#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/82/7028281.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_7028281
loop_
_publ_author_name
'Ghorai, Samir'
'Mukherjee, Chandan'
_publ_section_title
;
 Effect of ligand substituent on the reactivity of Ni(II) complexes
 towards oxygen.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              394
_journal_page_last               397
_journal_paper_doi               10.1039/c3dt52072b
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C36 H47 N2 Ni O2'
_chemical_formula_sum            'C36 H47 N2 Ni O2'
_chemical_formula_weight         598.47
_chemical_properties_physical    ' paramagnetic, oxygen-sensitive'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 114.585(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.2555(10)
_cell_length_b                   13.6775(4)
_cell_length_c                   19.3826(6)
_cell_measurement_temperature    296(2)
_cell_volume                     6811.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29563
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.59
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_recrystallization_method 'dichloromethane, acetonitrile'
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0800P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                4574
_reflns_number_total             5871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52072b.txt
_cod_data_source_block           sg_2
_cod_original_sg_symbol_H-M      'C1 2/c1'
_cod_database_code               7028281
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.153736(11) 0.343037(19) 0.481341(15) 0.03473(13) Uani 1 1 d .
C18 C 0.16716(9) 0.06090(16) 0.31006(12) 0.0398(5) Uani 1 1 d .
H18 H 0.1529 0.0041 0.2831 0.048 Uiso 1 1 calc R
C15 C 0.20670(8) 0.23350(15) 0.38416(11) 0.0341(5) Uani 1 1 d .
C7 C 0.15198(9) 0.55327(16) 0.47734(12) 0.0391(5) Uani 1 1 d .
C4 C 0.06421(9) 0.43787(17) 0.64480(13) 0.0432(6) Uani 1 1 d .
H4 H 0.0461 0.4297 0.6750 0.052 Uiso 1 1 calc R
C2 C 0.09858(9) 0.37180(16) 0.56215(12) 0.0384(5) Uani 1 1 d .
C20 C 0.16722(8) 0.18543(15) 0.39744(11) 0.0338(5) Uani 1 1 d .
C17 C 0.20919(9) 0.10422(16) 0.30000(12) 0.0394(5) Uani 1 1 d .
C3 C 0.07181(9) 0.35637(16) 0.60967(13) 0.0392(5) Uani 1 1 d .
C14 C 0.22707(9) 0.32605(15) 0.41893(12) 0.0368(5) Uani 1 1 d .
H14 H 0.2568 0.3492 0.4149 0.044 Uiso 1 1 calc R
C1 C 0.11545(8) 0.46762(15) 0.55389(12) 0.0367(5) Uani 1 1 d .
C19 C 0.14574(8) 0.09727(15) 0.35746(12) 0.0349(5) Uani 1 1 d .
C16 C 0.22793(9) 0.19006(16) 0.33712(12) 0.0385(5) Uani 1 1 d .
H16 H 0.2554 0.2209 0.3313 0.046 Uiso 1 1 calc R
C13 C 0.23467(8) 0.47250(15) 0.48928(13) 0.0408(5) Uani 1 1 d .
H13A H 0.2623 0.4836 0.4729 0.049 Uiso 1 1 calc R
H13B H 0.2504 0.4669 0.5441 0.049 Uiso 1 1 calc R
C12 C 0.19790(9) 0.55784(15) 0.46616(12) 0.0393(5) Uani 1 1 d .
C5 C 0.08146(9) 0.53341(17) 0.63917(13) 0.0424(6) Uani 1 1 d .
C11 C 0.20863(11) 0.64112(17) 0.43499(15) 0.0533(7) Uani 1 1 d .
H11 H 0.2393 0.6446 0.4282 0.064 Uiso 1 1 calc R
C6 C 0.10683(9) 0.54804(16) 0.59311(13) 0.0418(5) Uani 1 1 d .
H6 H 0.1182 0.6102 0.5877 0.050 Uiso 1 1 calc R
C10 C 0.17456(13) 0.71953(19) 0.41363(17) 0.0712(9) Uani 1 1 d .
H10 H 0.1826 0.7760 0.3940 0.085 Uiso 1 1 calc R
C8 C 0.11668(10) 0.63127(18) 0.45269(15) 0.0524(7) Uani 1 1 d .
H8 H 0.0852 0.6277 0.4573 0.063 Uiso 1 1 calc R
C9 C 0.12847(13) 0.71281(19) 0.42186(17) 0.0680(8) Uani 1 1 d .
H9 H 0.1050 0.7645 0.4062 0.082 Uiso 1 1 calc R
C21 C 0.23072(10) 0.05425(19) 0.24789(14) 0.0504(6) Uani 1 1 d .
C22 C 0.27910(11) 0.1069(2) 0.24959(17) 0.0664(8) Uani 1 1 d .
H22A H 0.2699 0.1719 0.2301 0.100 Uiso 1 1 calc R
H22B H 0.2926 0.0717 0.2189 0.100 Uiso 1 1 calc R
H22C H 0.3051 0.1099 0.3009 0.100 Uiso 1 1 calc R
C23 C 0.24617(12) -0.0519(2) 0.27445(19) 0.0751(9) Uani 1 1 d .
