Synthesis and Reactivity of Palladium Complexes Featuring a Diphosphinoborane Ligand
Schindler, Tobias; Lux, Marcel; Peters, Marius; Scharf, Lennart T.; Osseili, Hassan; Maron, Laurent; Tauchert, Michael E.; Organometallics 34 (2015) 1978–; doi:10.1021/acs.organomet.5b00217

data_4085804
_publ_section_title
;
 Synthesis and Reactivity of Palladium Complexes Featuring a
 Diphosphinoborane Ligand
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1978
_journal_paper_doi               10.1021/acs.organomet.5b00217
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C47 H38 B N P2 Pd'
_chemical_formula_sum            'C47 H38 B N P2 Pd'
_chemical_formula_weight         795.93
_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_creation_method           SHELXL-2013
_cell_angle_alpha                86.589(4)
_cell_angle_beta                 84.706(4)
_cell_angle_gamma                64.757(3)
_cell_formula_units_Z            2
_cell_length_a                   10.010(2)
_cell_length_b                   10.217(2)
_cell_length_c                   20.291(5)
_cell_measurement_reflns_used    5446
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.483
_cell_measurement_theta_min      2.395
_cell_volume                     1868.6(7)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20932
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.241
_diffrn_reflns_theta_min         2.204
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.421
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         10400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.4592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8752
_reflns_number_total             10400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00217_si_003.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4085802--4085804.cif.'
_cod_database_code               4085804
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.913
_shelxl_version_number           2013-4
_shelx_res_checksum              68674
_shelx_hkl_checksum              71808