# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Enrique Colacio' _publ_contact_author_email ECOLACIO@UGR.ES _publ_section_title ; Influence of Metal Ions, Coligands and Reaction Conditions on the Structural Versatility and Properties of 5-pyrimidyl-tetrazolate Containing Complexes ; loop_ _publ_author_name 'Enrique Colacio' 'Antonio J. Mota' 'M. Angeles Palacios' 'Antonio Rodriguez-Dieguez' ; A.Romerosa ; 'Jose M. Seco' # Attachment 'pmtz.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 734265' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6 Cu2 N12' _chemical_formula_weight 421.37 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' Cu Cu 0.3201 1.2651 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 20.535(6) _cell_length_b 12.631(4) _cell_length_c 11.271(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2923.4(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1599 _cell_measurement_theta_min 2.617 _cell_measurement_theta_max 17.965 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 2.932 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.877 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17193 _diffrn_reflns_av_R_equivalents 0.0883 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 20.73 _reflns_number_total 1517 _reflns_number_gt 1147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+1.6478P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1517 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.08654(4) 0.08300(7) 0.47266(6) 0.0530(3) Uani 1 1 d . . . Cu3 Cu 0.0000 -0.12164(9) 0.2500 0.0444(4) Uani 1 2 d S . . Cu2 Cu 0.0000 0.26815(11) 0.2500 0.0640(5) Uani 1 2 d S . . N7B N 0.1712(3) 0.1869(5) 0.4223(5) 0.0562(17) Uani 1 1 d . . . N11B N 0.2371(3) 0.2177(5) 0.2517(5) 0.0660(18) Uani 1 1 d . . . N1B N 0.1023(2) 0.0433(4) 0.3021(4) 0.0373(15) Uani 1 1 d . . . N3A N -0.0211(3) 0.1976(4) 0.5996(4) 0.0443(15) Uani 1 1 d . . . N2B N 0.0760(2) -0.0221(4) 0.2212(4) 0.0386(14) Uani 1 1 d . . . N3B N 0.1075(3) -0.0059(4) 0.1189(4) 0.0388(15) Uani 1 1 d . . . N2A N 0.0101(2) 0.1776(4) 0.4987(4) 0.0409(14) Uani 1 1 d . . . N4B N 0.1533(3) 0.0668(5) 0.1321(4) 0.0439(15) Uani 1 1 d . . . N1A N -0.0178(3) 0.2362(4) 0.4146(4) 0.0412(15) Uani 1 1 d . . . N4A N -0.0683(3) 0.2684(5) 0.5832(5) 0.0519(16) Uani 1 1 d . . . C5A C -0.0649(3) 0.2902(5) 0.4669(6) 0.0409(18) Uani 1 1 d . . . N7A N -0.0830(3) 0.3733(5) 0.2849(5) 0.0718(19) Uani 1 1 d . . . N11A N -0.1527(4) 0.4164(6) 0.4459(5) 0.083(2) Uani 1 1 d . . . C8B C 0.2091(4) 0.2540(7) 0.4827(6) 0.069(2) Uani 1 1 d . . . H2 H 0.1994 0.2672 0.5619 0.083 Uiso 1 1 calc R . . C9B C 0.2616(4) 0.3042(7) 0.4329(7) 0.080(3) Uani 1 1 d . . . H3 H 0.2877 0.3495 0.4773 0.097 Uiso 1 1 calc R . . C10B C 0.2742(4) 0.2853(6) 0.3166(7) 0.076(3) Uani 1 1 d . . . H4 H 0.3090 0.3196 0.2805 0.091 Uiso 1 1 calc R . . C6B C 0.1885(4) 0.1714(6) 0.3083(6) 0.0491(19) Uani 1 1 d . . . C5B C 0.1491(3) 0.0947(5) 0.2452(6) 0.0375(17) Uani 1 1 d . . . C6A C -0.1035(4) 0.3647(6) 0.3981(7) 0.057(2) Uani 1 1 d . . . C8A C -0.1152(5) 0.4416(8) 0.2162(7) 0.098(3) Uani 1 1 d . . . H2A H -0.1019 0.4505 0.1380 0.117 Uiso 1 1 calc R . . C10A C -0.1857(5) 0.4838(8) 0.3739(9) 0.101(3) Uani 1 1 d . . . H4A H -0.2214 0.5208 0.4031 0.121 Uiso 1 1 calc R . . C9A C -0.1662(6) 0.4980(8) 0.2565(9) 0.115(4) Uani 1 1 d . . . H3A H -0.1880 0.5453 0.2072 0.138 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0636(6) 0.0763(7) 0.0193(4) 0.0058(5) 0.0080(4) 0.0151(5) Cu3 0.0494(8) 0.0650(9) 0.0189(6) 0.000 0.0064(5) 0.000 Cu2 0.0739(10) 0.0969(11) 0.0213(7) 0.000 0.0036(6) 0.000 N7B 0.070(5) 0.072(5) 0.027(3) -0.001(3) -0.005(3) -0.006(4) N11B 0.065(5) 0.085(5) 0.048(4) -0.013(4) 0.004(4) -0.021(4) N1B 0.040(4) 0.054(4) 0.017(3) -0.005(3) -0.003(3) -0.002(3) N3A 0.054(4) 0.059(4) 0.019(3) 0.006(3) 0.005(3) 0.006(3) N2B 0.045(4) 0.054(4) 0.018(3) 0.000(3) 0.006(3) -0.001(3) N3B 0.048(4) 0.048(4) 0.020(3) -0.002(3) 0.007(3) -0.014(3) N2A 0.059(4) 0.048(4) 0.016(3) 0.001(3) 0.003(3) 0.004(3) N4B 0.061(4) 0.056(4) 0.014(3) -0.004(3) 0.007(3) -0.009(4) N1A 0.051(4) 0.049(4) 0.024(3) 0.002(3) -0.003(3) 0.007(3) N4A 0.061(5) 0.072(5) 0.023(4) 0.002(3) 0.001(3) 0.015(4) C5A 0.045(5) 0.049(5) 0.029(4) 0.000(4) 0.004(4) 0.010(4) N7A 0.094(5) 0.083(5) 0.038(4) 0.009(4) -0.008(4) 0.020(4) N11A 0.092(6) 0.090(5) 0.069(5) -0.013(5) -0.008(4) 0.046(5) C8B 0.091(7) 0.081(6) 0.034(5) -0.018(5) -0.013(5) -0.014(6) C9B 0.080(7) 0.103(8) 0.058(6) -0.023(6) -0.015(5) -0.020(6) C10B 0.081(7) 0.081(7) 0.065(6) -0.014(5) 0.006(5) -0.028(5) C6B 0.045(5) 0.068(6) 0.035(4) -0.001(4) 0.005(4) -0.002(4) C5B 0.040(4) 0.046(5) 0.026(4) 0.007(4) 0.003(4) -0.010(4) C6A 0.068(6) 0.054(5) 0.048(6) -0.011(4) -0.008(4) 0.019(5) C8A 0.134(9) 0.100(8) 0.059(6) 0.022(6) -0.005(6) 0.046(7) C10A 0.099(8) 0.095(8) 0.109(9) -0.016(7) -0.020(7) 0.058(6) C9A 0.155(11) 0.113(8) 0.078(8) -0.013(8) -0.019(7) 0.072(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 Cu1 N3B 1.962(5) 8_556 ? Cu1 N2A 1.995(5) . ? Cu1 N1B 2.014(5) . ? Cu1 N7B 2.251(6) . ? Cu3 N3A 1.995(5) 5_556 ? Cu3 N3A 1.995(5) 8 ? Cu3 N2B 2.030(5) . ? Cu3 N2B 2.030(5) 4 ? Cu2 N1A 1.933(5) . ? Cu2 N1A 1.933(5) 4 ? Cu2 N7A 2.197(6) 4 ? Cu2 N7A 2.197(6) . ? N7B C8B 1.337(8) . ? N7B C6B 1.347(8) . ? N11B C6B 1.322(8) . ? N11B C10B 1.357(8) . ? N1B C5B 1.324(7) . ? N1B N2B 1.343(6) . ? N3A N2A 1.330(6) . ? N3A N4A 1.331(6) . ? N3A Cu3 1.995(5) 5_556 ? N2B N3B 1.338(6) . ? N3B N4B 1.323(6) . ? N3B Cu1 1.962(5) 8 ? N2A N1A 1.331(6) . ? N4B C5B 1.325(7) . ? N1A C5A 1.323(7) . ? N4A C5A 1.342(7) . ? C5A C6A 1.454(9) . ? N7A C8A 1.333(9) . ? N7A C6A 1.348(8) . ? N11A C6A 1.318(8) . ? N11A C10A 1.357(9) . ? C8B C9B 1.371(10) . ? C8B H2 0.9300 . ? C9B C10B 1.357(9) . ? C9B H3 0.9300 . ? C10B H4 0.9300 . ? C6B C5B 1.450(9) . ? C8A C9A 1.347(11) . ? C8A H2A 0.9300 . ? C10A C9A 1.393(12) . ? C10A H4A 0.9300 . ? C9A H3A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3B Cu1 N2A 110.3(2) 8_556 . ? N3B Cu1 N1B 130.0(2) 8_556 . ? N2A Cu1 N1B 114.6(2) . . ? N3B Cu1 N7B 109.4(2) 8_556 . ? N2A Cu1 N7B 107.2(2) . . ? N1B Cu1 N7B 77.3(2) . . ? N3A Cu3 N3A 122.5(3) 5_556 8 ? N3A Cu3 N2B 105.5(2) 5_556 . ? N3A Cu3 N2B 109.2(2) 8 . ? N3A Cu3 N2B 109.2(2) 5_556 4 ? N3A Cu3 N2B 105.5(2) 8 4 ? N2B Cu3 N2B 103.4(3) . 4 ? N1A Cu2 N1A 155.9(3) . 4 ? N1A Cu2 N7A 116.4(2) . 4 ? N1A Cu2 N7A 78.9(2) 4 4 ? N1A Cu2 N7A 78.9(2) . . ? N1A Cu2 N7A 116.4(2) 4 . ? N7A Cu2 N7A 105.6(3) 4 . ? C8B N7B C6B 115.1(6) . . ? C8B N7B Cu1 133.7(5) . . ? C6B N7B Cu1 111.0(5) . . ? C6B N11B C10B 116.2(6) . . ? C5B N1B N2B 105.3(5) . . ? C5B N1B Cu1 117.2(5) . . ? N2B N1B Cu1 137.4(4) . . ? N2A N3A N4A 111.0(5) . . ? N2A N3A Cu3 122.1(5) . 5_556 ? N4A N3A Cu3 126.8(4) . 5_556 ? N3B N2B N1B 107.3(5) . . ? N3B N2B Cu3 127.1(4) . . ? N1B N2B Cu3 125.6(4) . . ? N4B N3B N2B 110.6(5) . . ? N4B N3B Cu1 126.5(4) . 8 ? N2B N3B Cu1 122.9(4) . 8 ? N3A N2A N1A 107.3(5) . . ? N3A N2A Cu1 128.2(4) . . ? N1A N2A Cu1 124.5(4) . . ? N3B N4B C5B 104.3(5) . . ? C5A N1A N2A 106.5(5) . . ? C5A N1A Cu2 117.3(5) . . ? N2A N1A Cu2 135.9(5) . . ? N3A N4A C5A 103.7(5) . . ? N1A C5A N4A 111.5(6) . . ? N1A C5A C6A 119.7(7) . . ? N4A C5A C6A 128.8(7) . . ? C8A N7A C6A 116.6(7) . . ? C8A N7A Cu2 132.2(6) . . ? C6A N7A Cu2 111.3(5) . . ? C6A N11A C10A 116.6(7) . . ? N7B C8B C9B 122.9(7) . . ? N7B C8B H2 118.6 . . ? C9B C8B H2 118.6 . . ? C10B C9B C8B 117.6(7) . . ? C10B C9B H3 121.2 . . ? C8B C9B H3 121.2 . . ? N11B C10B C9B 121.7(7) . . ? N11B C10B H4 119.2 . . ? C9B C10B H4 119.2 . . ? N11B C6B N7B 126.5(7) . . ? N11B C6B C5B 118.7(6) . . ? N7B C6B C5B 114.7(7) . . ? N4B C5B N1B 112.5(6) . . ? N4B C5B C6B 127.9(6) . . ? N1B C5B C6B 119.6(6) . . ? N11A C6A N7A 125.9(7) . . ? N11A C6A C5A 121.4(7) . . ? N7A C6A C5A 112.7(7) . . ? N7A C8A C9A 122.1(8) . . ? N7A C8A H2A 118.9 . . ? C9A C8A H2A 118.9 . . ? N11A C10A C9A 120.4(8) . . ? N11A C10A H4A 119.8 . . ? C9A C10A H4A 119.8 . . ? C8A C9A C10A 118.3(9) . . ? C8A C9A H3A 120.8 . . ? C10A C9A H3A 120.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.73 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.291 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.058 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 -0.013 139 15 ' ' 2 0.000 0.500 -0.011 139 15 ' ' _platon_squeeze_details ; ; data_compound2 _database_code_depnum_ccdc_archive 'CCDC 734266' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6 Cl2 N12 Pd2' _chemical_formula_weight 577.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M C2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.660(4) _cell_length_b 5.2273(10) _cell_length_c 14.055(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.884(3) _cell_angle_gamma 90.00 _cell_volume 1522.