Pyramidanes
Vladimir Ya. Lee; Yuki Ito; Akira Sekiguchi; Heinz Gornitzka; Olga A. Gapurenko; Vladimir I. Minkin; Ruslan M. Minyaev; Journal of the American Chemical Society 135 (2013) 8794–8797; doi:10.1021/ja403173e

data_4119946
_publ_section_title
;
 Pyramidanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8794
_journal_page_last               8797
_journal_paper_doi               10.1021/ja403173e
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C16 H36 Si4 Sn'
_chemical_formula_weight         459.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.742(2)
_cell_length_b                   17.046(3)
_cell_length_c                   6.3160(13)
_cell_measurement_reflns_used    6202
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.39
_cell_volume                     1167.9(5)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6104
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.532
_exptl_crystal_size_mid          0.438
_exptl_crystal_size_min          0.358
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.035(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2422
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0131
_refine_ls_R_factor_gt           0.0131
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0096P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0330
_refine_ls_wR_factor_ref         0.0330
_reflns_number_gt                2422
_reflns_number_total             2422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja403173e_si_003.cif
_cod_data_source_block           snc4_0m
_cod_original_cell_volume        1167.9(4)
_cod_database_code               4119946