#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/05/4310557.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_4310557
loop_
_publ_author_name
'Nizamuddin Shaikh'
'Anangamohan Panja'
'Sanchita Goswami'
'Pradyot Banerjee'
'Pavel Vojtíšek'
'Yuan-Zhu Zhang'
'Gang Su'
'Song Gao'
_publ_section_title
;
 Slow Magnetic Relaxation in a Mixed-Valence Mn(II/III) Complex:
 [MnII2(bispicen)2(μ3-Cl)2MnIII(Cl4Cat)2MnIII(Cl4Cat)2(H2O)2]∞
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              849
_journal_page_last               851
_journal_paper_doi               10.1021/ic035072g
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C52 H40 Cl18 Mn4 N8 O10'
_chemical_formula_weight         1794.78
_space_group_IT_number           23
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.348(2)
_cell_length_b                   12.654(2)
_cell_length_c                   28.525(5)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.86
_cell_volume                     3374.2(11)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            3874
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    1.505
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.083
_refine_diff_density_min         -1.427
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.53(2)
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0326
_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)+(0.0491P)²+3.5124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                3685
_reflns_number_total             3874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035072gsi20030910_105601.cif
_cod_data_source_block           NS7
_cod_depositor_comments
;
The following automatic conversions were performed:
'__diffrn_measurement_device_type' tag replaced with
'_diffrn_measurement_device_type'.

'__computing_data_collection' tag
replaced with '_computing_data_collection'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'no' was replaced with
'none' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        3374.21(11)
_cod_database_code               4310557
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-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
Mn1 Mn 0.5000 0.1390 0.0000 0.03230(13) Uani 1 2 d S . .
Mn2 Mn 0.0000 0.5000 0.0000 0.03756(18) Uani 1 4 d S . .
Mn3 Mn 0.0000 0.0000 0.0000 0.03514(17) Uani 1 4 d S . .
Cl1 Cl 0.3040 0.0000 0.0000 0.03571(17) Uani 1 2 d S . .
Cl12 Cl 0.03055(9) 0.24513(5) 0.13116(3) 0.0520(2) Uani 1 1 d . . .
Cl13 Cl 0.01018(16) 0.12325(7) 0.22743(3) 0.0681(3) Uani 1 1 d . . .
Cl22 Cl 0.33061(7) 0.46949(7) 0.13149(3) 0.0528(2) Uani 1 1 d . . .
Cl23 Cl 0.16643(11) 0.48418(15) 0.22683(3) 0.0858(4) Uani 1 1 d . . .
N1 N 0.4881(3) 0.15167(18) 0.07982(7) 0.0382(5) Uani 1 1 d . . .
N2 N 0.6413(3) 0.27533(18) 0.02074(9) 0.0358(5) Uani 1 1 d . . .
O11 O 0.0074(3) 0.10222(12) 0.04833(6) 0.0353(4) Uani 1 1 d . . .
O21 O 0.13874(18) 0.4923(2) 0.04842(6) 0.0370(4) Uani 1 1 d . . .
C1 C 0.5939(3) 0.2076(2) 0.09958(11) 0.0388(6) Uani 1 1 d . . .
C2 C 0.6038(5) 0.2204(3) 0.14752(13) 0.0573(9) Uani 1 1 d . . .
C3 C 0.5002(7) 0.1756(3) 0.17597(11) 0.0689(10) Uani 1 1 d . . .
C4 C 0.3918(5) 0.1192(4) 0.15588(14) 0.0634(10) Uani 1 1 d . . .
C5 C 0.3876(4) 0.1096(3) 0.10790(13) 0.0509(8) Uani 1 1 d . . .
C6 C 0.7040(3) 0.2535(2) 0.06696(10) 0.0389(6) Uani 1 1 d . . .
C7 C 0.5465(3) 0.3693(2) 0.02207(12) 0.0417(6) Uani 1 1 d . . .
C11 C 0.0046 0.05572(17) 0.0907 0.0323(4) Uani 1 1 d . . .
C13 C 0.0046(4) 0.0547(2) 0.17517(9) 0.0432(5) Uani 1 1 d . . .
C12 C 0.0116(3) 0.10968(18) 0.13262(10) 0.0375(5) Uani 1 1 d . . .
C21 C 0.0755(2) 0.4951(2) 0.09055(8) 0.0296(4) Uani 1 1 d . . .
C22 C 0.1475(2) 0.4883(2) 0.13243(8) 0.0330(5) Uani 1 1 d . . .
C23 C 0.0735(3) 0.4937(3) 0.17475(9) 0.0413(6) Uani 1 1 d . . .
O99 O 0.0000 0.3054(2) 0.0000 0.0556(8) Uani 1 2 d S . .
H1 H 0.709(4) 0.283(2) -0.0017(15) 0.039(7) Uiso 1 1 d . . .
