#------------------------------------------------------------------------------ #$Date: 2010-06-03 17:26:40 +0300 (Thu, 03 Jun 2010) $ #$Revision: 1186 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7005088.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_7005088 loop_ _publ_author_name 'Noh, Wontae' 'Girolami, Gregory S.' _publ_section_title ; Rhenium oxohalides: synthesis and crystal structures of ReO3Cl(THF)2, ReOCl4(THF), Re2O3Cl6(THF)2, and Re2O3Cl6(H2O)2. ; _journal_issue 6 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 674 _journal_page_last 679 _journal_year 2007 _chemical_formula_sum 'C4 H8 Cl4 O2 Re' _chemical_formula_weight 416.10 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.089(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 15.220(4) _cell_length_b 7.996(2) _cell_length_c 16.717(7) _cell_measurement_temperature 193(2) _cell_volume 2034.1(11) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1150 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 6260 _diffrn_reflns_theta_full 25.35 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_min 2.44 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 12.951 _exptl_absorpt_correction_T_max 0.675 _exptl_absorpt_correction_T_min 0.156 _exptl_absorpt_correction_type integration _exptl_crystal_density_diffrn 2.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.518 _refine_diff_density_min -2.130 _refine_diff_density_rms 0.242 _refine_ls_extinction_coef 0.00043(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 101 _refine_ls_number_reflns 1850 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0361 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.0789 _reflns_number_gt 1518 _reflns_number_total 1850 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b616495a.txt _[local]_cod_data_source_block f75yface _[local]_cod_cif_authors_sg_H-M I2/a _cod_original_cell_volume 2034.0(11) _cod_database_code 7005088 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' 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 0.628330(16) 0.18404(3) 0.133601(16) 0.02946(15) Uani 1 1 d . . . Cl1 Cl 0.63491(11) 0.4716(2) 0.13684(12) 0.0433(5) Uani 1 1 d . . . Cl2 Cl 0.59924(14) 0.1869(2) 0.26829(11) 0.0433(5) Uani 1 1 d . . . Cl3 Cl 0.58389(12) -0.0911(2) 0.12725(13) 0.0452(5) Uani 1 1 d . . . Cl4 Cl 0.62215(14) 0.1977(2) -0.00396(12) 0.0480(5) Uani 1 1 d . . . O1 O 0.7353(3) 0.1447(7) 0.1420(4) 0.0499(14) Uani 1 1 d . . . O2 O 0.4846(3) 0.2321(6) 0.1230(3) 0.0302(10) Uani 1 1 d . . . C1 C 0.4412(5) 0.3580(10) 0.0703(5) 0.0422(18) Uani 1 1 d . . . H1A H 0.4554 0.4727 0.0888 0.051 Uiso 1 1 calc R . . H1B H 0.4608 0.3454 0.0145 0.051 Uiso 1 1 calc R . . C2 C 0.3461(6) 0.3258(11) 0.0755(6) 0.057(3) Uani 1 1 d . . . H2A H 0.3260 0.2493 0.0323 0.069 Uiso 1 1 calc R . . H2B H 0.3124 0.4314 0.0713 0.069 Uiso 1 1 calc R . . C3 C 0.3347(5) 0.2461(12) 0.1566(5) 0.052(2) Uani 1 1 d . . . H3A H 0.3329 0.3315 0.1994 0.062 Uiso 1 1 calc R . . H3B H 0.2805 0.1778 0.1580 0.062 Uiso 1 1 calc R . . C4 C 0.4154(5) 0.1391(10) 0.1644(5) 0.0441(19) Uani 1 1 d . . . H4A H 0.4317 0.1220 0.2215 0.053 Uiso 1 1 calc R . . H4B H 0.4054 0.0286 0.1391 0.053 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 0.0257(2) 0.0282(2) 0.0344(2) -0.00417(12) -0.00030(12) 0.00015(11) Cl1 0.0396(11) 0.0306(10) 0.0600(12) -0.0026(8) 0.0099(9) -0.0089(7) Cl2 0.0547(13) 0.0434(11) 0.0315(10) 0.0003(8) -0.0055(8) 0.0014(8) Cl3 0.0437(12) 0.0263(9) 0.0654(13) -0.0085(9) -0.0034(9) 0.0021(7) Cl4 0.0472(13) 0.0647(14) 0.0324(10) -0.0074(9) 0.0075(8) 0.0089(9) O1 0.034(3) 0.052(3) 0.064(4) -0.011(3) -0.001(3) 0.005(2) O2 0.026(3) 0.033(2) 0.032(3) 0.005(2) 0.0036(19) -0.001(2) C1 0.032(4) 0.046(4) 0.048(5) 0.014(4) 0.004(3) 0.007(3) C2 0.030(5) 0.080(7) 0.062(6) 0.004(5) -0.006(4) 0.018(4) C3 0.038(5) 0.058(5) 0.061(6) -0.009(5) 0.004(4) -0.004(4) C4 0.034(5) 0.048(4) 0.050(5) 0.007(4) -0.003(4) -0.010(3) 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_3 _geom_angle_publ_flag O1 Re1 O2 179.0(2) . . ? O1 Re1 Cl1 98.34(19) . . ? O2 Re1 Cl1 82.62(13) . . ? O1 Re1 Cl4 96.6(2) . . ? O2 Re1 Cl4 83.72(13) . . ? Cl1 Re1 Cl4 88.69(7) . . ? O1 Re1 Cl2 97.2(2) . . ? O2 Re1 Cl2 82.50(13) . . ? Cl1 Re1 Cl2 88.64(7) . . ? Cl4 Re1 Cl2 166.19(8) . . ? O1 Re1 Cl3 96.28(19) . . ? O2 Re1 Cl3 82.76(13) . . ? Cl1 Re1 Cl3 165.38(6) . . ? Cl4 Re1 Cl3 89.59(7) . . ? Cl2 Re1 Cl3 89.58(7) . . ? C4 O2 C1 107.9(5) . . ? C4 O2 Re1 125.9(4) . . ? C1 O2 Re1 126.2(4) . . ? C2 C1 O2 105.9(6) . . ? C1 C2 C3 104.8(6) . . ? C4 C3 C2 102.2(7) . . ? O2 C4 C3 105.2(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O1 1.662(5) . ? Re1 O2 2.224(4) . ? Re1 Cl1 2.302(2) . ? Re1 Cl4 2.302(2) . ? Re1 Cl2 2.303(2) . ? Re1 Cl3 2.3034(18) . ? O2 C4 1.474(9) . ? O2 C1 1.484(8) . ? C1 C2 1.475(11) . ? C2 C3 1.511(13) . ? C3 C4 1.500(11) . ?