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_4320247
_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            'C58 H136 K4 N10 O24 Se10 Sn4'
_chemical_formula_weight         2778.53
_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                 97.548(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.003(2)
_cell_length_b                   18.966(2)
_cell_length_c                   24.392(2)
_cell_measurement_temperature    150(2)
_cell_volume                     10090.8(16)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(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  0.1614
_diffrn_reflns_av_sigmaI/netI    0.1649
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42373
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    4.815
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_F_000             5448
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.029
_refine_ls_goodness_of_fit_obs   1.134
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         15235
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.133
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_obs          0.0843
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+26.7015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1859
_refine_ls_wR_factor_obs         0.1668
_reflns_number_observed          10398
_reflns_number_total             15270
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010242f_2.cif
_cod_data_source_block           Sn4Se10(4-)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+26.7015P] 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^)+(0.0459P)^2^+26.7015P] 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        10091.0(17)
_cod_database_code               4320247