# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'G Reid' 'Chitra Gurnani' 'W Levason' 'Raju Ratnani' 'Michael Webster' _publ_contact_author_name 'G Reid' _publ_contact_author_email GR@SOTON.AC.UK _publ_section_title ; Synthesis, Characterisation and Structures of Thio-, Seleno- and Telluro-ether Complexes of Gallium(III) ; ############################################################################## ### CIF submission form for molecular structure report ### ### Version: 2.0.2 (6 July 1998). (Updated 20-Apr-2005) ### ############################################################################## # This is an electronic "form" for submitting structural details as a # Crystallographic Information File (CIF). # Full details of the format of such files 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 # www.iucr.org as a pdf file. The current version number is 2.3. # # CIFs can be checked for legal syntax and possible errors (ALERTS) by # using checkcif software. # See the web (http://journals.iucr.org/services/cif/checkcif.html). # The website http://checkcif.iucr.org produces o/p in pdf format. # #============================================================================== data_07mfd030 _database_code_depnum_ccdc_archive 'CCDC 691455' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-02-11 _audit_author_name 'Webster, M.' _chemical_name_systematic ; mu!2$-2,5-dithiahexane-bis(triiodogallium(III)) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Ga2 I6 S2' _chemical_formula_sum 'C4 H10 Ga2 I6 S2' _chemical_formula_structural '(C4 H10 S2) (Ga I3)2' _chemical_formula_weight 1023.08 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** 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' _cell_length_a 11.512(2) _cell_length_b 7.2820(15) _cell_length_c 12.535(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.119(10) _cell_angle_gamma 90.00 _cell_volume 1034.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9070 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 11.734 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5116 # 0.3333 _exptl_absorpt_correction_T_max 0.7456 # 0.5395 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11328 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.55 _reflns_number_total 2378 _reflns_number_gt 2061 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0106P)^2^+2.3210P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2378 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ga1 Ga 0.25186(4) -0.05003(7) 0.82138(4) 0.01770(12) Uani 1 1 d . . . I1 I 0.08865(3) -0.02587(4) 0.65787(2) 0.02593(10) Uani 1 1 d . . . I2 I 0.28932(3) -0.37071(4) 0.89143(3) 0.02888(10) Uani 1 1 d . . . I3 I 0.43203(3) 0.13710(5) 0.81285(3) 0.03058(10) Uani 1 1 d . . . S1 S 0.16127(10) 0.11312(15) 0.95207(9) 0.0179(2) Uani 1 1 d . . . C1 C 0.2572(5) 0.0564(8) 1.0768(4) 0.0301(12) Uani 1 1 d . . . H1A H 0.3298 0.1289 1.0833 0.045 Uiso 1 1 calc R . . H1B H 0.2766 -0.0746 1.0772 0.045 Uiso 1 1 calc R . . H1C H 0.2174 0.0840 1.1379 0.045 Uiso 1 1 calc R . . C2 C 0.0341(4) -0.0329(6) 0.9565(4) 0.0194(10) Uani 1 1 d . . . H2A H -0.0186 -0.0313 0.8850 0.023 Uiso 1 1 calc R . . H2B H 0.0607 -0.1609 0.9722 0.023 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 Ga1 0.0177(3) 0.0170(3) 0.0200(3) -0.0004(2) 0.0074(2) 0.0016(2) I1 0.02930(19) 0.02793(18) 0.01949(17) -0.00189(13) 0.00134(13) -0.00157(14) I2 0.0359(2) 0.01668(17) 0.0371(2) 0.00379(13) 0.01466(16) 0.00546(14) I3 0.01663(18) 0.02514(19) 0.0513(2) 0.00786(15) 0.00971(15) 0.00079(13) S1 0.0184(6) 0.0172(6) 0.0187(6) -0.0010(4) 0.0050(5) 0.0016(5) C1 0.026(3) 0.039(3) 0.023(3) -0.005(2) -0.001(2) 0.008(2) C2 0.020(2) 0.023(2) 0.017(2) 0.0000(19) 0.0081(19) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ga1 S1 2.4048(12) . ? Ga1 I3 2.4997(7) . ? Ga1 I2 2.5054(7) . ? Ga1 I1 2.5316(7) . ? S1 C1 1.796(5) . ? S1 C2 1.819(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C2 1.528(8) 3_557 ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? 