#------------------------------------------------------------------------------
#$Date: 2020-11-09 04:04:46 +0200 (Mon, 09 Nov 2020) $
#$Revision: 259049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/94/4339483.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_4339483
loop_
_publ_author_name
'Feng, Patrick L.'
'Beedle, Christopher C.'
'Wernsdorfer, Wolfgang'
'Koo, Changhyun'
'Nakano, Motohiro'
'Hill, Stephen'
'Hendrickson, David N.'
_publ_section_title
;
 Heterometallic cubane single-molecule magnets.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8126
_journal_page_last               8128
_journal_paper_doi               10.1021/ic7012107
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C41 H35 Cl6 Mn3 N12 Ni1 O10'
_chemical_formula_sum            'C41 H35 Cl6 Mn3 N12 Ni O10'
_chemical_formula_weight         1292.015
_space_group.centring_type       P
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.453(4)
_cell_length_b                   15.453
_cell_length_c                   38.060(10)
_cell_measurement_reflns_used    17761
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.63
_cell_volume                     7871(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP32
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_refln_scan_rate          10
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            17761
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3816
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
  SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent
 contributions.  Total electron count found = 673/unit cell.
 Calculated for 2 chloroform (the re'xtal solvent)
 = 696/unit cell.  The intensive properties (density, F(000), etc.)
 reflect these contributions.
;
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3097
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0626P)²+2.4088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                2870
_reflns_number_total             3097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7012107-file001.cif
_cod_data_source_block           import
_cod_depositor_comments
;
 Changed the value of the _symmetry_cell_setting data item from
 'rhombohedral' back to 'trigonal'.

 Antanas Vaitkus,
 2020-11-09

 Removed the _space_group.IT_number data item since it had an incorrect
 value, changed the value of the _symmetry_cell_setting data item from
 'trigonal' to 'rhombohedral' and renamed several space group related
 data items.

 Antanas Vaitkus,
 2020-11-08

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_space_group.centring_type' value 'primitive' was replaced with the
value 'P' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_original_cell_volume        7870(3)
_cod_original_sg_symbol_H-M      R3c
_cod_original_formula_sum        'C41 H35 Cl6 Mn3 N12 Ni1 O10'
_cod_database_code               4339483
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-y, -x, z+1/2'
'-x+y, -x, z'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
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
N3 N 0.2004(3) 0.2682(3) 0.92904(10) 0.0602(10) Uani 1 1 d .
Ni1 Ni 0.3333 0.6667 0.98881(2) 0.0336(2) Uani 1 3 d S
Mn1 Mn 0.25634(4) 0.53631(4) 0.918217(14) 0.03466(17) Uani 1 1 d .
O4 O 0.21516(18) 0.59927(18) 0.95439(10) 0.0352(5) Uani 1 1 d .
O3 O 0.3333 0.6667 0.89958(13) 0.0351(10) Uani 1 3 d S
O2 O 0.3210(2) 0.48311(18) 0.88881(7) 0.0418(7) Uani 1 1 d .
N1 N 0.1824(2) 0.4076(2) 0.94167(9) 0.0412(8) Uani 1 1 d .
N2 N 0.1931(3) 0.3374(2) 0.93435(9) 0.0425(8) Uani 1 1 d .
N4 N 0.2262(2) 0.6795(2) 1.01544(8) 0.0349(6) Uani 1 1 d .
O1 O 0.13510(19) 0.5217(2) 0.88499(8) 0.0443(6) Uani 1 1 d .
C009 C 0.0487(3) 0.6068(3) 1.02153(10) 0.0406(8) Uani 1 1 d .
H009 H -0.0154 0.5605 1.0140 0.049 Uiso 1 1 calc R
C010 C 0.1325(2) 0.6176(2) 1.00388(11) 0.0349(8) Uani 1 1 d .
C011 C 0.2376(3) 0.7359(3) 1.04377(11) 0.0417(9) Uani 1 1 d .
H011 H 0.3018 0.7798 1.0518 0.050 Uiso 1 1 calc R
C012 C 0.4405(3) 0.4600(3) 0.85854(10) 0.0435(9) Uani 1 1 d .
