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_4089566
_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            'C58 H76 B2 F8 Fe O2.5 P3 Pd'
_chemical_formula_weight         1241.97
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.477(2)
_cell_angle_beta                 86.866(2)
_cell_angle_gamma                76.638(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5777(5)
_cell_length_b                   13.0199(5)
_cell_length_c                   17.0800(6)
_cell_measurement_reflns_used    2894
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      21.73
_cell_measurement_theta_min      2.40
_cell_volume                     2702.52(18)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_sigmaI/netI    0.2485
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45666
_diffrn_reflns_theta_full        33.16
_diffrn_reflns_theta_max         33.16
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.9775
_exptl_absorpt_correction_T_min  0.8750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1286
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
There were multiple molecules of disordered diethylether solvent in
the difference map. The SQUEEZE results are consistet with 2.5 molecules of
diethylether. The empirical formula was modified to include these solvent
molecules.

PLATON Reference : Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
                     Spek, A.L. (2009). Acta Cryst. D65, 148-155.
;
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         20530
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1829
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                7543
_reflns_number_total             20530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400494t_si_001.cif
_cod_data_source_block           '[Pd(dppdtbpf)PPh3]'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2702.53(18)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C58 H76 B2 F8 Fe O2.50 P3 Pd'
_cod_database_code               4089566