A new <i>P</i>,<i>S</i>-coordinating ferrocenyl ligand: synthesis of a precursor and its coordination compounds with Pd^II^ and Pt^II^
Mouas Toma, Nardjes; Daran, Jean-Claude; Merazig, Hocine; Manoury, Eric; Acta Crystallographica Section C 70 (2014) 460–464; doi:10.1107/S2053229614007554

data_2019514
_publ_section_title
;
 A new <i>P</i>,<i>S</i>-coordinating ferrocenyl ligand: synthesis of a
 precursor and its coordination compounds with Pd^II^ and Pt^II^
;
_journal_coeditor_code           FA3335
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              460
_journal_page_last               464
_journal_paper_doi               10.1107/S2053229614007554
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Fe2 Pd2 (C5 H5)2 (C18 H15 P1 S1)2 Cl2] , 2C5 H12'
_chemical_formula_moiety         'C46 H40 Cl2 Fe2 P2 Pd2 S2, 2(C5 H12)'
_chemical_formula_sum            'C56 H64 Cl2 Fe2 P2 Pd2 S2'
_chemical_formula_weight         1258.53
_chemical_name_systematic
;(<i>R</i>,<i>R</i>/<i>S</i>,<i>S</i>)-Bis{\m-[2-(diphenylphosphanyl)ferrocen-1-yl]methanethiolato-\k^3^<i>P</i>,<i>S</i>:<i>S</i>}bis[chloridopalladium(II)]
pentane disolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL2013
_cell_angle_alpha                90
_cell_angle_beta                 105.6530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5734(4)
_cell_length_b                   11.0824(2)
_cell_length_c                   21.1091(4)
_cell_measurement_reflns_used    9010
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      36.28
_cell_measurement_theta_min      2.35
_cell_volume                     5084.96(16)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
2012) and
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0255
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78869
_diffrn_reflns_theta_full        26.400
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.874
_exptl_absorpt_coefficient_mu    1.544
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Some residual electron densities were difficult to modelize and therefore, the
SQUEEZE function of PLATON (Spek, 2009) was used to eliminate the contribution
of the electron density in the solvent region from the intensity data, and the
solvent-free model was employed for the final refinement.
There are two cavities of 682 \%A^3^ per unitl cell. PLATON estimated that
each cavity contains 197 electrons which might correspond roughly to 4 solvent
molecules of pentane as suggested by the crystallization process.
;
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0132P)^2^+14.9112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0508
_reflns_number_gt                4742
_reflns_number_total             5210
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3335sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 2019513--2019515.cif.'
_cod_database_code               2019514
_cod_database_fobs_code          2019514
_shelx_estimated_absorpt_t_min   0.422
_shelx_estimated_absorpt_t_max   0.749