#------------------------------------------------------------------------------
#$Date: 2015-07-05 10:43:49 +0300 (Sun, 05 Jul 2015) $
#$Revision: 140066 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513236.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_4513236
loop_
_publ_author_name
'Geyer, Florian L.'
'Rominger, Frank'
'Vogtland, Maximilian'
'Bunz, Uwe H. F.'
_publ_section_title
;
 Interpenetrated Frameworks with Anisotropic Pore Structures from a
 Tetrahedral Pyridine Ligand
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3539
_journal_paper_doi               10.1021/acs.cgd.5b00719
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C56 H32 N4 Si'
_chemical_formula_weight         788.94
_chemical_name_common            '1 (first modification) in manuscript'
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.518(7)
_cell_length_b                   26.518(7)
_cell_length_c                   6.3122(18)
_cell_measurement_reflns_used    3821
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      3.07
_cell_volume                     4439(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II Quazar'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            17280
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.210
_diffrn_reflns_theta_min         1.536
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.8380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). SADABS. University of Göttingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0740
_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)+(0.0820P)²+8.4847P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1554
_reflns_number_total             2009
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00719_si_002.cif
_cod_data_source_block           fge10
_cod_depositor_comments
'Adding full bibliography for 4513232--4513239.cif.'
_cod_original_cell_volume        4439(3)
_cod_database_code               4513236
_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. 
;
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.992
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 0.0000 0.2500 0.1250 0.0172(4) Uani 1 4 d S T P
C11 C 0.05673(10) 0.23339(10) 0.2919(4) 0.0180(6) Uani 1 1 d . . .
C12 C 0.08391(11) 0.18901(11) 0.2612(5) 0.0246(7) Uani 1 1 d . . .
H12 H 0.0733 0.1660 0.1548 0.029 Uiso 1 1 calc R U .
C13 C 0.12598(12) 0.17751(12) 0.3816(5) 0.0298(8) Uani 1 1 d . . .
H13 H 0.1438 0.1470 0.3569 0.036 Uiso 1 1 calc R U .
C14 C 0.14237(11) 0.21045(12) 0.5386(5) 0.0257(7) Uani 1 1 d . . .
C15 C 0.11625(11) 0.25555(12) 0.5689(5) 0.0245(7) Uani 1 1 d . . .
H15 H 0.1274 0.2788 0.6733 0.029 Uiso 1 1 calc R U .
C16 C 0.07423(11) 0.26655(11) 0.4473(5) 0.0217(7) Uani 1 1 d . . .
H16 H 0.0569 0.2974 0.4702 0.026 Uiso 1 1 calc R U .
C17 C 0.18391(12) 0.19749(13) 0.6747(6) 0.0311(8) Uani 1 1 d . . .
C18 C 0.21695(12) 0.18515(13) 0.7948(6) 0.0339(8) Uani 1 1 d . . .
C21 C 0.25417(12) 0.17011(14) 0.9476(6) 0.0348(9) Uani 1 1 d . . .
C22 C 0.29218(15) 0.13661(17) 0.9009(8) 0.0564(12) Uani 1 1 d . . .
H22 H 0.2951 0.1227 0.7628 0.068 Uiso 1 1 calc R U .
C23 C 0.32612(17) 0.1235(2) 1.0586(9) 0.0678(14) Uani 1 1 d . . .
H23 H 0.3521 0.1003 1.0235 0.081 Uiso 1 1 calc R U .
N24 N 0.32477(14) 0.14091(17) 1.2528(7) 0.0675(12) Uani 1 1 d . . .
C25 C 0.28869(18) 0.1740(2) 1.2941(7) 0.0740(16) Uani 1 1 d . . .
H25 H 0.2876 0.1883 1.4320 0.089 Uiso 1 1 calc R U .
C26 C 0.25273(16) 0.1890(2) 1.1506(7) 0.0588(13) Uani 1 1 d . . .
H26 H 0.2272 0.2122 1.1910 0.071 Uiso 1 1 calc R U .
