#------------------------------------------------------------------------------ #$Date: 2019-06-18 03:19:07 +0300 (Tue, 18 Jun 2019) $ #$Revision: 216033 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/14/1551458.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_1551458 loop_ _publ_author_name 'Hartmann, Deborah' 'Sch\"adler, Marcel' 'Greb, Lutz' _publ_section_title ; Bis(catecholato)silanes: assessment, rationale and increase of silicon’s Lewis superacidity ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC02167A _journal_year 2019 _chemical_formula_moiety 'C24 H30 F8 O6 P2 Si' _chemical_formula_sum 'C24 H30 F8 O6 P2 Si' _chemical_formula_weight 656.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-01-22 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-03-26 deposited with the CCDC. 2019-06-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.90(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.753(2) _cell_length_b 11.953(2) _cell_length_c 11.361(2) _cell_measurement_reflns_used 2084 _cell_measurement_temperature 120 _cell_measurement_theta_max 26 _cell_measurement_theta_min 1 _cell_volume 1389.6(5) _computing_cell_refinement 'DENZO/SCALEPACK (Bruker AXS, 1997-2009)' _computing_data_collection 'COLLECT (Bruker AXS, 1997-2009)' _computing_data_reduction 'DENZO/SCALEPACK (Bruker AXS, 1997-2009)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 120 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'NONIUS KAPPA CCD' _diffrn_measurement_method O-Scan _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_unetI/netI 0.0617 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7789 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.052 _diffrn_reflns_theta_min 2.282 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.292 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.569 _exptl_crystal_description irregular _exptl_crystal_F_000 676 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.739 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 285 _refine_ls_number_reflns 4058 _refine_ls_number_restraints 22 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0634 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+1.5163P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1574 _refine_ls_wR_factor_ref 0.1769 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2738 _reflns_number_total 4058 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc02167a2.cif _cod_data_source_block ms29c_p2_1 _cod_original_cell_volume 1389.4(5) _cod_database_code 1551458 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_max 0.892 _shelx_estimated_absorpt_t_min 0.880 