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 S1 Ga1 I3 102.84(4) . . ? S1 Ga1 I2 106.87(3) . . ? I3 Ga1 I2 115.47(2) . . ? S1 Ga1 I1 99.68(4) . . ? I3 Ga1 I1 115.52(2) . . ? I2 Ga1 I1 113.96(2) . . ? C1 S1 C2 102.4(2) . . ? C1 S1 Ga1 101.86(17) . . ? C2 S1 Ga1 100.37(15) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C2 S1 110.8(4) 3_557 . ? C2 C2 H2A 109.5 3_557 . ? S1 C2 H2A 109.5 . . ? C2 C2 H2B 109.5 3_557 . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.900 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.194 #===END OF CIF ============================================================== # 07mfd028b.cif data_07mfd028 _database_code_depnum_ccdc_archive 'CCDC 691456' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-02-15 _audit_author_name 'Webster, M.' _chemical_name_systematic ; mu!2$-(1,2-bis(phenylthio)ethane-S,S')bis(trichlorogallium(III)) dichloromethane solvate ; # Treatment of CH2Cl2 Model 2 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H14 Cl6 Ga2 S2, 1.25(C H2 Cl2)' _chemical_formula_sum 'C15.25 H16.50 Cl8.50 Ga2 S2' _chemical_formula_structural '((C14 H14 S2) (Cl3 Ga)2) (C H2 Cl2)1.25' _chemical_formula_weight 704.67 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' S S 0.1246 0.1234 '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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2595(10) _cell_length_b 10.370(2) _cell_length_c 10.453(2) _cell_angle_alpha 67.600(10) _cell_angle_beta 79.605(10) _cell_angle_gamma 71.498(10) _cell_volume 688.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13911 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 347 _exptl_absorpt_coefficient_mu 2.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6648 # 0.6017 _exptl_absorpt_correction_T_max 0.7456 # 0.6605 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14813 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.60 _reflns_number_total 3172 _reflns_number_gt 2640 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+1.9107P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3172 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Ga1 Ga 0.29503(6) 0.79596(4) 0.91270(4) 0.02388(15) Uani 1 1 d . . . Cl1 Cl 0.46738(15) 0.68855(11) 0.77344(11) 0.0311(2) Uani 1 1 d . . . Cl2 Cl 0.17999(15) 1.02703(10) 0.82519(11) 0.0304(2) Uani 1 1 d . . . Cl3 Cl 0.43106(18) 0.72471(12) 1.10358(12) 0.0391(3) Uani 1 1 d . . . S1 S 0.00310(14) 0.71998(10) 0.97344(10) 0.0247(2) Uani 1 1 d . . . C1 C -0.1092(6) 0.8153(4) 0.8119(4) 0.0275(9) Uani 1 1 d . . . C2 C -0.0442(6) 0.7752(5) 0.6962(5) 0.0327(9) Uani 1 1 d . . . H2 H 0.0587 0.6900 0.7008 0.039 Uiso 1 1 calc R . . C3 C -0.1332(7) 0.8627(6) 0.5726(5) 0.0393(11) Uani 1 1 d . . . H3 H -0.0930 0.8355 0.4927 0.047 Uiso 1 1 calc R . . C4 C -0.2786(7) 0.9882(5) 0.5653(5) 0.0439(13) Uani 1 1 d . . . H4 H -0.3355 1.0484 0.4798 0.053 Uiso 1 1 calc R . . C5 C -0.3424(7) 1.0272(5) 0.6826(6) 0.0418(12) Uani 1 1 d . . . H5 H -0.4434 1.1135 0.6772 0.050 Uiso 1 1 calc R . . C6 C -0.2590(6) 0.9401(4) 0.8075(5) 0.0329(10) Uani 1 1 d . . . H6 H -0.3032 0.9652 0.8884 0.040 Uiso 1 1 calc R . . C7 C 0.0850(3) 0.5322(2) 0.9847(2) 0.0257(8) Uani 1 1 d . . . H7A H 0.1553 0.5256 0.8960 0.031 Uiso 1 1 calc R . . H7B H 0.1767 0.4759 1.0589 0.031 Uiso 1 1 calc R . . Cl4 Cl 0.2652(3) 0.4225(2) 0.6421(2) 0.0620(8) Uani 0.50 1 d PR . . Cl5 Cl 0.0606(3) 0.5935(2) 0.3982(2) 0.0757(19) Uiso 0.25 1 d PR . . Cl6 Cl 0.1147(3) 0.4080(2) 0.6534(2) 0.062(2) Uiso 0.15 1 d PR . . Cl7 Cl -0.0778(3) 0.5373(2) 0.4497(2) 0.067(3) Uiso 0.15 1 d PR . . Cl8 Cl 0.2217(3) 0.5925(2) 0.4593(2) 0.054(3) Uiso 0.10 1 d PR . . Cl9 Cl 0.4351(3) 0.5257(2) 0.5519(2) 0.061(4) Uiso 0.10 1 d PR . . 