Organometallic Selenolates. IX. (18-Crown-6)-potassium (η^5^-cyclopentadienyl)bis(1,4-tetraselenido-<i>Se</i>^1^,<i>Se</i>^4^)tungstate(IV)
Thöne, Carsten; Jones, Peter G.; Laube, Jörg; Jäger, Stefan; Acta Crystallographica Section C 54 (1998) 1247–1249; doi:10.1107/S0108270198004752

data_2007616
_publ_section_title
;Organometallic Selenolates. IX. (18-Crown-6)-potassium
 (\h^5^-cyclopentadienyl)bis(1,4-tetraselenido-<i>Se</i>^1^,<i>Se</i>^4^)tungstate(IV)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1247
_journal_page_last               1249
_journal_paper_doi               10.1107/S0108270198004752
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '[K (C12 H24 O6)] [W (C5 H5) (Se4)2]'
_chemical_formula_moiety         'C12 H24 K O6 1+ , C5 H5 Se8 W 1-'
_chemical_formula_sum            'C17 H29 K O6 Se8 W'
_chemical_formula_weight         1184.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.78(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.488(5)
_cell_length_b                   10.113(3)
_cell_length_c                   22.223(10)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.5
_cell_volume                     2996(2)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'XP (Siemens, 1994b)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.089
_diffrn_reflns_av_sigmaI/netI    0.1572
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7747
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.744
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.113
_exptl_absorpt_correction_type
'\y scans (XEMP; Siemens, 1994a) assuming lamina 100'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.15
_refine_diff_density_min         -1.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.920
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    'H atoms constrained'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5238
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      0.906
_refine_ls_restrained_S_obs      1.043
_refine_ls_R_factor_all          0.146
_refine_ls_R_factor_obs          .065
_refine_ls_shift/esd_max         <0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0721P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.164
_refine_ls_wR_factor_obs         .135
_reflns_number_observed          2705
_reflns_number_total             5238
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            fg1451.cif
_cod_data_source_block           fg1451
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0721P)^2^] where P = (Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0721P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2007616