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 907 _cell_measurement_theta_min 2.978 _cell_measurement_theta_max 20.882 _exptl_crystal_description PRISMATIC _exptl_crystal_colour 'color less' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 2.741 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7453 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6073 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.64 _reflns_number_total 1443 _reflns_number_gt 1103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1443 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N7 N 0.37403(19) 0.3928(8) 0.4111(3) 0.0260(10) Uani 1 1 d . . . N1 N 0.26430(19) 0.4352(8) 0.4257(3) 0.0246(9) Uani 1 1 d . . . N3 N 0.1854(2) 0.7057(8) 0.3673(3) 0.0312(10) Uani 1 1 d . . . N4 N 0.2288(2) 0.7786(8) 0.3304(3) 0.0316(11) Uani 1 1 d . . . N2 N 0.20641(19) 0.4994(8) 0.4245(3) 0.0250(10) Uani 1 1 d . . . C10 C 0.4100(3) 0.7188(11) 0.2957(4) 0.0397(14) Uani 1 1 d . . . H10 H 0.4231 0.8322 0.2571 0.048 Uiso 1 1 calc R . . N11 N 0.3529(2) 0.7570(8) 0.3009(3) 0.0333(11) Uani 1 1 d . . . C8 C 0.4305(3) 0.3568(10) 0.4024(4) 0.0344(13) Uani 1 1 d . . . H8 H 0.4566 0.2192 0.4359 0.041 Uiso 1 1 calc R . . C5 C 0.2764(3) 0.6085(10) 0.3680(4) 0.0271(12) Uani 1 1 d . . . C6 C 0.3376(2) 0.5894(10) 0.3573(4) 0.0270(12) Uani 1 1 d . . . C9 C 0.4495(3) 0.5198(11) 0.3448(4) 0.0416(15) Uani 1 1 d . . . H9 H 0.4887 0.4963 0.3391 0.050 Uiso 1 1 calc R . . Cl1 Cl 0.42771(6) -0.0511(3) 0.57274(11) 0.0387(4) Uani 1 1 d . . . Pd1 Pd 0.336755(18) 0.18808(8) 0.49685(3) 0.02475(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N7 0.020(2) 0.030(3) 0.024(2) -0.0009(19) 0.0051(19) -0.0006(18) N1 0.021(2) 0.030(2) 0.022(2) -0.0008(19) 0.0074(19) -0.0001(19) N3 0.032(2) 0.030(2) 0.031(2) 0.009(2) 0.013(2) 0.005(2) N4 0.031(2) 0.035(3) 0.029(2) 0.008(2) 0.012(2) 0.003(2) N2 0.020(2) 0.032(3) 0.019(2) 0.0020(19) 0.0031(19) 0.0022(18) C10 0.034(3) 0.053(4) 0.034(3) 0.008(3) 0.016(3) -0.009(3) N11 0.036(3) 0.034(3) 0.031(3) 0.004(2) 0.015(2) -0.004(2) C8 0.029(3) 0.042(4) 0.035(3) 0.001(3) 0.015(3) 0.004(3) C5 0.030(3) 0.026(3) 0.019(3) -0.001(2) 0.005(2) -0.002(2) C6 0.026(3) 0.030(3) 0.024(3) -0.004(2) 0.009(2) -0.004(2) C9 0.034(3) 0.059(4) 0.038(3) 0.008(3) 0.021(3) 0.005(3) Cl1 0.0292(7) 0.0465(9) 0.0414(8) 0.0113(7) 0.0154(7) 0.0145(7) Pd1 0.0226(2) 0.0270(2) 0.0243(2) 0.00228(19) 0.00904(17) 0.00273(19) _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 N7 C6 1.343(6) . ? N7 C8 1.346(6) . ? N7 Pd1 2.034(4) . ? N1 C5 1.317(6) . ? N1 N2 1.348(5) . ? N1 Pd1 2.008(4) . ? N3 N2 1.314(5) . ? N3 N4 1.340(6) . ? N4 C5 1.331(6) . ? N2 Pd1 2.003(4) 7_556 ? C10 N11 1.340(7) . ? C10 C9 1.365(7) . ? N11 C6 1.318(6) . ? C8 C9 1.360(7) . ? C5 C6 1.457(7) . ? Cl1 Pd1 2.2735(14) . ? Pd1 N2 2.003(4) 7_556 ? 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 C6 N7 C8 116.5(4) . . ? C6 N7 Pd1 115.3(3) . . ? C8 N7 Pd1 128.2(4) . . ? C5 N1 N2 105.4(4) . . ? C5 N1 Pd1 114.6(3) . . ? N2 N1 Pd1 139.6(3) . . ? N2 N3 N4 109.3(4) . . ? C5 N4 N3 105.1(4) . . ? N3 N2 N1 108.7(4) . . ? N3 N2 Pd1 127.1(3) . 7_556 ? N1 N2 Pd1 124.2(3) . 7_556 ? N11 C10 C9 122.5(5) . . ? C6 N11 C10 115.4(5) . . ? N7 C8 C9 120.6(5) . . ? N1 C5 N4 111.5(5) . . ? N1 C5 C6 117.4(5) . . ? N4 C5 C6 131.0(5) . . ? N11 C6 N7 126.5(5) . . ? N11 C6 C5 120.6(5) . . ? N7 C6 C5 112.9(4) . . ? C8 C9 C10 118.5(5) . . ? N2 Pd1 N1 96.08(16) 7_556 . ? N2 Pd1 N7 175.58(16) 7_556 . ? N1 Pd1 N7 79.54(16) . . ? N2 Pd1 Cl1 91.40(12) 7_556 . ? N1 Pd1 Cl1 171.99(12) . . ? N7 Pd1 Cl1 93.00(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.766 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.130 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 734267' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H23 Cl N10 Ni O2' _chemical_formula_weight 397.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5313(6) _cell_length_b 8.8434(6) _cell_length_c 12.5234(8) _cell_angle_alpha 94.7760(10) _cell_angle_beta 108.3050(10) _cell_angle_gamma 105.4280(10) _cell_volume 850.22(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6120 _cell_measurement_theta_min 2430 _cell_measurement_theta_max 28240 _exptl_crystal_description prismatic _exptl_crystal_colour PINK _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 1.324 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.832676 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8383 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2980 _reflns_number_gt 2820 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker smart' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.1899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2980 _refine_ls_number_parameters 256 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.26944(16) 0.02777(15) 0.10476(11) 0.0334(3) Uani 1 1 d . . . N2 N 0.13764(18) -0.10824(17) 0.07416(12) 0.0397(3) Uani 1 1 d . . . C5 C 0.3021(2) 0.05293(19) 0.00948(13) 0.0336(3) Uani 1 1 d . . . C6 C 0.4421(2) 0.19411(19) 0.01350(13) 0.0336(3) Uani 1 1 d . . . N11 N 0.4784(2) 0.21653(18) -0.08094(12) 0.0432(4) Uani 1 1 d . . . N4 N 0.19791(19) -0.06168(17) -0.07967(12) 0.0423(3) Uani 1 1 d . . . N3 N 0.09542(19) -0.16112(18) -0.03619(13) 0.0450(4) Uani 1 1 d . . . C8 C 0.6570(2) 0.4160(2) 0.12496(15) 0.0407(4) Uani 1 1 d . . . H6A H 0.7174 0.4848 0.1950 0.049 Uiso 1 1 calc R . . C9 C 0.7060(3) 0.4482(2) 0.03268(16) 0.0466(4) Uani 1 1 d . . . H5A H 0.7989 0.5365 0.0391 0.056 Uiso 1 1 calc R . . C10 C 0.6125(3) 0.3449(2) -0.06912(16) 0.0476(4) Uani 1 1 d . . . H4A H 0.6434 0.3647 -0.1327 0.057 Uiso 1 1 calc R . . C2B C 0.7476(2) 0.1448(2) 0.40380(15) 0.0424(4) Uani 1 1 d . . . H1B2 H 0.8515 0.1132 0.4160 0.051 Uiso 1 1 calc R . . H2B2 H 0.6962 0.1070 0.4594 0.051 Uiso 1 1 calc R . . C3C C 0.1520(2) 0.1162(2) 0.33691(17) 0.0478(4) Uani 1 1 d . . . H1C3 H 0.1094 0.0941 0.3990 0.057 Uiso 1 1 calc R . . H2C3 H 0.0667 0.0482 0.2667 0.057 Uiso 1 1 calc R . . C3B C 0.7937(2) 0.3242(2) 0.41894(16) 0.0452(4) Uani 1 1 d . . . H2B3 H 0.8663 0.3718 0.4976 0.054 Uiso 1 1 calc R . . H1B3 H 0.8580 0.3631 0.3700 0.054 Uiso 1 1 calc R . . C2C C 0.1794(3) 0.2890(2) 0.32635(17) 0.0504(5) Uani 1 1 d . . . H2C2 H 0.0690 0.3106 0.3049 0.061 Uiso 1 1 calc R . . H1C2 H 0.2546 0.3567 0.3993 0.061 Uiso 1 1 calc R . . N4C N 0.31819(19) 0.08332(19) 0.35936(13) 0.0364(3) Uani 1 1 d . . . O1W O 0.0447(3) -0.2898(2) 0.24009(18) 0.0739(5) Uani 1 1 d D . . O2W O 0.8325(3) 0.7182(2) 0.37523(18) 0.0769(5) Uani 1 1 d . . . H21W H 0.877(4) 0.738(3) 0.329(2) 0.080(10) Uiso 1 1 d . . . H11W H 0.066(4) -0.241(4) 0.179(2) 0.125(12) Uiso 1 1 d D . . H12W H 0.129(4) -0.303(4) 0.274(3) 0.098(12) Uiso 1 1 d . . . H22W H 0.752(4) 0.759(4) 0.353(3) 0.113(13) Uiso 1 1 d . . . H1B1 H 0.578(2) -0.020(2) 0.2847(16) 0.036(5) Uiso 1 1 d . . . H2B4 H 0.657(2) 0.471(2) 0.3788(16) 0.042(5) Uiso 1 1 d . . . H1B4 H 0.603(2) 0.369(2) 0.4490(18) 0.043(5) Uiso 1 1 d . . . H2B1 H 0.676(3) 0.078(2) 0.2433(18) 0.045(6) Uiso 1 1 d . . . H1C4 H 0.380(2) 0.118(2) 0.4272(18) 0.037(5) Uiso 1 1 d . . . H1C1 H 0.308(3) 0.424(2) 0.2488(16) 0.041(5) Uiso 1 1 d . . . H2C1 H 0.180(3) 0.297(2) 0.1727(18) 0.048(6) Uiso 1 1 d . . . H2C4 H 0.303(3) -0.020(3) 0.3477(18) 0.053(6) Uiso 1 1 d . . . Ni1 Ni 0.43774(2) 0.19629(2) 0.251702(15) 0.02863(8) Uani 1 1 d . . . Cl2 Cl 0.55703(6) 0.28117(5) -0.36836(4) 0.04517(12) Uani 1 1 d . . . N4B N 0.63381(18) 0.36971(17) 0.38915(12) 0.0352(3) Uani 1 1 d . . . N1C N 0.2588(2) 0.32426(19) 0.23884(13) 0.0364(3) Uani 1 1 d . . . N7 N 0.52471(17) 0.28857(16) 0.11695(11) 0.0334(3) Uani 1 1 d . . . N1B N 0.6235(2) 0.0740(2) 0.28706(13) 0.0379(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0327(7) 0.0337(7) 0.0281(7) -0.0024(5) 0.0071(6) 0.0078(6) N2 0.0346(7) 0.0364(8) 0.0395(8) -0.0021(6) 0.0072(6) 0.0069(6) C5 0.0363(8) 0.0367(8) 0.0251(8) -0.0014(6) 0.0057(6) 0.0151(7) C6 0.0396(9) 0.0377(9) 0.0250(8) 0.0020(6) 0.0097(7) 0.0173(7) N11 0.0571(9) 0.0475(9) 0.0274(7) 0.0042(6) 0.0168(7) 0.0185(7) N4 0.0440(8) 0.0437(8) 0.0290(7) -0.0049(6) 0.0037(6) 0.0115(7) N3 0.0399(8) 0.0421(8) 0.0386(8) -0.0078(7) 0.0016(7) 0.0086(7) C8 0.0442(10) 0.0403(9) 0.0321(9) 0.0015(7) 0.0118(7) 0.0080(8) C9 0.0499(11) 0.0477(11) 0.0424(10) 0.0105(8) 0.0204(8) 0.0097(8) C10 0.0617(12) 0.0524(11) 0.0377(10) 0.0129(8) 0.0271(9) 0.0192(9) C2B 0.0358(9) 0.0538(11) 0.0350(9) 0.0068(8) 0.0086(7) 0.0149(8) C3C 0.0398(10) 0.0581(12) 0.0470(11) 0.0099(9) 0.0222(8) 0.0087(8) C3B 0.0323(9) 0.0515(11) 0.0389(10) -0.0002(8) 0.0070(7) 0.0014(8) C2C 0.0504(11) 0.0597(12) 0.0510(11) 0.0031(9) 0.0273(9) 0.0234(9) N4C 0.0386(8) 0.0366(8) 0.0278(8) 0.0014(6) 0.0102(6) 0.0044(6) O1W 0.0616(11) 0.0795(12) 0.0772(13) 0.0197(10) 0.0283(10) 0.0098(9) O2W 0.0709(12) 0.0802(12) 0.0855(14) 0.0215(10) 0.0319(11) 0.0257(10) Ni1 0.03031(12) 0.02962(12) 0.02227(12) -0.00070(8) 0.00833(8) 0.00601(8) Cl2 0.0555(3) 0.0434(2) 0.0311(2) 0.00162(17) 0.01555(19) 0.0074(2) N4B 0.0390(8) 0.0331(8) 0.0274(7) -0.0013(6) 0.0119(6) 0.0033(6) N1C 0.0383(8) 0.0331(8) 0.0340(8) 0.0000(6) 0.0098(7) 0.0099(6) N7 0.0378(7) 0.0366(7) 0.0248(7) 0.0016(5) 0.0105(6) 0.0117(6) N1B 0.0417(8) 0.0387(9) 0.0334(8) 0.0019(6) 0.0134(7) 0.0134(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 N1 C5 1.331(2) . ? N1 N2 1.3383(19) . ? N1 Ni1 2.1010(12) . ? N2 N3 1.322(2) . ? C5 N4 1.331(2) . ? C5 C6 1.465(2) . ? C6 N11 1.331(2) . ? C6 N7 1.344(2) . ? N11 C10 1.339(2) . ? N4 N3 1.343(2) . ? C8 N7 1.337(2) . ? C8 C9 1.374(3) . ? C9 C10 1.370(3) . ? C2B N1B 1.474(2) . ? C2B C3B 1.510(3) . ? C3C N4C 1.468(2) . ? C3C C2C 1.507(3) . ? C3B N4B 1.469(2) . ? C2C N1C 1.473(2) . ? N4C Ni1 2.0981(14) . ? Ni1 N1B 2.1043(15) . ? Ni1 N1C 2.1051(14) . ? Ni1 N4B 2.1213(14) . ? Ni1 N7 2.1812(13) . ? 