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_7702390
_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]2[Pb3I10]*DMF*0.5Et2O'
_chemical_formula_sum            'C61 H136 I10 N5 O1.5 Pb3'
_chemical_formula_weight         2854.32
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                72.963(5)
_cell_angle_beta                 70.719(5)
_cell_angle_gamma                74.467(4)
_cell_formula_units_Z            2
_cell_length_a                   15.3391(9)
_cell_length_b                   16.9204(10)
_cell_length_c                   20.6738(14)
_cell_measurement_reflns_used    68
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      '12.5 deg.'
_cell_measurement_theta_min      '10 deg.'
_cell_volume                     4754.8(5)
_computing_cell_refinement       'STOE STADI4 software'
_computing_data_collection       'STOE STADI4 software'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'SCHAKAL92 (Keller, 1992)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'STOE STADI IV'
_diffrn_measurement_method       'theta omega scans (1:1)'
_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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19324
_diffrn_reflns_theta_full        24.02
_diffrn_reflns_theta_max         24.02
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        '+/- 2%'
_diffrn_standards_interval_time  '2 h'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.578
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2650
_refine_diff_density_max         2.907
_refine_diff_density_min         -3.451
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    'idealized positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         14940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+48.1399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1246
_reflns_number_observed          11658
_reflns_number_total             14940
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902640a.txt
_cod_data_source_block           fv313
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'psi scan' was
changed to 'psi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+48.1399P] 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^)+(0.0464P)^2^+48.1399P] 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-1 (No. 2)'
_cod_database_code               7702390