#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/24/2202421.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202421 loop_ _publ_author_name 'Yim, Hing W.' 'Rabinovich, Daniel' 'Lam, Kin-Chung' 'Golen, James A.' 'Rheingold, Arnold L.' _publ_section_title Di-\m-iodo-bis{[methyltris(methylthiomethyl)silane-\k^2^S,S']copper(I)} _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m556 _journal_page_last m558 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Cu2 I2 (C7 H18 S3 Si)2]' _chemical_formula_moiety 'C14 H36 Cu2 I2 S6 Si2' _chemical_formula_sum 'C14 H36 Cu2 I2 S6 Si2' _chemical_formula_weight 833.85 _chemical_name_systematic ; Di-\m-iodo-bis{[methyltris(methylthiomethyl)silane-\k^2^S,S']copper(I)} ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 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 103.3160(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.33720(10) _cell_length_b 12.8346(3) _cell_length_c 13.0991(3) _cell_measurement_reflns_used 540 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 2 _cell_volume 1527.58(5) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _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 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 5836 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.24 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.904 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.5090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_meas none _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.482 _refine_diff_density_min -0.476 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.277 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 2641 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.277 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0420 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0168P)^2^+4.7233P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.0900 _reflns_number_gt 2191 _reflns_number_total 2641 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cf6260.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2202421 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol I1 0.70143(5) 0.42962(4) 0.59848(3) 0.04578(15) Uani d . 1 . . I Cu1 0.45075(9) 0.51598(7) 0.59455(7) 0.0500(2) Uani d . 1 . . Cu S1 0.48949(19) 0.66936(15) 0.69104(14) 0.0502(4) Uani d . 1 . . S S2 0.2840(2) 0.42532(15) 0.66557(14) 0.0530(4) Uani d . 1 . . S S3 0.1436(11) 0.547(4) 0.9347(13) 0.101(7) Uani d P 0.75(10) A 1 S S3A 0.161(5) 0.501(4) 0.925(2) 0.067(9) Uani d P 0.25(10) A 2 S Si1 0.1804(2) 0.63739(18) 0.73139(15) 0.0509(5) Uani d . 1 A . Si C1 0.3058(7) 0.7208(5) 0.6733(5) 0.0496(17) Uani d . 1 . . C H1A 0.2627 0.7289 0.5972 0.059 Uiso calc R 1 . . H H1B 0.3114 0.7909 0.7056 0.059 Uiso calc R 1 . . H C2 0.5673(8) 0.7572(6) 0.6115(6) 0.062(2) Uani d . 1 . . C H2A 0.5871 0.8245 0.6473 0.094 Uiso calc R 1 . . H H2B 0.4978 0.7669 0.5437 0.094 Uiso calc R 1 . . H H2C 0.6595 0.7280 0.6003 0.094 Uiso calc R 1 . . H C3 0.1329(7) 0.5156(6) 0.6507(6) 0.0543(19) Uani d . 1 . . C H3A 0.0494 0.4804 0.6713 0.065 Uiso calc R 1 . . H H3B 0.1004 0.5352 0.5758 0.065 Uiso calc R 1 . . H C4 0.2050(10) 0.3259(7) 0.5734(7) 0.076(3) Uani d . 1 . . C H4A 0.1332 0.2858 0.6012 0.114 Uiso calc R 1 . . H H4B 0.2829 0.2794 0.5617 0.114 Uiso calc R 1 . . H H4C 0.1557 0.3584 0.5068 0.114 Uiso calc R 1 . . H C5 0.2716(8) 0.6007(7) 0.8689(5) 0.058(2) Uani d . 1 . . C H5A 0.3504 0.5493 0.8681 0.070 Uiso calc R 1 A 1 H H5B 0.3175 0.6632 0.9072 0.070 Uiso calc R 1 A 1 H C6 0.2613(12) 0.4897(8) 1.0499(8) 0.092(3) Uani d . 1 . . C H6A 0.2011 0.4525 1.0902 0.139 Uiso calc R 1 A 1 H H6B 0.3172 0.5448 1.0934 0.139 Uiso calc R 1 A 1 H H6C 0.3297 0.4408 1.0286 0.139 Uiso calc R 1 A 1 H C7 0.0083(8) 0.7115(7) 0.7247(7) 0.074(3) Uani d . 