# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1402020'
#Added by publCIF



_audit_update_record             
;
2015-05-20 deposited with the CCDC.
2015-08-20 downloaded from the CCDC.
;


_symmetry_space_group_name_hall  ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H30 Fe7 N2 O40'
_chemical_formula_weight         1305.39

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'
Fe Fe 0.3463 0.8444 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8366(14)
_cell_length_b                   10.967(2)
_cell_length_c                   14.884(3)
_cell_angle_alpha                111.35(3)
_cell_angle_beta                 97.42(3)
_cell_angle_gamma                92.39(3)
_cell_volume                     1026.0(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             654
_exptl_absorpt_coefficient_mu    2.534
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8745
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3599
_reflns_number_gt                2774
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        "CrystalStructure (Rigaku/MSC'2004)"
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0908P)²+3.0194P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_reflns         3599
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0884
_refine_ls_wR_factor_ref         0.2038
_refine_ls_wR_factor_gt          0.1908
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.171
_refine_ls_shift/su_max          0.003
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O 0.9969(10) 0.7701(6) 0.1167(5) 0.0280(16) Uani 1 1 d . . .
C9 C 0.8369(14) 0.7171(9) 0.0634(7) 0.023(2) Uani 1 1 d . . .
H9A H 0.7459 0.7724 0.0517 0.028 Uiso 1 1 calc R . .
Fe1 Fe 0.5000 0.5000 0.0000 0.0177(5) Uani 1 2 d S . .
Fe2 Fe 0.08487(19) -0.04253(13) 0.21015(9) 0.0191(4) Uani 1 1 d . . .
Fe3 Fe 0.16393(19) 0.19804(13) 0.43013(9) 0.0202(4) Uani 1 1 d . . .
Fe4 Fe 0.30007(19) 0.25087(13) 0.23808(9) 0.0193(4) Uani 1 1 d . . .
O17 O 0.1386(10) 0.2718(6) 0.5730(4) 0.0258(15) Uani 1 1 d . . .
O19 O 0.1863(8) 0.1326(6) 0.2925(4) 0.0182(14) Uani 1 1 d . . .
O6 O 0.3371(9) -0.0848(6) 0.1463(5) 0.0265(16) Uani 1 1 d . . .
O7 O -0.0563(10) 0.0129(7) 0.1028(4) 0.0261(16) Uani 1 1 d . . .
O1 O 0.7887(9) 0.5978(6) 0.0248(4) 0.0214(14) Uani 1 1 d . . .
O12 O -0.1207(10) 0.1190(7) 0.4090(5) 0.0341(18) Uani 1 1 d . . .
O9 O 0.1958(11) -0.1275(6) 0.3042(5) 0.0312(17) Uani 1 1 d . . .
O13 O 0.4445(10) 0.2875(7) 0.4699(5) 0.0378(19) Uani 1 1 d . . .
O15 O 0.1672(10) 0.4119(6) 0.3121(5) 0.0304(17) Uani 1 1 d . . .
O16 O 0.0458(10) 0.3638(6) 0.4277(5) 0.0300(17) Uani 1 1 d . . .
O8 O 0.0607(10) 0.2194(7) 0.1331(5) 0.0298(17) Uani 1 1 d . . .
O4 O 0.4117(9) 0.3681(6) 0.1729(5) 0.0275(16) Uani 1 1 d . . .
O5 O 0.4493(10) 0.1094(7) 0.1467(5) 0.0310(17) Uani 1 1 d . . .
O3 O 0.6356(9) 0.3977(7) 0.0844(5) 0.0271(16) Uani 1 1 d . . .
C4 C 0.2551(15) -0.0801(11) 0.3940(8) 0.030(2) Uani 1 1 d . . .
H5A H 0.2951 -0.1394 0.4225 0.036 Uiso 1 1 calc R . .
O18 O 0.2566(11) 0.3377(7) 0.7300(5) 0.0384(19) Uani 1 1 d . . .
O10 O 0.2670(11) 0.0388(7) 0.4505(5) 0.0368(18) Uani 1 1 d . . .
