# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_4813
_database_code_depnum_ccdc_archive 'CCDC 1526599'
_audit_update_record
;
2017-01-10 deposited with the CCDC.
2017-02-03 downloaded from the CCDC.
;
_audit_creation_date 2016-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_chemical_name_common ?
_chemical_name_systematic PB-47
_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_melting_point ?
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'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.0079(2)
_cell_length_b 13.1369(3)
_cell_length_c 13.2698(2)
_cell_angle_alpha 92.8970(10)
_cell_angle_beta 97.6730(10)
_cell_angle_gamma 90.1710(10)
_cell_volume 1554.17(5)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 8272
_cell_measurement_temperature 123(2)
_cell_measurement_theta_max 29.13
_cell_measurement_theta_min 1.00
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_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_absorpt_process_details ?
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.917
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_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
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_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_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_source 'sealed tube'
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6878
_reflns_number_total 7498
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_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)'
_refine_diff_density_max 1.240
_refine_diff_density_min -1.625
_refine_diff_density_rms 0.125
_refine_ls_extinction_coef .
_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_R_factor_all 0.0304
_refine_ls_R_factor_gt 0.0263
_refine_ls_restrained_S_all 1.059
_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
_refine_special_details ?
_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)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
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)
_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
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_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
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_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
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) . . . . ?
_shelx_SHELXL_version_number 2014/7
_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
;
_olex2_submission_special_instructions 'No special instructions were received'
#END---------------------------------------------------------------------------
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_4012f
_database_code_depnum_ccdc_archive 'CCDC 1526597'
_audit_update_record
;
2017-01-10 deposited with the CCDC.
2017-02-03 downloaded from the CCDC.
;
_audit_creation_date 2017-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic AKY-488-2
_chemical_formula_moiety '2(C36 H34 F6 Li O11 P W), C4 H10 O'
_chemical_formula_sum 'C76 H78 F12 Li2 O23 P2 W2'
_chemical_formula_weight 2030.90
_chemical_melting_point ?
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'
Li Li -0.0003 0.0001 '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'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.7408(5)
_cell_length_b 18.5934(8)
_cell_length_c 20.0735(8)
_cell_angle_alpha 86.722(3)
_cell_angle_beta 74.872(2)
_cell_angle_gamma 73.209(3)
_cell_volume 4049.1(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9524
_cell_measurement_temperature 100
_cell_measurement_theta_max 29.31
_cell_measurement_theta_min 2.29
_shelx_estimated_absorpt_T_max 0.890
_shelx_estimated_absorpt_T_min 0.755
_exptl_absorpt_coefficient_mu 2.979
_exptl_absorpt_correction_T_max 0.5865
_exptl_absorpt_correction_T_min 0.4057
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1147 before and 0.0646 after correction. The Ratio
of minimum to maximum transmission is 0.6917. The \l/2 correction
factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.666
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 2020
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.04
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0818
_diffrn_reflns_av_unetI/netI 0.0858
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 105146
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 28.000
_diffrn_reflns_theta_min 2.468
_diffrn_ambient_temperature 100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 12783
_reflns_number_total 19509
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_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 'XS (Sheldrick, 2008)'
_refine_diff_density_max 4.023
_refine_diff_density_min -1.908
_refine_diff_density_rms 0.185
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.009
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1058
_refine_ls_number_reflns 19509
_refine_ls_number_restraints 27
_refine_ls_R_factor_all 0.0959
_refine_ls_R_factor_gt 0.0470
_refine_ls_restrained_S_all 1.012
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1073
_refine_ls_wR_factor_ref 0.1261
_refine_special_details ?
_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, All O(H) groups
2. Restrained distances
O12-C39
1.49 with sigma of 0.01
3. Rigid bond restraints
F5, C4
with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
F1', C3'
with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C18) \\sim Ueq, Uanis(C3') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
C1(H1A,H1B), C1'(H1'A,H1'B), C29(H29A,H29B), C28(H28A,H28B), C31(H31A,H31B),
C26(H26A,H26B), C30(H30A,H30B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B),
C38(H38A,H38B), C39(H39A,H39B), C24'(H24C,H24D), C30'(H30C,H30D), C29'(H29C,
H29D), C25'(H25C,H25D), C31'(H31C,H31D), C26'(H26C,H26D), C27'(H27C,H27D),
C28'(H28C,H28D)
5.b Aromatic/amide H refined with riding coordinates:
C20(H20), C7(H7), C14(H14), C11(H11), C23(H23), C11'(H11'), C17(H17),
C16'(H16'), C23'(H23'), C20'(H20'), C7'(H7'), C15(H15), C10(H10), C9'(H9'),
C8'(H8'), C17'(H17'), C22(H22), C13(H13), C14'(H14'), C21(H21), C19(H19),
C16(H16), C8(H8), C15'(H15'), C22'(H22'), C9(H9), C19'(H19'), C21'(H21'),
C10'(H10'), C13'(H13')
5.c Idealised Me refined as rotating group:
C37(H37A,H37B,H37C), C40(H40A,H40B,H40C)
5.d Idealised tetrahedral OH refined as rotating group:
O1(H1), O1'(H1')
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
W W 0.46039(2) 0.27415(2) 0.28589(2) 0.01891(7) Uani 1 1 d . . . . .
W' W -0.11250(2) 0.36912(2) -0.28980(2) 0.01853(7) Uani 1 1 d . . . . .
P' P -0.14039(13) 0.29227(8) -0.17967(7) 0.0173(3) Uani 1 1 d . . . . .
P P 0.60311(12) 0.23299(7) 0.36763(7) 0.0148(3) Uani 1 1 d . . . . .
O10' O 0.0162(4) 0.2488(2) -0.41266(19) 0.0265(9) Uani 1 1 d . . . . .
F5 F 0.4288(3) 0.30644(17) 0.62818(15) 0.0282(8) Uani 1 1 d . U . . .
F2 F 0.2860(3) 0.22447(18) 0.56256(17) 0.0310(8) Uani 1 1 d . . . . .
F4 F 0.5033(3) 0.18897(17) 0.59986(15) 0.0265(7) Uani 1 1 d . . . . .
F2' F -0.1249(4) 0.3981(2) 0.05283(17) 0.0420(10) Uani 1 1 d . . . . .
O11 O 0.5715(4) 0.1493(2) 0.1659(2) 0.0323(10) Uani 1 1 d . . . . .
C35' C -0.0290(5) 0.2885(3) -0.3655(3) 0.0186(12) Uani 1 1 d . . . . .
F1 F 0.2711(3) 0.29043(19) 0.47215(16) 0.0319(8) Uani 1 1 d . . . . .
O1 O 0.4657(3) 0.34535(19) 0.48827(18) 0.0230(9) Uani 1 1 d . . . . .
H1 H 0.5287 0.3403 0.4553 0.035 Uiso 1 1 calc GR . . . .
C1 C 0.5225(5) 0.2083(3) 0.4567(2) 0.0156(11) Uani 1 1 d . . . . .
H1A H 0.4626 0.1822 0.4516 0.019 Uiso 1 1 calc R . . . .
H1B H 0.5845 0.1722 0.4766 0.019 Uiso 1 1 calc R . . . .
C36 C 0.5373(5) 0.1917(3) 0.2109(3) 0.0238(13) Uani 1 1 d . . . . .
C18 C 0.6925(5) 0.0759(3) 0.3695(3) 0.0179(12) Uani 1 1 d . U . . .
F3 F 0.2479(3) 0.34477(18) 0.56798(16) 0.0308(8) Uani 1 1 d . . . . .
O1' O -0.2311(3) 0.4072(2) -0.05680(19) 0.0253(9) Uani 1 1 d . . . . .
H1' H -0.2592 0.3859 -0.0819 0.038 Uiso 1 1 calc GR . . . .
O2' O -0.2740(3) 0.31674(19) -0.13491(17) 0.0188(8) Uani 1 1 d . . . . .
O8 O 0.2943(4) 0.1742(2) 0.3689(2) 0.0371(11) Uani 1 1 d . . . . .
F6 F 0.6124(3) 0.26533(19) 0.56388(16) 0.0284(8) Uani 1 1 d . . . . .
O2 O 0.6526(3) 0.29726(18) 0.38199(17) 0.0165(8) Uani 1 1 d . . . . .
O10 O 0.6299(4) 0.3676(2) 0.1929(2) 0.0337(10) Uani 1 1 d . . . . .
C1' C -0.0480(5) 0.3053(3) -0.1187(3) 0.0191(12) Uani 1 1 d . . . . .
H1'A H -0.0307 0.2588 -0.0918 0.023 Uiso 1 1 calc R . . . .
H1'B H 0.0322 0.3101 -0.1470 0.023 Uiso 1 1 calc R . . . .
F4' F -0.0926(3) 0.49506(18) -0.04462(16) 0.0320(8) Uani 1 1 d . . . . .
C2 C 0.4529(5) 0.2748(3) 0.5094(3) 0.0176(11) Uani 1 1 d . . . . .
O7' O -0.0627(4) 0.4853(2) -0.4060(2) 0.0378(11) Uani 1 1 d . . . . .
F6' F -0.0497(4) 0.4605(2) -0.14982(17) 0.0433(10) Uani 1 1 d . . . . .
C2' C -0.1059(5) 0.3728(3) -0.0670(3) 0.0210(12) Uani 1 1 d . . . . .
C32' C -0.0857(5) 0.4428(3) -0.3641(3) 0.0264(13) Uani 1 1 d . . . . .
C33 C 0.3531(5) 0.2107(3) 0.3408(3) 0.0244(13) Uani 1 1 d . . . . .
C5' C -0.0858(5) 0.1829(3) -0.1877(3) 0.0195(12) Uani 1 1 d . . . . .
O9' O -0.3672(4) 0.3617(2) -0.3147(2) 0.0354(10) Uani 1 1 d . . . . .
C4 C 0.4973(5) 0.2576(3) 0.5755(3) 0.0270(14) Uani 1 1 d . U . . .
O11' O 0.1459(4) 0.3696(2) -0.2687(2) 0.0327(10) Uani 1 1 d . . . . .
C6' C -0.1465(5) 0.1424(3) -0.1248(3) 0.0190(12) Uani 1 1 d . . . . .
C33' C -0.2195(6) 0.4570(3) -0.2255(3) 0.0285(14) Uani 1 1 d . . . . .
C18' C -0.1259(5) 0.1625(3) -0.2494(3) 0.0190(12) Uani 1 1 d . . . . .
C20 C 0.6823(5) -0.0298(3) 0.4451(3) 0.0293(14) Uani 1 1 d . . . . .
H20 H 0.7114 -0.0618 0.4794 0.035 Uiso 1 1 calc R . . . .
C3' C -0.0865(5) 0.3436(3) 0.0004(3) 0.0252(13) Uani 1 1 d . U . . .
O9 O 0.3328(4) 0.4245(3) 0.3753(2) 0.0431(12) Uani 1 1 d . . . . .
O7 O 0.2596(4) 0.3411(2) 0.2043(2) 0.0367(11) Uani 1 1 d . . . . .
C34 C 0.3786(5) 0.3678(3) 0.3471(3) 0.0228(13) Uani 1 1 d . . . . .
C7 C 0.8210(5) 0.2056(3) 0.2353(3) 0.0245(13) Uani 1 1 d . . . . .
H7 H 0.8080 0.2481 0.2633 0.029 Uiso 1 1 calc R . . . .
C14 C 0.9277(5) 0.1686(3) 0.4701(3) 0.0246(13) Uani 1 1 d . . . . .
H14 H 0.9130 0.1924 0.5134 0.029 Uiso 1 1 calc R . . . .
C32 C 0.3351(6) 0.3167(3) 0.2336(3) 0.0260(13) Uani 1 1 d . . . . .
C36' C 0.0527(5) 0.3697(3) -0.2754(3) 0.0223(12) Uani 1 1 d . . . . .
C3 C 0.3131(5) 0.2842(3) 0.5283(3) 0.0243(13) Uani 1 1 d . . . . .
F1' F -0.1545(5) 0.2959(2) 0.02671(18) 0.0601(13) Uani 1 1 d . U . . .
C6 C 0.7908(5) 0.1425(3) 0.2659(3) 0.0182(12) Uani 1 1 d . . . . .
F3' F 0.0292(4) 0.3075(2) 0.0027(2) 0.0690(15) Uani 1 1 d . . . . .
C11 C 0.8169(5) 0.0799(3) 0.2237(3) 0.0247(13) Uani 1 1 d . . . . .
H11 H 0.8000 0.0352 0.2435 0.030 Uiso 1 1 calc R . . . .
F5' F 0.0774(3) 0.4126(2) -0.0896(2) 0.0530(11) Uani 1 1 d . . . . .
C23 C 0.6011(5) 0.0617(3) 0.3455(3) 0.0233(13) Uani 1 1 d . . . . .
H23 H 0.5728 0.0921 0.3102 0.028 Uiso 1 1 calc R . . . .
C11' C -0.1356(5) 0.0668(3) -0.1337(3) 0.0266(13) Uani 1 1 d . . . . .
H11' H -0.0978 0.0440 -0.1782 0.032 Uiso 1 1 calc R . . . .
C12 C 0.8483(5) 0.1432(3) 0.3761(3) 0.0188(12) Uani 1 1 d . . . . .
C5 C 0.7423(5) 0.1430(3) 0.3444(3) 0.0173(11) Uani 1 1 d . . . . .
C17 C 0.9681(5) 0.1004(3) 0.3450(3) 0.0248(13) Uani 1 1 d . . . . .
H17 H 0.9840 0.0759 0.3019 0.030 Uiso 1 1 calc R . . . .
C16' C 0.2577(5) 0.1619(3) -0.2626(3) 0.0292(14) Uani 1 1 d . . . . .
H16' H 0.3087 0.1763 -0.3031 0.035 Uiso 1 1 calc R . . . .
C23' C -0.2503(5) 0.1864(3) -0.2479(3) 0.0243(13) Uani 1 1 d . . . . .
H23' H -0.3067 0.2169 -0.2101 0.029 Uiso 1 1 calc R . . . .
C20' C -0.0900(6) 0.0971(3) -0.3571(3) 0.0281(14) Uani 1 1 d . . . . .
H20' H -0.0344 0.0664 -0.3948 0.034 Uiso 1 1 calc R . . . .
C7' C -0.2027(5) 0.1734(3) -0.0595(3) 0.0254(13) Uani 1 1 d . . . . .
H7' H -0.2126 0.2250 -0.0518 0.031 Uiso 1 1 calc R . . . .
C34' C -0.2759(6) 0.3637(3) -0.3049(3) 0.0238(13) Uani 1 1 d . . . . .
C15 C 1.0440(5) 0.1258(3) 0.4379(3) 0.0310(15) Uani 1 1 d . . . . .
H15 H 1.1098 0.1194 0.4590 0.037 Uiso 1 1 calc R . . . .
C10 C 0.8671(5) 0.0816(3) 0.1532(3) 0.0301(14) Uani 1 1 d . . . . .
H10 H 0.8832 0.0385 0.1251 0.036 Uiso 1 1 calc R . . . .
C9' C -0.2312(6) 0.0561(4) -0.0147(3) 0.0391(17) Uani 1 1 d . . . . .
H9' H -0.2580 0.0267 0.0231 0.047 Uiso 1 1 calc R . . . .
C8' C -0.2451(5) 0.1305(4) -0.0049(3) 0.0338(16) Uani 1 1 d . . . . .
H8' H -0.2840 0.1531 0.0396 0.041 Uiso 1 1 calc R . . . .
C35 C 0.5711(5) 0.3338(3) 0.2277(3) 0.0242(13) Uani 1 1 d . . . . .
C17' C 0.1328(5) 0.1802(3) -0.2549(3) 0.0258(13) Uani 1 1 d . . . . .
H17' H 0.0988 0.2073 -0.2901 0.031 Uiso 1 1 calc R . . . .
C22 C 0.5494(5) 0.0049(3) 0.3711(3) 0.0279(14) Uani 1 1 d . . . . .
H22 H 0.4850 -0.0021 0.3540 0.034 Uiso 1 1 calc R . . . .
C13 C 0.8317(5) 0.1770(3) 0.4394(3) 0.0225(12) Uani 1 1 d . . . . .
H13 H 0.7518 0.2068 0.4624 0.027 Uiso 1 1 calc R . . . .
C14' C 0.2336(5) 0.1034(3) -0.1533(3) 0.0276(14) Uani 1 1 d . . . . .
H14' H 0.2682 0.0773 -0.1179 0.033 Uiso 1 1 calc R . . . .
C21 C 0.5896(6) -0.0418(3) 0.4210(3) 0.0318(15) Uani 1 1 d . . . . .
H21 H 0.5544 -0.0813 0.4383 0.038 Uiso 1 1 calc R . . . .
C19 C 0.7339(5) 0.0277(3) 0.4206(3) 0.0244(13) Uani 1 1 d . . . . .
H19 H 0.7976 0.0348 0.4382 0.029 Uiso 1 1 calc R . . . .
C16 C 1.0643(6) 0.0928(3) 0.3754(3) 0.0321(15) Uani 1 1 d . . . . .
H16 H 1.1450 0.0642 0.3523 0.039 Uiso 1 1 calc R . . . .
C8 C 0.8695(6) 0.2079(3) 0.1650(3) 0.0322(15) Uani 1 1 d . . . . .
H8 H 0.8864 0.2525 0.1449 0.039 Uiso 1 1 calc R . . . .
C15' C 0.3099(5) 0.1230(3) -0.2122(3) 0.0296(14) Uani 1 1 d . . . . .
H15' H 0.3963 0.1098 -0.2179 0.036 Uiso 1 1 calc R . . . .
C22' C -0.2941(6) 0.1671(3) -0.2999(3) 0.0307(14) Uani 1 1 d . . . . .
H22' H -0.3794 0.1848 -0.2977 0.037 Uiso 1 1 calc R . . . .
C9 C 0.8937(6) 0.1452(3) 0.1238(3) 0.0340(16) Uani 1 1 d . . . . .
H9 H 0.9283 0.1463 0.0755 0.041 Uiso 1 1 calc R . . . .
C19' C -0.0460(6) 0.1163(3) -0.3051(3) 0.0259(13) Uani 1 1 d . . . . .
H19' H 0.0392 0.0980 -0.3071 0.031 Uiso 1 1 calc R . . . .
C21' C -0.2147(6) 0.1223(3) -0.3548(3) 0.0299(14) Uani 1 1 d . . . . .
H21' H -0.2446 0.1088 -0.3905 0.036 Uiso 1 1 calc R . . . .
C10' C -0.1780(6) 0.0240(4) -0.0799(3) 0.0346(15) Uani 1 1 d . . . . .
H10' H -0.1708 -0.0273 -0.0876 0.041 Uiso 1 1 calc R . . . .
C4' C -0.0429(5) 0.4357(3) -0.0875(3) 0.0294(14) Uani 1 1 d . . . . .
O5 O 0.9307(3) 0.3433(2) 0.31052(19) 0.0260(9) Uani 1 1 d . . . . .
O4 O 0.8427(4) 0.3496(2) 0.4491(2) 0.0278(9) Uani 1 1 d . . . . .
O6 O 0.7242(3) 0.4470(2) 0.29553(18) 0.0231(9) Uani 1 1 d . . . . .
O3 O 0.6353(4) 0.4517(2) 0.43478(19) 0.0263(9) Uani 1 1 d . . . . .
C29 C 0.8390(5) 0.4402(3) 0.2450(3) 0.0238(13) Uani 1 1 d . . . . .
H29A H 0.8399 0.4897 0.2241 0.029 Uiso 1 1 calc R . . . .
H29B H 0.8485 0.4045 0.2078 0.029 Uiso 1 1 calc R . . . .
C28 C 0.9436(5) 0.4126(3) 0.2788(3) 0.0267(14) Uani 1 1 d . . . . .
H28A H 1.0237 0.4042 0.2441 0.032 Uiso 1 1 calc R . . . .
H28B H 0.9385 0.4495 0.3139 0.032 Uiso 1 1 calc R . . . .
C31 C 0.5776(5) 0.5106(3) 0.3934(3) 0.0280(14) Uani 1 1 d . . . . .
H31A H 0.5434 0.5585 0.4202 0.034 Uiso 1 1 calc R . . . .
H31B H 0.5090 0.4976 0.3817 0.034 Uiso 1 1 calc R . . . .
C26 C 0.9676(6) 0.3513(4) 0.4226(3) 0.0343(15) Uani 1 1 d . . . . .
H26A H 1.0181 0.3251 0.4540 0.041 Uiso 1 1 calc R . . . .
H26B H 0.9717 0.4038 0.4179 0.041 Uiso 1 1 calc R . . . .
C30 C 0.6693(6) 0.5199(3) 0.3285(3) 0.0285(14) Uani 1 1 d . . . . .
H30A H 0.6281 0.5559 0.2979 0.034 Uiso 1 1 calc R . . . .
H30B H 0.7330 0.5391 0.3393 0.034 Uiso 1 1 calc R . . . .
C24 C 0.7058(6) 0.4741(3) 0.4739(3) 0.0331(15) Uani 1 1 d . . . . .
H24A H 0.6513 0.5104 0.5110 0.040 Uiso 1 1 calc R . . . .
H24B H 0.7657 0.4978 0.4437 0.040 Uiso 1 1 calc R . . . .
C25 C 0.7718(6) 0.4027(3) 0.5040(3) 0.0366(16) Uani 1 1 d . . . . .
H25A H 0.8265 0.4137 0.5296 0.044 Uiso 1 1 calc R . . . .
H25B H 0.7111 0.3815 0.5366 0.044 Uiso 1 1 calc R . . . .
C27 C 1.0136(5) 0.3122(4) 0.3534(3) 0.0380(17) Uani 1 1 d . . . . .
H27A H 1.0961 0.3178 0.3305 0.046 Uiso 1 1 calc R . . . .
H27B H 1.0214 0.2580 0.3595 0.046 Uiso 1 1 calc R . . . .
C12' C 0.0538(5) 0.1596(3) -0.1958(3) 0.0177(12) Uani 1 1 d . . . . .
O8' O -0.2894(4) 0.5074(2) -0.1926(2) 0.0408(12) Uani 1 1 d . . . . .
C13' C 0.1072(5) 0.1215(3) -0.1452(3) 0.0214(12) Uani 1 1 d . . . . .
H13' H 0.0567 0.1075 -0.1043 0.026 Uiso 1 1 calc R . . . .
O12 O 0.2940(7) 0.1194(4) 0.1404(4) 0.092(2) Uani 1 1 d D . . . .
C38 C 0.1853(7) 0.1708(5) 0.1869(4) 0.060(2) Uani 1 1 d . . . . .
H38A H 0.2078 0.1878 0.2263 0.071 Uiso 1 1 calc R . . . .
H38B H 0.1200 0.1456 0.2050 0.071 Uiso 1 1 calc R . . . .
C37 C 0.1414(8) 0.2376(5) 0.1419(5) 0.079(3) Uani 1 1 d . . . . .
H37A H 0.1314 0.2189 0.0997 0.119 Uiso 1 1 calc GR . . . .
H37B H 0.2025 0.2658 0.1296 0.119 Uiso 1 1 calc GR . . . .
H37C H 0.0625 0.2706 0.1676 0.119 Uiso 1 1 calc GR . . . .
Li' Li -0.4394(8) 0.3248(5) -0.1022(5) 0.026(2) Uani 1 1 d . . . . .
Li Li 0.7510(9) 0.3609(5) 0.3718(5) 0.023(2) Uani 1 1 d . . . . .
C39 C 0.3328(11) 0.0586(6) 0.1822(6) 0.105(4) Uani 1 1 d D U . . .
H39A H 0.2698 0.0318 0.2003 0.126 Uiso 1 1 calc R . . . .
H39B H 0.3605 0.0734 0.2206 0.126 Uiso 1 1 calc R . . . .
C40 C 0.4517(10) 0.0095(6) 0.1182(7) 0.114(4) Uani 1 1 d . U . . .
H40A H 0.4291 0.0183 0.0741 0.172 Uiso 1 1 calc GR . . . .
H40B H 0.4696 -0.0442 0.1282 0.172 Uiso 1 1 calc GR . . . .
H40C H 0.5246 0.0262 0.1154 0.172 Uiso 1 1 calc GR . . . .
O3' O -0.5624(3) 0.3863(2) -0.16037(19) 0.0259(9) Uani 1 1 d . . . . .
O5' O -0.4769(4) 0.2831(2) -0.0011(2) 0.0299(10) Uani 1 1 d . . . . .
O6' O -0.5114(3) 0.4257(2) -0.04590(18) 0.0250(9) Uani 1 1 d . . . . .
O4' O -0.5275(4) 0.2428(2) -0.1151(2) 0.0312(10) Uani 1 1 d . . . . .
C24' C -0.6225(6) 0.3376(3) -0.1820(3) 0.0312(14) Uani 1 1 d . . . . .
H24C H -0.5703 0.3111 -0.2256 0.037 Uiso 1 1 calc R . . . .
H24D H -0.7019 0.3678 -0.1903 0.037 Uiso 1 1 calc R . . . .
C30' C -0.5749(5) 0.4823(3) -0.0849(3) 0.0287(14) Uani 1 1 d . . . . .
H30C H -0.5147 0.5023 -0.1193 0.034 Uiso 1 1 calc R . . . .
H30D H -0.6312 0.5243 -0.0537 0.034 Uiso 1 1 calc R . . . .
C29' C -0.5843(5) 0.4138(3) 0.0212(3) 0.0296(14) Uani 1 1 d . . . . .
H29C H -0.6636 0.4075 0.0180 0.036 Uiso 1 1 calc R . . . .
H29D H -0.6014 0.4570 0.0526 0.036 Uiso 1 1 calc R . . . .
C25' C -0.6445(5) 0.2815(3) -0.1270(3) 0.0316(15) Uani 1 1 d . . . . .