C013 C 0.4044(4) 0.2980(3) 0.83931(13) 0.0589(12) Uani 1 1 d .
H013 H 0.3615 0.2292 0.8386 0.071 Uiso 1 1 calc R
C014 C 0.0628(3) 0.6661(3) 1.05024(11) 0.0471(10) Uani 1 1 d .
H014 H 0.0080 0.6617 1.0620 0.057 Uiso 1 1 calc R
C015 C 0.5280(3) 0.5017(3) 0.83993(13) 0.0557(12) Uani 1 1 d .
H015 H 0.5692 0.5707 0.8398 0.067 Uiso 1 1 calc R
C016 C 0.1232(3) 0.5566(3) 0.97206(12) 0.0403(9) Uani 1 1 d .
H01A H 0.1034 0.4888 0.9790 0.048 Uiso 1 1 calc R
H01B H 0.0723 0.5541 0.9565 0.048 Uiso 1 1 calc R
C017 C 0.4124(3) 0.5267(3) 0.87909(10) 0.0414(9) Uani 1 1 d .
C018 C 0.4933(4) 0.3387(4) 0.82170(13) 0.0633(13) Uani 1 1 d .
H018 H 0.5115 0.2972 0.8101 0.076 Uiso 1 1 calc R
C019 C 0.1568(3) 0.7312(3) 1.06149(11) 0.0450(9) Uani 1 1 d .
H019 H 0.1670 0.7720 1.0808 0.054 Uiso 1 1 calc R
C020 C 0.5568(3) 0.4417(3) 0.82099(14) 0.0609(13) Uani 1 1 d .
H020 H 0.6164 0.4702 0.8084 0.073 Uiso 1 1 calc R
C021 C 0.3766(3) 0.3574(3) 0.85823(12) 0.0551(11) Uani 1 1 d .
H021 H 0.3164 0.3289 0.8704 0.066 Uiso 1 1 calc R
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'
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'
Ni Ni 0.3393 1.1124 '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'
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
N4 Ni1 N4 97.31(12) . 4_565
N4 Ni1 N4 97.31(12) . 2_665
N4 Ni1 N4 97.31(12) 4_565 2_665
N4 Ni1 O4 78.87(12) . .
N4 Ni1 O4 161.16(11) 4_565 .
N4 Ni1 O4 101.47(11) 2_665 .
N4 Ni1 O4 101.47(11) . 4_565
N4 Ni1 O4 78.87(12) 4_565 4_565
N4 Ni1 O4 161.16(11) 2_665 4_565
O4 Ni1 O4 83.80(14) . 4_565
N4 Ni1 O4 161.16(11) . 2_665
N4 Ni1 O4 101.47(11) 4_565 2_665
N4 Ni1 O4 78.87(12) 2_665 2_665
O4 Ni1 O4 83.80(14) . 2_665
O4 Ni1 O4 83.80(14) 4_565 2_665
O3 Mn1 O2 92.98(12) . .
O3 Mn1 N1 174.62(19) . .
O2 Mn1 N1 89.70(12) . .
O3 Mn1 O4 85.55(15) . .
O2 Mn1 O4 168.05(12) . .
N1 Mn1 O4 90.85(14) . .
O3 Mn1 O1 86.75(11) . .
O2 Mn1 O1 102.72(12) . .
N1 Mn1 O1 97.21(13) . .
O4 Mn1 O1 89.06(12) . .
O3 Mn1 O4 74.82(14) . 2_665
O2 Mn1 O4 90.24(11) . 2_665
N1 Mn1 O4 100.52(12) . 2_665
O4 Mn1 O4 77.92(15) . 2_665
O1 Mn1 O4 158.06(9) . 2_665
O3 Mn1 Mn1 36.59(8) . 2_665
O2 Mn1 Mn1 82.51(8) . 2_665
N1 Mn1 Mn1 139.55(10) . 2_665
O4 Mn1 Mn1 89.35(8) . 2_665
O1 Mn1 Mn1 123.23(8) . 2_665
O4 Mn1 Mn1 40.31(7) 2_665 2_665
O3 Mn1 Mn1 36.59(8) . 4_565
O2 Mn1 Mn1 129.23(8) . 4_565
N1 Mn1 Mn1 141.06(10) . 4_565
O4 Mn1 Mn1 51.40(9) . 4_565
O1 Mn1 Mn1 75.70(7) . 4_565
O4 Mn1 Mn1 82.39(6) 2_665 4_565
Mn1 Mn1 Mn1 60.000(11) 2_665 4_565
C016 O4 Mn1 127.2(2) . .
