# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- Si_all7_1.cif' #============================================================================== # SUBMISSION DETAILS # ================== _publ_contact_author_name 'Professor W. Levason' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email wxl@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3792' _publ_contact_letter ; August 2010 Dear Sirs, This file contains crystallographic data in cif format for seven structures. It is offered as supporting information to accompany a paper to be submitted shortly. William Levason ; _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Hypervalent Neutral Oxygen Donor Complexes of Silicon Tetrafluoride and a Search for Soft Donor Ligand Complexes ; loop_ _publ_author_name _publ_author_address K.George ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; A.L.Hector ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; W.Levason ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; G.Reid ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; G.Sanderson ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; M.Webster ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; ; W.Zhang ; ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; #============================================================================ # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique (to this file) identifier. #============================================================================ # 08wz703 CCDC- # 08wz803 CCDC- # 10wz328a CCDC- # 09wz1101 CCDC- # 10wz218a CCDC- # 08wz801 CCDC- # 10wz729a CCDC- #============================================================================ # 08wz703 data_08wz703 _database_code_depnum_ccdc_archive 'CCDC 791398' #TrackingRef '- Si_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-09-04 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trans-tetrafluoridobis(trimethylphosphane oxide-O)silicon(IV) ; # trans-tetrafluorobis(trimethylphosphine oxide-O)silicon(IV) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 F4 O2 P2 Si' _chemical_formula_sum 'C6 H18 F4 O2 P2 Si' _chemical_formula_structural '((C H3)3 P O)2 (Si F4)' _chemical_formula_weight 288.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_IT_number 14 # New _space_group_name_Hall '-P 2yn' # New 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 6.285(2) _cell_length_b 9.560(3) _cell_length_c 10.287(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.845(15) _cell_angle_gamma 90.00 _cell_volume 613.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5577 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 0.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8169 # 0.6091 _exptl_absorpt_correction_T_max 1.0000 # 0.7456 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4787 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 5.84 _diffrn_reflns_theta_max 27.51 _reflns_number_total 1389 _reflns_number_gt 1238 _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^)+(0.0386P)^2^+0.2787P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1389 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.025 _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 Si1 Si 0.5000 1.0000 1.0000 0.01200(16) Uani 1 2 d S . . F1 F 0.41475(15) 1.14351(9) 1.07097(8) 0.0208(2) Uani 1 1 d . . . F2 F 0.35425(15) 0.89965(10) 1.08796(9) 0.0215(2) Uani 1 1 d . . . P1 P 0.16403(6) 0.90985(4) 0.77648(3) 0.01322(14) Uani 1 1 d . . . O1 O 0.27450(17) 1.01666(11) 0.87218(10) 0.0149(2) Uani 1 1 d . . . C1 C 0.0756(3) 0.75973(16) 0.85731(15) 0.0191(3) Uani 1 1 d . . . H1A H 0.1975 0.7170 0.9112 0.029 Uiso 1 1 calc R . . H1B H 0.0135 0.6920 0.7920 0.029 Uiso 1 1 calc R . . H1C H -0.0330 0.7875 0.9132 0.029 Uiso 1 1 calc R . . C2 C 0.3310(3) 0.85596(16) 0.65632(15) 0.0179(3) Uani 1 1 d . . . H2A H 0.3744 0.9381 0.6089 0.027 Uiso 1 1 calc R . . H2B H 0.2514 0.7913 0.5945 0.027 Uiso 1 1 calc R . . H2C H 0.4587 0.8089 0.6997 0.027 Uiso 1 1 calc R . . C3 C -0.0683(3) 0.98953(17) 0.69092(16) 0.0214(3) Uani 1 1 d . . . H3A H -0.1657 1.0181 0.7537 0.032 Uiso 1 1 calc R . . H3B H -0.1410 0.9224 0.6287 0.032 Uiso 1 1 calc R . . H3C H -0.0258 1.0718 0.6434 0.032 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 Si1 0.0147(3) 0.0113(3) 0.0094(3) -0.00102(19) -0.0009(2) 0.00171(19) F1 0.0243(5) 0.0188(5) 0.0173(4) -0.0074(4) -0.0058(4) 0.0085(4) F2 0.0209(5) 0.0275(5) 0.0152(4) 0.0057(4) -0.0010(4) -0.0060(4) P1 0.0148(2) 0.0140(2) 0.0103(2) -0.00133(13) -0.00039(14) -0.00035(13) O1 0.0175(5) 0.0138(5) 0.0123(5) -0.0020(4) -0.0030(4) 0.0014(4) C1 0.0235(8) 0.0176(7) 0.0167(7) -0.0006(6) 0.0037(6) -0.0045(6) C2 0.0207(7) 0.0180(7) 0.0153(7) -0.0028(6) 0.0029(6) -0.0003(6) C3 0.0176(8) 0.0262(9) 0.0189(8) -0.0021(6) -0.0040(6) 0.0019(6) _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 Si1 F2 1.6660(9) . ? Si1 F2 1.6660(9) 3_677 ? Si1 F1 1.6719(9) 3_677 ? Si1 F1 1.6719(9) . ? Si1 O1 1.8218(11) 3_677 ? Si1 O1 1.8218(11) . ? P1 O1 1.5267(11) . ? P1 C1 1.7805(16) . ? P1 C3 1.7835(17) . ? P1 C2 1.7898(15) . ? 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 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 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 Si1 F2 180.0 . 3_677 ? F2 Si1 F1 89.44(5) . 3_677 ? F2 Si1 F1 90.56(5) 3_677 3_677 ? F2 Si1 F1 90.56(5) . . ? F2 Si1 F1 89.44(5) 3_677 . ? F1 Si1 F1 180.000(1) 3_677 . ? F2 Si1 O1 89.34(5) . 3_677 ? F2 Si1 O1 90.66(5) 3_677 3_677 ? F1 Si1 O1 88.92(5) 3_677 3_677 ? F1 Si1 O1 91.08(5) . 3_677 ? F2 Si1 O1 90.66(5) . . ? F2 Si1 O1 89.34(5) 3_677 . ? F1 Si1 O1 91.08(5) 3_677 . ? F1 Si1 O1 88.92(5) . . ? O1 Si1 O1 180.0 3_677 . ? O1 P1 C1 112.41(7) . . ? O1 P1 C3 108.37(7) . . ? C1 P1 C3 106.97(8) . . ? O1 P1 C2 112.26(7) . . ? C1 P1 C2 109.39(8) . . ? C3 P1 C2 107.16(8) . . ? P1 O1 Si1 131.44(7) . . ? 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 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.329 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.064 #===END OF CIF ============================================================== # 08wz803 data_08wz803 _database_code_depnum_ccdc_archive 'CCDC 791399' #TrackingRef '- Si_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-09-03 _audit_author_name 'Webster, M.' _chemical_name_systematic ; trans-tetrafluoridobis(triphenylphosphane oxide-O)silicon(IV) ; # triphenylphosphine oxide = triphenylphosphane oxide _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 F4 O2 P2 Si' _chemical_formula_sum 'C36 H30 F4 O2 P2 Si' _chemical_formula_structural '((C6 H5)3 P O)2 (Si F4)' _chemical_formula_weight 660.