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_4310515
_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            'C51.78 H54.67 Cl1.78 N10.67 O12.22 Pd2.67'
_chemical_formula_weight         1368.71
_chemical_name_systematic
; 
 ? 
;
_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                 100.918(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            9
_cell_length_a                   14.678(4)
_cell_length_b                   28.666(8)
_cell_length_c                   29.930(7)
_cell_measurement_temperature    180(2)
_cell_volume                     12365(6)
_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 0.923
_diffrn_measured_fraction_theta_max 0.923
_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  0.1418
_diffrn_reflns_av_sigmaI/netI    0.3792
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            88054
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.3163
_exptl_absorpt_correction_T_min  0.2423
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6216
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .4
_refine_diff_density_max         1.513
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1486
_refine_ls_number_reflns         28649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.860
_refine_ls_R_factor_all          0.3013
_refine_ls_R_factor_gt           0.0963
_refine_ls_shift/su_max          1.036
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1110P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2122
_refine_ls_wR_factor_ref         0.2727
_reflns_number_gt                7185
_reflns_number_total             28649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034934asi20031105_013905.cif
_cod_data_source_block           cs236
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        12365(5)
_cod_database_code               4310515