data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof W Levason' _publ_contact_author_email WXL@SOTON.AC.UK _publ_section_title ; Complexes of germanium(IV) fluoride with phosphane ligands: Structural and spectroscopic authentication of germanium(IV) phosphane complexes ; loop_ _publ_author_name 'W Levason' 'Martin F. Davis' 'Gillian Reid' 'Michael Webster' # Attachment 'Ge_all6rev.cif' # Manuscript ref.: B716765B # Title: Complexes of germanium(IV) fluoride with phosphane ligands: # Structural and spectroscopic authentication of germanium(IV) # phosphane complexes # Authors: M.F. Davis, W. Levason, G. Reid, M. Webster # Journal (proposed): Dalton Trans. # CCDC ref. no(s).: # DOI: # ############################################################################## ### CIF submission form for molecular structure report ### ### Version: 2.0.2 (6 July 1998). (Updated 20-Apr-2005) ### ############################################################################## # This is an electronic "form" for submitting structural details as a # Crystallographic Information File (CIF). # Full details of the format of such files are given in the paper "The # Crystallographic Information File (CIF): a New Standard Archive File for # Crystallography" by S. R. Hall, F. H. Allen and I. D. Brown [Acta Cryst. # (1991), A47, 655-685]. # # The current version of the core CIF dictionary is obtainable from # www.iucr.org as a pdf file. The current version number is 2.3. # # CIFs can be checked for legal syntax and possible errors (ALERTS) by # using checkcif software. # See the web (http://journals.iucr.org/services/cif/checkcif.html). # The website http://checkcif.iucr.org produces o/p in pdf format. # #============================================================================== data_07mfd002_[C10H16F4GeP2] _database_code_depnum_ccdc_archive 'CCDC 665905' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-02-10 _audit_author_name 'Webster, M.' _audit_update_record '2007-11-02 corrected name' _chemical_name_systematic ; Tetrafluoro(1,2-bis(dimethylphosphino)benzene)germanium(IV) ; _chemical_name_common Tetrafluoro(1,2-bis(dimethylphosphino)benzene)germanium(IV) _chemical_melting_point ? _chemical_formula_moiety 'C10 H16 F4 Ge P2' _chemical_formula_sum 'C10 H16 F4 Ge P2' _chemical_formula_weight 346.76 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' F F 0.0171 0.0103 '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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_Int_Tables_number 33 # Superceded ** _symmetry_space_group_name_Hall 'P 2c -2n' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 12.307(3) _cell_length_b 10.1285(10) _cell_length_c 10.749(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1339.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6358 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 2.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7418 # 0.6861 _exptl_absorpt_correction_T_max 1.0000 # 0.8622 _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 8863 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0813 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.57 _reflns_number_total 2871 _reflns_number_gt 2529 _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^+0.3243P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.032(13) _refine_ls_number_reflns 2871 _refine_ls_number_parameters 158 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Ge1 Ge 0.14715(3) 0.48443(3) -0.05630(6) 0.01361(12) Uani 1 1 d . . . F1 F 0.27104(18) 0.4518(2) 0.0300(2) 0.0212(6) Uani 1 1 d . . . F2 F 0.2114(2) 0.6013(2) -0.1533(2) 0.0238(6) Uani 1 1 d . . . F3 F 0.1052(2) 0.6039(2) 0.0541(3) 0.0262(6) Uani 1 1 d . . . F4 F 0.0212(2) 0.4944(2) -0.1426(3) 0.0225(6) Uani 1 1 d . . . P1 P 0.20201(8) 0.30944(9) -0.19722(11) 0.0130(2) Uani 1 1 d . . . P2 P 0.06184(8) 0.31037(9) 0.06434(10) 0.0119(2) Uani 1 1 d . . . C1 C 0.1489(4) 0.3120(4) -0.3538(4) 0.0182(10) Uani 1 1 d . . . H1A H 0.1797 0.3872 -0.3991 0.027 Uiso 1 1 calc R . . H1B H 0.0696 0.3204 -0.3511 0.027 Uiso 1 1 calc R . . H1C H 0.1685 0.2298 -0.3964 0.027 Uiso 1 1 calc R . . C2 C 0.3476(3) 0.2988(4) -0.2160(5) 0.0201(10) Uani 1 1 d . . . H2A H 0.3825 0.3005 -0.1340 0.030 Uiso 1 1 calc R . . H2B H 0.3732 0.3739 -0.2655 0.030 Uiso 1 1 calc R . . H2C H 0.3661 0.2163 -0.2586 0.030 Uiso 1 1 calc R . . C3 C 0.1530(3) 0.1563(4) -0.1278(4) 0.0127(9) Uani 1 1 d . . . C4 C 0.1770(4) 0.0356(4) -0.1856(4) 0.0167(9) Uani 1 1 d . . . H4 H 0.2211 0.0341 -0.2581 0.020 Uiso 1 1 calc R . . C5 C 0.1364(4) -0.0822(4) -0.1371(4) 0.0200(10) Uani 1 1 d . . . H5 H 0.1550 -0.1640 -0.1747 0.024 Uiso 1 1 calc R . . C6 C 0.0693(3) -0.0795(3) -0.0346(4) 0.0201(11) Uani 1 1 d . . . H6 H 0.0397 -0.1597 -0.0037 0.024 Uiso 1 1 calc R . . C7 C 0.0442(3) 0.0398(4) 0.0248(4) 0.0177(9) Uani 1 1 d . . . H7 H -0.0020 0.0401 0.0956 0.021 Uiso 1 1 calc R . . C8 C 0.0870(3) 0.1579(3) -0.0201(4) 0.0106(9) Uani 1 1 d . . . C9 C -0.0823(3) 0.3297(4) 0.0835(4) 0.0182(10) Uani 1 1 d . . . H9A H -0.1162 0.2426 0.0914 0.027 Uiso 1 1 calc R . . H9B H -0.1124 0.3755 0.0110 0.027 Uiso 1 1 calc R . . H9C H -0.0968 0.3815 0.1587 0.027 Uiso 1 1 calc R . . C10 C 0.1150(4) 0.2792(4) 0.2178(4) 0.0174(10) Uani 1 1 d . . . H10A H 0.0766 0.2041 0.2549 0.026 Uiso 1 1 calc R . . H10B H 0.1047 0.3576 0.2698 0.026 Uiso 1 1 calc R . . H10C H 0.1927 0.2589 0.2120 0.026 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 0.0165(2) 0.00979(18) 0.0145(2) 0.0004(3) 0.0012(2) 0.00074(15) F1 0.0165(13) 0.0285(13) 0.0186(16) -0.0032(11) -0.0043(11) -0.0020(10) F2 0.0301(15) 0.0143(11) 0.0272(16) 0.0018(11) 0.0070(12) -0.0042(10) F3 0.0376(15) 0.0115(12) 0.0295(17) -0.0053(11) 0.0083(15) 0.0040(11) F4 0.0159(14) 0.0274(13) 0.0243(16) 0.0068(11) -0.0046(12) 0.0064(10) P1 0.0140(6) 0.0126(5) 0.0125(6) 0.0000(4) 0.0007(5) -0.0010(4) P2 0.0123(5) 0.0117(5) 0.0117(6) -0.0020(4) -0.0004(5) 0.0016(4) C1 0.019(3) 0.017(2) 0.018(3) -0.0002(19) -0.0048(19) 0.0021(17) C2 0.014(2) 0.027(2) 0.020(3) -0.0018(19) 0.005(2) -0.0026(18) C3 0.014(2) 0.012(2) 0.012(2) -0.0012(17) -0.0036(19) 