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_IT_number 2 # New _space_group_name_Hall '-P 1' # New loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6885(15) _cell_length_b 13.7509(15) _cell_length_c 14.869(2) _cell_angle_alpha 62.564(6) _cell_angle_beta 82.697(6) _cell_angle_gamma 80.305(6) _cell_volume 2266.0(5) _cell_formula_units_Z 3 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10084 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1026 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8588 # 0.9808 _exptl_absorpt_correction_T_max 1.0000 # 0.9952 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45143 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.60 _reflns_number_total 10387 _reflns_number_gt 6389 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.9197P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10387 _refine_ls_number_parameters 610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1490 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 Si1 Si 0.35918(9) 0.33047(9) 0.32959(9) 0.0172(2) Uani 1 1 d . . . Si2 Si 0.0000 0.0000 0.0000 0.0193(3) Uani 1 2 d S . . F1 F 0.28579(18) 0.41752(19) 0.36916(18) 0.0224(5) Uani 1 1 d . . . F2 F 0.36550(18) 0.23389(19) 0.44863(17) 0.0236(5) Uani 1 1 d . . . F3 F 0.43268(18) 0.24322(19) 0.29110(18) 0.0228(5) Uani 1 1 d . . . F4 F 0.35348(18) 0.42825(19) 0.21057(17) 0.0216(5) Uani 1 1 d . . . F5 F -0.06783(19) 0.1050(2) 0.01668(19) 0.0266(6) Uani 1 1 d . . . F6 F -0.00521(19) -0.0778(2) 0.12428(18) 0.0271(6) Uani 1 1 d . . . P1 P 0.11781(8) 0.31278(9) 0.32340(8) 0.0173(2) Uani 1 1 d . . . P2 P 0.60138(8) 0.34814(8) 0.33821(8) 0.0170(2) Uani 1 1 d . . . P3 P 0.24672(9) 0.01929(9) 0.00131(8) 0.0206(2) Uani 1 1 d . . . O1 O 0.2384(2) 0.2827(2) 0.3164(2) 0.0193(6) Uani 1 1 d . . . O2 O 0.4807(2) 0.3786(2) 0.3426(2) 0.0187(6) Uani 1 1 d . . . O3 O 0.1258(2) 0.0461(2) 0.0078(2) 0.0235(6) Uani 1 1 d . . . C1 C 0.0602(3) 0.2108(3) 0.3080(3) 0.0187(8) Uani 1 1 d . . . C2 C 0.0952(3) 0.1926(3) 0.2233(3) 0.0212(9) Uani 1 1 d . . . H2 H 0.1477 0.2338 0.1759 0.025 Uiso 1 1 calc R . . C3 C 0.0537(3) 0.1148(3) 0.2082(3) 0.0251(9) Uani 1 1 d . . . H3 H 0.0765 0.1034 0.1500 0.030 Uiso 1 1 calc R . . C4 C -0.0215(4) 0.0536(4) 0.2787(4) 0.0287(10) Uani 1 1 d . . . H4 H -0.0502 0.0002 0.2685 0.034 Uiso 1 1 calc R . . C5 C -0.0551(4) 0.0693(4) 0.3634(3) 0.0280(10) Uani 1 1 d . . . H5 H -0.1056 0.0257 0.4118 0.034 Uiso 1 1 calc R . . C6 C -0.0153(3) 0.1487(3) 0.3783(3) 0.0225(9) Uani 1 1 d . . . H6 H -0.0395 0.1605 0.4361 0.027 Uiso 1 1 calc R . . C7 C 0.0688(3) 0.4465(3) 0.2260(3) 0.0199(9) Uani 1 1 d . . . C8 C -0.0038(3) 0.4572(3) 0.1586(3) 0.0228(9) Uani 1 1 d . . . H8 H -0.0280 0.3934 0.1628 0.027 Uiso 1 1 calc R . . C9 C -0.0414(4) 0.5617(4) 0.0846(3) 0.0270(10) Uani 1 1 d . . . H9 H -0.0908 0.5693 0.0382 0.032 Uiso 1 1 calc R . . C10 C -0.0063(3) 0.6545(4) 0.0792(3) 0.0254(10) Uani 1 1 d . . . H10 H -0.0320 0.7258 0.0292 0.030 Uiso 1 1 calc R . . C11 C 0.0660(3) 0.6440(3) 0.1463(3) 0.0229(9) Uani 1 1 d . . . H11 H 0.0897 0.7080 0.1421 0.028 Uiso 1 1 calc R . . C12 C 0.1038(3) 0.5409(3) 0.2194(3) 0.0232(9) Uani 1 1 d . . . H12 H 0.1536 0.5340 0.2653 0.028 Uiso 1 1 calc R . . C13 C 0.0692(3) 0.3077(3) 0.4443(3) 0.0204(9) Uani 1 1 d . . . C14 C 0.1207(3) 0.2292(3) 0.5309(3) 0.0232(9) Uani 1 1 d . . . H14 H 0.1818 0.1814 0.5253 0.028 Uiso 1 1 calc R . . C15 C 0.0822(4) 0.2214(4) 0.6251(3) 0.0255(10) Uani 1 1 d . . . H15 H 0.1166 0.1680 0.6845 0.031 Uiso 1 1 calc R . . C16 C -0.0070(4) 0.2918(4) 0.6324(3) 0.0319(11) Uani 1 1 d . . . H16 H -0.0340 0.2855 0.6972 0.038 Uiso 1 1 calc R . . C17 C -0.0570(4) 0.3708(4) 0.5470(4) 0.0331(11) Uani 1 1 d . . . H17 H -0.1167 0.4199 0.5526 0.040 Uiso 1 1 calc R . . C18 C -0.0193(4) 0.3780(4) 0.4525(3) 0.0280(10) Uani 1 1 d . . . H18 H -0.0543 0.4313 0.3934 0.034 Uiso 1 1 calc R . . C19 C 0.6571(3) 0.4503(3) 0.3544(3) 0.0212(9) Uani 1 1 d . . . C20 C 0.6186(4) 0.4677(4) 0.4389(4) 0.0290(10) Uani 1 1 d . . . H20 H 0.5657 0.4258 0.4850 0.035 Uiso 1 1 calc R . . C21 C 0.6574(4) 0.5460(4) 0.4554(4) 0.0368(12) Uani 1 1 d . . . H21 H 0.6313 0.5576 0.5129 0.044 Uiso 1 1 calc R . . C22 C 0.7340(4) 0.6072(4) 0.3886(4) 0.0364(12) Uani 1 1 d . . . H22 H 0.7602 0.6613 0.3998 0.044 Uiso 1 1 calc R . . C23 C 0.7729(4) 0.5899(4) 0.3050(4) 0.0330(11) Uani 1 1 d . . . H23 H 0.8258 0.6321 0.2592 0.040 Uiso 1 1 calc R . . C24 C 0.7349(3) 0.5111(4) 0.2877(3) 0.0249(9) Uani 1 1 d . . . H24 H 0.7621 0.4991 0.2306 0.030 Uiso 1 1 calc R . . C25 C 0.6480(3) 0.2151(3) 0.4375(3) 0.0208(9) Uani 1 1 d . . . C26 C 0.7208(4) 0.2036(4) 0.5061(3) 0.0291(10) Uani 1 1 d . . . H26 H 0.7480 0.2668 0.5001 0.035 Uiso 1 1 calc R . . C27 C 0.7532(4) 0.1010(4) 0.5823(4) 0.0358(12) Uani 1 1 d . . . H27 H 0.8026 0.0937 0.6286 0.043 Uiso 1 1 calc R . . C28 C 0.7142(4) 0.0077(4) 0.5919(4) 0.0343(11) Uani 1 1 d . . . H28 H 0.7356 -0.0627 0.6456 0.041 Uiso 1 1 calc R . . C29 C 0.6445(3) 0.0180(4) 0.5235(4) 0.0293(10) Uani 1 1 d . . . H29 H 0.6195 -0.0459 0.5288 0.035 Uiso 1 1 calc R . . C30 C 0.6105(3) 0.1212(3) 0.4465(3) 0.0227(9) Uani 1 1 d . . . H30 H 0.5617 0.1277 0.4000 0.027 Uiso 1 1 calc R . . C31 C 0.6520(3) 0.3525(3) 0.2188(3) 0.0185(8) Uani 1 1 d . . . C32 C 0.5964(3) 0.4253(3) 0.1325(3) 0.0228(9) Uani 1 1 d . . . H32 H 0.5319 0.4690 0.1384 0.027 Uiso 1 1 calc R . . C33 C 0.6359(3) 0.4334(4) 0.0390(3) 0.0290(10) Uani 1 1 d . . . H33 H 0.5986 0.4834 -0.0199 0.035 Uiso 1 1 calc R . . C34 C 0.7291(4) 0.3696(4) 0.0299(3) 0.0313(11) Uani 1 1 d . . . H34 H 0.7552 0.3756 -0.0350 0.038 Uiso 1 1 calc R . . C35 C 0.7846(4) 0.2970(4) 0.1147(4) 0.0339(11) Uani 1 1 d . . . H35 H 0.8487 0.2533 0.1081 0.041 Uiso 1 1 calc R . . C36 C 0.7464(3) 0.2882(4) 0.2095(3) 0.0278(10) Uani 1 1 d . . . H36 H 0.7843 0.2384 0.2679 0.033 Uiso 1 1 calc R . . C37 C 0.2998(3) 0.1087(4) 0.0373(3) 0.0221(9) Uani 1 1 d . . . C38 C 0.3633(3) 0.0684(4) 0.1202(3) 0.0257(9) Uani 1 1 d . . . H38 H 0.3825 -0.0090 0.1578 0.031 Uiso 1 1 calc R . . C39 C 0.3989(4) 0.1405(4) 0.1482(3) 0.0279(10) Uani 1 1 d . . . H39 H 0.4409 0.1125 0.2055 0.034 Uiso 1 1 calc R . . C40 C 0.3727(4) 0.2527(4) 0.0923(3) 0.0286(10) Uani 1 1 d . . . H40 H 0.3972 0.3020 0.1110 0.034 Uiso 1 1 calc R . . C41 C 0.3102(3) 0.2946(4) 0.0081(3) 0.0269(10) Uani 1 1 d . . . H41 H 0.2928 0.3721 -0.0304 0.032 Uiso 1 1 calc R . . C42 C 0.2741(3) 0.2231(4) -0.0186(3) 0.0254(9) Uani 1 1 d . . . H42 H 0.2314 0.2516 -0.0754 0.031 Uiso 1 1 calc R . . C43 C 0.2934(3) -0.1205(4) 0.0872(3) 0.0238(9) Uani 1 1 d . . . C44 C 0.2429(4) -0.1690(4) 0.1833(3) 0.0299(10) Uani 1 1 d . . . H44 H 0.1816 -0.1301 0.2014 0.036 Uiso 1 1 calc R . . C45 C 0.2822(4) -0.2747(4) 0.2529(4) 0.0343(11) Uani 1 1 d . . . H45 H 0.2479 -0.3079 0.3187 0.041 Uiso 1 1 calc R . . C46 C 0.3704(4) -0.3310(4) 0.2267(4) 0.0344(11) Uani 1 1 d . . . H46 H 0.3971 -0.4030 0.2748 0.041 Uiso 1 1 calc R . . C47 C 0.4210(4) -0.2843(4) 0.1309(4) 0.0382(12) Uani 1 1 d . . . H47 H 0.4814 -0.3241 0.1129 0.046 Uiso 1 1 calc R . . C48 C 0.3824(4) -0.1787(4) 0.0619(4) 0.0314(11) Uani 1 1 d . . . H48 H 0.4172 -0.1458 -0.0037 0.038 Uiso 1 1 calc R . . C49 C 0.3022(3) 0.0439(3) -0.1235(3) 0.0225(9) Uani 1 1 d . . . C50 C 0.2667(4) -0.0117(4) -0.1707(4) 0.0324(11) Uani 1 1 d . . . H50 H 0.2132 -0.0596 -0.1377 0.039 Uiso 1 1 calc R . . C51 C 0.3102(4) 0.0038(5) -0.2658(4) 0.0412(13) Uani 1 1 d . . . H51 H 0.2869 -0.0344 -0.2974 0.049 Uiso 1 1 calc R . . C52 C 0.3869(4) 0.0742(4) -0.3154(4) 0.0403(13) Uani 1 1 d . . . H52 H 0.4160 0.0841 -0.3807 0.048 Uiso 1 1 calc R . . C53 C 0.4214(4) 0.1300(4) -0.2699(4) 0.0373(12) Uani 1 1 d . . . H53 H 0.4732 0.1795 -0.3044 0.045 Uiso 1 1 calc R . . C54 C 0.3799(4) 0.1137(4) -0.1730(4) 0.0334(11) Uani 1 1 d . . . H54 H 0.4050 0.1507 -0.1410 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0176(5) 0.0186(5) 0.0171(5) -0.0084(4) -0.0024(4) -0.0040(4) Si2 0.0195(8) 0.0189(8) 0.0203(8) -0.0084(7) -0.0044(6) -0.0036(6) F1 0.0210(12) 0.0258(13) 0.0261(13) -0.0165(11) -0.0019(10) -0.0024(10) F2 0.0241(13) 0.0250(13) 0.0176(12) -0.0042(10) -0.0011(10) -0.0084(10) F3 0.0202(12) 0.0243(13) 0.0273(13) -0.0140(11) -0.0044(10) -0.0015(10) F4 0.0213(12) 0.0237(12) 0.0165(12) -0.0049(10) -0.0014(9) -0.0067(10) F5 0.0218(13) 0.0280(13) 0.0352(15) -0.0188(12) 0.0008(11) -0.0043(10) F6 0.0268(14) 0.0312(14) 0.0209(13) -0.0084(11) -0.0035(10) -0.0057(11) P1 0.0169(5) 0.0192(5) 0.0164(5) -0.0076(4) -0.0009(4) -0.0049(4) P2 0.0168(5) 0.0183(5) 0.0165(5) -0.0074(4) -0.0022(4) -0.0038(4) P3 0.0216(6) 0.0224(6) 0.0192(5) -0.0099(5) -0.0011(4) -0.0048(4) O1 0.0156(14) 0.0235(15) 0.0218(15) -0.0120(12) -0.0013(11) -0.0045(11) O2 0.0175(14) 