O14 O 0.5456(10) 0.3076(7) 0.3397(5) 0.0339(18) Uani 1 1 d . . .
O11 O -0.1795(10) -0.0368(7) 0.2585(5) 0.0329(18) Uani 1 1 d . . .
C8 C 0.2667(15) 0.2823(11) 0.6446(7) 0.033(3) Uani 1 1 d . . .
H1A H 0.3825 0.2427 0.6301 0.040 Uiso 1 1 calc R . .
C1 C 0.5848(14) 0.3650(10) 0.1506(7) 0.026(2) Uani 1 1 d . . .
H8A H 0.6811 0.3362 0.1863 0.031 Uiso 1 1 calc R . .
C7 C 0.0598(15) 0.4308(9) 0.3768(7) 0.027(2) Uani 1 1 d . . .
H3A H -0.0166 0.5015 0.3879 0.032 Uiso 1 1 calc R . .
C6 C 0.5690(14) 0.3204(9) 0.4259(7) 0.027(2) Uani 1 1 d . . .
H2A H 0.6920 0.3585 0.4624 0.032 Uiso 1 1 calc R . .
C2 C 0.4508(14) -0.0107(10) 0.1254(7) 0.025(2) Uani 1 1 d . . .
H7A H 0.5483 -0.0504 0.0895 0.030 Uiso 1 1 calc R . .
C3 C -0.0619(14) 0.1216(10) 0.0929(7) 0.027(2) Uani 1 1 d . . .
H6A H -0.1695 0.1298 0.0511 0.032 Uiso 1 1 calc R . .
C5 C -0.2260(15) 0.0330(11) 0.3374(7) 0.030(2) Uani 1 1 d . . .
H4A H -0.3575 0.0195 0.3444 0.036 Uiso 1 1 calc R . .
N1 N 0.9393(12) 0.4665(9) 0.8320(6) 0.039(2) Uani 1 1 d . . .
H12 H 0.8438 0.4487 0.8579 0.046 Uiso 1 1 d R . .
H11 H 1.0007 0.4184 0.7879 0.046 Uiso 1 1 d R . .
H13 H 0.8999 0.5053 0.7939 0.046 Uiso 1 1 d R . .
H14 H 1.0129 0.4867 0.8857 0.046 Uiso 1 1 d R . .
O2W O 0.4331(10) 0.6482(6) 0.1317(4) 0.0257(15) Uani 1 1 d . . .
H2WB H 0.4222 0.7302 0.1488 0.031 Uiso 1 1 d R . .
H1W2 H 0.5034 0.6684 0.1874 0.031 Uiso 1 1 d R . .


_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
O2 C9 1.246(11) . ?
O2 Fe2 2.029(6) 1_665 ?
C9 O1 1.233(11) . ?
C9 H9A 0.9300 . ?
Fe1 O3 2.123(6) 2_665 ?
Fe1 O3 2.123(6) . ?
Fe1 O1 2.128(6) . ?
Fe1 O1 2.128(6) 2_665 ?
Fe1 O2W 2.160(6) . ?
Fe1 O2W 2.160(6) 2_665 ?
Fe2 O19 1.905(6) . ?
Fe2 O11 2.025(7) . ?
Fe2 O2 2.029(6) 1_445 ?
Fe2 O9 2.034(7) . ?
Fe2 O7 2.053(6) . ?
Fe2 O6 2.064(7) . ?
Fe3 O19 1.938(6) . ?
Fe3 O17 2.016(6) . ?
Fe3 O10 2.018(7) . ?
Fe3 O13 2.030(7) . ?
Fe3 O16 2.030(6) . ?
Fe3 O12 2.034(7) . ?
Fe4 O19 1.946(6) . ?
Fe4 O14 2.016(7) . ?
Fe4 O15 2.033(6) . ?
Fe4 O8 2.034(6) . ?
Fe4 O4 2.048(7) . ?
Fe4 O5 2.062(6) . ?
O17 C8 1.256(11) . ?
O6 C2 1.248(11) . ?
O7 C3 1.254(11) . ?
O12 C5 1.248(12) . ?
O9 C4 1.248(12) . ?
