ? ? ? ? C21 N21 Ct2 57.76(17) ? ? ? ? C25 N21 Ct2 58.10(17) ? ? ? ? N11 C11 C12 123.2(3) ? ? ? ? N11 C11 H11 118.8(3) ? ? ? ? N11 C11 Ct 62.67(19) ? ? ? ? N11 C11 E1a 123.2(4) ? ? ? ? N11 C11 E2 123.2(4) ? ? ? ? C12 C11 H11 118.0(3) ? ? ? ? C12 C11 Ct 60.53(19) ? ? ? ? C12 C11 E1a 0.02(12) ? ? ? ? C12 C11 E2 0.0 ? ? ? ? H11 C11 Ct 178.4(3) ? ? ? ? H11 C11 E1a 118.0(4) ? ? ? ? H11 C11 E2 118.0(4) ? ? ? ? Ct C11 E1a 60.54(23) ? ? ? ? Ct C11 E2 60.52(23) ? ? ? ? E1a C11 E2 0.1 ? ? ? ? C11 C12 C13 120.2(3) ? ? ? ? C11 C12 H12 119.8(3) ? ? ? ? C11 C12 Ct 58.55(18) ? ? ? ? C11 C12 E1a 0.02(12) ? ? ? ? C11 C12 E2 0.0 ? ? ? ? C13 C12 H12 119.9(3) ? ? ? ? C13 C12 Ct 61.70(20) ? ? ? ? C13 C12 E1a 120.3(4) ? ? ? ? C13 C12 E2 120.2(4) ? ? ? ? H12 C12 Ct 178.4(3) ? ? ? ? H12 C12 E1a 119.8(4) ? ? ? ? H12 C12 E2 119.8(4) ? ? ? ? Ct C12 E1a 58.56(22) ? ? ? ? Ct C12 E2 58.55(22) ? ? ? ? E1a C12 E2 0.1 ? ? ? ? C12 C13 C12a 116.4(3) ? ? ? ? C12 C13 C14b 121.82(19) ? ? ? ? C12 C13 Ct 58.18(19) ? ? ? ? C12a C13 C14b 121.82(19) ? ? ? ? C12a C13 Ct 58.18(19) ? ? ? ? C14b C13 Ct 180.0 ? ? ? ? C13c C14 C15 121.79(19) ? ? ? ? C13c C14 C15a 121.79(19) ? ? ? ? C13c C14 Ct3 180.0 ? ? ? ? C15 C14 C15a 116.4(3) ? ? ? ? C15 C14 Ct3 58.21(19) ? ? ? ? C15a C14 Ct3 58.21(19) ? ? ? ? C14 C15 C16 119.7(3) ? ? ? ? C14 C15 H15 119.8(3) ? ? ? ? C14 C15 Ct3 61.63(21) ? ? ? ? C14 C15 E5 119.7(4) ? ? ? ? C14 C15 E6a 119.7(4) ? ? ? ? C16 C15 H15 120.4(3) ? ? ? ? C16 C15 Ct3 58.12(19) ? ? ? ? C16 C15 E5 0.0 ? ? ? ? C16 C15 E6a 0.02(17) ? ? ? ? H15 C15 Ct3 178.2(3) ? ? ? ? H15 C15 E5 120.4(4) ? ? ? ? H15 C15 E6a 120.4(4) ? ? ? ? Ct3 C15 E5 58.11(23) ? ? ? ? Ct3 C15 E6a 58.12(23) ? ? ? ? E5 C15 E6a 0.1 ? ? ? ? N12 C16 C15 123.7(3) ? ? ? ? N12 C16 H16 117.3(3) ? ? ? ? N12 C16 Ct3 62.96(19) ? ? ? ? N12 C16 E5 123.7(4) ? ? ? ? N12 C16 E6a 123.7(4) ? ? ? ? C15 C16 H16 119.1(3) ? ? ? ? C15 C16 Ct3 60.72(20) ? ? ? ? C15 C16 E5 0.0 ? ? ? ? C15 C16 E6a 0.02(17) ? ? ? ? H16 C16 Ct3 179.4(3) ? ? ? ? H16 C16 E5 119.1(4) ? ? ? ? H16 C16 E6a 119.1(4) ? ? ? ? Ct3 C16 E5 60.71(23) ? ? ? ? Ct3 C16 E6a 60.71(23) ? ? ? ? E5 C16 E6a 0.1 ? ? ? ? N21 C21 C22 124.4(3) ? ? ? ? N21 C21 H21 117.5(3) ? ? ? ? N21 C21 Ct2 63.46(18) ? ? ? ? N21 C21 E3 124.4(4) ? ? ? ? C22 C21 H21 118.0(3) ? ? ? ? C22 C21 Ct2 60.97(20) ? ? ? ? C22 C21 E3 0.0 ? ? ? ? H21 C21 Ct2 178.0(4) ? ? ? ? H21 C21 E3 118.0(4) ? ? ? ? Ct2 C21 E3 60.96(24) ? ? ? ? C21 C22 C23 119.2(3) ? ? ? ? C21 C22 H22 120.4(3) ? ? ? ? C21 C22 Ct2 57.64(19) ? ? ? ? C21 C22 E3 0.0 ? ? ? ? C23 C22 H22 120.4(3) ? ? ? ? C23 C22 Ct2 61.60(18) ? ? ? ? C23 C22 E3 119.2(4) ? ? ? ? H22 C22 Ct2 178.0(3) ? ? ? ? H22 C22 E3 120.4(4) ? ? ? ? Ct2 C22 E3 57.63(23) ? ? ? ? C22 C23 C23d 121.7(3) ? ? ? ? C22 C23 C24 116.3(3) ? ? ? ? C22 C23 Ct2 58.25(17) ? ? ? ? C23d C23 C24 121.9(3) ? ? ? ? C23d C23 Ct2 179.7(3) ? ? ? ? C24 C23 Ct2 58.07(18) ? ? ? ? C23 C24 C25 120.1(3) ? ? ? ? C23 C24 H24 119.9(3) ? ? ? ? C23 C24 Ct2 62.11(18) ? ? ? ? C23 C24 E4 120.1(4) ? ? ? ? C25 C24 H24 119.9(3) ? ? ? ? C25 C24 Ct2 57.98(19) ? ? ? ? C25 C24 E4 0.0 ? ? ? ? H24 C24 Ct2 177.1(3) ? ? ? ? H24 C24 E4 119.9(4) ? ? ? ? Ct2 C24 E4 57.98(22) ? ? ? ? N21 C25 C24 124.1(3) ? ? ? ? N21 C25 H25 118.0(3) ? ? ? ? N21 C25 Ct2 63.63(18) ? ? ? ? N21 C25 E4 124.1(4) ? ? ? ? C24 C25 H25 117.9(3) ? ? ? ? C24 C25 Ct2 60.44(19) ? ? ? ? C24 C25 E4 0.02(6) ? ? ? ? H25 C25 Ct2 178.4(3) ? ? ? ? H25 C25 E4 117.9(4) ? ? ? ? Ct2 C25 E4 60.44(23) ? ? ? ? Cl1 C111 C112 120.7(4) ? ? ? ? Cl1 C111 C116 121.0(4) ? ? ? ? Cl1 C111 Ct4 179.4(3) ? ? ? ? Cl1 C111 E8 139.9(3) ? ? ? ? C112 C111 C116 118.3(5) ? ? ? ? C112 C111 Ct4 59.4(3) ? ? ? ? C112 C111 E8 99.3(4) ? ? ? ? C116 C111 Ct4 58.9(3) ? ? ? ? C116 C111 E8 18.95(24) ? ? ? ? Ct4 C111 E8 39.91(12) ? ? ? ? Cl2 C112 C111 119.9(5) ? ? ? ? Cl2 C112 C113 120.3(4) ? ? ? ? Cl2 C112 Ct4 177.7(3) ? ? ? ? Cl2 C112 E7 120.3(6) ? ? ? ? C111 C112 C113 119.8(5) ? ? ? ? C111 C112 Ct4 60.0(3) ? ? ? ? C111 C112 E7 119.8(6) ? ? ? ? C113 C112 Ct4 59.8(3) ? ? ? ? C113 C112 E7 0.0 ? ? ? ? Ct4 C112 E7 59.8(4) ? ? ? ? C112 C113 C114 118.4(5) ? ? ? ? C112 C113 H113 119.9(6) ? ? ? ? C112 C113 Ct4 60.0(3) ? ? ? ? C112 C113 E7 0.0 ? ? ? ? C114 C113 H113 121.7(6) ? ? ? ? C114 C113 Ct4 58.4(3) ? ? ? ? C114 C113 E7 118.4(6) ? ? ? ? H113 C113 Ct4 179.7(5) ? ? ? ? H113 C113 E7 119.9(8) ? ? ? ? Ct4 C113 E7 60.0(4) ? ? ? ? C113 C114 C115 121.9(6) ? ? ? ? C113 C114 H114 115.6(6) ? ? ? ? C113 C114 Ct4 59.9(4) ? ? ? ? C113 C114 E7 19.37(24) ? ? ? ? C113 C114 E8 101.7(4) ? ? ? ? C115 C114 H114 122.5(7) ? ? ? ? C115 C114 Ct4 62.0(4) ? ? ? ? C115 C114 E7 102.5(4) ? ? ? ? C115 C114 E8 20.2(3) ? ? ? ? H114 C114 Ct4 175.6(7) ? ? ? ? H114 C114 E7 135.0(5) ? ? ? ? H114 C114 E8 142.7(6) ? ? ? ? Ct4 C114 E7 40.56(19) ? ? ? ? Ct4 C114 E8 41.73(17) ? ? ? ? E7 C114 E8 82.3(3) ? ? ? ? C114 C115 C116 119.6(6) ? ? ? ? C114 C115 H115 119.6(6) ? ? ? ? C114 C115 Ct4 61.2(4) ? ? ? ? C114 C115 E8 119.6(7) ? ? ? ? C116 C115 H115 120.7(6) ? ? ? ? C116 C115 Ct4 58.4(3) ? ? ? ? C116 C115 E8 0.02(11) ? ? ? ? H115 C115 Ct4 179.0(5) ? ? ? ? H115 C115 E8 120.7(8) ? ? ? ? Ct4 C115 E8 58.4(4) ? ? ? ? C111 C116 C115 122.0(5) ? ? ? ? C111 C116 H116 119.4(5) ? ? ? ? C111 C116 Ct4 62.1(3) ? ? ? ? C111 C116 E8 122.0(6) ? ? ? ? C115 C116 H116 118.6(5) ? ? ? ? C115 C116 Ct4 59.9(3) ? ? ? ? C115 C116 E8 0.02(11) ? ? ? ? H116 C116 Ct4 178.1(5) ? ? ? ? H116 C116 E8 118.6(6) ? ? ? ? Ct4 C116 E8 59.9(4) ? ? ? ? C11 H11 E1a 24.62(18) ? ? ? ? C11 H11 E2 24.62(18) ? ? ? ? E1a H11 E2 0.0 ? ? ? ? C12 H12 E1a 23.82(18) ? ? ? ? C12 H12 E2 23.81(18) ? ? ? ? E1a H12 E2 0.0 ? ? ? ? C15 H15 E5 23.68(18) ? ? ? ? C15 