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#$Date: 2016-03-23 16:05:01 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179361 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/58/4325811.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_4325811
loop_
_publ_author_name
'Thomas Deschner'
'Karl Wilhelm Törnroos'
'Reiner Anwander'
_publ_contact_author_address
;
       Department of Chemistry,
       University of Bergen,
       Allegaten 41,
       N-5007 Bergen,
       Norway.
;
_publ_contact_author_email       karl.tornroos@kj.uib.no
_publ_contact_author_fax         '+47 55 58 3552'
_publ_contact_author_name
;
       Prof. Karl Wilhelm Törnroos
;
_publ_contact_author_phone       '+47 55 58 9490'
_publ_section_title
;
 Iron Silylamide-Grafted Periodic Mesoporous Silica
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7217
_journal_page_last               7228
_journal_paper_doi               10.1021/ic200788f
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C16 H56 Fe2 N4 Si8'
_chemical_formula_sum            'C16 H56 Fe2 N4 Si8'
_chemical_formula_weight         641.07
_chemical_name_systematic
; 
 ? 
;
_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                92.662(2)
_cell_angle_beta                 104.056(2)
_cell_angle_gamma                110.779(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7407(10)
_cell_length_b                   9.6694(11)
_cell_length_c                   11.8888(14)
_cell_measurement_reflns_used    10561
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.27
_cell_volume                     901.53(18)
_computing_cell_refinement
;
Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_data_collection
;
Bruker (1999). SMART, version 5.054, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_data_reduction
;
Bruker (2004). SAINT, version 6.45a, Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_molecular_graphics
;
Farrugia, L. J. (1999). ORTEP3 for Windows. Version 1.05. University 
of Glasgow, Scotland.
;
_computing_publication_material
;
Bruker AXS (2003). SHELXTL. Version 6.14. Bruker AXS Inc., Madison, 
Wisconsin, USA.
;
_computing_structure_refinement
;
Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122.
;
_computing_structure_solution
;     
Sheldrick, G. M. (2008). Acta Crystallographica, A64, 112-122.
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean '48 \um'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-AXS SMART 2K CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13242
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 1
_diffrn_standards_interval_time  28h
_diffrn_standards_number         313
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.710706
_exptl_absorpt_correction_T_min  0.710706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker AXS (2003). SHELXTL. Version 6.14. 
Bruker AXS Inc., Madison, Wisconsin, USA. 
;
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       'flat prism'
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.785
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4472
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0489
_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)+(0.1015P)²+0.2886P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                4042
_reflns_number_total             4472
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic200788f_si_002.cif
_cod_data_source_block           Compound9
_cod_database_code               4325811
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.07856(3) 0.07101(3) 0.10953(2) 0.01907(12) Uani 1 1 d .
Si1 Si 0.16306(9) 0.34658(7) 0.28879(5) 0.03113(17) Uani 1 1 d D
HI1 H 0.032(3) 0.350(3) 0.1859(16) 0.037 Uiso 1 1 d D
Si2 Si 0.33603(9) 0.12422(8) 0.35116(6) 0.03420(18) Uani 1 1 d D
HI2 H 0.310(4) -0.0208(17) 0.289(3) 0.041 Uiso 1 1 d D
Si3 Si -0.31553(7) -0.10767(6) 0.04564(5) 0.02305(15) Uani 1 1 d D
HI3 H -0.339(3) -0.004(2) -0.0377(19) 0.028 Uiso 1 1 d D
Si4 Si -0.09677(7) -0.29150(6) 0.08716(5) 0.02483(16) Uani 1 1 d D
HI4 H -0.227(2) -0.410(2) -0.0048(18) 0.030 Uiso 1 1 d D
N1 N 0.1978(2) 0.1865(2) 0.26012(16) 0.0261(4) Uani 1 1 d .
N2 N -0.1203(2) -0.12516(18) 0.04803(14) 0.0195(3) Uani 1 1 d .
C1 C 0.0829(5) 0.3540(4) 0.4199(3) 0.0547(8) Uani 1 1 d .
H1A H -0.0158 0.2619 0.4139 0.089(15) Uiso 1 1 calc R
H1B H 0.0492 0.4402 0.4237 0.083(14) Uiso 1 1 calc R
H1C H 0.1731 0.3636 0.4909 0.070(12) Uiso 1 1 calc R
C2 C 0.3559(4) 0.5200(3) 0.3053(3) 0.0533(8) Uani 1 1 d .
