#------------------------------------------------------------------------------ #$Date: 2017-03-05 07:17:42 +0200 (Sun, 05 Mar 2017) $ #$Revision: 193833 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/20/7042059.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7042059 loop_ _publ_author_name 'Kyri, A. W.' 'Brehm, P.' 'Schnakenburg, G.' 'Streubel, R.' _publ_section_title ; Ring opening of a sterically crowded 1,2-oxaphosphetane complex. ; _journal_issue 9 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 2904 _journal_page_last 2909 _journal_paper_doi 10.1039/c7dt00136c _journal_volume 46 _journal_year 2017 _chemical_formula_moiety 'C30 H23 F6 Ge O7 P W' _chemical_formula_sum 'C30 H23 F6 Ge O7 P W' _chemical_formula_weight 896.89 _chemical_name_systematic PB-47 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2016-09-02 _audit_creation_method ; Olex2 1.2 (compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221) ; _audit_update_record ; 2017-01-10 deposited with the CCDC. 2017-02-03 downloaded from the CCDC. ; _cell_angle_alpha 92.8970(10) _cell_angle_beta 97.6730(10) _cell_angle_gamma 90.1710(10) _cell_formula_units_Z 2 _cell_length_a 9.0079(2) _cell_length_b 13.1369(3) _cell_length_c 13.2698(2) _cell_measurement_reflns_used 8272 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 29.13 _cell_measurement_theta_min 1.00 _cell_volume 1554.17(5) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'fine slicing \w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_unetI/netI 0.0401 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 36507 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 27.998 _diffrn_reflns_theta_min 2.926 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 4.798 _exptl_absorpt_correction_T_max 0.7795 _exptl_absorpt_correction_T_min 0.3452 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.917 _exptl_crystal_description plate _exptl_crystal_F_000 868 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.240 _refine_diff_density_min -1.625 _refine_diff_density_rms 0.125 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 417 _refine_ls_number_reflns 7498 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0263 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+1.2297P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.0628 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6878 _reflns_number_total 7498 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 4813.res created by SHELXL-2014/7 TITL 4813_a.res in P-1 REM Old TITL REM SHELXT solution in P-1 REM R1 0.169, Rweak 0.017, Alpha 0.059, Orientation as input REM Formula found by SHELXT: C31 O13 I2 CELL 0.71073 9.0079 13.1369 13.2698 92.897 97.673 90.171 ZERR 2 0.0002 0.0003 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H F Ge O P W UNIT 60 46 12 2 14 2 2 L.S. 50 PLAN 20 TEMP -150(2) BOND $H list 4 MORE -1 CONF fmap 2 acta 52 OMIT -2 56 OMIT 0 -1 