# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Hui-Zhong Kou' 'Ai-Li Cui' 'Zhong-Hai Ni' 'Bing Zhang' _publ_contact_author_name 'Hui-Zhong Kou' _publ_contact_author_address ; Department of Chemistry Tsinghua University Beijing 100084 CHINA ; _publ_contact_author_email KOUHZ@MAIL.TSINGHUA.EDU.CN _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Heterometallic trinuclear CuIIMIII2 (M = Fe or Cr) complexes with novel bridges and unusual magnetic properties ; data_1 _database_code_depnum_ccdc_archive 'CCDC 614387' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 Cl2 Cu N6 O8' _chemical_formula_weight 520.86 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 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 8.8437(12) _cell_length_b 8.7562(11) _cell_length_c 13.5885(18) _cell_angle_alpha 90.00 _cell_angle_beta 102.355(3) _cell_angle_gamma 90.00 _cell_volume 1027.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 15.26 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 542 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 '\w scans' _diffrn_detector_area_resol_mean 0.77 _diffrn_standards_decay_% none _diffrn_reflns_number 6182 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2247 _reflns_number_gt 1634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (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^)+(0.0894P)^2^+1.5266P] 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 2247 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1921 _refine_ls_wR_factor_gt 0.1809 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 Cu1 Cu 0.5000 0.0000 0.0000 0.0491(3) Uani 1 2 d S . . Cl2 Cl 0.32345(17) 0.32184(17) 0.10851(11) 0.0604(4) Uani 1 1 d . . . N1 N 0.3950(5) -0.1147(5) 0.0939(3) 0.0473(10) Uani 1 1 d . . . H1A H 0.3591 -0.0432 0.1317 0.057 Uiso 1 1 calc R . . N2 N 0.6963(5) 0.0352(5) 0.1049(4) 0.0531(11) Uani 1 1 d . . . H2A H 0.6795 0.1153 0.1439 0.064 Uiso 1 1 calc R . . N3 N 0.6305(5) -0.1476(6) 0.2262(4) 0.0611(12) Uani 1 1 d . . . C1 C 0.1367(7) -0.2421(8) 0.0911(5) 0.0703(17) Uani 1 1 d . . . H1B H 0.0519 -0.2916 0.0466 0.106 Uiso 1 1 calc R . . H1C H 0.0993 -0.1542 0.1208 0.106 Uiso 1 1 calc R . . H1D H 0.1837 -0.3119 0.1432 0.106 Uiso 1 1 calc R . . C2 C 0.2547(6) -0.1929(7) 0.0325(4) 0.0557(13) Uani 1 1 d . . . H2B H 0.2891 -0.2835 0.0010 0.067 Uiso 1 1 calc R . . C3 C 0.4983(6) -0.2175(7) 0.1663(5) 0.0579(14) Uani 1 1 d . . . H3A H 0.4380 -0.2626 0.2106 0.070 Uiso 1 1 calc R . . H3B H 0.5323 -0.2999 0.1285 0.070 Uiso 1 1 calc R . . C4 C 0.5981(10) -0.0383(9) 0.3000(5) 0.081(2) Uani 1 1 d . . . H4A H 0.5199 -0.0789 0.3319 0.121 Uiso 1 1 calc R . . H4B H 0.5623 0.0558 0.2668 0.121 Uiso 1 1 calc R . . H4C H 0.6909 -0.0197 0.3499 0.121 Uiso 1 1 calc R . . C5 C 0.7461(7) -0.0984(8) 0.1728(5) 0.0653(16) Uani 1 1 d . . . H5A H 0.7709 -0.1829 0.1328 0.078 Uiso 1 1 calc R . . H5B H 0.8396 -0.0714 0.2213 0.078 Uiso 1 1 calc R . . C6 C 0.8157(6) 0.0816(7) 0.0501(4) 0.0555(13) Uani 1 1 d . . . H6A H 0.8547 -0.0074 0.0210 0.067 Uiso 1 1 calc R . . H6B H 0.9016 0.1295 0.0962 0.067 Uiso 1 1 calc R . . O1 O 0.4565(9) 0.2630(9) 0.0924(8) 0.175(4) Uani 1 1 d . . . O2 O 0.2357(7) 0.1971(7) 0.1399(5) 0.1063(18) Uani 1 1 d . . . O3 O 0.3521(9) 0.4292(7) 0.1861(5) 0.122(2) Uani 1 1 d . . . O4 O 0.2338(10) 0.3955(9) 0.0273(5) 0.145(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 Cu1 0.0343(4) 0.0495(5) 0.0673(6) 0.0096(4) 0.0195(4) 0.0006(4) Cl2 0.0578(8) 0.0563(8) 0.0667(9) -0.0044(7) 0.0122(6) 0.0080(6) N1 0.042(2) 0.042(2) 0.064(3) 0.001(2) 0.0237(19) 0.0003(18) N2 0.042(2) 0.052(3) 0.069(3) 0.008(2) 0.021(2) -0.0005(19) N3 0.051(3) 0.075(3) 0.060(3) 0.009(2) 0.016(2) -0.006(2) C1 0.050(3) 0.085(4) 0.080(4) 0.008(4) 0.022(3) -0.007(3) C2 0.041(3) 0.059(3) 0.074(3) -0.007(3) 0.026(2) -0.007(2) C3 0.051(3) 0.055(3) 0.071(3) 0.011(3) 0.019(3) 0.001(3) C4 0.087(5) 0.092(5) 0.065(4) 0.001(4) 0.020(4) -0.011(4) C5 0.046(3) 0.076(4) 0.074(4) 0.016(3) 0.015(3) -0.001(3) C6 0.036(3) 0.062(3) 0.072(4) 0.002(3) 0.018(2) -0.008(2) O1 0.141(6) 0.110(5) 0.314(11) 0.045(6) 0.136(8) 0.053(5) O2 0.113(4) 0.090(4) 0.130(5) -0.012(3) 0.058(4) -0.028(3) O3 0.156(6) 0.085(4) 0.118(5) -0.022(4) 0.011(4) -0.001(4) O4 0.149(6) 0.143(6) 0.124(5) 0.022(5) -0.018(5) 0.020(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.001(4) 3_655 ? Cu1 N1 2.001(4) . ? Cu1 N2 2.020(5) . ? Cu1 N2 2.020(5) 3_655 ? Cl2 O1 1.344(6) . ? Cl2 O4 1.374(7) . ? Cl2 O3 1.395(6) . ? Cl2 O2 1.456(5) . ? N1 C3 1.492(7) . ? N1 C2 1.504(7) . ? N1 H1A 0.9100 . ? N2 C6 1.473(6) . ? N2 C5 1.497(7) . ? N2 H2A 0.9100 . ? N3 C3 1.414(7) . ? N3 C5 1.441(7) . ? N3 C4 1.458(9) . ? C1 C2 1.504(7) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C6 1.517(8) 3_655 ? C2 H2B 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C2 1.517(8) 3_655 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? 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 N1 Cu1 N1 180.0(3) 3_655 . ? N1 Cu1 N2 85.81(17) 3_655 . ? N1 Cu1 N2 94.19(17) . . ? N1 Cu1 N2 94.19(17) 3_655 3_655 ? N1 Cu1 N2 85.81(17) . 3_655 ? N2 Cu1 N2 180.0(3) . 3_655 ? O1 Cl2 O4 115.0(6) . . ? O1 Cl2 O3 110.9(6) . . ? O4 Cl2 O3 105.8(4) . . ? O1 Cl2 O2 107.5(4) . . ? O4 Cl2 O2 109.6(5) . . ? O3 Cl2 O2 107.8(4) . . ? C3 N1 C2 114.0(4) . . ? C3 N1 Cu1 114.9(3) . . ? C2 N1 Cu1 108.4(3) . . ? C3 N1 H1A 106.3 . . ? C2 N1 H1A 106.3 . . ? Cu1 N1 H1A 106.3 . . ? C6 N2 C5 112.2(4) . . ? C6 N2 Cu1 106.7(3) . . ? C5 N2 Cu1 114.2(3) . . ? C6 N2 H2A 107.8 . . ? C5 N2 H2A 107.8 . . ? Cu1 N2 H2A 107.8 . . ? C3 N3 C5 115.3(5) . . ? C3 N3 C4 114.9(5) . . ? C5 N3 C4 114.6(5) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C2 C1 114.9(5) . . ? N1 C2 C6 106.1(4) . 