H25C H -0.7016 0.3073 -0.0841 0.038 Uiso 1 1 calc R . . . .
H25D H -0.6809 0.2456 -0.1424 0.038 Uiso 1 1 calc R . . . .
C31' C -0.6464(5) 0.4513(3) -0.1208(3) 0.0313(14) Uani 1 1 d . . . . .
H31C H -0.7137 0.4370 -0.0868 0.038 Uiso 1 1 calc R . . . .
H31D H -0.6830 0.4893 -0.1517 0.038 Uiso 1 1 calc R . . . .
C26' C -0.5338(6) 0.1957(4) -0.0569(4) 0.0400(17) Uani 1 1 d . . . . .
H26C H -0.4540 0.1567 -0.0619 0.048 Uiso 1 1 calc R . . . .
H26D H -0.5980 0.1701 -0.0543 0.048 Uiso 1 1 calc R . . . .
C27' C -0.5639(6) 0.2412(4) 0.0089(3) 0.0360(16) Uani 1 1 d . . . . .
H27C H -0.6485 0.2755 0.0181 0.043 Uiso 1 1 calc R . . . .
H27D H -0.5576 0.2075 0.0486 0.043 Uiso 1 1 calc R . . . .
C28' C -0.5092(6) 0.3439(3) 0.0469(3) 0.0327(15) Uani 1 1 d . . . . .
H28C H -0.4334 0.3525 0.0535 0.039 Uiso 1 1 calc R . . . .
H28D H -0.5567 0.3310 0.0921 0.039 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
W 0.01992(13) 0.01948(13) 0.01767(12) 0.00176(9) -0.00548(9) -0.00577(10)
W' 0.02052(13) 0.01873(13) 0.01675(12) 0.00101(9) -0.00453(9) -0.00657(10)
P' 0.0172(7) 0.0181(7) 0.0145(7) -0.0014(5) -0.0023(5) -0.0027(6)
P 0.0166(7) 0.0130(7) 0.0144(6) -0.0010(5) -0.0028(5) -0.0045(6)
O10' 0.029(2) 0.030(2) 0.019(2) -0.0068(18) -0.0029(17) -0.0075(19)
F5 0.0340(19) 0.0307(18) 0.0160(16) -0.0097(13) 0.0006(14) -0.0077(15)
F2 0.0236(18) 0.0300(19) 0.0370(19) 0.0090(16) -0.0028(15) -0.0102(15)
F4 0.0333(19) 0.0243(18) 0.0222(16) 0.0060(14) -0.0074(14) -0.0095(15)
F2' 0.062(3) 0.043(2) 0.0187(17) -0.0093(16) -0.0112(17) -0.0084(19)
O11 0.034(3) 0.036(3) 0.025(2) -0.0066(19) -0.0036(19) -0.010(2)
C35' 0.015(3) 0.024(3) 0.018(3) 0.005(2) -0.006(2) -0.008(2)
F1 0.0248(18) 0.041(2) 0.0258(18) -0.0006(15) -0.0053(15) -0.0035(16)
O1 0.030(2) 0.0125(19) 0.020(2) -0.0026(15) 0.0053(16) -0.0065(17)
C1 0.018(3) 0.013(3) 0.015(3) -0.001(2) -0.005(2) -0.003(2)
C36 0.023(3) 0.022(3) 0.025(3) 0.006(3) -0.007(2) -0.005(2)
C18 0.022(3) 0.017(2) 0.012(2) -0.0068(19) -0.004(2) 0.001(2)
F3 0.0230(18) 0.0286(19) 0.0314(18) -0.0067(15) 0.0020(14) 0.0004(15)
O1' 0.019(2) 0.028(2) 0.027(2) -0.0100(17) -0.0034(17) -0.0044(17)
O2' 0.0179(19) 0.0160(19) 0.0180(19) -0.0028(15) -0.0010(15) -0.0005(16)
O8 0.033(2) 0.044(3) 0.038(3) 0.006(2) -0.004(2) -0.022(2)
F6 0.0240(18) 0.042(2) 0.0234(17) -0.0049(15) -0.0049(14) -0.0151(16)
O2 0.0191(19) 0.0129(18) 0.0176(18) -0.0021(14) -0.0012(15) -0.0073(15)
O10 0.037(3) 0.036(2) 0.034(2) 0.011(2) -0.010(2) -0.021(2)
C1' 0.019(3) 0.019(3) 0.018(3) -0.002(2) -0.005(2) -0.001(2)
F4' 0.034(2) 0.0302(19) 0.0328(19) -0.0126(15) -0.0066(15) -0.0098(16)
C2 0.017(3) 0.017(3) 0.017(3) -0.004(2) -0.001(2) -0.004(2)
O7' 0.048(3) 0.039(3) 0.037(2) 0.014(2) -0.017(2) -0.025(2)
F6' 0.073(3) 0.042(2) 0.0236(19) 0.0004(16) -0.0063(18) -0.035(2)
C2' 0.019(3) 0.022(3) 0.019(3) -0.002(2) -0.005(2) -0.001(2)
C32' 0.029(3) 0.024(3) 0.031(3) 0.001(3) -0.012(3) -0.010(3)
C33 0.026(3) 0.028(3) 0.017(3) -0.001(2) -0.003(2) -0.006(3)
C5' 0.021(3) 0.021(3) 0.013(3) -0.002(2) 0.000(2) -0.004(2)
O9' 0.029(2) 0.044(3) 0.036(2) 0.000(2) -0.010(2) -0.013(2)
C4 0.015(3) 0.029(3) 0.030(3) 0.006(2) 0.006(2) -0.006(2)
O11' 0.027(2) 0.049(3) 0.030(2) 0.000(2) -0.0066(19) -0.023(2)
C6' 0.011(3) 0.025(3) 0.021(3) 0.006(2) -0.008(2) -0.003(2)
C33' 0.034(4) 0.022(3) 0.028(3) 0.005(3) -0.005(3) -0.009(3)
C18' 0.026(3) 0.014(3) 0.017(3) -0.001(2) -0.006(2) -0.005(2)
C20 0.033(4) 0.022(3) 0.036(3) 0.016(3) -0.012(3) -0.011(3)
C3' 0.028(3) 0.012(2) 0.031(3) -0.003(2) -0.011(2) 0.006(2)
O9 0.057(3) 0.033(3) 0.035(3) -0.009(2) -0.021(2) 0.003(2)
O7 0.028(2) 0.048(3) 0.037(3) 0.015(2) -0.018(2) -0.010(2)
C34 0.024(3) 0.016(3) 0.029(3) 0.005(2) -0.013(2) -0.001(2)
C7 0.032(3) 0.019(3) 0.020(3) 0.001(2) -0.004(2) -0.006(3)
C14 0.029(3) 0.028(3) 0.022(3) 0.009(2) -0.013(3) -0.013(3)
C32 0.031(3) 0.023(3) 0.021(3) 0.007(2) 0.000(3) -0.011(3)
C36' 0.030(3) 0.022(3) 0.015(3) -0.004(2) -0.002(2) -0.012(3)
C3 0.025(3) 0.027(3) 0.015(3) -0.002(2) -0.001(2) -0.003(3)
F1' 0.123(4) 0.040(2) 0.024(2) 0.0087(17) -0.018(2) -0.035(2)
C6 0.019(3) 0.013(3) 0.017(3) -0.004(2) -0.002(2) 0.002(2)
F3' 0.085(3) 0.059(3) 0.052(3) -0.019(2) -0.050(3) 0.029(3)
C11 0.026(3) 0.017(3) 0.029(3) -0.002(2) -0.007(3) -0.002(2)
F5' 0.022(2) 0.057(3) 0.081(3) -0.029(2) -0.0080(19) -0.0111(19)
C23 0.031(3) 0.014(3) 0.026(3) 0.002(2) -0.010(3) -0.007(2)
C11' 0.030(3) 0.029(3) 0.023(3) 0.006(3) -0.007(3) -0.011(3)
C12 0.022(3) 0.014(3) 0.020(3) 0.005(2) -0.006(2) -0.006(2)
C5 0.023(3) 0.013(3) 0.015(3) -0.001(2) -0.004(2) -0.005(2)
C17 0.027(3) 0.021(3) 0.028(3) -0.001(2) -0.008(3) -0.009(3)
C16' 0.022(3) 0.028(3) 0.031(3) -0.001(3) 0.001(3) -0.005(3)
C23' 0.027(3) 0.023(3) 0.020(3) -0.002(2) -0.006(2) -0.003(3)
C20' 0.039(4) 0.022(3) 0.021(3) -0.006(2) -0.006(3) -0.004(3)
C7' 0.019(3) 0.028(3) 0.025(3) 0.006(3) -0.005(2) -0.003(3)
C34' 0.029(3) 0.020(3) 0.021(3) 0.000(2) -0.007(3) -0.004(3)
C15 0.023(3) 0.031(3) 0.044(4) 0.016(3) -0.017(3) -0.010(3)
C10 0.035(4) 0.023(3) 0.025(3) -0.005(3) -0.004(3) 0.002(3)
C9' 0.035(4) 0.042(4) 0.037(4) 0.026(3) -0.004(3) -0.015(3)
C8' 0.025(3) 0.049(4) 0.021(3) 0.011(3) -0.003(3) -0.005(3)
C35 0.021(3) 0.026(3) 0.024(3) -0.001(3) -0.009(2) -0.003(3)
C17' 0.023(3) 0.029(3) 0.018(3) 0.002(2) -0.001(2) 0.000(3)
C22 0.028(3) 0.023(3) 0.034(3) -0.004(3) -0.008(3) -0.009(3)
C13 0.023(3) 0.023(3) 0.022(3) 0.005(2) -0.007(2) -0.008(2)
C14' 0.025(3) 0.028(3) 0.031(3) 0.006(3) -0.012(3) -0.006(3)
C21 0.038(4) 0.022(3) 0.036(4) 0.004(3) -0.004(3) -0.015(3)
C19 0.026(3) 0.020(3) 0.027(3) 0.004(2) -0.007(3) -0.006(3)
C16 0.023(3) 0.029(3) 0.043(4) 0.001(3) -0.008(3) -0.007(3)
C8 0.041(4) 0.023(3) 0.023(3) 0.004(3) 0.001(3) -0.003(3)
C15' 0.020(3) 0.025(3) 0.038(4) 0.001(3) -0.003(3) -0.002(3)
C22' 0.032(4) 0.029(3) 0.034(3) -0.004(3) -0.017(3) -0.005(3)
C9 0.038(4) 0.036(4) 0.020(3) -0.003(3) -0.005(3) 0.000(3)
C19' 0.031(3) 0.021(3) 0.022(3) -0.001(2) -0.004(3) -0.004(3)
C21' 0.049(4) 0.022(3) 0.024(3) -0.001(2) -0.018(3) -0.010(3)
C10' 0.031(4) 0.034(4) 0.042(4) 0.011(3) -0.012(3) -0.013(3)
C4' 0.026(3) 0.033(3) 0.029(3) -0.013(3) -0.006(3) -0.005(3)
O5 0.024(2) 0.024(2) 0.028(2) 0.0081(17) -0.0043(17) -0.0074(17)
O4 0.032(2) 0.027(2) 0.032(2) 0.0018(18) -0.0113(19) -0.0173(19)
O6 0.020(2) 0.023(2) 0.024(2) -0.0018(16) -0.0011(16) -0.0063(17)
O3 0.032(2) 0.023(2) 0.023(2) -0.0047(17) -0.0010(17) -0.0114(18)
C29 0.024(3) 0.026(3) 0.018(3) 0.002(2) 0.002(2) -0.009(3)
C28 0.022(3) 0.027(3) 0.032(3) 0.012(3) -0.005(3) -0.011(3)
C31 0.030(3) 0.014(3) 0.034(3) -0.004(2) -0.001(3) -0.003(3)
C26 0.040(4) 0.035(4) 0.040(4) 0.015(3) -0.022(3) -0.021(3)
C30 0.033(3) 0.022(3) 0.027(3) 0.000(2) -0.005(3) -0.004(3)
C24 0.049(4) 0.028(3) 0.025(3) -0.007(3) -0.003(3) -0.018(3)
C25 0.056(4) 0.040(4) 0.023(3) 0.002(3) -0.015(3) -0.024(3)
C27 0.019(3) 0.045(4) 0.046(4) 0.020(3) -0.007(3) -0.008(3)
C12' 0.017(3) 0.011(3) 0.020(3) -0.005(2) 0.000(2) 0.000(2)
O8' 0.049(3) 0.025(2) 0.036(3) -0.002(2) -0.002(2) 0.002(2)
C13' 0.020(3) 0.013(3) 0.024(3) 0.004(2) -0.002(2) 0.003(2)
O12 0.094(5) 0.125(6) 0.091(5) 0.015(5) -0.051(4) -0.060(5)
C38 0.051(5) 0.067(6) 0.055(5) -0.016(4) 0.003(4) -0.020(4)
C37 0.066(6) 0.092(7) 0.080(7) 0.015(6) -0.011(5) -0.031(6)
Li' 0.020(5) 0.030(5) 0.026(5) -0.005(4) -0.005(4) -0.006(4)
Li 0.028(5) 0.025(5) 0.020(5) 0.003(4) -0.006(4) -0.014(4)
C39 0.113(7) 0.107(7) 0.125(7) 0.010(6) -0.073(6) -0.040(6)
C40 0.091(8) 0.076(7) 0.180(11) -0.025(7) -0.066(8) 0.004(6)
O3' 0.024(2) 0.029(2) 0.027(2) -0.0069(17) -0.0081(17) -0.0074(18)
O5' 0.029(2) 0.030(2) 0.028(2) -0.0002(18) -0.0016(18) -0.0075(19)
O6' 0.022(2) 0.028(2) 0.022(2) -0.0031(17) -0.0027(16) -0.0031(18)
O4' 0.026(2) 0.025(2) 0.040(2) -0.0034(19) -0.0086(19) -0.0014(18)
C24' 0.028(3) 0.037(4) 0.029(3) -0.007(3) -0.012(3) -0.005(3)
C30' 0.029(3) 0.022(3) 0.033(3) -0.004(3) -0.006(3) -0.004(3)
C29' 0.029(3) 0.034(3) 0.024(3) -0.004(3) -0.003(3) -0.007(3)
C25' 0.018(3) 0.031(3) 0.048(4) -0.008(3) -0.011(3) -0.006(3)
C31' 0.024(3) 0.035(4) 0.035(4) -0.004(3) -0.012(3) -0.004(3)
C26' 0.038(4) 0.028(4) 0.058(5) 0.003(3) -0.015(3) -0.013(3)
C27' 0.033(4) 0.031(4) 0.043(4) 0.015(3) -0.006(3) -0.013(3)
C28' 0.036(4) 0.039(4) 0.019(3) -0.003(3) -0.003(3) -0.007(3)
_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
W P 2.5761(14) . ?
W C36 2.046(6) . ?
W C33 2.044(6) . ?
W C34 2.031(6) . ?
W C32 1.982(7) . ?
W C35 2.043(6) . ?
W' P' 2.5627(13) . ?
W' C35' 2.037(6) . ?
W' C32' 1.992(6) . ?
W' C33' 2.030(6) . ?
W' C36' 2.037(6) . ?
W' C34' 2.049(6) . ?
P' O2' 1.541(3) . ?
P' C1' 1.901(5) . ?
P' C5' 1.951(5) . ?
P C1 1.891(5) . ?
P O2 1.542(4) . ?
P C5 1.949(5) . ?
O10' C35' 1.146(6) . ?
F5 C4 1.353(6) . ?
F2 C3 1.346(6) . ?
F4 C4 1.330(6) . ?
F2' C3' 1.395(6) . ?
O11 C36 1.143(7) . ?
F1 C3 1.329(6) . ?
O1 H1 0.8400 . ?
O1 C2 1.393(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.559(7) . ?
C18 C23 1.378(8) . ?
C18 C5 1.532(7) . ?
C18 C19 1.414(7) . ?
F3 C3 1.332(6) . ?
O1' H1' 0.8400 . ?
O1' C2' 1.388(6) . ?
O2' Li' 1.845(10) . ?
O8 C33 1.132(6) . ?
F6 C4 1.358(6) . ?
O2 Li 1.848(10) . ?
O10 C35 1.145(6) . ?
C1' H1'A 0.9900 . ?
C1' H1'B 0.9900 . ?
C1' C2' 1.550(7) . ?
F4' C4' 1.332(6) . ?
C2 C4 1.534(8) . ?
C2 C3 1.545(8) . ?
O7' C32' 1.155(6) . ?
F6' C4' 1.322(7) . ?
C2' C3' 1.478(8) . ?
C2' C4' 1.540(8) . ?
C5' C6' 1.550(7) . ?
C5' C18' 1.537(7) . ?
C5' C12' 1.535(7) . ?
O9' C34' 1.151(7) . ?
O11' C36' 1.136(7) . ?
C6' C11' 1.392(8) . ?
C6' C7' 1.378(7) . ?
C33' O8' 1.154(6) . ?
C18' C23' 1.391(8) . ?
C18' C19' 1.401(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(9) . ?
C20 C19 1.383(8) . ?
C3' F1' 1.356(7) . ?
C3' F3' 1.341(7) . ?
O9 C34 1.141(7) . ?
O7 C32 1.160(7) . ?
C7 H7 0.9500 . ?
C7 C6 1.387(7) . ?
C7 C8 1.380(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.373(8) . ?
C14 C13 1.388(8) . ?
C6 C11 1.392(7) . ?
C6 C5 1.530(7) . ?
C11 H11 0.9500 . ?
C11 C10 1.387(8) . ?
F5' C4' 1.341(7) . ?
C23 H23 0.9500 . ?
C23 C22 1.375(8) . ?
C11' H11' 0.9500 . ?
C11' C10' 1.377(8) . ?
C12 C5 1.538(8) . ?
C12 C17 1.398(7) . ?
C12 C13 1.392(7) . ?
C17 H17 0.9500 . ?
C17 C16 1.387(8) . ?
C16' H16' 0.9500 . ?
C16' C17' 1.375(8) . ?
C16' C15' 1.381(8) . ?
C23' H23' 0.9500 . ?
C23' C22' 1.383(8) . ?
C20' H20' 0.9500 . ?
C20' C19' 1.384(8) . ?
C20' C21' 1.391(8) . ?
C7' H7' 0.9500 . ?
C7' C8' 1.390(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.364(9) . ?
C10 H10 0.9500 . ?
C10 C9 1.372(8) . ?
C9' H9' 0.9500 . ?
C9' C8' 1.364(9) . ?
C9' C10' 1.381(9) . ?
C8' H8' 0.9500 . ?
C17' H17' 0.9500 . ?
C17' C12' 1.412(7) . ?
C22 H22 0.9500 . ?
C22 C21 1.375(8) . ?
C13 H13 0.9500 . ?
C14' H14' 0.9500 . ?
C14' C15' 1.385(8) . ?
C14' C13' 1.391(8) . ?
C21 H21 0.9500 . ?
C19 H19 0.9500 . ?
C16 H16 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.387(8) . ?
C15' H15' 0.9500 . ?
C22' H22' 0.9500 . ?
C22' C21' 1.378(8) . ?
C9 H9 0.9500 . ?
C19' H19' 0.9500 . ?
C21' H21' 0.9500 . ?
C10' H10' 0.9500 . ?
O5 C28 1.433(6) . ?
O5 C27 1.442(7) . ?
O5 Li 2.089(10) . ?
O4 C26 1.432(7) . ?
O4 C25 1.432(7) . ?
O4 Li 2.078(10) . ?
O6 C29 1.437(6) . ?
O6 C30 1.437(6) . ?
O6 Li 2.164(10) . ?
O3 C31 1.453(7) . ?
O3 C24 1.432(7) . ?
O3 Li 2.078(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C28 1.505(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C30 1.495(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.498(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.512(8) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C12' C13' 1.387(7) . ?
C13' H13' 0.9500 . ?
O12 C38 1.480(10) . ?
O12 C39 1.409(8) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C37 1.540(11) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
Li' O3' 2.129(10) . ?
Li' O5' 2.113(10) . ?
Li' O6' 2.084(10) . ?
Li' O4' 2.133(10) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.701(15) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
O3' C24' 1.442(7) . ?
O3' C31' 1.441(7) . ?
O5' C27' 1.421(7) . ?
O5' C28' 1.428(7) . ?
O6' C30' 1.426(7) . ?
O6' C29' 1.439(6) . ?
O4' C25' 1.429(7) . ?
O4' C26' 1.419(7) . ?
C24' H24C 0.9900 . ?
C24' H24D 0.9900 . ?
C24' C25' 1.500(8) . ?
C30' H30C 0.9900 . ?
C30' H30D 0.9900 . ?
C30' C31' 1.485(8) . ?
C29' H29C 0.9900 . ?
C29' H29D 0.9900 . ?
C29' C28' 1.495(8) . ?
C25' H25C 0.9900 . ?
C25' H25D 0.9900 . ?
C31' H31C 0.9900 . ?
C31' H31D 0.9900 . ?
C26' H26C 0.9900 . ?
C26' H26D 0.9900 . ?
C26' C27' 1.516(9) . ?
C27' H27C 0.9900 . ?
C27' H27D 0.9900 . ?
C28' H28C 0.9900 . ?
C28' H28D 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
C36 W P 101.76(16) . . ?
C33 W P 88.98(16) . . ?
C33 W C36 89.7(2) . . ?
C34 W P 85.99(16) . . ?
C34 W C36 170.4(2) . . ?
C34 W C33 96.2(2) . . ?
C34 W C35 86.4(2) . . ?
C32 W P 171.67(16) . . ?
C32 W C36 86.5(2) . . ?
C32 W C33 89.7(2) . . ?
C32 W C34 86.0(2) . . ?
C32 W C35 90.2(2) . . ?
C35 W P 91.49(16) . . ?
C35 W C36 87.8(2) . . ?
C35 W C33 177.5(2) . . ?
C35' W' P' 102.98(15) . . ?
C35' W' C36' 91.5(2) . . ?
C35' W' C34' 86.6(2) . . ?
C32' W' P' 169.01(17) . . ?
C32' W' C35' 86.1(2) . . ?
C32' W' C33' 88.2(2) . . ?
C32' W' C36' 86.4(2) . . ?
C32' W' C34' 94.9(2) . . ?
C33' W' P' 83.80(16) . . ?
C33' W' C35' 168.9(2) . . ?
C33' W' C36' 97.6(2) . . ?
C33' W' C34' 84.4(2) . . ?
C36' W' P' 87.17(15) . . ?
C36' W' C34' 177.6(2) . . ?
C34' W' P' 91.79(15) . . ?
O2' P' W' 111.65(14) . . ?
O2' P' C1' 103.1(2) . . ?
O2' P' C5' 108.7(2) . . ?
C1' P' W' 114.07(17) . . ?
C1' P' C5' 98.9(2) . . ?
C5' P' W' 118.80(15) . . ?
C1 P W 113.46(17) . . ?
C1 P C5 100.2(2) . . ?
O2 P W 111.52(14) . . ?
O2 P C1 103.4(2) . . ?
O2 P C5 107.6(2) . . ?
C5 P W 119.13(17) . . ?
O10' C35' W' 173.2(4) . . ?
C2 O1 H1 109.5 . . ?
P C1 H1A 108.1 . . ?
P C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C2 C1 P 116.7(3) . . ?
C2 C1 H1A 108.1 . . ?
C2 C1 H1B 108.1 . . ?
O11 C36 W 173.2(5) . . ?
C23 C18 C5 121.6(5) . . ?
C23 C18 C19 116.8(5) . . ?
C19 C18 C5 121.6(5) . . ?
C2' O1' H1' 109.5 . . ?
P' O2' Li' 160.7(4) . . ?
P O2 Li 160.5(4) . . ?
P' C1' H1'A 107.9 . . ?
P' C1' H1'B 107.9 . . ?
H1'A C1' H1'B 107.2 . . ?
C2' C1' P' 117.5(4) . . ?
C2' C1' H1'A 107.9 . . ?
C2' C1' H1'B 107.9 . . ?
O1 C2 C1 116.7(4) . . ?
O1 C2 C4 106.8(4) . . ?
O1 C2 C3 105.4(4) . . ?
C4 C2 C1 109.1(4) . . ?
C4 C2 C3 108.2(4) . . ?
C3 C2 C1 110.2(4) . . ?
O1' C2' C1' 116.9(5) . . ?
O1' C2' C3' 106.9(4) . . ?
O1' C2' C4' 106.0(4) . . ?
C3' C2' C1' 106.3(4) . . ?
C3' C2' C4' 108.5(5) . . ?
C4' C2' C1' 111.9(4) . . ?
O7' C32' W' 175.3(5) . . ?
O8 C33 W 177.2(5) . . ?
C6' C5' P' 114.4(3) . . ?
C18' C5' P' 106.2(3) . . ?
C18' C5' C6' 106.1(4) . . ?
C12' C5' P' 106.3(4) . . ?
C12' C5' C6' 108.9(4) . . ?
C12' C5' C18' 115.1(4) . . ?
F5 C4 F6 104.7(5) . . ?
F5 C4 C2 113.3(4) . . ?
F4 C4 F5 106.8(4) . . ?
F4 C4 F6 106.4(4) . . ?
F4 C4 C2 115.5(5) . . ?
F6 C4 C2 109.5(4) . . ?
C11' C6' C5' 117.2(5) . . ?
C7' C6' C5' 125.5(5) . . ?
C7' C6' C11' 117.2(5) . . ?
O8' C33' W' 172.9(6) . . ?
C23' C18' C5' 118.4(5) . . ?
C23' C18' C19' 117.5(5) . . ?
C19' C18' C5' 123.9(5) . . ?
C21 C20 H20 119.3 . . ?
C21 C20 C19 121.5(5) . . ?
