Cooperative Lewis acidity in borane-substituted fluorophosphonium cations.
Möbus, Juri; Vom Stein, Thorsten; Stephan, Douglas W.; Chemical communications (Cambridge, England) 52 (2016) 6387–6390; doi:10.1039/c6cc02607a

data_7124631
_publ_section_title
;
 Cooperative Lewis acidity in borane-substituted fluorophosphonium
 cations.
;
_journal_issue                   38
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6387
_journal_page_last               6390
_journal_paper_doi               10.1039/c6cc02607a
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H32 B F5 P, B C24 F20'
_chemical_formula_sum            'C54 H32 B2 F25 P'
_chemical_formula_weight         1208.44
_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             2016-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-26 deposited with the CCDC.
2016-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.890(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7299(5)
_cell_length_b                   19.7985(8)
_cell_length_c                   12.1281(5)
_cell_measurement_reflns_used    6510
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      2.62
_cell_volume                     2562.84(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.9598
_diffrn_measured_fraction_theta_max 0.9596
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0803
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19974
_diffrn_reflns_theta_full        27.5269
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0681 before and 0.0619 after correction.
The Ratio of minimum to maximum transmission is 0.8692.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.5658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1213.3546
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.3420
_refine_diff_density_min         -0.3225
_refine_diff_density_rms         0.0717
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.11(9)
_refine_ls_d_res_high            0.7689
_refine_ls_d_res_low             12.0641
_refine_ls_goodness_of_fit_ref   1.0045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     738
_refine_ls_number_reflns         11300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0045
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.919
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              25
_reflns_limit_k_min              -22
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                8727
_reflns_number_total             11300
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6cc02607a2.cif
_cod_data_source_block           jm013_0m
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7124631
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C54(H54), C66(H66)
2.b Secondary CH2 refined with riding coordinates:
 C61(H61a,H61b), C69(H69a,H69b), C70(H70a,H70b), C71(H71a,H71b), C72(H72a,
 H72b), C74(H74a,H74b), C78(H78a,H78b), C79(H79a,H79b), C80(H80a,H80b),
 C81(H81a,H81b)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C37(H37), C44(H44), C47(H47), C49(H49), C53(H53), C56(H56),
 C60(H60), C73(H73), C76(H76)
;
_olex2_submission_special_instructions 'No special instructions were received'