#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/60/7026078.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_7026078
loop_
_publ_author_name
'Núñez, Cristina'
'Bastida, Rufina'
'Macías, Alejandro'
'Valencia, Laura'
'Ribas, Joan'
'Capelo, José Luis'
'Lodeiro, Carlos'
_publ_section_title
;
 New dinuclear nickel(II) and iron(II) complexes with a macrocyclic ligand
 containing a N6S2 donor-set: synthesis, structural, MALDI-TOF-MS,
 magnetic and spectroscopic studies.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7673
_journal_page_last               7683
_journal_paper_doi               10.1039/c0dt00182a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety
'[Ni2 (C22 H34 N6 S2) (CH3CN)4](BF4)4 . 3.5 (CH3CN)'
_chemical_formula_sum            'C18.5 H28.25 B2 F8 N6.75 Ni S'
_chemical_formula_weight         609.62
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.84
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.079
_cell_length_b                   18.517
_cell_length_c                   13.181
_cell_measurement_reflns_used    1805
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.62
_cell_measurement_theta_min      2.88
_cell_volume                     2896.895
_computing_cell_refinement       'BRUKER APEX'
_computing_data_collection       'BRUKER APEX'
_computing_data_reduction        'BRUKER SHELXTL'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  'Wingx publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR-92 (Altornare, Cascarano, Giacovazzo, and Gualardi, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega and phi 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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24504
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  0.9453
_exptl_absorpt_correction_T_min  0.7584
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            mauve
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1250
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         5899
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0546
_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)+(0.0913P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                3613
_reflns_number_total             5899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00182a.txt
_cod_data_source_block           ba19cn2n
_cod_original_cell_volume        2897.0
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C18.50 H28.25 B2 F8 N6.75 Ni S'
_cod_database_code               7026078
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 0.29057(4) 0.02101(2) 0.32493(4) 0.04389(18) Uani 1 1 d . . .
N1 N 0.1389(3) -0.01247(16) 0.2171(3) 0.0504(8) Uani 1 1 d . . .
N2 N 0.3268(3) -0.09145(15) 0.3105(3) 0.0455(7) Uani 1 1 d . . .
N3 N 0.2026(3) 0.11883(17) 0.2931(3) 0.0538(9) Uani 1 1 d . . .
N1S N 0.3528(3) 0.04364(18) 0.2073(3) 0.0567(9) Uani 1 1 d . . .
N2S N 0.2480(3) -0.00739(17) 0.4560(3) 0.0516(8) Uani 1 1 d . . .
N3S N 0.6471(6) -0.0993(4) 0.2123(6) 0.135(2) Uani 1 1 d . . .
N4S N 0.4390(8) -0.3927(5) -0.0327(9) 0.132(3) Uani 0.75 1 d P . .
S S 0.45032(8) 0.09430(5) 0.45625(8) 0.0482(3) Uani 1 1 d . . .
C1 C 0.0523(4) 0.0320(2) 0.1943(4) 0.0615(11) Uani 1 1 d . . .
C2 C -0.0557(4) 0.0091(3) 0.1245(5) 0.0828(15) Uani 1 1 d . . .
H2 H -0.1172 0.0395 0.1084 0.099 Uiso 1 1 calc R . .
C3 C -0.0703(5) -0.0598(3) 0.0790(5) 0.0944(17) Uani 1 1 d . . .
H3 H -0.1420 -0.0757 0.0313 0.113 Uiso 1 1 calc R . .
C4 C 0.0221(4) -0.1050(3) 0.1049(4) 0.0782(14) Uani 1 1 d . . .
H4 H 0.0137 -0.1514 0.0755 0.094 Uiso 1 1 calc R . .
C5 C 0.1267(3) -0.0788(2) 0.1756(3) 0.0543(10) Uani 1 1 d . . .
C6 C 0.2344(4) -0.1209(2) 0.2082(4) 0.0626(11) Uani 1 1 d . . .
H6A H 0.2211 -0.1708 0.2211 0.075 Uiso 1 1 calc R . .