H15 E6a 23.68(18) ? ? ? ? E5 H15 E6a 0.0 ? ? ? ? C16 H16 E5 24.29(18) ? ? ? ? C16 H16 E6a 24.29(18) ? ? ? ? E5 H16 E6a 0.0 ? ? ? ? C21 H21 E3 24.63(19) ? ? ? ? C22 H22 E3 23.73(19) ? ? ? ? C24 H24 E4 23.99(19) ? ? ? ? C25 H25 E4 24.64(19) ? ? ? ? C113 H113 E7 23.8(4) ? ? ? ? C115 H115 E8 23.8(3) ? ? ? ? C116 H116 E8 24.2(3) ? ? ? ? N11 Ct C11 58.96(13) ? ? ? ? N11 Ct C11a 58.96(13) ? ? ? ? N11 Ct C12 119.88(13) ? ? ? ? N11 Ct C12a 119.88(13) ? ? ? ? N11 Ct C13 180.0 ? ? ? ? N11 Ct E1 89.8 ? ? ? ? N11 Ct E1a 89.8 ? ? ? ? N11 Ct E2 89.8 ? ? ? ? N11 Ct E2a 89.8 ? ? ? ? C11 Ct C11a 117.92(19) ? ? ? ? C11 Ct C12 60.92(19) ? ? ? ? C11 Ct C12a 178.84(19) ? ? ? ? C11 Ct C13 121.04(13) ? ? ? ? C11 Ct E1 148.72(13) ? ? ? ? C11 Ct E1a 30.80(13) ? ? ? ? C11 Ct E2 30.80(13) ? ? ? ? C11 Ct E2a 148.72(13) ? ? ? ? C11a Ct C12 178.84(19) ? ? ? ? C11a Ct C12a 60.92(19) ? ? ? ? C11a Ct C13 121.04(13) ? ? ? ? C11a Ct E1 30.80(13) ? ? ? ? C11a Ct E1a 148.72(13) ? ? ? ? C11a Ct E2 148.72(13) ? ? ? ? C11a Ct E2a 30.80(13) ? ? ? ? C12 Ct C12a 120.24(19) ? ? ? ? C12 Ct C13 60.12(13) ? ? ? ? C12 Ct E1 150.36(13) ? ? ? ? C12 Ct E1a 30.12(13) ? ? ? ? C12 Ct E2 30.12(13) ? ? ? ? C12 Ct E2a 150.36(13) ? ? ? ? C12a Ct C13 60.12(13) ? ? ? ? C12a Ct E1 30.12(13) ? ? ? ? C12a Ct E1a 150.36(13) ? ? ? ? C12a Ct E2 150.36(13) ? ? ? ? C12a Ct E2a 30.12(13) ? ? ? ? C13 Ct E1 90.2 ? ? ? ? C13 Ct E1a 90.2 ? ? ? ? C13 Ct E2 90.2 ? ? ? ? C13 Ct E2a 90.2 ? ? ? ? E1 Ct E1a 179.5 ? ? ? ? E1 Ct E2 179.5 ? ? ? ? E1 Ct E2a 0.0 ? ? ? ? E1a Ct E2 0.0 ? ? ? ? E1a Ct E2a 179.5 ? ? ? ? E2 Ct E2a 179.5 ? ? ? ? N21 Ct2 C21 58.78(18) ? ? ? ? N21 Ct2 C22 120.17(17) ? ? ? ? N21 Ct2 C23 179.58(15) ? ? ? ? N21 Ct2 C24 119.86(17) ? ? ? ? N21 Ct2 C25 58.28(17) ? ? ? ? N21 Ct2 E3 90.06(10) ? ? ? ? N21 Ct2 E4 89.49(10) ? ? ? ? C21 Ct2 C22 61.39(20) ? ? ? ? C21 Ct2 C23 121.54(19) ? ? ? ? C21 Ct2 C24 178.58(20) ? ? ? ? C21 Ct2 C25 117.06(20) ? ? ? ? C21 Ct2 E3 31.28(14) ? ? ? ? C21 Ct2 E4 148.27(14) ? ? ? ? C22 Ct2 C23 60.15(18) ? ? ? ? C22 Ct2 C24 119.97(19) ? ? ? ? C22 Ct2 C25 178.44(20) ? ? ? ? C22 Ct2 E3 30.11(14) ? ? ? ? C22 Ct2 E4 150.34(14) ? ? ? ? C23 Ct2 C24 59.82(19) ? ? ? ? C23 Ct2 C25 121.41(19) ? ? ? ? C23 Ct2 E3 90.26(12) ? ? ? ? C23 Ct2 E4 90.19(12) ? ? ? ? C24 Ct2 C25 61.58(20) ? ? ? ? C24 Ct2 E3 150.08(14) ? ? ? ? C24 Ct2 E4 30.36(14) ? ? ? ? C25 Ct2 E3 148.34(14) ? ? ? ? C25 Ct2 E4 31.22(14) ? ? ? ? E3 Ct2 E4 179.5 ? ? ? ? N12 Ct3 C14 180.0 ? ? ? ? N12 Ct3 C15 119.84(13) ? ? ? ? N12 Ct3 C15a 119.84(13) ? ? ? ? N12 Ct3 C16 58.68(14) ? ? ? ? N12 Ct3 C16a 58.68(14) ? ? ? ? N12 Ct3 E5 89.7 ? ? ? ? N12 Ct3 E5a 89.7 ? ? ? ? N12 Ct3 E6 89.7 ? ? ? ? N12 Ct3 E6a 89.7 ? ? ? ? C14 Ct3 C15 60.16(13) ? ? ? ? C14 Ct3 C15a 60.16(13) ? ? ? ? C14 Ct3 C16 121.32(14) ? ? ? ? C14 Ct3 C16a 121.32(14) ? ? ? ? C14 Ct3 E5 90.3 ? ? ? ? C14 Ct3 E5a 90.3 ? ? ? ? C14 Ct3 E6 90.3 ? ? ? ? C14 Ct3 E6a 90.3 ? ? ? ? C15 Ct3 C15a 120.31(19) ? ? ? ? C15 Ct3 C16 61.17(19) ? ? ? ? C15 Ct3 C16a 178.52(19) ? ? ? ? C15 Ct3 E5 30.13(13) ? ? ? ? C15 Ct3 E5a 150.44(13) ? ? ? ? C15 Ct3 E6 150.44(13) ? ? ? ? C15 Ct3 E6a 30.13(13) ? ? ? ? C15a Ct3 C16 178.52(19) ? ? ? ? C15a Ct3 C16a 61.17(19) ? ? ? ? C15a Ct3 E5 150.44(13) ? ? ? ? C15a Ct3 E5a 30.13(13) ? ? ? ? C15a Ct3 E6 30.13(13) ? ? ? ? C15a Ct3 E6a 150.44(13) ? ? ? ? C16 Ct3 C16a 117.35(19) ? ? ? ? C16 Ct3 E5 31.04(14) ? ? ? ? C16 Ct3 E5a 148.39(14) ? ? ? ? C16 Ct3 E6 148.39(14) ? ? ? ? C16 Ct3 E6a 31.04(14) ? ? ? ? C16a Ct3 E5 148.39(14) ? ? ? ? C16a Ct3 E5a 31.04(14) ? ? ? ? C16a Ct3 E6 31.04(14) ? ? ? ? C16a Ct3 E6a 148.39(14) ? ? ? ? E5 Ct3 E5a 179.4 ? ? ? ? E5 Ct3 E6 179.4 ? ? ? ? E5 Ct3 E6a 0.0 ? ? ? ? E5a Ct3 E6 0.0 ? ? ? ? E5a Ct3 E6a 179.4 ? ? ? ? E6 Ct3 E6a 179.4 ? ? ? ? C111 Ct4 C112 60.6(3) ? ? ? ? C111 Ct4 C113 120.8(4) ? ? ? ? C111 Ct4 C114 177.5(3) ? ? ? ? C111 Ct4 C115 120.7(3) ? ? ? ? C111 Ct4 C116 59.1(3) ? ? ? ? C111 Ct4 E7 90.65(19) ? ? ? ? C111 Ct4 E8 90.15(19) ? ? ? ? C112 Ct4 C113 60.2(4) ? ? ? ? C112 Ct4 C114 121.8(4) ? ? ? ? C112 Ct4 C115 178.5(3) ? ? ? ? C112 Ct4 C116 119.6(3) ? ? ? ? C112 Ct4 E7 30.1(3) ? ? ? ? C112 Ct4 E8 150.7(3) ? ? ? ? C113 Ct4 C114 61.6(4) ? ? ? ? C113 Ct4 C115 118.5(4) ? ? ? ? C113 Ct4 C116 179.8(3) ? ? ? ? C113 Ct4 E7 30.1(3) ? ? ? ? C113 Ct4 E8 149.1(3) ? ? ? ? C114 Ct4 C115 56.9(4) ? ? ? ? C114 Ct4 C116 118.5(4) ? ? ? ? C114 Ct4 E7 91.8(3) ? ? ? ? C114 Ct4 E8 87.4(3) ? ? ? ? C115 Ct4 C116 61.7(3) ? ? ? ? C115 Ct4 E7 148.6(3) ? ? ? ? C115 Ct4 E8 30.6(3) ? ? ? ? C116 Ct4 E7 149.71(23) ? ? ? ? C116 Ct4 E8 31.09(23) ? ? ? ? E7 Ct4 E8 179.1 ? ? ? ? C11a E1 C12a 180.0(3) ? ? ? ? C11a E1 H11a 37.4(3) ? ? ? ? C11a E1 H12a 143.7(3) ? ? ? ? C11a E1 Ct 88.7(3) ? ? ? ? C12a E1 H11a 142.6(3) ? ? ? ? C12a E1 H12a 36.4(3) ? ? ? ? C12a E1 Ct 91.3(3) ? ? ? ? H11a E1 H12a 106.3 ? ? ? ? H11a E1 Ct 126.1 ? ? ? ? H12a E1 Ct 127.7 ? ? ? ? C11 E2 C12 180.0 ? ? ? ? C11 E2 H11 37.4(3) ? ? ? ? C11 E2 H12 143.6(3) ? ? ? ? C11 E2 Ct 88.7(3) ? ? ? ? C12 E2 H11 142.6(3) ? ? ? ? C12 E2 H12 36.4(3) ? ? ? ? C12 E2 Ct 91.3(3) ? ? ? ? H11 E2 H12 106.2 ? ? ? ? H11 E2 Ct 126.1 ? ? ? ? H12 E2 Ct 127.7 ? ? ? ? C21 E3 C22 180.0(3) ? ? ? ? C21 E3 H21 37.3(3) ? ? ? ? C21 E3 H22 144.1(3) ? ? ? ? C21 E3 Ct2 87.8(3) ? ? ? ? C22 E3 H21 142.6(3) ? ? ? ? C22 E3 H22 35.9(3) ? ? ? ? C22 E3 Ct2 92.3(3) ? ? ? ? H21 E3 H22 106.8 ? ? ? ? H21 E3 Ct2 125.1 ? ? ? ? H22 E3 Ct2 128.2 ? ? ? ? C24 E4 C25 180.0(3) ? ? ? ? C24 E4 H24 36.1(3) ? ? ? ? C24 E4 H25 142.6(3) ? ? ? ? C24 E4 Ct2 91.7(3) ? ? ? ? C25 E4 H24 143.9(3) ? ? ? ? C25 E4 H25 37.4(3) ? ? ? ? C25 E4 Ct2 88.3(3) ? ? ? ? H24 E4 H25 106.5 ? ? ? ? H24 E4 Ct2 