#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/34/4303430.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4303430
loop_
_publ_author_name
'Meghan A. Dureen'
'Gregory C. Welch'
'Thomas M. Gilbert'
'Douglas W. Stephan'
_publ_section_title
;
Heterolytic Cleavage of Disulfides by Frustrated Lewis Pairs
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9910
_journal_page_last               9917
_journal_paper_doi               10.1021/ic901590s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C36 H41 B F15 P S2'
_chemical_formula_weight         864.59
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.3890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9509(4)
_cell_length_b                   16.9921(4)
_cell_length_c                   15.2385(4)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.88
_cell_measurement_theta_min      2.39
_cell_volume                     3829.88(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62433
_diffrn_reflns_theta_full        31.97
_diffrn_reflns_theta_max         31.97
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.8958
_exptl_absorpt_correction_T_min  0.8383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         13250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0405P)²+1.5762P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                10005
_reflns_number_total             13250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901590s_si_002_3.cif
_cod_data_source_block           '[tBu3PSiPr][iPrSB(C6F5)3]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4303430
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.63685(2) 0.196697(18) 0.18553(2) 0.02411(7) Uani 1 1 d . . .
S2 S 1.00693(2) 0.22806(2) -0.01879(2) 0.02846(7) Uani 1 1 d . . .
P1 P 1.13544(2) 0.206415(18) 0.047566(19) 0.01938(6) Uani 1 1 d . . .
F6 F 0.78380(5) 0.19271(5) -0.04234(5) 0.02801(16) Uani 1 1 d . . .
F10 F 0.48446(5) 0.16205(5) 0.02327(6) 0.03255(18) Uani 1 1 d . . .
F2 F 0.94195(6) 0.38774(5) 0.21477(6) 0.03587(19) Uani 1 1 d . . .
F1 F 0.81249(6) 0.28678(5) 0.22688(5) 0.02977(17) Uani 1 1 d . . .
F15 F 0.50189(6) 0.28995(5) -0.08406(5) 0.03343(18) Uani 1 1 d . . .
F5 F 0.68763(6) 0.34168(5) -0.07116(5) 0.02937(17) Uani 1 1 d . . .
F7 F 0.75337(6) 0.07955(5) -0.16115(5) 0.03348(18) Uani 1 1 d . . .
F11 F 0.62499(6) 0.37162(5) 0.20660(5) 0.03296(18) Uani 1 1 d . . .
F9 F 0.45776(6) 0.04675(5) -0.09380(6) 0.0386(2) Uani 1 1 d . . .
F4 F 0.81631(7) 0.44874(5) -0.07914(6) 0.0392(2) Uani 1 1 d . . .
F12 F 0.50197(7) 0.48509(5) 0.19710(7) 0.0466(2) Uani 1 1 d . . .
F13 F 0.37641(7) 0.50151(6) 0.04939(8) 0.0501(3) Uani 1 1 d . . .
F8 F 0.59086(7) 0.00414(5) -0.19036(6) 0.0387(2) Uani 1 1 d . . .
F3 F 0.94748(6) 0.47223(5) 0.06377(7) 0.0448(2) Uani 1 1 d . . .
F14 F 0.38099(6) 0.40296(6) -0.09042(7) 0.0445(2) Uani 1 1 d . . .
B1 B 0.64897(9) 0.25278(8) 0.07597(9) 0.0199(2) Uani 1 1 d . . .
C13 C 0.63539(8) 0.18574(7) -0.00236(8) 0.0202(2) Uani 1 1 d . . .
C7 C 0.74151(8) 0.30703(7) 0.07744(8) 0.0200(2) Uani 1 1 d . . .
C9 C 0.87836(9) 0.37654(7) 0.14394(9) 0.0252(2) Uani 1 1 d . . .
C19 C 0.56791(8) 0.32007(7) 0.06461(8) 0.0224(2) Uani 1 1 d . . .
C14 C 0.70012(8) 0.16023(7) -0.05260(8) 0.0212(2) Uani 1 1 d . . .
C17 C 0.53808(9) 0.08392(8) -0.08162(9) 0.0266(3) Uani 1 1 d . . .
C15 C 0.68616(9) 0.10076(7) -0.11550(8) 0.0242(2) Uani 1 1 d . . .
C12 C 0.74943(9) 0.35169(7) 0.00230(8) 0.0226(2) Uani 1 1 d . . .
C10 C 0.88131(9) 0.41931(7) 0.06773(10) 0.0297(3) Uani 1 1 d . . .
C24 C 0.50450(9) 0.33387(8) -0.01005(9) 0.0260(2) Uani 1 1 d . . .
C20 C 0.56401(9) 0.37488(8) 0.13185(9) 0.0261(2) Uani 1 1 d . . .