O13 C6 1.255(12) . ?
O15 C7 1.249(11) . ?
O16 C7 1.242(11) . ?
O8 C3 1.241(12) . ?
O4 C1 1.268(11) . ?
O5 C2 1.238(11) . ?
O3 C1 1.248(11) . ?
C4 O10 1.260(12) . ?
C4 H5A 0.9300 . ?
O18 C8 1.205(11) . ?
O14 C6 1.227(11) . ?
O11 C5 1.236(11) . ?
C8 H1A 0.9300 . ?
C1 H8A 0.9300 . ?
C7 H3A 0.9300 . ?
C6 H2A 0.9300 . ?
C2 H7A 0.9300 . ?
C3 H6A 0.9300 . ?
C5 H4A 0.9300 . ?
N1 H12 0.8501 . ?
N1 H11 0.8500 . ?
N1 H13 0.8499 . ?
N1 H14 0.8360 . ?
O2W H2WB 0.8500 . ?
O2W H1W2 0.8500 . ?

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
C9 O2 Fe2 132.3(6) . 1_665 ?
O1 C9 O2 125.7(9) . . ?
O1 C9 H9A 117.2 . . ?
O2 C9 H9A 117.2 . . ?
O3 Fe1 O3 180.0(3) 2_665 . ?
O3 Fe1 O1 95.5(2) 2_665 . ?
O3 Fe1 O1 84.5(2) . . ?
O3 Fe1 O1 84.5(2) 2_665 2_665 ?
O3 Fe1 O1 95.5(2) . 2_665 ?
O1 Fe1 O1 180.0(3) . 2_665 ?
O3 Fe1 O2W 90.3(2) 2_665 . ?
O3 Fe1 O2W 89.7(2) . . ?
O1 Fe1 O2W 90.1(2) . . ?
O1 Fe1 O2W 89.9(2) 2_665 . ?
O3 Fe1 O2W 89.7(2) 2_665 2_665 ?
O3 Fe1 O2W 90.3(2) . 2_665 ?
O1 Fe1 O2W 89.9(2) . 2_665 ?
O1 Fe1 O2W 90.1(2) 2_665 2_665 ?
O2W Fe1 O2W 180.0(3) . 2_665 ?
O19 Fe2 O11 96.2(3) . . ?
O19 Fe2 O2 175.2(3) . 1_445 ?
O11 Fe2 O2 88.5(3) . 1_445 ?
O19 Fe2 O9 95.8(3) . . ?
O11 Fe2 O9 90.4(3) . . ?
O2 Fe2 O9 84.8(3) 1_445 . ?
O19 Fe2 O7 93.8(3) . . ?
O11 Fe2 O7 86.2(3) . . ?
O2 Fe2 O7 85.8(3) 1_445 . ?
O9 Fe2 O7 170.1(3) . . ?
O19 Fe2 O6 94.4(3) . . ?
O11 Fe2 O6 169.3(3) . . ?
O2 Fe2 O6 80.9(3) 1_445 . ?
O9 Fe2 O6 87.4(3) . . ?
O7 Fe2 O6 94.2(3) . . ?
O19 Fe3 O17 178.1(3) . . ?
O19 Fe3 O10 94.0(3) . . ?
O17 Fe3 O10 87.9(3) . . ?
O19 Fe3 O13 92.8(3) . . ?
O17 Fe3 O13 87.0(3) . . ?
O10 Fe3 O13 89.0(3) . . ?
O19 Fe3 O16 93.7(3) . . ?
O17 Fe3 O16 84.4(3) . . ?
O10 Fe3 O16 172.0(3) . . ?
O13 Fe3 O16 92.9(3) . . ?
O19 Fe3 O12 94.7(3) . . ?
O17 Fe3 O12 85.6(3) . . ?
O10 Fe3 O12 91.0(3) . . ?
O13 Fe3 O12 172.5(3) . . ?
O16 Fe3 O12 86.1(3) . . ?
O19 Fe4 O14 94.0(3) . . ?
O19 Fe4 O15 96.9(3) . . ?
O14 Fe4 O15 92.0(3) . . ?
