#------------------------------------------------------------------------------ #$Date: 2009-04-21 15:31:11 +0100 (Tue, 21 Apr 2009) $ #$Revision: 665 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002082.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_2002082 loop_ _publ_author_name 'Clegg, W.' 'Casals, I.' 'Gonz\'alez-Duarte, P.' _publ_section_title ; catena-[Cd{\m-S(CH~2~)~3~NHMe~2~}Br~2~] ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 129 _journal_page_last 130 _journal_volume 49 _journal_year 1993 _chemical_formula_sum 'C5 H13 Br2 Cd N S' _chemical_formula_weight 391.44 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; _cell_angle_alpha 90.00 _cell_angle_beta 96.000(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.9930(10) _cell_length_b 6.8236(6) _cell_length_c 16.398(2) _cell_measurement_reflns_used 32 _cell_measurement_temperature 240.0(10) _cell_measurement_theta_max 12.42 _cell_measurement_theta_min 10.04 _cell_volume 1112.0(2) _computing_cell_refinement 'Stoe DIF4' _computing_data_collection 'Stoe DIF4' _computing_data_reduction 'local programs' _computing_molecular_graphics SHELXTL/PC _computing_publication_material 'local programs' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1992)' _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1990)' _diffrn_ambient_temperature 240.0(10) _diffrn_measurement_device 'Stoe-Siemens diffractometer' _diffrn_measurement_method ; \w/\q scans with on-line profile fitting (Clegg, 1981) ; _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 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 5481 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_min 2.29 _diffrn_standards_decay_% 3 _diffrn_standards_interval_time 60 _diffrn_standards_number 5 _exptl_absorpt_coefficient_mu 9.279 _exptl_absorpt_correction_T_max 0.117 _exptl_absorpt_correction_T_min 0.074 _exptl_absorpt_correction_type 'empirical (SHELXTL/PC; Sheldrick, 1990)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.338 _exptl_crystal_F_000 736 _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.184 _refine_diff_density_min -0.597 _refine_ls_extinction_coef 0.0015(3) _refine_ls_extinction_method 'SHELXL92 (Sheldrick, 1992)' _refine_ls_goodness_of_fit_all 1.132 _refine_ls_goodness_of_fit_obs 1.168 _refine_ls_matrix_type full _refine_ls_number_parameters 94 _refine_ls_number_reflns 1934 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.381 _refine_ls_restrained_S_obs 1.168 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_obs 0.0420 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[s^2^(Fo^2^)+(0.0100P)^2^+24.2500P], where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1412 _refine_ls_wR_factor_obs 0.1102 _reflns_number_observed 1652 _reflns_number_total 1940 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file al1022.cif _[local]_cod_data_source_block al1022_structure_1_of_1 _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C C 0.0033 0.0016 H H 0.0000 0.0000 N N 0.0061 0.0033 S S 0.1246 0.1234 Br Br -0.2901 2.4595 Cd Cd -0.8075 1.2024 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Cd 0.35841(8) 0.52127(11) 0.23959(5) 0.0344(5) Uani d . 