#------------------------------------------------------------------------------
#$Date: 2018-09-05 04:24:25 +0300 (Wed, 05 Sep 2018) $
#$Revision: 210454 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/48/7104804.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_7104804
loop_
_publ_author_name
'Tsutsui, Shinobu'
'Sakamoto, Kenkichi'
_publ_section_title
;
 Preparation and structures of novel silamacrocyclic compounds:
 silacalix[4]quinone and silacalix[4]hydroquinone octamethyl ether
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   18
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2322
_journal_page_last               2323
_journal_paper_doi               10.1039/b307048d
_journal_year                    2003
_chemical_formula_sum            'C88 H94 O16 Si8'
_chemical_formula_weight         1632.35
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 122.575(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.866(4)
_cell_length_b                   13.099(2)
_cell_length_c                   16.060(3)
_cell_measurement_reflns_used    3417
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.55
_cell_volume                     4407.9(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      123(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  '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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13196
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        -0.13
_diffrn_standards_number         109
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.9764
_exptl_absorpt_correction_T_min  0.9298
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0570
_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)+(0.0991P)²+2.9113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1872
_reflns_number_gt                3185
_reflns_number_total             5135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307048d.txt
_cod_data_source_block           tetrasilacalix4quinone_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7104804
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.24607(13) 0.2794(2) 0.2806(2) 0.0250(6) Uani 1 1 d . . .
C2 C 0.17508(13) 0.2738(2) 0.2155(2) 0.0259(6) Uani 1 1 d . . .
C3 C 0.14931(14) 0.2612(2) 0.1184(2) 0.0310(7) Uani 1 1 d . . .
H3 H 0.1042 0.2567 0.0764 0.037 Uiso 1 1 calc R . .
C4 C 0.18756(14) 0.2539(2) 0.0736(2) 0.0324(7) Uani 1 1 d . . .
C5 C 0.25742(14) 0.2642(2) 0.1390(2) 0.0296(6) Uani 1 1 d . . .
H5 H 0.2826 0.2631 0.1109 0.036 Uiso 1 1 calc R . .
C6 C 0.28660(13) 0.2751(2) 0.2376(2) 0.0254(6) Uani 1 1 d . . .
C7 C 0.14799(17) 0.1675(3) 0.3593(3) 0.0424(8) Uani 1 1 d . . .
H7A H 0.1173 0.1627 0.3796 0.064 Uiso 1 1 calc R . .
H7B H 0.1911 0.1760 0.4179 0.064 Uiso 1 1 calc R . .
H7C H 0.1462 0.1050 0.3244 0.064 Uiso 1 1 calc R . .
C8 C 0.04147(15) 0.2803(3) 0.1769(3) 0.0443(8) Uani 1 1 d . . .
H8A H 0.0297 0.2145 0.1424 0.066 Uiso 1 1 calc R . .
H8B H 0.0330 0.3351 0.1299 0.066 Uiso 1 1 calc R . .
H8C H 0.0162 0.2918 0.2065 0.066 Uiso 1 1 calc R . .
C9 C 0.1365(2) 0.5000 0.2981(3) 0.0322(9) Uani 1 2 d S . .
C10 C 0.14953(14) 0.4004(2) 0.3511(2) 0.0305(7) Uani 1 1 d . . .
C11 C 0.17690(15) 0.4034(2) 0.4495(2) 0.0343(7) Uani 1 1 d . . .
H11 H 0.1863 0.3408 0.4845 0.041 Uiso 1 1 calc R . .
C12 C 0.1931(2) 0.5000 0.5055(3) 0.0373(10) Uani 1 2 d S . .
C13 C 0.37786(18) 0.5000 0.3452(3) 0.0266(8) Uani 1 2 d S . .
C14 C 0.39712(12) 0.4012(2) 0.3995(2) 0.0251(6) Uani 1 1 d . . .
C15 C 0.43039(13) 0.4042(2) 0.4985(2) 0.0285(6) Uani 1 1 d . . .
H15 H 0.4425 0.3415 0.5338 0.034 Uiso 1 1 calc R . .
C16 C 0.44908(19) 0.5000 0.5549(3) 0.0291(9) Uani 1 2 d S . .
C17 C 0.40134(16) 0.1685(2) 0.4125(2) 0.0386(7) Uani 1 1 d . . .
H17A H 0.3812 0.1059 0.3752 0.058 Uiso 1 1 calc R . .
H17B H 0.3885 0.1803 0.4598 0.058 Uiso 1 1 calc R . .
H17C H 0.4478 0.1616 0.4483 0.058 Uiso 1 1 calc R . .
C18 C 0.41559(14) 0.2767(3) 0.2564(2) 0.0356(7) Uani 1 1 d . . .
