Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' #============================================================================== # SUBMISSION DETAILS # ================== _journal_coden_Cambridge 0222 _publ_contact_author_name 'Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3609' _publ_contact_letter ; 23 March 2007 Dear Sirs, This file contains revised details of one of the three crystal structures in CIF format. The compound is [{Me2AsCH2C(Me)(CH2AsMe2)2}GaCl2][GaCl4]. Regards, Gillian Reid ; _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Remarkable structural diversity in gallium(III) complexes of a tripodal triarsine ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # Note order: Family_name, first name(s) or initials (or mixture). loop_ _publ_author_name _publ_author_address F.Cheng ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; A.L.Hector ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; W.Levason ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; G.Reid ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; M.Webster ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; W.Zhang ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; data_06fc033 _database_code_depnum_ccdc_archive 'CCDC 637886' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-02-06 _chemical_name_systematic ; dichlorogallium{1,1,1-tris(dimethylarsinomethyl)ethane}trichlorogallium tetrachlorogallate(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H27 As3 Cl5 Ga2 1+, Cl4 Ga 1-' _chemical_formula_sum 'C11 H27 As3 Cl9 Ga3' _chemical_formula_weight 912.30 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' As As 0.0499 2.0058 '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/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** 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' _cell_length_a 8.2067(15) _cell_length_b 19.623(5) _cell_length_c 18.758(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.321(10) _cell_angle_gamma 90.00 _cell_volume 2996.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6738 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 6.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8058 # 0.4972 _exptl_absorpt_correction_T_max 1.0000 # 0.7735 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. 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_% 0 _diffrn_reflns_number 26144 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.79 _reflns_number_total 6853 _reflns_number_gt 4869 _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^+58.0000P] 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 6853 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1439 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.63692(14) 0.41746(5) 0.19420(6) 0.0299(3) Uani 1 1 d . . . Ga2 Ga 0.46566(12) 0.06061(5) 0.09701(5) 0.0207(2) Uani 1 1 d . . . Ga3 Ga 0.20994(13) 0.71108(6) 0.06094(5) 0.0282(2) Uani 1 1 d . . . Cl1 Cl 0.7248(4) 0.49550(17) 0.12702(18) 0.0595(9) Uani 1 1 d . . . Cl2 Cl 0.5679(4) 0.46151(17) 0.29152(15) 0.0527(8) Uani 1 1 d . . . Cl3 Cl 0.8145(3) 0.33628(13) 0.21624(16) 0.0401(6) Uani 1 1 d . . . Cl4 Cl 0.3287(3) -0.02564(12) 0.14248(11) 0.0269(5) Uani 1 1 d . . . Cl5 Cl 0.6874(3) 0.03539(12) 0.05186(12) 0.0266(5) Uani 1 1 d . . . Cl6 Cl 0.0717(4) 0.62288(17) 0.01834(17) 0.0588(9) Uani 1 1 d . . . Cl7 Cl 0.0598(5) 0.77297(17) 0.12273(16) 0.0621(10) Uani 1 1 d . . . Cl8 Cl 0.4281(3) 0.67936(18) 0.12924(14) 0.0502(8) Uani 1 1 d . . . Cl9 Cl 0.2740(3) 0.77079(14) -0.03028(13) 0.0360(6) Uani 1 1 d . . . As1 As 0.37176(12) 0.38951(5) 0.12303(5) 0.0247(2) Uani 1 1 d . . . As2 As 0.28563(11) 0.13347(5) 0.01675(5) 0.0195(2) Uani 1 1 d . . . As3 As 0.53744(11) 0.13771(5) 0.19816(5) 0.0197(2) Uani 1 1 d . . . C1 C 0.2856(11) 0.2395(4) 0.1358(4) 0.0201(18) Uani 1 1 d . . . C2 C 0.2302(11) 0.3138(4) 0.1457(5) 0.0240(19) Uani 1 1 d . . . H2A H 0.2113 0.3190 0.1965 0.029 Uiso 1 1 calc R . . H2B H 0.1225 0.3197 0.1160 0.029 Uiso 1 1 calc R . . C3 C 0.2837(10) 0.2267(4) 0.0543(5) 0.0212(18) Uani 1 1 d . . . H3A H 0.3801 0.2506 0.0393 0.025 Uiso 1 1 calc R . . H3B H 0.1848 0.2495 0.0295 0.025 Uiso 1 1 calc R . . C4 C 0.4568(10) 0.2301(4) 0.1783(4) 0.0177(17) Uani 1 1 d . . . H4A H 0.4576 0.2538 0.2249 0.021 Uiso 1 1 calc R . . H4B H 0.5368 0.2538 0.1517 0.021 Uiso 1 1 calc R . . C5 C 0.1551(12) 0.1951(5) 0.1650(5) 0.029(2) Uani 1 1 d . . . H5A H 0.1826 0.1469 0.1598 0.044 Uiso 1 1 calc R . . H5B H 0.0473 0.2045 0.1379 0.044 Uiso 1 1 calc R . . H5C H 0.1521 0.2055 0.2159 0.044 Uiso 1 1 calc R . . C6 C 0.2318(15) 0.4661(6) 0.1371(7) 0.050(3) Uani 1 1 d . . . H6A H 0.2852 0.5083 0.1245 0.075 Uiso 1 1 calc R . . H6B H 0.2125 0.4679 0.1875 0.075 Uiso 1 1 calc R . . H6C H 0.1267 0.4609 0.1063 0.075 Uiso 1 1 calc R . . C7 C 0.3894(13) 0.3908(6) 0.0217(5) 0.036(2) Uani 1 1 d . . . H7A H 0.2817 