# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_Fe3L3-FeCl3
_database_code_depnum_ccdc_archive 'CCDC 1443923'
_audit_update_record             
;
2016-02-09 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C75 H66 Cl2.80 Fe4 Mn0 N12 O14'
_chemical_formula_weight         1682.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.398(3)
_cell_length_b                   33.496(7)
_cell_length_c                   12.868(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.64(3)
_cell_angle_gamma                90
_cell_volume                     5308.0(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9937
_cell_measurement_theta_min      0.83
_cell_measurement_theta_max      33.51

_exptl_crystal_description       Rod
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_F_000             1727
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.658
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.8832
_exptl_absorpt_correction_T_max  0.9391
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            71745
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.216
_diffrn_reflns_theta_max         25.391
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.841
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.841
_reflns_number_total             9914
_reflns_number_gt                7322
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9914
_refine_ls_number_parameters     539
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.1077
_refine_ls_wR_factor_ref         0.3279
_refine_ls_wR_factor_gt          0.3112
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_restrained_S_all      1.331
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.69786(6) 0.06952(2) 0.60443(5) 0.0402(3) Uani 1 1 d . . . . .
Fe2 Fe 0.5000 0.0000 0.5000 0.0444(3) Uani 1 2 d S . P . .
Fe3 Fe 1.21931(12) -0.2500 0.69427(15) 0.0732(5) Uani 1 2 d DS T P . .
Cl1 Cl 1.0963(6) -0.2500 0.4944(2) 0.171(3) Uani 1 2 d DS T P . .
Cl2 Cl 1.3502(3) -0.2500 0.8504(6) 0.157(2) Uani 1 2 d S T P . .
O1 O 1.3474(11) -0.2043(3) 0.6403(16) 0.260(8) Uani 1 1 d . . . . .
Cl3 Cl 0.7330(12) -0.2500 0.6553(12) 0.153(5) Uiso 0.4 2 d S . P . .
Cl4 Cl 0.8323(17) 0.2500 0.8333(17) 0.206(7) Uiso 0.4 2 d S . P . .
C1 C 0.7915(5) 0.15021(16) 0.7326(4) 0.0446(12) Uani 1 1 d . . . . .
H1A H 0.7317 0.1567 0.6773 0.054 Uiso 1 1 calc R U . . .
H1B H 0.8164 0.1754 0.7679 0.054 Uiso 1 1 calc R U . . .
C2 C 1.0698(10) -0.2500 0.8792(10) 0.083(3) Uani 1 2 d S T P . .
H2A H 1.0225 -0.2500 0.9361 0.100 Uiso 1 2 calc R U P . .
H2B H 1.1463 -0.2500 0.9113 0.100 Uiso 1 2 calc R U P . .
N11 N 0.6965(4) 0.08985(14) 0.7717(3) 0.0449(10) Uani 1 1 d . . . . .
N12 N 0.7515(4) 0.12308(13) 0.8087(3) 0.0439(10) Uani 1 1 d . . . . .
C13 C 0.7580(5) 0.1256(2) 0.9125(4) 0.0564(15) Uani 1 1 d . . . . .
C14 C 0.7039(6) 0.0934(2) 0.9468(4) 0.0596(17) Uani 1 1 d . . . . .
C15 C 0.6673(5) 0.07123(18) 0.8563(4) 0.0494(14) Uani 1 1 d . . . . .
C16 C 0.6067(7) 0.0328(2) 0.8467(5) 0.073(2) Uani 1 1 d . . . . .
H16A H 0.5561 0.0330 0.7823 0.109 Uiso 1 1 calc R U . . .
H16B H 0.5660 0.0295 0.9070 0.109 Uiso 1 1 calc R U . . .
H16C H 0.6581 0.0107 0.8444 0.109 Uiso 1 1 calc R U . . .
C17 C 0.8162(9) 0.1603(3) 0.9720(6) 0.099(3) Uani 1 1 d . . . . .
H17A H 0.7933 0.1855 0.9377 0.149 Uiso 1 1 calc R U . . .
H17B H 0.8949 0.1571 0.9725 0.149 Uiso 1 1 calc R U . . .
H17C H 0.7980 0.1605 1.0441 0.149 Uiso 1 1 calc R U . . .
C18 C 0.6908(6) 0.0832(2) 1.0565(4) 0.0593(16) Uani 1 1 d . . . . .
C19 C 0.6785(13) 0.1111(4) 1.1281(7) 0.083(4) Uani 0.65 1 d . . P A 1
H19 H 0.6792 0.1384 1.1076 0.099 Uiso 0.65 1 calc R U P A 1
C19A C 0.7643(14) 0.0897(8) 1.1289(12) 0.063(5) Uani 0.35 1 d . . P A 2
H19A H 0.8279 0.1037 1.1155 0.075 Uiso 0.35 1 calc R U P A 2
C20 C 0.6646(16) 0.1023(4) 1.2317(8) 0.105(6) Uani 0.65 1 d . . P A 1
H20 H 0.6552 0.1231 1.2801 0.126 Uiso 0.65 1 calc R U P A 1
C20A C 0.7530(15) 0.0764(8) 1.2296(15) 0.070(6) Uani 0.35 1 d . . P A 2
H20A H 0.8161 0.0774 1.2791 0.084 Uiso 0.35 1 calc R U P A 2
C21 C 0.6646(5) 0.06257(19) 1.2630(4) 0.0516(14) Uani 1 1 d . . . . .
C22 C 0.6865(9) 0.0334(3) 1.1979(7) 0.059(2) Uani 0.65 1 d . . P A 1
H22 H 0.6907 0.0065 1.2217 0.071 Uiso 0.65 1 calc R U P A 1
C22A C 0.5677(14) 0.0595(6) 1.1791(11) 0.056(5) Uani 0.35 1 d . . P A 2
H22A H 0.4998 0.0502 1.1968 0.067 Uiso 0.35 1 calc R U P A 2
C23 C 0.7033(9) 0.0423(3) 1.0940(7) 0.063(3) Uani 0.65 1 d . . P A 1
H23 H 0.7228 0.0218 1.0488 0.076 Uiso 0.65 1 calc R U P A 1
C23A C 0.5790(15) 0.0705(5) 1.0756(11) 0.054(5) Uani 0.35 1 d . . P A 2
H23A H 0.5200 0.0698 1.0216 0.064 Uiso 0.35 1 calc R U P A 2
C24 C 0.6513(5) 0.05323(19) 1.3735(5) 0.0506(13) Uani 1 1 d . . . . .
