Nickel and Palladium Complexes of Ferrocene-Backbone Bisphosphine-Borane and Trisphosphine Ligands
Cowie, Bradley E.; Emslie, David J. H.; Organometallics 34 (2015) 4093–; doi:10.1021/acs.organomet.5b00539

data_4087725
_publ_section_title
;
 Nickel and Palladium Complexes of Ferrocene-Backbone Bisphosphine-Borane
 and Trisphosphine Ligands
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4093
_journal_paper_doi               10.1021/acs.organomet.5b00539
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C61 H55 Fe O P3 Pd, C H2 Cl2'
_chemical_formula_sum            'C62 H57 Cl2 Fe O P3 Pd'
_chemical_formula_weight         1144.14
_chemical_name_common            '[Pd(dba)(FcPPP)]'
_chemical_name_systematic
;
 brad30
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 106.827(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8528(9)
_cell_length_b                   18.6413(16)
_cell_length_c                   15.5813(14)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.248
_cell_measurement_theta_min      2.1955
_cell_volume                     2739.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27598
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.8803
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.7
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.30(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         7570
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+1.6574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                6638
_reflns_number_total             7570
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00539_si_002.cif
_cod_data_source_block           brad30
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4087725