C19 C20 H20 119.3 . . ?
F2' C3' C2' 114.6(4) . . ?
F1' C3' F2' 102.3(4) . . ?
F1' C3' C2' 111.8(5) . . ?
F3' C3' F2' 103.3(5) . . ?
F3' C3' C2' 117.2(5) . . ?
F3' C3' F1' 106.1(5) . . ?
O9 C34 W 172.8(5) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C8 C7 C6 121.5(5) . . ?
C15 C14 H14 120.0 . . ?
C15 C14 C13 120.0(6) . . ?
C13 C14 H14 120.0 . . ?
O7 C32 W 178.4(5) . . ?
O11' C36' W' 178.7(5) . . ?
F2 C3 C2 111.3(4) . . ?
F1 C3 F2 106.9(5) . . ?
F1 C3 F3 107.1(4) . . ?
F1 C3 C2 111.4(4) . . ?
F3 C3 F2 107.1(4) . . ?
F3 C3 C2 112.8(5) . . ?
C7 C6 C11 117.7(5) . . ?
C7 C6 C5 118.3(5) . . ?
C11 C6 C5 123.7(5) . . ?
C6 C11 H11 119.5 . . ?
C10 C11 C6 121.0(5) . . ?
C10 C11 H11 119.5 . . ?
C18 C23 H23 118.9 . . ?
C22 C23 C18 122.2(5) . . ?
C22 C23 H23 118.9 . . ?
C6' C11' H11' 119.0 . . ?
C10' C11' C6' 122.0(6) . . ?
C10' C11' H11' 119.0 . . ?
C17 C12 C5 119.7(5) . . ?
C13 C12 C5 124.0(5) . . ?
C13 C12 C17 115.9(5) . . ?
C18 C5 P 106.8(3) . . ?
C18 C5 C12 110.9(4) . . ?
C6 C5 P 105.7(3) . . ?
C6 C5 C18 112.2(4) . . ?
C6 C5 C12 107.8(4) . . ?
C12 C5 P 113.4(3) . . ?
C12 C17 H17 119.1 . . ?
C16 C17 C12 121.7(5) . . ?
C16 C17 H17 119.1 . . ?
C17' C16' H16' 119.6 . . ?
C17' C16' C15' 120.7(5) . . ?
C15' C16' H16' 119.6 . . ?
C18' C23' H23' 119.2 . . ?
C22' C23' C18' 121.6(5) . . ?
C22' C23' H23' 119.2 . . ?
C19' C20' H20' 119.6 . . ?
C19' C20' C21' 120.8(5) . . ?
C21' C20' H20' 119.6 . . ?
C6' C7' H7' 119.4 . . ?
C6' C7' C8' 121.2(6) . . ?
C8' C7' H7' 119.4 . . ?
O9' C34' W' 178.3(5) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.4(6) . . ?
C16 C15 H15 120.3 . . ?
C11 C10 H10 119.9 . . ?
C9 C10 C11 120.3(6) . . ?
C9 C10 H10 119.9 . . ?
C8' C9' H9' 120.2 . . ?
C8' C9' C10' 119.6(5) . . ?
C10' C9' H9' 120.2 . . ?
C7' C8' H8' 119.8 . . ?
C9' C8' C7' 120.4(6) . . ?
C9' C8' H8' 119.8 . . ?
O10 C35 W 176.8(5) . . ?
C16' C17' H17' 119.3 . . ?
C16' C17' C12' 121.5(5) . . ?
C12' C17' H17' 119.3 . . ?
C23 C22 H22 119.6 . . ?
C23 C22 C21 120.9(6) . . ?
C21 C22 H22 119.6 . . ?
C14 C13 C12 122.3(5) . . ?
C14 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C15' C14' H14' 119.5 . . ?
C15' C14' C13' 121.0(5) . . ?
C13' C14' H14' 119.5 . . ?
C20 C21 H21 120.9 . . ?
C22 C21 C20 118.2(5) . . ?
C22 C21 H21 120.9 . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.4(6) . . ?
C20 C19 H19 119.8 . . ?
C17 C16 H16 119.7 . . ?
C15 C16 C17 120.6(6) . . ?
C15 C16 H16 119.7 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.9(6) . . ?
C9 C8 H8 120.1 . . ?
C16' C15' C14' 118.7(5) . . ?
C16' C15' H15' 120.7 . . ?
C14' C15' H15' 120.7 . . ?
C23' C22' H22' 119.8 . . ?
C21' C22' C23' 120.5(6) . . ?
C21' C22' H22' 119.8 . . ?
C10 C9 C8 119.6(5) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C18' C19' H19' 119.7 . . ?
C20' C19' C18' 120.7(6) . . ?
C20' C19' H19' 119.7 . . ?
C20' C21' H21' 120.6 . . ?
C22' C21' C20' 118.8(6) . . ?
C22' C21' H21' 120.6 . . ?
C11' C10' C9' 119.5(6) . . ?
C11' C10' H10' 120.2 . . ?
C9' C10' H10' 120.2 . . ?
F4' C4' C2' 113.0(5) . . ?
F4' C4' F5' 106.7(5) . . ?
F6' C4' F4' 106.8(5) . . ?
F6' C4' C2' 111.2(5) . . ?
F6' C4' F5' 106.1(5) . . ?
F5' C4' C2' 112.5(5) . . ?
C28 O5 C27 114.3(4) . . ?
C28 O5 Li 109.0(4) . . ?
C27 O5 Li 107.9(4) . . ?
C26 O4 Li 112.1(4) . . ?
C25 O4 C26 114.7(5) . . ?
C25 O4 Li 109.8(4) . . ?
C29 O6 C30 114.0(4) . . ?
C29 O6 Li 109.2(4) . . ?
C30 O6 Li 110.4(4) . . ?
C31 O3 Li 109.9(4) . . ?
C24 O3 C31 114.6(4) . . ?
C24 O3 Li 107.9(4) . . ?
O6 C29 H29A 109.7 . . ?
O6 C29 H29B 109.7 . . ?
O6 C29 C28 109.6(4) . . ?
H29A C29 H29B 108.2 . . ?
C28 C29 H29A 109.7 . . ?
C28 C29 H29B 109.7 . . ?
O5 C28 C29 105.6(4) . . ?
O5 C28 H28A 110.6 . . ?
O5 C28 H28B 110.6 . . ?
C29 C28 H28A 110.6 . . ?
C29 C28 H28B 110.6 . . ?
H28A C28 H28B 108.7 . . ?
O3 C31 H31A 109.6 . . ?
O3 C31 H31B 109.6 . . ?
O3 C31 C30 110.4(5) . . ?
H31A C31 H31B 108.1 . . ?
C30 C31 H31A 109.6 . . ?
C30 C31 H31B 109.6 . . ?
O4 C26 H26A 110.4 . . ?
O4 C26 H26B 110.4 . . ?
O4 C26 C27 106.8(5) . . ?
H26A C26 H26B 108.6 . . ?
C27 C26 H26A 110.4 . . ?
C27 C26 H26B 110.4 . . ?
O6 C30 C31 106.8(4) . . ?
O6 C30 H30A 110.4 . . ?
O6 C30 H30B 110.4 . . ?
C31 C30 H30A 110.4 . . ?
C31 C30 H30B 110.4 . . ?
H30A C30 H30B 108.6 . . ?
O3 C24 H24A 110.6 . . ?
O3 C24 H24B 110.6 . . ?
O3 C24 C25 105.6(5) . . ?
H24A C24 H24B 108.8 . . ?
C25 C24 H24A 110.6 . . ?
C25 C24 H24B 110.6 . . ?
O4 C25 C24 109.1(5) . . ?
O4 C25 H25A 109.9 . . ?
O4 C25 H25B 109.9 . . ?
C24 C25 H25A 109.9 . . ?
C24 C25 H25B 109.9 . . ?
H25A C25 H25B 108.3 . . ?
O5 C27 C26 110.7(5) . . ?
O5 C27 H27A 109.5 . . ?
O5 C27 H27B 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C17' C12' C5' 120.2(5) . . ?
C13' C12' C5' 122.5(5) . . ?
C13' C12' C17' 117.2(5) . . ?
C14' C13' H13' 119.5 . . ?
C12' C13' C14' 121.0(5) . . ?
C12' C13' H13' 119.5 . . ?
C39 O12 C38 104.4(8) . . ?
O12 C38 H38A 110.7 . . ?
O12 C38 H38B 110.7 . . ?
O12 C38 C37 105.1(7) . . ?
H38A C38 H38B 108.8 . . ?
C37 C38 H38A 110.7 . . ?
C37 C38 H38B 110.7 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O2' Li' O3' 118.6(5) . . ?
O2' Li' O5' 110.6(5) . . ?
O2' Li' O6' 104.1(5) . . ?
O2' Li' O4' 126.0(5) . . ?
O3' Li' O4' 79.3(4) . . ?
O5' Li' O3' 130.0(5) . . ?
O5' Li' O4' 79.1(4) . . ?
O6' Li' O3' 80.0(4) . . ?
O6' Li' O5' 80.2(4) . . ?
O6' Li' O4' 129.7(5) . . ?
O2 Li O5 127.5(5) . . ?
O2 Li O4 112.8(5) . . ?
O2 Li O6 115.2(5) . . ?
O2 Li O3 101.9(4) . . ?
O5 Li O6 78.9(3) . . ?
O4 Li O5 80.8(4) . . ?
O4 Li O6 130.7(5) . . ?
O3 Li O5 130.6(5) . . ?
O3 Li O4 80.7(4) . . ?
O3 Li O6 79.5(3) . . ?
O12 C39 H39A 112.8 . . ?
O12 C39 H39B 112.8 . . ?
O12 C39 C40 94.9(8) . . ?
H39A C39 H39B 110.2 . . ?
C40 C39 H39A 112.8 . . ?
C40 C39 H39B 112.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C24' O3' Li' 109.9(4) . . ?
C31' O3' Li' 109.5(4) . . ?
C31' O3' C24' 113.8(4) . . ?
C27' O5' Li' 112.0(4) . . ?
C27' O5' C28' 114.9(5) . . ?
C28' O5' Li' 108.6(4) . . ?
C30' O6' Li' 109.6(4) . . ?
C30' O6' C29' 114.8(4) . . ?
C29' O6' Li' 109.5(4) . . ?
C25' O4' Li' 108.1(4) . . ?
C26' O4' Li' 109.4(4) . . ?
C26' O4' C25' 114.1(5) . . ?
O3' C24' H24C 109.8 . . ?
O3' C24' H24D 109.8 . . ?
O3' C24' C25' 109.5(5) . . ?
H24C C24' H24D 108.2 . . ?
C25' C24' H24C 109.8 . . ?
C25' C24' H24D 109.8 . . ?
O6' C30' H30C 109.5 . . ?
O6' C30' H30D 109.5 . . ?
O6' C30' C31' 110.6(5) . . ?
H30C C30' H30D 108.1 . . ?
C31' C30' H30C 109.5 . . ?
C31' C30' H30D 109.5 . . ?
O6' C29' H29C 110.6 . . ?
O6' C29' H29D 110.6 . . ?
O6' C29' C28' 105.7(4) . . ?
H29C C29' H29D 108.7 . . ?
C28' C29' H29C 110.6 . . ?
C28' C29' H29D 110.6 . . ?
O4' C25' C24' 106.8(5) . . ?
O4' C25' H25C 110.4 . . ?
O4' C25' H25D 110.4 . . ?
C24' C25' H25C 110.4 . . ?
C24' C25' H25D 110.4 . . ?
H25C C25' H25D 108.6 . . ?
O3' C31' C30' 107.3(5) . . ?
O3' C31' H31C 110.3 . . ?
O3' C31' H31D 110.3 . . ?
C30' C31' H31C 110.3 . . ?
C30' C31' H31D 110.3 . . ?
H31C C31' H31D 108.5 . . ?
O4' C26' H26C 109.5 . . ?
O4' C26' H26D 109.5 . . ?
O4' C26' C27' 110.6(5) . . ?
H26C C26' H26D 108.1 . . ?
C27' C26' H26C 109.5 . . ?
C27' C26' H26D 109.5 . . ?
O5' C27' C26' 106.8(5) . . ?
O5' C27' H27C 110.4 . . ?
O5' C27' H27D 110.4 . . ?
C26' C27' H27C 110.4 . . ?
C26' C27' H27D 110.4 . . ?
H27C C27' H27D 108.6 . . ?
O5' C28' C29' 110.4(5) . . ?
O5' C28' H28C 109.6 . . ?
O5' C28' H28D 109.6 . . ?
C29' C28' H28C 109.6 . . ?
C29' C28' H28D 109.6 . . ?
H28C C28' H28D 108.1 . . ?
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
W P C1 C2 -84.2(4) . . . . ?
W P O2 Li -85.7(11) . . . . ?
W' P' O2' Li' 82.3(12) . . . . ?
P' O2' Li' O3' -72.5(13) . . . . ?
P' O2' Li' O5' 116.6(10) . . . . ?
P' O2' Li' O6' -158.7(9) . . . . ?
P' O2' Li' O4' 25.3(16) . . . . ?
P' C1' C2' O1' 15.8(6) . . . . ?
P' C1' C2' C3' 135.0(4) . . . . ?
P' C1' C2' C4' -106.7(5) . . . . ?
P' C5' C6' C11' 164.6(4) . . . . ?
P' C5' C6' C7' -20.3(7) . . . . ?
P' C5' C18' C23' -58.2(5) . . . . ?
P' C5' C18' C19' 126.8(5) . . . . ?
P' C5' C12' C17' -65.1(5) . . . . ?
P' C5' C12' C13' 111.5(5) . . . . ?
P C1 C2 O1 -5.6(6) . . . . ?
P C1 C2 C4 -126.8(4) . . . . ?
P C1 C2 C3 114.5(4) . . . . ?
P O2 Li O5 -18.3(16) . . . . ?
P O2 Li O4 -114.2(10) . . . . ?
P O2 Li O6 77.0(12) . . . . ?
P O2 Li O3 160.9(9) . . . . ?
O1 C2 C4 F5 62.7(5) . . . . ?
O1 C2 C4 F4 -173.7(4) . . . . ?
O1 C2 C4 F6 -53.7(5) . . . . ?
O1 C2 C3 F2 -167.5(4) . . . . ?
O1 C2 C3 F1 73.4(5) . . . . ?
O1 C2 C3 F3 -47.1(6) . . . . ?
C1 P O2 Li 152.1(11) . . . . ?
C1 C2 C4 F5 -170.3(4) . . . . ?
C1 C2 C4 F4 -46.7(6) . . . . ?
C1 C2 C4 F6 73.3(5) . . . . ?
C1 C2 C3 F2 65.7(5) . . . . ?
C1 C2 C3 F1 -53.4(6) . . . . ?
C1 C2 C3 F3 -173.9(4) . . . . ?
C18 C23 C22 C21 -1.7(9) . . . . ?
O1' C2' C3' F2' -58.9(6) . . . . ?
O1' C2' C3' F1' 56.9(6) . . . . ?
O1' C2' C3' F3' 179.7(5) . . . . ?
O1' C2' C4' F4' 50.2(6) . . . . ?
O1' C2' C4' F6' -69.9(5) . . . . ?
O1' C2' C4' F5' 171.2(4) . . . . ?
O2 P C1 C2 36.7(4) . . . . ?
C1' P' O2' Li' -154.8(11) . . . . ?
C1' C2' C3' F2' 175.5(5) . . . . ?
C1' C2' C3' F1' -68.6(6) . . . . ?
C1' C2' C3' F3' 54.2(7) . . . . ?
C1' C2' C4' F4' 178.8(4) . . . . ?
C1' C2' C4' F6' 58.6(6) . . . . ?
C1' C2' C4' F5' -60.3(6) . . . . ?
C5' P' O2' Li' -50.6(12) . . . . ?
C5' C6' C11' C10' 175.1(5) . . . . ?
C5' C6' C7' C8' -174.3(5) . . . . ?
C5' C18' C23' C22' -176.7(5) . . . . ?
C5' C18' C19' C20' 176.5(5) . . . . ?
C5' C12' C13' C14' -177.9(5) . . . . ?
C4 C2 C3 F2 -53.5(6) . . . . ?
C4 C2 C3 F1 -172.6(4) . . . . ?
C4 C2 C3 F3 66.9(6) . . . . ?
C6' C5' C18' C23' 64.0(6) . . . . ?
C6' C5' C18' C19' -111.0(5) . . . . ?
C6' C5' C12' C17' 171.1(5) . . . . ?
C6' C5' C12' C13' -12.2(7) . . . . ?
C6' C11' C10' C9' -1.1(9) . . . . ?
C6' C7' C8' C9' 0.4(9) . . . . ?
C18' C5' C6' C11' 47.9(6) . . . . ?
C18' C5' C6' C7' -137.0(5) . . . . ?
C18' C5' C12' C17' 52.1(7) . . . . ?
C18' C5' C12' C13' -131.2(5) . . . . ?
C18' C23' C22' C21' 0.8(9) . . . . ?
C3' C2' C4' F4' -64.3(6) . . . . ?
C3' C2' C4' F6' 175.6(4) . . . . ?
C3' C2' C4' F5' 56.7(6) . . . . ?
C7 C6 C11 C10 -2.4(8) . . . . ?
C7 C6 C5 P 54.2(6) . . . . ?
C7 C6 C5 C18 170.2(5) . . . . ?
C7 C6 C5 C12 -67.4(6) . . . . ?
C7 C8 C9 C10 1.0(10) . . . . ?
C14 C15 C16 C17 -1.6(9) . . . . ?
C3 C2 C4 F5 -50.3(6) . . . . ?
C3 C2 C4 F4 73.3(5) . . . . ?
C3 C2 C4 F6 -166.7(4) . . . . ?
C6 C7 C8 C9 -2.6(9) . . . . ?
C6 C11 C10 C9 0.9(9) . . . . ?
C11 C6 C5 P -131.9(5) . . . . ?
C11 C6 C5 C18 -15.9(7) . . . . ?
C11 C6 C5 C12 106.5(6) . . . . ?
C11 C10 C9 C8 -0.2(10) . . . . ?
C23 C18 C5 P 59.2(5) . . . . ?
C23 C18 C5 C6 -56.3(6) . . . . ?
C23 C18 C5 C12 -176.8(5) . . . . ?
C23 C18 C19 C20 -0.9(8) . . . . ?
C23 C22 C21 C20 0.6(9) . . . . ?
C11' C6' C7' C8' 0.8(8) . . . . ?
C12 C17 C16 C15 1.4(9) . . . . ?
C5 P C1 C2 147.7(4) . . . . ?
C5 P O2 Li 46.7(12) . . . . ?
C5 C18 C23 C22 -175.3(5) . . . . ?
C5 C18 C19 C20 176.2(5) . . . . ?
C5 C6 C11 C10 -176.3(5) . . . . ?
C5 C12 C17 C16 -173.4(5) . . . . ?
C5 C12 C13 C14 172.3(5) . . . . ?
C17 C12 C5 P -155.3(4) . . . . ?
C17 C12 C5 C18 84.6(6) . . . . ?
C17 C12 C5 C6 -38.6(6) . . . . ?
C17 C12 C13 C14 -0.3(8) . . . . ?
C16' C17' C12' C5' 178.1(5) . . . . ?
C16' C17' C12' C13' 1.3(8) . . . . ?
C23' C18' C19' C20' 1.5(8) . . . . ?
C23' C22' C21' C20' -0.2(9) . . . . ?
C7' C6' C11' C10' -0.4(9) . . . . ?
C15 C14 C13 C12 0.1(8) . . . . ?
C8' C9' C10' C11' 2.4(10) . . . . ?
C17' C16' C15' C14' -0.8(9) . . . . ?
C17' C12' C13' C14' -1.1(8) . . . . ?
C13 C14 C15 C16 0.9(8) . . . . ?
C13 C12 C5 P 32.4(6) . . . . ?
C13 C12 C5 C18 -87.7(6) . . . . ?
C13 C12 C5 C6 149.1(5) . . . . ?
C13 C12 C17 C16 -0.4(8) . . . . ?
C21 C20 C19 C18 -0.2(9) . . . . ?
C19 C18 C23 C22 1.8(8) . . . . ?
C19 C18 C5 P -117.8(5) . . . . ?
C19 C18 C5 C6 126.8(5) . . . . ?
C19 C18 C5 C12 6.2(7) . . . . ?
C19 C20 C21 C22 0.3(9) . . . . ?
C8 C7 C6 C11 3.2(9) . . . . ?
C8 C7 C6 C5 177.5(5) . . . . ?
C15' C16' C17' C12' -0.4(9) . . . . ?
C15' C14' C13' C12' 0.0(9) . . . . ?
C19' C18' C23' C22' -1.4(8) . . . . ?
C19' C20' C21' C22' 0.3(9) . . . . ?
C21' C20' C19' C18' -1.0(8) . . . . ?
C10' C9' C8' C7' -2.0(10) . . . . ?
C4' C2' C3' F2' 55.0(6) . . . . ?
C4' C2' C3' F1' 170.9(4) . . . . ?
C4' C2' C3' F3' -66.4(6) . . . . ?
O4 C26 C27 O5 51.9(6) . . . . ?
O6 C29 C28 O5 56.3(6) . . . . ?
O3 C31 C30 O6 53.6(6) . . . . ?
O3 C24 C25 O4 56.2(6) . . . . ?
C29 O6 C30 C31 -161.6(5) . . . . ?
C28 O5 C27 C26 79.5(6) . . . . ?
C31 O3 C24 C25 -171.9(4) . . . . ?
C26 O4 C25 C24 92.6(6) . . . . ?
C30 O6 C29 C28 91.1(6) . . . . ?
C24 O3 C31 C30 79.3(6) . . . . ?
C25 O4 C26 C27 -162.0(5) . . . . ?
C27 O5 C28 C29 -172.5(4) . . . . ?
C12' C5' C6' C11' -76.6(6) . . . . ?
C12' C5' C6' C7' 98.5(6) . . . . ?
C12' C5' C18' C23' -175.5(5) . . . . ?
C12' C5' C18' C19' 9.5(7) . . . . ?
C13' C14' C15' C16' 1.0(9) . . . . ?
C38 O12 C39 C40 178.9(7) . . . . ?
Li' O3' C24' C25' 35.0(6) . . . . ?
Li' O3' C31' C30' 39.6(6) . . . . ?
Li' O5' C27' C26' 39.3(6) . . . . ?
Li' O5' C28' C29' 37.6(6) . . . . ?
Li' O6' C30' C31' 40.6(6) . . . . ?
Li' O6' C29' C28' 45.7(6) . . . . ?
Li' O4' C25' C24' 48.7(6) . . . . ?
Li' O4' C26' C27' 39.6(6) . . . . ?
Li O5 C28 C29 -51.7(5) . . . . ?
Li O5 C27 C26 -41.9(6) . . . . ?
Li O4 C26 C27 -35.9(6) . . . . ?
Li O4 C25 C24 -34.7(6) . . . . ?
Li O6 C29 C28 -32.9(6) . . . . ?
Li O6 C30 C31 -38.2(6) . . . . ?
Li O3 C31 C30 -42.3(6) . . . . ?
Li O3 C24 C25 -49.1(5) . . . . ?
C39 O12 C38 C37 -179.9(8) . . . . ?
O3' C24' C25' O4' -56.4(6) . . . . ?
O6' C30' C31' O3' -53.9(6) . . . . ?
O6' C29' C28' O5' -55.9(6) . . . . ?
O4' C26' C27' O5' -52.7(7) . . . . ?
C24' O3' C31' C30' 163.0(5) . . . . ?
C30' O6' C29' C28' 169.5(5) . . . . ?
C29' O6' C30' C31' -83.2(6) . . . . ?
C25' O4' C26' C27' -81.6(6) . . . . ?
C31' O3' C24' C25' -88.2(6) . . . . ?
C26' O4' C25' C24' 170.6(5) . . . . ?
C27' O5' C28' C29' -88.7(6) . . . . ?
C28' O5' C27' C26' 163.9(5) . . . . ?
