#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4000114.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000114 _journal_name_full 'Chemistry of Materials' _journal_year 2002 _chemical_formula_sum 'C26 H33.50 Cl2 Cu N4 O2.75' _chemical_formula_weight 580.51 _symmetry_cell_setting 'Tetragonal' _space_group_IT_number 88 _symmetry_space_group_name_Hall '-I 4ad' _symmetry_space_group_name_H-M 'I 41/a :2' _[local]_cod_cif_authors_sg_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 17.2210(7) _cell_length_b 17.2210(7) _cell_length_c 40.9649(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12148.7(9) _cell_formula_units_Z 16 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5136 _cell_measurement_theta_min 3. _cell_measurement_theta_max 25. _exptl_crystal_description column _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4840 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.894 _exptl_absorpt_correction_T_max 1.000 _diffrn_ambient_temperature 223(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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 2 _diffrn_reflns_number 39109 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 3. _diffrn_reflns_theta_max 25. _reflns_number_total 5328 _reflns_number_observed 3921 _reflns_observed_criterion >2sigma(I) _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^)+(0.0921P)^2^+271.4605P] 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_number_reflns 5328 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1210 _refine_ls_R_factor_obs 0.0991 _refine_ls_wR_factor_all 0.2678 _refine_ls_wR_factor_obs 0.2555 _refine_ls_goodness_of_fit_all 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 1.428 _refine_ls_shift/su_mean 0.022 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 O1W O 0.427(3) 0.560(3) 0.1118(15) 0.21(3) Uiso 0.50 1 d P . . O2W O 0.574(2) 0.606(2) 0.0904(10) 0.209(15) Uiso 0.50 1 d P . . O3W O 0.5000 0.7500 0.100(2) 0.44(5) Uiso 0.50 2 d SP . . O4W O 0.402(3) 0.579(3) 0.1051(14) 0.20(2) Uiso 0.50 1 d P . . O5W O 0.630(4) 0.652(4) 0.0346(18) 0.34(3) Uiso 0.50 1 d P . . O6W O 0.598(4) 0.692(4) 0.0591(17) 0.30(3) Uiso 0.50 1 d P . . Cu1 Cu 0.0000 -0.2500 0.16412(3) 0.0518(5) Uani 1 2 d S . . Cl1 Cl 0.1236(2) -0.14153(14) 0.16360(6) 0.0672(8) Uani 1 1 d . . . Cu2 Cu 0.0000 0.2500 0.22114(3) 0.0201(3) Uani 1 2 d S . . Cl2 Cl 0.10851(9) 0.36147(10) 0.22147(4) 0.0297(4) Uani 1 1 d . . . N1 N -0.0609(5) -0.1898(4) 0.12971(16) 0.0415(17) Uani 1 1 d . . . C11 C -0.1386(6) -0.1838(5) 0.1307(2) 0.048(2) Uani 1 1 d . . . H11 H -0.1648 -0.2084 0.1477 0.058 Uiso 1 1 calc R . . C12 C -0.1813(6) -0.1438(4) 0.1084(2) 0.042(2) Uani 1 1 d . . . H12 H -0.2350 -0.1415 0.1104 0.050 Uiso 1 1 calc R . . C13 C -0.1444(5) -0.1065(5) 0.08261(17) 0.0363(19) Uani 1 1 d . . . C14 C -0.0645(6) -0.1097(5) 0.0818(2) 0.043(2) Uani 1 1 d . . . H14 H -0.0375 -0.0831 0.0656 0.052 Uiso 1 1 calc R . . C15 C -0.0241(6) -0.1517(5) 0.10486(19) 0.041(2) Uani 1 1 d . . . H15 H 0.0297 -0.1543 0.1035 0.049 Uiso 1 1 calc R . . C1A C -0.1918(6) -0.0605(5) 0.0575(2) 0.047(2) Uani 1 1 d . . . H1A1 H -0.2194 -0.0194 0.0688 0.057 Uiso 1 1 calc R . . H1A2 H -0.1563 -0.0364 0.0422 0.057 Uiso 1 1 calc R . . C2A C -0.2498(5) -0.1085(5) 0.0386(2) 0.046(2) Uani 1 1 d . . . H2A1 H -0.2852 -0.1334 0.0537 0.055 Uiso 1 1 calc R . . H2A2 H -0.2226 -0.1489 0.0267 0.055 Uiso 1 1 calc R . . C3A C -0.2961(6) -0.0595(6) 0.0147(2) 0.051(2) Uani 1 1 d . . . H3A1 H -0.3288 -0.0241 0.0269 0.061 Uiso 1 1 calc R . . H3A2 H -0.2603 -0.0286 0.0018 0.061 Uiso 1 1 calc R . . N2 N -0.4370(4) -0.1936(5) -0.05113(16) 0.049(2) Uani 1 1 d . . . C21 C -0.3591(5) -0.1960(6) -0.0523(2) 0.054(2) Uani 1 1 d . . . H21 H -0.3354 -0.2273 -0.0679 0.065 Uiso 1 1 calc R . . C22 C -0.3127(5) -0.1535(7) -0.0311(3) 0.062(3) Uani 1 1 d . . . H22 H -0.2589 -0.1570 -0.0326 0.074 Uiso 1 1 calc R . . C23 C -0.3460(5) -0.1063(6) -0.0079(2) 0.049(2) Uani 1 1 d . . . C24 C -0.4264(6) -0.1049(7) -0.0067(2) 0.058(3) Uani 1 1 d . . . H24 H -0.4515 -0.0734 0.0085 0.070 Uiso 1 1 calc R . . C25 C -0.4696(6) -0.1504(8) -0.0280(2) 0.065(3) Uani 1 1 d . . . H25 H -0.5234 -0.1507 -0.0261 0.078 Uiso 1 1 calc R . . N3 N 0.0580(3) -0.1869(3) 0.00561(13) 0.0226(12) Uani 1 1 d . . . C31 C 0.0616(4) -0.1094(4) 0.00379(16) 0.0242(14) Uani 1 1 d . . . H31 H 0.0336 -0.0847 -0.0126 0.029 Uiso 1 1 calc R . . C32 C 0.1044(4) -0.0642(4) 0.02486(17) 0.0278(15) Uani 1 1 d . . . H32 H 0.1050 -0.0105 0.0224 0.033 Uiso 1 1 calc R . . C33 C 0.1462(4) -0.0986(4) 0.04958(17) 0.0284(16) Uani 1 1 d . . . C34 C 0.1425(4) -0.1786(4) 0.05222(17) 0.0294(16) Uani 1 1 d . . . H34 H 0.1690 -0.2041 0.0689 0.035 Uiso 1 1 calc R . . C35 C 0.0989(4) -0.2204(4) 0.02978(17) 0.0271(15) Uani 1 1 d . . . H35 H 0.0979 -0.2742 0.0316 0.033 Uiso 1 1 calc R . . C1B C 0.1931(4) -0.0489(5) 0.07300(19) 0.0336(17) Uani 1 1 d . . . H1B1 H 0.2270 -0.0151 0.0605 0.040 Uiso 1 1 calc R . . H1B2 H 0.2255 -0.0823 0.0863 0.040 Uiso 1 1 calc R . . C2B C 0.1417(4) 0.0009(4) 0.09540(16) 0.0245(14) Uani 1 1 d . . . H2B1 H 0.1050 0.0302 0.0823 0.029 Uiso 1 1 calc R . . H2B2 H 0.1124 -0.0325 0.1100 0.029 Uiso 1 1 calc R . . C3B C 0.1912(4) 0.0562(5) 0.11523(18) 0.0308(17) Uani 1 1 d . . . H3B1 H 0.2314 0.0266 0.1262 0.037 Uiso 1 1 calc R . . H3B2 H 0.2166 0.0922 0.1005 0.037 Uiso 1 1 calc R . . N4 N 