H6B H 0.2572 -0.1197 0.1471 0.075 Uiso 1 1 calc R . .
C7 C 0.4367(3) -0.1174(2) 0.3141(4) 0.0540(10) Uani 1 1 d . . .
H7A H 0.4375 -0.1093 0.2417 0.065 Uiso 1 1 calc R . .
H7B H 0.4430 -0.1690 0.3281 0.065 Uiso 1 1 calc R . .
C8 C 0.4636(3) 0.0804(2) 0.5978(3) 0.0503(9) Uani 1 1 d . . .
H8A H 0.3957 0.0979 0.6023 0.060 Uiso 1 1 calc R . .
H8B H 0.4691 0.0290 0.6133 0.060 Uiso 1 1 calc R . .
C9 C 0.3726(4) 0.1792(2) 0.4187(4) 0.0611(11) Uani 1 1 d . . .
H9A H 0.4032 0.2120 0.4818 0.073 Uiso 1 1 calc R . .
H9B H 0.3836 0.2010 0.3570 0.073 Uiso 1 1 calc R . .
C10 C 0.2489(4) 0.1703(2) 0.3857(4) 0.0641(12) Uani 1 1 d . . .
H10A H 0.2364 0.1527 0.4490 0.077 Uiso 1 1 calc R . .
H10B H 0.2112 0.2165 0.3631 0.077 Uiso 1 1 calc R . .
C11 C 0.0810(4) 0.1024(2) 0.2561(4) 0.0695(12) Uani 1 1 d . . .
H11A H 0.0361 0.1408 0.2077 0.083 Uiso 1 1 calc R . .
H11B H 0.0635 0.0999 0.3206 0.083 Uiso 1 1 calc R . .
C1S C 0.3946(4) 0.0547(2) 0.1502(4) 0.0642(11) Uani 1 1 d . . .
C2S C 0.4485(6) 0.0673(4) 0.0749(6) 0.124(3) Uani 1 1 d . . .
H2S1 H 0.5140 0.0372 0.0964 0.186 Uiso 1 1 calc R . .
H2S2 H 0.4703 0.1171 0.0790 0.186 Uiso 1 1 calc R . .
H2S3 H 0.3966 0.0560 -0.0002 0.186 Uiso 1 1 calc R . .
C3S C 0.2317(4) -0.0291(2) 0.5265(4) 0.0610(11) Uani 1 1 d . . .
C4S C 0.2144(6) -0.0573(3) 0.6218(5) 0.113(2) Uani 1 1 d . . .
H4S1 H 0.2220 -0.1089 0.6243 0.170 Uiso 1 1 calc R . .
H4S2 H 0.1403 -0.0446 0.6139 0.170 Uiso 1 1 calc R . .
H4S3 H 0.2695 -0.0369 0.6897 0.170 Uiso 1 1 calc R . .
C5S C 0.6304(6) -0.1585(6) 0.1887(6) 0.106(2) Uani 1 1 d . . .
C6S C 0.6081(7) -0.2324(4) 0.1577(7) 0.141(3) Uani 1 1 d . . .
H6S1 H 0.5360 -0.2366 0.0952 0.212 Uiso 1 1 calc R . .
H6S2 H 0.6078 -0.2596 0.2196 0.212 Uiso 1 1 calc R . .
H6S3 H 0.6655 -0.2509 0.1374 0.212 Uiso 1 1 calc R . .
C7S C 0.4398(7) -0.3585(6) -0.0987(8) 0.096(3) Uani 0.75 1 d P . .
C8S C 0.4456(7) -0.3129(6) -0.1788(7) 0.112(3) Uani 0.75 1 d P . .
H8S1 H 0.4567 -0.2642 -0.1512 0.169 Uiso 0.75 1 calc PR . .
H8S2 H 0.3767 -0.3158 -0.2454 0.169 Uiso 0.75 1 calc PR . .
H8S3 H 0.5075 -0.3270 -0.1955 0.169 Uiso 0.75 1 calc PR . .
