Study of the Conformationally Flexible, Wide Bite-Angle Diphosphine 4,6-Bis(3-diisopropylphosphinophenyl)dibenzofuran in Rhodium(I) and Palladium(II) Coordination Complexes
Keying Ding; Deanna L. Miller; Victor G. Young; Connie C. Lu; Inorganic Chemistry 50 (2011) 2545–2552; doi:10.1021/ic102373w

data_4324675
_publ_section_title
;
 Study of the Conformationally Flexible, Wide Bite-Angle Diphosphine
 4,6-Bis(3-diisopropylphosphinophenyl)dibenzofuran in Rhodium(I) and
 Palladium(II) Coordination Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2545
_journal_page_last               2552
_journal_paper_doi               10.1021/ic102373w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C40 H48 N2 O P2 Pd, B F4, B F4, C2 H3 N'
_chemical_formula_sum            'C42 H51 B2 F8 N3 O P2 Pd'
_chemical_formula_weight         955.82
_chemical_name_common            complex5
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 95.942(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5799(9)
_cell_length_b                   11.3663(9)
_cell_length_c                   33.729(3)
_cell_measurement_reflns_used    3992
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.52
_cell_volume                     4415.6(6)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            42213
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.8958
_exptl_absorpt_correction_T_min  0.8062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R.Blessing, 1995'
_exptl_crystal_colour            light_yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         7836
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0327P)^2^+8.1982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                6233
_reflns_number_total             7836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102373w_si_001_3.cif
_cod_data_source_block           complex5
_cod_original_cell_volume        4415.5(6)
_cod_database_code               4324675