#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/61/2006118.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006118
loop_
_publ_author_name
'Stradiotto, Mark'
'Crowe, Grant'
'Ruffolo, Ralph'
'Brook, Michael A.'
_publ_section_title
;
 1-Styrylsilatrane
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              637
_journal_page_last               639
_journal_paper_doi               10.1107/S0108270197000310
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C14 H19 N O3 Si'
_chemical_formula_weight         277.39
_chemical_name_common            1-Styrylsilatrane
_chemical_name_systematic
;
E-1-(2-phenylethenyl)-2,8,9-trioxa-5-aza-1-silabicyclo[3.3.3]undecane
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.839(2)
_cell_length_b                   13.519(3)
_cell_length_c                   18.939(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.82
_cell_measurement_theta_min      7.58
_cell_volume                     2775.2(10)
_computing_cell_refinement       P3
_computing_data_collection       'P3 (Siemens, 1990)'
_computing_data_reduction        'XDISK (Siemens, 1989)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.2033
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3366
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_meas      1.337
_exptl_crystal_density_method    floatation
_exptl_crystal_description       'Irregular fragment'
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.761
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.766
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.2333
_refine_ls_R_factor_obs          .0554
_refine_ls_shift/esd_max         -0.019
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0346(Fo²+2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1305
_refine_ls_wR_factor_obs         .0879
_reflns_number_observed          725
_reflns_number_total             2636
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fr1023.cif
_cod_data_source_block           st
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w =
1/[\s^2^(Fo^2^)+(0.0346(Fo^2^+2Fc^2^)/3)^2^]' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0346(Fo^2^+2Fc^2^)/3)^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2006118
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Si1 .15713(14) .79420(10) .10774(8) .0548(4) Uani d . 1 . Si
O2 .2678(3) .8772(2) .1012(2) .0705(12) Uani d . 1 . O
C3 .3925(5) .8529(4) .0924(3) .089(2) Uani d . 1 . C
H3C .4379(5) .8646(4) .1358(3) .107 Uiso calc PR .149(12) 2 H
H3D .4290(5) .8924(4) .0551(3) .107 Uiso calc PR .149(12) 2 H
H3A .4436(5) .9033(4) .1128(3) .107 Uiso d PR .851(12) 1 H
H3B .4114(5) .8475(4) .0430(3) .107 Uiso d PR .851(12) 1 H
C4 .4190(8) .7526(6) .1200(6) .097(4) Uani d P .851(12) 1 C
H4A .4938(8) .7213(6) .1046(6) .116 Uiso d PR .851(12) 1 H
H4B .4217(8) .7609(6) .1703(6) .116 Uiso d PR .851(12) 1 H
C4A .395(5) .745(4) .073(4) .097(4) Uani d P .149(12) 2 C
H4AA .430(5) .725(4) .029(4) .116 Uiso d PR .149(12) 2 H
H4AB .456(5) .732(4) .109(4) .116 Uiso d PR .149(12) 2 H
N5 .3072(4) .6928(3) .1076(2) .0548(11) Uani d . 1 . N
C6 .2845(9) .6228(7) .1636(4) .087(3) Uani d P .851(12) 1 C
H6A .3559(9) .5891(7) .1815(4) .104 Uiso d PR .851(12) 1 H
H6B .2300(9) .5752(7) .1426(4) .104 Uiso d PR .851(12) 1 H
C6A .331(6) .685(4) .187(2) .087(3) Uani d P .149(12) 2 C
H6AA .406(6) .704(4) .210(2) .104 Uiso d PR .149(12) 2 H
H6AB .331(6) .615(4) .179(2) .104 Uiso d PR .149(12) 2 H
C7 .2036(6) .6727(4) .2166(3) .088(2) Uani d . 1 . C
H7C .1728(6) .6068(4) .2064(3) .106 Uiso calc PR .149(12) 2 H
