Triple <i>para</i>-substitution reactions of B(C<sub>6</sub>F<sub>5</sub>)<sub>3</sub> and [(C<sub>6</sub>F<sub>5</sub>)<sub>3</sub>PF]<sup>+</sup> with P(SiMe<sub>3</sub>)<sub>3</sub>.
Thomson, Jordan; Michailovich, Sofia; Miao, Linkun; Farrell, Jeffrey M.; Murray, Jillian A.; Lough, Alan; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5775–5778; doi:10.1039/d4dt00251b

data_7715319
_publ_section_title
;
 Triple <i>para</i>-substitution reactions of
 B(C<sub>6</sub>F<sub>5</sub>)<sub>3</sub> and
 [(C<sub>6</sub>F<sub>5</sub>)<sub>3</sub>PF]<sup>+</sup> with
 P(SiMe<sub>3</sub>)<sub>3</sub>.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5775
_journal_page_last               5778
_journal_paper_doi               10.1039/d4dt00251b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C48 H81 B F12 P4 Si6, 0.5[C5H12]'
_chemical_formula_sum            'C50.5 H87 B F12 P4 Si6'
_chemical_formula_weight         1225.466
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_Int_Tables_number      148
_audit_creation_date             2023-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-25 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   16.808(2)
_cell_length_b                   16.808(2)
_cell_length_c                   81.648(14)
_cell_measurement_reflns_used    9395
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      66.05
_cell_measurement_theta_min      6.10
_cell_volume                     19976(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.9762
_diffrn_measured_fraction_theta_max 0.9762
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CMOS PHOTON II'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.9762
_diffrn_reflns_Laue_measured_fraction_max 0.9762
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       95
_diffrn_reflns_limit_l_min       -96
_diffrn_reflns_number            130603
_diffrn_reflns_point_group_measured_fraction_full 0.9762
_diffrn_reflns_point_group_measured_fraction_max 0.9762
_diffrn_reflns_theta_full        24.9557
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.42
_diffrn_source_current           0.63
_diffrn_source_power             0.0282051
_diffrn_source_voltage           44.77
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0946 before and 0.0597 after correction.
The Ratio of minimum to maximum transmission is 0.8119.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       Shard
_exptl_crystal_F_000             7779.609
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.7956
_refine_diff_density_min         -0.2993
_refine_diff_density_rms         0.0461
_refine_ls_d_res_high            0.8423
_refine_ls_d_res_low             14.3301
_refine_ls_goodness_of_fit_ref   1.0420
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    74
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0420
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+32.7583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              96
_reflns_limit_l_min              -96
_reflns_number_gt                7188
_reflns_number_total             7620
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00251b2.cif
_cod_data_source_block           cu_d23122
_cod_depositor_comments
'Adding full bibliography for 7715319--7715320.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C50.5 H87 B1 F12 P4 Si6'
_cod_database_code               7715319
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C2(0.33333) C3(0.33333) C1(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C23(H23a,H23b), C36(H36a,H36b), C27(H27a,H27b), C28(H28a,
 H28b), C29(H29a,H29b)
3.b Idealised Me refined as rotating group:
 C30(H30a,H30b,H30c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C34(H34a,H34b,
 H34c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C56(H56a,H56b,H56c), C26(H26a,
 H26b,H26c), C31(H31a,H31b,H31c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c),
 C40(H40a,H40b,H40c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'