data_s18rlw22
_audit_creation_date               2019-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number             2014-3
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H.
 (2015). Acta Cryst. A71, 59-75.

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety           'C26 H20 P, C32 H12 B F24'
_chemical_formula_sum              'C60 H36 B Cl2 F24 P'
_chemical_formula_weight           1325.57
_chemical_melting_point            ?
_chemical_oxdiff_usercomment       'clear crystals'
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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'
 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl' 'Cl' 0.3639 0.7018 '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/c 1'
_space_group_name_Hall             '-P 2ybc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'

_cell_length_a                     13.4192(2)
_cell_length_b                     25.9960(4)
_cell_length_c                     18.4476(2)
_cell_angle_alpha                  90
_cell_angle_beta                   101.8820(10)
_cell_angle_gamma                  90
_cell_volume                       6297.48(15)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      15932
_cell_measurement_temperature      150.01(10)
_cell_measurement_theta_max        72.6830
_cell_measurement_theta_min        3.3620
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.145
_exptl_absorpt_correction_T_max    1.000
_exptl_absorpt_correction_T_min    0.559
_exptl_absorpt_correction_type     gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour              colourless
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      1.398
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               2664
_exptl_crystal_size_max            0.293
_exptl_crystal_size_mid            0.203
_exptl_crystal_size_min            0.168
_exptl_special_details
;
 ?
;
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0465
_diffrn_reflns_av_unetI/netI       0.0322
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.991
_diffrn_reflns_limit_h_max         14
_diffrn_reflns_limit_h_min         -16
_diffrn_reflns_limit_k_max         31
_diffrn_reflns_limit_k_min         -32
_diffrn_reflns_limit_l_max         22
_diffrn_reflns_limit_l_min         -22
_diffrn_reflns_number              63310
_diffrn_reflns_point_group_measured_fraction_full  0.999
_diffrn_reflns_point_group_measured_fraction_max  0.991
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           73.254
_diffrn_reflns_theta_min           2.980
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        150.01(10)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   8.1150
_diffrn_detector_type              EosS2
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.991
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method         'ω scans'
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  9795
_reflns_number_total               12536
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection         'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction          'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max           0.608
_refine_diff_density_min           -0.446
_refine_diff_density_rms           0.061
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.047
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       892
_refine_ls_number_reflns           12536
_refine_ls_number_restraints       418
_refine_ls_R_factor_all            0.0810
_refine_ls_R_factor_gt             0.0670
_refine_ls_restrained_S_all        1.114
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.1216P)²+2.9417P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1944
_refine_ls_wR_factor_ref           0.2087
_refine_special_details
;
The asymmetric unit comprises one cation, one BArF anion and two 
regions of solvent. The cation was entirely ordered, but (not 
unexpectedly) some of the anion CF3 groups fell foul of disorder. 
In particular, the fluorine atoms attached to C34 were treated 
for 55:45 disorder, while the entire trifluoromethyl groups 
based on C49, C50 and C85 were each split over 2 sites in 
respective disorder ratios of 65:35, 50:50 and 80:20. C-F, 
C-C and F...F distance restraints (along with some ADP 
restraints) were used in these regions to assist convergence.
The electron density for the guest solvent was very smeared, 
and an elaborate model would have been required in order to 
take account of same as part of the refinement. After 
multiple abortive attempts, an allowance for 2 molecules 
of CH2Cl2 per asymmetric unit was made in the formula as 
presented, alongside employment of the solvent mask algorithm 
available in Olex-2. Examination of the gross structure 
revealed that there are channels present in the lattice 
which accommodate said solvent. Thus, the accompanying 
disorder level was not surprising.

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F1-C34 \\sim F1A-C34
 with sigma of 0.02
 F2-C34 \\sim F2A-C34
 with sigma of 0.02
 F3-C34 \\sim F3A-C34
 with sigma of 0.02
 F16-C49 \\sim F16A-C49A
 with sigma of 0.02
 F17-C49 \\sim F17A-C49A
 with sigma of 0.02
 F18-C49 \\sim F18A-C49A
 with sigma of 0.02
 C47-C49 \\sim C47-C49A
 with sigma of 0.02
 F16-F17 \\sim F16A-F17A
 with sigma of 0.04
 F16-F18 \\sim F16A-F18A
 with sigma of 0.04
 F16-C47 \\sim F16A-C47
 with sigma of 0.04
 F17-F18 \\sim F17A-F18A
 with sigma of 0.04
 F17-C47 \\sim F17A-C47
 with sigma of 0.04
 F18-C47 \\sim F18A-C47
 with sigma of 0.04
 F13-C50 \\sim F13A-C50A
 with sigma of 0.02
 F14-C50 \\sim F14A-C50A
 with sigma of 0.02
 F15-C50 \\sim F15A-C50A
 with sigma of 0.02
 C45-C50 \\sim C45-C50A
 with sigma of 0.02
 F13-F14 \\sim F13A-F14A
 with sigma of 0.04
 F13-F15 \\sim F13A-F15A
 with sigma of 0.04
 F13-C45 \\sim F13A-C45
 with sigma of 0.04
 F14-F15 \\sim F14A-F15A
 with sigma of 0.04
 F14-C45 \\sim F14A-C45
 with sigma of 0.04
 F15-C45 \\sim F15A-C45
 with sigma of 0.04
 F10-C85 \\sim F10A-C85A
 with sigma of 0.02
 F11-C85 \\sim F11A-C85A
 with sigma of 0.02
 F12-C85 \\sim F12A-C85A
 with sigma of 0.02
 C39-C85 \\sim C39-C85A
 with sigma of 0.02
 F10-F11 \\sim F10A-F11A
 with sigma of 0.04
 F10-F12 \\sim F10A-F12A
 with sigma of 0.04
 F10-C39 \\sim F10A-C39
 with sigma of 0.04
 F11-F12 \\sim F11A-F12A
 with sigma of 0.04
 F11-C39 \\sim F11A-C39
 with sigma of 0.04
 F12-C39 \\sim F12A-C39
 with sigma of 0.04
 F13-F14 \\sim F13-F15 \\sim F14-F15
 with sigma of 0.01
 C50-F13 \\sim C50-F14 \\sim C50-F15
 with sigma of 0.005
 C49-C47 \\sim C49A-C47
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F1A \\sim F2A \\sim F3A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
F16 \\sim F17 \\sim F18 \\sim C49 \\sim F16A \\sim F17A \\sim F18A \\sim C49A:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
F13 \\sim F14 \\sim F15 \\sim C50 \\sim F13A \\sim F14A \\sim F15A \\sim C50A:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
F10 \\sim F11 \\sim F12 \\sim C85 \\sim F10A \\sim F11A \\sim F12A \\sim C85A:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: F1(0.55) F2(0.55) F3(0.55) F10(0.2) F11(0.8) F12(0.8) F13(0.5)
 F14(0.5) F15(0.5) F16(0.65) F17(0.65) F18(0.65) C49(0.65) C50(0.5) C85(0.8)
 F1A(0.45) F2A(0.45) F3A(0.45) F10A(0.2) F11A(0.2) F12A(0.8) F13A(0.5)
 F14A(0.5) F15A(0.5) F16A(0.35) F17A(0.35) F18A(0.35) C49A(0.35) C50A(0.5)
 C85A(0.2)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C30(H30), C32(H32),
 C36(H36), C38(H38), C40(H40), C44(H44), C46(H46), C48(H48), C52(H52), C54(H54),
  C56(H56)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       iterative
_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
 P1 P -0.18568(5) 0.39959(3) 0.18002(3) 0.03705(15) Uani 1 1 d . . . . .