H2A H 0.3913 0.5237 0.2330 0.102(18) Uiso 1 1 calc R
H2B H 0.4485 0.5194 0.3709 0.080(14) Uiso 1 1 calc R
H2C H 0.3289 0.6079 0.3208 0.083(14) Uiso 1 1 calc R
C3 C 0.2945(6) 0.0953(5) 0.4956(3) 0.0648(10) Uani 1 1 d .
H3A H 0.1780 0.0234 0.4841 0.057(11) Uiso 1 1 calc R
H3B H 0.3082 0.1907 0.5373 0.071(13) Uiso 1 1 calc R
H3C H 0.3753 0.0565 0.5419 0.079(13) Uiso 1 1 calc R
C4 C 0.5648(4) 0.2500(4) 0.3776(4) 0.0590(9) Uani 1 1 d .
H4A H 0.5924 0.2603 0.3026 0.108(19) Uiso 1 1 calc R
H4B H 0.6378 0.2069 0.4275 0.13(2) Uiso 1 1 calc R
H4C H 0.5838 0.3486 0.4167 0.079(14) Uiso 1 1 calc R
C5 C -0.4983(3) -0.2867(3) -0.0162(3) 0.0451(7) Uani 1 1 d .
H5A H -0.4877 -0.3276 -0.0896 0.064(11) Uiso 1 1 calc R
H5B H -0.6048 -0.2691 -0.0316 0.073(12) Uiso 1 1 calc R
H5C H -0.4991 -0.3579 0.0399 0.072(13) Uiso 1 1 calc R
C6 C -0.3157(4) -0.0328(4) 0.1920(3) 0.0497(7) Uani 1 1 d .
H6A H -0.2316 0.0699 0.2151 0.081(14) Uiso 1 1 calc R
H6B H -0.2866 -0.0953 0.2496 0.12(2) Uiso 1 1 calc R
H6C H -0.4291 -0.0335 0.1888 0.070(12) Uiso 1 1 calc R
C7 C 0.1152(3) -0.2913(3) 0.0852(2) 0.0297(4) Uani 1 1 d .
H7A H 0.1337 -0.2713 0.0086 0.047(9) Uiso 1 1 calc R
H7B H 0.1194 -0.3890 0.0996 0.069(12) Uiso 1 1 calc R
H7C H 0.2041 -0.2134 0.1465 0.036(8) Uiso 1 1 calc R
C8 C -0.1299(5) -0.3251(4) 0.2335(3) 0.0491(7) Uani 1 1 d .
H8A H -0.2451 -0.3329 0.2327 0.077(13) Uiso 1 1 calc R
H8B H -0.0461 -0.2418 0.2928 0.061(11) Uiso 1 1 calc R
H8C H -0.1160 -0.4184 0.2522 0.066(12) Uiso 1 1 calc R
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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
N1 Fe1 N2 134.96(7) . .
N1 Fe1 N2 127.18(7) . 2
N2 Fe1 N2 97.82(6) . 2
N1 Fe1 Fe1 175.33(6) . 2
N2 Fe1 Fe1 49.45(5) . 2
N2 Fe1 Fe1 48.37(5) 2 2
N1 Si1 C1 114.11(13) . .
N1 Si1 C2 112.78(13) . .
C1 Si1 C2 108.50(17) . .
N1 Si1 HI1 106.2(12) . .
C1 Si1 HI1 107.7(12) . .
C2 Si1 HI1 107.1(12) . .
N1 Si2 C3 113.86(14) . .
N1 Si2 C4 113.11(14) . .
C3 Si2 C4 107.9(2) . .
N1 Si2 HI2 104.9(13) . .
C3 Si2 HI2 108.6(13) . .
C4 Si2 HI2 108.2(12) . .
N2 Si3 C6 111.91(11) . .
N2 Si3 C5 111.31(11) . .
C6 Si3 C5 111.88(15) . .
N2 Si3 HI3 107.1(10) . .
C6 Si3 HI3 109.5(11) . .
C5 Si3 HI3 104.8(11) . .
N2 Si4 C8 111.78(11) . .
