Redox-active phosphines: synthesis and crystal structures of palladium(ii) complexes of a metallaphosphine in two different oxidation states.
Tohmé, Ayham; Labouille, Stéphanie; Roisnel, Thierry; Dorcet, Vincent; Carmichael, Duncan; Paul, Frédéric; Dalton transactions (Cambridge, England : 2003) 43 (2014) 7002–7005; doi:10.1039/c4dt00455h

data_7029598
_publ_section_title
;
 Redox-active phosphines: synthesis and crystal structures of
 palladium(ii) complexes of a metallaphosphine in two different oxidation
 states.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7002
_journal_page_last               7005
_journal_paper_doi               10.1039/c4dt00455h
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C100 H98 Cl4 Fe2 P6 Pd2, 2(F6 P)'
_chemical_formula_sum            'C100 H98 Cl4 F12 Fe2 P8 Pd2'
_chemical_formula_weight         2241.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-01-21T17:13:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                91.262(2)
_cell_angle_beta                 98.633(2)
_cell_angle_gamma                106.329(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1942(4)
_cell_length_b                   14.2910(6)
_cell_length_c                   19.6889(8)
_cell_measurement_reflns_used    4538
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.4
_cell_measurement_wavelength     0.71073
_cell_volume                     2448.90(18)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 1999),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.97
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28200
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.52
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.053
_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^)+(0.0344P)^2^+5.7105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                6740
_reflns_number_total             10716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00455h2.cif
_cod_data_source_block           AY243
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-12899/cifs/7029598.cif.
;
_cod_database_code               7029598