Syntheses and Structural Characterization of the Heavier Alkali-Metal Stannates Bearing the Tripodal Triamino Framework: Structural Trends in the Series of [MeSi{SiMe2N(4-CH3C6H4)}3Sn][M] (M = Na, K, Rb)
Matthias Lutz; Matti Haukka; Tapani A. Pakkanen; Lutz H. Gade; Inorganic Chemistry 42 (2003) 2798–2804; doi:10.1021/ic026226f

data_4313511
_publ_contact_author_address
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Laboratoire de Chimie Organom\'etallique et de Catalyse, UMR 7513, 
Institut Le Bel, Universit\'e Louis Pasteur, 
4, rue Blaise Pascal, 67070 Strasbourg, France. 
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_publ_contact_author_email       gade@chimie.u-strasbg.fr
_publ_contact_author_fax         0033-390-241531
_publ_contact_author_phone       0033-390-241530
_publ_section_title
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 Syntheses and Structural Characterization of the Heavier Alkali-Metal
 Stannates Bearing the Tripodal Triamino Framework: Structural Trends in
 the Series of [MeSi{SiMe2N(4-CH3C6H4)}3Sn][M] (M = Na, K, Rb)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2798
_journal_page_last               2804
_journal_paper_doi               10.1021/ic026226f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C31 H41 D4 N3 Rb Si4 Sn'
_chemical_formula_weight         780.24
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.4510(3)
_cell_length_b                   13.30710(10)
_cell_length_c                   21.7466(2)
_cell_measurement_temperature    150(2)
_cell_volume                     7365.12(12)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997-2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            103665
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.161
_exptl_absorpt_correction_T_max  0.27184
_exptl_absorpt_correction_T_min  0.23478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.12 (Bruker AXS, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0138P)^2^+8.7037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                6089
_reflns_number_total             7516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026226fsi20021202_082333_1.cif
_cod_data_source_block           st882
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_database_code               4313511