 C1 C 0.0434(2) 0.38760(12) 0.37329(15) 0.0460(6) Uani 1 1 d . . . . .
 H1 H 0.0461 0.3520 0.3687 0.055 Uiso 1 1 calc R . . . .
 C2 C 0.1039(2) 0.41213(15) 0.43309(17) 0.0569(8) Uani 1 1 d . . . . .
 H2 H 0.1474 0.3930 0.4688 0.068 Uiso 1 1 calc R . . . .
 C3 C 0.0998(3) 0.46474(16) 0.43991(18) 0.0634(9) Uani 1 1 d . . . . .
 H3 H 0.1414 0.4810 0.4799 0.076 Uiso 1 1 calc R . . . .
 C4 C 0.0349(3) 0.49333(15) 0.38822(19) 0.0660(9) Uani 1 1 d . . . . .
 H4 H 0.0320 0.5288 0.3936 0.079 Uiso 1 1 calc R . . . .
 C5 C -0.0265(3) 0.46945(12) 0.32770(17) 0.0529(7) Uani 1 1 d . . . . .
 H5 H -0.0706 0.4889 0.2927 0.063 Uiso 1 1 calc R . . . .
 C6 C -0.02172(19) 0.41666(11) 0.31981(14) 0.0404(5) Uani 1 1 d . . . . .
 C7 C -0.08653(19) 0.39160(11) 0.25705(13) 0.0391(5) Uani 1 1 d . . . . .
 C8 C -0.10957(18) 0.34799(10) 0.21851(14) 0.0394(5) Uani 1 1 d . . . . .
 C9 C -0.0796(2) 0.29577(11) 0.20582(15) 0.0421(5) Uani 1 1 d . . . . .
 C10 C -0.1416(2) 0.26525(13) 0.1543(2) 0.0628(9) Uani 1 1 d . . . . .
 H10 H -0.2051 0.2773 0.1304 0.075 Uiso 1 1 calc R . . . .
 C11 C -0.1102(3) 0.21706(14) 0.1378(2) 0.0744(11) Uani 1 1 d . . . . .
 H11 H -0.1535 0.1966 0.1037 0.089 Uiso 1 1 calc R . . . .
 C12 C -0.0173(3) 0.19888(13) 0.1705(2) 0.0642(9) Uani 1 1 d . . . . .
 H12 H 0.0040 0.1667 0.1579 0.077 Uiso 1 1 calc R . . . .
 C13 C 0.0452(3) 0.22837(14) 0.2224(2) 0.0697(10) Uani 1 1 d . . . . .
 H13 H 0.1087 0.2158 0.2457 0.084 Uiso 1 1 calc R . . . .
 C14 C 0.0146(2) 0.27659(13) 0.2402(2) 0.0599(8) Uani 1 1 d . . . . .
 H14 H 0.0575 0.2963 0.2756 0.072 Uiso 1 1 calc R . . . .
 C15 C -0.1643(2) 0.42573(11) 0.09489(14) 0.0427(6) Uani 1 1 d . . . . .
 C16 C -0.2217(3) 0.46618(13) 0.06036(17) 0.0572(7) Uani 1 1 d . . . . .
 H16 H -0.2745 0.4796 0.0802 0.069 Uiso 1 1 calc R . . . .
 C17 C -0.2001(3) 0.48660(17) -0.00389(19) 0.0717(10) Uani 1 1 d . . . . .
 H17 H -0.2384 0.5139 -0.0274 0.086 Uiso 1 1 calc R . . . .
 C18 C -0.1221(3) 0.46655(19) -0.03316(18) 0.0765(12) Uani 1 1 d . . . . .
 H18 H -0.1073 0.4807 -0.0760 0.092 Uiso 1 1 calc R . . . .
 C19 C -0.0657(3) 0.4257(2) 0.00069(18) 0.0771(12) Uani 1 1 d . . . . .
 H19 H -0.0132 0.4123 -0.0196 0.093 Uiso 1 1 calc R . . . .
 C20 C -0.0867(2) 0.40426(16) 0.06471(17) 0.0593(8) Uani 1 1 d . . . . .
 H20 H -0.0497 0.3762 0.0871 0.071 Uiso 1 1 calc R . . . .
 C21 C -0.3111(2) 0.41309(10) 0.19197(14) 0.0411(5) Uani 1 1 d . . . . .
 C22 C -0.3946(2) 0.40030(13) 0.13636(17) 0.0523(7) Uani 1 1 d . . . . .
 H22 H -0.3858 0.3822 0.0947 0.063 Uiso 1 1 calc R . . . .
 C23 C -0.4905(2) 0.41506(16) 0.1443(2) 0.0668(9) Uani 1 1 d . . . . .
 H23 H -0.5470 0.4063 0.1080 0.080 Uiso 1 1 calc R . . . .
 C24 C -0.5035(3) 0.44282(16) 0.2061(2) 0.0715(10) Uani 1 1 d . . . . .
 H24 H -0.5684 0.4531 0.2105 0.086 Uiso 1 1 calc R . . . .
 C25 C -0.4213(3) 0.45508(15) 0.2602(2) 0.0690(9) Uani 1 1 d . . . . .
 H25 H -0.4307 0.4732 0.3018 0.083 Uiso 1 1 calc R . . . .
 C26 C -0.3238(2) 0.44071(13) 0.25396(17) 0.0535(7) Uani 1 1 d . . . . .
 H26 H -0.2678 0.4494 0.2907 0.064 Uiso 1 1 calc R . . . .
 F4 F 0.11334(17) 0.60302(14) 0.50838(14) 0.0974(9) Uani 1 1 d . . . . .