3_655 ? C1 C2 C6 110.8(5) . 3_655 ? N1 C2 H2B 108.3 . . ? C1 C2 H2B 108.3 . . ? C6 C2 H2B 108.3 3_655 . ? N3 C3 N1 115.7(5) . . ? N3 C3 H3A 108.4 . . ? N1 C3 H3A 108.4 . . ? N3 C3 H3B 108.4 . . ? N1 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 N2 113.4(5) . . ? N3 C5 H5A 108.9 . . ? N2 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? N2 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N2 C6 C2 109.0(4) . 3_655 ? N2 C6 H6A 109.9 . . ? C2 C6 H6A 109.9 3_655 . ? N2 C6 H6B 109.9 . . ? C2 C6 H6B 109.9 3_655 . ? H6A C6 H6B 108.3 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.885 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.100 #===End data_2 _database_code_depnum_ccdc_archive 'CCDC 614388' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H62 Cu Fe2 N18 O8' _chemical_formula_weight 1242.44 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' 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 P2(1)/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 15.740(3) _cell_length_b 13.5539(16) _cell_length_c 13.4949(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.108(10) _cell_angle_gamma 90.00 _cell_volume 2879.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 43 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 15.26 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_process_details 'North, et al., 1968' _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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% none _diffrn_reflns_number 5254 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.1326 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5020 _reflns_number_gt 2029 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0421P)^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 5020 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1700 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1610 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 0.82376(6) 0.55554(8) 0.11713(7) 0.0449(3) Uani 1 1 d . . . Cu1 Cu 0.5000 0.5000 0.0000 0.0559(4) Uani 1 2 d S . . N1 N 0.4805(4) 0.6258(4) -0.0787(4) 0.0577(17) Uani 1 1 d . . . H1A H 0.5325 0.6534 -0.0881 0.069 Uiso 1 1 calc R . . N2 N 0.4668(4) 0.5786(4) 0.1176(4) 0.0577(17) Uani 1 1 d . . . H2A H 0.4112 0.5644 0.1294 0.069 Uiso 1 1 calc R . . N3 N 0.4906(5) 0.5470(7) -0.2388(5) 0.076(2) Uani 1 1 d . . . N4 N 0.6514(4) 0.5626(5) 0.0045(5) 0.0666(19) Uani 1 1 d . . . N5 N 1.0018(4) 0.5411(5) 0.2160(4) 0.070(2) Uani 1 1 d . . . N6 N 0.8701(4) 0.6612(4) 0.0281(4) 0.0472(15) Uani 1 1 d . . . N7 N 0.8413(4) 0.4204(4) 0.0602(4) 0.0510(16) Uani 1 1 d . . . N8 N 0.7761(3) 0.4829(4) 0.2219(4) 0.0459(15) Uani 1 1 d . . . N9 N 0.7916(3) 0.6653(4) 0.1943(4) 0.0427(14) Uani 1 1 d . . . C1 C 0.4301(6) 0.8018(6) -0.0461(8) 0.117(4) Uani 1 1 d . . . H1B H 0.4044 0.8050 -0.1106 0.176 Uiso 1 1 calc R . . H1C H 0.4871 0.8269 -0.0495 0.176 Uiso 1 1 calc R . . H1D H 0.3977 0.8407 -0.0004 0.176 Uiso 1 1 calc R . . C2 C 0.4321(5) 0.6950(6) -0.0112(6) 0.071(2) Uani 1 1 d . . . H2B H 0.3732 0.6717 -0.0083 0.086 Uiso 1 1 calc R . . C3 C 0.4434(6) 0.6126(7) -0.1774(6) 0.081(3) Uani 1 1 d . . . H3A H 0.3861 0.5874 -0.1703 0.097 Uiso 1 1 calc R . . H3B H 0.4399 0.6764 -0.2097 0.097 Uiso 1 1 calc R . . C4 C 0.5741(6) 0.5805(7) -0.2684(6) 0.100(3) Uani 1 1 d . . . H4A H 0.6010 0.5305 -0.3079 0.150 Uiso 1 1 calc R . . H4B H 0.6079 0.5931 -0.2105 0.150 Uiso 1 1 calc R . . H4C H 0.5689 0.6400 -0.3066 0.150 Uiso 1 1 calc R . . C5 C 0.4699(5) 0.6828(6) 0.0905(6) 0.073(2) Uani 1 1 d . . . H5A H 0.5283 0.7057 0.0908 0.088 Uiso 1 1 calc R . . H5B H 0.4381 0.7216 0.1381 0.088 Uiso 1 1 calc R . . C6 C 0.5137(5) 0.5564(7) 0.2118(5) 0.078(3) Uani 1 1 d . . . H6A H 0.5728 0.5752 0.2041 0.093 Uiso 1 1 calc R . . H6B H 0.4899 0.5957 0.2650 0.093 Uiso 1 1 calc R . . C7 C 0.7160(4) 0.5594(5) 0.0427(5) 0.0458(17) Uani 1 1 d . . . C8 C 0.9372(5) 0.5460(5) 0.1774(5) 0.0517(19) Uani 1 1 d . . . C9 C 0.8090(5) 0.7570(6) 0.1604(6) 0.058(2) Uani 1 1 d . . . C10 C 0.7781(5) 0.3840(6) 0.2188(6) 0.055(2) Uani 1 1 d . . . C11 C 0.7429(4) 0.5395(5) 0.2997(5) 0.0450(17) Uani 1 1 d . . . C12 C 0.7498(4) 0.6427(5) 0.2834(5) 0.0486(19) Uani 1 1 d . . . C13 C 0.7177(4) 0.7096(6) 0.3534(5) 0.057(2) Uani 1 1 d . . . H13 H 0.7212 0.7773 0.3429 0.069 Uiso 1 1 calc R . . C14 C 0.6807(5) 0.6721(7) 0.4381(6) 0.070(2) Uani 1 1 d . . . H14 H 0.6595 0.7155 0.4855 0.085 Uiso 1 1 calc R . . C15 C 0.6743(5) 0.5719(6) 0.4540(6) 0.076(3) Uani 1 1 d . . . H15 H 0.6491 0.5487 0.5118 0.092 Uiso 1 1 calc R . . C16 C 0.7047(5) 0.5060(6) 0.3860(5) 0.064(2) Uani 1 1 d . . . H16 H 0.6998 0.4386 0.3976 0.077 Uiso 1 1 calc R . . C17 C 0.8151(4) 0.3483(5) 0.1230(5) 0.0459(18) Uani 1 1 d . . . C18 C 0.8181(5) 0.2494(6) 0.0987(6) 0.065(2) Uani 1 1 d . . . H18 H 0.7995 0.2016 0.1431 0.077 Uiso 1 1 calc R . . C19 C 0.8492(5) 0.2232(6) 0.0077(7) 0.069(2) Uani 1 1 d . . . H19 H 0.8523 0.1571 -0.0107 0.082 Uiso 1 1 calc R . . C20 C 0.8757(5) 0.2956(7) -0.0560(6) 0.076(3) Uani 1 1 d . . . H20 H 0.8971 0.2790 -0.1180 0.091 Uiso 1 1 calc R . . C21 C 0.8705(5) 0.3918(6) -0.0283(5) 0.063(2) Uani 1 1 d . . . H21A H 0.8881 0.4400 -0.0728 0.076 Uiso 1 1 calc