#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/10/81/4108145.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_4108145
loop_
_publ_author_name
'Hongzhi Liu'
'Shin-ichi Kondo'
'Nobuhiro Takeda'
'Masafumi Unno'
_publ_section_title
;
 Synthesis of Octacarboxy Spherosilicate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10074
_journal_page_last               10075
_journal_paper_doi               10.1021/ja803513n
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C18 H22 O5 Si2 '
_chemical_formula_sum            'C18 H22 O5 Si2'
_chemical_formula_weight         374.54
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.1024(19)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   27.5603(18)
_cell_length_b                   9.3418(5)
_cell_length_c                   15.5154(10)
_cell_measurement_reflns_used    12120
_cell_measurement_temperature    153.1
_cell_measurement_theta_max      32.6
_cell_measurement_theta_min      1.5
_cell_volume                     3890.6(4)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.783
_diffrn_measured_fraction_theta_max 0.783
_diffrn_measurement_device_type  'Rigaku RAXIS-UNKNOWN'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14351
_diffrn_reflns_theta_full        32.17
_diffrn_reflns_theta_max         32.17
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.10
_refine_diff_density_min         -1.53
_refine_ls_extinction_coef       97(2)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   3.496
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     249
_refine_ls_number_reflns         10937
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/σ²(Fo²)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                10937
_reflns_number_total             5361
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja803513n-file004.cif
_cod_data_source_block           '__Q8COOH'
_cod_original_formula_sum        'C18 H22 O5 Si2 '
_cod_database_code               4108145
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-Y,1/2+Z
5 1/2+X,1/2+Y,+Z
6 1/2-X,1/2+Y,1/2-Z
7 1/2-X,1/2-Y,-Z
8 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_symmetry_multiplicity
_atom_site_calc_flag
Si(1) Si 0.11333(2) 0.16167(5) 0.27584(4) 0.02195(15) Uani 1.00 1 d
Si(2) Si 0.13817(2) 0.22495(6) 0.48033(4) 0.02246(15) Uani 1.00 1 d
O(1) O 0.12678(5) 0.14869(13) 0.38263(9) 0.0279(4) Uani 1.00 1 d
O(6) O 0.31260(5) 0.28517(14) 0.09035(10) 0.0315(4) Uani 1.00 1 d
O(7) O 0.35013(5) 0.14858(13) 0.20464(10) 0.0312(4) Uani 1.00 1 d
O(8) O -0.09975(5) 0.21523(15) 0.54708(10) 0.0367(4) Uani 1.00 1 d
O(9) O -0.06300(5) 0.35273(13) 0.65945(10) 0.0326(4) Uani 1.00 1 d
C(1) C 0.17340(7) 0.17775(16) 0.23932(13) 0.0170(5) Uani 1.00 1 d
C(2) C 0.21666(7) 0.1100(2) 0.28729(14) 0.0276(5) Uani 1.00 1 d
