Phosphole formation by 1,1-carboboration - reactions of bis-alkynyl phosphanes with a frustrated P/B Lewis pair.
Klose, Annika; Kehr, Gerald; Daniliuc, Constantin G.; Erker, Gerhard; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2023–2030; doi:10.1039/c5dt03055b

data_7036416
_publ_section_title
;
 Phosphole formation by 1,1-carboboration - reactions of bis-alkynyl
 phosphanes with a frustrated P/B Lewis pair.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2023
_journal_page_last               2030
_journal_paper_doi               10.1039/c5dt03055b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C63 H59 B F10 P2'
_chemical_formula_weight         1078.85
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-08-03 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                97.778(2)
_cell_angle_beta                 99.423(2)
_cell_angle_gamma                118.030(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8113(5)
_cell_length_b                   14.0951(5)
_cell_length_c                   16.4458(9)
_cell_measurement_reflns_used    8291
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     2703.8(2)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36369
_diffrn_reflns_theta_full        67.40
_diffrn_reflns_theta_max         67.40
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_T_max  0.9601
_exptl_absorpt_correction_T_min  0.8212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         9284
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0767P)^2^+1.1913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1546
_reflns_number_gt                6932
_reflns_number_total             9284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03055b2.cif
_cod_data_source_block           erk7416
_cod_depositor_comments
'Adding full bibliography for 7036415--7036417.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7036416