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#$Date: 2024-04-05 02:27:47 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290945 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/51/7715117.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_7715117
loop_
_publ_author_name
'Heczko, Michał'
'Nowicka, Beata'
_publ_section_title
;
 Switching of magnetic properties by topotactic reaction in a 1D
 CN-bridged Ni(II)-Nb(IV) system.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5788
_journal_page_last               5795
_journal_paper_doi               10.1039/d3dt03891b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C18 H28 Li2 N12 Nb Ni O2'
_chemical_formula_weight         610.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-07 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2706(4)
_cell_length_b                   14.4329(5)
_cell_length_c                   14.6110(5)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.52
_cell_volume                     2578.61(15)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0256
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15907
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.517
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       needle
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0230
_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)+(0.0075P)²+6.7387P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2455
_reflns_number_total             2641
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03891b2.cif
_cod_data_source_block           (2)_zigzag_NiNb_(100K)
_cod_depositor_comments
'Adding full bibliography for 7715116--7715117.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7715117
_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   0.642
_shelx_estimated_absorpt_t_max   0.964
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.500000 0.76871(2) 0.750000 0.00515(6) Uani 1 2 d S T P . .
Ni1 Ni 0.500000 0.500000 0.500000 0.00769(8) Uani 1 2 d S . P . .
C1 C 0.48589(15) 0.64159(13) 0.66232(12) 0.0098(4) Uani 1 1 d . . . . .
C2 C 0.32684(16) 0.71939(13) 0.75797(13) 0.0121(4) Uani 1 1 d . . . . .
C3 C 0.10762(15) 0.39629(13) 0.75590(13) 0.0105(4) Uani 1 1 d . . . . .
C4 C 0.50778(16) 0.81256(13) 0.89902(13) 0.0120(4) Uani 1 1 d . . . . .
C11 C 0.2663(2) 0.3992(2) 0.5439(2) 0.0510(9) Uani 1 1 d . . . . .
H11A H 0.199437 0.380634 0.572728 0.061 Uiso 1 1 calc R U . . .
H11B H 0.269717 0.361582 0.487518 0.061 Uiso 1 1 calc R U . . .
C12 C 0.2555(2) 0.5001(2) 0.5164(2) 0.0444(8) Uani 1 1 d . . . . .
H12A H 0.181395 0.511112 0.486289 0.053 Uiso 1 1 calc R U . . .
H12B H 0.264297 0.539189 0.572234 0.053 Uiso 1 1 calc R U . . .
C13 C 0.3361(2) 0.62667(18) 0.42836(19) 0.0401(8) Uani 1 1 d . . . . .
H13A H 0.337790 0.665168 0.484533 0.048 Uiso 1 1 calc R U . . .
H13B H 0.268503 0.641309 0.389289 0.048 Uiso 1 1 calc R U . . .
C14 C 0.4347(3) 0.64636(17) 0.37727(16) 0.0412(8) Uani 1 1 d . . . . .
H14A H 0.432102 0.608521 0.320618 0.049 Uiso 1 1 calc R U . . .
H14B H 0.435647 0.712551 0.359567 0.049 Uiso 1 1 calc R U . . .
C15 C 0.6359(3) 0.6242(2) 0.39104(18) 0.0446(8) Uani 1 1 d . . . . .
H15A H 0.646434 0.686226 0.364210 0.053 Uiso 1 1 calc R U . . .
H15B H 0.630023 0.578637 0.340221 0.053 Uiso 1 1 calc R U . . .
Li1 Li 0.1180(3) 0.6019(2) 0.7573(2) 0.0144(7) Uani 1 1 d . . . . .
N1 N 0.48189(14) 0.57680(12) 0.61695(11) 0.0131(3) Uani 1 1 d . . . . .
N2 N 0.24053(14) 0.68890(12) 0.76151(13) 0.0169(4) Uani 1 1 d . . . . .
N3 N 0.15488(14) 0.46511(12) 0.76012(12) 0.0149(4) Uani 1 1 d . . . . .
N4 N 0.51062(15) 0.83376(12) 0.97511(12) 0.0171(4) Uani 1 1 d . . . . .
N11 N 0.33827(15) 0.52767(14) 0.45285(13) 0.0241(4) Uani 1 1 d . . . . .
H11 H 0.322222 0.491878 0.394691 0.029 Uiso 1 1 calc R U . . .
N12 N 0.53401(17) 0.62380(12) 0.43702(12) 0.0225(4) Uani 1 1 d . . . . .
H12 H 0.541616 0.672162 0.486155 0.027 Uiso 1 1 calc R U . . .
O1 O 0.00104(12) 0.59508(11) 0.84933(10) 0.0133(3) Uani 1 1 d . . . . .
H1A H -0.0010(19) 0.6182(17) 0.8972(17) 0.016 Uiso 1 1 d . U . . .
H2A H 0.0008(19) 0.5414(19) 0.8619(16) 0.016 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'
Li Li -0.0003 0.0001 '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'
Nb Nb -2.0727 0.6215 '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'
O O 0.0106 0.0060 '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
C1 Nb1 C1 69.73(9) . 2_656 ?
C1 Nb1 C2 75.05(7) . . ?
C1 Nb1 C2 74.90(7) 2_656 . ?
C1 Nb1 C2 74.90(7) . 2_656 ?
C1 Nb1 C2 75.05(7) 2_656 2_656 ?
C2 Nb1 C2 143.17(9) . 2_656 ?
