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#$Date: 2024-04-27 00:31:41 +0200 (Sat 27 de Apr de 2024) $
#$Revision: 291369 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/85/7248546.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_7248546
loop_
_publ_author_name
'Paul, Anup'
'Gusmão, Filipe'
'Mahmoud, Abdallah G.'
'Hazra, Susanta'
'Rakočević, Lazar'
'Sljukic, Biljana'
'Khan, Rais Ahmad'
'Guedes da Silva, M. Fátima C.'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Catalyzing Towards Clean Energy: Tuning Oxygen Evolution Reaction by
 Amide-Functionalized Co(II) and Ni(II) Pristine Coordination Polymers
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D4CE00179F
_journal_year                    2024
_chemical_formula_moiety         'C24 H20 N6 Ni O8'
_chemical_formula_sum            'C24 H20 N6 Ni O8'
_chemical_formula_weight         579.17
_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
;
2023-11-16 deposited with the CCDC.	2024-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                108.5190(10)
_cell_angle_beta                 90.3980(10)
_cell_angle_gamma                114.6470(10)
_cell_formula_units_Z            1
_cell_length_a                   7.6921(2)
_cell_length_b                   7.8232(2)
_cell_length_c                   10.9612(3)
_cell_measurement_reflns_used    9433
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.95
_cell_volume                     560.99(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22787
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.086
_diffrn_reflns_theta_min         2.952
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       block
_exptl_crystal_F_000             298
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0241
_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)+(0.0301P)²+0.2332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2032
_reflns_number_total             2228
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00179f2.cif
_cod_data_source_block           Ni2
_cod_database_code               7248546
_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   0.754
_shelx_estimated_absorpt_t_max   0.929
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
C1 C -0.4071(3) 0.7279(2) 0.79068(16) 0.0251(4) Uani 1 1 d . . . . .
C2 C -0.5261(2) 0.7424(2) 0.89991(16) 0.0240(3) Uani 1 1 d . . . . .
C3 C -0.4706(3) 0.7304(3) 1.01681(17) 0.0281(4) Uani 1 1 d . . . . .
H3 H -0.355225 0.722494 1.030591 0.034 Uiso 1 1 calc R U . . .
C4 C -0.5867(3) 0.7303(3) 1.11261(17) 0.0291(4) Uani 1 1 d . . . . .
H4 H -0.551882 0.716297 1.189019 0.035 Uiso 1 1 calc R U . . .
C5 C -0.7553(2) 0.7509(3) 1.09530(16) 0.0242(3) Uani 1 1 d . . . . .
C6 C -0.8094(3) 0.7674(3) 0.97981(16) 0.0279(4) Uani 1 1 d . . . . .
H6 H -0.920904 0.783262 0.967951 0.033 Uiso 1 1 calc R U . . .
C7 C -0.6956(3) 0.7600(3) 0.88241(16) 0.0274(4) Uani 1 1 d . . . . .
H7 H -0.733716 0.766932 0.804116 0.033 Uiso 1 1 calc R U . . .
C8 C 0.1217(2) 0.7438(3) 0.20018(16) 0.0250(4) Uani 1 1 d . . . . .
C9 C -0.0971(2) 0.8754(3) 0.30992(16) 0.0226(3) Uani 1 1 d . . . . .
C10 C -0.1995(2) 0.7233(3) 0.35763(16) 0.0244(3) Uani 1 1 d . . . . .
H10 H -0.185183 0.605231 0.329530 0.029 Uiso 1 1 calc R U . . .
C11 C -0.3320(2) 0.9173(3) 0.48307(17) 0.0263(4) Uani 1 1 d . . . . .
H11 H -0.410519 0.933090 0.545635 0.032 Uiso 1 1 calc R U . . .
C12 C -0.1264(2) 1.0466(3) 0.35462(17) 0.0284(4) Uani 1 1 d . . . . .
H12 H -0.061887 1.149657 0.322844 0.034 Uiso 1 1 calc R U . . .
N1 N -0.31888(19) 0.7445(2) 0.44376(13) 0.0230(3) Uani 1 1 d . . . . .
N2 N -0.2432(2) 1.0699(2) 0.44132(15) 0.0300(3) Uani 1 1 d . . . . .
N3 N 0.0259(2) 0.8613(2) 0.21718(14) 0.0280(3) Uani 1 1 d . . . . .
O1 O -0.23908(18) 0.7505(2) 0.81563(13) 0.0360(3) Uani 1 1 d . . . . .
O2 O -0.49222(18) 0.69055(18) 0.67932(11) 0.0284(3) Uani 1 1 d . . . . .
O3 O 0.1073(2) 0.6398(2) 0.26506(13) 0.0381(3) Uani 1 1 d . . . . .
O4 O -0.25513(19) 0.4776(2) 0.55708(14) 0.0314(3) Uani 1 1 d . . . . .
Ni1 Ni -0.500000 0.500000 0.500000 0.02038(10) Uani 1 2 d S . P . .
H03A H 0.067(3) 0.961(3) 0.188(2) 0.031 Uiso 1 1 d . U . . .
H04B H -0.214(3) 0.530(3) 0.635(2) 0.031 Uiso 1 1 d . U . . .
H04A H -0.244(3) 0.374(3) 0.528(2) 0.031 Uiso 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 0.0033 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'
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'
Ni Ni 0.3393 1.1124 '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
O1 C1 O2 125.63(15) . . ?
O1 C1 C2 118.98(15) . . ?
O2 C1 C2 115.39(15) . . ?
C7 C2 C3 119.20(14) . . ?
C7 C2 C1 120.22(15) . . ?
