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_7053989
_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 H41 Cl2 Fe N2 P Pd, 0.5(C H4 O)'
_chemical_formula_sum            'C42.5 H43 Cl2 Fe N2 O0.5 P Pd'
_chemical_formula_weight         853.91
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                75.975(6)
_cell_angle_beta                 77.655(6)
_cell_angle_gamma                70.728(6)
_cell_formula_units_Z            2
_cell_length_a                   10.6863(8)
_cell_length_b                   13.7235(9)
_cell_length_c                   13.9621(9)
_cell_measurement_reflns_used    3579
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.1602
_cell_measurement_theta_min      3.6836
_cell_volume                     1855.1(2)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2012)'
_computing_data_reduction        CrysAlisPro
_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_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scan'
_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  0.0680
_diffrn_reflns_av_sigmaI/netI    0.1106
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11701
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
CrysAlisPro (Agilent Technologies)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       box
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_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 one cavity around the origin of 79 \%A^3^. PLATON 
estimated that the cavity contains 19 electrons which may correspond to a 
molecule of methanol CH~3~OH as suggested by the crystallization process 
;
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         5892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                4205
_reflns_number_total             5892
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3nj00863k.txt
_cod_data_source_block           4d-rac
_cod_original_formula_sum        'C42.50 H43 Cl2 Fe N2 O0.50 P Pd'
_cod_database_code               7053989