#------------------------------------------------------------------------------
#$Date: 2017-11-28 04:35:34 +0200 (Tue, 28 Nov 2017) $
#$Revision: 203651 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/09/7120922.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_7120922
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 H24 F24 N4 P4'
_chemical_formula_weight         948.35
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_atom_sites_solution_hydrogens   geom
_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                   7.6962(3)
_cell_length_b                   11.6651(4)
_cell_length_c                   19.3064(7)
_cell_measurement_reflns_used    4857
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.577
_cell_measurement_theta_min      3.164
_cell_volume                     1733.27(11)
_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 0.998
_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  0.0186
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6515
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         3.171
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.892
_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            colourless
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0291
_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)+(0.0366P)²+2.9292P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1085
_reflns_number_total             1108
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc08562a2.cif
_cod_data_source_block           bar_2015_A
_cod_database_code               7120922
_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'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+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
C1 C 0.0000 0.10354(15) 0.33553(9) 0.0123(3) Uani 0.5 2 d S T P A 1
N1 N 0.0000 0.10354(15) 0.33553(9) 0.0123(3) Uani 0.5 2 d S T P A 2
C4 C 0.0000 0.26717(15) 0.43730(9) 0.0121(3) Uani 0.5 2 d S T P B 1
N2 N 0.0000 0.26717(15) 0.43730(9) 0.0121(3) Uani 0.5 2 d S T P B 2
C5 C 0.0000 0.3437(2) 0.5000 0.0130(5) Uani 1 4 d S T P . .
H5A H 0.1044 0.3932 0.5000 0.016 Uiso 0.5 2 calc R U P B 1
H5B H -0.1044 0.3932 0.5000 0.016 Uiso 0.5 2 calc R U P B 1
C3 C 0.15462(18) 0.22872(12) 0.41075(7) 0.0145(3) Uani 1 1 d . . . . .
H3 H 0.2613 0.2588 0.4276 0.017 Uiso 1 1 calc R U . B 1
C2 C 0.15477(18) 0.14626(12) 0.35959(7) 0.0146(3) Uani 1 1 d . . . . .
H2 H 0.2615 0.1191 0.3411 0.018 Uiso 1 1 calc R U . A 1
C6 C 0.0000 0.0000 0.28888(14) 0.0141(5) Uani 1 4 d S T P . .
H6A H -0.1045 0.0000 0.2590 0.017 Uiso 0.5 2 calc R U P A 1
H6B H 0.1045 0.0000 0.2590 0.017 Uiso 0.5 2 calc R U P A 1
P1 P 0.0000 0.5000 0.29277(3) 0.01187(17) Uani 1 4 d S T P . .
F1 F 0.0000 0.5000 0.37554(9) 0.0182(4) Uani 1 4 d S T P . .
F2 F 0.14768(11) 0.40275(7) 0.29177(4) 0.0200(2) Uani 1 1 d . . . . .
F3 F 0.0000 0.5000 0.20852(8) 0.0185(4) Uani 1 4 d S T P . .
P3 P 0.0000 0.5000 0.0000 0.0126(2) Uani 1 8 d S T P . .
F5 F 0.0000 0.40289(13) 0.05874(7) 0.0281(3) Uani 1 2 d S T P . .
F4 F 0.2091(2) 0.5000 0.0000 0.0186(4) Uani 1 4 d S T P . .
P2 P 0.0000 0.0000 0.0000 0.0147(2) Uani 1 8 d S T P . .
F6 F 0.0000 0.13830(16) 0.0000 0.0298(5) Uani 1 4 d S T P . .
F7 F 0.14776(17) 0.0000 0.05817(7) 0.0271(3) Uani 1 2 d S T P . .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
C2 C1 C2 120.46(17) . 12
C2 C1 C6 119.57(9) . .
C2 C1 C6 119.57(9) 12 .
C3 C4 C3 120.43(17) . 12
C3 C4 C5 119.67(9) . .
C3 C4 C5 119.67(9) 12 .
C4 C5 C4 107.2(2) 10_556 .
C4 C3 C2 119.79(13) . .
C1 C2 C3 119.68(13) . .
C1 C6 C1 106.6(2) 2 .
F1 P1 F2 90.69(4) . .
F1 P1 F2 90.69(4) . 12
F2 P1 F2 90.10(7) . 12
F1 P1 F2 90.69(4) . 11_565
F2 P1 F2 89.88(7) . 11_565
F2 P1 F2 178.62(7) 12 11_565
F1 P1 F2 90.69(4) . 2_565
F2 P1 F2 178.62(7) . 2_565
F2 P1 F2 89.88(7) 12 2_565
F2 P1 F2 90.10(6) 11_565 2_565
F1 P1 F3 180.0 . .
F2 P1 F3 89.31(4) . .
F2 P1 F3 89.31(4) 12 .
F2 P1 F3 89.31(4) 11_565 .
F2 P1 F3 89.31(4) 2_565 .
F5 P3 F5 180.00(9) 10 2_565
F5 P3 F5 89.94(11) 10 9_565
F5 P3 F5 90.06(11) 2_565 9_565
F5 P3 F5 90.06(11) 10 .
F5 P3 F5 89.94(11) 2_565 .
F5 P3 F5 180.0 9_565 .
F5 P3 F4 90.0 10 9_565
F5 P3 F4 90.0 2_565 9_565
F5 P3 F4 90.0 9_565 9_565
F5 P3 F4 90.0 . 9_565
F5 P3 F4 90.0 10 .
F5 P3 F4 90.0 2_565 .
F5 P3 F4 90.0 9_565 .
F5 P3 F4 90.0 . .
F4 P3 F4 180.0 9_565 .
F7 P2 F7 180.0 . 9
F7 P2 F7 89.29(10) . 10
F7 P2 F7 90.71(10) 9 10
F7 P2 F7 90.71(10) . 2
F7 P2 F7 89.29(10) 9 2
F7 P2 F7 180.00(9) 10 2
F7 P2 F6 90.0 . .
F7 P2 F6 90.0 9 .
F7 P2 F6 90.0 10 .
F7 P2 F6 90.0 2 .
F7 P2 F6 90.0 . 9
F7 P2 F6 90.0 9 9
F7 P2 F6 90.0 10 9
F7 P2 F6 90.0 2 9
F6 P2 F6 180.0 . 9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.3722(16) .
C1 C2 1.3722(16) 12
C1 C6 1.507(2) .
C4 C3 1.3711(16) .
C4 C3 1.3711(16) 12
C4 C5 1.504(2) .
C5 N2 1.504(2) 10_556
C5 C4 1.504(2) 10_556
C3 C2 1.3787(19) .
C6 N1 1.507(2) 2
C6 C1 1.507(2) 2
P1 F1 1.5979(17) .
P1 F2 1.6060(8) .
P1 F2 1.6060(8) 12
P1 F2 1.6060(8) 11_565
P1 F2 1.6060(8) 2_565
P1 F3 1.6265(17) .
P3 F5 1.6029(13) 10
P3 F5 1.6029(13) 2_565
P3 F5 1.6029(13) 9_565
P3 F5 1.6029(13) .
P3 F4 1.6094(17) 9_565
P3 F4 1.6094(17) .
P2 F7 1.5983(13) .
P2 F7 1.5983(13) 9
P2 F7 1.5983(13) 10
P2 F7 1.5983(13) 2
P2 F6 1.6132(18) .
P2 F6 1.6133(18) 9
