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#$Date: 2019-11-10 00:56:00 +0200 (Sun, 10 Nov 2019) $
#$Revision: 225476 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/53/4515311.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_4515311
loop_
_publ_author_name
'Zhang, Jindan'
'Ouyang, Jun'
'Ye, Yingxiang'
'Li, Ziyin'
'Lin, Quanjie'
'Chen, Ting'
'Zhang, Zhangjing'
'Xiang, Shengchang'
_publ_section_title
;
 Mixed-Valence Cobalt(II/III) Metal-Organic Framework for Ammonia Sensing
 with Naked-Eye Color Switching.
;
_journal_issue                   32
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              27465
_journal_page_last               27471
_journal_paper_doi               10.1021/acsami.8b07770
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         '0.5(C42 H24 Co2 N26), 6(H1.5 N0.5)'
_chemical_formula_sum            'C21 H21 Co N16'
_chemical_formula_weight         556.47
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.3316(7)
_cell_length_b                   16.3316(7)
_cell_length_c                   7.5701(3)
_cell_measurement_reflns_used    1042
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      65.2920
_cell_measurement_theta_min      5.3900
_cell_volume                     1748.60(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6370
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         73.812
_diffrn_reflns_theta_min         5.417
_exptl_absorpt_coefficient_mu    4.126
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_description       flake
_exptl_crystal_F_000             572
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1330P)²+3.3780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                557
_reflns_number_total             706
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am8b07770_si_002.cif
_cod_data_source_block           FJU-56-NH3
_cod_original_cell_volume        1748.60(17)
_cod_database_code               4515311
_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, All N(H,H) groups
2. Others
 Fixed Sof: C4(0.5) H4(0.5) C3(0.5) H3(0.5) H4a(0.25)
3.a Riding coordinates:
 C4(H4), C3(H3), N4(H4a,H4b)
;
_shelx_shelxl_version_number     2014/7
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, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, 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'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -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
Co1 Co 0.0000 0.0000 0.0000 0.0236(6) Uani 1 12 d S T P
N1 N 0.1230(3) 0.06151(15) 0.1636(5) 0.0302(10) Uani 1 2 d S T P
N3 N 0.6667 0.3333 0.2500 0.049(4) Uani 1 12 d S T P
N2 N 0.2113(3) 0.10564(16) 0.1035(6) 0.0354(11) Uani 1 2 d S T P
C5 C 0.5663(5) 0.2832(3) 0.2500 0.0366(18) Uani 1 4 d S T P
C2 C 0.3691(6) 0.1845(3) 0.2500 0.0353(17) Uani 1 4 d S T P
C1 C 0.2642(6) 0.1321(3) 0.2500 0.0338(17) Uani 1 4 d S T P
C4 C 0.5171(7) 0.3095(10) 0.155(2) 0.116(7) Uani 0.5 1 d . . .
H4 H 0.5501 0.3654 0.0835 0.139 Uiso 0.5 1 d R . .
C3 C 0.4164(7) 0.2577(10) 0.148(2) 0.104(6) Uani 0.5 1 d . . .
H3 H 0.3829 0.2766 0.0687 0.125 Uiso 0.5 1 d R . .
N4 N 0.2885(6) 0.1442(3) -0.2500 0.116(6) Uani 1 4 d S T P
H4A H 0.3257 0.2072 -0.2500 0.139 Uiso 0.5 2 d RS T P
H4B H 0.2514 0.1257 -0.1533 0.139 Uiso 1 2 d R . .
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'
Co Co -2.3653 3.6143 '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'
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
N1 Co1 N1 89.74(16) 13 15
N1 Co1 N1 89.74(16) 15 17
N1 Co1 N1 90.26(16) 13 5
N1 Co1 N1 89.74(16) 3 5
N1 Co1 N1 90.26(16) 3 17
N1 Co1 N1 90.26(16) 17 .
N1 Co1 N1 89.74(16) 13 17
N1 Co1 N1 90.26(16) 13 3
N1 Co1 N1 89.74(16) 3 .
N1 Co1 N1 90.26(16) 15 .
N1 Co1 N1 89.74(16) 5 .
N1 Co1 N1 180.0(3) 15 3
N1 Co1 N1 180.0(3) 17 5
N1 Co1 N1 90.26(16) 15 5
N1 Co1 N1 180.00(13) 13 .
N1 N1 Co1 125.45(11) 16_556 .
N1 N1 N2 110.0(3) 16_556 .
N2 N1 Co1 124.5(3) . .
C5 N3 C5 120.000(1) 3_655 14_666
C5 N3 C5 119.999(2) 14_666 .
C5 N3 C5 120.001(1) 3_655 .
N1 N2 C1 104.0(5) . .
C4 C5 N3 122.3(6) 16_556 .
C4 C5 N3 122.3(6) 20 .
C4 C5 N3 122.3(6) 12 .
C4 C5 N3 122.3(6) . .
C4 C5 C4 115.4(11) 16_556 20
C4 C5 C4 79.4(15) . 20
C4 C5 C4 67.2(16) . 16_556
C4 C5 C4 115.4(11) . 12
C4 C5 C4 67.2(16) 20 12
C4 C5 C4 79.4(15) 16_556 12
C3 C2 C1 120.9(6) 16_556 .
C3 C2 C1 120.9(6) 12 .
C3 C2 C1 120.9(6) 20 .
C3 C2 C1 120.9(6) . .
C3 C2 C3 72.7(16) 12 20
C3 C2 C3 72.7(16) 16_556 .