H18A H 0.4619 0.2779 0.3032 0.053 Uiso 1 1 calc R . .
H18B H 0.4026 0.3367 0.2132 0.053 Uiso 1 1 calc R . .
H18C H 0.4035 0.2145 0.2164 0.053 Uiso 1 1 calc R . .
C19 C 0.0364(4) 1.0000 -0.0451(5) 0.079(2) Uani 1 2 d S . .
C20 C 0.0661(5) 1.0000 0.0561(5) 0.092(3) Uani 1 2 d S . .
H20 H 0.1114 1.0000 0.0969 0.110 Uiso 1 2 calc SR . .
C21 C 0.0291(4) 1.0000 0.1002(5) 0.085(2) Uani 1 2 d S . .
H21 H 0.0508 1.0000 0.1702 0.102 Uiso 1 2 calc SR . .
C22 C 0.0759(4) 1.0000 -0.0924(5) 0.098(3) Uani 1 2 d S . .
H22A H 0.1117 0.9525 -0.0567 0.147 Uiso 0.50 1 calc PR . .
H22B H 0.0922 1.0689 -0.0893 0.147 Uiso 0.50 1 calc PR . .
H22C H 0.0489 0.9786 -0.1616 0.147 Uiso 0.50 1 calc PR . .
C23 C 0.2084(6) 0.5000 0.8886(7) 0.129(5) Uani 1 2 d S . .
C24 C 0.2318(7) 0.5000 0.9869(10) 0.143(6) Uani 1 2 d S . .
H24 H 0.2766 0.5000 1.0332 0.171 Uiso 1 2 calc SR . .
C25 C 0.1908(7) 0.5000 1.0194(7) 0.147(6) Uani 1 2 d S . .
H25 H 0.2075 0.5000 1.0883 0.176 Uiso 1 2 calc SR . .
C26 C 0.1231(6) 0.5000 0.9504(6) 0.114(4) Uani 1 2 d S . .
C27 C 0.1023(6) 0.5000 0.8523(5) 0.118(4) Uani 1 2 d S . .
H27 H 0.0577 0.5000 0.8040 0.142 Uiso 1 2 calc SR . .
C28 C 0.1461(6) 0.5000 0.8217(7) 0.114(4) Uani 1 2 d S . .
H28 H 0.1309 0.5000 0.7533 0.137 Uiso 1 2 calc SR . .
C29 C 0.2560(6) 0.5000 0.8540(9) 0.141(4) Uani 1 2 d S . .
H29A H 0.2357 0.4683 0.7885 0.211 Uiso 0.50 1 calc PR . .
H29B H 0.2943 0.4613 0.9011 0.211 Uiso 0.50 1 calc PR . .
H29C H 0.2679 0.5704 0.8504 0.211 Uiso 0.50 1 calc PR . .
C30 C 0.0776(7) 0.5000 0.9865(6) 0.149(5) Uani 1 2 d S . .
H30A H 0.0368 0.5303 0.9358 0.224 Uiso 0.50 1 calc PR . .
H30B H 0.0961 0.5400 1.0475 0.224 Uiso 0.50 1 calc PR . .
H30C H 0.0705 0.4297 0.9993 0.224 Uiso 0.50 1 calc PR . .
O1 O 0.27146(9) 0.28711(16) 0.37008(14) 0.0333(5) Uani 1 1 d . . .
O2 O 0.16234(11) 0.2375(2) -0.01517(16) 0.0465(6) Uani 1 1 d . . .
O3 O 0.11512(19) 0.5000 0.2091(2) 0.0503(9) Uani 1 2 d S . .
O4 O 0.21825(18) 0.5000 0.5960(2) 0.0478(9) Uani 1 2 d S . .
O5 O 0.34525(15) 0.5000 0.2538(2) 0.0385(7) Uani 1 2 d S . .
O6 O 0.47939(16) 0.5000 0.6454(2) 0.0446(8) Uani 1 2 d S . .
Si1 Si 0.12777(4) 0.27928(6) 0.27578(6) 0.0298(2) Uani 1 1 d . . .
Si2 Si 0.37539(4) 0.27896(6) 0.32535(6) 0.0264(2) Uani 1 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 0.0033 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
_geom_angle_publ_flag
O1 C1 C2 119.6(2) . . ?
O1 C1 C6 119.7(2) . . ?
C2 C1 C6 120.7(2) . . ?
C3 C2 C1 117.8(2) . . ?
C3 C2 Si1 124.3(2) . . ?
C1 C2 Si1 117.91(19) . . ?
C2 C3 C4 123.1(3) . . ?
O2 C4 C3 121.2(3) . . ?
O2 C4 C5 120.8(3) . . ?
C3 C4 C5 118.0(3) . . ?
C6 C5 C4 122.0(3) . . ?
