A T-shape diphosphinoborane palladium(0) complex.
Steinhoff, Patrick; Tauchert, Michael E.; Beilstein journal of organic chemistry 12 (2016) 1573–1576; doi:10.3762/bjoc.12.152

data_4032041
_publ_section_title
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 A T-shape diphosphinoborane palladium(0) complex.
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_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              1573
_journal_page_last               1576
_journal_paper_doi               10.3762/bjoc.12.152
_journal_volume                  12
_journal_year                    2016
_chemical_formula_moiety         'C42 H57 B P2 Pd, C6 H14'
_chemical_formula_sum            'C48 H71 B P2 Pd'
_chemical_formula_weight         827.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.704(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3000(10)
_cell_length_b                   14.4355(13)
_cell_length_c                   26.239(2)
_cell_measurement_reflns_used    6767
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.29
_cell_volume                     4265.7(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            51374
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           600.0
_diffrn_source_power             30.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1529 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.7876.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0302P)^2^+3.0596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                7600
_reflns_number_total             8861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-12-152-S2.cif
_cod_data_source_block           q15_a78sadm
_cod_depositor_comments          'Adding full bibliography for 4032041.cif.'
_cod_original_cell_volume        4265.7(7)
_cod_database_code               4032041
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C50(H50), C70(H70), C60(H60), C40(H40)
2.b Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C62(H62A,H62B), C45(H45A,H45B), C74(H74A,H74B), C54(H54A,
 H54B), C51(H51A,H51B), C53(H53A,H53B), C63(H63A,H63B), C44(H44A,H44B),
 C42(H42A,H42B), C55(H55A,H55B), C52(H52A,H52B), C71(H71A,H71B), C75(H75A,H75B),
  C41(H41A,H41B), C72(H72A,H72B), C43(H43A,H43B), C61(H61A,H61B), C64(H64A,
 H64B), C73(H73A,H73B), C84(H84A,H84B), C81(H81A,H81B), C83(H83A,H83B),
 C82(H82A,H82B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C24(H24), C13(H13), C32(H32), C12(H12), C21(H21), C31(H31),
 C22(H22), C34(H34), C33(H33), C14(H14), C11(H11), C23(H23)
2.d Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C85(H85A,H85B,H85C)
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_olex2_submission_special_instructions 'No special instructions were received'