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances F4-C6 \\sim F4A-C6A with sigma of 0.02 F2-C4 \\sim F2A-C4A with sigma of 0.02 F3-C5 \\sim F3A-C5A with sigma of 0.02 C1-C6 \\sim C1-C6A with sigma of 0.02 C3-C4 \\sim C3-C4A with sigma of 0.02 C6-C5 \\sim C6A-C5A with sigma of 0.02 C4-C5 \\sim C4A-C5A with sigma of 0.02 F4-C1 \\sim F4A-C1 with sigma of 0.04 F4-C5 \\sim F4A-C5A with sigma of 0.04 F2-C3 \\sim F2A-C3 with sigma of 0.04 F2-C5 \\sim F2A-C5A with sigma of 0.04 F3-C6 \\sim F3A-C6A with sigma of 0.04 F3-C4 \\sim F3A-C4A with sigma of 0.04 C1-C5 \\sim C1-C5A with sigma of 0.04 C3-C5 \\sim C3-C5A with sigma of 0.04 C6-C4 \\sim C6A-C4A with sigma of 0.04 P1-C7 \\sim P1-C7A with sigma of 0.02 C7-C8 \\sim C7A-C8A with sigma of 0.02 P1-C8 \\sim P1-C8A with sigma of 0.04 P1-C11 \\sim P1-C11A with sigma of 0.02 C11-C12 \\sim C11A-C12A with sigma of 0.02 P1-C12 \\sim P1-C12A with sigma of 0.04 3. Rigid body (RIGU) restrains C12 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(F4A)=Sof(C6A)=Sof(F3A)=Sof(C5A)=Sof(C4A)=Sof(F2A)=1-FVAR(1) Sof(F4)=Sof(F2)=Sof(F3)=Sof(C6)=Sof(C4)=Sof(C5)=FVAR(1) Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(2) Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(2) Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(3) Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(3) 5.a Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C7(H7A,H7B), C11(H11A,H11B), C7A(H7AA,H7AB), C11A(H11C,H11D) 5.b Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C8A(H8AA,H8AB, H8AC), C12A(H12D,H12E,H12F) ; _shelx_res_file ; TITL ms29c_p2_1_a.res in P2(1)/n ms29c_p2_1.res created by SHELXL-2018/3 at 16:32:30 on 22-Jan-2019 REM Old TITL ms29c_p2_1_a.res in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.208, Rweak 0.013, Alpha 0.047, Orientation as input REM Formula found by SHELXT: C24 O8 F6 Si P2 CELL 0.71073 10.7526 11.953 11.3608 90 107.905 90 ZERR 2 0.0022 0.0024 0.0023 0 0.03 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F O P Si UNIT 48 60 16 12 4 2 SADI F4 C6 F4A C6A SADI F2 C4 F2A C4A SADI F3 C5 F3A C5A SADI C1 C6 C1 C6A SADI C3 C4 C3 C4A SADI C6 C5 C6A C5A SADI C4 C5 C4A C5A SADI 0.04 F4 C1 F4A C1 SADI 0.04 F4 C5 F4A C5A SADI 0.04 F2 C3 F2A C3 SADI 0.04 F2 C5 F2A C5A SADI 0.04 F3 C6 F3A C6A SADI 0.04 F3 C4 F3A C4A SADI 0.04 C1 C5 C1 C5A SADI 0.04 C3 C5 C3 C5A SADI 0.04 C6 C4 C6A C4A SADI P1 C7 P1 C7A SADI C7 C8 C7A C8A SADI 0.04 P1 C8 P1 C8A SADI P1 C11 P1 C11A SADI C11 C12 C11A C12A SADI 0.04 P1 C12 P1 C12A RIGU C12 L.S. 10 PLAN 20 SIZE 0.45 0.4 0.4 TEMP -153.15 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.075600 1.516300 FVAR 0.46596 0.61726 0.61896 0.55321 SI01 6 