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_7124632
_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 H32 B F6 P'
_chemical_formula_sum            'C30 H32 B F6 P'
_chemical_formula_weight         548.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_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                 92.863(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4351(8)
_cell_length_b                   9.5654(5)
_cell_length_c                   24.6131(17)
_cell_measurement_reflns_used    4037
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      2.28
_cell_volume                     2688.9(3)
_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      150.03
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_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  0.0629
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23820
_diffrn_reflns_theta_full        27.4315
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         1.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0647 before and 0.0597 after correction.
The Ratio of minimum to maximum transmission is 0.9504.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.3545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1145.1426
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.4582
_refine_diff_density_min         -0.4240
_refine_diff_density_rms         0.0992
_refine_ls_d_res_high            0.7714
_refine_ls_d_res_low             10.5611
_refine_ls_goodness_of_fit_ref   1.0406
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0406
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0374P)^2^+0.4861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              -12
_reflns_number_gt                4182
_reflns_number_total             6127
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6cc02607a2.cif
_cod_data_source_block           jm011_2_0m
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7124632
_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:
 C8(H8), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C20(H20a,H20b), C26(H26a,H26b), C27(H27a,H27b), C29(H29a,
 H29b), C31(H31a,H31b), C32(H32a,H32b), C33(H33a,H33b), C34(H34a,H34b),
 C37(H37a,H37b)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25),
 C30(H30), C35(H35), C36(H36)
;
_olex2_submission_special_instructions 'No special instructions were received'