#------------------------------------------------------------------------------
#$Date: 2019-11-10 19:17:10 +0200 (Sun, 10 Nov 2019) $
#$Revision: 226019 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/59/4515955.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_4515955
loop_
_publ_author_name
'Aghazadeh Meshgi, Mohammad'
'Zaitsev, Kirill V.'
'Vener, Mikhail V.'
'Churakov, Andrei V.'
'Baumgartner, Judith'
'Marschner, Christoph'
_publ_section_title
;
 Hypercoordinated Oligosilanes Based on Aminotrisphenols.
;
_journal_issue                   8
_journal_name_full               'ACS omega'
_journal_page_first              10317
_journal_page_last               10330
_journal_paper_doi               10.1021/acsomega.8b01402
_journal_volume                  3
_journal_year                    2018
_chemical_formula_sum            'C36 H57 N O3 Si5'
_chemical_formula_weight         692.28
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3 c 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            4
_cell_length_a                   14.3849(18)
_cell_length_b                   14.3849(18)
_cell_length_c                   22.169(4)
_cell_measurement_reflns_used    14110
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.504
_cell_measurement_theta_min      4.902
_cell_volume                     3972.7(10)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART APEX''
_diffrn_measurement_method       'ω 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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29652
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.9586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0599
_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)+(0.0292P)²+9.0313P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                2636
_reflns_number_total             2696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao8b01402_si_002.cif
_cod_data_source_block           1174j
_cod_original_cell_volume        3972.8(10)
_cod_original_sg_symbol_H-M      P-3c1
_cod_database_code               4515955
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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
Si1 Si 0.6667 0.3333 0.49637(5) 0.0147(3) Uani 1 3 d S
Si2 Si 0.6667 0.3333 0.38915(5) 0.0165(3) Uani 1 3 d S
Si3 Si 0.61136(7) 0.45759(7) 0.35980(3) 0.0225(2) Uani 1 1 d .
N1 N 0.6667 0.3333 0.59725(17) 0.0167(8) Uani 1 3 d S
O1 O 0.75092(15) 0.46488(15) 0.50314(8) 0.0185(4) Uani 1 1 d .
C1 C 0.7859(2) 0.5468(2) 0.54441(12) 0.0173(5) Uani 1 1 d .
C2 C 0.7435(2) 0.5307(2) 0.60225(12) 0.0186(6) Uani 1 1 d .
C3 C 0.7853(2) 0.6162(2) 0.64240(13) 0.0218(6) Uani 1 1 d .
H3 H 0.7571 0.6050 0.6822 0.026 Uiso 1 1 calc R
C4 C 0.8670(2) 0.7175(2) 0.62628(13) 0.0260(6) Uani 1 1 d .
C5 C 0.9110(3) 0.8090(3) 0.67109(15) 0.0411(8) Uani 1 1 d .
H5A H 0.8586 0.8327 0.6772 0.062 Uiso 1 1 calc R
H5B H 0.9780 0.8689 0.6555 0.062 Uiso 1 1 calc R
H5C H 0.9250 0.7848 0.7096 0.062 Uiso 1 1 calc R
C6 C 0.9062(2) 0.7316(2) 0.56757(13) 0.0241(6) Uani 1 1 d .
H6 H 0.9616 0.8007 0.5556 0.029 Uiso 1 1 calc R
C7 C 0.8675(2) 0.6482(2) 0.52580(13) 0.0205(6) Uani 1 1 d .
C8 C 0.9119(2) 0.6658(2) 0.46300(13) 0.0260(6) Uani 1 1 d .
H8A H 0.9603 0.6365 0.4596 0.039 Uiso 1 1 calc R
H8B H 0.9516 0.7429 0.4542 0.039 Uiso 1 1 calc R
H8C H 0.8528 0.6295 0.4342 0.039 Uiso 1 1 calc R
C9 C 0.7703(2) 0.3472(2) 0.62004(12) 0.0194(6) Uani 1 1 d .
H9A H 0.7716 0.3527 0.6646 0.023 Uiso 1 1 calc R
H9B H 0.8300 0.4152 0.6040 0.023 Uiso 1 1 calc R
C10 C 0.4786(3) 0.3954(3) 0.32002(14) 0.0344(8) Uani 1 1 d .
