#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000361.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_5000361 'minor manual editing of SDT2CIF v. 1.1 BETA output' _chemical_formula_sum 'C28 H28.2 Cl1 Cu2 N4 O9.4' _chemical_formula_moiety 'C28 H28.2 Cu2 N4 O5.4 1+, Cl O4 1-' _chemical_formula_weight 733.70 _cell_length_a 7.7392(18) _cell_length_b 34.342(7) _cell_length_c 11.052(3) _cell_angle_alpha 90 _cell_angle_beta 101.774(12) _cell_angle_gamma 90 _cell_volume 2875.5(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 60 _cell_measurement_theta_min 10.84 _cell_measurement_theta_max 17.56 _cell_measurement_temperature 105 _exptl_crystal_colour green _exptl_crystal_description prism _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.6361 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z x,1/2-y,1/2+z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 105 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8373 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_min 3.00976 _diffrn_reflns_theta_max 25.035 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_standards_number 4 _diffrn_standards_decay_% -1.7 _diffrn_standards_interval_count 300 -diffrn_special_details ; 59 reflections suspected of being affected by overlap (due to the 34A axis) were removed from the RAW data file, after an initial data processing run. ; _reflns_number_total 5069 _reflns_number_gt 3236 _reflns_threshold_expression F>3.0\s(F) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source CU Cu 0.263 1.266 'International Tables Vol. IV (1974) Table 2.2B' CL Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 5069 _refine_ls_number_parameters 400 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef -0.00000007(5) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.0553 _refine_ls_goodness_of_fit_ref 1.1265 _refine_ls_shift/su_max 0.1087 _refine_diff_density_max 0.93 _refine_diff_density_min -0.89 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_disorder_group _atom_site_disorder_assembly CU1 CU 0.51771(13) 0.18550(3) 0.97392(8) 0.0333(3) Uani 1 0 . CU2 CU 0.68410(11) 0.09943(3) 0.99362(7) 0.0216(3) Uani 1 0 . N3 N 0.5145(7) 0.24497(18) 0.9766(5) 0.024(2) Uani 1 0 . C4 C 0.6081(9) 0.2681(3) 1.0654(6) 0.032(3) Uani 1 0 . C5 C 0.6191(10) 0.3078(2) 1.0498(7) 0.031(3) Uani 1 0 . C6 C 0.5343(10) 0.3244(2) 0.9413(7) 0.030(3) Uani 1 0 . C7 C 0.4368(9) 0.3014(2) 0.8490(6) 0.027(3) Uani 1 0 . C8 C 0.4291(9) 0.2617(2) 0.8695(6) 0.024(2) Uani 1 0 . C9 C 0.3304(9) 0.2333(3) 0.7784(6) 0.028(3) Uani 1 0 . C10 C 0.2227(10) 0.2460(3) 0.6696(6) 0.029(3) Uani 1 0 . C11 C 0.1360(10) 0.2176(3) 0.5893(6) 0.038(3) Uani 1 0 . C12 C 0.1625(10) 0.1789(3) 0.6190(7) 0.034(3) Uani 1 0 . C13 C 0.2720(10) 0.1682(3) 0.7289(6) 0.030(3) Uani 1 0 . N14 N 0.3553(8) 0.1953(2) 0.8092(5) 0.028(2) Uani 1 0 . C15 C 0.3054(10) 0.1262(3) 0.7610(6) 0.030(3) Uani 1 0 . C16 C 