C31 C 0.2465(12) 0.0167(15) 0.365(14) 0.51(4) 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'
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
C11 Si1 C11 108.13(8) . 15
C11 Si1 C11 108.13(8) . 12_666
C11 Si1 C11 112.19(17) 15 12_666
C11 Si1 C11 112.19(17) . 6_454
C11 Si1 C11 108.13(8) 15 6_454
C11 Si1 C11 108.13(8) 12_666 6_454
C12 C11 C16 117.2(3) . .
C12 C11 Si1 122.1(2) . .
C16 C11 Si1 120.6(2) . .
C13 C12 C11 121.8(3) . .
C13 C12 H12 119.1 . .
C11 C12 H12 119.1 . .
C12 C13 C14 120.3(3) . .
C12 C13 H13 119.8 . .
C14 C13 H13 119.8 . .
C13 C14 C15 118.7(3) . .
C13 C14 C17 121.0(3) . .
C15 C14 C17 120.2(3) . .
C16 C15 C14 120.3(3) . .
C16 C15 H15 119.8 . .
C14 C15 H15 119.8 . .
C15 C16 C11 121.6(3) . .
C15 C16 H16 119.2 . .
C11 C16 H16 119.2 . .
C18 C17 C14 176.6(4) . .
C17 C18 C21 176.7(4) . .
C22 C21 C26 117.1(3) . .
C22 C21 C18 122.6(4) . .
C26 C21 C18 120.3(3) . .
C21 C22 C23 119.0(4) . .
C21 C22 H22 120.5 . .
C23 C22 H22 120.5 . .
N24 C23 C22 124.4(4) . .
N24 C23 H23 117.8 . .
C22 C23 H23 117.8 . .
C23 N24 C25 116.0(4) . .
N24 C25 C26 124.3(5) . .
N24 C25 H25 117.8 . .
C26 C25 H25 117.8 . .
C25 C26 C21 119.2(4) . .
C25 C26 H26 120.4 . .
C21 C26 H26 120.4 . .
C31 C31 C31 149(3) 7_444 8_444
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C11 1.889(3) .
Si1 C11 1.889(3) 15
Si1 C11 1.889(3) 12_666
Si1 C11 1.889(3) 6_454
C11 C12 1.394(4) .
C11 C16 1.397(4) .
C12 C13 1.384(4) .
C12 H12 0.9500 .
C13 C14 1.391(4) .
C13 H13 0.9500 .
C14 C15 1.395(4) .
C14 C17 1.438(4) .
C15 C16 1.384(4) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 C18 1.204(5) .
C18 C21 1.436(5) .
C21 C22 1.375(5) .
C21 C26 1.377(6) .
C22 C23 1.387(6) .
C22 H22 0.9500 .
C23 N24 1.310(6) .
C23 H23 0.9500 .
N24 C25 1.324(6) .
C25 C26 1.374(6) .
C25 H25 0.9500 .
C26 H26 0.9500 .
C31 C31 1.70(2) 7_444
C31 C31 1.70(2) 8_444
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
C11 Si1 C11 C12 9.1(2) 15
C11 Si1 C11 C12 -112.6(3) 12_666
C11 Si1 C11 C12 128.3(3) 6_454
C11 Si1 C11 C16 -173.3(2) 15
C11 Si1 C11 C16 65.00(17) 12_666
C11 Si1 C11 C16 -54.2(2) 6_454
C16 C11 C12 C13 1.1(5) .
Si1 C11 C12 C13 178.8(2) .
C11 C12 C13 C14 0.1(5) .
C12 C13 C14 C15 -1.3(5) .
C12 C13 C14 C17 175.7(3) .
C13 C14 C15 C16 1.4(5) .
C17 C14 C15 C16 -175.7(3) .
C14 C15 C16 C11 -0.1(5) .
C12 C11 C16 C15 -1.1(4) .
Si1 C11 C16 C15 -178.8(2) .
C26 C21 C22 C23 0.7(6) .
C18 C21 C22 C23 -179.0(4) .
C21 C22 C23 N24 0.0(8) .
C22 C23 N24 C25 -1.4(8) .
C23 N24 C25 C26 2.4(8) .
N24 C25 C26 C21 -1.8(8) .
C22 C21 C26 C25 0.2(7) .
C18 C21 C26 C25 179.8(4) .