0.500000 0.500000 0.500000 10.50000 0.02210 0.02031 = 0.01678 0.00025 0.00741 -0.00152 P1 5 0.659847 0.307036 0.671563 11.00000 0.03368 0.02642 = 0.02317 0.00598 0.01024 0.00672 F1 3 0.905815 0.604364 0.485125 11.00000 0.03669 0.05667 = 0.03478 -0.01806 0.01856 -0.02388 O2 4 0.663935 0.539738 0.521768 11.00000 0.02437 0.02564 = 0.01778 -0.00183 0.00777 -0.00265 O1 4 0.488804 0.442405 0.353821 11.00000 0.02402 0.02673 = 0.01957 -0.00376 0.00909 -0.00470 O3 4 0.550335 0.364028 0.571535 11.00000 0.02718 0.02278 = 0.02425 0.00284 0.00550 -0.00081 PART 1 F4 3 0.536083 0.375714 0.128671 21.00000 0.03262 0.05317 = 0.02138 -0.01620 0.00920 -0.01408 F2 3 0.955381 0.539518 0.273703 21.00000 0.03464 0.04436 = 0.04103 -0.01304 0.02382 -0.01233 F3 3 0.769547 0.425131 0.097134 21.00000 0.04119 0.04951 = 0.02491 -0.00882 0.02096 -0.00506 PART 0 C2 1 0.695377 0.520794 0.418149 11.00000 0.03127 0.03251 = 0.02254 -0.00328 0.01341 -0.00829 C1 1 0.597693 0.465900 0.324404 11.00000 0.03082 0.03572 = 0.02457 -0.00398 0.01406 -0.01083 C3 1 0.810654 0.550146 0.397353 11.00000 0.03845 0.04673 = 0.02890 -0.01218 0.01626 -0.02215 PART 1 C6 1 0.628520 0.428054 0.221338 21.00000 0.02655 0.02607 = 0.02055 -0.00439 0.00654 -0.00535 PART 0 C10 1 0.865319 0.344841 0.888443 11.00000 0.02796 0.05524 = 0.03951 0.01178 0.00366 0.00328 AFIX 137 H10A 2 0.922907 0.305369 0.850188 11.00000 -1.50000 H10B 2 0.828592 0.291350 0.934143 11.00000 -1.50000 H10C 2 0.915506 0.401865 0.945455 11.00000 -1.50000 AFIX 0 C9 1 0.753734 0.401285 0.787208 11.00000 0.02678 0.03912 = 0.04413 0.01053 -0.00561 -0.00260 AFIX 23 H9A 2 0.791366 0.459751 0.746572 11.00000 -1.20000 H9B 2 0.694634 0.438737 0.826649 11.00000 -1.20000 AFIX 0 PART 1 C4 1 0.840631 0.512690 0.292836 21.00000 0.02504 0.02455 = 0.03351 0.00117 0.01418 -0.00184 C5 1 0.746809 0.456683 0.202601 21.00000 0.03302 0.03140 = 0.02113 -0.00464 0.01637 -0.00095 C7 1 0.789322 0.255961 0.612856 31.00000 0.02740 0.03657 = 0.03241 -0.00689 0.00716 0.00112 AFIX 23 H7A 2 0.839110 0.320098 0.595257 31.00000 -1.20000 H7B 2 0.850385 0.208559 0.676253 31.00000 -1.20000 AFIX 0 C8 1 0.730690 0.187565 0.494031 31.00000 0.03675 0.03977 = 0.03484 -0.00698 0.00623 0.00012 AFIX 137 H8A 2 0.667367 0.233612 0.432692 31.00000 -1.50000 H8B 2 0.686709 0.121237 0.512888 31.00000 -1.50000 H8C 2 0.800629 0.164259 0.460789 31.00000 -1.50000 AFIX 0 C11 1 0.577729 0.215893 0.752255 41.00000 0.05109 0.01542 = 0.02792 0.00449 0.01166 0.00193 AFIX 23 H11A 2 0.525753 0.160230 0.692717 41.00000 -1.20000 H11B 2 0.644848 0.174507 0.816991 41.00000 -1.20000 AFIX 0 C12 1 0.487337 0.275639 0.812851 41.00000 0.03656 0.03688 = 0.04482 0.01753 0.01963 