0.3812 -0.0054 0.054 Uiso 1 1 calc R . . H7B H 0.4683 0.3560 0.0108 0.054 Uiso 1 1 calc R . . H7C H 0.4273 0.4358 0.0082 0.054 Uiso 1 1 calc R . . C8 C 0.3510(12) 0.1462(5) -0.0772(5) 0.027(2) Uani 1 1 d . . . H8A H 0.3158 0.1069 -0.1075 0.040 Uiso 1 1 calc R . . H8B H 0.4708 0.1506 -0.0730 0.040 Uiso 1 1 calc R . . H8C H 0.2997 0.1877 -0.0988 0.040 Uiso 1 1 calc R . . C9 C 0.0639(10) 0.0987(5) 0.0045(5) 0.027(2) Uani 1 1 d . . . H9A H -0.0137 0.1367 0.0031 0.040 Uiso 1 1 calc R . . H9B H 0.0486 0.0686 0.0448 0.040 Uiso 1 1 calc R . . H9C H 0.0442 0.0730 -0.0406 0.040 Uiso 1 1 calc R . . C10 C 0.7688(12) 0.1501(5) 0.2251(6) 0.036(2) Uani 1 1 d . . . H10A H 0.7870 0.1829 0.2648 0.055 Uiso 1 1 calc R . . H10B H 0.8185 0.1675 0.1839 0.055 Uiso 1 1 calc R . . H10C H 0.8193 0.1064 0.2404 0.055 Uiso 1 1 calc R . . C11 C 0.4546(13) 0.1075(5) 0.2843(5) 0.034(2) Uani 1 1 d . . . H11A H 0.4959 0.0616 0.2967 0.052 Uiso 1 1 calc R . . H11B H 0.3342 0.1067 0.2763 0.052 Uiso 1 1 calc R . . H11C H 0.4913 0.1388 0.3238 0.052 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 0.0346(6) 0.0237(5) 0.0293(6) -0.0001(4) -0.0040(4) -0.0034(5) Ga2 0.0210(5) 0.0200(5) 0.0211(5) -0.0006(4) 0.0032(4) 0.0004(4) Ga3 0.0244(5) 0.0385(6) 0.0218(5) 0.0044(5) 0.0032(4) 0.0056(5) Cl1 0.065(2) 0.0537(19) 0.0539(18) 0.0219(15) -0.0134(15) -0.0284(16) Cl2 0.064(2) 0.0608(19) 0.0294(13) -0.0106(13) -0.0081(13) 0.0143(16) Cl3 0.0292(13) 0.0331(13) 0.0559(17) -0.0063(12) -0.0029(12) 0.0041(11) Cl4 0.0263(12) 0.0329(12) 0.0219(10) -0.0101(9) 0.0037(9) 0.0022(9) Cl5 0.0224(11) 0.0286(12) 0.0293(11) -0.0044(9) 0.0051(9) 0.0027(9) Cl6 0.071(2) 0.0552(19) 0.0436(16) 0.0089(14) -0.0169(15) -0.0247(17) Cl7 0.086(2) 0.064(2) 0.0430(16) 0.0224(15) 0.0375(16) 0.0444(19) Cl8 0.0339(15) 0.083(2) 0.0314(13) 0.0110(14) -0.0045(11) 0.0116(15) Cl9 0.0313(13) 0.0496(16) 0.0279(12) 0.0089(11) 0.0070(10) 0.0017(11) As1 0.0295(5) 0.0199(5) 0.0237(5) -0.0018(4) -0.0011(4) 0.0032(4) As2 0.0183(4) 0.0206(4) 0.0192(4) -0.0013(4) 0.0010(3) -0.0008(4) As3 0.0195(4) 0.0208(4) 0.0185(4) 0.0004(3) 0.0016(3) 0.0003(4) C1 0.022(4) 0.018(4) 0.020(4) -0.003(3) 0.004(3) 0.000(4) C2 0.019(5) 0.027(5) 0.027(5) -0.001(4) 0.009(4) -0.005(4) C3 0.013(4) 0.023(5) 0.028(5) -0.001(4) 0.005(3) -0.003(3) C4 0.020(4) 0.012(4) 0.020(4) -0.007(3) 0.002(3) 0.002(3) C5 0.034(5) 0.037(6) 0.019(4) -0.002(4) 0.012(4) -0.010(4) C6 0.057(8) 0.030(6) 0.059(8) -0.007(6) -0.012(6) 0.015(5) C7 0.042(6) 0.038(6) 0.025(5) 0.004(4) -0.005(4) -0.007(5) C8 0.034(5) 0.026(5) 0.018(4) -0.002(4) -0.002(4) 0.003(4) C9 0.017(4) 0.023(5) 0.040(5) 0.000(4) 0.003(4) -0.010(4) C10 0.032(6) 0.032(6) 0.042(6) 0.000(5) -0.007(5) -0.005(4) C11 0.047(6) 0.032(5) 0.028(5) 0.006(4) 0.015(5) 0.004(5) _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 2.160(3) . ? Ga1 Cl3 2.163(3) . ? Ga1 Cl1 2.164(3) . ? Ga1 As1 2.4653(15) . ? Ga2 Cl5 2.160(2) . ? Ga2 Cl4 2.258(3) . ? Ga2 As2 2.4346(13) . ? Ga2 As3 2.4394(13) . ? Ga3 Cl8 2.156(3) . ? Ga3 Cl6 2.165(3) . ? Ga3 Cl7 2.168(3) . ? Ga3 Cl9 2.192(3) . ? As1 C7 1.924(10) . ? As1 C6 1.929(11) . ? As1 C2 1.966(8) . ? As2 C8 1.922(9) . ? As2 C9 1.930(8) . ? As2 C3 1.962(9) . ? As3 C10 1.918(10) . ? As3 C11 1.926(9) . ? As3 C4 1.949(8) . ? C1 C5 1.534(12) . ? C1 C4 1.535(11) . ? C1 C2 1.544(12) . ? C1 C3 1.548(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 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 Cl3 112.09(12) . . ? Cl2 Ga1 Cl1 110.58(15) . . ? Cl3 Ga1 Cl1 111.48(14) . . ? Cl2 Ga1 As1 103.79(10) . . ? Cl3 Ga1 As1 117.79(9) . . ? Cl1 Ga1 As1 100.29(9) . . ? Cl5 Ga2 Cl4 117.46(9) . . ? Cl5 Ga2 As2 111.55(8) . . ? Cl4 Ga2 As2 112.44(7) . . ? Cl5 Ga2 As3 108.36(7) . . ? Cl4 Ga2 As3 104.69(7) . . ? As2 Ga2 As3 100.61(5) . . ? Cl8 Ga3 Cl6 110.17(14) . . ? Cl8 Ga3 Cl7 109.23(13) . . ? Cl6 Ga3 Cl7 109.78(16) . . ? Cl8 Ga3 Cl9 110.77(11) . . ? Cl6 Ga3 Cl9 107.79(12) . . ? Cl7 Ga3 Cl9 109.08(12) . . ? C7 As1 C6 104.2(5) . . ? C7 As1 C2 110.2(4) . . ? C6 As1 C2 100.4(5) . . ? C7 As1 Ga1 111.1(3) . . ? C6 As1 Ga1 104.6(4) . . ? C2 As1 Ga1 123.8(3) . . ? C8 As2 C9 107.8(4) . . ? C8 As2 C3 102.9(4) . . ? C9 As2 C3 108.8(4) . . ? C8 As2 Ga2 115.2(3) . . ? C9 As2 Ga2 110.8(3) . . ? C3 As2 Ga2 111.0(3) . . ? C10 As3 C11 105.2(5) . . ? C10 As3 C4 103.5(4) . . ? C11 As3 C4 107.4(4) . . ? C10 As3 Ga2 114.6(3) . . ? C11 As3 Ga2 112.7(3) . . ? C4 As3 Ga2 112.7(2) . . ? C5 C1 C4 112.4(7) . . ? C5 C1 C2 105.3(7) . . ? C4 C1 C2 108.4(7) . . ? C5 C1 C3 109.9(7) . . ? C4 C1 C3 112.7(7) . . ? C2 C1 C3 107.8(7) . . ? C1 C2 As1 119.7(6) . . ? C1 C2 H2A 107.4 . . ? As1 C2 H2A 107.4 . . ? C1 C2 H2B 107.4 . . ? As1 C2 H2B 107.4 . . ? H2A C2 H2B 106.9 . . ? C1 C3 As2 120.5(6) . . ? C1 C3 H3A 107.2 . . ? As2 C3 H3A 107.2 . . ? C1 C3 H3B 107.2 . . ? As2 C3 H3B 107.2 . . ? H3A C3 H3B 106.8 . . ? C1 C4 As3 118.6(6) . . ? C1 C4 H4A 107.7 . . ? As3 C4 H4A 107.7 . . ? C1 C4 H4B 107.7 . . ? As3 C4 H4B 107.7 . . ? H4A C4 H4B 107.1 . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? As1 C6 H6A 109.5 . . ? As1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? As1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? As1 C7 H7A 109.5 . . ? As1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? As1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? As2 C8 H8A 109.5 . . ? As2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? As2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? As2 C9 H9A 109.5 . . ? As2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? As2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? As3 C10 H10A 109.5 . . ? As3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? As3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? As3 C11 H11A 109.5 . . ? As3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? As3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 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 As1 C7 152.6(4) . . . . ? Cl3 Ga1 As1 C7 -82.8(4) . . . . ? Cl1 Ga1 As1 C7 38.3(4) . . . . ? Cl2 Ga1 As1 C6 40.7(4) . . . . ? Cl3 Ga1 As1 C6 165.3(4) . . . . ? Cl1 Ga1 As1 C6 -73.6(4) . . . . ? Cl2 Ga1 As1 C2 -72.8(3) . . . . ? Cl3 Ga1 As1 C2 51.8(3) . . . . ? Cl1 Ga1 As1 C2 172.9(3) . . . . ? Cl5 Ga2 As2 C8 8.3(3) . . . . ? Cl4 Ga2 As2 C8 -126.0(3) . . . . ? As3 Ga2 As2 C8 123.1(3) . . . . ? Cl5 Ga2 As2 C9 131.0(3) . . . . ? Cl4 Ga2 As2 C9 -3.3(3) . . . . ? As3 Ga2 As2 C9 -114.2(3) . . . . ? Cl5 Ga2 As2 C3 -108.0(3) . . . . ? Cl4 Ga2 As2 C3 117.6(3) . . . . ? As3 Ga2 As2 C3 6.7(3) . . . . ? Cl5 Ga2 As3 C10 -8.0(4) . . . . ? Cl4 Ga2 As3 C10 118.1(4) . . . . ? As2 Ga2 As3 C10 -125.1(4) . . . . ? Cl5 Ga2 As3 C11 -128.3(4) . . . . ? Cl4 Ga2 As3 C11 -2.2(4) . . . . ? As2 Ga2 As3 C11 114.6(3) . . . . ? Cl5 Ga2 As3 C4 110.0(3) . . . . ? Cl4 Ga2 As3 C4 -123.9(3) . . . . ? As2 Ga2 As3 C4 -7.2(3) . . . . ? C5 C1 C2 As1 174.9(6) . . . . ? C4 C1 C2 As1 54.4(9) . . . . ? C3 C1 C2 As1 -67.9(8) . . . . ? C7 As1 C2 C1 65.5(8) . . . . ? C6 As1 C2 C1 175.0(7) . . . . ? Ga1 As1 C2 C1 -69.4(7) . . . . ? C5 C1 C3 As2 -48.5(9) . . . . ? C4 C1 C3 As2 77.6(8) . . . . ? C2 C1 C3 As2 -162.8(6) . . . . ? C8 As2 C3 C1 -162.7(7) . . . . ? C9 As2 C3 C1 83.1(7) . . . . ? Ga2 As2 C3 C1 -39.0(7) . . . . ? C5 C1 C4 As3 48.0(9) . . . . ? C2 C1 C4 As3 164.0(6) . . . . ? C3 C1 C4 As3 -76.8(8) . . . . ? C10 As3 C4 C1 163.8(7) . . . . ? C11 As3 C4 C1 -85.3(7) . . . . ? Ga2 As3 C4 C1 39.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.79 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 2.133 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.230 #===END OF CIF ============================================================== # 07fc002 data_07fc002 _database_code_depnum_ccdc_archive 'CCDC 637887' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-01-25 _chemical_name_systematic ; 1,1,1-tris(dimethylarsinomethyl)ethane-tris(triiodogallium(III)) dichloromethane solvate ; # (Me2AsCH2)3CMe = 1,1,1-tris(dimethylarsinomethyl)ethane _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H27 As3 Ga3 I9, C H2 Cl2' _chemical_formula_sum 'C12 H29 As3 Cl2 Ga3 I9' _chemical_formula_weight 1820.27 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' Cl Cl 0.1484 0.1585 '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 20.823(2) _cell_length_b 12.6145(15) _cell_length_c 15.486(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.030(7) _cell_angle_gamma 90.00 _cell_volume 4027.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 54142 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 11.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6220 # 0.5460 _exptl_absorpt_correction_T_max 1.0000 # 0.8030 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. 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 51077 _diffrn_reflns_av_R_equivalents 0.1417 _diffrn_reflns_av_sigmaI/netI 0.1374 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9248 _reflns_number_gt 5093 _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^)+(0.0214P)^2^+11.8988P] 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 9248 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1422 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.45206(6) 0.61460(10) 0.26389(10) 0.0290(3) Uani 1 1 d . . . Ga2 Ga 0.11858(6) 0.77960(11) 0.02568(9) 0.0308(3) Uani 1 1 d . . . Ga3 Ga 0.17029(6) 0.21997(10) 0.22494(10) 0.0313(4) Uani 1 1 d . . . I1 I 0.41246(4) 0.77474(7) 0.33992(6) 0.0397(2) Uani 1 1 d . . . I2 I 0.45691(4) 0.63930(7) 0.10341(6) 0.0404(2) Uani 1 1 d . . . I3 I 0.55590(4) 0.54182(7) 0.34667(7) 0.0452(3) Uani 1 1 d . . . I4 I 0.04160(4) 0.74852(7) 0.13536(6) 0.0349(2) Uani 1 1 d . . . I5 I 0.11765(4) 0.96733(7) -0.02841(6) 0.0444(3) Uani 1 1 d . . . I6 I 0.11390(4) 