#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/97/4329790.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_4329790
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            'C26 H38 N6 Ni2 O2 S2'
_chemical_formula_weight         648.16
_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                 90.697(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2781(5)
_cell_length_b                   12.2358(15)
_cell_length_c                   12.7526(10)
_cell_measurement_reflns_used    6681
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.70
_cell_volume                     1447.6(2)
_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 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6681
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.70
_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    1.480
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0376
_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)+(0.0384P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                2544
_reflns_number_total             4003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202748m_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4329790
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.12697(3) 0.05854(2) -0.05956(2) 0.03233(10) Uani 1 1 d . . .
C1 C 0.4200(3) -0.02189(19) -0.15843(16) 0.0350(5) Uani 1 1 d . . .
N1 N 0.3116(2) 0.00357(17) -0.12086(16) 0.0458(5) Uani 1 1 d . . .
S1 S 0.57148(7) -0.05908(7) -0.21453(5) 0.0514(2) Uani 1 1 d . . .
O11 O -0.07137(16) 0.08406(13) -0.00061(13) 0.0418(4) Uani 1 1 d . . .
C12 C -0.1208(2) 0.18753(18) 0.00392(16) 0.0293(5) Uani 1 1 d . A .
C13 C -0.2539(2) 0.21378(19) -0.03828(17) 0.0335(5) Uani 1 1 d . . .
H13 H -0.3121 0.1592 -0.0667 0.040 Uiso 1 1 calc R . .
C14 C -0.3014(2) 0.3216(2) -0.03849(16) 0.0351(5) Uani 1 1 d . . .
H14 H -0.3912 0.3384 -0.0674 0.042 Uiso 1 1 calc R . .
C15 C -0.2188(3) 0.4025(2) 0.00286(17) 0.0384(6) Uani 1 1 d . . .
H15 H -0.2512 0.4744 0.0022 0.046 Uiso 1 1 calc R . .
C16 C -0.0864(3) 0.3770(2) 0.04587(17) 0.0403(6) Uani 1 1 d . A .
H16 H -0.0301 0.4322 0.0753 0.048 Uiso 1 1 calc R . .
C17 C -0.0351(2) 0.2701(2) 0.04620(15) 0.0335(5) Uani 1 1 d . . .
C181 C 0.1066(3) 0.2425(3) 0.09691(19) 0.0641(10) Uani 0.606(7) 1 d P A 1
H181 H 0.1522 0.3141 0.1064 0.077 Uiso 0.606(7) 1 calc PR A 1
C183 C 0.0910(5) 0.2047(5) 0.2002(3) 0.060(2) Uani 0.606(7) 1 d P A 1
H18A H 0.0320 0.2548 0.2386 0.089 Uiso 0.606(7) 1 calc PR A 1
H18B H 0.1841 0.1994 0.2334 0.089 Uiso 0.606(7) 1 calc PR A 1
H18C H 0.0461 0.1340 0.1992 0.089 Uiso 0.606(7) 1 calc PR A 1
C182 C 0.1066(3) 0.2425(3) 0.09691(19) 0.0641(10) Uani 0.394(7) 1 d P A 2
H182 H 0.0735 0.1789 0.1366 0.077 Uiso 0.394(7) 1 calc PR A 2
C184 C 0.1673(8) 0.2983(7) 0.1802(5) 0.052(2) Uani 0.394(7) 1 d P A 2
H18D H 0.2072 0.3660 0.1557 0.078 Uiso 0.394(7) 1 calc PR A 2
H18E H 0.2423 0.2548 0.2115 0.078 Uiso 0.394(7) 1 calc PR A 2
H18F H 0.0947 0.3132 0.2312 0.078 Uiso 0.394(7) 1 calc PR A 2
C21 C 0.2409(3) 0.30662(19) -0.13011(18) 0.0428(6) Uani 1 1 d . . .
H21A H 0.3073 0.3606 -0.1572 0.051 Uiso 1 1 calc R . .
H21B H 0.1542 0.3449 -0.1095 0.051 Uiso 1 1 calc R . .
C22 C 0.2024(2) 0.22859(19) -0.21689(16) 0.0377(6) Uani 1 1 d . . .
H22A H 0.1749 0.2694 -0.2792 0.045 Uiso 1 1 calc R . .
H22B H 0.2857 0.1843 -0.2336 0.045 Uiso 1 1 calc R . .
C20 C 0.3073(2) 0.2558(2) -0.03489(18) 0.0434(6) Uani 1 1 d . A .
H20A H 0.3418 0.3138 0.0107 0.052 Uiso 1 1 calc R . .
H20B H 0.3905 0.2137 -0.0564 0.052 Uiso 1 1 calc R . .
C231 C 0.0264(3) 0.0938(3) -0.27416(19) 0.0615(8) Uani 1 1 d . . .
H23A H 0.0983 0.0427 -0.2964 0.092 Uiso 1 1 calc R . .
H23B H 0.0026 0.1422 -0.3310 0.092 Uiso 1 1 calc R . .
H23C H -0.0585 0.0548 -0.2534 0.092 Uiso 1 1 calc R . .
N23 N 0.08201(19) 0.15696(16) -0.18554(13) 0.0334(4) Uani 1 1 d . . .
H23 H 0.0093 0.2020 -0.1656 0.040 Uiso 1 1 calc R . .
N19 N 0.21104(19) 0.18257(18) 0.02748(13) 0.0386(5) Uani 1 1 d . . .