R . . C22 C 0.8561(5) 0.7523(6) 0.0652(5) 0.0517(19) Uani 1 1 d . . . C23 C 0.8861(5) 0.8368(6) 0.0195(6) 0.068(2) Uani 1 1 d . . . H23 H 0.8782 0.8984 0.0484 0.081 Uiso 1 1 calc R . . C24 C 0.9282(6) 0.8280(7) -0.0700(6) 0.074(3) Uani 1 1 d . . . H24 H 0.9475 0.8838 -0.1031 0.089 Uiso 1 1 calc R . . C25 C 0.9410(5) 0.7356(7) -0.1092(6) 0.072(2) Uani 1 1 d . . . H25 H 0.9696 0.7277 -0.1690 0.087 Uiso 1 1 calc R . . C26 C 0.9109(5) 0.6557(6) -0.0586(5) 0.063(2) Uani 1 1 d . . . H26 H 0.9193 0.5935 -0.0861 0.075 Uiso 1 1 calc R . . O1 O 0.7522(4) 0.3253(4) 0.2824(4) 0.0754(17) Uani 1 1 d . . . O2 O 0.7887(4) 0.8358(4) 0.2003(4) 0.0837(19) Uani 1 1 d . . . O1W O 0.8287(3) 1.0306(3) 0.2043(4) 0.0854(19) Uani 1 1 d . . . H1W1 H 0.8349 0.9681 0.1982 0.128 Uiso 1 1 d R . . H1W2 H 0.8628 1.0423 0.2554 0.128 Uiso 1 1 d R . . O2W O 0.6965(4) 0.1282(4) 0.2981(5) 0.107(2) Uani 1 1 d . . . H2W1 H 0.7167 0.1919 0.2704 0.160 Uiso 1 1 d R . . H2W2 H 0.7279 0.0878 0.2660 0.160 Uiso 1 1 d 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 Fe1 0.0457(6) 0.0428(6) 0.0461(6) -0.0001(5) 0.0008(5) 0.0003(6) Cu1 0.0710(10) 0.0490(8) 0.0478(8) -0.0032(7) -0.0033(7) 0.0118(7) N1 0.048(4) 0.070(5) 0.055(4) 0.010(4) 0.003(3) 0.006(3) N2 0.061(4) 0.051(4) 0.061(4) -0.009(3) 0.010(3) -0.006(3) N3 0.080(5) 0.097(6) 0.052(4) 0.007(4) 0.009(4) -0.010(5) N4 0.050(4) 0.074(5) 0.076(5) -0.001(4) -0.013(4) 0.003(4) N5 0.057(4) 0.091(6) 0.062(4) -0.006(4) -0.008(4) 0.010(4) N6 0.048(4) 0.045(4) 0.048(4) 0.005(3) -0.006(3) -0.003(3) N7 0.058(4) 0.049(4) 0.047(4) -0.005(3) 0.001(3) 0.005(3) N8 0.051(4) 0.035(3) 0.051(4) -0.002(3) -0.003(3) 0.005(3) N9 0.042(4) 0.041(4) 0.045(4) 0.000(3) 0.002(3) -0.001(3) C1 0.123(9) 0.062(6) 0.167(10) 0.029(7) 0.041(8) 0.014(6) C2 0.072(6) 0.057(6) 0.085(6) 0.010(5) 0.022(5) 0.010(5) C3 0.072(6) 0.114(8) 0.055(5) 0.029(5) -0.008(5) -0.006(6) C4 0.093(8) 0.121(9) 0.087(7) 0.036(6) 0.025(6) 0.006(6) C5 0.071(6) 0.057(6) 0.092(7) -0.011(5) 0.021(5) -0.002(5) C6 0.085(7) 0.103(8) 0.044(5) -0.020(5) -0.006(4) -0.013(6) C7 0.046(5) 0.042(4) 0.049(4) 0.004(4) 0.008(4) 0.006(4) C8 0.057(5) 0.052(5) 0.046(4) -0.006(4) 0.015(4) -0.002(4) C9 0.068(6) 0.046(5) 0.060(5) 0.006(4) -0.002(4) -0.012(4) C10 0.057(5) 0.049(5) 0.058(5) 0.009(4) 0.000(4) 0.002(4) C11 0.044(4) 0.047(5) 0.045(4) -0.003(4) 0.005(3) 0.006(4) C12 0.042(4) 0.058(5) 0.045(4) -0.008(4) -0.005(4) 0.003(4) C13 0.053(5) 0.063(5) 0.056(5) -0.015(4) 0.013(4) 0.006(4) C14 0.063(6) 0.079(7) 0.070(6) -0.024(5) 0.018(5) 0.011(5) C15 0.090(7) 0.067(6) 0.072(6) 0.002(5) 0.032(5) -0.003(5) C16 0.073(6) 0.058(5) 0.062(5) 0.002(5) 0.017(4) -0.008(4) C17 0.049(5) 0.045(5) 0.045(4) -0.002(4) -0.006(4) 0.000(4) C18 0.070(6) 0.037(4) 0.086(6) -0.004(5) 0.007(5) 0.002(4) C19 0.064(6) 0.048(5) 0.094(7) -0.016(5) -0.002(5) 0.000(4) C20 0.089(7) 0.066(6) 0.072(6) -0.019(5) 0.003(5) 0.010(6) C21 0.075(6) 0.067(6) 0.048(5) -0.006(4) 0.008(4) 0.000(5) C22 0.055(5) 0.051(5) 0.050(5) 0.004(4) -0.003(4) -0.008(4) C23 0.074(6) 0.051(5) 0.078(6) 0.011(5) 0.001(5) 0.003(5) C24 0.083(7) 0.072(7) 0.067(6) 0.027(5) -0.013(5) -0.021(5) C25 0.068(6) 0.091(7) 0.059(5) 0.014(5) 0.010(4) -0.006(5) C26 0.066(6) 0.075(6) 0.048(5) 0.005(4) 0.014(4) -0.004(5) O1 0.109(5) 0.050(4) 0.068(4) 0.012(3) 0.010(3) 0.000(3) O2 0.126(5) 0.039(3) 0.086(4) -0.010(3) 0.028(4) -0.007(3) O1W 0.076(4) 0.044(4) 0.135(5) -0.007(3) -0.023(4) -0.002(3) O2W 0.090(5) 0.067(4) 0.164(6) 0.000(4) 0.046(4) -0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N8 1.879(6) . ? Fe1 N9 1.885(5) . ? Fe1 C8 1.965(8) . ? Fe1 C7 1.970(7) . ? Fe1 N7 2.006(5) . ? Fe1 N6 2.007(6) . ? Cu1 N2 1.982(5) . ? Cu1 N2 1.982(5) 3_665 ? Cu1 N1 2.032(6) 3_665 ? Cu1 N1 2.032(6) . ? N1 C3 1.463(8) . ? N1 C2 1.515(9) . ? N1 H1A 0.9100 . ? N2 C5 1.460(8) . ? N2 C6 1.501(9) . ? N2 H2A 0.9100 . ? N3 C3 1.425(10) . ? N3 C4 1.448(10) . ? N3 C6 1.450(9) 3_665 ? N4 C7 1.139(7) . ? N5 C8 1.144(8) . ? N6 C26 1.338(8) . ? N6 C22 1.351(8) . ? N7 C21 1.337(8) . ? N7 C17 1.358(8) . ? N8 C10 1.341(8) . ? N8 C11 1.402(8) . ? N9 C9 1.353(8) . ? N9 C12 1.405(8) . ? C1 C2 1.522(10) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C5 1.504(10) . ? C2 H2B 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.450(9) 3_665 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C9 O2 1.238(8) . ? C9 C22 1.485(9) . ? C10 O1 1.240(8) . ? C10 C17 1.500(9) . ? C11 C16 1.387(9) . ? C11 C12 1.420(9) . ? C12 C13 1.404(9) . ? C13 C14 1.381(9) . ? C13 H13 0.9300 . ? C14 C15 1.380(10) . ? C14 H14 0.9300 . ? C15 C16 1.367(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.381(9) . ? C18 C19 1.369(10) . ? C18 H18 0.9300 . ? C19 C20 1.370(10) . ? C19 H19 0.9300 . ? C20 C21 1.360(10) . ? C20 H20 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.385(9) . ? C23 C24 1.383(10) . ? C23 H23 0.9300 . ? C24 C25 1.375(10) . ? C24 H24 0.9300 . ? C25 C26 1.366(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? O1W H1W1 0.8559 . ? O1W H1W2 0.8872 . ? O2W H2W1 0.9933 . ? O2W H2W2 0.8553 . ? 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 N8 Fe1 N9 83.7(2) . . ? N8 Fe1 C8 91.0(3) . . ? N9 Fe1 C8 93.9(3) . . ? N8 Fe1 C7 93.1(3) . . ? N9 Fe1 C7 91.7(3) . . ? C8 Fe1 C7 173.4(3) . . ? N8 Fe1 N7 82.3(2) . . ? N9 Fe1 N7 165.8(2) . . ? C8 Fe1 N7 88.5(3) . . ? C7 Fe1 N7 87.0(3) . . ? N8 Fe1 N6 165.8(2) . . ? N9 Fe1 N6 82.3(2) . . ? C8 Fe1 N6 87.9(3) . . ? C7 Fe1 N6 89.4(2) . . ? N7 Fe1 N6 111.8(3) . . ? N2 Cu1 N2 180.0(2) . 