0.0046(16) C4 0.018(2) 0.017(2) 0.015(2) -0.0025(18) 0.000(2) 0.0028(17) C5 0.025(3) 0.012(2) 0.023(3) -0.0028(19) -0.003(2) 0.0054(17) C6 0.025(2) 0.0103(18) 0.025(3) 0.0005(19) -0.003(2) 0.0009(16) C7 0.016(2) 0.023(2) 0.015(2) -0.0017(18) 0.001(2) -0.0010(18) C8 0.011(2) 0.0120(18) 0.009(2) 0.0022(14) -0.0018(16) 0.0021(15) C9 0.016(2) 0.020(2) 0.019(3) -0.0076(18) 0.002(2) 0.0039(16) C10 0.023(2) 0.020(2) 0.010(2) -0.0022(18) 0.003(2) -0.0032(19) _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 F2 1.765(2) . ? Ge1 F3 1.772(2) . ? Ge1 F4 1.809(2) . ? Ge1 F1 1.815(2) . ? Ge1 P1 2.4273(12) . ? Ge1 P2 2.4273(11) . ? P1 C1 1.806(5) . ? P1 C2 1.807(4) . ? P1 C3 1.824(4) . ? P2 C9 1.796(4) . ? P2 C10 1.802(5) . ? P2 C8 1.818(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.402(5) . ? C3 C8 1.414(5) . ? C4 C5 1.395(6) . ? C4 H4 0.9500 . ? C5 C6 1.377(6) . ? C5 H5 0.9500 . ? C6 C7 1.401(5) . ? C6 H6 0.9500 . ? C7 C8 1.394(5) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 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 F2 Ge1 F3 93.91(10) . . ? F2 Ge1 F4 92.49(12) . . ? F3 Ge1 F4 93.18(12) . . ? F2 Ge1 F1 92.76(12) . . ? F3 Ge1 F1 91.56(12) . . ? F4 Ge1 F1 172.68(10) . . ? F2 Ge1 P1 89.80(8) . . ? F3 Ge1 P1 176.16(9) . . ? F4 Ge1 P1 87.65(9) . . ? F1 Ge1 P1 87.26(8) . . ? F2 Ge1 P2 175.37(8) . . ? F3 Ge1 P2 90.70(9) . . ? F4 Ge1 P2 86.77(9) . . ? F1 Ge1 P2 87.59(8) . . ? P1 Ge1 P2 85.61(4) . . ? C1 P1 C2 104.8(2) . . ? C1 P1 C3 105.9(2) . . ? C2 P1 C3 108.84(19) . . ? C1 P1 Ge1 118.06(14) . . ? C2 P1 Ge1 112.89(15) . . ? C3 P1 Ge1 105.89(15) . . ? C9 P2 C10 105.8(2) . . ? C9 P2 C8 108.55(18) . . ? C10 P2 C8 104.26(18) . . ? C9 P2 Ge1 114.17(14) . . ? C10 P2 Ge1 117.32(15) . . ? C8 P2 Ge1 106.05(13) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C8 119.6(4) . . ? C4 C3 P1 119.4(3) . . ? C8 C3 P1 121.0(3) . . ? C5 C4 C3 120.3(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.9(4) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 119.9(4) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C3 119.4(4) . . ? C7 C8 P2 119.5(3) . . ? C3 C8 P2 121.1(3) . . ? P2 C9 H9A 109.5 . . ? P2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P2 C10 H10A 109.5 . . ? P2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 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 # F3 Ge1 P1 C1 131.8(13) . . . . ? # F3 Ge1 P1 C2 -105.5(13) . . . . ? # F3 Ge1 P1 C3 13.4(14) . . . . ? # F2 Ge1 P2 C9 -113.2(11) . . . . ? # F2 Ge1 P2 C10 122.2(11) . . . . ? # F2 Ge1 P2 C8 6.2(11) . . . . ? F2 Ge1 P1 C1 -63.28(18) . . . . ? F4 Ge1 P1 C1 29.22(18) . . . . ? F1 Ge1 P1 C1 -156.05(18) . . . . ? P2 Ge1 P1 C1 116.16(17) . . . . ? F2 Ge1 P1 C2 59.40(19) . . . . ? F4 Ge1 P1 C2 151.90(18) . . . . ? F1 Ge1 P1 C2 -33.37(18) . . . . ? P2 Ge1 P1 C2 -121.16(17) . . . . ? F2 Ge1 P1 C3 178.39(16) . . . . ? F4 Ge1 P1 C3 -89.11(16) . . . . ? F1 Ge1 P1 C3 85.62(15) . . . . ? P2 Ge1 P1 C3 -2.17(14) . . . . ? F3 Ge1 P2 C9 60.85(18) . . . . ? F4 Ge1 P2 C9 -32.29(18) . . . . ? F1 Ge1 P2 C9 152.39(17) . . . . ? P1 Ge1 P2 C9 -120.18(16) . . . . ? F3 Ge1 P2 C10 -63.76(19) . . . . ? F4 Ge1 P2 C10 -156.90(19) . . . . ? F1 Ge1 P2 C10 27.77(18) . . . . ? P1 Ge1 P2 C10 115.21(17) . . . . ? F3 Ge1 P2 C8 -179.67(16) . . . . ? F4 Ge1 P2 C8 87.18(15) . . . . ? F1 Ge1 P2 C8 -88.14(15) . . . . ? P1 Ge1 P2 C8 -0.71(13) . . . . ? C1 P1 C3 C4 56.8(4) . . . . ? C2 P1 C3 C4 -55.4(4) . . . . ? Ge1 P1 C3 C4 -177.0(3) . . . . ? C1 P1 C3 C8 -120.1(3) . . . . ? C2 P1 C3 C8 127.7(3) . . . . ? Ge1 P1 C3 C8 6.0(4) . . . . ? C8 C3 C4 C5 -0.2(6) . . . . ? P1 C3 C4 C5 -177.2(3) . . . . ? C3 C4 C5 C6 2.3(7) . . . . ? C4 C5 C6 C7 -2.3(6) . . . . ? C5 C6 C7 C8 0.2(6) . . . . ? C6 C7 C8 C3 1.9(6) . . . . ? C6 C7 C8 P2 -175.6(3) . . . . ? C4 C3 C8 C7 -1.9(6) . . . . ? P1 C3 C8 C7 175.1(3) . . . . ? C4 C3 C8 P2 175.5(3) . . . . ? P1 C3 C8 P2 -7.5(5) . . . . ? C9 P2 C8 C7 -54.8(4) . . . . ? C10 P2 C8 C7 57.7(4) . . . . ? Ge1 P2 C8 C7 -177.8(3) . . . . ? C9 P2 C8 C3 127.9(3) . . . . ? C10 P2 C8 C3 -119.7(3) . . . . ? Ge1 P2 C8 C3 4.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.457 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.108 #===END OF CIF ============================================================== # 07mfd005 data_07mfd005_[C26H24F4GeP2] _database_code_depnum_ccdc_archive 'CCDC 665906' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-04-26 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Tetrafluoro(1,2-bis(diphenylphosphino)ethane)germanium(IV) ; _chemical_name_common Tetrafluoro(1,2-bis(diphenylphosphino)ethane)germanium(IV) _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 F4 Ge P2' _chemical_formula_sum 'C26 H24 F4 Ge P2' _chemical_formula_weight 546.98 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' F F 0.0171 0.0103 '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 'C c' _symmetry_Int_Tables_number 9 # Superceded ** _symmetry_space_group_name_Hall 'C -2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.6765(12) _cell_length_b 16.466(2) _cell_length_c 14.2710(16) _cell_angle_alpha 90.00 _cell_angle_beta 105.003(8) _cell_angle_gamma 90.00 _cell_volume 2423.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2795 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8856 # 0.7617 _exptl_absorpt_correction_T_max 1.0000 # 0.8694 _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 12784 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4506 _reflns_number_gt 4410 _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^+1.6297P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(6) _chemical_absolute_configuration ad _refine_ls_number_reflns 4506 _refine_ls_number_parameters 298 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.85213(2) 0.937180(12) 0.079934(18) 0.01781(6) Uani 1 1 d . . . F1 F 0.85739(14) 1.04337(8) 0.05166(10) 0.0260(3) Uani 1 1 d . . . F2 F 0.84207(13) 0.83731(8) 0.12570(10) 0.0219(3) Uani 1 1 d . . . F3 F 0.99337(14) 0.91491(9) 0.04126(10) 0.0271(3) Uani 1 1 d . . . F4 F 0.74686(14) 0.91447(9) -0.03477(10) 0.0274(3) Uani 1 1 d . . . P1 P 0.97982(5) 0.97944(3) 0.24218(4) 