Tiara-like Octanuclear Palladium(II) and Platinum(II) Thiolates and Their Inclusion Complexes with Dihalo- or Iodoalkanes.
Yamashina, Yukari; Kataoka, Yasutaka; Ura, Yasuyuki; Inorganic chemistry 53 (2014) 3558–; doi:10.1021/ic403050c

data_4337872
_publ_section_title
;
 Tiara-like Octanuclear Palladium(II) and Platinum(II) Thiolates and Their
 Inclusion Complexes with Dihalo- or Iodoalkanes.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3558
_journal_paper_doi               10.1021/ic403050c
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C48 H80 O32 Pd8 S16, C H2 Br2'
_chemical_formula_sum            'C49 H82 Br2 O32 Pd8 S16'
_chemical_formula_weight         2707.12
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   44.4317(16)
_cell_length_b                   57.845(2)
_cell_length_c                   13.4171(5)
_cell_measurement_reflns_used    93800
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.701
_cell_volume                     34484(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'ChemBio3D Ultra 11.0.1'
_computing_publication_material  'ChemBio3D Ultra 11.0.1'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       75
_diffrn_reflns_limit_k_min       -75
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            93800
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.701
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    3.018
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             21216
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.620
_refine_diff_density_min         -1.933
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         19310
_refine_ls_number_restraints     969
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+275.4070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1670
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                16317
_reflns_number_total             19310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic403050c_si_002.cif
_cod_data_source_block           complex1-CH2Br2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4337867--4337876.cif.
;
_cod_database_code               4337872
_shelx_estimated_absorpt_t_min   0.584
_shelx_estimated_absorpt_t_max   0.915
_shelxl_version_number           2013-4
_shelx_res_checksum              67807