#------------------------------------------------------------------------------
#$Date: 2015-07-05 10:43:49 +0300 (Sun, 05 Jul 2015) $
#$Revision: 140066 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513239.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_4513239
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            'C32 H20 Si'
_chemical_formula_weight         432.57
_chemical_name_common            '4 in manuscript'
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            2
_cell_length_a                   13.491(2)
_cell_length_b                   13.491(2)
_cell_length_c                   6.7026(10)
_cell_measurement_reflns_used    904
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      3.02
_cell_volume                     1219.9(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5487
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.537
_diffrn_reflns_theta_min         2.135
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9580
_exptl_absorpt_correction_T_min  0.8398
_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    1.178
_exptl_crystal_description       needle
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
; 
 Flack x determined using 389 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.35(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0454
_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)+(0.0224P)²+0.7082P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.825
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.998
_reflns_number_gt                995
_reflns_number_total             1144
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00719_si_002.cif
_cod_data_source_block           fge11
_cod_depositor_comments
'Adding full bibliography for 4513232--4513239.cif.'
_cod_original_cell_volume        1219.9(4)
_cod_database_code               4513239
_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   0.978
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'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'
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 0.0000 0.5000 0.0317(5) Uani 1 4 d S T P
C11 C -0.1078(2) -0.0379(2) 0.3405(6) 0.0314(9) Uani 1 1 d . . .
C12 C -0.1594(3) -0.1263(3) 0.3717(6) 0.0365(9) Uani 1 1 d . . .
H12 H -0.1360 -0.1714 0.4698 0.044 Uiso 1 1 calc R U .
C13 C -0.2436(3) -0.1501(3) 0.2638(6) 0.0397(10) Uani 1 1 d . . .
H13 H -0.2765 -0.2112 0.2879 0.048 Uiso 1 1 calc R U .
C14 C -0.2803(3) -0.0852(3) 0.1202(6) 0.0317(9) Uani 1 1 d . . .
C15 C -0.2285(3) 0.0021(3) 0.0820(6) 0.0350(9) Uani 1 1 d . . .
H15 H -0.2511 0.0462 -0.0186 0.042 Uiso 1 1 calc R U .
C16 C -0.1441(3) 0.0246(3) 0.1905(6) 0.0355(9) Uani 1 1 d . . .
H16 H -0.1097 0.0844 0.1623 0.043 Uiso 1 1 calc R U .
C17 C -0.3712(3) -0.1079(3) 0.0160(7) 0.0380(9) Uani 1 1 d . . .
C18 C -0.4465(3) -0.1257(3) -0.0639(6) 0.0505(13) Uani 1 1 d . . .
H18 H -0.5075 -0.1400 -0.1286 0.061 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'
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 108.94(11) . 3_556
C11 Si1 C11 110.5(2) . 2
C11 Si1 C11 108.94(11) 3_556 2
C11 Si1 C11 108.94(11) . 4_556
C11 Si1 C11 110.5(2) 3_556 4_556
C11 Si1 C11 108.94(11) 2 4_556
C12 C11 C16 116.6(3) . .
C12 C11 Si1 122.3(3) . .
C16 C11 Si1 121.0(3) . .
C13 C12 C11 121.9(4) . .
C13 C12 H12 119.0 . .
C11 C12 H12 119.0 . .
C12 C13 C14 120.5(4) . .
C12 C13 H13 119.8 . .
C14 C13 H13 119.8 . .
C13 C14 C15 118.7(3) . .
C13 C14 C17 120.2(3) . .
C15 C14 C17 121.1(4) . .
C16 C15 C14 120.1(4) . .
C16 C15 H15 119.9 . .
C14 C15 H15 119.9 . .
C15 C16 C11 122.1(3) . .
C15 C16 H16 118.9 . .
C11 C16 H16 118.9 . .
C18 C17 C14 178.1(5) . .
C17 C18 H18 180.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C11 1.877(4) .
Si1 C11 1.877(4) 3_556
Si1 C11 1.877(4) 2
Si1 C11 1.877(4) 4_556
C11 C12 1.396(5) .
C11 C16 1.401(5) .
C12 C13 1.384(5) .
C12 H12 0.9500 .
C13 C14 1.393(5) .
C13 H13 0.9500 .
C14 C15 1.393(5) .
C14 C17 1.444(5) .
C15 C16 1.385(5) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 C18 1.173(5) .
C18 H18 0.9500 .
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 -109.5(4) 3_556
C11 Si1 C11 C12 130.8(3) 2
C11 Si1 C11 C12 11.1(3) 4_556
C11 Si1 C11 C16 66.7(2) 3_556
C11 Si1 C11 C16 -53.0(3) 2
C11 Si1 C11 C16 -172.6(3) 4_556
C16 C11 C12 C13 -1.6(6) .
Si1 C11 C12 C13 174.8(3) .
C11 C12 C13 C14 -0.6(6) .
C12 C13 C14 C15 2.5(6) .
C12 C13 C14 C17 -176.5(4) .
C13 C14 C15 C16 -2.2(6) .
C17 C14 C15 C16 176.9(4) .
C14 C15 C16 C11 -0.1(6) .
C12 C11 C16 C15 1.9(6) .
Si1 C11 C16 C15 -174.5(3) .