C3 C2 C3 118.2(11) . 12
C3 C2 C3 76.8(15) . 20
C3 C2 C3 118.2(11) 16_556 20
C3 C2 C3 76.8(15) 16_556 12
N2 C1 N2 112.0(7) 16_556 .
N2 C1 C2 124.0(3) 16_556 .
N2 C1 C2 124.0(3) . .
C5 C4 C4 50.3(8) . 20
C5 C4 C4 56.4(8) . 16_556
C5 C4 H4 118.5 . .
C5 C4 C3 122.9(11) . .
C4 C4 C4 90.002(1) 16_556 20
C4 C4 H4 124.2 16_556 .
C4 C4 H4 132.0 20 .
C3 C4 C4 89.1(9) . 20
C3 C4 C4 92.0(9) . 16_556
C3 C4 H4 118.6 . .
C2 C3 C4 120.2(10) . .
C2 C3 C3 51.6(8) . 20
C2 C3 C3 53.7(8) . 16_556
C2 C3 H3 119.6 . .
C4 C3 C3 90.9(9) . 20
C4 C3 C3 88.0(9) . 16_556
C4 C3 H3 120.3 . .
C3 C3 C3 90.000(1) 16_556 20
C3 C3 H3 127.3 20 .
C3 C3 H3 128.7 16_556 .
H4A N4 H4B 110.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.136(4) 13
Co1 N1 2.136(4) 17
Co1 N1 2.136(4) 3
Co1 N1 2.136(4) .
Co1 N1 2.136(4) 5
Co1 N1 2.136(4) 15
N1 N1 1.308(8) 16_556
N1 N2 1.329(6) .
N3 C5 1.419(8) 3_655
N3 C5 1.419(8) 14_666
N3 C5 1.419(8) .
N2 C1 1.338(6) .
C5 C4 1.304(14) .
C5 C4 1.304(14) 16_556
C5 C4 1.304(14) 20
C5 C4 1.304(14) 12
C2 C1 1.484(11) .
C2 C3 1.303(13) 16_556
C2 C3 1.303(13) 20
C2 C3 1.303(13) 12
C2 C3 1.303(13) .
C1 N2 1.338(6) 16_556
C4 C4 1.66(3) 20
C4 C4 1.44(3) 16_556
C4 H4 0.9599 .
C4 C3 1.425(14) .
C3 C3 1.54(3) 16_556
C3 C3 1.62(3) 20
C3 H3 0.9602 .
N4 H4A 0.8959 .
N4 H4B 0.9001 .
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
Co1 N1 N2 C1 180.000(0) . .
N1 N1 N2 C1 0.000(1) 16_556 .
N1 N2 C1 N2 0.004(2) . 16_556
N1 N2 C1 C2 180.000(1) . .
N3 C5 C4 C4 121.7(10) . 20
N3 C5 C4 C4 -114.9(8) . 16_556
N3 C5 C4 C3 177.5(13) . .
C5 N3 C5 C4 139.1(10) 14_666 20
C5 N3 C5 C4 -40.9(10) 3_655 20
C5 N3 C5 C4 40.9(10) 14_666 .
C5 N3 C5 C4 139.1(10) 3_655 16_556
C5 N3 C5 C4 40.9(10) 3_655 12
C5 N3 C5 C4 -139.1(10) 3_655 .
C5 N3 C5 C4 -40.9(10) 14_666 16_556
C5 N3 C5 C4 -139.1(10) 14_666 12
C5 C4 C3 C2 5(3) . .
C5 C4 C3 C3 50.4(15) . 16_556
C5 C4 C3 C3 -39.5(16) . 20
C1 C2 C3 C4 177.6(12) . .
C1 C2 C3 C3 -118.3(9) . 20
C1 C2 C3 C3 116.1(8) . 16_556
C4 C5 C4 C4 -123.5(7) 16_556 20
C4 C5 C4 C4 65.1(8) 12 16_556
C4 C5 C4 C4 -58.3(10) 12 20
C4 C5 C4 C4 123.5(7) 20 16_556
C4 C5 C4 C3 56(2) 20 .
C4 C5 C4 C3 -67.7(19) 16_556 .
C4 C5 C4 C3 -2.5(13) 12 .
C4 C4 C3 C2 -45.1(15) 16_556 .
C4 C4 C3 C2 44.9(14) 20 .
C4 C4 C3 C3 0.000(0) 20 20
C4 C4 C3 C3 89.97(4) 20 16_556
C4 C4 C3 C3 -0.002(1) 16_556 16_556
C4 C4 C3 C3 -89.97(4) 16_556 20
C3 C2 C1 N2 -133.7(10) 12 .
C3 C2 C1 N2 133.7(10) 20 16_556
C3 C2 C1 N2 -46.3(10) 20 .
C3 C2 C1 N2 46.3(10) 12 16_556
C3 C2 C1 N2 133.7(10) 16_556 .
C3 C2 C1 N2 46.3(10) . .
C3 C2 C1 N2 -46.3(10) 16_556 16_556
C3 C2 C1 N2 -133.7(10) . 16_556
C3 C2 C3 C4 -2.4(12) 12 .
C3 C2 C3 C4 -64.2(19) 20 .
C3 C2 C3 C4 61.5(18) 16_556 .
C3 C2 C3 C3 61.7(9) 12 20
C3 C2 C3 C3 125.6(8) 16_556 20
C3 C2 C3 C3 -125.6(8) 20 16_556
C3 C2 C3 C3 -63.9(8) 12 16_556
