Influence of the Ligand Backbone in Pincer Complexes: Indenediide-, Indolyl-, and Indenyl-Based SCS Palladium Complexes
Lisena, Jérôme; Monot, Julien; Mallet-Ladeira, Sonia; Martin-Vaca, Blanca; Bourissou, Didier; Organometallics 32 (2013) 4301–; doi:10.1021/om400464j

data_4081127
_publ_section_title
;
 Influence of the Ligand Backbone in Pincer Complexes: Indenediide-,
 Indolyl-, and Indenyl-Based SCS Palladium Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4301
_journal_paper_doi               10.1021/om400464j
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C50 H39 N P3 Pd S2, B F4, 2(C H2 Cl2)'
_chemical_formula_sum            'C52 H43 B Cl4 F4 N P3 Pd S2'
_chemical_formula_weight         1173.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 105.865(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1982(3)
_cell_length_b                   30.8703(14)
_cell_length_c                   18.8299(7)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.34
_cell_measurement_wavelength     0.71073
_cell_volume                     5143.1(3)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            58403
_diffrn_reflns_theta_full        30.58
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         1.3
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.491
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.163
_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     865
_refine_ls_number_reflns         15570
_refine_ls_number_restraints     689
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0988P)^2^+0.5811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1792
_reflns_number_gt                10400
_reflns_number_total             15570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400464j_si_002.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4081127