H7D .2050(6) .6815(4) .2674(3) .106 Uiso calc PR .149(12) 2 H
H7A .1556(6) .6284(4) .2452(3) .106 Uiso d PR .851(12) 1 H
H7B .2628(6) .7053(4) .2462(3) .106 Uiso d PR .851(12) 1 H
O8 .1272(3) .7439(2) .1854(2) .0674(12) Uani d . 1 . O
O9 .1167(3) .7338(2) .0352(2) .0658(11) Uani d . 1 . O
C10 .1785(5) .6491(4) .0110(3) .080(2) Uani d . 1 . C
H10C .2236(5) .6649(4) -.0318(3) .096 Uiso calc PR .149(12) 2 H
H10D .1186(5) .5981(4) -.0003(3) .096 Uiso calc PR .149(12) 2 H
H10A .1709(5) .6442(4) -.0394(3) .096 Uiso d PR .851(12) 1 H
H10B .1418(5) .5914(4) .0318(3) .096 Uiso d PR .851(12) 1 H
C11 .3069(9) .6461(7) .0373(4) .081(3) Uani d P .851(12) 1 C
H11A .3469(9) .5829(7) .0359(4) .097 Uiso d PR .851(12) 1 H
H11B .3509(9) .6920(7) .0080(4) .097 Uiso d PR .851(12) 1 H
C11A .266(5) .611(4) .066(3) .081(3) Uani d P .149(12) 2 C
H11C .255(5) .547(4) .086(3) .097 Uiso d PR .149(12) 2 H
H11D .336(5) .609(4) .035(3) .097 Uiso d PR .149(12) 2 H
C12 .0262(4) .8828(3) .1058(3) .0554(14) Uani d . 1 . C
H12A .0265(4) .9298(3) .0679(3) .066 Uiso d R 1 . H
C13 -.0674(5) .8907(3) .1494(3) .059(2) Uani d . 1 . C
H13A -.0654(5) .8456(3) .1886(3) .071 Uiso d R 1 . H
C14 -.1725(5) .9584(4) .1461(3) .0525(14) Uani d . 1 . C
C15 -.2744(5) .9416(4) .1884(3) .061(2) Uani d . 1 . C
H15A -.2744(5) .8863(4) .2202(3) .073 Uiso d R 1 . H
C16 -.3758(5) 1.0027(4) .1847(3) .070(2) Uani d . 1 . C
H16A -.4441(5) .9902(4) .2157(3) .084 Uiso d R 1 . H
C17 -.3789(6) 1.0817(5) .1391(3) .079(2) Uani d . 1 . C
H17A -.4503(6) 1.1235(5) .1358(3) .095 Uiso d R 1 . H
C18 -.2761(6) 1.0990(4) .0986(3) .076(2) Uani d . 1 . C
H18A -.2752(6) 1.1550(4) .0674(3) .091 Uiso d R 1 . H
C19 -.1758(5) 1.0387(4) .1011(3) .0612(15) Uani d . 1 . C
H19A -.1059(5) 1.0521(4) .0715(3) .073 Uiso d R 1 . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0522 0.0431 '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_publ_flag
O2 Si1 O8 119.4(2) y
O2 Si1 O9 117.7(2) y
O8 Si1 O9 118.9(2) y
O2 Si1 C12 96.6(2) y
O8 Si1 C12 97.6(2) y
O9 Si1 C12 95.7(2) y
O2 Si1 N5 83.2(2) y
O8 Si1 N5 83.4(2) y
O9 Si1 N5 83.3(2) y
C12 Si1 N5 178.8(3) y
C3 O2 Si1 123.5(3) ?
O2 C3 C4 111.1(6) ?
O2 C3 C4A 106.(2) ?
N5 C4 C3 106.6(6) ?
N5 C4A C3 112.(5) ?
C4A N5 C11A 111.(3) ?
C6 N5 C11 112.5(5) ?
C6 N5 C4 112.5(6) ?
C11 N5 C4 112.4(6) ?
C4A N5 C6A 113.(3) ?
C11A N5 C6A 123.(3) ?
C4A N5 Si1 102.(2) ?
C11A N5 Si1 105.(2) ?
C6 N5 Si1 106.9(4) ?
C11 N5 Si1 106.0(4) ?
C4 N5 Si1 106.0(4) ?
C6A N5 Si1 99.9(18) ?
N5 C6 C7 107.4(6) ?
C7 C6A N5 103.(4) ?
O8 C7 C6 111.9(5) ?
O8 C7 C6A 108.1(16) ?
C7 O8 Si1 122.9(3) ?
C10 O9 Si1 123.2(3) ?
O9 C10 C11 111.1(5) ?
O9 C10 C11A 111.(2) ?
N5 C11 C10 107.2(6) ?
N5 C11A C10 109.(4) ?
C13 C12 Si1 129.1(4) ?
C12 C13 C14 128.7(5) ?
C19 C14 C15 117.8(5) ?
C19 C14 C13 122.6(5) ?
C15 C14 C13 119.6(5) ?
C16 C15 C14 120.7(5) ?
C17 C16 C15 121.2(6) ?
C18 C17 C16 117.6(6) ?
C19 C18 C17 121.9(6) ?
C18 C19 C14 120.9(6) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 O2 . 1.647(3) y
Si1 O8 . 1.652(3) y
Si1 O9 . 1.657(3) y
Si1 C12 . 1.857(5) y
Si1 N5 . 2.127(4) y
O2 C3 . 1.401(5) ?
C3 C4 . 1.481(9) ?
C3 C4A . 1.50(5) ?
C4 N5 . 1.475(9) ?
C4A N5 . 1.35(7) ?
N5 C11A . 1.43(5) ?
N5 C6 . 1.442(7) ?
N5 C11 . 1.473(8) ?
N5 C6A . 1.53(4) ?
C6 C7 . 1.493(9) ?
C6A C7 . 1.50(6) ?
C7 O8 . 1.401(5) ?
O9 C10 . 1.404(5) ?
C10 C11 . 1.479(10) ?
C10 C11A . 1.50(6) ?
C12 C13 . 1.312(6) y
C13 C14 . 1.463(6) ?
C14 C19 . 1.381(6) ?
C14 C15 . 1.383(6) ?
C15 C16 . 1.376(6) ?
C16 C17 . 1.374(6) ?
C17 C18 . 1.373(7) ?
C18 C19 . 1.360(6) ?
