# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1347 data_bt37o _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Bert*GaCl2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H49 Cl2 Ga' _chemical_formula_weight 622.37 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' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pbcm' 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 11.069(2) _cell_length_b 12.170(2) _cell_length_c 25.275(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3404.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 49 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 20.72 _exptl_crystal_description 'fragment of hexagonal plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.8048 _exptl_absorpt_correction_T_max 0.9432 _exptl_absorpt_process_details ;XABS2 : an empirical absorption correction program. Parkin, S.; Moezzi ,B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5130 _diffrn_reflns_av_R_equivalents 0.1134 _diffrn_reflns_av_sigmaI/netI 0.1569 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2287 _reflns_number_gt 1184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'XDISK, Siemens' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 5.10, Siemens' _computing_publication_material 'XCIF, SHELXTL v. 5.10, Siemens' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0126P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2287 _refine_ls_number_parameters 190 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1522 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 0.78573(13) 0.05291(10) 0.7500 0.0302(4) Uani 1 2 d S . . Cl1 Cl 0.9563(3) -0.0270(3) 0.7500 0.0634(11) Uani 1 2 d S . . Cl2 Cl 0.6489(3) -0.0681(3) 0.7500 0.0761(13) Uani 1 2 d S . . C1 C 0.7654(8) 0.2104(7) 0.7500 0.015(2) Uani 1 2 d SU . . C2 C 0.7596(5) 0.2673(5) 0.7978(2) 0.0204(18) Uani 1 1 d U . . C3 C 0.7462(5) 0.3791(5) 0.7970(3) 0.0236(19) Uani 1 1 d . . . H3A H 0.7408 0.4179 0.8296 0.028 Uiso 1 1 calc R . . C4 C 0.7403(8) 0.4371(9) 0.7500 0.030(3) Uani 1 2 d S . . H4A H 0.7324 0.5148 0.7500 0.036 Uiso 1 2 calc SR . . C13 C 0.7667(6) 0.2034(5) 0.8487(3) 0.0223(18) Uani 1 1 d . . . C14 C 0.8768(6) 0.1832(5) 0.8728(3) 0.0214(19) Uani 1 1 d . . . C15 C 0.8791(7) 0.1223(6) 0.9195(3) 0.027(2) Uani 1 1 d . . . H15A H 0.9545 0.1090 0.9363 0.033 Uiso 1 1 calc R . . C16 C 0.7750(7) 0.0806(5) 0.9421(2) 0.0235(18) Uani 1 1 d . . . C17 C 0.6660(7) 0.1020(6) 0.9181(3) 0.030(2) Uani 1 1 d . . . H17A H 0.5940 0.0745 0.9338 0.036 Uiso 1 1 calc R . . C18 C 0.6581(6) 0.1635(6) 0.8711(3) 0.0210(19) Uani 1 1 d . . . C19 C 0.5352(6) 0.1919(6) 0.8478(3) 0.025(2) Uani 1 1 d . . . H19A H 0.5483 0.2198 0.8110 0.030 Uiso 1 1 calc R . . C20 C 0.4508(6) 0.0958(6) 0.8448(3) 0.046(2) Uani 1 1 d . . . H20A H 0.3769 0.1176 0.8262 0.069 Uiso 1 1 calc R . . H20B H 0.4303 0.0716 0.8807 0.069 Uiso 1 1 calc R . . H20C H 0.4898 0.0355 0.8257 0.069 Uiso 1 1 calc R . . C21 C 0.4770(6) 0.2821(6) 0.8795(3) 0.046(3) Uani 1 1 d . . . H21A H 0.5290 0.3473 0.8791 0.069 Uiso 1 1 calc R . . H21B H 0.4657 0.2573 0.9161 0.069 Uiso 1 1 calc R . . H21C H 0.3984 0.3005 0.8640 0.069 Uiso 1 1 calc R . . C22 C 0.7798(8) 0.0174(5) 0.9937(3) 0.035(2) Uani 1 1 d . . . H22A H 0.8668 0.0035 1.0019 0.041 Uiso 1 1 calc R . . C23 C 0.7292(7) 0.0859(5) 1.0382(2) 0.051(3) Uani 1 1 d . . . H23A H 0.7733 0.1556 1.0402 0.076 Uiso 1 1 calc R . . H23B H 0.7380 0.0461 1.0717 0.076 Uiso 1 1 calc R . . H23C H 0.6435 0.1006 1.0316 0.076 Uiso 1 1 calc R . . C24 C 0.7172(7) -0.0929(5) 0.9917(3) 0.047(2) Uani 1 1 d . . . H24A H 0.7509 -0.1367 0.9627 0.070 Uiso 1 1 calc R . . H24B