#------------------------------------------------------------------------------
#$Date: 2021-09-06 13:20:05 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268635 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/30/7243048.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_7243048
loop_
_publ_author_name
'Zhou, Chuan-Cong'
'Liu, Hou-Ting'
'Ding, Li'
'Lu, Jing'
'Wang, Su-Na'
'Li, Yun-Wu'
_publ_section_title
;
 Proton conductivities of four low dimensional MOFs: affected by the
 amount of chelated ligands
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              5106
_journal_page_last               5115
_journal_paper_doi               10.1039/D1CE00589H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C28 H44 N2 Ni3 O28'
_chemical_formula_sum            'C28 H44 N2 Ni3 O28'
_chemical_formula_weight         1032.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                114.548(12)
_cell_angle_beta                 94.882(12)
_cell_angle_gamma                103.487(12)
_cell_formula_units_Z            1
_cell_length_a                   7.0276(11)
_cell_length_b                   11.7785(14)
_cell_length_c                   13.2567(17)
_cell_measurement_reflns_used    1399
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.6340
_cell_measurement_theta_min      4.2620
_cell_volume                     949.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.1495
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5797
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.240
_diffrn_reflns_theta_max         67.240
_diffrn_reflns_theta_min         3.746
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87426
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       block
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3381
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1223P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2207
_refine_ls_wR_factor_ref         0.2572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2160
_reflns_number_total             3381
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00589h2.cif
_cod_data_source_block           exp_10877
_cod_depositor_comments
'Adding full bibliography for 7243047--7243050.cif.'
_cod_original_cell_volume        949.8(2)
_cod_database_code               7243048
_shelx_shelxl_version_number     2018/3
_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   0.813
_shelx_estimated_absorpt_t_max   0.833
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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
Ni1 Ni 0.500000 1.000000 0.500000 0.0123(4) Uani 1 2 d S . P . .
Ni2 Ni 0.500000 0.500000 0.000000 0.0146(5) Uani 1 2 d S . P . .
Ni3 Ni 0.000000 1.000000 1.000000 0.0318(6) Uani 1 2 d S . P . .
N1 N 0.4230(9) 0.8054(5) 0.4644(4) 0.0104(12) Uani 1 1 d . . . . .
O1 O 0.3815(9) 0.3778(5) 0.1860(4) 0.0227(12) Uani 1 1 d . . . . .
O2 O 0.4638(9) 0.5563(5) 0.1581(4) 0.0224(12) Uani 1 1 d . . . . .
O3 O 0.0757(8) 0.1984(5) 0.5436(4) 0.0217(12) Uani 1 1 d . . . . .
O4 O 0.0143(9) 0.2531(5) 0.7170(4) 0.0230(13) Uani 1 1 d . . . . .
O5 O 0.0859(9) 0.7223(5) 0.9710(4) 0.0227(13) Uani 1 1 d . . . . .
O6 O 0.0667(10) 0.8470(5) 0.8834(5) 0.0305(14) Uani 1 1 d . U . . .
O7 O 0.2485(8) 1.0180(5) 0.5715(4) 0.0197(12) Uani 1 1 d . . . . .
H7A H 0.176807 0.935170 0.566589 0.030 Uiso 1 1 d R U . . .
H7C H 0.163467 1.044938 0.531039 0.030 Uiso 1 1 d R U . . .
O8 O 0.3217(8) 0.9510(5) 0.3422(4) 0.0224(12) Uani 1 1 d . . . . .
H8A H 0.261004 0.858095 0.302710 0.034 Uiso 1 1 d R U . . .
H8C H 0.404195 0.978615 0.297610 0.034 Uiso 1 1 d R U . . .
O9 O 0.4573(9) 0.6733(5) 0.0055(4) 0.0233(12) Uani 1 1 d . . . . .
H9B H 0.327337 0.677459 0.020714 0.035 Uiso 1 1 d R U . . .
H9C H 0.557787 0.747056 0.064674 0.035 Uiso 1 1 d R U . . .
O10 O 0.1967(8) 0.4078(6) -0.0560(5) 0.0284(14) Uani 1 1 d . . . . .
H10B H 0.165145 0.367177 -0.137325 0.043 Uiso 1 1 d R U . . .
