# Supplementary Information (SI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ED_Mn2-NITImMe23_P212121_1_13_A_XDS_I_F_Fc_2021_11_17
_database_code_depnum_ccdc_archive 'CCDC 2330279'
loop_
_audit_author_name
_audit_author_address
'Dominique Housset'
;Institut de Biologie Structurale, Grenoble
France
;
_audit_update_record             
;
2024-02-01 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_ATOM007_ED_Mn2-NITImMe23_P212121_1_13_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: All atoms were refined with an isotropic displacement parameter.
;
_vrf_GEOM006_ED_Mn2-NITImMe23_P212121_1_13_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: REFMAC5 log file is unfortunately not providing it. A visualization of the model allows to easily identify it for each angle.
;
_vrf_THETM01_ED_Mn2-NITImMe23_P212121_1_13_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The highest resolution of the diffraction data is 1.18 \%A. sine(theta_max)/wavelength is thus less than 0.55.
;
_vrf_PLAT201_ED_Mn2-NITImMe23_P212121_1_13_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         56 Report
RESPONSE: All atoms were refined with an isotropic displacement parameter. Refinement tests with anisotropic displacement parameters did not improve significantly the free R factor.
;
_vrf_RINTA01_ED_Mn2-NITImMe23_P212121_1_13_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: High value of Rint is common in electron diffraction data. Such a high Rint value may originate from multiple diffraction and/or errors introduced rotation stage and microscope optics.
;

_audit_creation_method           'Refmac5 5.8.0267'
_audit_creation_date             2023-10-03
_chemical_name_systematic        
Tris(2-(4,5-dimethylimidazol-2-yl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazol-3-oxide-1-oxyl)dimanganese(II).perchlorate
_chemical_name_common            '[Mn2(NITImMe2)3].ClO4'
_chemical_melting_point          ?
_chemical_formula_moiety         '(Mn2 C36 H54 N12 O6), (Cl O4)'
_chemical_formula_sum            'C36 H54 Cl Mn2 N12 O10'
_chemical_formula_weight         960.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
H H 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
N N 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
O O 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
CL CL 0.0000 0.0000
'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
MN MN 0.0000 0.0000
'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'

_space_group_crystal_system      orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_IT_number           19

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   11.609
_cell_length_b                   18.371
_cell_length_c                   22.461
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_volume                     4790.23
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3780
_cell_measurement_theta_min      0.039111
_cell_measurement_theta_max      0.634703

_exptl_crystal_description       nanocrystal
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    ?
_exptl_crystal_F_000             ?
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.0250793

_diffrn_source                   'Field emission gun (FEG) electron microscope'
_diffrn_measurement_device       'transmission electron microscope'
_diffrn_measurement_device_type  'TECNAI F20 (200 keV)'
_diffrn_detector                 'hybrid pixel direct electron detector'
_diffrn_detector_type            'ASI MEDIPIX 3RX'
_diffrn_detector_dtime           0.0
_diffrn_radiation_type           electron
_exptl_special_details           
'data collected by continuous rotation 3D electron diffraction with low electron dose'
_diffrn_radiation_probe          electron

_diffrn_reflns_number            14640
_diffrn_reflns_av_unetI/netI     0.1192
_diffrn_reflns_av_R_equivalents  0.161
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_resolution_max    0.88353
_diffrn_reflns_theta_min         0.039111
_diffrn_reflns_theta_max         0.634703
_diffrn_reflns_theta_full        ?
_diffrn_measured_fraction_theta_max 0.719
_diffrn_measured_fraction_theta_full ?
_diffrn_reflns_Laue_measured_fraction_max ?
_diffrn_reflns_Laue_measured_fraction_full ?
_diffrn_reflns_point_group_measured_fraction_max ?
_diffrn_reflns_point_group_measured_fraction_full ?
_reflns_number_total             1433
_reflns_number_gt                ?
_reflns_threshold_expression     ?
_reflns_Friedel_coverage         ?
_reflns_Friedel_fraction_max     ?
_reflns_Friedel_fraction_full    ?
_reflns_d_resolution_high        18.371
_reflns_d_resolution_low         1.132

loop_
_reflns_shell_d_res_high
_reflns_shell_d_res_low
_reflns_shell_number_measured_all
_reflns_shell_number_unique_all
_reflns_shell_number_possible
_reflns_shell_Rmerge_I_all
_reflns_shell_meanI_over_sigI_all
18.37 4.23 230 32 48 0.048 23.86
4.23 2.99 445 50 78 0.077 22.91
2.99 2.45 644 71 96 0.096 20.05
2.45 2.12 810 81 115 0.120 17.31
2.12 1.89 875 85 122 0.125 16.54
1.89 1.73 1020 100 134 0.207 10.24
1.73 1.6 1103 104 145 0.224 9.94
1.6 1.5 1217 113 157 0.254 8.36
1.5 1.41 1156 114 156 0.265 7.82
1.41 1.34 1436 130 180 0.432 5.05
1.34 1.28 1320 126 174 0.775 3.1
1.28 1.22 1503 142 193 0.787 2.93
1.22 1.17 1568 140 195 1.028 2.11
1.17 1.13 1313 145 200 1.075 1.61
18.37 1.13 14640 1433 1993 0.161 8.39

_reflns_special_details          
;
 Electron diffraction, continuous rotation, flat field and geometrical correction of diffraction images with ImageJ
 2 data sets were indexed and processed with XDS and merged in the
P2(1)2(1)2(1) space group with XSCALE. Merging statistics provided by XSCALE are provided below:
 SUBSET OF INTENSITY DATA WITH SIGNAL/NOISE >= -3.0 AS FUNCTION OF RESOLUTION
 RESOLUTION     NUMBER OF REFLECTIONS    COMPLETENESS R-FACTOR  R-FACTOR COMPARED I/SIGMA   R-meas  CC(1/2)  Anomal  SigAno   Nano
   LIMIT     OBSERVED  UNIQUE  POSSIBLE     OF DATA   observed  expected                                      Corr

     4.23         230      32        48       66.7%       4.8%      7.2%      229   23.86      5.2%    99.9*    22    0.915      13
     2.99         445      50        78       64.1%       7.7%      7.7%      445   22.91      8.2%    99.9*     1    0.864      31
     2.45         644      71        96       74.0%       9.6%      9.1%      643   20.05     10.2%    99.5*     1    0.824      45
     2.12         810      81       115       70.4%      12.0%     11.0%      809   17.31     12.6%    99.5*    -6    0.858      56
     1.89         875      85       122       69.7%      12.5%     11.7%      874   16.54     13.1%    99.4*    15    1.003      62
     1.73        1020     100       134       74.6%      20.7%     20.1%     1016   10.24     21.8%    96.7*   -11    0.727      71
     1.60        1103     104       145       71.7%      22.4%     22.6%     1102    9.94     23.5%    97.8*     4    0.840      75
     1.50        1217     113       157       72.0%      25.4%     25.4%     1216    8.36     26.7%    98.0*    -4    0.810      90
     1.41        1156     114       156       73.1%      26.5%     26.2%     1154    7.82     27.9%    98.4*     6    0.839      85
     1.34        1436     130       180       72.2%      43.2%     45.3%     1434    5.05     45.3%    93.8*    -9    0.707     102
     1.28        1320     126       174       72.4%      77.5%     79.6%     1317    3.10     81.4%    77.3*     1    0.742      95
     1.22        1503     142       193       73.6%      78.7%     87.3%     1501    2.93     82.5%    79.0*   -10    0.756     115
     1.17        1568     140       195       71.8%     102.8%    135.3%     1566    2.11    107.5%    69.1*    -3    0.733     112
     1.13        1313     145       200       72.5%     107.5%    219.2%     1305    1.61    113.4%    71.5*    -1    0.646      93
    total       14640    1433      1993       71.9%      16.1%     18.0%    14611    8.39     17.0%    99.9*    -1    0.781    1045
;

_computing_data_collection       'DEXTER (ASI)'
_computing_cell_refinement       'XDS (IDXREF, CORRECT, CELLPARM)'
_computing_data_reduction        XSCALE
_computing_structure_solution    'PHASER version 2.8.3 in CCP4 suite'
_computing_structure_refinement  
'REFMAC5 version 5.8.0267 in CCP4 7.1.018 suite'
_computing_molecular_graphics    COOT
_computing_publication_material  ?
_refine_special_details          
;
 Refinement was performed with REFMAC5 in CCP4 suite. Electron scattering length used dufring the refinement were calculated by the
Mott-Bethe formula using the "source electron mb" command in REFMAC5. Stereochemical restraints have been applied. A library of restraints
has has been created for NITImME2 (PR7) and is provided below:
global_
_lib_name         mon_lib
_lib_version      5.52
_lib_update       17/08/20
# ------------------------------------------------
#
# ---   LIST OF MONOMERS ---
#
data_comp_list
loop_
_chem_comp.id
_chem_comp.three_letter_code
_chem_comp.name
_chem_comp.group
_chem_comp.number_atoms_all
_chem_comp.number_atoms_nh
_chem_comp.desc_level
PR7      PR7 'MOF Radical                         ' non-polymer        32  16 .
# ------------------------------------------------------
# ------------------------------------------------------
#
# --- DESCRIPTION OF MONOMERS ---
#
data_comp_PR7
#
loop_
_chem_comp_atom.comp_id
_chem_comp_atom.atom_id
_chem_comp_atom.type_symbol
_chem_comp_atom.type_energy
_chem_comp_atom.partial_charge
_chem_comp_atom.x
_chem_comp_atom.y
_chem_comp_atom.z
 PR7           O2     O    O         0.000      0.000    0.000    0.000
 PR7           N2     N    N         0.000      0.984    0.984    0.000
 PR7           C3     C    CT        0.000      2.390    0.608   -0.000
 PR7           C6     C    CH3       0.000      2.748   -0.222    1.227
 PR7           H6C    H    H         0.000      2.553    0.341    2.103
 PR7           H6B    H    H         0.000      2.165   -1.106    1.238
 PR7           H6A    H    H         0.000      3.776   -0.477    1.193
 PR7           C7     C    CH3       0.000      2.748   -0.222   -1.227
 PR7           H7C    H    H         0.000      2.165   -1.106   -1.238
 PR7           H7B    H    H         0.000      2.553    0.341   -2.103
 PR7           H7A    H    H         0.000      3.776   -0.477   -1.193
 PR7           C2     C    CT        0.000      3.298    1.831    0.000
 PR7           C5     C    CH3       0.000      3.053    2.694   -1.232
 PR7           H5C    H    H         0.000      3.248    2.126   -2.105
 PR7           H5B    H    H         0.000      2.045    3.019   -1.240
 PR7           H5A    H    H         0.000      3.695    3.535   -1.208
 PR7           C4     C    CH3       0.000      3.053    2.694    1.232
 PR7           H4C    H    H         0.000      2.045    3.019    1.240
 PR7           H4B    H    H         0.000      3.248    2.126    2.105
 PR7           H4A    H    H         0.000      3.695    3.535    1.208
 PR7           N1     N    N         0.000      4.704    1.455   -0.000
 PR7           O1     O    O         0.000      5.688    2.439   -0.000
 PR7           C1     C    C         0.000      0.640    2.269    0.000
 PR7           C8     C    CR5       0.000      1.694    3.323   -0.000
 PR7           N4     N    NRD5      0.000      1.482    4.656   -0.000
 PR7           C10    C    CR5       0.000      0.149    4.867    0.000
 PR7           C9     C    CR5       0.000     -0.477    3.638    0.000
 PR7           N3     N    NRD5      0.000     -1.811    3.849    0.000
 PR7           C11    C    CH3       0.000     -3.288    4.507    0.677
 PR7           H11C   H    H         0.000     -3.964    4.524    1.501
 PR7           H11B   H    H         0.000     -2.481    5.170    0.888
 PR7           H11A   H    H         0.000     -3.800    4.863   -0.187
 PR7           C12    C    CH3       0.000     -0.955    2.750   -1.754
 PR7           H12C   H    H         0.000     -0.252    2.063   -1.351
 PR7           H12B   H    H         0.000     -1.571    2.243   -2.455
 PR7           H12A   H    H         0.000     -0.430    3.527   -2.254
loop_
_chem_comp_tree.comp_id
_chem_comp_tree.atom_id
_chem_comp_tree.atom_back
_chem_comp_tree.atom_forward
_chem_comp_tree.connect_type
 PR7      O1     n/a    N1     START
 PR7      N1     O1     C1     .
 PR7      C2     N1     C3     .
 PR7      C5     C2     H51    .
 PR7      H5C    C5     .      .
 PR7      H5B    C5     .      .
 PR7      H5A    C5     .      .
 PR7      C4     C2     H41    .
 PR7      H4C    C4     .      .
 PR7      H4B    C4     .      .
 PR7      H4A    C4     .      .
 PR7      C3     C2     C6     .
 PR7      C7     C3     H71    .
 PR7      H7C    C7     .      .
 PR7      H7B    C7     .      .
 PR7      H7A    C7     .      .
 PR7      C6     C3     H61    .
 PR7      H6C    C6     .      .
 PR7      H6B    C6     .      .
 PR7      H6A    C6     .      .
 PR7      C1     N1     C8     .
 PR7      N2     C1     O2     .
 PR7      O2     N2     .      .
 PR7      C8     C1     N3     .
 PR7      N3     C8     C9     .
 PR7      C9     N3     C10    .
 PR7      C11    C9     H11A   .
 PR7      H11C   C11    .      .
 PR7      H11B   C11    .      .
 PR7      H11A   C11    .      .
 PR7      C10    C9     C12    .
 PR7      N4     C10    .      .
 PR7      C12    C10    H12A   .
 PR7      H12C   C12    .      .
 PR7      H12B   C12    .      .
 PR7      H12A   C12    .      END
 PR7      N2     C3     .    ADD
 PR7      C8     N4     .    ADD
loop_
_chem_comp_bond.comp_id
_chem_comp_bond.atom_id_1
_chem_comp_bond.atom_id_2
_chem_comp_bond.type
_chem_comp_bond.value_dist
_chem_comp_bond.value_dist_esd
 PR7      O1     N1        single      1.344    0.020
 PR7      N2     O2        single      1.344    0.020
 PR7      N1     C1        single      1.333    0.020
 PR7      C1     N2        single      1.333    0.020
 PR7      N1     C2        single      1.457    0.020
 PR7      C3     N2        single      1.457    0.020
 PR7      N3     C8        aromatic    1.350    0.020
 PR7      N4     C8        aromatic    1.350    0.020
 PR7      N3     C9        aromatic    1.350    0.020
 PR7      C10    N4        aromatic    1.350    0.020
 PR7      C8     C1        aromatic    1.495    0.020
 PR7      C2     C3        single      1.589    0.020
 PR7      C4     C2        single      1.532    0.020
 PR7      C5     C2        single      1.532    0.020
 PR7      C6     C3        single      1.532    0.020
 PR7      C7     C3        single      1.532    0.020
 PR7      H4A    C4        single      1.059    0.020
 PR7      H4B    C4        single      1.059    0.020
 PR7      H4C    C4        single      1.059    0.020
 PR7      H5A    C5        single      1.059    0.020
 PR7      H5B    C5        single      1.059    0.020
 PR7      H5C    C5        single      1.059    0.020
 PR7      H6A    C6        single      1.059    0.020
 PR7      H6B    C6        single      1.059    0.020
 PR7      H6C    C6        single      1.059    0.020
 PR7      H7A    C7        single      1.059    0.020
 PR7      H7B    C7        single      1.059    0.020
 PR7      H7C    C7        single      1.059    0.020
 PR7      C9     C10       aromatic    1.380    0.020
 PR7      C11    C9        single      1.506    0.020
 PR7      C12    C10       single      1.506    0.020
 PR7      H11A   C11       single      1.059    0.020
 PR7      H11B   C11       single      1.059    0.020
 PR7      H11C   C11       single      1.059    0.020
 PR7      H12A   C12       single      1.059    0.020
 PR7      H12B   C12       single      1.059    0.020
 PR7      H12C   C12       single      1.059    0.020
loop_
_chem_comp_angle.comp_id
_chem_comp_angle.atom_id_1
_chem_comp_angle.atom_id_2
_chem_comp_angle.atom_id_3
_chem_comp_angle.value_angle
_chem_comp_angle.value_angle_esd
 PR7      O2     N2     C3      122.550    3.000
 PR7      C2     N1     O1      122.550    3.000
 PR7      O2     N2     C1      126.710    3.000
 PR7      O1     N1     C1      126.710    3.000
 PR7      C3     N2     C1      110.740    3.000
 PR7      C2     N1     C1      110.740    3.000
 PR7      N2     C3     C6      106.580    3.000
 PR7      N2     C3     C7      106.580    3.000
 PR7      C5     C2     N1      106.580    3.000
 PR7      C4     C2     N1      106.580    3.000
 PR7      N2     C3     C2      102.670    3.000
 PR7      C3     C2     N1      102.670    3.000
 PR7      C6     C3     C7      106.850    3.000
 PR7      C5     C2     C4      106.850    3.000
 PR7      C6     C3     C2      116.600    3.000
 PR7      C7     C3     C2      116.600    3.000
 PR7      C3     C2     C5      116.600    3.000
 PR7      C3     C2     C4      116.600    3.000
 PR7      C3     C6     H6C     109.470    3.000
 PR7      C3     C6     H6B     109.470    3.000
 PR7      C3     C6     H6A     109.470    3.000
 PR7      H6C    C6     H6B     109.470    3.000
 PR7      H6C    C6     H6A     109.470    3.000
 PR7      H6B    C6     H6A     109.470    3.000
 PR7      C3     C7     H7C     109.470    3.000
 PR7      C3     C7     H7B     109.470    3.000
 PR7      C3     C7     H7A     109.470    3.000
 PR7      H7C    C7     H7B     109.470    3.000
 PR7      H7C    C7     H7A     109.470    3.000
 PR7      H7B    C7     H7A     109.470    3.000
 PR7      C2     C5     H5C     109.470    3.000
 PR7      C2     C5     H5B     109.470    3.000
 PR7      C2     C5     H5A     109.470    3.000
 PR7      H5C    C5     H5B     109.470    3.000
 PR7      H5C    C5     H5A     109.470    3.000
 PR7      H5B    C5     H5A     109.470    3.000
 PR7      C2     C4     H4C     109.470    3.000
 PR7      C2     C4     H4B     109.470    3.000
 PR7      C2     C4     H4A     109.470    3.000
 PR7      H4C    C4     H4B     109.470    3.000
 PR7      H4C    C4     H4A     109.470    3.000
 PR7      H4B    C4     H4A     109.470    3.000
 PR7      N2     C1     C8      123.240    3.000
 PR7      N1     C1     C8      123.240    3.000
 PR7      N2     C1     N1      113.520    3.000
 PR7      C1     C8     N4      126.180    3.000
 PR7      C1     C8     N3      126.180    3.000
 PR7      N4     C8     N3      107.640    3.000
 PR7      C8     N4     C10     108.900    3.000
 PR7      C9     N3     C8      108.900    3.000
 PR7      N4     C10    C9      107.270    3.000
 PR7      C10    C9     N3      107.270    3.000
 PR7      N3     C9     C11     126.180    3.000
 PR7      N4     C10    C12     126.180    3.000
 PR7      C11    C9     C10     126.550    3.000
 PR7      C9     C10    C12     126.550    3.000
 PR7      C9     C11    H11C    109.470    3.000
 PR7      C9     C11    H11B    109.470    3.000
 PR7      C9     C11    H11A    109.470    3.000
 PR7      H11C   C11    H11B    109.470    3.000
 PR7      H11C   C11    H11A    109.470    3.000
 PR7      H11B   C11    H11A    109.470    3.000
 PR7      C10    C12    H12C    109.470    3.000
 PR7      C10    C12    H12B    109.470    3.000
 PR7      C10    C12    H12A    109.470    3.000
 PR7      H12C   C12    H12B    109.470    3.000
 PR7      H12C   C12    H12A    109.470    3.000
 PR7      H12B   C12    H12A    109.470    3.000
loop_
_chem_comp_plane_atom.comp_id
_chem_comp_plane_atom.plane_id
_chem_comp_plane_atom.atom_id
_chem_comp_plane_atom.dist_esd
 PR7      plan-1            N3        0.020
 PR7      plan-1            C8        0.020
 PR7      plan-1            C9        0.020
 PR7      plan-1            N4        0.020
 PR7      plan-1            C10       0.020
 PR7      plan-1            C1        0.020
 PR7      plan-1            C11       0.020
 PR7      plan-1            C12       0.020
 PR7      plan-2            N1        0.020
 PR7      plan-2            O1        0.020
 PR7      plan-2            C1        0.020
 PR7      plan-2            C2        0.020
 PR7      plan-2            C8        0.020
 PR7      plan-2            N2        0.020
 PR7      plan-2            O2        0.020
 PR7      plan-2            C3        0.020
# ------------------------------------------------------