127.7 ? ? ? ? H25 E4 Ct2 125.8 ? ? ? ? C15 E5 C16 180.0 ? ? ? ? C15 E5 H15 35.9(3) ? ? ? ? C15 E5 H16 143.3(3) ? ? ? ? C15 E5 Ct3 91.8(3) ? ? ? ? C16 E5 H15 144.1(3) ? ? ? ? C16 E5 H16 36.6(3) ? ? ? ? C16 E5 Ct3 88.2(3) ? ? ? ? H15 E5 H16 107.5 ? ? ? ? H15 E5 Ct3 127.7 ? ? ? ? H16 E5 Ct3 124.9 ? ? ? ? C15a E6 C16a 180.0(4) ? ? ? ? C15a E6 H15a 35.9(3) ? ? ? ? C15a E6 H16a 143.3(3) ? ? ? ? C15a E6 Ct3 91.8(3) ? ? ? ? C16a E6 H15a 144.1(3) ? ? ? ? C16a E6 H16a 36.6(3) ? ? ? ? C16a E6 Ct3 88.2(3) ? ? ? ? H15a E6 H16a 107.5 ? ? ? ? H15a E6 Ct3 127.7 ? ? ? ? H16a E6 Ct3 124.9 ? ? ? ? Cl2 E7 C112 43.6(4) ? ? ? ? Cl2 E7 C113 136.4(5) ? ? ? ? Cl2 E7 C114 177.88(18) ? ? ? ? Cl2 E7 H113 100.06(8) ? ? ? ? Cl2 E7 Ct4 133.68(8) ? ? ? ? C112 E7 C113 180.0(3) ? ? ? ? C112 E7 C114 137.8(5) ? ? ? ? C112 E7 H113 143.6(4) ? ? ? ? C112 E7 Ct4 90.2(4) ? ? ? ? C113 E7 C114 42.2(5) ? ? ? ? C113 E7 H113 36.4(5) ? ? ? ? C113 E7 Ct4 89.9(5) ? ? ? ? C114 E7 H113 78.56(19) ? ? ? ? C114 E7 Ct4 47.67(19) ? ? ? ? H113 E7 Ct4 126.2 ? ? ? ? C111 E8 C114 100.8(3) ? ? ? ? C111 E8 C115 140.9(5) ? ? ? ? C111 E8 C116 39.1(4) ? ? ? ? C111 E8 H115 176.42(15) ? ? ? ? C111 E8 H116 76.25(15) ? ? ? ? C111 E8 Ct4 49.94(15) ? ? ? ? C114 E8 C115 40.2(6) ? ? ? ? C114 E8 C116 139.8(5) ? ? ? ? C114 E8 H115 75.64(22) ? ? ? ? C114 E8 H116 176.60(22) ? ? ? ? C114 E8 Ct4 50.84(22) ? ? ? ? C115 E8 C116 180.0(3) ? ? ? ? C115 E8 H115 35.5(5) ? ? ? ? C115 E8 H116 142.8(5) ? ? ? ? C115 E8 Ct4 91.0(5) ? ? ? ? C116 E8 H115 144.5(4) ? ? ? ? C116 E8 H116 37.2(4) ? ? ? ? C116 E8 Ct4 89.0(4) ? ? ? ? H115 E8 H116 107.3 ? ? ? ? H115 E8 Ct4 126.5 ? ? ? ? H116 E8 Ct4 126.2 ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? #=============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #=============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ data_2-2PhH #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common '2-2PhH' _chemical_formula_moiety 'Co N6 O6 C32 H28 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Co N6 O6 C32 H28 ' _chemical_formula_weight 651.54 _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co ? 0.299 0.973 'International Tables Vol. IV Table 2.2B' N ? 0.004 0.003 'International Tables Vol. IV Table 2.2B' O ? 0.008 0.006 'International Tables Vol. IV Table 2.2B' C ? 0.002 0.002 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' #=============================================================================== # 6. CRYSTAL DATA _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,z 1/2-x,1/2-y,-z -x,y,1/2-z x,-y,1/2+z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 21.3256(3) _cell_length_b 11.53050(10) _cell_length_c 12.60790(20) _cell_angle_alpha 90.0 _cell_angle_beta 100.7670(10) _cell_angle_gamma 90.0 _cell_volume 3045.64(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 20.00 _cell_measurement_theta_max 25.00 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method ? _exptl_crystal_F_000 1349.81 _exptl_absorpt_coefficient_mu 0.61 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Omega scan b/P/b ' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 8836 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.50 _diffrn_reflns_reduction_process ? _reflns_number_total 3177 _reflns_number_observed 2613 _reflns_observed_criterion 'Inet > 4.0\s(Inet)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX' _computing_publication_material 'NRCVAX TABLES Jan 94 Version' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 1/(\s^2^(F)+0.0000F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 2613 _refine_ls_number_parameters 206 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.039 _refine_ls_R_factor_obs 0.039 _refine_ls_wR_factor_all 0.049 _refine_ls_wR_factor_obs 0.049 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.19 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean ? _refine_diff_density_max 0.87 _refine_diff_density_min -0.88 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Co 0.50000 0.18353(3) 0.75000 0.01360(19) Uij ? S Co O1 0.47777(6) 0.18418(14) 0.90560(11) 0.0233(7) Uij ? . O O2 0.40701(9) 0.28742(19) 0.96403(19) 0.0565(12) Uij ? . O O3 0.39470(9) 0.10379(19) 0.94964(20) 0.0597(14) Uij ? . O N1 0.42470(8) 0.19131(17) 0.94043(14) 0.0236(9) Uij ? . N N11 0.50000 0.37344(22) 0.75000 0.0183(12) Uij ? S N N12 0.50000 0.99206(21) 0.75000 0.0170(11) Uij ? S N N21 0.59712(7) 0.19644(15) 0.83587(13) 0.0171(8) Uij ? . N C11 0.51583(10) 0.43469(19) 0.84211(16) 0.0219(11) Uij ? . C C12 0.51651(10) 0.55463(20) 0.84587(16) 0.0246(11) Uij ? . C C13 0.50000 0.6180(3) 0.75000 0.0213(15) Uij ? S C C14 0.50000 0.7465(3) 0.75000 0.0201(15) Uij ? S C C15 0.47829(11) 0.81004(20) 0.82994(17) 0.0250(11) Uij ? . C C16 0.47925(10) 0.93031(20) 0.82748(16) 0.0232(11) Uij ? . C C21 0.63797(9) 0.27525(20) 0.80857(16) 0.0215(9) Uij ? . C C22 0.69737(9) 0.29844(19) 0.86959(17) 0.0223(10) Uij ? . C C23 0.71813(8) 0.23870(19) 0.96567(15) 0.0168(9) Uij ? . C C24 0.67604(9) 0.15579(20) 0.99397(17) 0.0224(10) Uij ? . C C25 0.61743(9) 0.13729(20) 0.92779(16) 0.0207(10) Uij ? . C C31 0.23246(23) 0.5494(5) 0.3519(4) 0.105(3) Uij ? . C C32 0.20948(18) 0.4892(4) 0.2605(4) 0.080(3) Uij ? . C C33 0.24748(19) 0.4158(4) 0.2164(4) 0.088(3) Uij ? . C C34 0.31172(21) 0.4038(5) 0.2668(5) 0.114(4) Uij ? . C C35 0.33445(23) 0.4662(7) 0.3588(6) 0.134(5) Uij ? . C C36 0.2956(3) 0.5364(6) 0.4018(4) 0.119(4) Uij ? . C H11 0.528 0.390 0.912 0.0315 Uiso ? . H H12 0.528 0.597 0.917 0.0348 Uiso ? . H H15 0.462 0.767 0.890 0.0354 Uiso ? . H H16 0.463 0.975 0.886 0.0338 Uiso ? . H H21 0.624 0.320 0.739 0.0314 Uiso ? . H H22 0.726 0.358 0.844 0.0315 Uiso ? . H H24 0.689 0.110 1.062 0.0325 Uiso ? . H H25 0.588 0.077 0.950 0.0305 Uiso ? . H H31 0.202 0.606 0.385 0.1171 Uiso ? . H H32 0.163 0.498 0.225 0.0902 Uiso ? . H H33 0.229 0.370 0.146 0.1002 Uiso ? . H H34 0.343 0.349 0.235 0.1155 Uiso ? . H H35 0.380 0.455 0.395 0.1296 Uiso ? . H H36 0.315 0.582 0.474 0.1215 Uiso ? . H 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 _atom_site_aniso_type_symbol Co 0.01673(19) 0.00624(21) 0.01591(20) 0.00000 -0.00193(14) 0.00000 Co O1 0.0243(7) 0.0254(9) 0.0197(7) -0.0023(6) 0.0031(6) 0.0002(6) O O2 0.0442(10) 0.0419(14) 0.0797(15) 0.0143(9) 0.0018(10) -0.0341(11) O O3 0.0445(11) 0.0313(12) 0.1115(19) -0.0057(9) 0.0354(11) 0.0164(12) O N1 0.0275(9) 0.0202(11) 0.0216(9) 0.0046(8) 0.0012(7) -0.0016(8) N N11 0.0233(11) 0.0101(13) 0.0194(12) 0.00000 -0.0011(9) 0.00000 N N12 0.0195(11) 0.0095(13) 0.0201(12) 0.00000 -0.0008(9) 0.00000 N N21 0.0187(8) 0.0115(9) 0.0195(8) -0.0012(6) -0.0002(6) 0.0007(7) N C11 0.0323(11) 0.0117(11) 0.0193(10) -0.0007(9) -0.0010(8) 0.0011(9) C C12 0.0384(11) 0.0139(12) 0.0198(11) -0.0008(9) 0.0010(9) -0.0018(9) C C13 0.0275(14) 0.0116(16) 0.0243(15) 0.00000 0.0033(12) 0.00000 C C14 0.0277(14) 0.0111(16) 0.0197(14) 0.00000 -0.0003(11) 0.00000 C C15 0.0385(11) 0.0133(12) 0.0243(11) -0.0005(9) 0.0089(9) 0.0033(9) C C16 0.0342(11) 0.0122(12) 0.0239(11) 0.0007(9) 0.0069(9) -0.0012(9) C C21 0.0232(10) 0.0193(12) 0.0199(10) -0.0030(8) -0.0015(8) 0.0062(9) C C22 0.0215(9) 0.0211(13) 0.0224(10) -0.0061(8) -0.0006(8) 0.0056(9) C C23 0.0169(9) 0.0146(11) 0.0179(9) -0.0001(8) 0.0012(8) -0.0009(8) C C24 0.0210(9) 0.0216(13) 0.0222(10) -0.0030(8) -0.0022(8) 0.0078(9) C C25 0.0200(9) 0.0174(12) 0.0232(10) -0.0027(8) 0.0004(8) 0.0064(9) C C31 0.098(3) 0.101(4) 0.118(4) -0.045(3) 0.025(3) 0.050(3) C C32 0.0610(21) 0.085(3) 0.089(3) -0.0256(22) 0.0018(21) 0.057(3) C C33 0.0690(25) 0.081(3) 0.109(3) -0.0258(23) 0.0025(23) 0.055(3) C C34 0.069(3) 0.094(4) 0.173(5) -0.012(3) 0.012(3) 0.081(4) C C35 0.067(3) 0.157(7) 0.158(6) -0.062(4) -0.028(3) 0.092(5) C C36 0.095(4) 0.142(6) 0.112(4) -0.078(4) -0.005(3) 0.052(4) C #=============================================================================== # 10. MOLECULAR GEOMETRY 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 Co O1 2.1027(14) ? ? ? Co O1a 2.1027(14) ? ? ? O1 N1 1.2908(22) ? ? ? O2 N1 1.225(3) ? ? ? O3 N1 1.212(3) ? ? ? N11 C11 1.3472(24) ? ? ? N11 C11a 1.3472(24) ? ? ? N12 C16 1.349(3) ? ? ? N12 C16a 1.349(3) ? ? ? N21 C21 1.347(3) ? ? ? N21 C25 1.345(3) ? ? ? C11 C12 1.384(3) ? ? ? C11 H11 1.0139(20) ? ? ? C12 C13 1.400(3) ? ? ? C12 H12 1.0131(20) ? ? ? C13 C12a 1.400(3) ? ? ? C13 C14 1.482(4) ? ? ? C14 C15 1.393(3) ? ? ? C14 C15a 1.393(3) ? ? ? C15 C16 1.387(3) ? ? ? C15 H15 1.0171(21) ? ? ? C16 H16 1.0155(21) ? ? ? C21 C22 1.380(3) ? ? ? C21 H21 1.0103(20) ? ? ? C22 C23 1.392(3) ? ? ? C22 H22 1.0031(21) ? ? ? C23 C23b 1.492(3) ? ? ? C23 C24 1.402(3) ? ? ? C24 C25 1.384(3) ? ? ? C24 H24 1.0041(20) ? ? ? C25 H25 1.0061(20) ? ? ? C31 C32 1.357(8) ? ? ? C31 C36 1.383(8) ? ? ? C31 H31 1.059(6) ? ? ? C32 C33 1.360(8) ? ? ? C32 H32 1.022(4) ? ? ? C33 C34 1.405(6) ? ? ? C33 H33 1.040(5) ? ? ? C34 C35 1.374(11) ? ? ? C34 H34 1.055(6) ? ? ? C35 C36 1.344(12) ? ? ? C35 H35 1.001(5) ? ? ? C36 H36 1.058(6) ? ? ? 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 ? ? ? ? ? ? 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 Co O1a 179.59(6) ? ? ? ? Co O1 N1 133.04(12) ? ? ? ? O1 N1 O2 118.00(20) ? ? ? ? O1 N1 O3 119.45(19) ? ? ? ? O2 N1 O3 122.54(21) ? ? ? ? C11 N11 C11a 116.77(23) ? ? ? ? C16 N12 C16a 116.26(22) ? ? ? ? C21 N21 C25 116.28(16) ? ? ? ? N11 C11 C12 123.55(19) ? ? ? ? N11 C11 H11 117.62(21) ? ? ? ? C12 C11 H11 118.83(19) ? ? ? ? C11 C12 C13 119.52(20) ? ? ? ? C11 C12 H12 121.10(20) ? ? ? ? C13 C12 H12 119.37(22) ? ? ? ? C12 C13 C12a 117.1(3) ? ? ? ? C12 C13 C14 121.46(14) ? ? ? ? C12a C13 C14 121.46(14) ? ? ? ? C13 C14 C15 121.70(14) ? ? ? ? C13 C14 C15a 121.70(14) ? ? ? ? C15 C14 C15a 116.6(3) ? ? ? ? C14 C15 C16 120.05(21) ? ? ? ? C14 C15 H15 119.30(22) ? ? ? ? C16 C15 H15 120.64(21) ? ? ? ? N12 C16 C15 123.52(20) ? ? ? ? N12 C16 H16 117.51(22) ? ? ? ? C15 C16 H16 118.96(20) ? ? ? ? N21 C21 C22 123.94(18) ? ? ? ? N21 C21 H21 118.02(18) ? ? ? ? C22 C21 H21 118.03(20) ? ? ? ? C21 C22 C23 119.93(19) ? ? ? ? C21 C22 H22 120.13(19) ? ? ? ? C23 C22 H22 119.94(18) ? ? ? ? C22 C23 C23b 121.72(18) ? ? ? ? C22 C23 C24 116.37(16) ? ? ? ? C23b C23 C24 121.91(18) ? ? ? ? C23 C24 C25 120.05(18) ? ? ? ? C23 C24 H24 119.83(18) ? ? ? ? C25 C24 H24 120.12(19) ? ? ? ? N21 C25 C24 123.42(19) ? ? ? ? N21 C25 H25 118.26(17) ? ? ? ? C24 C25 H25 118.32(19) ? ? ? ? C32 C31 C36 119.8(6) ? ? ? ? C32 C31 H31 120.0(5) ? ? ? ? C36 C31 H31 120.1(6) ? ? ? ? C31 C32 C33 121.2(4) ? ? ? ? C31 C32 H32 119.3(6) ? ? ? ? C33 C32 H32 119.5(5) ? ? ? ? C32 C33 C34 118.8(5) ? ? ? ? C32 C33 H33 120.4(4) ? ? ? ? C34 C33 H33 120.8(6) ? ? ? ? C33 C34 C35 119.4(6) ? ? ? ? C33 C34 H34 121.5(7) ? ? ? ? C35 C34 H34 119.1(5) ? ? ? ? C34 C35 C36 120.6(5) ? ? ? ? C34 C35 H35 118.2(8) ? ? ? ? C36 C35 H35 121.1(8) ? ? ? ? C31 C36 C35 120.2(6) ? ? ? ? C31 C36 H36 121.5(7) ? ? ? ? C35 C36 H36 118.3(6) ? ? ? ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? #=============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #=============================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ data_2-3PhOMe _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '2-3PhOMe' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C41 H40 Co N6 O9' _chemical_formula_weight 819.72 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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' _cell_length_a 22.8114(11) _cell_length_b 15.4407(7) _cell_length_c 11.4207(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4022.