_iucr_refine_instructions_details
;
4012f.res created by SHELXL-2014/7
TITL 4012f in P-1 #2
REM reset to P-1 #2
CELL 0.71073 11.7408 18.5934 20.0735 86.7216 74.8723 73.209
ZERR 2 0.0005 0.0008 0.0008 0.0026 0.0024 0.0026
LATT 1
SFAC C H F Li O P W
UNIT 152 156 24 4 46 4 4
DFIX 1.49 0.01 O12 C39
DELU 0.005 0.005 F5 C4
DELU 0.005 0.005 F1' C3'
ISOR 0.01 0.02 C40 C39
ISOR 0.005 0.01 C18 C3'
L.S. 10 0 0
PLAN 10
SIZE 0.04 0.08 0.1
TEMP -173.15
BOND
MORE -1
BOND $H
CONF
fmap 2 53
acta 52
OMIT -2 56
OMIT 0 2 0
OMIT 0 0 1
OMIT 1 1 1
OMIT 0 1 0
OMIT 0 1 1
OMIT 1 0 1
OMIT 0 -1 1
OMIT 0 1 2
OMIT 1 1 0
OMIT 0 -2 1
OMIT -1 1 1
OMIT 0 2 2
REM
REM
REM
WGHT 0.067400
FVAR 0.06497
W 7 0.460390 0.274153 0.285889 11.00000 0.01992 0.01948 =
0.01767 0.00176 -0.00548 -0.00577
W' 7 -0.112505 0.369122 -0.289798 11.00000 0.02052 0.01873 =
0.01675 0.00101 -0.00453 -0.00657
P' 6 -0.140388 0.292271 -0.179667 11.00000 0.01719 0.01809 =
0.01447 -0.00139 -0.00234 -0.00270
P 6 0.603112 0.232987 0.367627 11.00000 0.01659 0.01301 =
0.01442 -0.00102 -0.00278 -0.00447
O10' 5 0.016248 0.248841 -0.412658 11.00000 0.02899 0.03017 =
0.01891 -0.00677 -0.00292 -0.00748
F5 3 0.428783 0.306438 0.628184 11.00000 0.03400 0.03073 =
0.01601 -0.00972 0.00060 -0.00772
F2 3 0.286017 0.224475 0.562564 11.00000 0.02364 0.02998 =
0.03705 0.00903 -0.00283 -0.01022
F4 3 0.503266 0.188973 0.599855 11.00000 0.03330 0.02429 =
0.02216 0.00598 -0.00744 -0.00945
F2' 3 -0.124949 0.398053 0.052832 11.00000 0.06182 0.04310 =
0.01871 -0.00929 -0.01117 -0.00842
O11 5 0.571482 0.149350 0.165890 11.00000 0.03418 0.03621 =
0.02474 -0.00655 -0.00360 -0.00958
C35' 1 -0.029006 0.288539 -0.365518 11.00000 0.01532 0.02436 =
0.01772 0.00497 -0.00587 -0.00761
F1 3 0.271103 0.290431 0.472148 11.00000 0.02478 0.04061 =
0.02582 -0.00059 -0.00527 -0.00345
O1 5 0.465696 0.345347 0.488266 11.00000 0.03003 0.01246 =
0.02043 -0.00256 0.00528 -0.00651
AFIX 147
H1 2 0.528657 0.340321 0.455264 11.00000 -1.50000
AFIX 0
C1 1 0.522454 0.208298 0.456673 11.00000 0.01769 0.01347 =
0.01544 -0.00103 -0.00471 -0.00335
AFIX 23
H1A 2 0.462609 0.182181 0.451591 11.00000 -1.20000
H1B 2 0.584472 0.172154 0.476587 11.00000 -1.20000
AFIX 0
C36 1 0.537259 0.191660 0.210938 11.00000 0.02293 0.02225 =
0.02493 0.00642 -0.00656 -0.00513
C18 1 0.692498 0.075901 0.369451 11.00000 0.02168 0.01711 =
0.01201 -0.00684 -0.00447 0.00058
F3 3 0.247884 0.344766 0.567985 11.00000 0.02304 0.02862 =
0.03145 -0.00672 0.00197 0.00040
O1' 5 -0.231136 0.407170 -0.056802 11.00000 0.01935 0.02784 =
0.02705 -0.01003 -0.00343 -0.00435
AFIX 147
H1' 2 -0.259229 0.385876 -0.081950 11.00000 -1.50000
AFIX 0
O2' 5 -0.273985 0.316737 -0.134914 11.00000 0.01791 0.01597 =
0.01799 -0.00284 -0.00102 -0.00048
O8 5 0.294260 0.174175 0.368879 11.00000 0.03290 0.04408 =
0.03797 0.00566 -0.00399 -0.02205
F6 3 0.612376 0.265327 0.563878 11.00000 0.02402 0.04166 =
0.02336 -0.00485 -0.00490 -0.01513
O2 5 0.652644 0.297264 0.381988 11.00000 0.01913 0.01287 =
0.01764 -0.00207 -0.00115 -0.00730
O10 5 0.629934 0.367640 0.192927 11.00000 0.03695 0.03599 =
0.03396 0.01067 -0.00961 -0.02070
C1' 1 -0.047954 0.305259 -0.118701 11.00000 0.01877 0.01854 =
0.01763 -0.00230 -0.00522 -0.00089
AFIX 23
H1'A 2 -0.030748 0.258837 -0.091810 11.00000 -1.20000
H1'B 2 0.032188 0.310084 -0.147004 11.00000 -1.20000
AFIX 0
F4' 3 -0.092645 0.495062 -0.044623 11.00000 0.03380 0.03021 =
0.03283 -0.01257 -0.00658 -0.00981
C2 1 0.452936 0.274791 0.509385 11.00000 0.01730 0.01681 =
0.01671 -0.00397 -0.00113 -0.00401
O7' 5 -0.062726 0.485287 -0.406011 11.00000 0.04809 0.03851 =
0.03711 0.01424 -0.01749 -0.02488
F6' 3 -0.049744 0.460513 -0.149817 11.00000 0.07298 0.04183 =
0.02357 0.00037 -0.00626 -0.03490
C2' 1 -0.105871 0.372818 -0.067042 11.00000 0.01920 0.02193 =
0.01924 -0.00181 -0.00526 -0.00131
C32' 1 -0.085729 0.442807 -0.364063 11.00000 0.02872 0.02355 =
0.03126 0.00075 -0.01165 -0.01031
C33 1 0.353092 0.210740 0.340845 11.00000 0.02564 0.02838 =
0.01706 -0.00078 -0.00335 -0.00623
C5' 1 -0.085753 0.182851 -0.187695 11.00000 0.02105 0.02108 =
0.01269 -0.00197 0.00014 -0.00389
O9' 5 -0.367247 0.361738 -0.314697 11.00000 0.02896 0.04423 =
0.03576 0.00029 -0.00976 -0.01316
C4 1 0.497294 0.257636 0.575544 11.00000 0.01463 0.02912 =
0.02984 0.00567 0.00620 -0.00630
O11' 5 0.145932 0.369618 -0.268747 11.00000 0.02674 0.04916 =
0.03001 0.00028 -0.00656 -0.02330
C6' 1 -0.146485 0.142377 -0.124765 11.00000 0.01122 0.02460 =
0.02127 0.00613 -0.00788 -0.00291
C33' 1 -0.219517 0.456959 -0.225483 11.00000 0.03382 0.02247 =
0.02773 0.00519 -0.00548 -0.00860
C18' 1 -0.125923 0.162484 -0.249397 11.00000 0.02629 0.01366 =
0.01714 -0.00075 -0.00599 -0.00541
C20 1 0.682270 -0.029815 0.445142 11.00000 0.03295 0.02162 =
0.03559 0.01551 -0.01189 -0.01130
AFIX 43
H20 2 0.711362 -0.061778 0.479440 11.00000 -1.20000
AFIX 0
C3' 1 -0.086486 0.343617 0.000404 11.00000 0.02790 0.01219 =
0.03054 -0.00320 -0.01105 0.00588
O9 5 0.332791 0.424475 0.375334 11.00000 0.05688 0.03323 =
0.03532 -0.00899 -0.02105 0.00318
O7 5 0.259593 0.341133 0.204329 11.00000 0.02831 0.04804 =
0.03743 0.01493 -0.01813 -0.01028
C34 1 0.378550 0.367768 0.347138 11.00000 0.02352 0.01647 =
0.02866 0.00467 -0.01275 -0.00142
C7 1 0.820977 0.205568 0.235283 11.00000 0.03154 0.01892 =
0.02049 0.00101 -0.00391 -0.00580
AFIX 43
H7 2 0.807974 0.248108 0.263342 11.00000 -1.20000
AFIX 0
C14 1 0.927736 0.168566 0.470137 11.00000 0.02936 0.02837 =
0.02182 0.00859 -0.01306 -0.01288
AFIX 43
H14 2 0.913026 0.192386 0.513425 11.00000 -1.20000
AFIX 0
C32 1 0.335056 0.316693 0.233629 11.00000 0.03068 0.02348 =
0.02132 0.00665 0.00020 -0.01098
C36' 1 0.052724 0.369684 -0.275429 11.00000 0.03042 0.02250 =
0.01513 -0.00403 -0.00213 -0.01159
C3 1 0.313080 0.284215 0.528264 11.00000 0.02534 0.02732 =
0.01480 -0.00239 -0.00052 -0.00267
F1' 3 -0.154506 0.295899 0.026706 11.00000 0.12257 0.03997 =
0.02443 0.00872 -0.01809 -0.03541
C6 1 0.790752 0.142483 0.265857 11.00000 0.01948 0.01286 =
0.01667 -0.00354 -0.00200 0.00222
F3' 3 0.029176 0.307547 0.002657 11.00000 0.08539 0.05921 =
0.05169 -0.01890 -0.05006 0.02890
C11 1 0.816875 0.079862 0.223696 11.00000 0.02567 0.01694 =
0.02909 -0.00210 -0.00662 -0.00202
AFIX 43
H11 2 0.800016 0.035231 0.243547 11.00000 -1.20000
AFIX 0
F5' 3 0.077370 0.412585 -0.089608 11.00000 0.02161 0.05700 =
0.08127 -0.02944 -0.00797 -0.01111
C23 1 0.601085 0.061697 0.345517 11.00000 0.03127 0.01427 =
0.02551 0.00238 -0.00965 -0.00663
AFIX 43
H23 2 0.572846 0.092147 0.310164 11.00000 -1.20000
AFIX 0
C11' 1 -0.135619 0.066772 -0.133653 11.00000 0.02988 0.02865 =
0.02255 0.00579 -0.00692 -0.01108
AFIX 43
H11' 2 -0.097784 0.044001 -0.178169 11.00000 -1.20000
AFIX 0
C12 1 0.848256 0.143184 0.376141 11.00000 0.02239 0.01414 =
0.01990 0.00481 -0.00561 -0.00604
C5 1 0.742348 0.143009 0.344439 11.00000 0.02295 0.01265 =
0.01548 -0.00099 -0.00364 -0.00465
C17 1 0.968072 0.100412 0.344975 11.00000 0.02726 0.02113 =
0.02818 -0.00102 -0.00844 -0.00875
AFIX 43
H17 2 0.984043 0.075928 0.301859 11.00000 -1.20000
AFIX 0
C16' 1 0.257711 0.161925 -0.262632 11.00000 0.02231 0.02784 =
0.03146 -0.00126 0.00138 -0.00479
AFIX 43
H16' 2 0.308705 0.176278 -0.303071 11.00000 -1.20000
AFIX 0
C23' 1 -0.250339 0.186445 -0.247857 11.00000 0.02683 0.02288 =
0.02049 -0.00244 -0.00555 -0.00278
AFIX 43
H23' 2 -0.306692 0.216858 -0.210123 11.00000 -1.20000
AFIX 0
C20' 1 -0.090013 0.097110 -0.357095 11.00000 0.03877 0.02165 =
0.02052 -0.00623 -0.00604 -0.00361
AFIX 43
H20' 2 -0.034384 0.066373 -0.394826 11.00000 -1.20000
AFIX 0
C7' 1 -0.202677 0.173396 -0.059540 11.00000 0.01940 0.02812 =
0.02489 0.00623 -0.00461 -0.00274
AFIX 43
H7' 2 -0.212620 0.225032 -0.051780 11.00000 -1.20000
AFIX 0
C34' 1 -0.275873 0.363717 -0.304856 11.00000 0.02879 0.01985 =
0.02145 0.00023 -0.00722 -0.00423
C15 1 1.044037 0.125838 0.437923 11.00000 0.02272 0.03058 =
0.04450 0.01550 -0.01654 -0.01047
AFIX 43
H15 2 1.109847 0.119357 0.459039 11.00000 -1.20000
AFIX 0
C10 1 0.867125 0.081577 0.153167 11.00000 0.03496 0.02281 =
0.02457 -0.00473 -0.00442 0.00200
AFIX 43
H10 2 0.883238 0.038524 0.125099 11.00000 -1.20000
AFIX 0
C9' 1 -0.231219 0.056144 -0.014696 11.00000 0.03522 0.04188 =
0.03670 0.02625 -0.00415 -0.01476
AFIX 43
H9' 2 -0.257989 0.026651 0.023093 11.00000 -1.20000
AFIX 0
C8' 1 -0.245090 0.130502 -0.004874 11.00000 0.02550 0.04867 =
0.02061 0.01137 -0.00332 -0.00461
AFIX 43
H8' 2 -0.283999 0.153120 0.039627 11.00000 -1.20000
AFIX 0
C35 1 0.571080 0.333795 0.227713 11.00000 0.02143 0.02637 =
0.02392 -0.00103 -0.00861 -0.00263
C17' 1 0.132750 0.180193 -0.254925 11.00000 0.02276 0.02851 =
0.01812 0.00205 -0.00059 0.00035
AFIX 43
H17' 2 0.098829 0.207276 -0.290148 11.00000 -1.20000
AFIX 0
C22 1 0.549372 0.004938 0.371079 11.00000 0.02841 0.02278 =
0.03419 -0.00375 -0.00790 -0.00896
AFIX 43
H22 2 0.484986 -0.002085 0.354044 11.00000 -1.20000
AFIX 0
C13 1 0.831656 0.176953 0.439443 11.00000 0.02328 0.02303 =
0.02192 0.00501 -0.00668 -0.00800
AFIX 43
H13 2 0.751798 0.206771 0.462430 11.00000 -1.20000
AFIX 0
C14' 1 0.233605 0.103431 -0.153327 11.00000 0.02501 0.02814 =
0.03106 0.00587 -0.01232 -0.00589
AFIX 43
H14' 2 0.268181 0.077303 -0.117940 11.00000 -1.20000
AFIX 0
C21 1 0.589613 -0.041796 0.420975 11.00000 0.03780 0.02179 =
0.03633 0.00368 -0.00363 -0.01499
AFIX 43
H21 2 0.554412 -0.081300 0.438310 11.00000 -1.20000
AFIX 0
C19 1 0.733921 0.027690 0.420613 11.00000 0.02647 0.01979 =
0.02651 0.00404 -0.00709 -0.00629
AFIX 43
H19 2 0.797592 0.034838 0.438239 11.00000 -1.20000
AFIX 0
C16 1 1.064288 0.092775 0.375352 11.00000 0.02279 0.02944 =
0.04350 0.00064 -0.00800 -0.00685
AFIX 43
H16 2 1.145042 0.064243 0.352348 11.00000 -1.20000
AFIX 0
C8 1 0.869529 0.207936 0.165001 11.00000 0.04057 0.02347 =
0.02273 0.00416 0.00114 -0.00299
AFIX 43
H8 2 0.886391 0.252471 0.144900 11.00000 -1.20000
AFIX 0
C15' 1 0.309856 0.122959 -0.212245 11.00000 0.02035 0.02530 =
0.03753 0.00058 -0.00299 -0.00176
AFIX 43
H15' 2 0.396298 0.109805 -0.217872 11.00000 -1.20000
AFIX 0
C22' 1 -0.294056 0.167094 -0.299896 11.00000 0.03184 0.02921 =
0.03417 -0.00415 -0.01684 -0.00480
AFIX 43
H22' 2 -0.379386 0.184833 -0.297748 11.00000 -1.20000
AFIX 0
C9 1 0.893653 0.145200 0.123780 11.00000 0.03787 0.03568 =
0.02014 -0.00297 -0.00459 0.00035
AFIX 43
H9 2 0.928339 0.146276 0.075485 11.00000 -1.20000
AFIX 0
C19' 1 -0.046013 0.116303 -0.305064 11.00000 0.03103 0.02090 =
0.02222 -0.00122 -0.00427 -0.00392
AFIX 43
H19' 2 0.039230 0.097979 -0.307115 11.00000 -1.20000
AFIX 0
C21' 1 -0.214703 0.122271 -0.354828 11.00000 0.04905 0.02168 =
0.02436 -0.00146 -0.01825 -0.00993
AFIX 43
H21' 2 -0.244605 0.108782 -0.390529 11.00000 -1.20000
AFIX 0
C10' 1 -0.178024 0.023990 -0.079906 11.00000 0.03125 0.03392 =
0.04167 0.01139 -0.01235 -0.01339
AFIX 43
H10' 2 -0.170759 -0.027269 -0.087606 11.00000 -1.20000
AFIX 0
C4' 1 -0.042851 0.435739 -0.087521 11.00000 0.02566 0.03253 =
0.02888 -0.01341 -0.00583 -0.00500
O5 5 0.930704 0.343332 0.310517 11.00000 0.02423 0.02427 =
0.02770 0.00806 -0.00434 -0.00739
O4 5 0.842674 0.349604 0.449108 11.00000 0.03179 0.02726 =
0.03183 0.00177 -0.01126 -0.01733
O6 5 0.724158 0.446998 0.295530 11.00000 0.02049 0.02258 =
0.02402 -0.00185 -0.00111 -0.00633
O3 5 0.635335 0.451707 0.434782 11.00000 0.03241 0.02316 =
0.02286 -0.00467 -0.00102 -0.01142
C29 1 0.838973 0.440214 0.244990 11.00000 0.02402 0.02557 =
0.01842 0.00221 0.00178 -0.00876
AFIX 23
H29A 2 0.839888 0.489655 0.224112 11.00000 -1.20000
H29B 2 0.848506 0.404508 0.207822 11.00000 -1.20000
AFIX 0
C28 1 0.943613 0.412582 0.278817 11.00000 0.02160 0.02714 =
0.03172 0.01154 -0.00512 -0.01090
AFIX 23
H28A 2 1.023700 0.404223 0.244090 11.00000 -1.20000
H28B 2 0.938460 0.449522 0.313888 11.00000 -1.20000
AFIX 0
C31 1 0.577621 0.510593 0.393382 11.00000 0.02967 0.01425 =
0.03430 -0.00387 -0.00097 -0.00292
AFIX 23
H31A 2 0.543405 0.558504 0.420208 11.00000 -1.20000
H31B 2 0.508969 0.497615 0.381716 11.00000 -1.20000
AFIX 0
C26 1 0.967574 0.351270 0.422553 11.00000 0.03971 0.03512 =
0.04006 0.01472 -0.02169 -0.02135
AFIX 23
H26A 2 1.018134 0.325125 0.453973 11.00000 -1.20000
H26B 2 0.971730 0.403809 0.417925 11.00000 -1.20000
AFIX 0
C30 1 0.669318 0.519892 0.328501 11.00000 0.03287 0.02200 =
0.02701 0.00004 -0.00515 -0.00448
AFIX 23
H30A 2 0.628130 0.555874 0.297893 11.00000 -1.20000
H30B 2 0.732967 0.539089 0.339287 11.00000 -1.20000
AFIX 0
C24 1 0.705828 0.474121 0.473861 11.00000 0.04853 0.02789 =
0.02454 -0.00658 -0.00317 -0.01763
AFIX 23
H24A 2 0.651335 0.510400 0.511031 11.00000 -1.20000
H24B 2 0.765706 0.497793 0.443734 11.00000 -1.20000
AFIX 0
C25 1 0.771750 0.402678 0.503969 11.00000 0.05586 0.03972 =
0.02348 0.00170 -0.01466 -0.02417
AFIX 23
H25A 2 0.826509 0.413684 0.529581 11.00000 -1.20000
H25B 2 0.711058 0.381495 0.536552 11.00000 -1.20000
AFIX 0
C27 1 1.013630 0.312233 0.353394 11.00000 0.01884 0.04475 =
0.04649 0.01959 -0.00749 -0.00750
AFIX 23
H27A 2 1.096138 0.317777 0.330504 11.00000 -1.20000
H27B 2 1.021425 0.257956 0.359471 11.00000 -1.20000
AFIX 0
C12' 1 0.053755 0.159582 -0.195817 11.00000 0.01695 0.01110 =
0.02023 -0.00493 0.00049 -0.00019
O8' 5 -0.289366 0.507449 -0.192623 11.00000 0.04861 0.02500 =
0.03592 -0.00192 -0.00245 0.00205
C13' 1 0.107205 0.121488 -0.145181 11.00000 0.01964 0.01334 =
0.02361 0.00389 -0.00196 0.00317
AFIX 43
H13' 2 0.056723 0.107516 -0.104316 11.00000 -1.20000
AFIX 0
O12 5 0.294043 0.119411 0.140372 11.00000 0.09379 0.12537 =
0.09116 0.01473 -0.05132 -0.05954
C38 1 0.185252 0.170819 0.186896 11.00000 0.05096 0.06656 =
0.05511 -0.01580 0.00341 -0.01952
AFIX 23
H38A 2 0.207837 0.187783 0.226253 11.00000 -1.20000
H38B 2 0.120027 0.145645 0.205021 11.00000 -1.20000
AFIX 0
C37 1 0.141408 0.237627 0.141863 11.00000 0.06587 0.09169 =
0.07968 0.01512 -0.01051 -0.03147
AFIX 137
H37A 2 0.131357 0.218939 0.099701 11.00000 -1.50000
H37B 2 0.202498 0.265830 0.129623 11.00000 -1.50000
H37C 2 0.062460 0.270637 0.167598 11.00000 -1.50000
AFIX 0
LI' 4 -0.439408 0.324750 -0.102199 11.00000 0.02003 0.03029 =
0.02613 -0.00535 -0.00457 -0.00645
LI 4 0.750989 0.360933 0.371754 11.00000 0.02791 0.02508 =
0.02039 0.00313 -0.00619 -0.01365
C39 1 0.332836 0.058625 0.182223 11.00000 0.11308 0.10700 =
0.12491 0.00958 -0.07292 -0.03979
AFIX 23
H39A 2 0.269764 0.031836 0.200261 11.00000 -1.20000
H39B 2 0.360470 0.073445 0.220573 11.00000 -1.20000
AFIX 0
C40 1 0.451658 0.009540 0.118216 11.00000 0.09083 0.07599 =
0.18045 -0.02501 -0.06598 0.00359
AFIX 137
H40A 2 0.429146 0.018310 0.074127 11.00000 -1.50000
H40B 2 0.469643 -0.044197 0.128206 11.00000 -1.50000
H40C 2 0.524647 0.026227 0.115436 11.00000 -1.50000
AFIX 0
O3' 5 -0.562445 0.386286 -0.160372 11.00000 0.02379 0.02861 =
0.02723 -0.00689 -0.00812 -0.00737
O5' 5 -0.476946 0.283053 -0.001107 11.00000 0.02858 0.02957 =
0.02803 -0.00022 -0.00161 -0.00755
O6' 5 -0.511449 0.425711 -0.045895 11.00000 0.02183 0.02776 =
0.02160 -0.00305 -0.00270 -0.00308
O4' 5 -0.527499 0.242835 -0.115099 11.00000 0.02584 0.02472 =
0.03987 -0.00342 -0.00859 -0.00138
C24' 1 -0.622525 0.337609 -0.182022 11.00000 0.02817 0.03722 =
0.02928 -0.00683 -0.01198 -0.00533
AFIX 23
H24C 2 -0.570297 0.311120 -0.225650 11.00000 -1.20000
H24D 2 -0.701927 0.367780 -0.190344 11.00000 -1.20000
AFIX 0
C30' 1 -0.574870 0.482347 -0.084881 11.00000 0.02893 0.02188 =
0.03281 -0.00366 -0.00612 -0.00408
AFIX 23
H30C 2 -0.514732 0.502298 -0.119259 11.00000 -1.20000
H30D 2 -0.631211 0.524325 -0.053696 11.00000 -1.20000
AFIX 0
C29' 1 -0.584313 0.413835 0.021241 11.00000 0.02854 0.03367 =
0.02361 -0.00441 -0.00285 -0.00670
AFIX 23
H29C 2 -0.663562 0.407492 0.017973 11.00000 -1.20000
H29D 2 -0.601414 0.456984 0.052646 11.00000 -1.20000
AFIX 0
C25' 1 -0.644471 0.281468 -0.127000 11.00000 0.01811 0.03116 =
0.04777 -0.00808 -0.01077 -0.00643
AFIX 23
H25C 2 -0.701554 0.307257 -0.084132 11.00000 -1.20000
H25D 2 -0.680904 0.245623 -0.142404 11.00000 -1.20000
AFIX 0
C31' 1 -0.646436 0.451312 -0.120841 11.00000 0.02363 0.03519 =
0.03542 -0.00396 -0.01188 -0.00433
AFIX 23
H31C 2 -0.713710 0.436974 -0.086848 11.00000 -1.20000
H31D 2 -0.683016 0.489275 -0.151700 11.00000 -1.20000
AFIX 0
C26' 1 -0.533835 0.195702 -0.056889 11.00000 0.03779 0.02801 =
0.05807 0.00320 -0.01539 -0.01292
AFIX 23
H26C 2 -0.454017 0.156728 -0.061935 11.00000 -1.20000
H26D 2 -0.597995 0.170119 -0.054288 11.00000 -1.20000
AFIX 0
C27' 1 -0.563850 0.241210 0.008912 11.00000 0.03263 0.03121 =
0.04316 0.01510 -0.00610 -0.01329
AFIX 23
H27C 2 -0.648536 0.275463 0.018092 11.00000 -1.20000
H27D 2 -0.557597 0.207527 0.048627 11.00000 -1.20000
AFIX 0
C28' 1 -0.509176 0.343887 0.046933 11.00000 0.03600 0.03878 =
0.01909 -0.00254 -0.00252 -0.00749
AFIX 23
H28C 2 -0.433437 0.352520 0.053511 11.00000 -1.20000
H28D 2 -0.556695 0.330970 0.092121 11.00000 -1.20000
AFIX 0
HKLF 4
REM 4012f in P-1 #2
REM R1 = 0.0470 for 12783 Fo > 4sig(Fo) and 0.0959 for all 19509 data
REM 1058 parameters refined using 27 restraints
END
WGHT 0.0674 0.0000
REM Highest difference peak 4.023, deepest hole -1.908, 1-sigma level 0.185
Q1 1 0.1916 0.0798 -0.2821 11.00000 0.05 4.02
Q2 1 0.7638 -0.0153 0.2963 11.00000 0.05 3.71
Q3 1 -0.2815 0.0150 0.0216 11.00000 0.05 3.14
Q4 1 0.0351 0.1788 -0.1391 11.00000 0.05 2.95
Q5 1 -0.3140 0.5378 -0.1338 11.00000 0.05 2.75
Q6 1 1.1405 0.1203 0.4587 11.00000 0.05 2.29
Q7 1 0.4986 0.2380 0.5423 11.00000 0.05 1.54
Q8 1 -0.0791 0.3412 -0.0240 11.00000 0.05 1.34
Q9 1 0.5045 0.0010 0.0195 11.00000 0.05 1.32
Q10 1 0.3606 0.0778 0.1097 11.00000 0.05 1.25
REM The information below was added by Olex2.