0.01882(12) Uani 1 1 d . . . P2 P 0.66325(5) 0.97462(3) 0.14213(4) 0.01718(12) Uani 1 1 d . . . C1 C 1.1186(2) 1.04518(14) 0.25032(18) 0.0226(5) Uani 1 1 d . . . C2 C 1.1564(3) 1.06638(15) 0.1670(2) 0.0258(6) Uani 1 1 d . . . H2 H 1.1137 1.0433 0.1061 0.031 Uiso 1 1 calc R . . C3 C 1.2570(2) 1.12144(17) 0.1739(2) 0.0306(6) Uani 1 1 d . . . H3 H 1.2827 1.1365 0.1173 0.037 Uiso 1 1 calc R . . C4 C 1.3199(3) 1.15444(17) 0.2626(2) 0.0345(6) Uani 1 1 d . . . H4 H 1.3884 1.1922 0.2669 0.041 Uiso 1 1 calc R . . C5 C 1.2831(3) 1.1325(2) 0.3451(2) 0.0426(8) Uani 1 1 d . . . H5 H 1.3271 1.1548 0.4062 0.051 Uiso 1 1 calc R . . C6 C 1.1826(3) 1.07838(18) 0.3393(2) 0.0364(7) Uani 1 1 d . . . H6 H 1.1573 1.0638 0.3961 0.044 Uiso 1 1 calc R . . C7 C 1.0319(2) 0.89529(14) 0.32382(16) 0.0205(5) Uani 1 1 d . . . C8 C 1.1171(2) 0.83930(16) 0.30101(18) 0.0279(5) Uani 1 1 d . . . H8 H 1.1497 0.8477 0.2458 0.034 Uiso 1 1 calc R . . C9 C 1.1543(3) 0.77165(17) 0.3585(2) 0.0346(6) Uani 1 1 d . . . H9 H 1.2135 0.7340 0.3432 0.042 Uiso 1 1 calc R . . C10 C 1.1060(3) 0.75818(16) 0.43830(19) 0.0348(7) Uani 1 1 d . . . H10 H 1.1315 0.7114 0.4776 0.042 Uiso 1 1 calc R . . C11 C 1.0208(3) 0.81294(18) 0.4602(2) 0.0389(7) Uani 1 1 d . . . H11 H 0.9866 0.8034 0.5145 0.047 Uiso 1 1 calc R . . C12 C 0.9839(3) 0.88232(16) 0.40395(17) 0.0291(6) Uani 1 1 d . . . H12 H 0.9262 0.9204 0.4204 0.035 Uiso 1 1 calc R . . C13 C 0.8653(2) 1.04094(14) 0.28722(18) 0.0223(5) Uani 1 1 d . . . H13A H 0.9006 1.0502 0.3577 0.027 Uiso 1 1 calc R . . H13B H 0.8553 1.0945 0.2546 0.027 Uiso 1 1 calc R . . C14 C 0.7317(2) 1.00016(15) 0.26932(17) 0.0242(5) Uani 1 1 d . . . H14A H 0.6717 1.0372 0.2909 0.029 Uiso 1 1 calc R . . H14B H 0.7401 0.9500 0.3087 0.029 Uiso 1 1 calc R . . C15 C 0.5399(2) 0.89953(13) 0.14451(16) 0.0182(4) Uani 1 1 d . . . C16 C 0.5799(2) 0.82360(14) 0.18513(17) 0.0223(5) Uani 1 1 d . . . H16 H 0.6697 0.8120 0.2087 0.027 Uiso 1 1 calc R . . C17 C 0.4890(2) 0.76534(15) 0.19108(19) 0.0263(5) Uani 1 1 d . . . H17 H 0.5161 0.7142 0.2202 0.032 Uiso 1 1 calc R . . C18 C 0.3573(2) 0.78206(16) 0.15412(19) 0.0286(6) Uani 1 1 d . . . H18 H 0.2948 0.7417 0.1570 0.034 Uiso 1 1 calc R . . C19 C 0.3175(2) 0.85655(17) 0.11357(19) 0.0299(6) Uani 1 1 d . . . H19 H 0.2276 0.8676 0.0887 0.036 Uiso 1 1 calc R . . C20 C 0.4085(2) 0.91556(16) 0.10899(18) 0.0248(5) Uani 1 1 d . . . H20 H 0.3808 0.9671 0.0814 0.030 Uiso 1 1 calc R . . C21 C 0.5850(2) 1.06290(14) 0.0788(2) 0.0248(5) Uani 1 1 d . . . C22 C 0.5724(2) 1.13517(15) 0.1251(2) 0.0357(7) Uani 1 1 d . . . H22 H 0.5988 1.1382 0.1939 0.043 Uiso 1 1 calc R . . C23 C 0.5213(3) 1.20308(18) 0.0712(3) 0.0546(11) Uani 1 1 d . . . H23 H 0.5138 1.2528 0.1031 0.066 Uiso 1 1 calc R . . C24 C 0.4814(3) 1.1988(2) -0.0282(4) 0.0637(12) Uani 1 1 d . . . H24 H 0.4477 1.2458 -0.0647 0.076 Uiso 1 1 calc R . . C25 C 0.4900(4) 1.1270(2) -0.0753(3) 0.0608(10) Uani 1 1 d . . . H25 H 0.4594 1.1240 -0.1440 0.073 Uiso 1 1 calc R . . C26 C 0.5434(4) 1.05850(19) -0.0228(3) 0.0417(9) Uani 1 1 d . . . H26 H 0.5517 1.0092 -0.0553 0.050 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 0.01778(10) 0.01970(10) 0.01689(10) 0.00254(10) 0.00617(7) 0.00073(10) F1 0.0233(7) 0.0248(6) 0.0319(8) 0.0103(6) 0.0108(6) 0.0016(6) F2 0.0228(7) 0.0178(6) 0.0251(7) 0.0032(5) 0.0061(5) 0.0008(5) F3 0.0242(7) 0.0341(8) 0.0259(7) -0.0014(6) 0.0116(6) 0.0008(6) F4 0.0272(7) 0.0385(8) 0.0157(6) 0.0009(6) 0.0041(5) 0.0012(6) P1 0.0200(3) 0.0194(3) 0.0173(3) 0.0014(2) 0.0052(2) -0.0022(2) P2 0.0180(3) 0.0164(3) 0.0181(3) -0.0001(2) 0.0064(2) -0.0005(2) C1 0.0189(12) 0.0221(11) 0.0260(12) 0.0025(10) 0.0040(9) -0.0024(9) C2 0.0219(14) 0.0290(14) 0.0299(15) 0.0003(10) 0.0126(11) -0.0026(10) C3 0.0249(13) 0.0350(14) 0.0334(13) 0.0047(11) 0.0102(10) -0.0061(11) C4 0.0256(13) 0.0338(14) 0.0412(15) 0.0057(12) 0.0034(12) -0.0115(11) C5 0.0413(17) 0.0515(18) 0.0300(14) 0.0021(13) 0.0002(12) -0.0240(14) C6 0.0381(16) 0.0434(15) 0.0247(13) 0.0035(12) 0.0026(11) -0.0177(13) C7 0.0215(11) 0.0221(11) 0.0160(10) 0.0003(9) 0.0014(9) -0.0031(9) C8 0.0222(12) 0.0335(13) 0.0281(12) 0.0050(11) 0.0066(10) 0.0022(10) C9 0.0303(14) 0.0353(14) 0.0343(14) 0.0040(12) 0.0012(11) 0.0082(11) C10 0.0437(17) 0.0255(13) 0.0275(13) 0.0073(11) -0.0046(12) -0.0010(12) C11 0.0542(18) 0.0424(16) 0.0206(12) 0.0076(12) 0.0109(12) -0.0013(14) C12 0.0411(15) 0.0269(12) 0.0203(11) 0.0033(10) 0.0096(10) 0.0024(11) C13 0.0227(12) 0.0221(11) 0.0228(11) -0.0024(9) 0.0071(9) -0.0030(9) C14 0.0256(12) 0.0259(12) 0.0233(11) -0.0039(10) 0.0103(10) -0.0053(10) C15 0.0214(11) 0.0183(10) 0.0162(10) -0.0044(8) 0.0071(8) -0.0023(9) C16 0.0212(12) 0.0224(11) 0.0256(11) -0.0007(9) 0.0103(9) -0.0012(9) C17 0.0308(13) 0.0212(12) 0.0315(13) -0.0021(10) 0.0164(10) -0.0045(10) C18 0.0271(13) 0.0300(13) 0.0328(13) -0.0067(11) 0.0153(11) -0.0129(10) C19 0.0163(12) 0.0423(15) 0.0311(13) -0.0013(12) 0.0066(10) -0.0047(10) C20 0.0219(12) 0.0297(12) 0.0247(12) 0.0011(10) 0.0095(9) 0.0006(10) C21 0.0198(12) 0.0198(11) 0.0385(14) 0.0064(10) 0.0140(10) 0.0016(9) C22 0.0190(12) 0.0212(12) 0.068(2) -0.0040(13) 0.0134(12) -0.0011(10) C23 0.0186(14) 0.0211(13) 0.122(4) 0.0084(17) 0.0147(18) 0.0044(11) C24 0.0295(17) 0.0431(19) 0.118(4) 0.046(2) 0.018(2) 0.0153(14) C25 0.054(2) 0.067(2) 0.064(2) 0.042(2) 0.0198(17) 0.0274(18) C26 0.046(2) 0.046(2) 0.0342(18) 0.0150(14) 0.0119(15) 0.0221(14) _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 F4 1.7692(14) . ? Ge1 F3 1.7731(14) . ? Ge1 F2 1.7829(13) . ? Ge1 F1 1.7987(14) . ? Ge1 P1 2.4636(7) . ? Ge1 P2 2.4822(7) . ? P1 C7 1.803(2) . ? P1 C1 1.814(2) . ? P1 C13 1.828(3) . ? P2 C21 1.799(2) . ? P2 C15 1.813(2) . ? P2 C14 1.822(2) . ? C1 C6 1.389(4) . ? C1 C2 1.396(4) . ? C2 C3 1.389(4) . ? C2 H2 0.9500 . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(4) . ? C4 H4 0.9500 . ? C5 C6 1.380(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.386(3) . ? C7 C8 1.392(4) . ? C8 C9 1.379(4) . ? C8 H8 0.9500 . ? C9 C10 1.385(4) . ? C9 H9 0.9500 . ? C10 C11 1.373(4) . ? C10 H10 0.9500 . ? C11 C12 1.394(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.537(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.388(3) . ? C15 C16 1.398(3) . ? C16 C17 1.383(3) . ? C16 H16 0.9500 . ? C17 C18 1.395(4) . ? C17 H17 0.9500 . ? C18 C19 1.376(4) . ? C18 H18 0.9500 . ? C19 C20 1.388(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.385(4) . ? C21 C26 1.403(4) . ? C22 C23 1.387(4) . ? C22 H22 0.9500 . ? C23 C24 1.373(6) . ? C23 H23 0.9500 . ? C24 C25 1.376(6) . ? C24 H24 0.9500 . ? C25 C26 1.392(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F4 Ge1 F3 93.21(7) . . ? F4 Ge1 F2 93.44(6) . . ? F3 Ge1 F2 93.44(7) . . ? F4 Ge1 F1 92.71(7) . . ? F3 Ge1 F1 93.02(7) . . ? F2 Ge1 F1 170.82(7) . . ? F4 Ge1 P1 173.57(5) . . ? F3 Ge1 P1 92.44(5) . . ? F2 Ge1 P1 89.28(4) . . ? F1 Ge1 P1 83.94(5) . . ? F4 Ge1 P2 90.18(5) . . ? F3 Ge1 P2 176.20(5) . . ? F2 Ge1 P2 88.08(5) . . ? F1 Ge1 P2 85.08(5) . . ? P1 Ge1 P2 84.08(2) . . ? C7 P1 C1 107.89(11) . . ? C7 P1 C13 108.72(11) . . ? C1 P1 C13 104.85(11) . . ? C7 P1 Ge1 113.15(7) . . ? C1 P1 Ge1 118.22(8) . . ? C13 P1 Ge1 103.26(8) . . ? C21 P2 C15 108.39(11) . . ? C21 P2 C14 109.18(12) . . ? C15 P2 C14 104.18(11) . . ? C21 P2 Ge1 109.59(9) . . ? C15 P2 Ge1 119.91(8) . . ? C14 P2 Ge1 105.06(9) . . ? C6 C1 C2 119.8(2) . . ? C6 C1 P1 119.6(2) . . ? C2 C1 P1 120.43(19) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.0(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 120.0(3) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C12 C7 C8 119.7(2) . . ? C12 C7 P1 122.26(19) . . ? C8 C7 P1 117.95(19) . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.5(3) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.5(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.8(3) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C7 C12 C11 119.5(3) . . ? C7 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 P1 112.08(16) . . ? C14 C13 H13A 109.2 . . ? P1 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? P1 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 P2 112.49(17) . . ? C13 C14 H14A 109.1 . . ? P2 C14 H14A 109.1 . . ? C13 C14 H14B 109.1 . . ? P2 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C20 C15 C16 119.5(2) . . ? C20 C15 P2 122.27(18) . . ? C16 C15 P2 118.18(17) . . ? C17 C16 C15 120.1(2) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.6(2) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 120.4(2) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.0(2) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C15 120.2(2) . . ? C19 C20 H20 119.9 . . ? C15 C20 H20 119.9 . . ? C22 C21 C26 119.6(3) . . ? C22 C21 P2 123.0(2) . . ? C26 C21 P2 117.3(2) . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.3(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.4(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 120.2(4) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 119.4(3) . . ? C25 C26 H26 120.3 . . ? C21 C26 H26 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C13 C14 P2 -55.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.291 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.048 #===END OF CIF ============================================================== # 06mfd018 data_06mfd018w_[C6H15AsCl2] _database_code_depnum_ccdc_archive 'CCDC 665907' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-07-17 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Dichloridotriethylarsenic(V) ; _chemical_name_common Dichloridotriethylarsenic(V) _chemical_melting_point ? _chemical_formula_moiety 'C6 H15 As Cl2' _chemical_formula_sum 'C6 H15 As Cl2' _chemical_formula_weight 233.00 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P -6' _symmetry_Int_Tables_number 174 # Superceded ** _symmetry_space_group_name_Hall 'P -6' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' _cell_length_a 8.354(2) _cell_length_b 8.354(2) _cell_length_c 8.629(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 521.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1250 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 236 _exptl_absorpt_coefficient_mu 3.702 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7212 _exptl_absorpt_correction_T_max 1.0000 _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 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \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 7342 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.66 _reflns_number_total 861 _reflns_number_gt 723 _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^)+(0.0441P)^2^+0.9648P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.41(4) _chemical_absolute_configuration unk _refine_ls_number_reflns 861 _refine_ls_number_parameters 36 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.036 _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 As1 As 0.6667 0.3333 0.0000 0.0295(6) Uani 1 6 d S . . Cl1 Cl 0.6667 0.3333 0.2760(5) 0.0521(13) Uani 1 3 d S . . C1 C 0.4038(9) 0.1645(9) 0.0000 0.0322(14) Uani 1 2 d SD . . H1A H 0.3459 0.1830 0.0933 0.039 Uiso 0.50 1 calc PR . . H1B H 0.3459 0.1830 -0.0933 0.039 Uiso 0.50 1 calc PR . . C2 C 0.3801(15) -0.0382(16) 0.0000 0.085(6) Uani 1 2 d SD . . H2A H 0.2483 -0.1312 0.0000 0.127 Uiso 1 2 calc SR . . H2B H 0.4388 -0.0536 0.0927 0.127 Uiso 0.50 1 calc PR . . H2C H 0.4388 -0.0536 -0.0927 0.127 Uiso 0.50 1 calc PR . . As2 As 0.0000 0.0000 0.5000 0.0266(5) Uani 1 6 d S . . Cl2 Cl 0.0000 0.0000 0.7738(5) 0.0541(13) Uani 1 3 d S . . C3 C 0.1918(10) -0.0627(11) 0.5000 0.047(2) Uani 1 2 d SD . . H3A H 0.2705 -0.0122 0.4068 0.056 Uiso 0.50 1 calc PR . . H3B H 0.2705 -0.0122 0.5932 0.056 Uiso 0.50 1 calc PR . . C4 C 0.0865(18) -0.2887(18) 0.5000 0.098(7) Uani 1 2 d SD . . H4A H 0.1785 -0.3288 0.5000 0.147 Uiso 1 2 calc SR . . H4B H 0.0090 -0.3364 0.4073 0.147 Uiso 0.50 1 calc PR . . H4C H 0.0090 -0.3364 0.5927 0.147 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0278(7) 0.0278(7) 0.0329(14) 0.000 0.000 0.0139(4) Cl1 0.064(2) 0.064(2) 0.028(2) 0.000 0.000 0.0321(10) C1 0.027(3) 0.031(4) 0.035(4) 0.000 0.000 0.012(3) C2 0.031(6) 0.043(9) 0.141(14) 0.000 0.000 -0.011(6) As2 0.0247(7) 0.0247(7) 0.0304(12) 0.000 0.000 0.0124(3) Cl2 0.067(2) 0.067(2) 0.027(2) 0.000 0.000 0.0337(10) C3 0.029(4) 0.044(4) 0.071(6) 0.000 0.000 0.020(3) C4 0.091(13) 0.096(13) 0.161(17) 0.000 0.000 0.087(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 As1 C1 1.927(6) 2_655 ? As1 C1 1.927(6) . ? As1 C1 1.927(6) 3_665 ? As1 Cl1 2.382(4) 4 ? As1 Cl1 2.382(4) . ? C1 C2 1.604(13) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? As2 C3 1.918(7) 3 ? As2 C3 1.918(7) . ? As2 C3 1.918(7) 2 ? As2 Cl2 2.362(4) . ? As2 Cl2 2.362(4) 4_556 ? C3 C4 1.637(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 As1 C1 120.0 2_655 . ? C1 As1 C1 120.0 2_655 3_665 ? C1 As1 C1 120.0 . 