O25 O 0.6950(4) 0.07557(18) 1.4431(3) 0.0765(16) Uani 1 1 d . . . . .
O26 O 0.6024(5) 0.02273(16) 1.3932(4) 0.0891(18) Uani 1 1 d . . . . .
N31 N 0.8581(4) 0.10005(14) 0.6237(3) 0.0441(10) Uani 1 1 d . . . . .
N32 N 0.8808(3) 0.13215(14) 0.6853(3) 0.0428(10) Uani 1 1 d . . . . .
C33 C 0.9869(5) 0.14015(19) 0.6991(5) 0.0515(14) Uani 1 1 d . . . . .
C34 C 1.0371(5) 0.1120(2) 0.6430(5) 0.0540(14) Uani 1 1 d . . . . .
C35 C 0.9518(5) 0.08719(19) 0.5977(5) 0.0515(14) Uani 1 1 d . . . . .
C36 C 1.0350(6) 0.1749(2) 0.7622(7) 0.079(2) Uani 1 1 d . . . . .
H36A H 1.1112 0.1782 0.7502 0.118 Uiso 1 1 calc R U . . .
H36B H 1.0309 0.1699 0.8366 0.118 Uiso 1 1 calc R U . . .
H36C H 0.9945 0.1992 0.7408 0.118 Uiso 1 1 calc R U . . .
C37 C 0.9601(6) 0.0521(2) 0.5284(6) 0.0679(19) Uani 1 1 d . . . . .
H37A H 0.9689 0.0278 0.5708 0.102 Uiso 1 1 calc R U . . .
H37B H 1.0230 0.0554 0.4895 0.102 Uiso 1 1 calc R U . . .
H37C H 0.8939 0.0501 0.4791 0.102 Uiso 1 1 calc R U . . .
C38 C 1.1523(5) 0.1080(2) 0.6314(6) 0.0607(16) Uani 1 1 d . . . . .
C39 C 1.2122(5) 0.1396(2) 0.6017(6) 0.0700(19) Uani 1 1 d . . . . .
H39 H 1.1791 0.1650 0.5884 0.084 Uiso 1 1 calc R U . . .
C40 C 1.3232(5) 0.1343(2) 0.5910(7) 0.0710(19) Uani 1 1 d . . . . .
H40 H 1.3648 0.1564 0.5722 0.085 Uiso 1 1 calc R U . . .
C41 C 1.3718(5) 0.0981(2) 0.6069(5) 0.0556(15) Uani 1 1 d . . . . .
C42 C 1.3105(5) 0.0656(2) 0.6361(6) 0.0603(16) Uani 1 1 d . . . . .
H42 H 1.3430 0.0400 0.6464 0.072 Uiso 1 1 calc R U . . .
C43 C 1.2028(5) 0.0711(2) 0.6498(6) 0.0632(17) Uani 1 1 d . . . . .
H43 H 1.1622 0.0493 0.6722 0.076 Uiso 1 1 calc R U . . .
C44 C 1.4885(5) 0.09141(19) 0.5951(5) 0.0512(13) Uani 1 1 d . . . . .
O45 O 1.5254(3) 0.05596(12) 0.5947(3) 0.0463(9) Uani 1 1 d . . . . .
O46 O 1.5508(3) 0.12109(14) 0.5892(4) 0.0660(12) Uani 1 1 d . . . . .
N51 N 1.1132(6) -0.20609(19) 0.7358(7) 0.088(2) Uani 1 1 d . . . . .
N52 N 1.0490(6) -0.21490(15) 0.8160(6) 0.081(2) Uani 1 1 d . . . . .
C53 C 0.9745(7) -0.1863(2) 0.8226(6) 0.074(2) Uani 1 1 d . . . . .
C54 C 0.9878(7) -0.1583(2) 0.7492(6) 0.075(2) Uani 1 1 d . . . . .
C55 C 1.0747(7) -0.1720(2) 0.6935(8) 0.084(2) Uani 1 1 d . . . . .
C56 C 1.1120(10) -0.1518(3) 0.6049(9) 0.122(4) Uani 1 1 d . . . . .
H56A H 1.1780 -0.1367 0.6282 0.183 Uiso 1 1 calc R U . . .
H56B H 1.0555 -0.1336 0.5740 0.183 Uiso 1 1 calc R U . . .
H56C H 1.1278 -0.1716 0.5526 0.183 Uiso 1 1 calc R U . . .
C57 C 0.8917(8) -0.1874(2) 0.9006(8) 0.093(3) Uani 1 1 d . . . . .
H57A H 0.8534 -0.1618 0.8995 0.140 Uiso 1 1 calc R U . . .
H57B H 0.9289 -0.1923 0.9709 0.140 Uiso 1 1 calc R U . . .
H57C H 0.8394 -0.2089 0.8817 0.140 Uiso 1 1 calc R U . . .
C58 C 0.9208(7) -0.1227(2) 0.7242(6) 0.079(2) Uani 1 1 d . . . . .
C59 C 0.8090(9) -0.1266(3) 0.6881(9) 0.117(4) Uani 1 1 d . . . . .
H59 H 0.7757 -0.1522 0.6828 0.140 Uiso 1 1 calc R U . . .
C60 C 0.7475(8) -0.0919(2) 0.6601(8) 0.092(3) Uani 1 1 d . . . . .
H60 H 0.6731 -0.0943 0.6335 0.110 Uiso 1 1 calc R U . . .
C61 C 0.7929(6) -0.05533(19) 0.6707(5) 0.0593(16) Uani 1 1 d . . . . .
C62 C 0.8962(7) -0.0512(2) 0.7136(6) 0.076(2) Uani 1 1 d . . . . .
H62 H 0.9257 -0.0252 0.7254 0.091 Uiso 1 1 calc R U . . .
C63 C 0.9608(8) -0.0844(2) 0.7413(7) 0.086(3) Uani 1 1 d . . . . .
H63 H 1.0335 -0.0807 0.7723 0.103 Uiso 1 1 calc R U . . .
C64 C 0.7249(5) -0.01978(18) 0.6335(4) 0.0515(14) Uani 1 1 d . . . . .
O65 O 0.6291(4) -0.02599(15) 0.5957(4) 0.0789(15) Uani 1 1 d . . . . .
O66 O 0.7650(4) 0.01371(13) 0.6463(3) 0.0577(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O25 2.082(4) 1_554 ?
