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_7700365
_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            'C62 H64 B F10 O2 P'
_chemical_formula_weight         1072.91
_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_update_record
;
2017-12-19 deposited with the CCDC.    2019-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                91.125(2)
_cell_angle_beta                 96.291(2)
_cell_angle_gamma                102.327(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7327(7)
_cell_length_b                   15.3551(9)
_cell_length_c                   16.4471(10)
_cell_measurement_reflns_used    9188
_cell_measurement_temperature    101.(2)
_cell_measurement_theta_max      27.5546
_cell_measurement_theta_min      2.4942
_cell_volume                     3119.5(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection
;

APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)

;
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      101.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51649
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'Mo ImS'
_diffrn_source_type              'micro focus tube'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2014). SADABS, Version 2014/2, Bruker AXS Inc., Madison, Wisconsin,
USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.102
_platon_squeeze_details
;
Two badly disordered dichloromethane molecules were found in the
asymmetrical unit and could not be satisfactorily refined. The program
SQUEEZE (A. L. Spek J. Appl. Cryst., 2003, 36, 7-13) was therefore used 
to remove mathematically the effect of the solvent. 
The quoted formula and derived parameters are not included the squeezed
solvent molecules.
;
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         11327
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+4.4804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                8673
_reflns_number_total             11327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02624j2.cif
_cod_data_source_block           erk8763
_cod_depositor_comments
'Adding full bibliography for 7700359--7700368.cif.'
_cod_database_code               7700365
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              59498
_shelx_fab_checksum              30567