1 OMIT 0 1 1 OMIT -1 0 1 OMIT 1 0 0 OMIT -1 -1 1 OMIT 1 1 0 OMIT -1 1 0 REM REM REM WGHT 0.026200 1.229700 FVAR 0.24830 W 7 0.727732 0.324244 0.452999 11.00000 0.01793 0.01971 = 0.01644 0.00161 0.00305 0.00179 GE 4 0.956031 0.108213 0.263253 11.00000 0.01971 0.01875 = 0.03868 0.00026 0.00561 0.00447 P 6 0.708926 0.262614 0.266848 11.00000 0.01423 0.01520 = 0.01793 0.00069 0.00362 0.00112 F1 3 0.484369 -0.032371 0.113176 11.00000 0.03869 0.04554 = 0.04548 -0.01070 -0.00344 -0.01432 F2 3 0.706918 0.008231 0.088347 11.00000 0.04579 0.02921 = 0.03022 -0.00217 0.01237 0.00145 F3 3 0.671549 -0.123083 0.171536 11.00000 0.08596 0.01597 = 0.04440 -0.00265 0.00906 0.00577 F4 3 0.417808 -0.017326 0.302178 11.00000 0.03118 0.04689 = 0.05901 0.01506 0.01251 -0.01200 F5 3 0.614425 -0.098564 0.360409 11.00000 0.05798 0.02569 = 0.05047 0.01712 0.01758 0.00274 F6 3 0.576655 0.051617 0.421058 11.00000 0.06259 0.03481 = 0.03203 0.00242 0.02040 -0.00711 O1 5 0.866420 0.227162 0.231936 11.00000 0.01564 0.01820 = 0.02585 0.00133 0.00524 0.00350 O2 5 0.800217 0.036850 0.297193 11.00000 0.02430 0.01907 = 0.03271 0.00534 0.00200 0.00212 O3 5 0.734835 0.411255 0.678666 11.00000 0.03438 0.05991 = 0.02129 -0.00214 0.00083 0.01020 O4 5 0.397304 0.242843 0.462673 11.00000 0.02982 0.04132 = 0.04405 -0.00295 0.01197 -0.01049 O5 5 0.854142 0.124925 0.557128 11.00000 0.06787 0.04174 = 0.05343 0.02039 0.00323 0.01763 O6 5 1.062101 0.398118 0.442464 11.00000 0.02206 0.03917 = 0.03116 -0.00398 0.00408 -0.00117 O7 5 0.607072 0.549976 0.430785 11.00000 0.03283 0.02646 = 0.02535 0.00412 0.01075 0.00900 C1 1 0.648855 0.040753 0.256242 11.00000 0.02368 0.01457 = 0.02560 0.00142 0.00461 0.00007 C2 1 0.584205 0.148213 0.232037 11.00000 0.01767 0.01769 = 0.02294 0.00138 0.00375 -0.00056 AFIX 23 H2A 2 0.494362 0.157581 0.266977 11.00000 -1.20000 H2B 2 0.550027 0.147848 0.157947 11.00000 -1.20000 AFIX 0 C3 1 0.626293 -0.028296 0.157216 11.00000 0.03793 0.01794 = 0.03744 0.00220 0.00560 -0.00128 C4 1 0.564501 -0.007219 0.336038 11.00000 0.03599 0.02311 = 0.03773 0.00649 0.01009 -0.00305 C5 1 1.030341 0.052331 0.142891 11.00000 0.03795 0.03355 = 0.06423 -0.00769 0.02660 0.00572 AFIX 137 H5A 2 0.978631 0.084016 0.082859 11.00000 -1.50000 H5B 2 1.012028 -0.021432 0.136500 11.00000 -1.50000 H5C 2 1.138182 0.065969 0.148059 11.00000 -1.50000 AFIX 0 C6 1 1.097948 0.120069 0.383979 11.00000 0.02581 0.03088 = 0.05538 0.00187 -0.00843 0.00729 AFIX 137 H6A 2 1.199635 0.115156 0.365671 11.00000 -1.50000 H6B 2 1.080821 0.065076 0.428432 11.00000 -1.50000 H6C 2 1.086169 0.186057 0.419746 11.00000 -1.50000 AFIX 0 C7 1 0.637029 0.354721 0.159698 11.00000 0.01481 0.01811 = 0.01653 0.00094 0.00245 0.00086 C8 1 0.712515 0.332736 0.062861 11.00000 0.01319 0.02238 = 0.01819 0.00201 0.00219 0.00179 C9 1 0.717017 0.235183 0.016945 11.00000 0.02542 0.02269 = 0.02307 0.00147 0.00991 -0.00095 AFIX 43 H9 2 0.674504 0.179814 0.046941 11.00000 -1.20000 AFIX 0 C10 1 0.781766 0.216595 -0.071273 11.00000 0.03000 0.02672 = 0.02532 -0.00599 0.00922 0.00367 AFIX 43 H10 2 0.783158 0.149141 -0.100507 11.00000 -1.20000 AFIX 0 C11 1 0.844040 0.295241 -0.116770 11.00000 0.02428 0.03608 = 0.02030 0.00373 0.00929 0.00574 AFIX 43 H11 2 0.890070 0.282262 -0.176444 11.00000 -1.20000 AFIX 0 C12 1 0.838739 0.393075 -0.074609 11.00000 0.02469 0.03286 = 0.02274 0.00797 0.00716 0.00009 AFIX 43 H12 2 0.879537 0.448011 -0.106255 11.00000 -1.20000 AFIX 0 C13 1 0.773814 0.411952 0.014283 11.00000 0.02150 0.02092 = 0.02015 0.00155 0.00329 -0.00013 AFIX 43 H13 2 0.771166 0.479796 0.042343 11.00000 -1.20000 AFIX 0 C14 1 0.465706 0.338824 0.139399 11.00000 0.01450 0.01541 = 0.01952 0.00251 0.00308 0.00193 C15 1 0.390170 0.309362 0.043346 11.00000 0.01917 0.02586 = 0.02037 0.00078 0.00459 0.00072 AFIX 43 H15 2 0.445155 0.298640 -0.012513 11.00000 -1.20000 AFIX 0 C16 1 0.235348 0.295544 0.028552 11.00000 0.02006 0.03616 = 0.02395 -0.00169 -0.00098 -0.00239 AFIX 43 H16 2 0.185640 0.276048 -0.037328 11.00000 -1.20000 AFIX 0 C17 1 0.153567 0.309943 0.108815 11.00000 0.01509 0.02919 = 0.03170 0.00403 0.00281 -0.00072 AFIX 43 H17 2 0.048086 0.299638 0.098479 11.00000 -1.20000 AFIX 0 C18 1 0.226090 0.339514 0.204587 11.00000 0.01822 0.02668 = 0.02633 0.00528 0.00767 0.00371 AFIX 43 H18 2 0.170470 0.349383 0.260229 11.00000 -1.20000 AFIX 0 C19 1 0.379954 0.354666 0.219040 11.00000 0.01857 0.01907 = 0.02143 0.00279 0.00308 0.00201 AFIX 43 H19 2 0.428317 0.376350 0.284681 11.00000 -1.20000 AFIX 0 C20 1 0.677290 0.463969 0.200284 11.00000 0.01732 0.01882 = 0.01514 0.00115 0.00578 -0.00093 C21 1 0.574802 0.543193 0.190799 11.00000 0.02102 0.01866 = 0.01891 0.00303 0.00441 -0.00026 AFIX 43 H21 2 0.474259 0.529335 0.161485 11.00000 -1.20000 AFIX 0 C22 1 0.618166 0.642775 0.223895 11.00000 0.03236 0.01876 = 0.02242 0.00396 0.00613 0.00560 AFIX 43 H22 2 0.547083 0.696101 0.217120 11.00000 -1.20000 AFIX 0 C23 1 0.764382 0.664036 0.266539 11.00000 0.03445 0.01796 = 0.02478 0.00139 0.00441 -0.00480 AFIX 43 H23 2 0.793399 0.731638 0.289942 11.00000 -1.20000 AFIX 0 C24 1 0.868344 0.586244 0.274959 11.00000 0.02296 0.02552 = 0.02457 0.00129 0.00228 -0.00580 AFIX 43 H24 2 0.968959 0.600669 0.303749 11.00000 -1.20000 AFIX 0 C25 1 0.825746 0.487487 0.241454 11.00000 0.01817 0.02287 = 0.01886 0.00191 0.00464 0.00078 AFIX 43 H25 2 0.898184 0.434937 0.246448 11.00000 -1.20000 AFIX 0 C26 1 0.734666 0.377335 0.597370 11.00000 0.02057 0.03145 = 0.02021 0.00115 0.00210 0.00494 C27 1 0.515563 0.271963 0.458316 11.00000 0.02907 0.02599 = 0.01978 -0.00388 0.00577 -0.00178 C28 1 0.807877 0.192644 0.512664 11.00000 0.03674 0.02623 = 0.03250 0.00788 0.00581 0.00597 C29 1 0.941090 0.372474 0.446070 11.00000 0.02110 0.02896 = 0.01656 -0.00545 0.00129 0.00117 C30 1 0.650192 0.468600 0.429067 11.00000 0.01677 0.02441 = 0.01661 0.00167 0.00505 0.00021 HKLF 4 REM 4813_a.res