Palladium(II) and Platinum(II) Compounds of 1,1′-Bis(phosphino)metallocene (M = Fe, Ru) Ligands with Metal‒Metal Interactions
Gramigna, Kathryn M.; Oria, Jeremy V.; Mandell, Chelsea L.; Tiedemann, Margaret A.; Dougherty, William G.; Piro, Nicholas A.; Kassel, W. Scott; Chan, Benny C.; Diaconescu, Paula L.; Nataro, Chip; Organometallics 32 (2013) 5966–; doi:10.1021/om400494t

data_4089571
_publ_section_title
;
 Palladium(II) and Platinum(II) Compounds of
 1,1&#x2032;-Bis(phosphino)metallocene (M = Fe, Ru) Ligands with
 Metal--Metal Interactions
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5966
_journal_paper_doi               10.1021/om400494t
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C26.5 H45 Cl8 Fe P2 Pd Sb'
_chemical_formula_weight         993.16
_chemical_name_common            '[(dtbpf)PdCl][SbCl6].0.5(CH2Cl2)'
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 97.657(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.495(10)
_cell_length_b                   16.945(14)
_cell_length_c                   19.559(16)
_cell_measurement_reflns_used    2054
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.07
_cell_measurement_theta_min      2.29
_cell_volume                     3776(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.674
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1686
_diffrn_reflns_av_unetI/netI     0.1102
_diffrn_reflns_Laue_measured_fraction_full 0.674
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24957
_diffrn_reflns_point_group_measured_fraction_full 0.674
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         21.964
_diffrn_reflns_theta_min         1.596
_exptl_absorpt_coefficient_mu    2.230
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         4610
_refine_ls_number_restraints     1481
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+7.5529P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3065
_reflns_number_total             4610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400494t_si_001.cif
_cod_data_source_block           '[Pd(dtbpf)Cl]100K'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C26.50 H45 Cl8 Fe P2 Pd Sb'
_cod_database_code               4089571
_shelx_estimated_absorpt_t_min   0.610
_shelx_estimated_absorpt_t_max   0.852
_shelxl_version_number           2013-2
_shelx_res_checksum              66223
_shelx_hkl_checksum              24008