0.0206(15) 0.0198(14) -0.0103(12) -0.0007(11) -0.0034(11) O3 0.0247(16) 0.0244(16) 0.0258(16) -0.0140(13) -0.0030(13) -0.0050(12) C1 0.016(2) 0.016(2) 0.021(2) -0.0048(17) -0.0094(16) 0.0009(15) C2 0.019(2) 0.024(2) 0.021(2) -0.0108(18) -0.0002(17) -0.0020(17) C3 0.026(2) 0.026(2) 0.028(2) -0.016(2) -0.0077(18) 0.0042(18) C4 0.029(2) 0.024(2) 0.037(3) -0.013(2) -0.012(2) -0.0049(19) C5 0.025(2) 0.026(2) 0.028(2) -0.005(2) -0.0059(19) -0.0071(18) C6 0.019(2) 0.027(2) 0.022(2) -0.0106(18) -0.0023(17) -0.0046(17) C7 0.023(2) 0.021(2) 0.0129(19) -0.0063(17) -0.0014(16) -0.0008(17) C8 0.024(2) 0.023(2) 0.023(2) -0.0123(18) -0.0050(18) -0.0003(17) C9 0.028(2) 0.031(2) 0.024(2) -0.014(2) -0.0076(19) 0.0013(19) C10 0.028(2) 0.021(2) 0.018(2) -0.0026(18) 0.0001(18) 0.0013(18) C11 0.025(2) 0.022(2) 0.021(2) -0.0096(18) 0.0048(17) -0.0052(17) C12 0.022(2) 0.027(2) 0.022(2) -0.0118(19) 0.0003(17) -0.0032(17) C13 0.023(2) 0.022(2) 0.020(2) -0.0110(18) 0.0006(17) -0.0067(17) C14 0.026(2) 0.021(2) 0.022(2) -0.0088(18) 0.0011(18) -0.0059(17) C15 0.034(3) 0.023(2) 0.021(2) -0.0074(18) -0.0001(19) -0.0164(19) C16 0.044(3) 0.037(3) 0.021(2) -0.016(2) 0.008(2) -0.019(2) C17 0.034(3) 0.033(3) 0.032(3) -0.017(2) 0.006(2) -0.002(2) C18 0.027(2) 0.031(2) 0.024(2) -0.012(2) 0.0030(19) -0.0034(19) C19 0.019(2) 0.024(2) 0.025(2) -0.0138(19) -0.0060(17) -0.0012(17) C20 0.028(2) 0.036(3) 0.032(3) -0.022(2) 0.004(2) -0.012(2) C21 0.029(3) 0.054(3) 0.047(3) -0.038(3) -0.004(2) -0.009(2) C22 0.032(3) 0.035(3) 0.051(3) -0.023(3) -0.014(2) -0.005(2) C23 0.030(3) 0.031(3) 0.038(3) -0.012(2) -0.004(2) -0.012(2) C24 0.024(2) 0.026(2) 0.026(2) -0.0115(19) -0.0018(18) -0.0061(18) C25 0.021(2) 0.020(2) 0.017(2) -0.0057(17) -0.0017(16) 0.0011(16) C26 0.033(3) 0.027(2) 0.027(2) -0.012(2) -0.0072(19) 0.0018(19) C27 0.038(3) 0.041(3) 0.028(3) -0.015(2) -0.019(2) 0.007(2) C28 0.033(3) 0.030(3) 0.024(2) -0.002(2) -0.002(2) 0.008(2) C29 0.025(2) 0.023(2) 0.035(3) -0.010(2) 0.004(2) -0.0020(18) C30 0.019(2) 0.021(2) 0.026(2) -0.0082(18) -0.0027(17) -0.0001(16) C31 0.019(2) 0.021(2) 0.017(2) -0.0087(17) -0.0003(16) -0.0057(16) C32 0.021(2) 0.026(2) 0.019(2) -0.0082(18) -0.0043(17) -0.0015(17) C33 0.023(2) 0.045(3) 0.017(2) -0.012(2) -0.0023(18) -0.006(2) C34 0.024(2) 0.049(3) 0.024(2) -0.019(2) 0.0046(19) -0.009(2) C35 0.027(2) 0.044(3) 0.031(3) -0.020(2) 0.005(2) -0.001(2) C36 0.023(2) 0.027(2) 0.028(2) -0.011(2) -0.0019(18) 0.0053(18) C37 0.016(2) 0.027(2) 0.025(2) -0.0133(19) -0.0010(17) -0.0020(17) C38 0.025(2) 0.025(2) 0.028(2) -0.0114(19) 0.0012(18) -0.0100(18) C39 0.028(2) 0.035(3) 0.021(2) -0.012(2) -0.0027(18) -0.0064(19) C40 0.029(2) 0.035(3) 0.030(2) -0.022(2) 0.002(2) -0.008(2) C41 0.027(2) 0.026(2) 0.027(2) -0.0103(19) 0.0026(19) -0.0088(18) C42 0.022(2) 0.028(2) 0.027(2) -0.012(2) -0.0015(18) -0.0065(18) C43 0.026(2) 0.025(2) 0.022(2) -0.0119(19) -0.0013(18) -0.0050(18) C44 0.027(2) 0.035(3) 0.022(2) -0.010(2) 0.0002(18) 0.000(2) C45 0.028(3) 0.036(3) 0.030(3) -0.007(2) -0.001(2) -0.007(2) C46 0.035(3) 0.022(2) 0.037(3) -0.004(2) -0.005(2) -0.005(2) C47 0.033(3) 0.030(3) 0.044(3) -0.013(2) 0.004(2) 0.002(2) C48 0.037(3) 0.023(2) 0.030(2) -0.010(2) 0.005(2) -0.005(2) C49 0.022(2) 0.025(2) 0.017(2) -0.0086(18) -0.0025(17) 0.0026(17) C50 0.024(2) 0.050(3) 0.030(3) -0.023(2) -0.0007(19) -0.007(2) C51 0.036(3) 0.061(4) 0.032(3) -0.028(3) -0.005(2) 0.004(3) C52 0.035(3) 0.053(3) 0.019(2) -0.010(2) -0.002(2) 0.012(2) C53 0.040(3) 0.033(3) 0.028(3) -0.008(2) 0.010(2) 0.000(2) C54 0.038(3) 0.032(3) 0.029(3) -0.014(2) 0.004(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 F2 1.654(2) . ? Si1 F4 1.659(2) . ? Si1 F3 1.660(3) . ? Si1 F1 1.667(2) . ? Si1 O1 1.832(3) . ? Si1 O2 1.842(3) . ? Si2 F6 1.654(2) 2 ? Si2 F6 1.654(2) . ? Si2 F5 1.657(2) 2 ? Si2 F5 1.657(2) . ? Si2 O3 1.848(3) 2 ? Si2 O3 1.848(3) . ? P1 O1 1.519(3) . ? P1 C13 1.798(4) . ? P1 C1 1.799(4) . ? P1 C7 1.804(4) . ? P2 O2 1.519(3) . ? P2 C31 1.787(4) . ? P2 C19 1.795(4) . ? P2 C25 1.801(4) . ? P3 O3 1.518(3) . ? P3 C43 1.795(4) . ? P3 C49 1.795(4) . ? P3 C37 1.797(4) . ? C1 C6 1.392(6) . ? C1 C2 1.400(6) . ? C2 C3 1.383(6) . ? C2 H2 0.9500 . ? C3 C4 1.385(6) . ? C3 H3 0.9500 . ? C4 C5 1.378(6) . ? C4 H4 0.9500 . ? C5 C6 1.391(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.389(6) . ? C7 C12 1.399(6) . ? C8 C9 1.396(6) . ? C8 H8 0.9500 . ? C9 C10 1.386(6) . ? C9 H9 0.9500 . ? C10 C11 1.382(6) . ? C10 H10 0.9500 . ? C11 C12 1.380(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.386(6) . ? C13 C14 1.395(6) . ? C14 C15 1.384(6) . ? C14 H14 0.9500 . ? C15 C16 1.389(7) . ? C15 H15 0.9500 . ? C16 C17 1.377(7) . ? C16 H16 0.9500 . ? C17 C18 1.388(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.387(6) . ? C19 C20 1.398(6) . ? C20 C21 1.384(6) . ? C20 H20 0.9500 . ? C21 C22 1.378(7) . ? C21 H21 0.9500 . ? C22 C23 1.386(7) . ? C22 H22 0.9500 . ? C23 C24 1.391(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.394(6) . ? C25 C26 1.401(6) . ? C26 C27 1.376(6) . ? C26 H26 0.9500 . ? C27 C28 1.392(7) . ? C27 H27 0.9500 . ? C28 C29 1.375(7) . ? C28 H28 0.9500 . ? C29 C30 1.390(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.396(6) . ? C31 C32 1.398(6) . ? C32 C33 1.378(6) . ? C32 H32 0.9500 . ? C33 C34 1.381(6) . ? C33 H33 0.9500 . ? C34 C35 1.383(7) . ? C34 H34 0.9500 . ? C35 C36 1.387(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.395(6) . ? C37 C42 1.401(6) . ? C38 C39 1.393(6) . ? C38 H38 0.9500 . ? C39 C40 1.377(6) . ? C39 H39 0.9500 . ? C40 C41 1.400(6) . ? C40 H40 0.9500 . ? C41 C42 1.375(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.387(6) . ? C43 C44 1.389(6) . ? C44 C45 1.390(6) . ? C44 H44 0.9500 . ? C45 C46 1.371(7) . ? C45 H45 0.9500 . ? C46 C47 1.384(7) . ? C46 H46 0.9500 . ? C47 C48 1.384(6) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.385(6) . ? C49 C50 1.404(6) . ? C50 C51 1.382(7) . ? C50 H50 0.9500 . ? C51 C52 1.381(8) . ? C51 H51 0.9500 . ? C52 C53 1.380(8) . ? C52 H52 0.9500 . ? C53 C54 1.397(6) . ? C53 H53 0.9500 . ? C54 H54 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 F2 Si1 F4 179.34(15) . . ? F2 Si1 F3 89.87(13) . . ? F4 Si1 F3 90.47(13) . . ? F2 Si1 F1 89.71(13) . . ? F4 Si1 F1 89.94(13) . . ? F3 Si1 F1 179.54(15) . . ? F2 Si1 O1 90.50(13) . . ? F4 Si1 O1 90.07(13) . . ? F3 Si1 O1 89.09(13) . . ? F1 Si1 O1 91.10(13) . . ? F2 Si1 O2 89.58(13) . . ? F4 Si1 O2 89.85(13) . . ? F3 Si1 O2 90.85(13) . . ? F1 Si1 O2 88.96(13) . . ? O1 Si1 O2 179.90(14) . . ? F6 Si2 F6 180.0(3) 2 . ? F6 Si2 F5 89.76(12) 2 2 ? F6 Si2 F5 90.24(12) . 2 ? F6 Si2 F5 90.24(12) 2 . ? F6 Si2 F5 89.76(12) . . ? F5 Si2 F5 180.0(2) 2 . ? F6 Si2 O3 90.16(12) 2 2 ? F6 Si2 O3 89.84(12) . 2 ? F5 Si2 O3 89.02(12) 2 2 ? F5 Si2 O3 90.98(12) . 