#------------------------------------------------------------------------------
#$Date: 2017-10-13 03:48:21 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201957 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/62/2016272.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_2016272
loop_
_publ_author_name
'Böhme, Uwe '
'Foehn, Ines C.'
_publ_section_title
;
 Two modifications of a five-coordinate silicon complex
;
_journal_coeditor_code           JZ3090
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o613
_journal_page_last               o616
_journal_paper_doi               10.1107/S0108270107045465
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C14 H19 N O2 Si'
_chemical_formula_moiety         'C14 H19 N O2 Si'
_chemical_formula_sum            'C14 H19 N O2 Si'
_chemical_formula_weight         261.39
_chemical_name_common
;
TBPY-5-34-[2-oxy-\kO-acetophenone-N-(2-oxy-\kO-ethyl)
iminato-\kN]silacyclopentane
;
_chemical_name_systematic
;
(Ethane-1,2-diyl)(2-{[1-(2-oxidophenyl)ethylidene-\kO]amino-\kN}ethanolato-\
\kO)silicon
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5798(4)
_cell_length_b                   9.9284(5)
_cell_length_c                   13.7788(6)
_cell_measurement_reflns_used    6464
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      32.05
_cell_measurement_theta_min      2.53
_cell_volume                     1310.53(10)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15312
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.234
_refine_ls_abs_structure_details 'Flack (1983), 1638 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.10(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0336
_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)+(0.0513P)²+0.2422P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                3525
_reflns_number_total             3813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jz3090.cif
_cod_data_source_block           IIo
_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 
;
_cod_database_code               2016272
_cod_database_fobs_code          2016272
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'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Si Si1 0.63018(4) 0.43223(4) 0.07930(3) 0.01239(9) Uani d . 1
O O1 0.70500(11) 0.43835(10) 0.18919(7) 0.0165(2) Uani d . 1
O O2 0.71257(11) 0.37059(9) -0.02158(7) 0.0147(2) Uani d . 1
N N1 0.60081(12) 0.23369(12) 0.11610(9) 0.0143(2) Uani d . 1
C C1 0.72175(16) 0.32158(14) 0.24785(10) 0.0176(3) Uani d . 1
H H1A 0.7157 0.3460 0.3174 0.021 Uiso calc R 1
H H1B 0.8142 0.2803 0.2358 0.021 Uiso calc R 1
C C2 0.60632(16) 0.22264(14) 0.22187(10) 0.0173(3) Uani d . 1
H H2A 0.6304 0.1300 0.2425 0.021 Uiso calc R 1
H H2B 0.5164 0.2490 0.2518 0.021 Uiso calc R 1
C C3 0.57243(14) 0.13512(13) 0.05852(9) 0.0132(3) Uani d . 1
C C4 0.52470(16) -0.00058(14) 0.09407(10) 0.0174(3) Uani d . 1
H H4A 0.5107 0.0028 0.1645 0.026 Uiso calc R 1
H H4B 0.5957 -0.0684 0.0786 0.026 Uiso calc R 1
