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_7053985
_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         'C33 H32 Fe N2 P S, B F4'
_chemical_formula_sum            'C33 H32 B F4 Fe N2 P S'
_chemical_formula_weight         662.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.896(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8546(5)
_cell_length_b                   7.6314(4)
_cell_length_c                   36.279(3)
_cell_measurement_reflns_used    9600
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.5841
_cell_measurement_theta_min      2.7839
_cell_volume                     2989.3(3)
_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 8.2632
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_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  0.0791
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            27251
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84287
_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, 2010)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       box
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.399
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5262
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0818
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+18.7798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1766
_reflns_number_gt                4694
_reflns_number_total             5262
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3nj00863k.txt
_cod_data_source_block           2c-rac
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7053985