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 Ga1 0.0257(2) 0.0161(2) 0.0272(3) 0.00007(17) -0.00791(17) -0.00815(17) Cl1 0.0260(5) 0.0267(5) 0.0380(6) -0.0078(4) -0.0011(4) -0.0083(4) Cl2 0.0335(5) 0.0157(4) 0.0363(5) 0.0003(4) -0.0075(4) -0.0081(4) Cl3 0.0505(7) 0.0292(5) 0.0332(6) -0.0011(4) -0.0198(5) -0.0079(5) S1 0.0242(5) 0.0150(4) 0.0301(5) -0.0010(4) -0.0030(4) -0.0067(4) C1 0.0236(19) 0.0170(18) 0.034(2) 0.0033(16) -0.0058(16) -0.0084(15) C2 0.029(2) 0.027(2) 0.035(2) 0.0001(18) -0.0048(18) -0.0100(17) C3 0.039(3) 0.047(3) 0.031(2) 0.001(2) -0.0092(19) -0.022(2) C4 0.034(2) 0.037(3) 0.045(3) 0.017(2) -0.020(2) -0.019(2) C5 0.027(2) 0.022(2) 0.065(3) 0.006(2) -0.016(2) -0.0090(17) C6 0.025(2) 0.022(2) 0.049(3) -0.0051(19) -0.0070(18) -0.0091(16) C7 0.0236(19) 0.0138(17) 0.034(2) -0.0001(15) -0.0056(16) -0.0063(15) Cl4 0.0442(15) 0.0496(16) 0.081(2) -0.0216(15) 0.0177(14) -0.0110(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ga1 Cl2 2.1473(11) . ? Ga1 Cl1 2.1492(12) . ? Ga1 Cl3 2.1509(12) . ? Ga1 S1 2.3892(11) . ? S1 C1 1.791(4) . ? S1 C7 1.810(2) . ? C1 C2 1.382(7) . ? C1 C6 1.393(6) . ? C2 C3 1.395(6) . ? C2 H2 0.9500 . ? C3 C4 1.376(8) . ? C3 H3 0.9500 . ? C4 C5 1.391(8) . ? C4 H4 0.9500 . ? C5 C6 1.388(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C7 1.513(4) 2_567 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? Cl4 Cl6 1.1289 . ? Cl4 Cl7 1.659(5) 2_566 ? Cl4 Cl9 1.7901 . ? Cl4 Cl8 2.0386 . ? Cl5 Cl7 1.2555 . ? Cl5 Cl8 1.4257 . ? Cl5 Cl6 1.476(5) 2_566 ? Cl5 Cl7 1.644(4) 2_566 ? Cl6 Cl7 1.047(5) 2_566 ? Cl6 Cl5 1.476(5) 2_566 ? Cl6 Cl8 2.4076 . ? Cl6 Cl7 2.4481 . ? Cl7 Cl6 1.047(5) 2_566 ? Cl7 Cl7 1.495(5) 2_566 ? Cl7 Cl5 1.644(4) 2_566 ? Cl7 Cl4 1.659(5) 2_566 ? Cl7 Cl8 1.835(4) 2_566 ? Cl7 Cl8 2.4449 . ? Cl8 Cl9 1.7793 . ? Cl8 Cl7 1.835(4) 2_566 ? Cl8 Cl9 2.406(4) 2_666 ? Cl9 Cl9 1.450(4) 2_666 ? Cl9 Cl8 2.406(4) 2_666 ? 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 Cl2 Ga1 Cl1 116.56(5) . . ? Cl2 Ga1 Cl3 113.72(5) . . ? Cl1 Ga1 Cl3 112.04(5) . . ? Cl2 Ga1 S1 101.16(4) . . ? Cl1 Ga1 S1 105.76(4) . . ? Cl3 Ga1 S1 106.06(5) . . ? C1 S1 C7 104.62(17) . . ? C1 S1 Ga1 99.62(13) . . ? C7 S1 Ga1 103.73(8) . . ? C2 C1 C6 121.8(4) . . ? C2 C1 S1 123.0(3) . . ? C6 C1 S1 115.0(4) . . ? C1 C2 C3 118.4(4) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 120.7(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 120.2(5) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 118.7(5) . . ? C5 C6 H6 120.7 . . ? C1 C6 H6 120.7 . . ? C7 C7 S1 111.0(2) 2_567 . ? C7 C7 H7A 109.4 2_567 . ? S1 C7 H7A 109.4 . . ? C7 C7 H7B 109.4 2_567 . ? S1 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.657 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.124 #===END OF CIF ============================================================== # 08mfd002b.cif data_08mfd002 _database_code_depnum_ccdc_archive 'CCDC 691457' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-02-14 _audit_author_name 'Webster, M.' _chemical_name_systematic ; mu!2$-(1,2-bis(methylthiomethyl)benzene-S,S')bis(trichlorogallium(III)) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H14 Cl6 Ga2 S2' _chemical_formula_sum 'C10 H14 Cl6 Ga2 S2' _chemical_formula_structural '(C10 H14 S2) (Cl3 Ga)2' _chemical_formula_weight 550.47 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' S S 0.1246 0.1234 '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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 # Superceded ** _symmetry_space_group_name_Hall '-C 2yc' # Superceded ** 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 17.329(4) _cell_length_b 10.987(2) _cell_length_c 13.041(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.542(10) _cell_angle_gamma 90.00 _cell_volume 1968.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12813 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 3.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5689 # 0.7535 _exptl_absorpt_correction_T_max 0.7456 # 0.9288 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11721 _diffrn_reflns_av_R_equivalents 0.1033 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.78 _reflns_number_total 2281 _reflns_number_gt 1516 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+5.1095P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2281 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Ga1 Ga 0.63274(4) 0.29771(5) 0.21663(5) 0.01781(18) Uani 1 1 d . . . Cl1 Cl 0.73292(10) 0.16560(12) 0.35769(12) 0.0257(3) Uani 1 1 d . . . Cl2 Cl 0.67769(10) 0.36449(12) 0.10418(12) 0.0239(3) Uani 1 1 d . . . Cl3 Cl 0.48223(10) 0.24323(13) 