3_665 ? C1 As1 Cl1 90.0 2_655 4 ? C1 As1 Cl1 90.0 . 4 ? C1 As1 Cl1 90.0 3_665 4 ? C1 As1 Cl1 90.0 2_655 . ? C1 As1 Cl1 90.0 . . ? C1 As1 Cl1 90.0 3_665 . ? Cl1 As1 Cl1 180.0 4 . ? C2 C1 As1 105.4(5) . . ? C2 C1 H1A 110.7 . . ? As1 C1 H1A 110.7 . . ? C2 C1 H1B 110.7 . . ? As1 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 As2 C3 120.0 3 . ? C3 As2 C3 120.0 3 2 ? C3 As2 C3 120.0 . 2 ? C3 As2 Cl2 90.0 3 . ? C3 As2 Cl2 90.0 . . ? C3 As2 Cl2 90.0 2 . ? C3 As2 Cl2 90.0 3 4_556 ? C3 As2 Cl2 90.0 . 4_556 ? C3 As2 Cl2 90.0 2 4_556 ? Cl2 As2 Cl2 180.0 . 4_556 ? C4 C3 As2 105.9(6) . . ? C4 C3 H3A 110.5 . . ? As2 C3 H3A 110.5 . . ? C4 C3 H3B 110.5 . . ? As2 C3 H3B 110.5 . . ? H3A C3 H3B 108.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.597 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.090 #===END OF CIF ============================================================== # 07mfd015 data_07mfd015_[C12H30As2Cl4Ge] _database_code_depnum_ccdc_archive 'CCDC 665908' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-08-19 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trans-tetrachloridobis(triethylarsane)germanium(IV) ; _chemical_name_common trans-tetrachloridobis(triethylarsane)germanium(IV) _chemical_melting_point ? _chemical_formula_moiety 'C12 H30 As2 Cl4 Ge' _chemical_formula_sum 'C12 H30 As2 Cl4 Ge' _chemical_formula_weight 538.59 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' As As 0.0499 2.0058 '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 '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 7.849(2) _cell_length_b 13.643(4) _cell_length_c 9.537(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.721(15) _cell_angle_gamma 90.00 _cell_volume 1019.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13122 _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 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 5.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7130 # _exptl_absorpt_correction_T_max 1.0000 # _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9942 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.57 _reflns_number_total 2340 _reflns_number_gt 1660 _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^+9.8379P] 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 2340 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_restrained_S_all 1.212 _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 Ge1 Ge 0.0000 0.0000 0.0000 0.0168(3) Uani 1 2 d S . . Cl1 Cl 0.1948(2) -0.12296(14) 0.0665(2) 0.0233(4) Uani 1 1 d . . . Cl2 Cl 0.1680(2) 0.04853(14) -0.1794(2) 0.0227(4) Uani 1 1 d . . . As1 As 0.17173(9) 0.11468(6) 0.15540(8) 0.0176(2) Uani 1 1 d . . . C1 C 0.4135(10) 0.0952(6) 0.1373(9) 0.0275(19) Uani 1 1 d . . . H1A H 0.4401 0.0248 0.1507 0.033 Uiso 1 1 calc R . . H1B H 0.4408 0.1132 0.0408 0.033 Uiso 1 1 calc R . . C2 C 0.5270(10) 0.1544(6) 0.2412(9) 0.030(2) Uani 1 1 d . . . H2A H 0.5038 0.2244 0.2273 0.046 Uiso 1 1 calc R . . H2B H 0.6471 0.1411 0.2260 0.046 Uiso 1 1 calc R . . H2C H 0.5033 0.1359 0.3373 0.046 Uiso 1 1 calc R . . C3 C 0.1302(10) 0.2513(6) 0.1062(9) 0.0241(18) Uani 1 1 d . . . H3A H 0.2342 0.2896 0.1338 0.029 Uiso 1 1 calc R . . H3B H 0.1105 0.2563 0.0029 0.029 Uiso 1 1 calc R . . C4 C -0.0196(10) 0.2973(6) 0.1735(10) 0.031(2) Uani 1 1 d . . . H4A H -0.1245 0.2620 0.1435 0.046 Uiso 1 1 calc R . . H4B H -0.0304 0.3661 0.1446 0.046 Uiso 1 1 calc R . . H4C H -0.0011 0.2937 0.2760 0.046 Uiso 1 1 calc R . . C5 C 0.1364(10) 0.1062(6) 0.3535(8) 0.0240(17) Uani 1 1 d . . . H5A H 0.1950 0.1618 0.4027 0.029 Uiso 1 1 calc R . . H5B H 0.0128 0.1121 0.3669 0.029 Uiso 1 1 calc R . . C6 C 0.2037(11) 0.0089(7) 0.4201(9) 0.0300(19) Uani 1 1 d . . . H6A H 0.1473 -0.0465 0.3709 0.045 Uiso 1 1 calc R . . H6B H 0.1791 0.0072 0.5195 0.045 Uiso 1 1 calc R . . H6C H 0.3273 0.0044 0.4120 0.045 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 0.0174(5) 0.0167(6) 0.0164(6) -0.0007(5) 0.0019(4) 0.0002(5) Cl1 0.0231(9) 0.0200(10) 0.0264(10) 0.0005(8) -0.0018(7) 0.0017(8) Cl2 0.0239(9) 0.0266(10) 0.0181(10) 0.0004(8) 0.0044(7) -0.0049(8) As1 0.0183(4) 0.0176(4) 0.0169(4) -0.0014(3) 0.0013(3) -0.0003(3) C1 0.024(4) 0.025(5) 0.034(5) -0.002(4) 0.006(4) -0.003(3) C2 0.023(4) 0.026(4) 0.042(6) -0.008(4) -0.002(4) -0.007(4) C3 0.022(4) 0.017(4) 0.032(5) -0.001(3) -0.007(3) -0.003(3) C4 0.026(4) 0.025(5) 0.040(5) -0.006(4) -0.007(4) 0.003(4) C5 0.029(4) 0.024(4) 0.020(4) 0.001(3) 0.005(3) -0.005(4) C6 0.029(4) 0.039(5) 0.022(4) 0.006(4) 0.002(3) 0.005(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 Ge1 Cl2 2.3233(19) . ? Ge1 Cl2 2.3233(19) 3 ? Ge1 Cl1 2.3296(19) 3 ? Ge1 Cl1 2.3296(19) . ? Ge1 As1 2.4904(9) . ? Ge1 As1 2.4904(9) 3 ? As1 C5 1.930(8) . ? As1 C1 1.935(8) . ? As1 C3 1.944(8) . ? C1 C2 1.521(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.512(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.551(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 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 Ge1 Cl2 180.00(11) . 3 ? Cl2 Ge1 Cl1 89.33(7) . 3 ? Cl2 Ge1 Cl1 90.67(7) 3 3 ? Cl2 Ge1 Cl1 90.67(7) . . ? Cl2 Ge1 Cl1 89.33(7) 3 . ? Cl1 Ge1 Cl1 180.00(13) 3 . ? Cl2 Ge1 As1 87.03(5) . . ? Cl2 Ge1 As1 92.97(5) 3 . ? Cl1 Ge1 As1 91.71(5) 3 . ? Cl1 Ge1 As1 88.29(5) . . ? Cl2 Ge1 As1 92.97(5) . 3 ? Cl2 Ge1 As1 87.03(5) 3 3 ? Cl1 Ge1 As1 88.29(5) 3 3 ? Cl1 Ge1 As1 91.71(5) . 3 ? As1 Ge1 As1 180.00(4) . 