Fe1 O66 2.091(4) . ?
Fe1 O45 2.175(4) 1_455 ?
Fe1 N31 2.223(5) . ?
Fe1 N11 2.260(4) . ?
Fe2 O65 2.093(5) . ?
Fe2 O65 2.093(5) 3_656 ?
Fe2 O26 2.118(5) 1_554 ?
Fe2 O26 2.118(5) 3_657 ?
Fe2 O45 2.238(4) 1_455 ?
Fe2 O45 2.238(4) 3_756 ?
Fe3 N51 2.084(8) 4 ?
Fe3 N51 2.084(8) . ?
Fe3 O1 2.367(15) . ?
Fe3 O1 2.367(15) 4 ?
Fe3 Cl2 2.433(6) . ?
C1 N32 1.456(7) . ?
C1 N12 1.464(7) . ?
C2 N52 1.436(9) . ?
C2 N52 1.436(9) 4 ?
N11 C15 1.340(7) . ?
N11 N12 1.362(6) . ?
N12 C13 1.332(7) . ?
C13 C14 1.371(9) . ?
C13 C17 1.525(9) . ?
C14 C15 1.410(8) . ?
C14 C18 1.479(7) . ?
C15 C16 1.488(8) . ?
C18 C19A 1.245(18) . ?
C18 C19 1.334(14) . ?
C18 C23 1.456(12) . ?
C18 C23A 1.498(18) . ?
C19 C20 1.396(13) . ?
C19A C20A 1.39(3) . ?
C20 C21 1.390(15) . ?
C20A C21 1.31(2) . ?
C21 C22 1.336(12) . ?
C21 C24 1.484(8) . ?
C21 C22A 1.523(17) . ?
C22 C23 1.408(12) . ?
C22A C23A 1.40(2) . ?
C24 O26 1.229(8) . ?
C24 O25 1.242(8) . ?
O25 Fe1 2.082(4) 1_556 ?
O26 Fe2 2.118(5) 1_556 ?
N31 C35 1.317(7) . ?
N31 N32 1.346(6) . ?
N32 C33 1.334(7) . ?
C33 C34 1.380(8) . ?
C33 C36 1.502(9) . ?
C34 C35 1.417(8) . ?
C34 C38 1.459(8) . ?
C35 C37 1.486(8) . ?
C38 C39 1.374(9) . ?
C38 C43 1.393(10) . ?
C39 C40 1.410(9) . ?
C40 C41 1.356(10) . ?
C41 C42 1.406(9) . ?
C41 C44 1.490(8) . ?
C42 C43 1.380(9) . ?
C44 O46 1.267(7) . ?
C44 O45 1.273(7) . ?
O45 Fe1 2.175(4) 1_655 ?
O45 Fe2 2.238(4) 1_655 ?
N51 C55 1.328(10) . ?
N51 N52 1.405(10) . ?
N52 C53 1.341(10) . ?
C53 C54 1.355(11) . ?
C53 C57 1.517(13) . ?
C54 C55 1.437(13) . ?
C54 C58 1.466(10) . ?
C55 C56 1.447(14) . ?
C58 C63 1.384(11) . ?
C58 C59 1.417(12) . ?
C59 C60 1.415(12) . ?
C60 C61 1.347(10) . ?
C61 C62 1.341(10) . ?
C61 C64 1.505(9) . ?
C62 C63 1.392(10) . ?
C64 O66 1.230(7) . ?
C64 O65 1.249(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O25 Fe1 O66 107.7(2) 1_554 . ?
O25 Fe1 O45 93.42(17) 1_554 1_455 ?
O66 Fe1 O45 100.80(17) . 1_455 ?
O25 Fe1 N31 88.76(17) 1_554 . ?
O66 Fe1 N31 93.35(18) . . ?
O45 Fe1 N31 164.26(16) 1_455 . ?
O25 Fe1 N11 156.8(2) 1_554 . ?
O66 Fe1 N11 94.06(17) . . ?
O45 Fe1 N11 90.12(16) 1_455 . ?
N31 Fe1 N11 81.97(16) . . ?
O65 Fe2 O65 180.0 . 3_656 ?
O65 Fe2 O26 93.3(3) . 1_554 ?
O65 Fe2 O26 86.7(3) 3_656 1_554 ?
O65 Fe2 O26 86.7(3) . 3_657 ?
O65 Fe2 O26 93.3(3) 3_656 3_657 ?
O26 Fe2 O26 180.0(3) 1_554 3_657 ?
O65 Fe2 O45 88.74(17) . 1_455 ?
O65 Fe2 O45 91.25(17) 3_656 1_455 ?
O26 Fe2 O45 89.72(17) 1_554 1_455 ?
O26 Fe2 O45 90.28(17) 3_657 1_455 ?
O65 Fe2 O45 91.26(17) . 3_756 ?
O65 Fe2 O45 88.75(17) 3_656 3_756 ?
O26 Fe2 O45 90.28(17) 1_554 3_756 ?
O26 Fe2 O45 89.72(17) 3_657 3_756 ?
O45 Fe2 O45 180.00(12) 1_455 3_756 ?
N51 Fe3 N51 89.8(4) 4 . ?
N51 Fe3 O1 175.3(4) 4 . ?
N51 Fe3 O1 94.8(3) . . ?
N51 Fe3 O1 94.8(3) 4 4 ?
N51 Fe3 O1 175.3(4) . 4 ?
O1 Fe3 O1 80.6(5) . 4 ?
N51 Fe3 Cl2 99.7(2) 4 . ?
N51 Fe3 Cl2 99.7(2) . . ?
O1 Fe3 Cl2 80.6(5) . . ?
O1 Fe3 Cl2 80.6(5) 4 . ?
N32 C1 N12 110.8(4) . . ?
N52 C2 N52 109.9(10) . 4 ?
C15 N11 N12 105.6(4) . . ?
C15 N11 Fe1 131.7(4) . . ?
N12 N11 Fe1 121.3(3) . . ?
C13 N12 N11 111.9(4) . . ?
C13 N12 C1 130.2(5) . . ?
N11 N12 C1 117.9(4) . . ?
N12 C13 C14 107.2(5) . . ?
N12 C13 C17 121.5(6) . . ?
C14 C13 C17 131.2(6) . . ?
C13 C14 C15 105.8(5) . . ?
C13 C14 C18 126.8(6) . . ?
C15 C14 C18 127.3(6) . . ?