H 0.6305 -0.0819 0.9858 0.070 Uiso 1 1 calc R . . H24C H 0.7295 -0.1315 1.0253 0.070 Uiso 1 1 calc R . . C25 C 0.9915(6) 0.2343(6) 0.8528(3) 0.028(2) Uani 1 1 d . . . H25A H 0.9777 0.2557 0.8151 0.033 Uiso 1 1 calc R . . C26 C 1.1013(6) 0.1578(6) 0.8541(3) 0.049(3) Uani 1 1 d . . . H26A H 1.0856 0.0933 0.8319 0.074 Uiso 1 1 calc R . . H26B H 1.1163 0.1342 0.8906 0.074 Uiso 1 1 calc R . . H26C H 1.1723 0.1970 0.8406 0.074 Uiso 1 1 calc R . . C27 C 1.0217(7) 0.3391(6) 0.8835(3) 0.051(3) Uani 1 1 d . . . H27A H 0.9582 0.3939 0.8776 0.077 Uiso 1 1 calc R . . H27B H 1.0993 0.3684 0.8712 0.077 Uiso 1 1 calc R . . H27C H 1.0269 0.3223 0.9214 0.077 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 0.0355(8) 0.0313(7) 0.0238(7) 0.000 0.000 0.0063(8) Cl1 0.058(3) 0.062(3) 0.070(2) 0.000 0.000 0.031(2) Cl2 0.080(3) 0.038(2) 0.110(3) 0.000 0.000 -0.021(2) C1 0.010(4) 0.021(4) 0.016(4) 0.000 0.000 -0.001(4) C2 0.009(4) 0.029(3) 0.024(3) 0.001(3) 0.000(3) -0.003(3) C3 0.016(5) 0.028(4) 0.027(4) -0.003(3) -0.003(4) 0.006(3) C4 0.032(8) 0.026(6) 0.032(6) 0.000 0.000 0.006(6) C13 0.022(5) 0.033(4) 0.013(4) -0.004(3) 0.004(4) 0.007(4) C14 0.017(5) 0.026(4) 0.020(5) 0.002(4) 0.005(4) 0.003(4) C15 0.016(5) 0.038(5) 0.028(5) -0.003(4) -0.003(4) -0.002(4) C16 0.021(5) 0.027(4) 0.023(4) 0.000(3) -0.004(4) 0.002(4) C17 0.036(6) 0.029(5) 0.024(5) 0.012(4) 0.003(4) -0.015(4) C18 0.012(4) 0.031(5) 0.020(5) -0.003(4) 0.001(4) -0.002(4) C19 0.011(5) 0.032(5) 0.033(5) 0.011(4) -0.001(4) -0.003(4) C20 0.022(5) 0.058(6) 0.058(6) -0.010(5) -0.017(5) 0.000(4) C21 0.024(5) 0.045(6) 0.068(6) -0.001(5) -0.008(5) 0.010(5) C22 0.037(5) 0.045(5) 0.022(4) 0.015(4) -0.007(5) -0.001(5) C23 0.079(7) 0.053(6) 0.021(4) 0.008(4) 0.001(5) -0.006(5) C24 0.066(6) 0.032(4) 0.042(5) 0.014(4) 0.009(6) -0.008(5) C25 0.013(4) 0.041(5) 0.028(5) 0.005(4) 0.002(4) -0.001(4) C26 0.024(5) 0.065(6) 0.059(7) 0.014(5) 0.009(5) 0.013(5) C27 0.035(6) 0.063(7) 0.057(6) -0.003(5) 0.004(5) -0.015(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 C1 1.930(8) . ? Ga1 Cl2 2.113(4) . ? Ga1 Cl1 2.124(3) . ? C1 C2 1.395(7) . ? C1 C2 1.395(7) 6_557 ? C2 C3 1.368(8) . ? C2 C13 1.505(9) . ? C3 C4 1.384(8) . ? C4 C3 1.384(8) 6_557 ? C13 C14 1.385(9) . ? C13 C18 1.415(8) . ? C14 C15 1.393(9) . ? C14 C25 1.502(9) . ? C15 C16 1.383(9) . ? C16 C17 1.375(9) . ? C16 C22 1.516(8) . ? C17 C18 1.407(9) . ? C18 C19 1.522(8) . ? C19 C20 1.499(8) . ? C19 C21 1.505(9) . ? C22 C23 1.507(9) . ? C22 C24 1.512(8) . ? C25 C26 1.531(9) . ? C25 C27 1.531(9) . ? 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 Ga1 Cl2 127.5(3) . . ? C1 Ga1 Cl1 124.0(3) . . ? Cl2 Ga1 Cl1 108.54(14) . . ? C2 C1 C2 120.2(8) . 6_557 ? C2 C1 Ga1 119.9(4) . . ? C2 C1 Ga1 119.9(4) 6_557 . ? C3 C2 C1 119.0(7) . . ? C3 C2 C13 122.2(6) . . ? C1 C2 C13 118.7(6) . . ? C2 C3 C4 121.7(8) . . ? C3 C4 C3 118.4(10) 6_557 . ? C14 C13 C18 120.7(6) . . ? C14 C13 C2 120.9(6) . . ? C18 C13 C2 118.4(6) . . ? C13 C14 C15 118.9(7) . . ? C13 C14 C25 121.5(7) . . ? C15 C14 C25 119.4(7) . . ? C16 C15 C14 122.0(7) . . ? C17 C16 C15 118.7(6) . . ? C17 C16 C22 120.4(7) . . ? C15 C16 C22 120.9(7) . . ? C16 C17 C18 121.8(7) . . ? C13 C18 C17 117.9(6) . . ? C13 C18 C19 121.7(6) . . ? C17 C18 C19 120.3(7) . . ? C20 C19 C21 109.1(6) . . ? C20 C19 C18 113.5(6) . . ? C21 C19 C18 109.9(6) . . ? C23 C22 C16 110.4(6) . . ? C23 C22 C24 110.3(6) . . ? C16 C22 C24 113.9(6) . . ? C14 C25 C26 114.3(6) . . ? C14 C25 C27 111.0(6) . . ? C26 C25 C27 108.8(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.438 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.084 data_bt45 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Bert*InCl2]2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H98 Cl4 In2' _chemical_formula_weight 1334.94 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' 'In' 'In' -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Cmca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 25.6540(13) _cell_length_b 21.2270(11) _cell_length_c 12.7609(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6949.