#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/93/7009368.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_7009368
loop_
_publ_author_name
'Rulkens, Ron'
'Coles, Martyn P.'
'Tilley, T. Don'
_publ_section_title
;
 Synthesis and structure of the (tetrahydroxy)oligosiloxane
 [(tBuO)3SiOSi(OH)2]2O
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              627
_journal_paper_doi               10.1039/b000322k
_journal_year                    2000
_chemical_formula_moiety         'C24 H60 O13 Si4 '
_chemical_formula_sum            'C24 H60 O13 Si4'
_chemical_formula_weight         669.07
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                112.688(1)
_cell_angle_beta                 93.374(1)
_cell_angle_gamma                90.217(1)
_cell_formula_units_Z            2
_cell_length_a                   9.4952(6)
_cell_length_b                   14.1078(8)
_cell_length_c                   15.3210(9)
_cell_measurement_temperature    273.2
_cell_volume                     1889.5(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            0
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.150
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4741
_refine_ls_R_factor_gt           0.0000
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00024|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                0
_reflns_number_total             0
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            b000322k.txt
_cod_data_source_block           Rulken's_starting_material
_cod_original_sg_symbol_H-M      'P -1         '
_cod_original_formula_sum        'C24 H60 O13 Si4 '
_cod_database_code               7009368
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.28692(9) 0.27073(6) 0.32826(6) 0.0232(2) Uani 1.00 d . . .
Si2 Si 0.06551(9) 0.10684(7) 0.18374(6) 0.0228(2) Uani 1.00 d . . .
Si3 Si 0.30142(8) -0.00712(6) 0.06766(6) 0.0202(2) Uani 1.00 d . . .
Si4 Si 0.33737(9) -0.15758(7) 0.17640(6) 0.0260(2) Uani 1.00 d . . .
O1 O 0.4340(2) 0.2121(2) 0.2948(1) 0.0257(6) Uani 1.00 d . . .
O2 O 0.2664(2) 0.2760(2) 0.4333(1) 0.0274(6) Uani 1.00 d . . .
O3 O 0.2892(2) 0.3857(2) 0.3294(1) 0.0332(6) Uani 1.00 d . . .
O4 O 0.1684(2) 0.1999(2) 0.2523(1) 0.0327(6) Uani 1.00 d . . .
O5 O 0.0212(3) 0.0321(2) 0.2340(2) 0.0430(9) Uani 1.00 d . . .
O6 O -0.0702(2) 0.1597(2) 0.1586(2) 0.0307(7) Uani 1.00 d . . .
O7 O 0.1512(2) 0.0449(1) 0.0906(1) 0.0252(6) Uani 1.00 d . . .
O8 O 0.4316(2) 0.0759(2) 0.1115(2) 0.0303(6) Uani 1.00 d . . .
O9 O 0.3079(2) -0.0560(2) -0.0461(1) 0.0260(6) Uani 1.00 d . . .
O10 O 0.3135(2) -0.0959(2) 0.1082(1) 0.0328(7) Uani 1.00 d . . .
O11 O 0.2367(2) -0.1015(2) 0.2632(1) 0.0326(6) Uani 1.00 d . . .
O12 O 0.4971(2) -0.1492(2) 0.2203(1) 0.0305(6) Uani 1.00 d . . .
O13 O 0.2955(2) -0.2776(2) 0.1182(1) 0.0316(6) Uani 1.00 d . . .
C1 C 0.5806(3) 0.2413(2) 0.3343(2) 0.0280(9) Uani 1.00 d . . .
C2 C 0.6480(3) 0.2930(3) 0.2765(2) 0.0355(10) Uani 1.00 d . . .
C3 C 0.5850(3) 0.3121(3) 0.4380(2) 0.043(1) Uani 1.00 d . . .
C4 C 0.6510(4) 0.1408(3) 0.3211(3) 0.040(1) Uani 1.00 d . . .
C5 C 0.1693(3) 0.3298(2) 0.5042(2) 0.0314(9) Uani 1.00 d . . .
C6 C 0.1815(5) 0.2793(4) 0.5751(3) 0.073(2) Uani 1.00 d . . .
C7 C 0.0223(4) 0.3188(4) 0.4590(3) 0.072(1) Uani 1.00 d . . .
C8 C 0.2166(5) 0.4413(3) 0.5501(3) 0.065(1) Uani 1.00 d . . .
C9 C 0.2577(4) 0.4261(3) 0.2567(2) 0.0349(10) Uani 1.00 d . . .
C10 C 0.3006(4) 0.3529(3) 0.1610(2) 0.044(1) Uani 1.00 d . . .
C11 C 0.1004(4) 0.4437(3) 0.2531(3) 0.057(1) Uani 1.00 d . . .