The refinement uses a loglikelihood residual derived from Rice distribution for centric and acentric cases of Fs.
Fxray = SUM(LLKcentric_hkl) + SUM(LLKacentric_hkl)

The statistics provided by REFMAC for the final structure refined on all reflections is presented below:
OMPND    ---
REMARK   3
REMARK   3 REFINEMENT.
REMARK   3   PROGRAM     : REFMAC 5.8.0267   
REMARK   3   AUTHORS     : MURSHUDOV,SKUBAK,LEBEDEV,PANNU,
REMARK   3                 STEINER,NICHOLLS,WINN,LONG,VAGIN
REMARK   3
REMARK   3    REFINEMENT TARGET : MAXIMUM LIKELIHOOD
REMARK   3
REMARK   3  DATA USED IN REFINEMENT.
REMARK   3   RESOLUTION RANGE HIGH (ANGSTROMS) :   1.13
REMARK   3   RESOLUTION RANGE LOW  (ANGSTROMS) :  10.32
REMARK   3   DATA CUTOFF            (SIGMA(F)) : NONE
REMARK   3   COMPLETENESS FOR RANGE        (%) :  71.92
REMARK   3   NUMBER OF REFLECTIONS             :    1432
REMARK   3
REMARK   3  FIT TO DATA USED IN REFINEMENT.
REMARK   3   CROSS-VALIDATION METHOD          : NULL
REMARK   3   FREE R VALUE TEST SET SELECTION  : NULL
REMARK   3   R VALUE     (WORKING + TEST SET) : 0.20990
REMARK   3   R VALUE            (WORKING SET) :  0.20990
REMARK   3   FREE R VALUE                     : NULL
REMARK   3   FREE R VALUE TEST SET SIZE   (%) : NULL
REMARK   3   FREE R VALUE TEST SET COUNT      : NULL
REMARK   3
REMARK   3  FIT IN THE HIGHEST RESOLUTION BIN.
REMARK   3   TOTAL NUMBER OF BINS USED           :      20
REMARK   3   BIN RESOLUTION RANGE HIGH           :    1.132
REMARK   3   BIN RESOLUTION RANGE LOW            :    1.161
REMARK   3   REFLECTION IN BIN     (WORKING SET) :      112
REMARK   3   BIN COMPLETENESS (WORKING+TEST) (%) :    71.79
REMARK   3   BIN R VALUE           (WORKING SET) :    0.328
REMARK   3   BIN FREE R VALUE SET COUNT          :        0
REMARK   3   BIN FREE R VALUE                    :    0.000
REMARK   3
REMARK   3  NUMBER OF NON-HYDROGEN ATOMS USED IN REFINEMENT.
REMARK   3   ALL ATOMS                :       61
REMARK   3
REMARK   3  B VALUES.
REMARK   3   FROM WILSON PLOT           (A**2) : NULL
REMARK   3   MEAN B VALUE      (OVERALL, A**2) :  10.843
REMARK   3   OVERALL ANISOTROPIC B VALUE.
REMARK   3    B11 (A**2) :    -1.00
REMARK   3    B22 (A**2) :    -0.43
REMARK   3    B33 (A**2) :     1.42
REMARK   3    B12 (A**2) :     0.00
REMARK   3    B13 (A**2) :     0.00
REMARK   3    B23 (A**2) :     0.00
REMARK   3
REMARK   3  ESTIMATED OVERALL COORDINATE ERROR.
REMARK   3   ESU BASED ON R VALUE                            (A):   0.060
REMARK   3   ESU BASED ON FREE R VALUE                       (A): NULL
REMARK   3   ESU BASED ON MAXIMUM LIKELIHOOD                 (A):   0.040
REMARK   3   ESU FOR B VALUES BASED ON MAXIMUM LIKELIHOOD (A**2):   0.982
REMARK   3
REMARK   3 CORRELATION COEFFICIENTS.
REMARK   3   CORRELATION COEFFICIENT FO-FC      :   0.963
REMARK   3   CORRELATION COEFFICIENT FO-FC FREE : NULL
REMARK   3
REMARK   3  RMS DEVIATIONS FROM IDEAL VALUES        COUNT    RMS    WEIGHT
REMARK   3   BOND LENGTHS REFINED ATOMS        (A):    61 ; 0.018 ; 0.020
REMARK   3   BOND LENGTHS OTHERS               (A):    54 ; 0.000 ; 0.020
REMARK   3   BOND ANGLES REFINED ATOMS   (DEGREES):   102 ; 3.367 ; 3.000
REMARK   3   BOND ANGLES OTHERS          (DEGREES):   108 ; 0.505 ; 3.000
REMARK   3   CHIRAL-CENTER RESTRAINTS       (A**3):     1 ; 0.102 ; 0.200
REMARK   3   GENERAL PLANES REFINED ATOMS      (A):    48 ; 0.032 ; 0.020
REMARK   3
REMARK   3  ISOTROPIC THERMAL FACTOR RESTRAINTS.     COUNT   RMS    WEIGHT
REMARK   3   SIDE-CHAIN BOND REFINED ATOMS  (A**2):    61 ; 1.704 ; 1.026
REMARK   3   SIDE-CHAIN BOND OTHER ATOMS  (A**2)  :    58 ; 0.959 ; 0.962
REMARK   3   SIDE-CHAIN ANGLE OTHER ATOMS (A**2)  :    97 ; 1.601 ; 1.475
REMARK   3   LONG RANGE B REFINED ATOMS (A**2)    :    87 ; 2.425 ;10.741
REMARK   3   LONG RANGE B OTHER ATOMS (A**2)      :    88 ; 2.858 ;10.829
REMARK   3
REMARK   3  NCS RESTRAINTS STATISTICS
REMARK   3   NUMBER OF NCS GROUPS : NULL
REMARK   3
REMARK   3  TWIN DETAILS
REMARK   3   NUMBER OF TWIN DOMAINS  : NULL
REMARK   3
REMARK   3
REMARK   3  TLS DETAILS
REMARK   3   NUMBER OF TLS GROUPS  : NULL
REMARK   3
REMARK   3
REMARK   3  BULK SOLVENT MODELLING.
REMARK   3   METHOD USED :  MASK
REMARK   3   PARAMETERS FOR MASK CALCULATION
REMARK   3   VDW PROBE RADIUS   :   1.20
REMARK   3   ION PROBE RADIUS   :   0.80
REMARK   3   SHRINKAGE RADIUS   :   0.80
REMARK   3
REMARK   3  OTHER REFINEMENT REMARKS:
REMARK   3  HYDROGENS HAVE BEEN ADDED IN THE RIDING POSITIONS
REMARK   3  U VALUES      : REFINED INDIVIDUALLY
REMARK   3

;
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_parameters     460
_refine_ls_number_restraints     332
_refine_ls_R_factor_gt           ?
_refine_ls_wR_factor_ref         ?
_refine_ls_wR_factor_gt          ?
_refine_ls_goodness_of_fit_ref   ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

loop_
_refine_ls_d_res_high
_refine_ls_d_res_low
_refine_ls_number_reflns
_refine_ls_R_factor_all
14.22 4.783 25 0.193
4.783 3.482 31 0.134
3.482 2.872 38 0.189
2.872 2.5 49 0.203
2.5 2.243 55 0.242
2.243 2.052 55 0.187
2.052 1.902 63 0.195
1.902 1.781 70 0.221
1.781 1.681 64 0.163
1.681 1.596 80 0.165
1.596 1.522 77 0.162
1.522 1.458 74 0.175
1.458 1.402 89 0.223
1.402 1.351 82 0.216
1.351 1.306 92 0.306
1.306 1.265 94 0.249
1.265 1.227 95 0.268
1.227 1.193 97 0.353
1.193 1.161 90 0.347
1.161 1.132 112 0.328
14.22 1.132 1432 0.210


