Syntheses, Vibrational Spectra, and Theoretical Studies of the Adamantanoid Sn4Ch104- (Ch = Se, Te) Anions: X-ray Crystal Structures of [18-Crown-6-K]4[Sn4Se10].5en and [18-Crown-6-K]4[Sn4Te10].3en.2THF
Ayaaz M. Pirani; Hélène P. A. Mercier; David A. Dixon; Horst Borrmann; Gary J. Schrobilgen; Inorganic Chemistry 40 (2001) 4823–4829; doi:10.1021/ic010242f

data_4320246
_publ_section_title
;
 Syntheses, Vibrational Spectra, and Theoretical Studies of the
 Adamantanoid Sn4Ch104- (Ch = Se, Te) Anions: X-ray Crystal Structures of
 [18-Crown-6-K]4[Sn4Se10].5en and [18-Crown-6-K]4[Sn4Te10].3en.2THF
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4823
_journal_page_last               4829
_journal_paper_doi               10.1021/ic010242f
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C62 H136 K4 N6 O26 Sn4 Te10'
_chemical_formula_weight         3288.93
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.90(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.420(5)
_cell_length_b                   19.570(4)
_cell_length_c                   24.680(5)
_cell_measurement_temperature    90(2)
_cell_volume                     10750(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59396
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    3.795
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_F_000             6216
_refine_diff_density_max         3.345
_refine_diff_density_min         -2.359
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.487
_refine_ls_goodness_of_fit_obs   1.530
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         16710
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.496
_refine_ls_restrained_S_obs      1.521
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_obs          0.0468
_refine_ls_shift/esd_max         -4.275
_refine_ls_shift/esd_mean        0.109
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1809
_refine_ls_wR_factor_obs         0.1741
_reflns_number_observed          15059
_reflns_number_total             16747
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010242f_1.cif
_cod_data_source_block           Sn4Te10(4-)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10750.2(37)
_cod_database_code               4320246