in P-1 REM R1 = 0.0263 for 6878 Fo > 4sig(Fo) and 0.0304 for all 7498 data REM 417 parameters refined using 0 restraints END WGHT 0.0262 1.2297 REM Highest difference peak 1.240, deepest hole -1.625, 1-sigma level 0.125 Q1 1 0.6954 0.2639 0.4567 11.00000 0.05 1.24 Q2 1 0.7578 0.3837 0.4410 11.00000 0.05 1.18 Q3 1 0.7792 0.2601 0.5135 11.00000 0.05 0.82 Q4 1 1.1832 -0.0256 0.3577 11.00000 0.05 0.81 Q5 1 0.6811 0.3995 0.4809 11.00000 0.05 0.75 Q6 1 0.4120 0.7584 0.1707 11.00000 0.05 0.63 Q7 1 0.7790 0.2595 0.4016 11.00000 0.05 0.63 Q8 1 0.4947 0.4560 0.3590 11.00000 0.05 0.61 Q9 1 0.6762 0.3998 0.3957 11.00000 0.05 0.56 Q10 1 0.7959 0.4596 0.4720 11.00000 0.05 0.54 Q11 1 0.7781 0.4393 0.3981 11.00000 0.05 0.54 Q12 1 0.8651 0.4090 0.4206 11.00000 0.05 0.54 Q13 1 0.8830 0.2517 0.4839 11.00000 0.05 0.53 Q14 1 1.1517 0.1940 0.3646 11.00000 0.05 0.50 Q15 1 0.5666 0.3985 0.4288 11.00000 0.05 0.49 Q16 1 0.8486 0.5374 0.2583 11.00000 0.05 0.47 Q17 1 0.8681 0.4999 0.4410 11.00000 0.05 0.47 Q18 1 0.9829 0.1753 0.2367 11.00000 0.05 0.47 Q19 1 1.1686 0.0582 0.3884 11.00000 0.05 0.46 Q20 1 0.6561 0.1985 0.2655 11.00000 0.05 0.45 REM The information below was added by Olex2. REM REM R1 = 0.0263 for 6878 Fo > 4sig(Fo) and 0.0304 for all 38662 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.24, deepest hole -1.63 REM Mean Shift 0, Max Shift 0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0304 REM R1_gt = 0.0263 REM wR_ref = 0.0628 REM GOOF = 1.059 REM Shift_max = 0.002 REM Shift_mean = 0 REM Reflections_all = 38662 REM Reflections_gt = 6878 REM Parameters = n/a REM Hole = -1.63 REM Peak = 1.24 REM Flack = n/a ; _cod_data_source_file c7dt00136c1.cif _cod_data_source_block 4813 _cod_depositor_comments 'Adding full bibliography for 7042059--7042062.cif.' _cod_database_code 7042059 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B) 2.b Aromatic/amide H refined with riding coordinates: C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25) 2.c Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C6(H6A,H6B,H6C) ; _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn W W 0.72773(2) 0.32424(2) 0.45300(2) 0.01793(4) Uani 1 1 d . Ge Ge 0.95603(4) 0.10821(3) 0.26325(3) 0.02559(8) Uani 1 1 d . P P 0.70893(8) 0.26261(6) 0.26685(5) 0.01565(14) Uani 1 1 d . F1 F 0.4844(2) -0.03237(18) 0.11318(17) 0.0445(5) Uani 1 1 d . F2 F 0.7069(2) 0.00823(15) 0.08835(15) 0.0345(5) Uani 1 1 d . F3 F 0.6715(3) -0.12308(15) 0.17154(17) 0.0489(6) Uani 1 1 d . F4 F 0.4178(2) -0.01733(18) 0.30218(18) 0.0447(5) Uani 1 1 d . F5 F 0.6144(3) -0.09856(16) 0.36041(17) 0.0433(5) Uani 1 1 d . F6 F 0.5767(3) 0.05162(16) 0.42106(15) 0.0419(5) Uani 1 1 d . O1 O 0.8664(2) 0.22716(16) 0.23194(15) 0.0197(4) Uani 1 1 d . O2 O 0.8002(2) 0.03685(16) 0.29719(17) 0.0254(5) Uani 1 1 d . O3 O 0.7348(3) 0.4113(2) 0.67867(17) 0.0389(6) Uani 1 1 d . O4 O 0.3973(3) 0.2428(2) 0.4627(2) 0.0380(6) Uani 1 1 d . O5 O 0.8541(4) 