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method ? _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25154 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.99 _reflns_number_total 7759 _reflns_number_observed 6067 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.37(2) _refine_ls_number_reflns 7759 _refine_ls_number_parameters 517 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_obs 0.0502 _refine_ls_wR_factor_all 0.1609 _refine_ls_wR_factor_obs 0.1501 _refine_ls_goodness_of_fit_all 1.134 _refine_ls_goodness_of_fit_obs 1.205 _refine_ls_restrained_S_all 1.134 _refine_ls_restrained_S_obs 1.205 _refine_ls_shift/esd_max 0.339 _refine_ls_shift/esd_mean 0.027 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.038345(14) 0.74617(3) 0.62754(7) 0.01820(12) Uani 1 d . . O1 O 0.04585(10) 0.88116(13) 0.6268(4) 0.0280(5) Uani 1 d . . O2 O 0.0131(2) 0.9898(3) 0.5282(4) 0.0832(15) Uani 1 d . . O3 O -0.03160(14) 0.9501(2) 0.6840(4) 0.0609(11) Uani 1 d . . O4 O 0.04661(10) 0.61092(13) 0.6264(3) 0.0270(5) Uani 1 d . . O5 O -0.0223(2) 0.5236(3) 0.5730(4) 0.0839(15) Uani 1 d . . O6 O -0.0044(2) 0.5371(2) 0.7525(4) 0.0686(11) Uani 1 d . . O31 O 0.3704(2) 0.8168(4) 0.0019(5) 0.104(2) Uani 1 d . . O41 O 0.2122(2) 0.4996(3) 0.3642(6) 0.089(2) Uani 1 d . . O51 O 0.3279(2) 1.0046(3) 0.3370(4) 0.0723(12) Uani 1 d . . N1 N 0.00828(14) 0.9424(2) 0.6139(4) 0.0321(8) Uani 1 d . . N2 N 0.0062(2) 0.5551(2) 0.6502(4) 0.0362(9) Uani 1 d . . N11 N 0.03993(14) 0.7469(2) 0.8152(4) 0.0216(10) Uani 1 d . . N12 N 0.04041(14) 0.7444(2) 0.4359(4) 0.0218(10) Uani 1 d . . N21 N 0.13241(10) 0.7485(2) 0.6251(5) 0.0221(5) Uani 1 d . . N22 N -0.05569(11) 0.7445(2) 0.6219(5) 0.0240(5) Uani 1 d . . C11 C 0.0163(2) 0.8106(2) 0.8775(4) 0.0301(8) Uani 1 d . . H11 H -0.0010(2) 0.8564(2) 0.8375(4) 0.036 Uiso 1 calc R . C12 C 0.0161(2) 0.8127(3) 0.9984(4) 0.0357(10) Uani 1 d . . H12 H -0.0008(2) 0.8591(3) 1.0380(4) 0.043 Uiso 1 calc R . C13 C 0.0410(2) 0.7454(2) 1.0595(6) 0.0285(14) Uani 1 d . . C14 C 0.0661(2) 0.6785(2) 0.9965(4) 0.0266(8) Uani 1 d . . H14 H 0.0830(2) 0.6316(2) 1.0349(4) 0.032 Uiso 1 calc R . C15 C 0.0655(2) 0.6823(2) 0.8765(4) 0.0267(8) Uani 1 d . . H15 H 0.0837(2) 0.6379(2) 0.8351(4) 0.032 Uiso 1 calc R . C16 C 0.0423(2) 0.7455(2) 1.1891(5) 0.0225(12) Uani 1 d . . C17 C 0.0518(2) 0.8208(2) 1.2542(4) 0.0320(9) Uani 1 d . . H17 H 0.0576(2) 0.8735(2) 1.2163(4) 0.038 Uiso 1 calc R . C18 C 0.0310(2) 0.6698(2) 1.2537(4) 0.0311(9) Uani 1 d . . H18 H 0.0242(2) 0.6178(2) 1.2148(4) 0.037 Uiso 1 calc R . C19 C 0.0300(2) 0.6722(2) 0.3731(4) 0.0282(9) Uani 1 d . . H19 H 0.0216(2) 0.6213(2) 0.4133(4) 0.034 Uiso 1 calc R . C110 C 0.0526(2) 0.8168(2) 0.3751(4) 0.0282(8) Uani 1 d . . H110 H 0.0622(2) 0.8667(2) 0.4166(4) 0.034 Uiso 1 calc R . C21 C 0.16339(14) 0.6960(2) 0.5568(4) 0.0268(9) Uani 1 d . . H21 H 0.14331(14) 0.6562(2) 0.5107(4) 0.032 Uiso 1 calc R . C22 C 0.2244(2) 0.6974(3) 0.5508(4) 0.0310(9) Uani 1 d . . H22 H 0.2440(2) 0.6605(3) 0.4998(4) 0.037 Uiso 1 calc R . C23 C 0.25550(12) 0.7540(2) 0.6211(6) 0.0229(6) Uani 1 d . . C24 C 0.2230(2) 0.8076(2) 0.6939(4) 0.0261(9) Uani 1 d . . H24 H 0.2421(2) 0.8466(2) 0.7428(4) 0.031 Uiso 1 calc R . C25 C 0.1623(2) 0.8036(2) 0.6943(4) 0.0263(8) Uani 1 d . . H25 H 0.1415(2) 0.8401(2) 0.7441(4) 0.032 Uiso 1 calc R . C26 C -0.08636(15) 0.7823(3) 0.5381(4) 0.0300(9) Uani 1 d . . H26 H -0.06566(15) 0.8103(3) 0.4790(4) 0.036 Uiso 1 calc R . C27 C -0.14681(14) 0.7835(3) 0.5316(4) 0.0289(8) Uani 1 d . . H27 H -0.16573(14) 0.8097(3) 0.4688(4) 0.035 Uiso 1 calc R . C28 C -0.17926(12) 0.7440(2) 0.6222(6) 0.0242(7) Uani 1 d . . C29 C -0.1480(2) 0.7054(2) 0.7102(4) 0.0300(9) Uani 1 d . . H29 H -0.1678(2) 0.6777(2) 0.7709(4) 0.036 Uiso 1 calc R . C210 C -0.08691(15) 0.7071(2) 0.7095(4) 0.0288(9) Uani 1 d . . H210 H -0.06679(15) 0.6817(2) 0.7715(4) 0.035 Uiso 1 calc R . C31 C 0.3165(3) 0.7954(5) 0.0502(7) 0.088(2) Uani 1 d . . C32 C 0.2931(2) 0.8350(5) 0.1469(7) 0.090(2) Uani 1 d . . H32 H 0.3139(2) 0.8768(5) 0.1881(7) 0.108 Uiso 1 calc R . C33 C 0.2361(3) 0.8100(5) 0.1816(8) 0.088(2) Uani 1 d . . H33 H 0.2201(3) 0.8334(5) 0.2495(8) 0.106 Uiso 1 calc R . C34 C 0.2049(2) 0.7538(4) 0.1190(13) 0.085(2) Uani 1 d . . H34 H 0.1663(2) 0.7415(4) 0.1398(13) 0.103 Uiso 1 calc R . C35 C 0.2299(3) 0.7136(4) 0.0229(7) 0.076(2) Uani 1 d . . H35 H 0.2079(3) 0.6736(4) -0.0193(7) 0.091 Uiso 1 calc R . C36 C 0.2840(3) 0.7303(4) -0.0106(7) 0.074(2) Uani 1 d . . H36 H 0.3008(3) 0.7002(4) -0.0727(7) 0.089 Uiso 1 calc R . C37 C 0.3999(3) 0.8952(6) 0.0461(9) 0.121(3) Uani 1 d . . H37A H 0.4341(18) 0.9066(27) -0.0004(39) 0.181 Uiso 1 calc R . H37B H 0.4113(28) 0.8864(18) 0.1261(20) 0.181 Uiso 1 calc R . H37C H 0.3736(11) 0.9435(11) 0.0413(61) 0.181 Uiso 1 calc R . C41 C 0.2703(3) 0.5128(4) 0.3512(6) 0.063(2) Uani 1 d . . C42 C 0.2961(3) 0.5587(5) 0.2649(7) 0.082(2) Uani 1 d . . H42 H 0.2724(3) 0.5843(5) 0.2083(7) 0.099 Uiso 1 calc R . C43 C 0.3580(4) 0.5696(5) 0.2565(8) 0.100(2) Uani 1 d . . H43 H 0.3744(4) 0.6015(5) 0.1958(8) 0.120 Uiso 1 calc R . C44 C 0.3920(3) 0.5327(5) 0.3386(9) 0.096(3) Uani 1 d . . H44 H 0.4325(3) 0.5377(5) 0.3348(9) 0.115 Uiso 1 calc R . C45 C 0.3656(3) 0.4866(5) 0.4296(7) 0.085(2) Uani 1 d . . H45 H 0.3886(3) 0.4614(5) 0.4875(7) 0.101 Uiso 1 calc R . C46 C 0.3075(3) 0.4788(4) 0.4336(7) 0.077(2) Uani 1 d . . H46 H 0.2912(3) 