H10C H 0.159547 0.342456 -0.030035 0.043 Uiso 1 1 d R U . . .
O11 O 0.3024(12) 1.1013(6) 1.0796(6) 0.052(2) Uani 1 1 d . . . . .
H11A H 0.384752 1.049873 1.040836 0.078 Uiso 1 1 d R U . . .
H11C H 0.321711 1.116019 1.157076 0.078 Uiso 1 1 d R U . . .
O12 O 0.0318(13) 1.0794(6) 0.8882(5) 0.053(2) Uani 1 1 d . . . . .
H12A H 0.065523 1.020463 0.821536 0.079 Uiso 1 1 d R U . . .
H12B H -0.092287 1.093024 0.867661 0.079 Uiso 1 1 d R U . . .
O13 O 0.1839(12) 0.1537(7) 0.3344(6) 0.053(2) Uani 1 1 d . . . . .
H13C H 0.137053 0.157664 0.392456 0.064 Uiso 1 1 d R U . . .
H13A H 0.304595 0.152614 0.343065 0.064 Uiso 1 1 d R U . . .
O14 O 0.521(2) 0.9781(14) 0.1567(13) 0.046(4) Uani 0.5 1 d . . P A 1
H14C H 0.469792 0.969413 0.209800 0.056 Uiso 0.5 1 d R U P A 1
H14A H 0.513972 0.903564 0.104350 0.056 Uiso 0.5 1 d R U P A 1
O14' O 0.615(4) 0.940(3) 0.178(3) 0.142(11) Uani 0.5 1 d . U P B 2
H14G H 0.579393 0.861126 0.127163 0.171 Uiso 0.5 1 d R U P B 2
H14H H 0.542735 0.945878 0.227143 0.171 Uiso 0.5 1 d R U P B 2
C1 C 0.4142(10) 0.4981(7) 0.2169(6) 0.0115(14) Uani 1 1 d . U . . .
C2 C 0.3915(10) 0.5856(6) 0.3332(6) 0.0099(13) Uani 1 1 d . . . . .
C3 C 0.4374(10) 0.7188(7) 0.3636(6) 0.0155(15) Uani 1 1 d . . . . .
H3 H 0.479518 0.748215 0.311726 0.019 Uiso 1 1 calc R U . . .
C4 C 0.3659(11) 0.7621(7) 0.5386(6) 0.0144(15) Uani 1 1 d . . . . .
H4 H 0.363055 0.823242 0.610360 0.017 Uiso 1 1 calc R U . . .
C5 C 0.3099(10) 0.6295(7) 0.5149(6) 0.0098(13) Uani 1 1 d . . . . .
C6 C 0.3306(10) 0.5425(6) 0.4110(6) 0.0102(13) Uani 1 1 d . . . . .
H6 H 0.303523 0.454365 0.393066 0.012 Uiso 1 1 calc R U . . .
C7 C 0.2349(10) 0.5919(7) 0.6026(6) 0.0104(14) Uani 1 1 d . . . . .
C8 C 0.1987(10) 0.6809(7) 0.7004(6) 0.0127(14) Uani 1 1 d . U . . .
H8 H 0.224129 0.767374 0.713085 0.015 Uiso 1 1 calc R U . . .
C9 C 0.1255(10) 0.6457(6) 0.7807(6) 0.0115(14) Uani 1 1 d . U . . .
C10 C 0.0885(10) 0.5167(7) 0.7621(6) 0.0111(14) Uani 1 1 d . . . . .
H10A H 0.042584 0.492377 0.816065 0.013 Uiso 1 1 calc R U . . .
C11 C 0.1194(10) 0.4237(7) 0.6633(6) 0.0113(14) Uani 1 1 d . . . . .
C12 C 0.1916(10) 0.4605(6) 0.5839(5) 0.0098(13) Uani 1 1 d . . . . .
H12 H 0.211716 0.398168 0.517646 0.012 Uiso 1 1 calc R U . . .
C13 C 0.0911(11) 0.7451(7) 0.8865(6) 0.0174(16) Uani 1 1 d . U . . .
C14 C 0.0644(10) 0.2818(6) 0.6398(6) 0.0115(14) Uani 1 1 d . U . . .
