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#$Date: 2024-10-06 10:33:53 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295230 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/91/7249147.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_7249147
loop_
_publ_author_name
'Feng, Shaoqiang'
'Xie, Fengxia'
'Wan, Chengan'
'Zhang, Feng'
'Feng, Lei'
'Wen, Chen'
'Liang, Xiaoqiang'
_publ_section_title
;
 Impact of the number of hydrogen bonds on proton conductivity in
 metallo-hydrogen-bonded organic frameworks: the more the number of
 hydrogen bonds, the better the proton conductivity at the maximum
 relative humidity
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              4855
_journal_page_last               4870
_journal_paper_doi               10.1039/D4CE00480A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C16 H22 N8 Ni O4'
_chemical_formula_sum            'C16 H22 N8 Ni O4'
_chemical_formula_weight         449.11
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2024-04-17 deposited with the CCDC.	2024-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.289(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9347(15)
_cell_length_b                   7.1605(8)
_cell_length_c                   8.9773(10)
_cell_measurement_reflns_used    3779
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      60.70
_cell_measurement_theta_min      3.02
_cell_volume                     891.94(17)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3779
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.712
_diffrn_reflns_theta_min         4.303
_exptl_absorpt_coefficient_mu    6.193
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             468
_exptl_crystal_preparation       'proton conduction'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0350
_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)+(0.0450P)²+0.6649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1047
_reflns_number_total             1102
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00480a2.cif
_cod_data_source_block           Ni-Ci-NH3
_cod_depositor_comments
'Adding full bibliography for 7249146--7249147.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7249147
_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_min   0.747
_shelx_estimated_absorpt_t_max   0.886
_shelxl_version_number           2014-3
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
C1 C 0.5888(2) 0.5000 0.3310(3) 0.0222(6) Uani 1 2 d S T P . .
H1 H 0.5263 0.5000 0.3655 0.027 Uiso 1 2 calc R U P . .
C2 C 0.67552(18) 0.5000 0.4253(3) 0.0163(5) Uani 1 2 d S T P . .
C3 C 0.74818(19) 0.5000 0.3268(3) 0.0163(5) Uani 1 2 d S T P . .
C4 C 0.84648(19) 0.5000 0.3800(3) 0.0202(6) Uani 1 2 d S T P . .
H4 H 0.8958 0.5000 0.3136 0.024 Uiso 1 2 calc R U P . .
C5 C 0.86764(19) 0.5000 0.5325(3) 0.0199(6) Uani 1 2 d S T P . .
H5 H 0.9334 0.5000 0.5715 0.024 Uiso 1 2 calc R U P . .
C6 C 0.69997(19) 0.5000 0.5807(3) 0.0182(5) Uani 1 2 d S T P . .
H6 H 0.6510 0.5000 0.6477 0.022 Uiso 1 2 calc R U P . .
C7 C 0.79552(19) 0.5000 0.6344(3) 0.0157(5) Uani 1 2 d S T P . .
C8 C 0.82456(19) 0.5000 0.8006(3) 0.0178(5) Uani 1 2 d S T P . .
H2 H 0.730(3) 0.5000 0.090(5) 0.042(11) Uiso 1 2 d S . P . .
N1 N 0.60559(16) 0.5000 0.1890(3) 0.0188(5) Uani 1 2 d S T P . .
N2 N 0.70351(16) 0.5000 0.1855(3) 0.0186(5) Uani 1 2 d S T P . .
N1W N 0.57720(11) 0.7144(2) -0.09523(17) 0.0182(3) Uani 1 1 d . . . . .
H1W1 H 0.5403 0.7652 -0.1738 0.027 Uiso 1 1 calc R U . . .
H1W2 H 0.6321 0.6667 -0.1277 0.027 Uiso 1 1 calc R U . . .
H1W3 H 0.5927 0.8041 -0.0254 0.027 Uiso 1 1 calc R U . . .
Ni1 Ni 0.5000 0.5000 0.0000 0.01416(18) Uani 1 4 d S T P . .
O1 O 0.75761(14) 0.5000 0.8875(2) 0.0250(5) Uani 1 2 d S T P . .
O2 O 0.91284(14) 0.5000 0.8431(2) 0.0268(5) Uani 1 2 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 0.0137 0.0067 '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 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -1.3357 3.2904 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 '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
_geom_angle_publ_flag
N1 C1 C2 111.2(2) . . ?
N1 C1 H1 124.4 . . ?
C2 C1 H1 124.4 . . ?
C3 C2 C6 120.1(2) . . ?
C3 C2 C1 104.5(2) . . ?
C6 C2 C1 135.4(2) . . ?
N2 C3 C2 107.0(2) . . ?
N2 C3 C4 131.5(2) . . ?
C2 C3 C4 121.5(2) . . ?
C5 C4 C3 116.8(2) . . ?
C5 C4 H4 121.6 . . ?