C12 C 0.3423(5) 0.5262(3) 0.2889(3) 0.058(1) Uani 1.00 d . . .
C13 C 0.2443(4) -0.0964(3) 0.3602(2) 0.037(1) Uani 1.00 d . . .
C14 C 0.2913(7) -0.1947(4) 0.3637(4) 0.109(2) Uani 1.00 d . . .
C15 C 0.1006(5) -0.0689(4) 0.3963(3) 0.077(2) Uani 1.00 d . . .
C16 C 0.3463(6) -0.0086(5) 0.4170(3) 0.094(2) Uani 1.00 d . . .
C17 C 0.6255(3) -0.1981(3) 0.1802(2) 0.0362(10) Uani 1.00 d . . .
C18 C 0.6186(4) -0.3103(3) 0.1686(3) 0.061(1) Uani 1.00 d . . .
C19 C 0.6445(4) -0.1866(3) 0.0880(3) 0.059(1) Uani 1.00 d . . .
C20 C 0.7441(4) -0.1414(3) 0.2525(3) 0.046(1) Uani 1.00 d . . .
C21 C 0.1991(3) -0.3329(3) 0.0381(2) 0.0359(10) Uani 1.00 d . . .
C22 C 0.1913(4) -0.4414(3) 0.0346(3) 0.055(1) Uani 1.00 d . . .
C23 C 0.2606(4) -0.3340(3) -0.0517(3) 0.055(1) Uani 1.00 d . . .
C24 C 0.0572(4) -0.2836(3) 0.0507(3) 0.063(1) Uani 1.00 d . . .
H1 H 0.7425 0.3134 0.3008 0.0426 Uiso 1.00 calc . . .
H2 H 0.6476 0.2464 0.2122 0.0426 Uiso 1.00 calc . . .
H3 H 0.5962 0.3518 0.2803 0.0426 Uiso 1.00 calc . . .
H4 H 0.6803 0.3296 0.4616 0.0512 Uiso 1.00 calc . . .
H5 H 0.5359 0.3728 0.4446 0.0512 Uiso 1.00 calc . . .
H6 H 0.5415 0.2783 0.4728 0.0512 Uiso 1.00 calc . . .
H7 H 0.6028 0.1070 0.3540 0.0478 Uiso 1.00 calc . . .
H8 H 0.6477 0.0981 0.2555 0.0478 Uiso 1.00 calc . . .
H9 H 0.7466 0.1543 0.3454 0.0478 Uiso 1.00 calc . . .
H10 H 0.1187 0.3103 0.6236 0.0880 Uiso 1.00 calc . . .
H11 H 0.1581 0.2082 0.5440 0.0880 Uiso 1.00 calc . . .
H12 H 0.2756 0.2879 0.6023 0.0880 Uiso 1.00 calc . . .
H13 H -0.0407 0.3547 0.5058 0.0864 Uiso 1.00 calc . . .
H14 H 0.0201 0.3467 0.4115 0.0864 Uiso 1.00 calc . . .
H15 H -0.0054 0.2482 0.4310 0.0864 Uiso 1.00 calc . . .
H16 H 0.3097 0.4463 0.5781 0.0781 Uiso 1.00 calc . . .
H17 H 0.2153 0.4703 0.5035 0.0781 Uiso 1.00 calc . . .
H18 H 0.1546 0.4774 0.5976 0.0781 Uiso 1.00 calc . . .
H19 H 0.2523 0.2886 0.1441 0.0527 Uiso 1.00 calc . . .
H20 H 0.2771 0.3806 0.1147 0.0527 Uiso 1.00 calc . . .
H21 H 0.3996 0.3434 0.1640 0.0527 Uiso 1.00 calc . . .
H22 H 0.0756 0.4914 0.3131 0.0681 Uiso 1.00 calc . . .
H23 H 0.0769 0.4703 0.2060 0.0681 Uiso 1.00 calc . . .
H24 H 0.0502 0.3804 0.2381 0.0681 Uiso 1.00 calc . . .
H25 H 0.4399 0.5130 0.2936 0.0699 Uiso 1.00 calc . . .
H26 H 0.3257 0.5573 0.2443 0.0699 Uiso 1.00 calc . . .
H27 H 0.3144 0.5712 0.3491 0.0699 Uiso 1.00 calc . . .
H28 H 0.2253 -0.2481 0.3273 0.1305 Uiso 1.00 calc . . .
H29 H 0.3813 -0.2100 0.3384 0.1305 Uiso 1.00 calc . . .
H30 H 0.2975 -0.1893 0.4275 0.1305 Uiso 1.00 calc . . .
H31 H 0.1012 -0.0640 0.4599 0.0928 Uiso 1.00 calc . . .
H32 H 0.0758 -0.0047 0.3939 0.0928 Uiso 1.00 calc . . .