H23A H 0.2719 -0.0519 0.3260 0.113 Uiso 1 1 calc R
H23B H 0.2602 -0.0827 0.2425 0.113 Uiso 1 1 calc R
H23C H 0.2160 -0.0873 0.2714 0.113 Uiso 1 1 calc R
C24 C 0.18905(12) 0.0542(3) 0.16650(15) 0.0754(9) Uani 1 1 d .
H24A H 0.1580 0.0237 0.1650 0.113 Uiso 1 1 calc R
H24B H 0.2015 0.0186 0.1347 0.113 Uiso 1 1 calc R
H24C H 0.1814 0.1203 0.1486 0.113 Uiso 1 1 calc R
C25 C 0.09971(9) 0.04694(16) 0.36675(13) 0.0407(5) Uani 1 1 d .
C26 C 0.07869(10) -0.03862(18) 0.31149(15) 0.0563(7) Uani 1 1 d .
H26A H 0.0668 -0.0151 0.2604 0.084 Uiso 1 1 calc R
H26B H 0.0502 -0.0686 0.3184 0.084 Uiso 1 1 calc R
H26C H 0.1058 -0.0859 0.3211 0.084 Uiso 1 1 calc R
C27 C 0.11757(10) 0.0074(2) 0.44791(14) 0.0565(7) Uani 1 1 d .
H27A H 0.1461 -0.0368 0.4587 0.085 Uiso 1 1 calc R
H27B H 0.0893 -0.0264 0.4525 0.085 Uiso 1 1 calc R
H27C H 0.1284 0.0608 0.4832 0.085 Uiso 1 1 calc R
C28 C 0.05501(9) 0.12014(19) 0.34991(16) 0.0564(7) Uani 1 1 d .
H28A H 0.0652 0.1687 0.3892 0.085 Uiso 1 1 calc R
H28B H 0.0248 0.0862 0.3481 0.085 Uiso 1 1 calc R
H28C H 0.0471 0.1512 0.3020 0.085 Uiso 1 1 calc R
C29 C 0.05507(10) 0.25332(18) 0.62112(14) 0.0488(6) Uani 1 1 d .
C30 C 0.10309(12) 0.1866(2) 0.65411(19) 0.0746(9) Uani 1 1 d .
H30A H 0.0923 0.1211 0.6583 0.112 Uiso 1 1 calc R
H30B H 0.1262 0.2098 0.7034 0.112 Uiso 1 1 calc R
H30C H 0.1208 0.1871 0.6212 0.112 Uiso 1 1 calc R
C32 C 0.02921(11) 0.2532(2) 0.67670(16) 0.0659(8) Uani 1 1 d .
H32A H -0.0010 0.2944 0.6574 0.099 Uiso 1 1 calc R
H32B H 0.0533 0.2774 0.7251 0.099 Uiso 1 1 calc R
H32C H 0.0191 0.1877 0.6824 0.099 Uiso 1 1 calc R
C31 C 0.01587(12) 0.2128(2) 0.54483(17) 0.0744(9) Uani 1 1 d .
H31A H -0.0146 0.2534 0.5259 0.112 Uiso 1 1 calc R
H31B H 0.0064 0.1474 0.5518 0.112 Uiso 1 1 calc R
H31C H 0.0314 0.2125 0.5091 0.112 Uiso 1 1 calc R
C33 C 0.07163(10) 0.61655(19) 0.68504(14) 0.0519(6) Uani 1 1 d .
C36 C 0.09543(14) 0.7132(2) 0.67603(18) 0.0779(9) Uani 1 1 d .
H36A H 0.1322 0.7050 0.6917 0.117 Uiso 1 1 calc R
H36B H 0.0894 0.7622 0.7069 0.117 Uiso 1 1 calc R
H36C H 0.0796 0.7331 0.6238 0.117 Uiso 1 1 calc R
C34 C 0.01262(12) 0.6294(2) 0.65803(18) 0.0724(9) Uani 1 1 d .
H34A H -0.0029 0.6427 0.6046 0.109 Uiso 1 1 calc R
H34B H 0.0059 0.6829 0.6847 0.109 Uiso 1 1 calc R
H34C H -0.0020 0.5706 0.6679 0.109 Uiso 1 1 calc R
C35 C 0.09618(13) 0.5892(2) 0.76974(15) 0.0734(9) Uani 1 1 d .
H35A H 0.0807 0.5299 0.7771 0.110 Uiso 1 1 calc R
H35B H 0.0902 0.6409 0.7987 0.110 Uiso 1 1 calc R
H35C H 0.1329 0.5798 0.7863 0.110 Uiso 1 1 calc R
O1 O 0.10973(6) 0.30196(11) 0.52512(9) 0.0435(4) Uani 1 1 d .
O2 O 0.15033(6) 0.21836(10) 0.44703(8) 0.0410(4) Uani 1 1 d .
