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#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/97/4329792.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_4329792
loop_
_publ_author_name
'Apurba Biswas'
'Lakshmi Kanta Das'
'Michael G. B. Drew'
'Guillem Aromí'
'Patrick Gamez'
'Ashutosh Ghosh'
_publ_section_title
;
 Synthesis, Crystal Structures, Magnetic Properties and Catecholase
 Activity of Double Phenoxido-Bridged Penta-Coordinated Dinuclear
 Nickel(II) Complexes Derived from Reduced Schiff-Base Ligands:
 Mechanistic Inference of Catecholase Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7993
_journal_page_last               8001
_journal_paper_doi               10.1021/ic202748m
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C28 H42 N6 Ni2 O2 S2'
_chemical_formula_weight         676.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 115.400(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.947(5)
_cell_length_b                   20.602(12)
_cell_length_c                   9.435(5)
_cell_measurement_reflns_used    10657
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      1.98
_cell_volume                     1571.0(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10657
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.98
_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    1.367
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0483
_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)+(0.0481P)²+1.6930P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                2053
_reflns_number_total             2758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202748m_si_002_3.cif
_cod_data_source_block           3
_cod_original_cell_volume        1571.0(16)
_cod_database_code               4329792
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni -0.04588(6) 0.95754(2) 0.61630(6) 0.03953(19) Uani 1 1 d .
S1 S -0.30318(18) 0.98783(9) 0.96206(17) 0.0822(5) Uani 1 1 d .
O11 O 0.0849(3) 0.95464(12) 0.4865(3) 0.0416(7) Uani 1 1 d .
N19 N 0.1143(4) 0.89076(17) 0.7711(4) 0.0452(9) Uani 1 1 d .
H19 H 0.1478 0.9107 0.8659 0.054 Uiso 1 1 calc R
N23 N -0.2495(4) 0.89906(18) 0.4809(4) 0.0507(9) Uani 1 1 d .
N1 N -0.1360(5) 0.97519(19) 0.7746(5) 0.0590(10) Uani 1 1 d .
C12 C 0.1464(5) 0.89798(19) 0.4610(5) 0.0403(10) Uani 1 1 d .
C17 C 0.2364(5) 0.8585(2) 0.5904(5) 0.0483(11) Uani 1 1 d .
C16 C 0.2933(6) 0.7989(2) 0.5642(7) 0.0691(15) Uani 1 1 d .
H16 H 0.3552 0.7724 0.6492 0.083 Uiso 1 1 calc R
C15 C 0.2592(7) 0.7784(3) 0.4141(8) 0.0776(17) Uani 1 1 d .
H15 H 0.2958 0.7379 0.3985 0.093 Uiso 1 1 calc R
C14 C 0.1709(6) 0.8179(3) 0.2866(7) 0.0665(14) Uani 1 1 d .
H14 H 0.1487 0.8042 0.1856 0.080 Uiso 1 1 calc R
C13 C 0.1159(5) 0.8779(2) 0.3105(5) 0.0497(11) Uani 1 1 d .
H13 H 0.0584 0.9049 0.2254 0.060 Uiso 1 1 calc R
C18 C 0.2742(6) 0.8829(3) 0.7531(5) 0.0606(13) Uani 1 1 d .
H18 H 0.3156 0.9272 0.7564 0.073 Uiso 1 1 calc R
C181 C 0.4063(7) 0.8489(3) 0.8909(7) 0.0913(19) Uani 1 1 d .
H18A H 0.3784 0.8039 0.8892 0.137 Uiso 1 1 calc R
H18B H 0.4147 0.8684 0.9864 0.137 Uiso 1 1 calc R
H18C H 0.5104 0.8529 0.8849 0.137 Uiso 1 1 calc R
C20 C 0.0355(6) 0.8308(2) 0.7907(6) 0.0617(13) Uani 1 1 d .
H20A H -0.0165 0.8398 0.8601 0.074 Uiso 1 1 calc R
H20B H 0.1207 0.7985 0.8412 0.074 Uiso 1 1 calc R
C21 C -0.0922(6) 0.8029(2) 0.6402(6) 0.0619(13) Uani 1 1 d .
H21A H -0.1149 0.7586 0.6595 0.074 Uiso 1 1 calc R
H21B H -0.0461 0.8015 0.5641 0.074 Uiso 1 1 calc R
C22 C -0.2532(5) 0.8397(2) 0.5700(6) 0.0572(12) Uani 1 1 d .
H22A H -0.3390 0.8110 0.5001 0.069 Uiso 1 1 calc R
H22B H -0.2829 0.8523 0.6537 0.069 Uiso 1 1 calc R
C24 C -0.4029(6) 0.9367(3) 0.4480(7) 0.0816(17) Uani 1 1 d .
H24A H -0.4020 0.9760 0.3938 0.122 Uiso 1 1 calc R
H24B H -0.4078 0.9472 0.5451 0.122 Uiso 1 1 calc R
H24C H -0.4978 0.9112 0.3840 0.122 Uiso 1 1 calc R
C25 C -0.2528(6) 0.8802(3) 0.3291(6) 0.0795(17) Uani 1 1 d .
