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_7124630
_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_formula_moiety         'C30 H36 B F2 P'
_chemical_formula_sum            'C30 H36 B F2 P'
_chemical_formula_weight         476.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2016-03-20
_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                76.806(2)
_cell_angle_beta                 71.844(2)
_cell_angle_gamma                82.615(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9138(3)
_cell_length_b                   10.3236(3)
_cell_length_c                   13.6951(4)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.28
_cell_volume                     1294.20(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      148.8
_diffrn_measured_fraction_theta_full 0.9919
_diffrn_measured_fraction_theta_max 0.9919
_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  0.0183
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20829
_diffrn_reflns_theta_full        27.4237
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0367 before and 0.0292 after correction.
The Ratio of minimum to maximum transmission is 0.9344.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             508.4330
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.3940
_refine_diff_density_min         -0.2997
_refine_diff_density_rms         0.0566
_refine_ls_d_res_high            0.7716
_refine_ls_d_res_low             12.7511
_refine_ls_goodness_of_fit_ref   1.0467
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    62
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0467
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0571P)^2^+0.4906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4919
_reflns_number_total             5868
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6cc02607a2.cif
_cod_data_source_block           TVS001_0m
_cod_database_code               7124630
_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:
 C7(H7), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C23(H23a,H23b), C25(H25a,H25b),
 C26(H26a,H26b), C27(H27a,H27b), C28(H28a,H28b), C29(H29a,H29b), C5(H5a,H5b)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16),
 C19(H19), C20(H20), C21(H21), C22(H22), C30(H30), C31(H31)
;
_olex2_submission_special_instructions 'No special instructions were received'