Synthesis and Characterization of the Largest Isolated Clusters of Tin, [Sn12]12-, in (AE)Na10Sn12 (AE = Ca or Sr)
Svilen Bobev; Slavi C. Sevov; Inorganic Chemistry 40 (2001) 5361–5364; doi:10.1021/ic0103953

data_4320349
_publ_contact_author
;
Slavi C. Sevov
Department of Chemistry and Biochemistry
251 Nieuwland Science Hall
University of Notre Dame
Notre Dame, IN 46556-5670
USA
;
_publ_contact_author_email       ssevov@nd.edu
_publ_contact_author_fax         'Intl. Code + (219)631-6652'
_publ_contact_author_phone       'Intl. Code + (219)631-5891'
_publ_section_title
;
 Synthesis and Characterization of the Largest Isolated Clusters of Tin,
 [Sn12]12-, in (AE)Na10Sn12 (AE = Ca or Sr)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5361
_journal_page_last               5364
_journal_paper_doi               10.1021/ic0103953
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         CaNa10Sn12
_chemical_formula_sum            'Ca Na10 Sn12'
_chemical_formula_weight         1694.26
_chemical_melting_point          ?
_chemical_name_common            CaNa10Sn12
_space_group_IT_number           217
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1847(6)
_cell_length_b                   11.1847(6)
_cell_length_c                   11.1847(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.48
_cell_measurement_theta_min      12.69
_cell_volume                     1399.18(13)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        SDS_Package_(Enraf-Nonius,_1985)
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXTL (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Enraf_Nonius_CAD4
_diffrn_measurement_method       omega-2theta
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1168
_diffrn_reflns_theta_full        29.89
_diffrn_reflns_theta_max         29.89
_diffrn_reflns_theta_min         2.58
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.831
_exptl_absorpt_correction_T_max  0.3124
_exptl_absorpt_correction_T_min  0.2459
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'average of 6 psi-scan reflections'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.021
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(11)
_refine_ls_extinction_coef       0.0049(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0136
_refine_ls_R_factor_gt           0.0131
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.065
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0083P)^2^+0.1566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0293
_refine_ls_wR_factor_ref         0.0295
_reflns_number_gt                233
_reflns_number_total             235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0103953_1.cif
_cod_data_source_block           CaNa10Sn12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Cubic' changed to 'cubic' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 
;
_cod_original_cell_volume        1399.2(1)
_cod_database_code               4320349