H H4C 0.4366 -0.0245 0.0623 0.026 Uiso calc R 1
C C5 0.59053(14) 0.15759(13) -0.04634(10) 0.0128(2) Uani d . 1
C C6 0.66265(13) 0.27264(13) -0.08047(10) 0.0127(2) Uani d . 1
C C7 0.68894(16) 0.28678(14) -0.18005(10) 0.0159(3) Uani d . 1
H H7 0.7371 0.3640 -0.2032 0.019 Uiso calc R 1
C C8 0.64512(16) 0.18897(14) -0.24482(10) 0.0182(3) Uani d . 1
H H8 0.6636 0.1997 -0.3121 0.022 Uiso calc R 1
C C9 0.57405(16) 0.07461(16) -0.21233(10) 0.0187(3) Uani d . 1
H H9 0.5445 0.0076 -0.2570 0.022 Uiso calc R 1
C C10 0.54730(15) 0.06039(15) -0.11421(10) 0.0159(3) Uani d . 1
H H10 0.4985 -0.0170 -0.0921 0.019 Uiso calc R 1
C C11 0.66296(15) 0.61671(13) 0.04632(11) 0.0159(3) Uani d . 1
H H11A 0.6566 0.6755 0.1042 0.019 Uiso calc R 1
H H11B 0.7557 0.6286 0.0157 0.019 Uiso calc R 1
C C12 0.54477(16) 0.64652(13) -0.02585(10) 0.0171(3) Uani d . 1
H H12A 0.5626 0.6006 -0.0884 0.021 Uiso calc R 1
H H12B 0.5378 0.7446 -0.0379 0.021 Uiso calc R 1
C C13 0.40912(15) 0.59374(14) 0.02016(11) 0.0178(3) Uani d . 1
H H13A 0.3335 0.5924 -0.0288 0.021 Uiso calc R 1
H H13B 0.3802 0.6535 0.0741 0.021 Uiso calc R 1
C C14 0.43547(15) 0.44991(13) 0.05872(10) 0.0153(3) Uani d . 1
H H14A 0.4030 0.3824 0.0109 0.018 Uiso calc R 1
H H14B 0.3843 0.4357 0.1203 0.018 Uiso calc R 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'
N N 0.0061 0.0033 '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_publ_flag
O1 Si1 O2 123.32(6) y
O1 Si1 C14 123.55(6) y
O2 Si1 C14 111.44(6) y
O1 Si1 C11 96.29(6) y
O2 Si1 C11 94.23(6) y
C14 Si1 C11 92.14(6) y
O1 Si1 N1 82.55(5) y
O2 Si1 N1 85.44(5) y
C14 Si1 N1 89.49(5) y
C11 Si1 N1 178.35(6) y
C1 O1 Si1 122.14(9) ?
C6 O2 Si1 125.50(9) ?
C3 N1 C2 124.33(12) ?
C3 N1 Si1 127.26(10) ?
C2 N1 Si1 108.24(9) ?
O1 C1 C2 108.09(11) ?
O1 C1 H1A 110.1 ?
C2 C1 H1A 110.1 ?
O1 C1 H1B 110.1 ?
C2 C1 H1B 110.1 ?
H1A C1 H1B 108.4 ?
N1 C2 C1 102.25(11) ?
N1 C2 H2A 111.3 ?
C1 C2 H2A 111.3 ?
N1 C2 H2B 111.3 ?
C1 C2 H2B 111.3 ?
H2A C2 H2B 109.2 ?
N1 C3 C5 117.66(12) ?
N1 C3 C4 122.94(12) ?
C5 C3 C4 119.40(11) ?
C3 C4 H4A 109.5 ?
C3 C4 H4B 109.5 ?
H4A C4 H4B 109.5 ?
C3 C4 H4C 109.5 ?
H4A C4 H4C 109.5 ?
H4B C4 H4C 109.5 ?
C10 C5 C6 118.47(12) ?
C10 C5 C3 120.93(12) ?
C6 C5 C3 120.39(12) ?
O2 C6 C7 116.82(11) ?
O2 C6 C5 123.57(12) ?
C7 C6 C5 119.58(12) ?
C8 C7 C6 120.42(13) ?
C8 C7 H7 119.8 ?
C6 C7 H7 119.8 ?
C7 C8 C9 120.75(13) ?
C7 C8 H8 119.6 ?
C9 C8 H8 119.6 ?
C10 C9 C8 119.09(13) ?
C10 C9 H9 120.5 ?
C8 C9 H9 120.5 ?
C9 C10 C5 121.69(13) ?
C9 C10 H10 119.2 ?
C5 C10 H10 119.2 ?
C12 C11 Si1 102.55(9) ?
C12 C11 H11A 111.3 ?
Si1 C11 H11A 111.3 ?
C12 C11 H11B 111.3 ?
Si1 C11 H11B 111.3 ?
H11A C11 H11B 109.2 ?
C11 C12 C13 106.88(11) ?
C11 C12 H12A 110.3 ?
C13 C12 H12A 110.3 ?
C11 C12 H12B 110.3 ?
C13 C12 H12B 110.3 ?
H12A C12 H12B 108.6 ?
C12 C13 C14 108.59(11) ?
C12 C13 H13A 110.0 ?
C14 C13 H13A 110.0 ?
C12 C13 H13B 110.0 ?
C14 C13 H13B 110.0 ?
H13A C13 H13B 108.4 ?
C13 C14 Si1 107.34(9) ?
C13 C14 H14A 110.2 ?
Si1 C14 H14A 110.2 ?
