#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100747.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_1100747 _publ_requested_journal 'Inorganic Chemistry' _chemical_formula_sum 'C22 H12 Br Cl N4 O4 Re' _chemical_formula_weight 697.92 _symmetry_cell_setting Monoclinic _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.506(5) _cell_length_b 18.043(5) _cell_length_c 13.320(5) _cell_angle_alpha 90.000 _cell_angle_beta 114.936(5) _cell_angle_gamma 90.000 _cell_volume 4251(2) _cell_formula_units_Z 8 _cell_measurement_temperature 164(2) _cell_measurement_reflns_used 9837 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.51 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 7.762 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.709676 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (Bruker, 1997)' _diffrn_ambient_temperature 164(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_number 26269 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.54 _diffrn_reflns_theta_full 26.54 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 4381 _reflns_number_gt 3956 _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^)+(0.0411P)^2^+40.1104P] 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_number_reflns 4381 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.203 _refine_diff_density_min -1.684 _refine_diff_density_rms 0.134 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 0 '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 0.006 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Re1 Re 0.656870(10) 0.154175(10) 0.580330(16) 0.02564(8) Uani 1 1 d . . . Br1 Br 1.26297(6) -0.10104(8) 1.06764(9) 0.0443(4) Uani 0.501(2) 1 d P A 1 Br1A Br 1.17956(9) -0.23632(9) 1.02240(13) 0.0662(6) Uani 0.499(2) 1 d P A 2 Cl1 Cl 0.69696(9) 0.10626(7) 0.44017(11) 0.0382(3) Uani 1 1 d . . . N2 N 0.7769(2) 0.1700(2) 0.6792(3) 0.0238(8) Uani 1 1 d . . . C300 C 0.5538(3) 0.1330(3) 0.4888(6) 0.0441(15) Uani 1 1 d . . . C3 C 0.7672(3) -0.0910(3) 0.7238(4) 0.0312(11) Uani 1 1 d . . . H3 H 0.7898 -0.137 0.7467 0.037 Uiso 1 1 calc R . . C6 C 0.8167(3) 0.1079(3) 0.7227(4) 0.0235(9) Uani 1 1 d . . . C100 C 0.6356(3) 0.2527(3) 0.5228(4) 0.0301(11) Uani 1 1 d . . . N1 N 0.6984(2) 0.0460(2) 0.6512(3) 0.0249(8) Uani 1 1 d . . . N3 N 1.0084(2) 0.0420(3) 0.8774(3) 0.0285(9) Uani 1 1 d . A . N4 N 0.9273(2) -0.0933(3) 0.8293(4) 0.0315(9) Uani 1 1 d . . . C4 C 0.8111(3) -0.0272(3) 0.7429(4) 0.0250(10) Uani 1 1 d . . . C7 C 0.8950(3) 0.1086(3) 0.7828(4) 0.0256(10) Uani 1 1 d . . . C10 C 0.8131(3) 0.2340(3) 0.6954(4) 0.0311(11) Uani 1 1 d . . . H10 H 0.7857 0.2769 0.6654 0.037 Uiso 1 1 calc R . . C11 C 0.9342(3) 0.0393(3) 0.8228(4) 0.0266(10) Uani 1 1 d . . . C9 C 0.8914(3) 0.2389(3) 0.7565(5) 0.0351(12) Uani 1 1 d . . . H9 H 0.9156 0.2846 0.7665 0.042 Uiso 1 1 calc R . . C13 C 1.0039(3) -0.0911(3) 0.8829(4) 0.0339(12) Uani 1 1 d . A . C200 C 0.6287(4) 0.1859(3) 0.6939(6) 0.0436(14) Uani 1 1 d . . . C2 C 0.6904(3) -0.0847(3) 0.6708(5) 0.0373(13) Uani 1 1 d . . . H2 H 0.66 -0.1265 0.6582 0.045 Uiso 1 1 calc R . . O3 O 0.4914(2) 0.1209(3) 0.4307(5) 0.0685(16) Uani 1 1 d . . . C16 C 1.1601(3) -0.0903(4) 0.9951(5) 0.0476(17) Uani 1 1 d . . . O1 O 0.6229(2) 0.3118(2) 0.4898(4) 0.0399(9) Uani 1 1 d . . . C8 C 