O19 Fe4 O8 93.9(3) . . ?
O14 Fe4 O8 171.5(3) . . ?
O15 Fe4 O8 83.7(3) . . ?
O19 Fe4 O4 176.7(3) . . ?
O14 Fe4 O4 88.9(3) . . ?
O15 Fe4 O4 84.7(3) . . ?
O8 Fe4 O4 83.4(3) . . ?
O19 Fe4 O5 94.4(3) . . ?
O14 Fe4 O5 89.6(3) . . ?
O15 Fe4 O5 168.5(3) . . ?
O8 Fe4 O5 93.2(3) . . ?
O4 Fe4 O5 83.9(3) . . ?
C8 O17 Fe3 128.0(6) . . ?
Fe2 O19 Fe3 120.3(3) . . ?
Fe2 O19 Fe4 120.4(3) . . ?
Fe3 O19 Fe4 119.2(3) . . ?
C2 O6 Fe2 128.7(6) . . ?
C3 O7 Fe2 132.6(6) . . ?
C9 O1 Fe1 127.1(6) . . ?
C5 O12 Fe3 132.4(6) . . ?
C4 O9 Fe2 131.3(6) . . ?
C6 O13 Fe3 134.6(7) . . ?
C7 O15 Fe4 131.2(6) . . ?
C7 O16 Fe3 133.5(6) . . ?
C3 O8 Fe4 129.7(6) . . ?
C1 O4 Fe4 123.8(6) . . ?
C2 O5 Fe4 133.4(6) . . ?
C1 O3 Fe1 133.4(6) . . ?
O9 C4 O10 127.7(9) . . ?
O9 C4 H5A 116.2 . . ?
O10 C4 H5A 116.2 . . ?
C4 O10 Fe3 131.5(6) . . ?
C6 O14 Fe4 130.5(7) . . ?
C5 O11 Fe2 129.8(7) . . ?
O18 C8 O17 127.3(10) . . ?
O18 C8 H1A 116.3 . . ?
O17 C8 H1A 116.3 . . ?
O3 C1 O4 124.9(9) . . ?
O3 C1 H8A 117.5 . . ?
O4 C1 H8A 117.5 . . ?
O16 C7 O15 126.0(9) . . ?
O16 C7 H3A 117.0 . . ?
O15 C7 H3A 117.0 . . ?
O14 C6 O13 126.9(9) . . ?
O14 C6 H2A 116.6 . . ?
O13 C6 H2A 116.6 . . ?
O5 C2 O6 127.7(9) . . ?
O5 C2 H7A 116.2 . . ?
O6 C2 H7A 116.2 . . ?
O8 C3 O7 127.0(9) . . ?
O8 C3 H6A 116.5 . . ?
O7 C3 H6A 116.5 . . ?
O11 C5 O12 128.9(10) . . ?
O11 C5 H4A 115.6 . . ?
O12 C5 H4A 115.6 . . ?
H12 N1 H11 132.0 . . ?
H12 N1 H13 110.4 . . ?
H11 N1 H13 88.2 . . ?
H12 N1 H14 88.8 . . ?
H11 N1 H14 107.7 . . ?
H13 N1 H14 136.5 . . ?
Fe1 O2W H2WB 133.4 . . ?
Fe1 O2W H1W2 123.6 . . ?
H2WB O2W H1W2 85.4 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.487
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.190
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1402021'
_audit_update_record             
;
2015-05-20 deposited with the CCDC.
2015-08-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H30 Fe6 Mn N2 O40'
_chemical_formula_weight         1304.48

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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   6.8216(14)
_cell_length_b                   10.968(2)
_cell_length_c                   14.889(3)
_cell_angle_alpha                111.14(3)
_cell_angle_beta                 97.28(3)
_cell_angle_gamma                92.22(3)
_cell_volume                     1026.3(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_F_000             653
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.487
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7750
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.160
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_full        25.009
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measured_fraction_theta_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_point_group_measured_fraction_full 0.902
_reflns_number_total             3261
_reflns_number_gt                2640
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0001P)²+59.0782P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3261
_refine_ls_number_parameters     305
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.1391
_refine_ls_wR_factor_ref         0.2829
_refine_ls_wR_factor_gt          0.2700
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.148
_refine_ls_shift/su_max          0.003
_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
O16 O 1.1428(18) 0.3956(13) 0.0877(10) 0.025(3) Uani 1 1 d . U . . .