0.64224(7) -0.09417(6) 0.0397(2) Uani 1 1 d . . . I7 I 0.26275(4) 0.15688(6) 0.14748(6) 0.0361(2) Uani 1 1 d . . . I8 I 0.20615(4) 0.26424(7) 0.38378(6) 0.0409(2) Uani 1 1 d . . . I9 I 0.07145(4) 0.10376(7) 0.20226(7) 0.0471(3) Uani 1 1 d . . . As1 As 0.37433(5) 0.47126(9) 0.28230(9) 0.0267(3) Uani 1 1 d . . . As2 As 0.22776(5) 0.76931(9) 0.11410(8) 0.0263(3) Uani 1 1 d . . . As3 As 0.12948(5) 0.38912(9) 0.15702(9) 0.0260(3) Uani 1 1 d . . . C1 C 0.2425(5) 0.5446(8) 0.1921(8) 0.025(3) Uani 1 1 d . . . C2 C 0.2920(5) 0.4559(9) 0.2075(8) 0.030(3) Uani 1 1 d . . . H2A H 0.3023 0.4347 0.1494 0.036 Uiso 1 1 calc R . . H2B H 0.2696 0.3949 0.2302 0.036 Uiso 1 1 calc R . . C3 C 0.2744(5) 0.6405(9) 0.1491(10) 0.038(4) Uani 1 1 d . . . H3A H 0.2906 0.6124 0.0965 0.046 Uiso 1 1 calc R . . H3B H 0.3130 0.6615 0.1902 0.046 Uiso 1 1 calc R . . C4 C 0.1837(6) 0.5073(9) 0.1261(8) 0.033(3) Uani 1 1 d . . . H4A H 0.2004 0.4876 0.0715 0.040 Uiso 1 1 calc R . . H4B H 0.1549 0.5693 0.1125 0.040 Uiso 1 1 calc R . . C5 C 0.2192(6) 0.5801(9) 0.2784(9) 0.037(3) Uani 1 1 d . . . H5A H 0.1879 0.6380 0.2664 0.056 Uiso 1 1 calc R . . H5B H 0.2565 0.6046 0.3192 0.056 Uiso 1 1 calc R . . H5C H 0.1986 0.5202 0.3040 0.056 Uiso 1 1 calc R . . C6 C 0.4136(6) 0.3373(9) 0.2616(10) 0.046(4) Uani 1 1 d . . . H6A H 0.4556 0.3314 0.2988 0.069 Uiso 1 1 calc R . . H6B H 0.4201 0.3326 0.2002 0.069 Uiso 1 1 calc R . . H6C H 0.3852 0.2795 0.2751 0.069 Uiso 1 1 calc R . . C7 C 0.3605(7) 0.4664(13) 0.4024(9) 0.058(4) Uani 1 1 d . . . H7A H 0.3402 0.3988 0.4141 0.088 Uiso 1 1 calc R . . H7B H 0.3320 0.5250 0.4142 0.088 Uiso 1 1 calc R . . H7C H 0.4022 0.4731 0.4401 0.088 Uiso 1 1 calc R . . C8 C 0.2919(6) 0.8355(11) 0.0523(9) 0.048(4) Uani 1 1 d . . . H8A H 0.2788 0.9086 0.0374 0.073 Uiso 1 1 calc R . . H8B H 0.2953 0.7957 -0.0012 0.073 Uiso 1 1 calc R . . H8C H 0.3341 0.8357 0.0895 0.073 Uiso 1 1 calc R . . C9 C 0.2282(6) 0.8574(9) 0.2156(8) 0.037(3) Uani 1 1 d . . . H9A H 0.2015 0.8246 0.2556 0.055 Uiso 1 1 calc R . . H9B H 0.2107 0.9274 0.1979 0.055 Uiso 1 1 calc R . . H9C H 0.2728 0.8651 0.2450 0.055 Uiso 1 1 calc R . . C10 C 0.0826(6) 0.3603(11) 0.0456(9) 0.043(4) Uani 1 1 d . . . H10A H 0.0523 0.3017 0.0502 0.064 Uiso 1 1 calc R . . H10B H 0.1129 0.3407 0.0052 0.064 Uiso 1 1 calc R . . H10C H 0.0583 0.4236 0.0237 0.064 Uiso 1 1 calc R . . C11 C 0.0659(5) 0.4461(9) 0.2224(9) 0.035(3) Uani 1 1 d . . . H11A H 0.0405 0.5005 0.1877 0.052 Uiso 1 1 calc R . . H11B H 0.0877 0.4778 0.2765 0.052 Uiso 1 1 calc R . . H11C H 0.0371 0.3892 0.2365 0.052 Uiso 1 1 calc R . . C12 C 0.3629(7) 0.0676(10) 0.4167(10) 0.050(4) Uani 1 1 d . . . H12A H 0.4021 0.0232 0.4169 0.060 Uiso 1 1 calc R . . H12B H 0.3555 0.1062 0.3606 0.060 Uiso 1 1 calc R . . Cl1 Cl 0.37619(17) 0.1598(3) 0.5027(3) 0.0513(10) Uani 1 1 d . . . Cl2 Cl 0.29507(17) -0.0156(3) 0.4254(3) 0.0502(10) Uani 1 1 d . . . 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 0.0196(7) 0.0301(8) 0.0368(9) -0.0023(7) 0.0023(6) -0.0032(6) Ga2 0.0268(7) 0.0373(8) 0.0274(9) 0.0022(7) 0.0005(6) 0.0012(6) Ga3 0.0257(7) 0.0254(7) 0.0448(10) -0.0020(7) 0.0119(6) -0.0005(6) I1 0.0389(5) 0.0344(5) 0.0455(6) -0.0107(5) 0.0050(4) -0.0002(4) I2 0.0317(5) 0.0563(6) 0.0342(6) -0.0029(5) 0.0080(4) -0.0067(4) I3 0.0239(5) 0.0503(6) 0.0575(7) 0.0025(5) -0.0081(4) 0.0007(4) I4 0.0296(5) 0.0422(5) 0.0335(6) -0.0014(4) 0.0067(4) 0.0012(4) I5 0.0558(6) 0.0388(5) 0.0377(6) 0.0093(5) 0.0029(5) 0.0051(4) I6 0.0396(5) 0.0506(6) 0.0286(6) -0.0056(4) 0.0040(4) 0.0018(4) I7 0.0288(5) 0.0322(5) 0.0501(6) -0.0072(4) 0.0149(4) -0.0024(4) I8 0.0470(5) 0.0384(5) 0.0384(6) 0.0014(4) 0.0098(4) -0.0002(4) I9 0.0383(5) 0.0370(5) 0.0713(8) -0.0138(5) 0.0268(5) -0.0154(4) As1 0.0211(6) 0.0253(7) 0.0326(9) 0.0006(6) -0.0002(6) -0.0005(5) As2 0.0231(6) 0.0262(7) 0.0291(8) 0.0028(6) 0.0020(5) -0.0027(5) As3 0.0191(6) 0.0254(7) 0.0336(8) -0.0039(6) 0.0039(5) -0.0033(5) C1 0.025(6) 0.012(6) 0.039(9) 0.003(6) 0.012(6) -0.005(5) C2 0.024(7) 0.030(7) 0.034(8) -0.005(6) -0.003(6) -0.009(5) C3 0.017(6) 0.035(7) 0.064(11) 0.005(7) 0.008(6) 0.004(5) C4 0.041(8) 0.033(7) 0.022(8) 0.000(6) -0.013(6) -0.005(6) C5 0.030(7) 0.029(7) 0.054(10) 0.004(7) 0.011(6) -0.005(6) C6 0.041(8) 0.020(7) 0.076(12) -0.013(7) 0.005(8) 0.012(6) C7 0.063(10) 0.081(12) 0.033(10) 0.000(9) 0.011(8) -0.002(9) C8 0.051(9) 0.058(10) 0.042(10) 0.015(8) 0.024(7) -0.004(7) C9 0.039(8) 0.029(7) 0.039(9) -0.014(6) -0.006(6) 0.012(6) C10 0.037(8) 0.051(9) 0.040(10) -0.013(7) 0.003(7) -0.004(7) C11 0.027(7) 0.033(7) 0.048(10) 0.006(7) 0.018(6) 0.007(6) C12 0.073(10) 0.041(8) 0.046(10) 0.004(7) 0.043(8) 0.012(7) Cl1 0.049(2) 0.054(2) 0.051(3) -0.016(2) 0.0048(18) -0.0008(18) Cl2 0.049(2) 0.046(2) 0.056(3) 0.0021(19) 0.0069(18) 0.0003(17) _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 As1 2.4697(17) . ? Ga1 I2 2.5207(18) . ? Ga1 I3 