3 ? C5 As1 C1 106.4(4) . . ? C5 As1 C3 105.1(4) . . ? C1 As1 C3 105.1(3) . . ? C5 As1 Ge1 116.0(2) . . ? C1 As1 Ge1 110.9(2) . . ? C3 As1 Ge1 112.5(2) . . ? C2 C1 As1 113.9(6) . . ? C2 C1 H1A 108.8 . . ? As1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? As1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 As1 114.7(6) . . ? C4 C3 H3A 108.6 . . ? As1 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? As1 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 As1 112.7(5) . . ? C6 C5 H5A 109.1 . . ? As1 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? As1 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 # As1 Ge1 As1 C5 -73(100) 3 . . . ? # As1 Ge1 As1 C1 49(99) 3 . . . ? # As1 Ge1 As1 C3 166(100) 3 . . . ? Cl2 Ge1 As1 C5 -170.3(3) . . . . ? Cl2 Ge1 As1 C5 9.7(3) 3 . . . ? Cl1 Ge1 As1 C5 100.4(3) 3 . . . ? Cl1 Ge1 As1 C5 -79.6(3) . . . . ? Cl2 Ge1 As1 C1 -48.8(3) . . . . ? Cl2 Ge1 As1 C1 131.2(3) 3 . . . ? Cl1 Ge1 As1 C1 -138.0(3) 3 . . . ? Cl1 Ge1 As1 C1 42.0(3) . . . . ? Cl2 Ge1 As1 C3 68.6(3) . . . . ? Cl2 Ge1 As1 C3 -111.4(3) 3 . . . ? Cl1 Ge1 As1 C3 -20.6(3) 3 . . . ? Cl1 Ge1 As1 C3 159.4(3) . . . . ? C5 As1 C1 C2 -46.3(7) . . . . ? C3 As1 C1 C2 64.8(7) . . . . ? Ge1 As1 C1 C2 -173.3(5) . . . . ? C5 As1 C3 C4 -40.7(6) . . . . ? C1 As1 C3 C4 -152.8(6) . . . . ? Ge1 As1 C3 C4 86.4(6) . . . . ? C1 As1 C5 C6 -55.6(6) . . . . ? C3 As1 C5 C6 -166.7(6) . . . . ? Ge1 As1 C5 C6 68.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.001 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.221 #===END OF CIF ============================================================== # 06mfd020 data_06mfd020_[C6H18Cl6Ge2P2] _database_code_depnum_ccdc_archive 'CCDC 665909' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-11-15 _audit_author_name 'Webster, M.' _chemical_name_systematic ; 1,2-bis(dimethylphosphonium)ethane bis(trichlorogermanate(II)) ; # 1,2-bis(dimethylphosphonium)ethane bis(trichlorogermanium(II)) # See CSD refcodes DEBLEB & MAKKAK for naming similar cations. mw 2007-10-06 _chemical_name_common '1,2-bis(dimethylphosphonium)ethane bis(trichlorogermanate(ii))' _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 P2 2+, 2(Cl3 Ge 1-)' _chemical_formula_sum 'C6 H18 Cl6 Ge2 P2' _chemical_formula_weight 510.02 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' P P 0.1023 0.0942 '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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_Int_Tables_number 29 # Superceded ** _symmetry_space_group_name_Hall 'P 2c -2ac' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.0377(13) _cell_length_b 12.5498(9) _cell_length_c 16.6597(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3771.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4763 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 4.185 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6765 # 0.4333 _exptl_absorpt_correction_T_max 1.0000 # 0.8180 _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 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \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 29683 _diffrn_reflns_av_R_equivalents 0.2016 _diffrn_reflns_av_sigmaI/netI 0.2750 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.58 _reflns_number_total 8233 _reflns_number_gt 3819 _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^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.031(19) _refine_ls_number_reflns 8233 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2079 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1453 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 Ge1 Ge 0.69216(8) 0.47366(11) 0.77880(8) 0.0323(4) Uani 1 1 d . . . Ge2 Ge 0.69925(8) 0.00075(12) 0.74953(8) 0.0327(4) Uani 1 1 d . . . Ge3 Ge 0.56534(7) 0.00058(11) 0.46071(8) 0.0280(3) Uani 1 1 d . . . Ge4 Ge 0.55197(8) 0.46739(12) 0.50111(8) 0.0345(4) Uani 1 1 d . . . Cl1 Cl 0.77474(17) 0.4275(3) 0.87803(18) 0.0345(8) Uani 1 1 d . . . Cl2 Cl 0.72116(18) 0.6544(3) 0.78723(19) 0.0378(8) Uani 1 1 d . . . Cl3 Cl 0.7733(2) 0.4425(3) 0.67433(18) 0.0388(9) Uani 1 1 d . . . Cl4 Cl 0.6998(2) -0.0431(3) 0.61547(19) 0.0416(9) Uani 1 1 d . . . Cl5 Cl 0.8258(2) -0.0076(3) 0.7668(2) 0.0444(10) Uani 1 1 d . . . Cl6 Cl 0.69428(18) 0.1807(3) 0.73022(19) 0.0372(9) Uani 1 1 d . . . Cl7 Cl 0.47549(18) 0.0227(3) 0.36267(18) 0.0326(8) Uani 1 1 d . . . Cl8 Cl 0.4807(2) 0.0011(2) 0.56474(19) 0.0344(9) Uani 1 1 d . . . Cl9 Cl 0.56984(17) -0.1840(3) 0.45064(17) 0.0328(8) Uani 1 1 d . . . Cl10 Cl 0.5419(2) 0.4973(3) 0.6368(2) 0.0459(10) Uani 1 1 d . . . Cl11 Cl 0.4322(2) 0.5184(3) 0.4702(2) 0.0420(10) Uani 1 1 d . . . Cl12 Cl 0.52530(18) 0.2895(3) 0.5062(2) 0.0392(8) Uani 1 1 d . . . P1 P 0.46509(19) 0.7981(3) 0.71192(18) 0.0271(8) Uani 1 1 d . . . H1 H 0.4545 0.9085 0.7162 0.030 Uiso 1 1 calc R . . P2 P 0.30903(18) 0.7471(3) 0.5135(2) 0.0280(8) Uani 1 1 d . . . H2 H 0.3089 0.6356 0.5155 0.030 Uiso 1 1 calc R . . P3 P 0.68662(18) 0.7360(3) 0.00465(19) 0.0287(8) Uani 1 1 d . . . H3 H 0.6370 0.6690 -0.0356 0.030 Uiso 1 1 calc R . . P4 P 0.58392(19) 0.7186(3) 0.24301(18) 0.0276(8) Uani 1 1 d . . . H4 H 0.6331 0.7865 0.2831 0.030 Uiso 1 1 calc R . . C1 C 0.4154(8) 0.7376(11) 0.7928(7) 0.057(5) Uani 1 1 d . . . H1A H 0.3626 0.7548 0.7881 0.085 Uiso 1 1 calc R . . H1B H 0.4344 0.7646 0.8440 0.085 Uiso 1 1 calc R . . H1C H 0.4219 0.6601 0.7906 0.085 Uiso 1 1 calc R . . C2 C 0.5609(6) 0.7724(11) 0.7145(8) 0.044(4) Uani 1 1 d . . . H2A H 0.5850 0.8082 0.6692 0.066 Uiso 1 1 calc R . . H2B H 0.5695 0.6955 0.7109 0.066 Uiso 1 1 calc R . . H2C H 0.5817 0.7994 0.7650 0.066 Uiso 1 1 calc R . . C3 C 0.4268(6) 0.7518(10) 0.6193(6) 0.019(3) Uani 1 1 d . . . H3A H 0.4594 0.7739 0.5744 0.023 Uiso 1 1 calc R . . H3B H 0.4247 0.6730 0.6198 0.023 Uiso 1 1 calc R . . C4 C 0.3495(6) 0.7963(9) 0.6062(6) 0.022(3) Uani 1 1 d . . . H4A H 0.3519 0.8751 0.6044 0.027 Uiso 1 1 calc R . . H4B H 0.3174 0.7758 0.6519 0.027 Uiso 1 1 calc R . . C5 C 0.2160(7) 0.7923(11) 0.5080(9) 0.055(4) Uani 1 1 d . . . H5A H 0.1886 0.7670 0.5551 0.083 Uiso 1 1 calc R . . H5B H 0.1928 0.7646 0.4591 0.083 Uiso 1 1 calc R . . H5C H 0.2153 0.8704 0.5069 0.083 Uiso 1 1 calc R . . C6 C 0.3625(8) 0.7894(11) 0.4308(6) 0.046(4) Uani 