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_4087722
_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_formula_moiety         'C44 H41 B Fe Ni P2, 0.7(C7 H8)'
_chemical_formula_sum            'C48.9 H46.6 B Fe Ni P2'
_chemical_formula_weight         821.588
_chemical_name_common            '[Ni(FcPPB)]'
_chemical_name_systematic
;
 brad42
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_cell_angle_alpha                90
_cell_angle_beta                 99.260(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.051(3)
_cell_length_b                   19.984(5)
_cell_length_c                   19.267(5)
_cell_measurement_reflns_used    2867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.558
_cell_measurement_theta_min      2.292
_cell_volume                     3819.5(18)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0911
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35960
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8548
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         0.5
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0561P)^2^+0.4918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.124
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                5983
_reflns_number_total             7868
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00539_si_002.cif
_cod_data_source_block           brad42
_cod_original_cell_volume        3819.6(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4087722