#------------------------------------------------------------------------------
#$Date: 2015-10-09 11:22:32 +0300 (Fri, 09 Oct 2015) $
#$Revision: 161269 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/59/7035952.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_7035952
loop_
_publ_author_name
'Zhang, Xiuling'
'Zhang, Yong-Zheng'
'Zhang, Da-Shuai'
'Zhu, Baoyong'
'Li, Jian-Rong'
_publ_section_title
;
 A hydrothermally stable Zn(ii)-based metal-organic framework: structural
 modulation and gas adsorption.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15697
_journal_page_last               15702
_journal_paper_doi               10.1039/c5dt01770j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C24 H13 N3 O10 Zn2'
_chemical_formula_sum            'C24 H13 N3 O10 Zn2'
_chemical_formula_weight         634.11
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-21
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.07.16 svn.r3196 for OlexSys, GUI svn.r5065)
;
_audit_update_record
;
2015-07-21 deposited with the CCDC.
2015-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.7612(16)
_cell_length_b                   16.7612(16)
_cell_length_c                   6.8980(9)
_cell_measurement_reflns_used    5905
_cell_measurement_temperature    100(10)
_cell_measurement_theta_max      74.5210
_cell_measurement_theta_min      5.2350
_cell_volume                     1678.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1688
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -50.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000   38.0000  120.0000 82

  2 omega  -49.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000   38.0000  -90.0000 69

  3 omega  -62.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5000   19.0000   30.0000 99

  4 omega   10.00   59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6040  -99.0000   30.0000 49

  5 omega   64.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6040 -122.0000 -117.0000 31

  6 omega   28.00   74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.6040 -125.0000 -180.0000 46

  7 omega   46.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -30.0000  120.0000 42

  8 omega   95.00  135.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -77.0000  -30.0000 40

  9 omega   40.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -45.0000 -180.0000 57

 10 omega  114.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324   15.0000   60.0000 63

 11 omega   38.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324 -125.0000  -30.0000 76

 12 omega   38.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -45.0000   90.0000 31

 13 omega   69.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324   15.0000   60.0000 25

 14 omega   28.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -94.0000   90.0000 26

 15 omega   47.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -77.0000  -30.0000 26

 16 omega   51.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -30.0000 -120.0000 26

 17 omega   25.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -94.0000 -180.0000 80

 18 omega   71.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -94.0000   90.0000 31

 19 omega   39.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -94.0000    0.0000 66

 20 omega   82.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324   45.0000  120.0000 96

 21 omega   96.00  122.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324   30.0000  -60.0000 26

 22 omega  153.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324   30.0000  -60.0000 25