REM
REM R1 = 0.0470 for 12783 Fo > 4sig(Fo) and 0.0959 for all 114197 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 4.02, deepest hole -1.91
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0959
REM R1_gt = 0.0470
REM wR_ref = 0.1261
REM GOOF = 1.009
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 114197
REM Reflections_gt = 12783
REM Parameters = n/a
REM Hole = -1.91
REM Peak = 4.02
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_4641f
_database_code_depnum_ccdc_archive 'CCDC 1526596'
_audit_update_record
;
2017-01-10 deposited with the CCDC.
2017-02-03 downloaded from the CCDC.
;
_audit_creation_date 2016-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_chemical_name_common ?
_chemical_name_systematic PB-13
_chemical_formula_moiety 'C28 H17 F6 O6 P W'
_chemical_formula_sum 'C28 H17 F6 O6 P W'
_chemical_formula_weight 778.23
_chemical_melting_point ?
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
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'
_cell_length_a 14.5390(8)
_cell_length_b 11.5901(6)
_cell_length_c 32.8290(18)
_cell_angle_alpha 90
_cell_angle_beta 100.6203(19)
_cell_angle_gamma 90
_cell_volume 5437.2(5)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9892
_cell_measurement_temperature 150
_cell_measurement_theta_max 29.59
_cell_measurement_theta_min 2.26
_shelx_estimated_absorpt_T_max 0.810
_shelx_estimated_absorpt_T_min 0.578
_exptl_absorpt_coefficient_mu 4.391
_exptl_absorpt_correction_T_max 0.7459
_exptl_absorpt_correction_T_min 0.4359
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1598 before and 0.0810 after correction.
The Ratio of minimum to maximum transmission is 0.5844.
The \l/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.901
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 3008
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1371
_diffrn_reflns_av_unetI/netI 0.0792
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 43
_diffrn_reflns_limit_l_min -43
_diffrn_reflns_number 106615
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 27.998
_diffrn_reflns_theta_min 2.150
_diffrn_ambient_temperature 150.0
_diffrn_detector 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8-Venture'
_diffrn_measurement_method 'fine slicing \w and \f scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_diffrn_special_details ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 9555
_reflns_number_total 13119
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_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 'XS (Sheldrick, 2008)'
_refine_diff_density_max 1.025
_refine_diff_density_min -1.079
_refine_diff_density_rms 0.159
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.008
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 757
_refine_ls_number_reflns 13119
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0720
_refine_ls_R_factor_gt 0.0384
_refine_ls_restrained_S_all 1.009
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0603
_refine_ls_wR_factor_ref 0.0665
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
P1', O1'
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Secondary CH2 refined with riding coordinates:
C2(H2A,H2B), C2'(H2'A,H2'B)
3.b Aromatic/amide H refined with riding coordinates:
C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C7'(H7'),
C8'(H8'), C9'(H9'), C10'(H10'), C11'(H11'), C13'(H13'), C14'(H14'),
C15'(H15'), C16'(H16'), C17'(H17'), C19'(H19'), C20'(H20'), C21'(H21'),
C22'(H22'), C23'(H23')
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
W W 0.84220(2) 0.65809(2) 0.59849(2) 0.01796(5) Uani 1 1 d . . . . .
P P 0.86238(7) 0.47781(9) 0.64112(3) 0.0169(2) Uani 1 1 d . . . . .
F1 F 0.71938(18) 0.3301(2) 0.74513(8) 0.0392(7) Uani 1 1 d . . . . .
F2 F 0.84352(17) 0.2663(2) 0.72680(7) 0.0333(6) Uani 1 1 d . . . . .
F3 F 0.70898(19) 0.2295(2) 0.68964(8) 0.0426(7) Uani 1 1 d . . . . .
F4 F 0.66252(17) 0.5729(2) 0.65847(8) 0.0361(7) Uani 1 1 d . . . . .
F5 F 0.68600(17) 0.5514(2) 0.72456(8) 0.0376(7) Uani 1 1 d . . . . .
F6 F 0.59996(16) 0.4307(2) 0.68446(8) 0.0366(7) Uani 1 1 d . . . . .
O1 O 0.76696(18) 0.3947(2) 0.64405(8) 0.0208(6) Uani 1 1 d . . . . .
O2 O 0.8141(2) 0.8833(3) 0.54403(11) 0.0458(9) Uani 1 1 d . . . . .
O3 O 0.7498(2) 0.7991(3) 0.66319(10) 0.0454(9) Uani 1 1 d . . . . .
O4 O 1.0296(2) 0.7718(3) 0.64649(10) 0.0434(9) Uani 1 1 d . . . . .
O5 O 0.9400(2) 0.5670(3) 0.52525(9) 0.0321(8) Uani 1 1 d . . . . .
O6 O 0.6438(2) 0.5625(3) 0.55253(10) 0.0352(8) Uani 1 1 d . . . . .
C1 C 0.7645(3) 0.4210(4) 0.68648(12) 0.0192(9) Uani 1 1 d . . . . .
C2 C 0.8579(3) 0.4870(4) 0.69675(12) 0.0200(9) Uani 1 1 d . . . . .
H2A H 0.9085 0.4442 0.7149 0.024 Uiso 1 1 calc R . . . .
H2B H 0.8520 0.5666 0.7069 0.024 Uiso 1 1 calc R . . . .
C3 C 0.7599(3) 0.3103(4) 0.71222(13) 0.0261(10) Uani 1 1 d . . . . .
C4 C 0.6773(3) 0.4950(4) 0.68891(13) 0.0251(10) Uani 1 1 d . . . . .
C5 C 0.9573(3) 0.3716(3) 0.63198(12) 0.0182(9) Uani 1 1 d . . . . .
C6 C 1.0448(3) 0.4494(3) 0.64149(12) 0.0177(9) Uani 1 1 d . . . . .
C7 C 1.0764(3) 0.4922(4) 0.68183(13) 0.0231(10) Uani 1 1 d . . . . .
H7 H 1.0434 0.4720 0.7032 0.028 Uiso 1 1 calc R . . . .
C8 C 1.1537(3) 0.5625(4) 0.69108(14) 0.0302(11) Uani 1 1 d . . . . .
H8 H 1.1744 0.5878 0.7188 0.036 Uiso 1 1 calc R . . . .
C9 C 1.2018(3) 0.5968(4) 0.66039(15) 0.0352(12) Uani 1 1 d . . . . .
H9 H 1.2549 0.6458 0.6667 0.042 Uiso 1 1 calc R . . . .
C10 C 1.1708(3) 0.5583(4) 0.62037(15) 0.0322(11) Uani 1 1 d . . . . .
H10 H 1.2033 0.5810 0.5991 0.039 Uiso 1 1 calc R . . . .
C11 C 1.0934(3) 0.4876(4) 0.61064(13) 0.0224(10) Uani 1 1 d . . . . .
H11 H 1.0726 0.4644 0.5827 0.027 Uiso 1 1 calc R . . . .
C12 C 0.9630(3) 0.2608(3) 0.65855(12) 0.0186(9) Uani 1 1 d . . . . .
C13 C 1.0378(3) 0.2333(4) 0.68999(12) 0.0234(10) Uani 1 1 d . . . . .
H13 H 1.0881 0.2863 0.6969 0.028 Uiso 1 1 calc R . . . .
C14 C 1.0402(3) 0.1299(4) 0.71152(14) 0.0334(12) Uani 1 1 d . . . . .
H14 H 1.0918 0.1132 0.7330 0.040 Uiso 1 1 calc R . . . .
C15 C 0.9684(4) 0.0510(4) 0.70194(14) 0.0381(13) Uani 1 1 d . . . . .
H15 H 0.9697 -0.0189 0.7171 0.046 Uiso 1 1 calc R . . . .
C16 C 0.8950(3) 0.0746(4) 0.67028(14) 0.0335(12) Uani 1 1 d . . . . .
H16 H 0.8457 0.0204 0.6631 0.040 Uiso 1 1 calc R . . . .
C17 C 0.8931(3) 0.1788(4) 0.64871(13) 0.0259(10) Uani 1 1 d . . . . .
H17 H 0.8424 0.1938 0.6266 0.031 Uiso 1 1 calc R . . . .
C18 C 0.9338(3) 0.3316(3) 0.58633(12) 0.0152(8) Uani 1 1 d . . . . .
C19 C 1.0023(3) 0.2747(3) 0.56911(13) 0.0216(10) Uani 1 1 d . . . . .
H19 H 1.0621 0.2609 0.5857 0.026 Uiso 1 1 calc R . . . .
C20 C 0.9847(3) 0.2382(4) 0.52858(12) 0.0238(10) Uani 1 1 d . . . . .
H20 H 1.0328 0.2016 0.5173 0.029 Uiso 1 1 calc R . . . .
C21 C 0.8978(3) 0.2544(4) 0.50413(13) 0.0251(10) Uani 1 1 d . . . . .
H21 H 0.8866 0.2325 0.4758 0.030 Uiso 1 1 calc R . . . .
C22 C 0.8273(3) 0.3029(4) 0.52158(12) 0.0224(10) Uani 1 1 d . . . . .
H22 H 0.7661 0.3102 0.5056 0.027 Uiso 1 1 calc R . . . .
C23 C 0.8456(3) 0.3410(3) 0.56219(12) 0.0194(9) Uani 1 1 d . . . . .
H23 H 0.7964 0.3743 0.5737 0.023 Uiso 1 1 calc R . . . .
C24 C 0.8238(3) 0.8020(4) 0.56390(13) 0.0269(10) Uani 1 1 d . . . . .
C25 C 0.7812(3) 0.7443(4) 0.64048(13) 0.0274(11) Uani 1 1 d . . . . .
C26 C 0.9640(3) 0.7258(4) 0.62921(14) 0.0273(10) Uani 1 1 d . . . . .
C27 C 0.9060(3) 0.5940(4) 0.55260(13) 0.0232(10) Uani 1 1 d . . . . .
C28 C 0.7146(3) 0.5965(4) 0.56893(13) 0.0247(10) Uani 1 1 d . . . . .
W1' W 0.44866(2) -0.10994(2) 0.64640(2) 0.01856(5) Uani 1 1 d . . . . .
P1' P 0.44040(7) 0.07945(9) 0.61001(3) 0.0187(2) Uani 1 1 d . U . . .
F1' F 0.5871(2) 0.2125(3) 0.50771(9) 0.0571(9) Uani 1 1 d . . . . .
F2' F 0.61357(19) 0.3174(2) 0.56283(10) 0.0556(9) Uani 1 1 d . . . . .
F3' F 0.47389(17) 0.2937(2) 0.52942(7) 0.0352(7) Uani 1 1 d . . . . .
F4' F 0.64908(16) -0.0151(2) 0.60012(8) 0.0334(6) Uani 1 1 d . . . . .
F5' F 0.71067(17) 0.1176(2) 0.56924(9) 0.0475(8) Uani 1 1 d . . . . .
F6' F 0.62191(18) -0.0086(3) 0.53370(8) 0.0454(8) Uani 1 1 d . . . . .
O1' O 0.5396(2) 0.1596(3) 0.61057(9) 0.0288(7) Uani 1 1 d . U . . .
O2' O 0.4698(2) -0.3548(3) 0.68953(10) 0.0423(9) Uani 1 1 d . . . . .
O3' O 0.5526(2) -0.2321(3) 0.58097(11) 0.0447(9) Uani 1 1 d . . . . .
O4' O 0.6364(2) -0.0189(3) 0.70301(10) 0.0367(8) Uani 1 1 d . . . . .
O5' O 0.3292(2) -0.0431(3) 0.71483(10) 0.0412(9) Uani 1 1 d . . . . .
O6' O 0.2674(2) -0.2036(3) 0.58644(11) 0.0450(9) Uani 1 1 d . . . . .
C1' C 0.5468(3) 0.1334(4) 0.56827(12) 0.0206(10) Uani 1 1 d . . . . .
C2' C 0.4543(3) 0.0737(4) 0.55669(12) 0.0180(9) Uani 1 1 d . . . . .
H2'A H 0.4589 -0.0057 0.5461 0.022 Uiso 1 1 calc R . . . .
H2'B H 0.4069 0.1191 0.5377 0.022 Uiso 1 1 calc R . . . .
C3' C 0.5550(3) 0.2419(4) 0.54212(15) 0.0331(12) Uani 1 1 d . . . . .
C4' C 0.6332(3) 0.0559(4) 0.56765(14) 0.0280(11) Uani 1 1 d . . . . .
C5' C 0.3469(3) 0.1891(3) 0.61784(12) 0.0159(9) Uani 1 1 d . . . . .
C6' C 0.3635(3) 0.2226(3) 0.66372(12) 0.0171(9) Uani 1 1 d . . . . .
C7' C 0.4469(3) 0.2035(4) 0.69141(12) 0.0213(9) Uani 1 1 d . . . . .
H7' H 0.4962 0.1631 0.6823 0.026 Uiso 1 1 calc R . . . .
C8' C 0.4595(3) 0.2423(4) 0.73197(12) 0.0250(10) Uani 1 1 d . . . . .
H8' H 0.5170 0.2280 0.7503 0.030 Uiso 1 1 calc R . . . .
C9' C 0.3894(3) 0.3015(4) 0.74591(13) 0.0276(11) Uani 1 1 d . . . . .
H9' H 0.3973 0.3254 0.7740 0.033 Uiso 1 1 calc R . . . .
C10' C 0.3076(3) 0.3256(4) 0.71881(13) 0.0249(10) Uani 1 1 d . . . . .
H10' H 0.2596 0.3684 0.7280 0.030 Uiso 1 1 calc R . . . .
C11' C 0.2949(3) 0.2878(4) 0.67818(12) 0.0207(9) Uani 1 1 d . . . . .
H11' H 0.2386 0.3063 0.6597 0.025 Uiso 1 1 calc R . . . .
C12' C 0.3498(3) 0.3027(3) 0.59366(11) 0.0160(9) Uani 1 1 d . . . . .
C13' C 0.4225(3) 0.3805(4) 0.60790(13) 0.0258(10) Uani 1 1 d . . . . .
H13' H 0.4688 0.3602 0.6312 0.031 Uiso 1 1 calc R . . . .
C14' C 0.4285(3) 0.4862(4) 0.58885(13) 0.0281(11) Uani 1 1 d . . . . .
H14' H 0.4791 0.5366 0.5989 0.034 Uiso 1 1 calc R . . . .
C15' C 0.3618(3) 0.5186(4) 0.55557(13) 0.0280(11) Uani 1 1 d . . . . .
H15' H 0.3666 0.5904 0.5422 0.034 Uiso 1 1 calc R . . . .
C16' C 0.2879(3) 0.4454(4) 0.54192(13) 0.0260(10) Uani 1 1 d . . . . .
H16' H 0.2403 0.4681 0.5195 0.031 Uiso 1 1 calc R . . . .
C17' C 0.2820(3) 0.3382(4) 0.56070(12) 0.0199(9) Uani 1 1 d . . . . .
H17' H 0.2306 0.2888 0.5507 0.024 Uiso 1 1 calc R . . . .
C18' C 0.2568(3) 0.1168(3) 0.60364(12) 0.0163(9) Uani 1 1 d . . . . .
C19' C 0.2004(3) 0.0798(3) 0.63104(12) 0.0201(9) Uani 1 1 d . . . . .
H19' H 0.2173 0.0990 0.6596 0.024 Uiso 1 1 calc R . . . .
C20' C 0.1201(3) 0.0155(4) 0.61758(13) 0.0255(10) Uani 1 1 d . . . . .
H20' H 0.0817 -0.0063 0.6368 0.031 Uiso 1 1 calc R . . . .
C21' C 0.0953(3) -0.0169(4) 0.57674(14) 0.0276(10) Uani 1 1 d . . . . .
H21' H 0.0406 -0.0615 0.5676 0.033 Uiso 1 1 calc R . . . .
C22' C 0.1520(3) 0.0169(4) 0.54899(13) 0.0262(10) Uani 1 1 d . . . . .
H22' H 0.1357 -0.0051 0.5207 0.031 Uiso 1 1 calc R . . . .
C23' C 0.2315(3) 0.0817(3) 0.56193(12) 0.0203(9) Uani 1 1 d . . . . .
H23' H 0.2697 0.1030 0.5426 0.024 Uiso 1 1 calc R . . . .
C24' C 0.4623(3) -0.2655(4) 0.67422(13) 0.0272(11) Uani 1 1 d . . . . .
C25' C 0.5181(3) -0.1831(4) 0.60437(14) 0.0301(11) Uani 1 1 d . . . . .
C26' C 0.5703(3) -0.0536(4) 0.68270(13) 0.0231(10) Uani 1 1 d . . . . .
C27' C 0.3721(3) -0.0611(4) 0.68961(14) 0.0278(10) Uani 1 1 d . . . . .
C28' C 0.3300(3) -0.1658(4) 0.60811(13) 0.0260(10) 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 0.02204(10) 0.01464(9) 0.01763(9) 0.00175(7) 0.00475(7) 0.00326(8)
P 0.0167(6) 0.0160(6) 0.0182(6) 0.0016(4) 0.0036(4) 0.0010(5)
F1 0.0432(16) 0.0488(19) 0.0307(15) 0.0106(13) 0.0206(13) -0.0022(14)
F2 0.0338(16) 0.0334(16) 0.0337(15) 0.0115(12) 0.0089(12) 0.0059(13)
F3 0.0480(18) 0.0320(17) 0.0477(18) -0.0021(13) 0.0089(14) -0.0180(14)
F4 0.0322(15) 0.0374(17) 0.0418(16) 0.0114(13) 0.0149(13) 0.0135(13)
F5 0.0315(15) 0.0482(19) 0.0346(16) -0.0154(13) 0.0103(12) 0.0027(13)
F6 0.0190(14) 0.0443(18) 0.0462(17) -0.0016(13) 0.0055(12) -0.0087(13)
O1 0.0213(15) 0.0241(17) 0.0184(15) -0.0010(12) 0.0071(12) -0.0003(13)
O2 0.059(2) 0.029(2) 0.052(2) 0.0221(17) 0.0177(19) 0.0179(18)
O3 0.070(3) 0.034(2) 0.038(2) -0.0054(17) 0.0243(19) 0.0119(19)
O4 0.047(2) 0.024(2) 0.052(2) 0.0005(16) -0.0093(18) -0.0056(18)
O5 0.0395(19) 0.0285(19) 0.0334(19) 0.0017(15) 0.0202(16) 0.0001(16)
O6 0.0277(19) 0.034(2) 0.043(2) -0.0049(16) 0.0017(16) 0.0004(16)
C1 0.018(2) 0.025(2) 0.014(2) -0.0013(17) 0.0003(17) -0.0018(19)
C2 0.018(2) 0.024(2) 0.019(2) 0.0012(18) 0.0064(18) 0.0008(19)
C3 0.029(3) 0.024(3) 0.026(3) 0.0011(19) 0.009(2) -0.008(2)
C4 0.023(2) 0.031(3) 0.022(2) -0.004(2) 0.0045(19) -0.006(2)
C5 0.018(2) 0.017(2) 0.020(2) 0.0026(17) 0.0063(18) 0.0040(18)
C6 0.017(2) 0.013(2) 0.024(2) -0.0025(17) 0.0059(18) 0.0064(18)
C7 0.019(2) 0.027(3) 0.023(2) 0.0014(19) 0.0044(19) 0.005(2)
C8 0.029(3) 0.025(3) 0.033(3) -0.001(2) -0.004(2) 0.004(2)
C9 0.023(3) 0.029(3) 0.054(3) -0.003(2) 0.008(2) -0.008(2)
C10 0.028(3) 0.026(3) 0.044(3) -0.001(2) 0.014(2) -0.005(2)
C11 0.021(2) 0.019(2) 0.028(2) -0.0025(18) 0.0057(19) -0.0012(19)
C12 0.024(2) 0.017(2) 0.017(2) 0.0025(17) 0.0082(18) 0.0071(19)
C13 0.024(2) 0.026(3) 0.022(2) 0.0023(18) 0.0063(19) 0.006(2)
C14 0.044(3) 0.033(3) 0.024(3) 0.010(2) 0.007(2) 0.018(2)
C15 0.055(3) 0.028(3) 0.035(3) 0.013(2) 0.016(3) 0.012(3)
C16 0.040(3) 0.023(3) 0.040(3) 0.003(2) 0.014(2) -0.004(2)
C17 0.028(3) 0.018(3) 0.031(3) 0.0079(19) 0.004(2) 0.005(2)
C18 0.019(2) 0.006(2) 0.021(2) 0.0026(16) 0.0044(17) 0.0025(17)
C19 0.020(2) 0.015(2) 0.029(2) 0.0033(18) 0.0021(19) 0.0020(18)
C20 0.030(3) 0.020(2) 0.024(2) 0.0001(18) 0.012(2) 0.003(2)
C21 0.035(3) 0.017(2) 0.023(2) 0.0001(18) 0.006(2) -0.002(2)
C22 0.023(2) 0.018(2) 0.025(2) 0.0011(18) -0.0011(19) -0.002(2)
C23 0.021(2) 0.016(2) 0.021(2) 0.0019(17) 0.0039(18) 0.0005(19)
C24 0.023(2) 0.028(3) 0.031(3) 0.000(2) 0.009(2) 0.009(2)
C25 0.038(3) 0.020(3) 0.026(3) 0.0035(19) 0.010(2) 0.002(2)
C26 0.035(3) 0.016(2) 0.029(3) 0.0060(19) 0.003(2) 0.002(2)
C27 0.021(2) 0.021(3) 0.027(3) 0.0060(19) 0.002(2) -0.0017(19)
C28 0.036(3) 0.015(2) 0.025(2) 0.0053(18) 0.013(2) 0.010(2)
W1' 0.02069(10) 0.01456(9) 0.02030(9) 0.00212(7) 0.00342(7) 0.00286(8)
P1' 0.0210(6) 0.0166(6) 0.0193(6) 0.0015(4) 0.0057(5) 0.0032(5)
F1' 0.069(2) 0.062(2) 0.0528(19) 0.0303(16) 0.0441(17) 0.0279(17)
F2' 0.0339(17) 0.0287(18) 0.104(3) 0.0134(17) 0.0114(17) -0.0130(14)
F3' 0.0297(15) 0.0410(17) 0.0364(16) 0.0166(13) 0.0096(12) 0.0126(13)
F4' 0.0276(14) 0.0348(17) 0.0370(16) 0.0099(12) 0.0041(12) 0.0093(12)
F5' 0.0192(14) 0.0412(18) 0.084(2) 0.0148(16) 0.0154(14) -0.0021(13)
F6' 0.0458(17) 0.055(2) 0.0356(17) -0.0134(14) 0.0072(13) 0.0186(15)
O1' 0.0271(15) 0.0295(19) 0.0314(18) 0.0014(14) 0.0093(14) -0.0010(12)
O2' 0.056(2) 0.024(2) 0.048(2) 0.0136(16) 0.0119(18) 0.0071(18)
O3' 0.050(2) 0.035(2) 0.055(2) -0.0139(18) 0.0258(19) 0.0015(18)
O4' 0.034(2) 0.038(2) 0.034(2) -0.0010(15) -0.0061(16) 0.0004(17)
O5' 0.054(2) 0.041(2) 0.035(2) 0.0040(16) 0.0252(18) 0.0069(18)
O6' 0.040(2) 0.024(2) 0.061(2) -0.0022(17) -0.0139(19) -0.0042(17)
C1' 0.021(2) 0.022(3) 0.018(2) -0.0022(17) 0.0036(18) 0.0011(19)
C2' 0.015(2) 0.015(2) 0.026(2) 0.0029(17) 0.0094(18) 0.0051(17)
C3' 0.027(3) 0.034(3) 0.041(3) 0.012(2) 0.014(2) 0.007(2)
C4' 0.017(2) 0.035(3) 0.032(3) -0.001(2) 0.004(2) -0.001(2)
C5' 0.016(2) 0.014(2) 0.017(2) 0.0015(16) 0.0026(17) 0.0044(17)
C6' 0.016(2) 0.018(2) 0.018(2) 0.0005(17) 0.0032(17) -0.0022(18)
C7' 0.018(2) 0.018(2) 0.025(2) 0.0010(18) -0.0026(19) 0.0011(19)
C8' 0.026(3) 0.021(3) 0.021(2) 0.0002(18) -0.0106(19) -0.004(2)
C9' 0.038(3) 0.023(3) 0.020(2) -0.0061(19) 0.000(2) -0.006(2)
C10' 0.028(3) 0.021(3) 0.026(2) -0.0048(18) 0.005(2) 0.000(2)
C11' 0.017(2) 0.025(2) 0.019(2) -0.0007(18) -0.0011(18) 0.0010(19)
C12' 0.019(2) 0.013(2) 0.016(2) -0.0006(16) 0.0024(17) 0.0025(18)
C13' 0.023(2) 0.024(3) 0.028(3) 0.0070(19) -0.0018(19) -0.001(2)
C14' 0.025(3) 0.022(3) 0.035(3) 0.005(2) 0.000(2) -0.009(2)
C15' 0.037(3) 0.016(2) 0.031(3) 0.0078(19) 0.006(2) 0.002(2)
C16' 0.028(3) 0.024(3) 0.023(2) 0.0063(19) -0.003(2) 0.002(2)
C17' 0.023(2) 0.017(2) 0.019(2) 0.0006(17) -0.0009(18) -0.0007(19)
C18' 0.012(2) 0.009(2) 0.027(2) -0.0018(17) 0.0000(17) 0.0027(17)
C19' 0.021(2) 0.019(2) 0.021(2) -0.0004(17) 0.0054(18) 0.0017(19)
C20' 0.019(2) 0.025(3) 0.034(3) -0.002(2) 0.009(2) 0.000(2)
C21' 0.021(2) 0.018(2) 0.042(3) -0.002(2) 0.000(2) -0.003(2)
C22' 0.035(3) 0.016(2) 0.024(2) -0.0006(18) -0.006(2) -0.002(2)
C23' 0.022(2) 0.018(2) 0.020(2) -0.0020(17) 0.0025(18) 0.0015(19)
C24' 0.030(3) 0.027(3) 0.026(3) 0.001(2) 0.007(2) 0.005(2)
C25' 0.032(3) 0.024(3) 0.034(3) 0.004(2) 0.005(2) 0.000(2)
C26' 0.029(3) 0.019(2) 0.020(2) 0.0017(18) 0.003(2) 0.007(2)
C27' 0.033(3) 0.020(3) 0.029(3) 0.002(2) 0.002(2) 0.002(2)
C28' 0.032(3) 0.018(2) 0.027(3) 0.0080(19) 0.003(2) 0.005(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
W P 2.5017(11) . ?
