# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1665 data_9/05437E_CuN4_mono #------------------------------------------------------------------------------ _audit_creation_date 'Mon Mar 8 15:03:28 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 7.660(4) _cell_length_b 19.209(3) _cell_length_c 7.265(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1069.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 493.2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.0 _cell_measurement_theta_max 17.8 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'pruple' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_meas ? _chemical_formula_weight 271.76 _chemical_formula_analytical ? _chemical_formula_sum 'C6 H16 Cu N4 O4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 564.00 _exptl_absorpt_coefficient_mu 2.046 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.837 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 493.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.09 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -1 -1 0 -1 -2 0 -3 -1 _diffrn_reflns_number 1066 _reflns_number_total 1066 _reflns_number_observed 930 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.03669 _diffrn_orient_matrix_UB_12 -0.04867 _diffrn_orient_matrix_UB_13 -0.02985 _diffrn_orient_matrix_UB_21 -0.08366 _diffrn_orient_matrix_UB_22 -0.01828 _diffrn_orient_matrix_UB_23 0.09396 _diffrn_orient_matrix_UB_31 -0.09325 _diffrn_orient_matrix_UB_32 -0.00275 _diffrn_orient_matrix_UB_33 -0.09605 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 24 0.003 0.002 'International Tables' H 0 64 0.000 0.000 'International Tables' N 0 16 0.006 0.003 'International Tables' O 0 16 0.011 0.006 'International Tables' Cu 0 4 0.320 1.265 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.4447(1) 0.05866(5) 0.5774(2) 0.0270(3) Uij ? ? O(1) -0.0601(9) 0.0878(3) 0.7025(9) 0.032(2) Uij ? ? O(2) 0.0223(8) -0.0520(3) 0.7255(9) 0.031(2) Uij ? ? O(3) -0.2022(9) 0.2027(3) 0.869(1) 0.046(2) Uij ? ? O(4) -0.0290(9) -0.1861(3) 0.6315(10) 0.037(2) Uij ? ? N(1) 0.543(1) 0.1568(4) 0.562(1) 0.038(2) Uij ? ? N(2) 0.2268(10) 0.1065(3) 0.615(1) 0.033(2) Uij ? ? N(3) 0.2993(9) -0.0217(4) 0.6297(10) 0.027(2) Uij ? ? N(4) 0.6391(8) -0.0122(4) 0.578(1) 0.029(2) Uij ? ? C(1) 0.415(2) 0.2037(5) 0.642(2) 0.058(4) Uij ? ? C(2) 0.233(1) 0.1812(4) 0.599(2) 0.042(3) Uij ? ? C(3) 0.091(1) 0.0693(5) 0.666(1) 0.031(3) Uij ? ? C(4) 0.139(1) -0.0104(4) 0.673(1) 0.020(2) Uij ? ? C(5) 0.389(1) -0.0874(5) 0.650(1) 0.033(3) Uij ? ? C(6) 0.579(1) -0.0718(5) 0.692(1) 0.037(3) Uij ? ? H(1) 0.4297 0.2046 0.7716 0.0693 Uij ? ? H(2) 0.4324 