Carbon-carbon bond forming reactions of acetylenic esters and ketones within frustrated phosphane/borane Lewis pair frameworks.
Wang, Long; Li, Jun; Deng, Dongsheng; Daniliuc, Constantin G.; Mück-Lichtenfeld, Christian; Kehr, Gerald; Erker, Gerhard; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11921–11926; doi:10.1039/c9dt02624j

data_7700360
_publ_section_title
;
 Carbon-carbon bond forming reactions of acetylenic esters and ketones
 within frustrated phosphane/borane Lewis pair frameworks.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11921
_journal_page_last               11926
_journal_paper_doi               10.1039/c9dt02624j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C52 H60 B F10 O4 P'
_chemical_formula_weight         980.78
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
;
2018-05-22 deposited with the CCDC.    2019-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                108.8480(10)
_cell_angle_beta                 105.7530(10)
_cell_angle_gamma                101.7290(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6159(2)
_cell_length_b                   14.1771(2)
_cell_length_c                   16.6822(4)
_cell_measurement_reflns_used    6969
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     2779.38(9)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25411
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.09
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.9963
_exptl_absorpt_correction_T_min  0.9843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
A badly disordered pentane molecule was found in the 
asymmetrical unit and could not be satisfactorily refined. The program 
SQUEEZE (Spek, A.L. (2015). Acta Cryst. C71, 9-18.) was therefore used to
remove mathematically the effect of the solvent.
The quoted formula and derived parameters are not included the squeezed
solvent molecule. 
;
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         9536
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0729
_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^)+(0.0542P)^2^+4.3632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                6984
_reflns_number_total             9536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt02624j2.cif
_cod_data_source_block           erk8623
_cod_depositor_comments
'Adding full bibliography for 7700359--7700368.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7700360
_platon_squeeze_void_probe_radius 1.20