2 ? F6 Si2 O3 89.84(12) 2 . ? F6 Si2 O3 90.16(12) . . ? F5 Si2 O3 90.98(12) 2 . ? F5 Si2 O3 89.02(12) . . ? O3 Si2 O3 180.00(18) 2 . ? O1 P1 C13 112.79(18) . . ? O1 P1 C1 105.88(17) . . ? C13 P1 C1 108.20(19) . . ? O1 P1 C7 114.33(18) . . ? C13 P1 C7 107.82(19) . . ? C1 P1 C7 107.53(19) . . ? O2 P2 C31 112.41(17) . . ? O2 P2 C19 105.81(17) . . ? C31 P2 C19 108.42(19) . . ? O2 P2 C25 114.01(18) . . ? C31 P2 C25 108.46(19) . . ? C19 P2 C25 107.5(2) . . ? O3 P3 C43 113.15(18) . . ? O3 P3 C49 113.96(18) . . ? C43 P3 C49 107.7(2) . . ? O3 P3 C37 106.12(17) . . ? C43 P3 C37 107.6(2) . . ? C49 P3 C37 108.0(2) . . ? P1 O1 Si1 137.86(18) . . ? P2 O2 Si1 138.66(18) . . ? P3 O3 Si2 142.47(19) . . ? C6 C1 C2 119.7(4) . . ? C6 C1 P1 122.2(3) . . ? C2 C1 P1 118.1(3) . . ? C3 C2 C1 120.4(4) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 119.5(4) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C8 C7 C12 119.7(4) . . ? C8 C7 P1 121.2(3) . . ? C12 C7 P1 119.2(3) . . ? C7 C8 C9 120.0(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 119.6(4) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.3(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 120.0(4) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C18 C13 C14 120.1(4) . . ? C18 C13 P1 121.1(3) . . ? C14 C13 P1 118.8(3) . . ? C15 C14 C13 119.6(4) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.7(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.9(4) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 119.5(4) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 120.1(4) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C24 C19 C20 119.8(4) . . ? C24 C19 P2 123.1(3) . . ? C20 C19 P2 117.1(3) . . ? C21 C20 C19 120.1(4) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.1(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.1(4) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.5(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 119.5(4) . . ? C19 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C30 C25 C26 119.1(4) . . ? C30 C25 P2 119.3(3) . . ? C26 C25 P2 121.7(3) . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.5(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 119.7(4) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C25 120.1(4) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C36 C31 C32 119.8(4) . . ? C36 C31 P2 121.9(3) . . ? C32 C31 P2 118.3(3) . . ? C33 C32 C31 119.6(4) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 120.6(4) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C35 120.3(4) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 119.8(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C31 119.9(4) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C38 C37 C42 118.9(4) . . ? C38 C37 P3 122.4(3) . . ? C42 C37 P3 118.6(3) . . ? C39 C38 C37 120.6(4) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C40 C39 C38 119.5(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 120.6(4) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C42 C41 C40 119.7(4) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C37 120.6(4) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? C48 C43 C44 119.3(4) . . ? C48 C43 P3 121.4(3) . . ? C44 C43 P3 119.1(3) . . ? C43 C44 C45 119.8(4) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 120.1(4) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.8(4) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C46 C47 C48 119.2(4) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? C47 C48 C43 120.8(4) . . ? C47 C48 H48 119.6 . . ? C43 C48 H48 119.6 . . ? C54 C49 C50 119.5(4) . . ? C54 C49 P3 122.0(3) . . ? C50 C49 P3 118.4(3) . . ? C51 C50 C49 119.4(5) . . ? C51 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C52 C51 C50 121.0(5) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C53 119.9(5) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C52 C53 C54 120.0(5) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C49 C54 C53 120.2(5) . . ? C49 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.459 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.094 #===END OF CIF ============================================================== # 10wz328a data_10wz328a _database_code_depnum_ccdc_archive 'CCDC 791400' #TrackingRef '- Si_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-04-07 _audit_author_name 'Webster, M.' _chemical_name_systematic ; tetrafluoro(methanediylbis(dimethylphosphane) dioxide)germanium(IV) ; # CH2{P(O)Me2}2 = C5H14O2P2 # methylenebis(dimethylphosphine) dioxide (ACD iLab defaults) looks wrong? # methanediylbis(dimethylphosphane) dioxide (ACD iLab selected options) # methanediylbis(dimethylphosphane) dioxide (chemspider) # bis(dimethylphosphanyl)methane dioxide (mw) # SMILES: CP(C)(=O)CP(C)(=O)C _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H14 F4 Ge O2 P2' _chemical_formula_sum 'C5 H14 F4 Ge O2 P2' _chemical_formula_weight 316.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C m c a' _space_group_IT_number 64 _space_group_name_Hall '-C 2bc 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 13.533(4) _cell_length_b 11.142(4) _cell_length_c 14.620(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2204.4(12) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2514 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 3.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3072 # 0.6055 _exptl_absorpt_correction_T_max 1.0000 # 0.9697 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12581 _diffrn_reflns_av_R_equivalents 0.1140 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.71 _reflns_number_total 1324 _reflns_number_gt 1096 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _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^)+(0.0175P)^2^+44.7600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1324 _refine_ls_number_parameters 72 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1357 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 0.22018(8) 0.16507(6) 0.0250(3) Uani 1 2 d S . . P1 P 0.11125(13) 0.29151(15) 0.34828(10) 0.0299(4) Uani 1 1 d . . . F1 F 0.0951(3) 0.1627(3) 0.0925(2) 0.0356(9) Uani 1 1 d . . . F2 F 0.0000 0.3598(5) 0.1069(4) 0.0383(13) Uani 1 2 d S . . F3 F 0.0000 0.0856(5) 0.2307(3) 0.0397(14) Uani 1 2 d S . . O1 O 0.1025(3) 0.2815(4) 0.2441(3) 0.0310(10) Uani 1 1 d . . . C1 C 0.1376(7) 0.1525(7) 0.4022(5) 0.048(2) Uani 1 1 d . . . H1A H 0.0891 0.0924 0.3828 0.073 Uiso 1 1 calc R . . H1B H 0.1343 0.1624 0.4687 0.073 Uiso 1 1 calc R . . H1C H 0.2040 0.1259 0.3848 0.073 Uiso 1 1 calc R . . C2 C 0.2062(5) 0.3951(7) 0.3762(5) 0.0412(17) Uani 1 1 d . . . H2A H 0.2692 0.3663 0.3517 0.062 Uiso 1 1 calc R . . H2B H 0.2110 0.4027 0.4428 0.062 Uiso 1 1 calc R . . H2C H 0.1906 0.4735 0.3495 0.062 Uiso 1 1 calc R . . C3 C 0.0000 0.3541(7) 0.3946(5) 0.0244(17) Uani 1 2 d S . . H3A H 0.0000 0.3418 0.4617 0.029 Uiso 1 2 calc SR . . H3B H 0.0000 0.4417 0.3832 0.029 Uiso 1 2 calc SR . . 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 0.0275(5) 0.0276(5) 0.0199(4) -0.0019(4) 0.000 0.000 P1 0.0293(9) 0.0340(8) 0.0263(8) -0.0050(6) -0.0033(6) 0.0026(7) F1 0.035(2) 0.049(2) 0.0230(17) -0.0097(16) 0.0016(15) 0.0055(18) F2 0.052(4) 0.033(3) 0.030(3) 0.006(2) 0.000 0.000 F3 0.066(4) 0.024(3) 0.029(3) -0.001(2) 0.000 0.000 O1 0.028(2) 0.038(2) 0.027(2) -0.0070(19) 0.0022(17) -0.0001(19) C1 0.066(5) 0.048(4) 0.032(3) -0.003(3) -0.012(3) 0.025(4) C2 0.025(3) 0.055(4) 0.044(4) -0.020(3) -0.005(3) -0.001(3) C3 0.031(4) 0.021(4) 0.021(4) 0.003(3) 0.000 0.000 _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 1.772(5) . ? Ge1 F3 1.780(5) . ? Ge1 F1 1.787(4) 12 ? Ge1 F1 1.787(4) . ? Ge1 O1 1.930(4) . ? Ge1 O1 1.930(4) 12 ? P1 O1 1.532(4) . ? P1 C1 1.774(7) . ? P1 C2 1.774(7) . ? P1 C3 1.792(5) . ? 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 P1 1.792(5) 12 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 Ge1 F3 176.0(2) . . ? F2 Ge1 F1 91.71(18) . 12 ? F3 Ge1 F1 91.04(17) . 12 ? F2 Ge1 F1 91.71(18) . . ? F3 Ge1 F1 91.04(17) . . ? F1 Ge1 F1 92.1(2) 12 . ? F2 Ge1 O1 88.64(18) . . ? F3 Ge1 O1 88.60(17) . . ? F1 Ge1 O1 179.62(19) 12 . ? F1 Ge1 O1 87.98(17) . . ? F2 Ge1 O1 88.64(18) . 12 ? F3 Ge1 O1 88.60(17) . 12 ? F1 Ge1 O1 87.98(17) 12 12 ? F1 Ge1 O1 179.62(19) . 12 ? O1 Ge1 O1 91.9(2) . 12 ? O1 P1 C1 113.2(3) . . ? O1 P1 C2 109.4(3) . . ? C1 P1 C2 108.7(4) . . ? O1 P1 C3 109.8(3) . . ? C1 P1 C3 109.9(4) . . ? C2 P1 C3 105.5(3) . . ? P1 O1 Ge1 132.6(3) . . ? 