0.2491 0.5936 0.0693 Uij ? ? H(3) 0.2023 0.1950 0.4780 0.0501 Uij ? ? H(4) 0.1538 0.2016 0.6846 0.0501 Uij ? ? H(5) 0.3385 -0.1132 0.7482 0.0392 Uij ? ? H(6) 0.3799 -0.1135 0.5392 0.0392 Uij ? ? H(7) 0.6480 -0.1116 0.6645 0.0444 Uij ? ? H(8) 0.5912 -0.0604 0.8183 0.0444 Uij ? ? H(9) 0.6493 0.1596 0.6286 0.0461 Uij ? ? H(10) 0.5633 0.1689 0.4369 0.0461 Uij ? ? H(11) 0.6622 -0.0273 0.4555 0.0353 Uij ? ? H(12) 0.7419 0.0075 0.6289 0.0353 Uij ? ? H(13) -0.02(1) -0.137(4) 0.66(1) 0.03(2) Uij ? ? H(14) -0.11(1) -0.193(4) 0.56(1) 0.01(2) Uij ? ? H(15) -0.13(1) 0.236(5) 0.83(1) 0.04(2) Uij ? ? H(16) -0.12(2) 0.162(7) 0.83(2) 0.14(2) Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0161(5) 0.0275(5) 0.0374(5) -0.0044(5) -0.0002(6) 0.0041(6) O(1) 0.018(3) 0.030(3) 0.048(4) 0.001(3) 0.004(4) -0.006(3) O(2) 0.027(4) 0.020(3) 0.047(4) -0.005(3) 0.014(3) -0.001(3) O(3) 0.030(4) 0.030(4) 0.077(6) -0.003(3) 0.013(4) 0.008(4) O(4) 0.033(4) 0.026(3) 0.052(5) 0.005(3) -0.007(4) 0.001(3) N(1) 0.035(5) 0.043(4) 0.037(4) -0.016(4) 0.009(5) -0.002(4) N(2) 0.030(4) 0.017(3) 0.052(6) -0.004(3) 0.006(4) 0.000(4) N(3) 0.025(5) 0.019(4) 0.036(5) 0.000(3) 0.002(4) -0.001(3) N(4) 0.016(4) 0.052(4) 0.021(3) 0.002(3) 0.000(4) 0.009(4) C(1) 0.070(8) 0.033(5) 0.070(8) -0.014(6) 0.034(7) -0.007(5) C(2) 0.039(6) 0.023(4) 0.063(7) -0.008(4) -0.004(6) 0.005(5) C(3) 0.014(5) 0.038(5) 0.041(5) -0.003(4) -0.004(4) -0.002(4) C(4) 0.020(5) 0.018(4) 0.022(4) 0.001(4) 0.002(4) 0.005(3) C(5) 0.030(7) 0.031(5) 0.038(5) 0.003(4) 0.001(5) 0.017(4) C(6) 0.024(5) 0.046(6) 0.041(5) 0.006(5) -0.005(5) 0.009(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 930 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0438 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0511 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.478 _refine_ls_shift/esd_max 0.0350 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.44 _refine_diff_density_max 0.32 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(1) 2.033(7) ? ? yes Cu(1) N(2) 1.924(7) ? ? yes Cu(1) N(3) 1.941(7) ? ? yes Cu(1) N(4) 2.018(7) ? ? yes O(1) C(3) 1.24(1) ? ? yes O(2) C(4) 1.258(9) ? ? yes N(1) C(1) 1.46(1) ? ? yes N(2) C(2) 1.441(10) ? ? yes N(2) C(3) 1.32(1) ? ? yes N(3) C(4) 1.29(1) ? ? yes N(3) C(5) 1.44(1) ? ? yes N(4) C(6) 1.49(1) ? ? yes C(1) C(2) 1.49(1) ? ? yes C(3) C(4) 1.58(1) ? ? yes C(5) C(6) 1.52(1) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(2) 83.5(3) ? ? ? yes N(1) Cu(1) N(3) 163.9(3) ? ? ? yes N(1) Cu(1) N(4) 110.6(3) ? ? ? yes N(2) Cu(1) N(3) 81.6(3) ? ? ? yes N(2) Cu(1) N(4) 164.2(3) ? ? ? yes N(3) Cu(1) N(4) 83.5(3) ? ? ? yes Cu(1) N(1) C(1) 