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 7840 _cell_measurement_theta_min 0 _cell_measurement_theta_max 31.5 _exptl_crystal_description 'cube' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.6278 _exptl_absorpt_correction_T_max 0.7834 _exptl_absorpt_process_details ;Blessing, R.H., Acta Cryst. (1995), A51, 33-38. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29264 _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 29.00 _reflns_number_total 4706 _reflns_number_gt 2824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Disorder in the methyl carbon sites c26 c27 were modelled with the occupancy allowed to freely refine. Methyl hydrogen atom sites were fixed in position. Methine hydrogen atom sites on c25 were fixed in the calculated positions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4706 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 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 In1 In 0.5000 0.423705(14) 0.07607(2) 0.04205(9) Uani 1 2 d S . . Cl1 Cl 0.56528(4) 0.5000 0.0000 0.0523(3) Uani 1 2 d S . . Cl2 Cl 0.5000 0.34963(6) -0.05911(9) 0.0747(3) Uani 1 2 d S . . C1 C 0.5000 0.40708(14) 0.2419(3) 0.0322(8) Uani 1 2 d S . . C2 C 0.54755(9) 0.40156(11) 0.2949(2) 0.0362(6) Uani 1 1 d . . . C3 C 0.54666(11) 0.39380(13) 0.4028(2) 0.0495(7) Uani 1 1 d . . . H3A H 0.5779 0.3907 0.4395 0.059 Uiso 1 1 calc R . . C4 C 0.5000 0.3906(2) 0.4564(3) 0.0600(12) Uani 1 2 d S . . H4A H 0.5000 0.3864 0.5289 0.072 Uiso 1 2 calc SR . . C13 C 0.59774(9) 0.39897(12) 0.2338(2) 0.0368(6) Uani 1 1 d . . . C14 C 0.62962(10) 0.45185(13) 0.2254(2) 0.0456(7) Uani 1 1 d . A . C15 C 0.67344(11) 0.44769(14) 0.1613(3) 0.0536(8) Uani 1 1 d . . . H15A H 0.6947 0.4829 0.1545 0.064 Uiso 1 1 calc R . . C16 C 0.68671(10) 0.39387(15) 0.1075(2) 0.0478(7) Uani 1 1 d . . . C17 C 0.65574(11) 0.34130(14) 0.1222(2) 0.0490(7) Uani 1 1 d . . . H17A H 0.6649 0.3039 0.0891 0.059 Uiso 1 1 calc R . . C18 C 0.61160(9) 0.34240(12) 0.1845(2) 0.0412(6) Uani 1 1 d . . . C19 C 0.58306(11) 0.28112(14) 0.2075(3) 0.0549(8) Uani 1 1 d . . . H19A H 0.5475 0.2920 0.2291 0.066 Uiso 1 1 calc R . . C20 C 0.60885(16) 0.24781(18) 0.2990(3) 0.0919(13) Uani 1 1 d . . . H20A H 0.6112 0.2762 0.3575 0.138 Uiso 1 1 calc R . . H20B H 0.6432 0.2344 0.2790 0.138 Uiso 1 1 calc R . . H20C H 0.5884 0.2118 0.3185 0.138 Uiso 1 1 calc R . . C21 C 0.57889(14) 0.23650(15) 0.1144(3) 0.0754(10) Uani 1 1 d . . . H21A H 0.5605 0.1991 0.1351 0.113 Uiso 1 1 calc R . . H21B H 0.6132 0.2253 0.0908 0.113 Uiso 1 1 calc R . . H21C H 0.5603 0.2569 0.0586 0.113 Uiso 1 1 calc R . . C22 C 0.73501(11) 0.39027(16) 0.0382(2) 0.0613(9) Uani 1 1 d . . . H22A H 0.7467 0.4336 0.0257 0.074 Uiso 1 1 calc R . . C23 C 0.77855(12) 0.3564(2) 0.0927(3) 0.0871(12) Uani 1 1 d . . . H23A H 0.7854 0.3764 0.1588 0.131 Uiso 1 1 calc R . . H23B H 0.8093 0.3579 0.0500 0.131 Uiso 1 1 calc R . . H23C H 0.7688 0.3133 0.1043 0.131 Uiso 1 1 calc R . . C24 C 0.72361(15) 0.3613(3) -0.0675(3) 0.1206(17) Uani 1 1 d . . . H24A H 0.7549 0.3605 -0.1087 0.181 Uiso 1 1 calc R . . H24B H 0.6976 0.3858 -0.1029 0.181 Uiso 1 1 calc R . . H24C H 0.7111 0.3190 -0.0581 0.181 Uiso 1 1 calc R . . C25 C 0.61931(13) 0.51199(16) 0.2899(4) 0.0788(12) Uani 1 1 d . . . H25A H 0.5826 0.5116 0.3104 0.095 Uiso 0.380(9) 1 d P A 1 C26A C 0.6461(7) 0.5132(7) 0.3861(11) 0.098(5) Uani 0.380(9) 1 d P A 1 H26A H 0.6378 0.5514 0.4227 0.147 Uiso 0.380(9) 1 calc PR A 1 H26B H 0.6829 0.5114 0.3734 0.147 Uiso 0.380(9) 1 calc PR A 1 H26C H 0.6357 0.4777 0.4277 0.147 Uiso 0.380(9) 1 calc PR A 1 C27A C 0.6333(7) 0.5692(5) 0.2168(11) 0.120(6) Uani 0.380(9) 1 d P A 1 H27A H 0.6277 0.6079 0.2541 0.180 Uiso 0.380(9) 1 calc PR A 1 H27B H 0.6115 0.5683 0.1557 0.180 Uiso 0.380(9) 1 calc PR A 1 H27C H 0.6692 0.5664 0.1962 0.180 Uiso 0.380(9) 1 calc PR A 1 H25B H 0.5996 0.4933 0.3470 0.144 Uiso 0.620(9) 1 d P A 2 C26B C 0.6674(3) 0.5412(4) 0.3400(7) 0.086(3) Uani 0.620(9) 1 d P A 2 H26D H 0.6575 0.5781 0.3787 0.128 Uiso 0.620(9) 1 calc PR A 2 H26E H 0.6919 0.5526 0.2864 0.128 Uiso 0.620(9) 1 calc PR A 2 H26F H 0.6832 0.5113 0.3867 0.128 Uiso 0.620(9) 1 calc PR A 2 C27B C 0.5800(3) 0.5543(3) 0.2580(5) 0.086(3) Uani 0.620(9) 1 d P A 2 H27E H 0.5788 0.5893 0.3058 0.130 Uiso 0.620(9) 1 calc PR A 2 H27D H 0.5470 0.5332 0.2579 0.130 Uiso 0.620(9) 1 calc PR A 2 H27F H 0.5876 0.5694 0.1888 0.130 Uiso 0.620(9) 1 calc PR A 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 In1 0.04701(15) 0.04452(15) 0.03462(13) 0.00479(15) 0.000 0.000 Cl1 0.0398(5) 0.0636(7) 0.0536(6) 0.0197(5) 0.000 0.000 Cl2 0.1037(9) 0.0629(7) 0.0575(7) -0.0143(6) 0.000 0.000 C1 0.0374(19) 0.029(2) 0.0305(17) 0.0029(13) 0.000 0.000 C2 0.0374(14) 0.0305(14) 0.0408(15) 0.0020(10) -0.0051(12) -0.0015(11) C3 0.0501(17) 0.0574(18) 0.0412(18) 0.0052(13) -0.0118(13) -0.0028(14) C4 0.074(3) 0.075(3) 0.032(2) 0.0061(19) 0.000 0.000 C13 0.0306(13) 0.0398(15) 0.0399(15) 0.0042(11) -0.0082(12) 0.0003(12) C14 0.0342(15) 0.0385(16) 0.0640(19) 0.0021(13) -0.0064(14) 0.0011(13) C15 0.0413(16) 0.0440(18) 0.075(2) 0.0133(16) -0.0030(15) -0.0097(14) C16 0.0361(15) 0.0549(19) 0.0524(18) 0.0087(14) -0.0030(12) -0.0035(14) C17 0.0469(17) 0.0453(18) 0.0547(17) -0.0058(13) 0.0026(14) -0.0018(14) C18 0.0359(15) 0.0389(16) 0.0488(16) 0.0019(12) -0.0059(12) -0.0067(13) C19 0.0450(17) 0.0417(18) 0.078(2) -0.0063(16) 0.0087(16) -0.0060(14) C20 0.137(4) 0.062(2) 0.076(3) 0.017(2) 0.000(2) -0.034(3) C21 0.085(2) 0.045(2) 0.096(3) -0.0095(18) -0.019(2) -0.0062(18) C22 0.0485(19) 0.069(2) 0.066(2) 0.0024(16) 0.0080(15) -0.0108(16) C23 0.051(2) 0.126(4) 0.084(3) 0.001(2) 0.0122(19) 0.010(2) C24 0.092(3) 0.206(5) 0.063(2) -0.014(3) 0.017(2) -0.038(3) C25 0.050(2) 0.045(2) 0.142(4) -0.018(2) 0.003(2) -0.0002(17) C26A 0.127(13) 0.078(10) 0.088(10) -0.025(7) -0.030(9) -0.004(8) C27A 0.166(16) 0.045(6) 0.149(11) -0.011(7) -0.028(10) -0.004(8) C26B 0.083(5) 0.077(6) 0.096(6) -0.030(5) -0.017(4) -0.010(4) C27B 0.113(6) 0.059(4) 0.087(5) -0.034(3) -0.036(4) 0.031(4) _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 In1 C1 2.145(3) . ? In1 Cl2 2.3341(12) . ? In1 Cl1 2.5239(7) . ? In1 Cl1 2.5239(7) 9_665 ? Cl1 In1 2.5239(7) 9_665 ? C1 C2 1.400(3) 12_655 ? C1 C2 1.400(3) . ? C2 C3 1.387(4) . ? C2 C13 1.506(4) . ? C3 C4 1.380(3) . ? C4 C3 1.380(3) 12_655 ? C13 C14 1.393(3) . ? C13 C18 1.402(3) . ? C14 C15 1.394(4) . ? C14 C25 1.541(4) . ? C15 C16 1.375(4) . ? C16 C17 1.383(4) . ? C16 C22 1.524(4) . ? C17 C18 1.384(4) . ? C18 C19 1.521(4) . ? C19 C20 1.517(5) . ? C19 C21 1.523(4) . ? C22 C23 1.499(4) . ? C22 C24 1.511(5) . ? C25 C26A 1.406(13) . ? C25 C27B 1.410(6) . ? C25 C26B 1.523(8) . ? C25 C27A 1.573(14) . ? 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 In1 Cl2 128.19(9) . . ? C1 In1 Cl1 119.01(6) . . ? Cl2 In1 Cl1 98.51(2) . . ? C1 In1 Cl1 119.01(6) . 