2.5272(15) . ? Ga1 I1 2.5334(16) . ? Ga2 As2 2.4880(17) . ? Ga2 I5 2.5112(17) . ? Ga2 I4 2.5235(16) . ? Ga2 I6 2.5310(17) . ? Ga3 As3 2.4762(18) . ? Ga3 I9 2.5111(15) . ? Ga3 I8 2.5312(18) . ? Ga3 I7 2.5346(16) . ? As1 C7 1.922(14) . ? As1 C6 1.924(11) . ? As1 C2 1.940(10) . ? As2 C9 1.924(12) . ? As2 C3 1.931(11) . ? As2 C8 1.938(12) . ? As3 C10 1.896(12) . ? As3 C11 1.915(11) . ? As3 C4 1.969(12) . ? C1 C2 1.517(15) . ? C1 C5 1.549(17) . ? C1 C4 1.555(15) . ? C1 C3 1.573(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Cl1 1.760(14) . ? C12 Cl2 1.779(14) . ? C12 H12A 0.9900 . ? C12 H12B 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 As1 Ga1 I2 108.75(6) . . ? As1 Ga1 I3 101.74(6) . . ? I2 Ga1 I3 113.31(6) . . ? As1 Ga1 I1 105.61(6) . . ? I2 Ga1 I1 114.84(6) . . ? I3 Ga1 I1 111.40(6) . . ? As2 Ga2 I5 101.34(6) . . ? As2 Ga2 I4 103.83(6) . . ? I5 Ga2 I4 113.27(6) . . ? As2 Ga2 I6 107.85(6) . . ? I5 Ga2 I6 113.78(6) . . ? I4 Ga2 I6 115.10(6) . . ? As3 Ga3 I9 102.58(6) . . ? As3 Ga3 I8 105.06(6) . . ? I9 Ga3 I8 112.92(6) . . ? As3 Ga3 I7 107.93(6) . . ? I9 Ga3 I7 114.35(6) . . ? I8 Ga3 I7 112.88(6) . . ? C7 As1 C6 105.0(7) . . ? C7 As1 C2 109.6(6) . . ? C6 As1 C2 100.0(5) . . ? C7 As1 Ga1 108.9(5) . . ? C6 As1 Ga1 108.9(4) . . ? C2 As1 Ga1 122.9(4) . . ? C9 As2 C3 108.2(6) . . ? C9 As2 C8 103.2(6) . . ? C3 As2 C8 98.4(6) . . ? C9 As2 Ga2 108.6(4) . . ? C3 As2 Ga2 125.7(4) . . ? C8 As2 Ga2 110.2(4) . . ? C10 As3 C11 104.3(6) . . ? C10 As3 C4 99.4(5) . . ? C11 As3 C4 107.8(5) . . ? C10 As3 Ga3 108.9(4) . . ? C11 As3 Ga3 108.7(4) . . ? C4 As3 Ga3 125.6(3) . . ? C2 C1 C5 111.5(10) . . ? C2 C1 C4 109.6(9) . . ? C5 C1 C4 110.0(9) . . ? C2 C1 C3 108.4(9) . . ? C5 C1 C3 110.2(9) . . ? C4 C1 C3 107.1(10) . . ? C1 C2 As1 123.0(8) . . ? C1 C2 H2A 106.6 . . ? As1 C2 H2A 106.6 . . ? C1 C2 H2B 106.6 . . ? As1 C2 H2B 106.6 . . ? H2A C2 H2B 106.5 . . ? C1 C3 As2 122.7(8) . . ? C1 C3 H3A 106.6 . . ? As2 C3 H3A 106.6 . . ? C1 C3 H3B 106.6 . . ? As2 C3 H3B 106.6 . . ? H3A C3 H3B 106.6 . . ? C1 C4 As3 119.6(8) . . ? C1 C4 H4A 107.4 . . ? As3 C4 H4A 107.4 . . ? C1 C4 H4B 107.4 . . ? As3 C4 H4B 107.4 . . ? H4A C4 H4B 106.9 . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? As1 C6 H6A 109.5 . . ? As1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? As1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? As1 C7 H7A 109.5 . . ? As1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? As1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? As2 C8 H8A 109.5 . . ? As2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? As2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? As2 C9 H9A 109.5 . . ? As2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? As2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? As3 C10 H10A 109.5 . . ? As3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? As3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? As3 C11 H11A 109.5 . . ? As3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? As3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Cl1 C12 Cl2 112.1(7) . . ? Cl1 C12 H12A 109.2 . . ? Cl2 C12 H12A 109.2 . . ? Cl1 C12 H12B 109.2 . . ? Cl2 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? 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 I2 Ga1 As1 C7 -171.4(5) . . . . ? I3 Ga1 As1 C7 68.8(5) . . . . ? I1 Ga1 As1 C7 -47.6(5) . . . . ? I2 Ga1 As1 C6 74.7(5) . . . . ? I3 Ga1 As1 C6 -45.1(5) . . . . ? I1 Ga1 As1 C6 -161.6(5) . . . . ? I2 Ga1 As1 C2 -41.3(4) . . . . ? I3 Ga1 As1 C2 -161.1(4) . . . . ? I1 Ga1 As1 C2 82.4(4) . . . . ? I5 Ga2 As2 C9 68.8(4) . . . . ? I4 Ga2 As2 C9 -48.9(4) . . . . ? I6 Ga2 As2 C9 -171.4(4) . . . . ? I5 Ga2 As2 C3 -160.9(5) . . . . ? I4 Ga2 As2 C3 81.5(5) . . . . ? I6 Ga2 As2 C3 -41.1(5) . . . . ? I5 Ga2 As2 C8 -43.7(5) . . . . ? I4 Ga2 As2 C8 -161.3(5) . . . . ? I6 Ga2 As2 C8 76.1(5) . . . . ? I9 Ga3 As3 C10 -48.0(4) . . . . ? I8 Ga3 As3 C10 -166.2(4) . . . . ? I7 Ga3 As3 C10 73.1(4) . . . . ? I9 Ga3 As3 C11 65.0(4) . . . . ? I8 Ga3 As3 C11 -53.2(4) . . . . ? I7 Ga3 As3 C11 -173.9(4) . . . . ? I9 Ga3 As3 C4 -165.2(5) . . . . ? I8 Ga3 As3 C4 76.5(5) . . . . ? I7 Ga3 As3 C4 -44.1(5) . . . . ? C5 C1 C2 As1 -60.3(12) . . . . ? C4 C1 C2 As1 177.6(8) . . . . ? C3 C1 C2 As1 61.1(13) . . . . ? C7 As1 C2 C1 75.5(11) . . . . ? C6 As1 C2 C1 -174.6(10) . . . . ? Ga1 As1 C2 C1 -54.3(11) . . . . ? C2 C1 C3 As2 177.7(9) . . . . ? C5 C1 C3 As2 -60.1(13) . . . . ? C4 C1 C3 As2 59.5(13) . . . . ? C9 As2 C3 C1 81.6(12) . . . . ? C8 As2 C3 C1 -171.4(11) . . . . ? Ga2 As2 C3 C1 -48.9(13) . . . . ? C2 C1 C4 As3 63.7(12) . . . . ? C5 C1 C4 As3 -59.2(12) . . . . ? C3 C1 C4 As3 -178.9(8) . . . . ? C10 As3 C4 C1 -166.6(9) . . . . ? C11 As3 C4 C1 84.9(10) . . . . ? Ga3 As3 C4 C1 -45.