N2 Si4 C7 111.77(9) . .
C8 Si4 C7 109.46(13) . .
N2 Si4 HI4 104.9(11) . .
C8 Si4 HI4 110.8(11) . .
C7 Si4 HI4 108.0(11) . .
Si2 N1 Si1 126.49(11) . .
Si2 N1 Fe1 116.67(10) . .
Si1 N1 Fe1 116.77(10) . .
Si4 N2 Si3 117.43(9) . .
Si4 N2 Fe1 118.93(9) . .
Si3 N2 Fe1 111.57(9) . .
Si4 N2 Fe1 115.72(9) . 2
Si3 N2 Fe1 105.11(8) . 2
Fe1 N2 Fe1 82.18(6) . 2
Si1 C1 H1A 109.5 . .
Si1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Si1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Si1 C2 H2A 109.5 . .
Si1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Si1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
Si2 C3 H3A 109.5 . .
Si2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Si2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
Si2 C4 H4A 109.5 . .
Si2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Si3 C5 H5A 109.5 . .
Si3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
Si3 C6 H6A 109.5 . .
Si3 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si3 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Si4 C7 H7A 109.5 . .
Si4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Si4 C8 H8A 109.5 . .
Si4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.9029(18) .
Fe1 N2 2.0170(17) .
Fe1 N2 2.0503(16) 2
Fe1 Fe1 2.6733(6) 2
Si1 N1 1.7144(19) .
Si1 C1 1.866(3) .
Si1 C2 1.869(3) .
Si1 HI1 1.4699(10) .
Si2 N1 1.713(2) .
Si2 C3 1.854(3) .
Si2 C4 1.873(3) .
Si2 HI2 1.4699(10) .
Si3 N2 1.7671(17) .
Si3 C6 1.854(3) .
Si3 C5 1.854(3) .
Si3 HI3 1.4699(10) .
Si4 N2 1.7617(17) .
Si4 C8 1.856(3) .
Si4 C7 1.857(2) .
Si4 HI4 1.4699(10) .
N2 Fe1 2.0503(16) 2
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
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
_geom_torsion_site_symmetry_4
C3 Si2 N1 Si1 58.1(2) . .
C4 Si2 N1 Si1 -65.6(2) . .
C3 Si2 N1 Fe1 -124.88(18) . .
C4 Si2 N1 Fe1 111.40(16) . .
C1 Si1 N1 Si2 -60.3(2) . .
C2 Si1 N1 Si2 64.06(19) . .
C1 Si1 N1 Fe1 122.66(15) . .
C2 Si1 N1 Fe1 -112.94(15) . .
N2 Fe1 N1 Si2 75.83(14) . .
N2 Fe1 N1 Si2 -106.74(12) 2 .
Fe1 Fe1 N1 Si2 -123.9(7) 2 .
N2 Fe1 N1 Si1 -106.87(12) . .
N2 Fe1 N1 Si1 70.55(14) 2 .
Fe1 Fe1 N1 Si1 53.4(8) 2 .
C8 Si4 N2 Si3 -56.92(17) . .
C7 Si4 N2 Si3 180.00(11) . .
C8 Si4 N2 Fe1 82.56(16) . .
C7 Si4 N2 Fe1 -40.53(14) . .
C8 Si4 N2 Fe1 177.93(13) . 2
C7 Si4 N2 Fe1 54.85(13) . 2
C6 Si3 N2 Si4 86.16(17) . .
C5 Si3 N2 Si4 -39.85(17) . .
C6 Si3 N2 Fe1 -56.14(16) . .
C5 Si3 N2 Fe1 177.85(12) . .
C6 Si3 N2 Fe1 -143.56(14) . 2
C5 Si3 N2 Fe1 90.43(14) . 2
N1 Fe1 N2 Si4 -66.95(14) . .
N2 Fe1 N2 Si4 115.12(11) 2 .
Fe1 Fe1 N2 Si4 115.12(11) 2 .
N1 Fe1 N2 Si3 74.72(13) . .
N2 Fe1 N2 Si3 -103.21(9) 2 .
Fe1 Fe1 N2 Si3 -103.21(9) 2 .
N1 Fe1 N2 Fe1 177.93(8) . 2
N2 Fe1 N2 Fe1 0.0 2 2