0.00427 AFIX 137 H12A 2 0.424921 0.322111 0.751210 41.00000 -1.50000 H12B 2 0.539452 0.323041 0.880464 41.00000 -1.50000 H12C 2 0.439730 0.220042 0.845698 41.00000 -1.50000 AFIX 0 PART 0 PART 2 F4A 3 0.509431 0.412400 0.109691 -21.00000 0.04243 0.03953 = 0.02510 -0.00877 0.01540 -0.00932 C6A 1 0.603511 0.461182 0.203502 -21.00000 0.03007 0.01903 = 0.01821 0.00266 0.01011 -0.00080 F3A 3 0.733320 0.481354 0.069905 -21.00000 0.04329 0.05597 = 0.02557 -0.00405 0.02179 -0.00608 C5A 1 0.717287 0.498460 0.181602 -21.00000 0.03266 0.03445 = 0.02200 -0.00360 0.01363 -0.00085 C4A 1 0.813911 0.547436 0.275179 -21.00000 0.02335 0.02424 = 0.03399 0.00488 0.01683 -0.00171 F2A 3 0.925433 0.581524 0.254060 -21.00000 0.03349 0.06835 = 0.04401 -0.01220 0.03053 -0.01842 C7A 1 0.735115 0.207687 0.595589 -31.00000 0.02768 0.01901 = 0.01936 0.00258 0.00540 0.00605 AFIX 23 H7AA 2 0.804979 0.167031 0.658403 -31.00000 -1.20000 H7AB 2 0.669075 0.152330 0.550604 -31.00000 -1.20000 AFIX 0 C8A 1 0.793908 0.266121 0.503809 -31.00000 0.03272 0.03071 = 0.03291 0.00737 0.01499 0.01240 AFIX 137 H8AA 2 0.723212 0.292312 0.431976 -31.00000 -1.50000 H8AB 2 0.848999 0.213109 0.476616 -31.00000 -1.50000 H8AC 2 0.846859 0.330063 0.544534 -31.00000 -1.50000 AFIX 0 C11A 1 0.598906 0.190348 0.735382 -41.00000 0.02982 0.01565 = 0.03055 -0.00030 0.00411 -0.00100 AFIX 23 H11C 2 0.571501 0.130267 0.672740 -41.00000 -1.20000 H11D 2 0.668414 0.160384 0.807385 -41.00000 -1.20000 AFIX 0 C12A 1 0.483573 0.227833 0.775254 -41.00000 0.03513 0.04610 = 0.05178 0.02119 0.01976 0.00230 AFIX 137 H12D 2 0.411288 0.249125 0.702250 -41.00000 -1.50000 H12E 2 0.509041 0.292237 0.830866 -41.00000 -1.50000 H12F 2 0.455689 0.166417 0.818472 -41.00000 -1.50000 AFIX 0 HKLF 4 REM ms29c_p2_1_a.res in P2(1)/n REM wR2 = 0.1769, GooF = S = 1.074, Restrained GooF = 1.074 for all data REM R1 = 0.0634 for 2738 Fo > 4sig(Fo) and 0.1055 for all 4058 data REM 285 parameters refined using 22 restraints END WGHT 0.0756 1.5164 REM Highest difference peak 0.739, deepest hole -0.396, 1-sigma level 0.090 Q1 1 0.6547 0.4993 0.6497 11.00000 0.05 0.74 Q2 1 0.7421 0.3145 0.7519 11.00000 0.05 0.62 Q3 1 0.4211 0.4935 0.4207 11.00000 0.05 0.58 Q4 1 0.8111 0.3134 0.8152 11.00000 0.05 0.54 Q5 1 0.5175 0.3097 0.5173 11.00000 0.05 0.50 Q6 1 0.6960 0.3696 0.7211 11.00000 0.05 0.49 Q7 1 0.6455 0.5028 0.3721 11.00000 0.05 0.44 Q8 1 0.5977 0.3060 0.5848 11.00000 0.05 0.44 Q9 1 0.5627 0.4539 0.2564 11.00000 0.05 0.38 Q10 1 0.7796 0.4989 0.2428 11.00000 0.05 0.34 Q11 1 0.7163 0.3031 0.6068 11.00000 0.05 0.33 Q12 1 0.8089 0.3812 0.8336 11.00000 0.05 0.33 Q13 1 0.6359 0.4360 -0.0370 11.00000 0.05 0.33 Q14 1 0.7815 