C5 C6 C1 118.3(2) . . ?
C5 C6 Si2 123.9(2) . . ?
C1 C6 Si2 117.70(19) . . ?
O3 C9 C10 119.21(18) . 6_565 ?
O3 C9 C10 119.21(18) . . ?
C10 C9 C10 121.6(4) 6_565 . ?
C11 C10 C9 117.5(3) . . ?
C11 C10 Si1 124.5(2) . . ?
C9 C10 Si1 118.0(2) . . ?
C10 C11 C12 122.7(3) . . ?
O4 C12 C11 121.09(19) . . ?
O4 C12 C11 121.09(19) . 6_565 ?
C11 C12 C11 117.8(4) . 6_565 ?
O5 C13 C14 119.62(17) . 6_565 ?
O5 C13 C14 119.62(17) . . ?
C14 C13 C14 120.8(3) 6_565 . ?
C15 C14 C13 117.9(3) . . ?
C15 C14 Si2 123.8(2) . . ?
C13 C14 Si2 118.3(2) . . ?
C14 C15 C16 123.0(3) . . ?
O6 C16 C15 121.33(17) . . ?
O6 C16 C15 121.33(17) . 6_565 ?
C15 C16 C15 117.3(3) . 6_565 ?
C21 C19 C20 117.1(8) 5_575 . ?
C21 C19 C22 122.5(7) 5_575 . ?
C20 C19 C22 120.5(8) . . ?
C19 C20 C21 120.4(8) . . ?
C19 C21 C20 122.5(7) 5_575 . ?
C28 C23 C24 121.7(15) . . ?
C28 C23 C29 119.4(11) . . ?
C24 C23 C29 118.9(12) . . ?
C23 C24 C25 120.0(14) . . ?
C24 C25 C26 120.6(11) . . ?
C27 C26 C25 116.8(13) . . ?
C27 C26 C30 122.6(11) . . ?
C25 C26 C30 120.6(10) . . ?
C26 C27 C28 120.9(11) . . ?
C23 C28 C27 120.0(11) . . ?
C8 Si1 C7 111.11(16) . . ?
C8 Si1 C2 108.33(14) . . ?
C7 Si1 C2 109.82(13) . . ?
C8 Si1 C10 109.97(15) . . ?
C7 Si1 C10 109.03(14) . . ?
C2 Si1 C10 108.54(12) . . ?
C18 Si2 C17 110.89(15) . . ?
C18 Si2 C6 110.32(13) . . ?
C17 Si2 C6 109.52(14) . . ?
C18 Si2 C14 109.10(13) . . ?
C17 Si2 C14 108.45(14) . . ?
C6 Si2 C14 108.52(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.224(3) . ?
C1 C2 1.492(4) . ?
C1 C6 1.498(4) . ?
C2 C3 1.339(4) . ?
C2 Si1 1.885(3) . ?
C3 C4 1.472(4) . ?
C4 O2 1.229(4) . ?
C4 C5 1.475(4) . ?
C5 C6 1.347(4) . ?
C6 Si2 1.874(3) . ?
C7 Si1 1.863(3) . ?
C8 Si1 1.859(3) . ?
C9 O3 1.228(5) . ?
C9 C10 1.494(4) 6_565 ?
C9 C10 1.494(4) . ?
C10 C11 1.343(4) . ?
C10 Si1 1.889(3) . ?
C11 C12 1.478(4) . ?
C12 O4 1.234(5) . ?
C12 C11 1.478(4) 6_565 ?
C13 O5 1.237(5) . ?
C13 C14 1.489(3) 6_565 ?
C13 C14 1.489(3) . ?
C14 C15 1.340(4) . ?
C14 Si2 1.892(3) . ?
C15 C16 1.469(4) . ?
C16 O6 1.225(5) . ?
C16 C15 1.469(4) 6_565 ?
C17 Si2 1.870(3) . ?
C18 Si2 1.848(3) . ?
C19 C21 1.374(11) 5_575 ?
C19 C20 1.376(9) . ?
C19 C22 1.530(11) . ?
C20 C21 1.431(12) . ?
C21 C19 1.374(11) 5_575 ?
C23 C28 1.327(14) . ?
C23 C24 1.357(15) . ?
C23 C29 1.556(15) . ?
C24 C25 1.374(17) . ?
C25 C26 1.432(16) . ?
C26 C27 1.368(11) . ?
C26 C30 1.524(15) . ?
C27 C28 1.416(14) . ?
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
C13 C14 C15 C16 -0.7(4) . . . . ?
C9 C10 C11 C12 1.2(5) . . . . ?
C4 C5 C6 C1 -1.5(4) . . . . ?
C1 C2 C3 C4 -0.8(4) . . . . ?
