#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322809.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_4322809
loop_
_publ_author_name
'T. M. Rajendiran'
'Corine Mathonière'
'Stéphane Golhen'
'Lahcène Ouahab'
'Olivier Kahn'
_publ_section_title
;
 Ferromagnetic Interactions in the Mn(N3)4[Ni(en)2(NO2)]2 Trinuclear
 Compound. Crystal Structure and Physical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2651
_journal_page_last               2654
_journal_paper_doi               10.1021/ic9708531
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C8 H32 Mn N22 Ni2 O4'
_chemical_formula_weight         672.92
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(10)
_cell_angle_beta                 90.14(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.631(14)
_cell_length_b                   15.636(2)
_cell_length_c                   13.430(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.991
_cell_measurement_theta_min      4.996
_cell_volume                     2652(4)
_computing_cell_refinement       'Nonius CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        MolEN
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-nonius CAD4'
_diffrn_measurement_method       θ-2θ
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3497
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.935
_exptl_absorpt_correction_T_max  0.999934
_exptl_absorpt_correction_T_min  0.942974
_exptl_absorpt_correction_type   'Semi empirical \y scan'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.869
_refine_ls_goodness_of_fit_obs   0.827
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         3416
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.872
_refine_ls_restrained_S_obs      0.827
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_obs          0.0355
_refine_ls_shift/esd_max         0.014
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0769P)²+5.5120P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1110
_refine_ls_wR_factor_obs         0.0909
_reflns_number_observed          2630
_reflns_number_total             3418
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9708531.cif
_cod_data_source_block           nimn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+5.5120P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+5.5120P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2652.4(44)
_cod_database_code               4322809
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni 0.23296(6) 0.88755(6) 0.39968(6) 0.0284(2) Uani 1 d . .
Mn1 Mn 0.0000 1.00619(9) 0.5000 0.0351(4) Uani 1 d S .
N1 N 0.0527(7) 1.1013(4) 0.3929(7) 0.063(3) Uani 1 d . .
N2 N 0.0541(5) 1.1760(4) 0.3892(5) 0.041(2) Uani 1 d . .
N3 N 0.0604(7) 1.2486(5) 0.3844(8) 0.067(3) Uani 1 d . .
N4 N 0.0648(5) 0.8993(4) 0.4016(5) 0.038(2) Uani 1 d . .
N5 N 0.0044(5) 0.8450(4) 0.3794(6) 0.039(2) Uani 1 d . .
N6 N -0.0557(6) 0.7924(6) 0.3588(7) 0.063(3) Uani 1 d . .
N7 N 0.3987(5) 0.9001(4) 0.4054(5) 0.038(2) Uani 1 d . .
H7A H 0.4191(5) 0.9128(4) 0.4679(5) 0.056(29) Uiso 1 calc R .
H7B H 0.4292(5) 0.8503(4) 0.3879(5) 0.049(26) Uiso 1 calc R .
C1 C 0.4332(7) 0.9681(6) 0.3375(9) 0.057(3) Uani 1 d . .
H1A H 0.4399(7) 0.9455(6) 0.2705(9) 0.068 Uiso 1 calc R .
H1B H 0.5018(7) 0.9896(6) 0.3583(9) 0.068 Uiso 1 calc R .
C2 C 0.3533(7) 1.0392(5) 0.3388(7) 0.047(2) Uani 1 d . .
H2A H 0.3540(7) 1.0674(5) 0.4032(7) 0.057 Uiso 1 calc R .
H2B H 0.3705(7) 1.0813(5) 0.2882(7) 0.057 Uiso 1 calc R .
N8 N 0.2475(5) 1.0023(4) 0.3191(5) 0.0356(14) Uani 1 d . .
H8A H 0.2398(5) 0.9920(4) 0.2536(5) 0.044(23) Uiso 1 calc R .
H8B H 0.1969(5) 1.0394(4) 0.3380(5) 0.021(16) Uiso 1 calc R .
N9 N 0.2328(6) 0.7721(4) 0.4777(6) 0.045(2) Uani 1 d . .
H9A H 0.2909(6) 0.7685(4) 0.5165(6) 0.099(50) Uiso 1 calc R .
H9B H 0.1753(6) 0.7691(4) 0.5171(6) 0.047(24) Uiso 1 calc R .
C3 C 0.2423(16) 0.7187(7) 0.3096(11) 0.104(5) Uani 1 d . .