C1 Nb1 C4 71.52(7) . 2_656 ?
C1 Nb1 C4 140.90(7) 2_656 2_656 ?
C2 Nb1 C4 100.01(7) . 2_656 ?
C2 Nb1 C4 90.17(7) 2_656 2_656 ?
C1 Nb1 C4 140.90(7) . . ?
C1 Nb1 C4 71.52(7) 2_656 . ?
C2 Nb1 C4 90.17(7) . . ?
C2 Nb1 C4 100.01(7) 2_656 . ?
C4 Nb1 C4 147.50(10) 2_656 . ?
C1 Nb1 C3 134.94(7) . 3 ?
C1 Nb1 C3 128.95(7) 2_656 3 ?
C2 Nb1 C3 143.59(7) . 3 ?
C2 Nb1 C3 73.10(7) 2_656 3 ?
C4 Nb1 C3 77.69(7) 2_656 3 ?
C4 Nb1 C3 76.00(7) . 3 ?
C1 Nb1 C3 128.95(7) . 4_556 ?
C1 Nb1 C3 134.94(7) 2_656 4_556 ?
C2 Nb1 C3 73.10(7) . 4_556 ?
C2 Nb1 C3 143.59(7) 2_656 4_556 ?
C4 Nb1 C3 76.00(7) 2_656 4_556 ?
C4 Nb1 C3 77.69(7) . 4_556 ?
C3 Nb1 C3 71.12(9) 3 4_556 ?
N1 Ni1 N1 180.0 5_666 . ?
N1 Ni1 N12 86.79(7) 5_666 5_666 ?
N1 Ni1 N12 93.21(7) . 5_666 ?
N1 Ni1 N12 93.21(7) 5_666 . ?
N1 Ni1 N12 86.79(7) . . ?
N12 Ni1 N12 180.0 5_666 . ?
N1 Ni1 N11 90.31(7) 5_666 5_666 ?
N1 Ni1 N11 89.69(7) . 5_666 ?
N12 Ni1 N11 84.80(8) 5_666 5_666 ?
N12 Ni1 N11 95.20(8) . 5_666 ?
N1 Ni1 N11 89.69(7) 5_666 . ?
N1 Ni1 N11 90.31(7) . . ?
N12 Ni1 N11 95.20(8) 5_666 . ?
N12 Ni1 N11 84.80(8) . . ?
N11 Ni1 N11 180.0 5_666 . ?
N1 C1 Nb1 177.94(17) . . ?
N2 C2 Nb1 175.95(16) . . ?
N3 C3 Nb1 174.49(16) . 3_445 ?
N4 C4 Nb1 178.92(18) . . ?
C15 C11 C12 115.5(2) 5_666 . ?
N11 C12 C11 112.0(2) . . ?
N11 C13 C14 107.8(2) . . ?
N12 C14 C13 108.92(19) . . ?
N12 C15 C11 112.0(2) . 5_666 ?
N2 Li1 N3 117.10(18) . . ?
N2 Li1 O1 123.55(18) . 2_556 ?
N3 Li1 O1 96.48(15) . 2_556 ?
N2 Li1 O1 126.05(19) . . ?
N3 Li1 O1 96.16(15) . . ?
O1 Li1 O1 90.15(14) 2_556 . ?
N2 Li1 Li1 140.02(11) . 2_556 ?
N3 Li1 Li1 102.86(10) . 2_556 ?
O1 Li1 Li1 45.24(10) 2_556 2_556 ?
O1 Li1 Li1 45.17(10) . 2_556 ?
C1 N1 Ni1 156.28(16) . . ?
C2 N2 Li1 161.98(19) . . ?
C3 N3 Li1 136.94(18) . . ?
C13 N11 C12 114.4(2) . . ?
C13 N11 Ni1 105.27(15) . . ?
C12 N11 Ni1 115.04(16) . . ?
C15 N12 C14 114.9(2) . . ?
C15 N12 Ni1 114.72(16) . . ?
C14 N12 Ni1 105.46(15) . . ?
Li1 O1 Li1 89.58(14) 2_556 . ?
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
Nb1 C1 2.2361(19) . ?
Nb1 C1 2.2361(19) 2_656 ?
Nb1 C2 2.253(2) . ?
Nb1 C2 2.253(2) 2_656 ?
Nb1 C4 2.262(2) 2_656 ?
Nb1 C4 2.262(2) . ?
Nb1 C3 2.263(2) 3 ?
Nb1 C3 2.263(2) 4_556 ?
Ni1 N1 2.0643(16) 5_666 ?
Ni1 N1 2.0643(16) . ?
Ni1 N12 2.0682(18) 5_666 ?
Ni1 N12 2.0683(18) . ?
Ni1 N11 2.0844(18) 5_666 ?
Ni1 N11 2.0844(18) . ?
C1 N1 1.145(3) . ?
C2 N2 1.152(3) . ?
C3 N3 1.149(3) . ?
C4 N4 1.151(3) . ?
C11 C15 1.506(5) 5_666 ?
C11 C12 1.514(5) . ?
C12 N11 1.486(3) . ?
C13 N11 1.473(3) . ?
C13 C14 1.500(4) . ?
C14 N12 1.475(3) . ?
C15 N12 1.468(3) . ?
Li1 N2 1.956(4) . ?
Li1 N3 2.025(4) . ?
Li1 O1 2.047(4) 2_556 ?
Li1 O1 2.049(4) . ?
Li1 Li1 2.886(7) 2_556 ?