N11 C15 C14 109.5(5) . . ?
N11 C15 C16 121.1(5) . . ?
C14 C15 C16 129.4(5) . . ?
C19 C18 C23 116.5(7) . . ?
C19A C18 C14 121.5(10) . . ?
C19 C18 C14 122.2(7) . . ?
C23 C18 C14 120.9(6) . . ?
C19A C18 C23A 122.6(10) . . ?
C14 C18 C23A 115.3(8) . . ?
C18 C19 C20 123.2(11) . . ?
C18 C19A C20A 119.8(17) . . ?
C21 C20 C19 118.9(11) . . ?
C21 C20A C19A 126.7(16) . . ?
C22 C21 C20 120.8(7) . . ?
C20A C21 C24 125.5(10) . . ?
C22 C21 C24 120.0(7) . . ?
C20 C21 C24 118.9(7) . . ?
C20A C21 C22A 114.4(11) . . ?
C24 C21 C22A 120.0(7) . . ?
C21 C22 C23 120.2(9) . . ?
C23A C22A C21 119.9(13) . . ?
C22 C23 C18 119.5(9) . . ?
C22A C23A C18 115.3(13) . . ?
O26 C24 O25 122.5(6) . . ?
O26 C24 C21 119.0(6) . . ?
O25 C24 C21 118.4(5) . . ?
C24 O25 Fe1 128.0(4) . 1_556 ?
C24 O26 Fe2 141.2(4) . 1_556 ?
C35 N31 N32 106.3(4) . . ?
C35 N31 Fe1 128.6(4) . . ?
N32 N31 Fe1 123.8(3) . . ?
C33 N32 N31 112.0(4) . . ?
C33 N32 C1 130.3(5) . . ?
N31 N32 C1 117.4(4) . . ?
N32 C33 C34 106.9(5) . . ?
N32 C33 C36 123.5(6) . . ?
C34 C33 C36 129.5(6) . . ?
C33 C34 C35 104.8(5) . . ?
C33 C34 C38 128.5(6) . . ?
C35 C34 C38 126.7(6) . . ?
N31 C35 C34 110.0(5) . . ?
N31 C35 C37 122.4(5) . . ?
C34 C35 C37 127.6(5) . . ?
C39 C38 C43 119.0(6) . . ?
C39 C38 C34 121.7(6) . . ?
C43 C38 C34 119.3(6) . . ?
C38 C39 C40 119.6(7) . . ?
C41 C40 C39 121.3(6) . . ?
C40 C41 C42 119.3(6) . . ?
C40 C41 C44 122.6(6) . . ?
C42 C41 C44 118.1(6) . . ?
C43 C42 C41 119.3(6) . . ?
C42 C43 C38 121.4(6) . . ?
O46 C44 O45 120.6(5) . . ?
O46 C44 C41 119.6(6) . . ?
O45 C44 C41 119.7(5) . . ?
C44 O45 Fe1 99.0(3) . 1_655 ?
C44 O45 Fe2 139.1(4) . 1_655 ?
Fe1 O45 Fe2 106.38(15) 1_655 1_655 ?
C55 N51 N52 105.9(7) . . ?
C55 N51 Fe3 135.2(8) . . ?
N52 N51 Fe3 117.9(5) . . ?
C53 N52 N51 110.4(7) . . ?
C53 N52 C2 129.0(10) . . ?
N51 N52 C2 120.6(8) . . ?
N52 C53 C54 108.1(9) . . ?
N52 C53 C57 123.2(7) . . ?
C54 C53 C57 128.6(8) . . ?
C53 C54 C55 106.4(7) . . ?
C53 C54 C58 127.2(9) . . ?
C55 C54 C58 126.1(8) . . ?
N51 C55 C54 109.1(8) . . ?
N51 C55 C56 126.2(10) . . ?
C54 C55 C56 124.7(8) . . ?
C63 C58 C59 117.2(7) . . ?
C63 C58 C54 122.3(7) . . ?
C59 C58 C54 120.3(7) . . ?
C60 C59 C58 119.0(7) . . ?
C61 C60 C59 121.1(8) . . ?
C62 C61 C60 120.1(7) . . ?
C62 C61 C64 121.5(6) . . ?
C60 C61 C64 118.4(6) . . ?
C61 C62 C63 121.2(7) . . ?
C58 C63 C62 120.9(8) . . ?
O66 C64 O65 123.7(6) . . ?
O66 C64 C61 118.5(6) . . ?
O65 C64 C61 117.7(6) . . ?
C64 O65 Fe2 142.0(5) . . ?
C64 O66 Fe1 129.7(4) . . ?

_refine_diff_density_max         3.359
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.155

_shelxl_version_number           2013-4


# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.003 -0.007 1757 394 ' '
_platon_squeeze_details          ?

# start Validation Reply Form
_vrf_DIFMX01_Fe3L3-FeCl3         
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: There is unresolved disorder around the post-synthetically
added metal centre that could not be resolved.
;
_vrf_PLAT097_Fe3L3-FeCl3         
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       3.36 eA-3  
RESPONSE: There is unresolved disorder around the post-synthetically
added metal centre that could not be resolved.
;
_vrf_PLAT232_Fe3L3-FeCl3         
;
PROBLEM: Hirshfeld Test Diff (M-X)  Fe3    --  O1      ..       13.6 s.u.  
RESPONSE: There is unresolved disorder around the post-synthetically
added metal centre that could not be resolved.  The oxygen site is 
likely partially occupied but the data is not of sufficient quality
to discern this. 
;
_vrf_PLAT242_Fe3L3-FeCl3         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Fe3 Check 
RESPONSE: There is unresolved disorder around the post-synthetically
added metal centre that could not be resolved.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_MnFeL3-FeCl2
_database_code_depnum_ccdc_archive 'CCDC 1443924'
_audit_update_record             
;
2016-02-09 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C75 H66 Cl0.80 Fe0.95 Mn2.45 N12 O13.20'
_chemical_formula_weight         1562.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.345(3)
_cell_length_b                   33.257(7)
_cell_length_c                   12.934(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.66(3)
_cell_angle_gamma                90
_cell_volume                     5274.4(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12199
_cell_measurement_theta_min      0.76
_cell_measurement_theta_max      33.25

_exptl_crystal_description       Rod
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_F_000             1610
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.486
_shelx_estimated_absorpt_T_min   0.868
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.8832
_exptl_absorpt_correction_T_max  0.9391
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            86249
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.661
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             11740
_reflns_number_gt                9672
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1714P)²+11.3272P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11740
_refine_ls_number_parameters     539
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.1036
_refine_ls_wR_factor_ref         0.2994
_refine_ls_wR_factor_gt          0.2907
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.20740(5) 0.06858(2) 0.59737(4) 0.03541(19) Uani 0.815 1 d . . P A 1
Mn2 Mn 0.0000 0.0000 0.5000 0.0362(2) Uani 0.82 2 d S . P B 1
Fe1 Fe 0.20740(5) 0.06858(2) 0.59737(4) 0.03541(19) Uani 0.185 1 d . . P A 2
Fe2 Fe 0.0000 0.0000 0.5000 0.0362(2) Uani 0.18 2 d S . P B 2
O26 O 1.0341(2) 0.05547(10) 0.5953(2) 0.0410(7) Uani 1 1 d . . . . .