 F5 F 0.2187(2) 0.63378(8) 0.60168(11) 0.0742(6) Uani 1 1 d . . . . .
 F6 F 0.2380(2) 0.55850(8) 0.56144(11) 0.0758(6) Uani 1 1 d . . . . .
 F7 F 0.51503(19) 0.42632(14) 0.45117(18) 0.1124(11) Uani 1 1 d . . . . .
 F8 F 0.4005(3) 0.44607(11) 0.50588(12) 0.1018(10) Uani 1 1 d . . . . .
 F9 F 0.3925(2) 0.37373(9) 0.45409(15) 0.0993(10) Uani 1 1 d . . . . .
 F19 F 0.4923(3) 0.62106(13) 0.04536(12) 0.1196(13) Uani 1 1 d . . . . .
 F20 F 0.61354(19) 0.56937(15) 0.06741(12) 0.1035(10) Uani 1 1 d . . . . .
 F21 F 0.4623(3) 0.54338(14) 0.05116(13) 0.1116(11) Uani 1 1 d . . . . .
 F22 F 0.78028(15) 0.63603(12) 0.31568(14) 0.0902(8) Uani 1 1 d . . . . .
 F23 F 0.70455(16) 0.62885(15) 0.40356(12) 0.1055(11) Uani 1 1 d . . . . .
 F24 F 0.7644(2) 0.56223(14) 0.3589(2) 0.1377(15) Uani 1 1 d . . . . .
 C27 C 0.32935(17) 0.61690(9) 0.37090(13) 0.0326(4) Uani 1 1 d . . . . .
 C28 C 0.38073(18) 0.66381(10) 0.38676(14) 0.0377(5) Uani 1 1 d . . . . .
 H28 H 0.4162 0.6772 0.3528 0.045 Uiso 1 1 calc R . . . .
 C29 C 0.38041(19) 0.69102(10) 0.45179(16) 0.0419(5) Uani 1 1 d . . . . .
 C30 C 0.32718(19) 0.67299(10) 0.50337(14) 0.0410(5) Uani 1 1 d . . . . .
 H30 H 0.3274 0.6909 0.5470 0.049 Uiso 1 1 calc R . . . .
 C31 C 0.27369(19) 0.62751(10) 0.48807(13) 0.0370(5) Uani 1 1 d . . . . .
 C32 C 0.27485(17) 0.60009(9) 0.42328(13) 0.0326(4) Uani 1 1 d . . . . .
 H32 H 0.2381 0.5696 0.4147 0.039 Uiso 1 1 calc R . . . .
 C33 C 0.2120(3) 0.60643(13) 0.54006(16) 0.0523(7) Uani 1 1 d . . . . .
 C34 C 0.4394(2) 0.74015(12) 0.46595(19) 0.0545(7) Uani 1 1 d D . . . .
 C35 C 0.31197(16) 0.52418(9) 0.30378(12) 0.0305(4) Uani 1 1 d . . . . .
 C36 C 0.36299(17) 0.49856(10) 0.36742(13) 0.0347(5) Uani 1 1 d . . . . .
 H36 H 0.4021 0.5177 0.4055 0.042 Uiso 1 1 calc R . . . .
 C37 C 0.35732(19) 0.44590(10) 0.37571(14) 0.0402(5) Uani 1 1 d . . . . .
 C38 C 0.2993(2) 0.41561(10) 0.32080(16) 0.0430(6) Uani 1 1 d . . . . .
 H38 H 0.2943 0.3802 0.3267 0.052 Uiso 1 1 calc R . . . .
 C39 C 0.24940(19) 0.43991(11) 0.25722(14) 0.0419(5) Uani 1 1 d D . . . .
 C40 C 0.25687(17) 0.49276(10) 0.24854(13) 0.0350(5) Uani 1 1 d . . . . .
 H40 H 0.2239 0.5077 0.2043 0.042 Uiso 1 1 calc R . . . .
 C42 C 0.4162(3) 0.42169(13) 0.44471(19) 0.0586(8) Uani 1 1 d . . . . .
 C43 C 0.22790(17) 0.61139(9) 0.23564(13) 0.0340(5) Uani 1 1 d . . . . .
 C44 C 0.12850(18) 0.59313(10) 0.23107(14) 0.0370(5) Uani 1 1 d . . . . .
 H44 H 0.1182 0.5647 0.2591 0.044 Uiso 1 1 calc R . . . .
 C45 C 0.04476(19) 0.61636(12) 0.18577(16) 0.0465(6) Uani 1 1 d D . . . .
 C46 C 0.0559(2) 0.65975(14) 0.14551(19) 0.0576(8) Uani 1 1 d . . . . .
 H46 H -0.0001 0.6754 0.1155 0.069 Uiso 1 1 calc R . . . .
 C47 C 0.1533(2) 0.67949(13) 0.1511(2) 0.0583(8) Uani 1 1 d D . . . .
 C48 C 0.23735(19) 0.65497(11) 0.19442(16) 0.0454(6) Uani 1 1 d . . . . .
 H48 H 0.3019 0.6683 0.1956 0.054 Uiso 1 1 calc R . . . .
 C51 C 0.43186(17) 0.59120(9) 0.26335(13) 0.0334(5) Uani 1 1 d . . . . .
 C52 C 0.52590(18) 0.59697(11) 0.31207(13) 0.0388(5) Uani 1 1 d . . . . .
 H52 H 0.5276 0.6003 0.3625 0.047 Uiso 1 1 calc R . . . .
 C53 C 0.61717(19) 0.59794(12) 0.28722(15) 0.0459(6) Uani 1 1 d . . . . .
 C54 C 0.6186(2) 0.59215(13) 0.21290(15) 0.0474(6) Uani 1 1 d . . . . .
 H54 H 0.6797 0.5927 0.1965 0.057 Uiso 1 1 calc R . . . .
 C55 C 0.5268(2) 0.58543(11) 0.16375(14) 0.0418(5) Uani 1 1 d . . . . .
 C56 C 0.43525(18) 0.58534(10) 0.18854(13) 0.0362(5) Uani 1 1 d . . . . .
 H56 H 0.3745 0.5812 0.1542 0.043 Uiso 1 1 calc R . . . .
 C57 C 0.5244(2) 0.57971(13) 0.08286(15) 0.0503(7) Uani 1 1 d . . . . .
 C58 C 0.7163(2) 0.60489(18) 0.34208(18) 0.0672(10) Uani 1 1 d . . . . .
 B1 B 0.32493(18) 0.58595(10) 0.29309(14) 0.0313(5) Uani 1 1 d . . . . .
