#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:04:14 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178932 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/61/4116127.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_4116127
loop_
_publ_author_name
'Reinhold Tacke'
'Christian Burschka'
'Ingo Richter'
'Brigitte Wagner'
'Reiner Willeke'
_publ_contact_author
;       Reinhold Tacke
    Institut für Anorganische Chemie
    Bayerische Julius-Maximilians-Universität Würzburg
    Am Hubland
    D-97074 Würzburg
    Bundesrepublik Deutschland
;
_publ_contact_author_email       r.tacke@mail.uni-wuerzburg.de
_publ_contact_author_fax         '049 931 8884609'
_publ_contact_author_phone       '049 931 8885250'
_publ_section_title
;
 Pentacoordinate Silicon Compounds with SiO5Skeletons Containing SiOH or
 SiOSi Groups: Derivatives of the Pentahydroxosilicate(1-) Anion
 [Si(OH)5]-and Its Anhydride [(HO)4Si-O-Si(OH)4]2-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8480
_journal_page_last               8485
_journal_paper_doi               10.1021/ja000637i
_journal_volume                  122
_journal_year                    2000
_chemical_formula_moiety         '(C28 H21 O7 Si), (C6 H8 N), (C4 H8 O) '
_chemical_formula_sum            'C38 H37 N O8 Si'
_chemical_formula_weight         663.78
_chemical_melting_point          472
_chemical_name_systematic
'Anilinium Bis[benzilato(2-)-O1,O2]hydroxosilicate-Tetrahydrofuran'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 91.155(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3633(14)
_cell_length_b                   12.5129(13)
_cell_length_c                   11.8372(14)
_cell_measurement_reflns_used    2750
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      4.95
_cell_volume                     1682.8(3)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Stoe-IPDS
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10398
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       platelet
_exptl_crystal_F_000             700
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0413
_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)+(0.0617P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                3455
_reflns_number_total             4114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja000637i_3.cif
_cod_data_source_block           ricabul
_cod_database_code               4116127
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, 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
Si Si -0.38765(9) -0.67920(9) -0.98345(8) 0.0225(3) Uani 1 1 d . . .
C1 C -0.3952(3) -0.4894(4) -0.8863(3) 0.0254(10) Uani 1 1 d . . .
C2 C -0.3739(3) -0.5718(3) -0.7910(3) 0.0249(9) Uani 1 1 d . . .
C3 C -0.2779(3) -0.8559(4) -1.0445(3) 0.0244(9) Uani 1 1 d . . .
C4 C -0.2189(3) -0.7632(3) -1.1083(3) 0.0239(9) Uani 1 1 d . . .
C5 C -0.2553(3) -0.5482(3) -0.7332(3) 0.0273(10) Uani 1 1 d . . .
C6 C -0.2396(4) -0.4571(4) -0.6652(3) 0.0382(11) Uani 1 1 d . . .
H6 H -0.3035 -0.4097 -0.6532 0.046 Uiso 1 1 calc R . .
C7 C -0.1295(5) -0.4366(4) -0.6155(4) 0.0477(13) Uani 1 1 d . . .
H7 H -0.1193 -0.3757 -0.5684 0.057 Uiso 1 1 calc R . .
C8 C -0.0357(5) -0.5032(5) -0.6336(4) 0.0513(14) Uani 1 1 d . . .
H8 H 0.0389 -0.4882 -0.5995 0.062 Uiso 1 1 calc R . .
C9 C -0.0501(4) -0.5909(4) -0.7007(4) 0.0459(13) Uani 1 1 d . . .
H9 H 0.0150 -0.6365 -0.7141 0.055 Uiso 1 1 calc R . .
C10 C -0.1589(4) -0.6141(4) -0.7495(3) 0.0344(10) Uani 1 1 d . . .
H10 H -0.1677 -0.6762 -0.7950 0.041 Uiso 1 1 calc R . .
C11 C -0.4793(3) -0.5708(3) -0.7121(3) 0.0257(10) Uani 1 1 d . . .
C12 C -0.4675(4) -0.5852(4) -0.5956(3) 0.0366(11) Uani 1 1 d . . .
H12 H -0.3913 -0.5926 -0.5620 0.044 Uiso 1 1 calc R . .
C13 C -0.5666(4) -0.5889(4) -0.5283(4) 0.0506(14) Uani 1 1 d . . .
H13 H -0.5579 -0.5970 -0.4488 0.061 Uiso 1 1 calc R . .
C14 C -0.6778(4) -0.5808(4) -0.5777(4) 0.0457(13) Uani 1 1 d . . .
H14 H -0.7455 -0.5838 -0.5320 0.055 Uiso 1 1 calc R . .
C15 C -0.6901(4) -0.5685(4) -0.6920(4) 0.0421(12) Uani 1 1 d . . .
