Tetrakis[(9-oxo-10-thiaxanthen-2-yloxyethyl)ammonium] decaiodotriplumbate(II)
Karen R. Maxcy; Roger D. Willett; David B. Mitzi; Ali Afzali; Acta Crystallographica Section E 59 (2003) m364–m366; doi:10.1107/S1600536803007414

data_2201746
_publ_section_title
;
 Tetrakis[(9-oxo-10-thiaxanthen-2-yloxyethyl)ammonium]
 decaiodotriplumbate(II)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m364
_journal_page_last               m366
_journal_paper_doi               10.1107/S1600536803007414
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C15 H14 N1 O2 S1)4 [Pb3 I10]'
_chemical_formula_moiety         '4C15 H14 N1 O2 S1 1+, Pb3 I10 4-'
_chemical_formula_sum            'C60 H56 I10 N4 O8 Pb3 S4'
_chemical_formula_weight         2979.90
_chemical_name_common            AETO4Pb3I10
_chemical_name_systematic
;
Tetrakis[(9-oxo-10-thiaxanthen-2-yloxyethyl)ammonium]
decaiodidotriplumbate(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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-97
_cell_angle_alpha                71.72(3)
_cell_angle_beta                 89.45(3)
_cell_angle_gamma                82.09(3)
_cell_formula_units_Z            1
_cell_length_a                   9.793(2)
_cell_length_b                   11.704(2)
_cell_length_c                   18.061(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.66
_cell_measurement_theta_min      1.85
_cell_volume                     1945.7(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'XCIF in SHELXTL'
_computing_structure_refinement  'XL in SHELXTL'
_computing_structure_solution    'XS in SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18436
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        3.8
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.597
_exptl_absorpt_correction_T_max  0.428
_exptl_absorpt_correction_T_min  0.249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.927
_refine_diff_density_min         -1.729
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6618
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0469P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                5205
_reflns_number_total             6618
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ac6035.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2201746
_cod_database_fobs_code          2201746