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'
Ni Ni -3.0029 0.5091 '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 Ni1 N1 180.00(10) . 2_676 ?
N1 Ni1 O7 90.3(2) . 2_676 ?
N1 Ni1 O7 89.7(2) 2_676 2_676 ?
N1 Ni1 O7 89.7(2) . . ?
N1 Ni1 O7 90.3(2) 2_676 . ?
O7 Ni1 O7 180.0 2_676 . ?
N1 Ni1 O8 90.1(2) . . ?
N1 Ni1 O8 89.9(2) 2_676 . ?
O7 Ni1 O8 91.7(2) 2_676 . ?
O7 Ni1 O8 88.3(2) . . ?
N1 Ni1 O8 89.9(2) . 2_676 ?
N1 Ni1 O8 90.1(2) 2_676 2_676 ?
O7 Ni1 O8 88.3(2) 2_676 2_676 ?
O7 Ni1 O8 91.7(2) . 2_676 ?
O8 Ni1 O8 180.00(18) . 2_676 ?
O2 Ni2 O2 180.0 2_665 . ?
O2 Ni2 O10 90.6(2) 2_665 . ?
O2 Ni2 O10 89.4(2) . . ?
O2 Ni2 O10 89.4(2) 2_665 2_665 ?
O2 Ni2 O10 90.6(2) . 2_665 ?
O10 Ni2 O10 180.0 . 2_665 ?
O2 Ni2 O9 89.9(2) 2_665 2_665 ?
O2 Ni2 O9 90.1(2) . 2_665 ?
O10 Ni2 O9 89.5(2) . 2_665 ?
O10 Ni2 O9 90.5(2) 2_665 2_665 ?
O2 Ni2 O9 90.1(2) 2_665 . ?
O2 Ni2 O9 89.9(2) . . ?
O10 Ni2 O9 90.5(2) . . ?
O10 Ni2 O9 89.5(2) 2_665 . ?
O9 Ni2 O9 180.0(3) 2_665 . ?
O6 Ni3 O6 180.0 . 2_577 ?
O6 Ni3 O12 93.9(2) . 2_577 ?
O6 Ni3 O12 86.1(2) 2_577 2_577 ?
O6 Ni3 O12 86.1(2) . . ?
O6 Ni3 O12 93.9(2) 2_577 . ?
O12 Ni3 O12 180.0 2_577 . ?
O6 Ni3 O11 86.9(3) . 2_577 ?
O6 Ni3 O11 93.1(3) 2_577 2_577 ?
O12 Ni3 O11 89.0(3) 2_577 2_577 ?
O12 Ni3 O11 91.0(3) . 2_577 ?
O6 Ni3 O11 93.1(3) . . ?
O6 Ni3 O11 86.9(3) 2_577 . ?
O12 Ni3 O11 91.0(3) 2_577 . ?
O12 Ni3 O11 89.0(3) . . ?
O11 Ni3 O11 180.0(3) 2_577 . ?
C4 N1 C3 118.2(6) . . ?
C4 N1 Ni1 123.3(4) . . ?
C3 N1 Ni1 118.4(5) . . ?
C1 O2 Ni2 134.6(5) . . ?
C13 O6 Ni3 130.6(5) . . ?
O1 C1 O2 125.9(6) . . ?
O1 C1 C2 119.9(6) . . ?
O2 C1 C2 114.1(6) . . ?
C6 C2 C3 118.7(6) . . ?
C6 C2 C1 124.3(6) . . ?
C3 C2 C1 117.0(6) . . ?
N1 C3 C2 122.2(6) . . ?
N1 C4 C5 123.9(6) . . ?
C6 C5 C4 116.5(6) . . ?
C6 C5 C7 124.4(6) . . ?
C4 C5 C7 119.0(6) . . ?
C5 C6 C2 120.3(6) . . ?
C8 C7 C12 118.0(6) . . ?
C8 C7 C5 122.0(6) . . ?
C12 C7 C5 119.9(6) . . ?
C7 C8 C9 122.1(6) . . ?
C10 C9 C8 119.0(6) . . ?
C10 C9 C13 120.3(6) . . ?