W C24 2.007(5) . ?
W C25 2.034(4) . ?
W C26 2.028(5) . ?
W C27 2.049(4) . ?
W C28 2.056(5) . ?
P O1 1.706(3) . ?
P C2 1.843(4) . ?
P C5 1.914(4) . ?
F1 C3 1.342(5) . ?
F2 C3 1.324(5) . ?
F3 C3 1.331(5) . ?
F4 C4 1.335(5) . ?
F5 C4 1.326(5) . ?
F6 C4 1.334(5) . ?
O1 C1 1.433(4) . ?
O2 C24 1.140(5) . ?
O3 C25 1.138(5) . ?
O4 C26 1.147(5) . ?
O5 C27 1.145(5) . ?
O6 C28 1.140(5) . ?
C1 C2 1.541(5) . ?
C1 C3 1.545(6) . ?
C1 C4 1.545(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C5 C6 1.543(6) . ?
C5 C12 1.546(5) . ?
C5 C18 1.546(5) . ?
C6 C7 1.410(5) . ?
C6 C11 1.409(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.386(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.380(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.391(5) . ?
C12 C17 1.386(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.389(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.380(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.373(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.398(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.398(5) . ?
C18 C23 1.383(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.374(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.378(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.383(5) . ?
C23 H23 0.9500 . ?
W1' P1' 2.4915(11) . ?
W1' C24' 2.015(5) . ?
W1' C25' 2.039(5) . ?
W1' C26' 2.048(5) . ?
W1' C27' 2.038(5) . ?
W1' C28' 2.043(5) . ?
P1' O1' 1.713(3) . ?
P1' C2' 1.800(4) . ?
P1' C5' 1.913(4) . ?
F1' C3' 1.343(5) . ?
F2' C3' 1.319(6) . ?
F3' C3' 1.320(5) . ?
F4' C4' 1.332(5) . ?
F5' C4' 1.327(5) . ?
F6' C4' 1.327(5) . ?
O1' C1' 1.444(5) . ?
O2' C24' 1.147(5) . ?
O3' C25' 1.143(5) . ?
O4' C26' 1.138(5) . ?
O5' C27' 1.143(5) . ?
O6' C28' 1.135(5) . ?
C1' C2' 1.499(5) . ?
C1' C3' 1.540(6) . ?
C1' C4' 1.547(6) . ?
C2' H2'A 0.9900 . ?
C2' H2'B 0.9900 . ?
C5' C6' 1.531(5) . ?
C5' C12' 1.542(5) . ?
C5' C18' 1.552(5) . ?
C6' C7' 1.393(5) . ?
C6' C11' 1.401(5) . ?
C7' H7' 0.9500 . ?
C7' C8' 1.385(5) . ?
C8' H8' 0.9500 . ?
C8' C9' 1.376(6) . ?
C9' H9' 0.9500 . ?
C9' C10' 1.376(6) . ?
C10' H10' 0.9500 . ?
C10' C11' 1.384(5) . ?
C11' H11' 0.9500 . ?
C12' C13' 1.402(6) . ?
C12' C17' 1.386(5) . ?
C13' H13' 0.9500 . ?
C13' C14' 1.385(6) . ?
C14' H14' 0.9500 . ?
C14' C15' 1.372(6) . ?
C15' H15' 0.9500 . ?
C15' C16' 1.379(6) . ?
C16' H16' 0.9500 . ?
C16' C17' 1.397(6) . ?
C17' H17' 0.9500 . ?
C18' C19' 1.392(5) . ?
C18' C23' 1.411(5) . ?
C19' H19' 0.9500 . ?
C19' C20' 1.387(5) . ?
C20' H20' 0.9500 . ?
C20' C21' 1.375(6) . ?
C21' H21' 0.9500 . ?
C21' C22' 1.393(6) . ?
C22' H22' 0.9500 . ?
C22' C23' 1.378(6) . ?
C23' H23' 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
C24 W P 179.05(13) . . ?
C24 W C25 86.92(17) . . ?
C24 W C26 88.44(18) . . ?
C24 W C27 85.20(16) . . ?
C24 W C28 90.39(17) . . ?
C25 W P 92.98(12) . . ?
C25 W C27 171.80(16) . . ?
C25 W C28 91.26(17) . . ?
C26 W P 92.50(12) . . ?
C26 W C25 85.60(18) . . ?
C26 W C27 91.93(17) . . ?
C26 W C28 176.70(17) . . ?
C27 W P 94.94(12) . . ?
C27 W C28 91.05(16) . . ?
C28 W P 88.67(12) . . ?
O1 P W 119.37(10) . . ?
O1 P C2 78.41(15) . . ?
O1 P C5 105.26(16) . . ?
C2 P W 118.95(14) . . ?
C2 P C5 110.55(18) . . ?
C5 P W 117.59(12) . . ?
C1 O1 P 95.8(2) . . ?
O1 C1 C2 98.0(3) . . ?
O1 C1 C3 111.5(3) . . ?
O1 C1 C4 109.6(3) . . ?
C2 C1 C3 114.7(3) . . ?
C2 C1 C4 114.3(3) . . ?
C3 C1 C4 108.3(3) . . ?
P C2 H2A 114.2 . . ?
P C2 H2B 114.2 . . ?
C1 C2 P 86.8(2) . . ?
C1 C2 H2A 114.2 . . ?
C1 C2 H2B 114.2 . . ?
H2A C2 H2B 111.3 . . ?
F1 C3 C1 111.6(4) . . ?
F2 C3 F1 106.6(3) . . ?
F2 C3 F3 108.0(4) . . ?
F2 C3 C1 112.8(3) . . ?
F3 C3 F1 106.7(3) . . ?
F3 C3 C1 110.8(3) . . ?
F4 C4 C1 110.9(3) . . ?
F5 C4 F4 107.6(4) . . ?
F5 C4 F6 108.3(3) . . ?
F5 C4 C1 111.9(3) . . ?
F6 C4 F4 106.3(3) . . ?
F6 C4 C1 111.6(4) . . ?
C6 C5 P 100.6(2) . . ?
C6 C5 C12 114.5(3) . . ?
C6 C5 C18 113.5(3) . . ?
C12 C5 P 114.3(2) . . ?
C18 C5 P 108.0(3) . . ?
C18 C5 C12 106.1(3) . . ?
C7 C6 C5 120.6(3) . . ?
C11 C6 C5 122.8(4) . . ?
C11 C6 C7 116.4(4) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 C6 121.8(4) . . ?
C8 C7 H7 119.1 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.7(4) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 120.7 . . ?
C10 C9 C8 118.6(4) . . ?
C10 C9 H9 120.7 . . ?
C9 C10 H10 119.3 . . ?
C11 C10 C9 121.4(4) . . ?
C11 C10 H10 119.3 . . ?
C6 C11 H11 119.5 . . ?
C10 C11 C6 121.0(4) . . ?
C10 C11 H11 119.5 . . ?
C13 C12 C5 124.2(4) . . ?
C17 C12 C5 118.5(4) . . ?
C17 C12 C13 117.0(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.3(4) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.5(4) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.4(4) . . ?
C16 C15 H15 120.3 . . ?
C15 C16 H16 120.2 . . ?
C15 C16 C17 119.7(5) . . ?
C17 C16 H16 120.2 . . ?
C12 C17 C16 122.0(4) . . ?
C12 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
C19 C18 C5 119.2(3) . . ?
C23 C18 C5 123.2(3) . . ?
C23 C18 C19 117.4(4) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 C18 121.1(4) . . ?
C20 C19 H19 119.5 . . ?
C19 C20 H20 119.7 . . ?
C19 C20 C21 120.7(4) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 120.5 . . ?
C20 C21 C22 118.9(4) . . ?
C22 C21 H21 120.5 . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.3(4) . . ?
C23 C22 H22 119.9 . . ?
C18 C23 H23 119.3 . . ?
C22 C23 C18 121.3(4) . . ?
C22 C23 H23 119.3 . . ?
O2 C24 W 179.3(4) . . ?
O3 C25 W 175.3(4) . . ?
O4 C26 W 174.9(4) . . ?
O5 C27 W 174.1(4) . . ?
O6 C28 W 179.9(5) . . ?
C24' W1' P1' 176.42(12) . . ?
C24' W1' C25' 85.12(17) . . ?
C24' W1' C26' 91.10(17) . . ?
C24' W1' C27' 87.37(17) . . ?
C24' W1' C28' 89.80(17) . . ?
C25' W1' P1' 91.59(13) . . ?
C25' W1' C26' 92.53(17) . . ?
C25' W1' C28' 85.35(18) . . ?
C26' W1' P1' 87.62(12) . . ?
C27' W1' P1' 96.01(13) . . ?
C27' W1' C25' 171.42(18) . . ?
C27' W1' C26' 91.74(17) . . ?
C27' W1' C28' 90.50(17) . . ?
C28' W1' P1' 91.35(12) . . ?
C28' W1' C26' 177.62(16) . . ?
O1' P1' W1' 120.44(11) . . ?
O1' P1' C2' 77.60(16) . . ?
O1' P1' C5' 104.85(16) . . ?
C2' P1' W1' 115.44(14) . . ?
C2' P1' C5' 111.42(18) . . ?
C5' P1' W1' 119.57(12) . . ?
C1' O1' P1' 95.0(2) . . ?
O1' C1' C2' 96.9(3) . . ?
O1' C1' C3' 113.0(3) . . ?
O1' C1' C4' 109.7(3) . . ?
C2' C1' C3' 113.2(4) . . ?
C2' C1' C4' 114.9(3) . . ?
C3' C1' C4' 108.7(3) . . ?
P1' C2' H2'A 113.7 . . ?
P1' C2' H2'B 113.7 . . ?
C1' C2' P1' 89.6(2) . . ?
C1' C2' H2'A 113.7 . . ?
C1' C2' H2'B 113.7 . . ?
H2'A C2' H2'B 111.0 . . ?
F1' C3' C1' 109.6(4) . . ?
F2' C3' F1' 108.1(4) . . ?
F2' C3' F3' 108.4(4) . . ?
F2' C3' C1' 111.3(4) . . ?
F3' C3' F1' 106.2(4) . . ?
F3' C3' C1' 113.0(4) . . ?
F4' C4' C1' 111.7(3) . . ?
F5' C4' F4' 106.3(3) . . ?
F5' C4' C1' 111.8(4) . . ?
F6' C4' F4' 107.5(4) . . ?
F6' C4' F5' 108.0(3) . . ?
F6' C4' C1' 111.3(3) . . ?
C6' C5' P1' 108.3(3) . . ?
C6' C5' C12' 106.0(3) . . ?
C6' C5' C18' 113.8(3) . . ?
C12' C5' P1' 114.2(2) . . ?
C12' C5' C18' 114.1(3) . . ?
C18' C5' P1' 100.5(2) . . ?
C7' C6' C5' 124.2(3) . . ?
C7' C6' C11' 116.9(4) . . ?
C11' C6' C5' 118.5(3) . . ?
C6' C7' H7' 119.3 . . ?
C8' C7' C6' 121.4(4) . . ?
C8' C7' H7' 119.3 . . ?
C7' C8' H8' 119.8 . . ?
C9' C8' C7' 120.4(4) . . ?
C9' C8' H8' 119.8 . . ?
C8' C9' H9' 120.3 . . ?
C8' C9' C10' 119.5(4) . . ?
C10' C9' H9' 120.3 . . ?
C9' C10' H10' 119.9 . . ?
C9' C10' C11' 120.3(4) . . ?
C11' C10' H10' 119.9 . . ?
C6' C11' H11' 119.3 . . ?
C10' C11' C6' 121.4(4) . . ?
C10' C11' H11' 119.3 . . ?
C13' C12' C5' 117.9(3) . . ?
C17' C12' C5' 124.9(4) . . ?
C17' C12' C13' 117.0(4) . . ?
C12' C13' H13' 119.2 . . ?
C14' C13' C12' 121.6(4) . . ?
C14' C13' H13' 119.2 . . ?
C13' C14' H14' 119.7 . . ?
C15' C14' C13' 120.5(4) . . ?
C15' C14' H14' 119.7 . . ?
C14' C15' H15' 120.5 . . ?
C14' C15' C16' 119.0(4) . . ?
C16' C15' H15' 120.5 . . ?
C15' C16' H16' 119.6 . . ?
C15' C16' C17' 120.8(4) . . ?
C17' C16' H16' 119.6 . . ?
C12' C17' C16' 121.0(4) . . ?
C12' C17' H17' 119.5 . . ?
C16' C17' H17' 119.5 . . ?
C19' C18' C5' 122.5(3) . . ?
C19' C18' C23' 117.3(4) . . ?
C23' C18' C5' 120.1(3) . . ?
C18' C19' H19' 119.3 . . ?
C20' C19' C18' 121.4(4) . . ?
C20' C19' H19' 119.3 . . ?
C19' C20' H20' 119.6 . . ?
C21' C20' C19' 120.7(4) . . ?
C21' C20' H20' 119.6 . . ?
C20' C21' H21' 120.6 . . ?
C20' C21' C22' 118.7(4) . . ?
C22' C21' H21' 120.6 . . ?
C21' C22' H22' 119.5 . . ?
C23' C22' C21' 121.0(4) . . ?
C23' C22' H22' 119.5 . . ?
C18' C23' H23' 119.7 . . ?
C22' C23' C18' 120.7(4) . . ?
C22' C23' H23' 119.7 . . ?
O2' C24' W1' 179.1(4) . . ?
O3' C25' W1' 174.3(4) . . ?
O4' C26' W1' 177.7(4) . . ?
O5' C27' W1' 174.3(4) . . ?
O6' C28' W1' 175.3(4) . . ?
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
W P O1 C1 -109.9(2) . . . . ?
W P C2 C1 110.9(2) . . . . ?
P O1 C1 C2 -8.2(3) . . . . ?
P O1 C1 C3 -128.9(3) . . . . ?
P O1 C1 C4 111.2(3) . . . . ?
P C5 C6 C7 65.7(4) . . . . ?
P C5 C6 C11 -110.0(4) . . . . ?
P C5 C12 C13 -112.4(4) . . . . ?
P C5 C12 C17 72.7(4) . . . . ?
P C5 C18 C19 165.7(3) . . . . ?
P C5 C18 C23 -19.6(5) . . . . ?
O1 P C2 C1 -6.4(2) . . . . ?
O1 C1 C2 P 7.6(3) . . . . ?
O1 C1 C3 F1 -154.0(3) . . . . ?
O1 C1 C3 F2 86.1(4) . . . . ?
O1 C1 C3 F3 -35.2(5) . . . . ?
O1 C1 C4 F4 -40.0(5) . . . . ?
O1 C1 C4 F5 -160.2(3) . . . . ?
O1 C1 C4 F6 78.3(4) . . . . ?
C2 P O1 C1 6.9(2) . . . . ?
C2 C1 C3 F1 95.7(4) . . . . ?
C2 C1 C3 F2 -24.2(5) . . . . ?
C2 C1 C3 F3 -145.5(3) . . . . ?
C2 C1 C4 F4 68.9(4) . . . . ?
C2 C1 C4 F5 -51.3(5) . . . . ?
C2 C1 C4 F6 -172.8(3) . . . . ?
C3 C1 C2 P 125.8(3) . . . . ?
C3 C1 C4 F4 -161.8(3) . . . . ?
C3 C1 C4 F5 78.0(4) . . . . ?
C3 C1 C4 F6 -43.5(4) . . . . ?
C4 C1 C2 P -108.3(3) . . . . ?
C4 C1 C3 F1 -33.3(5) . . . . ?
C4 C1 C3 F2 -153.2(3) . . . . ?
C4 C1 C3 F3 85.5(4) . . . . ?
C5 P O1 C1 115.3(2) . . . . ?
C5 P C2 C1 -108.6(2) . . . . ?
C5 C6 C7 C8 -179.4(4) . . . . ?
C5 C6 C11 C10 179.2(4) . . . . ?
C5 C12 C13 C14 -177.2(4) . . . . ?
C5 C12 C17 C16 177.7(4) . . . . ?
C5 C18 C19 C20 -179.6(4) . . . . ?
C5 C18 C23 C22 -179.3(4) . . . . ?
C6 C5 C12 C13 2.9(5) . . . . ?
C6 C5 C12 C17 -172.0(3) . . . . ?
C6 C5 C18 C19 55.0(5) . . . . ?
C6 C5 C18 C23 -130.2(4) . . . . ?
C6 C7 C8 C9 2.1(7) . . . . ?
C7 C6 C11 C10 3.3(6) . . . . ?
C7 C8 C9 C10 -0.4(7) . . . . ?
C8 C9 C10 C11 0.3(7) . . . . ?
C9 C10 C11 C6 -1.9(7) . . . . ?
C11 C6 C7 C8 -3.5(6) . . . . ?
C12 C5 C6 C7 -57.3(5) . . . . ?
C12 C5 C6 C11 127.0(4) . . . . ?
C12 C5 C18 C19 -71.5(4) . . . . ?
C12 C5 C18 C23 103.3(4) . . . . ?
C12 C13 C14 C15 0.5(6) . . . . ?
C13 C12 C17 C16 2.5(6) . . . . ?
C13 C14 C15 C16 1.3(7) . . . . ?
C14 C15 C16 C17 -1.1(7) . . . . ?
C15 C16 C17 C12 -0.8(7) . . . . ?
C17 C12 C13 C14 -2.3(6) . . . . ?
C18 C5 C6 C7 -179.3(3) . . . . ?
C18 C5 C6 C11 5.1(5) . . . . ?
C18 C5 C12 C13 128.8(4) . . . . ?
C18 C5 C12 C17 -46.1(4) . . . . ?
C18 C19 C20 C21 -1.7(6) . . . . ?
C19 C18 C23 C22 -4.5(6) . . . . ?
C19 C20 C21 C22 -3.0(6) . . . . ?
C20 C21 C22 C23 3.9(6) . . . . ?
C21 C22 C23 C18 -0.1(6) . . . . ?
C23 C18 C19 C20 5.4(6) . . . . ?
W1' P1' O1' C1' 105.3(2) . . . . ?
W1' P1' C2' C1' -111.2(2) . . . . ?
P1' O1' C1' C2' 8.4(3) . . . . ?
P1' O1' C1' C3' 127.2(3) . . . . ?
P1' O1' C1' C4' -111.2(3) . . . . ?
P1' C5' C6' C7' 17.4(5) . . . . ?
P1' C5' C6' C11' -169.9(3) . . . . ?
P1' C5' C12' C13' -73.3(4) . . . . ?
P1' C5' C12' C17' 111.9(4) . . . . ?
P1' C5' C18' C19' 111.4(4) . . . . ?
P1' C5' C18' C23' -65.8(4) . . . . ?
O1' P1' C2' C1' 6.8(2) . . . . ?
O1' C1' C2' P1' -7.9(3) . . . . ?
O1' C1' C3' F1' 163.0(3) . . . . ?
O1' C1' C3' F2' 43.4(5) . . . . ?
O1' C1' C3' F3' -78.8(5) . . . . ?
O1' C1' C4' F4' 33.2(5) . . . . ?
O1' C1' C4' F5' -85.8(4) . . . . ?
O1' C1' C4' F6' 153.4(3) . . . . ?
C2' P1' O1' C1' -7.1(2) . . . . ?
C2' C1' C3' F1' -88.2(4) . . . . ?
C2' C1' C3' F2' 152.3(3) . . . . ?
C2' C1' C3' F3' 30.1(5) . . . . ?
C2' C1' C4' F4' -74.7(5) . . . . ?
C2' C1' C4' F5' 166.4(3) . . . . ?
C2' C1' C4' F6' 45.5(5) . . . . ?
C3' C1' C2' P1' -126.7(3) . . . . ?
C3' C1' C4' F4' 157.3(4) . . . . ?
C3' C1' C4' F5' 38.4(5) . . . . ?
C3' C1' C4' F6' -82.5(5) . . . . ?
C4' C1' C2' P1' 107.6(3) . . . . ?
C4' C1' C3' F1' 40.8(5) . . . . ?
C4' C1' C3' F2' -78.7(4) . . . . ?
C4' C1' C3' F3' 159.0(4) . . . . ?
C5' P1' O1' C1' -116.3(2) . . . . ?
C5' P1' C2' C1' 108.1(3) . . . . ?
C5' C6' C7' C8' 175.9(4) . . . . ?
C5' C6' C11' C10' -176.9(4) . . . . ?
C5' C12' C13' C14' -177.7(4) . . . . ?
C5' C12' C17' C16' 176.6(4) . . . . ?
C5' C18' C19' C20' 179.8(4) . . . . ?
C5' C18' C23' C22' 179.6(4) . . . . ?
C6' C5' C12' C13' 45.7(4) . . . . ?
C6' C5' C12' C17' -129.0(4) . . . . ?
C6' C5' C18' C19' -4.1(5) . . . . ?
C6' C5' C18' C23' 178.7(3) . . . . ?
C6' C7' C8' C9' -0.2(6) . . . . ?
C7' C6' C11' C10' -3.6(6) . . . . ?
C7' C8' C9' C10' -2.4(6) . . . . ?
C8' C9' C10' C11' 1.9(6) . . . . ?
C9' C10' C11' C6' 1.2(6) . . . . ?
C11' C6' C7' C8' 3.1(6) . . . . ?
C12' C5' C6' C7' -105.5(4) . . . . ?
C12' C5' C6' C11' 67.2(4) . . . . ?
C12' C5' C18' C19' -125.9(4) . . . . ?
C12' C5' C18' C23' 56.9(5) . . . . ?
C12' C13' C14' C15' 1.0(7) . . . . ?
C13' C12' C17' C16' 1.9(6) . . . . ?
C13' C14' C15' C16' 1.3(7) . . . . ?
C14' C15' C16' C17' -2.0(6) . . . . ?
C15' C16' C17' C12' 0.3(6) . . . . ?
C17' C12' C13' C14' -2.6(6) . . . . ?
C18' C5' C6' C7' 128.2(4) . . . . ?
C18' C5' C6' C11' -59.1(5) . . . . ?
C18' C5' C12' C13' 171.8(3) . . . . ?
C18' C5' C12' C17' -2.9(5) . . . . ?
C18' C19' C20' C21' 2.1(6) . . . . ?
C19' C18' C23' C22' 2.3(6) . . . . ?
C19' C20' C21' C22' -0.6(6) . . . . ?
C20' C21' C22' C23' -0.1(6) . . . . ?
C21' C22' C23' C18' -0.8(6) . . . . ?
C23' C18' C19' C20' -2.9(6) . . . . ?
