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_7702391
_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[Pb7I22]'
_chemical_formula_sum            'C112 H248 I22 N8 Pb7'
_chemical_formula_weight         5949.31
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.730(2)
_cell_length_b                   26.823(3)
_cell_length_c                   20.496(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     8847.0(17)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32340
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    10.511
_exptl_absorpt_correction_T_max  0.3208
_exptl_absorpt_correction_T_min  0.2057
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5432
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    'idealized positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         13110
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                9337
_reflns_number_total             13110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902640a.txt
_cod_data_source_block           311neu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] 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^)+(0.0628P)^2^+0.0000P] 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      'P2(1)/n, No. 14'
_cod_database_code               7702391