107.6(6) ? ? ? yes Cu(1) N(2) C(2) 115.9(6) ? ? ? yes Cu(1) N(2) C(3) 117.8(6) ? ? ? yes C(2) N(2) C(3) 126.0(8) ? ? ? yes Cu(1) N(3) C(4) 117.5(6) ? ? ? yes Cu(1) N(3) C(5) 116.4(5) ? ? ? yes C(4) N(3) C(5) 125.1(7) ? ? ? yes Cu(1) N(4) C(6) 107.0(5) ? ? ? yes N(1) C(1) C(2) 111.7(8) ? ? ? yes N(2) C(2) C(1) 107.6(8) ? ? ? yes O(1) C(3) N(2) 130.0(9) ? ? ? yes O(1) C(3) C(4) 119.3(8) ? ? ? yes N(2) C(3) C(4) 110.7(7) ? ? ? yes O(2) C(4) N(3) 130.2(8) ? ? ? yes O(2) C(4) C(3) 117.5(7) ? ? ? yes N(3) C(4) C(3) 112.2(7) ? ? ? yes N(3) C(5) C(6) 107.6(8) ? ? ? yes N(4) C(6) C(5) 109.7(8) ? ? ? yes #------------------------------------------------------------------------------ #===END data_9/05437E_CuN4_di #------------------------------------------------------------------------------ _audit_creation_date 'Mon Mar 8 15:42:02 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.977(5) _cell_length_b 15.243(4) _cell_length_c 13.878(4) _cell_angle_alpha 90 _cell_angle_beta 100.53(3) _cell_angle_gamma 90 _cell_volume 2282(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 24.4 _cell_measurement_theta_max 24.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_meas ? _chemical_formula_weight 579.56 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H36 Cu2 N8 O10 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1208.00 _exptl_absorpt_coefficient_mu 1.928 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.31 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 0 -2 -3 -1 -1 -3 -1 0 _diffrn_reflns_number 4173 _reflns_number_total 3965 _reflns_number_observed 2612 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 9.30 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.05725 _diffrn_orient_matrix_UB_12 -0.04769 _diffrn_orient_matrix_UB_13 -0.02988 _diffrn_orient_matrix_UB_21 -0.07171 _diffrn_orient_matrix_UB_22 0.04131 _diffrn_orient_matrix_UB_23 -0.00548 _diffrn_orient_matrix_UB_31 0.01293 _diffrn_orient_matrix_UB_32 0.01797 _diffrn_orient_matrix_UB_33 -0.06670 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 48 0.003 0.002 'International Tables' H 0 144 0.000 0.000 'International Tables' O 0 40 0.011 0.006 'International Tables' N 0 32 0.006 0.003 'International Tables' Cu 0 8 0.320 1.265 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Cu(1) 0.65123(7) 0.18934(6) 0.64591(5) 0.0251(3) Uij ? ? Cu(2) 0.84098(7) 0.18949(6) 0.86464(5) 0.0254(3) Uij ? ? O(1) 1.0060(4) 0.2169(3) 0.6197(3) 0.035(1) Uij ? ? O(2) 0.8798(5) 0.3724(3) 0.5798(4) 0.044(2) Uij ? ? O(3) 0.6220(5) 0.3792(3) 0.9304(4) 0.048(2) Uij ? ? O(4) 0.4867(4) 0.2272(3) 0.8894(3) 0.032(1) Uij ? ? O(5) 0.8197(6) 0.5398(4) 