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_7053987
_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
'C36 H35 Cl2 Fe N2 P Pd, 1.5(C H2 Cl2), 0.5(C4 H10 0)'
_chemical_formula_sum            'C39.5 H43 Cl5 Fe N2 O0.5 P Pd'
_chemical_formula_weight         924.23
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 95.076(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.0431(10)
_cell_length_b                   9.7619(3)
_cell_length_c                   12.6606(4)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.67
_cell_measurement_theta_min      2.63
_cell_volume                     3821.6(2)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        APEX2
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32604
_diffrn_reflns_theta_full        30.72
_diffrn_reflns_theta_max         30.72
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_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 two  cavities of 188 \%A^3^ per unitl cell. PLATON estimated that
each cavity contains 86 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         0.567
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         11489
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                10600
_reflns_number_total             11489
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3nj00863k.txt
_cod_data_source_block           4B-S
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C39.50 H43 Cl5 Fe N2 O0.50 P Pd'
_cod_database_code               7053987