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 C5 N1 N2 105.25(12) . . ? C5 N1 Ni1 114.70(10) . . ? N2 N1 Ni1 139.95(11) . . ? N3 N2 N1 108.35(14) . . ? N1 C5 N4 112.26(15) . . ? N1 C5 C6 119.28(13) . . ? N4 C5 C6 128.46(15) . . ? N11 C6 N7 126.26(16) . . ? N11 C6 C5 119.26(14) . . ? N7 C6 C5 114.46(14) . . ? C6 N11 C10 115.61(15) . . ? C5 N4 N3 103.81(14) . . ? N2 N3 N4 110.34(13) . . ? N7 C8 C9 121.83(16) . . ? C10 C9 C8 117.26(17) . . ? N11 C10 C9 122.76(17) . . ? N1B C2B C3B 109.09(14) . . ? N4C C3C C2C 108.70(15) . . ? N4B C3B C2B 109.35(14) . . ? N1C C2C C3C 109.36(14) . . ? C3C N4C Ni1 107.63(11) . . ? N4C Ni1 N1 93.66(6) . . ? N4C Ni1 N1B 92.37(7) . . ? N1 Ni1 N1B 93.36(5) . . ? N4C Ni1 N1C 82.65(6) . . ? N1 Ni1 N1C 92.24(6) . . ? N1B Ni1 N1C 172.74(6) . . ? N4C Ni1 N4B 93.13(6) . . ? N1 Ni1 N4B 172.09(5) . . ? N1B Ni1 N4B 82.29(6) . . ? N1C Ni1 N4B 92.66(6) . . ? N4C Ni1 N7 170.62(5) . . ? N1 Ni1 N7 77.22(5) . . ? N1B Ni1 N7 90.37(6) . . ? N1C Ni1 N7 95.38(5) . . ? N4B Ni1 N7 96.13(6) . . ? C3B N4B Ni1 108.83(10) . . ? C2C N1C Ni1 108.16(11) . . ? C8 N7 C6 116.26(14) . . ? C8 N7 Ni1 129.29(11) . . ? C6 N7 Ni1 114.13(11) . . ? C2B N1B Ni1 107.30(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.196 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.045 data_compound4 _database_code_depnum_ccdc_archive 'CCDC 734268' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H21 Cl Cu N10 O4' _chemical_formula_weight 456.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.2828(5) _cell_length_b 7.8531(3) _cell_length_c 15.2177(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.5550(10) _cell_angle_gamma 90.00 _cell_volume 1731.45(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2743 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 25.04 _exptl_crystal_description prismatic _exptl_crystal_colour blu _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.102 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 1.461 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9209 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3054 _reflns_number_gt 2743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.4293P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3054 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.762256(17) 0.22072(3) 0.393581(18) 0.01164(11) Uani 1 1 d . . . Cl1 Cl 0.38430(4) 0.23288(7) 0.02406(4) 0.01527(15) Uani 1 1 d . . . O1 O 0.35313(12) 0.2344(2) 0.10412(13) 0.0262(4) Uani 1 1 d . . . O2 O 0.33815(13) 0.3637(2) -0.03917(12) 0.0319(5) Uani 1 1 d . . . O3 O 0.36269(13) 0.0708(2) -0.02154(12) 0.0312(4) Uani 1 1 d . . . O4 O 0.48173(12) 0.2619(3) 0.05370(13) 0.0337(5) Uani 1 1 d . . . N1A N 1.08475(12) 0.3488(2) 0.51579(13) 0.0155(4) Uani 1 1 d . . . N2A N 0.98478(12) 0.1461(2) 0.41515(12) 0.0139(4) Uani 1 1 d . . . N3A N 0.98107(14) 0.2700(2) 0.64073(14) 0.0160(4) Uani 1 1 d . . . N4A N 0.90460(14) 0.2587(2) 0.66676(14) 0.0177(5) Uani 1 1 d . . . N5A N 0.83169(14) 0.2329(2) 0.59398(14) 0.0172(4) Uani 1 1 d . . . N6A N 0.85878(13) 0.2252(2) 0.51800(13) 0.0135(4) Uani 1 1 d . . . N1B N 0.65568(13) 0.2328(2) 0.27021(13) 0.0119(4) Uani 1 1 d . . . N2B N 0.82410(12) 0.3943(2) 0.32988(12) 0.0136(4) Uani 1 1 d . . . H2B1 H 0.8594 0.4678 0.3717 0.016 Uiso 1 1 calc R . . H2B2 H 0.8598 0.3406 0.3016 0.016 Uiso 1 1 calc R . . N3B N 0.78516(12) -0.0270(2) 0.34490(13) 0.0159(4) Uani 1 1 d . . . H3B1 H 0.8457 -0.0437 0.3540 0.019 Uiso 1 1 calc R . . H3B2 H 0.7648 -0.1089 0.3750 0.019 Uiso 1 1 calc R . . N4B N 0.65810(13) 0.2168(2) 0.45154(14) 0.0170(4) Uani 1 1 d . . . H4B1 H 0.6654 0.1262 0.4894 0.020 Uiso 1 1 calc R . . H4B2 H 0.6611 0.3115 0.4857 0.020 Uiso 1 1 calc R . . C1A C 1.03833(15) 0.1503(3) 0.36065(15) 0.0163(5) Uani 1 1 d . . . H1A H 1.0234 0.0814 0.3082 0.020 Uiso 1 1 calc R . . C2A C 1.11488(17) 0.2535(3) 0.37984(18) 0.0196(5) Uani 1 1 d . . . H2A H 1.1506 0.2582 0.3406 0.023 Uiso 1 1 calc R . . C3A C 1.13641(15) 0.3497(3) 0.45958(16) 0.0189(5) Uani 1 1 d . . . H3A H 1.1889 0.4178 0.4749 0.023 Uiso 1 1 calc R . . C4A C 1.01028(16) 0.2472(3) 0.48979(16) 0.0129(5) Uani 1 1 d . . . C5A C 0.95089(16) 0.2479(3) 0.54886(16) 0.0130(5) Uani 1 1 d . . . C1B C 0.56652(15) 0.2075(3) 0.37911(16) 0.0180(5) Uani 1 1 d . . . H1B1 H 0.5204 0.2631 0.4006 0.022 Uiso 1 1 calc R . . H1B2 H 0.5485 0.0895 0.3655 0.022 Uiso 1 1 calc R . . C2B C 0.74775(15) 0.4846(3) 0.26158(15) 0.0155(5) Uani 1 1 d . . . H2B3 H 0.7713 0.5520 0.2206 0.019 Uiso 1 1 calc R . . H2B4 H 0.7173 0.5604 0.2930 0.019 Uiso 1 1 calc R . . C3B C 0.73277(15) -0.0295(3) 0.24517(15) 0.0162(5) Uani 1 1 d . . . H3B3 H 0.7230 -0.1461 0.2232 0.019 Uiso 1 1 calc R . . H3B4 H 0.7670 0.0296 0.2106 0.019 Uiso 1 1 calc R . . C4B C 0.64077(15) 0.0574(3) 0.23076(15) 0.0149(5) Uani 1 1 d . . . H4B3 H 0.6069 0.0630 0.1650 0.018 Uiso 1 1 calc R . . H4B4 H 0.6045 -0.0080 0.2608 0.018 Uiso 1 1 calc R . . C5B C 0.57318(15) 0.2953(3) 0.29294(16) 0.0159(5) Uani 1 1 d . . . H5B1 H 0.5178 0.2727 0.2414 0.019 Uiso 1 1 calc R . . H5B2 H 0.5779 0.4174 0.3030 0.019 Uiso 1 1 calc R . . C6B C 0.68016(15) 0.3527(3) 0.20640(15) 0.0142(5) Uani 1 1 d . . . H6B1 H 0.6249 0.4088 0.1674 0.017 Uiso 1 1 calc R . . H6B2 H 0.7075 0.2905 0.1667 0.017 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01320(17) 0.01315(18) 0.00877(17) 0.00025(10) 0.00378(12) -0.00114(10) Cl1 0.0172(3) 0.0164(3) 0.0125(3) 0.0008(2) 0.0052(2) 0.0006(2) O1 0.0278(10) 0.0349(11) 0.0211(10) -0.0040(7) 0.0151(8) 0.0003(8) O2 0.0394(11) 0.0214(10) 0.0257(10) 0.0083(8) -0.0026(8) 0.0018(8) O3 0.0476(12) 0.0202(10) 0.0265(10) -0.0074(8) 0.0127(8) 0.0015(8) O4 0.0155(9) 0.0657(14) 0.0193(10) 0.0002(9) 0.0048(8) -0.0038(8) N1A 0.0150(10) 0.0124(10) 0.0182(10) 0.0020(8) 0.0042(8) 0.0003(8) N2A 0.0165(10) 0.0139(10) 0.0107(9) 0.0007(8) 0.0034(8) 0.0022(8) N3A 0.0182(10) 0.0181(10) 0.0119(11) -0.0008(8) 0.0048(8) -0.0005(8) N4A 0.0204(11) 0.0219(11) 0.0111(10) -0.0011(8) 0.0055(9) -0.0003(8) N5A 0.0194(11) 0.0207(11) 0.0126(11) 0.0006(8) 0.0069(9) -0.0005(8) N6A 0.0157(10) 0.0146(10) 0.0114(10) 0.0005(7) 0.0062(8) -0.0001(7) N1B 0.0138(10) 0.0131(10) 0.0099(10) 0.0002(7) 0.0053(8) 0.0004(7) N2B 0.0153(9) 0.0131(10) 0.0128(10) -0.0001(8) 0.0049(7) -0.0012(7) N3B 0.0158(10) 0.0137(10) 0.0178(10) 0.0022(8) 0.0050(8) 0.0011(8) N4B 0.0172(10) 0.0216(11) 0.0125(10) -0.0001(8) 0.0054(8) -0.0020(8) C1A 0.0211(12) 0.0150(12) 0.0132(12) 0.0033(9) 0.0060(9) 0.0065(9) C2A 0.0216(13) 0.0196(13) 0.0228(14) 0.0037(10) 0.0145(11) 0.0049(10) C3A 0.0161(12) 0.0143(12) 0.0282(14) 0.0024(10) 0.0095(10) 0.0018(9) C4A 0.0145(12) 0.0110(11) 0.0112(12) 0.0041(8) 0.0014(9) 0.0039(8) C5A 0.0162(12) 0.0088(11) 0.0125(12) 0.0001(8) 0.0026(9) 0.0009(8) C1B 0.0136(12) 0.0258(14) 0.0159(12) -0.0005(10) 0.0065(10) -0.0003(9) C2B 0.0194(12) 0.0126(12) 0.0162(12) 0.0030(9) 0.0082(9) 0.0001(9) C3B 0.0205(12) 0.0137(12) 0.0148(12) -0.0014(9) 0.0062(9) 0.0009(9) C4B 0.0158(11) 0.0162(12) 0.0125(11) -0.0028(9) 0.0043(9) -0.0028(9) C5B 0.0119(11) 0.0205(13) 0.0160(12) -0.0006(10) 0.0054(9) 0.0019(9) C6B 0.0171(11) 0.0159(12) 0.0107(11) 0.0034(9) 0.0062(9) 0.0025(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6A 1.9962(19) . ? Cu1 N4B 2.0509(19) . ? Cu1 N1B 2.0592(19) . ? Cu1 N2B 2.0677(18) . ? Cu1 N3B 2.1493(19) . ? Cl1 O4 1.4301(19) . ? Cl1 O2 1.4307(17) . ? Cl1 O3 1.4369(18) . ? Cl1 O1 1.4425(18) . ? N1A C3A 1.336(3) . ? N1A C4A 1.342(3) . ? N2A C1A 1.338(3) . ? N2A C4A 1.338(3) . ? N3A C5A 1.337(3) . ? N3A N4A 1.351(3) . ? N4A N5A 1.313(3) . ? N5A N6A 1.348(3) . ? N6A C5A 1.346(3) . ? N1B C6B 1.484(3) . ? N1B C4B 1.491(3) . ? N1B C5B 1.493(3) . ? N2B C2B 1.474(3) . ? N3B C3B 1.474(3) . ? N4B C1B 1.482(3) . ? C1A C2A 1.376(3) . ? C2A C3A 1.377(3) . ? C4A C5A 1.467(3) . ? C1B C5B 1.514(3) . ? C2B C6B 1.514(3) . ? C3B C4B 1.515(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 N6A Cu1 N4B 91.88(8) . . ? N6A Cu1 N1B 174.47(7) . . ? N4B Cu1 N1B 84.02(7) . . ? N6A Cu1 N2B 97.07(7) . . ? N4B Cu1 N2B 138.13(8) . . ? N1B Cu1 N2B 83.63(7) . . ? N6A Cu1 N3B 100.98(7) . . ? N4B Cu1 N3B 111.62(7) . . ? N1B Cu1 N3B 84.01(7) . . ? N2B Cu1 N3B 106.64(7) . . ? O4 Cl1 O2 109.79(12) . . ? O4 Cl1 O3 110.47(12) . . ? O2 Cl1 O3 108.84(11) . . ? O4 Cl1 O1 108.83(11) . . ? O2 Cl1 O1 109.72(11) . . ? O3 Cl1 O1 109.17(11) . . ? C3A N1A C4A 115.6(2) . . ? C1A N2A C4A 116.17(19) . . ? C5A N3A N4A 104.79(18) . . ? N5A N4A N3A 110.12(19) . . ? N4A N5A N6A 108.70(18) . . ? C5A N6A N5A 105.50(18) . . ? C5A N6A Cu1 135.08(16) . . ? N5A N6A Cu1 118.58(14) . . ? C6B N1B C4B 111.16(17) . . ? C6B N1B C5B 110.50(17) . . ? C4B N1B C5B 111.41(17) . . ? C6B N1B Cu1 109.57(13) . . ? C4B N1B Cu1 107.45(13) . . ? C5B N1B Cu1 106.57(13) . . ? C2B N2B Cu1 105.68(13) . . ? C3B N3B Cu1 105.82(13) . . ? C1B N4B Cu1 111.06(14) . . ? N2A C1A C2A 122.0(2) . . ? C1A C2A C3A 117.3(2) . . ? N1A C3A C2A 122.5(2) . . ? N2A C4A N1A 126.4(2) . . ? N2A C4A C5A 116.91(19) . . ? N1A C4A C5A 116.7(2) . . ? N3A C5A N6A 110.9(2) . . ? N3A C5A C4A 124.5(2) . . ? N6A C5A C4A 124.6(2) . . ? N4B C1B C5B 108.28(18) . . ? N2B C2B C6B 108.05(18) . . ? N3B C3B C4B 108.55(17) . . ? N1B C4B C3B 110.00(17) . . ? N1B C5B C1B 110.21(18) . . ? N1B C6B C2B 109.92(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.549 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.077 data_compound5 _database_code_depnum_ccdc_archive 'CCDC 734269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H39 Cl3 Co2 N14 O17.50' _chemical_formula_weight 943.