############################################################################## ### ### ### Electronic paper (Acta Crystallographica Section E) ### ### ### ############################################################################## # # # This CIF contains the data in a paper accepted for publication in Acta # # Crystallographica Section E. It conforms to the requirements of Notes # # for Authors for Section E, and has been peer reviewed under the auspices # # of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4. # # # # Software is freely available for graphical display of the structure(s) in # # this CIF. For information consult the CIF home page http://www.iucr.org/ # # cif/home.html # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_I _audit_creation_method SHELXL-97 _chemical_name_systematic ; Diiodidobis(N,N,N',N'-tetramethylthiourea- \kS)cadmium(II) ; _chemical_name_common ? _chemical_formula_moiety 'C10 H24 Cd I2 N4 S2' _chemical_formula_sum 'C10 H24 Cd I2 N4 S2' _chemical_formula_iupac '[Cd I2 (C5 H12 N2 S)2]' _chemical_formula_weight 630.65 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 18.985(5) _cell_length_b 10.395(3) _cell_length_c 13.719(4) _cell_angle_alpha 90.00 _cell_angle_beta 130.740(4) _cell_angle_gamma 90.00 _cell_volume 2051.4(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13642 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.34 _cell_measurement_temperature 294(2) _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.042 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 4.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.3329 _exptl_absorpt_correction_T_max 0.4820 _exptl_special_details ; ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13642 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 28.34 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > \s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 2557 _reflns_number_gt 2235 _reflns_threshold_expression I>2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.0542 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_number_reflns 2557 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+2.9795P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.674 _refine_diff_density_min -0.578 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' 'N' 'N' 0.0061 0.0033 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'SMART (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' loop_ _atom_site_type_symbol _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 Cd Cd1 1.0000 0.71325(3) 0.2500 0.04562(8) Uani d S 1 . . I I1 1.155686(14) 0.56794(2) 0.35345(2) 0.06074(8) Uani d . 1 . . S S1 1.03756(5) 0.84000(9) 0.43960(7) 0.05829(19) Uani d . 1 . . N N1 0.92464(19) 0.7668(2) 0.4801(3) 0.0568(6) Uani d . 1 . . N N2 0.85712(18) 0.8932(3) 0.3011(2) 0.0569(6) Uani d . 1 . . C C1 0.93150(19) 0.8328(3) 0.4031(3) 0.0462(6) Uani d . 1 . . C C2 0.8634(3) 0.8067(4) 0.5045(4) 0.0777(10) Uani d . 1 . . H H2A 0.8343 0.8869 0.4619 0.116 Uiso calc R 1 . . H H2B 0.8992 0.8168 0.5954 0.116 Uiso calc R 1 . . H H2C 0.8165 0.7423 0.4722 0.116 Uiso calc R 1 . . C C3 0.9920(3) 0.6671(4) 0.5676(4) 0.0870(12) Uani d . 1 . . H H3A 1.0154 0.6268 0.5308 0.130 Uiso calc R 1 . . H H3B 0.9622 0.6037 0.5808 0.130 Uiso calc R 1 . . H H3C 1.0425 0.7054 0.6486 0.130 Uiso calc R 1 . . C C4 0.7619(2) 0.8470(4) 0.2310(4) 0.0808(11) Uani d . 1 . . H H4A 0.7637 0.7632 0.2621 0.121 Uiso calc R 1 . . H H4B 0.7299 0.8422 0.1408 0.121 Uiso calc R 1 . . H H4C 0.7297 0.9054 0.2444 0.121 Uiso calc R 1 . . C C5 0.8660(3) 0.9963(4) 0.2369(4) 0.0840(11) Uani d . 1 . . H H5A 0.9259 1.0360 0.2972 0.126 Uiso calc R 1 . . H H5B 0.8184 1.0594 0.2048 0.126 Uiso calc R 1 . . H H5C 0.8594 0.9610 0.1666 0.126 Uiso calc R 1 . . 