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_4089572
_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
_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                 98.126(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.617(4)
_cell_length_b                   17.131(6)
_cell_length_c                   19.290(6)
_cell_measurement_reflns_used    845
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.05
_cell_measurement_theta_min      2.27
_cell_volume                     3800(2)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.793
_diffrn_measured_fraction_theta_max 0.997
_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  0.1051
_diffrn_reflns_Laue_measured_fraction_full 0.793
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10984
_diffrn_reflns_point_group_measured_fraction_full 0.793
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.281
_diffrn_reflns_theta_min         1.597
_exptl_absorpt_coefficient_mu    2.215
_exptl_absorpt_correction_T_max  0.744894
_exptl_absorpt_correction_T_min  0.553388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.736
_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         0.843
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5572
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0439P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3354
_reflns_number_total             5572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400494t_si_001.cif
_cod_data_source_block           '[Pd(dtbpf)Cl]296KafterLT'
_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               4089572
_shelx_estimated_absorpt_t_min   0.612
_shelx_estimated_absorpt_t_max   0.853
_shelxl_version_number           2013-2
_shelx_res_checksum              91522
_shelx_hkl_checksum              49674