0.9319(3) 0.1770(3) 0.8008(4) 0.0314(11) Uani 1 1 d . . . H8 H 0.9838 0.1799 0.8429 0.038 Uiso 1 1 calc R . . C1 C 0.6579(3) -0.0155(3) 0.6359(4) 0.0314(11) Uani 1 1 d . . . H1 H 0.6055 -0.0122 0.6002 0.038 Uiso 1 1 calc R . . C15 C 1.1203(4) -0.1577(4) 0.9683(6) 0.0523(18) Uani 1 1 d . A . C17 C 1.1237(3) -0.0243(4) 0.9661(4) 0.0384(13) Uani 1 1 d . A . H17 H 1.1508 0.0199 0.9839 0.046 Uiso 1 1 calc R . . O2 O 0.6084(4) 0.2074(3) 0.7563(5) 0.0702(16) Uani 1 1 d . . . C12 C 0.8931(3) -0.0287(3) 0.8000(4) 0.0241(9) Uani 1 1 d . . . C18 C 1.0440(3) -0.0237(3) 0.9084(4) 0.0319(11) Uani 1 1 d . . . C5 C 0.7743(3) 0.0399(3) 0.7051(4) 0.0227(9) Uani 1 1 d . . . C14 C 1.0440(4) -0.1583(4) 0.9132(5) 0.0450(15) Uani 1 1 d . . . H14 H 1.0182 -0.2032 0.8954 0.054 Uiso 1 1 calc R A . O4 O 0.53070(19) -0.0542(2) 0.3695(2) 0.0268(7) Uani 1 1 d . . . H4 H 0.5488 -0.0955 0.3901 0.04 Uiso 1 1 calc R . . C19 C 0.5659(7) -0.0218(6) 0.3155(9) 0.109(5) Uani 1 1 d . . . H19A H 0.6011 0.0141 0.3628 0.164 Uiso 1 1 calc R . . H19B H 0.5295 0.0025 0.2509 0.164 Uiso 1 1 calc R . . H19C H 0.5926 -0.0585 0.2937 0.164 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 Re1 0.01763(11) 0.02622(12) 0.02963(13) 0.00241(7) 0.00663(8) -0.00129(7) Br1 0.0238(5) 0.0731(9) 0.0316(6) 0.0084(5) 0.0075(4) 0.0153(5) Br1A 0.0549(9) 0.0684(10) 0.0531(9) -0.0035(7) 0.0012(6) 0.0380(7) Cl1 0.0509(8) 0.0319(6) 0.0329(7) 0.0014(5) 0.0187(6) -0.0021(6) N2 0.0206(19) 0.026(2) 0.023(2) -0.0015(16) 0.0081(16) -0.0027(16) C300 0.027(3) 0.035(3) 0.059(4) 0.015(3) 0.007(3) 0.000(2) C3 0.030(3) 0.027(2) 0.033(3) 0.007(2) 0.010(2) -0.003(2) C6 0.021(2) 0.030(2) 0.020(2) -0.0024(18) 0.0091(18) -0.0049(18) C100 0.018(2) 0.036(3) 0.032(3) 0.001(2) 0.0055(19) -0.001(2) N1 0.0183(18) 0.030(2) 0.024(2) 0.0036(16) 0.0060(15) -0.0027(16) N3 0.0192(19) 0.046(3) 0.0195(19) 0.0039(18) 0.0071(16) -0.0006(18) N4 0.027(2) 0.041(2) 0.025(2) 0.0052(18) 0.0104(18) 0.0044(19) C4 0.021(2) 0.033(3) 0.021(2) 0.0051(19) 0.0086(18) -0.0020(19) C7 0.020(2) 0.035(3) 0.021(2) -0.0015(19) 0.0078(18) -0.0045(19) C10 0.030(2) 0.027(2) 0.035(3) -0.003(2) 0.012(2) -0.006(2) C11 0.021(2) 0.041(3) 0.019(2) -0.002(2) 0.0092(18) -0.002(2) C9 0.032(3) 0.032(3) 0.038(3) -0.005(2) 0.012(2) -0.011(2) C13 0.026(2) 0.052(3) 0.025(2) 0.009(2) 0.012(2) 0.010(2) C200 0.044(3) 0.038(3) 0.062(4) 0.008(3) 0.036(3) 0.007(3) C2 0.027(3) 0.035(3) 0.039(3) 0.010(2) 0.003(2) -0.010(2) O3 0.023(2) 0.056(3) 0.095(4) 0.018(3) -0.005(2) -0.009(2) C16 0.031(3) 0.085(5) 0.030(3) 0.018(3) 0.017(2) 0.023(3) O1 0.036(2) 0.030(2) 0.049(2) 0.0077(18) 0.0132(18) 0.0082(16) C8 0.021(2) 0.042(3) 0.027(3) -0.005(2) 0.007(2) -0.010(2) C1 0.019(2) 0.036(3) 0.032(3) 0.007(2) 0.003(2) -0.009(2) C15 0.042(3) 0.079(5) 0.038(3) 0.020(3) 0.019(3) 0.029(3) C17 0.022(2) 0.069(4) 0.023(2) 0.008(3) 0.008(2) 0.006(2) O2 0.092(4) 0.067(3) 0.079(4) 0.006(3) 0.063(4) 0.017(3) C12 0.021(2) 0.033(3) 0.018(2) 0.0049(19) 0.0079(18) 0.0020(19) C18 0.019(2) 0.057(3) 0.021(2) 0.005(2) 0.0108(19) 0.004(2) C5 0.021(2) 0.028(2) 0.019(2) -0.0004(18) 0.0082(17) -0.0060(18) C14 0.040(3) 0.056(4) 0.038(3) 0.016(3) 0.016(3) 0.015(3) O4 0.0300(17) 0.041(2) 0.0071(14) -0.0046(13) 0.0055(13) -0.0209(15) C19 0.175(11) 0.097(7) 0.104(8) -0.057(6) 0.106(8) -0.086(8)