0.4485(4) 0.4960(7) 0.093 Uiso 1 calc R . C47 C 0.1712(4) 0.5366(5) 0.2849(8) 0.103(3) Uani 1 d . . H47A H 0.1778(18) 0.5979(8) 0.2795(43) 0.154 Uiso 1 calc R . H47B H 0.1321(4) 0.5261(35) 0.3125(29) 0.154 Uiso 1 calc R . H47C H 0.1760(19) 0.5108(30) 0.2090(15) 0.154 Uiso 1 calc R . C51 C 0.2665(3) 1.0041(3) 0.3553(6) 0.0578(14) Uani 1 d . . C52 C 0.2402(3) 0.9721(3) 0.4510(6) 0.063(2) Uani 1 d . . H52 H 0.2623(3) 0.9478(3) 0.5110(6) 0.075 Uiso 1 calc R . C53 C 0.1794(3) 0.9756(4) 0.4595(6) 0.066(2) Uani 1 d . . H53 H 0.1607(3) 0.9540(4) 0.5257(6) 0.079 Uiso 1 calc R . C54 C 0.1468(3) 1.0111(3) 0.3697(7) 0.066(2) Uani 1 d . . H54 H 0.1061(3) 1.0130(3) 0.3748(7) 0.079 Uiso 1 calc R . C55 C 0.1743(3) 1.0431(3) 0.2741(6) 0.068(2) Uani 1 d . . H55 H 0.1524(3) 1.0673(3) 0.2137(6) 0.081 Uiso 1 calc R . C56 C 0.2340(3) 1.0403(3) 0.2655(6) 0.067(2) Uani 1 d . . H56 H 0.2527(3) 1.0626(3) 0.1997(6) 0.080 Uiso 1 calc R . C57 C 0.3623(3) 0.9598(4) 0.4162(7) 0.081(2) Uani 1 d . . H57A H 0.3522(15) 0.9771(24) 0.4944(7) 0.122 Uiso 1 calc R . H57B H 0.4029(3) 0.9725(26) 0.4019(29) 0.122 Uiso 1 calc R . H57C H 0.3558(17) 0.8988(4) 0.4074(31) 0.122 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0141(2) 0.0273(2) 0.0133(2) -0.0002(2) 0.0007(3) -0.0001(2) O1 0.0270(11) 0.0282(10) 0.0287(14) 0.001(2) -0.0026(14) 0.0032(8) O2 0.112(3) 0.068(2) 0.069(3) 0.040(2) 0.034(3) 0.045(2) O3 0.048(2) 0.079(2) 0.055(3) 0.009(2) 0.016(2) 0.034(2) O4 0.0265(11) 0.0289(10) 0.0255(13) 0.007(2) -0.0030(14) -0.0006(8) O5 0.111(3) 0.088(3) 0.052(3) 0.020(2) -0.040(2) -0.066(3) O6 0.103(3) 0.063(2) 0.040(2) 0.001(2) 0.014(2) -0.036(2) O31 0.080(3) 0.138(4) 0.095(4) -0.029(3) 0.010(3) 0.003(3) O41 0.072(3) 0.098(3) 0.096(4) -0.017(3) -0.023(3) 0.008(2) O51 0.071(3) 0.077(3) 0.068(3) 0.012(2) -0.004(2) -0.012(2) N1 0.038(2) 0.0284(14) 0.030(2) 0.001(2) 0.000(2) 0.0068(12) N2 0.047(2) 0.0302(15) 0.032(3) 0.0067(14) -0.007(2) -0.0109(14) N11 0.019(2) 0.031(2) 0.014(3) -0.0003(12) 0.0032(14) 0.0011(10) N12 0.020(2) 0.027(2) 0.019(3) 0.0004(12) 0.0038(15) 0.0002(10) N21 0.0155(10) 0.0301(11) 0.0207(12) -0.0024(11) 0.000(3) -0.0012(11) N22 0.0164(10) 0.0366(13) 0.0189(14) 0.0007(13) -0.002(3) -0.0012(10) C11 0.041(2) 0.036(2) 0.013(2) 0.005(2) 0.003(2) 0.010(2) C12 0.054(3) 0.032(2) 0.021(2) 0.001(2) 0.010(2) 0.014(2) C13 0.044(3) 0.027(3) 0.015(3) -0.0010(14) 0.003(2) -0.0055(15) C14 0.036(2) 0.026(2) 0.018(2) -0.0002(14) -0.004(2) 0.0070(14) C15 0.034(2) 0.029(2) 0.018(2) -0.0036(14) -0.002(2) 0.0049(14) C16 0.022(2) 0.028(3) 0.018(3) 0.0030(14) 0.002(2) -0.0023(13) C17 0.042(2) 0.031(2) 0.023(2) 0.002(2) 0.004(2) -0.005(2) C18 0.047(2) 0.027(2) 0.020(2) -0.003(2) -0.004(2) -0.0052(15) C19 0.037(2) 0.026(2) 0.023(2) 0.0023(15) -0.004(2) -0.0057(14) C110 0.033(2) 0.028(2) 0.023(2) -0.0014(15) 0.006(2) -0.0053(14) C21 0.014(2) 0.037(2) 0.029(2) -0.012(2) 0.001(2) 0.0000(14) C22 0.018(2) 0.045(2) 0.030(2) -0.018(2) 0.003(2) 0.003(2) C23 0.0138(12) 0.0279(14) 0.027(2) 0.000(2) -0.001(3) -0.0024(12) C24 0.019(2) 0.027(2) 0.032(2) -0.012(2) 0.001(2) -0.0031(13) C25 0.025(2) 0.027(2) 0.027(2) -0.008(2) 0.002(2) 0.0012(14) C26 0.018(2) 0.045(2) 0.028(2) 0.012(2) 0.002(2) -0.0032(15) C27 0.016(2) 0.044(2) 0.027(2) 0.014(2) 0.001(2) -0.0010(14) C28 0.0144(11) 0.0278(14) 0.030(2) 0.005(2) 0.001(3) -0.0029(11) C29 0.021(2) 0.040(2) 0.028(2) 0.009(2) 0.006(2) -0.0023(15) C210 0.016(2) 0.043(2) 0.027(2) 0.012(2) 0.000(2) -0.0003(14) C31 0.059(4) 0.130(6) 0.074(5) -0.037(5) -0.019(4) 0.028(4) C32 0.068(4) 0.115(5) 0.086(6) -0.056(5) -0.006(3) 0.006(3) C33 0.085(5) 0.104(5) 0.076(5) -0.018(4) 0.004(4) -0.005(4) C34 0.055(3) 0.085(4) 0.117(7) -0.043(4) -0.005(5) -0.002(3) C35 0.092(4) 0.054(3) 0.081(5) -0.005(3) 0.000(4) -0.005(3) C36 0.095(5) 0.078(4) 0.048(4) -0.015(3) 0.002(3) 0.005(3) C37 0.087(5) 0.161(8) 0.115(8) -0.037(6) -0.039(5) -0.036(5) C41 0.077(4) 0.056(3) 0.057(4) -0.029(3) -0.007(3) 0.011(3) C42 0.094(5) 0.098(5) 0.055(4) -0.014(4) -0.003(4) 0.021(4) C43 0.112(6) 0.112(6) 0.077(5) -0.029(5) -0.006(5) 0.021(5) C44 0.080(5) 0.115(6) 0.092(6) -0.062(5) -0.010(4) 0.020(4) C45 0.094(5) 0.089(5) 0.070(5) -0.029(4) -0.026(4) 0.025(4) C46 0.092(5) 0.067(3) 0.073(5) -0.017(3) -0.023(4) 0.018(3) C47 0.116(6) 0.102(5) 0.090(6) -0.024(5) -0.041(5) 0.036(4) C51 0.082(4) 0.039(2) 0.053(4) -0.006(3) 0.000(3) -0.015(3) C52 0.086(4) 0.058(3) 0.045(4) 0.009(3) -0.019(3) -0.023(3) C53 0.077(4) 0.071(4) 0.050(4) 0.010(3) -0.006(3) -0.025(3) C54 0.067(4) 0.053(3) 0.078(5) 0.002(3) -0.011(3) -0.012(3) C55 0.078(4) 0.055(3) 0.070(4) 0.017(3) -0.018(3) -0.003(3) C56 0.095(5) 0.053(3) 0.052(4) 0.013(3) 0.010(3) 0.002(3) C57 0.080(4) 0.072(4) 0.093(6) -0.005(4) -0.031(4) -0.009(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 Co1 O1 2.091(2) . ? Co1 O4 2.097(2) . ? Co1 N11 2.144(5) . ? Co1 N22 2.146(3) . ? Co1 N21 2.146(2) . ? Co1 N12 2.189(5) . ? O1 N1 1.285(4) . ? O2 N1 1.227(5) . ? O3 N1 1.218(5) . ? O4 N2 1.291(4) . ? O5 N2 1.198(5) . ? O6 N2 1.226(5) . ? O31 C31 1.387(9) . ? O31 C37 1.474(9) . ? O41 C41 1.349(8) . ? O41 C47 1.422(9) . ? O51 C57 1.383(8) . ? O51 C51 1.417(8) . ? N11 C11 1.329(5) . ? N11 C15 1.351(5) . ? N12 C110 1.345(5) . ? N12 C19 1.347(5) . ? N21 C21 1.329(5) . ? N21 C25 1.346(5) . ? N22 C26 1.322(6) . ? N22 C210 1.357(6) . ? C11 C12 1.381(6) . ? C12 C13 1.376(6) . ? C13 C14 1.382(6) . ? C13 C16 1.480(5) . ? C14 C15 1.372(6) . ? C16 C17 1.398(6) . ? C16 C18 1.405(6) . ? C17 C110 1.383(6) 1_556 ? C18 C19 1.365(6) 1_556 ? C19 C18 1.365(6) 1_554 ? C110 C17 1.383(6) 1_554 ? C21 C22 1.393(5) . ? C22 C23 1.384(6) . ? C23 