H15 H -0.7665 -0.5630 -0.7257 0.051 Uiso 1 1 calc R . .
C16 C -0.5912(4) -0.5641(3) -0.7593(4) 0.0320(10) Uani 1 1 d . . .
H16 H -0.6007 -0.5564 -0.8388 0.038 Uiso 1 1 calc R . .
C17 C -0.2405(4) -0.7749(3) -1.2358(3) 0.0268(10) Uani 1 1 d . . .
C18 C -0.1524(4) -0.7539(4) -1.3125(3) 0.0401(11) Uani 1 1 d . . .
H18 H -0.0752 -0.7367 -1.2861 0.048 Uiso 1 1 calc R . .
C19 C -0.1776(5) -0.7582(4) -1.4280(4) 0.0513(14) Uani 1 1 d . . .
H19 H -0.1174 -0.7427 -1.4800 0.062 Uiso 1 1 calc R . .
C20 C -0.2880(5) -0.7844(4) -1.4677(4) 0.0473(13) Uani 1 1 d . . .
H20 H -0.3039 -0.7878 -1.5467 0.057 Uiso 1 1 calc R . .
C21 C -0.3751(4) -0.8057(4) -1.3927(4) 0.0430(12) Uani 1 1 d . . .
H21 H -0.4517 -0.8238 -1.4199 0.052 Uiso 1 1 calc R . .
C22 C -0.3520(4) -0.8009(3) -1.2770(3) 0.0339(11) Uani 1 1 d . . .
H22 H -0.4132 -0.8156 -1.2257 0.041 Uiso 1 1 calc R . .
C23 C -0.0894(3) -0.7579(4) -1.0733(3) 0.0275(10) Uani 1 1 d . . .
C24 C -0.0403(4) -0.6665(4) -1.0297(3) 0.0391(11) Uani 1 1 d . . .
H24 H -0.0887 -0.6054 -1.0197 0.047 Uiso 1 1 calc R . .
C25 C 0.0792(4) -0.6608(5) -0.9995(4) 0.0481(14) Uani 1 1 d . . .
H25 H 0.1113 -0.5964 -0.9695 0.058 Uiso 1 1 calc R . .
C26 C 0.1502(4) -0.7489(5) -1.0134(4) 0.0505(13) Uani 1 1 d . . .
H26 H 0.2312 -0.7461 -0.9924 0.061 Uiso 1 1 calc R . .
C27 C 0.1019(4) -0.8416(5) -1.0584(4) 0.0494(14) Uani 1 1 d . . .
H27 H 0.1501 -0.9026 -1.0688 0.059 Uiso 1 1 calc R . .
C28 C -0.0158(4) -0.8454(4) -1.0882(4) 0.0389(11) Uani 1 1 d . . .
H28 H -0.0475 -0.9094 -1.1196 0.047 Uiso 1 1 calc R . .
C29 C -0.2970(3) -1.0241(3) -0.7795(3) 0.0268(10) Uani 1 1 d . . .
C30 C -0.2596(4) -1.1248(4) -0.7514(3) 0.0361(11) Uani 1 1 d . . .
H30 H -0.3054 -1.1853 -0.7731 0.043 Uiso 1 1 calc R . .
C31 C -0.1548(4) -1.1383(4) -0.6912(4) 0.0427(13) Uani 1 1 d . . .
H31 H -0.1281 -1.2080 -0.6717 0.051 Uiso 1 1 calc R . .
C32 C -0.0899(4) -1.0506(5) -0.6599(4) 0.0486(13) Uani 1 1 d . . .
H32 H -0.0181 -1.0600 -0.6187 0.058 Uiso 1 1 calc R . .
C33 C -0.1273(4) -0.9483(5) -0.6874(4) 0.0489(13) Uani 1 1 d . . .
H33 H -0.0820 -0.8881 -0.6644 0.059 Uiso 1 1 calc R . .
C34 C -0.2323(4) -0.9347(4) -0.7491(3) 0.0389(11) Uani 1 1 d . . .
H34 H -0.2588 -0.8652 -0.7697 0.047 Uiso 1 1 calc R . .