C3 C4 H4 121.6 . . ?
C4 C5 C7 122.9(3) . . ?
C4 C5 H5 118.6 . . ?
C7 C5 H5 118.6 . . ?
C7 C6 C2 119.1(2) . . ?
C7 C6 H6 120.4 . . ?
C2 C6 H6 120.4 . . ?
C6 C7 C5 119.6(2) . . ?
C6 C7 C8 120.7(2) . . ?
C5 C7 C8 119.7(2) . . ?
O2 C8 O1 124.7(3) . . ?
O2 C8 C7 117.8(2) . . ?
O1 C8 C7 117.5(2) . . ?
C1 N1 N2 106.8(2) . . ?
C1 N1 Ni1 126.63(19) . . ?
N2 N1 Ni1 126.60(17) . . ?
C3 N2 N1 110.5(2) . . ?
C3 N2 H2 130(2) . . ?
N1 N2 H2 119(2) . . ?
Ni1 N1W H1W1 109.5 . . ?
Ni1 N1W H1W2 109.5 . . ?
H1W1 N1W H1W2 109.5 . . ?
Ni1 N1W H1W3 109.5 . . ?
H1W1 N1W H1W3 109.5 . . ?
H1W2 N1W H1W3 109.5 . . ?
N1W Ni1 N1W 180.0 . 5_665 ?
N1W Ni1 N1W 93.88(9) . 6_565 ?
N1W Ni1 N1W 86.12(9) 5_665 6_565 ?
N1W Ni1 N1W 86.12(9) . 2_655 ?
N1W Ni1 N1W 93.88(9) 5_665 2_655 ?
N1W Ni1 N1W 180.00(7) 6_565 2_655 ?
N1W Ni1 N1 91.02(6) . 5_665 ?
N1W Ni1 N1 88.98(6) 5_665 5_665 ?
N1W Ni1 N1 91.02(6) 6_565 5_665 ?
N1W Ni1 N1 88.98(6) 2_655 5_665 ?
N1W Ni1 N1 88.98(6) . . ?
N1W Ni1 N1 91.02(6) 5_665 . ?
N1W Ni1 N1 88.98(6) 6_565 . ?
N1W Ni1 N1 91.02(6) 2_655 . ?
N1 Ni1 N1 180.0 5_665 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.317(4) . ?
C1 C2 1.410(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.404(3) . ?
C2 C6 1.405(4) . ?
C3 N2 1.361(4) . ?
C3 C4 1.408(4) . ?
C4 C5 1.374(4) . ?
C4 H4 0.9500 . ?
C5 C7 1.420(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.374(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.510(4) . ?
C8 O2 1.254(3) . ?
C8 O1 1.270(3) . ?
N1 N2 1.368(3) . ?
N1 Ni1 2.141(2) . ?
N2 H2 0.96(4) . ?
N1W Ni1 2.1010(15) . ?
N1W H1W1 0.9100 . ?
N1W H1W2 0.9100 . ?
N1W H1W3 0.9100 . ?
Ni1 N1W 2.1010(15) 5_665 ?
Ni1 N1W 2.1010(16) 6_565 ?
Ni1 N1W 2.1010(15) 2_655 ?
Ni1 N1 2.141(2) 5_665 ?
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
_geom_torsion_publ_flag
N1 C1 C2 C3 0.000(0) . . . . ?
N1 C1 C2 C6 180.000(0) . . . . ?
C6 C2 C3 N2 180.000(0) . . . . ?
C1 C2 C3 N2 0.000(0) . . . . ?
C6 C2 C3 C4 0.000(0) . . . . ?
C1 C2 C3 C4 180.000(0) . . . . ?
N2 C3 C4 C5 180.000(0) . . . . ?
C2 C3 C4 C5 0.000(0) . . . . ?
C3 C4 C5 C7 0.000(1) . . . . ?
C3 C2 C6 C7 0.000(1) . . . . ?
C1 C2 C6 C7 180.000(0) . . . . ?
C2 C6 C7 C5 0.000(1) . . . . ?
C2 C6 C7 C8 180.000(0) . . . . ?
C4 C5 C7 C6 0.000(1) . . . . ?
C4 C5 C7 C8 180.000(0) . . . . ?
C6 C7 C8 O2 180.000(1) . . . . ?
C5 C7 C8 O2 0.000(1) . . . . ?
C6 C7 C8 O1 0.000(1) . . . . ?
C5 C7 C8 O1 180.000(0) . . . . ?
C2 C1 N1 N2 0.000(0) . . . . ?
C2 C1 N1 Ni1 180.000(0) . . . . ?
C2 C3 N2 N1 0.000(0) . . . . ?
C4 C3 N2 N1 180.000(0) . . . . ?
C1 N1 N2 C3 0.000(0) . . . . ?
Ni1 N1 N2 C3 180.000(0) . . . . ?
