#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/24/4302462.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_4302462
loop_
_publ_author_name
'Pampa Mukherjee'
'Michael G. B. Drew'
'Carlos J. Gómez-García'
'Ashutosh Ghosh'
_publ_section_title
;
The Crucial Role of Polyatomic Anions in Molecular Architecture: Structural
And Magnetic Versatility of Five Nickel(II) Complexes Derived from A
N,N,O-Donor Schiff Base Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5848
_journal_page_last               5860
_journal_paper_doi               10.1021/ic9001863
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C22 H34 N10 Ni2 O4'
_chemical_formula_weight         620.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.880(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.8549(3)
_cell_length_b                   19.7038(9)
_cell_length_c                   10.2237(6)
_cell_measurement_reflns_used    7843
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.26
_cell_volume                     1367.85(12)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7843
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    1.424
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            'deep green'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3840
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.0423P)²+4.7489P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                3207
_reflns_number_total             3840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9001863_si_001_1.cif
_cod_data_source_block           1
_cod_database_code               4302462
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.18478(7) 0.46362(3) 0.09340(5) 0.01622(15) Uani 1 1 d . . .
O11 O 0.3231(4) 0.55484(15) 0.1118(3) 0.0205(6) Uani 1 1 d . . .
N19 N 0.2241(5) 0.45115(19) 0.2922(3) 0.0219(8) Uani 1 1 d . . .
N23 N 0.0483(5) 0.36952(19) 0.0449(4) 0.0211(7) Uani 1 1 d . . .
H23 H -0.0796 0.3805 0.0169 0.025 Uiso 1 1 calc R . .
C22 C 0.0366(8) 0.3191(3) 0.1506(5) 0.0344(11) Uani 1 1 d . . .
H22A H 0.1583 0.2934 0.1642 0.041 Uiso 1 1 calc R . .
H22B H -0.0696 0.2877 0.1222 0.041 Uiso 1 1 calc R . .
C21 C 0.0024(8) 0.3502(3) 0.2791(5) 0.0334(11) Uani 1 1 d . . .
H21A H -0.0387 0.3149 0.3355 0.040 Uiso 1 1 calc R . .
H21B H -0.1045 0.3827 0.2624 0.040 Uiso 1 1 calc R . .
C20 C 0.1825(8) 0.3861(3) 0.3524(5) 0.0338(11) Uani 1 1 d . . .
H20A H 0.1614 0.3939 0.4431 0.041 Uiso 1 1 calc R . .
H20B H 0.2964 0.3567 0.3538 0.041 Uiso 1 1 calc R . .
C18 C 0.2605(6) 0.5018(3) 0.3722(4) 0.0250(9) Uani 1 1 d . . .
H18 H 0.2558 0.4924 0.4609 0.030 Uiso 1 1 calc R . .
C17 C 0.3075(6) 0.5710(3) 0.3423(4) 0.0256(10) Uani 1 1 d . . .
C16 C 0.3272(8) 0.6170(3) 0.4489(5) 0.0335(11) Uani 1 1 d . . .
H16 H 0.3053 0.6018 0.5317 0.040 Uiso 1 1 calc R . .
C15 C 0.3776(8) 0.6836(3) 0.4341(5) 0.0380(12) Uani 1 1 d . . .
H15 H 0.3895 0.7130 0.5059 0.046 Uiso 1 1 calc R . .
C14 C 0.4106(7) 0.7066(3) 0.3107(5) 0.0337(11) Uani 1 1 d . . .
H14 H 0.4452 0.7517 0.2998 0.040 Uiso 1 1 calc R . .
C13 C 0.3924(6) 0.6629(3) 0.2041(5) 0.0274(9) Uani 1 1 d . . .
H13 H 0.4152 0.6793 0.1222 0.033 Uiso 1 1 calc R . .
C12 C 0.3405(6) 0.5943(2) 0.2158(4) 0.0195(8) Uani 1 1 d . . .
C231 C 0.1141(7) 0.3346(3) -0.0706(5) 0.0329(11) Uani 1 1 d . . .
H23A H 0.1044 0.3654 -0.1440 0.049 Uiso 1 1 calc R . .
H23B H 0.0320 0.2958 -0.0939 0.049 Uiso 1 1 calc R . .
H23C H 0.2483 0.3202 -0.0483 0.049 Uiso 1 1 calc R . .
N1 N 0.0966(5) 0.49088(19) -0.1040(3) 0.0182(7) Uani 1 1 d . . .
N2 N 0.1802(5) 0.4913(2) -0.1994(3) 0.0206(7) Uani 1 1 d . . .
N3 N 0.2593(6) 0.4933(3) -0.2913(4) 0.0421(12) Uani 1 1 d . . .
O100 O 0.4636(4) 0.41828(17) 0.0823(3) 0.0222(6) Uani 1 1 d D . .