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 Cd1 0.04989(15) 0.04876(16) 0.04920(15) 0.000 0.03717(13) 0.000 I1 0.05619(12) 0.06315(14) 0.06036(13) 0.01437(9) 0.03692(11) 0.00562(9) S1 0.0509(4) 0.0769(5) 0.0529(4) -0.0122(4) 0.0365(3) -0.0185(4) N1 0.0677(15) 0.0552(14) 0.0648(15) 0.0083(12) 0.0508(14) 0.0065(12) N2 0.0576(14) 0.0651(15) 0.0490(13) 0.0072(12) 0.0352(12) -0.0014(11) C1 0.0517(14) 0.0473(14) 0.0470(13) -0.0003(11) 0.0355(12) -0.0087(11) C2 0.092(3) 0.090(3) 0.091(3) 0.005(2) 0.077(2) 0.003(2) C3 0.109(3) 0.067(2) 0.103(3) 0.025(2) 0.077(3) 0.030(2) C4 0.0502(17) 0.118(3) 0.068(2) 0.0085(19) 0.0360(17) -0.014(2) C5 0.102(3) 0.081(3) 0.064(2) 0.019(2) 0.052(2) 0.0211(19) _geom_special_details ; All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. ; 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 Cd1 S1 . 2.5670(9) ? Cd1 S1 2_755 2.5670(10) ? Cd1 I1 2_755 2.7489(7) ? Cd1 I1 . 2.7489(7) ? S1 C1 . 1.731(3) ? N1 C1 . 1.335(4) ? N1 C2 . 1.465(4) ? N1 C3 . 1.466(4) ? N2 C1 . 1.330(4) ? N2 C5 . 1.464(5) ? N2 C4 . 1.468(4) ? C2 H2A . 0.9600 ? C2 H2B . 0.9600 ? C2 H2C . 0.9600 ? C3 H3A . 0.9600 ? C3 H3B . 0.9600 ? C3 H3C . 0.9600 ? C4 H4A . 0.9600 ? C4 H4B . 0.9600 ? C4 H4C . 0.9600 ? C5 H5A . 0.9600 ? C5 H5B . 0.9600 ? C5 H5C . 0.9600 ? 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 S1 Cd1 S1 . 2_755 118.23(5) ? S1 Cd1 I1 . 2_755 107.41(2) ? S1 Cd1 I1 2_755 2_755 105.36(2) ? S1 Cd1 I1 . . 105.36(2) ? S1 Cd1 I1 2_755 . 107.41(2) ? I1 Cd1 I1 2_755 . 113.34(3) ? C1 S1 Cd1 . . 100.59(9) ? C1 N1 C2 . . 122.5(3) ? C1 N1 C3 . . 121.9(3) ? C2 N1 C3 . . 114.3(3) ? C1 N2 C5 . . 121.3(3) ? C1 N2 C4 . . 122.9(3) ? C5 N2 C4 . . 114.9(3) ? N2 C1 N1 . . 119.4(3) ? N2 C1 S1 . . 121.3(2) ? N1 C1 S1 . . 119.3(2) ? N1 C2 H2A . . 109.5 ? N1 C2 H2B . . 109.5 ? H2A C2 H2B . . 109.5 ? N1 C2 H2C . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? N1 C3 H3A . . 109.5 ? N1 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? N1 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? N2 C4 H4A . . 109.5 ? N2 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? N2 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? N2 C5 H5A . . 109.5 ? N2 C5 H5B . . 109.5 ? H5A C5 H5B . . 109.5 ? N2 C5 H5C . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 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 _geom_hbond_publ_flag C2 H2A N2 . 0.96 2.51 2.859(6) 101 y C4 H4A N1 . 0.96 2.52 2.853(5) 100 y C5 H5A S1 . 0.96 2.66 3.026(5) 103 y data_global _journal_date_recd_electronic 2010-07-05 _journal_date_accepted 2010-07-14 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2010 _journal_volume 66 _journal_issue 8 _journal_page_first m951 _journal_page_last m951 _journal_paper_category QM _journal_coeditor_code WM2373 _publ_contact_author_name 'Saeed Ahmad' _publ_contact_author_address ; Department of Chemistry, University of Engineering and Technology, Lahore 54890, Pakistan ; _publ_contact_author_email 'saeed_a786@hotmail.com' _publ_contact_author_fax '-' _publ_contact_author_phone '+92-333-5248570' _publ_section_title ;\ Diiodidobis(N,N,N',N'-tetramethylthiourea-\ \kS)cadmium(II) ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Nawaz, Sidra' . ; Department of Chemistry, University of Engineering and Technology, Lahore 54890, Pakistan ; 'Sadaf, Sana' . ; Department of Chemistry, University of Engineering and Technology, Lahore 54890, Pakistan ; 'Fettouhi, Mohammed' . ; Department of Chemistry, King Fahd University of Petroleum and Minerals Dhahran 31261, Saudi Arabia ; 'Fazal, Atif' . ; Department of Chemistry, King Fahd University of Petroleum and Minerals Dhahran 31261, Saudi Arabia ; 'Ahmad, Saeed' . ; Department of Chemistry, University of Engineering and Technology, Lahore 54890, Pakistan ;