3_665 ? N2 Cu1 N1 94.1(2) . 3_665 ? N2 Cu1 N1 85.9(2) 3_665 3_665 ? N2 Cu1 N1 85.9(2) . . ? N2 Cu1 N1 94.1(2) 3_665 . ? N1 Cu1 N1 180.0(3) 3_665 . ? C3 N1 C2 115.0(7) . . ? C3 N1 Cu1 115.7(5) . . ? C2 N1 Cu1 106.3(4) . . ? C3 N1 H1A 106.4 . . ? C2 N1 H1A 106.4 . . ? Cu1 N1 H1A 106.4 . . ? C5 N2 C6 112.9(7) . . ? C5 N2 Cu1 108.1(5) . . ? C6 N2 Cu1 116.2(5) . . ? C5 N2 H2A 106.4 . . ? C6 N2 H2A 106.4 . . ? Cu1 N2 H2A 106.4 . . ? C3 N3 C4 116.1(8) . . ? C3 N3 C6 115.6(7) . 3_665 ? C4 N3 C6 114.5(8) . 3_665 ? C26 N6 C22 117.0(7) . . ? C26 N6 Fe1 131.2(6) . . ? C22 N6 Fe1 111.7(5) . . ? C21 N7 C17 117.0(6) . . ? C21 N7 Fe1 130.8(6) . . ? C17 N7 Fe1 112.1(4) . . ? C10 N8 C11 125.3(6) . . ? C10 N8 Fe1 119.4(5) . . ? C11 N8 Fe1 115.3(4) . . ? C9 N9 C12 125.8(6) . . ? C9 N9 Fe1 118.9(5) . . ? C12 N9 Fe1 115.3(5) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C5 C2 N1 106.4(6) . . ? C5 C2 C1 113.3(8) . . ? N1 C2 C1 114.4(7) . . ? C5 C2 H2B 107.5 . . ? N1 C2 H2B 107.5 . . ? C1 C2 H2B 107.5 . . ? N3 C3 N1 113.5(7) . . ? N3 C3 H3A 108.9 . . ? N1 C3 H3A 108.9 . . ? N3 C3 H3B 108.9 . . ? N1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C2 108.7(7) . . ? N2 C5 H5A 109.9 . . ? C2 C5 H5A 109.9 . . ? N2 C5 H5B 109.9 . . ? C2 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? N3 C6 N2 112.5(6) 3_665 . ? N3 C6 H6A 109.1 3_665 . ? N2 C6 H6A 109.1 . . ? N3 C6 H6B 109.1 3_665 . ? N2 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N4 C7 Fe1 176.1(6) . . ? N5 C8 Fe1 177.3(6) . . ? O2 C9 N9 126.3(7) . . ? O2 C9 C22 122.9(7) . . ? N9 C9 C22 110.8(7) . . ? O1 C10 N8 127.8(8) . . ? O1 C10 C17 121.2(7) . . ? N8 C10 C17 111.0(7) . . ? C16 C11 N8 127.8(7) . . ? C16 C11 C12 119.0(7) . . ? N8 C11 C12 113.2(6) . . ? C13 C12 N9 127.2(7) . . ? C13 C12 C11 120.3(7) . . ? N9 C12 C11 112.5(6) . . ? C14 C13 C12 118.2(7) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C15 C14 C13 121.5(8) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 120.8(8) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C11 120.2(8) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? N7 C17 C18 122.7(7) . . ? N7 C17 C10 115.1(6) . . ? C18 C17 C10 122.1(7) . . ? C19 C18 C17 118.5(8) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C20 C19 C18 119.1(8) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C21 C20 C19 119.7(8) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? N7 C21 C20 123.0(8) . . ? N7 C21 H21A 118.5 . . ? C20 C21 H21A 118.5 . . ? N6 C22 C23 122.3(7) . . ? N6 C22 C9 116.2(7) . . ? C23 C22 C9 121.5(8) . . ? C24 C23 C22 118.9(8) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C25 C24 C23 119.1(8) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 C24 118.6(8) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? N6 C26 C25 124.1(8) . . ? N6 C26 H26 117.9 . . ? C25 C26 H26 117.9 . . ? H1W1 O1W H1W2 100.5 . . ? H2W1 O2W H2W2 100.4 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.393 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.080 #===End data_3 _database_code_depnum_ccdc_archive 'CCDC 614389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H62 Cr2 Cu N18 O8' _chemical_formula_weight 1234.74 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' Cr Cr 0.3209 0.6236 '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 P2(1)/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 15.969(4) _cell_length_b 13.5984(15) _cell_length_c 13.4235(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.115(12) _cell_angle_gamma 90.00 _cell_volume 2914.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 18.56 _exptl_crystal_description block _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1282 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details 'North, et al., 1968' _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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% none _diffrn_reflns_number 5363 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5123 _reflns_number_gt 2361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0867P)^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 5123 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1571 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 0.5000 0.5000 0.0000 0.0588(4) Uani 1 2 d S . . Cr1 Cr 0.82700(7) 0.55396(8) 0.11328(7) 0.0487(3) Uani 1 1 d . . . N1 N 0.4796(4) 0.6253(5) -0.0788(4) 0.0712(18) Uani 1 1 d . . . H1A H 0.5309 0.6526 -0.0890 0.085 Uiso 1 1 calc R . . N2 N 0.4684(4) 0.5799(5) 0.1185(4) 0.0675(17) Uani 1 1 d . . . H2A H 0.4136 0.5664 0.1308 0.081 Uiso 1 1 calc R . . N3 N 0.4889(5) 0.5443(7) -0.2386(5) 0.085(2) Uani 1 1 d . . . N4 N 0.6484(4) 0.5617(5) 0.0025(5) 0.0755(19) Uani 1 1 d . . . N5 N 1.0068(4) 0.5400(5) 0.2195(5) 0.081(2) Uani 1 1 d . . . N6 N 0.8716(3) 0.6692(4) 0.0260(4) 0.0539(15) Uani 1 1 d . . . N7 N 0.8434(3) 0.4120(4) 0.0598(4) 0.0534(14) Uani 1 1 d . . . N8 N 0.7763(3) 0.4801(4) 0.2226(4) 0.0491(14) Uani 1 1 d . . . N9 N 0.7930(3) 0.6657(4) 0.1966(4) 0.0522(14) Uani 1 1 d . . . C1 C 0.4300(6) 0.7998(7) -0.0474(8) 0.124(4) Uani 1 1 d . . . H1B H 0.4042 0.8028 -0.1120 0.186 Uiso 1 1 calc R . . H1C H 0.4859 0.8255 -0.0513 0.186 Uiso 1 1 calc R . . H1D H 0.3980 0.8382 -0.0011 0.186 Uiso 1 1 calc R . . C2 C 0.4330(6) 0.6951(6) -0.0130(6) 0.080(2) Uani 1 1 d . . . H2B H 0.3751 0.6715 -0.0084 0.096 Uiso 1 1 calc R . . C3 C 0.4430(6) 0.6099(7) -0.1780(6) 0.088(3) Uani 1 1 d . . . H3A H 0.3865 