C(3) C 0.26152(7) 0.11930(18) 0.26149(14) 0.0235(5) Uani 1.00 1 d
C(4) C 0.26427(7) 0.19838(18) 0.18655(14) 0.0215(5) Uani 1.00 1 d
C(5) C 0.22215(7) 0.26412(18) 0.13769(14) 0.0237(5) Uani 1.00 1 d
C(6) C 0.17751(7) 0.25420(18) 0.16406(14) 0.0253(5) Uani 1.00 1 d
C(7) C 0.31261(7) 0.20757(18) 0.16079(13) 0.0194(5) Uani 1.00 1 d
C(8) C 0.07451(8) 0.3216(2) 0.23918(17) 0.0437(7) Uani 1.00 1 d
C(9) C 0.08105(8) -0.0059(2) 0.23210(15) 0.0356(6) Uani 1.00 1 d
C(10) C 0.07642(7) 0.24997(17) 0.51001(14) 0.0206(5) Uani 1.00 1 d
C(11) C 0.03493(8) 0.1767(2) 0.46714(15) 0.0322(6) Uani 1.00 1 d
C(12) C -0.01074(8) 0.1875(2) 0.49093(15) 0.0329(6) Uani 1.00 1 d
C(13) C -0.01460(7) 0.27389(19) 0.56152(13) 0.0210(5) Uani 1.00 1 d
C(14) C 0.02731(7) 0.3488(2) 0.60841(15) 0.0300(6) Uani 1.00 1 d
C(15) C 0.07158(7) 0.3371(2) 0.58151(14) 0.0265(5) Uani 1.00 1 d
C(16) C -0.06269(7) 0.27863(19) 0.58928(14) 0.0237(5) Uani 1.00 1 d
C(17) C 0.16915(8) 0.4013(2) 0.47777(16) 0.0404(7) Uani 1.00 1 d
C(18) C 0.17720(8) 0.1024(2) 0.56033(16) 0.0404(7) Uani 1.00 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.082 0.070
;
International Tables for Crystallography
(1992, 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_publ_flag
O(1) Si(1) C(1) 107.62(7) yes
O(1) Si(1) C(8) 110.95(9) yes
O(1) Si(1) C(9) 106.94(8) yes
C(1) Si(1) C(8) 109.35(9) yes
C(1) Si(1) C(9) 109.94(9) yes
C(8) Si(1) C(9) 111.94(9) yes
O(1) Si(2) C(10) 106.67(8) yes
O(1) Si(2) C(17) 110.96(9) yes
O(1) Si(2) C(18) 108.22(8) yes
C(10) Si(2) C(17) 109.96(9) yes
C(10) Si(2) C(18) 109.59(10) yes
C(17) Si(2) C(18) 111.31(9) yes
Si(1) O(1) Si(2) 149.93(8) yes
Si(1) C(1) C(2) 120.38(15) yes
Si(1) C(1) C(6) 122.63(13) yes
C(2) C(1) C(6) 116.99(18) yes
C(1) C(2) C(3) 121.63(19) yes
C(2) C(3) C(4) 119.65(16) yes
C(3) C(4) C(5) 119.77(19) yes
C(3) C(4) C(7) 118.63(15) yes
C(5) C(4) C(7) 121.59(18) yes
C(4) C(5) C(6) 120.10(19) yes
C(1) C(6) C(5) 121.85(16) yes
O(6) C(7) O(7) 123.31(19) yes
O(6) C(7) C(4) 115.32(15) yes
O(7) C(7) C(4) 121.34(18) yes
Si(2) C(10) C(11) 121.53(16) yes
Si(2) C(10) C(15) 121.28(13) yes
C(11) C(10) C(15) 117.03(19) yes
C(10) C(11) C(12) 122.7(2) yes
C(11) C(12) C(13) 119.20(18) yes
C(12) C(13) C(14) 119.93(19) yes
C(12) C(13) C(16) 118.75(16) yes
C(14) C(13) C(16) 121.23(18) yes
C(13) C(14) C(15) 118.90(19) yes
C(10) C(15) C(14) 122.18(17) yes
O(8) C(16) O(9) 122.83(19) yes
O(8) C(16) C(13) 121.23(18) yes
O(9) C(16) C(13) 115.94(15) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Si(1) O(1) 1.6183(14) yes
Si(1) C(1) 1.873(2) yes
Si(1) C(8) 1.8504(19) yes
Si(1) C(9) 1.8517(19) yes
Si(2) O(1) 1.6396(14) yes
Si(2) C(10) 1.876(2) yes
Si(2) C(17) 1.860(2) yes
Si(2) C(18) 1.845(2) yes
O(6) C(7) 1.311(2) yes
O(7) C(7) 1.232(2) yes
O(8) C(16) 1.233(2) yes
