Os~3~Sn~15~O~14~, ein ternäres Oxid mit osmiumgefüllten Sn~6~-Oktaedern
Söhnel, T.; Reichelt, W.; Acta Crystallographica Section C 53 (1997) 9–11; doi:10.1107/S0108270196009560

data_2005895
_publ_contact_author
;
W. Reichelt
Institut f\"ur Anorganische Chemie
TU Dresden
01062 Dresden
Mommsenstra\&se 6
Deutschland
;
_publ_section_title
;
 Os~3~Sn~15~O~14~, ein tern\"ares Oxid mit osmiumgef\"ullten
 Sn~6~-Oktaedern
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              9
_journal_page_last               11
_journal_paper_doi               10.1107/S0108270196009560
_journal_volume                  53
_journal_year                    1997
_chemical_formula_analytical     'Os Sn5 O4'
_chemical_formula_moiety         'Os3 Sn15 O14'
_chemical_formula_structural     'Os3 Sn15 O14'
_chemical_formula_sum            'O14 Os3 Sn15'
_chemical_formula_weight         2574.95
_chemical_name_systematic        Osmiumstannat
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.49(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.399(1)
_cell_length_b                   7.090(1)
_cell_length_c                   12.939(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.4
_cell_measurement_theta_min      7.9
_cell_volume                     1078.7(2)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4PC (Enraf Nonius, 1994)'
_computing_molecular_graphics    'ATOMS (Dowty, 1994)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD-4
_diffrn_measurement_method       \w-2\q
_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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7133
_diffrn_reflns_theta_max         39.97
_diffrn_reflns_theta_min         3.32
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 800
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    34.653
_exptl_absorpt_correction_T_max  0.12
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_type   'empirical,\DF (XEMP; Siemens, 1989)'
_exptl_crystal_colour            Rot
_exptl_crystal_density_diffrn    7.927
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Isometric
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         '6.161 (nahe Os3)'
_refine_diff_density_min         -6.305
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.034(8)
_refine_ls_extinction_coef       0.00036(5)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3650
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_obs          0.0344
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0570P)^2^+10.7521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0893
_refine_ls_wR_factor_obs         0.0871
_reflns_number_observed          3323
_reflns_number_total             3650
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1025.cif
_cod_data_source_block           default
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (18
times).

'_geom_bond_publ_flag' value 'No' changed to 'no' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (62
times).

'_geom_angle_publ_flag' value 'No' changed to 'no' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (173 times).

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0570P)^2^+10.7521P] 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^)+(0.0570P)^2^+10.7521P] 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      'C m'
_cod_database_code               2005895