#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:29:03 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234861 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/95/4349534.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_4349534
loop_
_publ_author_name
'Lin, Jing-Xiang'
'Liang, Jun'
'Feng, Ji-Fei'
'Karadeniz, Bahar'
'Lü, Jian'
'Cao, Rong'
_publ_section_title
;
 Iodine uptake and enhanced electrical conductivity in a porous
 coordination polymer based on cucurbit[6]uril
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1393
_journal_paper_doi               10.1039/C6QI00305B
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         C36H36N24O12,2Na+3H2O,2I-,2H2O
_chemical_formula_sum            'C36 H36 I2 N24 Na2 O20'
_chemical_formula_weight         1440.67
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-04-07 deposited with the CCDC.
2016-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6184(7)
_cell_length_b                   15.9574(10)
_cell_length_c                   15.0119(11)
_cell_measurement_reflns_used    4327
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.22
_cell_measurement_theta_min      4.04
_cell_volume                     2783.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Agilent Supranova'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6700
_diffrn_reflns_theta_full        73.22
_diffrn_reflns_theta_max         73.22
_diffrn_reflns_theta_min         4.04
_exptl_absorpt_coefficient_mu    9.857
_exptl_absorpt_correction_T_max  0.5060
_exptl_absorpt_correction_T_min  0.2699
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.700
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1443P)²+4.6915P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2235
_reflns_number_gt                2196
_reflns_number_total             2829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00305b2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Pnnm
_cod_database_code               4349534
loop_
_symmetry_equiv_pos_as_xyz
'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, -y, -z'
'x, y, -z'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
I1 I 0.73393(6) -0.00206(3) 0.0000 0.0521(3) Uani 1 2 d S
N2 N 0.3724(4) -0.5401(3) -0.2858(3) 0.0437(11) Uani 1 1 d .
N3 N 0.4305(4) -0.4080(3) -0.2978(4) 0.0475(12) Uani 1 1 d .
C5 C 0.4291(6) -0.3187(4) -0.2889(4) 0.0491(14) Uani 1 1 d .
H5A H 0.3480 -0.2999 -0.2850 0.059 Uiso 1 1 calc R
H5B H 0.4627 -0.2937 -0.3434 0.059 Uiso 1 1 calc R
O2 O 0.2535(4) -0.4347(3) -0.2360(4) 0.0614(13) Uani 1 1 d .
C4 C 0.3427(5) -0.4588(4) -0.2696(4) 0.0458(13) Uani 1 1 d .
C2 C 0.2891(5) -0.6074(4) -0.2823(4) 0.0475(14) Uani 1 1 d .
H2A H 0.2913 -0.6388 -0.3391 0.057 Uiso 1 1 calc R
H2B H 0.2111 -0.5832 -0.2757 0.057 Uiso 1 1 calc R
C3 C 0.4769(5) -0.5454(4) -0.3386(4) 0.0438(13) Uani 1 1 d .
H3 H 0.4607 -0.5656 -0.4004 0.053 Uiso 1 1 calc R
N4 N 0.4910(4) -0.2866(3) -0.2123(4) 0.0440(12) Uani 1 1 d .
N5 N 0.5175(4) -0.2268(3) -0.0807(4) 0.0433(11) Uani 1 1 d .
C9 C 0.4893(7) -0.1827(5) 0.0000 0.0436(19) Uani 1 2 d S
H9A H 0.5304 -0.1283 0.0000 0.052 Uiso 1 2 calc SR
H9B H 0.4057 -0.1705 0.0000 0.052 Uiso 1 2 calc SR
N1 N 0.3105(4) -0.6650(3) -0.2090(3) 0.0438(11) Uani 1 1 d .
C10 C 0.4373(5) -0.2619(3) -0.1358(4) 0.0448(13) Uani 1 1 d .
C7 C 0.6298(5) -0.2217(3) -0.1230(4) 0.0396(12) Uani 1 1 d .
H7 H 0.6549 -0.1622 -0.1305 0.048 Uiso 1 1 calc R
C6 C 0.6122(5) -0.2651(3) -0.2139(4) 0.0430(13) Uani 1 1 d .
H6 H 0.6313 -0.2270 -0.2647 0.052 Uiso 1 1 calc R
O1 O 0.1747(4) -0.6117(3) -0.1128(3) 0.0592(12) Uani 1 1 d .
N6 N 0.7177(4) -0.2712(3) -0.0805(3) 0.0413(11) Uani 1 1 d .
O3 O 0.3346(4) -0.2691(3) -0.1197(3) 0.0577(12) Uani 1 1 d .
C1 C 0.2495(4) -0.6623(4) -0.1315(4) 0.0414(12) Uani 1 1 d .