C18 C 0.55424(9) 0.14390(7) -0.02021(8) 0.0236(2) Uani 1 1 d . . .
C1 C 0.69579(10) 0.10272(7) 0.17938(9) 0.0277(3) Uani 1 1 d . . .
H1A H 0.6706 0.0760 0.1227 0.033 Uiso 1 1 calc R . .
C11 C 0.81560(9) 0.40717(7) -0.00373(9) 0.0273(3) Uani 1 1 d . . .
C8 C 0.80918(8) 0.32259(7) 0.14794(8) 0.0216(2) Uani 1 1 d . . .
C3 C 0.79699(10) 0.11241(9) 0.18142(10) 0.0350(3) Uani 1 1 d . . .
H3A H 0.8249 0.0606 0.1776 0.053 Uiso 1 1 calc R . .
H3B H 0.8229 0.1381 0.2369 0.053 Uiso 1 1 calc R . .
H3C H 0.8085 0.1448 0.1311 0.053 Uiso 1 1 calc R . .
C21 C 0.50139(10) 0.43525(8) 0.12811(10) 0.0319(3) Uani 1 1 d . . .
C33 C 1.10373(10) 0.15211(9) 0.14744(9) 0.0323(3) Uani 1 1 d . . .
C4 C 1.00884(9) 0.25609(9) -0.13659(8) 0.0309(3) Uani 1 1 d . . .
H4A H 1.0726 0.2589 -0.1490 0.037 Uiso 1 1 calc R . .
C23 C 0.44064(9) 0.39367(9) -0.01629(10) 0.0315(3) Uani 1 1 d . . .
C16 C 0.60454(10) 0.06241(7) -0.13054(8) 0.0269(3) Uani 1 1 d . . .
C22 C 0.43866(10) 0.44413(8) 0.05393(11) 0.0342(3) Uani 1 1 d . . .
C31 C 1.28107(12) 0.10102(11) 0.04497(12) 0.0449(4) Uani 1 1 d . . .
H31A H 1.3170 0.0684 0.0101 0.067 Uiso 1 1 calc R . .
H31B H 1.2537 0.0676 0.0862 0.067 Uiso 1 1 calc R . .
H31C H 1.3203 0.1402 0.0786 0.067 Uiso 1 1 calc R . .
C29 C 1.20601(10) 0.14331(9) -0.01782(9) 0.0321(3) Uani 1 1 d . . .
C25 C 1.19140(10) 0.30346(9) 0.07832(10) 0.0339(3) Uani 1 1 d . . .
C36 C 1.02376(12) 0.19273(12) 0.18308(11) 0.0474(4) Uani 1 1 d . . .
H36A H 1.0088 0.1636 0.2345 0.071 Uiso 1 1 calc R . .
H36B H 0.9711 0.1935 0.1366 0.071 Uiso 1 1 calc R . .
H36C H 1.0407 0.2468 0.2007 0.071 Uiso 1 1 calc R . .
C2 C 0.67565(13) 0.05168(9) 0.25649(10) 0.0409(4) Uani 1 1 d . . .
H2A H 0.7063 0.0008 0.2546 0.061 Uiso 1 1 calc R . .
H2B H 0.6103 0.0432 0.2517 0.061 Uiso 1 1 calc R . .
H2C H 0.6974 0.0782 0.3126 0.061 Uiso 1 1 calc R . .
C32 C 1.25307(12) 0.19157(12) -0.08391(11) 0.0476(5) Uani 1 1 d . . .
H32A H 1.2887 0.1562 -0.1161 0.071 Uiso 1 1 calc R . .
H32B H 1.2931 0.2308 -0.0514 0.071 Uiso 1 1 calc R . .
H32C H 1.2073 0.2183 -0.1261 0.071 Uiso 1 1 calc R . .
C35 C 1.18289(12) 0.14720(12) 0.22347(10) 0.0477(4) Uani 1 1 d . . .
H35A H 1.1637 0.1188 0.2735 0.071 Uiso 1 1 calc R . .
H35B H 1.2022 0.2004 0.2423 0.071 Uiso 1 1 calc R . .
H35C H 1.2334 0.1192 0.2032 0.071 Uiso 1 1 calc R . .
C6 C 0.95678(12) 0.19401(12) -0.19478(11) 0.0473(4) Uani 1 1 d . . .
H6A H 0.9568 0.2075 -0.2573 0.071 Uiso 1 1 calc R . .
H6B H 0.8944 0.1919 -0.1822 0.071 Uiso 1 1 calc R . .
H6C H 0.9856 0.1426 -0.1824 0.071 Uiso 1 1 calc R . .
C26 C 1.18530(12) 0.35599(9) -0.00467(12) 0.0411(4) Uani 1 1 d . . .
