#------------------------------------------------------------------------------
#$Date: 2017-03-02 19:20:33 +0200 (Thu, 02 Mar 2017) $
#$Revision: 192782 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/82/4318291.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_4318291
loop_
_publ_author_name
'Ingo Richter'
'Martin Penka'
'Reinhold Tacke'
_publ_contact_author
;
        Reinhold Tacke
        Institut für Anorganische Chemie
        Universität Würzburg
        Am Hubland 
        97074 Würzburg
        Bundesrepublik Deutschland
;
_publ_contact_author_email       r.tacke@mail.uni-wuerzburg.de
_publ_contact_author_fax         '049 931 888-4609'
_publ_contact_author_phone       '049 931 888-5250'
_publ_section_title
;
 The Hexacoordinate Silicate Dianions
 mer-Tris[glycolato(2-)-O1,O2]silicate and
 fac-Tris[benzilato(2-)-O1,O2]silicate: Syntheses and Structural
 Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3950
_journal_page_last               3955
_journal_paper_doi               10.1021/ic025597t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C6 H6 O9 Si(2-); 2 * C4 H10 N O(+)'
_chemical_formula_sum            'C14 H26 N2 O11 Si'
_chemical_formula_weight         426.46
_chemical_melting_point          458
_chemical_name_common
'Morpholinium mer-Tris[glycolato(2-)-O1,O2]silicate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.08(3)
_cell_angle_beta                 106.35(3)
_cell_angle_gamma                98.01(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3934(19)
_cell_length_b                   10.313(2)
_cell_length_c                   10.955(2)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    173(2)
_cell_volume                     950.9(4)
_computing_cell_refinement       'Stoe-IPDS cell'
_computing_data_collection       'Stoe-IPDS expose'
_computing_data_reduction        'Stoe-IPDS integrate'
_computing_molecular_graphics    Bruker-Shelxtl
_computing_publication_material  Bruker-Shextl
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Phi-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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14417
_diffrn_reflns_theta_full        28.16
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0790P)²+0.1352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                3418
_reflns_number_total             4268
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025597t_s2_2.cif
_cod_data_source_block           mer-7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.1352P] where P=(Fo^2^+2Fc^2^)/3' 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^)+(0.0790P)^2^+0.1352P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:
data name '_publ_contact_autor' replaced with '_publ_contact_author'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        951.0(3)
_cod_database_code               4318291
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
Si Si 0.24730(5) 0.59714(4) 0.80135(4) 0.02157(13) Uani 1 d . . .
O1 O 0.19575(15) 0.41388(11) 0.71139(12) 0.0276(3) Uani 1 d . . .
O2 O 0.40808(14) 0.61290(11) 0.75467(11) 0.0251(2) Uani 1 d . . .
O3 O 0.31117(14) 0.77917(11) 0.90629(11) 0.0252(3) Uani 1 d . . .
O4 O 0.32773(15) 0.55792(12) 0.94810(12) 0.0279(3) Uani 1 d . . .
O5 O 0.06781(14) 0.57905(12) 0.83868(11) 0.0267(3) Uani 1 d . . .
O6 O 0.14916(13) 0.64195(11) 0.66390(11) 0.0230(2) Uani 1 d . . .
O7 O 0.28001(19) 0.25036(13) 0.58946(16) 0.0444(4) Uani 1 d . . .
O8 O 0.42882(18) 0.91786(14) 1.11907(13) 0.0401(3) Uani 1 d . . .
O9 O -0.17539(16) 0.58938(15) 0.76236(13) 0.0397(3) Uani 1 d . . .
C1 C 0.2912(2) 0.37164(17) 0.65057(17) 0.0285(4) Uani 1 d . . .
C2 C 0.4154(2) 0.49051(17) 0.66404(19) 0.0314(4) Uani 1 d . . .
H2A H 0.516(3) 0.469(2) 0.694(2) 0.038 Uiso 1 d . . .
H2B H 0.404(3) 0.495(2) 0.573(2) 0.038 Uiso 1 d . . .
C3 C 0.3755(2) 0.80255(17) 1.03439(16) 0.0264(3) Uani 1 d . . .