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.107(5) _cell_length_b 10.106(5) _cell_length_c 19.944(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 115.106(5) _cell_angle_gamma 90.000(5) _cell_volume 3487(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4998 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 23.26 _exptl_crystal_description prismatic _exptl_crystal_colour purple _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16048 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4998 _reflns_number_gt 4360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+30.0718P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4998 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2265 _refine_ls_wR_factor_gt 0.2091 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.03851(5) 0.22326(9) 0.20724(5) 0.0150(3) Uani 1 1 d . . . Co2 Co 0.85229(5) 0.01357(10) 0.14401(5) 0.0223(3) Uani 1 1 d . . . Cl1 Cl 0.77595(11) 0.43105(18) 0.94984(10) 0.0283(5) Uani 1 1 d . . . Cl2 Cl 0.61213(11) 0.77964(18) 0.78479(13) 0.0357(5) Uani 1 1 d . . . Cl3 Cl 0.36491(17) 0.9407(4) 0.75702(16) 0.0693(9) Uani 1 1 d . . . C1 C 0.9632(6) 0.1702(11) 0.5615(5) 0.052(3) Uani 1 1 d . . . H1 H 0.9661 0.1774 0.6092 0.063 Uiso 1 1 calc R . . C2 C 1.0078(7) 0.2458(10) 0.5394(5) 0.054(3) Uani 1 1 d . . . H2 H 1.0420 0.3053 0.5730 0.064 Uiso 1 1 calc R . . C3 C 0.9135(5) 0.0827(10) 0.5118(5) 0.040(2) Uani 1 1 d . . . H3 H 0.8822 0.0301 0.5260 0.047 Uiso 1 1 calc R . . C4 C 0.9559(4) 0.1517(8) 0.4269(4) 0.0263(18) Uani 1 1 d . . . C5 C 0.9521(4) 0.1406(7) 0.3518(4) 0.0213(16) Uani 1 1 d . . . C6 C 1.1767(4) 0.3660(8) 0.2877(4) 0.0249(17) Uani 1 1 d . . . H6A H 1.2109 0.2916 0.3097 0.030 Uiso 1 1 calc R . . H6B H 1.2007 0.4452 0.3155 0.030 Uiso 1 1 calc R . . C7 C 1.1617(4) 0.3822(7) 0.2067(4) 0.0235(16) Uani 1 1 d . . . H7A H 1.1431 0.4710 0.1902 0.028 Uiso 1 1 calc R . . H7B H 1.2096 0.3698 0.2017 0.028 Uiso 1 1 calc R . . C8 C 1.1396(4) 0.1625(8) 0.1459(4) 0.0273(18) Uani 1 1 d . . . H23A H 1.1806 0.1875 0.1319 0.033 Uiso 1 1 calc R . . H23B H 1.1019 0.1105 0.1061 0.033 Uiso 1 1 calc R . . C9 C 1.1723(4) 0.0826(8) 0.2162(5) 0.0300(18) Uani 1 1 d . . . H9A H 1.1826 -0.0071 0.2056 0.036 Uiso 1 1 calc R . . H9B H 1.2205 0.1214 0.2510 0.036 Uiso 1 1 calc R . . C10 C 0.9947(4) 0.4356(8) 0.1032(4) 0.0300(19) Uani 1 1 d . . . H10A H 1.0214 0.5151 0.1284 0.036 Uiso 1 1 calc R . . H10B H 0.9520 0.4611 0.0571 0.036 Uiso 1 1 calc R . . C11 C 1.0494(4) 0.3458(8) 0.0879(4) 0.0283(18) Uani 1 1 d . . . H11A H 1.0205 0.2786 0.0522 0.034 Uiso 1 1 calc R . . H11B H 1.0789 0.3966 0.0676 0.034 Uiso 1 1 calc R . . C12 C 0.7115(5) 0.1362(10) 0.0456(5) 0.042(2) Uani 1 1 d . . . H12A H 0.6932 0.2202 0.0208 0.051 Uiso 1 1 calc R . . H12B H 0.6689 0.0925 0.0509 0.051 Uiso 1 1 calc R . . C13 C 0.7414(5) 0.0507(9) 0.0015(4) 0.0334(19) Uani 1 1 d . . . H13A H 0.6989 0.0193 -0.0432 0.040 Uiso 1 1 calc R . . H13B H 0.7763 0.1012 -0.0126 0.040 Uiso 1 1 calc R . . C14 C 0.7287(6) -0.1524(11) 0.1329(5) 0.054(3) Uani 1 1 d . . . H14A H 0.6853 -0.0995 0.1302 0.065 Uiso 1 1 calc R . . H14B H 0.7222 -0.2409 0.1483 0.065 Uiso 1 1 calc R . . C15 C 0.7271(5) -0.1598(10) 0.0591(5) 0.044(2) Uani 1 1 d . . . H15A H 0.6752 -0.1410 0.0224 0.053 Uiso 1 1 calc R . . H15B H 0.7401 -0.2492 0.0505 0.053 Uiso 1 1 calc R . . C16 C 0.8907(5) -0.2150(8) 0.0828(5) 0.036(2) Uani 1 1 d . . . H16A H 0.8657 -0.2913 0.0927 0.043 Uiso 1 1 calc R . . H16B H 0.9315 -0.2462 0.0699 0.043 Uiso 1 1 calc R . . C17 C 0.8327(5) -0.1352(8) 0.0199(5) 0.0308(18) Uani 1 1 d . . . H17A H 0.8590 -0.0726 0.0017 0.037 Uiso 1 1 calc R . . H17B H 0.8013 -0.1931 -0.0205 0.037 Uiso 1 1 calc R . . N1 N 1.0051(5) 0.2392(7) 0.4717(4) 0.0418(18) Uani 1 1 d . . . N2 N 0.9087(4) 0.0705(7) 0.4426(4) 0.0330(16) Uani 1 1 d . . . N3 N 1.0039(3) 0.1966(6) 0.3316(3) 0.0203(13) Uani 1 1 d . . . N4 N 0.9804(3) 0.1645(6) 0.2611(3) 0.0182(13) Uani 1 1 d . . . N5 N 0.9167(3) 0.0900(6) 0.2398(3) 0.0226(14) Uani 1 1 d . . . N6 N 0.8983(4) 0.0736(7) 0.2964(3) 0.0283(15) Uani 1 1 d . . . N7 N 0.7831(4) -0.0635(7) 0.0491(4) 0.0285(15) Uani 1 1 d . . . N8 N 0.7973(4) -0.0978(9) 0.1870(4) 0.047(2) Uani 1 1 d . . . H8A H 0.8288 -0.1638 0.2130 0.056 Uiso 1 1 calc R . . H8B H 0.7857 -0.0488 0.2187 0.056 Uiso 1 1 calc R . . N9 N 0.7767(4) 0.1577(8) 0.1197(4) 0.0378(18) Uani 1 1 d . . . H9C H 0.7583 0.1620 0.1544 0.045 Uiso 1 1 calc R . . H9D H 0.8000 0.2351 0.1198 0.045 Uiso 1 1 calc R . . N10 N 0.9240(4) -0.1279(6) 0.1499(4) 0.0307(15) Uani 1 1 d . . . H10C H 0.9687 -0.0927 0.1535 0.037 Uiso 1 1 calc R . . H10D H 0.9342 -0.1767 0.1907 0.037 Uiso 1 1 calc R . . N11 N 1.1026(3) 0.2824(6) 0.1589(3) 0.0200(13) Uani 1 1 d . . . N12 N 1.1012(3) 0.3432(6) 0.2889(3) 0.0242(14) Uani 1 1 d . . . H12C H 1.0763 0.4208 0.2839 0.029 Uiso 1 1 calc R . . H12D H 1.1080 0.3072 0.3325 0.029 Uiso 1 1 calc R . . N13 N 0.9657(3) 0.3609(6) 0.1506(3) 0.0216(13) Uani 1 1 d . . . H13C H 0.9199 0.3237 0.1219 0.026 Uiso 1 1 calc R . . H13D H 0.9583 0.4172 0.1820 0.026 Uiso 1 1 calc R . . N14 N 1.1149(3) 0.0813(6) 0.2487(4) 0.0261(15) Uani 1 1 d . . . H14C H 1.1397 0.0913 0.2981 0.031 Uiso 1 1 calc R . . H14D H 1.0905 0.0026 0.2396 0.031 Uiso 1 1 calc R . . O1P O 0.9005(3) 0.1205(5) 0.0980(3) 0.0187(10) Uani 1 1 d . . . O2P O 0.9846(3) 0.1038(5) 0.1298(3) 0.0191(11) Uani 1 1 d . . . O1 O 0.8061(4) 0.3903(10) 1.0228(4) 0.079(3) Uani 1 1 d . . . O2 O 0.8198(5) 0.3817(9) 0.9125(5) 0.074(2) Uiso 1 1 d . . . O3 O 0.7778(5) 0.5690(7) 0.9446(6) 0.097(4) Uani 1 1 d . . . O4 O 0.6977(3) 0.3844(7) 0.9128(3) 0.0429(15) Uani 1 1 d . . . O5 O 0.6628(6) 0.8300(10) 0.8554(5) 0.088(3) Uiso 1 1 d . . . O6 O 0.6595(6) 0.7448(9) 0.7489(8) 0.119(5) Uani 1 1 d . . . O7 O 0.5569(4) 0.8775(6) 0.7439(4) 0.0526(18) Uani 1 1 d . . . O8 O 0.5724(3) 0.6660(5) 0.7928(3) 0.0293(12) Uani 1 1 d . . . O1W O 0.1974(7) 0.1283(12) 0.6499(6) 0.123(5) Uani 1 1 d . . . O2W O 0.5620(4) 0.0276(7) 0.9222(5) 0.067(2) Uani 1 1 d . . . O3W O 0.9051(9) 0.1431(10) 0.9534(5) 0.132(5) Uani 1 1 d . . . O4W O 0.9796(11) 0.002(2) 0.0090(12) 0.090(6) Uiso 0.50 1 d P . . O9 O 0.4130(10) 0.8032(17) 0.7753(10) 0.0737(17) Uiso 0.50 1 d P . . O10 O 0.4151(12) 0.9389(19) 0.7947(11) 0.0737(17) Uiso 0.50 1 d P . . O11 O 0.3059(11) 0.9077(19) 0.7784(10) 0.0737(17) Uiso 0.50 1 d P . . O12 O 0.3966(10) 0.9812(17) 0.8334(10) 0.0737(17) Uiso 0.50 1 d P . . O13 O 0.4146(10) 1.0416(19) 0.7828(10) 0.0737(17) Uiso 0.50 1 d P . . O14 O 0.3586(10) 1.1032(17) 0.7322(10) 0.0737(17) Uiso 0.50 1 d P . . O15 O 0.3539(10) 0.9450(17) 0.6901(10) 0.0737(17) Uiso 0.50 1 d P . . O16 O 0.2831(11) 0.9191(19) 0.7443(10) 0.0737(17) Uiso 0.50 1 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 Co1 0.0126(5) 0.0151(5) 0.0153(5) 0.0012(4) 0.0039(4) -0.0017(4) Co2 0.0160(5) 0.0305(6) 0.0187(6) -0.0019(4) 0.0058(4) -0.0090(4) Cl1 0.0246(10) 0.0219(10) 0.0275(10) -0.0010(8) 0.0008(8) -0.0002(8) Cl2 0.0225(10) 0.0204(10) 0.0586(14) -0.0048(9) 0.0119(10) -0.0022(8) Cl3 0.0477(16) 0.114(3) 0.0501(16) -0.0267(16) 0.0248(14) -0.0332(17) C1 0.076(7) 0.058(6) 0.035(5) 0.008(5) 0.035(6) 0.034(6) C2 0.088(8) 0.048(6) 0.035(5) -0.006(5) 0.035(6) 0.007(6) C3 0.040(5) 0.055(6) 0.034(5) 0.021(5) 0.026(4) 0.029(5) C4 0.030(4) 0.029(4) 0.024(4) 0.008(3) 0.015(4) 0.014(4) C5 0.021(4) 0.023(4) 0.023(4) 0.000(3) 0.012(3) 0.005(3) C6 0.026(4) 0.022(4) 0.022(4) 0.003(3) 0.005(3) -0.007(3) C7 0.021(4) 0.024(4) 0.021(4) -0.001(3) 0.005(3) -0.009(3) C8 0.013(4) 0.040(5) 0.031(4) -0.007(4) 0.011(3) -0.004(3) C9 0.013(4) 0.031(4) 0.044(5) -0.003(4) 0.009(3) 0.002(3) C10 0.022(4) 0.023(4) 0.031(4) 0.013(3) -0.003(3) -0.003(3) C11 0.024(4) 0.038(5) 0.017(4) 0.005(3) 0.003(3) -0.016(4) C12 0.020(4) 0.061(6) 0.036(5) -0.006(4) 0.002(4) 0.001(4) C13 0.022(4) 0.047(5) 0.025(4) -0.002(4) 0.004(3) -0.004(4) C14 0.052(6) 0.070(7) 0.041(6) -0.014(5) 0.022(5) -0.040(6) C15 0.034(5) 0.057(6) 0.041(5) -0.011(4) 0.015(4) -0.031(5) C16 0.040(5) 0.023(4) 0.040(5) -0.004(4) 0.012(4) -0.008(4) C17 0.030(4) 0.031(4) 0.031(4) -0.009(4) 0.013(4) -0.008(4) N1 0.058(5) 0.039(4) 0.032(4) -0.012(3) 0.023(4) -0.002(4) N2 0.023(4) 0.051(4) 0.024(4) 0.011(3) 0.009(3) 0.014(3) N3 0.021(3) 0.022(3) 0.017(3) -0.001(3) 0.007(3) 0.000(3) N4 0.016(3) 0.018(3) 0.019(3) 0.001(2) 0.006(2) 0.001(2) N5 0.018(3) 0.032(4) 0.020(3) 0.001(3) 0.010(3) -0.007(3) N6 0.021(3) 0.043(4) 0.022(3) 0.004(3) 0.010(3) -0.001(3) N7 0.020(3) 0.036(4) 0.025(3) -0.004(3) 0.006(3) -0.012(3) N8 0.038(4) 0.070(6) 0.033(4) -0.006(4) 0.017(3) -0.034(4) N9 0.022(4) 0.055(5) 0.037(4) -0.010(4) 0.013(3) 0.004(3) N10 0.032(4) 0.025(3) 0.027(4) 0.003(3) 0.005(3) -0.007(3) N11 0.016(3) 0.023(3) 0.017(3) 0.000(3) 0.003(2) -0.005(3) N12 0.023(3) 0.028(3) 0.019(3) -0.003(3) 0.007(3) -0.010(3) N13 0.020(3) 0.017(3) 0.023(3) -0.002(3) 0.004(3) 0.002(2) N14 0.014(3) 0.021(3) 0.038(4) 0.010(3) 0.006(3) -0.001(3) O1P 0.011(2) 0.024(3) 0.020(3) -0.001(2) 0.005(2) -0.001(2) O2P 0.009(2) 0.020(3) 0.025(3) -0.004(2) 0.005(2) 0.0004(19) O1 0.031(4) 0.157(9) 0.035(4) 0.031(5) 0.001(3) -0.018(5) O3 0.069(6) 0.023(4) 0.157(9) -0.004(5) 0.007(6) -0.009(4) O4 0.030(3) 0.056(4) 0.028(3) -0.001(3) -0.002(3) -0.014(3) O6 0.107(8) 0.063(5) 0.257(15) -0.011(7) 0.144(10) -0.014(5) O7 0.035(4) 0.031(3) 0.074(5) 0.019(3) 0.005(3) 0.000(3) O8 0.035(3) 0.020(3) 0.034(3) -0.004(2) 0.016(3) -0.002(2) O1W 0.128(9) 0.140(10) 0.078(7) 0.013(6) 0.021(6) -0.091(8) O2W 0.048(4) 0.051(4) 0.087(6) 0.019(4) 0.013(4) 0.004(4) O3W 0.215(14) 0.074(7) 0.057(6) -0.003(5) 0.009(7) -0.053(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 Co1 O2P 1.885(5) . ? Co1 N4 1.937(6) . ? Co1 N11 1.946(6) . ? Co1 N13 1.953(6) . ? Co1 N14 1.962(6) . ? Co1 N12 1.975(6) . ? Co2 O1P 1.890(5) . ? Co2 N5 1.941(6) . ? Co2 N10 1.949(7) . ? Co2 N7 1.953(6) . ? Co2 N9 1.962(7) . ? Co2 N8 1.967(7) . ? Cl1 O1 1.381(7) . ? Cl1 O3 1.399(8) . ? Cl1 O2 1.425(9) . ? Cl1 O4 1.437(6) . ? Cl2 O6 1.416(9) . ? Cl2 O5 1.422(10) . ? Cl2 O8 1.422(6) . ? Cl2 O7 1.424(6) . ? Cl3 O10 0.93(2) . ? Cl3 O15 1.260(17) . ? Cl3 O13 1.338(19) . ? Cl3 O11 1.405(19) . ? Cl3 O12 1.438(18) . ? Cl3 O16 1.489(19) . ? Cl3 O9 1.620(18) . ? Cl3 O14 1.704(18) . ? C1 C2 1.351(15) . ? C1 C3 1.367(15) . ? C2 