#------------------------------------------------------------------------------
#$Date: 2016-12-19 12:49:07 +0200 (Mon, 19 Dec 2016) $
#$Revision: 189226 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/72/7227282.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_7227282
loop_
_publ_author_name
'Ye, Yingxiang'
'Wu, Xiuzhen'
'Yao, Zizhu'
'Wu, Ling'
'Cai, Zetao'
'Wang, Lihua'
'Ma, Xiuling'
'Chen, Qian-Huo'
'Zhang, Zhangjing'
'Xiang, Shengchang'
_publ_section_title
;
 Metal--organic frameworks with a large breathing effect to host hydroxyl
 compounds for high anhydrous proton conductivity over a wide temperature
 range from subzero to 125 Â°C
;
_journal_issue                   11
_journal_name_full               'J. Mater. Chem. A'
_journal_page_first              4062
_journal_page_last               4070
_journal_paper_doi               10.1039/c5ta10765b
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety         '0.5(C40 H24 N12 O16 Zn6)'
_chemical_formula_sum            'C20 H12 N6 O8 Zn3'
_chemical_formula_weight         660.47
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-12 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.810(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1742(4)
_cell_length_b                   18.9858(5)
_cell_length_c                   9.1980(3)
_cell_measurement_reflns_used    4889
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.1970
_cell_measurement_theta_min      4.4680
_cell_volume                     2012.45(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9912
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.911
_diffrn_reflns_theta_min         4.488
_exptl_absorpt_coefficient_mu    2.400
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         2083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0255
_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)+(0.0445P)²+0.9935P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1888
_reflns_number_total             2083
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ta10765b2.cif
_cod_data_source_block           FJU-31-Bu
_cod_original_cell_volume        2012.46(11)
_cod_database_code               7227282
_shelxl_version_number           2013-2
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C1(H1), C2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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
Zn1 Zn 0.5000 0.0000 0.0000 0.02928(12) Uani 1 4 d S T P . .
Zn2 Zn 0.38367(3) 0.0000 0.31148(3) 0.03225(11) Uani 1 2 d S T P . .
O2 O 0.31199(14) 0.08656(8) 0.21823(18) 0.0545(4) Uani 1 1 d . . . . .
O1 O 0.39177(18) 0.07976(9) 0.03411(19) 0.0735(6) Uani 1 1 d . . . . .
N2 N 0.55573(16) 0.0000 0.3467(2) 0.0327(4) Uani 1 2 d S T P . .
N1 N 0.6392(2) 0.0000 0.4810(2) 0.0458(5) Uani 1 2 d S T P . .
N3 N 0.6001(2) 0.0000 0.2333(2) 0.0450(5) Uani 1 2 d S T P . .
C6 C 0.3155(3) 0.21344(13) -0.0715(3) 0.0655(7) Uani 1 1 d . . . . .
H6 H 0.3598 0.1890 -0.1203 0.079 Uiso 1 1 calc R . . . .
C5 C 0.2248(2) 0.21986(13) 0.1212(3) 0.0656(7) Uani 1 1 d . . . . .
H5 H 0.2075 0.1998 0.2035 0.079 Uiso 1 1 calc R . . . .
C4 C 0.29029(19) 0.18292(11) 0.0499(2) 0.0465(4) Uani 1 1 d . . . . .
C3 C 0.33518(18) 0.11054(10) 0.1033(2) 0.0456(4) Uani 1 1 d . . . . .
C1 C 0.7392(3) 0.0000 0.4516(4) 0.0952(18) Uani 1 2 d S T P . .
H1 H 0.8128 0.0000 0.5244 0.114 Uiso 1 2 calc RS T P . .
C2 C 0.7155(3) 0.0000 0.2979(4) 0.0959(18) Uani 1 2 d S T P . .
H2 H 0.7697 0.0000 0.2462 0.115 Uiso 1 2 calc RS 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 0.0181 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'
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'
Zn Zn -1.5491 0.6778 '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
O1 Zn1 O1 180.00(10) 6 2_655
O1 Zn1 O1 92.50(12) 6 .
O1 Zn1 O1 87.50(12) 2_655 .
O1 Zn1 O1 92.50(12) 2_655 5_655
O1 Zn1 O1 87.50(12) 6 5_655
O1 Zn1 O1 180.0 5_655 .