0.09580(12) 0.0264(3) Uani 1 1 d . . . S1 S 0.63891(10) 0.46670(12) 0.33280(12) 0.0178(3) Uani 1 1 d . . . C1 C 0.7579(4) 0.5323(5) 0.4059(5) 0.0256(13) Uani 1 1 d . . . H1A H 0.8074 0.4845 0.4821 0.038 Uiso 1 1 calc R . . H1B H 0.7590 0.6163 0.4320 0.038 Uiso 1 1 calc R . . H1C H 0.7715 0.5316 0.3432 0.038 Uiso 1 1 calc R . . C2 C 0.5578(4) 0.5693(5) 0.1950(5) 0.0205(12) Uani 1 1 d . . . H2A H 0.5904 0.5930 0.1567 0.025 Uiso 1 1 calc R . . H2B H 0.4977 0.5244 0.1281 0.025 Uiso 1 1 calc R . . C3 C 0.5301(4) 0.6831(4) 0.2303(4) 0.0155(12) Uani 1 1 d . . . C4 C 0.5593(4) 0.7940(5) 0.2137(5) 0.0231(13) Uani 1 1 d . . . H4 H 0.6003 0.7947 0.1883 0.028 Uiso 1 1 calc R . . C5 C 0.5306(4) 0.9040(5) 0.2332(5) 0.0275(14) Uani 1 1 d . . . H5 H 0.5530 0.9787 0.2233 0.033 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 Ga1 0.0176(3) 0.0155(3) 0.0188(3) 0.0013(3) 0.0103(3) 0.0018(3) Cl1 0.0279(8) 0.0225(8) 0.0236(7) 0.0060(6) 0.0141(6) 0.0086(6) Cl2 0.0265(8) 0.0251(8) 0.0249(7) 0.0031(6) 0.0182(7) 0.0018(6) Cl3 0.0194(7) 0.0305(8) 0.0246(7) -0.0047(6) 0.0109(6) -0.0034(6) S1 0.0188(7) 0.0168(7) 0.0185(7) 0.0005(5) 0.0117(6) 0.0011(6) C1 0.027(3) 0.026(3) 0.022(3) 0.000(2) 0.014(3) -0.005(3) C2 0.022(3) 0.018(3) 0.019(3) 0.002(2) 0.011(2) 0.000(2) C3 0.018(3) 0.015(3) 0.008(2) 0.002(2) 0.005(2) 0.000(2) C4 0.016(3) 0.025(3) 0.022(3) 0.006(2) 0.008(2) 0.004(3) C5 0.026(4) 0.015(3) 0.028(3) 0.004(2) 0.010(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ga1 Cl1 2.1478(14) . ? Ga1 Cl3 2.1530(16) . ? Ga1 Cl2 2.1650(15) . ? Ga1 S1 2.3573(15) . ? S1 C1 1.812(6) . ? S1 C2 1.843(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.508(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.386(7) . ? C3 C3 1.416(10) 2_655 ? C4 C5 1.389(7) . ? C4 H4 0.9500 . ? C5 C5 1.371(11) 2_655 ? C5 H5 0.9500 . ? 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 Cl1 Ga1 Cl3 115.18(6) . . ? Cl1 Ga1 Cl2 111.88(6) . . ? Cl3 Ga1 Cl2 111.95(6) . . ? Cl1 Ga1 S1 106.58(5) . . ? Cl3 Ga1 S1 104.46(6) . . ? Cl2 Ga1 S1 105.91(6) . . ? C1 S1 C2 102.5(3) . . ? C1 S1 Ga1 104.06(19) . . ? C2 S1 Ga1 98.40(17) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 113.9(3) . . ? C3 C2 H2A 108.8 . . ? S1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? S1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C3 118.5(3) . 2_655 ? C4 C3 C2 117.8(5) . . ? C3 C3 C2 123.6(3) 2_655 . ? C3 C4 C5 122.1(5) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C5 C5 C4 119.4(3) 2_655 . ? C5 C5 H5 120.3 2_655 . ? C4 C5 H5 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Ga1 S1 C1 70.01(19) . . . . ? Cl3 Ga1 S1 C1 -167.64(18) . . . . ? Cl2 Ga1 S1 C1 -49.28(19) . . . . ? Cl1 Ga1 S1 C2 175.26(19) . . . . ? Cl3 Ga1 S1 C2 -62.39(19) . . . . ? Cl2 Ga1 S1 C2 55.97(19) . . . . ? C1 S1 C2 C3 -83.2(4) . . . . ? Ga1 S1 C2 C3 170.3(4) . . . . ? S1 C2 C3 C4 116.9(4) . . . . ? S1 C2 C3 C3 -68.0(7) . . . 2_655 ? C3 C3 C4 C5 -0.8(8) 2_655 . . . ? C2 C3 C4 C5 174.5(5) . . . . ? C3 C4 C5 C5 -1.6(9) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.78 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.717 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.164 #===END OF CIF ============================================================== # 08cg02a.cif data_08cg02 _database_code_depnum_ccdc_archive 'CCDC 691458' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-04-20 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trichloro(dimethylselenide)gallium(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H6 Cl3 Ga Se' _chemical_formula_sum 'C2 H6 Cl3 Ga Se' _chemical_formula_weight 285.10 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c m' _symmetry_Int_Tables_number 57 # Superceded ** _symmetry_space_group_name_Hall '-P 2c 2b' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 6.2002(15) _cell_length_b 12.596(3) _cell_length_c 10.443(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 815.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1089 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 8.