 F1 F 0.5152(5) 0.7430(3) 0.4305(4) 0.1062(19) Uani 0.55 1 d D U P A 1
 F2 F 0.3844(4) 0.78058(16) 0.4530(5) 0.099(2) Uani 0.55 1 d D U P A 1
 F3 F 0.4836(6) 0.7460(2) 0.5370(3) 0.106(2) Uani 0.55 1 d D U P A 1
 F10 F 0.2440(13) 0.3929(6) 0.1514(8) 0.078(2) Uani 0.2 1 d D U P B 1
 F11 F 0.1531(3) 0.36666(11) 0.21290(16) 0.0748(7) Uani 0.8 1 d D U P B 1
 F12 F 0.0943(2) 0.43632(14) 0.1682(2) 0.0921(10) Uani 0.8 1 d D U P B 1
 F13 F -0.0749(5) 0.5558(3) 0.1413(4) 0.0810(17) Uani 0.5 1 d D U P C 1
 F14 F -0.1340(3) 0.62935(19) 0.1636(3) 0.0684(11) Uani 0.5 1 d D U P C 1
 F15 F -0.0689(6) 0.5801(3) 0.2530(4) 0.0602(15) Uani 0.5 1 d D U P C 1
 F16 F 0.1879(5) 0.7197(2) 0.0482(3) 0.1226(16) Uani 0.65 1 d D U P D 1
 F17 F 0.2438(3) 0.75766(17) 0.1487(3) 0.1161(16) Uani 0.65 1 d D U P D 1
 F18 F 0.0885(3) 0.7598(2) 0.1000(3) 0.1048(15) Uani 0.65 1 d D U P D 1
 C49 C 0.1692(9) 0.7283(4) 0.1128(7) 0.0910(18) Uani 0.65 1 d D U P D 1
 C50 C -0.0586(7) 0.5961(3) 0.1863(4) 0.062(2) Uani 0.5 1 d D U P C 1
 C85 C 0.1869(4) 0.41122(18) 0.1943(3) 0.0617(11) Uani 0.8 1 d D U P B 1
 F1A F 0.5347(4) 0.7334(3) 0.4803(6) 0.094(2) Uani 0.45 1 d D U P A 2
 F2A F 0.4194(7) 0.7713(3) 0.4098(5) 0.106(2) Uani 0.45 1 d D U P A 2
 F3A F 0.4218(8) 0.7658(3) 0.5237(6) 0.112(2) Uani 0.45 1 d D U P A 2
 F10A F 0.2241(10) 0.3531(4) 0.2068(6) 0.073(2) Uani 0.2 1 d D U P B 2
 F11A F 0.1049(9) 0.4042(6) 0.1895(7) 0.080(2) Uani 0.2 1 d D U P B 2
 F12A F 0.2228(3) 0.41200(14) 0.13430(17) 0.0810(11) Uani 0.8 1 d D U P B 2
 F13A F -0.0905(6) 0.5884(4) 0.2389(5) 0.0713(17) Uani 0.5 1 d D U P C 2
 F14A F -0.0544(5) 0.5384(2) 0.1596(4) 0.0654(13) Uani 0.5 1 d D U P C 2
 F15A F -0.1278(4) 0.6073(3) 0.1219(4) 0.0955(17) Uani 0.5 1 d D U P C 2
 F16A F 0.1373(9) 0.7630(4) 0.1230(7) 0.121(2) Uani 0.35 1 d D U P D 2
 F17A F 0.1074(7) 0.7167(4) 0.0285(5) 0.115(2) Uani 0.35 1 d D U P D 2
 F18A F 0.2531(6) 0.7224(4) 0.0783(6) 0.1054(19) Uani 0.35 1 d D U P D 2
 C49A C 0.166(2) 0.7218(6) 0.0994(12) 0.109(3) Uani 0.35 1 d D U P D 2
 C50A C -0.0566(6) 0.5899(3) 0.1764(5) 0.0571(16) Uani 0.5 1 d D U P C 2
 C85A C 0.2025(15) 0.4019(7) 0.2019(10) 0.079(3) Uani 0.2 1 d D U P B 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
 P1 C7 1.748(2) . ?
 P1 C8 1.746(3) . ?
 P1 C15 1.788(3) . ?
 P1 C21 1.777(3) . ?
 C1 C2 1.383(4) . ?
 C1 C6 1.397(4) . ?
 C2 C3 1.375(5) . ?
 C3 C4 1.370(5) . ?
 C4 C5 1.390(4) . ?
 C5 C6 1.383(4) . ?
 C6 C7 1.451(3) . ?
 C7 C8 1.340(4) . ?
 C8 C9 1.448(4) . ?
 C9 C10 1.378(4) . ?
 C9 C14 1.386(4) . ?
 C10 C11 1.375(5) . ?
 C11 C12 1.354(5) . ?
 C12 C13 1.370(5) . ?
 C13 C14 1.380(5) . ?
 C15 C16 1.379(4) . ?
 C15 C20 1.395(5) . ?
 C16 C17 1.383(5) . ?
 C17 C18 1.376(6) . ?
 C18 C19 1.378(7) . ?
 C19 C20 1.386(5) . ?
 C21 C22 1.395(4) . ?
 C21 C26 1.390(4) . ?
 C22 C23 1.380(5) . ?
 C23 C24 1.390(6) . ?
 C24 C25 1.366(6) . ?
 C25 C26 1.388(5) . ?
 F4 C33 1.335(4) . ?
 F5 C33 1.328(3) . ?
 F6 C33 1.332(4) . ?
 F7 C42 1.313(4) . ?
 F8 C42 1.348(5) . ?
 F9 C42 1.307(4) . ?
 F19 C57 1.303(4) . ?
 F20 C57 1.313(4) . ?
 F21 C57 1.314(4) . ?
 F22 C58 1.342(5) . ?
 F23 C58 1.332(4) . ?
 F24 C58 1.288(5) . ?
 C27 C28 1.402(3) . ?
 C27 C32 1.397(3) . ?
 C27 B1 1.636(3) . ?
 C28 C29 1.393(4) . ?
 C29 C30 1.384(4) . ?
 C29 C34 1.497(4) . ?
 C30 C31 1.382(4) . ?
 C31 C32 1.394(3) . ?
 C31 C33 1.494(4) . ?
 C34 F1 1.320(6) . ?
 C34 F2 1.279(5) . ?
 C34 F3 1.331(6) . ?
 C34 F1A 1.263(7) . ?
 C34 F2A 1.298(7) . ?
 C34 F3A 1.319(8) . ?
 C35 C36 1.400(3) . ?
 C35 C40 1.394(3) . ?
 C35 B1 1.632(3) . ?
 C36 C37 1.382(4) . ?
 C37 C38 1.388(4) . ?