9_665 ? Cl2 In1 Cl1 98.51(2) . 9_665 ? Cl1 In1 Cl1 83.15(3) . 9_665 ? In1 Cl1 In1 96.85(3) . 9_665 ? C2 C1 C2 121.3(3) 12_655 . ? C2 C1 In1 119.37(15) 12_655 . ? C2 C1 In1 119.37(15) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 C13 121.6(2) . . ? C1 C2 C13 119.9(2) . . ? C4 C3 C2 120.8(3) . . ? C3 C4 C3 120.3(4) 12_655 . ? C14 C13 C18 120.5(2) . . ? C14 C13 C2 120.8(2) . . ? C18 C13 C2 118.7(2) . . ? C15 C14 C13 117.9(3) . . ? C15 C14 C25 120.3(3) . . ? C13 C14 C25 121.7(3) . . ? C16 C15 C14 123.1(3) . . ? C15 C16 C17 117.4(3) . . ? C15 C16 C22 122.2(3) . . ? C17 C16 C22 120.4(3) . . ? C16 C17 C18 122.3(3) . . ? C17 C18 C13 118.7(2) . . ? C17 C18 C19 119.4(3) . . ? C13 C18 C19 121.6(2) . . ? C18 C19 C20 109.7(3) . . ? C18 C19 C21 114.5(3) . . ? C20 C19 C21 110.0(3) . . ? C23 C22 C24 111.3(3) . . ? C23 C22 C16 111.1(2) . . ? C24 C22 C16 112.4(3) . . ? C26A C25 C27B 126.0(7) . . ? C26A C25 C26B 39.6(6) . . ? C27B C25 C26B 116.2(5) . . ? C26A C25 C14 113.4(6) . . ? C27B C25 C14 119.8(4) . . ? C26B C25 C14 115.0(4) . . ? C26A C25 C27A 113.0(8) . . ? C27B C25 C27A 60.0(6) . . ? C26B C25 C27A 75.5(6) . . ? C14 C25 C27A 106.5(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.711 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.065 data_bt47z _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Bert*Ga(mu-OH)Cl]2 2 C6H6' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H112 Cl2 Ga2 O2' _chemical_formula_weight 1364.08 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' 'O' 'O' 0.0106 0.0060 '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 'P2 (1)/c' 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 14.2605(10) _cell_length_b 15.9037(10) _cell_length_c 18.0905(12) _cell_angle_alpha 90.00 _cell_angle_beta 108.613(2) _cell_angle_gamma 90.00 _cell_volume 3888.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 4086 _cell_measurement_theta_min 0 _cell_measurement_theta_max 31.5 _exptl_crystal_description 'cube' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.8555 _exptl_absorpt_correction_T_max 0.9095 _exptl_absorpt_process_details ;Blessing, R.H., Acta Cryst. (1995), A51, 33-38. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19629 _diffrn_reflns_av_R_equivalents 0.1720 _diffrn_reflns_av_sigmaI/netI 0.1754 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5074 _reflns_number_gt 2371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5074 _refine_ls_number_parameters 419 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1533 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.10130(5) 0.01630(4) 0.05131(4) 0.0500(2) Uani 1 1 d . . . Cl1 Cl 0.09834(15) 0.06630(12) 0.16075(11) 0.0896(7) Uani 1 1 d . . . H1 H 0.008(4) -0.080(3) 0.0791(14) 0.05(2) Uiso 1 1 d D . . O1 O 0.0041(3) -0.0727(2) 0.0247(2) 0.0514(12) Uani 1 1 d D . . C1 C 0.2190(4) -0.0049(4) 0.0216(3) 0.0406(16) Uani 1 1 d . . . C2 C 0.2549(4) 0.0561(4) -0.0179(4) 0.0401(17) Uani 1 1 d . . . C3 C 0.3310(5) 0.0381(4) -0.0452(4) 0.0528(19) Uani 1 1 d . . . H3A H 0.3550 0.0794 -0.0708 0.063 Uiso 1 1 calc R . . C4 C 0.3727(5) -0.0406(4) -0.0352(4) 0.058(2) Uani 1 1 d . . . H4A H 0.4220 -0.0530 -0.0570 0.069 Uiso 1 1 calc R . . C5 C 0.3429(5) -0.1010(4) 0.0064(4) 0.0486(18) Uani 1 1 d . . . H5A H 0.3744 -0.1530 0.0151 0.058 Uiso 1 1 calc R . . C6 C 0.2655(4) -0.0850(4) 0.0359(4) 0.0400(17) Uani 1 1 d . . . C7 C 0.2406(5) -0.1513(4) 0.0857(5) 0.0488(18) Uani 1 1 d . . . C8 C 0.1853(5) -0.2227(5) 0.0519(5) 0.055(2) Uani 1 1 d . . . C9 C 0.1774(5) -0.2869(4) 0.1029(6) 0.071(2) Uani 1 1 d . . . H9A H 0.1399 -0.3341 0.0816 0.086 Uiso 1 1 