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.614 _refine_diff_density_min -1.385 _refine_diff_density_rms 0.299 #============================================================================ # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique (to this file) identifier. #============================================================================ # 07fc004 data_07fc004 _database_code_depnum_ccdc_archive 'CCDC 637888' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-03-23 _audit_update_record ; 2007-03-23 Small amount of I found in ligand & complex. Re-ran refinement with I1 (close to Cl1). ; _chemical_name_systematic ; Dichloro(1,1,1-tris(dimethylarsinomethyl)ethane)gallium(III) tetrachlorogallate(III) ; _chemical_name_common ; Dichloro(1,1,1-tris(dimethylarsinomethyl)ethane)gallium(iii) tetrachlorogallate(iii) ; _chemical_melting_point ? _chemical_formula_moiety 'C11 H27 As3 Cl1.75 Ga1 I0.25 1+, Cl4 Ga1 1-' _chemical_formula_sum 'C11 H27 As3 Cl5.75 Ga2 I0.25' _chemical_formula_weight 759.09 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' As As 0.0499 2.0058 '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 9.7853(15) _cell_length_b 15.267(3) _cell_length_c 17.119(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.952(10) _cell_angle_gamma 90.00 _cell_volume 2510.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5758 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.008 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 6.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7330 # 0.6794 _exptl_absorpt_correction_T_max 1.0000 # 0.8179 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; Three sets of data were collected from three different crystals from the same batch of crystals. The crystals formed in an oil over several weeks. A second batch of crystals were obtained from a new experiment with essentially the same results. The same cell and the same systematic absences were obtained for all data sets and the initial solution showed the same structure. Features of the structure suggested disorder, this being most pronounced for two of the GaCl4 anion Cl's and the 'free' As atom and its bonded methyl groups which had very elongated thermal ellipsoids. Data set three is reported here as it had good intensity peaks, the lowest merging R and a plausible model for disorder in the anion was developed. Disorder at As3/C10/C11 is modelled as two orientations (A & B) of this group with equal populations. The largest peak in the final difference map is close (0.2 Angstrom) to Cl1. The Ga1-Cl1 distance is larger than expected and the inclusion of a fractional I at this largest peak gave a significant reduction in R1 (0.0840 to 0.0546) together with a shorter Cl1-Ga1 distance. It seems clear that the model is improved by the inclusion of I and further experiments confirmed the prescence of small amounts of I in the ligand/complex presumably from the initial synthesis. ; _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_% 0 _diffrn_reflns_number 17722 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4396 _reflns_number_gt 3299 _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^)+(0.0001P)^2^+22.2800P] 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 4396 _refine_ls_number_parameters 259 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.142 _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 0.12626(9) 0.98439(6) 0.22964(5) 0.0308(2) Uani 1 1 d D . . Ga2 Ga 0.52695(11) 0.74082(7) 0.39478(6) 0.0467(3) Uani 1 1 d D . . As1 As 0.29510(9) 0.94309(5) 0.14838(5) 0.0338(2) Uani 1 1 d . . . As2 As 0.01765(9) 0.84236(6) 0.24282(5) 0.0394(2) Uani 1 1 d . . . As3A As 0.3371(3) 0.60317(19) 0.13506(17) 0.0414(7) Uani 0.50 1 d P A 1 As3B As 0.2674(3) 0.5910(2) 0.13879(19) 0.0447(7) Uani 0.50 1 d P B 2 Cl1 Cl 0.1869(7) 1.0518(4) 0.3453(4) 0.0419(15) Uani 0.751(4) 1 d PD . . I1 I 0.2151(6) 1.0626(4) 0.3515(4) 0.0382(15) Uiso 0.249(4) 1 d PD . . Cl2 Cl -0.0369(2) 1.05875(14) 0.15002(12) 0.0456(6) Uani 1 1 d . . . Cl3A Cl 0.6266(7) 0.7559(4) 0.5173(3) 0.063(3) Uani 0.480(10) 1 d PD . . Cl3B Cl 0.7050(7) 0.8005(5) 0.4805(4) 0.080(3) Uani 0.520(10) 1 d PD . . Cl4A Cl 0.3587(7) 0.6380(4) 0.3972(5) 0.056(2) Uani 0.480(10) 1 d PD . . Cl4B Cl 0.4294(15) 0.6459(5) 0.4459(7) 0.128(5) Uani 0.520(10) 1 d PD . . Cl5A Cl 0.6608(11) 0.6954(10) 0.3195(7) 0.065(3) Uani 0.520(10) 1 d PD . . Cl5B Cl 0.6213(12) 0.6918(10) 0.2947(7) 0.058(3) Uani 0.480(10) 1 d PD . . Cl6 Cl 0.3954(3) 0.85044(17) 0.34844(15) 0.0638(7) Uani 1 1 d D . . C1 C 0.1494(10) 0.7689(5) 0.1121(5) 0.047(2) Uani 1 1 d . A . C2 C 0.2888(10) 0.8177(5) 0.1255(5) 0.044(2) Uani 1 1 d . . . H2A H 0.3295 0.8089 0.0773 0.053 Uiso 1 1 calc R . . H2B H 0.3515 0.7884 0.1700 0.053 Uiso 1 1 calc R . . C3 C 0.0998(10) 0.7488(5) 0.1905(5) 0.049(3) Uani 1 1 d . . . H3A H 0.1806 0.7260 0.2288 0.058 Uiso 1 1 calc R . . H3B H 0.0308 0.7008 0.1798 0.058 Uiso 1 1 calc R . . C4 