0.5163(4) 0.045(2) Uij ? ? O(6) 1.1778(7) 0.3675(6) 0.6577(6) 0.068(3) Uij ? ? O(7) 1.2345(7) 0.1481(6) 0.6569(6) 0.100(3) Uij ? ? O(8) 0.3297(6) 0.1126(4) 0.3400(5) 0.048(2) Uij ? ? O(9) 0.2588(6) 0.1550(4) 0.8556(4) 0.057(2) Uij ? ? O(10) 0.6809(7) 0.5476(4) 0.9736(5) 0.052(2) Uij ? ? N(1) 0.8298(5) 0.1568(4) 0.6612(4) 0.024(2) Uij ? ? N(2) 0.7141(5) 0.3045(4) 0.6287(4) 0.030(2) Uij ? ? N(3) 0.4849(5) 0.2537(4) 0.6063(4) 0.030(2) Uij ? ? N(4) 0.5698(5) 0.0746(4) 0.6558(4) 0.029(2) Uij ? ? N(5) 0.9161(5) 0.0719(4) 0.8567(4) 0.031(2) Uij ? ? N(6) 1.0103(5) 0.2508(4) 0.9035(4) 0.029(2) Uij ? ? N(7) 0.7836(5) 0.3063(4) 0.8805(4) 0.029(2) Uij ? ? N(8) 0.6599(5) 0.1613(3) 0.8506(4) 0.024(2) Uij ? ? C(1) 0.8958(6) 0.2202(4) 0.6323(4) 0.023(2) Uij ? ? C(2) 0.8265(6) 0.3085(5) 0.6116(5) 0.027(2) Uij ? ? C(3) 0.6285(7) 0.3769(4) 0.6107(5) 0.030(2) Uij ? ? C(4) 0.5063(7) 0.3465(5) 0.6346(6) 0.037(2) Uij ? ? C(5) 0.8903(6) 0.0718(4) 0.6750(4) 0.026(2) Uij ? ? C(6) 0.9783(6) 0.0608(5) 0.7702(5) 0.030(2) Uij ? ? C(7) 0.9933(7) 0.3434(5) 0.8723(6) 0.039(2) Uij ? ? C(8) 0.8726(7) 0.3767(4) 0.8968(5) 0.032(2) Uij ? ? C(9) 0.6709(6) 0.3140(5) 0.8983(4) 0.027(2) Uij ? ? C(10) 0.5978(6) 0.2271(4) 0.8780(4) 0.024(2) Uij ? ? C(11) 0.5959(6) 0.0769(4) 0.8374(4) 0.027(2) Uij ? ? C(12) 0.5064(7) 0.0678(5) 0.7422(5) 0.028(2) Uij ? ? H(1) 0.6593 0.4252 0.6511 0.0364 Uij ? ? H(2) 0.6177 0.3939 0.5438 0.0364 Uij ? ? H(3) 0.5081 0.3526 0.7030 0.0451 Uij ? ? H(4) 0.4411 0.3813 0.5996 0.0451 Uij ? ? H(5) 0.8275 0.0282 0.6716 0.0317 Uij ? ? H(6) 0.9347 0.0631 0.6233 0.0317 Uij ? ? H(7) 1.0422 0.1033 0.7737 0.0361 Uij ? ? H(8) 1.0133 0.0036 0.7722 0.0361 Uij ? ? H(9) 0.9907 0.3477 0.8035 0.0467 Uij ? ? H(10) 1.0602 0.3778 0.9057 0.0467 Uij ? ? H(11) 0.8850 0.3946 0.9634 0.0380 Uij ? ? H(12) 0.8433 0.4251 0.8558 0.0380 Uij ? ? H(13) 0.6562 0.0320 0.8405 0.0323 Uij ? ? H(14) 0.5511 0.0696 0.8893 0.0323 Uij ? ? H(15) 0.4460 0.1128 0.7381 0.0338 Uij ? ? H(16) 0.4671 0.0121 0.7409 0.0338 Uij ? ? H(17) 0.4569 0.2491 0.5376 0.0368 Uij ? ? H(18) 0.4248 0.2289 0.6397 0.0368 Uij ? ? H(19) 0.5101 0.0658 0.5979 0.0341 Uij ? ? H(20) 0.6312 0.0299 0.6610 0.0341 Uij ? ? H(21) 0.8527 0.0291 0.8529 0.0366 Uij ? ? H(22) 0.9760 0.0628 0.9145 0.0366 Uij ? ? H(23) 1.0373 0.2478 0.9725 0.0342 Uij ? ? H(24) 1.0697 0.2235 0.8716 0.0342 Uij ? ? H(25) 0.784(6) 0.575(4) 0.562(5) 0.0380 Uij ? ? H(26) 0.839(7) 0.489(5) 0.535(5) 0.0380 Uij ? ? H(27) 1.176(6) 0.386(4) 0.573(5) 0.0380 Uij ? ? H(28) 1.133(8) 0.349(6) 0.640(7) 0.0380 Uij ? ? H(29) 1.158(6) 0.169(5) 0.644(5) 0.0380 Uij ? ? H(30) 1.200(7) 0.089(5) 0.668(6) 0.0380 Uij ? ? H(31) 0.379(7) 