H3A H 0.1891(16) 0.6854(7) 0.2749(11) 0.125 Uiso 1 calc R .
H3B H 0.3109(16) 0.6971(7) 0.2893(11) 0.125 Uiso 1 calc R .
C4 C 0.2316(17) 0.7037(7) 0.4083(10) 0.128(8) Uani 1 d . .
H4A H 0.2877(17) 0.6646(7) 0.4274(10) 0.154 Uiso 1 calc R .
H4B H 0.1653(17) 0.6734(7) 0.4172(10) 0.154 Uiso 1 calc R .
N10 N 0.2338(6) 0.8070(5) 0.2756(5) 0.041(2) Uani 1 d . .
H10A H 0.1738(6) 0.8140(5) 0.2403(5) 0.077(37) Uiso 1 calc R .
H10B H 0.2889(6) 0.8199(5) 0.2360(5) 0.069(31) Uiso 1 calc R .
N11 N 0.2294(5) 0.9567(4) 0.5435(5) 0.037(2) Uani 1 d . .
O1 O 0.1527(5) 0.9953(4) 0.5790(4) 0.0470(14) Uani 1 d . .
O2 O 0.3084(6) 0.9541(5) 0.5972(6) 0.066(2) Uani 1 d . .
Ni2 Ni 0.23341(6) 0.38731(6) 0.10019(6) 0.0283(2) Uani 1 d . .
Mn2 Mn 0.5000 1.00592(9) 0.0000 0.0356(4) Uani 1 d S .
N16 N 0.0651(4) 0.4002(4) 0.0974(5) 0.033(2) Uani 1 d . .
N17 N 0.0046(5) 0.3457(4) 0.1202(5) 0.0348(15) Uani 1 d . .
N18 N -0.0563(6) 0.2917(5) 0.1409(7) 0.060(2) Uani 1 d . .
N12 N 0.3997(5) 0.3998(4) 0.0946(5) 0.039(2) Uani 1 d . .
H12A H 0.4304(5) 0.3503(4) 0.1131(5) 0.039(23) Uiso 1 calc R .
H12B H 0.4200(5) 0.4117(4) 0.0319(5) 0.125(54) Uiso 1 calc R .
C5 C 0.3528(7) 0.5400(6) 0.1614(8) 0.052(2) Uani 1 d . .
H5A H 0.3698(7) 0.5818(6) 0.2123(8) 0.062 Uiso 1 calc R .
H5B H 0.3533(7) 0.5686(6) 0.0973(8) 0.062 Uiso 1 calc R .
C6 C 0.4336(7) 0.4695(6) 0.1622(8) 0.051(2) Uani 1 d . .
H6A H 0.5016(7) 0.4916(6) 0.1409(8) 0.061 Uiso 1 calc R .
H6B H 0.4415(7) 0.4474(6) 0.2293(8) 0.061 Uiso 1 calc R .
N13 N 0.2477(5) 0.5034(4) 0.1802(5) 0.0371(14) Uani 1 d . .
H13A H 0.1972(5) 0.5403(4) 0.1605(5) 0.065(31) Uiso 1 calc R .
H13B H 0.2396(5) 0.4936(4) 0.2458(5) 0.038(21) Uiso 1 calc R .
N14 N 0.2332(6) 0.3077(5) 0.2242(6) 0.044(2) Uani 1 d . .
H14A H 0.2920(6) 0.3167(5) 0.2607(6) 0.092(45) Uiso 1 calc R .
H14B H 0.1765(6) 0.3192(5) 0.2624(6) 0.052(25) Uiso 1 calc R .
C7 C 0.2346(17) 0.2034(7) 0.0953(10) 0.131(8) Uani 1 d . .
H7C H 0.1760(17) 0.1657(7) 0.0796(10) 0.157 Uiso 1 calc R .
H7D H 0.2990(17) 0.1710(7) 0.0842(10) 0.157 Uiso 1 calc R .
C8 C 0.2297(15) 0.2195(7) 0.1910(9) 0.104(6) Uani 1 d . .
H8C H 0.2878(15) 0.1895(7) 0.2229(9) 0.125 Uiso 1 calc R .
H8D H 0.1647(15) 0.1945(7) 0.2159(9) 0.125 Uiso 1 calc R .
N15 N 0.2330(6) 0.2720(4) 0.0226(6) 0.045(2) Uani 1 d . .