_shelx_res_file
;
mo_4641f.res created by SHELXL-2014/7
TITL mo_4641f in P21/n #14
REM reset to P21/n #14
CELL 0.71073 14.539 11.5901 32.829 90 100.6203 90
ZERR 8 0.0008 0.0006 0.0018 0 0.0019 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H O F P W
UNIT 224 136 48 48 8 8
DELU 0.001 0.001 P1' O1'
L.S. 4 0 0
PLAN 5
SIZE 0.05 0.12 0.14
TEMP -123.15
FREE P1' C1'
FREE P C1
BOND
fmap 2 53
MORE -1
BOND $H
ACTA 52
CONF
OMIT -2 56
REM
REM
REM
WGHT 0.016800
FVAR 0.04973
W 6 0.842205 0.658091 0.598493 11.00000 0.02204 0.01464 =
0.01763 0.00175 0.00475 0.00326
P 5 0.862385 0.477814 0.641117 11.00000 0.01673 0.01603 =
0.01822 0.00162 0.00358 0.00103
F1 4 0.719384 0.330138 0.745131 11.00000 0.04323 0.04884 =
0.03067 0.01063 0.02064 -0.00223
F2 4 0.843520 0.266298 0.726798 11.00000 0.03378 0.03339 =
0.03368 0.01150 0.00885 0.00588
F3 4 0.708976 0.229530 0.689645 11.00000 0.04800 0.03199 =
0.04772 -0.00208 0.00885 -0.01803
F4 4 0.662522 0.572948 0.658469 11.00000 0.03217 0.03744 =
0.04184 0.01142 0.01489 0.01352
F5 4 0.685999 0.551407 0.724559 11.00000 0.03151 0.04820 =
0.03464 -0.01541 0.01029 0.00265
F6 4 0.599956 0.430660 0.684462 11.00000 0.01899 0.04429 =
0.04623 -0.00156 0.00546 -0.00870
O1 3 0.766957 0.394686 0.644054 11.00000 0.02130 0.02405 =
0.01839 -0.00100 0.00709 -0.00034
O2 3 0.814064 0.883300 0.544032 11.00000 0.05876 0.02913 =
0.05242 0.02212 0.01772 0.01791
O3 3 0.749754 0.799144 0.663187 11.00000 0.06974 0.03371 =
0.03821 -0.00539 0.02426 0.01188
O4 3 1.029603 0.771808 0.646486 11.00000 0.04709 0.02370 =
0.05238 0.00053 -0.00928 -0.00556
O5 3 0.939961 0.567037 0.525253 11.00000 0.03953 0.02848 =
0.03345 0.00166 0.02015 0.00011
O6 3 0.643813 0.562502 0.552527 11.00000 0.02767 0.03350 =
0.04274 -0.00485 0.00171 0.00044
C1 1 0.764512 0.421009 0.686481 11.00000 0.01781 0.02496 =
0.01389 -0.00131 0.00033 -0.00182
C2 1 0.857897 0.487038 0.696752 11.00000 0.01807 0.02384 =
0.01922 0.00119 0.00645 0.00084
AFIX 23
H2A 2 0.908462 0.444250 0.714906 11.00000 -1.20000
H2B 2 0.852049 0.566618 0.706932 11.00000 -1.20000
AFIX 0
C3 1 0.759862 0.310312 0.712225 11.00000 0.02950 0.02436 =
0.02597 0.00114 0.00926 -0.00751
C4 1 0.677280 0.494973 0.688909 11.00000 0.02290 0.03093 =
0.02177 -0.00433 0.00454 -0.00638
C5 1 0.957329 0.371621 0.631980 11.00000 0.01827 0.01692 =
0.02037 0.00256 0.00631 0.00403
C6 1 1.044835 0.449365 0.641491 11.00000 0.01691 0.01287 =
0.02422 -0.00245 0.00586 0.00644
C7 1 1.076384 0.492183 0.681834 11.00000 0.01915 0.02718 =
0.02327 0.00135 0.00437 0.00497
AFIX 43
H7 2 1.043377 0.471969 0.703224 11.00000 -1.20000
AFIX 0
C8 1 1.153729 0.562495 0.691078 11.00000 0.02947 0.02483 =
0.03258 -0.00124 -0.00421 0.00430
AFIX 43
H8 2 1.174392 0.587751 0.718783 11.00000 -1.20000
AFIX 0
C9 1 1.201757 0.596814 0.660394 11.00000 0.02287 0.02877 =
0.05412 -0.00310 0.00776 -0.00838
AFIX 43
H9 2 1.254884 0.645760 0.666734 11.00000 -1.20000
AFIX 0
C10 1 1.170751 0.558342 0.620369 11.00000 0.02819 0.02646 =
0.04443 -0.00082 0.01353 -0.00497
AFIX 43
H10 2 1.203338 0.581039 0.599113 11.00000 -1.20000
AFIX 0
C11 1 1.093415 0.487623 0.610636 11.00000 0.02101 0.01862 =
0.02816 -0.00248 0.00573 -0.00116
AFIX 43
H11 2 1.072630 0.464394 0.582704 11.00000 -1.20000
AFIX 0
C12 1 0.963048 0.260836 0.658553 11.00000 0.02355 0.01682 =
0.01707 0.00254 0.00820 0.00710
C13 1 1.037776 0.233299 0.689991 11.00000 0.02373 0.02569 =
0.02154 0.00226 0.00627 0.00630
AFIX 43
H13 2 1.088109 0.286269 0.696870 11.00000 -1.20000
AFIX 0
C14 1 1.040246 0.129862 0.711525 11.00000 0.04434 0.03253 =
0.02359 0.00997 0.00687 0.01782
AFIX 43
H14 2 1.091825 0.113247 0.733024 11.00000 -1.20000
AFIX 0
C15 1 0.968370 0.051012 0.701943 11.00000 0.05495 0.02761 =
0.03482 0.01333 0.01632 0.01187
AFIX 43
H15 2 0.969674 -0.018949 0.717116 11.00000 -1.20000
AFIX 0
C16 1 0.894972 0.074605 0.670284 11.00000 0.04000 0.02284 =
0.04026 0.00332 0.01419 -0.00441
AFIX 43
H16 2 0.845663 0.020374 0.663074 11.00000 -1.20000
AFIX 0
C17 1 0.893148 0.178798 0.648714 11.00000 0.02780 0.01842 =
0.03076 0.00794 0.00368 0.00451
AFIX 43
H17 2 0.842437 0.193835 0.626631 11.00000 -1.20000
AFIX 0
C18 1 0.933844 0.331556 0.586329 11.00000 0.01887 0.00602 =
0.02112 0.00259 0.00444 0.00252
C19 1 1.002343 0.274652 0.569114 11.00000 0.02007 0.01498 =
0.02874 0.00333 0.00213 0.00198
AFIX 43
H19 2 1.062105 0.260924 0.585705 11.00000 -1.20000
AFIX 0
C20 1 0.984666 0.238231 0.528577 11.00000 0.03016 0.02025 =
0.02372 0.00012 0.01175 0.00268
AFIX 43
H20 2 1.032783 0.201580 0.517296 11.00000 -1.20000
AFIX 0
C21 1 0.897811 0.254359 0.504129 11.00000 0.03507 0.01683 =
0.02348 0.00009 0.00550 -0.00230
AFIX 43
H21 2 0.886573 0.232466 0.475757 11.00000 -1.20000
AFIX 0
C22 1 0.827309 0.302928 0.521579 11.00000 0.02262 0.01753 =
0.02504 0.00105 -0.00108 -0.00208
AFIX 43
H22 2 0.766083 0.310173 0.505600 11.00000 -1.20000
AFIX 0
C23 1 0.845556 0.340996 0.562190 11.00000 0.02125 0.01639 =
0.02066 0.00191 0.00392 0.00053
AFIX 43
H23 2 0.796449 0.374310 0.573743 11.00000 -1.20000
AFIX 0
C24 1 0.823829 0.801955 0.563902 11.00000 0.02339 0.02750 =
0.03122 0.00013 0.00854 0.00861
C25 1 0.781159 0.744273 0.640478 11.00000 0.03816 0.01973 =
0.02585 0.00353 0.00991 0.00160
C26 1 0.964047 0.725828 0.629209 11.00000 0.03493 0.01627 =
0.02942 0.00602 0.00275 0.00175
C27 1 0.906003 0.593984 0.552598 11.00000 0.02122 0.02084 =
0.02667 0.00601 0.00220 -0.00166
C28 1 0.714610 0.596509 0.568929 11.00000 0.03632 0.01535 =
0.02532 0.00535 0.01304 0.01027
W1' 6 0.448662 -0.109945 0.646404 11.00000 0.02069 0.01456 =
0.02030 0.00212 0.00342 0.00286
P1' 5 0.440399 0.079450 0.610010 11.00000 0.02105 0.01661 =
0.01927 0.00151 0.00568 0.00319
F1' 4 0.587088 0.212518 0.507711 11.00000 0.06880 0.06220 =
0.05278 0.03032 0.04408 0.02789
F2' 4 0.613568 0.317439 0.562829 11.00000 0.03389 0.02874 =
0.10380 0.01345 0.01141 -0.01297
F3' 4 0.473887 0.293712 0.529418 11.00000 0.02968 0.04098 =
0.03640 0.01663 0.00956 0.01264
F4' 4 0.649083 -0.015059 0.600119 11.00000 0.02764 0.03479 =
0.03703 0.00990 0.00412 0.00929
F5' 4 0.710668 0.117557 0.569241 11.00000 0.01915 0.04117 =
0.08442 0.01479 0.01536 -0.00215
F6' 4 0.621909 -0.008599 0.533704 11.00000 0.04578 0.05466 =
0.03562 -0.01341 0.00720 0.01862
O1' 3 0.539596 0.159592 0.610565 11.00000 0.02707 0.02954 =
0.03142 0.00137 0.00934 -0.00098
O2' 3 0.469840 -0.354811 0.689534 11.00000 0.05635 0.02357 =
0.04792 0.01357 0.01189 0.00708
O3' 3 0.552637 -0.232070 0.580970 11.00000 0.05039 0.03534 =
0.05459 -0.01390 0.02585 0.00149
O4' 3 0.636359 -0.018851 0.703007 11.00000 0.03363 0.03799 =
0.03366 -0.00104 -0.00606 0.00036
O5' 3 0.329211 -0.043090 0.714831 11.00000 0.05353 0.04102 =
0.03538 0.00403 0.02517 0.00690
O6' 3 0.267418 -0.203558 0.586437 11.00000 0.04048 0.02446 =
0.06124 -0.00224 -0.01393 -0.00422
C1' 1 0.546841 0.133421 0.568271 11.00000 0.02121 0.02237 =
0.01836 -0.00217 0.00364 0.00108
C2' 1 0.454288 0.073698 0.556694 11.00000 0.01514 0.01466 =
0.02641 0.00291 0.00942 0.00508
AFIX 23
H2'A 2 0.458928 -0.005694 0.546132 11.00000 -1.20000
H2'B 2 0.406926 0.119058 0.537731 11.00000 -1.20000
AFIX 0
C3' 1 0.554985 0.241927 0.542116 11.00000 0.02688 0.03396 =
0.04126 0.01248 0.01377 0.00652
C4' 1 0.633162 0.055868 0.567651 11.00000 0.01732 0.03451 =
0.03212 -0.00140 0.00442 -0.00140
C5' 1 0.346853 0.189109 0.617840 11.00000 0.01643 0.01447 =
0.01655 0.00151 0.00259 0.00440
C6' 1 0.363486 0.222608 0.663720 11.00000 0.01554 0.01756 =
0.01810 0.00051 0.00321 -0.00216
C7' 1 0.446906 0.203544 0.691411 11.00000 0.01823 0.01796 =
0.02518 0.00102 -0.00258 0.00111
AFIX 43
H7' 2 0.496196 0.163074 0.682283 11.00000 -1.20000
AFIX 0
C8' 1 0.459548 0.242315 0.731966 11.00000 0.02646 0.02147 =
0.02124 0.00023 -0.01062 -0.00377
AFIX 43
H8' 2 0.517048 0.227970 0.750273 11.00000 -1.20000
AFIX 0
C9' 1 0.389383 0.301464 0.745914 11.00000 0.03827 0.02264 =
0.02001 -0.00613 0.00025 -0.00598
AFIX 43
H9' 2 0.397329 0.325448 0.774016 11.00000 -1.20000
AFIX 0
C10' 1 0.307575 0.325606 0.718815 11.00000 0.02813 0.02074 =
0.02589 -0.00482 0.00543 -0.00026
AFIX 43
H10' 2 0.259595 0.368422 0.728041 11.00000 -1.20000
AFIX 0
C11' 1 0.294925 0.287759 0.678176 11.00000 0.01713 0.02480 =
0.01855 -0.00067 -0.00106 0.00100
AFIX 43
H11' 2 0.238575 0.306343 0.659694 11.00000 -1.20000
AFIX 0
C12' 1 0.349841 0.302737 0.593656 11.00000 0.01874 0.01338 =
0.01568 -0.00060 0.00240 0.00253
C13' 1 0.422543 0.380492 0.607900 11.00000 0.02315 0.02413 =
0.02765 0.00699 -0.00177 -0.00143
AFIX 43
H13' 2 0.468843 0.360208 0.631171 11.00000 -1.20000
AFIX 0
C14' 1 0.428473 0.486194 0.588849 11.00000 0.02534 0.02190 =
0.03506 0.00472 -0.00001 -0.00887
AFIX 43
H14' 2 0.479081 0.536628 0.598904 11.00000 -1.20000
AFIX 0
C15' 1 0.361839 0.518638 0.555573 11.00000 0.03678 0.01603 =
0.03112 0.00782 0.00567 0.00197
AFIX 43
H15' 2 0.366613 0.590434 0.542157 11.00000 -1.20000
AFIX 0
C16' 1 0.287856 0.445391 0.541919 11.00000 0.02815 0.02366 =
0.02320 0.00629 -0.00284 0.00183
AFIX 43
H16' 2 0.240324 0.468107 0.519465 11.00000 -1.20000
AFIX 0
C17' 1 0.281951 0.338186 0.560704 11.00000 0.02271 0.01664 =
0.01862 0.00057 -0.00087 -0.00069
AFIX 43
H17' 2 0.230580 0.288803 0.550730 11.00000 -1.20000
AFIX 0
C18' 1 0.256823 0.116809 0.603639 11.00000 0.01184 0.00883 =
0.02676 -0.00176 0.00001 0.00270
C19' 1 0.200395 0.079822 0.631042 11.00000 0.02071 0.01903 =
0.02117 -0.00042 0.00541 0.00171
AFIX 43
H19' 2 0.217267 0.099027 0.659576 11.00000 -1.20000
AFIX 0
C20' 1 0.120066 0.015531 0.617581 11.00000 0.01889 0.02472 =
0.03448 -0.00179 0.00928 -0.00007
AFIX 43
H20' 2 0.081721 -0.006337 0.636795 11.00000 -1.20000
AFIX 0
C21' 1 0.095324 -0.016898 0.576739 11.00000 0.02132 0.01762 =
0.04182 -0.00200 0.00040 -0.00261
AFIX 43
H21' 2 0.040580 -0.061498 0.567619 11.00000 -1.20000
AFIX 0
C22' 1 0.152045 0.016883 0.548991 11.00000 0.03515 0.01582 =
0.02353 -0.00058 -0.00564 -0.00221
AFIX 43
H22' 2 0.135688 -0.005112 0.520704 11.00000 -1.20000
AFIX 0
C23' 1 0.231535 0.081723 0.561928 11.00000 0.02191 0.01801 =
0.02035 -0.00202 0.00255 0.00150
AFIX 43
H23' 2 0.269675 0.102997 0.542561 11.00000 -1.20000
AFIX 0
C24' 1 0.462299 -0.265544 0.674219 11.00000 0.02959 0.02722 =
0.02558 0.00087 0.00729 0.00482
C25' 1 0.518107 -0.183082 0.604365 11.00000 0.03151 0.02397 =
0.03421 0.00375 0.00451 -0.00023
C26' 1 0.570261 -0.053646 0.682698 11.00000 0.02940 0.01876 =
0.02040 0.00175 0.00256 0.00711
C27' 1 0.372066 -0.061085 0.689609 11.00000 0.03279 0.01988 =
0.02949 0.00237 0.00217 0.00201
C28' 1 0.330032 -0.165835 0.608107 11.00000 0.03238 0.01793 =
0.02692 0.00797 0.00308 0.00522
HKLF 4
REM mo_4641f in P21/n #14
REM R1 = 0.0384 for 9555 Fo > 4sig(Fo) and 0.0720 for all 13119 data
REM 757 parameters refined using 1 restraints
END
WGHT 0.0168 0.0000
REM Highest difference peak 1.025, deepest hole -1.079, 1-sigma level 0.159
Q1 1 0.8868 0.6596 0.6224 11.00000 0.05 1.03
Q2 1 0.4027 -0.1078 0.6168 11.00000 0.05 0.85
Q3 1 0.4808 0.0794 0.5781 11.00000 0.05 0.71
Q4 1 0.4581 -0.1138 0.5987 11.00000 0.05 0.62
Q5 1 0.7667 0.6655 0.5793 11.00000 0.05 0.61
;
_shelx_res_checksum 45195
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_4737
_database_code_depnum_ccdc_archive 'CCDC 1526598'
_audit_update_record
;
2017-01-10 deposited with the CCDC.
2017-02-03 downloaded from the CCDC.
;
_audit_creation_date 2016-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number 2013-2
_chemical_name_common ?
_chemical_name_systematic PB-35
_chemical_formula_moiety 'C30 H23 F6 O7 P Si W'
_chemical_formula_sum 'C30 H23 F6 O7 P Si W'
_chemical_formula_weight 852.39
_chemical_melting_point ?
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.9870(3)
_cell_length_b 13.1455(3)
_cell_length_c 13.3173(2)
_cell_angle_alpha 87.0836(15)
_cell_angle_beta 82.7857(15)
_cell_angle_gamma 89.8868(13)
_cell_volume 1558.80(7)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 5798
_cell_measurement_temperature 123
_cell_measurement_theta_max 29.13
_cell_measurement_theta_min 1.00
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.877
_exptl_absorpt_correction_T_max 1.071
_exptl_absorpt_correction_T_min 0.5781
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.816
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 832
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.1
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0446
_diffrn_reflns_av_unetI/netI 0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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 20755
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 27.999
_diffrn_reflns_theta_min 2.591
_diffrn_ambient_temperature 123
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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_source 'sealed tube'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7053
_reflns_number_total 7500
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_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 'XS (Sheldrick, 2008)'
_refine_diff_density_max 1.141
_refine_diff_density_min -1.740
_refine_diff_density_rms 0.154
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 417
_refine_ls_number_reflns 7500
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0277
_refine_ls_R_factor_gt 0.0249
_refine_ls_restrained_S_all 1.025
_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^)+(0.0224P)^2^+2.0713P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0582
_refine_ls_wR_factor_ref 0.0598
_refine_special_details
;
?
;
_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:
C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
W W 0.72701(2) 0.82418(2) 0.54809(2) 0.01911(4) Uani 1 1 d . . . . .
P P 0.70739(7) 0.76208(5) 0.73286(5) 0.01585(12) Uani 1 1 d . . . . .
Si Si 0.94548(10) 0.61043(6) 0.74400(7) 0.02701(17) Uani 1 1 d . . . . .
F1 F 0.4769(3) 0.46819(17) 0.88068(18) 0.0519(6) Uani 1 1 d . . . . .
F2 F 0.6959(3) 0.50559(14) 0.91590(14) 0.0401(5) Uani 1 1 d . . . . .
F3 F 0.6659(3) 0.37611(14) 0.82926(17) 0.0536(6) Uani 1 1 d . . . . .
F4 F 0.6372(3) 0.40413(15) 0.63615(17) 0.0490(6) Uani 1 1 d . . . . .
F5 F 0.5919(3) 0.55359(15) 0.57765(16) 0.0483(6) Uani 1 1 d . . . . .
F6 F 0.4309(3) 0.47797(18) 0.68843(19) 0.0547(6) Uani 1 1 d . . . . .
O1 O 0.8651(2) 0.72216(14) 0.76752(14) 0.0205(4) Uani 1 1 d . . . . .
O2 O 0.8060(2) 0.53928(15) 0.71406(16) 0.0274(4) Uani 1 1 d . . . . .
O3 O 0.7322(3) 0.9095(2) 0.32274(16) 0.0415(6) Uani 1 1 d . . . . .
O4 O 0.3974(3) 0.74073(19) 0.53701(18) 0.0383(5) Uani 1 1 d . . . . .
O5 O 0.6067(2) 1.05042(16) 0.56986(15) 0.0267(4) Uani 1 1 d . . . . .
O6 O 1.0621(3) 0.89787(18) 0.55844(17) 0.0328(5) Uani 1 1 d . . . . .
O7 O 0.8605(4) 0.6266(2) 0.4445(2) 0.0636(9) Uani 1 1 d . . . . .
C1 C 0.6504(3) 0.54135(19) 0.7460(2) 0.0214(5) Uani 1 1 d . . . . .
C2 C 0.5829(3) 0.64879(19) 0.7679(2) 0.0199(5) Uani 1 1 d . . . . .
H2A H 0.5475 0.6495 0.8414 0.024 Uiso 1 1 calc R . . . .
H2B H 0.4936 0.6573 0.7317 0.024 Uiso 1 1 calc R . . . .
C3 C 1.0221(4) 0.5592(3) 0.8582(3) 0.0449(9) Uani 1 1 d . . . . .
H3A H 1.1205 0.5901 0.8614 0.067 Uiso 1 1 calc GR . . . .
H3B H 1.0327 0.4852 0.8554 0.067 Uiso 1 1 calc GR . . . .
H3C H 0.9539 0.5752 0.9186 0.067 Uiso 1 1 calc GR . . . .
C4 C 1.0909(4) 0.6183(3) 0.6341(3) 0.0417(8) Uani 1 1 d . . . . .
H4A H 1.0496 0.6508 0.5759 0.063 Uiso 1 1 calc GR . . . .
H4B H 1.1253 0.5496 0.6178 0.063 Uiso 1 1 calc GR . . . .
H4C H 1.1757 0.6587 0.6500 0.063 Uiso 1 1 calc GR . . . .
C5 C 0.6209(4) 0.4710(2) 0.8431(3) 0.0340(7) Uani 1 1 d . . . . .
C6 C 0.5778(4) 0.4934(2) 0.6605(3) 0.0333(7) Uani 1 1 d . . . . .
C7 C 0.6383(3) 0.85394(18) 0.84000(18) 0.0148(5) Uani 1 1 d . . . . .
C8 C 0.6793(3) 0.96317(18) 0.79915(18) 0.0155(5) Uani 1 1 d . . . . .
C9 C 0.8275(3) 0.9857(2) 0.75921(19) 0.0187(5) Uani 1 1 d . . . . .
H9 H 0.8994 0.9326 0.7542 0.022 Uiso 1 1 calc R . . . .
C10 C 0.8716(3) 1.0845(2) 0.7266(2) 0.0237(6) Uani 1 1 d . . . . .
H10 H 0.9726 1.0984 0.6990 0.028 Uiso 1 1 calc R . . . .
C11 C 0.7673(4) 1.1630(2) 0.7345(2) 0.0263(6) Uani 1 1 d . . . . .
H11 H 0.7962 1.2304 0.7112 0.032 Uiso 1 1 calc R . . . .
C12 C 0.6214(3) 1.1422(2) 0.7764(2) 0.0235(6) Uani 1 1 d . . . . .
H12 H 0.5505 1.1959 0.7832 0.028 Uiso 1 1 calc R . . . .
C13 C 0.5771(3) 1.04285(19) 0.80880(19) 0.0190(5) Uani 1 1 d . . . . .
H13 H 0.4765 1.0296 0.8377 0.023 Uiso 1 1 calc R . . . .
C14 C 0.4676(3) 0.83951(18) 0.86026(19) 0.0161(5) Uani 1 1 d . . . . .
C15 C 0.3804(3) 0.8558(2) 0.7807(2) 0.0193(5) Uani 1 1 d . . . . .
H15 H 0.4281 0.8764 0.7151 0.023 Uiso 1 1 calc R . . . .
C16 C 0.2260(3) 0.8425(2) 0.7958(2) 0.0232(6) Uani 1 1 d . . . . .
H16 H 0.1697 0.8530 0.7404 0.028 Uiso 1 1 calc R . . . .
C17 C 0.1530(3) 0.8139(2) 0.8914(2) 0.0256(6) Uani 1 1 d . . . . .
H17 H 0.0472 0.8048 0.9019 0.031 Uiso 1 1 calc R . . . .
C18 C 0.2377(3) 0.7988(2) 0.9712(2) 0.0260(6) Uani 1 1 d . . . . .
H18 H 0.1892 0.7796 1.0370 0.031 Uiso 1 1 calc R . . . .
C19 C 0.3928(3) 0.8115(2) 0.9560(2) 0.0206(5) Uani 1 1 d . . . . .
H19 H 0.4486 0.8009 1.0117 0.025 Uiso 1 1 calc R . . . .
C20 C 0.7149(3) 0.8319(2) 0.93671(19) 0.0172(5) Uani 1 1 d . . . . .
C21 C 0.7731(3) 0.9110(2) 0.98652(19) 0.0202(5) Uani 1 1 d . . . . .
H21 H 0.7687 0.9789 0.9590 0.024 Uiso 1 1 calc R . . . .
C22 C 0.8373(3) 0.8925(2) 1.0756(2) 0.0250(6) Uani 1 1 d . . . . .
H22 H 0.8762 0.9476 1.1080 0.030 Uiso 1 1 calc R . . . .
C23 C 0.8446(3) 0.7940(2) 1.1170(2) 0.0261(6) Uani 1 1 d . . . . .
H23 H 0.8900 0.7809 1.1770 0.031 Uiso 1 1 calc R . . . .
C24 C 0.7852(4) 0.7156(2) 1.0702(2) 0.0273(6) Uani 1 1 d . . . . .
H24 H 0.7883 0.6479 1.0986 0.033 Uiso 1 1 calc R . . . .
C25 C 0.7208(3) 0.7343(2) 0.9814(2) 0.0235(6) Uani 1 1 d . . . . .
H25 H 0.6797 0.6790 0.9506 0.028 Uiso 1 1 calc R . . . .
C26 C 0.7332(3) 0.8766(2) 0.4034(2) 0.0269(6) Uani 1 1 d . . . . .
C27 C 0.5152(3) 0.7713(2) 0.5421(2) 0.0247(6) Uani 1 1 d . . . . .
C28 C 0.6487(3) 0.9682(2) 0.57156(19) 0.0199(5) Uani 1 1 d . . . . .
C29 C 0.9416(3) 0.8720(2) 0.5550(2) 0.0225(6) Uani 1 1 d . . . . .