N1 1.332(11) . ? C3 N2 1.348(11) . ? C4 N1 1.323(11) . ? C4 N2 1.351(11) . ? C4 C5 1.472(10) . ? C5 N6 1.331(10) . ? C5 N3 1.342(9) . ? C6 N12 1.471(9) . ? C6 C7 1.526(10) . ? C7 N11 1.513(9) . ? C8 N11 1.480(10) . ? C8 C9 1.505(12) . ? C9 N14 1.493(10) . ? C10 N13 1.489(10) . ? C10 C11 1.509(12) . ? C11 N11 1.492(9) . ? C12 N9 1.490(11) . ? C12 C13 1.509(12) . ? C13 N7 1.492(11) . ? C14 N8 1.410(11) . ? C14 C15 1.461(13) . ? C15 N7 1.520(10) . ? C16 N10 1.499(10) . ? C16 C17 1.507(12) . ? C17 N7 1.494(10) . ? N3 N4 1.322(8) . ? N4 N5 1.338(8) . ? N5 N6 1.327(9) . ? O1P O2P 1.466(6) . ? O4W O4W 0.99(3) 3_755 ? O9 O10 1.42(3) . ? O10 O13 1.06(2) . ? O10 O12 1.06(2) . ? O11 O16 0.64(2) . ? O11 O12 1.77(3) . ? O12 O13 1.34(2) . ? O13 O14 1.28(2) . ? O14 O15 1.79(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 O2P Co1 N4 90.9(2) . . ? O2P Co1 N11 91.8(2) . . ? N4 Co1 N11 176.5(2) . . ? O2P Co1 N13 88.5(2) . . ? N4 Co1 N13 95.9(2) . . ? N11 Co1 N13 86.5(2) . . ? O2P Co1 N14 85.8(2) . . ? N4 Co1 N14 92.3(2) . . ? N11 Co1 N14 85.5(2) . . ? N13 Co1 N14 170.1(3) . . ? O2P Co1 N12 176.4(2) . . ? N4 Co1 N12 91.2(2) . . ? N11 Co1 N12 86.0(2) . . ? N13 Co1 N12 94.2(3) . . ? N14 Co1 N12 91.1(3) . . ? O1P Co2 N5 90.8(2) . . ? O1P Co2 N10 88.5(2) . . ? N5 Co2 N10 95.6(3) . . ? O1P Co2 N7 91.5(2) . . ? N5 Co2 N7 177.0(3) . . ? N10 Co2 N7 86.3(3) . . ? O1P Co2 N9 85.1(3) . . ? N5 Co2 N9 92.3(3) . . ? N10 Co2 N9 169.9(3) . . ? N7 Co2 N9 86.1(3) . . ? O1P Co2 N8 177.1(3) . . ? N5 Co2 N8 91.8(3) . . ? N10 Co2 N8 92.6(3) . . ? N7 Co2 N8 85.8(3) . . ? N9 Co2 N8 93.4(4) . . ? O1 Cl1 O3 111.3(7) . . ? O1 Cl1 O2 111.7(5) . . ? O3 Cl1 O2 105.7(6) . . ? O1 Cl1 O4 108.8(4) . . ? O3 Cl1 O4 110.0(5) . . ? O2 Cl1 O4 109.3(5) . . ? O6 Cl2 O5 106.1(7) . . ? O6 Cl2 O8 110.0(4) . . ? O5 Cl2 O8 110.5(5) . . ? O6 Cl2 O7 111.2(6) . . ? O5 Cl2 O7 110.2(5) . . ? O8 Cl2 O7 108.9(4) . . ? O10 Cl3 O15 120.4(15) . . ? O10 Cl3 O13 52.2(13) . . ? O15 Cl3 O13 98.8(11) . . ? O10 Cl3 O11 115.7(14) . . ? O15 Cl3 O11 122.3(11) . . ? O13 Cl3 O11 126.5(11) . . ? O10 Cl3 O12 47.7(12) . . ? O15 Cl3 O12 156.5(11) . . ? O13 Cl3 O12 57.7(10) . . ? O11 Cl3 O12 77.1(10) . . ? O10 Cl3 O16 141.2(14) . . ? O15 Cl3 O16 97.6(11) . . ? O13 Cl3 O16 134.4(11) . . ? O11 Cl3 O16 25.5(9) . . ? O12 Cl3 O16 99.3(10) . . ? O10 Cl3 O9 60.7(14) . . ? O15 Cl3 O9 95.3(10) . . ? O13 Cl3 O9 108.9(10) . . ? O11 Cl3 O9 100.3(10) . . ? O12 Cl3 O9 93.5(10) . . ? O16 Cl3 O9 111.5(10) . . ? O10 Cl3 O14 100.1(14) . . ? O15 Cl3 O14 72.6(10) . . ? O13 Cl3 O14 47.9(9) . . ? O11 Cl3 O14 110.5(10) . . ? O12 Cl3 O14 88.8(9) . . ? O16 Cl3 O14 98.7(10) . . ? O9 Cl3 O14 148.8(9) . . ? C2 C1 C3 117.9(9) . . ? N1 C2 C1 123.0(10) . . ? N2 C3 C1 121.8(9) . . ? N1 C4 N2 127.1(7) . . ? N1 C4 C5 116.8(7) . . ? N2 C4 C5 116.1(7) . . ? N6 C5 N3 111.9(6) . . ? N6 C5 C4 124.8(7) . . ? N3 C5 C4 123.3(7) . . ? N12 C6 C7 106.7(6) . . ? N11 C7 C6 110.5(6) . . ? N11 C8 C9 108.5(6) . . ? N14 C9 C8 108.6(6) . . ? N13 C10 C11 107.5(6) . . ? N11 C11 C10 108.5(6) . . ? N9 C12 C13 107.3(7) . . ? N7 C13 C12 107.7(7) . . ? N8 C14 C15 114.0(7) . . ? C14 C15 N7 112.6(7) . . ? N10 C16 C17 108.2(6) . . ? N7 C17 C16 107.5(7) . . ? C4 N1 C2 115.4(8) . . ? C3 N2 C4 114.7(8) . . ? N4 N3 C5 104.9(6) . . ? N3 N4 N5 109.1(5) . . ? N3 N4 Co1 120.0(4) . . ? N5 N4 Co1 131.0(4) . . ? N6 N5 N4 109.5(6) . . ? N6 N5 Co2 120.1(5) . . ? N4 N5 Co2 130.3(4) . . ? N5 N6 C5 104.6(6) . . ? C13 N7 C17 112.5(6) . . ? C13 N7 C15 111.3(6) . . ? C17 N7 C15 109.8(7) . . ? C13 N7 Co2 105.5(5) . . ? C17 N7 Co2 106.9(5) . . ? C15 N7 Co2 110.7(5) . . ? C14 N8 Co2 112.6(6) . . ? C12 N9 Co2 110.8(6) . . ? C16 N10 Co2 110.9(5) . . ? C8 N11 C11 111.7(6) . . ? C8 N11 C7 111.7(5) . . ? C11 N11 C7 109.7(5) . . ? C8 N11 Co1 106.5(4) . . ? C11 N11 Co1 106.5(4) . . ? C7 N11 Co1 110.6(4) . . ? C6 N12 Co1 109.9(5) . . ? C10 N13 Co1 111.2(4) . . ? C9 N14 Co1 111.2(5) . . ? O2P O1P Co2 113.3(3) . . ? O1P O2P Co1 113.5(3) . . ? O10 O9 Cl3 35.0(9) . . ? Cl3 O10 O13 83.8(19) . . ? Cl3 O10 O12 92(2) . . ? O13 O10 O12 78.3(19) . . ? Cl3 O10 O9 84.2(17) . . ? O13 O10 O9 152(2) . . ? O12 O10 O9 127(2) . . ? O16 O11 Cl3 85(3) . . ? O16 O11 O12 128(3) . . ? Cl3 O11 O12 52.3(9) . . ? O10 O12 O13 50.8(14) . . ? O10 O12 Cl3 40.5(13) . . ? O13 O12 Cl3 57.4(11) . . ? O10 O12 O11 85.6(18) . . ? O13 O12 O11 102.8(15) . . ? Cl3 O12 O11 50.6(8) . . ? O10 O13 O14 125(2) . . ? O10 O13 Cl3 44.0(13) . . ? O14 O13 Cl3 81.2(13) . . ? O10 O13 O12 50.9(14) . . ? O14 O13 O12 114.7(17) . . ? Cl3 O13 O12 64.9(12) . . ? O13 O14 Cl3 50.9(10) . . ? O13 O14 O15 78.1(13) . . ? Cl3 O14 O15 42.2(7) . . ? Cl3 O15 O14 65.2(9) . . ? O11 O16 Cl3 70(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.458 _refine_diff_density_min -1.160 _refine_diff_density_rms 0.183 data_compound6 _database_code_depnum_ccdc_archive 'CCDC 734270' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H26 Fe2 N24 O8' _chemical_formula_weight 842.35 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3468(5) _cell_length_b 11.8734(6) _cell_length_c 15.1610(8) _cell_angle_alpha 70.3580(10) _cell_angle_beta 77.8460(10) _cell_angle_gamma 71.2250(10) _cell_volume 1649.86(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 279 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 27.08 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 0.965 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16296 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5790 _reflns_number_gt 5287 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+2.1259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5790 _refine_ls_number_parameters 543 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.47761(3) 0.24195(3) 0.23320(2) 0.01285(10) Uani 1 1 d . . . Fe2 Fe 0.14369(3) 0.42741(3) 0.24141(2) 0.01316(10) Uani 1 1 d . . . N1A N 0.6221(2) 0.33959(18) 0.15859(14) 0.0156(4) Uani 1 1 d . . . N2A N 0.6135(2) 0.46051(19) 0.11578(15) 0.0183(5) Uani 1 1 d . . . N3A N 0.7386(2) 0.47277(19) 0.09483(15) 0.0194(5) Uani 1 1 d . . . N4A N 0.8319(2) 0.3610(2) 0.12271(15) 0.0189(5) Uani 1 1 d . . . C5A C 0.7558(2) 0.2814(2) 0.16158(16) 0.0152(5) Uani 1 1 d . . . C6A C 0.7962(2) 0.1462(2) 0.20665(17) 0.0157(5) Uani 1 1 d . . . N7A N 0.6881(2) 0.10060(19) 0.25020(14) 0.0154(4) Uani 1 1 d . . . C8A C 0.7158(3) -0.0214(2) 0.29453(17) 0.0171(5) Uani 1 1 d . . . H8A H 0.6439 -0.0565 0.3249 0.021 Uiso 1 1 calc R . . C9A C 0.8498(3) -0.0962(2) 0.29587(17) 0.0197(5) Uani 1 1 d . . . H9A H 0.8694 -0.1807 0.3277 0.024 Uiso 1 1 calc R . . C10A C 0.9523(3) -0.0411(2) 0.24845(18) 0.0207(6) Uani 1 1 d . . . H10A H 1.0428 -0.0902 0.2482 0.025 Uiso 1 1 calc R . . N11A N 0.9277(2) 0.0814(2) 0.20221(15) 0.0191(5) Uani 1 1 d . . . N1B N 0.3967(2) 0.11554(18) 0.34452(14) 0.0150(4) Uani 1 1 d . . . N2B N 0.3230(2) 0.03688(19) 0.35257(15) 0.0179(5) Uani 1 1 d . . . N3B N 0.2733(2) 0.00119(19) 0.44184(15) 0.0212(5) Uani 1 1 d . . . N4B N 0.3122(2) 0.05492(19) 0.49331(15) 0.0199(5) Uani 1 1 d . . . C5B C 0.3877(2) 0.1246(2) 0.43094(17) 0.0158(5) Uani 1 1 d . . . C6B C 0.4559(2) 0.2071(2) 0.44468(17) 0.0155(5) Uani 1 1 d . . . N7B N 0.5125(2) 0.27319(18) 0.36327(14) 0.0151(4) Uani 1 1 d . . . C8B C 0.5799(2) 0.3482(2) 0.37097(19) 0.0185(5) Uani 1 1 d . . . H8B H 0.6209 0.3951 0.3166 0.022 Uiso 1 1 calc R . . C9B C 0.5901(3) 0.3579(2) 0.45721(19) 0.0214(6) Uani 1 1 d . . . H9B H 0.6378 0.4092 0.4624 0.026 Uiso 1 1 calc R . . C10B C 0.5260(3) 0.2875(2) 0.53541(19) 0.0242(6) Uani 1 1 d . . . H10B H 0.5299 0.2934 0.5944 0.029 Uiso 1 1 calc R . . N11B N 0.4582(2) 0.21089(19) 0.53049(15) 0.0205(5) Uani 1 1 d . . . N1C N -0.0687(2) 0.53871(19) 0.24502(14) 0.0152(4) Uani 1 1 d . . . N2C N -0.1939(2) 0.52255(19) 0.28264(15) 0.0188(5) Uani 1 1 d . . . N3C N -0.2864(2) 0.6273(2) 0.25060(15) 0.0216(5) Uani 1 1 d . . . N4C N -0.2251(2) 0.7146(2) 0.19134(16) 0.0210(5) Uani 1 1 d . . . C5C C -0.0915(2) 0.6560(2) 0.18975(17) 0.0166(5) Uani 1 1 d . . . C6C C 0.0274(2) 0.6997(2) 0.13618(17) 0.0165(5) Uani 1 1 d . . . N7C N 0.1482(2) 0.61094(18) 0.15047(14) 0.0154(4) Uani 1 1 d . . . C8C C 0.2636(2) 0.6422(2) 0.10514(17) 0.0173(5) Uani 1 1 d . . . H8C H 0.3484 0.5838 0.1139 0.021 Uiso 1 1 calc R . . C9C C 0.2570(3) 0.7605(2) 0.04557(18) 0.0199(5) Uani 1 1 d . . . H9C H 0.3363 0.7835 0.0143 0.024 Uiso 1 1 calc R . . C10C C 0.1291(3) 0.8434(2) 0.03403(18) 0.0219(6) Uani 1 1 d . . . H10C H 0.1232 0.9228 -0.0071 0.026 Uiso 1 1 calc R . . N11C N 0.0123(2) 0.81462(19) 0.07960(15) 0.0205(5) Uani 1 1 d . . . N1D N 0.1727(2) 0.45956(19) 0.36260(15) 0.0163(4) Uani 1 1 d . . . N2D N 0.2421(2) 0.5229(2) 0.38477(16) 0.0205(5) Uani 1 1 d . . . N3D N 0.2335(2) 0.4924(2) 0.47753(16) 0.0225(5) Uani 1 1 d . . . N4D N 0.1594(2) 0.4088(2) 0.51784(16) 0.0209(5) Uani 1 1 d . . . C5D C 0.1245(2) 0.3912(2) 0.44521(17) 0.0163(5) Uani 1 1 d . . . C6D C 0.0515(2) 0.3048(2) 0.44354(17) 0.0151(5) Uani 1 1 d . . . N7D N 0.06102(19) 0.29245(18) 0.35724(14) 0.0145(4) Uani 1 1 d . . . C8D C -0.0022(2) 0.2145(2) 0.34930(18) 0.0172(5) Uani 1 1 d . . . H8D H 0.0031 0.2028 0.2909 0.021 Uiso 1 1 calc R . . C9D C -0.0747(3) 0.1517(2) 0.42643(18) 0.0196(5) Uani 1 1 d . . . H9D H -0.1201 0.0984 0.4213 0.024 Uiso 1 1 calc R . . C10D C -0.0776(2) 0.1708(2) 0.51188(18) 0.0201(6) Uani 1 1 d . . . H10D H -0.1263 0.1291 0.5647 0.024 Uiso 1 1 calc R . . N11D N -0.0138(2) 0.2465(2) 0.52232(15) 0.0192(5) Uani 1 1 d . . . O1 O 0.32194(16) 0.36097(15) 0.20915(12) 0.0153(4) Uani 1 1 d . . . O1W O 0.4790(2) 0.1647(2) 0.13421(14) 0.0200(4) Uani 1 1 d . . . O2W O 0.0869(2) 0.37020(18) 