H25A H -0.3546 0.8580 0.2674 0.119 Uiso 1 1 calc R
H25B H -0.1612 0.8520 0.3466 0.119 Uiso 1 1 calc R
H25C H -0.2449 0.9184 0.2743 0.119 Uiso 1 1 calc R
C1 C -0.2039(5) 0.9803(2) 0.8534(5) 0.0482(11) 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'
S S 0.1246 0.1234 '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
O11 Ni1 N1 98.82(14) 3_576 .
O11 Ni1 O11 76.17(11) 3_576 .
N1 Ni1 O11 166.86(14) . .
O11 Ni1 N19 149.61(12) 3_576 .
N1 Ni1 N19 88.44(15) . .
O11 Ni1 N19 90.14(12) . .
O11 Ni1 N23 107.27(13) 3_576 .
N1 Ni1 N23 92.07(16) . .
O11 Ni1 N23 101.00(13) . .
N19 Ni1 N23 101.87(14) . .
C12 O11 Ni1 133.5(2) . 3_576
C12 O11 Ni1 121.1(2) . .
Ni1 O11 Ni1 103.83(11) 3_576 .
C20 N19 C18 116.7(4) . .
C20 N19 Ni1 115.0(3) . .
C18 N19 Ni1 113.0(3) . .
C20 N19 H19 103.3 . .
C18 N19 H19 103.3 . .
Ni1 N19 H19 103.3 . .
C25 N23 C24 107.6(4) . .
C25 N23 C22 109.7(4) . .
C24 N23 C22 107.6(4) . .
C25 N23 Ni1 113.2(3) . .
C24 N23 Ni1 108.0(3) . .
C22 N23 Ni1 110.5(3) . .
C1 N1 Ni1 171.3(4) . .
O11 C12 C13 121.4(4) . .
O11 C12 C17 118.1(4) . .
C13 C12 C17 120.4(4) . .
C16 C17 C12 118.4(4) . .
C16 C17 C18 122.4(4) . .
C12 C17 C18 119.1(4) . .
C15 C16 C17 121.0(5) . .
C15 C16 H16 119.5 . .
C17 C16 H16 119.5 . .
C16 C15 C14 120.3(5) . .
C16 C15 H15 119.9 . .
C14 C15 H15 119.9 . .
C15 C14 C13 119.6(5) . .
C15 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
C14 C13 C12 120.3(5) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C181 C18 C17 118.3(4) . .
C181 C18 N19 112.4(4) . .
C17 C18 N19 109.8(4) . .
C181 C18 H18 105.0 . .
C17 C18 H18 105.0 . .
N19 C18 H18 105.0 . .
C18 C181 H18A 109.5 . .
C18 C181 H18B 109.5 . .
H18A C181 H18B 109.5 . .
C18 C181 H18C 109.5 . .
H18A C181 H18C 109.5 . .
H18B C181 H18C 109.5 . .
N19 C20 C21 114.4(4) . .
N19 C20 H20A 108.7 . .
C21 C20 H20A 108.7 . .
N19 C20 H20B 108.7 . .
C21 C20 H20B 108.7 . .
H20A C20 H20B 107.6 . .
C20 C21 C22 114.7(4) . .
C20 C21 H21A 108.6 . .
C22 C21 H21A 108.6 . .
C20 C21 H21B 108.6 . .
C22 C21 H21B 108.6 . .
H21A C21 H21B 107.6 . .
N23 C22 C21 114.3(4) . .
N23 C22 H22A 108.7 . .
C21 C22 H22A 108.7 . .
N23 C22 H22B 108.7 . .
C21 C22 H22B 108.7 . .
H22A C22 H22B 107.6 . .
N23 C24 H24A 109.5 . .
N23 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
N23 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
N23 C25 H25A 109.5 . .
N23 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
N23 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
N1 C1 S1 178.9(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O11 2.011(3) 3_576
Ni1 N1 2.012(4) .
Ni1 O11 2.025(3) .
Ni1 N19 2.070(3) .
Ni1 N23 2.099(4) .
S1 C1 1.626(5) .
O11 C12 1.355(4) .
O11 Ni1 2.011(3) 3_576
N19 C20 1.472(5) .
N19 C18 1.520(5) .
N19 H19 0.9100 .
N23 C25 1.471(6) .
N23 C24 1.488(6) .
N23 C22 1.492(6) .
N1 C1 1.149(5) .
C12 C13 1.389(6) .
C12 C17 1.399(6) .
C17 C16 1.391(6) .
C17 C18 1.510(6) .
C16 C15 1.381(7) .
C16 H16 0.9300 .
C15 C14 1.384(7) .
C15 H15 0.9300 .
C14 C13 1.385(6) .
C14 H14 0.9300 .
C13 H13 0.9300 .
C18 C181 1.503(7) .
C18 H18 0.9800 .
C181 H18A 0.9600 .
C181 H18B 0.9600 .
C181 H18C 0.9600 .
C20 C21 1.504(7) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 C22 1.507(6) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139137534