 C37 C42 1.492(4) . ?
 C38 C39 1.378(4) . ?
 C39 C40 1.389(4) . ?
 C39 C85 1.486(5) . ?
 C39 C85A 1.466(15) . ?
 C43 C44 1.402(3) . ?
 C43 C48 1.385(4) . ?
 C43 B1 1.639(3) . ?
 C44 C45 1.392(3) . ?
 C45 C46 1.375(4) . ?
 C45 C50 1.486(10) . ?
 C45 C50A 1.502(9) . ?
 C46 C47 1.388(4) . ?
 C47 C48 1.395(4) . ?
 C47 C49 1.490(5) . ?
 C47 C49A 1.488(6) . ?
 C51 C52 1.398(3) . ?
 C51 C56 1.398(3) . ?
 C51 B1 1.644(3) . ?
 C52 C53 1.394(4) . ?
 C53 C54 1.384(4) . ?
 C53 C58 1.507(4) . ?
 C54 C55 1.382(4) . ?
 C55 C56 1.397(4) . ?
 C55 C57 1.493(4) . ?
 F10 C85 1.300(16) . ?
 F11 C85 1.315(5) . ?
 F12 C85 1.398(7) . ?
 F13 C50 1.326(5) . ?
 F14 C50 1.331(5) . ?
 F15 C50 1.332(5) . ?
 F16 C49 1.287(15) . ?
 F17 C49 1.322(15) . ?
 F18 C49 1.339(12) . ?
 F10A C85A 1.30(2) . ?
 F11A C85A 1.284(17) . ?
 F12A C85A 1.357(19) . ?
 F13A C50A 1.323(10) . ?
 F14A C50A 1.376(10) . ?
 F15A C50A 1.317(9) . ?
 F16A C49A 1.25(2) . ?
 F17A C49A 1.39(2) . ?
 F18A C49A 1.31(2) . ?

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
 C7 P1 C15 121.77(12) . . ?
 C7 P1 C21 120.30(12) . . ?
 C8 P1 C7 45.12(12) . . ?
 C8 P1 C15 117.58(13) . . ?
 C8 P1 C21 126.23(12) . . ?
 C21 P1 C15 111.19(12) . . ?
 C2 C1 C6 119.5(3) . . ?
 C3 C2 C1 120.2(3) . . ?
 C4 C3 C2 120.5(3) . . ?
 C3 C4 C5 120.2(3) . . ?
 C6 C5 C4 119.7(3) . . ?
 C1 C6 C7 120.4(3) . . ?
 C5 C6 C1 119.9(2) . . ?
 C5 C6 C7 119.7(3) . . ?
 C6 C7 P1 145.7(2) . . ?
 C8 C7 P1 67.37(15) . . ?
 C8 C7 C6 146.9(3) . . ?
 C7 C8 P1 67.51(16) . . ?
 C7 C8 C9 146.9(2) . . ?
 C9 C8 P1 144.4(2) . . ?
 C10 C9 C8 120.2(3) . . ?
 C10 C9 C14 118.2(3) . . ?
 C14 C9 C8 121.4(2) . . ?
 C11 C10 C9 120.5(3) . . ?
 C12 C11 C10 121.0(3) . . ?
 C11 C12 C13 119.4(3) . . ?
 C12 C13 C14 120.4(3) . . ?
 C13 C14 C9 120.4(3) . . ?
 C16 C15 P1 121.3(2) . . ?
 C16 C15 C20 120.8(3) . . ?
 C20 C15 P1 117.8(2) . . ?
 C15 C16 C17 119.5(4) . . ?
 C18 C17 C16 120.1(4) . . ?
 C17 C18 C19 120.4(3) . . ?
 C18 C19 C20 120.5(4) . . ?
 C19 C20 C15 118.6(4) . . ?
 C22 C21 P1 120.0(2) . . ?
 C26 C21 P1 118.9(2) . . ?
 C26 C21 C22 120.8(3) . . ?
 C23 C22 C21 118.8(3) . . ?
 C22 C23 C24 120.6(3) . . ?
 C25 C24 C23 120.1(3) . . ?
 C24 C25 C26 120.6(3) . . ?
 C25 C26 C21 119.0(3) . . ?
 C28 C27 B1 122.6(2) . . ?
 C32 C27 C28 115.7(2) . . ?
 C32 C27 B1 121.6(2) . . ?
 C29 C28 C27 122.2(2) . . ?
 C28 C29 C34 119.2(3) . . ?
 C30 C29 C28 120.9(2) . . ?
 C30 C29 C34 119.9(3) . . ?
 C31 C30 C29 118.0(2) . . ?
 C30 C31 C32 121.0(2) . . ?
 C30 C31 C33 121.1(2) . . ?
 C32 C31 C33 117.9(2) . . ?
 C31 C32 C27 122.2(2) . . ?
 F4 C33 C31 112.0(3) . . ?
 F5 C33 F4 107.3(3) . . ?
 F5 C33 F6 106.2(2) . . ?
 F5 C33 C31 113.8(3) . . ?
 F6 C33 F4 104.1(3) . . ?
 F6 C33 C31 112.8(3) . . ?
 F1 C34 C29 113.3(3) . . ?
 F1 C34 F3 104.4(5) . . ?
 F2 C34 C29 113.8(3) . . ?
 F2 C34 F1 109.7(6) . . ?
 F2 C34 F3 102.3(5) . . ?
 F3 C34 C29 112.5(3) . . ?
 F1A C34 C29 113.3(4) . . ?
 F1A C34 F2A 106.8(6) . . ?
 F1A C34 F3A 104.0(7) . . ?
 F2A C34 C29 112.1(4) . . ?
 F2A C34 F3A 106.7(7) . . ?
 F3A C34 C29 113.3(4) . . ?
 C36 C35 B1 121.6(2) . . ?
 C40 C35 C36 115.4(2) . . ?
 C40 C35 B1 122.8(2) . . ?
 C37 C36 C35 122.4(2) . . ?
 C36 C37 C38 121.1(2) . . ?
 C36 C37 C42 118.7(2) . . ?
 C38 C37 C42 120.1(3) . . ?
 C39 C38 C37 117.5(2) . . ?
 C38 C39 C40 121.2(2) . . ?
 C38 C39 C85 122.2(3) . . ?
 C38 C39 C85A 110.3(8) . . ?
 C40 C39 C85 116.7(3) . . ?
 C40 C39 C85A 128.1(8) . . ?
 C39 C40 C35 122.4(2) . . ?
 F7 C42 F8 102.1(3) . . ?
 F7 C42 C37 112.7(3) . . ?
 F8 C42 C37 111.7(3) . . ?