0.1249(2) 0.5571(2) 0.0541(8) Uani 1 1 d . O6 O 1.0621(2) 0.3981(2) 0.44246(18) 0.0310(5) Uani 1 1 d . O7 O 0.6071(3) 0.54998(18) 0.43078(16) 0.0275(5) Uani 1 1 d . C1 C 0.6489(3) 0.0408(2) 0.2562(2) 0.0212(6) Uani 1 1 d . C2 C 0.5842(3) 0.1482(2) 0.2320(2) 0.0193(6) Uani 1 1 d . H2A H 0.4944 0.1576 0.2670 0.023 Uiso 1 1 calc R H2B H 0.5500 0.1478 0.1579 0.023 Uiso 1 1 calc R C3 C 0.6263(4) -0.0283(3) 0.1572(3) 0.0310(7) Uani 1 1 d . C4 C 0.5645(4) -0.0072(3) 0.3360(3) 0.0316(7) Uani 1 1 d . C5 C 1.0303(4) 0.0523(3) 0.1429(3) 0.0438(10) Uani 1 1 d . H5A H 0.9786 0.0840 0.0829 0.066 Uiso 1 1 calc GR H5B H 1.0120 -0.0214 0.1365 0.066 Uiso 1 1 calc GR H5C H 1.1382 0.0660 0.1481 0.066 Uiso 1 1 calc GR C6 C 1.0979(4) 0.1201(3) 0.3840(3) 0.0386(9) Uani 1 1 d . H6A H 1.1996 0.1152 0.3657 0.058 Uiso 1 1 calc GR H6B H 1.0808 0.0651 0.4284 0.058 Uiso 1 1 calc GR H6C H 1.0862 0.1861 0.4197 0.058 Uiso 1 1 calc GR C7 C 0.6370(3) 0.3547(2) 0.1597(2) 0.0164(5) Uani 1 1 d . C8 C 0.7125(3) 0.3327(2) 0.0629(2) 0.0179(6) Uani 1 1 d . C9 C 0.7170(3) 0.2352(2) 0.0169(2) 0.0231(6) Uani 1 1 d . H9 H 0.6745 0.1798 0.0469 0.028 Uiso 1 1 calc R C10 C 0.7818(4) 0.2166(3) -0.0713(2) 0.0271(7) Uani 1 1 d . H10 H 0.7832 0.1491 -0.1005 0.033 Uiso 1 1 calc R C11 C 0.8440(3) 0.2952(3) -0.1168(2) 0.0262(7) Uani 1 1 d . H11 H 0.8901 0.2823 -0.1764 0.031 Uiso 1 1 calc R C12 C 0.8387(3) 0.3931(3) -0.0746(2) 0.0262(7) Uani 1 1 d . H12 H 0.8795 0.4480 -0.1063 0.031 Uiso 1 1 calc R C13 C 0.7738(3) 0.4120(2) 0.0143(2) 0.0208(6) Uani 1 1 d . H13 H 0.7712 0.4798 0.0423 0.025 Uiso 1 1 calc R C14 C 0.4657(3) 0.3388(2) 0.1394(2) 0.0163(5) Uani 1 1 d . C15 C 0.3902(3) 0.3094(2) 0.0433(2) 0.0216(6) Uani 1 1 d . H15 H 0.4452 0.2986 -0.0125 0.026 Uiso 1 1 calc R C16 C 0.2353(3) 0.2955(3) 0.0286(2) 0.0272(7) Uani 1 1 d . H16 H 0.1856 0.2760 -0.0373 0.033 Uiso 1 1 calc R C17 C 0.1536(3) 0.3099(3) 0.1088(2) 0.0253(6) Uani 1 1 d . H17 H 0.0481 0.2996 0.0985 0.030 Uiso 1 1 calc R C18 C 0.2261(3) 0.3395(2) 0.2046(2) 0.0232(6) Uani 1 1 d . H18 H 0.1705 0.3494 0.2602 0.028 Uiso 1 1 calc R C19 C 0.3800(3) 0.3547(2) 0.2190(2) 0.0196(6) Uani 1 1 d . H19 H 0.4283 0.3763 0.2847 0.024 Uiso 1 1 calc R C20 C 0.6773(3) 0.4640(2) 0.2003(2) 0.0168(5) Uani 1 1 d . C21 C 0.5748(3) 0.5432(2) 0.1908(2) 0.0193(6) Uani 1 1 d . H21 H 0.4743 0.5293 0.1615 0.023 Uiso 1 1 calc R C22 C 0.6182(4) 0.6428(2) 0.2239(2) 0.0242(6) Uani 1 1 d . H22 H 0.5471 0.6961 0.2171 0.029 Uiso 1 1 calc R C23 C 0.7644(4) 0.6640(2) 0.2665(2) 0.0257(6) Uani 1 1 d . H23 H 0.7934 0.7316 0.2899 0.031 Uiso 1 1 calc R C24 C 0.8683(3) 0.5862(2) 0.2750(2) 0.0244(6) Uani 1 1 d . H24 H 0.9690 0.6007 0.3037 0.029 Uiso 1 1 calc R C25 C 0.8257(3) 0.4875(2) 0.2415(2) 0.0197(6) Uani 1 1 d . H25 H 0.8982 0.4349 0.2464 0.024 Uiso 1 1 calc R C26 C 0.7347(3) 0.3773(3) 0.5974(2) 0.0241(6) Uani 1 1 d . C27 C 0.5156(4) 0.2720(3) 0.4583(2) 0.0249(6) Uani 1 1 d . C28 C 0.8079(4) 0.1926(3) 