C 0.1702(13) 0.6800(6) 0.0727(6) 0.071(4) Uani 1 1 d . . . H4A H 0.1869 0.6911 0.0183 0.085 Uiso 1 1 calc R A 1 H4B H 0.0831 0.6457 0.0676 0.085 Uiso 1 1 calc R A 1 C5 C 0.0384(10) 0.8193(6) 0.0541(5) 0.054(3) Uani 1 1 d . . . H5A H 0.0245 0.8770 0.0764 0.082 Uiso 1 1 calc R A . H5B H -0.0494 0.7866 0.0456 0.082 Uiso 1 1 calc R . . H5C H 0.0691 0.8265 0.0033 0.082 Uiso 1 1 calc R . . C6 C 0.2516(11) 1.0042(6) 0.0473(5) 0.050(2) Uani 1 1 d . . . H6A H 0.1529 0.9962 0.0241 0.075 Uiso 1 1 calc R . . H6B H 0.3086 0.9804 0.0109 0.075 Uiso 1 1 calc R . . H6C H 0.2715 1.0668 0.0557 0.075 Uiso 1 1 calc R . . C7 C 0.4889(9) 0.9640(7) 0.1868(6) 0.055(3) Uani 1 1 d . . . H7A H 0.5035 1.0262 0.2000 0.083 Uiso 1 1 calc R . . H7B H 0.5415 0.9481 0.1455 0.083 Uiso 1 1 calc R . . H7C H 0.5209 0.9285 0.2344 0.083 Uiso 1 1 calc R . . C8 C -0.1783(9) 0.8464(8) 0.1951(7) 0.076(4) Uani 1 1 d . . . H8A H -0.1891 0.8674 0.1402 0.114 Uiso 1 1 calc R . . H8B H -0.2265 0.8863 0.2257 0.114 Uiso 1 1 calc R . . H8C H -0.2183 0.7876 0.1954 0.114 Uiso 1 1 calc R . . C9 C 0.0258(10) 0.8006(6) 0.3490(5) 0.050(2) Uani 1 1 d . . . H9A H -0.0148 0.8445 0.3797 0.076 Uiso 1 1 calc R . . H9B H 0.1230 0.7902 0.3742 0.076 Uiso 1 1 calc R . . H9C H -0.0267 0.7458 0.3476 0.076 Uiso 1 1 calc R . . C10A C 0.401(2) 0.5435(13) 0.0494(11) 0.053(5) Uani 0.50 1 d P A 1 H10A H 0.4677 0.5806 0.0290 0.064 Uiso 0.50 1 calc PR A 1 H10B H 0.3211 0.5314 0.0066 0.064 Uiso 0.50 1 calc PR A 1 H10C H 0.4453 0.4883 0.0691 0.064 Uiso 0.50 1 calc PR A 1 C11A C 0.209(2) 0.5162(15) 0.1558(17) 0.074(7) Uani 0.50 1 d P A 1 H11A H 0.1641 0.5358 0.1993 0.089 Uiso 0.50 1 calc PR A 1 H11B H 0.2584 0.4612 0.1708 0.089 Uiso 0.50 1 calc PR A 1 H11C H 0.1376 0.5069 0.1079 0.089 Uiso 0.50 1 calc PR A 1 C10B C 0.192(3) 0.4920(14) 0.072(2) 0.089(9) Uani 0.50 1 d P B 2 H10D H 0.2318 0.4373 0.0959 0.107 Uiso 0.50 1 calc PR B 2 H10E H 0.2163 0.4985 0.0189 0.107 Uiso 0.50 1 calc PR B 2 H10F H 0.0906 0.4906 0.0662 0.107 Uiso 0.50 1 calc PR B 2 C11B C 0.429(2) 0.6077(15) 0.0884(14) 0.065(6) Uani 0.50 1 d P B 2 H11D H 0.5028 0.5667 0.1116 0.078 Uiso 0.50 1 calc PR B 2 H11E H 0.4630 0.6679 0.0972 0.078 Uiso 0.50 1 calc PR B 2 H11F H 0.4022 0.5967 0.0311 0.078 Uiso 0.50 1 calc PR B 2 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 0.0345(5) 0.0277(5) 0.0288(5) 0.0017(4) 0.0026(4) 0.0039(4) Ga2 0.0610(7) 0.0418(6) 0.0384(6) 0.0006(5) 0.0125(5) 0.0123(5) As1 0.0410(5) 0.0297(4) 0.0308(4) 0.0000(4) 0.0067(4) 0.0054(4) As2 0.0394(5) 0.0349(5) 0.0403(5) 0.0097(4) -0.0016(4) -0.0057(4) As3A 0.0635(19) 0.0297(12) 0.0302(12) 0.0011(9) 0.0067(15) 0.0130(15) As3B 0.0592(18) 0.0422(15) 0.0378(12) 0.0086(10) 0.0221(16) 0.0168(15) Cl1 0.036(3) 0.030(2) 0.057(3) -0.0017(17) 0.003(2) -0.001(2) Cl2 0.0630(14) 0.0333(11) 0.0350(11) 0.0096(9) -0.0049(10) 0.0064(10) Cl3A 0.052(4) 0.080(4) 0.049(4) -0.005(3) -0.015(3) 0.020(3) Cl3B 0.065(4) 0.105(6) 0.060(4) -0.023(4) -0.017(3) 0.043(4) Cl4A 0.058(4) 0.045(3) 0.075(5) 0.004(3) 0.039(3) -0.006(3) Cl4B 0.233(14) 0.051(4) 0.151(10) 0.004(5) 0.166(10) 0.000(6) Cl5A 0.055(5) 0.064(4) 0.092(8) -0.026(6) 0.051(6) -0.025(4) Cl5B 0.068(7) 0.054(4) 0.062(6) -0.017(4) 0.038(5) -0.025(5) Cl6 0.0784(18) 0.0568(16) 0.0485(15) 0.0045(12) -0.0074(13) 0.0152(14) C1 0.077(7) 0.021(4) 0.032(5) 0.000(4) -0.016(5) 0.001(4) C2 0.072(6) 0.029(4) 0.029(5) -0.007(4) 0.005(4) 0.017(4) C3 0.076(7) 0.023(4) 0.037(5) 0.009(4) -0.015(5) -0.006(4) C4 0.137(10) 0.027(5) 0.033(5) 0.004(4) -0.019(6) 0.005(6) C5 0.074(7) 0.045(6) 0.036(5) 0.002(4) -0.010(5) -0.002(5) C6 0.076(7) 0.042(5) 0.033(5) 0.010(4) 0.016(5) 0.008(5) C7 0.037(5) 0.059(6) 0.069(7) 0.005(5) 0.008(5) 0.006(5) C8 0.030(5) 0.082(8) 0.104(9) 0.039(7) -0.017(5) -0.016(5) C9 0.065(6) 0.045(5) 0.044(5) 0.012(4) 0.018(5) 0.004(5) C10A 0.074(14) 0.048(12) 0.045(11) 0.016(10) 0.030(10) 0.025(11) C11A 0.064(14) 0.063(15) 0.11(2) 0.033(15) 0.052(15) 0.009(12) C10B 0.078(17) 0.035(12) 0.15(3) -0.009(15) 0.021(18) -0.005(11) C11B 0.067(14) 0.060(14) 0.080(16) 0.007(13) 0.042(13) 0.038(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 # added by hand Ga1 Cl2 2.207(2) . ? Ga1 Cl1 2.210(7) . ? Ga1 I1 2.418(6) . ? Ga1 As1 2.4362(13) . ? Ga1 As2 2.4440(13) . ? Ga2 Cl4B 2.024(7) . ? Ga2 Cl5A 2.121(8) . ? Ga2 Cl3A 2.151(5) . ? Ga2 Cl6 2.168(3) . ? Ga2 Cl5B 2.225(9) . ? Ga2 Cl3B 2.247(6) . ? Ga2 Cl4A 2.281(6) . ? As1 C7 1.912(9) . ? As1 C6 1.941(8) . ? As1 C2 1.953(8) . ? As2 C9 1.914(9) . ? As2 C8 1.937(8) . ? As2 C3 1.939(9) . ? As3A C11A 1.91(2) . ? As3A C10A 1.926(19) . ? As3A C4 2.126(10) . ? As3B C11B 1.96(2) . ? As3B C10B 1.96(2) . ? As3B C4 1.902(9) . ? Cl3A Cl3B 1.278(9) . ? Cl4A Cl4B 0.984(14) . ? Cl5A Cl5B 0.521(18) . ? C1 C5 1.532(11) . ? C1 C2 1.533(13) . ? C1 C3 1.542(13) . ? C1 C4 1.547(12) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 