Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Kieran Molloy' 'Leonardo Apostolico' 'R. Binions' 'Christopher S. Blackman' 'Claire J. Carmalt' 'M. Mahon' 'Ivan P. Parkin' _publ_contact_author_name 'Dr Kieran Molloy' _publ_contact_author_address ; Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_email CHSKCM@BATH.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The reaction of GeCl4 with primary and secondary phosphines ; data_k01kcm19 _database_code_CSD 207700 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cl3 Ge P' _chemical_formula_weight 366.13 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.2760(2) _cell_length_b 14.4920(3) _cell_length_c 10.3050(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.6530(9) _cell_angle_gamma 90.00 _cell_volume 1491.25(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 2.674 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 1.158 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details ; Sortav Blessing (1995) multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27361 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 30.02 _reflns_number_total 4344 _reflns_number_gt 3296 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0391P)^2^+0.1583P] 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 SHELXL _refine_ls_extinction_coef 0.0056(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4344 _refine_ls_number_parameters 163 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.025 _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 Ge1 Ge 0.31977(2) 0.092503(16) 0.44909(2) 0.02839(9) Uani 1 1 d . . . P1 P 0.14377(5) 0.35813(4) 0.35280(5) 0.02053(12) Uani 1 1 d D . . H1A H 0.193(2) 0.3427(17) 0.4815(17) 0.043(7) Uiso 1 1 d D . . H1B H 0.180(2) 0.2854(15) 0.284(2) 0.041(7) Uiso 1 1 d D . . Cl1 Cl 0.23113(6) 0.11082(4) 0.22365(5) 0.03465(14) Uani 1 1 d . . . Cl2 Cl 0.12959(5) 0.15218(4) 0.50179(5) 0.03253(14) Uani 1 1 d . . . Cl3 Cl 0.43683(5) 0.22981(4) 0.47840(6) 0.03820(15) Uani 1 1 d . . . C1 C -0.03426(19) 0.36301(13) 0.3255(2) 0.0220(4) Uani 1 1 d . . . C2 C -0.0921(2) 0.36623(15) 0.4355(2) 0.0278(4) Uani 1 1 d . . . H2 H -0.0372 0.3698 0.5235 0.033 Uiso 1 1 calc R . . C3 C -0.2303(2) 0.36422(16) 0.4148(2) 0.0306(5) Uani 1 1 d . . . H3 H -0.2705 0.3667 0.4888 0.037 Uiso 1 1 calc R . . C4 C -0.3100(2) 0.35863(14) 0.2861(2) 0.0298(5) Uani 1 1 d . . . H4 H -0.4047 0.3562 0.2724 0.036 Uiso 1 1 calc R . . C5 C -0.2527(2) 0.35658(15) 0.1776(2) 0.0300(5) Uani 1 1 d . . . H5 H -0.3082 0.3538 0.0898 0.036 Uiso 1 1 calc R . . C6 C -0.1149(2) 0.35851(15) 0.1961(2) 0.0276(4) Uani 1 1 d . . . H6 H -0.0756 0.3568 0.1214 0.033 Uiso 1 1 calc R . . C7 C 0.21886(19) 0.46174(14) 0.30995(18) 0.0216(4) Uani 1 1 d . . . C8 C 0.1442(2) 0.53462(14) 0.2430(2) 0.0266(4) Uani 1 1 d . . . H8 H 0.0491 0.5319 0.2205 0.032 Uiso 1 1 calc R . . C9 C 0.2098(2) 0.61155(15) 0.2094(2) 0.0303(5) Uani 1 1 d . . . H9 H 0.1596 0.6618 0.1638 0.036 Uiso 1 1 calc R . . C10 C 0.3481(2) 0.61526(15) 0.2420(2) 0.0313(5) Uani 1 1 d . . . H10 H 0.3923 0.6680 0.2185 0.038 Uiso 1 1 calc R . . C11 C 0.4226(2) 0.54292(16) 0.3085(2) 0.0333(5) Uani 1 1 d . . . H11 H 0.5176 0.5461 0.3306 0.040 Uiso 1 1 calc R . . C12 C 0.3590(2) 0.46579(15) 0.3432(2) 0.0287(4) Uani 1 1 d . . . H12 H 0.4099 0.4160 0.3891 0.034 