C1 C 1.092(3) 0.364(2) 0.1503(16) 0.030(5) Uani 1 1 d . . . . .
H1A H 1.1868 0.3342 0.1859 0.037 Uiso 1 1 calc R U . . .
Fe1 Fe 0.6636(4) 0.1978(3) 0.43036(17) 0.0153(7) Uani 1 1 d . . . . .
Fe2 Fe 0.8013(4) 0.2516(2) 0.23977(19) 0.0159(7) Uani 1 1 d . . . . .
Fe3 Fe 0.5872(4) -0.0412(2) 0.21135(18) 0.0159(7) Uani 1 1 d . . . . .
Mn1 Mn 0.0000 -0.5000 0.0000 0.0159(9) Uani 1 2 d S . P . .
O1 O 0.6777(17) 0.1338(10) 0.2914(8) 0.011(2) Uani 1 1 d . . . . .
O4 O 0.8402(18) -0.0834(12) 0.1486(9) 0.023(3) Uani 1 1 d . . . . .
O10 O 0.9457(19) 0.2903(15) 0.4720(10) 0.033(4) Uani 1 1 d . . . . .
O12 O 0.666(2) 0.4133(13) 0.3118(10) 0.030(3) Uani 1 1 d . . . . .
O20 O 0.649(2) 0.2679(13) 0.5744(8) 0.025(3) Uani 1 1 d . U . . .
O2 O 0.5614(19) 0.2181(14) 0.1339(9) 0.028(3) Uani 1 1 d . . . . .
O6 O 0.695(2) -0.1245(13) 0.3072(10) 0.031(3) Uani 1 1 d . . . . .
O8 O 0.380(2) 0.1208(17) 0.4085(11) 0.040(4) Uani 1 1 d . . . . .
O9 O 0.3250(18) -0.0353(13) 0.2608(9) 0.023(3) Uani 1 1 d . . . . .
O3 O 0.4442(19) 0.0127(13) 0.1042(9) 0.025(3) Uani 1 1 d . . . . .
O5 O 0.950(2) 0.1114(14) 0.1490(11) 0.035(4) Uani 1 1 d . . . . .
O14 O 0.4996(18) -0.2297(12) 0.1194(9) 0.022(3) Uani 1 1 d . . . . .
O15 O 0.2994(18) -0.3987(12) 0.0254(9) 0.021(3) Uani 1 1 d . . . . .
C3 C 0.949(3) -0.0093(17) 0.1267(12) 0.018(4) Uani 1 1 d . . . . .
H3A H 1.0423 -0.0493 0.0881 0.022 Uiso 1 1 calc R U . . .
O18 O 0.762(2) 0.3392(16) 0.7310(9) 0.037(4) Uani 1 1 d . . . . .
O1W O -0.0613(19) -0.3449(12) 0.1357(9) 0.024(3) Uani 1 1 d . . . . .
H1WA H -0.0355 -0.2549 0.1423 0.029 Uiso 1 1 d R U . . .
H1WB H 0.0810 -0.3417 0.1591 0.029 Uiso 1 1 d R U . . .
O7 O 0.765(2) 0.0369(15) 0.4512(11) 0.036(4) Uani 1 1 d . . . . .
O17 O 0.9124(18) 0.3682(13) 0.1734(10) 0.026(3) Uani 1 1 d . . . . .
C4 C 0.763(3) 0.283(2) 0.6442(17) 0.036(5) Uani 1 1 d . . . . .
H4A H 0.8790 0.2430 0.6301 0.043 Uiso 1 1 calc R U . . .
C5 C 0.557(3) 0.430(2) 0.3779(13) 0.025(4) Uani 1 1 d . . . . .
H5A H 0.4811 0.5014 0.3901 0.031 Uiso 1 1 calc R U . . .