calc R . . C10 C 0.2216(7) -0.2842(6) 0.1817(6) 0.083(3) Uani 1 1 d . . . C11 C 0.2698(6) -0.2121(6) 0.2124(5) 0.081(3) Uani 1 1 d . . . H11A H 0.2950 -0.2074 0.2664 0.097 Uiso 1 1 calc R . . C12 C 0.2833(5) -0.1446(5) 0.1670(5) 0.065(2) Uani 1 1 d . . . C13 C 0.2159(4) 0.1455(4) -0.0249(4) 0.0411(17) Uani 1 1 d . . . C14 C 0.1496(5) 0.1762(4) -0.0946(4) 0.0449(18) Uani 1 1 d . . . C15 C 0.1213(5) 0.2604(4) -0.0990(4) 0.059(2) Uani 1 1 d . . . H15A H 0.0771 0.2804 -0.1454 0.071 Uiso 1 1 calc R . . C16 C 0.1565(5) 0.3147(4) -0.0374(5) 0.055(2) Uani 1 1 d . . . C17 C 0.2208(5) 0.2837(4) 0.0305(4) 0.058(2) Uani 1 1 d . . . H17A H 0.2447 0.3200 0.0726 0.070 Uiso 1 1 calc R . . C18 C 0.2521(5) 0.2002(5) 0.0393(4) 0.0527(19) Uani 1 1 d . . . C19 C 0.3271(7) 0.1720(4) 0.1166(5) 0.087(3) Uani 1 1 d . . . H19A H 0.3196 0.1110 0.1199 0.105 Uiso 1 1 calc R . . C20 C 0.4320(6) 0.1875(6) 0.1164(5) 0.151(4) Uani 1 1 d . . . H20A H 0.4780 0.1629 0.1621 0.227 Uiso 1 1 calc R . . H20B H 0.4438 0.2470 0.1161 0.227 Uiso 1 1 calc R . . H20C H 0.4408 0.1625 0.0707 0.227 Uiso 1 1 calc R . . C21 C 0.3091(7) 0.2101(5) 0.1883(4) 0.127(4) Uani 1 1 d . . . H21A H 0.3418 0.1767 0.2334 0.191 Uiso 1 1 calc R . . H21B H 0.2393 0.2112 0.1807 0.191 Uiso 1 1 calc R . . H21C H 0.3347 0.2664 0.1960 0.191 Uiso 1 1 calc R . . C22 C 0.1217(6) 0.4066(5) -0.0470(5) 0.095(3) Uani 1 1 d . . . H22A H 0.0497 0.4057 -0.0713 0.114 Uiso 1 1 calc R . . C23 C 0.1421(6) 0.4537(4) 0.0255(5) 0.124(3) Uani 1 1 d . . . H23A H 0.1139 0.5089 0.0146 0.187 Uiso 1 1 calc R . . H23B H 0.2123 0.4582 0.0500 0.187 Uiso 1 1 calc R . . H23C H 0.1135 0.4249 0.0598 0.187 Uiso 1 1 calc R . . C24 C 0.1641(7) 0.4482(5) -0.1038(5) 0.145(4) Uani 1 1 d . . . H24A H 0.1315 0.5010 -0.1200 0.218 Uiso 1 1 calc R . . H24B H 0.1542 0.4125 -0.1485 0.218 Uiso 1 1 calc R . . H24C H 0.2336 0.4575 -0.0793 0.218 Uiso 1 1 calc R . . C25 C 0.1117(5) 0.1211(4) -0.1673(4) 0.0543(19) Uani 1 1 d . . . H25A H 0.1209 0.0624 -0.1501 0.065 Uiso 1 1 calc R . . C26 C 0.0014(5) 0.1335(4) -0.2113(3) 0.080(2) Uani 1 1 d . . . H26A H -0.0337 0.1418 -0.1746 0.120 Uiso 1 1 calc R . . H26B H -0.0240 0.0846 -0.2424 0.120 Uiso 1 1 calc R . . H26C H -0.0071 0.1818 -0.2446 0.120 Uiso 1 1 calc R . . C27 C 0.1728(5) 0.1355(4) -0.2212(4) 0.094(3) Uani 1 1 d . . . H27A H 0.2403 0.1200 -0.1950 0.140 Uiso 1 1 calc R . . H27B H 0.1697 0.1938 -0.2355 0.140 Uiso 1 1 calc R . . H27C H 0.1469 0.1018 -0.2673 0.140 Uiso 1 1 calc R . . C28 C 0.1404(6) -0.2311(4) -0.0357(5) 0.065(2) Uani 1 1 d . . . H28A H 0.1386 -0.1749 -0.0583 0.078 Uiso 1 1 calc R . . C29 C 0.2020(6) -0.2858(5) -0.0690(4) 0.091(3) Uani 1 1 d . . . H29A H 0.2669 -0.2619 -0.0577 0.136 Uiso 1 1 calc R . . H29B H 0.1716 -0.2899 -0.1245 0.136 Uiso 1 1 calc R . . H29C H 0.2072 -0.3409 -0.0463 0.136 Uiso 1 1 calc R . . C30 C 0.0320(5) -0.2646(4) -0.0600(4) 0.088(3) Uani 1 1 d . . . H30A H -0.0055 -0.2318 -0.0348 0.132 Uiso 1 1 calc R . . H30B H 0.0323 -0.3224 -0.0445 0.132 Uiso 1 1 calc R . . H30C H 0.0026 -0.2602 -0.1155 0.132 Uiso 1 1 calc R . . C31 C 0.2166(5) -0.3593(4) 0.2335(3) 0.129(4) Uani 1 1 d . . . H31A H 0.2517 -0.3319 0.2831 0.155 Uiso 1 1 calc R . . C32 C 0.2930(5) -0.4216(4) 0.2373(3) 0.111(3) Uani 1 1 d R . . H32A H 0.2830 -0.4700 0.2656 0.166 Uiso 1 1 calc R . . H32B H 0.3569 -0.3979 0.2634 0.166 Uiso 1 1 calc R . . H32C H 0.2895 -0.4380 0.1854 0.166 Uiso 1 1 calc R . . C33 C 0.1323(7) -0.3726(5) 0.2494(6) 0.159(5) Uani 1 1 d . . . H33A H 0.1448 -0.4099 0.2933 0.238 Uiso 1 1 calc R . . H33B H 0.0843 -0.3975 0.2049 0.238 Uiso 1 1 calc R . . H33C H 0.1075 -0.3201 0.2615 0.238 Uiso 1 1 