#------------------------------------------------------------------------------
#$Date: 2025-10-18 19:09:19 +0200 (Sat 18 de Oct de 2025) $
#$Revision: 302968 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/11/7011129.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_7011129
loop_
_publ_author_name
'Adams, Harry'
'Clunas, Scott'
'Fenton, David E.'
'Spey, Sharon E.'
_publ_section_title
;
 The systematic generation of monodentate bridging ethanoates in
 dinuclear nickel(II) complexes of asymmetric compartmental ligands
;
_journal_coden_ASTM              JCSDAA
_journal_issue                   3
_journal_name_full
;
 Journal of the Chemical Society, Dalton Transactions
;
_journal_page_first              441
_journal_page_last               448
_journal_paper_doi               10.1039/b107928j
_journal_year                    2002
_chemical_formula_sum            'C28 H41 N5 Ni2 O6 S'
_chemical_formula_weight         693.14
_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                 107.076(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6287(12)
_cell_length_b                   14.3404(13)
_cell_length_c                   18.0340(16)
_cell_measurement_reflns_used    86
_cell_measurement_temperature    150(2)
_cell_volume                     3122.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1798
_diffrn_reflns_av_sigmaI/netI    0.1315
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19465
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  0.8575
_exptl_absorpt_correction_T_min  0.7688
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.062
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7462
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0761P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                5637
_reflns_number_total             7462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107928j.txt
_cod_data_source_block           ifn193m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7011129
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 0.13473(4) 0.22416(3) 0.01876(2) 0.02065(13) Uani 1 1 d . . .
Ni2 Ni 0.26730(4) 0.35082(3) 0.15290(2) 0.02047(13) Uani 1 1 d . . .
S1 S -0.24254(10) 0.20692(7) 0.02977(6) 0.0400(2) Uani 1 1 d . . .
O1 O 0.2063(2) 0.21891(14) 0.13341(11) 0.0226(5) Uani 1 1 d . . .
O2 O 0.3915(2) 0.31462(16) 0.11139(12) 0.0257(5) Uani 1 1 d . . .
O3 O 0.2853(2) 0.25487(16) -0.00098(12) 0.0254(5) Uani 1 1 d . . .
O4 O 0.1285(2) 0.37236(15) 0.05094(12) 0.0240(5) Uani 1 1 d . . .
O5 O 0.1122(2) 0.39134(15) 0.16773(12) 0.0253(5) Uani 1 1 d . . .
N1 N 0.3475(3) 0.31961(19) 0.26712(14) 0.0248(6) Uani 1 1 d . . .
N2 N 0.3304(3) 0.49340(18) 0.17986(14) 0.0240(6) Uani 1 1 d . . .
N3 N 0.0667(3) 0.24532(19) -0.09950(14) 0.0247(6) Uani 1 1 d . . .
N4 N 0.1664(3) 0.08777(18) 0.00922(14) 0.0235(6) Uani 1 1 d . . .
N5 N -0.0218(3) 0.19976(19) 0.02898(15) 0.0263(6) Uani 1 1 d . . .
C1 C 0.2735(4) 0.6660(3) 0.1806(3) 0.0416(10) Uani 1 1 d . . .
H1A H 0.3268 0.6751 0.2319 0.062 Uiso 1 1 calc R . .
H1B H 0.2081 0.7050 0.1759 0.062 Uiso 1 1 calc R . .
H1C H 0.3078 0.6837 0.1404 0.062 Uiso 1 1 calc R . .
C2 C 0.2386(3) 0.5628(2) 0.1704(2) 0.0292(8) Uani 1 1 d . . .
H2A H 0.1984 0.5478 0.2085 0.035 Uiso 1 1 calc R . .
H2B H 0.1858 0.5549 0.1180 0.035 Uiso 1 1 calc R . .
C3 C 0.3474(4) 0.5271(3) 0.0474(2) 0.0370(9) Uani 1 1 d . . .
H3A H 0.3012 0.4717 0.0302 0.056 Uiso 1 1 calc R . .
H3B H 0.4024 0.5314 0.0189 0.056 Uiso 1 1 calc R . .
H3C H 0.3005 0.5829 0.0373 0.056 Uiso 1 1 calc R . .
C4 C 0.4064(3) 0.5197(2) 0.13406(19) 0.0284(7) Uani 1 1 d . . .
H4A H 0.4660 0.4725 0.1425 0.034 Uiso 1 1 calc R . .
H4B H 0.4414 0.5803 0.1530 0.034 Uiso 1 1 calc R . .