C4 C 0.3764(2) 0.67012(18) 1.06832(17) 0.0292(4) Uani 1 d . . .
H4A H 0.479(3) 0.674(2) 1.127(2) 0.035 Uiso 1 d . . .
H4B H 0.306(3) 0.661(2) 1.120(2) 0.035 Uiso 1 d . . .
C5 C -0.0468(2) 0.59978(17) 0.75359(16) 0.0274(3) Uani 1 d . . .
C6 C -0.0057(2) 0.6396(2) 0.64394(17) 0.0300(4) Uani 1 d . . .
H6A H -0.075(3) 0.569(2) 0.554(2) 0.036 Uiso 1 d . . .
H6B H -0.025(3) 0.730(2) 0.648(2) 0.036 Uiso 1 d . . .
N1 N 0.36222(19) 0.86411(14) 0.67426(14) 0.0280(3) Uani 1 d . . .
H1N H 0.302(3) 0.784(2) 0.664(2) 0.034 Uiso 1 d . . .
H2N H 0.425(3) 0.907(2) 0.759(2) 0.034 Uiso 1 d . . .
C7 C 0.1769(3) 0.8924(2) 0.48185(19) 0.0381(4) Uani 1 d . . .
H7A H 0.114(3) 0.810(3) 0.466(2) 0.046 Uiso 1 d . . .
H7B H 0.114(3) 0.958(2) 0.451(2) 0.046 Uiso 1 d . . .
C8 C 0.2634(2) 0.95488(19) 0.63137(18) 0.0327(4) Uani 1 d . . .
H8A H 0.195(3) 0.964(2) 0.689(2) 0.039 Uiso 1 d . . .
H8B H 0.325(3) 1.046(2) 0.652(2) 0.039 Uiso 1 d . . .
O10 O 0.27884(17) 0.87110(14) 0.40737(13) 0.0368(3) Uani 1 d . . .
C9 C 0.4641(2) 0.83638(19) 0.59220(19) 0.0322(4) Uani 1 d . . .
H9A H 0.523(3) 0.777(2) 0.623(2) 0.039 Uiso 1 d . . .
H9B H 0.531(3) 0.921(2) 0.611(2) 0.039 Uiso 1 d . . .
C10 C 0.3679(3) 0.7793(2) 0.44436(19) 0.0355(4) Uani 1 d . . .
H10A H 0.301(3) 0.693(2) 0.428(2) 0.043 Uiso 1 d . . .
H10B H 0.434(3) 0.770(2) 0.388(2) 0.043 Uiso 1 d . . .
N2 N 0.17024(17) 0.33262(14) 0.97237(15) 0.0254(3) Uani 1 d . . .
H3N H 0.216(3) 0.410(2) 0.960(2) 0.030 Uiso 1 d . . .
H4N H 0.163(3) 0.360(2) 1.054(2) 0.030 Uiso 1 d . . .
C11 C 0.2723(2) 0.23478(18) 0.96844(19) 0.0300(4) Uani 1 d . . .
H11A H 0.368(3) 0.286(2) 1.048(2) 0.036 Uiso 1 d . . .
H11B H 0.288(3) 0.219(2) 0.879(2) 0.036 Uiso 1 d . . .
C12 C 0.1966(2) 0.10237(19) 0.9804(2) 0.0353(4) Uani 1 d . . .
H12A H 0.185(3) 0.119(2) 1.069(2) 0.042 Uiso 1 d . . .
H12B H 0.256(3) 0.037(2) 0.977(2) 0.042 Uiso 1 d . . .
O11 O 0.05314(16) 0.04011(12) 0.87538(14) 0.0351(3) Uani 1 d . . .
C13 C -0.0468(2) 0.13126(19) 0.8867(2) 0.0322(4) Uani 1 d . . .
H13A H -0.062(3) 0.147(2) 0.970(2) 0.039 Uiso 1 d . . .
H13B H -0.143(3) 0.081(2) 0.813(2) 0.039 Uiso 1 d . . .
C14 C 0.0161(2) 0.26632(19) 0.8705(2) 0.0325(4) Uani 1 d . . .
H14B H 0.027(3) 0.255(2) 0.785(2) 0.039 Uiso 1 d . . .