C24 1.387(6) . ? C23 C28 1.489(4) 3_565 ? C24 C25 1.386(5) . ? C26 C27 1.381(5) . ? C27 C28 1.411(7) . ? C28 C29 1.368(7) . ? C28 C23 1.489(4) 3_465 ? C29 C210 1.395(5) . ? C31 C32 1.370(9) . ? C31 C36 1.429(10) . ? C32 C33 1.412(9) . ? C33 C34 1.332(11) . ? C34 C35 1.384(13) . ? C35 C36 1.318(9) . ? C41 C42 1.349(10) . ? C41 C46 1.372(10) . ? C42 C43 1.426(10) . ? C43 C44 1.343(12) . ? C44 C45 1.396(12) . ? C45 C46 1.331(10) . ? C51 C52 1.342(9) . ? C51 C56 1.383(9) . ? C52 C53 1.392(9) . ? C53 C54 1.380(9) . ? C54 C55 1.353(9) . ? C55 C56 1.366(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O4 170.12(8) . . ? O1 Co1 N11 89.87(14) . . ? O4 Co1 N11 90.55(13) . . ? O1 Co1 N22 95.37(9) . . ? O4 Co1 N22 94.47(9) . . ? N11 Co1 N22 92.7(2) . . ? O1 Co1 N21 84.32(9) . . ? O4 Co1 N21 85.81(9) . . ? N11 Co1 N21 89.8(2) . . ? N22 Co1 N21 177.5(2) . . ? O1 Co1 N12 90.36(14) . . ? O4 Co1 N12 88.84(13) . . ? N11 Co1 N12 177.76(8) . . ? N22 Co1 N12 89.5(2) . . ? N21 Co1 N12 88.0(2) . . ? N1 O1 Co1 132.8(2) . . ? N2 O4 Co1 126.8(2) . . ? C31 O31 C37 117.6(6) . . ? C41 O41 C47 121.0(7) . . ? C57 O51 C51 117.5(5) . . ? O3 N1 O2 122.2(3) . . ? O3 N1 O1 119.7(4) . . ? O2 N1 O1 118.1(4) . . ? O5 N2 O6 120.1(4) . . ? O5 N2 O4 120.3(4) . . ? O6 N2 O4 119.5(4) . . ? C11 N11 C15 116.4(5) . . ? C11 N11 Co1 122.2(3) . . ? C15 N11 Co1 121.4(3) . . ? C110 N12 C19 116.7(5) . . ? C110 N12 Co1 120.7(3) . . ? C19 N12 Co1 122.6(3) . . ? C21 N21 C25 117.5(2) . . ? C21 N21 Co1 121.9(3) . . ? C25 N21 Co1 120.6(3) . . ? C26 N22 C210 116.4(3) . . ? C26 N22 Co1 123.1(3) . . ? C210 N22 Co1 120.5(3) . . ? N11 C11 C12 123.7(4) . . ? C13 C12 C11 119.2(4) . . ? C12 C13 C14 118.1(5) . . ? C12 C13 C16 121.0(4) . . ? C14 C13 C16 120.9(4) . . ? C15 C14 C13 119.0(4) . . ? N11 C15 C14 123.6(4) . . ? C17 C16 C18 116.2(5) . . ? C17 C16 C13 122.4(4) . . ? C18 C16 C13 121.4(4) . . ? C110 C17 C16 119.7(4) 1_556 . ? C19 C18 C16 120.4(4) 1_556 . ? N12 C19 C18 123.5(4) . 1_554 ? N12 C110 C17 123.4(4) . 1_554 ? N21 C21 C22 123.4(3) . . ? C23 C22 C21 119.6(3) . . ? C22 C23 C24 116.8(3) . . ? C22 C23 C28 122.1(4) . 3_565 ? C24 C23 C28 121.1(4) . 3_565 ? C25 C24 C23 120.6(3) . . ? N21 C25 C24 122.1(3) . . ? N22 C26 C27 125.0(4) . . ? C26 C27 C28 118.6(4) . . ? C29 C28 C27 117.0(3) . . ? C29 C28 C23 122.4(4) . 3_465 ? C27 C28 C23 120.6(4) . 3_465 ? C28 C29 C210 120.5(4) . . ? N22 C210 C29 122.5(4) . . ? C32 C31 O31 124.1(7) . . ? C32 C31 C36 120.2(7) . . ? O31 C31 C36 115.7(6) . . ? C31 C32 C33 117.6(6) . . ? C34 C33 C32 121.3(8) . . ? C33 C34 C35 119.9(7) . . ? C36 C35 C34 121.9(7) . . ? C35 C36 C31 118.8(7) . . ? C42 C41 O41 126.0(7) . . ? C42 C41 C46 115.6(7) . . ? O41 C41 C46 118.4(8) . . ? C41 C42 C43 122.9(7) . . ? C44 C43 C42 118.3(9) . . ? C43 C44 C45 119.2(8) . . ? C46 C45 C44 120.0(7) . . ? C45 C46 C41 123.9(8) . . ? C52 C51 C56 120.9(6) . . ? C52 C51 O51 124.4(6) . . ? C56 C51 O51 114.7(6) . . ? C51 C52 C53 119.2(6) . . ? C54 C53 C52 120.1(6) . . ? C55 C54 C53 119.6(6) . . ? C54 C55 C56 120.6(6) . . ? C55 C56 C51 119.6(6) . . ? _refine_diff_density_max 0.387 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.067 data_2-2PhNO2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '2-2PhNO2' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H26 Co N8 O10' _chemical_formula_weight 741.54 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 21.7003(11) _cell_length_b 11.4961(6) _cell_length_c 12.8598(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.5260(10) _cell_angle_gamma 90.00 _cell_volume 3131.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method ? _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9721 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.90 _reflns_number_total 3662 _reflns_number_observed 3263 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3662 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_obs 0.0296 _refine_ls_wR_factor_all 0.1094 _refine_ls_wR_factor_obs 0.1047 _refine_ls_goodness_of_fit_all 0.923 _refine_ls_goodness_of_fit_obs 0.939 _refine_ls_restrained_S_all 0.923 _refine_ls_restrained_S_obs 0.939 _refine_ls_shift/esd_max -0.018 _refine_ls_shift/esd_mean 0.004 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.5000 0.18447(2) 0.7500 0.01483(11) Uani 1 d S . O1 O 0.47594(5) 0.18757(8) 0.89985(8) 0.0234(2) Uani 1 d . . O2 O 0.38972(6) 0.09492(11) 0.90964(13) 0.0472(3) Uani 1 d . . O3 O 0.40105(6) 0.27366(13) 0.95800(11) 0.0474(3) Uani 1 d . . O31 O 0.33827(11) 0.6379(3) 0.7522(2) 0.1049(8) Uani 1 d . . O32 O 0.38819(8) 0.6076(2) 0.9137(2) 0.0799(6) Uani 1 d . . N11 N 0.42054(6) 0.18543(10) 0.92266(10) 0.0242(3) Uani 1 d . . N12 N 0.59618(5) 0.19846(9) 0.84000(9) 0.0190(2) Uani 1 d . . N21 N 0.5000 0.37417(13) 0.7500 0.0186(3) Uani 1 d S . N22 N 0.5000 -0.00658(13) 0.7500 0.0174(3) Uani 1 d S . N31 N 0.34275(8) 0.5940(2) 0.8398(2) 0.0559(5) Uani 1 d . . C11 C 0.63659(6) 0.27306(13) 0.80989(11) 0.0236(3) Uani 1 d . . H11 H 0.62355(6) 0.31208(13) 0.74552(11) 0.028 Uiso 1 calc R . C12 C 0.69667(7) 0.29503(13) 0.86952(12) 0.0247(3) Uani 1 d . . H12 H 0.72283(7) 0.34738(13) 0.84472(12) 0.030 Uiso 1 calc R . C13 C 0.71794(6) 0.23880(11) 0.96663(10) 0.0185(3) Uani 1 d . . C14 C 0.67612(6) 0.16116(13) 0.99740(11) 0.0226(3) Uani 1 d . . H14 H 0.68788(6) 0.12125(13) 1.06155(11) 0.027 Uiso 1 calc R . C15 C 0.61667(6) 0.14300(12) 0.93239(11) 0.0219(3) Uani 1 d . . H15 H 0.58989(6) 0.08964(12) 0.95434(11) 0.026 Uiso 1 calc R . C21 C 0.51679(6) 0.43526(12) 0.84111(10) 0.0225(3) Uani 1 d . . H21 H 0.52828(6) 0.39456(12) 0.90488(10) 0.027 Uiso 1 calc R . C22 C 0.51779(7) 0.55550(12) 