C5 C 0.3960(4) 0.4864(2) 0.26350(18) 0.0327(8) Uani 1 1 d . . .
H5A H 0.3952 0.5473 0.2891 0.039 Uiso 1 1 calc R . .
H5B H 0.4739 0.4709 0.2675 0.039 Uiso 1 1 calc R . .
C6 C 0.3484(4) 0.4117(2) 0.30470(17) 0.0312(8) Uani 1 1 d . . .
H6A H 0.3935 0.4079 0.3597 0.037 Uiso 1 1 calc R . .
H6B H 0.2719 0.4289 0.3033 0.037 Uiso 1 1 calc R . .
C7 C 0.4608(3) 0.2818(2) 0.28407(19) 0.0302(8) Uani 1 1 d . . .
H7A H 0.5075 0.3261 0.2666 0.045 Uiso 1 1 calc R . .
H7B H 0.4586 0.2224 0.2568 0.045 Uiso 1 1 calc R . .
H7C H 0.4915 0.2718 0.3401 0.045 Uiso 1 1 calc R . .
C8 C 0.2758(3) 0.2533(2) 0.29461(18) 0.0275(7) Uani 1 1 d . . .
H8A H 0.1997 0.2788 0.2812 0.033 Uiso 1 1 calc R . .
H8B H 0.3038 0.2486 0.3518 0.033 Uiso 1 1 calc R . .
C9 C 0.2717(3) 0.1570(2) 0.26025(17) 0.0260(7) Uani 1 1 d . . .
C10 C 0.2964(3) 0.0789(2) 0.30811(18) 0.0288(8) Uani 1 1 d . . .
H10 H 0.3190 0.0880 0.3627 0.035 Uiso 1 1 calc R . .
C11 C 0.2896(3) -0.0128(2) 0.27932(19) 0.0299(8) Uani 1 1 d . . .
C12 C 0.3146(4) -0.0960(3) 0.3330(2) 0.0379(9) Uani 1 1 d . . .
H12A H 0.2938 -0.1534 0.3026 0.057 Uiso 1 1 calc R . .
H12B H 0.2722 -0.0913 0.3705 0.057 Uiso 1 1 calc R . .
H12C H 0.3939 -0.0975 0.3607 0.057 Uiso 1 1 calc R . .
C13 C 0.2591(3) -0.0230(2) 0.2000(2) 0.0304(8) Uani 1 1 d . . .
H13 H 0.2556 -0.0840 0.1789 0.037 Uiso 1 1 calc R . .
C14 C 0.2328(3) 0.0540(2) 0.14857(18) 0.0256(7) Uani 1 1 d . . .
C15 C 0.2356(3) 0.1451(2) 0.17856(17) 0.0231(7) Uani 1 1 d . . .
C16 C 0.2019(3) 0.0309(2) 0.06591(18) 0.0273(7) Uani 1 1 d . . .
H16 H 0.2089 -0.0325 0.0530 0.033 Uiso 1 1 calc R . .
C17 C 0.1423(4) 0.0505(2) -0.06938(18) 0.0324(9) Uani 1 1 d . . .
H17A H 0.1475 -0.0184 -0.0671 0.039 Uiso 1 1 calc R . .
H17B H 0.1981 0.0738 -0.0937 0.039 Uiso 1 1 calc R . .
C18 C 0.0268(4) 0.0791(2) -0.11876(19) 0.0352(9) Uani 1 1 d . . .
H18A H 0.0021 0.0352 -0.1628 0.042 Uiso 1 1 calc R . .
H18B H -0.0249 0.0732 -0.0871 0.042 Uiso 1 1 calc R . .
C19 C 0.0193(3) 0.1768(2) -0.15025(18) 0.0277(7) Uani 1 1 d . . .
C20 C -0.0297(4) 0.1967(3) -0.22782(18) 0.0352(9) Uani 1 1 d . . .
H20 H -0.0626 0.1479 -0.2626 0.042 Uiso 1 1 calc R . .
C21 C -0.0312(4) 0.2862(3) -0.25512(19) 0.0387(10) Uani 1 1 d . . .
H21 H -0.0653 0.2998 -0.3084 0.046 Uiso 1 1 calc R . .
C22 C 0.0174(4) 0.3558(3) -0.2040(2) 0.0356(9) Uani 1 1 d . . .
H22 H 0.0176 0.4185 -0.2210 0.043 Uiso 1 1 calc R . .
C23 C 0.0660(3) 0.3320(2) -0.12703(18) 0.0292(8) Uani 1 1 d . . .
H23 H 0.1008 0.3798 -0.0919 0.035 Uiso 1 1 calc R . .
