#------------------------------------------------------------------------------
#$Date: 2019-11-24 08:45:28 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237353 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/81/4088190.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_4088190
loop_
_publ_author_name
'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'
_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            'C16 H36 Ge Si4'
_chemical_formula_weight         413.40
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6135(6)
_cell_length_b                   17.5625(9)
_cell_length_c                   11.4704(6)
_cell_measurement_reflns_used    9116
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.32
_cell_volume                     2339.5(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11688
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    1.509
_exptl_absorpt_correction_T_max  0.7824
_exptl_absorpt_correction_T_min  0.5386
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0242
_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/[σ²(Fo²)+(0.0450P)²+0.5985P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                2357
_reflns_number_total             2487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00924_si_001.cif
_cod_data_source_block           gec4_0ma
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'Pnma '
_cod_database_code               4088190
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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
C1 C 0.29112(15) 0.7500 0.36125(15) 0.0170(3) Uani 1 2 d S
C2 C 0.25793(11) 0.69009(7) 0.44604(10) 0.0171(2) Uani 1 1 d .
C3 C 0.22339(15) 0.7500 0.53119(16) 0.0175(3) Uani 1 2 d S
C4 C 0.25847(18) 0.66544(10) 0.13040(14) 0.0436(4) Uani 1 1 d .
H4A H 0.1757 0.6649 0.1469 0.065 Uiso 1 1 calc R
H4B H 0.2937 0.6188 0.1609 0.065 Uiso 1 1 calc R
H4C H 0.2706 0.6682 0.0460 0.065 Uiso 1 1 calc R
C5 C 0.4833(2) 0.7500 0.1761(2) 0.0494(7) Uani 1 2 d S
H5A H 0.4989 0.7375 0.0944 0.074 Uiso 0.50 1 calc PR
H5B H 0.5197 0.7120 0.2267 0.074 Uiso 0.50 1 calc PR
H5C H 0.5146 0.8005 0.1939 0.074 Uiso 0.50 1 calc PR
C6 C 0.39375(14) 0.54990(10) 0.36492(16) 0.0354(4) Uani 1 1 d .
H6A H 0.3822 0.5636 0.2829 0.053 Uiso 1 1 calc R
H6B H 0.4002 0.4945 0.3720 0.053 Uiso 1 1 calc R
H6C H 0.4645 0.5738 0.3937 0.053 Uiso 1 1 calc R
C7 C 0.13322(14) 0.53794(9) 0.40005(15) 0.0344(3) Uani 1 1 d .
H7A H 0.0679 0.5559 0.4467 0.052 Uiso 1 1 calc R
H7B H 0.1401 0.4825 0.4077 0.052 Uiso 1 1 calc R
H7C H 0.1207 0.5512 0.3180 0.052 Uiso 1 1 calc R
C8 C 0.29831(16) 0.55505(9) 0.60686(13) 0.0351(3) Uani 1 1 d .
H8A H 0.3707 0.5782 0.6328 0.053 Uiso 1 1 calc R
H8B H 0.3046 0.4995 0.6112 0.053 Uiso 1 1 calc R
H8C H 0.2353 0.5723 0.6572 0.053 Uiso 1 1 calc R
C9 C 0.03304(14) 0.66554(9) 0.66275(15) 0.0354(4) Uani 1 1 d .
H9A H 0.0790 0.6188 0.6658 0.053 Uiso 1 1 calc R
H9B H -0.0128 0.6660 0.5910 0.053 Uiso 1 1 calc R
H9C H -0.0184 0.6675 0.7304 0.053 Uiso 1 1 calc R
C10 C 0.2156(2) 0.7500 0.80270(19) 0.0527(8) Uani 1 2 d S
H10A H 0.1649 0.7626 0.8682 0.079 Uiso 0.50 1 calc PR
H10B H 0.2773 0.7879 0.7974 0.079 Uiso 0.50 1 calc PR
H10C H 0.2492 0.6995 0.8150 0.079 Uiso 0.50 1 calc PR
Ge1 Ge 0.405553(16) 0.7500 0.507834(17) 0.02049(9) Uani 1 2 d S
Si1 Si 0.32574(4) 0.7500 0.20158(4) 0.01944(13) Uani 1 2 d S
Si2 Si 0.26836(3) 0.58407(2) 0.45296(3) 0.02163(11) Uani 1 1 d .