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
MN1 Mn -0.200448 0.226444 -0.234406 1 0.086 Uiso D U
MN2 Mn -0.299854 -0.119264 -0.259205 1 0.0955 Uiso D U
C1A C -0.169007 0.045996 -0.295134 1 0.11627 Uiso D U
C10A C -0.389956 0.023243 -0.180936 1 0.1112 Uiso D U
C11A C -0.404944 0.14463 -0.126842 1 0.11424 Uiso D U
C12A C -0.4798 -0.018507 -0.146966 1 0.11753 Uiso D U
C2A C -0.008356 0.078602 -0.349361 1 0.144 Uiso D U
C3A C -0.069257 0.008927 -0.37781 1 0.1416 Uiso D U
C4A C 0.019295 0.147733 -0.384355 1 0.15262 Uiso D U
C5A C 0.099233 0.059387 -0.312942 1 0.16237 Uiso D U
C6A C 0.003446 -0.05906 -0.385735 1 0.1516 Uiso D U
C7A C -0.12766 0.025094 -0.438226 1 0.15072 Uiso D U
C8A C -0.255405 0.051385 -0.246205 1 0.10335 Uiso D U
C9A C -0.355758 0.094551 -0.172833 1 0.10525 Uiso D U
H11AA H -0.482643 0.167383 -0.143092 1 0.11145 Uiso D U
H11BA H -0.421742 0.115127 -0.087262 1 0.11145 Uiso D U
H11CA H -0.345336 0.186762 -0.117849 1 0.11133 Uiso D U
H12AA H -0.508915 -0.062109 -0.173901 1 0.11563 Uiso D U
H12BA H -0.441985 -0.038648 -0.107342 1 0.11563 Uiso D U
H12CA H -0.549143 0.016874 -0.136815 1 0.11563 Uiso D U
H4AA H 0.10087 0.168526 -0.371934 1 0.14996 Uiso D U
H4BA H 0.019898 0.135866 -0.430479 1 0.14996 Uiso D U
H4CA H -0.044362 0.18785 -0.376208 1 0.14983 Uiso D U
H5AA H 0.165303 0.041315 -0.341881 1 0.15641 Uiso D U
H5BA H 0.128866 0.105601 -0.289301 1 0.15629 Uiso D U
H5CA H 0.07899 0.017473 -0.282312 1 0.15629 Uiso D U
H6AA H 0.008356 -0.087203 -0.344642 1 0.14844 Uiso D U
H6BA H -0.034714 -0.093136 -0.418192 1 0.14844 Uiso D U
H6CA H 0.087604 -0.044581 -0.399626 1 0.14844 Uiso D U
H7AA H -0.064347 0.024658 -0.472152 1 0.1478 Uiso D U
H7BA H -0.19037 -0.015078 -0.447887 1 0.1478 Uiso D U
H7CA H -0.166853 0.077078 -0.436312 1 0.1478 Uiso D U
N1A N -0.088035 0.097218 -0.301901 1 0.11728 Uiso D U
N2A N -0.164872 -0.006042 -0.336672 1 0.12133 Uiso D U
N3A N -0.271427 0.111262 -0.212635 1 0.10031 Uiso D U
N4A N -0.326471 -0.001579 -0.226927 1 0.10753 Uiso D U
O1A O -0.064863 0.153394 -0.269 1 0.11044 Uiso D U
O2A O -0.233181 -0.062544 -0.343484 1 0.12956 Uiso D U
C1B C 0.076234 0.262261 -0.181069 1 0.1112 Uiso D U
C10B C 0.053665 0.381634 -0.310894 1 0.09777 Uiso D U
C11B C -0.163408 0.37864 -0.338676 1 0.1074 Uiso D U
C12B C 0.103799 0.431713 -0.358399 1 0.11373 Uiso D U
C2B C 0.065983 0.18834 -0.09866 1 0.14046 Uiso D U
C3B C 0.195366 0.199336 -0.115801 1 0.14286 Uiso D U
C4B C 0.038591 0.235208 -0.043676 1 0.15059 Uiso D U
C5B C 0.017056 0.114093 -0.086639 1 0.15806 Uiso D U
C6B C 0.246877 0.130967 -0.14376 1 0.15717 Uiso D U
C7B C 0.285296 0.220511 -0.069632 1 0.15046 Uiso D U
C8B C 0.044965 0.307169 -0.233249 1 0.09929 Uiso D U
C9B C -0.059523 0.357792 -0.302747 1 0.10081 Uiso D U
H11AB H -0.168404 0.436122 -0.341436 1 0.10537 Uiso D U
H11BB H -0.15643 0.355996 -0.381862 1 0.10537 Uiso D U
H11CB H -0.238522 0.358337 -0.317662 1 0.10537 Uiso D U
H12AB H 0.105694 0.48582 -0.342104 1 0.10867 Uiso D U
H12BB H 0.188474 0.414675 -0.368906 1 0.10867 Uiso D U
H12CB H 0.05177 0.429372 -0.397088 1 0.10867 Uiso D U
H4AB H -0.050995 0.233956 -0.034905 1 0.14742 Uiso D U
H4BB H 0.083642 0.214632 -0.006278 1 0.14742 Uiso D U
H4CB H 0.064347 0.289641 -0.051734 1 0.1473 Uiso D U
H5AB H 0.072788 0.085787 -0.057388 1 0.15236 Uiso D U
H5BB H -0.065553 0.118665 -0.06705 1 0.15236 Uiso D U
H5CB H 0.010337 0.085243 -0.127287 1 0.15236 Uiso D U
H6AB H 0.32449 0.144249 -0.166021 1 0.15249 Uiso D U
H6BB H 0.263933 0.092102 -0.110057 1 0.15262 Uiso D U
H6CB H 0.18813 0.108758 -0.174925 1 0.15262 Uiso D U
H7AB H 0.368766 0.218769 -0.088643 1 0.14806 Uiso D U
H7BB H 0.268843 0.274073 -0.05445 1 0.14806 Uiso D U
H7CB H 0.280903 0.184421 -0.032946 1 0.14806 Uiso D U
N1B N 0.003704 0.225627 -0.146164 1 0.11652 Uiso D U
N2B N 0.186321 0.252626 -0.165353 1 0.12159 Uiso D U
N3B N -0.061073 0.312667 -0.25502 1 0.09448 Uiso D U
N4B N 0.115255 0.351913 -0.26615 1 0.0936 Uiso D U
O1B O -0.107331 0.223287 -0.147678 1 0.11728 Uiso D U
O2B O 0.277716 0.279244 -0.192556 1 0.13134 Uiso D U
C1C C -0.465759 0.275053 -0.302346 1 0.11361 Uiso D U
C10C C -0.464209 0.373796 -0.163617 1 0.09613 Uiso D U
C11C C -0.267982 0.345599 -0.110503 1 0.11411 Uiso D U
C12C C -0.51908 0.421915 -0.118695 1 0.10537 Uiso D U
C2C C -0.446033 0.203636 -0.385335 1 0.14261 Uiso D U
C3C C -0.570592 0.231397 -0.377232 1 0.15262 Uiso D U
C4C C -0.387027 0.245223 -0.435867 1 0.16591 Uiso D U
C5C C -0.424068 0.122095 -0.395263 1 0.16363 Uiso D U
C6C C -0.631837 0.169506 -0.342683 1 0.17085 Uiso D U
C7C C -0.656043 0.245387 -0.428387 1 0.17288 Uiso D U
C8C C -0.441468 0.310054 -0.244557 1 0.10094 Uiso D U
C9C C -0.357395 0.340646 -0.159922 1 0.10271 Uiso D U
H11AC H -0.282884 0.392902 -0.084725 1 0.11095 Uiso D U
H11BC H -0.273839 0.298895 -0.082988 1 0.11057 Uiso D U
H11CC H -0.184943 0.348321 -0.129914 1 0.11057 Uiso D U
H12AC H -0.526919 0.47526 -0.136103 1 0.10259 Uiso D U
H12BC H -0.601516 0.401012 -0.107965 1 0.10259 Uiso D U
H12CC H -0.468774 0.422731 -0.079382 1 0.10284 Uiso D U
H4AC H -0.298648 0.23118 -0.437469 1 0.15831 Uiso D U
H4BC H -0.426738 0.231615 -0.476826 1 0.15831 Uiso D U
H4CC H -0.395038 0.301889 -0.428342 1 0.15831 Uiso D U
H5AC H -0.490654 0.099668 -0.421798 1 0.15692 Uiso D U
H5BC H -0.344388 0.114746 -0.417435 1 0.15692 Uiso D U
H5CC H -0.42088 0.09515 -0.353635 1 0.15692 Uiso D U
H6AC H -0.708071 0.189647 -0.322693 1 0.16477 Uiso D U
H6BC H -0.655095 0.127592 -0.372735 1 0.1649 Uiso D U
H6CC H -0.578603 0.147624 -0.308846 1 0.16465 Uiso D U
H7AC H -0.741838 0.243699 -0.412448 1 0.16642 Uiso D U
H7BC H -0.639504 0.297371 -0.446908 1 0.16642 Uiso D U
H7CC H -0.644586 0.20516 -0.461645 1 0.16642 Uiso D U
N1C N -0.39478 0.229438 -0.329638 1 0.12412 Uiso D U
N2C N -0.566543 0.282402 -0.329148 1 0.1269 Uiso D U
N3C N -0.345077 0.301943 -0.210988 1 0.10183 Uiso D U
N4C N -0.516151 0.353546 -0.216019 1 0.09739 Uiso D U
O1C O -0.285124 0.213761 -0.315258 1 0.13007 Uiso D U
O2C O -0.657421 0.318437 -0.31036 1 0.14109 Uiso D U
CL Cl -0.259712 0.531925 -0.00935 1 0.20771 Uiso D U
O1 O -0.338186 0.515432 -0.055073 1 0.28522 Uiso D U
O2 O -0.203807 0.599532 -0.021727 1 0.27344 Uiso D U
O3 O -0.313722 0.535736 0.047371 1 0.29041 Uiso D U
O4 O -0.178913 0.473355 -0.00601 1 0.25964 Uiso D U

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
O2A N2A 1.315 . .
N2A C3A 1.47 . .
N2A C1A 1.337 . .
C3A C6A 1.518 . .
C3A C7A 1.546 . .
C3A C2A 1.596 . .
C6A H6CA 1.06 . .
C6A H6BA 1.058 . .
C6A H6AA 1.059 . .
C7A H7CA 1.059 . .
C7A H7BA 1.059 . .
C7A H7AA 1.059 . .
C2A C5A 1.534 . .
C2A C4A 1.528 . .
C2A N1A 1.452 . .
C5A H5BA 1.059 . .
C5A H5AA 1.059 . .
C4A H4CA 1.06 . .
C4A H4BA 1.059 . .
C4A H4AA 1.059 . .
N1A O1A 1.298 . .
N1A C1A 1.339 . .
C1A C8A 1.491 . .
C8A N4A 1.347 . .
C8A N3A 1.347 . .
N4A C10A 1.348 . .
C10A C9A 1.381 . .
C10A C12A 1.503 . .
C9A N3A 1.361 . .
C9A C11A 1.497 . .
C11A H11CA 1.058 . .
C11A H11BA 1.059 . .
C11A H11AA 1.059 . .
C12A H12CA 1.059 . .
C12A H12BA 1.059 . .
C12A H12AA 1.059 . .
O2B N2B 1.318 . .
N2B C3B 1.486 . .
N2B C1B 1.338 . .
C3B C6B 1.526 . .
C3B C7B 1.522 . .
C3B C2B 1.564 . .
C6B H6CB 1.059 . .
C6B H6BB 1.059 . .
C6B H6AB 1.059 . .
C7B H7CB 1.059 . .
C7B H7BB 1.059 . .
C7B H7AB 1.059 . .
C2B C5B 1.502 . .
C2B C4B 1.539 . .
C2B N1B 1.46 . .
C5B H5CB 1.059 . .
C5B H5BB 1.058 . .
C5B H5AB 1.059 . .
C4B H4CB 1.059 . .
C4B H4BB 1.059 . .
C4B H4AB 1.059 . .
N1B O1B 1.29 . .
N1B C1B 1.333 . .
C1B C8B 1.479 . .
C8B N4B 1.374 . .
C8B N3B 1.328 . .
N4B C10B 1.349 . .
C10B C9B 1.397 . .
C10B C12B 1.524 . .
C9B N3B 1.355 . .
C9B C11B 1.501 . .
C11B H11CB 1.059 . .
C11B H11BB 1.059 . .
C11B H11AB 1.059 . .
C12B H12CB 1.059 . .
C12B H12BB 1.058 . .
C12B H12AB 1.059 . .
O2C N2C 1.315 . .
N2C C3C 1.431 . .
N2C C1C 1.323 . .
C3C C6C 1.549 . .
C3C C7C 1.54 . .
C3C C2C 1.544 . .
C6C H6CC 1.059 . .
C6C H6BC 1.059 . .
C6C H6AC 1.059 . .
C7C H7CC 1.059 . .
C7C H7BC 1.059 . .
C7C H7AC 1.059 . .
C2C C5C 1.536 . .
C2C C4C 1.53 . .
C2C N1C 1.464 . .
C5C H5CC 1.059 . .
C5C H5BC 1.059 . .
C5C H5AC 1.059 . .
C4C H4CC 1.059 . .
C4C H4BC 1.059 . .
C4C H4AC 1.059 . .
N1C O1C 1.345 . .
N1C C1C 1.326 . .
C1C C8C 1.476 . .
C8C N4C 1.342 . .
C8C N3C 1.358 . .
N4C C10C 1.374 . .
C10C C9C 1.384 . .
C10C C12C 1.485 . .
C9C N3C 1.357 . .
C9C C11C 1.522 . .
C11C H11CC 1.059 . .
C11C H11BC 1.06 . .
C11C H11AC 1.058 . .
C12C H12CC 1.059 . .
C12C H12BC 1.059 . .
C12C H12AC 1.059 . .
O4 CL 1.429 . .
CL O1 1.406 . .
CL O2 1.429 . .
CL O3 1.422 . .