H33 H 0.0336 -0.1205 0.3579 0.0928 Uiso 1.00 calc . . .
H34 H 0.3553 -0.0028 0.4810 0.1132 Uiso 1.00 calc . . .
H35 H 0.4360 -0.0216 0.3909 0.1132 Uiso 1.00 calc . . .
H36 H 0.3119 0.0536 0.4148 0.1132 Uiso 1.00 calc . . .
H37 H 0.6102 -0.3138 0.2287 0.0737 Uiso 1.00 calc . . .
H38 H 0.5391 -0.3440 0.1275 0.0737 Uiso 1.00 calc . . .
H39 H 0.7023 -0.3429 0.1423 0.0737 Uiso 1.00 calc . . .
H40 H 0.7290 -0.2183 0.0625 0.0707 Uiso 1.00 calc . . .
H41 H 0.5665 -0.2186 0.0446 0.0707 Uiso 1.00 calc . . .
H42 H 0.6499 -0.1157 0.0988 0.0707 Uiso 1.00 calc . . .
H43 H 0.8316 -0.1706 0.2306 0.0552 Uiso 1.00 calc . . .
H44 H 0.7456 -0.0709 0.2613 0.0552 Uiso 1.00 calc . . .
H45 H 0.7292 -0.1471 0.3111 0.0552 Uiso 1.00 calc . . .
H46 H 0.1591 -0.4404 0.0925 0.0660 Uiso 1.00 calc . . .
H47 H 0.1277 -0.4820 -0.0165 0.0660 Uiso 1.00 calc . . .
H48 H 0.2824 -0.4700 0.0257 0.0660 Uiso 1.00 calc . . .
H49 H 0.3481 -0.3678 -0.0598 0.0655 Uiso 1.00 calc . . .
H50 H 0.1970 -0.3694 -0.1047 0.0655 Uiso 1.00 calc . . .
H51 H 0.2753 -0.2653 -0.0467 0.0655 Uiso 1.00 calc . . .
H52 H 0.0674 -0.2147 0.0557 0.0755 Uiso 1.00 calc . . .
H53 H -0.0055 -0.3209 -0.0023 0.0755 Uiso 1.00 calc . . .
H54 H 0.0202 -0.2842 0.1068 0.0755 Uiso 1.00 calc . . .
H55 H 0.058(4) 0.004(3) 0.242(3) 0.016(5) Uiso 1.00 calc . . .
H56 H -0.125(3) 0.130(2) 0.132(2) 0.0156 Uiso 1.00 calc . . .
H57 H 0.425(3) 0.109(2) 0.159(2) 0.0156 Uiso 1.00 calc . . .
H58 H 0.383(3) -0.065(2) -0.063(2) 0.0156 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.082 0.070
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
? ? ? ? ? ? ? ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
SI1 O1 1.632(2) . . yes
SI1 O2 1.607(2) . . yes
SI1 O3 1.615(2) . . yes
SI1 O4 1.599(2) . . yes
SI2 O4 1.609(2) . . yes
SI2 O5 1.594(3) . . yes
SI2 O6 1.593(2) . . yes
SI2 O7 1.625(2) . . yes
SI3 O7 1.602(2) . . yes
SI3 O8 1.624(2) . . yes
SI3 O9 1.613(2) . . yes
SI3 O10 1.600(2) . . yes
SI4 O10 1.605(2) . . yes
SI4 O11 1.629(2) . . yes
SI4 O12 1.608(2) . . yes
SI4 O13 1.615(2) . . yes
O1 C1 1.476(3) . . yes
O2 C5 1.446(3) . . yes
O3 C9 1.452(4) . . yes
O11 C13 1.458(4) . . yes
O12 C17 1.452(4) . . yes
O13 C21 1.442(4) . . yes
C1 C2 1.512(4) . . yes
C1 C3 1.514(4) . . yes
C1 C4 1.516(5) . . yes
C5 C6 1.510(5) . . yes
C5 C7 1.501(5) . . yes
C5 C8 1.508(5) . . yes
C9 C10 1.513(5) . . yes
C9 C11 1.516(5) . . yes
C9 C12 1.513(5) . . yes
C13 C14 1.477(6) . . yes
C13 C15 1.499(5) . . yes
C13 C16 1.513(6) . . yes
C17 C18 1.523(5) . . yes
C17 C19 1.503(5) . . yes
C17 C20 1.516(5) . . yes
C21 C22 1.513(5) . . yes
C21 C23 1.521(5) . . yes
C21 C24 1.507(5) . . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O6 O9 2.788(3) . 2_555 ?
O6 C2 3.457(4) . 1_455 ?
O8 O9 2.698(3) . 2_655 ?
O8 O8 3.584(4) . 2_655 ?
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
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21148271