1 . Cd Br1 0.49686(13) 0.6731(2) 0.13100(8) 0.0528(7) Uani d . 1 . Br Br2 0.52522(12) 0.2874(2) 0.32915(7) 0.0408(7) Uani d . 1 . Br S 0.1909(3) 0.2932(4) 0.1640(2) 0.0328(14) Uani d . 1 . S N 0.2035(10) -0.1672(15) -0.0891(6) 0.046(6) Uani d . 1 . N H0 0.1262(10) -0.0952(15) -0.1051(6) 0.055 Uiso calc R 1 . H C1 0.2964(11) 0.1765(16) 0.0930(7) 0.038(6) Uani d . 1 . C H1A 0.3370(11) 0.2776(16) 0.0610(7) 0.045 Uiso calc R 1 . H H1B 0.3693(11) 0.1040(16) 0.1242(7) 0.045 Uiso calc R 1 . H C2 0.2154(11) 0.0380(18) 0.0355(6) 0.042(6) Uani d . 1 . C H2A 0.1850(11) -0.0718(18) 0.0673(6) 0.050 Uiso calc R 1 . H H2B 0.1352(11) 0.1069(18) 0.0106(6) 0.050 Uiso calc R 1 . H C3 0.2914(11) -0.0417(17) -0.0316(6) 0.040(6) Uani d . 1 . C H3A 0.3263(11) 0.0673(17) -0.0620(6) 0.048 Uiso calc R 1 . H H3B 0.3681(11) -0.1189(17) -0.0074(6) 0.048 Uiso calc R 1 . H C4 0.1601(15) -0.3495(19) -0.0507(9) 0.063(9) Uani d . 1 . C H4A 0.2389(17) -0.431(6) -0.034(5) 0.075 Uiso calc R 1 . H H4B 0.099(7) -0.422(6) -0.0904(19) 0.075 Uiso calc R 1 . H H4C 0.114(8) -0.317(2) -0.003(3) 0.075 Uiso calc R 1 . H C5 0.2677(16) -0.212(2) -0.1649(7) 0.070(11) Uani d . 1 . C H5A 0.291(8) -0.090(2) -0.191(3) 0.083 Uiso calc R 1 . H H5B 0.205(4) -0.287(12) -0.203(3) 0.083 Uiso calc R 1 . H H5C 0.349(6) -0.290(12) -0.1507(10) 0.083 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 Cd 0.0425(5) 0.0275(4) 0.0331(4) -0.0014(3) 0.0038(3) -0.0002(3) Br1 0.0549(7) 0.0491(8) 0.0564(8) -0.0041(6) 0.0154(6) 0.0187(6) Br2 0.0482(7) 0.0307(6) 0.0430(6) 0.0070(5) 0.0030(5) 0.0053(5) S 0.0386(14) 0.0247(13) 0.0347(13) -0.0003(11) 0.0019(11) -0.0007(11) N 0.050(6) 0.048(6) 0.040(5) 0.017(5) -0.002(4) -0.011(5) C1 0.042(6) 0.030(6) 0.042(6) -0.004(5) 0.002(5) -0.006(5) C2 0.049(6) 0.044(7) 0.034(5) -0.006(6) 0.013(5) -0.003(5) C3 0.048(6) 0.033(6) 0.039(6) -0.002(5) 0.005(5) 0.000(5) C4 0.072(9) 0.038(7) 0.078(9) -0.010(7) 0.007(7) -0.024(7) C5 0.102(11) 0.075(11) 0.032(6) 0.017(9) 0.009(7) -0.021(7) 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 Cd S . 2.515(3) yes Cd S 2 2.520(3) yes Cd Br1 . 2.5834(15) yes Cd Br2 . 2.6400(14) yes S C1 . 1.833(11) yes S Cd 2_545 2.520(3) ? N C4 . 1.479(17) yes N C3 . 1.490(14) yes N C5 . 1.489(15) yes C1 C2 . 1.509(15) yes C2 C3 . 1.503(14) yes 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 S Cd S . 2 126.95(5) yes S Cd Br1 . . 106.57(7) yes S Cd Br1 2 . 106.92(7) yes S Cd Br2 . . 104.43(7) yes S Cd Br2 2 . 104.47(7) yes Br1 Cd Br2 . . 105.86(5) yes C1 S Cd . . 100.7(3) yes C1 S Cd . 2_545 104.0(4) yes Cd S Cd . 2_545 108.08(9) yes C4 N C3 . . 113.2(9) yes C4 N C5 . . 110.6(11) yes C3 N C5 . . 111.7(10) yes C2 C1 S . . 111.3(7) yes C3 C2 C1 . . 113.9(9) yes N C3 C2 . . 111.2(9) yes