0.5127(3) 0.0315(7) Uani 1 1 d . C29 C 0.9411(3) 0.3725(3) 0.4461(2) 0.0225(6) Uani 1 1 d . C30 C 0.6502(3) 0.4686(2) 0.4291(2) 0.0190(6) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.01793(7) 0.01971(7) 0.01644(6) 0.00161(4) 0.00305(4) 0.00179(5) Ge 0.01971(16) 0.01875(17) 0.03868(19) 0.00026(14) 0.00561(13) 0.00447(13) P 0.0142(3) 0.0152(4) 0.0179(3) 0.0007(3) 0.0036(3) 0.0011(3) F1 0.0387(12) 0.0455(14) 0.0455(12) -0.0107(10) -0.0034(10) -0.0143(10) F2 0.0458(12) 0.0292(11) 0.0302(10) -0.0022(8) 0.0124(9) 0.0014(9) F3 0.0860(18) 0.0160(10) 0.0444(13) -0.0026(9) 0.0091(12) 0.0058(11) F4 0.0312(11) 0.0469(14) 0.0590(14) 0.0151(11) 0.0125(10) -0.0120(10) F5 0.0580(14) 0.0257(11) 0.0505(13) 0.0171(10) 0.0176(11) 0.0027(10) F6 0.0626(14) 0.0348(12) 0.0320(11) 0.0024(9) 0.0204(10) -0.0071(11) O1 0.0156(9) 0.0182(11) 0.0258(10) 0.0013(8) 0.0052(8) 0.0035(8) O2 0.0243(11) 0.0191(11) 0.0327(12) 0.0053(9) 0.0020(9) 0.0021(9) O3 0.0344(13) 0.0599(18) 0.0213(12) -0.0021(11) 0.0008(10) 0.0102(12) O4 0.0298(13) 0.0413(16) 0.0441(15) -0.0029(12) 0.0120(11) -0.0105(11) O5 0.068(2) 0.0417(17) 0.0534(17) 0.0204(14) 0.0032(15) 0.0176(15) O6 0.0221(11) 0.0392(14) 0.0312(12) -0.0040(10) 0.0041(9) -0.0012(10) O7 0.0328(12) 0.0265(13) 0.0253(11) 0.0041(9) 0.0107(9) 0.0090(10) C1 0.0237(15) 0.0146(14) 0.0256(15) 0.0014(11) 0.0046(12) 0.0001(12) C2 0.0177(13) 0.0177(14) 0.0229(14) 0.0014(11) 0.0038(11) -0.0006(11) C3 0.0379(19) 0.0179(16) 0.0374(18) 0.0022(14) 0.0056(15) -0.0013(14) C4 0.0360(18) 0.0231(17) 0.0377(18) 0.0065(14) 0.0101(15) -0.0030(14) C5 0.038(2) 0.034(2) 0.064(3) -0.0077(18) 0.0266(19) 0.0057(17) C6 0.0258(17) 0.031(2) 0.055(2) 0.0019(17) -0.0084(16) 0.0073(15) C7 0.0148(12) 0.0181(14) 0.0165(12) 0.0009(10) 0.0024(10) 0.0009(11) C8 0.0132(12) 0.0224(15) 0.0182(13) 0.0020(11) 0.0022(10) 0.0018(11) C9 0.0254(15) 0.0227(16) 0.0231(14) 0.0015(12) 0.0099(12) -0.0010(12) C10 0.0300(16) 0.0267(17) 0.0253(15) -0.0060(13) 0.0092(13) 0.0037(13) C11 0.0243(15) 0.0361(19) 0.0203(14) 0.0037(13) 0.0093(12) 0.0057(13) C12 0.0247(15) 0.0329(18) 0.0227(15) 0.0080(13) 0.0072(12) 0.0001(13) C13 0.0215(14) 0.0209(15) 0.0202(14) 0.0015(11) 0.0033(11) -0.0001(12) C14 0.0145(12) 0.0154(14) 0.0195(13) 0.0025(10) 0.0031(10) 0.0019(10) C15 0.0192(14) 0.0259(16) 0.0204(14) 0.0008(12) 0.0046(11) 0.0007(12) C16 0.0201(15) 0.0362(19) 0.0239(15) -0.0017(13) -0.0010(12) -0.0024(13) C17 0.0151(14) 0.0292(17) 0.0317(16) 0.0040(13) 0.0028(12) -0.0007(12) C18 0.0182(14) 0.0267(17) 0.0263(15) 0.0053(12) 0.0077(11) 0.0037(12) C19 0.0186(14) 0.0191(15) 0.0214(14) 0.0028(11) 0.0031(11) 0.0020(11) C20 0.0173(13) 0.0188(14) 0.0151(12) 0.0011(10) 0.0058(10) -0.0009(11) C21 0.0210(14) 0.0187(15) 0.0189(13) 0.0030(11) 0.0044(11) -0.0003(11) C22 0.0324(17) 0.0188(15) 0.0224(14) 0.0040(12) 0.0061(12) 0.0056(13) C23 0.0344(17) 0.0180(15) 0.0248(15) 0.0014(12) 0.0044(13) -0.0048(13) C24 0.0230(15) 0.0255(17) 