Reactions of LiE(SiMe3)3, E = Si, Ge: X-ray Crystal Structure of the Cyclotetrastannane [ClSnSi(SiMe3)3]4
S. P. Mallela; Yochen Saar; Sven Hill; R. A. Geanangel; Inorganic Chemistry 38 (1999) 2957–2960; doi:10.1021/ic9900455

data_4322088
_publ_section_title
;
 Reactions of LiE(SiMe3)3, E = Si, Ge: X-ray Crystal Structure of the
 Cyclotetrastannane [ClSnSi(SiMe3)3]4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2957
_journal_page_last               2960
_journal_paper_doi               10.1021/ic9900455
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C36 H108 Si16 Cl4 Sn4, 2 C5 H12'
_chemical_formula_sum            'C46 H132 Cl4 Si16 Sn4'
_chemical_formula_weight         1751.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                76.94(1)
_cell_angle_beta                 76.19(1)
_cell_angle_gamma                62.11(1)
_cell_formula_units_Z            2
_cell_length_a                   14.735(2)
_cell_length_b                   14.976(2)
_cell_length_c                   24.066(3)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      7.5
_cell_volume                     4517.5(11)
_computing_cell_refinement       'Bruker Xscans'
_computing_data_collection       'Bruker Xscans'
_computing_data_reduction        'Bruker Xscans'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12402
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        10
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  0.9200
_exptl_absorpt_correction_T_min  0.7412
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         11702
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.233
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+6.9220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                9383
_reflns_number_total             11702
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic9900455.cif
_cod_data_source_block           k391
_cod_original_cell_volume        4517.5(10)
_cod_database_code               4322088