C13 C14 H14B 110.2 ?
Si1 C14 H14B 110.2 ?
H14A C14 H14B 108.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 O1 1.6760(10) y
Si1 O2 1.7120(10) y
Si1 C14 1.895(2) y
Si1 C11 1.9130(10) y
Si1 N1 2.0550(10) y
O1 C1 1.4225(17) ?
O2 C6 1.3539(16) ?
N1 C3 1.2889(18) ?
N1 C2 1.4625(17) ?
C1 C2 1.522(2) ?
C1 H1A 0.9900 ?
C1 H1B 0.9900 ?
C2 H2A 0.9900 ?
C2 H2B 0.9900 ?
C3 C5 1.4723(18) ?
C3 C4 1.5046(19) ?
C4 H4A 0.9800 ?
C4 H4B 0.9800 ?
C4 H4C 0.9800 ?
C5 C10 1.4062(19) ?
C5 C6 1.4154(18) ?
C6 C7 1.4020(19) ?
C7 C8 1.384(2) ?
C7 H7 0.9500 ?
C8 C9 1.398(2) ?
C8 H8 0.9500 ?
C9 C10 1.3832(19) ?
C9 H9 0.9500 ?
C10 H10 0.9500 ?
C11 C12 1.536(2) ?
C11 H11A 0.9900 ?
C11 H11B 0.9900 ?
C12 C13 1.538(2) ?
C12 H12A 0.9900 ?
C12 H12B 0.9900 ?
C13 C14 1.5444(19) ?
C13 H13A 0.9900 ?
C13 H13B 0.9900 ?
C14 H14A 0.9900 ?
C14 H14B 0.9900 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C7 H7 O1 2_664 0.95 2.52 3.424(2) 158.8
C4 H4C O2 4_455 0.98 2.69 3.406(2) 129.9
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
O2 Si1 O1 C1 -75.75(12)
C14 Si1 O1 C1 88.18(12)
C11 Si1 O1 C1 -175.03(11)
N1 Si1 O1 C1 3.77(10)
O1 Si1 O2 C6 125.96(11)
C14 Si1 O2 C6 -39.69(12)
C11 Si1 O2 C6 -133.66(11)
N1 Si1 O2 C6 47.96(11)
O1 Si1 N1 C3 -162.39(13)
O2 Si1 N1 C3 -37.91(12)
C14 Si1 N1 C3 73.65(12)
O1 Si1 N1 C2 22.15(9)
O2 Si1 N1 C2 146.63(10)
C14 Si1 N1 C2 -101.81(10)
Si1 O1 C1 C2 -27.84(15)
C3 N1 C2 C1 145.95(13)
Si1 N1 C2 C1 -38.43(12)
O1 C1 C2 N1 41.34(15)
C2 N1 C3 C5 -171.47(13)
Si1 N1 C3 C5 13.75(18)
C2 N1 C3 C4 7.4(2)
Si1 N1 C3 C4 -167.34(10)
N1 C3 C5 C10 -172.95(13)
C4 C3 C5 C10 8.1(2)
N1 C3 C5 C6 12.43(19)
C4 C3 C5 C6 -166.51(12)
Si1 O2 C6 C7 142.94(10)
Si1 O2 C6 C5 -38.96(17)
C10 C5 C6 O2 -178.04(12)
C3 C5 C6 O2 -3.3(2)
C10 C5 C6 C7 0.01(19)
C3 C5 C6 C7 174.76(12)
O2 C6 C7 C8 178.04(13)
C5 C6 C7 C8 -0.1(2)
C6 C7 C8 C9 0.0(2)
C7 C8 C9 C10 0.3(2)
C8 C9 C10 C5 -0.4(2)
C6 C5 C10 C9 0.3(2)
C3 C5 C10 C9 -174.46(14)
O1 Si1 C11 C12 -153.64(9)
O2 Si1 C11 C12 82.15(10)
C14 Si1 C11 C12 -29.54(10)
Si1 C11 C12 C13 47.92(12)
C11 C12 C13 C14 -47.39(14)
C12 C13 C14 Si1 22.89(13)
O1 Si1 C14 C13 103.25(9)
O2 Si1 C14 C13 -91.13(9)
C11 Si1 C14 C13 4.25(9)
N1 Si1 C14 C13 -176.04(9)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21121427
