#------------------------------------------------------------------------------
#$Date: 2015-09-08 16:41:49 +0300 (Tue, 08 Sep 2015) $
#$Revision: 155249 $
#$URL: svn://www.crystallography.net/cod/cif/1/52/39/1523946.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_1523946
loop_
_publ_author_name
'Kaßner, L.'
'Nagel, K.'
'Grützner, R.-E.'
'Korb, M.'
'Rüffer, T.'
'Lang, H.'
'Spange, S.'
_publ_section_title
;
 Polyamide 6/silica hybrid materials by a coupled polymerization reaction
;
_journal_issue                   35
_journal_name_full               'Polym. Chem.'
_journal_page_first              6297
_journal_paper_doi               10.1039/C5PY00815H
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C24 H40 N4 O4 Si'
_chemical_formula_sum            'C24 H40 N4 O4 Si'
_chemical_formula_weight         476.69
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-04-07 deposited with the CCDC.
2015-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9688(3)
_cell_length_b                   13.9688(3)
_cell_length_c                   13.3347(4)
_cell_measurement_reflns_used    2460
_cell_measurement_temperature    110
_cell_measurement_theta_max      28.5752
_cell_measurement_theta_min      3.0491
_cell_volume                     2601.96(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3191
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.602
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.131
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 427 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.35(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0344P)²+0.6068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.700
_reflns_friedel_fraction_full    0.914
_reflns_friedel_fraction_max     0.914
_reflns_number_gt                1060
_reflns_number_total             1107
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5py00815h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 1523945--1523946.cif.'
_cod_original_cell_volume        2601.97(14)
_cod_database_code               1523946
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Si1 Si 1.5000 1.0000 1.2500 0.0204(3) Uani 1 4 d S T P
O1 O 1.46927(9) 1.09118(10) 1.18015(9) 0.0243(4) Uani 1 1 d . . .
N2 N 1.55231(12) 1.11749(12) 1.11965(13) 0.0264(4) Uani 1 1 d . . .
C6 C 1.42856(15) 1.18268(14) 1.00361(15) 0.0263(5) Uani 1 1 d . . .
H6A H 1.4138 1.2498 1.0143 0.032 Uiso 1 1 calc R U .
H6B H 1.3829 1.1449 1.0415 0.032 Uiso 1 1 calc R U .
C2 C 1.60943(15) 1.19822(16) 0.97722(15) 0.0312(5) Uani 1 1 d . . .
H2A H 1.6689 1.1707 1.0014 0.037 Uiso 1 1 calc R U .
H2B H 1.6139 1.2672 0.9839 0.037 Uiso 1 1 calc R U .
C1 C 1.52785(14) 1.16211(14) 1.04030(15) 0.0245(5) Uani 1 1 d . . .
C4 C 1.4985(2) 1.20564(19) 0.83059(15) 0.0419(6) Uani 1 1 d . . .
H4A H 1.4909 1.1889 0.7604 0.050 Uiso 1 1 calc R U .
H4B H 1.4939 1.2747 0.8365 0.050 Uiso 1 1 calc R U .
C3 C 1.59637(17) 1.17266(17) 0.86718(17) 0.0388(6) Uani 1 1 d . . .
H3A H 1.6021 1.1039 0.8587 0.047 Uiso 1 1 calc R U .
H3B H 1.6461 1.2031 0.8276 0.047 Uiso 1 1 calc R U .
C5 C 1.41922(18) 1.15893(19) 0.89183(18) 0.0401(6) Uani 1 1 d . . .
H5A H 1.4219 1.0901 0.8829 0.048 Uiso 1 1 calc R U .
H5B H 1.3576 1.1810 0.8676 0.048 Uiso 1 1 calc R U .
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
O1 Si1 O1 108.93(4) . 11_577
O1 Si1 O1 110.56(9) . 2_875
O1 Si1 O1 108.93(4) 11_577 2_875
O1 Si1 O1 108.93(4) . 12_747
O1 Si1 O1 110.56(9) 11_577 12_747
O1 Si1 O1 108.93(4) 2_875 12_747
N2 O1 Si1 107.59(10) . .
C1 N2 O1 111.64(15) . .
C1 C6 C5 110.78(18) . .
C1 C6 H6A 109.5 . .
C5 C6 H6A 109.5 . .
C1 C6 H6B 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 108.1 . .
C1 C2 C3 111.71(18) . .
C1 C2 H2A 109.3 . .
C3 C2 H2A 109.3 . .
C1 C2 H2B 109.3 . .
C3 C2 H2B 109.3 . .
H2A C2 H2B 107.9 . .
N2 C1 C6 127.80(18) . .
N2 C1 C2 115.16(17) . .
C6 C1 C2 117.04(16) . .
C3 C4 C5 110.58(19) . .
C3 C4 H4A 109.5 . .
C5 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
C5 C4 H4B 109.5 . .
H4A C4 H4B 108.1 . .
C2 C3 C4 110.23(18) . .
C2 C3 H3A 109.6 . .
C4 C3 H3A 109.6 . .
C2 C3 H3B 109.6 . .
C4 C3 H3B 109.6 . .
H3A C3 H3B 108.1 . .
C4 C5 C6 111.52(19) . .
C4 C5 H5A 109.3 . .
C6 C5 H5A 109.3 . .
C4 C5 H5B 109.3 . .
C6 C5 H5B 109.3 . .
H5A C5 H5B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O1 1.6353(13) .
Si1 O1 1.6353(13) 11_577
Si1 O1 1.6353(13) 2_875
Si1 O1 1.6353(13) 12_747
O1 N2 1.460(2) .
N2 C1 1.275(3) .
C6 C1 1.498(3) .
C6 C5 1.533(3) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C2 C1 1.504(3) .
C2 C3 1.521(3) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C4 C3 1.523(3) .
C4 C5 1.523(3) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
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
O1 Si1 O1 N2 58.71(8) 11_577
O1 Si1 O1 N2 -60.95(9) 2_875
O1 Si1 O1 N2 179.38(11) 12_747
Si1 O1 N2 C1 156.50(14) .
O1 N2 C1 C6 -4.0(3) .
O1 N2 C1 C2 175.75(16) .
C5 C6 C1 N2 -133.3(2) .
C5 C6 C1 C2 47.0(2) .
C3 C2 C1 N2 131.8(2) .
C3 C2 C1 C6 -48.4(2) .
C1 C2 C3 C4 52.8(2) .
C5 C4 C3 C2 -59.1(3) .
C3 C4 C5 C6 58.8(3) .
C1 C6 C5 C4 -51.1(3) .