N12 N 0.3856(3) 0.13270(11) 0.6856(3) 0.0387(7) Uani 1 1 d . . . . .
O46 O 0.2097(3) 0.06721(16) 1.4355(3) 0.0738(13) Uani 1 1 d . . . . .
O25 O 1.0615(3) 0.12068(11) 0.5791(3) 0.0584(9) Uani 1 1 d . . . . .
O65 O 0.2807(3) 0.01361(11) 0.6480(3) 0.0585(9) Uani 1 1 d . . . . .
N11 N 0.3641(3) 0.10194(12) 0.6163(3) 0.0424(8) Uani 1 1 d . . . . .
N32 N 0.2549(3) 0.12204(11) 0.8040(3) 0.0403(8) Uani 1 1 d . . . . .
O45 O 0.0712(4) 0.02699(13) 1.3775(3) 0.0768(14) Uani 1 1 d . . . . .
N31 N 0.2032(3) 0.08749(11) 0.7671(3) 0.0419(8) Uani 1 1 d . . . . .
C1 C 0.2943(4) 0.14940(13) 0.7312(4) 0.0429(9) Uani 1 1 d . . . . .
H1A H 0.3169 0.1748 0.7673 0.052 Uiso 1 1 calc R U . . .
H1B H 0.2348 0.1556 0.6755 0.052 Uiso 1 1 calc R U . . .
C24 C 0.9981(4) 0.09152(15) 0.5930(4) 0.0470(10) Uani 1 1 d . . . . .
C64 C 0.2342(4) -0.02035(14) 0.6263(3) 0.0445(10) Uani 1 1 d . . . . .
C14 C 0.5451(4) 0.11371(16) 0.6433(4) 0.0480(10) Uani 1 1 d . . . . .
C13 C 0.4935(4) 0.14037(15) 0.7028(4) 0.0457(10) Uani 1 1 d . . . . .
C35 C 0.1728(4) 0.06835(14) 0.8490(3) 0.0479(11) Uani 1 1 d . . . . .
C21 C 0.8832(4) 0.09862(15) 0.6100(4) 0.0492(11) Uani 1 1 d . . . . .
C22 C 0.8208(4) 0.06673(15) 0.6434(4) 0.0509(11) Uani 1 1 d . . . . .
H22 H 0.8533 0.0411 0.6572 0.061 Uiso 1 1 calc R U . . .
C23 C 0.7146(4) 0.07253(15) 0.6560(4) 0.0518(11) Uani 1 1 d . . . . .
H23 H 0.6739 0.0507 0.6793 0.062 Uiso 1 1 calc R U . . .
C33 C 0.2592(4) 0.12420(15) 0.9091(3) 0.0484(11) Uani 1 1 d . . . . .
C41 C 0.1635(4) 0.06111(16) 1.2556(3) 0.0471(10) Uani 1 1 d . . . . .
C61 C 0.2923(4) -0.05674(15) 0.6697(4) 0.0490(11) Uani 1 1 d . . . . .
C15 C 0.4616(4) 0.09013(16) 0.5911(4) 0.0474(10) Uani 1 1 d . . . . .
C34 C 0.2083(4) 0.09038(15) 0.9415(3) 0.0475(11) Uani 1 1 d . . . . .
C18 C 0.6628(4) 0.10953(17) 0.6358(5) 0.0548(12) Uani 1 1 d . . . . .
C44 C 0.1468(4) 0.05075(16) 1.3646(3) 0.0460(10) Uani 1 1 d . . . . .
C38 C 0.1908(4) 0.08012(17) 1.0485(3) 0.0523(12) Uani 1 1 d . . . . .
C20 C 0.8353(4) 0.13591(17) 0.5941(6) 0.0693(17) Uani 1 1 d . . . . .
H20 H 0.8770 0.1579 0.5734 0.083 Uiso 1 1 calc R U . . .
C43 C 0.0865(5) 0.0675(2) 1.0725(5) 0.0524(17) Uani 0.772(7) 1 d . . P C 1
H43 H 0.0264 0.0662 1.0197 0.063 Uiso 0.772(7) 1 calc R U P C 1
C37 C 0.1154(6) 0.02934(17) 0.8378(4) 0.0671(17) Uani 1 1 d . . . . .
H37A H 0.0486 0.0323 0.7896 0.101 Uiso 1 1 calc R U . . .
H37B H 0.0968 0.0206 0.9059 0.101 Uiso 1 1 calc R U . . .
H37C H 0.1629 0.0093 0.8105 0.101 Uiso 1 1 calc R U . . .
C17 C 0.5420(5) 0.1717(2) 0.7767(6) 0.0723(18) Uani 1 1 d . . . . .
H17A H 0.5070 0.1977 0.7592 0.108 Uiso 1 1 calc R U . . .
H17B H 0.6204 0.1739 0.7715 0.108 Uiso 1 1 calc R U . . .
H17C H 0.5306 0.1642 0.8479 0.108 Uiso 1 1 calc R U . . .
C36 C 0.3132(6) 0.1583(2) 0.9709(4) 0.0734(19) Uani 1 1 d . . . . .
H36A H 0.3924 0.1564 0.9712 0.110 Uiso 1 1 calc R U . . .
H36B H 0.2949 0.1570 1.0426 0.110 Uiso 1 1 calc R U . . .
H36C H 0.2876 0.1839 0.9394 0.110 Uiso 1 1 calc R U . . .