C24 C 0.3771(3) 0.2758(2) 0.04562(18) 0.0268(7) Uani 1 1 d . . .
C25 C 0.0684(3) 0.3921(2) 0.09570(18) 0.0240(7) Uani 1 1 d . . .
C26 C -0.1138(3) 0.2022(2) 0.02847(18) 0.0261(7) Uani 1 1 d . . .
C27 C -0.0500(3) 0.4191(2) 0.0608(2) 0.0334(8) Uani 1 1 d . . .
H27A H -0.0906 0.4095 0.0989 0.050 Uiso 1 1 calc R . .
H27B H -0.0829 0.3806 0.0149 0.050 Uiso 1 1 calc R . .
H27C H -0.0542 0.4850 0.0458 0.050 Uiso 1 1 calc R . .
C28 C 0.4785(4) 0.2570(4) 0.0211(2) 0.0525(12) Uani 1 1 d . . .
H28A H 0.4611 0.2109 -0.0209 0.079 Uiso 1 1 calc R . .
H28B H 0.5373 0.2327 0.0653 0.079 Uiso 1 1 calc R . .
H28C H 0.5034 0.3150 0.0028 0.079 Uiso 1 1 calc R . .
O1WA O 0.4442(15) 0.0034(11) 0.0118(8) 0.175(5) Uiso 0.568(9) 1 d PU . 1
O1WB O 0.4189(18) -0.0662(14) 0.0686(10) 0.170(5) Uiso 0.432(9) 1 d PU . 2
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
_geom_angle_publ_flag
O1 Ni1 N4 90.62(9) . . ?
O1 Ni1 N5 93.18(10) . . ?
N4 Ni1 N5 93.58(12) . . ?
O1 Ni1 N3 173.42(10) . . ?
N4 Ni1 N3 94.99(10) . . ?
N5 Ni1 N3 89.91(11) . . ?
O1 Ni1 O3 91.50(10) . . ?
N4 Ni1 O3 88.65(11) . . ?
N5 Ni1 O3 174.79(10) . . ?
N3 Ni1 O3 85.21(11) . . ?
O1 Ni1 O4 78.75(8) . . ?
N4 Ni1 O4 168.35(10) . . ?
N5 Ni1 O4 91.77(10) . . ?
N3 Ni1 O4 95.36(10) . . ?
O3 Ni1 O4 86.90(9) . . ?
O2 Ni2 O1 89.57(10) . . ?
O2 Ni2 N1 96.24(11) . . ?
O1 Ni2 N1 91.19(10) . . ?
O2 Ni2 O5 165.86(9) . . ?
O1 Ni2 O5 87.72(10) . . ?
N1 Ni2 O5 97.69(11) . . ?
O2 Ni2 O4 104.41(9) . . ?
O1 Ni2 O4 79.30(9) . . ?
N1 Ni2 O4 157.09(12) . . ?
O5 Ni2 O4 61.45(9) . . ?
O2 Ni2 N2 92.94(10) . . ?
O1 Ni2 N2 176.83(9) . . ?
N1 Ni2 N2 86.61(10) . . ?
O5 Ni2 N2 90.30(10) . . ?
O4 Ni2 N2 101.91(9) . . ?
O2 Ni2 C25 135.64(10) . . ?
O1 Ni2 C25 82.24(10) . . ?
N1 Ni2 C25 127.29(12) . . ?
O5 Ni2 C25 30.22(9) . . ?
O4 Ni2 C25 31.24(10) . . ?
N2 Ni2 C25 97.27(11) . . ?
C15 O1 Ni1 128.84(19) . . ?
C15 O1 Ni2 128.0(2) . . ?
Ni1 O1 Ni2 100.19(9) . . ?
C24 O2 Ni2 123.4(2) . . ?
C24 O3 Ni1 130.4(2) . . ?
C25 O4 Ni2 88.77(18) . . ?
C25 O4 Ni1 116.57(19) . . ?
Ni2 O4 Ni1 90.21(9) . . ?
C25 O5 Ni2 90.9(2) . . ?
C7 N1 C6 110.9(3) . . ?
C7 N1 C8 110.0(3) . . ?
C6 N1 C8 109.8(3) . . ?
C7 N1 Ni2 116.7(2) . . ?
C6 N1 Ni2 101.48(19) . . ?
C8 N1 Ni2 107.6(2) . . ?
C4 N2 C5 108.7(3) . . ?
C4 N2 C2 111.9(3) . . ?
C5 N2 C2 109.9(3) . . ?
C4 N2 Ni2 111.35(19) . . ?
