#------------------------------------------------------------------------------
#$Date: 2021-02-18 12:54:05 +0200 (Thu, 18 Feb 2021) $
#$Revision: 262073 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/04/1560479.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_1560479
loop_
_publ_author_name
'Xue, Chen'
'Yao, Zhi-Yuan'
'Liu, Shao-Xian'
'Luo, Hong-Bin'
'Zou, Yang'
'Li, Li'
'Ren, Xiao-Ming'
_publ_section_title
;
 Dielectric anomaly and relaxation natures in a Zn-Cr
 pillar−layered metal−organic framework with cages and
 channels
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              107
_journal_page_last               113
_journal_paper_doi               10.1016/j.jssc.2017.03.029
_journal_volume                  250
_journal_year                    2017
_chemical_formula_moiety         'C54 H30 Cr3 N6 O28 Zn3 '
_chemical_formula_sum            'C54 H30 Cr3 N6 O28 Zn3'
_chemical_formula_weight         1563.01
_space_group_crystal_system      hexagonal
_space_group_IT_number           189
_space_group_name_Hall           'P -6 -2'
_space_group_name_H-M_alt        'P -6 2 m'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   16.7714(8)
_cell_length_b                   16.7714(8)
_cell_length_c                   14.4687(14)
_cell_measurement_reflns_used    5370
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      57.509
_cell_measurement_theta_min      4.759
_cell_volume                     3524.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25605
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.429
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  27.421
_exptl_absorpt_correction_T_min  2.429
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.736
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.024
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 1012 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         2972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0609
_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)+(0.1254P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2471
_reflns_number_total             2972
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            JSSC-2017-250-107.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        3524.5(5)
_cod_original_formula_sum        'C54 H30 Cr3 N6 O28 Zn3 '
_cod_database_code               1560479
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+y, -x, -z'
'-y, x-y, z'
'x, y, -z'
'-x+y, -x, z'
'-y, x-y, -z'
'y, x, z'
'x-y, -y, -z'
'-x, -x+y, z'
'y, x, -z'
'x-y, -y, z'
'-x, -x+y, -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 0.0000 0.34512(5) 1.0000 0.0376(3) Uani 1 4 d S T P . .
C1 C 0.2450(4) 0.6506(4) 1.0000 0.0368(14) Uani 1 2 d S T P . .
H1 H 0.1836 0.6394 1.0000 0.044 Uiso 1 2 calc R U P . .
C2 C 0.2599(4) 0.5770(4) 1.0000 0.0376(15) Uani 1 2 d S T P . .
C3 C 0.1805(4) 0.4782(4) 1.0000 0.0358(13) Uani 1 2 d S T P . .
C4 C -0.0745(9) 0.1999(8) 0.8535(10) 0.058(3) Uani 0.5 1 d . . P . .
H4 H -0.1270 0.1708 0.8924 0.070 Uiso 0.5 1 calc R U P . .
C5 C -0.0758(11) 0.1594(9) 0.7711(12) 0.073(5) Uani 0.5 1 d . . P . .
H5 H -0.1300 0.1054 0.7515 0.087 Uiso 0.5 1 calc R U P . .
C6 C 0.0000 0.1966(4) 0.7182(5) 0.0425(15) Uani 1 2 d S T P . .
C7 C 0.0752(9) 0.2810(11) 0.7454(13) 0.077(5) Uani 0.5 1 d . . P . .
H7 H 0.1275 0.3117 0.7063 0.092 Uiso 0.5 1 calc R U P . .
C8 C 0.0732(10) 0.3163(11) 0.8226(13) 0.080(5) Uani 0.5 1 d . . P . .
H8 H 0.1269 0.3716 0.8404 0.096 Uiso 0.5 1 calc R U P . .
C9 C 0.0000 0.1484(4) 0.6314(5) 0.0443(15) Uani 1 2 d S T P . .
N1 N 0.0000 0.2812(3) 0.8822(4) 0.0417(12) Uani 1 2 d S T P . .
O1 O 0.1024(3) 0.4694(3) 1.0000 0.0464(13) Uani 1 2 d S T P . .
O2 O 0.1961(3) 0.4145(3) 1.0000 0.0459(11) Uani 1 2 d S T P . .
Cr1 Cr 0.11486(9) 0.11486(9) 0.5000 0.0416(4) Uani 1 4 d S T P . .
O3 O 0.0775(2) 0.1696(2) 0.5982(3) 0.0523(9) Uani 1 1 d . . . . .
O4 O 0.0000 0.0000 0.5000 0.035(2) Uani 1 12 d S T P . .
O5 O 0.2345(4) 0.2345(4) 0.5000 0.0362(13) Uani 1 4 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'
Cr Cr 0.3209 0.6236 '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'
Zn Zn 0.2839 1.4301 '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 101.1(3) . 9
O1 Zn1 N1 109.77(11) . 4_557
O1 Zn1 N1 109.77(11) 9 4_557
O1 Zn1 N1 109.77(11) . .