0.5908 0.3591 11.00000 0.05 0.32 Q15 1 0.6392 0.4625 0.0799 11.00000 0.05 0.32 Q16 1 0.8982 0.1027 0.4821 11.00000 0.05 0.31 Q17 1 0.9181 0.3952 0.9178 11.00000 0.05 0.31 Q18 1 0.5848 0.4085 0.1779 11.00000 0.05 0.31 Q19 1 0.6624 0.5421 0.7979 11.00000 0.05 0.30 Q20 1 0.8065 0.5660 0.1416 11.00000 0.05 0.30 ; _shelx_res_checksum 67736 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_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' 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si01 Si 0.500000 0.500000 0.500000 0.0194(2) Uani 1 2 d S T P . . P1 P 0.65985(8) 0.30704(7) 0.67156(7) 0.0274(2) Uani 1 1 d D . . . . F1 F 0.90581(18) 0.60436(18) 0.48512(17) 0.0410(5) Uani 1 1 d . . . . . O2 O 0.66394(18) 0.53974(16) 0.52177(16) 0.0223(4) Uani 1 1 d . . . . . O1 O 0.48880(18) 0.44240(16) 0.35382(16) 0.0229(4) Uani 1 1 d . . . . . O3 O 0.55034(19) 0.36403(16) 0.57153(17) 0.0253(4) Uani 1 1 d . . . . . F4 F 0.5361(8) 0.3757(8) 0.1287(7) 0.0355(16) Uani 0.62(2) 1 d D . . A 1 F2 F 0.9554(7) 0.5395(7) 0.2737(7) 0.0373(14) Uani 0.62(2) 1 d D . . A 1 F3 F 0.7695(6) 0.4251(8) 0.0971(5) 0.0361(18) Uani 0.62(2) 1 d D . . A 1 C2 C 0.6954(3) 0.5208(3) 0.4181(3) 0.0276(6) Uani 1 1 d . . . . . C1 C 0.5977(3) 0.4659(3) 0.3244(3) 0.0291(6) Uani 1 1 d D . . . . C3 C 0.8107(3) 0.5501(3) 0.3974(3) 0.0367(8) Uani 1 1 d D . . . . C6 C 0.6285(8) 0.4281(8) 0.2213(7) 0.0246(17) Uani 0.62(2) 1 d D . . A 1 C10 C 0.8653(3) 0.3448(3) 0.8884(3) 0.0424(8) Uani 1 1 d . . . . . H10A H 0.922907 0.305369 0.850188 0.064 Uiso 1 1 calc GR . . . . H10B H 0.828592 0.291350 0.934143 0.064 Uiso 1 1 calc GR . . . . H10C H 0.915506 0.401865 0.945455 0.064 Uiso 1 1 calc GR . . . . C9 C 0.7537(3) 0.4013(3) 0.7872(3) 0.0404(8) Uani 1 1 d . . . . . H9A H 0.791366 0.459751 0.746572 0.048 Uiso 1 1 calc R . . . . H9B H 0.694634 0.438737 0.826649 0.048 Uiso 1 1 calc R . . . . C4 C 0.8406(8) 0.5127(8) 0.2928(7) 0.0265(17) Uani 0.62(2) 1 d D . . A 1 C5 C 0.7468(8) 0.4567(8) 0.2026(7) 0.0267(16) Uani 0.62(2) 1 d D . . A 1 C7 C 0.7893(5) 0.2560(6) 0.6129(5) 0.0326(13) Uani 0.619(8) 1 d D . . B 1 H7A H 0.839110 0.320098 0.595257 0.039 Uiso 0.619(8) 1 calc R . . B 1 H7B H 0.850385 0.208559 0.676253 0.039 Uiso 0.619(8) 1 calc R . . B 1 C8 C 0.7307(5) 0.1876(5) 0.4940(5) 0.0382(15) Uani 0.619(8) 1 d D . . B 1 H8A H 0.667367 0.233612 0.432692 0.057 Uiso 0.619(8) 1 calc GR . . B 1 H8B H 0.686709 0.121237 0.512888 0.057 Uiso 0.619(8) 1 calc GR . . B 1 H8C H 0.800629 0.164259 0.460789 0.057 Uiso 0.619(8) 1 calc GR . . B 1 C11 C 0.5777(15) 0.2159(12) 0.7523(13) 0.032(3) Uani 0.55(4) 1 d D . . B 1 H11A H 0.525753 0.160230 0.692717 0.038 Uiso 0.55(4) 1 calc R . . B 1 