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#$Date: 2019-12-13 10:13:05 +0200 (Fri, 13 Dec 2019) $
#$Revision: 245046 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556546.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_1556546
loop_
_publ_author_name
'Kahr, J.'
'Belaj, F.'
'Pietschnig, R.'
_publ_section_title
;
 Preparation and Molecular Structure of a Cyclopentyl-Substituted Cage
 Hexasilsesquioxane T6 (T = cyclopentyl-SiO1.5) Starting from the
 Corresponding Silanetriol
;
_journal_name_full               Inorganics
_journal_page_first              66
_journal_paper_doi               10.3390/inorganics5040066
_journal_volume                  5
_journal_year                    2017
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C10 H22 O5 Si2'
_chemical_formula_sum            'C10 H22 O5 Si2'
_chemical_formula_weight         278.45
_chemical_name_common
' 1,3-di-cyclopentyl-1,1,3,3-tetrahydroxysiloxane'
_chemical_name_systematic
' 1,3-di-cyclopentyl-1,1,3,3-tetrahydroxysiloxane'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1476(5)
_cell_length_b                   20.7484(10)
_cell_length_c                   6.7022(3)
_cell_measurement_reflns_used    5433
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      3.62
_cell_volume                     1411.12(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0264
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6765
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         734
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0342P)²+2.4756P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                683
_reflns_number_total             734
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Inorganics-2017-5-66.cif
_cod_data_source_block           JK22_5B
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_sg_symbol_H-M      'C m c a'
_cod_database_code               1556546
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.908
_shelx_estimated_absorpt_t_max   0.970
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5000 0.5000 0.5000 0.0333(6) Uani 1 4 d S T P . .
Si1 Si 0.5000 0.45273(3) 0.68993(9) 0.0183(2) Uani 1 2 d S T P A .
O2 O 0.62849(12) 0.46760(7) 0.82794(17) 0.0289(4) Uani 1 1 d D . . . .
H2 H 0.7019(3) 0.4694(17) 0.7703(10) 0.046(10) Uiso 0.5 1 d D U P . .
H3 H 0.621(3) 0.4910(3) 0.9296(6) 0.046(10) Uiso 0.5 1 d D U P . .
C1 C 0.5000 0.36904(12) 0.5998(4) 0.0281(6) Uani 1 2 d S T P . .
H1 H 0.5000 0.3397 0.7181 0.059(11) Uiso 1 2 d R . P A .
C2 C 0.611(3) 0.3518(4) 0.464(2) 0.038(2) Uani 0.5 1 d . . P A 1
H21 H 0.6710 0.3213 0.5324 0.061(6) Uiso 0.5 1 calc R U P A 1
H22 H 0.6618 0.3910 0.4302 0.061(6) Uiso 0.5 1 calc R U P A 1
C3 C 0.5600(8) 0.3216(4) 0.2771(11) 0.0553(18) Uani 0.5 1 d . . P A 1
H31 H 0.6162 0.2850 0.2354 0.059(7) Uiso 0.5 1 calc R U P A 1
H32 H 0.5559 0.3534 0.1672 0.059(7) Uiso 0.5 1 calc R U P A 1
C4 C 0.4229(7) 0.2986(3) 0.3342(10) 0.0334(12) Uani 0.5 1 d . . P A 1
H41 H 0.4271 0.2568 0.4051 0.059(7) Uiso 0.5 1 calc R U P A 1
H42 H 0.3665 0.2938 0.2146 0.059(7) Uiso 0.5 1 calc R U P A 1
C5 C 0.369(3) 0.3527(4) 0.474(2) 0.038(2) Uani 0.5 1 d . . P A 1
H51 H 0.2974 0.3368 0.5611 0.061(6) Uiso 0.5 1 calc R U P A 1
H52 H 0.3379 0.3905 0.3975 0.061(6) Uiso 0.5 1 calc R U P A 1
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'
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
Si1 O1 Si1 180.0 . 9_666
O1 Si1 O2 109.54(5) . .
O1 Si1 O2 109.54(5) . 12_655
O2 Si1 O2 106.42(9) . 12_655
O1 Si1 C1 108.43(9) . .
O2 Si1 C1 111.44(7) . .
O2 Si1 C1 111.45(7) 12_655 .
Si1 O2 H2 117.2(7) . .
Si1 O2 H3 119.9(19) . .
H2 O2 H3 115(3) . .
C2 C1 C5 104.7(3) . .
C2 C1 Si1 115.3(4) . .
C5 C1 Si1 111.8(3) . .
C2 C1 H1 109.8 . .
C5 C1 H1 106.7 . .
Si1 C1 H1 108.3 . .
C1 C2 C3 110.6(18) . .
C1 C2 H21 109.5 . .
C3 C2 H21 109.5 . .
C1 C2 H22 109.5 . .
C3 C2 H22 109.5 . .
H21 C2 H22 108.1 . .
C2 C3 C4 103.7(14) . .
C2 C3 H31 111.0 . .
C4 C3 H31 111.0 . .
C2 C3 H32 111.0 . .
C4 C3 H32 111.0 . .
H31 C3 H32 109.0 . .
C3 C4 C5 104.2(12) . .
C3 C4 H41 110.9 . .
C5 C4 H41 110.9 . .
C3 C4 H42 110.9 . .
C5 C4 H42 110.9 . .
H41 C4 H42 108.9 . .
C4 C5 C1 100.2(15) . .
C4 C5 H51 111.7 . .
C1 C5 H51 111.7 . .
C4 C5 H52 111.7 . .
C1 C5 H52 111.7 . .
H51 C5 H52 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 Si1 1.6070(6) .
O1 Si1 1.6070(6) 9_666
Si1 O2 1.6282(12) .
Si1 O2 1.6282(12) 12_655
Si1 C1 1.838(3) .
O2 H2 0.84 .
O2 H3 0.84 .
C1 C2 1.49(3) .
C1 C5 1.61(3) .
C1 H1 1.00 .
C2 C3 1.493(11) .
C2 H21 0.99 .
C2 H22 0.99 .
C3 C4 1.519(6) .
C3 H31 0.99 .
C3 H32 0.99 .
C4 C5 1.562(10) .
C4 H41 0.99 .
C4 H42 0.99 .
C5 H51 0.99 .
C5 H52 0.99 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H3 O2 0.84 1.840(4) 2.670(2) 169(2) 4_567
O2 H2 O2 0.84 1.843(3) 2.678(2) 172.5(19) 7_646
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O1 Si1 C1 C2 56.6(6) . . . .
O2 Si1 C1 C2 -64.0(6) . . . .
O2 Si1 C1 C2 177.2(6) 12_655 . . .
O1 Si1 C1 C5 -62.7(4) . . . .
O2 Si1 C1 C5 176.6(4) . . . .
O2 Si1 C1 C5 57.9(4) 12_655 . . .
C5 C1 C2 C3 -4.9(5) . . . .
Si1 C1 C2 C3 -128.1(5) . . . .
C1 C2 C3 C4 -20.3(7) . . . .
C2 C3 C4 C5 37.9(8) . . . .
C3 C4 C5 C1 -39.8(6) . . . .
C2 C1 C5 C4 27.1(4) . . . .
Si1 C1 C5 C4 152.5(4) . . . .