1 1 d . . . H6A H 0.4132 0.7621 0.4362 0.069 Uiso 1 1 calc R . . H6B H 0.3636 0.8674 0.4291 0.069 Uiso 1 1 calc R . . H6C H 0.3405 0.7620 0.3811 0.069 Uiso 1 1 calc R . . C7 C 0.7019(7) 0.8511(10) -0.0556(6) 0.040(4) Uani 1 1 d . . . H7A H 0.7247 0.8300 -0.1066 0.060 Uiso 1 1 calc R . . H7B H 0.7349 0.9004 -0.0272 0.060 Uiso 1 1 calc R . . H7C H 0.6544 0.8864 -0.0663 0.060 Uiso 1 1 calc R . . C8 C 0.7705(7) 0.6640(10) 0.0221(7) 0.037(4) Uani 1 1 d . . . H8A H 0.7918 0.6418 -0.0293 0.056 Uiso 1 1 calc R . . H8B H 0.7598 0.6010 0.0548 0.056 Uiso 1 1 calc R . . H8C H 0.8058 0.7098 0.0505 0.056 Uiso 1 1 calc R . . C9 C 0.6446(7) 0.7772(9) 0.0975(6) 0.027(3) Uani 1 1 d . . . H9A H 0.6794 0.8237 0.1272 0.033 Uiso 1 1 calc R . . H9B H 0.5993 0.8189 0.0860 0.033 Uiso 1 1 calc R . . C10 C 0.6246(7) 0.6807(10) 0.1496(6) 0.034(4) Uani 1 1 d . . . H10A H 0.6699 0.6385 0.1602 0.040 Uiso 1 1 calc R . . H10B H 0.5894 0.6348 0.1199 0.040 Uiso 1 1 calc R . . C11 C 0.4991(7) 0.7872(10) 0.2281(7) 0.035(3) Uani 1 1 d . . . H11A H 0.5077 0.8499 0.1943 0.053 Uiso 1 1 calc R . . H11B H 0.4792 0.8099 0.2802 0.053 Uiso 1 1 calc R . . H11C H 0.4635 0.7398 0.2017 0.053 Uiso 1 1 calc R . . C12 C 0.5685(7) 0.6056(9) 0.3033(7) 0.036(4) Uani 1 1 d . . . H12A H 0.6154 0.5676 0.3113 0.054 Uiso 1 1 calc R . . H12B H 0.5329 0.5584 0.2768 0.054 Uiso 1 1 calc R . . H12C H 0.5487 0.6279 0.3555 0.054 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 0.0266(8) 0.0450(10) 0.0253(8) 0.0024(7) -0.0009(7) -0.0025(7) Ge2 0.0306(9) 0.0366(10) 0.0309(8) 0.0037(6) 0.0054(7) -0.0038(7) Ge3 0.0255(8) 0.0318(9) 0.0268(7) 0.0018(6) -0.0009(6) -0.0046(7) Ge4 0.0282(9) 0.0399(10) 0.0354(8) 0.0064(7) 0.0065(7) -0.0006(7) Cl1 0.030(2) 0.041(2) 0.0325(18) 0.0082(16) 0.0011(15) -0.0031(17) Cl2 0.042(2) 0.031(2) 0.0403(19) -0.0046(16) 0.0009(16) 0.0112(16) Cl3 0.060(3) 0.027(2) 0.0298(19) -0.0014(15) 0.0129(16) -0.0057(19) Cl4 0.046(2) 0.045(3) 0.0329(19) -0.0051(16) -0.0059(16) 0.011(2) Cl5 0.038(2) 0.040(2) 0.055(2) 0.0052(18) -0.0137(18) -0.0021(17) Cl6 0.036(2) 0.034(2) 0.0421(19) -0.0058(15) 0.0133(15) 0.0017(17) Cl7 0.0287(19) 0.038(2) 0.0316(18) 0.0084(14) -0.0028(14) -0.0016(16) Cl8 0.045(2) 0.026(2) 0.0317(18) -0.0010(14) 0.0125(15) 0.0059(17) Cl9 0.038(2) 0.032(2) 0.0278(16) -0.0015(14) 0.0021(15) 0.0082(16) Cl10 0.054(3) 0.047(3) 0.037(2) 0.0000(16) -0.0141(17) -0.005(2) Cl11 0.042(2) 0.040(3) 0.044(2) 0.0051(16) -0.0112(17) 0.0045(18) Cl12 0.041(2) 0.033(2) 0.0430(18) -0.0004(17) 0.0097(18) 0.0073(17) P1 0.024(2) 0.028(2) 0.0298(18) 0.0001(15) -0.0031(15) -0.0031(17) P2 0.0216(19) 0.028(2) 0.0348(19) -0.0041(16) -0.0068(16) -0.0007(17) P3 0.030(2) 0.029(2) 0.0266(17) -0.0004(16) 0.0061(16) 0.0004(17) P4 0.030(2) 0.026(2) 0.0264(17) -0.0014(15) 0.0023(15) 0.0006(16) C1 0.082(13) 0.054(12) 0.034(9) 0.006(8) 0.006(8) -0.032(9) C2 0.016(8) 0.052(11) 0.063(9) -0.012(8) -0.018(7) 0.019(7) C3 0.013(7) 0.024(8) 0.020(6) -0.004(5) -0.002(5) -0.005(6) C4 0.027(8) 0.017(8) 0.023(6) -0.004(5) -0.013(5) -0.003(6) C5 0.042(10) 0.047(11) 0.077(10) -0.023(9) -0.030(9) 0.020(8) C6 0.064(11) 0.049(11) 0.025(7) 0.012(6) 0.001(7) -0.030(9) C7 0.060(11) 0.037(10) 0.023(7) 0.005(6) 0.023(6) -0.008(7) C8 0.035(9) 0.040(9) 0.036(8) 0.014(6) 0.023(6) 0.008(7) C9 0.029(8) 0.020(8) 0.032(7) -0.004(6) 0.006(6) -0.007(6) C10 0.035(9) 0.049(11) 0.017(6) -0.005(6) 0.006(5) -0.002(7) C11 0.042(9) 0.035(9) 0.029(7) 0.015(6) 0.005(6) 0.011(7) C12 0.055(10) 0.013(8) 0.040(8) 0.000(6) 0.010(6) -0.010(7) _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 2.300(3) . ? Ge1 Cl3 2.308(3) . ? Ge1 Cl2 2.332(4) . ? Ge2 Cl6 2.283(4) . ? Ge2 Cl4 2.300(3) . ? Ge2 Cl5 2.303(4) . ? Ge3 Cl8 2.310(3) . ? Ge3 Cl7 2.318(3) . ? Ge3 Cl9 2.324(3) . ? Ge4 Cl12 2.285(3) . ? Ge4 Cl10 2.299(4) . ? Ge4 Cl11 2.311(4) . ? P1 C2 1.759(11) . ? P1 C3 1.788(10) . ? P1 C1 1.788(13) . ? P1 H1 1.4000 . ? P2 C6 1.763(11) . ? P2 C5 1.773(13) . ? P2 C4 1.816(10) . ? P2 H2 1.4000 . ? P3 C7 1.781(12) . ? P3 C8 1.785(12) . ? P3 C9 1.799(11) . ? P3 H3 1.4000 . ? P4 C12 1.760(11) . ? P4 C11 1.774(12) . ? P4 C10 1.784(11) . ? P4 H4 1.4000 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.519(13) . ? 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 C10 1.533(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 Cl1 Ge1 Cl3 95.08(12) . . ? Cl1 Ge1 Cl2 93.24(13) . . ? Cl3 Ge1 Cl2 93.89(13) . . ? Cl6 Ge2 Cl4 95.75(13) . . ? Cl6 Ge2 Cl5 95.82(13) . . ? Cl4 Ge2 Cl5 96.10(14) . . ? Cl8 Ge3 Cl7 93.78(12) . . ? Cl8 Ge3 Cl9 94.61(12) . . ? Cl7 Ge3 Cl9 95.34(13) . . ? Cl12 Ge4 Cl10 96.10(13) . . ? Cl12 Ge4 Cl11 94.71(13) . . ? Cl10 Ge4 Cl11 95.72(14) . . ? C2 P1 C3 109.9(6) . . ? C2 P1 C1 113.4(7) . . ? C3 P1 C1 108.6(6) . . ? C2 P1 H1 108.3 . . ? C3 P1 H1 108.3 . . ? C1 P1 H1 108.3 . . ? C6 P2 C5 112.4(7) . . ? C6 P2 C4 110.0(6) . . ? C5 P2 C4 108.3(6) . . ? C6 P2 H2 108.7 . . ? C5 P2 H2 108.7 . . ? C4 P2 H2 108.7 . . ? C7 P3 C8 111.8(6) . . ? C7 P3 C9 108.5(6) . . ? C8 P3 C9 111.2(6) . . ? C7 P3 H3 108.4 . . ? C8 P3 H3 108.4 . . ? C9 P3 H3 108.4 . . ? C12 P4 C11 109.6(6) . . ? C12 P4 C10 110.4(6) . . ? C11 P4 C10 111.3(6) . . ? C12 P4 H4 108.5 . . ? C11 P4 H4 108.5 . . ? C10 P4 H4 108.5 . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 111.1(7) . . ? C4 C3 H3A 109.4 . . ? P1 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? P1 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 P2 111.5(7) . . ? C3 C4 H4A 109.3 . . ? P2 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? P2 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P3 111.0(8) . . ? C10 C9 H9A 109.4 . . ? P3 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? P3 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 P4 112.3(8) . . ? C9 C10 H10A 109.1 . . ? P4 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? P4 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.813 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.184 #===END OF CIF ============================================================== # 07mfd020 data_07mfd020_[C6H17Cl3GeO2P2] _database_code_depnum_ccdc_archive 'CCDC 665910' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2007-10-05 _audit_author_name 'Webster, M.' _chemical_name_systematic ; (2-(dimethylphosphinoyl)ethyl)-hydroxy-dimethylphosphonium trichloridogermanate(II) ; # See CSD refcode CURCUN & IBUHAP for examples of naming cation. mw _chemical_name_common ; (2-(dimethylphosphinoyl)ethyl)-hydroxy-dimethylphosphonium trichloridogermanate(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C6 H17 O2 P2 1+, Cl3 Ge 1-' _chemical_formula_sum 'C6 H17 Cl3 Ge O2 P2' _chemical_formula_weight 362.08 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' Ge Ge 0.1547 1.8001 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0978(15) _cell_length_b 9.2599(15) _cell_length_c 11.1713(15) _cell_angle_alpha 66.397(10) _cell_angle_beta 89.283(10) _cell_angle_gamma 60.695(10) _cell_volume 731.