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 . . ? P1 C3 P1 114.3(4) 12 . ? P1 C3 H3A 108.7 12 . ? P1 C3 H3A 108.7 . . ? P1 C3 H3B 108.7 12 . ? P1 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.510 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.157 #===END OF CIF ============================================================== # 09wz1101 data_09wz1101 _database_code_depnum_ccdc_archive 'CCDC 791401' #TrackingRef '- Si_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-03-20 _audit_author_name 'Zhang, W.' _chemical_name_systematic ; tetrafluoro(bis(diphenylphosphino)methane dioxide)germanium(IV) dichloromethane solvate ; # C25H22O2P2 = dppmO2 # methylenebis(diphenylphosphine) dioxide (iLab defaults) # methanediylbis(diphenylphosphane) dioxide (iLab selected options) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H22 F4 Ge O2 P2, C H2 Cl2' _chemical_formula_sum 'C26 H24 Cl2 F4 Ge O2 P2' _chemical_formula_weight 649.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' 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 12.870(3) _cell_length_b 13.779(3) _cell_length_c 15.830(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.748(12) _cell_angle_gamma 90.00 _cell_volume 2804.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6449 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.447 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3720 # shelxl 0.8930 _exptl_absorpt_correction_T_max 1.0000 # 0.9444 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26962 _diffrn_reflns_av_R_equivalents 0.1214 _diffrn_reflns_av_sigmaI/netI 0.1055 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5479 _reflns_number_gt 3667 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _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^+28.2000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5479 _refine_ls_number_parameters 344 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1540 _refine_ls_R_factor_gt 0.0963 _refine_ls_wR_factor_ref 0.1861 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.125 _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 0.39250(6) 0.32987(6) 0.71559(5) 0.0248(2) Uani 1 1 d . . . P1 P 0.34360(14) 0.15350(14) 0.83396(12) 0.0224(4) Uani 1 1 d . . . P2 P 0.33390(15) 0.12338(14) 0.64703(12) 0.0211(4) Uani 1 1 d . . . F1 F 0.3858(3) 0.4291(3) 0.7861(3) 0.0361(11) Uani 1 1 d . . . F2 F 0.2557(3) 0.3146(3) 0.7145(3) 0.0355(11) Uani 1 1 d . . . F3 F 0.5292(3) 0.3326(3) 0.7200(3) 0.0296(10) Uani 1 1 d . . . F4 F 0.3836(4) 0.4033(3) 0.6237(3) 0.0428(13) Uani 1 1 d . . . O1 O 0.4048(4) 0.2440(4) 0.8117(3) 0.0278(12) Uani 1 1 d . . . O2 O 0.3984(4) 0.2156(4) 0.6458(3) 0.0259(12) Uani 1 1 d . . . C1 C 0.2627(6) 0.1795(6) 0.9195(4) 0.0268(17) Uani 1 1 d . . . C2 C 0.1823(6) 0.1190(6) 0.9428(5) 0.0333(19) Uani 1 1 d . . . H2 H 0.1661 0.0618 0.9113 0.040 Uiso 1 1 calc R . . C3 C 0.1265(7) 0.1429(7) 1.0118(6) 0.046(2) Uani 1 1 d . . . H3 H 0.0710 0.1022 1.0273 0.055 Uiso 1 1 calc R . . C4 C 0.1496(7) 0.2240(7) 1.0582(5) 0.043(2) Uani 1 1 d . . . H4 H 0.1113 0.2387 1.1064 0.052 Uiso 1 1 calc R . . C5 C 0.2290(7) 0.2853(6) 1.0350(5) 0.038(2) Uani 1 1 d . . . H5 H 0.2442 0.3425 1.0667 0.046 Uiso 1 1 calc R . . C6 C 0.2857(6) 0.2631(6) 0.9661(5) 0.0311(18) Uani 1 1 d . . . H6 H 0.3404 0.3047 0.9504 0.037 Uiso 1 1 calc R . . C7 C 0.4326(6) 0.0577(6) 0.8605(5) 0.0282(18) Uani 1 1 d . . . C8 C 0.5357(6) 0.0683(6) 0.8387(5) 0.0337(19) Uani 1 1 d . . . H8 H 0.5587 0.1270 0.8143 0.040 Uiso 1 1 calc R . . C9 C 0.6048(7) -0.0092(7) 0.8536(6) 0.043(2) Uani 1 1 d . . . H9 H 0.6749 -0.0037 0.8379 0.052 Uiso 1 1 calc R . . C10 C 0.5715(7) -0.0929(7) 0.8906(6) 0.042(2) Uani 1 1 d . . . H10 H 0.6191 -0.1447 0.9013 0.051 Uiso 1 1 calc R . . C11 C 0.4713(7) -0.1023(7) 0.9121(6) 0.042(2) Uani 1 1 d . . . H11 H 0.4493 -0.1610 0.9371 0.051 Uiso 1 1 calc R . . C12 C 0.4007(7) -0.0281(6) 0.8982(5) 0.0335(19) Uani 1 1 d . . . H12 H 0.3309 -0.0353 0.9142 0.040 Uiso 1 1 calc R . . C13 C 0.2634(6) 0.1127(5) 0.7433(5) 0.0248(16) Uani 1 1 d . . . H13A H 0.2430 0.0443 0.7515 0.030 Uiso 1 1 calc R . . H13B H 0.1993 0.1524 0.7381 0.030 Uiso 1 1 calc R . . C14 C 0.4197(6) 0.0220(5) 0.6402(4) 0.0215(16) Uani 1 1 d . . . C15 C 0.3896(6) -0.0723(6) 0.6636(5) 0.0323(19) Uani 1 1 d . . . H15 H 0.3222 -0.0836 0.6836 0.039 Uiso 1 1 calc R . . C16 C 0.4582(7) -0.1472(6) 0.6574(6) 0.042(2) Uani 1 1 d . . . H16 H 0.4376 -0.2108 0.6726 0.050 Uiso 1 1 calc R . . C17 C 0.5570(7) -0.1325(6) 0.6295(6) 0.038(2) Uani 1 1 d . . . H17 H 0.6045 -0.1851 0.6266 0.046 Uiso 1 1 calc R . . C18 C 0.5859(6) -0.0399(6) 0.6057(5) 0.035(2) Uani 1 1 d . . . H18 H 0.6534 -0.0291 0.5858 0.042 Uiso 1 1 calc R . . C19 C 0.5177(6) 0.0362(6) 0.6107(5) 0.0321(19) Uani 1 1 d . . . H19 H 0.5382 0.0993 0.5938 0.039 Uiso 1 1 calc R . . C20 C 0.2411(6) 0.1243(6) 0.5585(4) 0.0276(18) Uani 1 1 d . . . C21 C 0.1825(6) 0.0412(7) 0.5387(5) 0.036(2) Uani 1 1 d . . . H21 H 0.1879 -0.0150 0.5733 0.043 Uiso 1 1 calc R . . C22 C 0.1158(7) 0.0432(9) 0.4665(6) 0.055(3) Uani 1 1 d . . . H22 H 0.0750 -0.0122 0.4514 0.066 Uiso 1 1 calc R . . C23 C 0.1091(8) 0.1259(10) 0.4172(6) 0.059(3) Uani 1 1 d . . . H23 H 0.0636 0.1270 0.3681 0.071 Uiso 1 1 calc R . . C24 C 0.1671(9) 0.2058(9) 0.4382(6) 0.063(3) Uani 1 1 d . . . H24 H 0.1604 0.2620 0.4036 0.075 Uiso 1 1 calc R . . C25 C 0.2356(7) 0.2074(7) 0.5084(5) 0.041(2) Uani 1 1 d . . . H25 H 0.2770 0.2629 0.5218 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.3823(3) 0.4003(3) 0.3777(4) 0.139(2) Uani 1 1 d D . . Cl2 Cl 0.4608(6) 0.3508(3) 0.1984(4) 0.096(3) Uani 0.732(13) 1 d PD . . Cl3 Cl 0.344(2) 0.3633(11) 0.2346(12) 0.158(16) Uani 0.268(13) 1 d PD A 2 C26 C 0.4323(11) 0.4408(10) 0.2795(7) 0.123(7) Uani 1 1 d D A 1 H26A H 0.4972 0.4773 0.2931 0.147 Uiso 1 1 calc R A 1 H26B H 0.3816 0.4875 0.2537 0.147 Uiso 1 1 calc R A 1 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 0.0277(4) 0.0196(4) 0.0273(4) -0.0022(3) 0.0040(3) 0.0025(4) P1 0.0213(9) 0.0250(11) 0.0213(10) -0.0012(8) 0.0050(8) 0.0004(8) P2 0.0221(10) 0.0194(10) 0.0220(10) -0.0025(8) 0.0024(8) 0.0002(8) F1 0.035(3) 0.031(3) 0.043(3) -0.012(2) 0.006(2) 0.005(2) F2 0.024(2) 0.038(3) 0.044(3) -0.008(2) -0.001(2) 0.004(2) F3 0.030(2) 0.024(2) 0.035(2) -0.0046(19) 0.0101(19) -0.008(2) F4 0.064(3) 0.020(2) 0.044(3) 0.008(2) -0.001(3) 0.002(2) O1 0.032(3) 0.030(3) 0.022(3) 0.004(2) 0.004(2) -0.007(2) O2 0.033(3) 0.021(3) 0.025(3) -0.005(2) 0.009(2) -0.005(2) C1 0.032(4) 0.027(4) 0.022(4) 0.002(3) 0.007(3) 0.005(4) C2 0.034(5) 0.026(4) 0.041(5) 0.002(4) 0.019(4) 0.001(4) C3 0.044(5) 0.045(6) 0.050(6) 0.012(5) 0.024(5) -0.001(5) C4 0.056(6) 0.039(5) 0.037(5) 0.009(4) 0.023(4) 0.024(5) C5 0.059(6) 0.022(4) 0.033(5) -0.004(4) 0.007(4) 0.006(4) C6 0.029(4) 0.035(5) 0.029(4) -0.003(4) 0.009(3) 0.005(4) C7 0.029(4) 0.035(5) 0.021(4) -0.009(3) 0.005(3) -0.001(4) C8 0.027(4) 0.043(5) 0.030(4) -0.001(4) -0.001(3) 0.000(4) C9 0.026(5) 0.061(7) 0.041(5) -0.011(5) -0.008(4) 0.018(4) C10 0.041(5) 0.044(6) 0.041(5) 0.001(4) -0.009(4) 0.025(5) C11 0.055(6) 0.032(5) 0.041(5) 0.001(4) 0.009(4) 0.010(4) C12 0.034(5) 0.032(5) 0.035(5) 0.008(4) 0.011(4) 0.009(4) C13 0.024(4) 0.021(4) 0.030(4) -0.003(3) 0.002(3) -0.004(3) C14 0.026(4) 0.024(4) 0.014(4) -0.004(3) -0.004(3) 0.003(3) C15 0.028(4) 0.029(5) 0.041(5) -0.001(4) 0.010(4) -0.005(4) C16 0.039(5) 0.028(5) 0.058(6) 0.000(4) 0.013(4) -0.002(4) C17 0.034(5) 0.033(5) 0.048(5) -0.006(4) 0.010(4) 0.012(4) C18 0.024(4) 0.046(5) 0.036(5) 0.002(4) 0.010(4) 0.009(4) C19 0.033(5) 0.025(4) 0.039(5) -0.006(4) 0.006(4) -0.003(4) C20 0.026(4) 0.039(5) 0.018(4) -0.003(3) 0.007(3) 0.011(4) C21 0.026(4) 0.047(5) 0.035(5) -0.001(4) 0.001(4) -0.006(4) C22 0.032(5) 0.094(9) 