0.14676(13) 0.0193(4) Uani 1 1 d . . . O3W O 0.27900(19) 0.2811(2) 0.02258(14) 0.0213(4) Uani 1 1 d . . . O4W O 0.4134(2) 0.67680(19) 0.25436(16) 0.0275(5) Uani 1 1 d . . . O5W O 0.2820(2) -0.0805(2) 0.22955(17) 0.0351(5) Uani 1 1 d . . . O6W O 0.2003(2) 0.0701(2) 0.06960(16) 0.0342(5) Uani 1 1 d D . . O7W O 0.6561(3) 0.9692(2) 0.09772(16) 0.0406(6) Uani 1 1 d D . . H62W H 0.236(5) 0.013(4) 0.127(2) 0.115(19) Uiso 1 1 d D . . H11W H 0.522(4) 0.104(4) 0.127(2) 0.040(11) Uiso 1 1 d . . . H12W H 0.424(3) 0.201(3) 0.098(2) 0.017(8) Uiso 1 1 d . . . H21W H 0.144(4) 0.343(4) 0.113(3) 0.049(12) Uiso 1 1 d . . . H22W H 0.013(4) 0.371(4) 0.137(3) 0.058(12) Uiso 1 1 d . . . H31W H 0.261(4) 0.220(4) 0.017(3) 0.068(14) Uiso 1 1 d . . . H32W H 0.274(4) 0.340(4) -0.023(3) 0.055(12) Uiso 1 1 d . . . H41W H 0.375(4) 0.628(4) 0.290(3) 0.048(12) Uiso 1 1 d . . . H42W H 0.499(5) 0.646(4) 0.257(3) 0.064(13) Uiso 1 1 d . . . H51W H 0.303(4) -0.045(4) 0.265(3) 0.057(12) Uiso 1 1 d . . . H52W H 0.333(4) -0.164(4) 0.240(3) 0.068(13) Uiso 1 1 d . . . H72W H 0.689(5) 0.887(2) 0.130(3) 0.12(2) Uiso 1 1 d D . . H61W H 0.251(4) 0.067(4) 0.0088(19) 0.086(15) Uiso 1 1 d D . . H71W H 0.570(3) 0.955(5) 0.102(3) 0.093(17) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00857(18) 0.01292(18) 0.01592(19) -0.00236(14) -0.00002(13) -0.00421(13) Fe2 0.00879(18) 0.01239(18) 0.01729(19) -0.00267(14) -0.00045(13) -0.00395(13) N1A 0.0125(10) 0.0152(10) 0.0177(11) -0.0023(8) -0.0006(8) -0.0054(8) N2A 0.0169(11) 0.0168(11) 0.0201(11) -0.0003(9) -0.0023(9) -0.0082(9) N3A 0.0154(11) 0.0201(11) 0.0218(11) -0.0013(9) -0.0029(9) -0.0084(9) N4A 0.0163(11) 0.0211(11) 0.0186(11) -0.0019(9) -0.0023(9) -0.0078(9) C5A 0.0125(12) 0.0201(13) 0.0139(12) -0.0032(10) -0.0007(9) -0.0078(10) C6A 0.0127(12) 0.0210(13) 0.0147(12) -0.0056(10) -0.0028(9) -0.0050(10) N7A 0.0131(10) 0.0167(11) 0.0161(11) -0.0039(9) -0.0003(8) -0.0053(8) C8A 0.0181(13) 0.0168(13) 0.0164(13) -0.0038(10) -0.0007(10) -0.0065(10) C9A 0.0216(14) 0.0178(13) 0.0173(13) -0.0044(10) -0.0036(10) -0.0020(11) C10A 0.0138(13) 0.0230(14) 0.0224(14) -0.0085(11) -0.0053(10) 0.0027(11) N11A 0.0112(10) 0.0242(12) 0.0207(11) -0.0060(9) -0.0009(8) -0.0043(9) N1B 0.0105(10) 0.0139(10) 0.0200(11) -0.0024(9) -0.0005(8) -0.0058(8) N2B 0.0136(10) 0.0137(10) 0.0260(12) -0.0037(9) -0.0009(9) -0.0060(8) N3B 0.0151(11) 0.0175(11) 0.0266(12) -0.0026(9) 0.0036(9) -0.0064(9) N4B 0.0159(11) 0.0180(11) 0.0224(12) -0.0031(9) 0.0023(9) -0.0057(9) C5B 0.0102(12) 0.0126(12) 0.0191(13) -0.0014(10) -0.0002(10) -0.0003(10) C6B 0.0102(12) 0.0134(12) 0.0184(13) -0.0021(10) -0.0011(10) 0.0000(10) N7B 0.0104(10) 0.0140(10) 0.0182(11) -0.0034(8) -0.0011(8) -0.0014(8) C8B 0.0132(12) 0.0136(12) 0.0275(14) -0.0048(11) -0.0024(10) -0.0033(10) C9B 0.0162(13) 0.0168(13) 0.0327(15) -0.0099(11) -0.0052(11) -0.0019(10) C10B 0.0238(14) 0.0248(14) 0.0252(15) -0.0116(12) -0.0068(11) -0.0012(12) N11B 0.0191(11) 0.0177(11) 0.0212(12) -0.0042(9) -0.0024(9) -0.0021(9) N1C 0.0094(10) 0.0155(10) 0.0195(11) -0.0037(9) -0.0005(8) -0.0039(8) N2C 0.0117(10) 0.0195(11) 0.0246(12) -0.0053(9) 0.0004(9) -0.0059(9) N3C 0.0161(11) 0.0204(11) 0.0260(12) -0.0047(10) 0.0005(9) -0.0060(9) N4C 0.0127(11) 0.0188(11) 0.0300(13) -0.0066(10) 0.0009(9) -0.0050(9) C5C 0.0139(12) 0.0143(12) 0.0211(13) -0.0048(10) -0.0024(10) -0.0032(10) C6C 0.0153(13) 0.0164(13) 0.0188(13) -0.0064(10) -0.0017(10) -0.0047(10) N7C 0.0123(10) 0.0140(10) 0.0188(11) -0.0030(8) -0.0017(8) -0.0038(8) C8C 0.0130(12) 0.0197(13) 0.0206(13) -0.0066(11) -0.0019(10) -0.0058(10) C9C 0.0176(13) 0.0209(13) 0.0224(14) -0.0052(11) 0.0033(10) -0.0116(11) C10C 0.0241(14) 0.0172(13) 0.0229(14) -0.0018(11) -0.0018(11) -0.0086(11) N11C 0.0179(11) 0.0148(11) 0.0262(12) -0.0027(9) -0.0004(9) -0.0058(9) N1D 0.0114(10) 0.0158(11) 0.0236(11) -0.0080(9) -0.0016(8) -0.0040(8) N2D 0.0133(11) 0.0202(11) 0.0314(13) -0.0117(10) -0.0017(9) -0.0053(9) N3D 0.0179(11) 0.0237(12) 0.0299(13) -0.0122(10) -0.0044(9) -0.0051(9) N4D 0.0153(11) 0.0215(12) 0.0275(12) -0.0098(10) -0.0043(9) -0.0030(9) C5D 0.0089(11) 0.0181(13) 0.0202(13) -0.0068(10) -0.0014(10) -0.0003(10) C6D 0.0094(11) 0.0138(12) 0.0187(13) -0.0041(10) -0.0015(9) 0.0004(9) N7D 0.0084(10) 0.0140(10) 0.0194(11) -0.0033(8) -0.0001(8) -0.0035(8) C8D 0.0141(12) 0.0166(12) 0.0204(13) -0.0048(10) -0.0034(10) -0.0033(10) C9D 0.0146(13) 0.0176(13) 0.0255(14) -0.0013(11) -0.0039(10) -0.0070(10) C10D 0.0134(12) 0.0188(13) 0.0230(14) 0.0017(11) -0.0011(10) -0.0064(10) N11D 0.0135(10) 0.0207(11) 0.0189(11) -0.0021(9) -0.0011(9) -0.0029(9) O1 0.0099(8) 0.0148(8) 0.0203(9) -0.0034(7) -0.0002(7) -0.0050(7) O1W 0.0151(10) 0.0205(11) 0.0244(11) -0.0095(9) -0.0059(8) 0.0005(8) O2W 0.0106(9) 0.0282(11) 0.0219(10) -0.0111(8) 0.0004(8) -0.0065(8) O3W 0.0230(10) 0.0199(10) 0.0209(10) -0.0044(9) -0.0020(8) -0.0075(8) O4W 0.0175(11) 0.0264(11) 0.0374(12) -0.0061(10) -0.0039(9) -0.0071(9) O5W 0.0343(12) 0.0288(12) 0.0475(14) -0.0126(11) -0.0154(10) -0.0073(10) O6W 0.0375(12) 0.0303(12) 0.0360(13) -0.0071(10) -0.0078(10) -0.0113(10) O7W 0.0487(15) 0.0252(12) 0.0360(13) -0.0073(10) -0.0029(11) 0.0031(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 Fe1 O1 1.7777(16) . ? Fe1 O1W 2.0002(19) . ? Fe1 N1B 2.077(2) . ? Fe1 N1A 2.093(2) . ? Fe1 N7B 2.244(2) . ? Fe1 N7A 2.285(2) . ? Fe2 O1 1.7906(16) . ? Fe2 O2W 2.0330(19) . ? Fe2 N1D 2.095(2) . ? Fe2 N7C 2.161(2) . ? Fe2 N1C 2.170(2) . ? Fe2 N7D 2.177(2) . ? N1A C5A 1.336(3) . ? N1A N2A 1.344(3) . ? N2A N3A 1.310(3) . ? N3A N4A 1.357(3) . ? N4A C5A 1.330(3) . ? C5A C6A 1.473(3) . ? C6A N11A 1.330(3) . ? C6A N7A 1.348(3) . ? N7A C8A 1.338(3) . ? C8A C9A 1.385(4) . ? C9A C10A 1.372(4) . ? C10A N11A 1.350(3) . ? N1B C5B 1.332(3) . ? N1B N2B 1.346(3) . ? N2B N3B 1.318(3) . ? N3B N4B 1.346(3) . ? N4B C5B 1.330(3) . ? C5B C6B 1.464(3) . ? C6B N11B 1.322(3) . ? C6B N7B 1.350(3) . ? N7B C8B 1.341(3) . ? C8B C9B 1.379(4) . ? C9B C10B 1.380(4) . ? C10B N11B 1.342(3) . ? N1C C5C 1.336(3) . ? N1C N2C 1.347(3) . ? N2C N3C 1.313(3) . ? N3C N4C 1.357(3) . ? N4C C5C 1.332(3) . ? C5C C6C 1.466(3) . ? C6C N11C 1.324(3) . ? C6C N7C 1.354(3) . ? N7C C8C 1.343(3) . ? C8C C9C 1.380(3) . ? C9C C10C 1.376(4) . ? C10C N11C 1.346(3) . ? N1D C5D 1.338(3) . ? N1D N2D 1.347(3) . ? N2D N3D 1.320(3) . ? N3D N4D 1.353(3) . ? N4D C5D 1.326(3) . ? C5D C6D 1.466(3) . ? C6D N11D 1.329(3) . ? C6D N7D 1.345(3) . ? N7D C8D 1.340(3) . ? C8D C9D 1.376(4) . ? C9D C10D 1.382(4) . ? C10D N11D 1.338(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 Fe1 O1W 96.19(8) . . ? O1 Fe1 N1B 97.99(8) . . ? O1W Fe1 N1B 95.83(8) . . ? O1 Fe1 N1A 100.66(8) . . ? O1W Fe1 N1A 96.74(8) . . ? N1B Fe1 N1A 156.18(8) . . ? O1 Fe1 N7B 98.78(7) . . ? O1W Fe1 N7B 163.46(8) . . ? N1B Fe1 N7B 75.18(8) . . ? N1A Fe1 N7B 87.40(8) . . ? O1 Fe1 N7A 174.08(7) . . ? O1W Fe1 N7A 82.28(8) . . ? N1B Fe1 N7A 87.86(7) . . ? N1A Fe1 N7A 73.91(7) . . ? N7B Fe1 N7A 83.51(7) . . ? O1 Fe2 O2W 91.64(8) . . ? O1 Fe2 N1D 95.55(8) . . ? O2W Fe2 N1D 165.95(8) . . ? O1 Fe2 N7C 93.10(7) . . ? O2W Fe2 N7C 96.94(8) . . ? N1D Fe2 N7C 94.70(8) . . ? O1 Fe2 N1C 165.68(8) . . ? O2W Fe2 N1C 82.80(8) . . ? N1D Fe2 N1C 92.78(8) . . ? N7C Fe2 N1C 74.59(7) . . ? O1 Fe2 N7D 110.08(7) . . ? O2W Fe2 N7D 90.34(8) . . ? N1D Fe2 N7D 75.87(8) . . ? N7C Fe2 N7D 155.52(8) . . ? N1C Fe2 N7D 83.24(7) . . ? C5A N1A N2A 106.28(19) . . ? C5A N1A Fe1 119.23(16) . . ? N2A N1A Fe1 133.64(16) . . ? N3A N2A N1A 107.78(19) . . ? N2A N3A N4A 110.67(19) . . ? C5A N4A N3A 104.09(19) . . ? N4A C5A N1A 111.2(2) . . ? N4A C5A C6A 130.6(2) . . ? N1A C5A C6A 118.2(2) . . ? N11A C6A N7A 126.4(2) . . ? N11A C6A C5A 120.7(2) . . ? N7A C6A C5A 113.0(2) . . ? C8A N7A C6A 116.9(2) . . ? C8A N7A Fe1 127.86(16) . . ? C6A N7A Fe1 115.16(16) . . ? N7A C8A C9A 121.1(2) . . ? C10A C9A C8A 117.5(2) . . ? N11A C10A C9A 122.9(2) . . ? C6A N11A C10A 115.3(2) . . ? C5B N1B N2B 105.80(19) . . ? C5B N1B Fe1 117.54(16) . . ? N2B N1B Fe1 135.17(16) . . ? N3B N2B N1B 107.7(2) . . ? N2B N3B N4B 110.71(19) . . ? C5B N4B N3B 104.1(2) . . ? N4B C5B N1B 111.7(2) . . ? N4B C5B C6B 129.5(2) . . ? N1B C5B C6B 118.7(2) . . ? N11B C6B N7B 126.6(2) . . ? N11B C6B C5B 120.2(2) . . ? N7B C6B C5B 113.2(2) . . ? C8B N7B C6B 116.3(2) . . ? C8B N7B Fe1 129.22(17) . . ? C6B N7B Fe1 114.50(16) . . ? N7B C8B C9B 121.8(2) . . ? C8B C9B C10B 116.7(2) . . ? N11B C10B C9B 123.2(2) . . ? C6B N11B C10B 115.5(2) . . ? C5C N1C N2C 105.62(19) . . ? C5C N1C Fe2 115.89(15) . . ? N2C N1C Fe2 138.22(16) . . ? N3C N2C N1C 108.19(19) . . ? N2C N3C N4C 110.53(19) . . ? C5C N4C N3C 103.9(2) . . ? N4C C5C N1C 111.8(2) . . ? N4C C5C C6C 130.1(2) . . ? N1C C5C C6C 118.1(2) . . ? N11C C6C N7C 125.7(2) . . ? N11C C6C C5C 121.3(2) . . ? N7C C6C C5C 113.0(2) . . ? C8C N7C C6C 117.5(2) . . ? C8C N7C Fe2 124.09(16) . . ? C6C N7C Fe2 118.37(15) . . ? N7C C8C C9C 120.4(2) . . ? C10C C9C C8C 117.7(2) . . ? N11C C10C C9C 122.9(2) . . ? C6C N11C C10C 115.7(2) . . ? C5D N1D N2D 105.3(2) . . ? C5D N1D Fe2 116.43(16) . . ? N2D N1D Fe2 137.74(17) . . ? N3D N2D N1D 108.1(2) . . ? N2D N3D N4D 110.4(2) . . ? C5D N4D N3D 104.0(2) . . ? N4D C5D N1D 112.2(2) . . ? N4D C5D C6D 129.8(2) . . ? N1D C5D C6D 117.9(2) . . ? N11D C6D N7D 126.4(2) . . ? N11D C6D C5D 120.5(2) . . ? N7D C6D C5D 113.1(2) . . ? C8D N7D C6D 117.1(2) . . ? C8D N7D Fe2 126.15(17) . . ? C6D N7D Fe2 115.65(15) . . ? N7D C8D C9D 120.9(2) . . ? C8D C9D C10D 117.3(2) . . ? N11D C10D C9D 123.2(2) . . ? C6D N11D C10D 115.1(2) . . ? Fe1 O1 Fe2 150.51(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.473 