#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:02:56 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178970 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/99/4119946.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4119946
loop_
_publ_author_name
'Vladimir Ya. Lee'
'Yuki Ito'
'Akira Sekiguchi'
'Heinz Gornitzka'
'Olga A. Gapurenko'
'Vladimir I. Minkin'
'Ruslan M. Minyaev'
_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/[σ²(Fo²)+(0.0096P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 0.185800(3) 1.0000 1.334491(3) 0.02208(5) Uani 1 2 d S
Si1 Si 0.18214(4) 0.83278(3) 0.91779(8) 0.02335(10) Uani 1 1 d .
Si2 Si -0.08594(6) 1.0000 0.82843(12) 0.02214(13) Uani 1 2 d S
Si3 Si 0.45143(6) 1.0000 1.19647(11) 0.02239(13) Uani 1 2 d S
C1 C 0.18253(14) 0.93862(9) 1.0003(3) 0.0197(3) Uani 1 1 d .
C2 C 0.0855(2) 1.0000 0.9353(4) 0.0201(4) Uani 1 2 d S
C3 C 0.2793(2) 1.0000 1.0668(4) 0.0204(4) Uani 1 2 d S
C4 C 0.1845(2) 0.76318(10) 1.1474(4) 0.0395(4) Uani 1 1 d .
H4A H 0.2595 0.7715 1.2841 0.059 Uiso 1 1 calc R
H4B H 0.1830 0.7092 1.0933 0.059 Uiso 1 1 calc R
H4C H 0.1121 0.7723 1.1853 0.059 Uiso 1 1 calc R
C5 C 0.31747(19) 0.81488(12) 0.8374(4) 0.0350(4) Uani 1 1 d .
H5A H 0.3203 0.8554 0.7294 0.053 Uiso 1 1 calc R
H5B H 0.3095 0.7632 0.7653 0.053 Uiso 1 1 calc R
H5C H 0.3935 0.8167 0.9752 0.053 Uiso 1 1 calc R
C6 C 0.04355(18) 0.81270(11) 0.6511(4) 0.0349(4) Uani 1 1 d .
H6A H -0.0313 0.8204 0.6820 0.052 Uiso 1 1 calc R
H6B H 0.0465 0.7585 0.6019 0.052 Uiso 1 1 calc R
H6C H 0.0429 0.8487 0.5296 0.052 Uiso 1 1 calc R
C7 C -0.1546(3) 1.0000 0.5099(5) 0.0377(6) Uani 1 2 d S
H7A H -0.2408 1.0168 0.4568 0.057 Uiso 0.50 1 calc PR
H7B H -0.1504 0.9470 0.4533 0.057 Uiso 0.50 1 calc PR
H7C H -0.1086 1.0363 0.4516 0.057 Uiso 0.50 1 calc PR
C8 C -0.14052(18) 0.91111(11) 0.9382(4) 0.0325(4) Uani 1 1 d .
H8A H -0.1041 0.8639 0.9013 0.049 Uiso 1 1 calc R
H8B H -0.2306 0.9078 0.8657 0.049 Uiso 1 1 calc R
H8C H -0.1154 0.9152 1.1047 0.049 Uiso 1 1 calc R
C9 C 0.50659(17) 0.91025(11) 1.3803(3) 0.0317(4) Uani 1 1 d .
H9A H 0.5294 0.9245 1.5416 0.048 Uiso 1 1 calc R
H9B H 0.5786 0.8885 1.3584 0.048 Uiso 1 1 calc R
H9C H 0.4406 0.8710 1.3366 0.048 Uiso 1 1 calc R
C10 C 0.5189(2) 1.0000 0.9733(5) 0.0346(6) Uani 1 2 d S
H10A H 0.4698 0.9660 0.8460 0.052 Uiso 0.50 1 calc PR
H10B H 0.6038 0.9805 1.0398 0.052 Uiso 0.50 1 calc PR
H10C H 0.5187 1.0536 0.9166 0.052 Uiso 0.50 1 calc PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 Sn1 C3 53.39(8) . .
C2 Sn1 C1 36.97(5) . 2_575
C3 Sn1 C1 36.88(5) . 2_575
C2 Sn1 C1 36.97(5) . .
C3 Sn1 C1 36.88(5) . .
C1 Sn1 C1 53.04(8) 2_575 .
C4 Si1 C5 110.27(10) . .
C4 Si1 C6 109.41(10) . .
C5 Si1 C6 105.20(9) . .
C4 Si1 C1 113.44(8) . .
C5 Si1 C1 108.67(8) . .
C6 Si1 C1 109.53(8) . .
C7 Si2 C2 110.68(12) . .
C7 Si2 C8 109.37(8) . .
C2 Si2 C8 109.90(8) . .
C7 Si2 C8 109.37(8) . 2_575
C2 Si2 C8 109.90(8) . 2_575
C8 Si2 C8 107.57(12) . 2_575
C10 Si3 C3 111.75(12) . .
C10 Si3 C9 108.76(8) . 2_575
C3 Si3 C9 109.28(8) . 2_575
C10 Si3 C9 108.76(8) . .
C3 Si3 C9 109.28(8) . .
C9 Si3 C9 108.97(13) 2_575 .
C3 C1 C2 90.28(13) . .
C3 C1 Si1 132.63(12) . .
C2 C1 Si1 132.89(12) . .
C3 C1 Sn1 71.51(11) . .
C2 C1 Sn1 71.36(11) . .
Si1 C1 Sn1 132.57(8) . .
C1 C2 C1 89.62(18) 2_575 .
C1 C2 Si2 135.17(9) 2_575 .
C1 C2 Si2 135.17(9) . .
C1 C2 Sn1 71.67(11) 2_575 .
C1 C2 Sn1 71.67(11) . .
Si2 C2 Sn1 114.80(11) . .
C1 C3 C1 89.81(18) 2_575 .
C1 C3 Si3 135.05(9) 2_575 .
C1 C3 Si3 135.05(9) . .
C1 C3 Sn1 71.61(11) 2_575 .
C1 C3 Sn1 71.61(11) . .
Si3 C3 Sn1 114.26(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 C2 2.339(2) .
Sn1 C3 2.342(2) .
Sn1 C1 2.3432(16) 2_575
Sn1 C1 2.3432(16) .
Si1 C4 1.866(2) .
Si1 C5 1.8692(19) .
Si1 C6 1.872(2) .
Si1 C1 1.8774(17) .
Si2 C7 1.859(3) .
Si2 C2 1.862(2) .
Si2 C8 1.8780(19) .
Si2 C8 1.8780(19) 2_575
Si3 C10 1.863(3) .
Si3 C3 1.868(2) .
Si3 C9 1.8794(19) 2_575
Si3 C9 1.8794(19) .
C1 C3 1.482(2) .
C1 C2 1.485(2) .
C2 C1 1.485(2) 2_575
C3 C1 1.482(2) 2_575
