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_4324673
_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         'C43 H50 O P2 Rh, BF4, C6 H5.30 F0.7'
_chemical_formula_sum            'C49 H55.3 B F4.7 O P2 Rh'
_chemical_formula_weight         925.19
_chemical_name_common            complex3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                103.481(2)
_cell_angle_beta                 108.628(2)
_cell_angle_gamma                104.214(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8880(14)
_cell_length_b                   13.1496(14)
_cell_length_c                   14.7016(16)
_cell_measurement_reflns_used    4068
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.34
_cell_measurement_theta_min      2.56
_cell_volume                     2153.0(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            81982
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.528
_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            orange
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      1.427
_exptl_crystal_description       plate
_exptl_crystal_F_000             959
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         9711
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+2.3449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                7369
_reflns_number_total             9711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102373w_si_001_1.cif
_cod_data_source_block           complex3
_cod_original_formula_sum        'C49 H55.30 B F4.70 O P2 Rh'
_cod_database_code               4324673