0.0246(15) 0.0013(12) 0.0023(12) -0.0058(13) C25 0.0182(13) 0.0229(15) 0.0189(13) 0.0019(11) 0.0046(11) 0.0008(11) C26 0.0206(14) 0.0314(18) 0.0202(15) 0.0011(12) 0.0021(11) 0.0049(13) C27 0.0291(16) 0.0260(17) 0.0198(14) -0.0039(12) 0.0058(12) -0.0018(13) C28 0.0367(18) 0.0262(18) 0.0325(17) 0.0079(14) 0.0058(14) 0.0060(15) C29 0.0211(15) 0.0290(17) 0.0166(13) -0.0055(12) 0.0013(11) 0.0012(12) C30 0.0168(13) 0.0244(16) 0.0166(13) 0.0017(11) 0.0050(10) 0.0002(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C26 W P 177.27(9) C26 W C27 88.69(12) C26 W C28 85.72(14) C26 W C29 92.35(12) C26 W C30 80.43(12) C27 W P 90.12(8) C27 W C30 91.00(12) C28 W P 96.72(10) C28 W C27 88.84(14) C28 W C29 90.00(14) C28 W C30 166.15(13) C29 W P 88.89(8) C29 W C27 178.38(12) C29 W C30 90.40(12) C30 W P 97.13(8) O1 Ge O2 100.62(9) O1 Ge C5 107.66(15) O1 Ge C6 112.88(13) O2 Ge C5 113.23(14) O2 Ge C6 105.46(14) C6 Ge C5 116.01(18) O1 P W 113.93(8) O1 P C2 103.45(12) O1 P C7 101.05(11) C2 P W 114.23(9) C2 P C7 102.04(12) C7 P W 119.96(9) P O1 Ge 124.16(12) C1 O2 Ge 128.42(18) O2 C1 C2 116.8(2) O2 C1 C3 107.9(2) O2 C1 C4 104.6(2) C3 C1 C2 108.6(3) C4 C1 C2 110.0(2) C4 C1 C3 108.7(3) P C2 H2A 107.7 P C2 H2B 107.7 C1 C2 P 118.4(2) C1 C2 H2A 107.7 C1 C2 H2B 107.7 H2A C2 H2B 107.1 F1 C3 F2 106.4(3) F1 C3 C1 112.9(3) F2 C3 C1 110.0(3) F3 C3 F1 107.9(3) F3 C3 F2 106.4(3) F3 C3 C1 112.9(3) F4 C4 C1 111.1(3) F5 C4 F4 107.2(3) F5 C4 F6 107.6(3) F5 C4 C1 113.1(3) F6 C4 F4 107.0(3) F6 C4 C1 110.6(3) Ge C5 H5A 109.5 Ge C5 H5B 109.5 Ge C5 H5C 109.5 H5A C5 H5B 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 Ge C6 H6A 109.5 Ge C6 H6B 109.5 Ge C6 H6C 109.5 H6A C6 H6B 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C8 C7 P 111.48(19) C14 C7 P 105.75(18) C14 C7 C8 112.2(2) C20 C7 P 107.91(18) C20 C7 C8 108.4(2) C20 C7 C14 111.0(2) C9 C8 C7 122.3(3) C9 C8 C13 116.7(3) C13 C8 C7 120.9(3) C8 C9 H9 119.0 C10 C9 C8 121.9(3) C10 C9 H9 119.0 C9 C10 H10 119.8 C11 C10 C9 120.5(3) C11 C10 H10 119.8 C10 C11 H11 120.4 C10 C11 C12 119.2(3) C12 C11 H11 120.4 C11 C12 H12 119.8 C11 C12 C13 120.5(3) C13 C12 H12 119.8 C8 C13 H13 119.4 C12 C13 C8 121.3(3) C12 C13 H13 119.4 C15 C14 C7 122.7(2) C19 C14 C7 119.7(2) C19 C14 C15 117.6(3) C14 C15 H15 119.6 C16 C15 C14 120.8(3) C16 C15 H15 119.6 C15 C16 H16 119.7 C17 C16 C15 120.5(3) C17 C16 H16 119.7 C16 C17 H17 120.2 C16 C17 C18 119.6(3) C18 C17 H17 120.2 C17 C18 H18 120.1 C17 C18 C19 119.9(3) C19 C18 H18 120.1 C14 C19 H19 119.2 C18 C19 C14 121.6(3) C18 C19 H19 119.2 C21 C20 C7 122.5(2) C21 C20 C25 118.2(3) C25 C20 C7 119.1(2) C20 C21 H21 119.6 C20 C21 C22 120.7(3) C22 C21 H21 119.6 C21 C22 H22 119.9 C23 C22 C21 120.2(3) C23 C22 H22 119.9 C22 C23 H23 120.1 C22 C23 C24 119.7(3) C24 C23 H23 120.1 C23 C24 H24 119.9 C25 C24 C23 120.1(3) C25 C24 H24 119.9 C20 C25 H25 119.5 C24 C25 C20 121.0(3) C24 C25 H25 119.5 O3 C26 W 177.0(3) O4 C27 W 179.1(3) O5 C28 W 171.9(3) O6 C29 W 