C8 C 0.7777(7) -0.2477(6) 0.0000 0.0426(18) Uani 1 2 d S
H8A H 0.8546 -0.2744 0.0000 0.051 Uiso 1 2 calc SR
H8B H 0.7894 -0.1862 0.0000 0.051 Uiso 1 2 calc SR
Na7 Na 0.133(3) -0.5011(9) 0.0000 0.300(15) Uani 1 2 d S
O4W O 0.0000 -0.5000 -0.3318(16) 0.168(9) Uani 1 2 d S
O3W O 0.1054(13) -0.2463(15) 0.0000 0.208(8) Uani 1 2 d S
O2W O 0.295(2) -0.437(3) 0.0000 0.286(15) Uani 1 2 d S
O1W O 0.0689(16) -0.402(2) -0.1248(17) 0.210(12) Uani 0.50 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 '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
C4 N2 C2 122.1(5) . .
C4 N2 C3 111.4(5) . .
C2 N2 C3 122.4(5) . .
C4 N3 C5 123.5(5) . .
C4 N3 C3 112.4(5) . 2_645
C5 N3 C3 124.1(5) . 2_645
N3 C5 N4 114.8(5) . .
O2 C4 N2 126.2(6) . .
O2 C4 N3 125.2(6) . .
N2 C4 N3 108.6(5) . .
N2 C2 N1 112.6(5) . .
N3 C3 N2 115.0(5) 2_645 .
N3 C3 C3 103.0(5) 2_645 2_645
N2 C3 C3 103.6(6) . 2_645
C10 N4 C5 122.9(5) . .
C10 N4 C6 112.9(5) . .
C5 N4 C6 123.5(5) . .
C10 N5 C9 123.7(5) . .
C10 N5 C7 111.7(5) . .
C9 N5 C7 123.0(5) . .
N5 C9 N5 114.6(7) 6 .
C1 N1 C6 113.2(5) . 2_645
C1 N1 C2 122.4(5) . .
C6 N1 C2 124.1(5) 2_645 .
O3 C10 N4 125.7(6) . .
O3 C10 N5 125.8(6) . .
N4 C10 N5 108.5(5) . .
N6 C7 N5 114.4(5) . .
N6 C7 C6 103.9(4) . .
N5 C7 C6 104.0(4) . .
N1 C6 N4 115.0(5) 2_645 .
N1 C6 C7 102.7(4) 2_645 .
N4 C6 C7 102.7(5) . .
C1 O1 Na7 139.7(9) . .
C1 N6 C7 112.1(5) 2_645 .
C1 N6 C8 122.5(5) 2_645 .
C7 N6 C8 124.8(5) . .
O1 C1 N1 126.0(6) . .
O1 C1 N6 125.8(6) . 2_645
N1 C1 N6 108.0(5) . 2_645
N6 C8 N6 113.6(6) 6 .
O2W Na7 O1 99.8(14) . 6
O2W Na7 O1 99.8(14) . .
O1 Na7 O1 85.6(6) 6 .
O2W Na7 O1W 87.8(12) . 6
O1 Na7 O1W 89.8(7) 6 6
O1 Na7 O1W 171.7(15) . 6
O2W Na7 O1W 87.8(12) . .
O1 Na7 O1W 171.7(15) 6 .
O1 Na7 O1W 89.8(7) . .
O1W Na7 O1W 93.9(14) 6 .
O2W Na7 Na7 150.8(16) . 5_545
O1 Na7 Na7 101.6(10) 6 5_545
O1 Na7 Na7 101.6(10) . 5_545
O1W Na7 Na7 72.6(10) 6 5_545
O1W Na7 Na7 72.6(10) . 5_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N2 C4 1.364(9) .
N2 C2 1.446(7) .
N2 C3 1.452(8) .
N3 C4 1.370(8) .
N3 C5 1.432(7) .
N3 C3 1.444(8) 2_645
C5 N4 1.450(8) .
O2 C4 1.215(8) .
C2 N1 1.455(8) .
C3 N3 1.444(8) 2_645
C3 C3 1.545(12) 2_645
N4 C10 1.365(8) .
N4 C6 1.450(7) .
N5 C10 1.366(8) .
N5 C9 1.439(7) .
N5 C7 1.454(7) .
C9 N5 1.439(7) 6
N1 C1 1.362(7) .
N1 C6 1.434(7) 2_645
C10 O3 1.223(7) .
C7 N6 1.439(7) .
C7 C6 1.543(8) .
C6 N1 1.434(7) 2_645
O1 C1 1.220(7) .
O1 Na7 2.492(14) .
N6 C1 1.363(8) 2_645
N6 C8 1.445(6) .
C1 N6 1.363(8) 2_645
C8 N6 1.445(6) 6
Na7 O2W 2.13(4) .
Na7 O1 2.492(14) 6
Na7 O1W 2.56(3) 6
Na7 O1W 2.56(3) .
Na7 Na7 3.10(8) 5_545