Si3 Si 0.13083(5) 0.7500 0.66480(4) 0.02145(13) Uani 1 2 d S
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'
Ge Ge 0.1547 1.8001 '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 C1 C2 90.33(14) 7_575 .
C2 C1 Si1 134.10(7) 7_575 .
C2 C1 Si1 134.10(7) . .
C2 C1 Ge1 69.32(8) 7_575 .
C2 C1 Ge1 69.32(8) . .
Si1 C1 Ge1 129.30(9) . .
C1 C2 C3 89.93(10) . .
C1 C2 Si2 135.89(9) . .
C3 C2 Si2 133.90(9) . .
C1 C2 Ge1 70.07(8) . .
C3 C2 Ge1 69.53(8) . .
Si2 C2 Ge1 115.19(6) . .
C2 C3 C2 89.81(14) 7_575 .
C2 C3 Si3 133.71(7) 7_575 .
C2 C3 Si3 133.70(7) . .
C2 C3 Ge1 69.56(8) 7_575 .
C2 C3 Ge1 69.56(8) . .
Si3 C3 Ge1 132.26(10) . .
Si1 C4 H4A 109.5 . .
Si1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Si1 C5 H5A 109.5 . .
Si1 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si1 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
Si2 C6 H6A 109.5 . .
Si2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Si2 C7 H7A 109.5 . .
Si2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Si2 C8 H8A 109.5 . .
Si2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
Si3 C9 H9A 109.5 . .
Si3 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
Si3 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
Si3 C10 H10A 109.5 . .
Si3 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
Si3 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C2 Ge1 C2 59.12(7) 7_575 .
C2 Ge1 C3 40.91(5) 7_575 .
C2 Ge1 C3 40.91(5) . .
C2 Ge1 C1 40.61(4) 7_575 .
C2 Ge1 C1 40.61(4) . .
C3 Ge1 C1 58.89(7) . .
C5 Si1 C4 110.16(8) . .
C5 Si1 C4 110.16(8) . 7_575
C4 Si1 C4 105.46(12) . 7_575
C5 Si1 C1 111.44(10) . .
C4 Si1 C1 109.73(6) . .
C4 Si1 C1 109.73(6) 7_575 .
C8 Si2 C7 110.17(8) . .
C8 Si2 C6 106.10(8) . .
C7 Si2 C6 109.85(8) . .
C8 Si2 C2 108.90(6) . .
C7 Si2 C2 111.36(7) . .
C6 Si2 C2 110.33(7) . .
C10 Si3 C9 109.38(7) . .
C10 Si3 C9 109.38(7) . 7_575
C9 Si3 C9 105.11(10) . 7_575
C10 Si3 C3 113.06(10) . .
C9 Si3 C3 109.80(6) . .
C9 Si3 C3 109.80(6) 7_575 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.4838(17) 7_575
C1 C2 1.4839(17) .
C1 Si1 1.8751(18) .
C1 Ge1 2.1432(17) .
C2 C3 1.4906(17) .
C2 Si2 1.8675(13) .
C2 Ge1 2.1328(13) .
C3 C2 1.4906(17) 7_575
C3 Si3 1.8720(19) .
C3 Ge1 2.1325(18) .
C4 Si1 1.8661(16) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 Si1 1.853(3) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 Si2 1.8709(16) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 Si2 1.8676(16) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 Si2 1.8700(15) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 Si3 1.8683(16) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 Si3 1.863(2) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
Ge1 C2 2.1328(13) 7_575
Si1 C4 1.8661(16) 7_575
Si3 C9 1.8683(16) 7_575