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3396 # 0.2746 _exptl_absorpt_correction_T_max 1.0000 # 0.9179 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7192 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 979 _reflns_number_gt 907 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.8806P] 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_extinction_coef ? _refine_ls_number_reflns 979 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Ga1 Ga 0.05504(6) -0.05671(3) 0.2500 0.01859(12) Uani 1 2 d S . . Se1 Se 0.13454(6) 0.13492(2) 0.2500 0.02160(12) Uani 1 2 d S . . Cl1 Cl -0.29321(13) -0.07385(7) 0.2500 0.02402(19) Uani 1 2 d S . . Cl2 Cl 0.18707(11) -0.12402(5) 0.42341(6) 0.02934(17) Uani 1 1 d . . . C1 C 0.3436(4) 0.1410(2) 0.1112(3) 0.0276(6) Uani 1 1 d . . . H1A H 0.4213 0.2087 0.1148 0.041 Uiso 1 1 calc R . . H1B H 0.2684 0.1351 0.0289 0.041 Uiso 1 1 calc R . . H1C H 0.4462 0.0823 0.1199 0.041 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 Ga1 0.0166(2) 0.01648(19) 0.0227(2) 0.000 0.000 -0.00068(13) Se1 0.0207(2) 0.01535(18) 0.0287(2) 0.000 0.000 0.00041(12) Cl1 0.0170(4) 0.0252(4) 0.0298(4) 0.000 0.000 -0.0012(3) Cl2 0.0275(3) 0.0275(3) 0.0331(4) 0.0101(2) -0.0062(3) -0.0013(2) C1 0.0352(15) 0.0273(13) 0.0204(12) 0.0031(9) 0.0013(11) -0.0075(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ga1 Cl2 2.1606(8) . ? Ga1 Cl2 2.1606(8) 6_556 ? Ga1 Cl1 2.1700(10) . ? Ga1 Se1 2.4637(7) . ? Se1 C1 1.946(3) 6_556 ? Se1 C1 1.946(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? 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 Cl2 Ga1 Cl2 113.89(4) . 6_556 ? Cl2 Ga1 Cl1 109.75(2) . . ? Cl2 Ga1 Cl1 109.75(2) 6_556 . ? Cl2 Ga1 Se1 107.98(2) . . ? Cl2 Ga1 Se1 107.98(2) 6_556 . ? Cl1 Ga1 Se1 107.25(3) . . ? C1 Se1 C1 96.31(17) 6_556 . ? C1 Se1 Ga1 99.90(8) 6_556 . ? C1 Se1 Ga1 99.90(8) . . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Ga1 Se1 C1 12.65(9) . . . 6_556 ? Cl2 Ga1 Se1 C1 -110.91(9) 6_556 . . 6_556 ? Cl1 Ga1 Se1 C1 130.87(8) . . . 6_556 ? Cl2 Ga1 Se1 C1 110.91(9) . . . . ? Cl2 Ga1 Se1 C1 -12.65(9) 6_556 . . . ? Cl1 Ga1 Se1 C1 -130.87(8) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.633 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.102 #===END OF CIF ============================================================== # 08mj24a.cif data_08mj24 _database_code_depnum_ccdc_archive 'CCDC 691459' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-04-28 _audit_author_name 'Webster, M.' _chemical_name_systematic ; (\m~2~-5,8-diselenadodecane-Se,Se')bis(trichlorogallium(III)) ; # Se ligand = 1,2-bis(n-butylselena)ethane ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H22 Cl6 Ga2 Se2' _chemical_formula_sum 'C10 H22 Cl6 Ga2 Se2' _chemical_formula_structural '(C10 H22 Se2) (Ga Cl3)2' _chemical_formula_weight 652.34 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.287(2) _cell_length_b 7.220(3) _cell_length_c 13.008(5) _cell_angle_alpha 85.58(2) _cell_angle_beta 84.83(2) _cell_angle_gamma 65.54(2) _cell_volume 534.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16479 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.026 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 314 _exptl_absorpt_coefficient_mu 6.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5328 # 0.5020 _exptl_absorpt_correction_T_max 0.7456 # 0.8783 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12089 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.65 _reflns_number_total 2454 _reflns_number_gt 1736 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.4407P] 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_extinction_coef ? _refine_ls_number_reflns 2454 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Ga1 Ga 0.74895(9) 0.47112(9) 0.19316(5) 0.01866(17) Uani 1 1 d . . . Cl1 Cl 0.5639(2) 0.7071(2) 0.08073(12) 0.0300(3) Uani 1 1 d . . . Cl2 Cl 0.5782(2) 0.5256(2) 0.34546(11) 0.0291(3) Uani 1 1 d . . . Cl3 Cl 1.1134(2) 0.4233(2) 0.18642(12) 0.0266(3) Uani 1 1 d . . . Se1 Se 0.75237(9) 0.14670(8) 0.14355(4) 0.01846(16) Uani 1 1 d . . . C1 C 0.9846(9) 0.0971(8) 0.0258(4) 0.0204(12) Uani 1 1 d . . . H1A H 0.9317 0.2144 -0.0247 0.024 