C016 O4 Ni1 111.5(3) . .
Mn1 O4 Ni1 105.74(10) . .
C016 O4 Mn1 124.9(2) . 4_565
Mn1 O4 Mn1 88.29(13) . 4_565
Ni1 O4 Mn1 92.46(9) . 4_565
Mn1 O3 Mn1 106.81(15) 4_565 2_665
Mn1 O3 Mn1 106.81(15) 4_565 .
Mn1 O3 Mn1 106.81(15) 2_665 .
C017 O2 Mn1 127.8(2) . .
N2 N1 Mn1 122.5(3) . .
N3 N2 N1 176.2(4) . .
C011 N4 C010 117.9(3) . .
C011 N4 Ni1 128.0(3) . .
C010 N4 Ni1 113.9(2) . .
C017 O1 Mn1 125.9(2) 4_565 .
C014 C009 C010 118.5(4) . .
N4 C010 C009 122.1(3) . .
N4 C010 C016 116.2(3) . .
C009 C010 C016 121.6(3) . .
N4 C011 C019 122.3(4) . .
C015 C012 C021 120.3(4) . .
C015 C012 C017 119.8(4) . .
C021 C012 C017 119.9(4) . .
C018 C013 C021 121.3(4) . .
C019 C014 C009 120.0(4) . .
C012 C015 C020 121.2(4) . .
O4 C016 C010 109.6(3) . .
O1 C017 O2 127.9(4) 2_665 .
O1 C017 C012 118.0(3) 2_665 .
O2 C017 C012 114.0(3) . .
C013 C018 C020 120.5(4) . .
C014 C019 C011 119.2(4) . .
C018 C020 C015 117.9(4) . .
C012 C021 C013 118.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N3 N2 1.148(5) .
Ni1 N4 2.033(3) .
Ni1 N4 2.033(3) 4_565
Ni1 N4 2.033(3) 2_665
Ni1 O4 2.058(3) .
Ni1 O4 2.058(3) 4_565
Ni1 O4 2.058(3) 2_665
Mn1 O3 1.8919(19) .
Mn1 O2 1.936(3) .
Mn1 N1 1.946(3) .
Mn1 O4 1.966(3) .
Mn1 O1 2.176(3) .
Mn1 O4 2.375(3) 2_665
Mn1 Mn1 3.0380(11) 2_665
Mn1 Mn1 3.0380(10) 4_565
O4 C016 1.403(5) .
O4 Mn1 2.375(3) 4_565
O3 Mn1 1.8919(19) 4_565
O3 Mn1 1.8919(19) 2_665
O2 C017 1.278(5) .
N1 N2 1.207(5) .
N4 C011 1.342(5) .
N4 C010 1.349(4) .
O1 C017 1.233(5) 4_565
C009 C014 1.371(6) .
C009 C010 1.394(5) .
C010 C016 1.497(6) .
C011 C019 1.388(6) .
C012 C015 1.369(6) .
C012 C021 1.386(6) .
C012 C017 1.519(5) .
C013 C018 1.367(7) .
C013 C021 1.393(6) .
C014 C019 1.358(6) .
C015 C020 1.410(7) .
C017 O1 1.233(5) 2_665
C018 C020 1.391(6) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.103 332.4 111.9
2 0.000 0.000 0.437 14.3 -0.8
3 0.000 0.000 0.603 332.4 112.4
4 0.000 0.000 0.937 14.3 -0.8
5 0.333 0.667 0.270 334.5 112.3
6 0.333 0.667 0.770 334.5 111.9
7 0.333 0.667 0.103 15.1 -0.8
8 0.333 0.667 0.603 15.1 -0.8
9 0.667 0.333 0.436 332.9 112.0
10 0.667 0.333 0.936 332.9 112.5
11 0.666 0.333 0.270 14.9 -0.8
12 0.666 0.333 0.770 14.9 -0.8
