#------------------------------------------------------------------------------
#$Date: 2023-04-12 04:26:11 +0300 (Wed, 12 Apr 2023) $
#$Revision: 282610 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/65/7246598.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_7246598
loop_
_publ_author_name
'Jana, Narayan Ch.'
'Jagodič, Marko'
'Brandão, Paula'
'Patra, Moumita'
'Herchel, Radovan'
'Jagličić, Zvonko'
'Panja, Anangamohan'
_publ_section_title
;
 Magneto-structural studies on a number of doubly end-on cyanate and azide
 bridged dinuclear nickel(ii) complexes with {N3O} donor Schiff base
 ligands
;
_journal_issue                   17
_journal_name_full               'RSC Advances'
_journal_page_first              11311
_journal_page_last               11323
_journal_paper_doi               10.1039/D3RA00737E
_journal_volume                  13
_journal_year                    2023
_chemical_formula_sum            'C32 H46 N10 Ni2 O8'
_chemical_formula_weight         816.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-01-26 deposited with the CCDC.	2023-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.741(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.489(4)
_cell_length_b                   14.894(5)
_cell_length_c                   10.892(4)
_cell_measurement_reflns_used    502
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.90
_cell_volume                     1765.0(11)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18536
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.122
_diffrn_reflns_theta_min         1.872
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5732
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0384
_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)+(0.0216P)²+1.0513P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3282
_reflns_number_total             4254
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ra00737e6.cif
_cod_data_source_block           complex-5
_cod_original_cell_volume        1764.8(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7246598
_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   0.713
_shelx_estimated_absorpt_t_max   0.935
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Ni Ni 0.64007(3) 0.51464(2) 0.48962(3) 0.01614(9) Uani 1 1 d . . . . .
O1 O 0.68880(14) 0.55116(10) 0.67721(15) 0.0203(3) Uani 1 1 d . . . . .
O2 O 0.95674(17) 0.40601(13) 1.22653(16) 0.0381(5) Uani 1 1 d . . . . .
O3 O 1.00994(17) 0.30244(11) 1.11530(16) 0.0307(4) Uani 1 1 d . . . . .
O4 O 0.43083(18) 0.74650(11) 0.45471(18) 0.0372(5) Uani 1 1 d . . . . .
N1 N 0.77692(17) 0.41735(12) 0.53632(17) 0.0190(4) Uani 1 1 d . . . . .
N2 N 0.56734(19) 0.47976(13) 0.29262(18) 0.0189(4) Uani 1 1 d . . . . .
H2A H 0.504(2) 0.4540(17) 0.301(3) 0.030(8) Uiso 1 1 d . . . . .
N3 N 0.74502(18) 0.62642(13) 0.44387(18) 0.0205(4) Uani 1 1 d . . . . .
N4 N 0.48138(17) 0.59127(13) 0.46949(17) 0.0184(4) Uani 1 1 d . . . . .
N5 N 0.95656(18) 0.37361(14) 1.12237(19) 0.0243(5) Uani 1 1 d . . . . .
C1 C 0.7568(2) 0.50993(15) 0.7773(2) 0.0175(5) Uani 1 1 d . . . . .
C2 C 0.7674(2) 0.54478(16) 0.9027(2) 0.0207(5) Uani 1 1 d . . . . .
H2 H 0.7279 0.5998 0.9090 0.025 Uiso 1 1 calc R U . . .
C3 C 0.8327(2) 0.50107(16) 1.0136(2) 0.0221(5) Uani 1 1 d . . . . .
H3 H 0.8384 0.5255 1.0959 0.027 Uiso 1 1 calc R U . . .
C4 C 0.8911(2) 0.42008(16) 1.0052(2) 0.0200(5) Uani 1 1 d . . . . .
C5 C 0.8882(2) 0.38586(15) 0.8868(2) 0.0197(5) Uani 1 1 d . . . . .
H5 H 0.9308 0.3317 0.8833 0.024 Uiso 1 1 calc R U . . .