H1 H 0.533(6) 0.435(2) 0.149(3) 0.027 Uiso 1 1 d D . .
H2 H 0.530(7) 0.431(3) 0.023(4) 0.027 Uiso 1 1 d 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
N19 Ni1 O11 91.04(13) . . ?
N19 Ni1 N1 167.73(14) . . ?
O11 Ni1 N1 86.08(13) . . ?
N19 Ni1 N23 97.06(15) . . ?
O11 Ni1 N23 171.54(13) . . ?
N1 Ni1 N23 86.50(14) . . ?
N19 Ni1 O100 90.32(13) . . ?
O11 Ni1 O100 88.01(12) . . ?
N1 Ni1 O100 101.49(12) . . ?
N23 Ni1 O100 89.49(13) . . ?
N19 Ni1 N1 89.82(13) . 3_565 ?
O11 Ni1 N1 92.12(13) . 3_565 ?
N1 Ni1 N1 78.39(13) . 3_565 ?
N23 Ni1 N1 90.36(14) . 3_565 ?
O100 Ni1 N1 179.81(15) . 3_565 ?
C12 O11 Ni1 126.2(3) . . ?
C18 N19 C20 116.2(4) . . ?
C18 N19 Ni1 121.9(3) . . ?
C20 N19 Ni1 121.3(3) . . ?
C22 N23 C231 108.8(4) . . ?
C22 N23 Ni1 119.1(3) . . ?
C231 N23 Ni1 114.8(3) . . ?
C22 N23 H23 104.1 . . ?
C231 N23 H23 104.1 . . ?
Ni1 N23 H23 104.1 . . ?
N23 C22 C21 113.4(4) . . ?
N23 C22 H22A 108.9 . . ?
C21 C22 H22A 108.9 . . ?
N23 C22 H22B 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C22 C21 C20 114.0(4) . . ?
C22 C21 H21A 108.7 . . ?
C20 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
C20 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
N19 C20 C21 112.9(4) . . ?
N19 C20 H20A 109.0 . . ?
C21 C20 H20A 109.0 . . ?
N19 C20 H20B 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
N19 C18 C17 128.6(4) . . ?
N19 C18 H18 115.7 . . ?
C17 C18 H18 115.7 . . ?
C16 C17 C12 119.0(5) . . ?
C16 C17 C18 116.4(4) . . ?
C12 C17 C18 124.6(4) . . ?
C15 C16 C17 121.9(5) . . ?
C15 C16 H16 119.0 . . ?
C17 C16 H16 119.0 . . ?
C16 C15 C14 119.3(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C13 C14 C15 120.3(5) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C13 C12 121.9(5) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
O11 C12 C13 119.8(4) . . ?
O11 C12 C17 122.6(4) . . ?
C13 C12 C17 117.6(4) . . ?
N23 C231 H23A 109.5 . . ?
N23 C231 H23B 109.5 . . ?
H23A C231 H23B 109.5 . . ?
N23 C231 H23C 109.5 . . ?
H23A C231 H23C 109.5 . . ?
H23B C231 H23C 109.5 . . ?
N2 N1 Ni1 132.8(3) . . ?
N2 N1 Ni1 125.0(3) . 3_565 ?
Ni1 N1 Ni1 101.61(13) . 3_565 ?
N3 N2 N1 178.4(5) . . ?
Ni1 O100 H1 102(4) . . ?
Ni1 O100 H2 120(4) . . ?
H1 O100 H2 99(5) . . ?
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 N19 2.028(3) . ?
Ni1 O11 2.029(3) . ?
Ni1 N1 2.096(3) . ?
Ni1 N23 2.105(4) . ?
Ni1 O100 2.126(3) . ?
Ni1 N1 2.143(3) 3_565 ?
O11 C12 1.310(5) . ?
N19 C18 1.293(6) . ?
N19 C20 1.467(6) . ?
N23 C22 1.477(6) . ?
N23 C231 1.489(6) . ?
N23 H23 0.9100 . ?
C22 C21 1.496(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C21 C20 1.527(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C18 C17 1.443(7) . ?
C18 H18 0.9300 . ?
C17 C16 1.410(6) . ?
C17 C12 1.419(6) . ?
C16 C15 1.369(8) . ?
C16 H16 0.9300 . ?
C15 C14 1.388(8) . ?
C15 H15 0.9300 . ?
C14 C13 1.381(7) . ?
C14 H14 0.9300 . ?
C13 C12 1.406(6) . ?
C13 H13 0.9300 . ?
C231 H23A 0.9600 . ?
C231 H23B 0.9600 . ?
C231 H23C 0.9600 . ?
N1 N2 1.197(4) . ?
N1 Ni1 2.143(3) 3_565 ?
N2 N3 1.147(5) . ?
O100 H1 0.843(19) . ?
O100 H2 0.844(19) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168336764