0.038(5) -0.004(6) -0.009(4) -0.006(5) C23 0.037(5) 0.103(10) 0.036(6) -0.002(6) -0.015(4) 0.028(6) C24 0.073(8) 0.075(8) 0.037(6) 0.017(5) -0.011(5) 0.016(7) C25 0.051(6) 0.034(5) 0.038(5) 0.001(4) -0.002(4) 0.011(4) Cl1 0.082(3) 0.054(2) 0.282(7) 0.039(3) 0.029(3) 0.0107(19) Cl2 0.122(6) 0.039(2) 0.121(4) 0.010(2) -0.071(4) -0.008(3) Cl3 0.28(4) 0.070(10) 0.116(15) 0.017(9) -0.13(2) -0.042(14) C26 0.086(11) 0.054(9) 0.23(2) 0.041(11) 0.012(12) -0.015(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 F3 1.757(4) . ? Ge1 F1 1.770(4) . ? Ge1 F4 1.771(5) . ? Ge1 F2 1.772(4) . ? Ge1 O2 1.926(5) . ? Ge1 O1 1.928(5) . ? P1 O1 1.525(5) . ? P1 C1 1.784(7) . ? P1 C7 1.784(8) . ? P1 C13 1.816(7) . ? P2 O2 1.519(5) . ? P2 C14 1.787(7) . ? P2 C20 1.797(8) . ? P2 C13 1.816(7) . ? C1 C6 1.392(11) . ? C1 C2 1.392(11) . ? C2 C3 1.376(11) . ? C2 H2 0.9500 . ? C3 C4 1.363(13) . ? C3 H3 0.9500 . ? C4 C5 1.389(12) . ? C4 H4 0.9500 . ? C5 C6 1.375(11) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.394(11) . ? C7 C12 1.395(11) . ? C8 C9 1.403(12) . ? C8 H8 0.9500 . ? C9 C10 1.372(13) . ? C9 H9 0.9500 . ? C10 C11 1.356(13) . ? C10 H10 0.9500 . ? C11 C12 1.378(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C19 1.381(11) . ? C14 C15 1.410(10) . ? C15 C16 1.364(11) . ? C15 H15 0.9500 . ? C16 C17 1.381(12) . ? C16 H16 0.9500 . ? C17 C18 1.386(12) . ? C17 H17 0.9500 . ? C18 C19 1.372(11) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.393(11) . ? C20 C21 1.398(11) . ? C21 C22 1.396(12) . ? C21 H21 0.9500 . ? C22 C23 1.381(15) . ? C22 H22 0.9500 . ? C23 C24 1.362(15) . ? C23 H23 0.9500 . ? C24 C25 1.386(13) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? Cl1 C26 1.799(11) . ? Cl1 Cl3 2.350(18) . ? Cl2 Cl3 1.64(3) . ? Cl2 C26 1.835(12) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 Ge1 F1 92.1(2) . . ? F3 Ge1 F4 92.6(2) . . ? F1 Ge1 F4 94.2(2) . . ? F3 Ge1 F2 174.2(2) . . ? F1 Ge1 F2 91.1(2) . . ? F4 Ge1 F2 92.0(2) . . ? F3 Ge1 O2 88.5(2) . . ? F1 Ge1 O2 175.8(2) . . ? F4 Ge1 O2 89.9(2) . . ? F2 Ge1 O2 87.9(2) . . ? F3 Ge1 O1 86.4(2) . . ? F1 Ge1 O1 88.9(2) . . ? F4 Ge1 O1 176.8(2) . . ? F2 Ge1 O1 88.8(2) . . ? O2 Ge1 O1 87.0(2) . . ? O1 P1 C1 109.8(3) . . ? O1 P1 C7 109.0(3) . . ? C1 P1 C7 111.1(4) . . ? O1 P1 C13 110.5(3) . . ? C1 P1 C13 109.4(4) . . ? C7 P1 C13 106.9(4) . . ? O2 P2 C14 108.3(3) . . ? O2 P2 C20 109.1(3) . . ? C14 P2 C20 110.4(3) . . ? O2 P2 C13 111.9(3) . . ? C14 P2 C13 108.8(3) . . ? C20 P2 C13 108.3(3) . . ? P1 O1 Ge1 131.3(3) . . ? P2 O2 Ge1 129.8(3) . . ? C6 C1 C2 119.8(7) . . ? C6 C1 P1 116.8(6) . . ? C2 C1 P1 123.3(6) . . ? C3 C2 C1 119.2(8) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 121.1(8) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 120.0(8) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0(8) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 119.8(8) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C8 C7 C12 119.8(8) . . ? C8 C7 P1 118.2(6) . . ? C12 C7 P1 121.9(6) . . ? C7 C8 C9 118.8(8) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 120.2(8) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.5(8) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 121.2(9) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 119.4(8) . . ? C11 C12 H12 120.3 . . ? C7 C12 H12 120.3 . . ? P2 C13 P1 110.5(4) . . ? P2 C13 H13A 109.5 . . ? P1 C13 H13A 109.5 . . ? P2 C13 H13B 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C19 C14 C15 119.1(7) . . ? C19 C14 P2 119.1(6) . . ? C15 C14 P2 121.8(6) . . ? C16 C15 C14 119.4(7) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 121.4(8) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C18 119.0(8) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 120.5(8) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C14 120.5(8) . . ? C18 C19 H19 119.7 . . ? C14 C19 H19 119.7 . . ? C25 C20 C21 122.2(8) . . ? C25 C20 P2 117.6(7) . . ? C21 C20 P2 120.0(6) . . ? C22 C21 C20 118.2(9) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C23 C22 C21 119.8(10) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.7(9) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 121.9(10) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C24 C25 C20 117.2(9) . . ? C24 C25 H25 121.4 . . ? C20 C25 H25 121.4 . . ? C26 Cl1 Cl3 45.6(6) . . ? Cl3 Cl2 C26 57.8(6) . . ? Cl2 Cl3 Cl1 102.1(8) . . ? Cl1 C26 Cl2 119.1(8) . . ? Cl1 C26 H26A 107.5 . . ? Cl2 C26 H26A 107.5 . . ? Cl1 C26 H26B 107.5 . . ? Cl2 C26 H26B 107.5 . . ? H26A C26 H26B 107.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.120 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.138 #===END OF CIF ============================================================== # 10wz218a data_10wz218a _database_code_depnum_ccdc_archive 'CCDC 791402' #TrackingRef '- Si_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-06-29 _audit_author_name 'Webster, M.' _chemical_name_systematic ; methanediylbis(dimethylphosphane) dioxide ; # CH2{P(O)Me2}2 = Me2P(O)CH2P(O)Me2 = C5H14O2P2 # methanediylbis(dimethylphosphane) dioxide (ACD iLab selected options) # methanediylbis(dimethylphosphane) dioxide (chemspider) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C5 H14 O2 P2' _chemical_formula_sum 'C5 H14 O2 P2' _chemical_formula_weight 168.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' 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 31.360(6) _cell_length_b 5.7109(15) _cell_length_c 9.488(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.231(15) _cell_angle_gamma 90.00 _cell_volume 1692.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2064 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6474 # _exptl_absorpt_correction_T_max 0.7456 # _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11012 _diffrn_reflns_av_R_equivalents 0.1402 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1645 _reflns_number_gt 1024 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _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^)+(0.0555P)^2^+2.9765P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1645 _refine_ls_number_parameters 86 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.42339(3) 0.13406(18) 0.48958(11) 0.0244(3) Uani 1 1 d . . . P2 P 0.32502(3) 0.12341(18) 0.45181(11) 0.0247(3) Uani 1 1 d . . . O1 O 0.42697(9) -0.1206(4) 0.5223(3) 0.0312(7) Uani 1 1 d . . . O2 O 0.32115(9) 0.2212(5) 0.5959(3) 0.0304(7) Uani 1 1 d . . . C1 C 0.46514(13) 0.2447(8) 0.3918(5) 0.0328(11) Uani 1 1 d . . . H1A H 0.4930 0.2069 0.4419 0.049 Uiso 1 1 calc R . . H1B H 0.4623 0.4149 0.3822 0.049 Uiso 1 1 calc R . . H1C H 0.4630 0.1727 0.2976 0.049 Uiso 1 1 calc R . . C2 C 0.42456(14) 0.3142(8) 0.6431(5) 0.0329(11) Uani 1 1 d . . . H2A H 0.3998 0.2781 0.6953 0.049 Uiso 1 1 calc R . . H2B H 0.4235 0.4793 0.6147 0.049 Uiso 1 1 calc R . . H2C H 0.4510 0.2844 0.7038 0.049 Uiso 1 1 calc R . . C3 C 0.37434(13) 0.2079(7) 0.3814(4) 0.0252(9) Uani 1 1 d . . . H3A H 0.3738 0.3795 0.3663 0.030 Uiso 1 1 calc R . . H3B H 0.3753 0.1331 0.2876 0.030 Uiso 1 1 calc R . . C4 C 0.28427(13) 0.2180(7) 0.3203(5) 0.0301(10) Uani 1 1 d . . . H4A H 0.2562 0.2032 0.3571 0.045 Uiso 1 1 calc R . . H4B H 0.2850 0.1206 0.2355 0.045 Uiso 1 1 calc R . . H4C H 0.2893 0.3819 0.2961 0.045 Uiso 1 1 calc R . . C5 C 0.32338(14) -0.1893(7) 0.4446(5) 0.0299(10) Uani 1 1 d . . . H5A H 0.3468 -0.2536 0.5087 0.045 Uiso 1 1 calc R . . H5B H 0.3266 -0.2412 0.3477 0.045 Uiso 1 1 calc R . . H5C H 0.2959 -0.2444 0.4735 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 P1 0.0246(6) 0.0252(6) 0.0233(7) 0.0024(4) 0.0012(5) 0.0011(5) P2 0.0250(6) 0.0268(6) 0.0227(7) -0.0019(5) 0.0048(5) 0.0000(5) O1 0.0301(17) 0.0257(15) 0.0367(19) 0.0058(14) -0.0025(13) 0.0039(13) O2 0.0330(17) 0.0373(17) 0.0219(17) -0.0054(13) 0.0077(13) -0.0016(13) C1 0.026(2) 0.042(3) 0.031(3) 0.004(2) 0.003(2) 0.000(2) C2 0.032(3) 0.041(3) 0.025(3) -0.001(2) -0.002(2) -0.003(2) C3 0.029(2) 0.025(2) 0.022(2) -0.0013(18) 0.0038(18) 0.0030(18) C4 0.022(2) 0.030(2) 0.039(3) -0.003(2) 0.004(2) 0.0003(18) C5 0.029(2) 0.032(2) 0.028(3) 0.0014(19) 0.005(2) -0.0041(18) _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 P1 O1 1.489(3) . ? P1 C2 1.781(4) . ? P1 C1 1.788(4) . ? P1 C3 1.819(4) . ? P2 O2 1.492(3) . ? P2 C4 1.786(4) . ? P2 C5 1.788(4) . ? P2 C3 1.805(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 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 P1 C2 113.5(2) . . ? O1 P1 C1 114.11(19) . . ? C2 P1 C1 105.0(2) . . ? O1 P1 C3 112.82(18) . . ? C2 P1 C3 106.3(2) . . ? C1 P1 C3 104.3(2) . . ? O2 P2 C4 114.46(19) . . ? O2 P2 C5 113.87(19) . . ? C4 P2 C5 105.0(2) . . ? O2 P2 C3 112.51(18) . . ? C4 P2 C3 104.1(2) . . ? C5 P2 C3 106.0(2) . . ? 