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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/7/71/51/7715116.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_7715116
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 H36 Li2 N12 Nb Ni O6'
_chemical_formula_weight         682.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 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                 105.385(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2590(8)
_cell_length_b                   9.6405(7)
_cell_length_c                   15.8896(12)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.50
_cell_volume                     1515.2(2)
_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 0.999
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21012
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.496
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0112P)²+2.0605P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3293
_reflns_number_total             3483
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03891b2.cif
_cod_data_source_block           1_straight_chain_NiNb
_cod_depositor_comments
'Adding full bibliography for 7715116--7715117.cif.'
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               7715116
_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   0.842
_shelx_estimated_absorpt_t_max   0.969
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.250000 0.63036(2) 0.250000 0.00491(6) Uani 1 2 d S T P . .
Ni1 Ni 0.000000 0.500000 0.500000 0.00764(8) Uani 1 2 d S . P . .
C1 C 0.1199(2) 0.5586(2) 0.33560(13) 0.0097(4) Uani 1 1 d . . . . .
C2 C 0.3537(2) 0.7102(2) 0.38455(13) 0.0098(4) Uani 1 1 d . . . . .
C3 C 0.6341(2) 0.5546(2) 0.68053(12) 0.0097(4) Uani 1 1 d . . . . .
C4 C 0.3813(2) 0.8113(2) 0.23557(12) 0.0111(4) Uani 1 1 d . . . . .
C11 C -0.2608(2) 0.5577(2) 0.36505(14) 0.0177(4) Uani 1 1 d . . . . .
H11A H -0.354678 0.528973 0.336227 0.021 Uiso 1 1 calc R U . . .
H11B H -0.210423 0.561682 0.319898 0.021 Uiso 1 1 calc R U . . .
C12 C -0.1904(2) 0.3141(2) 0.39342(14) 0.0181(5) Uani 1 1 d . . . . .
H12A H -0.153727 0.321529 0.341894 0.022 Uiso 1 1 calc R U . . .
H12B H -0.281880 0.272883 0.374468 0.022 Uiso 1 1 calc R U . . .
C13 C -0.0989(2) 0.2230(2) 0.46250(15) 0.0186(5) Uani 1 1 d . . . . .
H13A H -0.137554 0.212231 0.512967 0.022 Uiso 1 1 calc R U . . .
H13B H -0.090603 0.129919 0.438159 0.022 Uiso 1 1 calc R U . . .
C14 C 0.1267(2) 0.2243(2) 0.56816(14) 0.0181(5) Uani 1 1 d . . . . .
H14A H 0.141246 0.126025 0.554971 0.022 Uiso 1 1 calc R U . . .
H14B H 0.083587 0.226250 0.617002 0.022 Uiso 1 1 calc R U . . .
C15 C 0.2628(2) 0.2983(2) 0.59582(15) 0.0205(5) Uani 1 1 d . . . . .
H15A H 0.326219 0.239537 0.639145 0.025 Uiso 1 1 calc R U . . .
H15B H 0.299106 0.306414 0.544173 0.025 Uiso 1 1 calc R U . . .
Li1 Li 0.5120(4) 0.8182(4) 0.5717(2) 0.0128(7) Uani 1 1 d . . . . .
N1 N 0.05842(17) 0.53000(18) 0.38397(11) 0.0112(3) Uani 1 1 d . . . . .
N2 N 0.40503(18) 0.75545(18) 0.45223(11) 0.0135(3) Uani 1 1 d . . . . .
N3 N 0.57990(18) 0.65373(18) 0.64871(11) 0.0133(4) Uani 1 1 d . . . . .
N4 N 0.44970(19) 0.90482(19) 0.23196(12) 0.0166(4) Uani 1 1 d . . . . .
N11 N -0.19766(17) 0.45309(18) 0.43117(11) 0.0128(3) Uani 1 1 d . . . . .
H11 H -0.253348 0.445671 0.473963 0.015 Uiso 1 1 calc R U . . .
N12 N 0.03562(17) 0.28975(17) 0.49068(11) 0.0121(3) Uani 1 1 d . . . . .
H12 H 0.078996 0.278208 0.441693 0.015 Uiso 1 1 calc R U . . .
O1 O 0.40051(17) 0.95934(17) 0.60533(11) 0.0166(3) Uani 1 1 d . . . . .
H1A H 0.372(3) 1.009(3) 0.5694(19) 0.020 Uiso 1 1 d . U . . .
H1B H 0.433(3) 1.004(3) 0.6471(18) 0.020 Uiso 1 1 d . U . . .
O2 O 0.67465(17) 0.92750(17) 0.56831(10) 0.0164(3) Uani 1 1 d . . . . .
H2A H 0.671(3) 1.004(3) 0.5834(17) 0.020 Uiso 1 1 d . U . . .
H2B H 0.739(3) 0.896(3) 0.6009(18) 0.020 Uiso 1 1 d . U . . .
O3 O 0.90599(17) 0.81650(18) 0.67521(10) 0.0174(3) Uani 1 1 d . . . . .
H3A H 0.900(3) 0.771(3) 0.7113(18) 0.021 Uiso 1 1 d . U . . .
H3B H 0.936(3) 0.886(3) 0.6987(18) 0.021 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 144.23(10) . 2 ?