O8 O -0.4244(5) -0.4447(4) -0.3052(5) 0.0669(8) Uiso 0.738(8) 1 d PD A 1
C39 C -0.3207(5) -0.5078(5) -0.3122(5) 0.0669(8) Uiso 0.738(8) 1 d PD A 1
H39A H -0.2972 -0.5159 -0.3918 0.080 Uiso 0.738(8) 1 calc PR A 1
H39B H -0.3335 -0.5796 -0.2796 0.080 Uiso 0.738(8) 1 calc PR A 1
C40 C -0.2277(7) -0.4476(6) -0.2450(8) 0.0669(8) Uiso 0.738(8) 1 d PD A 1
H40A H -0.2374 -0.4578 -0.1627 0.080 Uiso 0.738(8) 1 calc PR A 1
H40B H -0.1476 -0.4703 -0.2657 0.080 Uiso 0.738(8) 1 calc PR A 1
C37 C -0.2498(5) -0.3386(5) -0.2775(5) 0.0669(8) Uiso 0.738(8) 1 d PD A 1
H37A H -0.2132 -0.3217 -0.3506 0.080 Uiso 0.738(8) 1 calc PR A 1
H37B H -0.2199 -0.2881 -0.2192 0.080 Uiso 0.738(8) 1 calc PR A 1
C38 C -0.3877(6) -0.3346(6) -0.2878(7) 0.0669(8) Uiso 0.738(8) 1 d PD A 1
H38A H -0.4217 -0.3054 -0.2179 0.080 Uiso 0.738(8) 1 calc PR A 1
H38B H -0.4131 -0.2894 -0.3524 0.080 Uiso 0.738(8) 1 calc PR A 1
O9 O -0.4176(6) -0.4392(6) -0.2769(7) 0.0669(8) Uiso 0.262(8) 1 d PRD A 2
C52 C -0.3558(15) -0.3528(16) -0.2122(18) 0.0669(8) Uiso 0.262(8) 1 d PD A 2
H52A H -0.4034 -0.2865 -0.2106 0.080 Uiso 0.262(8) 1 calc PR A 2
H52B H -0.3368 -0.3754 -0.1338 0.080 Uiso 0.262(8) 1 calc PR A 2
C56 C -0.2498(5) -0.3386(5) -0.2775(5) 0.0669(8) Uiso 0.262(8) 1 d PD A 2
H56A H -0.2671 -0.2965 -0.3467 0.080 Uiso 0.262(8) 1 calc PR A 2
H56B H -0.1884 -0.3010 -0.2322 0.080 Uiso 0.262(8) 1 calc PR A 2
C55 C -0.2117(12) -0.4449(13) -0.306(2) 0.0669(8) Uiso 0.262(8) 1 d PD A 2
H55A H -0.1572 -0.4735 -0.2470 0.080 Uiso 0.262(8) 1 calc PR A 2
H55B H -0.1715 -0.4453 -0.3794 0.080 Uiso 0.262(8) 1 calc PR A 2
C54 C -0.3207(5) -0.5078(5) -0.3122(5) 0.0669(8) Uiso 0.262(8) 1 d PD A 2
H54A H -0.3352 -0.5332 -0.3905 0.080 Uiso 0.262(8) 1 calc PR A 2
H54B H -0.3142 -0.5708 -0.2619 0.080 Uiso 0.262(8) 1 calc PR A 2
N N -0.4052(3) -1.0099(3) -0.8437(3) 0.0339(9) Uani 1 1 d . . .
H42 H -0.3962 -0.9563 -0.8947 0.051 Uiso 1 1 calc R . .
H43 H -0.4643 -0.9930 -0.7961 0.051 Uiso 1 1 calc R . .
H44 H -0.4234 -1.0716 -0.8808 0.051 Uiso 1 1 calc R . .
O1 O -0.4037(2) -0.5362(2) -0.9853(2) 0.0249(7) Uani 1 1 d . . .
O2 O -0.3692(2) -0.6737(2) -0.84425(19) 0.0245(6) Uani 1 1 d . . .
O3 O -0.3608(2) -0.8207(2) -0.9778(2) 0.0244(7) Uani 1 1 d . . .
O4 O -0.2777(2) -0.6684(2) -1.07301(19) 0.0253(6) Uani 1 1 d . . .
O5 O -0.5218(2) -0.6933(2) -1.0373(2) 0.0290(7) Uani 1 1 d . . .
H1 H -0.535(4) -0.754(4) -1.042(4) 0.035 Uiso 1 1 d . . .
O6 O -0.4033(2) -0.3933(2) -0.8711(2) 0.0264(7) Uani 1 1 d . . .
O7 O -0.2538(2) -0.9493(2) -1.0547(2) 0.0295(7) 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'
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
O5 Si O2 119.05(14) y
O5 Si O4 117.61(14) y
O2 Si O4 123.32(13) y
O5 Si O3 93.66(15) y
O2 Si O3 89.19(14) y
O4 Si O3 88.58(13) y
O5 Si O1 90.51(15) y
O2 Si O1 88.94(14) y
O4 Si O1 89.34(13) y
O3 Si O1 175.83(14) y
O6 C1 O1 124.5(4) ?
O6 C1 C2 124.2(4) ?
O1 C1 C2 111.3(4) ?
O2 C2 C5 109.3(3) ?
O2 C2 C11 108.3(3) ?
C5 C2 C11 114.7(3) ?
O2 C2 C1 106.3(3) ?