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_2
_geom_angle_site_symmetry_3
O2A ? C3A 121.99 . . .
O2A ? C1A 128.61 . . .
N2A ? C6A 109.85 . . .
N2A ? C7A 104.86 . . .
N2A ? C2A 103.47 . . .
N2A ? N1A 113.47 . . .
N2A ? C8A 125.88 . . .
C3A ? C1A 109.39 . . .
C3A ? H6CA 109.92 . . .
C3A ? H6BA 109.56 . . .
C3A ? H6AA 109.23 . . .
C3A ? H7CA 109.04 . . .
C3A ? H7BA 110.33 . . .
C3A ? H7AA 109.02 . . .
C3A ? C5A 112.93 . . .
C3A ? C4A 123.63 . . .
C3A ? N1A 101.57 . . .
C6A ? C7A 107.4 . . .
C6A ? C2A 117.43 . . .
H6CA ? H6BA 109.37 . . .
H6CA ? H6AA 109.23 . . .
H6BA ? H6AA 109.51 . . .
C7A ? C2A 113.06 . . .
H7CA ? H7BA 109.97 . . .
H7CA ? H7AA 109.54 . . .
H7BA ? H7AA 108.93 . . .
C2A ? H5CA 109.45 . . .
C2A ? H5BA 110.33 . . .
C2A ? H5AA 109.55 . . .
C2A ? H4CA 110.05 . . .
C2A ? H4BA 109.49 . . .
C2A ? H4AA 110.63 . . .
C2A ? O1A 118.25 . . .
C2A ? C1A 111.41 . . .
C5A ? C4A 107.13 . . .
C5A ? N1A 100.45 . . .
H5CA ? H5BA 109.23 . . .
H5CA ? H5AA 109.37 . . .
H5BA ? H5AA 108.9 . . .
C4A ? N1A 108.41 . . .
H4CA ? H4BA 108.47 . . .
H4CA ? H4AA 109.11 . . .
H4BA ? H4AA 109.04 . . .
N1A ? C8A 120.62 . . .
O1A ? C1A 129.79 . . .
C1A ? N4A 126.93 . . .
C1A ? N3A 124.04 . . .
C8A ? C10A 109.68 . . .
C8A ? C9A 106.44 . . .
N4A ? N3A 108.99 . . .
N4A ? C9A 105.35 . . .
N4A ? C12A 126.56 . . .
C10A ? N3A 109.53 . . .
C10A ? C11A 124.37 . . .
C10A ? H12CA 108.87 . . .
C10A ? H12BA 108.5 . . .
C10A ? H12AA 108.51 . . .
C9A ? C12A 128.08 . . .
C9A ? H11CA 109.39 . . .
C9A ? H11BA 109.57 . . .
C9A ? H11AA 109.25 . . .
N3A ? C11A 126.11 . . .
H11CA ? H11BA 109.55 . . .
H11CA ? H11AA 109.53 . . .
H11BA ? H11AA 109.54 . . .
H12CA ? H12BA 110.39 . . .
H12CA ? H12AA 110.15 . . .
H12BA ? H12AA 110.37 . . .
O2B ? C3B 122.32 . . .
O2B ? C1B 126.69 . . .
N2B ? C6B 105.17 . . .
N2B ? C7B 112.98 . . .
N2B ? C2B 101.63 . . .
N2B ? N1B 112.43 . . .
N2B ? C8B 121.17 . . .
C3B ? C1B 110.63 . . .
C3B ? H6CB 109.67 . . .
C3B ? H6BB 109.5 . . .
C3B ? H6AB 109.76 . . .
C3B ? H7CB 109.7 . . .
C3B ? H7BB 109.46 . . .
C3B ? H7AB 110.19 . . .
C3B ? C5B 121.66 . . .
C3B ? C4B 108.9 . . .
C3B ? N1B 103.6 . . .
C6B ? C7B 102.82 . . .
C6B ? C2B 111.8 . . .
H6CB ? H6BB 109.45 . . .
H6CB ? H6AB 108.94 . . .
H6BB ? H6AB 109.49 . . .
C7B ? C2B 121.61 . . .
H7CB ? H7BB 108.82 . . .
H7CB ? H7AB 109.8 . . .
H7BB ? H7AB 108.84 . . .
C2B ? H5CB 109.12 . . .
C2B ? H5BB 110.2 . . .
C2B ? H5AB 109.06 . . .
C2B ? H4CB 109.44 . . .
C2B ? H4BB 109.56 . . .
C2B ? H4AB 109.89 . . .
C2B ? O1B 119.9 . . .
C2B ? C1B 110.73 . . .
C5B ? C4B 106.6 . . .
C5B ? N1B 111.73 . . .
H5CB ? H5BB 109.36 . . .
H5CB ? H5AB 109.53 . . .
H5BB ? H5AB 109.56 . . .
C4B ? N1B 102.81 . . .
H4CB ? H4BB 109.45 . . .
H4CB ? H4AB 109.24 . . .
H4BB ? H4AB 109.25 . . .
N1B ? C8B 126.36 . . .
O1B ? C1B 129.23 . . .
C1B ? N4B 127.91 . . .
C1B ? N3B 124.18 . . .
C8B ? C10B 109.15 . . .
C8B ? C9B 108.99 . . .
N4B ? N3B 107.87 . . .
N4B ? C9B 105.91 . . .
N4B ? C12B 124.3 . . .
C10B ? N3B 107.93 . . .
C10B ? C11B 127.25 . . .
C10B ? H12CB 109.39 . . .
C10B ? H12BB 109.4 . . .
C10B ? H12AB 109.41 . . .
C9B ? C12B 129.79 . . .
C9B ? H11CB 109.39 . . .
C9B ? H11BB 109.33 . . .
C9B ? H11AB 109.26 . . .
N3B ? C11B 124.8 . . .
H11CB ? H11BB 109.44 . . .
H11CB ? H11AB 109.39 . . .
H11BB ? H11AB 110.02 . . .
H12CB ? H12BB 109.56 . . .
H12CB ? H12AB 109.47 . . .
H12BB ? H12AB 109.59 . . .
O2C ? C3C 123.07 . . .
O2C ? C1C 127.95 . . .
N2C ? C6C 96.75 . . .
N2C ? C7C 118.38 . . .
N2C ? C2C 105.94 . . .
N2C ? N1C 113.82 . . .
N2C ? C8C 121.66 . . .
C3C ? C1C 107.81 . . .
C3C ? H6CC 111.73 . . .
C3C ? H6BC 109.35 . . .
C3C ? H6AC 109.84 . . .
C3C ? H7CC 109.21 . . .
C3C ? H7BC 109.08 . . .
C3C ? H7AC 110.42 . . .
C3C ? C5C 119.65 . . .
C3C ? C4C 109.98 . . .
C3C ? N1C 99.96 . . .
C6C ? C7C 101.57 . . .
C6C ? C2C 104.26 . . .
H6CC ? H6BC 109.28 . . .
H6CC ? H6AC 108.42 . . .
H6BC ? H6AC 108.13 . . .
C7C ? C2C 124.79 . . .
H7CC ? H7BC 109.23 . . .
H7CC ? H7AC 109.64 . . .
H7BC ? H7AC 109.25 . . .
C2C ? H5CC 109.49 . . .
C2C ? H5BC 109.73 . . .
C2C ? H5AC 109.87 . . .
C2C ? H4CC 109.46 . . .
C2C ? H4BC 109.37 . . .
C2C ? H4AC 109.72 . . .
C2C ? O1C 121.38 . . .
C2C ? C1C 110.32 . . .
C5C ? C4C 107.76 . . .
C5C ? N1C 111.86 . . .
H5CC ? H5BC 108.98 . . .
H5CC ? H5AC 109.91 . . .
H5BC ? H5AC 108.85 . . .
C4C ? N1C 106.87 . . .
H4CC ? H4BC 109.42 . . .
H4CC ? H4AC 109.28 . . .
H4BC ? H4AC 109.56 . . .
N1C ? C8C 124.29 . . .
O1C ? C1C 127.8 . . .
C1C ? N4C 123.79 . . .
C1C ? N3C 126.74 . . .
C8C ? C10C 106.67 . . .
C8C ? C9C 108.97 . . .
N4C ? N3C 109.43 . . .
N4C ? C9C 109 . . .
N4C ? C12C 123.71 . . .
C10C ? N3C 105.92 . . .
C10C ? C11C 128.92 . . .
C10C ? H12CC 109.78 . . .
C10C ? H12BC 109.05 . . .
C10C ? H12AC 109.69 . . .
C9C ? C12C 127.27 . . .
C9C ? H11CC 108.86 . . .
C9C ? H11BC 109.46 . . .
C9C ? H11AC 109.66 . . .
N3C ? C11C 125.15 . . .
H11CC ? H11BC 109.68 . . .
H11CC ? H11AC 109.58 . . .
H11BC ? H11AC 109.59 . . .
H12CC ? H12BC 108.29 . . .
H12CC ? H12AC 110.01 . . .
H12BC ? H12AC 109.99 . . .
O4 ? O1 107.54 . . .
O4 ? O2 111.5 . . .
O4 ? O3 106.23 . . .
O1 ? O2 109.85 . . .
O1 ? O3 112.3 . . .
O2 ? O3 109.39 . . .















_exptl_crystal_recrystallization_method 'Crystallization upon mixing reactants'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17
_database_code_depnum_ccdc_archive 'CCDC 2330280'
loop_
_audit_author_name
_audit_author_address
'Dominique Housset'
;Institut de Biologie Structurale, Grenoble
France
;
_audit_update_record             
;
2024-02-01 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_ATOM007_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: All atoms were refined with an isotropic displacement parameter.
;
_vrf_GEOM006_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: REFMAC5 log file is unfortunately not providing it. A visualization of the model allows to easily identify it for each angle.
;
_vrf_THETM01_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The highest resolution of the diffraction data is 1.18 \%A. sine(theta_max)/wavelength is thus less than 0.55.
;
_vrf_PLAT201_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......        100 Report
RESPONSE: All atoms were refined with an isotropic displacement parameter. Refinement tests with anisotropic displacement parameters did not improve significantly the free R factor.
;
_vrf_PLAT602_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check
RESPONSE: No interpretable peak was found in the resisual (F_obs - F_calc) Coulomb potential map.
;
_vrf_RINTA01_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High value of Rint is common in electron diffraction data. Such a high Rint value may originate from multiple diffraction and/or errors introduced rotation stage and microscope optics.
;
_vrf_PLAT242_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Mn4 Check
RESPONSE: No restraint was applied on atomic displacement parameteres for Mn atoms.
;
_vrf_PLAT420_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17 
;
PROBLEM: D-H Bond Without Acceptor  Om1      --HoM1     .     Please Check
RESPONSE: Hydrogens from methanol hydroxyl groups were not observed in the resisual Coulomb potential map. They were placed automatically by REFMAC5.
;
_vrf_PLAT420_ED_Mn2-NITIm3_P21_1_18_A_XDS_I_F_Fc_2021_11_17_2 
;
PROBLEM: D-H Bond Without Acceptor  Om2      --HoM2     .     Please Check
RESPONSE: Hydrogens from methanol hydroxyl groups were not observed in the resisual Coulomb potential map. They were placed automatically by REFMAC5.
;

_audit_creation_method           'Refmac5 5.8.0267'
_audit_creation_date             2023-10-03
_chemical_name_systematic        
Tris(2-(2-imidazolyl)--4,4,5,5-tetramethyl-4,5-dihydro-imidazol-3-oxide-1-oxyl)dimanganese(II).triflate.methanol
_chemical_name_common            '[Mn2(NITIm)3].Triflate.Methanol'
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(Mn2 C30 H42 N12 O6), 2(C F3 S O3), 2(C H4 O)'
_chemical_formula_sum            'C64 H92 F6 Mn4 N24 O20 S2'
_chemical_formula_weight         1915.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
H H 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
N N 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
O O 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
S S 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
F F 0.0000 0.0000 'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'
MN MN 0.0000 0.0000
'electron scat. length: CCP4 atomsf.lib & Mott-Bethe formula'

_space_group_crystal_system      monoclinic
_symmetry_space_group_name_H-M   P2(1)
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_IT_number           4

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x,  y+1/2, -z'

_cell_length_a                   9.832
_cell_length_b                   19.906
_cell_length_c                   27.716
_cell_angle_alpha                90.000
_cell_angle_beta                 98.151
_cell_angle_gamma                90.000
_cell_volume                     5369.66
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6192
_cell_measurement_theta_min      0.036093
_cell_measurement_theta_max      0.607339

_exptl_crystal_description       nanocrystal
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    ?
_exptl_crystal_F_000             ?
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.0250793

_diffrn_source                   'Field emission gun (FEG) electron microscope'
_diffrn_measurement_device       'transmission electron microscope'
_diffrn_measurement_device_type  'TECNAI F20 (200 keV)'
_diffrn_detector                 'hybrid pixel direct electron detector'
_diffrn_detector_type            'ASI MEDIPIX 3RX'
_diffrn_detector_dtime           0.0
_diffrn_radiation_type           electron
_exptl_special_details           
'data collected by continuous rotation 3D electron diffraction with low electron dose'
_diffrn_radiation_probe          electron

_diffrn_reflns_number            39340
_diffrn_reflns_av_unetI/netI     0.1447
_diffrn_reflns_av_R_equivalents  0.241
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_resolution_max    0.8453
_diffrn_reflns_theta_min         0.036093
_diffrn_reflns_theta_max         0.607339
_diffrn_reflns_theta_full        ?
_diffrn_measured_fraction_theta_max 0.728
_diffrn_measured_fraction_theta_full ?
_diffrn_reflns_Laue_measured_fraction_max ?
_diffrn_reflns_Laue_measured_fraction_full ?
_diffrn_reflns_point_group_measured_fraction_max ?
_diffrn_reflns_point_group_measured_fraction_full ?
_reflns_number_total             2585
_reflns_number_gt                ?
_reflns_threshold_expression     ?
_reflns_Friedel_coverage         ?
_reflns_Friedel_fraction_max     ?
_reflns_Friedel_fraction_full    ?
_reflns_d_resolution_high        19.906
_reflns_d_resolution_low         1.183

loop_
_reflns_shell_d_res_high
_reflns_shell_d_res_low
_reflns_shell_number_measured_all
_reflns_shell_number_unique_all
_reflns_shell_number_possible
_reflns_shell_Rmerge_I_all
_reflns_shell_meanI_over_sigI_all
19.91 5.29 531 31 42 0.077 29.65
5.29 3.74 1178 60 81 0.089 30.52
3.74 3.06 1504 80 98 0.118 20.63
3.06 2.65 1811 85 112 0.164 19.59
2.65 2.37 1961 104 132 0.201 14.7
2.37 2.16 2240 107 136 0.213 14.24
2.16 2 2226 112 145 0.256 12.62
2 1.87 2875 138 174 0.363 9.36
1.87 1.76 2966 140 177 0.496 7.17
1.76 1.67 2857 139 178 0.751 4.96
1.67 1.6 3215 158 197 0.697 5.27
1.6 1.53 3369 159 200 0.688 5.14
1.53 1.47 3322 158 204 0.784 4.24
1.47 1.41 3074 166 210 1.032 3.2
1.41 1.37 2312 173 239 0.916 3.04
1.37 1.32 1282 150 220 1.028 2.13
1.32 1.28 1235 154 250 1.649 1.25
1.28 1.25 434 144 231 1.166 0.95
1.25 1.21 511 168 261 0.99 1.03
1.21 1.18 437 159 264 0.984 0.86
19.91 1.18 39340 2585 3551 0.241 6.91


_reflns_special_details          
;
 Electron diffraction, continuous rotation, flat field and geometrical correction of diffraction images with ImageJ
 8 data sets were indexed and processed with XDS and merged in the
P2(1) space group with XSCALE. Merging statistics provided by XSCALE are provided below:
 SUBSET OF INTENSITY DATA WITH SIGNAL/NOISE >= -3.0 AS FUNCTION OF RESOLUTION
 RESOLUTION     NUMBER OF REFLECTIONS    COMPLETENESS R-FACTOR  R-FACTOR COMPARED I/SIGMA   R-meas  CC(1/2)  Anomal  SigAno   Nano
   LIMIT     OBSERVED  UNIQUE  POSSIBLE     OF DATA   observed  expected                                      Corr

     5.29         531      31        42       73.8%       7.7%      8.0%      531   29.65      7.9%    99.9*    -2    0.914      25
     3.74        1178      60        81       74.1%       8.9%      8.3%     1178   30.52      9.2%    99.9*   -18    0.823      51
     3.06        1504      80        98       81.6%      11.8%     11.6%     1503   20.63     12.2%    99.6*    -9    0.767      68
     2.65        1811      85       112       75.9%      16.4%     14.7%     1811   19.59     16.8%    99.8*   -10    0.876      79
     2.37        1961     104       132       78.8%      20.1%     19.5%     1960   14.70     20.7%    99.6*    -1    0.868      92
     2.16        2240     107       136       78.7%      21.3%     20.4%     2239   14.24     21.8%    99.3*   -17    0.801      96
     2.00        2226     112       145       77.2%      25.6%     25.4%     2224   12.62     26.3%    98.9*   -14    0.704     105
     1.87        2875     138       174       79.3%      36.3%     36.5%     2874    9.36     37.3%    98.2*     9    0.830     121
     1.76        2966     140       177       79.1%      49.6%     51.7%     2966    7.17     50.9%    97.5*    -9    0.731     132
     1.67        2857     139       178       78.1%      75.1%     94.0%     2855    4.96     77.1%    88.5*    -3    0.755     127
     1.60        3215     158       197       80.2%      69.7%     90.1%     3212    5.27     71.5%    90.6*   -11    0.640     139
     1.53        3369     159       200       79.5%      68.8%     89.8%     3368    5.14     70.5%    93.0*    -9    0.706     148
     1.47        3322     158       204       77.5%      78.4%    115.2%     3320    4.24     80.3%    94.0*    -1    0.716     149
     1.41        3074     166       210       79.0%     103.2%    224.0%     3073    3.20    106.3%    73.3*    -6    0.713     156
     1.37        2312     173       239       72.4%      91.6%    148.7%     2309    3.04     95.2%    77.3*     1    0.720     148
     1.32        1282     150       220       68.2%     102.8%    115.2%     1281    2.13    109.1%    68.9*    -6    0.645     132
     1.28        1235     154       250       61.6%     164.9%    232.3%     1230    1.25    175.5%    46.6*    10    0.707     132
     1.25         434     144       231       62.3%     116.6%    123.1%      430    0.95    143.0%    25.4    -15    0.631      69
     1.21         511     168       261       64.4%      99.0%    118.1%      507    1.03    121.1%    33.2*    17    0.744      82
     1.18         437     159       264       60.2%      98.4%    172.8%      416    0.86    120.9%    47.0*    -7    0.665      62
    total       39340    2585      3551       72.8%      24.1%     28.7%    39287    6.91     24.9%    99.8*    -4    0.735    2113
;

