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_4089568
_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            'C134 H84 B2 Cl4 F48 Fe2 P4 Pd2'
_chemical_formula_weight         3217.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                64.5900(10)
_cell_angle_beta                 78.8830(10)
_cell_angle_gamma                81.4070(10)
_cell_formula_units_Z            1
_cell_length_a                   14.6916(4)
_cell_length_b                   14.7206(4)
_cell_length_c                   16.7870(4)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      2.43
_cell_volume                     3208.64(15)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49892
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.502
_diffrn_reflns_theta_min         1.357
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       block
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         17806
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0289P)^2^+2.5256P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13918
_reflns_number_total             17806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400494t_si_001.cif
_cod_data_source_block           '[Pd2(dppf)2(u-Cl)2]'
_cod_database_code               4089568
_shelx_estimated_absorpt_t_min   0.864
_shelx_estimated_absorpt_t_max   0.929
_shelxl_version_number           2013-2
_shelx_res_checksum              56607
_shelx_hkl_checksum              4569