H10A H 0.4229 0.3413 0.3462 0.052 Uiso 1 1 calc R
H10B H 0.4828 0.3613 0.2826 0.052 Uiso 1 1 calc R
H10C H 0.4607 0.4511 0.3104 0.052 Uiso 1 1 calc R
C11 C 0.5968(3) 0.5266(2) 0.42816(14) 0.0285(7) Uani 1 1 d .
H11A H 0.5694 0.5739 0.4159 0.043 Uiso 1 1 calc R
H11B H 0.6669 0.5692 0.4476 0.043 Uiso 1 1 calc R
H11C H 0.5465 0.4727 0.4566 0.043 Uiso 1 1 calc R
C12 C 0.7059(3) 0.5680(3) 0.30774(18) 0.0475(10) Uani 1 1 d .
H12A H 0.7128 0.5367 0.2699 0.071 Uiso 1 1 calc R
H12B H 0.7765 0.6087 0.3269 0.071 Uiso 1 1 calc R
H12C H 0.6776 0.6161 0.2993 0.071 Uiso 1 1 calc R
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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
O1 Si1 O1 119.20(2) 2_655 3_665
O1 Si1 O1 119.20(2) 2_655 .
O1 Si1 O1 119.20(2) 3_665 .
O1 Si1 N1 84.83(7) 2_655 .
O1 Si1 N1 84.83(7) 3_665 .
O1 Si1 N1 84.83(7) . .
O1 Si1 Si2 95.17(7) 2_655 .
O1 Si1 Si2 95.17(7) 3_665 .
O1 Si1 Si2 95.17(7) . .
N1 Si1 Si2 180.000(1) . .
Si1 Si2 Si3 105.85(3) . 2_655
Si1 Si2 Si3 105.85(3) . 3_665
Si3 Si2 Si3 112.84(3) 2_655 3_665
Si1 Si2 Si3 105.85(3) . .
Si3 Si2 Si3 112.83(3) 2_655 .
Si3 Si2 Si3 112.83(3) 3_665 .
C10 Si3 C11 105.97(15) . .
C10 Si3 C12 104.34(17) . .
C11 Si3 C12 105.83(18) . .
C10 Si3 Si2 114.41(11) . .
C11 Si3 Si2 110.08(10) . .
C12 Si3 Si2 115.43(12) . .
C9 N1 C9 109.11(17) 3_665 .
C9 N1 C9 109.11(17) 3_665 2_655
C9 N1 C9 109.11(17) . 2_655
C9 N1 Si1 109.83(17) 3_665 .
C9 N1 Si1 109.83(17) . .
C9 N1 Si1 109.83(17) 2_655 .
C1 O1 Si1 141.32(18) . .
O1 C1 C2 122.0(2) . .
O1 C1 C7 117.0(2) . .
C2 C1 C7 121.0(2) . .
C3 C2 C1 119.0(3) . .
C3 C2 C9 121.1(2) . 2_655
C1 C2 C9 119.9(2) . 2_655
C4 C3 C2 122.0(3) . .
C3 C4 C6 117.6(3) . .
C3 C4 C5 120.8(3) . .
C6 C4 C5 121.6(3) . .
C7 C6 C4 122.5(3) . .
C6 C7 C1 117.8(3) . .
C6 C7 C8 121.3(3) . .
C1 C7 C8 120.9(2) . .
N1 C9 C2 112.5(2) . 3_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O1 1.6669(18) 2_655
Si1 O1 1.6669(18) 3_665
Si1 O1 1.6669(18) .
Si1 N1 2.237(4) .
Si1 Si2 2.3770(17) .
Si2 Si3 2.3818(9) 2_655
Si2 Si3 2.3818(9) 3_665
Si2 Si3 2.3818(9) .
Si3 C10 1.875(3) .
Si3 C11 1.880(3) .
Si3 C12 1.882(4) .
N1 C9 1.489(3) 3_665
N1 C9 1.489(3) .
