Discrete and polymeric iodoplumbates with Pb3I10 building blocks: [Pb3I10]4−, [Pb7I22]8−, [Pb10I28]8−, 1\ιnfty [Pb3I10]4− and 2∞[Pb7I18]4−
Krautscheid, Harald; Vielsack, Frieder; Journal of the Chemical Society, Dalton Transactions  (1999) 2731–; doi:10.1039/a902640a

data_7702392
_publ_section_title
;
 Discrete and polymeric iodoplumbates with Pb3I10 building blocks:
 [Pb3I10]4&#x2212;, [Pb7I22]8&#x2212;, [Pb10I28]8&#x2212;, 1\\infty
 [Pb3I10]4&#x2212; and 2\\infty [Pb7I18]4&#x2212;
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2731
_journal_paper_doi               10.1039/a902640a
_journal_year                    1999
_chemical_formula_moiety         '[Bu3N-(CH2)4-NBu3]4[Pb10I28]'
_chemical_formula_sum            'C112 H248 I28 N8 Pb10'
_chemical_formula_weight         7332.28
_space_group_IT_number           112
_space_group_name_Hall           'P -4 2c'
_space_group_name_H-M_alt        'P -4 2 c'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P -4 2 c'
_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                   22.9116(9)
_cell_length_b                   22.9116(9)
_cell_length_c                   18.5203(7)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     9722.1(7)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software, X-RED'
_computing_molecular_graphics    'SCHAKAL92 (Keller, 1992)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measurement_device       'STOE IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39676
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    13.105
_exptl_absorpt_correction_T_max  0.2737
_exptl_absorpt_correction_T_min  0.1723
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.505
_exptl_crystal_description       'flat octahedron'
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.042
_refine_ls_hydrogen_treatment    'idelized positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         8532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_restrained_S_obs      1.042
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_obs          0.0278
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0302P)^2^+22.3512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0630
_refine_ls_wR_factor_obs         0.0605
_reflns_number_observed          7772
_reflns_number_total             8541
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902640a.txt
_cod_data_source_block           fv314y
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[s^2^(Fo^2^)+( 0.0302P)^2^+22.3512P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. A new data item '_refine_ls_weighting_details'
was created with the value set to 'w=1/[s^2^(Fo^2^)+(
0.0302P)^2^+22.3512P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P-42c, No. 112'
_cod_database_code               7702392