178.9(3) O7 C30 W 170.0(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance W P 2.5439(7) W C26 1.998(3) W C27 2.040(3) W C28 2.032(3) W C29 2.037(3) W C30 2.048(3) Ge O1 1.803(2) Ge O2 1.804(2) Ge C5 1.926(4) Ge C6 1.911(4) P O1 1.613(2) P C2 1.875(3) P C7 1.959(3) F1 C3 1.333(4) F2 C3 1.346(4) F3 C3 1.326(4) F4 C4 1.342(4) F5 C4 1.323(4) F6 C4 1.327(4) O2 C1 1.401(4) O3 C26 1.146(4) O4 C27 1.140(4) O5 C28 1.141(4) O6 C29 1.148(4) O7 C30 1.139(4) C1 C2 1.561(4) C1 C3 1.549(4) C1 C4 1.541(4) C2 H2A 0.9900 C2 H2B 0.9900 C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 C8 1.547(4) C7 C14 1.542(4) C7 C20 1.532(4) C8 C9 1.394(4) C8 C13 1.401(4) C9 H9 0.9500 C9 C10 1.387(4) C10 H10 0.9500 C10 C11 1.377(5) C11 H11 0.9500 C11 C12 1.379(5) C12 H12 0.9500 C12 C13 1.397(4) C13 H13 0.9500 C14 C15 1.398(4) C14 C19 1.398(4) C15 H15 0.9500 C15 C16 1.392(4) C16 H16 0.9500 C16 C17 1.379(4) C17 H17 0.9500 C17 C18 1.386(4) C18 H18 0.9500 C18 C19 1.386(4) C19 H19 0.9500 C20 C21 1.393(4) C20 C25 1.403(4) C21 H21 0.9500 C21 C22 1.396(4) C22 H22 0.9500 C22 C23 1.384(5) C23 H23 0.9500 C23 C24 1.387(5) C24 H24 0.9500 C24 C25 1.386(4) C25 H25 0.9500 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 W P O1 Ge 75.92(14) W P C2 C1 -81.2(2) Ge O2 C1 C2 -40.0(3) Ge O2 C1 C3 82.6(3) Ge O2 C1 C4 -161.8(2) P C7 C8 C9 51.1(3) P C7 C8 C13 -132.0(2) P C7 C14 C15 -122.6(3) P C7 C14 C19 57.8(3) P C7 C20 C21 -132.8(2) P C7 C20 C25 52.4(3) O1 Ge O2 C1 34.0(3) O1 P C2 C1 43.2(2) O2 Ge O1 P 18.41(16) O2 C1 C2 P -3.8(3) O2 C1 C3 F1 178.3(2) O2 C1 C3 F2 -63.1(3) O2 C1 C3 F3 55.6(3) O2 C1 C4 F4 -174.2(3) O2 C1 C4 F5 -53.6(4) O2 C1 C4 F6 67.2(3) C2 P O1 Ge -48.67(17) C2 C1 C3 F1 -54.2(3) C2 C1 C3 F2 64.4(3) C2 C1 C3 F3 -176.9(3) C2 C1 C4 F4 59.7(3) C2 C1 C4 F5 -179.7(3) C2 C1 C4 F6 -59.0(3) C3 C1 C2 P -126.0(2) C3 C1 C4 F4 -59.1(4) C3 C1 C4 F5 61.5(4) C3 C1 C4 F6 -177.8(3) C4 C1 C2 P 115.1(2) C4 C1 C3 F1 65.4(4) C4 C1 C3 F2 -176.0(3) C4 C1 C3 F3 -57.3(4) C5 Ge O1 P 137.15(18) C5 Ge O2 C1 -80.6(3) C6 Ge O1 P -93.51(19) C6 Ge O2 C1 151.5(2) C7 P O1 Ge -154.05(14) C7 P C2 C1 147.8(2) C7 C8 C9 C10 178.4(3) C7 C8 C13 C12 -178.4(3) C7 C14 C15 C16 179.8(3) C7 C14 C19 C18 -178.8(3) C7 C20 C21 C22 -176.5(2) C7 C20 C25 C24 177.2(2) C8 C7 C14 C15 -0.9(4) C8 C7 C14 C19 179.5(3) C8 C7 C20 C21 106.3(3) C8 C7 C20 C25 -68.5(3) C8 C9 C10 C11 -0.2(5) C9 C8 C13 C12 -1.3(4) C9 C10 C11 C12 -1.2(5) C10 C11 C12 C13 1.3(5) C11 C12 C13 C8 0.0(5) C13 C8 C9 C10 1.4(4) C14 C7 C8 C9 -67.3(3) C14 C7 C8 C13 109.6(3) C14 C7 C20 C21 -17.3(3) C14 C7 C20 C25 167.8(2) C14 C15 C16 C17 -0.5(5) C15 C14 C19 C18 1.5(4) C15 C16 C17 C18 0.7(5) C16 C17 C18 C19 0.2(5) C17 C18 C19 C14 -1.3(5) C19 C14 C15 C16 -0.6(5) C20 C7 C8 C9 169.7(3) C20 C7 C8 C13 -13.3(3) C20 C7 C14 C15 120.6(3) C20 C7 C14 C19 -59.0(3) C20 C21 C22 C23 0.1(4) C21 C20 C25 C24 2.1(4) C21 C22 C23 C24 0.9(4) C22 C23 C24 C25 -0.4(4) C23 C24 C25 C20 -1.1(4) C25 C20 C21 C22 -1.6(4)