 F9 C42 F7 110.1(3) . . ?
 F9 C42 F8 104.7(3) . . ?
 F9 C42 C37 114.5(3) . . ?
 C44 C43 B1 121.4(2) . . ?
 C48 C43 C44 115.9(2) . . ?
 C48 C43 B1 122.3(2) . . ?
 C45 C44 C43 122.0(2) . . ?
 C44 C45 C50 118.8(3) . . ?
 C44 C45 C50A 118.1(4) . . ?
 C46 C45 C44 121.1(2) . . ?
 C46 C45 C50 120.0(3) . . ?
 C46 C45 C50A 120.6(4) . . ?
 C45 C46 C47 117.9(2) . . ?
 C46 C47 C48 120.8(3) . . ?
 C46 C47 C49 120.3(5) . . ?
 C46 C47 C49A 117.0(11) . . ?
 C48 C47 C49 118.9(5) . . ?
 C48 C47 C49A 121.3(11) . . ?
 C43 C48 C47 122.3(2) . . ?
 C52 C51 B1 121.9(2) . . ?
 C56 C51 C52 115.9(2) . . ?
 C56 C51 B1 121.9(2) . . ?
 C53 C52 C51 121.9(2) . . ?
 C52 C53 C58 119.7(2) . . ?
 C54 C53 C52 121.1(2) . . ?
 C54 C53 C58 119.2(2) . . ?
 C55 C54 C53 118.1(2) . . ?
 C54 C55 C56 120.7(2) . . ?
 C54 C55 C57 120.1(2) . . ?
 C56 C55 C57 119.2(2) . . ?
 C55 C56 C51 122.2(2) . . ?
 F19 C57 F20 105.6(3) . . ?
 F19 C57 F21 104.3(3) . . ?
 F19 C57 C55 112.7(3) . . ?
 F20 C57 F21 106.2(3) . . ?
 F20 C57 C55 113.8(2) . . ?
 F21 C57 C55 113.4(3) . . ?
 F22 C58 C53 111.8(3) . . ?
 F23 C58 F22 102.9(3) . . ?
 F23 C58 C53 112.6(3) . . ?
 F24 C58 F22 106.3(3) . . ?
 F24 C58 F23 109.8(4) . . ?
 F24 C58 C53 112.8(4) . . ?
 C27 B1 C43 104.44(19) . . ?
 C27 B1 C51 112.05(19) . . ?
 C35 B1 C27 111.32(18) . . ?
 C35 B1 C43 112.64(19) . . ?
 C35 B1 C51 104.13(18) . . ?
 C43 B1 C51 112.48(18) . . ?
 F16 C49 C47 111.5(10) . . ?
 F16 C49 F17 107.0(8) . . ?
 F16 C49 F18 104.3(8) . . ?
 F17 C49 C47 114.9(8) . . ?
 F17 C49 F18 103.7(10) . . ?
 F18 C49 C47 114.5(8) . . ?
 F13 C50 C45 108.0(6) . . ?
 F13 C50 F14 107.4(6) . . ?
 F13 C50 F15 107.2(6) . . ?
 F14 C50 C45 114.7(6) . . ?
 F14 C50 F15 106.1(5) . . ?
 F15 C50 C45 113.0(6) . . ?
 F10 C85 C39 110.5(8) . . ?
 F10 C85 F11 96.6(8) . . ?
 F10 C85 F12 123.8(8) . . ?
 F11 C85 C39 114.0(4) . . ?
 F11 C85 F12 99.8(4) . . ?
 F12 C85 C39 110.7(4) . . ?
 F16A C49A C47 109.2(15) . . ?
 F16A C49A F17A 104.9(17) . . ?
 F16A C49A F18A 116.9(16) . . ?
 F17A C49A C47 114.7(15) . . ?
 F18A C49A C47 115.3(15) . . ?
 F18A C49A F17A 95.0(15) . . ?
 F13A C50A C45 112.3(8) . . ?
 F13A C50A F14A 101.3(7) . . ?
 F14A C50A C45 114.1(7) . . ?
 F15A C50A C45 115.3(6) . . ?
 F15A C50A F13A 110.5(8) . . ?
 F15A C50A F14A 102.0(7) . . ?
 F10A C85A C39 123.5(14) . . ?
 F10A C85A F12A 99.7(13) . . ?
 F11A C85A C39 111.7(13) . . ?
 F11A C85A F10A 105.2(15) . . ?
 F11A C85A F12A 102.6(14) . . ?
 F12A C85A C39 111.7(13) . . ?

_smtbx_masks_special_details       ?
loop_
  _smtbx_masks_void_nr
  _smtbx_masks_void_average_x
  _smtbx_masks_void_average_y
  _smtbx_masks_void_average_z
  _smtbx_masks_void_volume
  _smtbx_masks_void_count_electrons
  _smtbx_masks_void_content
 1 0.314 0.250 0.375 605.4 240.5 ?
 2 -0.314 0.750 -0.299 605.4 240.5 ?
 3 0.292 0.622 0.042 8.1 0.0 ?
 4 0.292 0.878 0.542 8.1 0.0 ?
 5 0.708 0.122 0.458 8.1 0.0 ?
 6 0.708 0.378 0.958 8.1 0.0 ?


#===end
data_s20rlw58
_audit_creation_date               2020-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number             2014-3
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety           'C F3 O3 S, C28 H24 O2 P'
_chemical_formula_sum              'C29 H24 F3 O5 P S'
_chemical_formula_weight           572.51
_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' 0.0181 0.0091 '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' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S' 'S' 0.3331 0.5567 '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                     10.5938(2)
_cell_length_b                     15.2705(2)
_cell_length_c                     16.8486(2)
_cell_angle_alpha                  90
_cell_angle_beta                   95.4560(10)
_cell_angle_gamma                  90
_cell_volume                       2713.29(7)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      9254
_cell_measurement_temperature      150.00(10)
_cell_measurement_theta_max        72.8520
_cell_measurement_theta_min        3.9110
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.136
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.87554
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour              colourless
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      1.402
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1184
_exptl_crystal_size_max            0.189
_exptl_crystal_size_mid            0.102
_exptl_crystal_size_min            0.068
_exptl_special_details
;
 ?