C6 C 0.8239(2) 0.42942(15) 0.7724(2) 0.0179(5) Uani 1 1 d . . . . .
C7 C 0.8293(2) 0.39005(15) 0.6521(2) 0.0191(5) Uani 1 1 d . . . . .
H7 H 0.8780 0.3374 0.6607 0.023 Uiso 1 1 calc R U . . .
C8 C 0.8032(2) 0.36317(16) 0.4344(2) 0.0253(5) Uani 1 1 d . . . . .
H8A H 0.8466 0.3077 0.4744 0.030 Uiso 1 1 calc R U . . .
H8B H 0.8593 0.3976 0.3996 0.030 Uiso 1 1 calc R U . . .
C9 C 0.6904(2) 0.33719(16) 0.3229(2) 0.0255(5) Uani 1 1 d . . . . .
H9A H 0.6290 0.3108 0.3587 0.031 Uiso 1 1 calc R U . . .
H9B H 0.7138 0.2901 0.2710 0.031 Uiso 1 1 calc R U . . .
C10 C 0.6306(2) 0.41407(16) 0.2337(2) 0.0257(5) Uani 1 1 d . . . . .
H10A H 0.6945 0.4459 0.2074 0.031 Uiso 1 1 calc R U . . .
H10B H 0.5703 0.3891 0.1544 0.031 Uiso 1 1 calc R U . . .
C11 C 0.5228(2) 0.55663(16) 0.2026(2) 0.0221(5) Uani 1 1 d . . . . .
H11A H 0.4585 0.5890 0.2275 0.027 Uiso 1 1 calc R U . . .
H11B H 0.4846 0.5332 0.1137 0.027 Uiso 1 1 calc R U . . .
C12 C 0.6234(2) 0.62219(16) 0.2022(2) 0.0249(5) Uani 1 1 d . . . . .
H12A H 0.5905 0.6640 0.1285 0.030 Uiso 1 1 calc R U . . .
H12B H 0.6914 0.5882 0.1869 0.030 Uiso 1 1 calc R U . . .
C13 C 0.6754(2) 0.67710(16) 0.3247(2) 0.0242(5) Uani 1 1 d . . . . .
H13A H 0.7306 0.7234 0.3085 0.029 Uiso 1 1 calc R U . . .
H13B H 0.6066 0.7088 0.3421 0.029 Uiso 1 1 calc R U . . .
C14 C 0.7784(2) 0.69241(16) 0.5511(2) 0.0262(6) Uani 1 1 d . . . . .
H14A H 0.8332 0.6641 0.6296 0.039 Uiso 1 1 calc R U . . .
H14B H 0.7037 0.7132 0.5674 0.039 Uiso 1 1 calc R U . . .
H14C H 0.8202 0.7436 0.5273 0.039 Uiso 1 1 calc R U . . .
C15 C 0.8611(2) 0.59323(17) 0.4282(2) 0.0278(6) Uani 1 1 d . . . . .
H15A H 0.9073 0.6439 0.4097 0.042 Uiso 1 1 calc R U . . .
H15B H 0.8422 0.5503 0.3563 0.042 Uiso 1 1 calc R U . . .
H15C H 0.9105 0.5635 0.5083 0.042 Uiso 1 1 calc R U . . .
C16 C 0.4573(2) 0.66832(17) 0.4623(2) 0.0213(5) Uani 1 1 d . . . . .
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 Ni N1 89.89(7) . . ?
O1 Ni N4 84.73(7) . . ?
N1 Ni N4 165.26(7) . . ?
O1 Ni N2 173.13(7) . . ?
N1 Ni N2 95.67(7) . . ?
N4 Ni N2 88.90(7) . . ?
O1 Ni N3 91.80(7) . . ?
N1 Ni N3 98.99(8) . . ?
N4 Ni N3 94.90(8) . . ?
N2 Ni N3 91.31(8) . . ?
O1 Ni N4 88.65(7) . 3_666 ?
N1 Ni N4 86.04(8) . 3_666 ?
N4 Ni N4 80.13(8) . 3_666 ?