H2 H 0.680(5) 0.256(3) 0.1561(14) 0.053(10) Uiso 1 1 d . . .
H3 H 0.497(7) 0.184(3) 0.2055(15) 0.079(12) Uiso 1 1 d . . .
H4 H 0.322(5) 0.086(3) 0.1697(15) 0.058(11) Uiso 1 1 d . . .
H5 H 0.312(5) 0.072(3) 0.0912(14) 0.055(11) Uiso 1 1 d . . .
H6A H 0.740(4) 0.316(3) 0.0832(12) 0.044(10) Uiso 1 1 d . . .
H6B H 0.780(5) 0.199(3) 0.0652(13) 0.054(10) Uiso 1 1 d . . .
H7B H 0.480(4) 0.356(3) 0.0540(11) 0.042(8) Uiso 1 1 d . . .
H7A H 0.595(5) 0.435(4) 0.0257(15) 0.069(13) Uiso 1 1 d . . .
H99 H 0.009(7) 0.260(4) 0.0214(14) 0.082(14) 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
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'
Cl Cl 0.1484 0.1585 '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'
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
N2 Mn1 N2 79.99(12) . 4_655 ?
N2 Mn1 N1 100.34(9) . 4_655 ?
N2 Mn1 N1 73.32(9) 4_655 4_655 ?
N2 Mn1 N1 73.32(9) . . ?
N2 Mn1 N1 100.34(9) 4_655 . ?
N1 Mn1 N1 171.95(11) 4_655 . ?
N2 Mn1 Cl1 162.50(7) . . ?
N2 Mn1 Cl1 96.16(6) 4_655 . ?
N1 Mn1 Cl1 94.80(6) 4_655 . ?
N1 Mn1 Cl1 90.77(6) . . ?
N2 Mn1 Cl1 96.16(6) . 2_655 ?
N2 Mn1 Cl1 162.50(7) 4_655 2_655 ?
N1 Mn1 Cl1 90.77(6) 4_655 2_655 ?
N1 Mn1 Cl1 94.80(6) . 2_655 ?
Cl1 Mn1 Cl1 92.339(1) . 2_655 ?
O21 Mn2 O21 86.56(10) . 2_565 ?
O21 Mn2 O21 174.09(15) . 4 ?
O21 Mn2 O21 93.74(10) 2_565 4 ?
O21 Mn2 O21 93.74(10) . 3_565 ?
O21 Mn2 O21 174.09(15) 2_565 3_565 ?
O21 Mn2 O21 86.56(10) 4 3_565 ?
O21 Mn2 O99 87.04(8) . . ?
O21 Mn2 O99 92.96(8) 2_565 . ?
O21 Mn2 O99 87.04(8) 4 . ?
O21 Mn2 O99 92.96(8) 3_565 . ?
O21 Mn2 O99 92.96(8) . 2_565 ?
O21 Mn2 O99 87.04(8) 2_565 2_565 ?
O21 Mn2 O99 92.96(8) 4 2_565 ?
O21 Mn2 O99 87.04(8) 3_565 2_565 ?
O99 Mn2 O99 180.0 . 2_565 ?
O11 Mn3 O11 86.44(10) 2 . ?
O11 Mn3 O11 93.71(10) 2 3 ?
O11 Mn3 O11 175.80(15) . 3 ?
O11 Mn3 O11 175.80(15) 2 4 ?
O11 Mn3 O11 93.71(10) . 4 ?
O11 Mn3 O11 86.44(10) 3 4 ?
O11 Mn3 Cl1 92.10(8) 2 . ?
O11 Mn3 Cl1 87.90(8) . . ?
O11 Mn3 Cl1 87.90(8) 3 . ?
O11 Mn3 Cl1 92.10(8) 4 . ?
O11 Mn3 Cl1 87.90(8) 2 2 ?
O11 Mn3 Cl1 92.10(8) . 2 ?
O11 Mn3 Cl1 92.10(8) 3 2 ?
O11 Mn3 Cl1 87.90(8) 4 2 ?
Cl1 Mn3 Cl1 180.0 . 2 ?
Mn1 Cl1 Mn1 87.661(1) . 2_655 ?
Mn1 Cl1 Mn3 136.169(1) . . ?
Mn1 Cl1 Mn3 136.169(1) 2_655 . ?
C1 N1 C5 118.3(3) . . ?
C1 N1 Mn1 114.85(19) . . ?
C5 N1 Mn1 126.8(2) . . ?
C6 N2 C7 111.5(2) . . ?
C6 N2 Mn1 108.98(17) . . ?
C7 N2 Mn1 105.69(16) . . ?
C6 N2 H1 112(2) . . ?
C7 N2 H1 111(2) . . ?
Mn1 N2 H1 108(2) . . ?
C11 O11 Mn3 110.80(12) . . ?
