Tin-Based Organo-Zintl Ions: Alkylation and Alkenylation of Sn94-
Donald J. Chapman; Slavi C. Sevov; Inorganic Chemistry 47 (2008) 6009–6013; doi:10.1021/ic800383c

data_4305397
_publ_section_title
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Tin-Based Organo-Zintl Ions: Alkylation and Alkenylation of Sn94-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6009
_journal_page_last               6013
_journal_paper_doi               10.1021/ic800383c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C68 H127 K3 N8 O18 Sn9'
_chemical_formula_weight         2530.29
_chemical_name_systematic
; 
 (K-crypt)3[Sn9-C(CH3)3].2py
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.0920(10)
_cell_angle_beta                 78.9520(10)
_cell_angle_gamma                65.1140(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4259(3)
_cell_length_b                   16.2725(4)
_cell_length_c                   22.5593(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4714.48(19)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       'Phi and Omega Scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31433
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    2.534
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'brick like'
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.878
_refine_diff_density_min         -.687
_refine_diff_density_rms         .118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1966
_refine_ls_number_reflns         31433
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+17.9684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                28446
_reflns_number_total             31433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800383c-file002_3.cif
_cod_data_source_block           all
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        4714.48(18)
_cod_database_code               4305397