C1 Nb1 C4 73.16(7) . 2 ?
C1 Nb1 C4 139.94(7) 2 2 ?
C1 Nb1 C4 139.94(7) . . ?
C1 Nb1 C4 73.16(7) 2 . ?
C4 Nb1 C4 78.47(10) 2 . ?
C1 Nb1 C2 74.83(7) . . ?
C1 Nb1 C2 118.12(7) 2 . ?
C4 Nb1 C2 77.50(7) 2 . ?
C4 Nb1 C2 71.81(7) . . ?
C1 Nb1 C2 118.12(7) . 2 ?
C1 Nb1 C2 74.83(7) 2 2 ?
C4 Nb1 C2 71.81(7) 2 2 ?
C4 Nb1 C2 77.50(7) . 2 ?
C2 Nb1 C2 140.10(10) . 2 ?
C1 Nb1 C3 74.55(7) . 4_565 ?
C1 Nb1 C3 77.42(7) 2 4_565 ?
C4 Nb1 C3 114.15(7) 2 4_565 ?
C4 Nb1 C3 144.30(7) . 4_565 ?
C2 Nb1 C3 141.84(7) . 4_565 ?
C2 Nb1 C3 75.62(7) 2 4_565 ?
C1 Nb1 C3 77.42(7) . 3_666 ?
C1 Nb1 C3 74.55(7) 2 3_666 ?
C4 Nb1 C3 144.30(7) 2 3_666 ?
C4 Nb1 C3 114.14(7) . 3_666 ?
C2 Nb1 C3 75.63(7) . 3_666 ?
C2 Nb1 C3 141.84(7) 2 3_666 ?
C3 Nb1 C3 75.94(10) 4_565 3_666 ?
N12 Ni1 N12 180.0 3_566 . ?
N12 Ni1 N11 94.84(7) 3_566 . ?
N12 Ni1 N11 85.16(7) . . ?
N12 Ni1 N11 85.16(7) 3_566 3_566 ?
N12 Ni1 N11 94.84(7) . 3_566 ?
N11 Ni1 N11 180.0 . 3_566 ?
N12 Ni1 N1 88.57(7) 3_566 3_566 ?
N12 Ni1 N1 91.42(7) . 3_566 ?
N11 Ni1 N1 88.07(7) . 3_566 ?
N11 Ni1 N1 91.93(7) 3_566 3_566 ?
N12 Ni1 N1 91.43(7) 3_566 . ?
N12 Ni1 N1 88.58(7) . . ?
N11 Ni1 N1 91.93(7) . . ?
N11 Ni1 N1 88.07(7) 3_566 . ?
N1 Ni1 N1 180.0 3_566 . ?
N1 C1 Nb1 174.55(17) . . ?
N2 C2 Nb1 177.64(17) . . ?
N3 C3 Nb1 175.99(17) . 3_666 ?
N4 C4 Nb1 177.09(17) . . ?
N11 C11 C15 112.53(17) . 3_566 ?
N11 C12 C13 108.59(17) . . ?
N12 C13 C12 108.36(17) . . ?
N12 C14 C15 111.65(17) . . ?
C11 C15 C14 115.67(18) 3_566 . ?
O1 Li1 O2 101.33(17) . . ?
O1 Li1 N3 121.27(19) . . ?
O2 Li1 N3 106.09(17) . . ?
O1 Li1 N2 104.83(17) . . ?
O2 Li1 N2 112.64(18) . . ?
N3 Li1 N2 110.49(18) . . ?
C1 N1 Ni1 162.33(16) . . ?
C2 N2 Li1 173.3(2) . . ?
C3 N3 Li1 165.8(2) . . ?
C11 N11 C12 112.99(17) . . ?
C11 N11 Ni1 114.05(13) . . ?
C12 N11 Ni1 105.25(13) . . ?
C14 N12 C13 113.56(17) . . ?
C14 N12 Ni1 116.33(13) . . ?
C13 N12 Ni1 106.19(13) . . ?
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 2.252(2) . ?
Nb1 C1 2.252(2) 2 ?
Nb1 C4 2.253(2) 2 ?
Nb1 C4 2.253(2) . ?
Nb1 C2 2.256(2) . ?
Nb1 C2 2.256(2) 2 ?
Nb1 C3 2.262(2) 4_565 ?
Nb1 C3 2.262(2) 3_666 ?
Ni1 N12 2.0718(17) 3_566 ?
Ni1 N12 2.0718(17) . ?
Ni1 N11 2.0823(17) . ?
Ni1 N11 2.0823(17) 3_566 ?
Ni1 N1 2.1044(17) 3_566 ?
Ni1 N1 2.1044(17) . ?
C1 N1 1.150(3) . ?
C2 N2 1.150(3) . ?
C3 N3 1.153(3) . ?
C4 N4 1.153(3) . ?
C11 N11 1.476(3) . ?
C11 C15 1.523(3) 3_566 ?
C12 N11 1.478(3) . ?
C12 C13 1.520(3) . ?
C13 N12 1.480(3) . ?
C14 N12 1.475(3) . ?
C14 C15 1.526(3) . ?
Li1 O1 1.942(4) . ?
Li1 O2 1.986(4) . ?
Li1 N3 2.011(4) . ?
Li1 N2 2.017(4) . ?