O1 Zn1 N1 109.77(11) 9 .
N1 Zn1 N1 115.7(3) 4_557 .
C2 C1 C2 121.5(6) . 2_567
C2 C1 H1 119.2 . .
C2 C1 H1 119.2 2_567 .
C1 C2 C1 118.5(6) . 3_665
C1 C2 C3 121.6(6) . .
C1 C2 C3 119.9(5) 3_665 .
O2 C3 O1 124.7(5) . .
O2 C3 C2 120.0(6) . .
O1 C3 C2 115.3(5) . .
C5 C4 N1 122.5(11) . .
C5 C4 H4 118.7 . .
N1 C4 H4 118.7 . .
C6 C5 C4 119.3(11) . .
C6 C5 H5 120.3 . .
C4 C5 H5 120.3 . .
C5 C6 C5 110.4(16) 9 .
C5 C6 C7 36.4(10) 9 .
C5 C6 C7 118.4(8) . .
C5 C6 C7 118.4(8) 9 9
C5 C6 C7 36.4(10) . 9
C7 C6 C7 102.5(15) . 9
C5 C6 C9 119.0(6) 9 .
C5 C6 C9 119.0(6) . .
C7 C6 C9 122.6(7) . .
C7 C6 C9 122.6(7) 9 .
C8 C7 C6 119.7(12) . .
C8 C7 H7 120.1 . .
C6 C7 H7 120.1 . .
C7 C8 N1 125.4(11) . .
C7 C8 H8 117.3 . .
N1 C8 H8 117.3 . .
O3 C9 O3 126.9(7) . 9
O3 C9 C6 116.6(4) . .
O3 C9 C6 116.6(3) 9 .
C8 N1 C8 101.9(15) 9 .
C8 N1 C4 35.8(8) 9 .
C8 N1 C4 114.3(8) . .
C8 N1 C4 114.3(8) 9 9
C8 N1 C4 35.8(8) . 9
C4 N1 C4 103.8(13) . 9
C8 N1 Zn1 122.9(7) 9 .
C8 N1 Zn1 122.9(7) . .
C4 N1 Zn1 122.8(6) . .
C4 N1 Zn1 122.8(6) 9 .
C3 O1 Zn1 116.5(4) . .
O4 Cr1 O3 94.28(11) . .
O4 Cr1 O3 94.28(11) . 7
O3 Cr1 O3 86.3(3) . 7
O4 Cr1 O3 94.28(11) . 10_556
O3 Cr1 O3 171.4(2) . 10_556
O3 Cr1 O3 93.1(3) 7 10_556
O4 Cr1 O3 94.28(11) . 4_556
O3 Cr1 O3 93.1(3) . 4_556
O3 Cr1 O3 171.4(2) 7 4_556
O3 Cr1 O3 86.3(3) 10_556 4_556
O4 Cr1 O5 180.0(3) . .
O3 Cr1 O5 85.72(11) . .
O3 Cr1 O5 85.72(11) 7 .
O3 Cr1 O5 85.72(11) 10_556 .
O3 Cr1 O5 85.72(11) 4_556 .
C9 O3 Cr1 132.2(4) . .
Cr1 O4 Cr1 120.0 3 2_556
Cr1 O4 Cr1 120.0 3 .
Cr1 O4 Cr1 120.0 2_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.927(4) .
Zn1 O1 1.927(4) 9
Zn1 N1 2.014(6) 4_557
Zn1 N1 2.014(6) .
C1 C2 1.376(8) .
C1 C2 1.378(8) 2_567
C1 H1 0.9500 .
C2 C1 1.378(8) 3_665
C2 C3 1.520(7) .
C3 O2 1.220(7) .
C3 O1 1.243(8) .
C4 C5 1.367(19) .
C4 N1 1.374(10) .
C4 H4 0.9500 .
C5 C6 1.341(17) .
C5 H5 0.9500 .
C6 C5 1.341(17) 9
C6 C7 1.401(13) .
C6 C7 1.401(13) 9
C6 C9 1.494(10) .
C7 C8 1.27(2) .
C7 H7 0.9500 .
C8 N1 1.368(16) .
C8 H8 0.9500 .
C9 O3 1.259(5) .
C9 O3 1.259(5) 9
N1 C8 1.368(16) 9
N1 C4 1.374(10) 9
Cr1 O4 1.9264(16) .
Cr1 O3 1.957(3) .
Cr1 O3 1.957(3) 7
Cr1 O3 1.957(3) 10_556
Cr1 O3 1.957(3) 4_556
Cr1 O5 2.007(6) .
O4 Cr1 1.9264(16) 3
O4 Cr1 1.9264(16) 2_556
