Pyramidanes: The Covalent Form of the Ionic Compounds
Lee, Vladimir Ya.; Gapurenko, Olga A.; Ito, Yuki; Meguro, Takahiko; Sugasawa, Haruka; Sekiguchi, Akira; Minyaev, Ruslan M.; Minkin, Vladimir I.; Herber, Rolfe H.; Gornitzka, Heinz; Organometallics 35 (2016) 346–; doi:10.1021/acs.organomet.5b00924

data_4088191
_publ_section_title
;
 Pyramidanes: The Covalent Form of the Ionic Compounds
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              346
_journal_paper_doi               10.1021/acs.organomet.5b00924
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C36 H84 Si8 Sn'
_chemical_formula_weight         860.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                68.3480(10)
_cell_angle_beta                 87.9350(10)
_cell_angle_gamma                76.5840(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7913(8)
_cell_length_b                   12.8192(8)
_cell_length_c                   16.8594(11)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.430
_cell_measurement_theta_min      1.301
_cell_volume                     2495.6(3)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (George Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Incoatec ImS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34840
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.430
_diffrn_reflns_theta_min         1.301
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.161
_refine_diff_density_max         2.095
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         10150
_refine_ls_number_restraints     500
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+1.7509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9808
_reflns_number_total             10150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00924_si_003.cif
_cod_data_source_block           SnSi4third_0m
_cod_database_code               4088191
_shelx_estimated_absorpt_t_min   0.850
_shelx_estimated_absorpt_t_max   0.892
_shelxl_version_number           2014-3
_shelx_res_checksum              66127
_shelx_hkl_checksum              45085