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.064 data_compound7 _database_code_depnum_ccdc_archive 'CCDC 734271' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6 N12 O22 U4' _chemical_formula_weight 1598.39 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2860(8) _cell_length_b 9.1012(10) _cell_length_c 13.1812(14) _cell_angle_alpha 82.6680(10) _cell_angle_beta 79.381(2) _cell_angle_gamma 73.6240(10) _cell_volume 821.59(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2971 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.6 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 694 _exptl_absorpt_coefficient_mu 19.751 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.346 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8698 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.60 _reflns_number_total 4158 _reflns_number_gt 3394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+23.7520P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4158 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 0.797 _refine_ls_restrained_S_all 0.797 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O6 O 0.7857(8) 0.7790(6) 0.5384(4) 0.0153(11) Uani 1 1 d . . . O7 O 1.2648(8) 0.5744(6) 0.5824(4) 0.0154(11) Uani 1 1 d . . . O3 O 0.9180(8) 0.8061(6) 0.2527(4) 0.0177(11) Uani 1 1 d . . . O5 O 1.4066(7) 0.5986(6) 0.2694(4) 0.0143(10) Uani 1 1 d . . . O4 O 1.2828(8) 0.9123(6) 0.1919(4) 0.0166(11) Uani 1 1 d . . . O8 O 1.0680(8) 0.8904(6) 0.6258(4) 0.0156(11) Uani 1 1 d . . . N7 N 0.7793(9) 0.3108(7) 0.9419(5) 0.0147(12) Uani 1 1 d . . . N2 N 0.8918(9) 0.6687(7) 0.7546(5) 0.0134(12) Uani 1 1 d . . . N3 N 0.8432(10) 0.7728(7) 0.8235(5) 0.0162(13) Uani 1 1 d . . . N4 N 0.7914(9) 0.7110(7) 0.9185(5) 0.0147(12) Uani 1 1 d . . . C5 C 0.8100(11) 0.5634(8) 0.9042(5) 0.0132(14) Uani 1 1 d . . . C6 C 0.7718(11) 0.4405(8) 0.9826(6) 0.0148(14) Uani 1 1 d . . . N11 N 0.7349(10) 0.4689(8) 1.0816(5) 0.0178(13) Uani 1 1 d . . . C10 C 0.7048(11) 0.3528(9) 1.1491(6) 0.0191(16) Uani 1 1 d . . . H10 H 0.6765 0.3670 1.2195 0.023 Uiso 1 1 calc R . . C8 C 0.7551(13) 0.1916(9) 1.0113(6) 0.0220(17) Uani 1 1 d . . . H8 H 0.7653 0.0966 0.9885 0.026 Uiso 1 1 calc R . . C9 C 0.7147(12) 0.2121(10) 1.1169(6) 0.0222(17) Uani 1 1 d . . . H9 H 0.6947 0.1318 1.1650 0.027 Uiso 1 1 calc R . . O1W O 1.5403(8) 0.7706(6) 0.4008(5) 0.0217(12) Uani 1 1 d . . . O2W O 0.5880(8) 0.0732(6) 1.3469(4) 0.0207(12) Uani 1 1 d . . . O3W O 1.6492(8) 0.8679(6) 0.1081(4) 0.0209(12) Uani 1 1 d . . . U1 U 1.15994(4) 0.69821(3) 0.266887(19) 0.00973(7) Uani 1 1 d . . . U2 U 1.02657(4) 0.66821(3) 0.555570(19) 0.00858(7) Uani 1 1 d . . . N1 N 0.8709(10) 0.5354(7) 0.8055(5) 0.0156(13) Uani 1 1 d . . . O1 O 1.1509(7) 0.8207(5) 0.4131(4) 0.0107(9) Uani 1 1 d . . . O2 O 1.0613(7) 0.5540(5) 0.4042(4) 0.0111(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O6 0.015(3) 0.018(3) 0.014(3) 0.001(2) -0.006(2) -0.005(2) O7 0.015(3) 0.013(2) 0.021(3) -0.003(2) -0.006(2) -0.004(2) O3 0.017(3) 0.019(3) 0.018(3) 0.001(2) -0.010(2) -0.001(2) O5 0.012(3) 0.012(2) 0.017(3) -0.002(2) 0.000(2) 0.000(2) O4 0.020(3) 0.011(2) 0.018(3) -0.001(2) 0.002(2) -0.006(2) O8 0.020(3) 0.015(3) 0.014(3) -0.004(2) -0.002(2) -0.007(2) N7 0.020(3) 0.013(3) 0.013(3) -0.003(2) -0.001(2) -0.007(3) N2 0.017(3) 0.012(3) 0.012(3) -0.005(2) 0.000(2) -0.004(2) N3 0.022(3) 0.009(3) 0.018(3) -0.004(2) 0.002(3) -0.006(2) N4 0.020(3) 0.013(3) 0.011(3) -0.004(2) 0.003(2) -0.004(2) C5 0.014(3) 0.017(3) 0.011(3) -0.004(3) 0.000(3) -0.008(3) C6 0.013(4) 0.016(3) 0.013(3) -0.003(3) 0.002(3) -0.003(3) N11 0.021(3) 0.022(3) 0.010(3) 0.000(2) -0.004(3) -0.004(3) C10 0.018(4) 0.020(4) 0.014(4) -0.001(3) 0.002(3) -0.001(3) C8 0.036(5) 0.011(3) 0.018(4) 0.001(3) -0.004(3) -0.005(3) C9 0.024(4) 0.023(4) 0.019(4) 0.002(3) -0.002(3) -0.008(3) O1W 0.015(3) 0.020(3) 0.033(3) -0.002(2) -0.008(2) -0.005(2) O2W 0.020(3) 0.018(3) 0.023(3) 0.001(2) -0.002(2) -0.005(2) O3W 0.017(3) 0.021(3) 0.022(3) -0.007(2) -0.001(2) 0.000(2) U1 0.01146(13) 0.00849(12) 0.00891(12) -0.00156(9) -0.00016(9) -0.00265(10) U2 0.00974(13) 0.00739(12) 0.00849(12) -0.00157(9) -0.00081(9) -0.00207(9) N1 0.025(4) 0.011(3) 0.012(3) -0.001(2) -0.002(3) -0.009(3) O1 0.017(3) 0.006(2) 0.009(2) -0.0011(17) -0.0028(19) -0.0032(19) O2 0.014(2) 0.010(2) 0.008(2) -0.0009(18) 0.0011(19) -0.0033(19) _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 O6 U2 1.800(5) . ? O7 U2 1.784(5) . ? O3 U1 1.790(5) . ? O5 U1 1.775(5) . ? O4 U1 2.396(5) . ? O8 U2 2.442(5) . ? N7 C6 1.341(9) . ? N7 C8 1.357(10) . ? N7 U1 2.713(6) 2_766 ? N2 N3 1.326(8) . ? N2 N1 1.342(8) . ? N2 U2 2.627(6) . ? N3 N4 1.339(8) . ? N4 C5 1.345(9) . ? C5 N1 1.328(9) . ? C5 C6 1.474(10) . ? C6 N11 1.327(9) . ? N11 C10 1.332(10) . ? C10 C9 1.379(11) . ? C8 C9 1.394(11) . ? U1 O2 2.227(5) . ? U1 O1 2.329(5) . ? U1 N1 2.520(6) 2_766 ? U1 N7 2.713(6) 2_766 ? U1 U2 3.7443(5) . ? U2 O2 2.261(5) 2_766 ? U2 O2 2.306(5) . ? U2 O1 2.385(5) . ? U2 U2 3.7004(6) 2_766 ? N1 U1 2.520(6) 2_766 ? O2 U2 2.261(5) 2_766 ? 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 C6 N7 C8 115.5(6) . . ? C6 N7 U1 119.7(5) . 2_766 ? C8 N7 U1 124.8(5) . 2_766 ? N3 N2 N1 107.5(6) . . ? N3 N2 U2 134.7(5) . . ? N1 N2 U2 117.7(4) . . ? N2 N3 N4 110.9(6) . . ? N3 N4 C5 103.9(6) . . ? N1 C5 N4 111.4(6) . . ? N1 C5 C6 120.7(6) . . ? N4 C5 C6 127.9(6) . . ? N7 C6 N11 128.3(7) . . ? N7 C6 C5 113.4(6) . . ? N11 C6 C5 118.3(7) . . ? C10 N11 C6 115.7(7) . . ? N11 C10 C9 121.4(7) . . ? N7 C8 C9 119.8(7) . . ? C10 C9 C8 119.2(7) . . ? O5 U1 O3 174.7(2) . . ? O5 U1 O2 92.0(2) . . ? O3 U1 O2 93.1(2) . . ? O5 U1 O1 90.9(2) . . ? O3 U1 O1 91.8(2) . . ? O2 U1 O1 72.84(17) . . ? O5 U1 O4 85.0(2) . . ? O3 U1 O4 91.0(2) . . ? O2 U1 O4 151.06(18) . . ? O1 U1 O4 78.41(17) . . ? O5 U1 N1 86.7(2) . 2_766 ? O3 U1 N1 93.4(2) . 2_766 ? O2 U1 N1 74.94(19) . 2_766 ? O1 U1 N1 147.58(18) . 2_766 ? O4 U1 N1 133.37(19) . 2_766 ? O5 U1 N7 89.6(2) . 2_766 ? O3 U1 N7 85.8(2) . 2_766 ? O2 U1 N7 136.50(18) . 2_766 ? O1 U1 N7 150.61(17) . 2_766 ? O4 U1 N7 72.36(18) . 2_766 ? N1 U1 N7 61.77(19) 2_766 2_766 ? O5 U1 U2 93.86(17) . . ? O3 U1 U2 91.04(17) . . ? O2 U1 U2 35.00(12) . . ? O1 U1 U2 37.94(12) . . ? O4 U1 U2 116.35(13) . . ? N1 U1 U2 109.94(14) 2_766 . ? N7 U1 U2 170.85(13) 2_766 . ? O7 U2 O6 173.4(2) . . ? O7 U2 O2 90.8(2) . 2_766 ? O6 U2 O2 93.3(2) . 2_766 ? O7 U2 O2 95.6(2) . . ? O6 U2 O2 90.6(2) . . ? O2 U2 O2 71.78(19) 2_766 . ? O7 U2 O1 91.2(2) . . ? O6 U2 O1 88.7(2) . . ? O2 U2 O1 142.18(16) 2_766 . ? O2 U2 O1 70.43(16) . . ? O7 U2 O8 85.4(2) . . ? O6 U2 O8 88.3(2) . . ? O2 U2 O8 144.79(17) 2_766 . ? O2 U2 O8 143.41(17) . . ? O1 U2 O8 72.98(16) . . ? O7 U2 N2 90.6(2) . . ? O6 U2 N2 85.4(2) . . ? O2 U2 N2 75.50(17) 2_766 . ? O2 U2 N2 146.74(18) . . ? O1 U2 N2 142.23(17) . . ? O8 U2 N2 69.58(18) . . ? O7 U2 U2 93.93(16) . 2_766 ? O6 U2 U2 92.42(16) . 2_766 ? O2 U2 U2 36.30(12) 2_766 2_766 ? O2 U2 U2 35.49(12) . 2_766 ? O1 U2 U2 105.90(11) . 2_766 ? O8 U2 U2 178.68(13) . 2_766 ? N2 U2 U2 111.60(13) . 2_766 ? O7 U2 U1 96.19(17) . . ? O6 U2 U1 87.73(16) . . ? O2 U2 U1 105.41(12) 2_766 . ? O2 U2 U1 33.64(12) . . ? O1 U2 U1 36.88(11) . . ? O8 U2 U1 109.79(12) . . ? N2 U2 U1 173.10(14) . . ? U2 U2 U1 69.118(9) 2_766 . ? C5 N1 N2 106.3(6) . . ? C5 N1 U1 122.4(5) . 2_766 ? N2 N1 U1 128.5(4) . 2_766 ? U1 O1 U2 105.18(18) . . ? U1 O2 U2 140.4(2) . 2_766 ? U1 O2 U2 111.4(2) . . ? U2 O2 U2 108.22(19) 2_766 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.60 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.210 _refine_diff_density_min -1.892 _refine_diff_density_rms 0.262 data_compound8 _database_code_depnum_ccdc_archive 'CCDC 734272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H18 Dy2 N36 O12' _chemical_formula_weight 1399.80 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' Dy Dy -0.1892 4.4098 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 22.844(3) _cell_length_b 11.4283(14) _cell_length_c 19.349(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5051.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9087 _cell_measurement_theta_min 2.248 _cell_measurement_theta_max 27.615 _exptl_crystal_description prismatic _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 3.029 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5650 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11047 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4225 _reflns_number_gt 2943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4225 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy3 Dy 0.352322(12) 0.20295(3) 0.464160(15) 0.02740(12) Uani 1 1 d . . . O2 O 0.38398(18) 0.3948(4) 0.4937(2) 0.0370(11) Uani 1 1 d . . . O3 O 0.40283(18) 0.1561(4) 0.5685(2) 0.0400(12) Uani 1 1 d . . . N7B N 0.4659(2) 0.2056(5) 0.4332(3) 0.0346(14) Uani 1 1 d . . . N7A N 0.2855(2) 0.2956(5) 0.5706(3) 0.0355(14) Uani 1 1 d . . . N7F N 0.2875(2) 0.0738(5) 0.3756(2) 0.0310(13) Uani 1 1 d . . . N11B N 0.5506(2) 0.0858(5) 0.4130(3) 0.0395(15) Uani 1 1 d . . . N11A N 0.1960(2) 0.3940(5) 0.5951(3) 0.0448(16) Uani 1 1 d . . . N1B N 0.3972(2) 0.0113(5) 0.4357(3) 0.0381(14) Uani 1 1 d . . . N1A N 0.2619(2) 0.3078(5) 0.4328(3) 0.0339(13) Uani 1 1 d . . . N1F N 0.2864(2) 0.0621(5) 0.5198(2) 0.0335(13) Uani 1 1 d . . . N2B N 0.3764(3) -0.0991(6) 0.4328(3) 0.0475(16) Uani 1 1 d . . . N2A N 0.2396(3) 0.3353(5) 0.3699(3) 0.0470(16) Uani 1 1 d . . . N2F N 0.2717(3) 0.0373(5) 0.5854(3) 0.0526(18) Uani 1 1 d . . . N3B N 0.4194(3) -0.1712(5) 0.4219(3) 0.0487(17) Uani 1 1 d . . . N3A N 0.1931(3) 0.4004(5) 