C5 C2 C1 108.8(3) ?
C11 C2 C1 109.1(3) ?
O7 C3 O3 123.4(4) ?
O7 C3 C4 125.2(3) ?
O3 C3 C4 111.4(4) ?
O4 C4 C23 109.8(3) ?
O4 C4 C17 107.5(3) ?
C23 C4 C17 114.0(3) ?
O4 C4 C3 105.7(3) ?
C23 C4 C3 109.1(3) ?
C17 C4 C3 110.4(3) ?
C10 C5 C6 118.1(4) ?
C10 C5 C2 121.0(4) ?
C6 C5 C2 120.9(4) ?
C7 C6 C5 119.5(4) ?
C8 C7 C6 121.0(5) ?
C9 C8 C7 119.7(5) ?
C8 C9 C10 120.5(5) ?
C9 C10 C5 121.2(4) ?
C16 C11 C12 118.5(4) ?
C16 C11 C2 118.5(3) ?
C12 C11 C2 122.7(4) ?
C11 C12 C13 120.5(4) ?
C14 C13 C12 119.8(4) ?
C15 C14 C13 120.0(4) ?
C14 C15 C16 120.2(5) ?
C11 C16 C15 120.9(4) ?
C22 C17 C18 118.7(4) ?
C22 C17 C4 119.7(3) ?
C18 C17 C4 121.5(4) ?
C17 C18 C19 119.8(4) ?
C20 C19 C18 121.0(4) ?
C21 C20 C19 119.5(4) ?
C20 C21 C22 120.4(5) ?
C17 C22 C21 120.6(4) ?
C24 C23 C28 117.7(4) ?
C24 C23 C4 121.5(4) ?
C28 C23 C4 120.7(4) ?
C23 C24 C25 121.6(5) ?
C26 C25 C24 119.7(5) ?
C25 C26 C27 119.2(4) ?
C28 C27 C26 120.2(5) ?
C27 C28 C23 121.5(5) ?
C30 C29 C34 121.4(4) ?
C30 C29 N 119.8(4) ?
C34 C29 N 118.7(4) ?
C29 C30 C31 119.7(4) ?
C32 C31 C30 119.6(5) ?
C31 C32 C33 121.1(4) ?
C32 C33 C34 119.4(5) ?
C29 C34 C33 118.7(5) ?
C39 O8 C38 107.4(5) ?
O8 C39 C40 105.3(5) ?
C37 C40 C39 102.4(6) ?
C40 C37 C38 102.7(5) ?
O8 C38 C37 105.3(5) ?
C1 O1 Si 115.3(3) ?
C2 O2 Si 118.2(2) ?
C3 O3 Si 115.4(3) ?
C4 O4 Si 118.7(2) ?
H1 O5 Si 108(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Si O5 1.650(3) y
Si O2 1.658(2) y
Si O4 1.660(2) y
Si O3 1.798(3) y
Si O1 1.798(3) y
C1 O6 1.220(5) ?
C1 O1 1.312(5) ?
C1 C2 1.543(6) ?
C2 O2 1.424(5) ?
C2 C5 1.528(6) ?
C2 C11 1.534(5) ?
C3 O7 1.207(5) ?
C3 O3 1.317(5) ?
C3 C4 1.544(6) ?
C4 O4 1.429(5) ?
C4 C23 1.523(5) ?
C4 C17 1.532(5) ?
C5 C10 1.388(6) ?
C5 C6 1.405(6) ?
C6 C7 1.396(7) ?
C7 C8 1.373(8) ?
C8 C9 1.363(7) ?
C9 C10 1.385(6) ?
C11 C16 1.381(6) ?
C11 C12 1.393(6) ?
C12 C13 1.394(6) ?
C13 C14 1.386(7) ?
C14 C15 1.366(7) ?
C15 C16 1.392(6) ?
C17 C22 1.387(6) ?
C17 C18 1.390(6) ?
C18 C19 1.392(6) ?
C19 C20 1.370(7) ?
C20 C21 1.369(7) ?
C21 C22 1.390(6) ?
C23 C24 1.369(6) ?
C23 C28 1.390(6) ?
C24 C25 1.400(6) ?
C25 C26 1.378(8) ?
C26 C27 1.385(8) ?
C27 C28 1.377(7) ?
C29 C30 1.369(6) ?
C29 C34 1.382(6) ?
C29 N 1.444(5) ?
C30 C31 1.387(7) ?
C31 C32 1.369(7) ?
C32 C33 1.385(8) ?
C33 C34 1.397(7) ?
O8 C39 1.421(7) ?
O8 C38 1.453(9) ?
C39 C40 1.511(9) ?
C40 C37 1.438(10) ?
C37 C38 1.569(8) ?
O9 C52 1.493(14) ?
O5 H1 0.78(5) ?