0.5848 -0.1703 0.106 Uiso 1 1 calc R . . H3B H 0.4392 0.6729 -0.2117 0.106 Uiso 1 1 calc R . . C4 C 0.5723(6) 0.5793(8) -0.2694(7) 0.115(4) Uani 1 1 d . . . H4A H 0.5992 0.5296 -0.3087 0.172 Uiso 1 1 calc R . . H4B H 0.6055 0.5928 -0.2113 0.172 Uiso 1 1 calc R . . H4C H 0.5663 0.6382 -0.3081 0.172 Uiso 1 1 calc R . . C5 C 0.4721(5) 0.6849(6) 0.0891(6) 0.082(2) Uani 1 1 d . . . H5A H 0.5298 0.7070 0.0875 0.098 Uiso 1 1 calc R . . H5B H 0.4418 0.7248 0.1369 0.098 Uiso 1 1 calc R . . C6 C 0.5148(6) 0.5560(8) 0.2117(5) 0.091(3) Uani 1 1 d . . . H6A H 0.5730 0.5746 0.2035 0.109 Uiso 1 1 calc R . . H6B H 0.4920 0.5950 0.2657 0.109 Uiso 1 1 calc R . . C7 C 0.7139(5) 0.5585(5) 0.0364(5) 0.0496(16) Uani 1 1 d . . . C8 C 0.9450(5) 0.5448(5) 0.1805(5) 0.0550(18) Uani 1 1 d . . . C9 C 0.8084(4) 0.7572(5) 0.1653(5) 0.0575(18) Uani 1 1 d . . . C10 C 0.7750(4) 0.3811(5) 0.2198(5) 0.0555(18) Uani 1 1 d . . . C11 C 0.7420(4) 0.5374(5) 0.3011(5) 0.0556(18) Uani 1 1 d . . . C12 C 0.7498(4) 0.6399(5) 0.2843(5) 0.0511(17) Uani 1 1 d . . . C13 C 0.7167(4) 0.7053(5) 0.3554(5) 0.0599(19) Uani 1 1 d . . . H13 H 0.7195 0.7728 0.3451 0.072 Uiso 1 1 calc R . . C14 C 0.6805(5) 0.6685(7) 0.4398(6) 0.076(2) Uani 1 1 d . . . H14 H 0.6600 0.7119 0.4874 0.091 Uiso 1 1 calc R . . C15 C 0.6736(5) 0.5692(7) 0.4559(6) 0.079(2) Uani 1 1 d . . . H15 H 0.6482 0.5460 0.5136 0.094 Uiso 1 1 calc R . . C16 C 0.7043(5) 0.5040(6) 0.3866(5) 0.070(2) Uani 1 1 d . . . H16 H 0.6996 0.4367 0.3977 0.084 Uiso 1 1 calc R . . C17 C 0.8130(4) 0.3450(5) 0.1241(5) 0.0578(19) Uani 1 1 d . . . C18 C 0.8158(5) 0.2452(6) 0.1009(6) 0.072(2) Uani 1 1 d . . . H18 H 0.7965 0.1989 0.1464 0.086 Uiso 1 1 calc R . . C19 C 0.8473(5) 0.2153(6) 0.0099(7) 0.081(3) Uani 1 1 d . . . H19 H 0.8481 0.1491 -0.0072 0.098 Uiso 1 1 calc R . . C20 C 0.8772(5) 0.2850(7) -0.0545(6) 0.080(2) Uani 1 1 d . . . H20 H 0.8997 0.2665 -0.1156 0.096 Uiso 1 1 calc R . . C21 C 0.8736(5) 0.3827(6) -0.0278(5) 0.068(2) Uani 1 1 d . . . H21 H 0.8929 0.4299 -0.0724 0.082 Uiso 1 1 calc R . . C22 C 0.8568(4) 0.7577(5) 0.0684(5) 0.0548(17) Uani 1 1 d . . . C23 C 0.8838(5) 0.8438(6) 0.0255(6) 0.077(2) Uani 1 1 d . . . H23 H 0.8739 0.9038 0.0566 0.092 Uiso 1 1 calc R . . C24 C 0.9255(6) 0.8400(7) -0.0641(7) 0.083(3) Uani 1 1 d . . . H24 H 0.9442 0.8977 -0.0939 0.099 Uiso 1 1 calc R . . C25 C 0.9395(5) 0.7514(7) -0.1091(6) 0.075(2) Uani 1 1 d . . . H25 H 0.9670 0.7476 -0.1700 0.090 Uiso 1 1 calc R . . C26 C 0.9117(5) 0.6680(6) -0.0617(5) 0.062(2) Uani 1 1 d . . . H26 H 0.9212 0.6076 -0.0920 0.074 Uiso 1 1 calc R . . O1 O 0.7476(4) 0.3231(4) 0.2823(4) 0.0815(17) Uani 1 1 d . . . O2 O 0.7879(4) 0.8345(4) 0.2050(4) 0.0891(19) Uani 1 1 d . . . O1W O 0.8220(2) 1.0293(3) 0.2123(3) 0.0943(19) Uani 1 1 d . . . H1W1 H 0.8346 0.9663 0.1970 0.141 Uiso 1 1 d R . . H1W2 H 0.8625 1.0404 0.2543 0.141 Uiso 1 1 d R . . O2W O 0.6941(2) 0.1298(3) 0.3057(3) 0.117(2) Uani 1 1 d R . . H2W1 H 0.7080 0.1940 0.2899 0.176 Uiso 1 1 d R . . H2W2 H 0.7302 0.0870 0.2656 0.176 Uiso 1 1 d 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 0.0751(9) 0.0542(8) 0.0472(7) -0.0033(6) -0.0052(6) 0.0102(7) Cr1 0.0531(7) 0.0441(6) 0.0490(6) 0.0004(5) -0.0008(5) 0.0000(6) N1 0.058(4) 0.083(5) 0.072(4) 0.014(4) -0.006(3) 0.007(4) N2 0.072(4) 0.068(4) 0.063(4) -0.010(3) 0.001(3) -0.001(3) N3 0.081(6) 0.110(6) 0.062(4) 0.007(4) 0.001(4) 0.002(5) N4 0.053(4) 0.080(5) 0.093(5) -0.006(4) -0.008(4) 0.000(4) N5 0.058(4) 0.106(6) 0.080(5) -0.011(4) -0.007(4) 0.008(4) N6 0.048(4) 0.058(4) 0.055(3) 0.006(3) -0.009(3) -0.004(3) N7 0.052(4) 0.052(4) 0.056(3) 0.006(3) -0.004(3) 0.000(3) N8 0.058(4) 0.039(3) 0.050(3) 0.002(2) 0.003(3) -0.002(3) N9 0.056(4) 0.045(3) 0.056(3) -0.003(3) -0.003(3) -0.003(3) C1 0.114(9) 0.078(7) 0.179(11) 0.034(7) 0.038(8) 0.018(6) C2 0.073(6) 0.065(6) 0.101(6) -0.001(5) 0.021(5) 0.008(5) C3 0.087(7) 0.105(7) 0.074(6) 0.016(5) 0.002(5) 0.013(6) C4 0.114(9) 0.134(10) 0.096(7) 0.034(6) 0.034(6) 0.025(7) C5 0.084(6) 0.065(6) 0.097(6) -0.025(5) 0.007(5) -0.003(5) C6 0.095(7) 0.126(9) 0.051(5) -0.014(5) -0.001(4) -0.010(7) C7 0.054(5) 0.039(4) 0.056(4) -0.001(3) -0.001(3) -0.002(4) C8 0.047(4) 0.058(5) 0.060(4) -0.007(4) 0.003(3) -0.001(4) C9 0.063(5) 0.045(4) 0.064(5) 0.000(4) -0.001(4) -0.002(4) C10 0.056(5) 0.049(4) 0.061(4) 0.007(4) -0.007(4) 0.003(4) C11 0.059(5) 0.056(5) 0.052(4) 0.001(3) -0.004(3) 0.000(4) C12 0.053(4) 0.048(4) 0.052(4) -0.002(3) -0.005(3) 0.001(3) C13 0.061(5) 0.052(4) 0.067(5) -0.008(4) 0.004(4) -0.001(4) C14 0.080(6) 0.085(7) 0.064(5) -0.016(5) 0.018(4) 0.003(5) C15 0.086(6) 0.088(7) 0.062(5) 0.005(5) 0.014(4) -0.007(5) C16 0.096(6) 0.060(5) 0.053(4) 0.003(4) 0.008(4) -0.005(4) C17 0.060(5) 0.050(4) 0.063(5) -0.002(4) -0.002(4) -0.001(4) C18 0.079(6) 0.051(5) 0.086(6) 0.000(4) -0.001(5) -0.002(4) C19 0.093(7) 0.055(5) 0.096(6) -0.024(5) -0.001(5) 0.004(5) C20 0.089(7) 0.078(6) 0.074(5) -0.023(5) 0.001(5) 0.001(5) C21 0.086(6) 0.065(5) 0.053(4) -0.003(4) -0.007(4) 0.002(5) C22 0.058(5) 0.050(4) 0.056(4) 0.001(4) -0.004(3) -0.002(4) C23 0.101(7) 0.055(5) 0.073(5) 0.016(4) 0.001(5) -0.015(5) C24 0.083(7) 0.080(7) 0.085(6) 0.028(5) -0.009(5) -0.021(5) C25 0.072(6) 0.096(7) 0.057(5) 0.020(5) 0.007(4) -0.012(5) C26 0.063(5) 0.074(6) 0.047(4) 0.002(4) -0.006(4) -0.005(4) O1 0.114(5) 0.048(3) 0.082(4) 0.016(3) 0.019(3) 0.001(3) O2 0.132(5) 0.043(3) 0.092(4) -0.006(3) 0.031(4) -0.008(3) O1W 0.073(4) 0.054(4) 0.155(5) -0.013(3) -0.009(4) 