0.3784(3) 0.0517(17) Uani 1 1 d . . . N4B N 0.4712(3) -0.1107(5) 0.4183(3) 0.0433(15) Uani 1 1 d . . . N4A N 0.1830(2) 0.4169(5) 0.4460(3) 0.0447(16) Uani 1 1 d . . . C8B C 0.5003(3) 0.3002(7) 0.4291(4) 0.0445(18) Uani 1 1 d . . . H2B H 0.4835 0.3738 0.4341 0.053 Uiso 1 1 calc R . . C8A C 0.2946(3) 0.2849(6) 0.6381(4) 0.0460(19) Uani 1 1 d . . . H2D H 0.3284 0.2473 0.6530 0.055 Uiso 1 1 calc R . . C8F C 0.2876(3) 0.0707(7) 0.3064(3) 0.046(2) Uani 1 1 d . . . C9B C 0.5607(3) 0.2923(8) 0.4173(4) 0.054(2) Uani 1 1 d . . . H3B H 0.5844 0.3584 0.4147 0.065 Uiso 1 1 calc R . . C9A C 0.2563(4) 0.3270(6) 0.6869(4) 0.051(2) Uani 1 1 d . . . H3D H 0.2634 0.3195 0.7341 0.061 Uiso 1 1 calc R . . C9F C 0.2500 0.0000 0.2687(5) 0.058(3) Uani 1 2 d S . . C10B C 0.5828(3) 0.1813(8) 0.4099(4) 0.053(2) Uani 1 1 d . . . H4B H 0.6228 0.1730 0.4023 0.063 Uiso 1 1 calc R . . C10A C 0.2068(3) 0.3806(7) 0.6618(4) 0.057(2) Uani 1 1 d . . . H4D H 0.1796 0.4091 0.6933 0.068 Uiso 1 1 calc R . . C6B C 0.4934(3) 0.1029(6) 0.4243(3) 0.0341(17) Uani 1 1 d . . . C6A C 0.2356(3) 0.3508(6) 0.5528(3) 0.0323(16) Uani 1 1 d . . . C6F C 0.2500 0.0000 0.4064(4) 0.027(2) Uani 1 2 d S . . C5B C 0.4555(3) 0.0020(6) 0.4273(3) 0.0336(17) Uani 1 1 d . . . C5A C 0.2256(3) 0.3602(6) 0.4790(3) 0.0333(16) Uani 1 1 d . . . C5F C 0.2500 0.0000 0.4813(4) 0.027(2) Uani 1 2 d S . . N2R N 0.4727(3) 0.3978(7) 0.2617(4) 0.079(2) Uani 1 1 d . . . N7R N 0.4466(5) 0.0448(8) 0.2574(4) 0.111(4) Uani 1 1 d . . . N1R N 0.4543(3) 0.2873(7) 0.2696(4) 0.070(2) Uani 1 1 d . . . C7R C 0.4486(6) -0.0759(12) 0.2554(6) 0.135(5) Uiso 1 1 d . . . H2R H 0.4145 -0.1200 0.2578 0.162 Uiso 1 1 calc R . . C8R C 0.5000 -0.1272(16) 0.2500 0.112(5) Uiso 1 2 d S . . H3R H 0.5000 -0.2086 0.2500 0.134 Uiso 1 2 calc SR . . C6R C 0.5000 0.0914(15) 0.2500 0.080(5) Uani 1 2 d S . . C5R C 0.5000 0.2239(12) 0.2500 0.060(3) Uani 1 2 d S . . O1W O 0.0694(2) 0.3909(6) 0.1235(3) 0.0823(19) Uani 1 1 d . . . O2W O 0.0467(2) 0.4026(5) 0.3994(4) 0.086(2) Uani 1 1 d . . . O3W O 0.1133(3) 0.4299(7) 0.2560(3) 0.114(3) Uani 1 1 d . . . O1 O 0.36357(19) 0.2857(4) 0.3532(2) 0.0452(13) Uani 1 1 d . . . H3F H 0.2500 0.0000 0.214(5) 0.05(3) Uiso 1 2 d S . . H2F H 0.314(3) 0.126(6) 0.279(4) 0.07(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy3 0.01884(18) 0.0252(2) 0.03816(18) 0.00332(14) 0.00097(13) 0.00226(15) O2 0.027(3) 0.028(3) 0.056(3) -0.002(2) 0.007(2) 0.002(2) O3 0.027(3) 0.046(3) 0.047(3) 0.005(2) -0.007(2) 0.008(2) N7B 0.029(3) 0.025(4) 0.050(3) 0.005(3) 0.003(3) 0.004(3) N7A 0.031(3) 0.030(4) 0.046(3) 0.003(3) 0.004(3) 0.000(3) N7F 0.031(3) 0.030(3) 0.032(3) 0.003(2) 0.005(2) 0.001(3) N11B 0.024(3) 0.042(4) 0.053(4) 0.001(3) 0.004(3) 0.005(3) N11A 0.028(3) 0.046(4) 0.060(4) -0.013(3) 0.015(3) -0.004(3) N1B 0.032(4) 0.025(4) 0.057(4) -0.003(3) -0.002(3) 0.003(3) N1A 0.023(3) 0.032(4) 0.047(3) -0.002(3) -0.002(3) 0.006(3) N1F 0.041(3) 0.032(3) 0.027(3) -0.002(2) -0.002(2) -0.010(3) N2B 0.037(4) 0.030(4) 0.076(4) -0.003(3) -0.004(3) 0.002(3) N2A 0.040(4) 0.047(4) 0.054(4) -0.005(3) -0.005(3) 0.008(3) N2F 0.068(5) 0.050(5) 0.040(3) 0.003(3) -0.003(3) -0.022(4) N3B 0.054(4) 0.027(4) 0.065(4) 0.004(3) -0.001(3) 0.008(3) N3A 0.038(4) 0.047(5) 0.070(5) 0.002(4) -0.010(3) 0.015(3) N4B 0.043(4) 0.039(4) 0.048(4) 0.001(3) 0.000(3) 0.012(3) N4A 0.028(3) 0.042(4) 0.065(4) -0.007(3) -0.005(3) 0.011(3) C8B 0.037(4) 0.034(5) 0.062(5) 0.005(4) 0.001(4) 0.002(4) C8A 0.046(5) 0.045(5) 0.048(4) 0.004(4) -0.001(4) 0.003(4) C8F 0.055(5) 0.045(5) 0.038(4) 0.004(4) 0.007(4) -0.011(4) C9B 0.031(4) 0.059(6) 0.072(5) 0.005(5) 0.005(4) -0.007(4) C9A 0.056(5) 0.047(6) 0.050(4) -0.001(4) 0.008(4) -0.010(4) C9F 0.078(9) 0.066(9) 0.029(6) 0.000 0.000 -0.011(7) C10B 0.020(4) 0.068(7) 0.070(5) -0.002(5) 0.005(4) 0.003(4) C10A 0.044(5) 0.053(6) 0.073(6) -0.021(5) 0.024(4) -0.014(5) C6B 0.036(4) 0.033(5) 0.033(4) 0.003(3) -0.001(3) 0.008(4) C6A 0.024(4) 0.021(4) 0.052(4) -0.005(3) 0.008(3) -0.009(3) C6F 0.022(5) 0.029(6) 0.030(5) 0.000 0.000 0.009(4) C5B 0.029(4) 0.029(5) 0.043(4) -0.007(3) -0.002(3) 0.012(4) C5A 0.020(4) 0.028(4) 0.053(4) 0.001(3) 0.000(3) -0.003(3) C5F 0.028(5) 0.028(6) 0.024(5) 0.000 0.000 0.004(4) N2R 0.071(6) 0.086(6) 0.081(5) -0.002(5) 0.037(4) 0.008(5) N7R 0.192(11) 0.089(7) 0.052(5) -0.003(5) 0.013(6) -0.043(8) N1R 0.067(5) 0.074(6) 0.069(5) 0.006(4) 0.027(4) -0.001(5) C6R 0.130(15) 0.084(14) 0.026(6) 0.000 0.009(8) 0.000 C5R 0.079(10) 0.066(11) 0.037(6) 0.000 0.014(6) 0.000 O1W 0.065(4) 0.096(5) 0.087(4) -0.008(4) 0.022(3) 0.007(4) O2W 0.059(4) 0.052(4) 0.147(6) 0.017(4) -0.005(4) 0.006(3) O3W 0.090(5) 0.160(7) 0.091(5) 0.010(5) 0.003(4) 0.046(5) O1 0.035(3) 0.054(4) 0.046(3) 0.013(2) 0.002(2) -0.001(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 Dy3 O1 2.360(4) . ? Dy3 O2 2.379(5) . ? Dy3 O3 2.385(4) . ? Dy3 N1F 2.454(5) . ? Dy3 N1A 2.464(5) . ? Dy3 N1B 2.480(6) . ? Dy3 N7B 2.662(5) . ? Dy3 N7F 2.703(5) . ? Dy3 N7A 2.775(5) . ? N7B C8B 1.339(8) . ? N7B C6B 1.342(7) . ? N7A C8A 1.328(8) . ? N7A C6A 1.348(8) . ? N7F C8F 1.340(8) . ? N7F C6F 1.341(6) . ? N11B C10B 1.317(9) . ? N11B C6B 1.339(8) . ? N11A C6A 1.317(8) . ? N11A C10A 1.323(9) . ? N1B C5B 1.345(8) . ? N1B N2B 1.349(8) . ? N1A N2A 1.355(7) . ? N1A C5A 1.358(8) . ? N1F C5F 1.322(6) . ? N1F N2F 1.344(7) . ? N2B N3B 1.299(8) . ? N2A N3A 1.308(7) . ? N2F N2F 1.308(11) 2 ? N3B N4B 1.372(8) . ? N3A N4A 1.342(8) . ? N4B C5B 1.349(8) . ? N4A C5A 1.331(8) . ? C8B C9B 1.403(10) . ? C8B H2B 0.9300 . ? C8A C9A 1.374(10) . ? C8A H2D 0.9300 . ? C8F C9F 1.388(9) . ? C8F H2F 1.02(7) . ? C9B C10B 1.373(10) . ? C9B H3B 0.9300 . ? C9A C10A 1.374(10) . ? C9A H3D 0.9300 . ? C9F C8F 1.388(9) 2 ? C9F H3F 1.05(9) . ? C10B H4B 0.9300 . ? C10A H4D 0.9300 . ? C6B C5B 1.443(9) . ? C6A C5A 1.450(9) . ? C6F N7F 1.341(6) 2 ? C6F C5F 1.450(11) . ? C5F N1F 1.322(6) 2 ? N2R N2R 1.328(12) 4_655 ? N2R N1R 1.338(8) . ? N7R C6R 1.339(10) . ? N7R C7R 1.380(13) . ? N1R C5R 1.325(9) . ? C7R C8R 1.316(13) . ? C7R H2R 0.9300 . ? C8R C7R 1.316(13) 4_655 ? C8R H3R 0.9300 . ? C6R N7R 1.339(10) 4_655 ? C6R C5R 1.515(18) . ? C5R N1R 1.325(9) 4_655 ? 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 Dy3 O2 79.40(16) . . ? O1 Dy3 O3 143.79(14) . . ? O2 Dy3 O3 81.76(16) . . ? O1 Dy3 N1F 136.79(16) . . ? O2 Dy3 N1F 133.33(15) . . ? O3 Dy3 N1F 77.21(16) . . ? O1 Dy3 N1A 70.88(16) . . ? O2 Dy3 N1A 82.30(16) . . ? O3 Dy3 N1A 136.30(17) . . ? N1F Dy3 N1A 84.95(18) . . ? O1 Dy3 N1B 96.16(17) . . ? O2 Dy3 N1B 137.86(17) . . ? O3 Dy3 N1B 77.83(17) . . ? N1F Dy3 N1B 76.81(18) . . ? N1A Dy3 N1B 136.18(18) . . ? O1 Dy3 N7B 71.63(16) . . ? O2 Dy3 N7B 75.37(16) . . ? O3 Dy3 N7B 73.83(15) . . ? N1F Dy3 N7B 134.78(18) . . ? N1A Dy3 N7B 139.12(17) . . ? N1B Dy3 N7B 63.71(18) . . ? O1 Dy3 N7F 72.67(15) . . ? O2 Dy3 N7F 145.32(15) . . ? O3 Dy3 N7F 132.72(16) . . ? N1F Dy3 N7F 65.37(15) . . ? N1A Dy3 N7F 69.52(16) . . ? N1B Dy3 N7F 66.66(16) . . ? N7B Dy3 N7F 113.41(16) . . ? O1 Dy3 N7A 125.63(16) . . ? O2 Dy3 N7A 68.72(15) . . ? O3 Dy3 N7A 73.97(16) . . ? N1F Dy3 N7A 65.59(16) . . ? N1A Dy3 N7A 62.34(17) . . ? N1B Dy3 N7A 136.82(17) . . ? N7B Dy3 N7A 134.35(17) . . ? N7F Dy3 N7A 112.18(16) . . ? C8B N7B C6B 115.0(6) . . ? C8B N7B Dy3 126.5(4) . . ? C6B N7B Dy3 118.4(4) . . ? C8A N7A C6A 115.3(6) . . ? C8A N7A Dy3 127.5(5) . . ? C6A N7A Dy3 117.0(4) . . ? C8F N7F C6F 115.3(6) . . ? C8F N7F Dy3 130.3(5) . . ? C6F N7F Dy3 114.4(4) . . ? C10B N11B C6B 115.6(6) . . ? C6A N11A C10A 115.8(7) . . ? C5B N1B N2B 105.6(6) . . ? C5B N1B Dy3 120.4(5) . . ? N2B N1B Dy3 133.6(4) . . ? N2A N1A C5A 105.0(5) . . ? N2A N1A Dy3 130.4(4) . . ? C5A N1A Dy3 124.4(4) . . ? C5F N1F N2F 105.2(5) . . ? C5F N1F Dy3 119.4(4) . . ? N2F N1F Dy3 134.9(4) . . ? N3B N2B N1B 109.5(6) . . ? N3A N2A N1A 108.9(6) . . ? N2F N2F N1F 109.0(3) 2 . ? N2B N3B N4B 109.9(6) . . ? N2A N3A N4A 109.9(6) . . ? C5B N4B N3B 104.1(6) . . ? C5A N4A N3A 105.9(6) . . ? N7B C8B C9B 122.4(7) . . ? N7B C8B H2B 118.8 . . ? C9B C8B H2B 118.8 . . ? N7A C8A C9A 123.0(7) . . ? N7A C8A H2D 118.5 . . ? C9A C8A H2D 118.5 . . ? N7F C8F C9F 122.7(8) . . ? N7F C8F H2F 120(4) . . ? C9F C8F H2F 117(4) . . ? C10B C9B C8B 116.0(7) . . ? C10B C9B H3B 122.0 . . ? C8B C9B H3B 122.0 . . ? C10A C9A C8A 115.9(7) . . ? C10A C9A H3D 122.1 . . ? C8A C9A H3D 122.1 . . ? C8F C9F C8F 116.5(10) . 2 ? C8F C9F H3F 121.8(5) . . ? C8F C9F H3F 121.8(5) 2 . ? N11B C10B C9B 123.7(7) . . ? N11B C10B H4B 118.1 . . ? C9B C10B H4B 118.1 . . ? N11A C10A C9A 123.4(7) . . ? N11A C10A H4D 118.3 . . ? C9A C10A H4D 118.3 . . ? N11B C6B N7B 127.3(7) . . ? N11B C6B C5B 118.4(6) . . ? N7B C6B C5B 114.3(6) . . ? N11A C6A N7A 126.6(6) . . ? N11A C6A C5A 118.5(6) . . ? N7A C6A C5A 114.9(6) . . ? N7F C6F N7F 127.4(8) 2 . ? N7F C6F C5F 116.3(4) 2 . ? N7F C6F C5F 116.3(4) . . ? N1B C5B N4B 110.8(6) . . ? N1B C5B C6B 122.4(6) . . ? N4B C5B C6B 126.7(6) . . ? N4A C5A N1A 110.2(6) . . ? N4A C5A C6A 128.5(6) . . ? N1A C5A C6A 121.3(6) . . ? N1F C5F N1F 111.5(7) . 2 ? N1F C5F C6F 124.3(4) . . ? N1F C5F C6F 124.3(4) 2 . ? N2R N2R N1R 109.4(4) 4_655 . ? C6R N7R C7R 111.3(14) . . ? C5R N1R N2R 103.7(8) . . ? C8R C7R N7R 118.5(16) . . ? C8R C7R H2R 120.7 . . ? N7R C7R H2R 120.7 . . ? C7R C8R C7R 127(2) 4_655 . ? C7R C8R H3R 116.4 4_655 . ? C7R C8R H3R 116.4 . . ? N7R C6R N7R 133.1(17) 4_655 . ? N7R C6R C5R 113.4(8) 4_655 . ? N7R C6R C5R 113.4(8) . . ? N1R C5R N1R 113.7(12) 4_655 . ? N1R C5R C6R 123.2(6) 4_655 . ? N1R C5R C6R 123.2(6) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 1.578 _refine_diff_density_min -1.134 _refine_diff_density_rms 0.133