Uiso 1 1 calc R . . H1B H 1.1362 0.0818 0.0499 0.024 Uiso 1 1 calc R . . C2 C 0.9575(9) -0.0337(8) 0.2489(4) 0.0211(12) Uani 1 1 d . . . H2A H 1.0475 -0.1709 0.2217 0.025 Uiso 1 1 calc R . . H2B H 1.0701 0.0212 0.2658 0.025 Uiso 1 1 calc R . . C3 C 0.8085(9) -0.0481(8) 0.3459(4) 0.0233(12) Uani 1 1 d . . . H3A H 0.7269 0.0883 0.3749 0.028 Uiso 1 1 calc R . . H3B H 0.6881 -0.0924 0.3271 0.028 Uiso 1 1 calc R . . C4 C 0.9551(10) -0.1970(8) 0.4275(4) 0.0250(13) Uani 1 1 d . . . H4A H 1.0772 -0.1538 0.4450 0.030 Uiso 1 1 calc R . . H4B H 1.0348 -0.3337 0.3985 0.030 Uiso 1 1 calc R . . C5 C 0.8102(11) -0.2110(9) 0.5254(5) 0.0294(14) Uani 1 1 d . . . H5A H 0.7256 -0.0751 0.5529 0.044 Uiso 1 1 calc R . . H5B H 0.9138 -0.3019 0.5769 0.044 Uiso 1 1 calc R . . H5C H 0.6977 -0.2649 0.5096 0.044 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 Ga1 0.0173(3) 0.0170(3) 0.0197(3) -0.0021(2) 0.0002(2) -0.0050(2) Cl1 0.0279(7) 0.0258(8) 0.0330(8) 0.0068(6) -0.0073(6) -0.0080(6) Cl2 0.0324(7) 0.0302(8) 0.0237(8) -0.0088(6) 0.0070(6) -0.0123(6) Cl3 0.0193(6) 0.0285(7) 0.0321(8) -0.0040(6) 0.0001(6) -0.0096(6) Se1 0.0179(3) 0.0175(3) 0.0179(3) -0.0025(2) 0.0016(2) -0.0053(2) C1 0.022(3) 0.016(3) 0.019(3) -0.002(2) 0.006(2) -0.004(2) C2 0.021(3) 0.019(3) 0.021(3) -0.002(2) 0.002(2) -0.006(2) C3 0.024(3) 0.019(3) 0.025(3) -0.001(2) 0.000(2) -0.007(2) C4 0.025(3) 0.019(3) 0.023(3) -0.003(2) 0.004(2) -0.001(2) C5 0.036(3) 0.028(3) 0.022(3) 0.005(3) 0.000(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ga1 Cl2 2.1491(17) . ? Ga1 Cl1 2.1624(17) . ? Ga1 Cl3 2.1658(16) . ? Ga1 Se1 2.4683(11) . ? Se1 C1 1.963(5) . ? Se1 C2 1.972(5) . ? C1 C1 1.534(10) 2_755 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.526(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.520(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.520(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? 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 Cl2 Ga1 Cl1 112.47(7) . . ? Cl2 Ga1 Cl3 113.82(6) . . ? Cl1 Ga1 Cl3 110.08(6) . . ? Cl2 Ga1 Se1 106.29(5) . . ? Cl1 Ga1 Se1 108.40(5) . . ? Cl3 Ga1 Se1 105.32(5) . . ? C1 Se1 C2 99.1(2) . . ? C1 Se1 Ga1 97.65(15) . . ? C2 Se1 Ga1 98.00(16) . . ? C1 C1 Se1 109.5(5) 2_755 . ? C1 C1 H1A 109.8 2_755 . ? Se1 C1 H1A 109.8 . . ? C1 C1 H1B 109.8 2_755 . ? Se1 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? C3 C2 Se1 109.4(4) . . ? C3 C2 H2A 109.8 . . ? Se1 C2 H2A 109.8 . . ? C3 C2 H2B 109.8 . . ? Se1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 112.0(4) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 112.8(5) . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Ga1 Se1 C1 -165.17(17) . . . . ? Cl1 Ga1 Se1 C1 73.71(17) . . . . ? Cl3 Ga1 Se1 C1 -44.08(17) . . . . ? Cl2 Ga1 Se1 C2 -64.84(17) . . . . ? Cl1 Ga1 Se1 C2 174.03(16) . . . . ? Cl3 Ga1 Se1 C2 56.25(17) . . . . ? C2 Se1 C1 C1 83.3(5) . . . 2_755 ? Ga1 Se1 C1 C1 -177.3(5) . . . 2_755 ? C1 Se1 C2 C3 -171.2(4) . . . . ? Ga1 Se1 C2 C3 89.6(4) . . . . ? Se1 C2 C3 C4 176.0(4) . . . . ? C2 C3 C4 C5 179.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.682 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.175 #===END OF CIF ============================================================== # 08mfd001a.cif data_08mfd001 _database_code_depnum_ccdc_archive 'CCDC 691460' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-02-13 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 2-methyl-1,3-dihydro-benzo[c]selenophenium tetrachlorogallate(III) ; # Name from Beilstein Crossfire autonom. # Cation name from previous example using ACD/ILAB, but ACD/Ilab Name # Web service at Daresbury currently no longer available. # Unique SMILES string for cation: C[Se+]1Cc2ccccc2C1 # Very similar Te compound found in CSD (refcode: CIZSIN, (1984)) as # [BPh4]- salt. Name: 1-Methyl-3,4-benzo-1-tellura-cyclopentane but # clearly obsolete nomenclature. mw 14-02-2008. _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H11 Se 1+, Cl4 Ga 1-' _chemical_formula_sum 'C9 H11 Cl4 Ga Se' _chemical_formula_weight 409.66 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** 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' _cell_length_a 7.4417(10) _cell_length_b 13.976(3) _cell_length_c 13.527(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.527(10) _cell_angle_gamma 90.00 _cell_volume 1402.