0.4444(10) 0.1088(2) 0.6970(6) 0.032(3) Uani 1 0 . C17 C 0.4901(9) 0.0677(3) 0.7353(6) 0.028(3) Uani 1 0 . C18 C 0.4284(9) 0.0370(3) 0.6559(6) 0.030(3) Uani 1 0 . C19 C 0.4651(10) -0.0006(3) 0.6917(7) 0.031(3) Uani 1 0 . C20 C 0.5657(9) -0.0078(2) 0.8067(7) 0.027(3) Uani 1 0 . C21 C 0.6306(8) 0.0237(2) 0.8834(6) 0.024(2) Uani 1 0 . N22 N 0.5923(7) 0.0607(2) 0.8500(5) 0.026(2) Uani 1 0 . C23 C 0.7423(8) 0.0172(2) 1.0083(6) 0.023(2) Uani 1 0 . C24 C 0.8041(9) -0.0181(3) 1.0541(7) 0.031(3) Uani 1 0 . C25 C 0.9090(10) -0.0210(3) 1.1726(7) 0.032(3) Uani 1 0 . C26 C 0.9456(9) 0.0127(3) 1.2420(7) 0.032(3) Uani 1 0 . C27 C 0.8780(9) 0.0471(3) 1.1913(6) 0.027(3) Uani 1 0 . N28 N 0.7777(7) 0.05017(19) 1.0765(5) 0.023(2) Uani 1 0 . O29 O 0.3356(7) 0.15921(17) 1.0644(4) 0.033(2) Uani 1 0 . C30 C 0.3495(9) 0.1239(2) 1.0977(6) 0.025(2) Uani 1 0 . O31 O 0.4358(6) 0.09855(17) 1.0555(4) 0.0255(17) Uani 1 0 . C32 C 0.2499(10) 0.1109(3) 1.1936(7) 0.037(3) Uani 1 0 . O33 O 0.6826(7) 0.18706(17) 1.1320(4) 0.038(2) Uani 1 0 . C34 C 0.7919(9) 0.1616(2) 1.1830(6) 0.024(3) Uani 1 0 . O35 O 0.8086(6) 0.12806(17) 1.1433(4) 0.0305(19) Uani 1 0 . C36 C 0.9082(9) 0.1743(3) 1.3031(6) 0.029(3) Uani 1 0 . O37 O 0.6753(6) 0.14847(16) 0.9036(4) 0.0256(17) Uani 1 0 . C38 C 0.8624(19) 0.1564(4) 0.8886(10) 0.021(3) Uiso 0.6 0 . C39 C 0.891(2) 0.1992(5) 0.8797(13) 0.041(4) Uiso 0.6 0 . C40 C 0.800(3) 0.1697(7) 0.8876(16) 0.024(4) Uiso 0.4 0 . O41 O 0.803(2) 0.2055(5) 0.8713(13) 0.038(4) Uiso 0.4 0 . C42 C 0.961(3) 0.1453(6) 0.8860(16) 0.027(4) Uiso 0.4 0 . CL43 CL 0.8536(2) 0.41967(6) 1.01623(16) 0.0299(6) Uani 1 0 . O44 O 0.7084(7) 0.40959(18) 0.9164(5) 0.039(2) Uani 1 0 . O45 O 1.0178(7) 0.41262(19) 0.9782(5) 0.043(2) Uani 1 0 . O46 O 0.8465(8) 0.3962(2) 1.1218(5) 0.064(3) Uani 1 0 . O47 O 0.8395(8) 0.4595(2) 1.0461(6) 0.060(3) Uani 1 0 . H1 H 0.668 0.257 1.1409 0.0445 Uiso 1 0 . H2 H 0.6849 0.3234 1.1143 0.0426 Uiso 1 0 . H3 H 0.5419 0.3515 0.9297 0.0431 Uiso 1 0 . H4 H 0.3769 0.3126 0.7735 0.0397 Uiso 1 0 . H5 H 0.2098 0.2731 0.6499 0.0425 Uiso 1 0 . H6 H 0.058 0.2252 0.5147 0.0508 Uiso 1 0 . H7 H 0.1049 0.1594 0.5644 0.0467 Uiso 1 0 . H8 H 0.3446 0.1237 0.848 0.0428 Uiso 1 0 . H9 H 0.198 0.1121 0.7359 0.0428 Uiso 1 0 . H10 H 0.401 0.1094 0.6101 0.0448 Uiso 1 0 . H11 H 0.5487 0.1242 0.7169 0.0448 Uiso 1 0 . H12 H 0.3599 0.0423 0.5759 0.0428 Uiso 1 0 . H13 H 0.4219 -0.0217 0.6377 0.0439 Uiso 1 0 . H14 H 0.5925 -0.0336 0.8339 0.0398 Uiso 1 0 . H15 H 0.7764 -0.0411 1.005 0.0427 Uiso 1 0 . H16 H 0.9533 -0.0455 1.2045 0.0459 Uiso 1 0 . H17 H 1.0175 0.0118 1.3226 0.0448 Uiso 1 0 . H18 H 0.9033 0.0704 1.2391 0.0396 Uiso 1 0 . H19 H 0.1598 0.1296 1.2012 0.0495 Uiso 1 0 . H20 H 0.1904 0.0865 1.1693 0.0495 Uiso 1 0 . H21 H 0.3254 0.1076 1.2712 0.0495 Uiso 1 0 . H22 H 0.9806 0.1526 1.3396 0.0422 Uiso 1 0 . H23 H 0.9851 0.1946 1.2887 0.0422 Uiso 1 0 . H24 H 0.8399 0.1828 1.3599 0.0422 Uiso 1 0 .