H15A H 0.1746(6) 0.2682(4) -0.0157(6) 0.047(27) Uiso 1 calc R .
H15B H 0.2903(6) 0.2687(4) -0.0170(6) 0.075(35) Uiso 1 calc R .
O3 O 0.3471(4) 0.9935(4) 0.0794(4) 0.0472(15) Uani 1 d . .
N19 N 0.2702(5) 0.9566(4) 0.0442(5) 0.037(2) Uani 1 d . .
O4 O 0.1905(5) 0.9525(5) 0.0976(5) 0.062(2) Uani 1 d . .
N20 N 0.5495(8) 1.1012(5) 0.1082(8) 0.069(3) Uani 1 d . .
N21 N 0.5541(5) 1.1757(4) 0.1113(5) 0.037(2) Uani 1 d . .
N22 N 0.5599(7) 1.2484(5) 0.1167(8) 0.060(2) Uani 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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
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
N9 Ni1 N10 83.1(3) . . ?
N9 Ni1 N7 93.7(3) . . ?
N10 Ni1 N7 94.5(3) . . ?
N9 Ni1 N8 175.0(3) . . ?
N10 Ni1 N8 95.9(3) . . ?
N7 Ni1 N8 81.4(3) . . ?
N9 Ni1 N4 93.8(3) . . ?
N10 Ni1 N4 93.9(3) . . ?
N7 Ni1 N4 169.3(3) . . ?
N8 Ni1 N4 91.2(3) . . ?
N9 Ni1 N11 89.1(3) . . ?
N10 Ni1 N11 172.1(3) . . ?
N7 Ni1 N11 86.8(3) . . ?
N8 Ni1 N11 92.0(2) . . ?
N4 Ni1 N11 85.7(3) . . ?
N1 Mn1 N1 93.7(4) 2_556 . ?
N1 Mn1 O1 95.9(3) 2_556 2_556 ?
N1 Mn1 O1 90.2(3) . 2_556 ?
N1 Mn1 O1 90.2(3) 2_556 . ?
N1 Mn1 O1 95.9(3) . . ?
O1 Mn1 O1 171.2(3) 2_556 . ?
N1 Mn1 N4 173.7(4) 2_556 . ?
N1 Mn1 N4 90.4(2) . . ?
O1 Mn1 N4 88.8(3) 2_556 . ?
O1 Mn1 N4 84.7(2) . . ?
N1 Mn1 N4 90.4(2) 2_556 2_556 ?
N1 Mn1 N4 173.7(4) . 2_556 ?
O1 Mn1 N4 84.7(2) 2_556 2_556 ?
O1 Mn1 N4 88.8(3) . 2_556 ?
N4 Mn1 N4 85.9(3) . 2_556 ?
N2 N1 Mn1 135.7(6) . . ?
N3 N2 N1 176.8(8) . . ?
N5 N4 Ni1 125.3(5) . . ?
N5 N4 Mn1 116.2(4) . . ?
Ni1 N4 Mn1 115.4(3) . . ?
N6 N5 N4 178.9(7) . . ?
C1 N7 Ni1 110.0(5) . . ?
N7 C1 C2 109.2(6) . . ?
N8 C2 C1 108.4(7) . . ?
C2 N8 Ni1 108.7(5) . . ?
C4 N9 Ni1 108.7(7) . . ?
C4 C3 N10 117.6(9) . . ?
C3 C4 N9 120.9(10) . . ?
C3 N10 Ni1 108.7(7) . . ?
O2 N11 O1 115.1(7) . . ?
O2 N11 Ni1 118.5(5) . . ?
O1 N11 Ni1 126.3(6) . . ?
N11 O1 Mn1 122.4(5) . . ?
N14 Ni2 N15 83.3(3) . . ?
N14 Ni2 N12 95.0(3) . . ?
N15 Ni2 N12 93.6(3) . . ?
N14 Ni2 N16 93.9(3) . . ?
N15 Ni2 N16 94.1(3) . . ?
N12 Ni2 N16 168.9(3) . . ?
N14 Ni2 N13 96.1(3) . . ?
N15 Ni2 N13 175.2(3) . . ?
N12 Ni2 N13 81.7(3) . . ?
N16 Ni2 N13 90.7(2) . . ?
N14 Ni2 N19 172.3(3) . 4_545 ?
N15 Ni2 N19 89.1(3) . 4_545 ?