N2 Ni N4 87.72(7) . 3_666 ?
N3 Ni N4 174.95(7) . 3_666 ?
C1 O1 Ni 129.17(15) . . ?
C7 N1 C8 114.96(19) . . ?
C7 N1 Ni 122.94(15) . . ?
C8 N1 Ni 121.15(14) . . ?
C10 N2 C11 109.60(18) . . ?
C10 N2 Ni 121.03(15) . . ?
C11 N2 Ni 114.98(14) . . ?
C10 N2 H2A 107.8(17) . . ?
C11 N2 H2A 107.2(18) . . ?
Ni N2 H2A 94.0(18) . . ?
C14 N3 C15 107.33(19) . . ?
C14 N3 C13 106.31(18) . . ?
C15 N3 C13 108.63(18) . . ?
C14 N3 Ni 110.18(14) . . ?
C15 N3 Ni 110.59(14) . . ?
C13 N3 Ni 113.53(14) . . ?
C16 N4 Ni 135.54(17) . . ?
C16 N4 Ni 123.42(17) . 3_666 ?
Ni N4 Ni 99.87(8) . 3_666 ?
O2 N5 O3 122.5(2) . . ?
O2 N5 C4 118.4(2) . . ?
O3 N5 C4 119.09(19) . . ?
O1 C1 C2 118.8(2) . . ?
O1 C1 C6 124.0(2) . . ?
C2 C1 C6 117.2(2) . . ?
C3 C2 C1 121.7(2) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 119.5(2) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.9(2) . . ?
C5 C4 N5 120.2(2) . . ?
C3 C4 N5 118.9(2) . . ?
C4 C5 C6 120.9(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.6(2) . . ?
C5 C6 C7 117.1(2) . . ?
C1 C6 C7 123.3(2) . . ?
N1 C7 C6 128.2(2) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
N1 C8 C9 114.4(2) . . ?
N1 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C8 C9 C10 114.6(2) . . ?
C8 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
C8 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
N2 C10 C9 113.91(19) . . ?
N2 C10 H10A 108.8 . . ?
C9 C10 H10A 108.8 . . ?
N2 C10 H10B 108.8 . . ?
C9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 C12 113.42(19) . . ?
N2 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
N2 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 C13 115.57(19) . . ?
C11 C12 H12A 108.4 . . ?
C13 C12 H12A 108.4 . . ?
C11 C12 H12B 108.4 . . ?
C13 C12 H12B 108.4 . . ?
H12A C12 H12B 107.4 . . ?
N3 C13 C12 116.27(19) . . ?
N3 C13 H13A 108.2 . . ?
C12 C13 H13A 108.2 . . ?
N3 C13 H13B 108.2 . . ?
C12 C13 H13B 108.2 . . ?
H13A C13 H13B 107.4 . . ?
N3 C14 H14A 109.5 . . ?
N3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 O4 178.9(3) . . ?
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
Ni O1 2.0122(17) . ?
Ni N1 2.0776(19) . ?
Ni N4 2.1018(19) . ?
Ni N2 2.102(2) . ?
Ni N3 2.205(2) . ?
Ni N4 2.2434(19) 3_666 ?
O1 C1 1.276(3) . ?
O2 N5 1.232(3) . ?
O3 N5 1.239(3) . ?
O4 C16 1.199(3) . ?
N1 C7 1.277(3) . ?
N1 C8 1.480(3) . ?
N2 C10 1.483(3) . ?
N2 C11 1.487(3) . ?
N2 H2A 0.85(3) . ?
N3 C14 1.479(3) . ?
N3 C15 1.482(3) . ?
N3 C13 1.492(3) . ?
N4 C16 1.177(3) . ?
N4 Ni 2.2433(19) 3_666 ?
N5 C4 1.434(3) . ?
C1 C2 1.429(3) . ?
C1 C6 1.436(3) . ?
C2 C3 1.365(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.397(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(3) . ?
C5 C6 1.388(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.455(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.514(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.516(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.513(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.515(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