N1 C9 1.489(3) 2_655
O1 C1 1.374(3) .
C1 C2 1.389(4) .
C1 C7 1.401(4) .
C2 C3 1.388(4) .
C2 C9 1.496(4) 2_655
C3 C4 1.385(4) .
C4 C6 1.393(4) .
C4 C5 1.513(4) .
C6 C7 1.392(4) .
C7 C8 1.499(4) .
C9 C2 1.496(4) 3_665
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 Si1 Si2 Si3 -56.71(7) 2_655 2_655
O1 Si1 Si2 Si3 63.29(7) 3_665 2_655
O1 Si1 Si2 Si3 -176.71(7) . 2_655
N1 Si1 Si2 Si3 -171(87) . 2_655
O1 Si1 Si2 Si3 -176.71(7) 2_655 3_665
O1 Si1 Si2 Si3 -56.71(7) 3_665 3_665
O1 Si1 Si2 Si3 63.29(7) . 3_665
N1 Si1 Si2 Si3 69(58) . 3_665
O1 Si1 Si2 Si3 63.29(7) 2_655 .
O1 Si1 Si2 Si3 -176.71(7) 3_665 .
O1 Si1 Si2 Si3 -56.71(7) . .
N1 Si1 Si2 Si3 -51(47) . .
Si1 Si2 Si3 C10 -114.08(12) . .
Si3 Si2 Si3 C10 1.24(14) 2_655 .
Si3 Si2 Si3 C10 130.60(12) 3_665 .
Si1 Si2 Si3 C11 5.10(11) . .
Si3 Si2 Si3 C11 120.42(12) 2_655 .
Si3 Si2 Si3 C11 -110.21(12) 3_665 .
Si1 Si2 Si3 C12 124.80(16) . .
Si3 Si2 Si3 C12 -119.88(16) 2_655 .
Si3 Si2 Si3 C12 9.48(17) 3_665 .
O1 Si1 N1 C9 46.31(13) 2_655 3_665
O1 Si1 N1 C9 -73.69(13) 3_665 3_665
O1 Si1 N1 C9 166.31(13) . 3_665
Si2 Si1 N1 C9 160(100) . 3_665
O1 Si1 N1 C9 166.31(13) 2_655 .
O1 Si1 N1 C9 46.31(13) 3_665 .
O1 Si1 N1 C9 -73.69(13) . .
Si2 Si1 N1 C9 -80(56) . .
O1 Si1 N1 C9 -73.69(13) 2_655 2_655
O1 Si1 N1 C9 166.31(13) 3_665 2_655
O1 Si1 N1 C9 46.31(13) . 2_655
Si2 Si1 N1 C9 40(49) . 2_655
O1 Si1 O1 C1 64.3(3) 2_655 .
O1 Si1 O1 C1 -98.0(3) 3_665 .
N1 Si1 O1 C1 -16.9(3) . .
Si2 Si1 O1 C1 163.1(3) . .
Si1 O1 C1 C2 -2.8(4) . .
Si1 O1 C1 C7 176.6(2) . .
O1 C1 C2 C3 177.6(2) . .
C7 C1 C2 C3 -1.8(4) . .
O1 C1 C2 C9 -3.5(4) . 2_655
C7 C1 C2 C9 177.1(2) . 2_655
C1 C2 C3 C4 1.0(4) . .
C9 C2 C3 C4 -177.9(3) 2_655 .
C2 C3 C4 C6 0.4(4) . .
C2 C3 C4 C5 -179.9(3) . .
C3 C4 C6 C7 -0.9(4) . .
C5 C4 C6 C7 179.4(3) . .
C4 C6 C7 C1 0.0(4) . .
C4 C6 C7 C8 -179.7(3) . .
O1 C1 C7 C6 -178.1(2) . .
C2 C1 C7 C6 1.3(4) . .
O1 C1 C7 C8 1.6(4) . .
C2 C1 C7 C8 -179.0(3) . .
C9 N1 C9 C2 57.4(4) 3_665 3_665
C9 N1 C9 C2 176.48(19) 2_655 3_665
Si1 N1 C9 C2 -63.1(2) . 3_665