O1 Zn1 N3 88.11(6) 2_655 .
O1 Zn1 N3 88.11(6) 6 5_655
O1 Zn1 N3 91.89(6) 6 .
O1 Zn1 N3 88.12(6) 5_655 .
O1 Zn1 N3 88.11(6) . 5_655
O1 Zn1 N3 91.89(6) 5_655 5_655
O1 Zn1 N3 91.89(6) . .
O1 Zn1 N3 91.89(6) 2_655 5_655
N3 Zn1 N3 180.00(7) . 5_655
O2 Zn2 O2 117.00(10) . 6
O2 Zn2 N2 111.70(5) 6 .
O2 Zn2 N2 111.70(5) . .
O2 Zn2 N1 103.91(5) . 5_656
O2 Zn2 N1 103.91(6) 6 5_656
N2 Zn2 N1 107.57(8) . 5_656
C3 O2 Zn2 119.23(13) . .
C3 O1 Zn1 155.13(15) . .
N1 N2 Zn2 126.59(15) . .
N3 N2 Zn2 122.87(15) . .
N3 N2 N1 110.54(19) . .
N2 N1 Zn2 125.83(17) . 5_656
N2 N1 C1 106.7(2) . .
C1 N1 Zn2 127.5(2) . 5_656
N2 N3 Zn1 123.83(17) . .
N2 N3 C2 106.7(2) . .
C2 N3 Zn1 129.43(19) . .
C4 C6 C5 120.4(2) . 7
C4 C5 C6 120.5(2) . 7
C6 C4 C5 119.11(19) . .
C6 C4 C3 119.85(17) . .
C5 C4 C3 121.03(18) . .
O2 C3 C4 116.60(17) . .
O1 C3 O2 125.22(18) . .
O1 C3 C4 118.17(18) . .
N1 C1 C2 108.3(3) . .
N3 C2 C1 107.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.0962(14) 6
Zn1 O1 2.0962(14) 2_655
Zn1 O1 2.0962(14) 5_655
Zn1 O1 2.0962(14) .
Zn1 N3 2.099(2) .
Zn1 N3 2.099(2) 5_655
Zn2 O2 1.9274(13) .
Zn2 O2 1.9275(13) 6
Zn2 N2 2.0138(19) .
Zn2 N1 2.016(2) 5_656
O2 C3 1.263(3) .
O1 C3 1.227(2) .
N2 N1 1.323(3) .
N2 N3 1.320(3) .
N1 Zn2 2.016(2) 5_656
N1 C1 1.329(4) .
N3 C2 1.337(4) .
C6 C5 1.381(3) 7
C6 C4 1.377(3) .
C5 C6 1.381(3) 7
C5 C4 1.377(3) .
C4 C3 1.502(3) .
C1 C2 1.348(5) .
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Zn1 O1 C3 O2 -10.5(6) . . . .
Zn1 O1 C3 C4 168.8(3) . . . .
Zn1 N3 C2 C1 180.000(1) . . . .
Zn2 O2 C3 O1 7.7(3) . . . .
Zn2 O2 C3 C4 -171.59(14) . . . .
Zn2 N2 N1 Zn2 0.000(0) . . . 5_656
Zn2 N2 N1 C1 180.000(1) . . . .
Zn2 N2 N3 Zn1 0.000(0) . . . .
Zn2 N2 N3 C2 180.000(0) . . . .
Zn2 N1 C1 C2 180.000(0) 5_656 . . .
N2 N1 C1 C2 0.000(1) . . . .
N2 N3 C2 C1 0.000(1) . . . .
N1 N2 N3 Zn1 180.000(0) . . . .
N1 N2 N3 C2 0.000(0) . . . .
N1 C1 C2 N3 0.000(0) . . . .
N3 N2 N1 Zn2 180.000(0) . . . 5_656
N3 N2 N1 C1 0.000(0) . . . .
C6 C5 C4 C6 0.2(5) 7 . . .
C6 C5 C4 C3 179.6(3) 7 . . .
C6 C4 C3 O2 177.8(2) . . . .
C6 C4 C3 O1 -1.5(4) . . . .
C5 C6 C4 C5 -0.2(5) 7 . . .
C5 C6 C4 C3 -179.7(3) 7 . . .
C5 C4 C3 O2 -1.6(3) . . . .
C5 C4 C3 O1 179.0(2) . . . .