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7977 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 5.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7999 # 0.5964 _exptl_absorpt_correction_T_max 1.0000 # 0.7456 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13908 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3224 _reflns_number_gt 2758 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.0000P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3224 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0610 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ga1 Ga 0.90925(3) 0.305722(19) 0.47341(2) 0.01502(9) Uani 1 1 d . . . Cl1 Cl 0.64430(8) 0.37233(4) 0.44769(5) 0.02015(15) Uani 1 1 d . . . Cl2 Cl 0.96409(8) 0.28133(4) 0.63230(4) 0.01959(14) Uani 1 1 d . . . Cl3 Cl 0.90971(9) 0.16731(5) 0.39916(5) 0.02402(15) Uani 1 1 d . . . Cl4 Cl 1.11332(9) 0.39621(5) 0.41612(6) 0.03144(18) Uani 1 1 d . . . Se1 Se 0.38466(3) 0.126971(18) 0.166203(18) 0.01684(8) Uani 1 1 d . . . C1 C 0.6020(3) 0.05152(18) 0.19855(18) 0.0168(5) Uani 1 1 d . . . H1A H 0.6282 0.0102 0.1420 0.020 Uiso 1 1 calc R . . H1B H 0.7069 0.0938 0.2149 0.020 Uiso 1 1 calc R . . C2 C 0.5629(3) -0.00817(16) 0.28699(17) 0.0138(5) Uani 1 1 d . . . C3 C 0.6968(3) -0.05699(18) 0.34489(19) 0.0194(6) Uani 1 1 d . . . H3 H 0.8191 -0.0526 0.3300 0.023 Uiso 1 1 calc R . . C4 C 0.6501(4) -0.11201(19) 0.4243(2) 0.0243(6) Uani 1 1 d . . . H4 H 0.7408 -0.1451 0.4642 0.029 Uiso 1 1 calc R . . C5 C 0.4706(4) -0.11889(19) 0.44562(19) 0.0237(6) Uani 1 1 d . . . H5 H 0.4392 -0.1573 0.4996 0.028 Uiso 1 1 calc R . . C6 C 0.3381(3) -0.07030(18) 0.38896(19) 0.0216(6) Uani 1 1 d . . . H6 H 0.2161 -0.0745 0.4046 0.026 Uiso 1 1 calc R . . C7 C 0.3831(3) -0.01507(17) 0.30879(17) 0.0155(5) Uani 1 1 d . . . C8 C 0.2457(3) 0.03969(18) 0.24367(18) 0.0168(5) Uani 1 1 d . . . H8A H 0.1641 0.0759 0.2844 0.020 Uiso 1 1 calc R . . H8B H 0.1727 -0.0043 0.1995 0.020 Uiso 1 1 calc R . . C9 C 0.4307(4) 0.22303(19) 0.2682(2) 0.0250(6) Uani 1 1 d . . . H9A H 0.4729 0.1919 0.3307 0.037 Uiso 1 1 calc R . . H9B H 0.3194 0.2583 0.2772 0.037 Uiso 1 1 calc R . . H9C H 0.5232 0.2675 0.2484 0.037 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 Ga1 0.01268(15) 0.01859(16) 0.01391(15) -0.00041(11) 0.00179(11) -0.00121(11) Cl1 0.0152(3) 0.0248(3) 0.0202(3) 0.0000(3) 0.0001(3) 0.0029(2) Cl2 0.0196(3) 0.0252(3) 0.0138(3) -0.0019(3) 0.0000(2) -0.0001(3) Cl3 0.0258(3) 0.0259(3) 0.0204(3) -0.0083(3) 0.0024(3) 0.0026(3) Cl4 0.0202(3) 0.0376(4) 0.0370(4) 0.0128(3) 0.0050(3) -0.0087(3) Se1 0.01701(14) 0.02111(15) 0.01221(14) 0.00138(10) 0.00004(10) 0.00114(10) C1 0.0121(11) 0.0201(13) 0.0181(13) 0.0016(11) 0.0004(10) 0.0023(10) C2 0.0169(12) 0.0108(11) 0.0136(12) -0.0036(10) 0.0010(9) -0.0014(10) C3 0.0156(12) 0.0174(13) 0.0250(14) -0.0045(11) -0.0004(11) -0.0003(10) C4 0.0311(16) 0.0175(13) 0.0230(15) -0.0011(11) -0.0065(12) 0.0034(12) C5 0.0333(16) 0.0191(14) 0.0185(14) 0.0041(11) 0.0012(12) -0.0042(12) C6 0.0223(13) 0.0205(14) 0.0229(14) -0.0021(11) 0.0071(11) -0.0043(11) C7 0.0184(12) 0.0139(12) 0.0143(12) -0.0032(10) 0.0021(10) -0.0004(10) C8 0.0132(11) 0.0190(13) 0.0186(13) -0.0023(11) 0.0033(10) -0.0010(10) C9 0.0339(16) 0.0165(13) 0.0236(15) -0.0025(11) -0.0043(12) -0.0003(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ga1 Cl4 2.1661(7) . ? Ga1 Cl3 2.1798(8) . ? Ga1 Cl2 2.1827(8) . ? Ga1 Cl1 2.1833(7) . ? Se1 C9 1.936(3) . ? Se1 C1 1.952(2) . ? Se1 C8 1.956(2) . ? C1 C2 1.506(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.396(3) . ? C2 C3 1.396(3) . ? C3 C4 1.387(4) . ? C3 H3 0.9500 . ? C4 C5 1.392(4) . ? C4 H4 0.9500 . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C6 C7 1.393(3) . ? C6 H6 0.9500 . ? C7 C8 1.505(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? 