C8 C9 C13 120.7(6) . . ?
C9 C10 C11 120.5(6) . . ?
C12 C11 C10 119.7(6) . . ?
C12 C11 C14 120.2(6) . . ?
C10 C11 C14 120.1(6) . . ?
C11 C12 C7 120.7(6) . . ?
O5 C13 O6 124.8(7) . . ?
O5 C13 C9 118.7(6) . . ?
O6 C13 C9 116.5(6) . . ?
O4 C14 O3 123.5(6) . . ?
O4 C14 C11 118.5(6) . . ?
O3 C14 C11 118.0(6) . . ?
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
Ni1 N1 2.061(5) . ?
Ni1 N1 2.061(5) 2_676 ?
Ni1 O7 2.088(5) 2_676 ?
Ni1 O7 2.088(5) . ?
Ni1 O8 2.120(5) . ?
Ni1 O8 2.120(5) 2_676 ?
Ni2 O2 1.978(5) 2_665 ?
Ni2 O2 1.978(5) . ?
Ni2 O10 2.062(6) . ?
Ni2 O10 2.062(6) 2_665 ?
Ni2 O9 2.104(5) 2_665 ?
Ni2 O9 2.104(5) . ?
Ni3 O6 2.015(5) . ?
Ni3 O6 2.015(5) 2_577 ?
Ni3 O12 2.057(6) 2_577 ?
Ni3 O12 2.057(6) . ?
Ni3 O11 2.108(8) 2_577 ?
Ni3 O11 2.108(8) . ?
N1 C4 1.333(8) . ?
N1 C3 1.333(9) . ?
O1 C1 1.256(8) . ?
O2 C1 1.255(8) . ?
O3 C14 1.269(8) . ?
O4 C14 1.257(8) . ?
O5 C13 1.257(9) . ?
O6 C13 1.269(9) . ?
C1 C2 1.505(9) . ?
C2 C6 1.383(9) . ?
C2 C3 1.394(10) . ?
C4 C5 1.405(9) . ?
C5 C6 1.379(9) . ?
C5 C7 1.500(9) . ?
C7 C8 1.377(9) . ?
C7 C12 1.413(9) . ?
C8 C9 1.390(9) . ?
C9 C10 1.390(9) . ?
C9 C13 1.490(10) . ?
C10 C11 1.389(10) . ?
C11 C12 1.386(9) . ?
C11 C14 1.511(9) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O7 H7A O3 0.96 2.03 2.735(7) 129.1 2_566 yes
O7 H7C O3 0.96 1.99 2.812(7) 142.3 1_565 yes
O8 H8A O4 0.96 1.99 2.727(7) 131.6 2_566 yes
O8 H8C O14^a 0.96 2.10 3.024(17) 160.5 . yes
O8 H8C O14'^b 0.96 2.24 3.11(3) 149.4 . yes
O9 H9B O5 0.96 2.03 2.842(8) 141.5 1_554 yes
O9 H9C O14^a 0.96 2.57 3.198(15) 123.6 . yes
O9 H9C O14'^b 0.96 2.05 2.88(3) 143.3 . yes
O10 H10B O4 0.96 1.87 2.778(7) 157.2 1_554 yes
O10 H10C O5 0.96 2.07 2.821(8) 133.9 2_566 yes
O11 H11A O14^a 0.96 2.66 3.315(17) 125.8 2_676 yes
O11 H11C O13 0.96 2.53 3.388(10) 149.3 1_566 yes
O12 H12A O13 0.96 2.40 3.019(10) 122.2 2_566 yes
O12 H12A O14'^b 0.96 2.18 2.73(3) 114.9 2_676 yes
O13 H13C O3 0.85 1.97 2.807(9) 168.4 . yes
O13 H13A O8 0.85 2.40 2.813(9) 110.5 1_545 yes
O14^a H14C^a O8 0.85 2.18 3.024(17) 176.2 . yes
O14^a H14A^a O9 0.85 2.38 3.198(15) 160.3 . yes
O14'^b H14G^b O9 0.85 2.04 2.88(3) 172.6 . yes
O14'^b H14H^b O8 0.85 2.26 3.11(3) 173.8 . yes