0.004(3) O2W 0.095(5) 0.065(4) 0.193(7) -0.003(4) 0.057(5) -0.013(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 Cu1 N2 1.992(6) 3_665 ? Cu1 N2 1.992(6) . ? Cu1 N1 2.031(6) 3_665 ? Cu1 N1 2.031(6) . ? Cr1 N8 1.955(5) . ? Cr1 N9 1.963(5) . ? Cr1 N7 2.077(6) . ? Cr1 C7 2.080(7) . ? Cr1 N6 2.082(6) . ? Cr1 C8 2.091(8) . ? N1 C3 1.469(9) . ? N1 C2 1.496(9) . ? N1 H1A 0.9100 . ? N2 C5 1.482(9) . ? N2 C6 1.489(9) . ? N2 H2A 0.9100 . ? N3 C6 1.412(10) 3_665 ? N3 C3 1.414(10) . ? N3 C4 1.474(11) . ? N4 C7 1.140(8) . ? N5 C8 1.120(8) . ? N6 C26 1.341(8) . ? N6 C22 1.353(8) . ? N7 C21 1.332(8) . ? N7 C17 1.347(8) . ? N8 C10 1.347(8) . ? N8 C11 1.421(8) . ? N9 C9 1.336(8) . ? N9 C12 1.411(8) . ? C1 C2 1.498(10) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C5 1.511(11) . ? C2 H2B 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.412(10) 3_665 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C9 O2 1.223(8) . ? C9 C22 1.515(9) . ? C10 O1 1.232(8) . ? C10 C17 1.504(9) . ? C11 C16 1.375(9) . ? C11 C12 1.417(9) . ? C12 C13 1.408(9) . ? C13 C14 1.368(10) . ? C13 H13 0.9300 . ? C14 C15 1.372(10) . ? C14 H14 0.9300 . ? C15 C16 1.377(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.393(9) . ? C18 C19 1.383(10) . ? C18 H18 0.9300 . ? C19 C20 1.369(11) . ? C19 H19 0.9300 . ? C20 C21 1.378(10) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.374(9) . ? C23 C24 1.377(11) . ? C23 H23 0.9300 . ? C24 C25 1.367(11) . ? C24 H24 0.9300 . ? C25 C26 1.374(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? O1W H1W1 0.9041 . ? O1W H1W2 0.8706 . ? O2W H2W1 0.9251 . ? O2W H2W2 0.9803 . ? 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 N2 Cu1 N2 180.000(1) 3_665 . ? N2 Cu1 N1 85.3(3) 3_665 3_665 ? N2 Cu1 N1 94.7(3) . 3_665 ? N2 Cu1 N1 94.7(3) 3_665 . ? N2 Cu1 N1 85.3(3) . . ? N1 Cu1 N1 180.0(3) 3_665 . ? N8 Cr1 N9 81.7(2) . . ? N8 Cr1 N7 80.5(2) . . ? N9 Cr1 N7 162.1(2) . . ? N8 Cr1 C7 91.5(2) . . ? N9 Cr1 C7 91.1(2) . . ? N7 Cr1 C7 88.1(2) . . ? N8 Cr1 N6 162.0(2) . . ? N9 Cr1 N6 80.4(2) . . ? N7 Cr1 N6 117.5(2) . . ? C7 Cr1 N6 89.8(2) . . ? N8 Cr1 C8 91.2(2) . . ? N9 Cr1 C8 92.9(2) . . ? N7 Cr1 C8 88.9(2) . . ? C7 Cr1 C8 175.5(3) . . ? N6 Cr1 C8 88.8(2) . . ? C3 N1 C2 115.3(7) . . ? C3 N1 Cu1 114.6(5) . . ? C2 N1 Cu1 107.7(5) . . ? C3 N1 H1A 106.2 . . ? C2 N1 H1A 106.2 . . ? Cu1 N1 H1A 106.2 . . ? C5 N2 C6 114.4(7) . . ? C5 N2 Cu1 107.6(5) . . ? C6 N2 Cu1 115.2(5) . . ? C5 N2 H2A 106.3 . . ? C6 N2 H2A 106.3 . . ? Cu1 N2 H2A 106.3 . . ? C6 N3 C3 116.2(8) 3_665 . ? C6 N3 C4 114.9(8) 3_665 . ? C3 N3 C4 115.3(8) . . ? C26 N6 C22 117.6(6) . . ? C26 N6 Cr1 130.5(5) . . ? C22 N6 Cr1 111.9(5) . . ? C21 N7 C17 119.7(6) . . ? C21 N7 Cr1 129.0(5) . . ? C17 N7 Cr1 111.2(4) . . ? C10 N8 C11 124.2(6) . . ? C10 N8 Cr1 119.9(5) . . ? C11 N8 Cr1 115.8(4) . . ? C9 N9 C12 125.7(6) . . ? C9 N9 Cr1 119.4(5) . . ? C12 N9 Cr1 114.8(4) . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C2 C1 115.9(7) . . ? N1 C2 C5 105.8(6) . . ? C1 C2 C5 112.3(8) . . ? N1 C2 H2B 107.5 . . ? C1 C2 H2B 107.5 . . ? C5 C2 H2B 107.5 . . ? N3 C3 N1 113.9(7) . . ? N3 C3 H3A 108.8 . . ? N1 C3 H3A 108.8 . . ? N3 C3 H3B 108.8 . . ? N1 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C2 108.2(6) . . ? N2 C5 H5A 110.1 . . ? C2 C5 H5A 110.1 . . ? N2 C5 H5B 110.1 . . ? C2 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N3 C6 N2 113.9(7) 3_665 . ? N3 C6 H6A 108.8 3_665 . ? N2 C6 H6A 108.8 . . ? N3 C6 H6B 108.8 3_665 . ? N2 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? N4 C7 Cr1 173.8(6) . . ? N5 C8 Cr1 177.6(6) . . ? O2 C9 N9 127.9(7) . . ? O2 C9 C22 120.5(7) . . ? N9 C9 C22 111.6(6) . . ? O1 C10 N8 128.8(7) . . ? O1 C10 C17 121.1(7) . . ? N8 C10 C17 110.1(6) . . ? C16 C11 C12 119.8(7) . . ? C16 C11 N8 127.4(7) . . ? C12 C11 N8 112.8(6) . . ? C13 C12 N9 126.4(6) . . ? C13 C12 C11 118.7(6) . . ? N9 C12 C11 114.8(6) . . ? C14 C13 C12 119.4(7) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.6(7) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C16 119.9(7) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C11 C16 C15 120.6(8) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? N7 C17 C18 120.3(7) . . ? N7 C17 C10 118.3(6) . . ? C18 C17 C10 121.5(7) . . ? C19 C18 C17 119.7(8) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C18 118.9(8) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 119.2(8) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N7 C21 C20 122.2(8) . . ? N7 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? N6 C22 C23 121.8(7) . . ? N6 C22 C9 116.5(6) . . ? C23 C22 C9 121.6(7) . . ? C22 C23 C24 119.1(8) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C23 120.0(8) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 118.0(7) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? N6 C26 C25 123.5(7) . . ? N6 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? H1W1 O1W H1W2 98.3 . . ? H2W1 O2W H2W2 107.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.493 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.077 #===End data_4 _database_code_depnum_ccdc_archive 'CCDC 614390' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H48 Cu Fe2 N16 O6' _chemical_formula_weight 1096.24 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' 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 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 10.761(2) _cell_length_b 15.6358(19) _cell_length_c 14.1161(18) _cell_angle_alpha 90.00 _cell_angle_beta 94.630(12) _cell_angle_gamma 90.00 _cell_volume 2367.