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 110.70(19) . . ? Cl2 Ga1 I1 112.22(17) . . ? Cl1 Ga1 I1 6.1(3) . . ? Cl2 Ga1 As1 105.67(7) . . ? Cl1 Ga1 As1 122.43(18) . . ? I1 Ga1 As1 116.67(15) . . ? Cl2 Ga1 As2 103.72(7) . . ? Cl1 Ga1 As2 112.19(18) . . ? I1 Ga1 As2 116.74(15) . . ? As1 Ga1 As2 100.20(4) . . ? Cl4B Ga2 Cl5A 115.2(5) . . ? Cl4B Ga2 Cl3A 79.5(4) . . ? Cl5A Ga2 Cl3A 114.2(4) . . ? Cl4B Ga2 Cl6 114.5(4) . . ? Cl5A Ga2 Cl6 115.0(4) . . ? Cl3A Ga2 Cl6 113.69(17) . . ? Cl4B Ga2 Cl5B 113.0(4) . . ? Cl5A Ga2 Cl5B 13.5(5) . . ? Cl3A Ga2 Cl5B 127.6(4) . . ? Cl6 Ga2 Cl5B 106.4(4) . . ? Cl4B Ga2 Cl3B 112.3(4) . . ? Cl5A Ga2 Cl3B 92.1(4) . . ? Cl3A Ga2 Cl3B 33.7(2) . . ? Cl6 Ga2 Cl3B 104.99(18) . . ? Cl5B Ga2 Cl3B 104.8(4) . . ? Cl4B Ga2 Cl4A 25.6(4) . . ? Cl5A Ga2 Cl4A 108.5(4) . . ? Cl3A Ga2 Cl4A 104.5(3) . . ? Cl6 Ga2 Cl4A 99.1(2) . . ? Cl5B Ga2 Cl4A 100.9(4) . . ? Cl3B Ga2 Cl4A 137.7(3) . . ? C7 As1 C6 105.1(4) . . ? C7 As1 C2 103.0(4) . . ? C6 As1 C2 107.4(4) . . ? C7 As1 Ga1 119.8(3) . . ? C6 As1 Ga1 109.1(3) . . ? C2 As1 Ga1 111.7(3) . . ? C9 As2 C8 105.7(5) . . ? C9 As2 C3 104.3(4) . . ? C8 As2 C3 107.0(5) . . ? C9 As2 Ga1 116.3(3) . . ? C8 As2 Ga1 110.2(3) . . ? C3 As2 Ga1 112.7(3) . . ? C11A As3A C10A 97.6(11) . . ? C11A As3A C4 90.4(8) . . ? C10A As3A C4 101.9(6) . . ? C11B As3B C10B 94.9(11) . . ? Cl3B Cl3A Ga2 77.3(4) . . ? Cl3A Cl3B Ga2 69.0(4) . . ? Cl4B Cl4A Ga2 62.5(6) . . ? Cl4A Cl4B Ga2 92.0(7) . . ? Cl5B Cl5A Ga2 94.7(19) . . ? Cl5A Cl5B Ga2 71.8(17) . . ? C5 C1 C2 110.7(7) . . ? C5 C1 C3 111.3(8) . . ? C2 C1 C3 112.7(7) . . ? C5 C1 C4 107.1(7) . . ? C2 C1 C4 107.7(8) . . ? C3 C1 C4 107.2(7) . . ? C1 C2 As1 120.0(6) . . ? C1 C2 H2A 107.3 . . ? As1 C2 H2A 107.3 . . ? C1 C2 H2B 107.3 . . ? As1 C2 H2B 107.3 . . ? H2A C2 H2B 106.9 . . ? C1 C3 As2 118.8(5) . . ? C1 C3 H3A 107.6 . . ? As2 C3 H3A 107.6 . . ? C1 C3 H3B 107.6 . . ? As2 C3 H3B 107.6 . . ? H3A C3 H3B 107.0 . . ? C1 C4 As3A 114.7(6) . . ? C1 C4 H4A 108.6 . . ? As3A C4 H4A 108.6 . . ? C1 C4 H4B 108.6 . . ? As3A C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? As1 C6 H6A 109.5 . . ? As1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? As1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? As1 C7 H7A 109.5 . . ? As1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? As1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? As2 C8 H8A 109.5 . . ? As2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? As2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? As2 C9 H9A 109.5 . . ? As2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? As2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? As3A C10A H10A 109.5 . . ? As3A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? As3A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? As3A C11A H11A 109.5 . . ? As3A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? As3A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? As3B C10B H10D 109.5 . . ? As3B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? As3B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? As3B C11B H11D 109.5 . . ? As3B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? As3B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 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 As1 C7 130.8(4) . . . . ? Cl1 Ga1 As1 C7 3.0(4) . . . . ? I1 Ga1 As1 C7 5.3(4) . . . . ? As2 Ga1 As1 C7 -121.7(4) . . . . ? Cl2 Ga1 As1 C6 9.7(3) . . . . ? Cl1 Ga1 As1 C6 -118.1(4) . . . . ? I1 Ga1 As1 C6 -115.8(4) . . . . ? As2 Ga1 As1 C6 117.2(3) . . . . ? Cl2 Ga1 As1 C2 -108.8(3) . . . . ? Cl1 Ga1 As1 C2 123.3(3) . . . . ? I1 Ga1 As1 C2 125.7(3) . . . . ? As2 Ga1 As1 C2 -1.3(3) . . . . ? Cl2 Ga1 As2 C9 -128.9(3) . . . . ? Cl1 Ga1 As2 C9 -9.4(4) . . . . ? I1 Ga1 As2 C9 -5.0(4) . . . . ? As1 Ga1 As2 C9 122.0(3) . . . . ? Cl2 Ga1 As2 C8 -8.8(4) . . . . ? Cl1 Ga1 As2 C8 110.8(5) . . . . ? I1 Ga1 As2 C8 115.2(5) . . . . ? As1 Ga1 As2 C8 -117.8(4) . . . . ? Cl2 Ga1 As2 C3 110.7(3) . . . . ? Cl1 Ga1 As2 C3 -129.8(3) . . . . ? I1 Ga1 As2 C3 -125.3(3) . . . . ? As1 Ga1 As2 C3 1.7(3) . . . . ? C5 C1 C2 As1 47.5(9) . . . . ? C3 C1 C2 As1 -77.7(8) . . . . ? C4 C1 C2 As1 164.3(6) . . . . ? C7 As1 C2 C1 165.3(7) . . . . ? C6 As1 C2 C1 -84.0(7) . . . . ? Ga1 As1 C2 C1 35.5(7) . . . . ? C5 C1 C3 As2 -47.6(9) . . . . ? C2 C1 C3 As2 77.3(9) . . . . ? C4 C1 C3 As2 -164.4(7) . . . . ? C9 As2 C3 C1 -162.7(7) . . . . ? C8 As2 C3 C1 85.6(8) . . . . ? Ga1 As2 C3 C1 -35.7(7) . . . . ? C5 C1 C4 As3A 173.0(7) . . . . ? C2 C1 C4 As3A 53.9(9) . . . . ? C3 C1 C4 As3A -67.6(10) . . . . ? C11A As3A C4 C1 114.7(12) . . . . ? C10A As3A C4 C1 -147.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.308 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.145 #===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 =============================================================