#------------------------------------------------------------------------------ #$Date: 2008-02-21 19:48:52 +0200 (Thu, 21 Feb 2008) $ #$Revision: 136 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4000321.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_4000321 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_formula_sum 'C20 H27 Br3.50 Cu1.50 N2 O2.50' _chemical_formula_weight 710.43 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 17.931(3) _cell_length_b 14.611(2) _cell_length_c 9.5135(15) _cell_angle_alpha 90.00 _cell_angle_beta 106.905(3) _cell_angle_gamma 90.00 _cell_volume 2384.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 7.236 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 11453 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.1848 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 33.45 _reflns_number_total 6394 _reflns_number_gt 2129 _reflns_threshold_expression >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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 6394 _refine_ls_number_parameters 268 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1408 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 0.503 _refine_ls_restrained_S_all 0.503 _refine_ls_shift/su_max 0.003 _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 Br4 Br 0.45150(5) 0.36022(7) 0.27288(11) 0.0429(3) Uani 1 1 d . . . Br3 Br 0.5000 0.15997(10) 0.0000 0.0422(4) Uani 1 2 d S . . Br2 Br 0.66015(5) 0.34785(7) 0.16824(11) 0.0431(2) Uani 1 1 d . . . Br1 Br 0.60432(6) 0.17084(8) 0.44614(12) 0.0606(4) Uani 1 1 d . . . Cu2 Cu 0.55174(6) 0.26338(11) 0.21484(14) 0.0540(4) Uani 1 1 d . . . Cu1 Cu 0.5000 0.25662(17) 0.5000 0.0643(6) Uani 1 2 d S . . N2 N 0.6938(4) 0.1734(6) -0.0414(8) 0.0429(19) Uani 1 1 d . . . H2C H 0.6543 0.2005 -0.0146 0.051 Uiso 1 1 calc R . . C20 C 0.8899(5) 0.0619(10) 0.5490(11) 0.056(3) Uani 1 1 d . . . C19 C 0.8060(5) 0.0740(7) 0.0419(10) 0.047(2) Uani 1 1 d . . . H19A H 0.7901 0.0111 0.0492 0.056 Uiso 1 1 calc R . . H19B H 0.8592 0.0810 0.1039 0.056 Uiso 1 1 calc R . . C18 C 0.8350(5) 0.1096(7) 0.4382(10) 0.042(2) Uani 1 1 d . . . O1 O 0.6577(4) 0.0344(5) 0.1422(8) 0.055(2) Uani 1 1 d . . . H1A H 0.6379 0.0155 0.2040 0.083 Uiso 1 1 calc R . . C17 C 0.7149(5) 0.1008(7) 0.2064(10) 0.039(2) Uani 1 1 d . . . H17A H 0.6901 0.1516 0.2431 0.047 Uiso 1 1 calc R . . C16 C 0.7741(6) -0.0343(9) 0.3542(11) 0.051(3) Uani 1 1 d . . . H16A H 0.7347 -0.0687 0.2911 0.061 Uiso 1 1 calc R . . N1 N 0.8845(6) -0.0330(9) 0.5552(10) 0.068(3) Uani 1 1 d . . . H1B H 0.9188 -0.0624 0.6219 0.081 Uiso 1 1 calc R . . C15 C 0.7328(5) 0.2444(8) -0.1138(11) 0.053(3) Uani 1 1 d . . . H15A H 0.7453 0.2988 -0.0532 0.064 Uiso 1 1 calc R . . H15B H 0.6983 0.2615 -0.2091 0.064 Uiso 1 1 calc R . . C14 C 0.7749(5) 0.0564(7) 0.3351(10) 0.039(2) Uani 1 1 d . . . C13 C 0.7254(6) 0.0648(8) -0.2107(11) 0.065(3) Uani 1 1 d . . . H13A H 0.7238 -0.0015 -0.2129 0.078 Uiso 1 1 calc R . . H13B H 0.7181 0.0865 -0.3101 0.078 Uiso 1 1 calc R . . C12 C 0.7532(4) 0.1378(6) 0.0933(8) 0.036(2) Uani 1 1 d . . . H12A H 0.7851 0.1902 0.1392 0.043 Uiso 1 1 calc R . . C11 C 0.8295(7) -0.0781(8) 0.4638(14) 0.060(3) Uani 1 1 d . . . H11A H 0.8273 -0.1414 0.4724 0.072 Uiso 1 1 calc R . . O2 O 0.9187(7) 0.3352(13) 0.5575(12) 