C6 C 0.342(2) -0.2815(17) 0.0659(13) 0.017(4) Uani 1 1 d . U . . .
H6A H 0.2485 -0.2263 0.0559 0.021 Uiso 1 1 calc R U . . .
O11 O 1.0490(19) 0.3080(15) 0.3404(10) 0.030(3) Uani 1 1 d . . . . .
C7 C 0.755(3) -0.076(2) 0.3964(14) 0.024(4) Uani 1 1 d . U . . .
H7A H 0.7984 -0.1352 0.4247 0.029 Uiso 1 1 calc R U . . .
C8 C 0.275(3) 0.034(2) 0.3392(14) 0.029(5) Uani 1 1 d . . . . .
H8A H 0.1443 0.0181 0.3471 0.035 Uiso 1 1 calc R U . . .
O13 O 0.542(2) 0.3616(13) 0.4279(10) 0.031(3) Uani 1 1 d . . . . .
C9 C 1.068(3) 0.3215(19) 0.4253(15) 0.028(5) Uani 1 1 d . U . . .
H9A H 1.1905 0.3607 0.4615 0.034 Uiso 1 1 calc R U . . .
C10 C 0.442(3) 0.119(2) 0.0932(14) 0.028(5) Uani 1 1 d . . . . .
H10A H 0.3373 0.1257 0.0490 0.033 Uiso 1 1 calc R U . . .
N1 N 0.561(2) 0.5336(17) 0.1707(12) 0.028(4) Uani 1 1 d . . . . .
H21A H 0.5580 0.6253 0.1819 0.041 Uiso 1 1 d R U . . .
H21B H 0.6525 0.4964 0.1265 0.041 Uiso 1 1 d R U . . .
H21C H 0.4305 0.4896 0.1431 0.041 Uiso 1 1 d R U . . .
H21D H 0.6060 0.5220 0.2376 0.041 Uiso 1 1 d R U . . .


_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
O16 C1 1.19(2) . ?
O16 Mn1 2.193(12) 1_665 ?
C1 O17 1.31(2) . ?
C1 H1A 0.9300 . ?
Fe1 O1 1.947(11) . ?
Fe1 O13 2.017(14) . ?
Fe1 O20 2.019(12) . ?
Fe1 O8 2.019(14) . ?
Fe1 O7 2.032(14) . ?
Fe1 O10 2.052(13) . ?
Fe2 O1 1.941(10) . ?
Fe2 O11 2.022(13) . ?
Fe2 O12 2.037(13) . ?
Fe2 O2 2.045(13) . ?
Fe2 O5 2.047(13) . ?
Fe2 O17 2.052(12) . ?
Fe3 O1 1.886(11) . ?
Fe3 O9 2.013(12) . ?
Fe3 O6 2.034(13) . ?
Fe3 O14 2.040(12) . ?
Fe3 O3 2.043(13) . ?
Fe3 O4 2.056(12) . ?
Mn1 O16 2.193(12) 2_655 ?
Mn1 O16 2.193(12) 1_445 ?
Mn1 O15 2.208(12) . ?
Mn1 O15 2.208(12) 2_545 ?
Mn1 O1W 2.222(12) . ?
Mn1 O1W 2.222(12) 2_545 ?
O4 C3 1.23(2) . ?
O10 C9 1.26(2) . ?
O12 C5 1.27(2) . ?
O20 C4 1.17(2) . ?
O2 C10 1.24(2) . ?
O6 C7 1.25(2) . ?
O8 C8 1.24(3) . ?
O9 C8 1.24(2) . ?
O3 C10 1.23(2) . ?
O5 C3 1.24(2) . ?
O14 C6 1.23(2) . ?
O15 C6 1.21(2) . ?
C3 H3A 0.9300 . ?
O18 C4 1.22(3) . ?
O1W H1WA 0.9631 . ?
O1W H1WB 0.9835 . ?
O7 C7 1.21(2) . ?
C4 H4A 0.9300 . ?
C5 O13 1.24(2) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
O11 C9 1.21(2) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
N1 H21A 0.9600 . ?
N1 H21B 0.9600 . ?