_computing_data_collection       'DEXTER (ASI)'
_computing_cell_refinement       'XDS (IDXREF, CORRECT, CELLPARM)'
_computing_data_reduction        XSCALE
_computing_structure_solution    'PHASER version 2.8.3 in CCP4 suite'
_computing_structure_refinement  
'REFMAC5 version 5.8.0267 in CCP4 7.1.018 suite'
_computing_molecular_graphics    COOT
_computing_publication_material  ?
_refine_special_details          
;
 Refinement was performed with REFMAC5 in CCP4 suite. Electron scattering length used dufring the refinement were calculated by the
Mott-Bethe formula using the "source electron mb" command in REFMAC5. Stereochemical restraints have been applied. A library of restraints
has has been created for NITIm (PR5) and Triflate (F3O) is provided below:
global_
_lib_name         mon_lib
_lib_version      5.52
_lib_update       17/08/20
# ------------------------------------------------
#
# ---   LIST OF MONOMERS ---
#
data_comp_list_CCDC1
loop_
_chem_comp.id
_chem_comp.three_letter_code
_chem_comp.name
_chem_comp.group
_chem_comp.number_atoms_all
_chem_comp.number_atoms_nh
_chem_comp.desc_level
F3O      F3O 'CF3-SO3                             ' non-polymer         8   8 .
PR5      PR5 'MOF Radical NITImH                  ' non-polymer        30  16 .
# ------------------------------------------------------
#
# --- DESCRIPTION OF MONOMERS ---
#
data_comp_F3O
#
loop_
_chem_comp_atom.comp_id
_chem_comp_atom.atom_id
_chem_comp_atom.type_symbol
_chem_comp_atom.type_energy
_chem_comp_atom.partial_charge
_chem_comp_atom.x
_chem_comp_atom.y
_chem_comp_atom.z
 F3O           F3     F    F         0.000      0.000    0.000    0.000
 F3O           C1     C    CT        0.000      0.934    0.933    0.000
 F3O           F1     F    F         0.000      1.685    0.804    1.078
 F3O           F2     F    F         0.000      1.685    0.804   -1.078
 F3O           S1     S    ST        0.000      0.218    2.433    0.000
 F3O           O1     O    OS       -0.330     -0.624    2.578    1.208
 F3O           O2     O    OS       -0.330     -0.624    2.578   -1.208
 F3O           O3     O    OS       -0.330      1.265    3.479   -0.000
loop_
_chem_comp_bond.comp_id
_chem_comp_bond.atom_id_1
_chem_comp_bond.atom_id_2
_chem_comp_bond.type
_chem_comp_bond.value_dist
_chem_comp_bond.value_dist_esd
 F3O      O1     S1        deloc       1.437    0.020
 F3O      O2     S1        deloc       1.437    0.020
 F3O      O3     S1        deloc       1.437    0.020
 F3O      S1     C1        single      1.820    0.020
 F3O      F1     C1        single      1.334    0.020
 F3O      F2     C1        single      1.334    0.020
 F3O      C1     F3        single      1.334    0.020
loop_
_chem_comp_angle.comp_id
_chem_comp_angle.atom_id_1
_chem_comp_angle.atom_id_2
_chem_comp_angle.atom_id_3
_chem_comp_angle.value_angle
_chem_comp_angle.value_angle_esd
 F3O      F3     C1     F1      107.321    3.000
 F3O      F3     C1     F2      107.321    3.000
 F3O      F3     C1     S1      111.544    3.000
 F3O      F1     C1     F2      107.321    3.000
 F3O      F1     C1     S1      111.544    3.000
 F3O      F2     C1     S1      111.544    3.000
 F3O      C1     S1     O1      102.944    3.000
 F3O      C1     S1     O2      102.944    3.000
 F3O      C1     S1     O3      102.944    3.000
 F3O      O1     S1     O2      115.132    3.000
 F3O      O1     S1     O3      115.132    3.000
 F3O      O2     S1     O3      115.132    3.000
loop_
_chem_comp_tor.comp_id
_chem_comp_tor.id
_chem_comp_tor.atom_id_1
_chem_comp_tor.atom_id_2
_chem_comp_tor.atom_id_3
_chem_comp_tor.atom_id_4
_chem_comp_tor.value_angle
_chem_comp_tor.value_angle_esd
_chem_comp_tor.period
 F3O      var_1            F3     C1     S1     O3               180.000           20.000   3
loop_
_chem_comp_chir.comp_id
_chem_comp_chir.id
_chem_comp_chir.atom_id_centre
_chem_comp_chir.atom_id_1
_chem_comp_chir.atom_id_2
_chem_comp_chir.atom_id_3
_chem_comp_chir.volume_sign
 F3O      chir_01          S1     O1     O2     O3        negativ
 F3O      chir_02          C1     S1     F1     F2        positiv
#
data_comp_PR5
#
loop_
_chem_comp_atom.comp_id
_chem_comp_atom.atom_id
_chem_comp_atom.type_symbol
_chem_comp_atom.type_energy
_chem_comp_atom.partial_charge
_chem_comp_atom.x
_chem_comp_atom.y
_chem_comp_atom.z
 PR5           O2     O    O         0.000      0.000    0.000    0.000
 PR5           N2     N    N         0.000      0.984    0.984    0.000
 PR5           C3     C    CT        0.000      2.390    0.608   -0.000
 PR5           C6     C    CH3       0.000      2.748   -0.222    1.227
 PR5           H6C    H    H         0.000      2.553    0.341    2.103
 PR5           H6B    H    H         0.000      2.165   -1.106    1.238
 PR5           H6A    H    H         0.000      3.776   -0.477    1.193
 PR5           C7     C    CH3       0.000      2.748   -0.222   -1.227
 PR5           H7C    H    H         0.000      2.165   -1.106   -1.238
 PR5           H7B    H    H         0.000      2.553    0.341   -2.103
 PR5           H7A    H    H         0.000      3.776   -0.477   -1.193
 PR5           C2     C    CT        0.000      3.298    1.831    0.000
 PR5           C5     C    CH3       0.000      3.053    2.694   -1.232
 PR5           H5C    H    H         0.000      3.248    2.126   -2.105
 PR5           H5B    H    H         0.000      2.045    3.019   -1.240
 PR5           H5A    H    H         0.000      3.695    3.535   -1.208
 PR5           C4     C    CH3       0.000      3.053    2.694    1.232
 PR5           H4C    H    H         0.000      2.045    3.019    1.240
 PR5           H4B    H    H         0.000      3.248    2.126    2.105
 PR5           H4A    H    H         0.000      3.695    3.535    1.208
 PR5           N1     N    N         0.000      4.704    1.455   -0.000
 PR5           O1     O    O         0.000      5.688    2.439   -0.000
 PR5           C1     C    C         0.000      0.640    2.269    0.000
 PR5           C8     C    CR5       0.000      1.694    3.323   -0.000
 PR5           N4     N    NRD5      0.000      1.482    4.656   -0.000
 PR5           C10    C    CR15      0.000      0.149    4.867    0.000
 PR5           H10    H    H         0.000     -0.343    5.832    0.000
 PR5           C9     C    CR15      0.000     -0.477    3.638    0.000
 PR5           H9     H    H         0.000      0.014    2.673    0.000
 PR5           N3     N    NRD5      0.000     -1.811    3.849    0.000
loop_
_chem_comp_bond.comp_id
_chem_comp_bond.atom_id_1
_chem_comp_bond.atom_id_2
_chem_comp_bond.type
_chem_comp_bond.value_dist
_chem_comp_bond.value_dist_esd
 PR5      O1     N1        single      1.344    0.020
 PR5      N2     O2        single      1.344    0.020
 PR5      N1     C1        single      1.333    0.020
 PR5      C1     N2        single      1.333    0.020
 PR5      N1     C2        single      1.457    0.020
 PR5      C3     N2        single      1.457    0.020
 PR5      N3     C8        aromatic    1.350    0.020
 PR5      N4     C8        aromatic    1.350    0.020
 PR5      N3     C9        aromatic    1.350    0.020
 PR5      C10    N4        aromatic    1.350    0.020
 PR5      C8     C1        aromatic    1.495    0.020
 PR5      C2     C3        single      1.589    0.020
 PR5      C4     C2        single      1.532    0.020
 PR5      C5     C2        single      1.532    0.020
 PR5      C6     C3        single      1.532    0.020
 PR5      C7     C3        single      1.532    0.020
 PR5      H4A    C4        single      1.059    0.020
 PR5      H4B    C4        single      1.059    0.020
 PR5      H4C    C4        single      1.059    0.020
 PR5      H5A    C5        single      1.059    0.020
 PR5      H5B    C5        single      1.059    0.020
 PR5      H5C    C5        single      1.059    0.020
 PR5      H6A    C6        single      1.059    0.020
 PR5      H6B    C6        single      1.059    0.020
 PR5      H6C    C6        single      1.059    0.020
 PR5      H7A    C7        single      1.059    0.020
 PR5      H7B    C7        single      1.059    0.020
 PR5      H7C    C7        single      1.059    0.020
 PR5      C9     C10       aromatic    1.380    0.020
 PR5      H9     C9        single      1.083    0.020
 PR5      H10    C10       single      1.083    0.020
loop_
_chem_comp_angle.comp_id
_chem_comp_angle.atom_id_1
_chem_comp_angle.atom_id_2
_chem_comp_angle.atom_id_3
_chem_comp_angle.value_angle
_chem_comp_angle.value_angle_esd
 PR5      O2     N2     C3      122.550    3.000
 PR5      C2     N1     O1      122.550    3.000
 PR5      O2     N2     C1      126.710    3.000
 PR5      O1     N1     C1      126.710    3.000
 PR5      C3     N2     C1      110.740    3.000
 PR5      C2     N1     C1      110.740    3.000
 PR5      N2     C3     C6      106.580    3.000
 PR5      N2     C3     C7      106.580    3.000
 PR5      C5     C2     N1      106.580    3.000
 PR5      C4     C2     N1      106.580    3.000
 PR5      N2     C3     C2      102.670    3.000
 PR5      C3     C2     N1      102.670    3.000
 PR5      C6     C3     C7      106.850    3.000
 PR5      C5     C2     C4      106.850    3.000
 PR5      C6     C3     C2      116.600    3.000
 PR5      C7     C3     C2      116.600    3.000
 PR5      C3     C2     C5      116.600    3.000
 PR5      C3     C2     C4      116.600    3.000
 PR5      C3     C6     H6C     109.470    3.000
 PR5      C3     C6     H6B     109.470    3.000
 PR5      C3     C6     H6A     109.470    3.000
 PR5      H6C    C6     H6B     109.470    3.000
 PR5      H6C    C6     H6A     109.470    3.000
 PR5      H6B    C6     H6A     109.470    3.000
 PR5      C3     C7     H7C     109.470    3.000
 PR5      C3     C7     H7B     109.470    3.000
 PR5      C3     C7     H7A     109.470    3.000
 PR5      H7C    C7     H7B     109.470    3.000
 PR5      H7C    C7     H7A     109.470    3.000
 PR5      H7B    C7     H7A     109.470    3.000
 PR5      C2     C5     H5C     109.470    3.000
 PR5      C2     C5     H5B     109.470    3.000
 PR5      C2     C5     H5A     109.470    3.000
 PR5      H5C    C5     H5B     109.470    3.000
 PR5      H5C    C5     H5A     109.470    3.000
 PR5      H5B    C5     H5A     109.470    3.000
 PR5      C2     C4     H4C     109.470    3.000
 PR5      C2     C4     H4B     109.470    3.000
 PR5      C2     C4     H4A     109.470    3.000
 PR5      H4C    C4     H4B     109.470    3.000
 PR5      H4C    C4     H4A     109.470    3.000
 PR5      H4B    C4     H4A     109.470    3.000
 PR5      N2     C1     C8      123.240    3.000
 PR5      N1     C1     C8      123.240    3.000
 PR5      N2     C1     N1      113.520    3.000
 PR5      C1     C8     N4      126.180    3.000
 PR5      C1     C8     N3      126.180    3.000
 PR5      N4     C8     N3      107.640    3.000
 PR5      C8     N4     C10     108.900    3.000
 PR5      C9     N3     C8      108.900    3.000
 PR5      N4     C10    C9      107.270    3.000
 PR5      C10    C9     N3      107.270    3.000
 PR5      N4     C10    H10     126.000    3.000
 PR5      H10    C10    C9      126.000    3.000
 PR5      C10    C9     H9      126.000    3.000
 PR5      H9     C9     N3      126.000    3.000
loop_
_chem_comp_plane_atom.comp_id
_chem_comp_plane_atom.plane_id
_chem_comp_plane_atom.atom_id
_chem_comp_plane_atom.dist_esd
 PR5      plan-1            N1        0.020
 PR5      plan-1            O1        0.020
 PR5      plan-1            C1        0.020
 PR5      plan-1            C8        0.020
 PR5      plan-1            C2        0.020
 PR5      plan-1            N2        0.020
 PR5      plan-1            O2        0.020
 PR5      plan-1            C3        0.020
 PR5      plan-2            N3        0.020
 PR5      plan-2            C8        0.020
 PR5      plan-2            C9        0.020
 PR5      plan-2            N4        0.020
 PR5      plan-2            C10       0.020
 PR5      plan-2            C1        0.020
 PR5      plan-2            H9        0.020
 PR5      plan-2            H10       0.020
# ------------------------------------------------------
# ------------------------------------------------------

The refinement uses a loglikelihood residual derived from Rice distribution for centric and acentric cases of Fs.
Fxray = SUM(LLKcentric_hkl) + SUM(LLKacentric_hkl)
The refinement is performed with structure factors (F) calculated by the program Truncate from the CCP4 suite.