0.136(5) 0.357(6) 0.0380 Uij ? ? H(32) 0.283(6) 0.131(4) 0.286(5) 0.0380 Uij ? ? H(33) 0.340(6) 0.177(5) 0.866(5) 0.0380 Uij ? ? H(34) 0.234(7) 0.132(4) 0.796(5) 0.0380 Uij ? ? H(35) 0.692(8) 0.504(5) 0.968(6) 0.0380 Uij ? ? H(36) 0.686(6) 0.568(4) 1.032(5) 0.0380 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0219(5) 0.0219(6) 0.0322(5) 0.0015(4) 0.0067(4) 0.0036(4) Cu(2) 0.0221(5) 0.0221(6) 0.0326(5) -0.0014(4) 0.0068(4) -0.0027(4) O(1) 0.025(3) 0.035(3) 0.047(3) 0.003(2) 0.012(2) 0.003(2) O(2) 0.035(3) 0.029(4) 0.071(4) 0.000(3) 0.019(3) 0.015(3) O(3) 0.038(3) 0.031(4) 0.079(4) -0.001(3) 0.020(3) -0.019(3) O(4) 0.024(3) 0.034(3) 0.040(3) -0.005(2) 0.008(2) -0.006(2) O(5) 0.065(4) 0.027(4) 0.044(3) 0.002(3) 0.012(3) 0.004(3) O(6) 0.066(5) 0.079(6) 0.053(4) -0.036(4) -0.004(4) 0.001(4) O(7) 0.060(5) 0.169(9) 0.066(5) 0.063(6) -0.002(4) -0.025(6) O(8) 0.052(5) 0.040(4) 0.050(4) -0.011(3) 0.002(3) 0.006(3) O(9) 0.040(4) 0.082(5) 0.050(4) -0.030(3) 0.012(3) -0.010(3) O(10) 0.082(5) 0.032(4) 0.043(3) 0.000(4) 0.010(3) -0.001(3) N(1) 0.022(3) 0.021(4) 0.028(3) 0.005(3) 0.002(3) -0.002(2) N(2) 0.029(3) 0.026(4) 0.037(3) 0.006(3) 0.010(3) 0.003(3) N(3) 0.027(3) 0.026(4) 0.039(3) 0.002(3) 0.009(3) 0.008(3) N(4) 0.029(3) 0.026(4) 0.030(3) -0.004(3) 0.005(3) -0.007(3) N(5) 0.031(3) 0.028(4) 0.032(3) 0.001(3) 0.005(3) 0.004(3) N(6) 0.027(3) 0.027(4) 0.033(3) 0.002(3) 0.008(3) -0.004(3) N(7) 0.024(3) 0.026(4) 0.037(3) -0.002(3) 0.004(3) -0.001(3) N(8) 0.023(3) 0.017(4) 0.030(3) -0.004(3) 0.000(3) 0.003(2) C(1) 0.021(4) 0.028(4) 0.019(3) 0.004(3) 0.001(3) 0.004(3) C(2) 0.027(4) 0.022(4) 0.031(4) -0.002(4) 0.002(3) 0.000(3) C(3) 0.033(4) 0.014(4) 0.043(4) 0.003(3) 0.010(4) -0.002(3) C(4) 0.030(4) 0.035(5) 0.047(4) 0.013(4) 0.009(4) 0.001(4) C(5) 0.031(4) 0.024(4) 0.024(3) 0.003(3) 0.004(3) 0.002(3) C(6) 0.029(4) 0.026(5) 0.034(4) 0.005(3) 0.005(3) -0.004(3) C(7) 0.033(4) 0.041(5) 0.046(4) -0.013(4) 0.016(4) -0.003(4) C(8) 0.033(4) 0.019(4) 0.043(4) -0.006(3) 0.007(4) -0.007(3) C(9) 0.028(4) 0.027(5) 0.026(3) -0.001(4) 0.002(3) 0.000(3) C(10) 0.024(4) 0.024(4) 0.023(3) 0.003(3) 0.002(3) -0.003(3) C(11) 0.030(4) 0.024(4) 0.026(3) -0.006(3) 0.005(3) 0.000(3) C(12) 0.024(4) 0.026(4) 0.034(4) -0.005(3) 0.003(3) 0.002(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 2.13155 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2612 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0456 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0438 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.527 _refine_ls_shift/esd_max 0.8800 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.71 _refine_diff_density_max 0.51 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(1) 1.995(5) ? ? yes Cu(1) N(2) 1.917(6) ? ? yes Cu(1) N(3) 2.057(6) ? ? yes Cu(1) N(4) 1.981(5) ? ? yes Cu(2) N(5) 1.985(6) ? ? yes Cu(2) N(6) 2.062(6) ? ? yes Cu(2) N(7) 1.915(6) ? ? yes Cu(2) N(8) 2.008(5) ? ? yes O(1) C(1) 1.255(8) ? ? yes O(2) C(2) 1.258(8) ? ? yes O(3) C(9) 1.249(8) ? ? yes O(4) C(10) 1.258(8) ? ? yes N(1) C(1) 1.313(8) ? ? yes N(1) C(5) 1.452(8) ? ? yes N(2) C(2) 1.300(8) ? ? yes N(2) C(3) 1.441(8) ? ? yes N(3) C(4) 1.475(9) ? ? yes N(4) C(12) 1.495(8) ? ? yes N(5) C(6) 1.495(7) ? ? yes N(6) C(7) 1.478(9) ? ? yes N(7) C(8) 1.440(8) ? ? yes N(7) C(9) 1.311(8) ? ? yes N(8) C(10) 1.308(8) ? ? yes N(8) C(11) 1.461(8) ? ? yes C(1) C(2) 1.547(9) ? ? yes C(3) C(4) 1.513(10) ? ? yes C(5) C(6) 1.497(9) ? ? yes C(7) C(8) 1.514(10) ? ? yes C(9) C(10) 1.549(9) ? ? yes C(11) C(12) 1.502(10) ? ? yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(2) 82.6(2) ? ? ? yes N(1) Cu(1) N(3) 162.5(2) ? ? ? yes N(1) Cu(1) N(4) 102.7(2) ? ? ? yes N(2) Cu(1) N(3) 81.5(2) ? ? ? yes N(2) Cu(1) N(4) 174.1(2) ? ? ? yes N(3) Cu(1) N(4) 92.9(2) ? ? ? yes N(5) Cu(2) N(6) 93.5(2) ? ? ? yes N(5) Cu(2) N(7) 174.3(2) ? ? ? yes N(5) Cu(2) N(8) 102.4(2) ? ? ? yes N(6) Cu(2) N(7) 81.2(2) ? ? ? yes N(6) Cu(2) N(8) 162.0(2) ? ? ? yes N(7) Cu(2) N(8) 82.5(2) ? ? ? yes Cu(1) N(1) C(1) 111.8(4) ? ? ? yes Cu(1) N(1) C(5) 130.7(4) ? ? ? yes C(1) N(1) C(5) 115.6(5) ? ? ? yes Cu(1) N(2) C(2) 116.2(5) ? ? ? yes Cu(1) N(2) C(3) 119.0(4) ? ? ? yes C(2) N(2) C(3) 122.8(6) ? ? ? yes Cu(1) N(3) C(4) 107.2(4) ? ? ? yes Cu(1) N(4) C(12) 113.5(4) ? ? ? yes Cu(2) N(5) C(6) 113.7(4) ? ? ? yes Cu(2) N(6) C(7) 107.3(4) ? ? ? yes Cu(2) N(7) C(8) 118.9(4) ? ? ? yes Cu(2) N(7) C(9) 116.5(5) ? ? ? yes C(8) N(7) C(9) 122.7(6) ? ? ? yes Cu(2) N(8) C(10) 111.5(4) ? ? ? yes Cu(2) N(8) C(11) 130.1(4) ? ? ? yes C(10) N(8) C(11) 116.6(5) ? ? ? yes O(1) C(1) N(1) 127.8(6) ? ? ? yes O(1) C(1) C(2) 117.6(6) ? ? ? yes N(1) C(1) C(2) 114.6(5) ? ? ? yes O(2) C(2) N(2) 128.2(7) ? ? ? yes O(2) C(2) C(1) 119.7(6) ? ? ? yes N(2) C(2) C(1) 112.1(6) ? ? ? yes N(2) C(3) C(4) 107.6(5) ? ? ? yes N(3) C(4) C(3) 109.9(5) ? ? ? yes N(1) C(5) C(6) 115.0(5) ? ? ? yes N(5) C(6) C(5) 112.3(5) ? ? ? yes N(6) C(7) C(8) 108.8(5) ? ? ? yes N(7) C(8) C(7) 108.1(5) ? ? ? yes O(3) C(9) N(7) 128.3(7) ? ? ? yes O(3) C(9) C(10) 120.2(6) ? ? ? yes N(7) C(9) C(10) 111.4(6) ? ? ? yes O(4) C(10) N(8) 127.4(6) ? ? ? yes O(4) C(10) C(9) 117.2(6) ? ? ? yes N(8) C(10) C(9) 115.4(6) ? ? ? yes N(8) C(11) C(12) 114.4(5) ? ? ? yes N(4) C(12) C(11) 111.9(5) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END