C21 O21 Mn2 110.47(14) . . ?
N1 C1 C2 121.9(3) . . ?
N1 C1 C6 116.6(3) . . ?
C2 C1 C6 121.4(3) . . ?
C1 C2 C3 119.0(4) . . ?
C1 C2 H2 113(3) . . ?
C3 C2 H2 128(3) . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3 117(4) . . ?
C2 C3 H3 124(4) . . ?
C3 C4 C5 119.0(4) . . ?
C3 C4 H4 128(3) . . ?
C5 C4 H4 113(3) . . ?
N1 C5 C4 122.6(4) . . ?
N1 C5 H5 114(2) . . ?
C4 C5 H5 123(2) . . ?
N2 C6 C1 110.8(2) . . ?
N2 C6 H6A 114(2) . . ?
C1 C6 H6A 105(2) . . ?
N2 C6 H6B 112(2) . . ?
C1 C6 H6B 105(2) . . ?
H6A C6 H6B 110(3) . . ?
N2 C7 C7 108.6(2) . 4_655 ?
N2 C7 H7B 103.4(17) . . ?
C7 C7 H7B 110.6(19) 4_655 . ?
N2 C7 H7A 115(3) . . ?
C7 C7 H7A 111(3) 4_655 . ?
H7B C7 H7A 108(3) . . ?
O11 C11 C12 124.2(2) . . ?
O11 C11 C11 115.98(10) . 2 ?
C12 C11 C11 119.82(13) . 2 ?
C13 C13 C12 119.90(15) 2 . ?
C13 C13 Cl13 120.22(10) 2 . ?
C12 C13 Cl13 119.9(2) . . ?
C11 C12 C13 120.2(2) . . ?
C11 C12 Cl12 118.45(19) . . ?
C13 C12 Cl12 121.3(2) . . ?
O21 C21 C22 124.2(2) . . ?
O21 C21 C21 116.24(12) . 2_565 ?
C22 C21 C21 119.59(13) . 2_565 ?
C21 C22 C23 120.4(2) . . ?
C21 C22 Cl22 118.72(18) . . ?
C23 C22 Cl22 120.82(19) . . ?
C23 C23 C22 119.95(14) 2_565 . ?
C23 C23 Cl23 120.55(10) 2_565 . ?
C22 C23 Cl23 119.5(2) . . ?
Mn2 O99 H99 133(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
Mn1 N2 2.252(2) . ?
Mn1 N2 2.252(2) 4_655 ?
Mn1 N1 2.285(2) 4_655 ?
Mn1 N1 2.285(2) . ?
Mn1 Cl1 2.5398 . ?
Mn1 Cl1 2.5398 2_655 ?
Mn2 O21 1.8971(16) . ?
Mn2 O21 1.8971(16) 2_565 ?
Mn2 O21 1.8971(16) 4 ?
Mn2 O21 1.8971(16) 3_565 ?
Mn2 O99 2.462(3) . ?
Mn2 O99 2.462(3) 2_565 ?
Mn3 O11 1.8916(16) 2 ?
Mn3 O11 1.8916(16) . ?
Mn3 O11 1.8916(16) 3 ?
Mn3 O11 1.8916(16) 4 ?
Mn3 Cl1 2.8418 . ?
Mn3 Cl1 2.8418 2 ?
Cl1 Mn1 2.5398 2_655 ?
Cl12 C12 1.724(2) . ?
Cl13 C13 1.725(3) . ?
Cl22 C22 1.728(2) . ?
Cl23 C23 1.725(3) . ?
N1 C1 1.340(4) . ?
N1 C5 1.345(4) . ?
N2 C6 1.469(4) . ?
N2 C7 1.484(4) . ?
N2 H1 0.90(4) . ?
O11 C11 1.3447(19) . ?
O21 C21 1.340(3) . ?
C1 C2 1.380(5) . ?
C1 C6 1.504(4) . ?
C2 C3 1.385(7) . ?
C2 H2 0.87(4) . ?
C3 C4 1.365(7) . ?
C3 H3 0.85(4) . ?
C4 C5 1.375(5) . ?
C4 H4 0.87(5) . ?
C5 H5 0.98(4) . ?
C6 H6A 0.98(4) . ?
C6 H6B 0.99(4) . ?
C7 C7 1.530(6) 4_655 ?
C7 H7B 1.12(4) . ?
C7 H7A 0.95(5) . ?
C11 C12 1.379(3) . ?
C11 C11 1.413(4) 2 ?
C13 C13 1.388(6) 2 ?
C13 C12 1.400(4) . ?
C21 C22 1.374(3) . ?
C21 C21 1.416(4) 2_565 ?
C22 C23 1.393(3) . ?
C23 C23 1.383(6) 2_565 ?
O99 H99 0.85(4) . ?
