Palladium(ii) complexes with planar chiral ferrocenyl phosphane‒(benz)imidazol-2-ylidene ligands
Loxq, Pauline; Debono, Nathalie; Gülcemal, Süleyman; Daran, Jean-Claude; Manoury, Eric; Poli, Rinaldo; Çetinkaya, Bekir; Labande, Agnès; New Journal of Chemistry 38 (2014) 338–; doi:10.1039/c3nj00863k

data_7053986
_publ_section_title
;
 Palladium(ii) complexes with planar chiral ferrocenyl
 phosphane--(benz)imidazol-2-ylidene ligands
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              338
_journal_paper_doi               10.1039/c3nj00863k
_journal_volume                  38
_journal_year                    2014
_chemical_formula_moiety
'C42 H42 Fe N2 P S, B F4, 0.5(C H2 Cl2), 0.5(C4 H10 O)'
_chemical_formula_sum            'C44.5 H48 B Cl F4 Fe N2 O0.5 P S'
_chemical_formula_weight         859.99
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.942(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.6211(11)
_cell_length_b                   9.1000(4)
_cell_length_c                   34.9740(13)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.89
_cell_measurement_theta_min      2.36
_cell_volume                     8055.2(6)
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            42944
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Some residual electron density were difficult to modelize and therefore, the
SQUEEZE function of PLATON (Spek, 2003) 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 four cavities of 226 \%A^3^ per unitl cell. PLATON estimated that
each cavity contains 89 electrons which may correspond to a mixture of
dichloromethane CH~2~Cl~2~ and ether (C~2~H~5~)~2~O as suggested by the 
crystallization process.
;
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+9.1186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1029
_reflns_number_gt                6886
_reflns_number_total             8245
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3nj00863k.txt
_cod_data_source_block           2d-rac
_cod_original_sg_symbol_H-M      C2/C
_cod_original_formula_sum        'C44.50 H48 B Cl F4 Fe N2 O0.50 P S'
_cod_database_code               7053986