Phosphirenium borate betaines from alkynylphosphanes and the halogeno-B(C<sub>6</sub>F<sub>5</sub>)<sub>2</sub> reagents.
Ueno, Atsushi; Möricke, Jennifer; Daniliuc, Constantin G.; Kehr, Gerald; Erker, Gerhard; Chemical communications (Cambridge, England) 54 (2018) 13746–13749; doi:10.1039/c8cc07189f

data_7122592
_publ_section_title
;
 Phosphirenium borate betaines from alkynylphosphanes and the
 halogeno-B(C<sub>6</sub>F<sub>5</sub>)<sub>2</sub> reagents.
;
_journal_issue                   97
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13746
_journal_page_last               13749
_journal_paper_doi               10.1039/c8cc07189f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C28 H23 B Br F10 P'
_chemical_formula_weight         671.15
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'APEX3 v2016.1-0'
_audit_update_record
;
2018-09-03 deposited with the CCDC.
2018-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9577(2)
_cell_length_b                   18.6647(5)
_cell_length_c                   16.5940(4)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    105.(2)
_cell_measurement_theta_max      72.1240
_cell_measurement_theta_min      3.5647
_cell_volume                     2773.50(12)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection
;

APEX3 v2016.1-0 (Bruker AXS Inc., 2016)
;
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      105.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'MX mirror'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46108
_diffrn_reflns_theta_full        72.39
_diffrn_reflns_theta_max         72.39
_diffrn_reflns_theta_min         3.56
_diffrn_source                   'Cu ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    3.351
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/5, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.419
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+2.1158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                4799
_reflns_number_total             5453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07189f2.cif
_cod_data_source_block           erk9221
_cod_depositor_comments
'Adding full bibliography for 7122588--7122592.cif.'
_cod_database_code               7122592
_shelx_res_checksum              81761