C30 C 0.8126(4) 0.6939(3) 0.4891(3) 0.0379(8) 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 0.01856(6) 0.02209(6) 0.01714(6) -0.00456(4) -0.00269(4) 0.00196(4)
P 0.0143(3) 0.0134(3) 0.0204(3) -0.0030(2) -0.0037(2) 0.0005(2)
Si 0.0221(4) 0.0186(4) 0.0409(5) -0.0037(3) -0.0055(3) 0.0048(3)
F1 0.0489(14) 0.0449(12) 0.0574(14) 0.0099(10) 0.0067(11) -0.0187(10)
F2 0.0596(14) 0.0271(9) 0.0344(10) 0.0028(8) -0.0107(9) -0.0017(9)
F3 0.0919(19) 0.0163(9) 0.0522(13) -0.0005(8) -0.0080(12) 0.0048(10)
F4 0.0695(16) 0.0274(10) 0.0544(13) -0.0190(9) -0.0172(11) 0.0033(10)
F5 0.0760(17) 0.0339(11) 0.0397(11) -0.0070(8) -0.0236(11) -0.0077(10)
F6 0.0378(13) 0.0584(14) 0.0717(16) -0.0259(12) -0.0124(11) -0.0135(11)
O1 0.0164(9) 0.0184(9) 0.0276(10) -0.0041(7) -0.0049(7) 0.0024(7)
O2 0.0248(11) 0.0198(9) 0.0381(11) -0.0076(8) -0.0028(9) 0.0018(8)
O3 0.0313(13) 0.0737(18) 0.0185(10) 0.0009(10) -0.0006(9) 0.0093(12)
O4 0.0317(13) 0.0431(13) 0.0415(13) -0.0009(10) -0.0100(10) -0.0132(11)
O5 0.0290(11) 0.0281(11) 0.0245(10) -0.0028(8) -0.0092(8) 0.0051(9)
O6 0.0223(11) 0.0432(13) 0.0327(11) 0.0003(10) -0.0035(9) -0.0023(10)
O7 0.077(2) 0.0487(17) 0.067(2) -0.0330(15) -0.0044(17) 0.0183(16)
C1 0.0224(14) 0.0143(12) 0.0278(13) -0.0035(10) -0.0037(11) -0.0024(10)
C2 0.0184(13) 0.0158(12) 0.0257(13) -0.0019(10) -0.0031(10) -0.0019(10)
C3 0.042(2) 0.0272(16) 0.068(2) 0.0049(16) -0.0212(19) 0.0089(15)
C4 0.0287(18) 0.0304(17) 0.064(2) -0.0130(16) 0.0080(16) 0.0049(14)
C5 0.045(2) 0.0177(13) 0.0392(17) -0.0024(12) -0.0030(15) -0.0041(13)
C6 0.0368(18) 0.0212(14) 0.0433(18) -0.0112(13) -0.0072(14) -0.0036(13)
C7 0.0133(12) 0.0144(11) 0.0174(11) -0.0019(9) -0.0037(9) 0.0014(9)
C8 0.0164(12) 0.0153(11) 0.0161(11) -0.0029(9) -0.0055(9) -0.0008(9)
C9 0.0184(13) 0.0200(12) 0.0185(11) -0.0041(9) -0.0041(10) 0.0006(10)
C10 0.0232(14) 0.0240(13) 0.0238(13) -0.0028(10) -0.0018(11) -0.0063(11)
C11 0.0359(17) 0.0167(12) 0.0266(14) -0.0016(10) -0.0045(12) -0.0045(12)
C12 0.0287(15) 0.0176(12) 0.0249(13) -0.0050(10) -0.0051(11) 0.0053(11)
C13 0.0199(13) 0.0173(12) 0.0200(12) -0.0039(9) -0.0022(10) 0.0009(10)
C14 0.0143(12) 0.0146(11) 0.0196(11) -0.0025(9) -0.0026(9) 0.0009(9)
C15 0.0167(13) 0.0206(12) 0.0212(12) -0.0029(10) -0.0037(10) 0.0008(10)
C16 0.0162(13) 0.0289(14) 0.0262(13) -0.0050(11) -0.0070(11) 0.0013(11)
C17 0.0142(13) 0.0298(15) 0.0326(15) -0.0051(12) -0.0006(11) -0.0012(11)
C18 0.0195(14) 0.0311(15) 0.0260(14) -0.0004(11) 0.0017(11) -0.0025(11)
C19 0.0179(13) 0.0228(13) 0.0212(12) -0.0012(10) -0.0019(10) -0.0004(10)
C20 0.0140(12) 0.0208(12) 0.0172(11) -0.0024(9) -0.0035(9) 0.0012(10)
C21 0.0209(13) 0.0208(12) 0.0192(12) -0.0041(10) -0.0027(10) 0.0003(10)
C22 0.0254(15) 0.0287(14) 0.0224(13) -0.0075(11) -0.0070(11) -0.0012(12)
C23 0.0252(15) 0.0341(15) 0.0204(13) -0.0025(11) -0.0076(11) 0.0057(12)
C24 0.0305(16) 0.0261(14) 0.0263(14) 0.0028(11) -0.0091(12) 0.0055(12)
C25 0.0278(15) 0.0199(13) 0.0242(13) -0.0005(10) -0.0089(11) 0.0000(11)
C26 0.0194(14) 0.0400(17) 0.0221(13) -0.0080(12) -0.0026(11) 0.0063(12)
C27 0.0246(15) 0.0295(15) 0.0207(13) -0.0032(11) -0.0043(11) -0.0010(12)
C28 0.0171(13) 0.0265(14) 0.0165(11) -0.0016(10) -0.0037(9) -0.0008(11)
C29 0.0201(14) 0.0297(14) 0.0171(12) -0.0008(10) -0.0011(10) 0.0052(11)
C30 0.040(2) 0.0378(18) 0.0368(17) -0.0115(14) -0.0063(15) 0.0062(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W P 2.5376(7) . ?
W C26 2.007(3) . ?
W C27 2.040(3) . ?
W C28 2.044(3) . ?
W C29 2.044(3) . ?
W C30 2.030(3) . ?
P O1 1.623(2) . ?
P C2 1.869(3) . ?
P C7 1.957(3) . ?
Si O1 1.662(2) . ?
Si O2 1.665(2) . ?
Si C3 1.844(4) . ?
Si C4 1.834(4) . ?
F1 C5 1.327(4) . ?
F2 C5 1.347(4) . ?
F3 C5 1.326(4) . ?
F4 C6 1.326(4) . ?
F5 C6 1.318(4) . ?
F6 C6 1.339(4) . ?
O2 C1 1.410(3) . ?
O3 C26 1.139(4) . ?
O4 C27 1.144(4) . ?
O5 C28 1.144(3) . ?
O6 C29 1.143(4) . ?
O7 C30 1.145(4) . ?
C1 C2 1.563(4) . ?
C1 C5 1.545(4) . ?
C1 C6 1.544(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C7 C8 1.538(3) . ?
C7 C14 1.535(3) . ?
C7 C20 1.549(3) . ?
C8 C9 1.397(4) . ?
C8 C13 1.392(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.391(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.381(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.397(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.403(4) . ?
C14 C19 1.397(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.392(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.398(4) . ?
C20 C25 1.391(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.393(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.387(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.374(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.391(4) . ?
C25 H25 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
C26 W P 177.30(8) . . ?
C26 W C27 88.72(12) . . ?
C26 W C28 80.73(11) . . ?
C26 W C29 92.21(11) . . ?
C26 W C30 85.42(13) . . ?
C27 W P 89.56(8) . . ?
C27 W C28 91.29(11) . . ?
C27 W C29 177.99(11) . . ?
C28 W P 97.23(7) . . ?
C29 W P 89.58(7) . . ?
C29 W C28 90.62(11) . . ?
C30 W P 96.66(10) . . ?
C30 W C27 89.89(14) . . ?
C30 W C28 166.07(12) . . ?
C30 W C29 88.41(13) . . ?
O1 P W 113.69(7) . . ?
O1 P C2 101.81(11) . . ?
O1 P C7 101.67(10) . . ?
C2 P W 114.98(9) . . ?
C2 P C7 101.91(11) . . ?
C7 P W 120.28(7) . . ?
O1 Si O2 103.66(11) . . ?
O1 Si C3 109.34(15) . . ?
O1 Si C4 112.58(13) . . ?
O2 Si C3 112.45(15) . . ?
O2 Si C4 107.57(15) . . ?
C4 Si C3 111.05(19) . . ?
P O1 Si 126.51(12) . . ?
C1 O2 Si 131.04(18) . . ?
O2 C1 C2 115.7(2) . . ?
O2 C1 C5 107.1(2) . . ?
O2 C1 C6 105.0(2) . . ?
C5 C1 C2 109.3(2) . . ?
C6 C1 C2 110.8(2) . . ?
C6 C1 C5 108.8(2) . . ?
P C2 H2A 107.9 . . ?
P C2 H2B 107.9 . . ?
C1 C2 P 117.63(19) . . ?
C1 C2 H2A 107.9 . . ?
C1 C2 H2B 107.9 . . ?
H2A C2 H2B 107.2 . . ?
Si C3 H3A 109.5 . . ?
Si C3 H3B 109.5 . . ?
Si C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si C4 H4A 109.5 . . ?
Si C4 H4B 109.5 . . ?
Si C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
F1 C5 F2 106.6(3) . . ?
F1 C5 C1 112.2(3) . . ?
F2 C5 C1 110.1(2) . . ?
F3 C5 F1 108.0(3) . . ?
F3 C5 F2 106.4(3) . . ?
F3 C5 C1 113.2(3) . . ?
F4 C6 F6 107.2(3) . . ?
F4 C6 C1 112.7(3) . . ?
F5 C6 F4 107.6(3) . . ?
F5 C6 F6 107.3(3) . . ?
F5 C6 C1 111.2(2) . . ?
F6 C6 C1 110.6(3) . . ?
C8 C7 P 107.55(16) . . ?
C8 C7 C20 108.3(2) . . ?
C14 C7 P 105.68(16) . . ?
C14 C7 C8 111.0(2) . . ?
C14 C7 C20 112.1(2) . . ?
C20 C7 P 112.17(16) . . ?
C9 C8 C7 119.2(2) . . ?
C13 C8 C7 122.3(2) . . ?
C13 C8 C9 118.3(2) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 C8 121.2(3) . . ?
C10 C9 H9 119.4 . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.8(3) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(3) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.6(3) . . ?
C13 C12 H12 119.7 . . ?
C8 C13 C12 120.5(3) . . ?
C8 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C7 119.7(2) . . ?
C19 C14 C7 122.8(2) . . ?
C19 C14 C15 117.5(2) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.4(2) . . ?
C16 C15 H15 119.3 . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.5(3) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 H17 120.6 . . ?
C18 C17 C16 118.7(3) . . ?
C18 C17 H17 120.6 . . ?
C17 C18 H18 119.6 . . ?
C17 C18 C19 120.8(3) . . ?
C19 C18 H18 119.6 . . ?
C14 C19 H19 119.5 . . ?
C18 C19 C14 121.0(2) . . ?
C18 C19 H19 119.5 . . ?
C21 C20 C7 120.9(2) . . ?
C25 C20 C7 122.0(2) . . ?
C25 C20 C21 117.0(2) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 C20 121.5(2) . . ?
C22 C21 H21 119.3 . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.2(3) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 120.4 . . ?
C24 C23 C22 119.1(3) . . ?
C24 C23 H23 120.4 . . ?
C23 C24 H24 119.7 . . ?
C23 C24 C25 120.6(3) . . ?
C25 C24 H24 119.7 . . ?
C20 C25 H25 119.2 . . ?
C24 C25 C20 121.7(3) . . ?
C24 C25 H25 119.2 . . ?
O3 C26 W 177.0(3) . . ?
O4 C27 W 178.6(3) . . ?
O5 C28 W 170.2(2) . . ?
O6 C29 W 179.3(3) . . ?
O7 C30 W 171.6(3) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W P O1 Si -77.94(15) . . . . ?
W P C2 C1 82.4(2) . . . . ?
P C7 C8 C9 -53.4(3) . . . . ?
P C7 C8 C13 132.6(2) . . . . ?
P C7 C14 C15 -57.2(3) . . . . ?
P C7 C14 C19 123.5(2) . . . . ?
P C7 C20 C21 133.9(2) . . . . ?
P C7 C20 C25 -50.2(3) . . . . ?
Si O2 C1 C2 33.4(3) . . . . ?
Si O2 C1 C5 -88.7(3) . . . . ?
Si O2 C1 C6 155.8(2) . . . . ?
O1 P C2 C1 -41.0(2) . . . . ?
O1 Si O2 C1 -30.4(3) . . . . ?
O2 Si O1 P -18.16(18) . . . . ?
O2 C1 C2 P 8.2(3) . . . . ?
O2 C1 C5 F1 179.3(2) . . . . ?
O2 C1 C5 F2 60.7(3) . . . . ?
O2 C1 C5 F3 -58.2(3) . . . . ?
O2 C1 C6 F4 51.4(3) . . . . ?
O2 C1 C6 F5 -69.6(3) . . . . ?
O2 C1 C6 F6 171.4(2) . . . . ?
C2 P O1 Si 46.32(17) . . . . ?
C2 C1 C5 F1 53.3(3) . . . . ?
C2 C1 C5 F2 -65.2(3) . . . . ?
C2 C1 C5 F3 175.8(3) . . . . ?
C2 C1 C6 F4 176.9(2) . . . . ?
C2 C1 C6 F5 56.0(3) . . . . ?
C2 C1 C6 F6 -63.1(3) . . . . ?
C3 Si O1 P -138.28(18) . . . . ?
C3 Si O2 C1 87.6(3) . . . . ?
C4 Si O1 P 97.8(2) . . . . ?
C4 Si O2 C1 -149.9(2) . . . . ?
C5 C1 C2 P 129.1(2) . . . . ?
C5 C1 C6 F4 -62.9(3) . . . . ?
C5 C1 C6 F5 176.1(3) . . . . ?
C5 C1 C6 F6 57.0(3) . . . . ?
C6 C1 C2 P -111.1(2) . . . . ?
C6 C1 C5 F1 -67.8(3) . . . . ?
C6 C1 C5 F2 173.7(3) . . . . ?
C6 C1 C5 F3 54.7(4) . . . . ?
C7 P O1 Si 151.31(14) . . . . ?
C7 P C2 C1 -145.8(2) . . . . ?
C7 C8 C9 C10 -176.4(2) . . . . ?
C7 C8 C13 C12 176.0(2) . . . . ?
C7 C14 C15 C16 179.3(2) . . . . ?
C7 C14 C19 C18 -179.8(2) . . . . ?
C7 C20 C21 C22 177.7(2) . . . . ?
C7 C20 C25 C24 -177.8(3) . . . . ?
C8 C7 C14 C15 59.1(3) . . . . ?
C8 C7 C14 C19 -120.1(3) . . . . ?
C8 C7 C20 C21 15.3(3) . . . . ?
C8 C7 C20 C25 -168.7(2) . . . . ?
C8 C9 C10 C11 0.6(4) . . . . ?
C9 C8 C13 C12 1.9(4) . . . . ?
C9 C10 C11 C12 1.2(4) . . . . ?
C10 C11 C12 C13 -1.4(4) . . . . ?
C11 C12 C13 C8 -0.2(4) . . . . ?
C13 C8 C9 C10 -2.1(4) . . . . ?
C14 C7 C8 C9 -168.6(2) . . . . ?
C14 C7 C8 C13 17.4(3) . . . . ?
C14 C7 C20 C21 -107.4(3) . . . . ?
C14 C7 C20 C25 68.5(3) . . . . ?
C14 C15 C16 C17 1.0(4) . . . . ?
C15 C14 C19 C18 1.0(4) . . . . ?
C15 C16 C17 C18 -0.1(4) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
C17 C18 C19 C14 -0.1(4) . . . . ?
C19 C14 C15 C16 -1.4(4) . . . . ?
C20 C7 C8 C9 68.0(3) . . . . ?
C20 C7 C8 C13 -106.0(3) . . . . ?
C20 C7 C14 C15 -179.7(2) . . . . ?
C20 C7 C14 C19 1.1(3) . . . . ?
C20 C21 C22 C23 -0.1(4) . . . . ?
C21 C20 C25 C24 -1.7(4) . . . . ?
C21 C22 C23 C24 -1.2(5) . . . . ?
C22 C23 C24 C25 1.0(5) . . . . ?
C23 C24 C25 C20 0.5(5) . . . . ?
C25 C20 C21 C22 1.6(4) . . . . ?
_shelx_res_file
;
TITL 4737 in P-1 #2
REM reset to P-1 #2
CELL 0.71073 8.987 13.1455 13.3173 87.0836 82.7857 89.8868
ZERR 2 0.00029 0.00029 0.0002 0.0015 0.0015 0.0013
LATT 1
SFAC C H F O P Si W
UNIT 60 46 12 14 2 2 2
L.S. 4
PLAN 5
TEMP -150.15
BOND
MORE -1
BOND $H
CONF
fmap 2
acta 52
OMIT -2 56
OMIT 0 1 1
OMIT 0 1 0
OMIT 0 -1 1
OMIT 1 1 1
REM
REM
REM
WGHT 0.022400 2.071300
FVAR 0.35736
W 7 0.727011 0.824176 0.548093 11.00000 0.01856 0.02209 =
0.01714 -0.00456 -0.00269 0.00196
P 5 0.707393 0.762078 0.732864 11.00000 0.01432 0.01343 =
0.02041 -0.00298 -0.00371 0.00054
SI 6 0.945483 0.610431 0.743997 11.00000 0.02207 0.01864 =
0.04092 -0.00365 -0.00548 0.00477
F1 3 0.476920 0.468192 0.880679 11.00000 0.04891 0.04491 =
0.05736 0.00989 0.00673 -0.01868
F2 3 0.695943 0.505585 0.915901 11.00000 0.05956 0.02707 =
0.03442 0.00284 -0.01067 -0.00174
F3 3 0.665944 0.376106 0.829264 11.00000 0.09189 0.01630 =
0.05218 -0.00053 -0.00797 0.00478
F4 3 0.637234 0.404126 0.636150 11.00000 0.06947 0.02735 =
0.05443 -0.01899 -0.01719 0.00330
F5 3 0.591883 0.553590 0.577651 11.00000 0.07602 0.03391 =
0.03971 -0.00701 -0.02362 -0.00771
F6 3 0.430918 0.477965 0.688432 11.00000 0.03782 0.05839 =
0.07174 -0.02586 -0.01238 -0.01347
O1 4 0.865115 0.722157 0.767516 11.00000 0.01640 0.01842 =
0.02757 -0.00415 -0.00490 0.00236
O2 4 0.806028 0.539278 0.714055 11.00000 0.02481 0.01978 =
0.03805 -0.00760 -0.00275 0.00184
O3 4 0.732230 0.909491 0.322737 11.00000 0.03131 0.07374 =
0.01846 0.00095 -0.00057 0.00926
O4 4 0.397442 0.740733 0.537011 11.00000 0.03171 0.04309 =
0.04146 -0.00089 -0.01001 -0.01319
O5 4 0.606749 1.050423 0.569857 11.00000 0.02899 0.02811 =
0.02453 -0.00278 -0.00923 0.00509
O6 4 1.062092 0.897873 0.558439 11.00000 0.02228 0.04322 =
0.03274 0.00027 -0.00353 -0.00229
O7 4 0.860530 0.626569 0.444516 11.00000 0.07688 0.04867 =
0.06709 -0.03301 -0.00440 0.01835
C1 1 0.650427 0.541353 0.746032 11.00000 0.02239 0.01433 =
0.02779 -0.00355 -0.00369 -0.00243
C2 1 0.582902 0.648788 0.767938 11.00000 0.01836 0.01582 =
0.02575 -0.00190 -0.00306 -0.00188
AFIX 23
H2A 2 0.547548 0.649540 0.841362 11.00000 -1.20000
H2B 2 0.493629 0.657258 0.731719 11.00000 -1.20000
AFIX 0
C3 1 1.022128 0.559213 0.858235 11.00000 0.04198 0.02723 =
0.06821 0.00490 -0.02120 0.00886
AFIX 137
H3A 2 1.120505 0.590056 0.861414 11.00000 -1.50000
H3B 2 1.032746 0.485172 0.855362 11.00000 -1.50000
H3C 2 0.953873 0.575187 0.918649 11.00000 -1.50000
AFIX 0
C4 1 1.090945 0.618284 0.634141 11.00000 0.02868 0.03040 =
0.06355 -0.01295 0.00804 0.00486
AFIX 137
H4A 2 1.049591 0.650779 0.575892 11.00000 -1.50000
H4B 2 1.125270 0.549564 0.617835 11.00000 -1.50000
H4C 2 1.175688 0.658704 0.650006 11.00000 -1.50000
AFIX 0
C5 1 0.620869 0.471020 0.843052 11.00000 0.04461 0.01765 =
0.03918 -0.00244 -0.00298 -0.00407
C6 1 0.577789 0.493357 0.660494 11.00000 0.03684 0.02123 =
0.04327 -0.01118 -0.00716 -0.00362
C7 1 0.638346 0.853942 0.840000 11.00000 0.01333 0.01441 =
0.01735 -0.00190 -0.00366 0.00139
C8 1 0.679326 0.963174 0.799146 11.00000 0.01639 0.01526 =
0.01606 -0.00293 -0.00552 -0.00085
C9 1 0.827472 0.985739 0.759214 11.00000 0.01837 0.02000 =
0.01851 -0.00407 -0.00406 0.00059
AFIX 43
H9 2 0.899424 0.932608 0.754249 11.00000 -1.20000
AFIX 0
C10 1 0.871603 1.084530 0.726590 11.00000 0.02316 0.02400 =
0.02384 -0.00281 -0.00183 -0.00632
AFIX 43
H10 2 0.972624 1.098411 0.699014 11.00000 -1.20000
AFIX 0
C11 1 0.767288 1.162957 0.734482 11.00000 0.03586 0.01666 =
0.02659 -0.00164 -0.00454 -0.00451
AFIX 43
H11 2 0.796231 1.230399 0.711195 11.00000 -1.20000
AFIX 0
C12 1 0.621391 1.142165 0.776378 11.00000 0.02866 0.01760 =
0.02493 -0.00496 -0.00508 0.00531
AFIX 43
H12 2 0.550538 1.195878 0.783203 11.00000 -1.20000
AFIX 0
C13 1 0.577114 1.042852 0.808800 11.00000 0.01988 0.01732 =
0.01996 -0.00385 -0.00225 0.00090
AFIX 43
H13 2 0.476485 1.029579 0.837658 11.00000 -1.20000
AFIX 0
C14 1 0.467607 0.839512 0.860256 11.00000 0.01428 0.01459 =
0.01961 -0.00249 -0.00255 0.00085
C15 1 0.380428 0.855830 0.780665 11.00000 0.01673 0.02064 =
0.02119 -0.00290 -0.00367 0.00079
AFIX 43
H15 2 0.428130 0.876442 0.715074 11.00000 -1.20000
AFIX 0
C16 1 0.226024 0.842492 0.795756 11.00000 0.01618 0.02886 =
0.02615 -0.00502 -0.00703 0.00130
AFIX 43
H16 2 0.169692 0.852990 0.740372 11.00000 -1.20000
AFIX 0
C17 1 0.152982 0.813855 0.891374 11.00000 0.01422 0.02982 =
0.03257 -0.00509 -0.00064 -0.00122
AFIX 43
H17 2 0.047227 0.804768 0.901871 11.00000 -1.20000
AFIX 0
C18 1 0.237745 0.798807 0.971216 11.00000 0.01947 0.03110 =
0.02603 -0.00042 0.00169 -0.00245
AFIX 43
H18 2 0.189249 0.779627 1.036973 11.00000 -1.20000
AFIX 0
C19 1 0.392785 0.811485 0.956038 11.00000 0.01788 0.02277 =
0.02116 -0.00119 -0.00193 -0.00041
AFIX 43
H19 2 0.448624 0.800919 1.011663 11.00000 -1.20000
AFIX 0
C20 1 0.714890 0.831894 0.936706 11.00000 0.01405 0.02081 =
0.01719 -0.00237 -0.00349 0.00119
C21 1 0.773053 0.911046 0.986522 11.00000 0.02091 0.02078 =
0.01924 -0.00414 -0.00271 0.00030
AFIX 43
H21 2 0.768650 0.978947 0.959037 11.00000 -1.20000
AFIX 0
C22 1 0.837315 0.892537 1.075565 11.00000 0.02541 0.02868 =
0.02244 -0.00747 -0.00700 -0.00124
AFIX 43
H22 2 0.876236 0.947560 1.107976 11.00000 -1.20000
AFIX 0
C23 1 0.844598 0.794002 1.116992 11.00000 0.02517 0.03410 =
0.02044 -0.00247 -0.00761 0.00569
AFIX 43
H23 2 0.890046 0.780890 1.176984 11.00000 -1.20000
AFIX 0
C24 1 0.785230 0.715554 1.070152 11.00000 0.03046 0.02615 =
0.02626 0.00284 -0.00909 0.00554
AFIX 43
H24 2 0.788256 0.647949 1.098623 11.00000 -1.20000
AFIX 0
C25 1 0.720764 0.734276 0.981440 11.00000 0.02777 0.01985 =
0.02424 -0.00048 -0.00885 0.00002
AFIX 43
H25 2 0.679696 0.678986 0.950611 11.00000 -1.20000
AFIX 0
C26 1 0.733194 0.876589 0.403432 11.00000 0.01935 0.03999 =
0.02211 -0.00803 -0.00257 0.00626
C27 1 0.515169 0.771298 0.542099 11.00000 0.02458 0.02949 =
0.02074 -0.00317 -0.00426 -0.00105
C28 1 0.648696 0.968241 0.571560 11.00000 0.01709 0.02650 =
0.01649 -0.00160 -0.00365 -0.00076
C29 1 0.941562 0.872007 0.554989 11.00000 0.02010 0.02973 =
0.01713 -0.00081 -0.00105 0.00517
C30 1 0.812641 0.693944 0.489140 11.00000 0.04046 0.03781 =
0.03679 -0.01146 -0.00626 0.00625
HKLF 4
REM 4737 in P-1 #2
REM R1 = 0.0249 for 7053 Fo > 4sig(Fo) and 0.0277 for all 7500 data
REM 417 parameters refined using 0 restraints
END
WGHT 0.0224 2.0692
REM Highest difference peak 1.141, deepest hole -1.740, 1-sigma level 0.154
Q1 1 0.6484 0.7952 0.5761 11.00000 0.05 1.14
Q2 1 1.1872 0.4743 0.6473 11.00000 0.05 1.00
Q3 1 1.1807 0.6391 0.7307 11.00000 0.05 0.77
Q4 1 0.3014 0.8352 0.7756 11.00000 0.05 0.61
Q5 1 1.2000 0.7246 0.7382 11.00000 0.05 0.55
;
_shelx_res_checksum 42099
_olex2_submission_special_instructions 'No special instructions were received'