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 . . ? P2 C3 P1 116.0(2) . . ? P2 C3 H3A 108.3 . . ? P1 C3 H3A 108.3 . . ? P2 C3 H3B 108.3 . . ? P1 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? 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 . . ? 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 O2 P2 C3 P1 56.2(3) . . . . ? C4 P2 C3 P1 -179.4(2) . . . . ? C5 P2 C3 P1 -68.9(3) . . . . ? O1 P1 C3 P2 56.5(3) . . . . ? C2 P1 C3 P2 -68.5(3) . . . . ? C1 P1 C3 P2 -179.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.387 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.095 #===END OF CIF ============================================================== # 08wz801 data_08wz801 _database_code_depnum_ccdc_archive 'CCDC 791403' #TrackingRef '- Si_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2008-09-02 _audit_author_name 'Webster, M.' _chemical_name_systematic ; Bis(trimethylhydroxoarsonium) hexafluoridosilicate(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C3 H10 As O 1+), F6 Si 2-' _chemical_formula_sum 'C6 H20 As2 F6 O2 Si' _chemical_formula_weight 416.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 tetragonal _symmetry_space_group_name_H-M 'P 43' _space_group_IT_number 78 # New _space_group_name_Hall 'P 4cw' # New loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 7.9450(5) _cell_length_b 7.9450(5) _cell_length_c 22.347(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1410.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1576 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 4.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8142 # 0.5696 _exptl_absorpt_correction_T_max 1.0000 # 0.8288 _exptl_absorpt_process_details 'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8762 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2712 _reflns_number_gt 2536 _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^+6.0330P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.307(19) _chemical_absolute_configuration ad _refine_ls_number_reflns 2712 _refine_ls_number_parameters 167 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 Si1 Si 0.5302(2) 0.0451(2) 0.33051(12) 0.0167(3) Uani 1 1 d . . . F1 F 0.4626(5) -0.1515(5) 0.3208(2) 0.0284(10) Uani 1 1 d . . . F2 F 0.3295(5) 0.1086(5) 0.3426(2) 0.0312(10) Uani 1 1 d . . . F3 F 0.5042(5) 0.0859(5) 0.2555(2) 0.0304(9) Uani 1 1 d . . . F4 F 0.7285(4) -0.0170(5) 0.3171(2) 0.0267(9) Uani 1 1 d . . . F5 F 0.5552(5) 0.0071(5) 0.40487(19) 0.0268(9) Uani 1 1 d . . . F6 F 0.5978(5) 0.2438(5) 0.3416(2) 0.0281(10) Uani 1 1 d . . . As1 As 0.52349(8) 0.54733(7) 0.41995(2) 0.01655(17) Uani 1 1 d . . . As2 As 1.03382(7) 0.02825(8) 0.24158(2) 0.01482(16) Uani 1 1 d . . . O1 O 0.4914(6) 0.7272(6) 0.4621(2) 0.0259(11) Uani 1 1 d D . . O2 O 1.2168(6) 0.0471(6) 0.1996(2) 0.0247(11) Uani 1 1 d D . . C1 C 0.5389(9) 0.3788(8) 0.4794(3) 0.0223(15) Uani 1 1 d . . . H1A H 0.6396 0.3981 0.5038 0.033 Uiso 1 1 calc R . . H1B H 0.5465 0.2681 0.4602 0.033 Uiso 1 1 calc R . . H1C H 0.4387 0.3828 0.5049 0.033 Uiso 1 1 calc R . . C2 C 0.3300(8) 0.5151(8) 0.3705(3) 0.0211(14) Uani 1 1 d . . . H2A H 0.2300 0.5581 0.3912 0.032 Uiso 1 1 calc R . . H2B H 0.3155 0.3948 0.3623 0.032 Uiso 1 1 calc R . . H2C H 0.3451 0.5758 0.3327 0.032 Uiso 1 1 calc R . . C3 C 0.7323(9) 0.5829(9) 0.3803(3) 0.0246(16) Uani 1 1 d . . . H3A H 0.7192 0.6720 0.3503 0.037 Uiso 1 1 calc R . . H3B H 0.7676 0.4786 0.3606 0.037 Uiso 1 1 calc R . . H3C H 0.8177 0.6165 0.4096 0.037 Uiso 1 1 calc R . . C4 C 0.8710(8) -0.0144(9) 0.1818(3) 0.0243(15) Uani 1 1 d . . . H4A H 0.8666 0.0810 0.1540 0.036 Uiso 1 1 calc R . . H4B H 0.7605 -0.0295 0.2005 0.036 Uiso 1 1 calc R . . H4C H 0.9015 -0.1167 0.1598 0.036 Uiso 1 1 calc R . . C5 C 1.0648(8) -0.1570(8) 0.2927(3) 0.0205(15) Uani 1 1 d . . . H5A H 1.0936 -0.2566 0.2689 0.031 Uiso 1 1 calc R . . H5B H 0.9607 -0.1783 0.3150 0.031 Uiso 1 1 calc R . . H5C H 1.1562 -0.1327 0.3208 0.031 Uiso 1 1 calc R . . C6 C 0.9925(8) 0.2408(8) 0.2769(3) 0.0203(14) Uani 1 1 d . . . H6A H 1.0911 0.2755 0.3001 0.031 Uiso 1 1 calc R . . H6B H 0.8944 0.2331 0.3033 0.031 Uiso 1 1 calc R . . H6C H 0.9705 0.3239 0.2454 0.031 Uiso 1 1 calc R . . H1 H 0.505(11) 0.802(9) 0.436(3) 0.050 Uiso 1 1 d D . . H2 H 1.293(9) 0.076(11) 0.223(3) 0.050 Uiso 1 1 d 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 Si1 0.0166(10) 0.0122(10) 0.0214(8) 0.0028(7) 0.0021(7) 0.0001(7) F1 0.0162(19) 0.0197(19) 0.049(3) -0.0033(18) -0.0031(18) -0.0010(14) F2 0.021(2) 0.022(2) 0.050(3) -0.0032(19) 0.0094(19) -0.0009(15) F3 0.023(2) 0.040(2) 0.028(3) 0.0047(19) -0.0039(17) 0.0003(17) F4 0.0127(18) 0.030(2) 0.037(3) -0.0034(18) -0.0018(17) 0.0038(14) F5 0.041(2) 0.023(2) 0.017(2) 0.0030(16) 0.0000(17) -0.0036(16) F6 0.033(2) 0.0156(19) 0.035(3) 0.0016(17) 0.0030(18) 0.0011(16) As1 0.0191(4) 0.0147(3) 0.0158(5) -0.0006(3) -0.0001(3) -0.0014(2) As2 0.0154(4) 0.0146(4) 0.0145(4) -0.0005(3) 0.0001(3) 0.0007(2) O1 0.037(3) 0.019(2) 0.021(3) -0.002(2) -0.002(2) -0.0046(19) O2 0.020(2) 0.040(3) 0.014(3) 0.002(2) 0.0035(19) -0.0040(19) C1 0.038(4) 0.019(3) 0.010(4) 0.004(2) 0.001(3) 0.005(3) C2 0.011(3) 0.025(4) 0.027(4) -0.002(3) -0.005(3) -0.002(2) C3 0.020(3) 0.035(4) 0.019(4) 0.000(3) -0.003(3) -0.002(3) C4 0.021(3) 0.033(4) 0.019(4) -0.003(3) 0.000(3) -0.001(3) C5 0.018(3) 0.012(3) 0.031(4) 0.003(3) 0.005(3) 0.000(2) C6 0.021(3) 0.015(3) 0.025(4) -0.004(3) 0.002(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 F1 1.666(4) . ? Si1 F4 1.678(4) . ? Si1 F6 1.686(4) . ? Si1 F2 1.694(4) . ? Si1 F5 1.701(5) . ? Si1 F3 1.720(5) . ? As1 O1 1.731(5) . ? As1 C1 1.890(6) . ? As1 C3 1.902(7) . ? As1 C2 1.910(6) . ? As2 O2 1.737(5) . ? As2 C5 1.879(7) . ? As2 C4 1.891(7) . ? As2 C6 1.893(6) . ? O1 H1 0.84(2) . ? O2 H2 0.84(2) . ? 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 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? 