0.0591(3) 0.1880(3) 0.18574(13) 0.0205(11) Uani 1 1 d . . . C41 C 0.0635(4) 0.1100(4) 0.18757(17) 0.0237(14) Uani 1 1 d . . . H41 H 0.0371 0.0846 0.2042 0.028 Uiso 1 1 calc R . . C42 C 0.1062(4) 0.0664(4) 0.16543(17) 0.0262(15) Uani 1 1 d . . . H42 H 0.1078 0.0126 0.1676 0.031 Uiso 1 1 calc R . . C43 C 0.1464(4) 0.1017(4) 0.14024(17) 0.0235(14) Uani 1 1 d . . . C44 C 0.1412(4) 0.1827(4) 0.13875(16) 0.0274(15) Uani 1 1 d . . . H44 H 0.1665 0.2098 0.1222 0.033 Uiso 1 1 calc R . . C45 C 0.0982(4) 0.2228(4) 0.16197(16) 0.0260(15) Uani 1 1 d . . . H45 H 0.0966 0.2767 0.1608 0.031 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 0.0876(13) 0.0397(9) 0.0280(8) 0.000 0.000 0.0218(8) Cl1 0.113(2) 0.0369(13) 0.0516(15) 0.0011(10) -0.0023(14) 0.0075(13) Cu2 0.0172(6) 0.0279(6) 0.0153(6) 0.000 0.000 0.0084(4) Cl2 0.0179(8) 0.0353(10) 0.0359(10) -0.0027(8) 0.0005(7) -0.0009(6) N1 0.065(5) 0.031(4) 0.029(4) 0.001(3) 0.008(3) 0.011(3) C11 0.064(6) 0.039(5) 0.041(5) -0.003(4) 0.015(4) 0.002(4) C12 0.057(5) 0.027(4) 0.042(5) -0.001(3) 0.005(4) 0.001(4) C13 0.053(5) 0.036(4) 0.019(4) -0.009(3) -0.001(3) -0.009(4) C14 0.059(6) 0.041(5) 0.030(4) 0.002(4) 0.002(4) -0.004(4) C15 0.059(5) 0.038(4) 0.026(4) -0.002(3) 0.005(4) 0.002(4) C1A 0.057(6) 0.042(5) 0.043(5) 0.004(4) -0.012(4) -0.006(4) C2A 0.052(5) 0.052(5) 0.034(4) -0.002(4) 0.000(4) -0.005(4) C3A 0.051(5) 0.061(6) 0.041(5) 0.001(4) -0.008(4) -0.007(5) N2 0.036(4) 0.087(6) 0.023(3) -0.002(4) 0.000(3) -0.012(4) C21 0.038(5) 0.080(7) 0.044(5) -0.007(5) -0.002(4) 0.000(5) C22 0.026(4) 0.095(8) 0.064(7) -0.010(6) -0.001(4) -0.005(5) C23 0.045(5) 0.065(6) 0.037(5) 0.011(4) -0.006(4) -0.006(4) C24 0.046(5) 0.087(8) 0.043(5) -0.012(5) -0.003(4) 0.012(5) C25 0.039(5) 0.120(10) 0.035(5) -0.004(6) 0.001(4) -0.005(6) N3 0.034(3) 0.016(3) 0.018(3) 0.003(2) 0.000(2) -0.002(2) C31 0.031(4) 0.021(3) 0.020(3) 0.000(3) -0.005(3) 0.001(3) C32 0.036(4) 0.020(3) 0.027(4) -0.005(3) -0.004(3) -0.003(3) C33 0.028(4) 0.030(4) 0.027(4) -0.011(3) 0.001(3) 0.002(3) C34 0.042(4) 0.028(4) 0.018(3) -0.001(3) -0.006(3) 0.003(3) C35 0.041(4) 0.016(3) 0.024(4) 0.001(3) -0.003(3) 0.001(3) C1B 0.030(4) 0.038(4) 0.033(4) -0.018(3) -0.006(3) 0.005(3) C2B 0.024(3) 0.027(4) 0.022(3) -0.005(3) -0.002(3) 0.001(3) C3B 0.023(4) 0.041(4) 0.029(4) -0.018(3) 0.003(3) -0.006(3) N4 0.018(3) 0.024(3) 0.019(3) 0.003(2) 0.002(2) 0.001(2) C41 0.027(4) 0.020(3) 0.024(3) 0.001(3) 0.005(3) 0.005(3) C42 0.024(4) 0.024(4) 0.030(4) -0.001(3) 0.002(3) 0.000(3) C43 0.016(3) 0.027(4) 0.027(4) -0.012(3) -0.001(3) 0.006(3) C44 0.035(4) 0.029(4) 0.018(3) -0.003(3) 0.000(3) -0.006(3) C45 0.031(4) 0.021(3) 0.026(4) -0.003(3) -0.001(3) 0.003(3)