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 Ge1 0.02963(14) 0.02759(13) 0.02555(13) 0.00459(9) 0.00169(9) 0.00567(9) P1 0.0175(2) 0.0239(3) 0.0205(2) 0.00063(19) 0.00509(19) -0.00045(19) Cl1 0.0397(3) 0.0413(3) 0.0230(2) 0.0004(2) 0.0074(2) 0.0095(2) Cl2 0.0328(3) 0.0407(3) 0.0273(2) 0.0040(2) 0.0134(2) -0.0032(2) Cl3 0.0205(2) 0.0366(3) 0.0536(3) -0.0014(3) 0.0009(2) 0.0014(2) C1 0.0179(9) 0.0221(9) 0.0265(9) -0.0015(8) 0.0067(8) -0.0004(7) C2 0.0279(11) 0.0303(11) 0.0268(10) -0.0030(9) 0.0098(8) -0.0004(9) C3 0.0288(11) 0.0335(11) 0.0344(11) -0.0045(9) 0.0174(9) 0.0006(9) C4 0.0187(10) 0.0263(10) 0.0454(13) -0.0036(9) 0.0101(9) -0.0006(8) C5 0.0234(10) 0.0337(11) 0.0305(10) -0.0013(9) 0.0017(8) -0.0041(9) C6 0.0236(10) 0.0356(12) 0.0245(10) -0.0029(9) 0.0072(8) -0.0042(8) C7 0.0208(9) 0.0243(9) 0.0210(8) -0.0030(8) 0.0073(7) -0.0016(8) C8 0.0232(10) 0.0283(10) 0.0271(10) -0.0024(8) 0.0035(8) 0.0001(8) C9 0.0342(12) 0.0253(10) 0.0307(11) 0.0024(9) 0.0062(9) 0.0004(9) C10 0.0369(12) 0.0265(10) 0.0346(11) -0.0036(9) 0.0165(10) -0.0073(9) C11 0.0222(10) 0.0337(12) 0.0460(13) -0.0015(10) 0.0119(9) -0.0038(9) C12 0.0214(10) 0.0268(10) 0.0389(11) 0.0019(9) 0.0090(9) 0.0021(8) _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 Ge1 Cl1 2.3017(6) . ? Ge1 Cl3 2.3078(6) . ? Ge1 Cl2 2.3158(6) . ? P1 H1A 1.323(16) . ? P1 H1B 1.368(16) . ? P1 C1 1.7856(19) . ? P1 C7 1.790(2) . ? C1 C6 1.396(3) . ? C1 C2 1.400(3) . ? C2 C3 1.386(3) . ? C3 C4 1.387(3) . ? C4 C5 1.382(3) . ? C5 C6 1.383(3) . ? C7 C8 1.390(3) . ? C7 C12 1.400(3) . ? C8 C9 1.389(3) . ? C9 C10 1.382(3) . ? C10 C11 1.381(3) . ? C11 C12 1.383(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ge1 Cl3 95.88(2) . . ? Cl1 Ge1 Cl2 92.22(2) . . ? Cl3 Ge1 Cl2 95.16(2) . . ? H1A P1 H1B 107.4(15) . . ? H1A P1 C1 107.5(11) . . ? H1B P1 C1 110.2(10) . . ? H1A P1 C7 107.7(11) . . ? H1B P1 C7 109.4(11) . . ? C1 P1 C7 114.40(9) . . ? C6 C1 C2 120.38(18) . . ? C6 C1 P1 120.24(15) . . ? C2 C1 P1 119.28(15) . . ? C3 C2 C1 119.4(2) . . ? C2 C3 C4 120.08(19) . . ? C5 C4 C3 120.44(19) . . ? C4 C5 C6 120.4(2) . . ? C5 C6 C1 119.32(19) . . ? C8 C7 C12 120.34(19) . . ? C8 C7 P1 122.70(15) . . ? C12 C7 P1 116.93(15) . . ? C9 C8 C7 119.34(19) . . ? C10 C9 C8 120.2(2) . . ? C11 C10 C9 120.6(2) . . ? C10 C11 C12 120.1(2) . . ? C11 C12 C7 119.5(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.565 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.097 data_k01kcm21 _database_code_CSD 207701 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H14 Cl3 Ge P' _chemical_formula_weight 296.08 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.2955(9) _cell_length_b 6.1385(2) _cell_length_c 12.9839(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.9990(10) _cell_angle_gamma 90.00 _cell_volume 2342.89(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 3.381 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5512 _exptl_absorpt_correction_T_max 0.6310 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11615 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2664 _reflns_number_gt 2074 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0426P)^2^+0.8790P] 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 SHELXL _refine_ls_extinction_coef 0.00125(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2664 _refine_ls_number_parameters 113 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.011 _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 Ge1 Ge 0.045030(10) 0.02040(5) 0.91410(2) 0.02747(13) Uani 1 1 d . . . P1 P -0.09210(3) 0.46208(11) 0.83073(6) 0.02794(19) Uani 1 1 d D . . H1A H -0.0540(9) 0.498(5) 0.796(3) 0.045(10) Uiso 1 1 d D . . H1B H -0.1020(12) 0.645(4) 0.880(3) 0.062(11) Uiso 1 1 d D . . H1C H -0.0858(12) 0.300(4) 0.906(2) 0.055(11) Uiso 1 1 d D . . Cl2 Cl 0.05984(2) -0.01943(10) 0.74746(6) 0.02798(18) Uani 1 1 d . . . Cl3 Cl 0.12232(2) 0.04093(11) 1.00505(6) 0.03073(18) Uani 1 1 d . . . Cl1 Cl 0.03577(2) 0.39382(12) 0.90425(6) 0.0333(2) Uani 1 1 d . . . C1 C -0.14098(9) 0.4052(4) 0.7239(2) 0.0243(6) Uani 1 1 d . . . H1 H -0.1345 0.2704 0.6868 0.029 Uiso 1 1 calc R . . C2 C -0.18220(12) 0.3606(8) 0.7694(3) 0.0534(10) Uani 1 1 d . . . H2A H -0.1880 0.4882 0.8109 0.064 Uiso 1 1 calc R . . H2B H -0.1759 0.2334 0.8177 0.064 Uiso 1 1 calc R . . C3 C -0.22425(13) 0.3151(8) 0.6791(3) 0.0725(15) Uani 1 1 d . . . H3A H -0.2196 0.1777 0.6431 0.087 Uiso 1 1 calc R . . H3B H -0.2511 0.2958 0.7091 0.087 Uiso 1 1 calc R . . C4 C -0.23340(12) 0.4965(6) 0.5992(3) 0.0478(9) Uani 1 1 d . . . H4A H -0.2596 0.4570 0.5403 0.057 Uiso 1 1 calc R . . H4B H -0.2414 0.6302 0.6332 0.057 Uiso 1 1 calc R . . C5 C -0.19278(12) 0.5409(5) 0.5555(3) 0.0399(8) Uani 1 1 d . . . H5A H -0.1993 0.6665 0.5064 0.048 Uiso 1 1 calc R . . H5B H -0.1869 0.4126 0.5146 0.048 Uiso 1 1 calc R . . C6 C -0.15062(12) 0.5896(6) 0.6431(3) 0.0423(8) Uani 1 1 d . . . H6A H -0.1552 0.7270 0.6791 0.051 Uiso 1 1 calc R . . H6B H -0.1242 0.6091 0.6117 0.051 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 Ge1 0.0297(2) 0.02718(19) 0.02633(19) 0.00167(12) 0.00837(14) 0.00062(11) P1 0.0301(4) 0.0240(4) 0.0254(4) 0.0020(3) -0.0016(3) 0.0014(3) Cl2 0.0315(4) 0.0256(3) 0.0266(4) -0.0024(3) 0.0065(3) 0.0013(3) Cl3 0.0323(4) 0.0319(4) 0.0262(4) 0.0031(3) 0.0037(3) 0.0056(3) Cl1 0.0352(4) 0.0291(4) 0.0321(4) -0.0048(3) 0.0015(3) 0.0082(3) C1 0.0257(15) 0.0276(14) 0.0170(13) -0.0018(11) 0.0000(11) 0.0023(11) C2 0.036(2) 0.088(3) 0.034(2) 0.0226(19) 0.0030(16) -0.0092(18) C3 0.042(2) 0.109(4) 0.056(3) 0.036(2) -0.0105(19) -0.035(2) C4 0.0339(19) 0.069(3) 0.035(2) -0.0017(16) -0.0023(15) 0.0079(16) C5 0.0418(19) 0.0392(18) 0.0320(18) 0.0099(13) -0.0039(15) 0.0008(14) C6 0.0427(19) 0.0423(18) 0.0361(19) 0.0137(15) -0.0019(15) -0.0064(15) _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 Ge1 Cl1 2.3091(8) . ? Ge1 Cl2 2.3264(8) . ? Ge1 Cl3 2.3571(8) . ? P1 H1A 1.358(18) . ? P1 H1B 1.359(18) . ? P1 H1C 1.371(18) . ? P1 C1 1.802(3) . ? C1 C6 1.523(4) . ? C1 C2 1.530(4) . ? C2 C3 1.534(5) . ? C3 C4 1.501(5) . ? C4 C5 1.499(5) . ? C5 C6 1.521(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ge1 Cl2 95.80(3) . . ? Cl1 Ge1 Cl3 93.86(3) . . ? Cl2 Ge1 Cl3 94.58(3) . . ? H1A P1 H1B 109(2) . . ? H1A P1 H1C 112(2) . . ? H1B P1 H1C 106(2) . . ? H1A P1 C1 112.4(17) . . ? H1B P1 C1 106.7(15) . . ? H1C P1 C1 110.8(15) . . ? C6 C1 C2 111.2(3) . . ? C6 C1 P1 111.8(2) . . ? C2 C1 P1 109.4(2) . . ? C1 C2 C3 110.0(3) . . ? C4 C3 C2 111.9(3) . . ? C5 C4 C3 111.4(3) . . ? C4 C5 C6 111.8(3) . . ? C5 C6 C1 110.8(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.617 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.091