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 49 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 18.56 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1130 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details 'North, et al., 1968' _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 P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% none _diffrn_reflns_number 3484 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2568 _reflns_number_gt 1928 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0472P)^2^+2.1066P] 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 2568 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 0.09710(11) 0.36021(4) 0.33481(4) 0.0473(5) Uani 1 1 d . . . Cu1 Cu 0.0000 0.0000 0.5000 0.0651(4) Uani 1 2 d S . . N1 N 0.0899(5) -0.0716(2) 0.4082(2) 0.0724(16) Uani 1 1 d . . . H1A H 0.0339 -0.0860 0.3600 0.087 Uiso 1 1 calc R . . H1B H 0.1468 -0.0377 0.3836 0.087 Uiso 1 1 calc R . . N2 N 0.1530(5) -0.0108(2) 0.5914(2) 0.0609(14) Uani 1 1 d . . . H2A H 0.2133 0.0220 0.5697 0.073 Uiso 1 1 calc R . . H2B H 0.1349 0.0112 0.6476 0.073 Uiso 1 1 calc R . . N3 N -0.1699(7) 0.3746(4) 0.4003(4) 0.079(3) Uani 1 1 d . . . N4 N 0.3813(8) 0.3718(3) 0.3054(3) 0.067(3) Uani 1 1 d . . . N5 N 0.0973(4) 0.2386(2) 0.3344(2) 0.0444(12) Uani 1 1 d . . . N6 N 0.1495(4) 0.3424(2) 0.4716(2) 0.0483(13) Uani 1 1 d . . . N7 N 0.0885(4) 0.4849(2) 0.3003(3) 0.0499(13) Uani 1 1 d . . . N8 N 0.0426(4) 0.3478(2) 0.2053(2) 0.0463(13) Uani 1 1 d . . . C1 C 0.2045(6) -0.0970(3) 0.6089(3) 0.0641(18) Uani 1 1 d . . . H1C H 0.1403 -0.1337 0.6312 0.077 Uiso 1 1 calc R . . H1D H 0.2724 -0.0941 0.6583 0.077 Uiso 1 1 calc R . . C2 C 0.2514(6) -0.1350(3) 0.5208(3) 0.069(2) Uani 1 1 d . . . H2C H 0.3142 -0.0972 0.4985 0.083 Uiso 1 1 calc R . . H2D H 0.2918 -0.1890 0.5376 0.083 Uiso 1 1 calc R . . C3 C 0.1541(6) -0.1504(3) 0.4411(3) 0.0662(19) Uani 1 1 d . . . H3A H 0.1929 -0.1761 0.3884 0.079 Uiso 1 1 calc R . . H3B H 0.0932 -0.1905 0.4618 0.079 Uiso 1 1 calc R . . C4 C -0.0723(9) 0.3682(3) 0.3753(4) 0.047(3) Uani 1 1 d . . . C5 C 0.2778(9) 0.3667(3) 0.3147(3) 0.039(4) Uani 1 1 d . . . C6 C 0.1266(5) 0.1973(3) 0.4158(3) 0.0486(16) Uani 1 1 d . . . C7 C 0.1560(5) 0.2590(3) 0.4950(3) 0.0454(15) Uani 1 1 d . . . C8 C 0.0071(6) 0.4178(3) 0.1550(3) 0.0542(17) Uani 1 1 d . . . C9 C 0.0448(5) 0.4966(3) 0.2083(3) 0.0511(17) Uani 1 1 d . . . C10 C 0.0436(6) 0.5756(3) 0.1656(4) 0.0631(18) Uani 1 1 d . . . H10 H 0.0159 0.5816 0.1019 0.076 Uiso 1 1 calc R . . C11 C 0.0839(6) 0.6458(3) 0.2183(4) 0.075(2) Uani 1 1 d . . . H11 H 0.0831 0.7000 0.1911 0.090 Uiso 1 1 calc R . . C12 C 0.1252(6) 0.6342(3) 0.3117(4) 0.073(2) Uani 1 1 d . . . H12 H 0.1523 0.6808 0.3488 0.088 Uiso 1 1 calc R . . C13 C 0.1265(5) 0.5536(3) 0.3507(4) 0.0624(18) Uani 1 1 d . . . H13 H 0.1547 0.5467 0.4143 0.075 Uiso 1 1 calc R . . C14 C 0.1899(6) 0.2313(3) 0.5868(3) 0.0610(18) Uani 1 1 d . . . H14 H 0.1956 0.1732 0.6007 0.073 Uiso 1 1 calc R . . C15 C 0.2153(6) 0.2921(3) 0.6575(3) 0.0665(19) Uani 1 1 d . . . H15 H 0.2367 0.2754 0.7199 0.080 Uiso 1 1 calc R . . C16 C 0.2083(6) 0.3769(3) 0.6336(3) 0.070(2) Uani 1 1 d . . . H16 H 0.2259 0.4187 0.6797 0.084 Uiso 1 1 calc R . . C17 C 0.1749(6) 0.4000(3) 0.5410(3) 0.0623(18) Uani 1 1 d . . . H17 H 0.1698 0.4579 0.5258 0.075 Uiso 1 1 calc R . . C18 C 0.0647(5) 0.2021(3) 0.2446(3) 0.0438(15) Uani 1 1 d . . . C19 C 0.0641(6) 0.1155(3) 0.2215(3) 0.0557(17) Uani 1 1 d . . . H19 H 0.0830 0.0748 0.2685 0.067 Uiso 1 1 calc R . . C20 C 0.0353(6) 0.0901(3) 0.1286(3) 0.0660(19) Uani 1 1 d . . . H20 H 0.0347 0.0322 0.1134 0.079 Uiso 1 1 calc R . . C21 C 0.0075(6) 0.1498(3) 0.0583(3) 0.0632(19) Uani 1 1 d . . . H21 H -0.0105 0.1318 -0.0041 0.076 Uiso 1 1 calc R . . C22 C 0.0059(5) 0.2359(3) 0.0794(3) 0.0558(17) Uani 1 1 d . . . H22 H -0.0142 0.2758 0.0317 0.067 Uiso 1 1 calc R . . C23 C 0.0349(5) 0.2627(3) 0.1730(3) 0.0459(15) Uani 1 1 d . . . O1 O 0.1264(4) 0.11838(18) 0.4295(2) 0.0630(12) Uani 1 1 d . . . O2 O -0.0518(4) 0.4215(2) 0.0760(2) 0.0754(13) Uani 1 1 d . . . O1W O 0.1238(4) 0.0903(3) 0.7656(2) 0.0793(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 Fe1 0.0603(16) 0.0409(3) 0.0404(3) -0.0001(2) 0.0015(4) -0.0014(4) Cu1 0.1015(12) 0.0523(5) 0.0391(4) -0.0072(3) -0.0092(5) 0.0243(5) N1 0.109(5) 0.059(2) 0.046(2) -0.0108(17) -0.012(2) 0.018(3) N2 0.083(5) 0.059(2) 0.0409(19) -0.0054(16) 0.004(2) 0.001(2) N3 0.039(9) 0.112(4) 0.086(4) 0.002(3) 0.011(4) 0.014(4) N4 0.064(10) 0.076(3) 0.062(3) 0.008(2) 0.016(4) -0.010(4) N5 0.051(4) 0.0406(17) 0.0409(18) -0.0016(14) -0.0016(19) -0.0036(19) N6 0.051(4) 0.051(2) 0.0437(18) -0.0043(15) 0.009(2) -0.005(2) N7 0.046(4) 0.050(2) 0.054(2) -0.0024(17) 0.008(2) -0.001(2) N8 0.047(4) 0.0470(19) 0.0447(18) 0.0021(15) 0.004(2) -0.005(2) C1 0.058(6) 0.078(3) 0.055(3) 0.010(2) 0.004(3) 0.015(3) C2 0.078(7) 0.074(3) 0.055(3) -0.002(2) 0.004(3) 0.010(3) C3 0.079(6) 0.056(3) 0.064(3) -0.010(2) 0.007(3) 0.011(3) C4 0.030(11) 0.059(3) 0.054(3) 0.001(2) 0.012(4) 0.007(4) C5 0.037(13) 0.042(2) 0.040(2) 0.0011(17) 0.011(4) -0.008(4) C6 0.053(5) 0.047(2) 0.046(2) 0.0038(18) 0.006(2) -0.005(3) C7 0.045(5) 0.049(2) 0.043(2) 0.0021(18) 0.006(2) -0.005(3) C8 0.059(6) 0.054(3) 0.050(3) 0.010(2) 0.007(3) 0.000(3) C9 0.047(6) 0.054(2) 0.053(3) 0.006(2) 0.004(3) 0.004(3) C10 0.060(6) 0.047(3) 0.082(3) 0.014(2) 