B1 B 0.2352(17) 0.2399(10) 0.0617(14) 0.067(4) Uani 0.616(13) 1 d PDU A 1
F1 F 0.3169(8) 0.2235(6) 0.1595(6) 0.141(4) Uani 0.616(13) 1 d PDU A 1
F2 F 0.1347(9) 0.2333(7) 0.0745(12) 0.137(5) Uani 0.616(13) 1 d PDU A 1
F3 F 0.2431(11) 0.3108(4) 0.0452(9) 0.110(4) Uani 0.616(13) 1 d PDU A 1
F4 F 0.2346(9) 0.1991(4) -0.0203(7) 0.112(3) Uani 0.616(13) 1 d PDU A 1
B1' B 0.214(2) 0.2489(13) 0.050(2) 0.068(6) Uani 0.384(13) 1 d PDU A 2
F1' F 0.158(2) 0.2276(12) 0.108(2) 0.155(8) Uani 0.384(13) 1 d PDU A 2
F2' F 0.2837(19) 0.1907(9) 0.061(3) 0.242(16) Uani 0.384(13) 1 d PDU A 2
F3' F 0.1455(16) 0.2505(11) -0.0588(9) 0.178(9) Uani 0.384(13) 1 d PDU A 2
F4' F 0.2747(17) 0.3082(10) 0.077(2) 0.135(8) Uani 0.384(13) 1 d PDU A 2
B2 B 0.275(2) -0.159(2) -0.069(3) 0.098(6) Uani 0.484(19) 1 d PDU B 1
F5 F 0.240(2) -0.1320(8) -0.1641(9) 0.181(7) Uani 0.484(19) 1 d PDU B 1
F6 F 0.334(2) -0.2185(11) -0.064(2) 0.321(13) Uani 0.484(19) 1 d PDU B 1
F7 F 0.3411(19) -0.1148(16) 0.0178(16) 0.229(10) Uani 0.484(19) 1 d PDU B 1
F8 F 0.1825(16) -0.1853(12) -0.0557(17) 0.179(7) Uani 0.484(19) 1 d PDU B 1
B2' B 0.2941(18) -0.155(2) -0.054(3) 0.068(4) Uani 0.516(19) 1 d PDU B 2
F5' F 0.3634(8) -0.1970(8) 0.0165(14) 0.153(6) Uani 0.516(19) 1 d PDU B 2
F6' F 0.3126(10) -0.0870(5) -0.0171(14) 0.125(5) Uani 0.516(19) 1 d PDU B 2
F7' F 0.3077(17) -0.1615(10) -0.1517(13) 0.162(7) Uani 0.516(19) 1 d PDU B 2
F8' F 0.1860(8) -0.1721(7) -0.0697(14) 0.115(5) Uani 0.516(19) 1 d PDU B 2
H2N H 0.306(3) -0.107(2) 0.367(4) 0.062(12) Uiso 1 1 d . . .
H3N H 0.209(3) 0.139(2) 0.236(3) 0.055(12) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 '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'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
N1 Ni1 N1S 96.63(13) . .
N1 Ni1 N3 80.07(13) . .
N1S Ni1 N3 91.77(14) . .
N1 Ni1 N2S 88.87(13) . .
N1S Ni1 N2S 172.70(13) . .
N3 Ni1 N2S 93.92(13) . .
N1 Ni1 N2 80.03(12) . .
N1S Ni1 N2 87.69(12) . .
N3 Ni1 N2 159.90(14) . .
N2S Ni1 N2 88.53(12) . .
N1 Ni1 S 164.02(9) . .
N1S Ni1 S 86.06(10) . .
N3 Ni1 S 84.10(10) . .
N2S Ni1 S 89.98(9) . .
N2 Ni1 S 115.88(9) . .
C5 N1 C1 122.5(4) . .
C5 N1 Ni1 119.6(3) . .
C1 N1 Ni1 117.9(3) . .
C6 N2 C7 108.4(3) . .
C6 N2 Ni1 107.9(2) . .
C7 N2 Ni1 123.3(2) . .