0.139(5) Uani 1 1 d . . . C10 C 0.9570(7) 0.1948(14) 0.6513(13) 0.094(5) Uani 1 1 d . . . H10A H 0.9967 0.2242 0.7221 0.113 Uiso 1 1 calc R . . C9 C 0.8018(6) 0.0957(8) -0.1158(10) 0.056(3) Uani 1 1 d . . . H9A H 0.8439 0.0644 -0.1431 0.067 Uiso 1 1 calc R . . C8 C 0.8390(6) 0.2060(8) 0.4340(13) 0.061(3) Uani 1 1 d . . . H8A H 0.8026 0.2407 0.3651 0.073 Uiso 1 1 calc R . . C7 C 0.8995(8) 0.2447(11) 0.5371(15) 0.079(4) Uani 1 1 d . . . C6 C 0.6604(6) 0.1005(9) -0.1547(11) 0.065(3) Uani 1 1 d . . . H6A H 0.6192 0.1261 -0.2351 0.078 Uiso 1 1 calc R . . H6B H 0.6386 0.0512 -0.1109 0.078 Uiso 1 1 calc R . . C5 C 0.9488(7) 0.1043(12) 0.6472(14) 0.077(4) Uani 1 1 d . . . H5A H 0.9852 0.0690 0.7151 0.093 Uiso 1 1 calc R . . C4 C 0.8757(9) 0.3814(14) 0.469(2) 0.132(8) Uani 1 1 d . . . H4A H 0.8909 0.4444 0.4861 0.197 Uiso 1 1 calc R . . H4B H 0.8237 0.3738 0.4758 0.197 Uiso 1 1 calc R . . H4C H 0.8773 0.3637 0.3727 0.197 Uiso 1 1 calc R . . O1W O 1.0000 0.0135(6) 1.0000 0.036(2) Uani 1 2 d S . . C3 C 0.8088(6) 0.2000(8) -0.1314(11) 0.057(3) Uani 1 1 d . . . H3A H 0.8087 0.2113 -0.2331 0.068 Uiso 1 1 calc R . . C2 C 0.8959(10) 0.3166(12) 0.0216(19) 0.121(6) Uani 1 1 d . . . H2A H 0.8556 0.3589 0.0061 0.145 Uiso 1 1 calc R . . H2B H 0.9457 0.3321 0.0796 0.145 Uiso 1 1 calc R . . C1 C 0.8833(7) 0.2389(11) -0.0356(14) 0.076(4) Uani 1 1 d . . . H1C H 0.9261 0.2000 -0.0156 0.091 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 Br4 0.0357(5) 0.0540(8) 0.0389(6) -0.0016(5) 0.0106(4) 0.0014(5) Br3 0.0399(7) 0.0417(10) 0.0418(9) 0.000 0.0067(7) 0.000 Br2 0.0502(5) 0.0329(5) 0.0516(6) -0.0023(5) 0.0234(4) -0.0008(5) Br1 0.0767(8) 0.0676(9) 0.0455(8) 0.0166(7) 0.0303(6) 0.0295(7) Cu2 0.0533(8) 0.0555(10) 0.0545(9) -0.0045(7) 0.0178(7) -0.0018(7) Cu1 0.0601(11) 0.0672(16) 0.0739(16) 0.000 0.0328(11) 0.000 N2 0.044(4) 0.054(5) 0.035(4) 0.011(4) 0.018(3) 0.026(4) C20 0.036(6) 0.099(11) 0.038(7) 0.003(6) 0.016(5) 0.007(6) C19 0.045(5) 0.047(6) 0.050(6) 0.006(5) 0.018(5) 0.028(5) C18 0.051(5) 0.050(6) 0.029(5) 0.005(4) 0.020(4) 0.011(5) O1 0.049(4) 0.056(5) 0.055(5) 0.022(4) 0.006(4) 0.005(3) C17 0.037(5) 0.042(6) 0.039(6) 0.007(4) 0.013(4) 0.018(4) C16 0.054(6) 0.061(8) 0.039(6) 0.009(5) 0.016(5) 0.018(5) N1 0.071(7) 0.088(9) 0.054(7) 0.034(6) 0.035(6) 0.043(6) C15 0.061(6) 0.055(7) 0.054(6) 0.031(5) 0.033(5) 0.035(5) C14 0.046(5) 0.040(6) 0.044(6) 0.013(4) 0.034(5) 0.012(4) C13 0.084(7) 0.074(8) 0.035(6) -0.014(5) 0.014(6) 0.040(6) C12 0.035(4) 0.052(6) 0.019(4) 0.004(4) 0.005(3) 0.015(4) C11 0.075(8) 0.048(7) 0.062(8) 0.023(6) 0.028(7) 0.022(6) O2 0.107(9) 0.219(18) 0.074(8) 0.006(10) 0.002(6) -0.010(11) C10 0.050(7) 0.185(19) 0.038(7) 0.008(9) -0.003(6) -0.004(9) C9 0.069(6) 0.076(8) 0.028(5) 0.015(5) 0.023(5) 0.041(6) C8 0.067(7) 0.071(9) 0.054(7) -0.015(6) 0.032(6) 0.000(6) C7 0.108(11) 0.076(10) 0.071(10) -0.021(8) 0.055(9) -0.033(9) C6 0.072(7) 0.089(9) 0.030(6) 0.007(6) 0.007(5) 0.032(7) C5 0.071(8) 0.109(12) 0.052(8) 0.012(8) 0.018(7) 0.021(8) C4 0.090(11) 0.142(18) 0.15(2) -0.084(15) 0.008(11) -0.020(11) O1W 0.022(4) 0.051(6) 0.034(5) 0.000 0.006(3) 0.000 C3 0.056(6) 0.081(9) 0.042(6) 0.023(6) 0.026(5) 0.030(6) C2 0.116(13) 0.089(14) 0.134(16) 0.007(11) -0.002(11) -0.002(10) C1 0.085(9) 0.080(10) 0.078(10) 0.028(8) 0.047(8) 0.021(8)