1 . . C H7A 0.0306 0.7756 0.7660 0.112 Uiso calc R 1 A . H H7B -0.0606 0.6689 0.7529 0.112 Uiso calc R 1 . . H H7C -0.0361 0.7294 0.6515 0.112 Uiso calc R 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.0369(2) 0.0561(3) 0.0443(2) 0.0061(2) 0.00924(17) 0.0066(2) Cu1 0.0418(5) 0.0545(5) 0.0551(5) 0.0034(4) 0.0144(4) -0.0014(4) S1 0.0426(9) 0.0619(12) 0.0460(10) -0.0022(8) 0.0100(8) -0.0092(9) S2 0.0582(11) 0.0580(11) 0.0462(10) 0.0003(9) 0.0190(8) 0.0041(9) S3 0.074(3) 0.16(2) 0.079(4) -0.011(6) 0.038(3) 0.027(7) S3A 0.068(11) 0.077(19) 0.058(8) -0.015(8) 0.018(7) -0.001(8) Si1 0.0398(10) 0.0707(14) 0.0449(11) 0.0001(9) 0.0152(8) -0.0138(10) C1 0.052(4) 0.052(4) 0.047(4) 0.006(3) 0.015(3) -0.012(3) C2 0.056(5) 0.071(5) 0.062(5) -0.018(4) 0.017(4) -0.012(4) C3 0.037(4) 0.077(5) 0.051(4) -0.008(3) 0.015(3) -0.014(4) C4 0.097(7) 0.061(5) 0.079(6) -0.012(5) 0.040(5) -0.011(4) C5 0.051(4) 0.079(6) 0.047(4) -0.006(4) 0.015(3) -0.011(4) C6 0.109(8) 0.094(7) 0.084(7) -0.011(6) 0.041(6) 0.004(6) C7 0.050(4) 0.101(7) 0.074(6) 0.012(5) 0.016(4) -0.023(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag I1 Cu1 . 2.5796(9) yes I1 Cu1 3_666 2.6916(10) yes Cu1 S2 . 2.304(2) yes Cu1 S1 . 2.322(2) yes Cu1 I1 3_666 2.6916(10) ? Cu1 Cu1 3_666 2.8633(17) yes S1 C2 . 1.798(8) yes S1 C1 . 1.803(7) yes S2 C4 . 1.794(8) yes S2 C3 . 1.801(7) yes S3 C5 . 1.767(13) ? S3 C6 . 1.81(2) ? S3A C6 . 1.69(3) ? S3A C5 . 1.89(3) ? Si1 C7 . 1.853(8) ? Si1 C5 . 1.867(8) ? Si1 C1 . 1.872(7) yes Si1 C3 . 1.882(7) yes C1 H1A . 0.990 ? C1 H1B . 0.990 ? C2 H2A . 0.980 ? C2 H2B . 0.980 ? C2 H2C . 0.980 ? C3 H3A . 0.990 ? C3 H3B . 0.990 ? C4 H4A . 0.980 ? C4 H4B . 0.980 ? C4 H4C . 0.980 ? C5 H5A . 0.990 ? C5 H5B . 0.990 ? C6 H6A . 0.980 ? C6 H6B . 0.980 ? C6 H6C . 0.980 ? C7 H7A . 0.980 ? C7 H7B . 0.980 ? C7 H7C . 0.980 ? 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cu1 I1 Cu1 . 3_666 65.76(3) yes S2 Cu1 S1 . . 104.08(7) yes S2 Cu1 I1 . . 117.98(6) ? S1 Cu1 I1 . . 109.06(5) ? S2 Cu1 I1 . 3_666 104.52(6) ? S1 Cu1 I1 . 3_666 105.89(6) ? I1 Cu1 I1 . 3_666 114.24(3) ? S2 Cu1 Cu1 . 3_666 131.17(7) ? S1 Cu1 Cu1 . 3_666 123.47(7) ? I1 Cu1 Cu1 . 3_666 59.00(3) ? I1 Cu1 Cu1 3_666 3_666 55.24(3) ? C2 S1 C1 . . 101.3(4) ? C2 S1 Cu1 . . 104.4(3) ? C1 S1 Cu1 . . 102.5(2) yes C4 S2 C3 . . 101.2(4) ? C4 S2 Cu1 . . 107.4(3) ? C3 S2 Cu1 . . 102.5(3) yes C5 S3 C6 . . 102.5(7) ? C6 S3A C5 . . 101.8(13) ? C7 Si1 C5 . . 111.9(4) ? C7 Si1 C1 . . 107.7(4) ? C5 Si1 C1 . . 110.4(3) ? C7 Si1 C3 . . 108.1(4) ? C5 Si1 C3 . . 109.2(4) ? C1 Si1 C3 . . 109.6(3) ? S1 C1 Si1 . . 113.8(4) yes S1 C1 H1A . . 108.8 ? Si1 C1 H1A . . 108.8 ? S1 C1 H1B . . 108.8 ? Si1 C1 H1B . . 108.8 ? H1A C1 H1B . . 107.7 ? S1 C2 H2A . . 109.5 ? S1 C2 H2B . . 109.5 ? H2A C2 H2B . . 109.5 ? S1 C2 H2C . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? S2 C3 Si1 . . 113.3(4) yes S2 C3 H3A . . 108.9 ? Si1 C3 H3A . . 108.9 ? S2 C3 H3B . . 108.9 ? Si1 C3 H3B . . 108.9 ? H3A C3 H3B . . 107.7 ? S2 C4 H4A . . 109.5 ? S2 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? S2 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? S3 C5 Si1 . . 111.1(5) ? S3 C5 S3A . . 19.5(6) ? Si1 C5 S3A . . 112.2(10) ? S3 C5 H5A . . 109.4 ? Si1 C5 H5A . . 109.4 ? S3A C5 H5A . . 91.4 ? S3 C5 H5B . . 109.4 ? Si1 C5 H5B . . 109.4 ? S3A C5 H5B . . 124.2 ? H5A C5 H5B . . 108.0 ? S3A C6 S3 . . 20.6(7) ? S3A C6 H6A . . 107.8 ? S3 C6 H6A . . 109.5 ? S3A C6 H6B . . 127.0 ? S3 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? S3A C6 H6C . . 91.7 ? S3 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? Si1 C7 H7A . . 109.5 ? Si1 C7 H7B . . 109.5 ? H7A C7 H7B . . 109.5 ? Si1 C7 H7C . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C1 H1B I1 2_656 0.99 3.15 4.027(6) 149 C2 H2A S2 2_656 0.98 2.79 3.639(8) 146 _cod_database_fobs_code 2202421 _journal_paper_doi 10.1107/S1600536803012947