N12 Ni2 N19 86.7(3) . 4_545 ?
N16 Ni2 N19 85.4(2) . 4_545 ?
N13 Ni2 N19 91.5(3) . 4_545 ?
N20 Mn2 N20 93.4(5) . 2_655 ?
N20 Mn2 O3 89.3(3) . . ?
N20 Mn2 O3 97.6(3) 2_655 . ?
N20 Mn2 O3 97.6(3) . 2_655 ?
N20 Mn2 O3 89.3(3) 2_655 2_655 ?
O3 Mn2 O3 169.9(3) . 2_655 ?
N20 Mn2 N16 172.7(3) . 4 ?
N20 Mn2 N16 90.6(3) 2_655 4 ?
O3 Mn2 N16 84.2(2) . 4 ?
O3 Mn2 N16 88.5(2) 2_655 4 ?
N20 Mn2 N16 90.6(3) . 3 ?
N20 Mn2 N16 172.7(3) 2_655 3 ?
O3 Mn2 N16 88.5(2) . 3 ?
O3 Mn2 N16 84.2(2) 2_655 3 ?
N16 Mn2 N16 86.0(4) 4 3 ?
N17 N16 Ni2 124.8(5) . . ?
N17 N16 Mn2 116.2(5) . 3_445 ?
Ni2 N16 Mn2 116.1(2) . 3_445 ?
N18 N17 N16 178.7(10) . . ?
C6 N12 Ni2 109.4(4) . . ?
N13 C5 C6 109.1(7) . . ?
N12 C6 C5 109.9(9) . . ?
C5 N13 Ni2 108.8(4) . . ?
C8 N14 Ni2 108.9(6) . . ?
C8 C7 N15 121.2(9) . . ?
C7 C8 N14 118.8(9) . . ?
C7 N15 Ni2 107.6(6) . . ?
N19 O3 Mn2 123.2(4) . . ?
O3 N19 O4 116.5(7) . . ?
O3 N19 Ni2 125.6(4) . 4 ?
O4 N19 Ni2 117.7(6) . 4 ?
N21 N20 Mn2 136.2(9) . . ?
N22 N21 N20 178.1(10) . . ?
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 N9 2.088(7) . ?
Ni1 N10 2.089(7) . ?
Ni1 N7 2.104(7) . ?
Ni1 N8 2.104(6) . ?
Ni1 N4 2.132(7) . ?
Ni1 N11 2.214(7) . ?
Mn1 N1 2.174(7) 2_556 ?
Mn1 N1 2.174(7) . ?
Mn1 O1 2.206(7) 2_556 ?
Mn1 O1 2.206(7) . ?
Mn1 N4 2.283(6) . ?
Mn1 N4 2.283(6) 2_556 ?
N1 N2 1.170(9) . ?
N2 N3 1.138(9) . ?
N4 N5 1.180(10) . ?
N5 N6 1.152(11) . ?
N7 C1 1.467(11) . ?
C1 C2 1.503(12) . ?
C2 N8 1.479(11) . ?
N9 C4 1.419(15) . ?
C3 C4 1.35(2) . ?
C3 N10 1.458(14) . ?
N11 O2 1.231(11) . ?
N11 O1 1.238(8) . ?
Ni2 N14 2.079(7) . ?
Ni2 N15 2.082(7) . ?
Ni2 N12 2.111(6) . ?
Ni2 N16 2.136(6) . ?
Ni2 N13 2.117(7) . ?
Ni2 N19 2.221(7) 4_545 ?
Mn2 N20 2.171(9) . ?
Mn2 N20 2.171(9) 2_655 ?
Mn2 O3 2.216(5) . ?
Mn2 O3 2.216(5) 2_655 ?
Mn2 N16 2.262(7) 4 ?
Mn2 N16 2.262(7) 3 ?
N16 N17 1.184(8) . ?
N16 Mn2 2.262(7) 3_445 ?
N17 N18 1.176(10) . ?
N12 C6 1.481(12) . ?
C5 N13 1.468(10) . ?
C5 C6 1.502(12) . ?
N14 C8 1.450(14) . ?
C7 C8 1.31(2) . ?
C7 N15 1.451(14) . ?
O3 N19 1.224(9) . ?
N19 O4 1.239(7) . ?
N19 Ni2 2.221(7) 4 ?
N20 N21 1.168(10) . ?
N21 N22 1.141(9) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168337498
