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_7715320
_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_absolute_configuration unk
_chemical_formula_moiety         'C39 H63 B F12 P4 Si6'
_chemical_formula_sum            'C39 H63 B F12 P4 Si6'
_chemical_formula_weight         1063.148
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_audit_creation_date             2023-10-16
_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                 111.988(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6989(9)
_cell_length_b                   23.5345(17)
_cell_length_c                   8.3881(5)
_cell_measurement_reflns_used    5612
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      23.40
_cell_measurement_theta_min      2.48
_cell_volume                     2690.6(3)
_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      150.02
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.1308
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            46965
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9996
_diffrn_reflns_theta_full        24.9997
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1110.523
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.5121
_refine_diff_density_min         -0.4125
_refine_diff_density_rms         0.1014
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.09(6)
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             13.6297
_refine_ls_goodness_of_fit_ref   1.0347
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     580
_refine_ls_number_reflns         9445
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0347
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.3515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.999
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              27
_reflns_limit_k_min              -27
_reflns_limit_l_max              9
_reflns_limit_l_min              -9
_reflns_number_gt                7102
_reflns_number_total             9445
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt00251b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7715319--7715320.cif.'
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7715320
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C34(H34a,H34b,H34c), C37(H37a,H37b,H37c), C38(H38a,H38b,
 H38c), C39(H39a,H39b,H39c), C40(H40a,H40b,H40c), C41(H41a,H41b,H41c), C42(H42a,
 H42b,H42c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c), C45(H45a,H45b,H45c),
 C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c), C49(H49a,H49b,
 H49c), C50(H50a,H50b,H50c), C51(H51a,H51b,H51c), C52(H52a,H52b,H52c), C53(H53a,
 H53b,H53c), C57(H57a,H57b,H57c), C65(H65a,H65b,H65c)
;
_olex2_submission_special_instructions 'No special instructions were received'