H26A H 1.2146 0.4066 0.0114 0.062 Uiso 1 1 calc R . .
H26B H 1.1217 0.3648 -0.0287 0.062 Uiso 1 1 calc R . .
H26C H 1.2158 0.3300 -0.0495 0.062 Uiso 1 1 calc R . .
C34 C 1.07200(13) 0.06831(10) 0.11982(12) 0.0472(4) Uani 1 1 d . . .
H34A H 1.0557 0.0403 0.1714 0.071 Uiso 1 1 calc R . .
H34B H 1.1209 0.0401 0.0969 0.071 Uiso 1 1 calc R . .
H34C H 1.0192 0.0712 0.0736 0.071 Uiso 1 1 calc R . .
C30 C 1.14639(15) 0.08183(11) -0.07178(12) 0.0538(5) Uani 1 1 d . . .
H30A H 1.1837 0.0494 -0.1053 0.081 Uiso 1 1 calc R . .
H30B H 1.0996 0.1085 -0.1130 0.081 Uiso 1 1 calc R . .
H30C H 1.1178 0.0483 -0.0315 0.081 Uiso 1 1 calc R . .
C28 C 1.29083(12) 0.29304(12) 0.11951(13) 0.0550(5) Uani 1 1 d . . .
H28A H 1.3178 0.3447 0.1348 0.083 Uiso 1 1 calc R . .
H28B H 1.3240 0.2670 0.0768 0.083 Uiso 1 1 calc R . .
H28C H 1.2941 0.2608 0.1732 0.083 Uiso 1 1 calc R . .
C5 C 0.96322(13) 0.33562(12) -0.15314(12) 0.0482(4) Uani 1 1 d . . .
H5A H 0.9639 0.3512 -0.2150 0.072 Uiso 1 1 calc R . .
H5B H 0.9958 0.3749 -0.1136 0.072 Uiso 1 1 calc R . .
H5C H 0.9006 0.3321 -0.1416 0.072 Uiso 1 1 calc R . .
C27 C 1.14121(16) 0.34708(11) 0.14476(12) 0.0553(5) Uani 1 1 d . . .
H27A H 1.1711 0.3975 0.1605 0.083 Uiso 1 1 calc R . .
H27B H 1.1420 0.3150 0.1983 0.083 Uiso 1 1 calc R . .
H27C H 1.0785 0.3566 0.1179 0.083 Uiso 1 1 calc R . .
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'
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 B1 106.03(6) . . ?
C4 S2 P1 111.90(5) . . ?
C25 P1 C29 111.57(7) . . ?
C25 P1 C33 112.41(7) . . ?
C29 P1 C33 111.80(7) . . ?
C25 P1 S2 108.31(5) . . ?
C29 P1 S2 113.18(5) . . ?
C33 P1 S2 98.95(5) . . ?
C13 B1 C19 113.08(10) . . ?
C13 B1 C7 114.19(9) . . ?
C19 B1 C7 102.34(9) . . ?
C13 B1 S1 105.42(8) . . ?
C19 B1 S1 105.56(8) . . ?
C7 B1 S1 116.13(8) . . ?
C14 C13 C18 112.88(11) . . ?
C14 C13 B1 126.56(11) . . ?
C18 C13 B1 120.42(10) . . ?
C8 C7 C12 113.09(11) . . ?
C8 C7 B1 128.87(10) . . ?
C12 C7 B1 117.52(11) . . ?
F2 C9 C10 119.80(12) . . ?
F2 C9 C8 120.13(12) . . ?
C10 C9 C8 120.06(12) . . ?
C24 C19 C20 113.12(11) . . ?
C24 C19 B1 127.08(11) . . ?
C20 C19 B1 119.55(11) . . ?
F6 C14 C15 114.80(11) . . ?
F6 C14 C13 121.02(10) . . ?
C15 C14 C13 124.18(12) . . ?
F9 C17 C16 120.08(11) . . ?
F9 C17 C18 120.28(12) . . ?
C16 C17 C18 119.64(12) . . ?
F7 C15 C16 119.80(11) . . ?
F7 C15 C14 120.09(12) . . ?
C16 C15 C14 120.10(12) . . ?
F5 C12 C11 116.12(11) . . ?
F5 C12 C7 118.78(11) . . ?
C11 C12 C7 125.10(12) . . ?
F3 C10 C11 120.75(13) . . ?
F3 C10 C9 120.35(13) . . ?
C11 C10 C9 118.90(12) . . ?
F15 C24 C23 114.35(12) . . ?
F15 C24 C19 121.61(11) . . ?
C23 C24 C19 124.02(12) . . ?
F11 C20 C21 115.71(12) . . ?
