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_7122591
_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            'C39.5 H35 B Br F10 P'
_chemical_formula_weight         821.36
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                82.3630(10)
_cell_angle_beta                 76.1530(10)
_cell_angle_gamma                76.8730(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5895(3)
_cell_length_b                   10.8563(3)
_cell_length_c                   18.7360(5)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      66.6946
_cell_measurement_theta_min      4.6758
_cell_volume                     1837.99(9)
_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    'APEX3 v2016.1-0 (Bruker AXS Inc., 2016)'
_computing_publication_material  'APEX3 v2016.1-0 (Bruker AXS Inc., 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Kappa CCD APEXII'
_diffrn_measurement_method       'phi / omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24093
_diffrn_reflns_theta_full        66.69
_diffrn_reflns_theta_max         66.69
_diffrn_reflns_theta_min         4.68
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.642
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.72
_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    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         6361
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0455P)^2^+0.6136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                5558
_reflns_number_total             6361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07189f2.cif
_cod_data_source_block           erk9236
_cod_depositor_comments
'Adding full bibliography for 7122588--7122592.cif.'
_cod_original_formula_sum        'C39.50 H35 B Br F10 P'
_cod_database_code               7122591
_shelx_res_checksum              28350