C42 C 0.0741(6) 0.0572(2) 1.1750(4) 0.0532(17) Uani 0.772(7) 1 d . . P C 1
H42 H 0.0058 0.0475 1.1916 0.064 Uiso 0.772(7) 1 calc R U P C 1
C16 C 0.4702(5) 0.0557(2) 0.5184(5) 0.0712(18) Uani 1 1 d . . . . .
H16A H 0.4725 0.0304 0.5575 0.107 Uiso 1 1 calc R U . . .
H16B H 0.5371 0.0584 0.4848 0.107 Uiso 1 1 calc R U . . .
H16C H 0.4069 0.0556 0.4652 0.107 Uiso 1 1 calc R U . . .
C60 C 0.3896(8) -0.0551(2) 0.7218(7) 0.112(4) Uani 1 1 d . . . . .
H60 H 0.4250 -0.0298 0.7330 0.135 Uiso 1 1 calc R U . . .
C58 C 0.4134(8) -0.1249(2) 0.7349(7) 0.106(3) Uani 1 1 d . . . . .
C40 C 0.2629(7) 0.0723(4) 1.2281(5) 0.085(3) Uani 0.772(7) 1 d . . P C 1
H40 H 0.3243 0.0726 1.2797 0.102 Uiso 0.772(7) 1 calc R U P C 1
C39 C 0.2765(6) 0.0834(3) 1.1261(5) 0.079(3) Uani 0.772(7) 1 d . . P C 1
H39 H 0.3451 0.0932 1.1104 0.094 Uiso 0.772(7) 1 calc R U P C 1
C59 C 0.4421(11) -0.0900(3) 0.7613(10) 0.181(7) Uani 1 1 d . . . . .
H59 H 0.5040 -0.0870 0.8117 0.217 Uiso 1 1 calc R U . . .
O66 O 0.1470(4) -0.02464(14) 0.5718(4) 0.0795(14) Uani 1 1 d . . . . .
C19 C 0.7257(4) 0.14157(17) 0.6083(6) 0.0671(16) Uani 1 1 d . . . . .
H19 H 0.6940 0.1675 0.5991 0.080 Uiso 1 1 calc R U . . .
C55 C 0.4735(6) -0.18765(17) 0.8355(5) 0.077(2) Uani 1 1 d . . . . .
C54 C 0.4856(9) -0.1615(2) 0.7639(8) 0.122(4) Uani 1 1 d . . . . .
N52 N 0.6242(8) -0.2068(2) 0.7571(7) 0.120(3) Uani 1 1 d . . . . .
C53 C 0.5765(9) -0.1752(3) 0.7214(10) 0.136(5) Uani 1 1 d . . . . .
C62 C 0.2417(10) -0.0924(2) 0.6589(9) 0.155(6) Uani 1 1 d . . . . .
H62 H 0.1671 -0.0946 0.6315 0.186 Uiso 1 1 calc R U . . .
C56 C 0.3714(13) -0.1868(3) 0.9163(8) 0.181(8) Uani 1 1 d . . . . .
H56A H 0.3636 -0.1595 0.9427 0.271 Uiso 1 1 calc R U . . .
H56B H 0.3902 -0.2052 0.9749 0.271 Uiso 1 1 calc R U . . .
H56C H 0.3024 -0.1953 0.8772 0.271 Uiso 1 1 calc R U . . .
C57 C 0.6270(11) -0.1548(3) 0.6240(10) 0.142(4) Uani 1 1 d . . . . .
H57A H 0.6661 -0.1752 0.5881 0.213 Uiso 1 1 calc R U . . .
H57B H 0.6776 -0.1333 0.6493 0.213 Uiso 1 1 calc R U . . .
H57C H 0.5679 -0.1435 0.5755 0.213 Uiso 1 1 calc R U . . .
C63 C 0.3072(13) -0.1273(2) 0.6914(12) 0.215(10) Uani 1 1 d . . . . .
H63 H 0.2747 -0.1531 0.6822 0.258 Uiso 1 1 calc R U . . .
N51 N 0.5543(8) -0.21497(17) 0.8406(7) 0.131(4) Uani 1 1 d . . . . .
C2 C 0.5693(13) -0.2500 0.9135(10) 0.125(6) Uani 1 2 d S T P . .
H2A H 0.5140 -0.2500 0.9631 0.150 Uiso 1 2 calc R U P . .
H2B H 0.6430 -0.2500 0.9529 0.150 Uiso 1 2 calc R U P . .
Fe3 Fe 0.7527(3) -0.2500 0.7241(2) 0.0562(7) Uani 0.4 2 d S T P . .
Cl2 Cl 0.8545(7) -0.2500 0.9036(8) 0.112(3) Uani 0.4 2 d S T P . .
O1 O 0.8688(12) -0.2037(3) 0.6879(13) 0.100(5) Uani 0.4 1 d . . P . .
O2 O 0.670(2) -0.2500 0.5629(14) 0.109(8) Uani 0.4 2 d S T P . .
C39B C 0.2045(17) 0.0401(5) 1.0903(14) 0.043(5) Uani 0.228(7) 1 d . . P C 2
H39B H 0.2248 0.0189 1.0471 0.051 Uiso 0.228(7) 1 calc R U P C 2
C42B C 0.1653(18) 0.1014(6) 1.2258(14) 0.044(5) Uani 0.228(7) 1 d . . P C 2
H42B H 0.1606 0.1222 1.2754 0.053 Uiso 0.228(7) 1 calc R U P C 2
C40B C 0.1884(17) 0.0319(5) 1.1935(14) 0.042(5) Uani 0.228(7) 1 d . . P C 2
H40B H 0.1954 0.0051 1.2191 0.051 Uiso 0.228(7) 1 calc R U P C 2
C43B C 0.174(2) 0.1104(5) 1.1237(14) 0.050(6) Uani 0.228(7) 1 d . . P C 2
H43B H 0.1689 0.1377 1.1021 0.060 Uiso 0.228(7) 1 calc R U P C 2
Cl1 Cl 0.3356(6) 0.2500 0.8198(4) 0.0782(18) Uani 0.4 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O46 2.097(3) 1_554 ?
Mn1 O65 2.110(4) . ?
Mn1 O26 2.180(3) 1_455 ?
Mn1 N11 2.219(4) . ?
Mn1 N31 2.289(3) . ?
Mn1 O25 2.490(4) 1_455 ?
Mn2 O45 2.101(4) 3_557 ?
Mn2 O45 2.101(4) 1_554 ?
Mn2 O66 2.106(4) 3_556 ?
Mn2 O66 2.106(4) . ?