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 23743 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 2.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8416 # 0.7271 _exptl_absorpt_correction_T_max 1.0000 # 0.9455 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11628 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.54 _reflns_number_total 3353 _reflns_number_gt 2956 _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^)+(0.0088P)^2^+0.8933P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # H1 found in difference map _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3353 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0590 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 0.17941(3) 0.91616(3) 0.59609(2) 0.02009(7) Uani 1 1 d . . . Cl1 Cl 0.44100(8) 0.84382(9) 0.69724(7) 0.03001(14) Uani 1 1 d . . . Cl2 Cl 0.28353(8) 0.64833(8) 0.57268(6) 0.02747(14) Uani 1 1 d . . . Cl3 Cl 0.09163(9) 0.81317(9) 0.79075(6) 0.03101(15) Uani 1 1 d . . . P1 P 0.64799(8) 0.12460(8) 0.91491(6) 0.01802(13) Uani 1 1 d . . . P2 P 0.90404(8) 0.43385(8) 0.73053(6) 0.01779(12) Uani 1 1 d . . . O1 O 0.7283(2) -0.0652(2) 1.03445(16) 0.0254(4) Uani 1 1 d . . . O2 O 1.0810(2) 0.2706(2) 0.74076(16) 0.0246(4) Uani 1 1 d . . . C1 C 0.5780(3) 0.1193(3) 0.7690(2) 0.0242(5) Uani 1 1 d . . . H1A H 0.6786 0.0348 0.7467 0.036 Uiso 1 1 calc R . . H1B H 0.5197 0.2444 0.6937 0.036 Uiso 1 1 calc R . . H1C H 0.4974 0.0759 0.7865 0.036 Uiso 1 1 calc R . . C2 C 0.4690(3) 0.3007(3) 0.9406(2) 0.0254(5) Uani 1 1 d . . . H2A H 0.3801 0.2692 0.9589 0.038 Uiso 1 1 calc R . . H2B H 0.4206 0.4197 0.8599 0.038 Uiso 1 1 calc R . . H2C H 0.5075 0.3104 1.0171 0.038 Uiso 1 1 calc R . . C3 C 0.8048(3) 0.1922(3) 0.8811(2) 0.0190(5) Uani 1 1 d . . . H3A H 0.8344 0.2100 0.9570 0.023 Uiso 1 1 calc R . . H3B H 0.9116 0.0893 0.8772 0.023 Uiso 1 1 calc R . . C4 C 0.7462(3) 0.3695(3) 0.7509(2) 0.0190(5) Uani 1 1 d . . . H4A H 0.6360 0.4721 0.7516 0.023 Uiso 1 1 calc R . . H4B H 0.7245 0.3501 0.6736 0.023 Uiso 1 1 calc R . . C5 C 0.9185(3) 0.5024(4) 0.8551(2) 0.0259(5) Uani 1 1 d . . . H5A H 0.9634 0.3955 0.9440 0.039 Uiso 1 1 calc R . . H5B H 0.8033 0.6007 0.8507 0.039 Uiso 1 1 calc R . . H5C H 0.9968 0.5490 0.8394 0.039 Uiso 1 1 calc R . . C6 C 0.8343(3) 0.6244(3) 0.5694(2) 0.0257(5) Uani 1 1 d . . . H6A H 0.9202 0.6607 0.5555 0.039 Uiso 1 1 calc R . . H6B H 0.7227 0.7292 0.5632 0.039 Uiso 1 1 calc R . . H6C H 0.8214 0.5885 0.5006 0.039 Uiso 1 1 calc R . . H1 H 1.1616 0.1780 0.8238 0.050 Uiso 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 Ge1 0.02023(13) 0.01570(12) 0.01971(13) -0.00535(10) 0.00103(10) -0.00836(10) Cl1 0.0233(3) 0.0307(3) 0.0394(4) -0.0200(3) 0.0029(3) -0.0131(3) Cl2 0.0320(3) 0.0235(3) 0.0231(3) -0.0135(2) 0.0000(2) -0.0096(3) Cl3 0.0407(4) 0.0324(3) 0.0313(3) -0.0195(3) 0.0188(3) -0.0232(3) P1 0.0202(3) 0.0155(3) 0.0169(3) -0.0045(2) 0.0018(2) -0.0106(2) P2 0.0191(3) 0.0174(3) 0.0168(3) -0.0060(2) 0.0041(2) -0.0109(2) O1 0.0276(9) 0.0185(8) 0.0233(8) -0.0010(7) 0.0003(7) -0.0140(7) O2 0.0205(8) 0.0221(9) 0.0213(8) -0.0062(7) 0.0036(7) -0.0075(7) C1 0.0296(13) 0.0250(12) 0.0249(12) -0.0117(10) 0.0034(10) -0.0187(11) C2 0.0259(13) 0.0236(12) 0.0243(12) -0.0092(10) 0.0091(10) -0.0127(11) C3 0.0208(11) 0.0162(11) 0.0166(11) -0.0045(9) 0.0012(9) -0.0097(9) C4 0.0214(11) 0.0189(11) 0.0182(11) -0.0066(9) 0.0026(9) -0.0131(10) C5 0.0296(13) 0.0287(13) 0.0275(13) -0.0146(11) 0.0057(10) -0.0195(11) C6 0.0254(12) 0.0210(12) 0.0241(12) -0.0046(10) 0.0079(10) -0.0122(10) _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 2.3000(8) . ? Ge1 Cl3 2.3059(7) . ? Ge1 Cl2 2.3087(8) . ? P1 O1 1.5147(17) . ? P1 C2 1.777(3) . ? P1 C1 1.784(2) . ? P1 C3 1.800(2) . ? P2 O2 1.5409(17) . ? P2 C6 1.773(2) . ? P2 C5 1.776(2) . ? P2 C4 1.786(2) . ? O2 H1 0.9475 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.531(3) . ? 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 . ? 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 96.66(3) . . ? Cl1 Ge1 Cl2 96.76(3) . . ? Cl3 Ge1 Cl2 95.00(3) . . ? O1 P1 C2 112.82(11) . . ? O1 P1 C1 110.12(11) . . ? C2 P1 C1 108.74(12) . . ? O1 P1 C3 110.29(10) . . ? C2 P1 C3 106.96(12) . . ? C1 P1 C3 107.73(11) . . ? O2 P2 C6 109.27(11) . . ? O2 P2 C5 110.79(11) . . ? C6 P2 C5 109.30(12) . . ? O2 P2 C4 110.32(11) . . ? C6 P2 C4 108.09(11) . . ? C5 P2 C4 109.02(12) . . ? P2 O2 H1 122.4 . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 114.97(15) . . ? C4 C3 H3A 108.5 . . ? P1 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? P1 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 P2 111.92(15) . . ? C3 C4 H4A 109.2 . . ? P2 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? P2 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 O1 P1 C3 C4 171.96(16) . . . . ? C2 P1 C3 C4 -65.01(19) . . . . ? C1 P1 C3 C4 51.7(2) . . . . ? P1 C3 C4 P2 176.45(12) . . . . ? O2 P2 C4 C3 54.26(19) . . . . ? C6 P2 C4 C3 173.68(17) . . . . ? C5 P2 C4 C3 -67.61(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H1 O1 0.95 1.51 2.447(2) 167.0 2_757 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.368 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.078 #===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 =============================================================