calc R . . C34 C 0.3467(6) -0.0712(5) 0.2079(4) 0.080(2) Uani 1 1 d . . . H34A H 0.3267 -0.0226 0.1731 0.096 Uiso 1 1 calc R . . C35 C 0.4549(6) -0.0854(5) 0.2201(5) 0.130(4) Uani 1 1 d . . . H35A H 0.4644 -0.0967 0.1708 0.194 Uiso 1 1 calc R . . H35B H 0.4778 -0.1325 0.2543 0.194 Uiso 1 1 calc R . . H35C H 0.4917 -0.0361 0.2429 0.194 Uiso 1 1 calc R . . C36 C 0.3316(6) -0.0463(5) 0.2858(4) 0.121(3) Uani 1 1 d . . . H36A H 0.2621 -0.0429 0.2788 0.182 Uiso 1 1 calc R . . H36B H 0.3618 0.0074 0.3023 0.182 Uiso 1 1 calc R . . H36C H 0.3615 -0.0878 0.3246 0.182 Uiso 1 1 calc R . . C50 C 0.4575(11) 0.2234(6) 0.3868(6) 0.115(3) Uani 1 1 d . . . H50A H 0.4271 0.2665 0.3530 0.137 Uiso 1 1 calc R . . C51 C 0.5431(10) 0.1890(10) 0.3804(7) 0.122(4) Uani 1 1 d . . . H51A H 0.5724 0.2095 0.3448 0.146 Uiso 1 1 calc R . . C52 C 0.5828(9) 0.1236(9) 0.4286(9) 0.143(5) Uani 1 1 d . . . H52A H 0.6379 0.0964 0.4230 0.171 Uiso 1 1 calc R . . C55 C 0.4165(9) 0.1978(9) 0.4389(9) 0.154(5) Uani 1 1 d . . . H55A H 0.3603 0.2245 0.4428 0.185 Uiso 1 1 calc R . . C53 C 0.5454(11) 0.0966(8) 0.4841(9) 0.174(6) Uani 1 1 d . . . H53A H 0.5778 0.0554 0.5196 0.209 Uiso 1 1 calc R . . C54 C 0.4573(12) 0.1317(10) 0.4871(9) 0.189(6) Uani 1 1 d . . . H54A H 0.4265 0.1106 0.5214 0.227 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 0.0493(4) 0.0506(5) 0.0530(5) 0.0005(5) 0.0204(4) 0.0057(5) Cl1 0.1131(18) 0.0963(17) 0.0704(15) -0.0161(12) 0.0446(13) 0.0086(13) O1 0.034(3) 0.065(3) 0.052(4) 0.003(3) 0.009(3) 0.003(2) C1 0.049(4) 0.028(5) 0.044(4) -0.004(3) 0.014(3) -0.006(4) C2 0.041(5) 0.025(5) 0.054(5) -0.009(3) 0.015(4) 0.000(3) C3 0.057(5) 0.029(5) 0.078(5) 0.011(4) 0.030(4) 0.007(4) C4 0.052(5) 0.052(6) 0.081(6) -0.008(4) 0.037(4) 0.000(4) C5 0.049(5) 0.038(5) 0.059(5) -0.003(4) 0.017(4) 0.009(4) C6 0.036(4) 0.032(5) 0.049(5) 0.000(4) 0.010(4) 0.000(3) C7 0.051(5) 0.034(5) 0.062(6) 0.006(4) 0.020(4) 0.013(4) C8 0.054(5) 0.043(6) 0.066(6) 0.003(5) 0.016(5) 0.005(4) C9 0.076(6) 0.040(6) 0.113(8) 0.023(6) 0.051(6) 0.006(4) C10 0.128(9) 0.057(7) 0.084(8) 0.046(6) 0.062(7) 0.035(6) C11 0.111(8) 0.074(7) 0.067(7) 0.024(6) 0.042(6) 0.026(6) C12 0.072(6) 0.071(7) 0.049(6) 0.016(5) 0.016(5) 0.018(5) C13 0.035(4) 0.037(5) 0.053(5) -0.001(4) 0.017(4) -0.005(4) C14 0.055(5) 0.031(5) 0.048(5) -0.004(4) 0.016(4) -0.004(4) C15 0.080(6) 0.030(5) 0.060(6) -0.002(4) 0.010(4) 0.012(4) C16 0.080(6) 0.027(5) 0.062(6) 0.001(4) 0.026(5) -0.003(4) C17 0.082(6) 0.029(6) 0.061(6) -0.013(4) 0.018(5) 0.000(4) C18 0.062(5) 0.034(5) 0.059(6) 0.000(4) 0.015(4) -0.001(4) C19 0.117(8) 0.050(6) 0.068(7) 0.002(5) -0.007(6) 0.010(5) C20 0.064(7) 0.192(11) 0.153(10) -0.046(8) -0.028(7) 0.035(7) C21 0.204(11) 0.101(7) 0.055(7) -0.016(5) 0.011(7) -0.008(7) C22 0.146(8) 0.029(6) 0.089(7) -0.001(5) 0.008(6) 0.004(5) C23 0.183(10) 0.042(6) 0.153(9) -0.010(6) 0.061(7) 0.013(5) C24 0.292(14) 0.042(6) 0.132(9) 0.010(5) 0.108(9) -0.002(7) C25 0.081(6) 0.028(5) 0.049(5) 0.005(4) 0.014(5) 0.001(4) C26 0.081(6) 0.086(6) 0.053(5) 0.008(4) -0.007(5) -0.020(5) C27 0.128(8) 0.101(7) 0.063(6) -0.007(5) 0.045(5) 0.013(5) C28 0.073(6) 0.042(5) 0.074(6) 0.005(4) 0.015(5) 0.000(4) C29 0.108(7) 0.084(6) 0.084(7) -0.014(5) 0.035(6) -0.002(5) C30 0.069(6) 0.067(6) 0.116(7) -0.025(5) 0.011(5) -0.004(5) C31 0.141(10) 0.086(8) 0.205(11) 0.082(7) 0.116(9) 0.042(7) C32 0.119(8) 0.083(7) 0.131(8) 0.049(6) 0.041(6) 0.018(6) C33 0.131(9) 0.118(9) 0.249(13) 0.109(8) 0.091(9) 0.014(7) C34 0.099(7) 0.071(6) 0.047(6) -0.001(4) -0.008(5) 0.003(5) C35 0.076(7) 0.148(9) 0.146(9) -0.035(7) 0.009(6) -0.020(6) C36 0.156(9) 0.122(8) 0.066(7) -0.024(5) 