Palladium(II) Complexes of Bowls, Pinwheels, Cages, and N,C,N-Pincers of Starburst Ligands 1,3,5-Tris(di-2-pyridylamino)benzene and 2,4,6-Tris(di-2-pyridylamino)-1,3,5-triazene
Corey Seward; Wen-li Jia; Rui-Yao Wang; Suning Wang; Inorganic Chemistry 43 (2004) 978–985; doi:10.1021/ic034934a

data_4310516
_publ_section_title
;
 Palladium(II) Complexes of Bowls, Pinwheels, Cages, and N,C,N-Pincers of
 Starburst Ligands 1,3,5-Tris(di-2-pyridylamino)benzene and
 2,4,6-Tris(di-2-pyridylamino)-1,3,5-triazene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              978
_journal_page_last               985
_journal_paper_doi               10.1021/ic034934a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C3.22 H3.3 Cl0.11 N0.49 O0.7 Pd0.16'
_chemical_formula_weight         81.10
_chemical_name_systematic
; 
 ? 
;
_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                69.253(8)
_cell_angle_beta                 74.993(9)
_cell_angle_gamma                82.484(10)
_cell_formula_units_Z            37
_cell_length_a                   12.611(6)
_cell_length_b                   15.569(7)
_cell_length_c                   17.267(8)
_cell_measurement_temperature    180(2)
_cell_volume                     3059(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.1764
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22013
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1514
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         13839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                6559
_reflns_number_total             13839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034934asi20031105_014323.cif
_cod_data_source_block           cs230
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3060(2)
_cod_original_formula_sum        'C3.22 H3.30 Cl0.11 N0.49 O0.70 Pd0.16'
_cod_database_code               4310516