H14A H -0.052(3) 0.329(2) 0.886(2) 0.039 Uiso 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Si O6 89.68(6) . . y
O2 Si O4 97.26(7) . . y
O6 Si O4 172.66(6) . . y
O2 Si O1 90.00(6) . . y
O6 Si O1 95.09(7) . . y
O4 Si O1 87.34(6) . . y
O2 Si O3 89.52(6) . . y
O6 Si O3 90.46(6) . . y
O4 Si O3 87.22(6) . . y
O1 Si O3 174.43(6) . . y
O2 Si O5 175.90(6) . . y
O6 Si O5 86.47(6) . . y
O4 Si O5 86.65(6) . . y
O1 Si O5 88.95(7) . . y
O3 Si O5 91.91(6) . . y
C1 O1 Si 113.59(12) . . ?
C2 O2 Si 113.65(11) . . ?
C3 O3 Si 115.34(11) . . ?
C4 O4 Si 115.19(10) . . ?
C5 O5 Si 115.43(10) . . ?
C6 O6 Si 116.48(10) . . ?
O7 C1 O1 123.58(18) . . ?
O7 C1 C2 124.03(17) . . ?
O1 C1 C2 112.39(14) . . ?
O2 C2 C1 109.60(15) . . ?
O8 C3 O3 124.37(16) . . ?
O8 C3 C4 123.12(15) . . ?
O3 C3 C4 112.51(14) . . ?
O4 C4 C3 108.58(13) . . ?
O9 C5 O5 123.73(16) . . ?
O9 C5 C6 123.39(16) . . ?
O5 C5 C6 112.88(15) . . ?
O6 C6 C5 108.69(14) . . ?
H1N N1 H2N 113(2) . . ?
H1N N1 C8 108.1(15) . . ?
H2N N1 C8 109.7(13) . . ?
H1N N1 C9 109.3(14) . . ?
H2N N1 C9 105.5(15) . . ?
C8 N1 C9 111.42(13) . . ?
O10 C7 C8 111.01(18) . . ?
N1 C8 C7 109.53(15) . . ?
C10 O10 C7 111.02(14) . . ?
N1 C9 C10 109.03(17) . . ?
O10 C10 C9 111.35(15) . . ?
H4N N2 H3N 106.8(19) . . ?
H4N N2 C14 109.6(15) . . ?
H3N N2 C14 112.1(14) . . ?
H4N N2 C11 109.0(13) . . ?
H3N N2 C11 108.0(13) . . ?
C14 N2 C11 111.26(14) . . ?
N2 C11 C12 109.55(15) . . ?
O11 C12 C11 111.07(15) . . ?
C13 O11 C12 109.48(14) . . ?
O11 C13 C14 110.94(16) . . ?
N2 C14 C13 109.88(14) . . ?
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
Si O2 1.7266(13) . y
Si O6 1.7474(12) . y
Si O4 1.7552(13) . y
Si O1 1.7950(14) . y
Si O3 1.8188(14) . y
Si O5 1.8406(13) . y
O1 C1 1.312(2) . ?
O2 C2 1.397(2) . ?
O3 C3 1.299(2) . ?
O4 C4 1.397(2) . ?
O5 C5 1.297(2) . ?
O6 C6 1.405(2) . ?
O7 C1 1.218(2) . ?
O8 C3 1.219(2) . ?
O9 C5 1.231(2) . ?
C1 C2 1.513(3) . ?
C3 C4 1.512(2) . ?
C5 C6 1.500(2) . ?
N1 H1N 0.89(2) . ?
N1 H2N 0.90(2) . ?
N1 C8 1.483(2) . ?
N1 C9 1.491(2) . ?
C7 O10 1.424(2) . ?
C7 C8 1.510(3) . ?
O10 C10 1.416(2) . ?
C9 C10 1.512(3) . ?
N2 H4N 0.89(2) . ?
N2 H3N 0.92(2) . ?
N2 C14 1.483(3) . ?
N2 C11 1.486(2) . ?
C11 C12 1.506(3) . ?
C12 O11 1.425(3) . ?
O11 C13 1.424(2) . ?
C13 C14 1.512(2) . ?
