An octanuclear pyromellitimidato(2−) palladium complex: coordinative assembly of a molecular box
Colquhoun, Howard M.; Fairman, Richard A.; Tootell, Paula; Williams, David J.; Journal of the Chemical Society, Dalton Transactions  (1999) 2651–; doi:10.1039/a904857j

data_7027611
_publ_section_title
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 An octanuclear pyromellitimidato(2&#x2212;) palladium complex:
 coordinative assembly of a molecular box
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_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2651
_journal_paper_doi               10.1039/a904857j
_journal_year                    1999
_chemical_formula_sum            'C148 H192 Cl8 N16 O24 Pd8'
_chemical_formula_weight         3713.98
_chemical_name_systematic
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 ? 
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_space_group_IT_number           126
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.0685(8)
_cell_length_b                   22.0685(8)
_cell_length_c                   17.4908(15)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      6.45
_cell_volume                     8518.3(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4/RA'
_diffrn_measurement_method       '\w 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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6174
_diffrn_reflns_theta_max         59.97
_diffrn_reflns_theta_min         2.83
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.335
_exptl_absorpt_correction_T_max  0.2820
_exptl_absorpt_correction_T_min  0.1541
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       prisms
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.000054(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.032
_refine_ls_goodness_of_fit_obs   1.131
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         2866
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.131
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_obs          0.0501
_refine_ls_shift/esd_max         0.060
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1277
_refine_ls_wR_factor_obs         0.1080
_reflns_number_observed          2107
_reflns_number_total             3175
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904857jsup1.cif
_cod_data_source_block           hmc9813
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      P4/nnc
_cod_database_code               7027611