H11B H 0.644848 0.174507 0.816991 0.038 Uiso 0.55(4) 1 calc R . . B 1 C12 C 0.4873(8) 0.2756(15) 0.8129(13) 0.038(3) Uani 0.55(4) 1 d D U . B 1 H12A H 0.424921 0.322111 0.751210 0.057 Uiso 0.55(4) 1 calc GR . . B 1 H12B H 0.539452 0.323041 0.880464 0.057 Uiso 0.55(4) 1 calc GR . . B 1 H12C H 0.439730 0.220042 0.845698 0.057 Uiso 0.55(4) 1 calc GR . . B 1 F4A F 0.5094(13) 0.4124(11) 0.1097(11) 0.035(2) Uani 0.38(2) 1 d D . . A 2 C6A C 0.6035(12) 0.4612(12) 0.2035(10) 0.022(3) Uani 0.38(2) 1 d D . . A 2 F3A F 0.7333(10) 0.4814(14) 0.0699(7) 0.039(3) Uani 0.38(2) 1 d D . . A 2 C5A C 0.7173(12) 0.4985(14) 0.1816(9) 0.029(3) Uani 0.38(2) 1 d D . . A 2 C4A C 0.8139(12) 0.5474(13) 0.2752(9) 0.025(3) Uani 0.38(2) 1 d D . . A 2 F2A F 0.9254(12) 0.5815(15) 0.2541(11) 0.044(3) Uani 0.38(2) 1 d D . . A 2 C7A C 0.7351(9) 0.2077(7) 0.5956(7) 0.0224(18) Uani 0.381(8) 1 d D . . B 2 H7AA H 0.804979 0.167031 0.658403 0.027 Uiso 0.381(8) 1 calc R . . B 2 H7AB H 0.669075 0.152330 0.550604 0.027 Uiso 0.381(8) 1 calc R . . B 2 C8A C 0.7939(8) 0.2661(7) 0.5038(7) 0.031(2) Uani 0.381(8) 1 d D . . B 2 H8AA H 0.723212 0.292312 0.431976 0.047 Uiso 0.381(8) 1 calc GR . . B 2 H8AB H 0.848999 0.213109 0.476616 0.047 Uiso 0.381(8) 1 calc GR . . B 2 H8AC H 0.846859 0.330063 0.544534 0.047 Uiso 0.381(8) 1 calc GR . . B 2 C11A C 0.5989(16) 0.1903(12) 0.7354(16) 0.027(3) Uani 0.45(4) 1 d D . . B 2 H11C H 0.571501 0.130267 0.672740 0.032 Uiso 0.45(4) 1 calc R . . B 2 H11D H 0.668414 0.160384 0.807385 0.032 Uiso 0.45(4) 1 calc R . . B 2 C12A C 0.4836(10) 0.228(2) 0.775(2) 0.043(4) Uani 0.45(4) 1 d D . . B 2 H12D H 0.411288 0.249125 0.702250 0.064 Uiso 0.45(4) 1 calc GR . . B 2 H12E H 0.509041 0.292237 0.830866 0.064 Uiso 0.45(4) 1 calc GR . . B 2 H12F H 0.455689 0.166417 0.818472 0.064 Uiso 0.45(4) 1 calc GR . . B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si01 0.0221(5) 0.0203(5) 0.0168(5) 0.0002(4) 0.0074(4) -0.0015(4) P1 0.0337(4) 0.0264(4) 0.0232(4) 0.0060(3) 0.0102(3) 0.0067(3) F1 0.0367(10) 0.0567(13) 0.0348(10) -0.0181(9) 0.0186(8) -0.0239(9) O2 0.0244(9) 0.0256(10) 0.0178(8) -0.0018(7) 0.0078(8) -0.0026(8) O1 0.0240(10) 0.0267(10) 0.0196(9) -0.0038(7) 0.0091(8) -0.0047(8) O3 0.0272(10) 0.0228(10) 0.0242(9) 0.0028(8) 0.0055(8) -0.0008(8) F4 0.033(3) 0.053(4) 0.021(2) -0.016(3) 0.0092(19) -0.014(3) F2 0.035(3) 0.044(3) 0.041(3) -0.013(2) 0.024(2) -0.012(2) F3 0.041(2) 0.050(4) 0.0249(19) -0.009(2) 0.0210(18) -0.005(2) C2 0.0313(15) 0.0325(16) 0.0225(13) -0.0033(11) 0.0134(12) -0.0083(12) C1 0.0308(15) 0.0357(16) 0.0246(13) -0.0040(12) 0.0141(12) -0.0108(12) C3 0.0384(17) 0.0467(19) 0.0289(15) -0.0122(14) 0.0163(14) -0.0222(15) C6 