N1 N 0.14225(7) 0.46800(12) 0.50897(10) 0.0367(4) Uani 1 1 d .
N2 N 0.20724(7) 0.38004(12) 0.45555(10) 0.0340(4) 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
O2 Ni1 N2 94.74(7)
O2 Ni1 O1 86.55(7)
N2 Ni1 O1 169.34(7)
O2 Ni1 N1 168.04(7)
N2 Ni1 N1 94.97(8)
O1 Ni1 N1 85.20(7)
C19 C18 C17 124.4(2)
C20 C15 C16 120.2(2)
C20 C15 C14 121.26(19)
C16 C15 C14 118.5(2)
N1 C7 C12 117.94(19)
N1 C7 C8 122.9(2)
C12 C7 C8 119.1(2)
C3 C4 C5 125.7(2)
O1 C2 C1 116.2(2)
O1 C2 C3 123.9(2)
C1 C2 C3 119.9(2)
O2 C20 C15 121.92(19)
O2 C20 C19 118.97(19)
C15 C20 C19 119.09(19)
C16 C17 C18 116.93(19)
C16 C17 C21 123.8(2)
C18 C17 C21 119.3(2)
C4 C3 C2 115.8(2)
C4 C3 C29 123.7(2)
C2 C3 C29 120.5(2)
N2 C14 C15 125.2(2)
N1 C1 C6 127.0(2)
N1 C1 C2 111.93(18)
C6 C1 C2 120.9(2)
C18 C19 C20 117.4(2)
C18 C19 C25 122.53(19)
C20 C19 C25 120.11(18)
C17 C16 C15 121.7(2)
N2 C13 C12 111.15(17)
C11 C12 C7 119.3(2)
C11 C12 C13 121.4(2)
C7 C12 C13 119.25(19)
C6 C5 C4 118.4(2)
C6 C5 C33 122.5(2)
C4 C5 C33 119.2(2)
C12 C11 C10 121.2(2)
C5 C6 C1 119.3(2)
C9 C10 C11 119.1(2)
C9 C8 C7 120.0(2)
C8 C9 C10 121.1(3)
C24 C21 C22 108.7(2)
C24 C21 C17 109.4(2)
C22 C21 C17 111.7(2)
C24 C21 C23 109.5(2)
C22 C21 C23 108.0(2)
C17 C21 C23 109.5(2)
C26 C25 C27 108.3(2)
C26 C25 C28 107.72(19)
C27 C25 C28 109.7(2)
C26 C25 C19 111.05(18)
C27 C25 C19 110.00(18)
C28 C25 C19 109.99(19)
C3 C29 C32 111.7(2)
C3 C29 C31 109.6(2)
C32 C29 C31 108.2(2)
C3 C29 C30 109.5(2)
C32 C29 C30 107.7(2)
C31 C29 C30 110.2(2)
C36 C33 C34 109.2(2)
C36 C33 C5 112.3(2)
C34 C33 C5 108.6(2)
C36 C33 C35 107.9(2)
C34 C33 C35 109.6(2)
C5 C33 C35 109.1(2)
C2 O1 Ni1 112.87(14)
C20 O2 Ni1 127.39(13)
C1 N1 C7 122.91(18)
C1 N1 Ni1 112.83(14)
C7 N1 Ni1 123.44(14)
C14 N2 C13 117.32(19)
C14 N2 Ni1 125.31(16)
C13 N2 Ni1 116.71(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 O2 1.8183(14)
Ni1 N2 1.8494(18)
Ni1 O1 1.8599(15)
Ni1 N1 1.8596(17)
C18 C19 1.386(3)
C18 C17 1.411(3)
C15 C20 1.408(3)
C15 C16 1.414(3)
C15 C14 1.437(3)
C7 N1 1.397(3)
C7 C12 1.403(3)
C7 C8 1.402(3)
C4 C3 1.369(3)
C4 C5 1.415(3)
C2 O1 1.310(3)
C2 C1 1.426(3)
C2 C3 1.430(3)
C20 O2 1.318(2)
C20 C19 1.425(3)
C17 C16 1.364(3)
C17 C21 1.539(3)
C3 C29 1.532(3)
C14 N2 1.302(3)
C1 N1 1.371(3)
C1 C6 1.415(3)
C19 C25 1.547(3)
C13 N2 1.485(3)
C13 C12 1.502(3)
C12 C11 1.381(3)
C5 C6 1.372(3)
C5 C33 1.538(3)
C11 C10 1.384(4)
C10 C9 1.379(4)
C8 C9 1.370(4)
C21 C24 1.526(4)
C21 C22 1.533(4)
C21 C23 1.542(4)
C25 C26 1.530(3)
C25 C27 1.537(3)
C25 C28 1.537(3)
C29 C32 1.533(3)
C29 C31 1.535(4)
C29 C30 1.537(4)
C33 C36 1.526(4)
C33 C34 1.536(4)
C33 C35 1.539(4)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139163025