F11 C20 C19 119.81(11) . . ?
C21 C20 C19 124.47(13) . . ?
F10 C18 C17 115.45(11) . . ?
F10 C18 C13 119.92(11) . . ?
C17 C18 C13 124.62(12) . . ?
C3 C1 C2 110.74(12) . . ?
C3 C1 S1 112.93(9) . . ?
C2 C1 S1 107.80(10) . . ?
F4 C11 C10 120.23(12) . . ?
F4 C11 C12 120.60(13) . . ?
C10 C11 C12 119.17(12) . . ?
F1 C8 C7 122.28(11) . . ?
F1 C8 C9 114.07(11) . . ?
C7 C8 C9 123.65(11) . . ?
F12 C21 C22 120.03(13) . . ?
F12 C21 C20 120.38(14) . . ?
C22 C21 C20 119.60(13) . . ?
C35 C33 C34 109.23(14) . . ?
C35 C33 C36 108.07(13) . . ?
C34 C33 C36 106.59(14) . . ?
C35 C33 P1 112.14(10) . . ?
C34 C33 P1 109.47(10) . . ?
C36 C33 P1 111.16(11) . . ?
C6 C4 C5 110.00(13) . . ?
C6 C4 S2 107.87(11) . . ?
C5 C4 S2 108.55(10) . . ?
F14 C23 C22 119.62(13) . . ?
F14 C23 C24 120.64(13) . . ?
C22 C23 C24 119.74(13) . . ?
F8 C16 C15 120.50(12) . . ?
F8 C16 C17 120.92(12) . . ?
C15 C16 C17 118.56(11) . . ?
F13 C22 C21 120.61(14) . . ?
F13 C22 C23 120.42(14) . . ?
C21 C22 C23 118.96(13) . . ?
C30 C29 C31 109.20(14) . . ?
C30 C29 C32 107.25(14) . . ?
C31 C29 C32 107.00(13) . . ?
C30 C29 P1 110.14(11) . . ?
C31 C29 P1 110.45(10) . . ?
C32 C29 P1 112.66(10) . . ?
C27 C25 C28 108.83(15) . . ?
C27 C25 C26 106.60(14) . . ?
C28 C25 C26 109.88(13) . . ?
C27 C25 P1 110.22(12) . . ?
C28 C25 P1 111.72(12) . . ?
C26 C25 P1 109.47(10) . . ?
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 C1 1.8328(14) . ?
S1 B1 1.9536(13) . ?
S2 C4 1.8613(14) . ?
S2 P1 2.0694(4) . ?
P1 C25 1.8774(14) . ?
P1 C29 1.8875(14) . ?
P1 C33 1.8982(13) . ?
F6 C14 1.3554(14) . ?
F10 C18 1.3506(15) . ?
F2 C9 1.3437(15) . ?
F1 C8 1.3424(14) . ?
F15 C24 1.3481(15) . ?
F5 C12 1.3543(15) . ?
F7 C15 1.3518(15) . ?
F11 C20 1.3522(16) . ?
F9 C17 1.3455(15) . ?
F4 C11 1.3501(15) . ?
F12 C21 1.3490(16) . ?
F13 C22 1.3427(16) . ?
F8 C16 1.3412(14) . ?
F3 C10 1.3448(15) . ?
F14 C23 1.3427(17) . ?
B1 C13 1.6410(17) . ?
B1 C19 1.6568(18) . ?
B1 C7 1.6599(18) . ?
C13 C14 1.3882(17) . ?
C13 C18 1.3983(17) . ?
C7 C8 1.3895(17) . ?
C7 C12 1.3930(16) . ?
C9 C10 1.376(2) . ?
C9 C8 1.3900(17) . ?
C19 C24 1.3904(18) . ?
C19 C20 1.3922(17) . ?
C14 C15 1.3875(17) . ?
C17 C16 1.376(2) . ?
C17 C18 1.3809(17) . ?
C15 C16 1.3729(19) . ?
C12 C11 1.3794(18) . ?
C10 C11 1.372(2) . ?
C24 C23 1.3879(19) . ?
C20 C21 1.3844(19) . ?
C1 C3 1.518(2) . ?
C1 C2 1.5254(19) . ?
C21 C22 1.368(2) . ?
C33 C35 1.533(2) . ?
C33 C34 1.540(2) . ?
C33 C36 1.546(2) . ?
C4 C6 1.518(2) . ?
C4 C5 1.518(2) . ?
C23 C22 1.375(2) . ?
C31 C29 1.542(2) . ?
C29 C30 1.532(3) . ?
C29 C32 1.545(2) . ?
C25 C27 1.536(3) . ?
C25 C28 1.537(2) . ?
C25 C26 1.540(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660744
2 PubChem 139127186
