Platinum(0)-Catalyzed Diboration of Alkynylboronates and Alkynylphosphonates with Bis(pinacolato)diborane(4): Molecular Structures of [((Me4C2O2)B)(C6H5)CC(P(O)(OC2H5)2)(B(O2C2Me4))] and [((Me4C2O2)B)(C4H9)CC(B(O2C2Me4))2]
Ali, Hijazi Abu; El Aziz Al Quntar, Abed; Goldberg, Israel; Srebnik, Morris; Organometallics 21 (2002) 4533–; doi:10.1021/om020334s

data_4076947
_publ_section_title
;
 Platinum(0)-Catalyzed Diboration of Alkynylboronates and
 Alkynylphosphonates with Bis(pinacolato)diborane(4):&#x00A0; Molecular
 Structures of [((Me4C2O2)B)(C6H5)CC(P(O)(OC2H5)2)(B(O2C2Me4))] and
 [((Me4C2O2)B)(C4H9)CC(B(O2C2Me4))2]
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4533
_journal_paper_doi               10.1021/om020334s
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C24 H39 B2 O7 P'
_chemical_formula_weight         492.14
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2840(2)
_cell_length_b                   11.9170(2)
_cell_length_c                   21.7700(5)
_cell_measurement_reflns_used    2653
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      1.95
_cell_volume                     2668.01(9)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3572
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_correction_T_min  0.9518
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     404
_refine_ls_number_reflns         3572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.478
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+2.2118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                2653
_reflns_number_total             3572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020334s.cif
_cod_data_source_block           5b
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4076947