O(9) C(16) 1.292(2) yes
C(1) C(2) 1.405(2) yes
C(1) C(6) 1.395(2) yes
C(2) C(3) 1.386(3) yes
C(3) C(4) 1.394(2) yes
C(4) C(5) 1.379(2) yes
C(4) C(7) 1.478(2) yes
C(5) C(6) 1.385(3) yes
C(10) C(11) 1.369(2) yes
C(10) C(15) 1.407(2) yes
C(11) C(12) 1.393(3) yes
C(12) C(13) 1.384(3) yes
C(13) C(14) 1.405(2) yes
C(13) C(16) 1.484(2) yes
C(14) C(15) 1.380(3) yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
O(6) O(8) 2.650(2) 8_554
O(6) O(9) 3.5912(18) 8_554
O(6) C(5) 3.480(2) 7_555
O(6) C(16) 3.492(2) 8_554
O(7) O(8) 3.322(2) 8_554
O(7) O(9) 2.643(2) 8_554
O(7) C(15) 3.527(2) 7_556
O(7) C(16) 3.375(2) 8_554
O(7) C(17) 3.598(2) 6_545
O(8) O(6) 2.650(2) 8_455
O(8) O(7) 3.322(2) 8_455
O(8) C(6) 3.503(2) 2_555
O(8) C(7) 3.376(2) 8_455
O(9) O(6) 3.5912(18) 8_455
O(9) O(7) 2.643(2) 8_455
O(9) C(7) 3.479(2) 8_455
O(9) C(8) 3.472(2) 3_566
O(9) C(14) 3.512(2) 2_556
C(5) O(6) 3.480(2) 7_555
C(6) O(8) 3.503(2) 2_555
C(7) O(8) 3.376(2) 8_554
C(7) O(9) 3.479(2) 8_554
C(8) O(9) 3.472(2) 3_566
C(11) C(12) 3.555(2) 3_556
C(12) C(11) 3.555(2) 3_556
C(12) C(12) 3.553(2) 3_556
C(14) O(9) 3.512(2) 2_556
C(15) O(7) 3.527(2) 7_556
C(16) O(6) 3.492(2) 8_455
C(16) O(7) 3.375(2) 8_455
C(17) O(7) 3.598(2) 6_555
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
O(1) Si(1) C(1) C(2) 31.75(15)
O(1) Si(1) C(1) C(6) -149.12(14)
C(1) Si(1) O(1) Si(2) 88.3(2)
C(8) Si(1) O(1) Si(2) -31.3(2)
C(9) Si(1) O(1) Si(2) -153.62(19)
C(8) Si(1) C(1) C(2) 152.35(14)
C(8) Si(1) C(1) C(6) -28.52(17)
C(9) Si(1) C(1) C(2) -84.38(16)
C(9) Si(1) C(1) C(6) 94.75(15)
O(1) Si(2) C(10) C(11) 17.12(18)
O(1) Si(2) C(10) C(15) -167.47(14)
C(10) Si(2) O(1) Si(1) 88.1(2)
C(17) Si(2) O(1) Si(1) -31.7(2)
C(18) Si(2) O(1) Si(1) -154.10(19)
C(17) Si(2) C(10) C(11) 137.52(16)
C(17) Si(2) C(10) C(15) -47.08(18)
C(18) Si(2) C(10) C(11) -99.83(17)
C(18) Si(2) C(10) C(15) 75.58(16)
Si(1) C(1) C(2) C(3) 179.56(14)
Si(1) C(1) C(6) C(5) -179.54(13)
C(2) C(1) C(6) C(5) -0.4(2)
C(6) C(1) C(2) C(3) 0.4(2)
C(1) C(2) C(3) C(4) 0.5(2)
C(2) C(3) C(4) C(5) -1.4(2)
C(2) C(3) C(4) C(7) 179.53(16)
C(3) C(4) C(5) C(6) 1.4(2)
C(3) C(4) C(7) O(6) -179.16(16)
C(3) C(4) C(7) O(7) -0.9(2)
C(5) C(4) C(7) O(6) 1.8(2)
C(5) C(4) C(7) O(7) -179.96(13)
C(7) C(4) C(5) C(6) -179.54(16)
C(4) C(5) C(6) C(1) -0.5(2)
Si(2) C(10) C(11) C(12) 176.49(15)
Si(2) C(10) C(15) C(14) -175.24(15)
C(11) C(10) C(15) C(14) 0.4(2)
C(15) C(10) C(11) C(12) 0.9(2)
C(10) C(11) C(12) C(13) -0.9(3)
C(11) C(12) C(13) C(14) -0.3(2)
C(11) C(12) C(13) C(16) -176.83(17)
C(12) C(13) C(14) C(15) 1.5(2)
C(12) C(13) C(16) O(8) -5.0(2)
C(12) C(13) C(16) O(9) 175.09(16)
C(14) C(13) C(16) O(8) 178.50(17)
C(14) C(13) C(16) O(9) -1.4(2)
C(16) C(13) C(14) C(15) 177.93(17)
C(13) C(14) C(15) C(10) -1.5(2)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 453150