0.027(3) 0.026(4) 0.021(3) -0.004(3) 0.007(2) -0.005(3) C10 0.0280(16) 0.055(2) 0.0395(18) 0.0118(16) 0.0037(14) 0.0033(15) C9 0.0268(15) 0.0391(19) 0.0441(19) 0.0105(15) -0.0056(14) -0.0026(14) C4 0.025(3) 0.025(4) 0.034(3) 0.001(3) 0.014(3) -0.002(3) C5 0.033(3) 0.031(4) 0.021(3) -0.005(3) 0.016(2) -0.001(3) C7 0.027(3) 0.037(3) 0.032(3) -0.007(2) 0.007(2) 0.001(2) C8 0.037(3) 0.040(3) 0.035(3) -0.007(2) 0.006(2) 0.000(2) C11 0.051(6) 0.015(4) 0.028(4) 0.004(4) 0.012(3) 0.002(4) C12 0.037(4) 0.037(7) 0.045(5) 0.018(5) 0.020(3) 0.004(3) F4A 0.042(5) 0.040(5) 0.025(4) -0.009(3) 0.015(3) -0.009(4) C6A 0.030(5) 0.019(6) 0.018(4) 0.003(4) 0.010(4) -0.001(4) F3A 0.043(4) 0.056(7) 0.026(3) -0.004(3) 0.022(3) -0.006(4) C5A 0.033(5) 0.034(7) 0.022(4) -0.004(4) 0.014(4) -0.001(5) C4A 0.023(5) 0.024(6) 0.034(5) 0.005(4) 0.017(4) -0.002(4) F2A 0.033(4) 0.068(8) 0.044(4) -0.012(5) 0.031(4) -0.018(5) C7A 0.028(4) 0.019(4) 0.019(3) 0.003(3) 0.005(3) 0.006(3) C8A 0.033(4) 0.031(5) 0.033(4) 0.007(3) 0.015(4) 0.012(4) C11A 0.030(5) 0.016(5) 0.031(5) 0.000(4) 0.004(4) -0.001(4) C12A 0.035(5) 0.046(9) 0.052(7) 0.021(7) 0.020(5) 0.002(5) 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' 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' Si Si 0.0817 0.0704 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O2 Si01 O2 180.0 . 3_666 O2 Si01 O3 88.25(9) 3_666 . O2 Si01 O3 91.75(9) 3_666 3_666 O2 Si01 O3 91.75(9) . . O2 Si01 O3 88.25(9) . 3_666 O1 Si01 O2 89.25(9) 3_666 . O1 Si01 O2 90.75(9) . . O1 Si01 O2 89.25(9) . 3_666 O1 Si01 O2 90.75(9) 3_666 3_666 O1 Si01 O1 180.0 3_666 . O1 Si01 O3 90.19(9) 3_666 . O1 Si01 O3 89.81(9) 3_666 3_666 O1 Si01 O3 90.19(9) . 3_666 O1 Si01 O3 89.81(9) . . O3 Si01 O3 180.0 . 3_666 O3 P1 C9 113.50(14) . . O3 P1 C7 112.26(19) . . O3 P1 C11 105.1(5) . . O3 P1 C7A 107.2(3) . . O3 P1 C11A 110.9(6) . . C9 P1 C7 99.1(2) . . C9 P1 C11 105.0(5) . . C9 P1 C7A 122.2(3) . . C11 P1 C7 121.8(6) . . C11A P1 C9 112.8(6) . . C11A P1 C7A 87.4(7) . . C2 O2 Si01 109.98(17) . . C1 O1 Si01 109.86(17) . . P1 O3 Si01 141.89(13) . . O2 C2 C1 114.4(2) . . O2 C2 C3 126.2(3) . . C3 C2 C1 119.4(3) . . O1 C1 C2 114.5(2) . . O1 C1 C6 126.5(4) . . O1 C1 C6A 122.9(5) . . C6 C1 C2 118.3(4) . . C6A C1 C2 121.0(5) . . F1 C3 C2 120.8(3) . . F1 C3 C4 117.4(4) . . F1 C3 C4A 119.8(5) . . C2 C3 C4 121.3(4) . . C2 C3 C4A 117.6(5) . . F4 C6 C1 119.8(6) . . F4 C6 C5 118.6(6) . . C1 C6 C5 121.0(5) . . H10A C10 H10B 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . C9 C10 H10A 109.5 . . C9 C10 H10B 109.5 . . C9 C10 H10C 109.5 . . P1 C9 H9A 108.7 . . P1 C9 H9B 108.7 . . C10 C9 P1 114.0(3) . . C10 C9 H9A 108.7 . . C10 C9 H9B 108.7 . . H9A C9 H9B 107.6 . . F2 C4 C3 121.3(6) . . F2 C4 C5 119.5(6) . . C5 C4 C3 118.9(5) . . F3 C5 C6 119.3(5) . . F3 C5 C4 120.5(5) . . C4 C5 C6 120.1(5) . . P1 C7 H7A 109.6 . . P1 C7 H7B 109.6 . . H7A C7 H7B 108.1 . . C8 C7 P1 110.2(4) . . C8 C7 H7A 109.6 . . C8 C7 H7B 109.6 . . C7 C8 H8A 109.5 . . C7 C8 H8B 109.5 . . C7 C8 H8C 109.5 . . H8A C8 H8B 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . P1 C11 H11A 108.5 . . P1 C11 H11B 108.5 . . H11A C11 H11B 107.5 . . C12 C11 P1 114.9(7) . . C12 C11 H11A 108.5 . . C12 C11 H11B 108.5 . . C11 C12 H12A 109.5 . . C11 C12 H12B 109.5 . . C11 C12 H12C 109.5 . . H12A C12 H12B 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . F4A C6A C1 122.9(9) . . F4A C6A C5A 118.7(9) . . C5A C6A C1 118.0(8) . . F3A C5A C6A 119.5(8) . . F3A C5A C4A 120.7(8) . . C4A C5A C6A 119.8(8) . . C5A C4A C3 122.4(8) . . F2A C4A C3 117.5(9) . . F2A C4A C5A 119.5(9) . . P1 C7A H7AA 109.4 . . P1 C7A H7AB 109.4 . . H7AA C7A H7AB 108.0 . . C8A C7A P1 111.3(5) . . C8A C7A H7AA 109.4 . . C8A C7A H7AB 109.4 . . C7A C8A H8AA 109.5 . . C7A C8A H8AB 109.5 . . C7A C8A H8AC 109.5 . . H8AA C8A H8AB 109.5 . . H8AA C8A H8AC 109.5 . . H8AB C8A H8AC 109.5 . . P1 C11A H11C 109.9 . . P1 C11A H11D 109.9 . . H11C C11A H11D 108.3 . . C12A C11A P1 109.1(7) . . C12A C11A H11C 109.9 . . C12A C11A H11D 109.9 . . C11A C12A H12D 109.5 . . C11A C12A H12E 109.5 . . C11A C12A H12F 109.5 . . H12D C12A H12E 109.5 . . H12D C12A H12F 109.5 . . H12E C12A H12F 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si01 O2 1.7681(19) 3_666 Si01 O2 1.7680(19) . Si01 O1 1.7673(18) 3_666 Si01 O1 1.7673(18) . Si01 O3 1.8233(19) . Si01 O3 1.823(2) 3_666 P1 O3 1.523(2) . P1 C9 1.789(4) . P1 C7 1.824(5) . P1 C11 1.818(9) . P1 C7A 1.800(7) . P1 C11A 1.787(10) . F1 C3 1.354(3) . O2 C2 1.340(3) . O1 C1 1.342(3) . F4 C6 1.358(7) . F2 C4 1.356(7) . F3 C5 1.348(6) . C2 C1 1.407(4) . C2 C3 1.377(4) . C1 C6 1.387(7) . C1 C6A 1.395(10) . C3 C4 1.396(7) . C3 C4A 1.400(10) . C6 C5 1.395(8) . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 H10C 0.9800 . C10 C9 1.539(4) . C9 H9A 0.9900 . C9 H9B 0.9900 . C4 C5 1.371(8) . C7 H7A 0.9900 . C7 H7B 0.9900 . C7 C8 1.538(7) . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . C11 H11A 0.9900 . C11 H11B 0.9900 . C11 C12 1.530(9) . C12 H12A 0.9800 . C12 H12B 0.9800 . C12 H12C 0.9800 . F4A C6A 1.355(11) . C6A C5A 1.394(11) . F3A C5A 1.348(9) . C5A C4A 1.369(11) . C4A F2A 1.356(10) . C7A H7AA 0.9900 . C7A H7AB 0.9900 . C7A C8A 1.543(10) . C8A H8AA 0.9800 . C8A H8AB 0.9800 . C8A H8AC 0.9800 . C11A H11C 0.9900 . C11A H11D 0.9900 . C11A C12A 1.513(12) . C12A H12D 0.9800 . C12A H12E 0.9800 . C12A H12F 0.9800 .