Synthesis and Characterization of Pd Complexes of a Carbazolyl/Bis(Imine) NNN Pincer Ligand
Aaron M. Hollas; Weixing Gu; Nattamai Bhuvanesh; Oleg V. Ozerov; Inorganic Chemistry 50 (2011) 3673–3679; doi:10.1021/ic200026p

data_4324897
_publ_section_title
;
 Synthesis and Characterization of Pd Complexes of a Carbazolyl/Bis(Imine)
 NNN Pincer Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3673
_journal_page_last               3679
_journal_paper_doi               10.1021/ic200026p
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C136 H136 Cl4 N12 Pd4'
_chemical_formula_weight         2505.97
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.777(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   13.7812(16)
_cell_length_b                   11.6200(13)
_cell_length_c                   20.450(3)
_cell_measurement_reflns_used    1314
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      49.38
_cell_measurement_theta_min      3.66
_cell_volume                     2870.4(7)
_computing_cell_refinement
; 
  CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) 
;
_computing_data_collection       'FRAMBO (BRUKER-NONIUS, 2003)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'BRUKER GADDS D8 Discover'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_sigmaI/netI    0.1033
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15774
_diffrn_reflns_theta_full        59.16
_diffrn_reflns_theta_max         59.16
_diffrn_reflns_theta_min         3.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.276
_exptl_absorpt_correction_T_max  0.8341
_exptl_absorpt_correction_T_min  0.6336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.766
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.766
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                2384
_reflns_number_total             4075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200026p_si_002.cif
_cod_data_source_block           tri
_cod_original_cell_volume        2870.4(6)
_cod_database_code               4324897