Increasing the Brønsted acidity of Ph2PO2H by the Lewis acid B(C6F5)3. Formation of an eight-membered boraphosphinate ring [Ph2POB(C6F5)2O]2.
Kather, Ralf; Rychagova, Elena; Sanz Camacho, Paula; Ashbrook, Sharon E.; Woollins, J. Derek; Robben, Lars; Lork, Enno; Ketkov, Sergey; Beckmann, Jens; Chemical communications (Cambridge, England) 52 (2016) 10992–10995; doi:10.1039/c6cc06102h

data_7125000
_publ_section_title
;
 Increasing the Br\/onsted acidity of Ph2PO2H by the Lewis acid B(C6F5)3.
 Formation of an eight-membered boraphosphinate ring [Ph2POB(C6F5)2O]2.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10992
_journal_page_last               10995
_journal_paper_doi               10.1039/c6cc06102h
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C24 H18 As Br'
_chemical_formula_weight         461.21
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1jccbl
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-07 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.2420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8919(3)
_cell_length_b                   8.4344(2)
_cell_length_c                   20.3175(6)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    100
_cell_measurement_theta_max      38.42
_cell_measurement_theta_min      2.62
_cell_volume                     1861.39(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Venture D8'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            79501
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         38.52
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    3.977
_exptl_absorpt_correction_T_max  0.3816
_exptl_absorpt_correction_T_min  0.2991
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.598
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         10457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.3135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                8700
_reflns_number_total             10457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc06102h3.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7125000