0.005(3) -0.003(3) C11 0.071(7) 0.050(3) 0.105(4) 0.017(3) 0.012(4) -0.001(3) C12 0.083(7) 0.043(3) 0.093(4) -0.007(3) -0.001(4) -0.003(3) C13 0.065(6) 0.054(3) 0.067(3) -0.004(2) 0.002(3) 0.000(3) C14 0.074(6) 0.061(3) 0.047(2) 0.005(2) 0.001(3) -0.004(3) C15 0.078(6) 0.081(3) 0.041(2) -0.002(2) 0.003(3) -0.009(4) C16 0.092(7) 0.071(3) 0.046(2) -0.010(2) -0.001(3) -0.003(3) C17 0.084(6) 0.053(3) 0.050(2) -0.005(2) 0.000(3) -0.004(3) C18 0.040(5) 0.050(2) 0.042(2) 0.0020(18) 0.004(2) -0.003(3) C19 0.063(6) 0.047(2) 0.056(3) 0.000(2) 0.001(3) -0.004(3) C20 0.086(6) 0.052(3) 0.060(3) -0.015(2) 0.006(3) -0.009(3) C21 0.075(6) 0.068(3) 0.046(2) -0.014(2) 0.005(3) -0.008(3) C22 0.061(6) 0.062(3) 0.044(2) 0.000(2) 0.002(3) -0.006(3) C23 0.042(5) 0.051(2) 0.045(2) -0.0037(18) 0.003(2) -0.007(3) O1 0.092(4) 0.0459(16) 0.0497(16) 0.0056(13) -0.0024(19) -0.0053(19) O2 0.104(4) 0.064(2) 0.0541(19) 0.0147(16) -0.017(2) -0.003(2) O1W 0.069(4) 0.112(3) 0.058(2) -0.0189(19) 0.010(2) -0.004(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 Fe1 N8 1.884(3) . ? Fe1 N5 1.901(3) . ? Fe1 C4 1.958(9) . ? Fe1 N6 1.987(3) . ? Fe1 C5 1.990(10) . ? Fe1 N7 2.010(4) . ? Cu1 N2 2.016(4) 3_556 ? Cu1 N2 2.016(4) . ? Cu1 N1 2.018(4) 3_556 ? Cu1 N1 2.018(4) . ? N1 C3 1.469(6) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C1 1.470(6) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C4 1.139(7) . ? N4 C5 1.135(7) . ? N5 C6 1.334(5) . ? N5 C18 1.408(5) . ? N6 C17 1.342(5) . ? N6 C7 1.346(5) . ? N7 C13 1.335(6) . ? N7 C9 1.357(6) . ? N8 C8 1.344(5) . ? N8 C23 1.406(5) . ? C1 C2 1.502(7) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 C3 1.493(7) . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C6 O1 1.248(5) . ? C6 C7 1.491(6) . ? C7 C14 1.386(6) . ? C8 O2 1.238(5) . ? C8 C9 1.482(6) . ? C9 C10 1.374(6) . ? C10 C11 1.377(7) . ? C10 H10 0.9300 . ? C11 C12 1.369(7) . ? C11 H11 0.9300 . ? C12 C13 1.375(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.389(6) . ? C14 H14 0.9300 . ? C15 C16 1.370(7) . ? C15 H15 0.9300 . ? C16 C17 1.377(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.393(6) . ? C18 C23 1.404(6) . ? C19 C20 1.380(6) . ? C19 H19 0.9300 . ? C20 C21 1.377(7) . ? C20 H20 0.9300 . ? C21 C22 1.380(6) . ? C21 H21 0.9300 . ? C22 C23 1.397(6) . ? C22 H22 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 N8 Fe1 N5 83.94(14) . . ? N8 Fe1 C4 93.8(2) . . ? N5 Fe1 C4 93.8(2) . . ? N8 Fe1 N6 165.95(15) . . ? N5 Fe1 N6 82.10(14) . . ? C4 Fe1 N6 85.6(2) . . ? N8 Fe1 C5 95.61(19) . . ? N5 Fe1 C5 92.85(19) . . ? C4 Fe1 C5 169.1(2) . . ? N6 Fe1 C5 86.70(19) . . ? N8 Fe1 N7 81.94(14) . . ? N5 Fe1 N7 165.76(14) . . ? C4 Fe1 N7 89.04(19) . . ? N6 Fe1 N7 112.06(15) . . ? C5 Fe1 N7 86.69(19) . . ? N2 Cu1 N2 180.00(16) 3_556 . ? N2 Cu1 N1 87.46(16) 3_556 3_556 ? N2 Cu1 N1 92.54(16) . 3_556 ? N2 Cu1 N1 92.54(16) 3_556 . ? N2 Cu1 N1 87.46(16) . . ? N1 Cu1 N1 180.00(14) 3_556 . ? C3 N1 Cu1 120.0(3) . . ? C3 N1 H1A 107.3 . . ? Cu1 N1 H1A 107.3 . . ? C3 N1 H1B 107.3 . . ? Cu1 N1 H1B 107.3 . . ? H1A N1 H1B 106.9 . . ? C1 N2 Cu1 117.5(3) . . ? C1 N2 H2A 107.9 . . ? Cu1 N2 H2A 107.9 . . ? C1 N2 H2B 107.9 . . ? Cu1 N2 H2B 107.9 . . ? H2A N2 H2B 107.2 . . ? C6 N5 C18 127.1(3) . . ? C6 N5 Fe1 118.9(3) . . ? C18 N5 Fe1 114.1(3) . . ? C17 N6 C7 117.9(4) . . ? C17 N6 Fe1 129.8(3) . . ? C7 N6 Fe1 112.3(3) . . ? C13 N7 C9 118.1(4) . . ? C13 N7 Fe1 130.2(3) . . ? C9 N7 Fe1 111.6(3) . . ? C8 N8 C23 126.3(4) . . ? C8 N8 Fe1 118.8(3) . . ? C23 N8 Fe1 114.7(3) . . ? N2 C1 C2 111.8(4) . . ? N2 C1 H1C 109.3 . . ? C2 C1 H1C 109.3 . . ? N2 C1 H1D 109.3 . . ? C2 C1 H1D 109.3 . . ? H1C C1 H1D 107.9 . . ? C3 C2 C1 115.2(5) . . ? C3 C2 H2C 108.5 . . ? C1 C2 H2C 108.5 . . ? C3 C2 H2D 108.5 . . ? C1 C2 H2D 108.5 . . ? H2C C2 H2D 107.5 . . ? N1 C3 C2 112.8(4) . . ? N1 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? N1 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N3 C4 Fe1 178.2(6) . . ? N4 C5 Fe1 178.1(5) . . ? O1 C6 N5 127.6(4) . . ? O1 C6 C7 121.7(4) . . ? N5 C6 C7 110.7(4) . . ? N6 C7 C14 122.4(4) . . ? N6 C7 C6 116.1(3) . . ? C14 C7 C6 121.5(4) . . ? O2 C8 N8 128.1(4) . . ? O2 C8 C9 121.1(4) . . ? N8 C8 C9 110.7(4) . . ? N7 C9 C10 122.0(4) . . ? N7 C9 C8 115.7(4) . . ? C10 C9 C8 122.1(4) . . ? C9 C10 C11 119.3(5) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 118.5(5) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 120.0(5) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? N7 C13 C12 122.1(5) . . ? N7 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C7 C14 C15 118.7(4) . . ? C7 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C16 C15 C14 118.8(4) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.5(4) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N6 C17 C16 122.6(4) . . ? N6 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C19 C18 C23 119.4(4) . . ? C19 C18 N5 127.0(4) . . ? C23 C18 N5 113.6(4) . . ? C20 C19 C18 119.9(4) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.6(4) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 120.8(4) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 119.4(4) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C18 119.9(4) . . ? C22 C23 N8 126.4(4) . . ? C18 C23 N8 113.6(3) . . ? _diffrn_measured_fraction_theta_max 0.616 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.616 _refine_diff_density_max 0.357 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.054 #===End