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_4085802
_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 H41 B O2 P2 Pd, 1.5(C6 H6)'
_chemical_formula_sum            'C56 H50 B O2 P2 Pd'
_chemical_formula_weight         934.11
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-11-17
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                66.69(3)
_cell_angle_beta                 77.83(3)
_cell_angle_gamma                71.49(3)
_cell_formula_units_Z            2
_cell_length_a                   9.874(2)
_cell_length_b                   14.424(3)
_cell_length_c                   18.105(4)
_cell_measurement_reflns_used    7315
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.292
_cell_measurement_theta_min      2.257
_cell_volume                     2234.8(10)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.928
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33952
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.67
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           600.0
_diffrn_source_power             30.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0893 before and 0.0517 after correction.
The Ratio of minimum to maximum transmission is 0.8063.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             966
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         12824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0450P)^2^+0.5873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                10936
_reflns_number_total             12824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00217_si_004.cif
_cod_data_source_block           mp29c
_cod_depositor_comments
'Adding full bibliography for 4085802--4085804.cif.'
_cod_original_cell_volume        2234.8(8)
_cod_database_code               4085802