C3 C2 C1 120.54(15) . . ?
C4 C3 C2 120.16(16) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.37(16) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.74(15) . . ?
C6 C5 C8 122.04(15) . 1_456 ?
C4 C5 C8 118.14(15) . 1_456 ?
C7 C6 C5 119.39(16) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C2 C7 C6 121.07(16) . . ?
C2 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
O3 C8 N3 122.61(15) . . ?
O3 C8 C5 121.96(15) . 1_654 ?
N3 C8 C5 115.43(14) . 1_654 ?
C12 C9 C10 116.73(14) . . ?
C12 C9 N3 119.34(15) . . ?
C10 C9 N3 123.89(15) . . ?
N1 C10 C9 120.84(15) . . ?
N1 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
N1 C11 N2 126.13(15) . . ?
N1 C11 H11 116.9 . . ?
N2 C11 H11 116.9 . . ?
N2 C12 C9 122.83(16) . . ?
N2 C12 H12 118.6 . . ?
C9 C12 H12 118.6 . . ?
C11 N1 C10 117.49(14) . . ?
C11 N1 Ni1 121.42(10) . . ?
C10 N1 Ni1 120.82(11) . . ?
C11 N2 C12 115.92(15) . . ?
C8 N3 C9 124.40(14) . . ?
C8 N3 H03A 119.4(13) . . ?
C9 N3 H03A 113.5(13) . . ?
C1 O2 Ni1 130.89(11) . . ?
Ni1 O4 H04B 114.9(15) . . ?
Ni1 O4 H04A 122.2(15) . . ?
H04B O4 H04A 110(2) . . ?
O2 Ni1 O2 180.00(5) 2_466 . ?
O2 Ni1 O4 85.96(5) 2_466 . ?
O2 Ni1 O4 94.04(5) . . ?
O2 Ni1 O4 94.04(5) 2_466 2_466 ?
O2 Ni1 O4 85.96(5) . 2_466 ?
O4 Ni1 O4 180.0 . 2_466 ?
O2 Ni1 N1 91.48(5) 2_466 2_466 ?
O2 Ni1 N1 88.52(5) . 2_466 ?
O4 Ni1 N1 91.17(5) . 2_466 ?
O4 Ni1 N1 88.83(5) 2_466 2_466 ?
O2 Ni1 N1 88.52(5) 2_466 . ?
O2 Ni1 N1 91.48(5) . . ?
O4 Ni1 N1 88.83(5) . . ?
O4 Ni1 N1 91.17(5) 2_466 . ?
N1 Ni1 N1 180.0 2_466 . ?
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 O1 1.246(2) . ?
C1 O2 1.267(2) . ?
C1 C2 1.516(2) . ?
C2 C7 1.385(2) . ?
C2 C3 1.391(2) . ?
C3 C4 1.383(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(2) . ?
C5 C8 1.494(2) 1_456 ?
C6 C7 1.388(2) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O3 1.214(2) . ?
C8 N3 1.372(2) . ?
C9 C12 1.385(2) . ?
C9 C10 1.389(2) . ?
C9 N3 1.404(2) . ?
C10 N1 1.3422(19) . ?
C10 H10 0.9300 . ?
C11 N1 1.329(2) . ?
C11 N2 1.331(2) . ?
C11 H11 0.9300 . ?
C12 N2 1.335(2) . ?
C12 H12 0.9300 . ?
N1 Ni1 2.1257(13) . ?
N3 H03A 0.87(2) . ?
O2 Ni1 2.0376(11) . ?
O4 Ni1 2.0731(13) . ?
O4 H04B 0.81(2) . ?
O4 H04A 0.81(2) . ?
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
O1 C1 C2 C7 166.54(16) . . . . ?
O2 C1 C2 C7 -14.3(2) . . . . ?
O1 C1 C2 C3 -16.0(2) . . . . ?
O2 C1 C2 C3 163.21(16) . . . . ?
C7 C2 C3 C4 1.8(3) . . . . ?
C1 C2 C3 C4 -175.68(16) . . . . ?
C2 C3 C4 C5 -2.8(3) . . . . ?
C3 C4 C5 C6 1.4(3) . . . . ?
C3 C4 C5 C8 178.26(16) . . . 1_456 ?
C4 C5 C6 C7 1.0(3) . . . . ?
C8 C5 C6 C7 -175.78(16) 1_456 . . . ?
C3 C2 C7 C6 0.5(3) . . . . ?
C1 C2 C7 C6 178.06(16) . . . . ?
C5 C6 C7 C2 -1.9(3) . . . . ?
C12 C9 C10 N1 -0.6(2) . . . . ?
N3 C9 C10 N1 -178.20(15) . . . . ?
C10 C9 C12 N2 1.4(3) . . . . ?
N3 C9 C12 N2 179.07(16) . . . . ?
N2 C11 N1 C10 2.8(3) . . . . ?
N2 C11 N1 Ni1 -171.31(14) . . . . ?
C9 C10 N1 C11 -1.3(2) . . . . ?
C9 C10 N1 Ni1 172.85(12) . . . . ?
N1 C11 N2 C12 -2.0(3) . . . . ?
C9 C12 N2 C11 -0.2(3) . . . . ?
O3 C8 N3 C9 0.2(3) . . . . ?
C5 C8 N3 C9 179.76(15) 1_654 . . . ?
C12 C9 N3 C8 155.17(17) . . . . ?
C10 C9 N3 C8 -27.3(3) . . . . ?
O1 C1 O2 Ni1 42.2(2) . . . . ?
C2 C1 O2 Ni1 -136.90(13) . . . . ?