0.84457(10) 0.0229(3) Uani 1 d . . H22 H 0.53021(7) 0.59396(12) 0.90936(10) 0.027 Uiso 1 calc R . C23 C 0.5000 0.6188(2) 0.7500 0.0197(4) Uani 1 d S . C24 C 0.5000 -0.2523(2) 0.7500 0.0195(4) Uani 1 d S . C25 C 0.48856(7) -0.18881(11) 0.83631(11) 0.0220(3) Uani 1 d . . H25 H 0.48035(7) -0.22722(11) 0.89549(11) 0.026 Uiso 1 calc R . C26 C 0.48947(6) -0.06861(12) 0.83360(10) 0.0214(3) Uani 1 d . . H26 H 0.48243(6) -0.02826(12) 0.89262(10) 0.026 Uiso 1 calc R . C31 C 0.29033(8) 0.5212(2) 0.85732(14) 0.0367(4) Uani 1 d . . C32 C 0.29826(10) 0.4622(2) 0.95274(15) 0.0457(5) Uani 1 d . . H32 H 0.33583(10) 0.4673(2) 1.00361(15) 0.055 Uiso 1 calc R . C33 C 0.24845(12) 0.3949(2) 0.9704(2) 0.0562(6) Uani 1 d . . H33 H 0.25211(12) 0.3554(2) 1.0346(2) 0.067 Uiso 1 calc R . C34 C 0.19366(11) 0.3865(2) 0.8934(2) 0.0547(5) Uani 1 d . . H34 H 0.16099(11) 0.3394(2) 0.9052(2) 0.066 Uiso 1 calc R . C35 C 0.18652(9) 0.4472(2) 0.7984(2) 0.0459(5) Uani 1 d . . H35 H 0.14911(9) 0.4414(2) 0.7473(2) 0.055 Uiso 1 calc R . C36 C 0.23503(8) 0.5161(2) 0.78002(13) 0.0371(4) Uani 1 d . . H36 H 0.23069(8) 0.5582(2) 0.71709(13) 0.045 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0121(2) 0.0130(2) 0.0173(2) 0.000 -0.00119(10) 0.000 O1 0.0195(5) 0.0285(6) 0.0217(5) -0.0006(4) 0.0036(4) -0.0015(4) O2 0.0336(6) 0.0384(7) 0.0742(10) -0.0068(6) 0.0217(6) -0.0123(5) O3 0.0419(7) 0.0456(8) 0.0546(8) -0.0183(6) 0.0102(6) 0.0170(6) O31 0.0783(14) 0.131(2) 0.108(2) 0.041(2) 0.0242(13) -0.0282(14) O32 0.0383(8) 0.0985(15) 0.0998(14) -0.0395(12) 0.0082(8) -0.0127(9) N11 0.0228(6) 0.0269(6) 0.0226(6) -0.0012(4) 0.0044(5) 0.0040(4) N12 0.0132(5) 0.0198(5) 0.0212(5) -0.0008(4) -0.0025(4) 0.0000(4) N21 0.0189(7) 0.0127(7) 0.0215(8) 0.000 -0.0012(6) 0.000 N22 0.0157(7) 0.0137(7) 0.0211(7) 0.000 0.0005(6) 0.000 N31 0.0388(9) 0.0543(11) 0.0770(13) -0.0131(9) 0.0181(9) 0.0004(8) C11 0.0184(6) 0.0268(7) 0.0223(6) 0.0053(5) -0.0032(5) -0.0031(5) C12 0.0177(6) 0.0288(7) 0.0250(7) 0.0063(6) -0.0013(5) -0.0068(5) C13 0.0132(6) 0.0213(6) 0.0195(6) -0.0016(5) 0.0001(5) 0.0002(5) C14 0.0159(6) 0.0273(7) 0.0218(6) 0.0054(5) -0.0021(5) -0.0010(5) C15 0.0148(6) 0.0233(7) 0.0258(7) 0.0052(5) 0.0003(5) -0.0021(5) C21 0.0274(7) 0.0166(6) 0.0205(6) 0.0013(5) -0.0011(5) 0.0006(5) C22 0.0294(7) 0.0167(6) 0.0206(6) -0.0025(5) 0.0011(5) -0.0006(5) C23 0.0207(8) 0.0155(8) 0.0226(9) 0.000 0.0043(7) 0.000 C24 0.0188(8) 0.0156(8) 0.0220(9) 0.000 -0.0002(7) 0.000 C25 0.0280(7) 0.0163(7) 0.0220(7) 0.0017(4) 0.0059(6) 0.0003(5) C26 0.0246(6) 0.0169(6) 0.0225(6) -0.0015(5) 0.0049(5) 0.0005(5) C31 0.0313(8) 0.0347(8) 0.0446(9) -0.0109(7) 0.0094(7) 0.0075(7) C32 0.0488(10) 0.0396(10) 0.0438(10) -0.0063(8) -0.0010(8) 0.0195(8) C33 0.087(2) 0.0352(10) 0.0500(12) 0.0052(8) 0.0231(12) 0.0190(10) C34 0.0620(13) 0.0379(10) 0.0749(15) -0.0055(9) 0.0383(12) -0.0026(9) C35 0.0324(8) 0.0513(11) 0.0540(11) -0.0197(9) 0.0094(8) 0.0023(8) C36 0.0366(8) 0.0410(9) 0.0346(8) -0.0054(7) 0.0093(7) 0.0092(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.1033(10) 2_656 ? Co1 O1 2.1033(10) . ? Co1 N12 2.1619(11) 2_656 ? Co1 N12 2.1619(11) . ? Co1 N21 2.181(2) . ? Co1 N22 2.196(2) . ? O1 N11 1.298(2) . ? O2 N11 1.229(2) . ? O3 N11 1.224(2) . ? O31 N31 1.218(3) . ? O32 N31 1.222(2) . ? N12 C15 1.337(2) . ? N12 C11 1.342(2) . ? N21 C21 1.3466(15) . ? N21 C21 1.3466(15) 2_656 ? N22 C26 1.350(2) 2_656 ? N22 C26 1.350(2) . ? N31 C31 1.469(3) . ? C11 C12 1.385(2) . ? C12 C13 1.393(2) . ? C13 C14 1.390(2) . ? C13 C13 1.491(2) 7_657 ? C14 C15 1.393(2) . ? C21 C22 1.383(2) . ? C22 C23 1.398(2) . ? C23 C22 1.398(2) 2_656 ? C23 C24 1.482(3) 1_565 ? C24 C25 1.395(2) . ? C24 C25 1.395(2) 2_656 ? C24 C23 1.482(3) 1_545 ? C25 C26 1.382(2) . ? C31 C36 1.383(2) . ? C31 C32 1.380(3) . ? C32 C33 1.387(3) . ? C33 C34 1.376(3) . ? C34 C35 1.386(3) . ? C35 C36 1.378(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 178.06(5) 2_656 . ? O1 Co1 N12 84.89(4) 2_656 2_656 ? O1 Co1 N12 94.97(4) . 2_656 ? O1 Co1 N12 94.97(4) 2_656 . ? O1 Co1 N12 84.89(4) . . ? N12 Co1 N12 171.47(6) 2_656 . ? O1 Co1 N21 89.03(3) 2_656 . ? O1 Co1 N21 89.03(3) . . ? N12 Co1 N21 85.73(3) 2_656 . ? N12 Co1 N21 85.73(3) . . ? O1 Co1 N22 90.97(3) 2_656 . ? O1 Co1 N22 90.97(3) . . ? N12 Co1 N22 94.27(3) 2_656 . ? N12 Co1 N22 94.27(3) . . ? N21 Co1 N22 180.0 . . ? N11 O1 Co1 129.26(8) . . ? O3 N11 O2 122.06(15) . . ? O3 N11 O1 118.68(13) . . ? O2 N11 O1 119.25(12) . . ? C15 N12 C11 116.68(11) . . ? C15 N12 Co1 122.46(9) . . ? C11 N12 Co1 120.56(9) . . ? C21 N21 C21 117.1(2) . 2_656 ? C21 N21 Co1 121.43(8) . . ? C21 N21 Co1 121.43(8) 2_656 . ? C26 N22 C26 116.2(2) 2_656 . ? C26 N22 Co1 121.88(8) 2_656 . ? C26 N22 Co1 121.88(8) . . ? O31 N31 O32 123.7(2) . . ? O31 N31 C31 118.0(2) . . ? O32 N31 C31 118.3(2) . . ? N12 C11 C12 123.52(12) . . ? C11 C12 C13 120.05(12) . . ? C14 C13 C12 116.32(11) . . ? C14 C13 C13 122.18(14) . 7_657 ? C12 C13 C13 121.50(15) . 7_657 ? C13 C14 C15 120.15(12) . . ? N12 C15 C14 123.26(12) . . ? N21 C21 C22 123.28(12) . . ? C21 C22 C23 119.53(13) . . ? C22 C23 C22 117.3(2) 2_656 . ? C22 C23 C24 121.37(9) 2_656 1_565 ? C22 C23 C24 121.37(9) . 1_565 ? C25 C24 C25 116.9(2) . 2_656 ? C25 C24 C23 121.55(8) . 1_545 ? C25 C24 C23 121.55(8) 2_656 1_545 ? C26 C25 C24 119.80(13) . . ? N22 C26 C25 123.62(13) . . ? C36 C31 C32 122.7(2) . . ? C36 C31 N31 119.6(2) . . ? C32 C31 N31 117.7(2) . . ? C33 C32 C31 117.9(2) . . ? C34 C33 C32 120.2(2) . . ? C33 C34 C35 120.8(2) . . ? C34 C35 C36 119.8(2) . . ? C31 C36 C35 118.5(2) . . ? _refine_diff_density_max 0.313 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.050