Bis{2-[(3,5-diphenyl-1<i>H</i>-pyrrol-2-ylidene-κ<i>N</i>)amino]-3,5-diphenylpyrrol-1-ido-κ<i>N</i>}palladium(II): a homoleptic four-coordinate tetraphenylazadipyrromethene complex of palladium
Jones, Roderick C.; Müller-Bunz, Helge; Evans, Paul; O'Shea, Donal F.; Acta Crystallographica Section C 70 (2014) 165–168; doi:10.1107/S2053229614000084

data_2019387
_publ_section_title
;
 Bis{2-[(3,5-diphenyl-1<i>H</i>-pyrrol-2-ylidene-\k<i>N</i>)amino]-3,5-diphenylpyrrol-1-ido-\k<i>N</i>}palladium(II):
 a homoleptic four-coordinate tetraphenylazadipyrromethene complex of
 palladium
;
_journal_coeditor_code           GZ3242
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              165
_journal_page_last               168
_journal_paper_doi               10.1107/S2053229614000084
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Pd (C32 H22 N3)2]'
_chemical_formula_moiety         'C64 H44 N6 Pd'
_chemical_formula_sum            'C64 H44 N6 Pd'
_chemical_formula_weight         1003.45
_chemical_name_systematic
Bis{2-[(3,5-diphenyl-1<i>H</i>-pyrrol-2-ylidene-\k<i>N</i>)amino]-3,5-diphenylpyrrol-1-ido-\k<i>N</i>}palladium(II)
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.665(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.9269(4)
_cell_length_b                   11.9137(3)
_cell_length_c                   14.0158(5)
_cell_measurement_reflns_used    3352
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.1084
_cell_measurement_theta_min      3.1719
_cell_volume                     2309.80(12)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type
'Agilent SuperNova Dual diffractometer (Cu at zero) with Atlas detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8633
_diffrn_reflns_theta_full        58.00
_diffrn_reflns_theta_max         62.20
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    3.638
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2011), based on expressions derived by Clark &
Reid
(1995)]
;
_exptl_crystal_colour            'metallic brown'
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.0628
_exptl_crystal_size_mid          0.0304
_exptl_crystal_size_min          0.0167
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.540
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         3515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0552P)^2^+3.8109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                2879
_reflns_number_total             3515
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3242sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019387
_cod_database_fobs_code          2019387