#------------------------------------------------------------------------------
#$Date: 2017-11-28 04:35:34 +0200 (Tue, 28 Nov 2017) $
#$Revision: 203651 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/09/7120921.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_7120921
loop_
_publ_author_name
'Kosiorek, Sandra'
'Rosa, Bartłomiej'
'Boinski, Tomasz'
'Butkiewicz, Helena'
'Szymański, Marek P.'
'Danylyuk, Oksana'
'Szumna, Agnieszka'
'Sashuk, Volodymyr'
_publ_section_title
;
 Pillar[4]pyridinium. A Square-Shaped Molecular Box
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC08562A
_journal_year                    2017
_chemical_formula_sum            'C24 H26 I4 N4 O5'
_chemical_formula_weight         958.09
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-08-31 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3986(5)
_cell_length_b                   13.3986(5)
_cell_length_c                   8.7112(6)
_cell_measurement_reflns_used    1507
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.480
_cell_measurement_theta_min      3.034
_cell_volume                     1563.86(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 16.297
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3064
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.354
_diffrn_reflns_theta_min         3.041
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.023
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_description       plate
_exptl_crystal_F_000             900
_refine_diff_density_max         1.897
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         848
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0394
_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)+(0.0381P)²+15.0839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                762
_reflns_number_total             848
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc08562a2.cif
_cod_data_source_block           bar_2_mo
_cod_original_cell_volume        1563.86(16)
_cod_database_code               7120921
_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           2013-3
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'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O -0.5000 0.5000 0.0000 0.079(5) Uani 1 8 d DS T P . .
H1W1 H -0.4726 0.5142 -0.0971 0.118 Uiso 0.125 1 d D U P . .
H2W1 H -0.5591 0.4756 0.0000 0.118 Uiso 0.25 2 d DS U P . .
O2W O -0.002(2) 0.096(2) 0.0000 0.137(9) Uiso 0.5 2 d S . P A 1
O2WA O 0.015(4) 0.057(2) 0.196(4) 0.114(11) Uiso 0.25 1 d . . P B 2
I1 I 0.00002(4) 0.31437(4) 0.0000 0.0333(2) Uani 1 2 d S T P . .
N1 N -0.2654(5) 0.4107(5) 0.0000 0.0300(15) Uani 0.5 2 d S T P C 1
C1A C -0.2654(5) 0.4107(5) 0.0000 0.0300(15) Uani 0.5 2 d S T P C 2
C5 C -0.4103(5) 0.2653(5) 0.0000 0.0305(15) Uani 0.5 2 d S T P D 1
N1A N -0.4103(5) 0.2653(5) 0.0000 0.0305(15) Uani 0.5 2 d S T P D 2
C4 C -0.3708(5) 0.2985(5) 0.1346(7) 0.0433(14) Uani 1 1 d . . . . .
H4 H -0.3938 0.2715 0.2291 0.052 Uiso 1 1 calc R U . D 1
C3 C -0.2980(5) 0.3706(5) 0.1349(7) 0.0431(14) Uani 1 1 d . . . . .
H3 H -0.2703 0.3927 0.2293 0.052 Uiso 1 1 calc R U . C 1
C1 C -0.1969(6) 0.5004(6) 0.0000 0.038(2) Uani 1 2 d S T P . .
H1A H -0.1539 0.5004 0.0924 0.046 Uiso 0.5 1 calc R U P C 1
H1B H -0.1539 0.5004 -0.0924 0.046 Uiso 0.5 1 calc R U P C 1
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'
I I -0.4742 1.8119 '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
O2WA O2WA O2WA 89.998(7) 3 4
O2WA O2WA O2WA 44.999(3) 3 2
O2WA O2WA O2WA 44.999(9) 4 2
C3 N1 C3 119.0(7) . 10
C3 N1 C1 120.5(4) . .
C3 N1 C1 120.5(4) 10 .
C4 C5 C4 119.0(7) 10 .
C4 C5 C1 120.5(4) 10 11_455
C4 C5 C1 120.5(4) . 11_455
C5 C4 C3 120.5(6) . .
N1 C3 C4 120.2(6) . .
C5 C1 N1 105.2(6) 3_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O2WA O2WA 1.11(4) 3
O2WA O2WA 1.11(4) 4
O2WA O2WA 1.57(5) 2
N1 C3 1.364(7) .
N1 C3 1.364(7) 10
N1 C1 1.512(10) .
C5 C4 1.361(7) 10
C5 C4 1.361(7) .
C5 C1 1.507(10) 11_455
C4 C3 1.373(9) .
C1 N1A 1.507(10) 3_565
C1 C5 1.507(10) 3_565