C10 N3 C11 114.7(3) . .
C10 N3 Ni1 113.4(3) . .
C11 N3 Ni1 108.1(2) . .
C1S N1S Ni1 174.5(4) . .
C3S N2S Ni1 172.5(3) . .
C8 S C9 101.67(18) . .
C8 S Ni1 109.13(13) . .
C9 S Ni1 94.15(15) . .
N1 C1 C2 119.6(4) . .
N1 C1 C11 114.9(4) . .
C2 C1 C11 125.3(4) . .
C1 C2 C3 119.0(5) . .
C2 C3 C4 120.0(5) . .
C5 C4 C3 117.9(5) . .
N1 C5 C4 121.2(4) . .
N1 C5 C6 115.1(4) . .
C4 C5 C6 123.7(4) . .
N2 C6 C5 112.1(3) . .
N2 C7 C8 112.9(3) . 3_656
C7 C8 S 114.0(3) 3_656 .
C10 C9 S 113.2(3) . .
N3 C10 C9 109.4(3) . .
N3 C11 C1 110.2(3) . .
N1S C1S C2S 178.6(5) . .
N2S C3S C4S 178.0(5) . .
N3S C5S C6S 179.2(11) . .
N4S C7S C8S 176.9(12) . .
F4 B1 F1 113.2(15) . .
F4 B1 F3 113.8(11) . .
F1 B1 F3 107.3(17) . .
F4 B1 F2 111.6(17) . .
F1 B1 F2 106.1(11) . .
F3 B1 F2 104.2(15) . .
F1' B1' F4' 121(3) . .
F1' B1' F3' 110(2) . .
F4' B1' F3' 109.2(16) . .
F1' B1' F2' 102.1(19) . .
F4' B1' F2' 109(2) . .
F3' B1' F2' 104(2) . .
F5 B2 F6 110(3) . .
F5 B2 F7 116(3) . .
F6 B2 F7 107(3) . .
F5 B2 F8 108(2) . .
F6 B2 F8 103(3) . .
F7 B2 F8 113(2) . .
F5' B2' F6' 110(2) . .
F5' B2' F7' 108(2) . .
F6' B2' F7' 111(2) . .
F5' B2' F8' 110(2) . .
F6' B2' F8' 107(2) . .
F7' B2' F8' 112(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.993(3) .
Ni1 N1S 2.075(3) .
Ni1 N3 2.092(3) .
Ni1 N2S 2.093(3) .
Ni1 N2 2.162(3) .
Ni1 S 2.4830(11) .
N1 C5 1.327(5) .
N1 C1 1.328(5) .
N2 C6 1.485(5) .
N2 C7 1.498(5) .
N3 C10 1.464(5) .
N3 C11 1.486(5) .
N1S C1S 1.119(5) .
N2S C3S 1.112(5) .
N3S C5S 1.136(9) .
N4S C7S 1.079(11) .
S C8 1.818(4) .
S C9 1.825(4) .
C1 C2 1.389(6) .
C1 C11 1.499(6) .
C2 C3 1.388(7) .
C3 C4 1.390(7) .
C4 C5 1.380(6) .
C5 C6 1.505(6) .
C7 C8 1.499(5) 3_656
C8 C7 1.499(5) 3_656
C9 C10 1.499(6) .
C1S C2S 1.457(6) .
C3S C4S 1.463(6) .
C5S C6S 1.424(11) .
C7S C8S 1.379(12) .
B1 F4 1.32(2) .
B1 F1 1.319(17) .
B1 F3 1.341(18) .
B1 F2 1.399(19) .
B1' F1' 1.32(2) .
B1' F4' 1.32(3) .
B1' F3' 1.33(2) .
B1' F2' 1.38(2) .
B2 F5 1.25(4) .
B2 F6 1.33(4) .
B2 F7 1.38(3) .
B2 F8 1.376(16) .
B2' F5' 1.26(4) .
B2' F6' 1.34(4) .
B2' F7' 1.37(3) .
B2' F8' 1.379(12) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139161945