;
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0353
_diffrn_reflns_av_unetI/netI       0.0272
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.995
_diffrn_reflns_limit_h_max         11
_diffrn_reflns_limit_h_min         -13
_diffrn_reflns_limit_k_max         18
_diffrn_reflns_limit_k_min         -18
_diffrn_reflns_limit_l_max         20
_diffrn_reflns_limit_l_min         -20
_diffrn_reflns_number              23939
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.995
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           73.046
_diffrn_reflns_theta_min           3.915
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        150.00(10)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   8.1150
_diffrn_detector_type              EosS2
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.995
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method         'ω scans'
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  4649
_reflns_number_total               5389
_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 > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection         'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction          'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.273
_refine_diff_density_min           -0.388
_refine_diff_density_rms           0.042
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.028
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       354
_refine_ls_number_reflns           5389
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0426
_refine_ls_R_factor_gt             0.0354
_refine_ls_restrained_S_all        1.028
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0424P)²+0.8770P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0869
_refine_ls_wR_factor_ref           0.0914
_refine_special_details
;
 ?
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C)
;
_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
 S1 S 0.67771(4) 0.24292(2) 0.08328(2) 0.02892(10) Uani 1 1 d . . . . .
 F1 F 0.48831(12) 0.33964(8) 0.02162(8) 0.0543(3) Uani 1 1 d . . . . .
 F2 F 0.55504(13) 0.24531(9) -0.05941(7) 0.0532(3) Uani 1 1 d . . . . .
 F3 F 0.66472(13) 0.36135(9) -0.03001(8) 0.0627(4) Uani 1 1 d . . . . .
 O3 O 0.58838(12) 0.17664(8) 0.10190(7) 0.0368(3) Uani 1 1 d . . . . .
 O4 O 0.70082(12) 0.31039(8) 0.14251(8) 0.0396(3) Uani 1 1 d . . . . .
 O5 O 0.78928(12) 0.21029(8) 0.04998(7) 0.0360(3) Uani 1 1 d . . . . .
 C29 C 0.59254(18) 0.30020(12) -0.00048(11) 0.0399(4) Uani 1 1 d . . . . .
 P1 P 0.59541(4) 0.24408(3) 0.40620(2) 0.02558(10) Uani 1 1 d . . . . .
 O1 O 0.52235(14) -0.02691(9) 0.73952(8) 0.0440(3) Uani 1 1 d . . . . .
 O2 O 1.08057(12) 0.01665(9) 0.23161(8) 0.0413(3) Uani 1 1 d . . . . .
 C1 C 0.4280(2) 0.00520(14) 0.78723(11) 0.0438(4) Uani 1 1 d . . . . .
 H1A H 0.3475 0.0070 0.7559 0.066 Uiso 1 1 calc GR . . . .
 H1B H 0.4506 0.0631 0.8058 0.066 Uiso 1 1 calc GR . . . .
 H1C H 0.4225 -0.0329 0.8321 0.066 Uiso 1 1 calc GR . . . .
 C2 C 0.54034(17) 0.01718(11) 0.67129(10) 0.0316(3) Uani 1 1 d . . . . .
 C3 C 0.46683(16) 0.08757(11) 0.64195(10) 0.0302(3) Uani 1 1 d . . . . .
 H3 H 0.3989 0.1067 0.6685 0.036 Uiso 1 1 calc R . . . .
 C4 C 0.49557(15) 0.12890(10) 0.57293(9) 0.0277(3) Uani 1 1 d . . . . .
 H4 H 0.4464 0.1760 0.5534 0.033 Uiso 1 1 calc R . . . .
 C5 C 0.59690(15) 0.10129(10) 0.53210(9) 0.0260(3) Uani 1 1 d . . . . .
 C6 C 0.66945(17) 0.02969(11) 0.56184(10) 0.0320(3) Uani 1 1 d . . . . .
 H6 H 0.7369 0.0101 0.5351 0.038 Uiso 1 1 calc R . . . .
 C7 C 0.64131(18) -0.01178(11) 0.63058(10) 0.0361(4) Uani 1 1 d . . . . .
 H7 H 0.6898 -0.0593 0.6500 0.043 Uiso 1 1 calc R . . . .
 C8 C 0.62483(15) 0.14790(10) 0.46094(9) 0.0265(3) Uani 1 1 d . . . . .
 C9 C 0.69399(15) 0.15410(10) 0.39795(9) 0.0275(3) Uani 1 1 d . . . . .
 C10 C 0.79237(15) 0.11825(10) 0.35356(9) 0.0267(3) Uani 1 1 d . . . . .
 C11 C 0.83906(16) 0.16818(11) 0.29366(10) 0.0319(3) Uani 1 1 d . . . . .
 H11 H 0.8047 0.2232 0.2818 0.038 Uiso 1 1 calc R . . . .
 C12 C 0.93591(17) 0.13729(12) 0.25145(10) 0.0343(4) Uani 1 1 d . . . . .
 H12 H 0.9670 0.1715 0.2120 0.041 Uiso 1 1 calc R . . . .
 C13 C 0.98598(16) 0.05473(11) 0.26869(10) 0.0314(3) Uani 1 1 d . . . . .
 C14 C 0.93784(17) 0.00293(11) 0.32711(10) 0.0339(4) Uani 1 1 d . . . . .
 H14 H 0.9701 -0.0530 0.3375 0.041 Uiso 1 1 calc R . . . .
 C15 C 0.84269(16) 0.03458(11) 0.36933(10) 0.0309(3) Uani 1 1 d . . . . .
 H15 H 0.8116 0.0002 0.4086 0.037 Uiso 1 1 calc R . . . .
 C16 C 1.1443(2) 0.06874(15) 0.17747(14) 0.0525(5) Uani 1 1 d . . . . .
 H16A H 1.0861 0.0839 0.1324 0.079 Uiso 1 1 calc GR . . . .
 H16B H 1.2139 0.0362 0.1598 0.079 Uiso 1 1 calc GR . . . .
 H16C H 1.1757 0.1212 0.2038 0.079 Uiso 1 1 calc GR . . . .
 C17 C 0.45941(15) 0.26290(10) 0.33797(9) 0.0261(3) Uani 1 1 d . . . . .
 C18 C 0.34901(18) 0.29736(15) 0.36352(11) 0.0433(4) Uani 1 1 d . . . . .
 H18 H 0.3427 0.3074 0.4174 0.052 Uiso 1 1 calc R . . . .
 C19 C 0.24838(19) 0.31667(15) 0.30777(13) 0.0483(5) Uani 1 1 d . . . . .
 H19 H 0.1737 0.3392 0.3244 0.058 Uiso 1 1 calc R . . . .
 C20 C 0.25816(18) 0.30273(13) 0.22794(11) 0.0395(4) Uani 1 1 d . . . . .
 H20 H 0.1904 0.3163 0.1907 0.047 Uiso 1 1 calc R . . . .
 C21 C 0.36809(19) 0.26879(14) 0.20308(11) 0.0429(4) Uani 1 1 d . . . . .
 H21 H 0.3745 0.2597 0.1490 0.051 Uiso 1 1 calc R . . . .