The statistics provided by REFMAC for the final structure refined on all reflections is presented below:
REMARK   3
REMARK   3 REFINEMENT.
REMARK   3   PROGRAM     : REFMAC 5.8.0267   
REMARK   3   AUTHORS     : MURSHUDOV,SKUBAK,LEBEDEV,PANNU,
REMARK   3                 STEINER,NICHOLLS,WINN,LONG,VAGIN
REMARK   3
REMARK   3    REFINEMENT TARGET : MAXIMUM LIKELIHOOD
REMARK   3
REMARK   3  DATA USED IN REFINEMENT.
REMARK   3   RESOLUTION RANGE HIGH (ANGSTROMS) :   1.19
REMARK   3   RESOLUTION RANGE LOW  (ANGSTROMS) :  16.12
REMARK   3   DATA CUTOFF            (SIGMA(F)) : NONE
REMARK   3   COMPLETENESS FOR RANGE        (%) :  73.02
REMARK   3   NUMBER OF REFLECTIONS             :    2582
REMARK   3
REMARK   3  FIT TO DATA USED IN REFINEMENT.
REMARK   3   CROSS-VALIDATION METHOD          : NULL
REMARK   3   FREE R VALUE TEST SET SELECTION  : NULL
REMARK   3   R VALUE     (WORKING + TEST SET) : 0.19919
REMARK   3   R VALUE            (WORKING SET) :  0.19919
REMARK   3   FREE R VALUE                     : NULL
REMARK   3   FREE R VALUE TEST SET SIZE   (%) : NULL
REMARK   3   FREE R VALUE TEST SET COUNT      : NULL
REMARK   3
REMARK   3  FIT IN THE HIGHEST RESOLUTION BIN.
REMARK   3   TOTAL NUMBER OF BINS USED           :      20
REMARK   3   BIN RESOLUTION RANGE HIGH           :    1.185
REMARK   3   BIN RESOLUTION RANGE LOW            :    1.216
REMARK   3   REFLECTION IN BIN     (WORKING SET) :      167
REMARK   3   BIN COMPLETENESS (WORKING+TEST) (%) :    61.62
REMARK   3   BIN R VALUE           (WORKING SET) :    0.379
REMARK   3   BIN FREE R VALUE SET COUNT          :        0
REMARK   3   BIN FREE R VALUE                    :    0.000
REMARK   3
REMARK   3  NUMBER OF NON-HYDROGEN ATOMS USED IN REFINEMENT.
REMARK   3   ALL ATOMS                :      120
REMARK   3
REMARK   3  B VALUES.
REMARK   3   FROM WILSON PLOT           (A**2) : NULL
REMARK   3   MEAN B VALUE      (OVERALL, A**2) :  15.602
REMARK   3   OVERALL ANISOTROPIC B VALUE.
REMARK   3    B11 (A**2) :    -0.64
REMARK   3    B22 (A**2) :    -1.03
REMARK   3    B33 (A**2) :     1.56
REMARK   3    B12 (A**2) :    -0.00
REMARK   3    B13 (A**2) :     0.16
REMARK   3    B23 (A**2) :    -0.00
REMARK   3
REMARK   3  ESTIMATED OVERALL COORDINATE ERROR.
REMARK   3   ESU BASED ON R VALUE                            (A):   0.063
REMARK   3   ESU BASED ON FREE R VALUE                       (A): NULL
REMARK   3   ESU BASED ON MAXIMUM LIKELIHOOD                 (A):   0.051
REMARK   3   ESU FOR B VALUES BASED ON MAXIMUM LIKELIHOOD (A**2):   1.347
REMARK   3
REMARK   3 CORRELATION COEFFICIENTS.
REMARK   3   CORRELATION COEFFICIENT FO-FC      :   0.970
REMARK   3   CORRELATION COEFFICIENT FO-FC FREE : NULL
REMARK   3
REMARK   3  RMS DEVIATIONS FROM IDEAL VALUES        COUNT    RMS    WEIGHT
REMARK   3   BOND LENGTHS REFINED ATOMS        (A):   118 ; 0.017 ; 0.020
REMARK   3   BOND LENGTHS OTHERS               (A):    92 ; 0.000 ; 0.020
REMARK   3   BOND ANGLES REFINED ATOMS   (DEGREES):   192 ; 2.939 ; 3.000
REMARK   3   BOND ANGLES OTHERS          (DEGREES):   182 ; 0.350 ; 2.901
REMARK   3   CHIRAL-CENTER RESTRAINTS       (A**3):     4 ; 0.084 ; 0.200
REMARK   3   GENERAL PLANES REFINED ATOMS      (A):    84 ; 0.035 ; 0.020
REMARK   3   GENERAL PLANES OTHERS             (A):    12 ; 0.000 ; 0.020
REMARK   3
REMARK   3  ISOTROPIC THERMAL FACTOR RESTRAINTS.     COUNT   RMS    WEIGHT
REMARK   3   MAIN-CHAIN BOND REFINED ATOMS  (A**2):     2 ; 0.984 ; 3.046
REMARK   3   SIDE-CHAIN BOND REFINED ATOMS  (A**2):   116 ; 0.837 ; 1.500
REMARK   3   SIDE-CHAIN BOND OTHER ATOMS  (A**2)  :   117 ; 0.834 ; 1.512
REMARK   3   SIDE-CHAIN ANGLE OTHER ATOMS (A**2)  :   193 ; 1.360 ; 2.296
REMARK   3   LONG RANGE B REFINED ATOMS (A**2)    :   137 ; 2.509 ;16.418
REMARK   3   LONG RANGE B OTHER ATOMS (A**2)      :   138 ; 2.501 ;16.562
REMARK   3
REMARK   3  NCS RESTRAINTS STATISTICS
REMARK   3   NUMBER OF NCS GROUPS : NULL
REMARK   3
REMARK   3  TWIN DETAILS
REMARK   3   NUMBER OF TWIN DOMAINS  : NULL
REMARK   3
REMARK   3
REMARK   3  TLS DETAILS
REMARK   3   NUMBER OF TLS GROUPS  : NULL
REMARK   3
REMARK   3
REMARK   3  BULK SOLVENT MODELLING.
REMARK   3   METHOD USED :  MASK
REMARK   3   PARAMETERS FOR MASK CALCULATION
REMARK   3   VDW PROBE RADIUS   :   1.20
REMARK   3   ION PROBE RADIUS   :   0.80
REMARK   3   SHRINKAGE RADIUS   :   0.80
REMARK   3
REMARK   3  OTHER REFINEMENT REMARKS:
REMARK   3  HYDROGENS HAVE BEEN USED IF PRESENT IN THE INPUT
REMARK   3  U VALUES      : REFINED INDIVIDUALLY
REMARK   3

;
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           sparse
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     ?
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_parameters     848
_refine_ls_number_restraints     604
_refine_ls_R_factor_gt           ?
_refine_ls_wR_factor_ref         ?
_refine_ls_wR_factor_gt          ?
_refine_ls_goodness_of_fit_ref   ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

loop_
_refine_ls_d_res_high
_refine_ls_d_res_low
_refine_ls_number_reflns
_refine_ls_R_factor_all
19.906 5.208 45 0.188
5.208 3.716 79 0.133
3.716 3.044 99 0.161
3.044 2.64 114 0.148
2.64 2.364 128 0.202
2.364 2.159 137 0.178
2.159 2 143 0.15
2 1.871 173 0.176
1.871 1.765 178 0.168
1.765 1.674 178 0.189
1.674 1.597 193 0.201
1.597 1.529 198 0.187
1.529 1.469 199 0.195
1.469 1.416 214 0.245
1.416 1.368 236 0.258
1.368 1.325 218 0.272
1.325 1.285 248 0.299
1.285 1.249 230 0.365
1.249 1.216 254 0.363
1.216 1.185 271 0.379
19.906 1.185 2582 0.1992

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
MN1 Mn 0.246763 0.148649 0.002843 1 0.08726 Uiso D U
MN2 Mn -0.239209 -0.042048 0.051684 1 0.09068 Uiso D U
MN3 Mn 0.73839 0.004371 0.502551 1 0.15325 Uiso D U
MN4 Mn 0.738641 -0.305134 0.450503 1 0.13488 Uiso D U
C1A C -0.061486 0.112378 0.046435 1 0.09929 Uiso D U
C10A C 0.02353 -0.042098 -0.00831 1 0.09904 Uiso D U
C2A C -0.112002 0.220235 0.064076 1 0.11665 Uiso D U
C3A C -0.172671 0.173365 0.099577 1 0.10575 Uiso D U
C4A C -0.22863 0.243494 0.024457 1 0.11867 Uiso D U
C5A C -0.032779 0.281724 0.084415 1 0.12197 Uiso D U
C6A C -0.319935 0.183965 0.109017 1 0.10993 Uiso D U
C7A C -0.078814 0.173264 0.149402 1 0.11386 Uiso D U
C8A C -0.006328 0.055863 0.021067 1 0.09613 Uiso D U
C9A C 0.125589 -0.000954 -0.020411 1 0.09702 Uiso D U
H10A H 0.008422 -0.094343 -0.018625 1 0.09714 Uiso D U
H4AA H -0.288784 0.201798 0.010606 1 0.11791 Uiso D U
H4BA H -0.291645 0.278861 0.039328 1 0.11804 Uiso D U
H4CA H -0.186161 0.266603 -0.00441 1 0.11804 Uiso D U
H5AA H -0.01764 0.314126 0.055365 1 0.12032 Uiso D U
H5BA H -0.088868 0.307194 0.108726 1 0.12032 Uiso D U
H5CA H 0.064184 0.267055 0.103076 1 0.12032 Uiso D U
H6AA H -0.388953 0.164222 0.079603 1 0.10867 Uiso D U
H6BA H -0.335448 0.1595 0.141712 1 0.10867 Uiso D U
H6CA H -0.338762 0.235959 0.112553 1 0.10867 Uiso D U
H7AA H -0.089068 0.219431 0.167517 1 0.11133 Uiso D U
H7BA H -0.108011 0.133628 0.171271 1 0.1112 Uiso D U
H7CA H 0.02488 0.166382 0.14419 1 0.11133 Uiso D U
H9A H 0.207647 -0.015171 -0.040567 1 0.09702 Uiso D U
N1A N -0.033889 0.175726 0.036849 1 0.10145 Uiso D U
N2A N -0.147133 0.105797 0.080259 1 0.09904 Uiso D U
N3A N 0.106487 0.05953 -0.001531 1 0.0955 Uiso D U
N4A N -0.059759 -0.005576 0.016402 1 0.09334 Uiso D U
O1A O 0.038668 0.199186 0.003608 1 0.10195 Uiso D U
O2A O -0.185093 0.050538 0.100561 1 0.09094 Uiso D U
C1B C 0.176358 0.28514 -0.075084 1 0.11652 Uiso D U
C10B C 0.352516 0.359791 0.03612 1 0.11589 Uiso D U
C2B C 0.048086 0.220135 -0.133656 1 0.12868 Uiso D U
C3B C 0.039381 0.294785 -0.149329 1 0.1321 Uiso D U
C4B C 0.053526 0.163468 -0.169668 1 0.134 Uiso D U
C5B C -0.087192 0.204963 -0.110512 1 0.13818 Uiso D U
C6B C -0.10011 0.326083 -0.167517 1 0.13476 Uiso D U
C7B C 0.131865 0.303175 -0.188949 1 0.14831 Uiso D U
C8B C 0.257454 0.30222 -0.027664 1 0.10854 Uiso D U
C9B C 0.367725 0.290817 0.046435 1 0.11703 Uiso D U
H10B H 0.39058 0.400633 0.060103 1 0.11399 Uiso D U
H4AB H 0.039421 0.116899 -0.152537 1 0.13235 Uiso D U
H4BB H -0.025242 0.17015 -0.199555 1 0.13235 Uiso D U
H4CB H 0.150296 0.163418 -0.182279 1 0.13235 Uiso D U
H5AB H -0.106637 0.244198 -0.086638 1 0.13514 Uiso D U
H5BB H -0.171814 0.199789 -0.138504 1 0.13514 Uiso D U
H5CB H -0.074123 0.1595 -0.090538 1 0.13514 Uiso D U
H6AB H -0.151703 0.337788 -0.137556 1 0.134 Uiso D U
H6BB H -0.085789 0.370793 -0.186908 1 0.134 Uiso D U
H6CB H -0.160041 0.292023 -0.19099 1 0.134 Uiso D U
H7AB H 0.082705 0.282478 -0.222117 1 0.14312 Uiso D U
H7BB H 0.149979 0.354968 -0.194015 1 0.14312 Uiso D U
H7CB H 0.226887 0.278559 -0.178452 1 0.14312 Uiso D U
H9B H 0.420474 0.268914 0.079676 1 0.11424 Uiso D U
N1B N 0.153936 0.221441 -0.09072 1 0.11779 Uiso D U
N2B N 0.110854 0.329197 -0.106393 1 0.12171 Uiso D U
N3B N 0.306906 0.257058 0.007253 1 0.10753 Uiso D U
N4B N 0.281011 0.365819 -0.00944 1 0.10765 Uiso D U
O1B O 0.203158 0.164875 -0.068086 1 0.11804 Uiso D U
O2B O 0.108968 0.395308 -0.102967 1 0.13007 Uiso D U
C1C C 0.463113 0.037024 0.074136 1 0.11576 Uiso D U
C10C C 0.610169 0.051643 -0.03838 1 0.12007 Uiso D U
C2C C 0.349183 0.043806 0.14204 1 0.12095 Uiso D U
C3C C 0.464659 -0.009947 0.149512 1 0.12678 Uiso D U
C4C C 0.347204 0.097458 0.181623 1 0.1321 Uiso D U
C5C C 0.204281 0.010901 0.131943 1 0.12108 Uiso D U
C6C C 0.44008 -0.079021 0.168683 1 0.13716 Uiso D U
C7C C 0.596769 0.017985 0.18206 1 0.13159 Uiso D U
C8C C 0.500927 0.050136 0.025477 1 0.10613 Uiso D U
C9C C 0.499995 0.096152 -0.046581 1 0.11779 Uiso D U
H10C H 0.683708 0.041244 -0.063056 1 0.1188 Uiso D U
H4AC H 0.252202 0.12338 0.17601 1 0.12855 Uiso D U
H4BC H 0.35946 0.074299 0.216358 1 0.12855 Uiso D U
H4CC H 0.42809 0.132121 0.17991 1 0.12855 Uiso D U
H5AC H 0.202741 -0.025319 0.103915 1 0.12108 Uiso D U
H5BC H 0.181226 -0.012659 0.164091 1 0.12108 Uiso D U
H5CC H 0.129732 0.048377 0.121009 1 0.12095 Uiso D U
H6AC H 0.376106 -0.106501 0.141712 1 0.13387 Uiso D U
H6BC H 0.534504 -0.104793 0.177686 1 0.13387 Uiso D U
H6CC H 0.391147 -0.074651 0.200211 1 0.13387 Uiso D U
H7AC H 0.577569 0.023008 0.218508 1 0.13045 Uiso D U
H7BC H 0.680213 -0.015422 0.181149 1 0.13007 Uiso D U
H7CC H 0.622792 0.065508 0.168793 1 0.13007 Uiso D U
H9C H 0.469739 0.124887 -0.079531 1 0.1169 Uiso D U
N1C N 0.37196 0.073445 0.094948 1 0.11614 Uiso D U
N2C N 0.51513 -0.014167 0.102238 1 0.11728 Uiso D U
N3C N 0.432109 0.093992 -0.006998 1 0.11234 Uiso D U
N4C N 0.610695 0.025369 0.006451 1 0.11804 Uiso D U
O1C O 0.303897 0.127951 0.076068 1 0.11817 Uiso D U
O2C O 0.605135 -0.05963 0.094839 1 0.12273 Uiso D U
C1D C 0.679067 -0.132171 0.421308 1 0.18554 Uiso D U
C10D C 0.860227 -0.200392 0.534845 1 0.18871 Uiso D U
C2D C 0.574413 -0.070431 0.355664 1 0.22278 Uiso D U
C3D C 0.560598 -0.147091 0.344511 1 0.20632 Uiso D U
C4D C 0.611643 -0.020396 0.317502 1 0.23519 Uiso D U
C5D C 0.443676 -0.042249 0.371337 1 0.24114 Uiso D U
C6D C 0.674858 -0.165528 0.313821 1 0.2224 Uiso D U
C7D C 0.429512 -0.177987 0.31783 1 0.21645 Uiso D U
C8D C 0.755443 -0.14689 0.470404 1 0.16984 Uiso D U
C9D C 0.866571 -0.131317 0.544102 1 0.18339 Uiso D U
H10D H 0.902025 -0.239827 0.55952 1 0.18719 Uiso D U
H4AD H 0.680346 -0.041997 0.295743 1 0.23203 Uiso D U
H4BD H 0.521098 -0.005827 0.29454 1 0.23114 Uiso D U
H4CD H 0.657386 0.022807 0.335253 1 0.23165 Uiso D U
H5AD H 0.459336 0.00854 0.382016 1 0.23507 Uiso D U
H5BD H 0.362525 -0.045012 0.34185 1 0.23519 Uiso D U
H5CD H 0.416449 -0.070381 0.400933 1 0.23494 Uiso D U
H6AD H 0.684345 -0.218477 0.312618 1 0.21733 Uiso D U
H6BD H 0.648856 -0.147393 0.277774 1 0.21746 Uiso D U
H6CD H 0.769842 -0.144831 0.329822 1 0.21784 Uiso D U
H7AD H 0.442948 -0.230433 0.314295 1 0.21328 Uiso D U
H7BD H 0.347076 -0.169095 0.337804 1 0.21328 Uiso D U
H7CD H 0.406751 -0.156134 0.282767 1 0.21328 Uiso D U
H9D H 0.915019 -0.107505 0.577271 1 0.18212 Uiso D U
N1D N 0.663399 -0.069828 0.402719 1 0.19302 Uiso D U
N2D N 0.616223 -0.178489 0.390545 1 0.19086 Uiso D U
N3D N 0.803093 -0.099668 0.504374 1 0.17288 Uiso D U
N4D N 0.791235 -0.208832 0.489211 1 0.18934 Uiso D U
O1D O 0.711952 -0.013463 0.425463 1 0.19023 Uiso D U
O2D O 0.617043 -0.244298 0.396668 1 0.19846 Uiso D U
C1E C 0.446521 0.043957 0.550736 1 0.21227 Uiso D U
C10E C 0.524909 0.201598 0.494168 1 0.20492 Uiso D U
C2E C 0.420832 -0.064302 0.578072 1 0.23519 Uiso D U
C3E C 0.328362 -0.01487 0.603987 1 0.24013 Uiso D U
C4E C 0.354093 -0.122677 0.546982 1 0.23165 Uiso D U
C5E C 0.536802 -0.096403 0.613245 1 0.25482 Uiso D U
C6E C 0.354733 -0.008791 0.65979 1 0.26141 Uiso D U
C7E C 0.173185 -0.02768 0.59185 1 0.24824 Uiso D U
C8E C 0.499178 0.100874 0.523946 1 0.20644 Uiso D U
C9E C 0.628842 0.160856 0.481411 1 0.21011 Uiso D U
H10E H 0.507492 0.253893 0.484436 1 0.2053 Uiso D U
H4AE H 0.429602 -0.148247 0.530289 1 0.23279 Uiso D U
H4BE H 0.308565 -0.156536 0.569471 1 0.23279 Uiso D U
H4CE H 0.277841 -0.103738 0.519573 1 0.23279 Uiso D U
H5AE H 0.494605 -0.126394 0.638978 1 0.24862 Uiso D U
H5BE H 0.598126 -0.126947 0.593636 1 0.24849 Uiso D U
H5CE H 0.599284 -0.058324 0.631652 1 0.24862 Uiso D U
H6AE H 0.284102 0.025269 0.671891 1 0.25457 Uiso D U
H6BE H 0.343068 -0.056516 0.675645 1 0.25457 Uiso D U
H6CE H 0.455771 0.009093 0.670834 1 0.25457 Uiso D U
H7AE H 0.150559 -0.076861 0.60293 1 0.24558 Uiso D U
H7BE H 0.118558 0.007535 0.610402 1 0.2457 Uiso D U
H7CE H 0.142924 -0.022857 0.553798 1 0.24558 Uiso D U
H9E H 0.708312 0.175424 0.460125 1 0.20809 Uiso D U
N1E N 0.484744 -0.019843 0.546107 1 0.21227 Uiso D U
N2E N 0.359057 0.050638 0.583576 1 0.21657 Uiso D U
N3E N 0.610626 0.099015 0.500219 1 0.20708 Uiso D U
N4E N 0.446722 0.163619 0.519937 1 0.20087 Uiso D U
O1E O 0.567679 -0.044509 0.516948 1 0.21493 Uiso D U
O2E O 0.303466 0.106953 0.597682 1 0.22354 Uiso D U
C1F C 0.965683 0.118105 0.576031 1 0.18567 Uiso D U
C10F C 1.107186 0.101176 0.461583 1 0.18415 Uiso D U
C2F C 0.859165 0.109766 0.645939 1 0.21049 Uiso D U
C3F C 0.955893 0.172812 0.648746 1 0.21632 Uiso D U
C4F C 0.704081 0.125188 0.639379 1 0.21911 Uiso D U
C5F C 0.884141 0.058475 0.687564 1 0.22709 Uiso D U
C6F C 1.082939 0.167236 0.687964 1 0.23367 Uiso D U
C7F C 0.889004 0.241284 0.654432 1 0.23101 Uiso D U
C8F C 1.003598 0.10223 0.526862 1 0.17377 Uiso D U
C9F C 0.996753 0.056465 0.454767 1 0.17858 Uiso D U
H10F H 1.178923 0.111223 0.436215 1 0.1825 Uiso D U
H4AF H 0.647338 0.079875 0.634568 1 0.21632 Uiso D U
H4BF H 0.679239 0.150407 0.670615 1 0.21645 Uiso D U
H4CF H 0.677925 0.155983 0.608288 1 0.21645 Uiso D U
H5AF H 0.878568 0.082839 0.721205 1 0.22189 Uiso D U
H5BF H 0.808683 0.020245 0.682242 1 0.22177 Uiso D U
H5CF H 0.982465 0.036471 0.688256 1 0.22189 Uiso D U
H6AF H 1.146926 0.209635 0.68596 1 0.2281 Uiso D U
H6BF H 1.051663 0.165377 0.722955 1 0.2281 Uiso D U
H6CF H 1.138553 0.123179 0.68206 1 0.2281 Uiso D U
H7AF H 0.965595 0.279062 0.659024 1 0.22633 Uiso D U
H7BF H 0.818399 0.252035 0.622831 1 0.22633 Uiso D U
H7CF H 0.836859 0.240581 0.685304 1 0.22633 Uiso D U
H9F H 0.965451 0.026474 0.42251 1 0.18023 Uiso D U
N1F N 0.882379 0.080227 0.599176 1 0.18554 Uiso D U
N2F N 1.011029 0.172159 0.602201 1 0.19188 Uiso D U
N3F N 0.933343 0.058575 0.494861 1 0.17731 Uiso D U
N4F N 1.109921 0.127801 0.506087 1 0.18301 Uiso D U
O1F O 0.822208 0.02336 0.582993 1 0.17225 Uiso D U
O2F O 1.091482 0.220135 0.589991 1 0.19264 Uiso D U
CM1 C 0.872879 0.23621 0.350452 1 0.39617 Uiso D U
H1M1 H 0.861102 0.23837 0.384604 1 0.39553 Uiso D U
H2M1 H 0.897293 0.280368 0.339517 1 0.39553 Uiso D U
H3M1 H 0.94551 0.204561 0.346406 1 0.39553 Uiso D U
HOM1 H 0.751859 0.224254 0.292973 1 0.39452 Uiso D U
OM1 O 0.74974 0.215011 0.322787 1 0.39401 Uiso D U
CM2 C 0.403746 0.19788 0.327927 1 0.38527 Uiso D U
H1M2 H 0.380601 0.155782 0.342543 1 0.3797 Uiso D U
H2M2 H 0.337882 0.206671 0.299023 1 0.3797 Uiso D U
H3M2 H 0.40053 0.2341 0.351181 1 0.3797 Uiso D U
HOM2 H 0.587863 0.172159 0.336893 1 0.37312 Uiso D U
OM2 O 0.536376 0.193509 0.314951 1 0.3678 Uiso D U
C1T1 C 0.548969 0.099819 -0.206262 1 0.4139 Uiso D U
F1T1 F 0.423807 0.086456 -0.194963 1 0.43024 Uiso D U
F2T1 F 0.643351 0.087009 -0.168355 1 0.4163 Uiso D U
F3T1 F 0.570696 0.062042 -0.244022 1 0.3968 Uiso D U
O1T1 O 0.433783 0.192957 -0.256524 1 0.41719 Uiso D U
O2T1 O 0.684483 0.192153 -0.240013 1 0.43011 Uiso D U
O3T1 O 0.550426 0.217623 -0.174625 1 0.38958 Uiso D U
S1T1 S 0.555405 0.186778 -0.221206 1 0.4068 Uiso D U
C1T2 C 0.983367 -0.043756 0.311343 1 0.41428 Uiso D U
F1T2 F 1.057918 -0.089822 0.338059 1 0.42859 Uiso D U
F2T2 F 0.890386 -0.075203 0.279232 1 0.4258 Uiso D U
F3T2 F 0.914656 -0.007787 0.34021 1 0.43365 Uiso D U
O1T2 O 1.144695 0.05742 0.314696 1 0.39249 Uiso D U
O2T2 O 0.986199 0.032151 0.240049 1 0.39186 Uiso D U
O3T2 O 1.189164 -0.037426 0.266147 1 0.40858 Uiso D U
S1T2 S 1.088312 0.008892 0.279232 1 0.40338 Uiso D U