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 F1 Si1 F4 90.2(2) . . ? F1 Si1 F6 179.0(3) . . ? F4 Si1 F6 90.1(2) . . ? F1 Si1 F2 89.8(2) . . ? F4 Si1 F2 178.9(3) . . ? F6 Si1 F2 89.9(2) . . ? F1 Si1 F5 89.9(2) . . ? F4 Si1 F5 90.7(2) . . ? F6 Si1 F5 89.2(2) . . ? F2 Si1 F5 90.4(2) . . ? F1 Si1 F3 90.7(2) . . ? F4 Si1 F3 89.7(2) . . ? F6 Si1 F3 90.2(2) . . ? F2 Si1 F3 89.2(2) . . ? F5 Si1 F3 179.3(2) . . ? O1 As1 C1 102.2(3) . . ? O1 As1 C3 105.0(3) . . ? C1 As1 C3 112.1(3) . . ? O1 As1 C2 107.9(3) . . ? C1 As1 C2 111.3(3) . . ? C3 As1 C2 116.9(3) . . ? O2 As2 C5 106.6(3) . . ? O2 As2 C4 101.9(3) . . ? C5 As2 C4 112.3(3) . . ? O2 As2 C6 107.1(3) . . ? C5 As2 C6 117.9(3) . . ? C4 As2 C6 109.6(3) . . ? As1 O1 H1 101(7) . . ? As2 O2 H2 107(7) . . ? As1 C1 H1A 109.5 . . ? As1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? As1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? As1 C2 H2A 109.5 . . ? As1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? As1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? As1 C3 H3A 109.5 . . ? As1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? As1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? As2 C4 H4A 109.5 . . ? As2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? As2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? As2 C5 H5A 109.5 . . ? As2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? As2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? As2 C6 H6A 109.5 . . ? As2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? As2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? 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 O1 H1 F5 0.84(2) 1.82(4) 2.616(6) 159(10) 1_565 O2 H2 F3 0.84(2) 1.83(4) 2.621(6) 158(9) 1_655 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.773 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.121 #===END OF CIF ============================================================== # 10wz729a data_10wz729a _database_code_depnum_ccdc_archive 'CCDC 791404' #TrackingRef '- Si_all7_1.cif' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2010-08-05 _audit_author_name 'Webster, M.' _chemical_name_systematic ; cis-tetrafluorobis(pyridine 1-oxide)silicon(IV) ; # pyridine-N-oxide = C5H5NO # pyridine 1-oxide (chemspider systematic name) # Pyridine-N-oxide (chemspider synonym) _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 F4 N2 O2 Si' _chemical_formula_sum 'C10 H10 F4 N2 O2 Si' _chemical_formula_structural '(C5 H5 N O)2 (F4 Si)' _chemical_formula_weight 294.29 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7086(15) _cell_length_b 12.844(3) _cell_length_c 12.532(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.119(10) _cell_angle_gamma 90.00 _cell_volume 1197.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2775 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8612 # _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_% ? _diffrn_reflns_number 13512 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.69 _reflns_number_total 2737 _reflns_number_gt 1937 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _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^+3.8546P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2737 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Si1 Si 0.17307(12) 0.21331(7) 0.20575(8) 0.0163(2) Uani 1 1 d . . . F1 F 0.3903(2) 0.21450(15) 0.21114(15) 0.0189(4) Uani 1 1 d . . . F2 F 0.2010(3) 0.11814(15) 0.29836(16) 0.0240(5) Uani 1 1 d . . . F3 F 0.1218(3) 0.13161(15) 0.09968(15) 0.0224(5) Uani 1 1 d . . . F4 F -0.0404(2) 0.23142(15) 0.20248(15) 0.0197(4) Uani 1 1 d . . . O1 O 0.2085(3) 0.31213(18) 0.31815(18) 0.0193(5) Uani 1 1 d . . . O2 O 0.1634(3) 0.32346(18) 0.10579(18) 0.0174(5) Uani 1 1 d . . . N1 N 0.3760(4) 0.3456(2) 0.3694(2) 0.0183(6) Uani 1 1 d . . . N2 N -0.0022(4) 0.3500(2) 0.0426(2) 0.0153(6) Uani 1 1 d . . . C1 C 0.4439(5) 0.3216(3) 0.4765(3) 0.0216(7) Uani 1 1 d . . . H1 H 0.3777 0.2793 0.5140 0.026 Uiso 1 1 calc R . . C2 C 0.6113(5) 0.3592(3) 0.5314(3) 0.0257(8) Uani 1 1 d . . . H2 H 0.6608 0.3428 0.6072 0.031 Uiso 1 1 calc R . . C3 C 0.7064(5) 0.4203(3) 0.4764(3) 0.0282(9) Uani 1 1 d . . . H3 H 0.8220 0.4458 0.5136 0.034 Uiso 1 1 calc R . . C4 C 0.6320(5) 0.4443(3) 0.3663(3) 0.0277(8) Uani 1 1 d . . . H4 H 0.6952 0.4873 0.3274 0.033 Uiso 1 1 calc R . . C5 C 0.4659(5) 0.4054(3) 0.3140(3) 0.0238(8) Uani 1 1 d . . . H5 H 0.4142 0.4208 0.2382 0.029 Uiso 1 1 calc R . . C6 C -0.0626(4) 0.3047(3) -0.0567(3) 0.0174(7) Uani 1 1 d . . . H6 H 0.0090 0.2551 -0.0821 0.021 Uiso 1 1 calc R . . C7 C -0.2305(4) 0.3315(3) -0.1213(3) 0.0188(7) Uani 1 1 d . . . H7 H -0.2758 0.2996 -0.1915 0.023 Uiso 1 1 calc R . . C8 C -0.3330(5) 0.4043(3) -0.0846(3) 0.0202(7) Uani 1 1 d . . . H8 H -0.4498 0.4217 -0.1282 0.024 Uiso 1 1 calc R . . C9 C -0.2626(5) 0.4520(3) 0.0173(3) 0.0233(8) Uani 1 1 d . . . H9 H -0.3299 0.5038 0.0429 0.028 Uiso 1 1 calc R . . C10 C -0.0953(4) 0.4237(3) 0.0808(3) 0.0186(7) Uani 1 1 d . . . H10 H -0.0461 0.4556 0.1506 0.022 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 Si1 0.0147(4) 0.0190(4) 0.0140(4) 0.0011(4) 0.0018(3) -0.0009(4) F1 0.0135(9) 0.0235(10) 0.0180(10) 0.0009(8) 0.0012(7) 0.0031(8) F2 0.0241(11) 0.0226(11) 0.0234(11) 0.0086(8) 0.0027(8) 0.0017(8) F3 0.0236(11) 0.0221(10) 0.0183(10) -0.0043(8) -0.0001(8) 0.0003(8) F4 0.0147(10) 0.0263(11) 0.0173(10) 0.0020(8) 0.0028(8) -0.0013(8) O1 0.0123(11) 0.0258(13) 0.0187(11) -0.0041(10) 0.0020(9) -0.0032(9) O2 0.0133(11) 0.0224(12) 0.0151(11) 0.0031(9) 0.0014(9) 0.0011(9) N1 0.0161(14) 0.0211(15) 0.0166(14) -0.0011(12) 0.0023(11) -0.0024(12) N2 0.0146(13) 0.0169(14) 0.0141(13) 0.0036(11) 0.0035(11) 0.0010(11) C1 0.0258(19) 0.0245(18) 0.0151(16) -0.0012(14) 0.0067(14) 0.0041(15) C2 0.0229(19) 0.031(2) 0.0198(17) -0.0028(15) -0.0007(14) 0.0067(16) C3 0.0192(18) 0.028(2) 0.033(2) -0.0117(17) -0.0004(16) -0.0019(15) C4 0.027(2) 0.0209(18) 0.035(2) -0.0015(16) 0.0070(16) -0.0058(15) C5 0.031(2) 0.0204(18) 0.0189(17) 0.0008(14) 0.0038(15) -0.0049(15) C6 0.0181(16) 0.0185(17) 0.0166(16) 0.0010(13) 0.0065(13) 0.0013(13) C7 0.0186(17) 0.0201(17) 0.0163(16) 0.0009(13) 0.0019(13) -0.0005(13) C8 0.0161(16) 0.0230(18) 0.0207(17) 0.0061(14) 0.0034(13) 0.0016(14) C9 0.0207(18) 0.0255(19) 0.0234(18) -0.0010(15) 0.0055(14) 0.0022(15) C10 0.0182(17) 0.0186(17) 0.0187(16) -0.0039(13) 0.0041(13) -0.0033(13) _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 Si1 F4 1.651(2) . ? Si1 F1 1.658(2) . ? Si1 F3 1.658(2) . ? Si1 F2 1.660(2) . ? Si1 O1 1.863(2) . ? Si1 O2 1.878(2) . ? O1 N1 1.354(3) . ? O2 N2 1.359(3) . ? N1 C5 1.343(4) . ? N1 C1 1.343(4) . ? N2 C6 1.343(4) . ? N2 C10 1.349(4) . ? C1 C2 1.382(5) . ? C1 H1 0.9500 . ? C2 C3 1.376(6) . ? C2 H2 0.9500 . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.372(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.380(5) . ? C6 H6 0.9500 . ? C7 C8 1.378(5) . ? C7 H7 0.9500 . ? C8 C9 1.393(5) . ? C8 H8 0.9500 . ? C9 C10 1.376(5) . ? C9 H9 0.9500 . ? C10 H10 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 Si1 F1 171.33(11) . . ? F4 Si1 F3 92.39(11) . . ? F1 Si1 F3 93.75(11) . . ? F4 Si1 F2 93.89(11) . . ? F1 Si1 F2 91.87(11) . . ? F3 Si1 F2 93.14(11) . . ? F4 Si1 O1 82.61(10) . . ? F1 Si1 O1 90.90(10) . . ? F3 Si1 O1 174.08(11) . . ? F2 Si1 O1 90.36(11) . . ? F4 Si1 O2 90.66(10) . . ? F1 Si1 O2 83.34(10) . . ? F3 Si1 O2 88.99(11) . . ? F2 Si1 O2 174.89(11) . . ? O1 Si1 O2 87.91(11) . . ? N1 O1 Si1 120.57(19) . . ? N2 O2 Si1 116.46(18) . . ? C5 N1 C1 121.9(3) . . ? C5 N1 O1 119.6(3) . . ? C1 N1 O1 118.4(3) . . ? C6 N2 C10 123.1(3) . . ? C6 N2 O2 118.5(3) . . ? C10 N2 O2 118.4(3) . . ? N1 C1 C2 119.2(3) . . ? N1 C1 H1 120.4 . . ? C2 C1 H1 120.4 . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.4(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 120.3(3) . . ? N1 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? N2 C6 C7 118.8(3) . . ? N2 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C6 C7 C8 120.4(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 119.0(3) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 119.0(3) . . ? N2 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.377 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.088 #===END OF CIF ============================================================== # #===END OF FILE =============================================================