 C22 C 0.46886(18) 0.24816(12) 0.25783(10) 0.0364(4) Uani 1 1 d . . . . .
 H22 H 0.5426 0.2245 0.2409 0.044 Uiso 1 1 calc R . . . .
 C23 C 0.66642(15) 0.34435(10) 0.44187(9) 0.0275(3) Uani 1 1 d . . . . .
 C24 C 0.6186(2) 0.42445(12) 0.41427(12) 0.0453(5) Uani 1 1 d . . . . .
 H24 H 0.5454 0.4268 0.3792 0.054 Uiso 1 1 calc R . . . .
 C25 C 0.6807(2) 0.50088(13) 0.43926(14) 0.0509(5) Uani 1 1 d . . . . .
 H25 H 0.6484 0.5547 0.4212 0.061 Uiso 1 1 calc R . . . .
 C26 C 0.78959(19) 0.49786(12) 0.49049(11) 0.0395(4) Uani 1 1 d . . . . .
 H26 H 0.8306 0.5495 0.5070 0.047 Uiso 1 1 calc R . . . .
 C27 C 0.83795(18) 0.41852(13) 0.51740(12) 0.0407(4) Uani 1 1 d . . . . .
 H27 H 0.9119 0.4165 0.5518 0.049 Uiso 1 1 calc R . . . .
 C28 C 0.77654(17) 0.34152(12) 0.49331(11) 0.0362(4) Uani 1 1 d . . . . .
 H28 H 0.8092 0.2879 0.5117 0.043 Uiso 1 1 calc R . . . .


_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
 S1 O3 1.4403(12) . ?
 S1 O4 1.4391(12) . ?
 S1 O5 1.4444(13) . ?
 S1 C29 1.8244(19) . ?
 F1 C29 1.341(2) . ?
 F2 C29 1.331(2) . ?
 F3 C29 1.333(2) . ?
 P1 C8 1.7464(16) . ?
 P1 C9 1.7394(16) . ?
 P1 C17 1.7790(16) . ?
 P1 C23 1.7848(17) . ?
 O1 C1 1.428(2) . ?
 O1 C2 1.3612(19) . ?
 O2 C13 1.361(2) . ?
 O2 C16 1.427(2) . ?
 C2 C3 1.390(2) . ?
 C2 C7 1.396(2) . ?
 C3 C4 1.382(2) . ?
 C4 C5 1.394(2) . ?
 C5 C6 1.402(2) . ?
 C5 C8 1.449(2) . ?
 C6 C7 1.377(2) . ?
 C8 C9 1.349(2) . ?
 C9 C10 1.447(2) . ?
 C10 C11 1.393(2) . ?
 C10 C15 1.400(2) . ?
 C11 C12 1.385(2) . ?
 C12 C13 1.388(2) . ?
 C13 C14 1.396(2) . ?
 C14 C15 1.375(2) . ?
 C17 C18 1.388(2) . ?
 C17 C22 1.382(2) . ?
 C18 C19 1.384(3) . ?
 C19 C20 1.375(3) . ?
 C20 C21 1.376(3) . ?
 C21 C22 1.379(3) . ?
 C23 C24 1.387(2) . ?
 C23 C28 1.386(2) . ?
 C24 C25 1.385(3) . ?
 C25 C26 1.374(3) . ?
 C26 C27 1.375(3) . ?
 C27 C28 1.386(3) . ?

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
 O3 S1 O5 114.91(7) . . ?
 O3 S1 C29 102.62(8) . . ?
 O4 S1 O3 115.09(8) . . ?
 O4 S1 O5 115.13(8) . . ?
 O4 S1 C29 103.42(9) . . ?
 O5 S1 C29 103.16(8) . . ?
 F1 C29 S1 111.11(13) . . ?
 F2 C29 S1 111.45(13) . . ?
 F2 C29 F1 107.14(16) . . ?
 F2 C29 F3 107.69(16) . . ?
 F3 C29 S1 111.44(14) . . ?
 F3 C29 F1 107.80(16) . . ?
 C8 P1 C17 124.75(8) . . ?
 C8 P1 C23 119.69(8) . . ?
 C9 P1 C8 45.54(7) . . ?
 C9 P1 C17 122.10(8) . . ?
 C9 P1 C23 117.87(8) . . ?
 C17 P1 C23 111.63(7) . . ?
 C2 O1 C1 117.86(15) . . ?
 C13 O2 C16 117.97(15) . . ?
 O1 C2 C3 124.33(16) . . ?
 O1 C2 C7 115.69(15) . . ?
 C3 C2 C7 119.97(15) . . ?
 C4 C3 C2 119.43(15) . . ?
 C3 C4 C5 121.24(15) . . ?
 C4 C5 C6 118.77(14) . . ?
 C4 C5 C8 119.15(14) . . ?
 C6 C5 C8 122.08(14) . . ?
 C7 C6 C5 120.28(15) . . ?
 C6 C7 C2 120.31(16) . . ?
 C5 C8 P1 144.09(12) . . ?
 C9 C8 P1 66.96(9) . . ?
 C9 C8 C5 148.69(15) . . ?
 C8 C9 P1 67.51(9) . . ?
 C8 C9 C10 148.41(15) . . ?
 C10 C9 P1 143.87(13) . . ?
 C11 C10 C9 119.37(15) . . ?
 C11 C10 C15 118.81(15) . . ?
 C15 C10 C9 121.82(14) . . ?
 C12 C11 C10 121.13(16) . . ?
 C11 C12 C13 119.26(15) . . ?
 O2 C13 C12 125.14(16) . . ?
 O2 C13 C14 114.57(16) . . ?
 C12 C13 C14 120.28(15) . . ?
 C15 C14 C13 120.01(16) . . ?
 C14 C15 C10 120.47(15) . . ?
 C18 C17 P1 121.03(13) . . ?
 C22 C17 P1 118.40(13) . . ?
 C22 C17 C18 120.42(16) . . ?
 C19 C18 C17 119.20(17) . . ?
 C20 C19 C18 120.39(17) . . ?
 C19 C20 C21 120.04(17) . . ?
 C20 C21 C22 120.41(17) . . ?
 C21 C22 C17 119.53(16) . . ?
 C24 C23 P1 120.99(13) . . ?
 C28 C23 P1 119.12(12) . . ?
 C28 C23 C24 119.72(16) . . ?
 C25 C24 C23 119.57(18) . . ?
 C26 C25 C24 120.55(18) . . ?
 C25 C26 C27 120.05(18) . . ?
 C26 C27 C28 120.07(18) . . ?
 C27 C28 C23 120.03(16) . . ?


#===end