 23 omega   32.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      106.3324  -30.0000  -30.0000 39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0984929000
_diffrn_orient_matrix_UB_12      0.0237243000
_diffrn_orient_matrix_UB_13      0.0553124000
_diffrn_orient_matrix_UB_21      -0.0343614000
_diffrn_orient_matrix_UB_22      -0.1026994000
_diffrn_orient_matrix_UB_23      0.0368924000
_diffrn_orient_matrix_UB_31      0.0197006000
_diffrn_orient_matrix_UB_32      -0.0116611000
_diffrn_orient_matrix_UB_33      -0.2134310000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.064
_diffrn_reflns_theta_max         67.064
_diffrn_reflns_theta_min         5.278
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       needle
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1091
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0711
_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)+(0.0984P)²+4.4893P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.2018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                983
_reflns_number_total             1091
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01770j2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7035952.cif.'
_cod_original_cell_volume        1678.3(4)
_cod_database_code               7035952
_chemical_oxdiff_formula         CHONZn
_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_max   0.958
_shelx_estimated_absorpt_t_min   0.695
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 O3-Zn1
 1.95 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: O3(0.16667) H3A(0.16667)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), O3(H3A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -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
Zn1 Zn 0.6667 0.3333 0.00190(14) 0.0428(5) Uani 1 3 d DS T P
O2 O 0.1270(3) -0.0461(3) 0.2500 0.0443(11) Uani 1 2 d S T P
C6 C 0.0642(4) -0.0199(4) 0.2500 0.0375(13) Uani 1 2 d S T P
N1 N 0.0909(3) 0.0689(3) 0.2500 0.0371(11) Uani 1 2 d S T P
C5 C 0.2216(4) 0.0217(4) 0.2500 0.0418(14) Uani 1 2 d S T P
C2 C 0.4062(4) 0.1494(5) 0.2500 0.0533(18) Uani 1 2 d S T P
C4 C 0.2661(3) 0.0522(4) 0.4243(9) 0.0594(14) Uani 1 1 d . . .
H4 H 0.2338 0.0296 0.5431 0.071 Uiso 1 1 calc R . .
C3 C 0.3585(4) 0.1162(4) 0.4233(10) 0.0655(15) Uani 1 1 d . . .
H3 H 0.3902 0.1382 0.5428 0.079 Uiso 1 1 calc R . .
O1 O 0.5445(3) 0.2454(3) 0.0867(9) 0.0911(16) Uani 1 1 d . . .
C1 C 0.5053(6) 0.2183(6) 0.2500 0.073(3) Uani 1 2 d S T P
O3 O 0.6160(11) 0.2788(9) -0.2500 0.103(7) Uani 0.3333 2 d DS TU P
H3A H 0.5616 0.2201 -0.2500 0.123 Uiso 0.3333 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 111.15(17) 3_655 5_665
O1 Zn1 O1 111.15(17) 3_655 .
O1 Zn1 O1 111.16(17) 5_665 .
O1 Zn1 O3 82.2(3) 3_655 3_655
O1 Zn1 O3 126.8(7) . 3_655
O1 Zn1 O3 110.5(8) 5_665 3_655
O1 Zn1 O3 110.5(8) 3_655 .
O1 Zn1 O3 126.8(7) 5_665 .
O1 Zn1 O3 110.5(8) . 8_665
O1 Zn1 O3 126.8(7) 3_655 8_665
O1 Zn1 O3 82.2(3) 5_665 8_665
O1 Zn1 O3 82.2(3) . .
O3 Zn1 O3 46.22(14) 3_655 8_665
O3 Zn1 O3 46.22(14) 3_655 .
O3 Zn1 O3 46.22(14) . 8_665
C6 O2 C5 119.2(4) . .
O2 C6 N1 112.9(5) . 8_556
N1 C6 O2 119.7(5) . .
N1 C6 N1 127.5(5) . 8_556
C6 N1 C6 112.5(5) . 3
C4 C5 O2 118.8(3) 10_556 .
C4 C5 O2 118.8(3) . .
C4 C5 C4 122.4(6) 10_556 .
C3 C2 C3 118.6(6) 10_556 .
C3 C2 C1 120.7(3) 10_556 .
C3 C2 C1 120.7(3) . .
C5 C4 H4 120.8 . .
C5 C4 C3 118.5(6) . .
C3 C4 H4 120.8 . .
C2 C3 H3 119.5 . .
C4 C3 C2 121.0(6) . .
C4 C3 H3 119.5 . .
C1 O1 Zn1 135.0(5) . .
O1 C1 C2 117.3(4) 10_556 .
O1 C1 C2 117.3(4) . .
O1 C1 O1 125.4(8) . 10_556
Zn1 O3 Zn1 126.10(17) 8_665 .
Zn1 O3 H3A 117.0 . .
Zn1 O3 H3A 117.0 8_665 .
O3 O3 Zn1 66.89(7) 3_655 8_665
O3 O3 Zn1 66.89(7) 8_665 8_665
O3 O3 Zn1 66.89(7) 8_665 .
O3 O3 Zn1 66.89(7) 3_655 .
O3 O3 O3 59.998(1) 8_665 3_655
O3 O3 H3A 150.0 8_665 .
O3 O3 H3A 150.0 3_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.921(4) 3_655
Zn1 O1 1.921(4) 5_665
Zn1 O1 1.921(4) .
Zn1 O3 1.9493(11) 3_655
Zn1 O3 1.9493(11) .
Zn1 O3 1.9493(11) 8_665
O2 C6 1.327(7) .
O2 C5 1.416(7) .
C6 N1 1.336(7) 8_556
C6 N1 1.323(7) .
N1 C6 1.336(7) 3
C5 C4 1.372(6) 10_556
C5 C4 1.372(6) .
C2 C3 1.390(7) 10_556
C2 C3 1.390(7) .
C2 C1 1.476(10) .
C4 H4 0.9500 .
C4 C3 1.373(7) .
C3 H3 0.9500 .
O1 C1 1.268(6) .
C1 O1 1.268(6) 10_556
O3 Zn1 1.9493(11) 8_665
O3 O3 1.530(5) 3_655
O3 O3 1.530(5) 8_665
O3 H3A 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
_geom_torsion_site_symmetry_4
Zn1 O1 C1 C2 177.8(5) . .
Zn1 O1 C1 O1 -2.3(15) . 10_556
O2 C6 N1 C6 180.0 . 3
O2 C5 C4 C3 178.3(5) . .
C6 O2 C5 C4 -91.1(5) . 10_556
C6 O2 C5 C4 91.1(5) . .
N1 C6 N1 C6 0.0 8_556 3
C5 O2 C6 N1 180.0 . 8_556
C5 O2 C6 N1 0.0 . .
C5 C4 C3 C2 -0.2(9) . .
C4 C5 C4 C3 0.6(11) 10_556 .
C3 C2 C3 C4 -0.2(11) 10_556 .
C3 C2 C1 O1 179.9(7) . .
C3 C2 C1 O1 0.0(11) . 10_556
C3 C2 C1 O1 0.0(11) 10_556 .
C3 C2 C1 O1 -179.9(7) 10_556 10_556
C1 C2 C3 C4 179.9(6) . .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.000 0.500 -0.442 215.9 39.6
2 0.500 0.000 -0.463 215.9 39.6
3 0.500 0.500 -0.111 215.9 39.6