0.007(6) 0.028(6) C50 0.126(12) 0.127(9) 0.080(9) -0.017(7) 0.019(7) -0.008(8) C51 0.096(10) 0.158(13) 0.126(11) -0.033(9) 0.059(9) -0.026(8) C52 0.141(12) 0.125(12) 0.152(14) 0.014(9) 0.033(10) 0.005(9) C55 0.164(12) 0.167(14) 0.177(14) 0.013(10) 0.118(12) 0.024(10) C53 0.145(13) 0.181(13) 0.207(16) 0.074(11) 0.072(11) 0.057(10) C54 0.170(15) 0.180(15) 0.259(18) 0.074(12) 0.126(13) 0.038(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 O1 1.906(4) 3 ? Ga1 O1 1.932(4) . ? Ga1 C1 1.949(5) . ? Ga1 Cl1 2.1465(19) . ? Ga1 Ga1 2.9392(15) 3 ? O1 Ga1 1.906(4) 3 ? C1 C2 1.395(7) . ? C1 C6 1.421(7) . ? C2 C3 1.358(7) . ? C2 C13 1.517(7) . ? C3 C4 1.372(7) . ? C4 C5 1.371(7) . ? C5 C6 1.394(7) . ? C6 C7 1.501(8) . ? C7 C12 1.405(8) . ? C7 C8 1.406(8) . ? C8 C9 1.404(8) . ? C8 C28 1.514(9) . ? C9 C10 1.363(9) . ? C10 C11 1.360(10) . ? C10 C31 1.534(8) . ? C11 C12 1.402(9) . ? C12 C34 1.517(9) . ? C13 C14 1.400(7) . ? C13 C18 1.411(8) . ? C14 C15 1.392(7) . ? C14 C25 1.529(8) . ? C15 C16 1.373(8) . ? C16 C17 1.368(8) . ? C16 C22 1.535(9) . ? C17 C18 1.393(8) . ? C18 C19 1.531(9) . ? C19 C20 1.518(10) . ? C19 C21 1.527(9) . ? C22 C23 1.456(9) . ? C22 C24 1.503(9) . ? C25 C27 1.519(7) . ? C25 C26 1.531(7) . ? C28 C29 1.494(8) . ? C28 C30 1.559(8) . ? C31 C33 1.339(8) . ? C31 C32 1.4581 . ? C34 C35 1.505(9) . ? C34 C36 1.543(9) . ? C50 C55 1.322(11) . ? C50 C51 1.376(12) . ? C51 C52 1.359(12) . ? C52 C53 1.349(13) . ? C55 C54 1.372(14) . ? C53 C54 1.392(13) . ? 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 O1 Ga1 O1 80.06(19) 3 . ? O1 Ga1 C1 115.6(2) 3 . ? O1 Ga1 C1 114.7(2) . . ? O1 Ga1 Cl1 104.33(14) 3 . ? O1 Ga1 Cl1 106.13(14) . . ? C1 Ga1 Cl1 126.23(17) . . ? O1 Ga1 Ga1 40.35(12) 3 3 ? O1 Ga1 Ga1 39.70(12) . 3 ? C1 Ga1 Ga1 123.70(16) . 3 ? Cl1 Ga1 Ga1 110.07(7) . 3 ? Ga1 O1 Ga1 99.94(19) 3 . ? C2 C1 C6 119.4(5) . . ? C2 C1 Ga1 120.7(5) . . ? C6 C1 Ga1 119.8(5) . . ? C3 C2 C1 120.3(6) . . ? C3 C2 C13 118.8(6) . . ? C1 C2 C13 120.7(5) . . ? C2 C3 C4 120.6(6) . . ? C5 C4 C3 120.9(6) . . ? C4 C5 C6 120.3(6) . . ? C5 C6 C1 118.3(6) . . ? C5 C6 C7 117.9(6) . . ? C1 C6 C7 123.7(6) . . ? C12 C7 C8 120.8(7) . . ? C12 C7 C6 117.9(7) . . ? C8 C7 C6 121.0(7) . . ? C9 C8 C7 117.0(7) . . ? C9 C8 C28 121.9(7) . . ? C7 C8 C28 121.1(7) . . ? C10 C9 C8 123.8(8) . . ? C11 C10 C9 117.3(7) . . ? C11 C10 C31 121.5(9) . . ? C9 C10 C31 121.2(9) . . ? C10 C11 C12 123.5(8) . . ? C11 C12 C7 117.4(8) . . ? C11 C12 C34 118.4(8) . . ? C7 C12 C34 124.2(7) . . ? C14 C13 C18 119.3(6) . . ? C14 C13 C2 121.8(6) . . ? C18 C13 C2 118.8(6) . . ? C15 C14 C13 119.2(6) . . ? C15 C14 C25 119.0(6) . . ? C13 C14 C25 121.7(6) . . ? C16 C15 C14 122.2(6) . . ? C17 C16 C15 117.9(6) . . ? C17 C16 C22 123.0(7) . . ? C15 C16 C22 119.1(7) . . ? C16 C17 C18 123.0(6) . . ? C17 C18 C13 118.3(6) . . ? C17 C18 C19 119.2(7) . . ? C13 C18 C19 122.4(6) . . ? C20 C19 C21 111.8(7) . . ? C20 C19 C18 110.6(7) . . ? C21 C19 C18 113.7(7) . . ? C23 C22 C24 112.5(7) . . ? C23 C22 C16 115.0(7) . . ? C24 C22 C16 108.0(7) . . ? C27 C25 C14 110.4(6) . . ? C27 C25 C26 110.5(6) . . ? C14 C25 C26 113.4(5) . . ? C29 C28 C8 111.6(6) . . ? C29 C28 C30 110.2(6) . . ? C8 C28 C30 112.0(6) . . ? C33 C31 C32 126.2(4) . . ? C33 C31 C10 118.3(7) . . ? C32 C31 C10 112.3(4) . . ? C35 C34 C12 112.3(7) . . ? C35 C34 C36 109.9(6) . . ? C12 C34 C36 114.1(7) . . ? C55 C50 C51 123.0(12) . . ? C52 C51 C50 116.6(13) . . ? C53 C52 C51 122.6(14) . . ? C50 C55 C54 119.7(13) . . ? C52 C53 C54 118.5(14) . . ? C55 C54 C53 119.1(14) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.655 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.065