H19 H 0.2721 0.1487 0.0734 0.046 Uiso 1 1 calc R A 1
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'
O O 0.0106 0.0060 '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'
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 94.78(7) 3 .
O11 Ni1 O11 75.46(7) 3 .
N1 Ni1 O11 169.09(8) . .
O11 Ni1 N19 123.22(7) 3 .
N1 Ni1 N19 98.01(8) . .
O11 Ni1 N19 91.53(7) . .
O11 Ni1 N23 140.55(7) 3 .
N1 Ni1 N23 93.33(7) . .
O11 Ni1 N23 91.33(7) . .
N19 Ni1 N23 93.59(8) . .
N1 C1 S1 178.5(2) . .
C1 N1 Ni1 175.9(2) . .
C12 O11 Ni1 136.21(12) . 3
C12 O11 Ni1 118.21(12) . .
Ni1 O11 Ni1 104.54(7) 3 .
O11 C12 C13 120.3(2) . .
O11 C12 C17 120.43(19) . .
C13 C12 C17 119.1(2) . .
C12 C13 C14 120.3(2) . .
C12 C13 H13 119.9 . .
C14 C13 H13 119.9 . .
C15 C14 C13 121.0(2) . .
C15 C14 H14 119.5 . .
C13 C14 H14 119.5 . .
C14 C15 C16 119.2(2) . .
C14 C15 H15 120.4 . .
C16 C15 H15 120.4 . .
C15 C16 C17 121.2(2) . .
C15 C16 H16 119.4 . .
C17 C16 H16 119.4 . .
C12 C17 C16 119.2(2) . .
C12 C17 C182 119.9(2) . .
C16 C17 C182 120.8(2) . .
C12 C17 C181 119.9(2) . .
C16 C17 C181 120.8(2) . .
C182 C17 C181 0.0(4) . .
C183 C181 C17 112.3(3) . .
C183 C181 N19 117.6(3) . .
C17 C181 N19 115.01(18) . .
C183 C181 H181 103.2 . .
C17 C181 H181 103.2 . .
N19 C181 H181 103.2 . .
C184 C182 C17 124.8(4) . .
C184 C182 N19 115.7(3) . .
C17 C182 N19 115.01(18) . .
C184 C182 H182 97.1 . .
C17 C182 H182 97.1 . .
N19 C182 H182 97.1 . .
C182 C184 H18D 109.5 . .
C182 C184 H18E 109.5 . .
H18D C184 H18E 109.5 . .
C182 C184 H18F 109.5 . .
H18D C184 H18F 109.5 . .
H18E C184 H18F 109.5 . .
C20 C21 C22 115.3(2) . .
C20 C21 H21A 108.5 . .
C22 C21 H21A 108.5 . .
C20 C21 H21B 108.5 . .
C22 C21 H21B 108.5 . .
H21A C21 H21B 107.5 . .
N23 C22 C21 110.56(17) . .
N23 C22 H22A 109.5 . .
C21 C22 H22A 109.5 . .
N23 C22 H22B 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 108.1 . .
C21 C20 N19 116.01(18) . .
C21 C20 H20A 108.3 . .
N19 C20 H20A 108.3 . .
C21 C20 H20B 108.3 . .
N19 C20 H20B 108.3 . .
H20A C20 H20B 107.4 . .
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 . .
C231 N23 C22 111.48(18) . .
C231 N23 Ni1 111.29(17) . .
C22 N23 Ni1 114.42(13) . .
C231 N23 H23 106.4 . .
C22 N23 H23 106.4 . .
Ni1 N23 H23 106.4 . .
C20 N19 C182 114.3(2) . .
C20 N19 C181 114.3(2) . .
C182 N19 C181 0.0(3) . .
C20 N19 Ni1 112.57(13) . .
C182 N19 Ni1 116.00(16) . .
C181 N19 Ni1 116.00(16) . .
C20 N19 H19 104.1 . .
C182 N19 H19 104.1 . .
C181 N19 H19 104.1 . .
Ni1 N19 H19 104.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O11 1.9771(15) 3
Ni1 N1 2.0079(19) .
Ni1 O11 2.0205(14) .
Ni1 N19 2.030(2) .
Ni1 N23 2.0468(17) .
C1 N1 1.162(3) .
C1 S1 1.649(2) .
O11 C12 1.348(2) .
O11 Ni1 1.9771(15) 3
C12 C13 1.379(3) .
C12 C17 1.390(3) .
C13 C14 1.391(3) .
C13 H13 0.9300 .
C14 C15 1.355(3) .
C14 H14 0.9300 .
C15 C16 1.375(3) .
C15 H15 0.9300 .
C16 C17 1.391(3) .
C16 H16 0.9300 .
C17 C182 1.497(3) .
C17 C181 1.497(3) .
C181 C183 1.406(5) .
C181 N19 1.511(3) .
C181 H181 0.9800 .
C183 H18A 0.9600 .
C183 H18B 0.9600 .
C183 H18C 0.9600 .
C182 C184 1.377(7) .
C182 N19 1.511(3) .
C182 H182 0.9800 .
C184 H18D 0.9600 .
C184 H18E 0.9600 .
C184 H18F 0.9600 .
C21 C20 1.491(3) .
C21 C22 1.501(3) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 N23 1.479(3) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C20 N19 1.500(3) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C231 N23 1.458(3) .
C231 H23A 0.9600 .
C231 H23B 0.9600 .
C231 H23C 0.9600 .
N23 H23 0.9100 .
N19 H19 0.9100 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139137530