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
O2A N2A 1.314 . .
N2A C3A 1.482 . .
N2A C1A 1.352 . .
C3A C6A 1.522 . .
C3A C7A 1.548 . .
C3A C2A 1.537 . .
C6A H6CA 1.058 . .
C6A H6BA 1.059 . .
C6A H6AA 1.06 . .
C7A H7CA 1.059 . .
C7A H7BA 1.059 . .
C7A H7AA 1.059 . .
C2A C5A 1.516 . .
C2A C4A 1.542 . .
C2A N1A 1.452 . .
C5A H5CA 1.059 . .
C5A H5BA 1.059 . .
C5A H5AA 1.058 . .
C4A H4CA 1.059 . .
C4A H4BA 1.059 . .
C4A H4AA 1.059 . .
N1A O1A 1.327 . .
N1A C1A 1.325 . .
C1A C8A 1.47 . .
C8A N4A 1.33 . .
C8A N3A 1.351 . .
N4A C10A 1.352 . .
C10A H10A 1.083 . .
C10A C9A 1.373 . .
C9A H9A 1.082 . .
C9A N3A 1.337 . .
O2B N2B 1.32 . .
N2B C3B 1.464 . .
N2B C1B 1.334 . .
C3B C6B 1.525 . .
C3B C7B 1.531 . .
C3B C2B 1.547 . .
C6B H6CB 1.059 . .
C6B H6BB 1.059 . .
C6B H6AB 1.059 . .
C7B H7CB 1.059 . .
C7B H7AB 1.059 . .
C2B C5B 1.585 . .
C2B C4B 1.512 . .
C2B N1B 1.466 . .
C5B H5CB 1.059 . .
C5B H5BB 1.059 . .
C5B H5AB 1.058 . .
C4B H4CB 1.059 . .
C4B H4BB 1.059 . .
C4B H4AB 1.06 . .
N1B O1B 1.345 . .
N1B C1B 1.348 . .
C1B C8B 1.477 . .
C8B N4B 1.371 . .
C8B N3B 1.359 . .
N4B C10B 1.361 . .
C10B H10B 1.083 . .
C10B C9B 1.406 . .
C9B H9B 1.083 . .
C9B N3B 1.343 . .
O2C N2C 1.302 . .
N2C C3C 1.468 . .
N2C C1C 1.339 . .
C3C C6C 1.506 . .
C3C C7C 1.574 . .
C3C C2C 1.552 . .
C6C H6CC 1.059 . .
C6C H6BC 1.059 . .
C6C H6AC 1.058 . .
C7C H7CC 1.059 . .
C7C H7BC 1.059 . .
C7C H7AC 1.058 . .
C2C C5C 1.557 . .
C2C C4C 1.533 . .
C2C N1C 1.478 . .
C5C H5CC 1.06 . .
C5C H5BC 1.059 . .
C5C H5AC 1.058 . .
C4C H4BC 1.059 . .
C4C H4AC 1.059 . .
N1C O1C 1.341 . .
N1C C1C 1.345 . .
C1C C8C 1.472 . .
C8C N4C 1.359 . .
C8C N3C 1.363 . .
N4C C10C 1.347 . .
C10C H10C 1.083 . .
C10C C9C 1.393 . .
C9C H9C 1.083 . .
C9C N3C 1.363 . .
O2D N2D 1.321 . .
N2D C3D 1.456 . .
N2D C1D 1.345 . .
C3D C6D 1.546 . .
C3D C7D 1.522 . .
C3D C2D 1.559 . .
C6D H6CD 1.059 . .
C6D H6BD 1.059 . .
C6D H6AD 1.059 . .
C7D H7CD 1.059 . .
C7D H7BD 1.059 . .
C7D H7AD 1.059 . .
C2D C5D 1.521 . .
C2D C4D 1.534 . .
C2D N1D 1.464 . .
C5D H5CD 1.058 . .
C5D H5BD 1.06 . .
C5D H5AD 1.059 . .
C4D H4CD 1.059 . .
C4D H4BD 1.059 . .
C4D H4AD 1.059 . .
N1D O1D 1.341 . .
N1D C1D 1.344 . .
C1D C8D 1.487 . .
C8D N4D 1.365 . .
C8D N3D 1.365 . .
N4D C10D 1.358 . .
C10D H10D 1.083 . .
C10D C9D 1.399 . .
C9D H9D 1.083 . .
C9D N3D 1.343 . .
O2E N2E 1.33 . .
N2E C3E 1.47 . .
N2E C1E 1.344 . .
C3E C6E 1.536 . .
C3E C7E 1.536 . .
C3E C2E 1.58 . .
C6E H6CE 1.059 . .
C6E H6BE 1.06 . .
C6E H6AE 1.059 . .
C7E H7CE 1.059 . .
C7E H7BE 1.06 . .
C7E H7AE 1.059 . .
C2E C5E 1.531 . .
C2E C4E 1.537 . .
C2E N1E 1.456 . .
C5E H5CE 1.06 . .
C5E H5AE 1.059 . .
C4E H4CE 1.058 . .
C4E H4BE 1.059 . .
C4E H4AE 1.059 . .
N1E O1E 1.321 . .
N1E C1E 1.336 . .
C1E C8E 1.487 . .
C8E N4E 1.35 . .
C8E N3E 1.356 . .
N4E C10E 1.352 . .
C10E H10E 1.083 . .
C10E C9E 1.389 . .
C9E H9E 1.083 . .
C9E N3E 1.359 . .
O2F N2F 1.315 . .
N2F C3F 1.469 . .
N2F C1F 1.338 . .
C3F C6F 1.539 . .
C3F C7F 1.531 . .
C3F C2F 1.57 . .
C6F H6CF 1.058 . .
C6F H6BF 1.059 . .
C6F H6AF 1.059 . .
C7F H7CF 1.058 . .
C7F H7BF 1.059 . .
C7F H7AF 1.059 . .
C2F C5F 1.534 . .
C2F C4F 1.541 . .
C2F N1F 1.47 . .
C5F H5BF 1.058 . .
C5F H5AF 1.059 . .
C4F H4CF 1.059 . .
C4F H4BF 1.059 . .
C4F H4AF 1.059 . .
N1F O1F 1.326 . .
N1F C1F 1.342 . .
C1F C8F 1.497 . .
C8F N4F 1.362 . .
C8F N3F 1.358 . .
N4F C10F 1.339 . .
C10F H10F 1.083 . .
C10F C9F 1.396 . .
C9F H9F 1.083 . .
C9F N3F 1.35 . .
F3T1 C1T1 1.33 . .
C1T1 F1T1 1.339 . .
C1T1 F2T1 1.324 . .
C1T1 S1T1 1.783 . .
S1T1 O1T1 1.439 . .
S1T1 O2T1 1.443 . .
S1T1 O3T1 1.437 . .
F3T2 C1T2 1.328 . .
C1T2 F1T2 1.331 . .
C1T2 F2T2 1.338 . .
C1T2 S1T2 1.793 . .
S1T2 O1T2 1.433 . .
S1T2 O2T2 1.447 . .
S1T2 O3T2 1.438 . .
CM1 OM1 1.403 . .
CM1 H1M1 0.971 . .
CM1 H2M1 0.971 . .
CM1 H3M1 0.971 . .
OM1 HOM1 0.85 . .
CM2 OM2 1.404 . .
CM2 H1M2 0.972 . .
CM2 H2M2 0.972 . .
CM2 H3M2 0.971 . .
OM2 HOM2 0.848 . .