Mn2 O26 2.232(3) 3_656 ?
Mn2 O26 2.232(3) 1_455 ?
O26 C24 1.278(6) . ?
O26 Fe1 2.180(3) 1_655 ?
O26 Mn1 2.180(3) 1_655 ?
O26 Fe2 2.232(3) 1_655 ?
O26 Mn2 2.232(3) 1_655 ?
N12 C13 1.349(5) . ?
N12 N11 1.366(5) . ?
N12 C1 1.442(6) . ?
O46 C44 1.257(6) . ?
O46 Fe1 2.097(3) 1_556 ?
O46 Mn1 2.097(3) 1_556 ?
O25 C24 1.273(6) . ?
O25 Mn1 2.490(4) 1_655 ?
O65 C64 1.283(6) . ?
N11 C15 1.343(6) . ?
N32 C33 1.356(5) . ?
N32 N31 1.373(5) . ?
N32 C1 1.435(6) . ?
O45 C44 1.249(6) . ?
O45 Fe2 2.101(4) 1_556 ?
O45 Mn2 2.101(4) 1_556 ?
N31 C35 1.327(6) . ?
C24 C21 1.479(6) . ?
C64 O66 1.225(6) . ?
C64 C61 1.483(6) . ?
C14 C13 1.377(6) . ?
C14 C15 1.404(6) . ?
C14 C18 1.474(6) . ?
C13 C17 1.492(7) . ?
C35 C34 1.428(6) . ?
C35 C37 1.477(7) . ?
C21 C20 1.379(7) . ?
C21 C22 1.408(7) . ?
C22 C23 1.354(7) . ?
C23 C18 1.397(7) . ?
C33 C34 1.377(7) . ?
C33 C36 1.499(6) . ?
C41 C40B 1.32(2) . ?
C41 C40 1.367(9) . ?
C41 C42B 1.40(2) . ?
C41 C42 1.434(7) . ?
C41 C44 1.488(6) . ?
C61 C60 1.309(9) . ?
C61 C62 1.339(10) . ?
C15 C16 1.494(7) . ?
C34 C38 1.465(6) . ?
C18 C19 1.389(8) . ?
C38 C39 1.376(8) . ?
C38 C43 1.422(8) . ?
C38 C43B 1.433(19) . ?
C38 C39B 1.439(19) . ?
C20 C19 1.400(7) . ?
C43 C42 1.395(8) . ?
C60 C59 1.397(11) . ?
C58 C59 1.251(12) . ?
C58 C63 1.368(15) . ?
C58 C54 1.529(10) . ?
C40 C39 1.399(10) . ?
C55 C54 1.291(13) . ?
C55 N51 1.345(10) . ?
C55 C56 1.728(18) . ?
C54 C53 1.383(17) . ?
N52 C53 1.265(11) . ?
N52 N51 1.483(13) . ?
N52 Fe3 2.218(9) . ?
C53 C57 1.619(18) . ?
C62 C63 1.450(13) . ?
N51 C2 1.497(11) . ?
C2 N51 1.497(11) 4 ?
Fe3 O1 2.189(11) . ?
Fe3 O1 2.189(11) 4 ?
Fe3 O2 2.21(2) . ?
Fe3 N52 2.218(9) 4 ?
Fe3 Cl2 2.508(10) . ?
C39B C40B 1.40(3) . ?
C42B C43B 1.37(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O46 Mn1 O65 103.63(19) 1_554 . ?
O46 Mn1 O26 96.35(13) 1_554 1_455 ?
O65 Mn1 O26 102.45(14) . 1_455 ?
O46 Mn1 N11 90.48(14) 1_554 . ?
O65 Mn1 N11 93.55(15) . . ?
O26 Mn1 N11 160.54(13) 1_455 . ?
O46 Mn1 N31 165.29(18) 1_554 . ?
O65 Mn1 N31 89.85(15) . . ?
O26 Mn1 N31 86.29(12) 1_455 . ?
N11 Mn1 N31 82.71(13) . . ?
O46 Mn1 O25 90.81(18) 1_554 1_455 ?
O65 Mn1 O25 155.74(14) . 1_455 ?
O26 Mn1 O25 55.97(12) 1_455 1_455 ?
N11 Mn1 O25 105.90(13) . 1_455 ?
N31 Mn1 O25 78.65(15) . 1_455 ?
O45 Mn2 O45 180.0(2) 3_557 1_554 ?
O45 Mn2 O66 94.8(2) 3_557 3_556 ?
O45 Mn2 O66 85.2(2) 1_554 3_556 ?
O45 Mn2 O66 85.2(2) 3_557 . ?
O45 Mn2 O66 94.8(2) 1_554 . ?
O66 Mn2 O66 180.0 3_556 . ?
O45 Mn2 O26 89.71(14) 3_557 3_656 ?
O45 Mn2 O26 90.29(14) 1_554 3_656 ?
O66 Mn2 O26 88.86(14) 3_556 3_656 ?
O66 Mn2 O26 91.13(14) . 3_656 ?
O45 Mn2 O26 90.29(14) 3_557 1_455 ?
O45 Mn2 O26 89.71(14) 1_554 1_455 ?
O66 Mn2 O26 91.14(14) 3_556 1_455 ?
O66 Mn2 O26 88.87(14) . 1_455 ?
O26 Mn2 O26 180.00(9) 3_656 1_455 ?
C24 O26 Fe1 98.7(3) . 1_655 ?
C24 O26 Mn1 98.7(3) . 1_655 ?
C24 O26 Fe2 136.0(3) . 1_655 ?
Fe1 O26 Fe2 107.09(13) 1_655 1_655 ?
C24 O26 Mn2 136.0(3) . 1_655 ?
Mn1 O26 Mn2 107.09(13) 1_655 1_655 ?
C13 N12 N11 111.3(3) . . ?
C13 N12 C1 131.5(4) . . ?
N11 N12 C1 117.1(3) . . ?
C44 O46 Fe1 131.2(3) . 1_556 ?
C44 O46 Mn1 131.2(3) . 1_556 ?
C24 O25 Mn1 84.6(3) . 1_655 ?
C64 O65 Mn1 122.0(3) . . ?
C15 N11 N12 105.5(4) . . ?
C15 N11 Mn1 128.5(3) . . ?
N12 N11 Mn1 123.2(3) . . ?
C33 N32 N31 110.9(3) . . ?
C33 N32 C1 130.4(4) . . ?