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 Cl4 Ga1 Cl3 109.07(3) . . ? Cl4 Ga1 Cl2 111.20(3) . . ? Cl3 Ga1 Cl2 107.95(3) . . ? Cl4 Ga1 Cl1 110.11(3) . . ? Cl3 Ga1 Cl1 109.83(3) . . ? Cl2 Ga1 Cl1 108.65(3) . . ? C9 Se1 C1 96.77(11) . . ? C9 Se1 C8 97.01(11) . . ? C1 Se1 C8 90.39(10) . . ? C2 C1 Se1 105.58(15) . . ? C2 C1 H1A 110.6 . . ? Se1 C1 H1A 110.6 . . ? C2 C1 H1B 110.6 . . ? Se1 C1 H1B 110.6 . . ? H1A C1 H1B 108.8 . . ? C7 C2 C3 120.1(2) . . ? C7 C2 C1 117.1(2) . . ? C3 C2 C1 122.9(2) . . ? C4 C3 C2 119.6(2) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.1(2) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.0(2) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 119.7(2) . . ? C6 C7 C8 122.9(2) . . ? C2 C7 C8 117.4(2) . . ? C7 C8 Se1 105.50(16) . . ? C7 C8 H8A 110.6 . . ? Se1 C8 H8A 110.6 . . ? C7 C8 H8B 110.6 . . ? Se1 C8 H8B 110.6 . . ? H8A C8 H8B 108.8 . . ? Se1 C9 H9A 109.5 . . ? Se1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Se1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.465 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.098 #===END OF CIF ============================================================== # 08mj27a.cif data_08mj27 _database_code_depnum_ccdc_archive 'CCDC 691461' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-06-06 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Di-iodo-dimethyl-tellurium ; # See: L. Y. Y. Chan & F. W. B. Einstein, J. Chem. Soc., Dalton Trans., # 1972, 316-3??. (Room temp., alpha polymorph). CSD refcode: DIDMTE. _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H6 I2 Te' _chemical_formula_sum 'C2 H6 I2 Te' _chemical_formula_weight 411.47 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' Te Te -0.5308 1.6751 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_IT_number 15 # New _space_group_name_Hall '-C 2yc' # New 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 7.020(2) _cell_length_b 15.223(5) _cell_length_c 7.574(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.00(2) _cell_angle_gamma 90.00 _cell_volume 801.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5933 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 11.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7474 # 0.5504 _exptl_absorpt_correction_T_max 1.0000 # 0.8954 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5128 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.53 _reflns_number_total 917 _reflns_number_gt 778 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2sigma(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.9700P] 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_extinction_coef ? _refine_ls_number_reflns 917 _refine_ls_number_parameters 25 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Te1 Te 0.5000 0.58416(3) 0.2500 0.02118(14) Uani 1 2 d S . . I1 I 0.21060(6) 0.59099(3) -0.06569(5) 0.03119(14) Uani 1 1 d . . . C1 C 0.6676(9) 0.6767(4) 0.1266(8) 0.0331(14) Uani 1 1 d . . . H1A H 0.5841 0.7091 0.0345 0.040 Uiso 1 1 calc R . . H1B H 0.7668 0.6456 0.0721 0.040 Uiso 1 1 calc R . . H1C H 0.7288 0.7179 0.2165 0.040 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 Te1 0.0216(3) 0.0197(3) 0.0228(3) 0.000 0.0050(2) 0.000 I1 0.0294(2) 0.0330(2) 0.0296(2) -0.00297(15) -0.00142(17) 0.00271(16) C1 0.035(3) 0.031(3) 0.035(3) 0.005(3) 0.009(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Te1 C1 2.132(6) . ? Te1 C1 2.132(6) 2_655 ? Te1 I1 2.9159(9) 2_655 ? Te1 I1 2.9159(9) . ? Te1 I1 3.7383(9) 5_665 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? 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 C1 Te1 C1 97.3(4) . 2_655 ? C1 Te1 I1 88.39(17) . 2_655 ? C1 Te1 I1 88.91(17) 2_655 2_655 ? C1 Te1 I1 88.91(17) . . ? C1 Te1 I1 88.39(17) 2_655 . ? I1 Te1 I1 175.91(2) 2_655 . ? C1 Te1 I1 86.89(18) . 5_665 ? C1 Te1 I1 175.14(18) 2_655 5_665 ? I1 Te1 I1 88.79(2) 2_655 5_665 ? I1 Te1 I1 94.132(19) . 5_665 ? Te1 C1 H1A 109.5 . . ? Te1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Te1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.395 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.190 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================