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_2
_geom_angle_site_symmetry_3
O2A ? C3A 122.15 . . .
O2A ? C1A 128.37 . . .
N2A ? C6A 113.7 . . .
N2A ? C7A 102.18 . . .
N2A ? C2A 102.63 . . .
N2A ? N1A 113.37 . . .
N2A ? C8A 124.43 . . .
C3A ? C1A 108.45 . . .
C3A ? H6CA 109.55 . . .
C3A ? H6BA 109.84 . . .
C3A ? H6AA 109.72 . . .
C3A ? H7CA 110.01 . . .
C3A ? H7BA 109.62 . . .
C3A ? H7AA 109.7 . . .
C3A ? C5A 118.54 . . .
C3A ? C4A 108.74 . . .
C3A ? N1A 104.14 . . .
C6A ? C7A 107.94 . . .
C6A ? C2A 119.41 . . .
H6CA ? H6BA 108.8 . . .
H6CA ? H6AA 109.43 . . .
H6BA ? H6AA 109.49 . . .
C7A ? C2A 109.61 . . .
H7CA ? H7BA 109.03 . . .
H7CA ? H7AA 109.59 . . .
H7BA ? H7AA 108.87 . . .
C2A ? H5CA 109.78 . . .
C2A ? H5BA 109.68 . . .
C2A ? H5AA 109.23 . . .
C2A ? H4CA 109.6 . . .
C2A ? H4BA 109.84 . . .
C2A ? H4AA 110.09 . . .
C2A ? O1A 121.46 . . .
C2A ? C1A 109.76 . . .
C5A ? C4A 108.26 . . .
C5A ? N1A 113.84 . . .
H5CA ? H5BA 109.59 . . .
H5CA ? H5AA 109 . . .
H5BA ? H5AA 109.54 . . .
C4A ? N1A 101.99 . . .
H4CA ? H4BA 108.69 . . .
H4CA ? H4AA 109.05 . . .
H4BA ? H4AA 109.55 . . .
N1A ? C8A 122.17 . . .
O1A ? C1A 128.29 . . .
C1A ? N4A 125.63 . . .
C1A ? N3A 124.27 . . .
C8A ? C10A 106.53 . . .
C8A ? C9A 107.64 . . .
N4A ? N3A 110.09 . . .
N4A ? H10A 125.44 . . .
N4A ? C9A 108.61 . . .
C10A ? H9A 126.46 . . .
C10A ? N3A 107.07 . . .
H10A ? C9A 125.86 . . .
H9A ? N3A 126.45 . . .
O2B ? C3B 121.01 . . .
O2B ? C1B 128.27 . . .
N2B ? C6B 112.52 . . .
N2B ? C7B 105.46 . . .
N2B ? C2B 102.72 . . .
N2B ? N1B 111.56 . . .
N2B ? C8B 125.28 . . .
C3B ? C1B 110.68 . . .
C3B ? H6CB 109.72 . . .
C3B ? H6BB 109.44 . . .
C3B ? H6AB 109.82 . . .
C3B ? H7CB 110.07 . . .
C3B ? H7BB 109.24 . . .
C3B ? H7AB 109.61 . . .
C3B ? C5B 106.28 . . .
C3B ? C4B 122.47 . . .
C3B ? N1B 102.45 . . .
C6B ? C7B 108.42 . . .
C6B ? C2B 119.76 . . .
H6CB ? H6BB 109.19 . . .
H6CB ? H6AB 109.64 . . .
H6BB ? H6AB 109.03 . . .
C7B ? C2B 106.94 . . .
H7CB ? H7BB 109.19 . . .
H7CB ? H7AB 109.56 . . .
H7BB ? H7AB 109.16 . . .
C2B ? H5CB 109.13 . . .
C2B ? H5BB 109.82 . . .
C2B ? H5AB 110.4 . . .
C2B ? H4CB 109.64 . . .
C2B ? H4BB 109.4 . . .
C2B ? H4AB 109.74 . . .
C2B ? O1B 122.06 . . .
C2B ? C1B 110.04 . . .
C5B ? C4B 103.6 . . .
C5B ? N1B 102.4 . . .
H5CB ? H5BB 108.92 . . .
H5CB ? H5AB 108.85 . . .
H5BB ? H5AB 109.69 . . .
C4B ? N1B 117.49 . . .
H4CB ? H4BB 109.48 . . .
H4CB ? H4AB 109.14 . . .
H4BB ? H4AB 109.43 . . .
N1B ? C8B 123.07 . . .
O1B ? C1B 127.29 . . .
C1B ? N4B 125.61 . . .
C1B ? N3B 125.08 . . .
C8B ? C10B 107.38 . . .
C8B ? C9B 108.54 . . .
N4B ? N3B 108.89 . . .
N4B ? H10B 126.27 . . .
N4B ? C9B 107.51 . . .
C10B ? H9B 126.19 . . .
C10B ? N3B 107.57 . . .
H10B ? C9B 126.22 . . .
H9B ? N3B 126.23 . . .
O2C ? C3C 120.24 . . .
O2C ? C1C 130.48 . . .
N2C ? C6C 110.74 . . .
N2C ? C7C 100.13 . . .
N2C ? C2C 104.7 . . .
N2C ? N1C 112.55 . . .
N2C ? C8C 122.85 . . .
C3C ? C1C 109.03 . . .
C3C ? H6CC 109.3 . . .
C3C ? H6BC 110.26 . . .
C3C ? H6AC 109.37 . . .
C3C ? H7CC 109.68 . . .
C3C ? H7BC 110.1 . . .
C3C ? H7AC 109.63 . . .
C3C ? C5C 111.55 . . .
C3C ? C4C 117.9 . . .
C3C ? N1C 101.15 . . .
C6C ? C7C 106.32 . . .
C6C ? C2C 121.7 . . .
H6CC ? H6BC 109.33 . . .
H6CC ? H6AC 109.34 . . .
H6BC ? H6AC 109.23 . . .
C7C ? C2C 111.19 . . .
H7CC ? H7BC 109.05 . . .
H7CC ? H7AC 109.36 . . .
H7BC ? H7AC 109.01 . . .
C2C ? H5CC 109.48 . . .
C2C ? H5BC 109.54 . . .
C2C ? H5AC 109.63 . . .
C2C ? H4CC 109.63 . . .
C2C ? H4BC 109.63 . . .
C2C ? H4AC 109.55 . . .
C2C ? O1C 122.52 . . .
C2C ? C1C 110.93 . . .
C5C ? C4C 108.51 . . .
C5C ? N1C 104.99 . . .
H5CC ? H5BC 109.29 . . .
H5CC ? H5AC 109.41 . . .
H5BC ? H5AC 109.46 . . .
C4C ? N1C 111.88 . . .
H4CC ? H4BC 109.58 . . .
H4CC ? H4AC 109.16 . . .
H4BC ? H4AC 109.27 . . .
N1C ? C8C 124.58 . . .
O1C ? C1C 126.49 . . .
C1C ? N4C 127.49 . . .
C1C ? N3C 123.53 . . .
C8C ? C10C 108.51 . . .
C8C ? C9C 107.33 . . .
N4C ? N3C 108.86 . . .
N4C ? H10C 126.32 . . .
N4C ? C9C 107.37 . . .
C10C ? H9C 126.01 . . .
C10C ? N3C 107.86 . . .
H10C ? C9C 126.28 . . .
H9C ? N3C 126.02 . . .
O2D ? C3D 122.21 . . .
O2D ? C1D 127.19 . . .
N2D ? C6D 99.69 . . .
N2D ? C7D 116.06 . . .
N2D ? C2D 103.6 . . .
N2D ? N1D 111.87 . . .
N2D ? C8D 124.88 . . .
C3D ? C1D 110.06 . . .
C3D ? H6CD 110.1 . . .
C3D ? H6BD 109.94 . . .
C3D ? H6AD 109.12 . . .
C3D ? H7CD 109.51 . . .
C3D ? H7BD 109.67 . . .
C3D ? H7AD 109.59 . . .
C3D ? C5D 111.36 . . .
C3D ? C4D 121.42 . . .
C3D ? N1D 102.06 . . .
C6D ? C7D 105.55 . . .
C6D ? C2D 106.96 . . .
H6CD ? H6BD 110.07 . . .
H6CD ? H6AD 108.91 . . .
H6BD ? H6AD 108.67 . . .
C7D ? C2D 122.4 . . .
H7CD ? H7BD 109.46 . . .
H7CD ? H7AD 109.45 . . .
H7BD ? H7AD 109.14 . . .
C2D ? H5CD 110.06 . . .
C2D ? H5BD 109.57 . . .
C2D ? H5AD 109.68 . . .
C2D ? H4CD 109.52 . . .
C2D ? H4BD 109.25 . . .
C2D ? H4AD 111.28 . . .
C2D ? O1D 123.61 . . .
C2D ? C1D 110.82 . . .
C5D ? C4D 104.55 . . .
C5D ? N1D 99.5 . . .
H5CD ? H5BD 108.95 . . .
H5CD ? H5AD 109.35 . . .
H5BD ? H5AD 109.21 . . .
C4D ? N1D 115.97 . . .
H4CD ? H4BD 108.81 . . .
H4CD ? H4AD 109.35 . . .
H4BD ? H4AD 108.6 . . .
O1D ? C1D 125.34 . . .
C1D ? N4D 126.63 . . .
C1D ? N3D 125.08 . . .
C8D ? C10D 108.15 . . .
C8D ? C9D 108.45 . . .
N4D ? N3D 108.29 . . .
N4D ? H10D 126.37 . . .
N4D ? C9D 107.21 . . .
C10D ? H9D 126.08 . . .
C10D ? N3D 107.9 . . .
H10D ? C9D 126.42 . . .
H9D ? N3D 126.02 . . .
O2E ? C3E 121.29 . . .
O2E ? C1E 127.69 . . .
N2E ? C6E 107.64 . . .
N2E ? C7E 108.34 . . .
N2E ? C2E 102.4 . . .
N2E ? N1E 112.01 . . .
N2E ? C8E 124.33 . . .
C3E ? C1E 111.03 . . .
C3E ? H6CE 109.57 . . .
C3E ? H6BE 109.52 . . .
C3E ? H6AE 110.17 . . .
C3E ? H7CE 109.46 . . .
C3E ? H7BE 109.87 . . .
C3E ? H7AE 109.44 . . .
C3E ? C5E 113.28 . . .
C3E ? C4E 119.88 . . .
C3E ? N1E 102.93 . . .
C6E ? C7E 104.72 . . .
C6E ? C2E 118.74 . . .
H6CE ? H6BE 109.5 . . .
H6CE ? H6AE 108.89 . . .
H6BE ? H6AE 109.17 . . .
C7E ? C2E 114.5 . . .
H7CE ? H7BE 109.46 . . .
H7CE ? H7AE 109.37 . . .
H7BE ? H7AE 109.21 . . .
C2E ? H5CE 109.67 . . .
C2E ? H5BE 109.86 . . .
C2E ? H5AE 109.68 . . .
C2E ? H4CE 109.62 . . .
C2E ? H4BE 109.48 . . .
C2E ? H4AE 109.77 . . .
C2E ? O1E 120.21 . . .
C2E ? C1E 111.58 . . .
C5E ? C4E 105.17 . . .
C5E ? N1E 107.12 . . .
H5CE ? H5BE 108.92 . . .
H5CE ? H5AE 109.56 . . .
H5BE ? H5AE 109.14 . . .
C4E ? N1E 107.76 . . .
H4CE ? H4BE 109.49 . . .
H4CE ? H4AE 109.07 . . .
H4BE ? H4AE 109.4 . . .
N1E ? C8E 123.62 . . .
O1E ? C1E 128.2 . . .
C1E ? N4E 126.16 . . .
C1E ? N3E 125.71 . . .
C8E ? C10E 108.76 . . .
C8E ? C9E 108.72 . . .
N4E ? N3E 108.11 . . .
N4E ? H10E 125.97 . . .
N4E ? C9E 107.57 . . .
C10E ? H9E 126.57 . . .
C10E ? N3E 106.84 . . .
H10E ? C9E 126.44 . . .
H9E ? N3E 126.59 . . .
O2F ? C3F 122.02 . . .
O2F ? C1F 127.66 . . .
N2F ? C6F 104.84 . . .
N2F ? C7F 108.4 . . .
N2F ? C2F 104.23 . . .
N2F ? N1F 111.83 . . .
N2F ? C8F 123.81 . . .
C3F ? C1F 110.31 . . .
C3F ? H6CF 109.63 . . .
C3F ? H6BF 109.72 . . .
C3F ? H6AF 109.52 . . .
C3F ? H7CF 109.63 . . .
C3F ? H7BF 109.6 . . .
C3F ? H7AF 109.63 . . .
C3F ? C5F 117.62 . . .
C3F ? C4F 115.4 . . .
C3F ? N1F 101.23 . . .
C6F ? C7F 107.99 . . .
C6F ? C2F 113.74 . . .
H6CF ? H6BF 109.64 . . .
H6CF ? H6AF 109.18 . . .
H6BF ? H6AF 109.14 . . .
C7F ? C2F 116.79 . . .
H7CF ? H7BF 109.6 . . .
H7CF ? H7AF 109.27 . . .
H7BF ? H7AF 109.11 . . .
C2F ? H5CF 109.71 . . .
C2F ? H5BF 109.84 . . .
C2F ? H5AF 109.54 . . .
C2F ? H4CF 109.48 . . .
C2F ? H4BF 109.7 . . .
C2F ? H4AF 109.88 . . .
C2F ? O1F 121.48 . . .
C2F ? C1F 112.23 . . .
C5F ? C4F 105.76 . . .
C5F ? N1F 111.62 . . .
H5CF ? H5BF 108.98 . . .
H5CF ? H5AF 109.54 . . .
H5BF ? H5AF 109.22 . . .
C4F ? N1F 104.5 . . .
H4CF ? H4AF 109.13 . . .
H4BF ? H4AF 109.16 . . .
N1F ? C8F 124.37 . . .
O1F ? C1F 126.27 . . .
C1F ? N4F 127.69 . . .
C1F ? N3F 124.08 . . .
C8F ? C10F 108.98 . . .
C8F ? C9F 107.82 . . .
N4F ? N3F 108.23 . . .
N4F ? H10F 126.52 . . .
N4F ? C9F 106.89 . . .
C10F ? H9F 126 . . .
C10F ? N3F 108.06 . . .
H10F ? C9F 126.56 . . .
H9F ? N3F 125.91 . . .
F3T1 ? F1T1 109.1 . . .
F3T1 ? F2T1 110.04 . . .
F3T1 ? S1T1 110.55 . . .
C1T1 ? O1T1 100.81 . . .
C1T1 ? O2T1 102.59 . . .
C1T1 ? O3T1 101.5 . . .
F1T1 ? F2T1 109.88 . . .
F1T1 ? S1T1 108.14 . . .
F2T1 ? S1T1 109.1 . . .
O1T1 ? O2T1 115.88 . . .
O1T1 ? O3T1 116.35 . . .
O2T1 ? O3T1 115.9 . . .
F3T2 ? F1T2 108.87 . . .
F3T2 ? F2T2 107.17 . . .
F3T2 ? S1T2 111.2 . . .
C1T2 ? O1T2 104.33 . . .
C1T2 ? O2T2 99.95 . . .
C1T2 ? O3T2 102.5 . . .
F1T2 ? F2T2 108.55 . . .
F1T2 ? S1T2 111.62 . . .
F2T2 ? S1T2 109.29 . . .
O1T2 ? O2T2 117.33 . . .
O1T2 ? O3T2 113.07 . . .
O2T2 ? O3T2 116.49 . . .
CM1 ? HOM1 109.15 . . .
OM1 ? H1M1 109.46 . . .
OM1 ? H2M1 109.52 . . .
OM1 ? H3M1 109.49 . . .
H1M1 ? H2M1 109.46 . . .
H1M1 ? H3M1 109.44 . . .
H2M1 ? H3M1 109.45 . . .
CM2 ? HOM2 109.21 . . .
OM2 ? H1M2 109.53 . . .
OM2 ? H2M2 109.55 . . .
OM2 ? H3M2 109.58 . . .
H1M2 ? H2M2 109.32 . . .
H1M2 ? H3M2 109.4 . . .
H2M2 ? H3M2 109.45 . . .
















_exptl_crystal_recrystallization_method 'Crystallization upon mixing reactants'
_exptl_crystal_preparation       'Magnetic properties'