C5 N2 Ni2 102.60(19) . . ?
C2 N2 Ni2 112.0(2) . . ?
C23 N3 C19 118.0(3) . . ?
C23 N3 Ni1 118.2(2) . . ?
C19 N3 Ni1 123.7(2) . . ?
C16 N4 C17 117.8(3) . . ?
C16 N4 Ni1 125.6(2) . . ?
C17 N4 Ni1 116.6(2) . . ?
C26 N5 Ni1 167.3(3) . . ?
N2 C2 C1 116.1(3) . . ?
N2 C4 C3 112.7(3) . . ?
N2 C5 C6 110.9(3) . . ?
N1 C6 C5 110.7(3) . . ?
N1 C8 C9 113.4(3) . . ?
C10 C9 C15 119.5(3) . . ?
C10 C9 C8 120.5(3) . . ?
C15 C9 C8 119.9(3) . . ?
C9 C10 C11 123.0(3) . . ?
C13 C11 C10 116.8(3) . . ?
C13 C11 C12 121.6(3) . . ?
C10 C11 C12 121.6(3) . . ?
C11 C13 C14 122.5(3) . . ?
C15 C14 C13 119.7(3) . . ?
C15 C14 C16 124.7(3) . . ?
C13 C14 C16 115.6(3) . . ?
O1 C15 C14 122.4(3) . . ?
O1 C15 C9 119.4(3) . . ?
C14 C15 C9 118.3(3) . . ?
N4 C16 C14 126.5(3) . . ?
N4 C17 C18 111.0(3) . . ?
C19 C18 C17 114.5(3) . . ?
N3 C19 C20 120.7(3) . . ?
N3 C19 C18 117.0(3) . . ?
C20 C19 C18 122.3(3) . . ?
C21 C20 C19 120.7(3) . . ?
C20 C21 C22 118.8(3) . . ?
C21 C22 C23 118.1(3) . . ?
N3 C23 C22 123.6(3) . . ?
O3 C24 O2 125.5(3) . . ?
O3 C24 C28 117.5(3) . . ?
O2 C24 C28 116.9(3) . . ?
O5 C25 O4 118.9(3) . . ?
O5 C25 C27 121.5(3) . . ?
O4 C25 C27 119.6(3) . . ?
O5 C25 Ni2 58.92(18) . . ?
O4 C25 Ni2 60.00(18) . . ?
C27 C25 Ni2 178.6(2) . . ?
N5 C26 S1 178.6(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
Ni1 O1 2.000(2) . ?
Ni1 N4 2.014(3) . ?
Ni1 N5 2.068(3) . ?
Ni1 N3 2.074(3) . ?
Ni1 O3 2.081(3) . ?
Ni1 O4 2.210(2) . ?
Ni2 O2 1.995(3) . ?
Ni2 O1 2.034(2) . ?
Ni2 N1 2.060(3) . ?
Ni2 O5 2.134(3) . ?
Ni2 O4 2.158(2) . ?
Ni2 N2 2.196(3) . ?
Ni2 C25 2.491(4) . ?
S1 C26 1.635(4) . ?
O1 C15 1.321(4) . ?
O2 C24 1.274(4) . ?
O3 C24 1.252(4) . ?
O4 C25 1.292(4) . ?
O5 C25 1.254(4) . ?
N1 C7 1.475(5) . ?
N1 C6 1.483(4) . ?
N1 C8 1.495(5) . ?
N2 C4 1.487(5) . ?
N2 C5 1.496(4) . ?
N2 C2 1.499(5) . ?
N3 C23 1.337(4) . ?
N3 C19 1.357(4) . ?
N4 C16 1.281(4) . ?
N4 C17 1.461(4) . ?
N5 C26 1.160(5) . ?
C1 C2 1.539(5) . ?
C3 C4 1.526(5) . ?
C5 C6 1.524(5) . ?
C8 C9 1.509(5) . ?
C9 C10 1.391(4) . ?
C9 C15 1.419(4) . ?
C10 C11 1.407(5) . ?
C11 C13 1.376(5) . ?
C11 C12 1.511(4) . ?
C13 C14 1.417(4) . ?
C14 C15 1.410(4) . ?
C14 C16 1.464(4) . ?
C17 C18 1.525(6) . ?
C18 C19 1.503(5) . ?
C19 C20 1.383(5) . ?
C20 C21 1.372(6) . ?
C21 C22 1.375(6) . ?
C22 C23 1.386(5) . ?
C24 C28 1.496(6) . ?
C25 C27 1.492(5) . ?
O1WA O1WA 1.59(3) 3_655 ?