N31 N32 C1 118.8(3) . . ?
C44 O45 Fe2 139.1(3) . 1_556 ?
C44 O45 Mn2 139.1(3) . 1_556 ?
C35 N31 N32 106.6(3) . . ?
C35 N31 Mn1 132.3(3) . . ?
N32 N31 Mn1 120.2(2) . . ?
N32 C1 N12 111.4(4) . . ?
O25 C24 O26 120.0(4) . . ?
O25 C24 C21 121.0(4) . . ?
O26 C24 C21 118.9(4) . . ?
O66 C64 O65 124.7(4) . . ?
O66 C64 C61 118.5(5) . . ?
O65 C64 C61 116.8(4) . . ?
C13 C14 C15 105.5(4) . . ?
C13 C14 C18 128.4(4) . . ?
C15 C14 C18 126.1(4) . . ?
N12 C13 C14 107.4(4) . . ?
N12 C13 C17 123.6(4) . . ?
C14 C13 C17 129.0(4) . . ?
N31 C35 C34 109.6(4) . . ?
N31 C35 C37 121.3(4) . . ?
C34 C35 C37 129.0(4) . . ?
C20 C21 C22 118.9(4) . . ?
C20 C21 C24 121.5(5) . . ?
C22 C21 C24 119.5(4) . . ?
C23 C22 C21 120.1(5) . . ?
C22 C23 C18 122.1(5) . . ?
N32 C33 C34 107.2(4) . . ?
N32 C33 C36 122.5(4) . . ?
C34 C33 C36 130.3(4) . . ?
C40B C41 C42B 121.8(11) . . ?
C40 C41 C42 118.3(5) . . ?
C40B C41 C44 118.2(9) . . ?
C40 C41 C44 122.5(5) . . ?
C42B C41 C44 119.5(8) . . ?
C42 C41 C44 119.2(4) . . ?
C60 C61 C62 118.7(6) . . ?
C60 C61 C64 122.4(5) . . ?
C62 C61 C64 118.9(5) . . ?
N11 C15 C14 110.4(4) . . ?
N11 C15 C16 120.6(4) . . ?
C14 C15 C16 129.0(4) . . ?
C33 C34 C35 105.7(4) . . ?
C33 C34 C38 126.9(4) . . ?
C35 C34 C38 127.4(4) . . ?
C19 C18 C23 117.8(4) . . ?
C19 C18 C14 121.9(5) . . ?
C23 C18 C14 120.2(5) . . ?
O45 C44 O46 125.9(4) . . ?
O45 C44 C41 117.5(4) . . ?
O46 C44 C41 116.6(4) . . ?
C39 C38 C43 120.2(5) . . ?
C43B C38 C39B 114.6(10) . . ?
C39 C38 C34 119.1(5) . . ?
C43 C38 C34 120.7(5) . . ?
C43B C38 C34 121.7(8) . . ?
C39B C38 C34 123.1(9) . . ?
C21 C20 C19 120.3(5) . . ?
C42 C43 C38 118.8(5) . . ?
C43 C42 C41 120.6(5) . . ?
C61 C60 C59 120.8(8) . . ?
C59 C58 C63 113.2(8) . . ?
C59 C58 C54 122.2(7) . . ?
C63 C58 C54 124.0(7) . . ?
C41 C40 C39 121.8(7) . . ?
C38 C39 C40 120.0(6) . . ?
C58 C59 C60 124.6(8) . . ?
C64 O66 Mn2 149.7(4) . . ?
C18 C19 C20 120.5(5) . . ?
C54 C55 N51 110.1(10) . . ?
C54 C55 C56 125.2(8) . . ?
N51 C55 C56 124.7(8) . . ?
C55 C54 C53 103.3(8) . . ?
C55 C54 C58 126.8(12) . . ?
C53 C54 C58 129.9(11) . . ?
C53 N52 N51 97.6(10) . . ?
C53 N52 Fe3 141.3(10) . . ?
N51 N52 Fe3 120.8(5) . . ?
N52 C53 C54 119.6(14) . . ?
N52 C53 C57 115.3(11) . . ?
C54 C53 C57 125.1(8) . . ?
C61 C62 C63 116.1(9) . . ?
C58 C63 C62 123.3(8) . . ?
C55 N51 N52 109.4(7) . . ?
C55 N51 C2 126.5(13) . . ?
N52 N51 C2 124.1(10) . . ?
N51 C2 N51 102.2(9) . 4 ?
O1 Fe3 O1 89.3(7) . 4 ?
O1 Fe3 O2 92.3(7) . . ?
O1 Fe3 O2 92.3(7) 4 . ?
O1 Fe3 N52 175.2(4) . 4 ?
O1 Fe3 N52 95.0(4) 4 4 ?
O2 Fe3 N52 85.3(6) . 4 ?
O1 Fe3 N52 95.0(4) . . ?
O1 Fe3 N52 175.2(4) 4 . ?
O2 Fe3 N52 85.3(6) . . ?
N52 Fe3 N52 80.7(5) 4 . ?
O1 Fe3 Cl2 85.9(5) . . ?
O1 Fe3 Cl2 85.9(5) 4 . ?
O2 Fe3 Cl2 177.5(7) . . ?
N52 Fe3 Cl2 96.6(3) 4 . ?
N52 Fe3 Cl2 96.6(3) . . ?
C40B C39B C38 121.0(15) . . ?
C43B C42B C41 118.8(16) . . ?
C41 C40B C39B 120.4(15) . . ?
C42B C43B C38 122.3(15) . . ?

_refine_diff_density_max         1.537
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.120

_shelxl_version_number           2013-4


# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.500 0.102 0.111 1878 373 ' '
_platon_squeeze_details          ?

# start Validation Reply Form
_vrf_PLAT374_MnFeL3-FeCl2        
;
PROBLEM: Long    N - N         Bond  N51    -   N52    ..       1.48 Ang.  
RESPONSE: 
The N-N bond in question is part of the ligand molecule that
provides the free coordinating site in this MOF. In this structure
the metal occupancy of this site is only 40% meaning that 60% of
the ligand does not have a metal centre. In other structures of this
MOF we see quite a number of conformations for this non-
coordinated ligand. Thus, for this structure the low occupancy results
in disorder for sites involving the bis-pyrazole binding site and
the surrounding phenyl ring but the data is not of sufficient 
quality to allow this disorder to be modelled.  
Other B-level alerts relate to this problem.
;
# end Validation Reply Form