N1 H21C 0.9600 . ?
N1 H21D 1.0582 . ?

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
C1 O16 Mn1 132.4(13) . 1_665 ?
O16 C1 O17 125.5(19) . . ?
O16 C1 H1A 117.2 . . ?
O17 C1 H1A 117.2 . . ?
O1 Fe1 O13 92.6(5) . . ?
O1 Fe1 O20 178.8(5) . . ?
O13 Fe1 O20 86.3(6) . . ?
O1 Fe1 O8 92.7(5) . . ?
O13 Fe1 O8 85.0(6) . . ?
O20 Fe1 O8 87.6(6) . . ?
O1 Fe1 O7 95.4(6) . . ?
O13 Fe1 O7 171.2(6) . . ?
O20 Fe1 O7 85.8(6) . . ?
O8 Fe1 O7 91.0(7) . . ?
O1 Fe1 O10 95.0(5) . . ?
O13 Fe1 O10 92.9(6) . . ?
O20 Fe1 O10 84.6(5) . . ?
O8 Fe1 O10 172.1(6) . . ?
O7 Fe1 O10 90.1(6) . . ?
O1 Fe2 O11 96.5(5) . . ?
O1 Fe2 O12 96.8(5) . . ?
O11 Fe2 O12 92.8(6) . . ?
O1 Fe2 O2 91.3(5) . . ?
O11 Fe2 O2 171.7(6) . . ?
O12 Fe2 O2 83.7(6) . . ?
O1 Fe2 O5 95.1(5) . . ?
O11 Fe2 O5 89.4(6) . . ?
O12 Fe2 O5 167.6(6) . . ?
O2 Fe2 O5 92.4(6) . . ?
O1 Fe2 O17 174.5(5) . . ?
O11 Fe2 O17 88.8(5) . . ?
O12 Fe2 O17 84.2(5) . . ?
O2 Fe2 O17 83.4(5) . . ?
O5 Fe2 O17 83.6(6) . . ?
O1 Fe3 O9 94.5(5) . . ?
O1 Fe3 O6 96.7(5) . . ?
O9 Fe3 O6 88.9(6) . . ?
O1 Fe3 O14 176.8(5) . . ?
O9 Fe3 O14 88.4(5) . . ?
O6 Fe3 O14 84.7(5) . . ?
O1 Fe3 O3 92.8(5) . . ?
O9 Fe3 O3 86.3(5) . . ?
O6 Fe3 O3 169.7(5) . . ?
O14 Fe3 O3 86.0(5) . . ?
O1 Fe3 O4 95.9(5) . . ?
O9 Fe3 O4 169.5(5) . . ?
O6 Fe3 O4 88.1(6) . . ?
O14 Fe3 O4 81.3(5) . . ?
O3 Fe3 O4 94.9(5) . . ?
O16 Mn1 O16 180.0 2_655 1_445 ?
O16 Mn1 O15 96.0(5) 2_655 . ?
O16 Mn1 O15 84.0(5) 1_445 . ?
O16 Mn1 O15 84.0(5) 2_655 2_545 ?
O16 Mn1 O15 96.0(5) 1_445 2_545 ?
O15 Mn1 O15 180.0 . 2_545 ?
O16 Mn1 O1W 90.6(5) 2_655 . ?
O16 Mn1 O1W 89.4(5) 1_445 . ?
O15 Mn1 O1W 88.4(5) . . ?
O15 Mn1 O1W 91.6(5) 2_545 . ?
O16 Mn1 O1W 89.4(5) 2_655 2_545 ?
O16 Mn1 O1W 90.6(5) 1_445 2_545 ?
O15 Mn1 O1W 91.6(5) . 2_545 ?
O15 Mn1 O1W 88.4(5) 2_545 2_545 ?
O1W Mn1 O1W 180.0 . 2_545 ?
Fe3 O1 Fe2 121.3(6) . . ?
Fe3 O1 Fe1 120.5(5) . . ?
Fe2 O1 Fe1 118.1(5) . . ?
C3 O4 Fe3 127.5(12) . . ?
C9 O10 Fe1 132.3(13) . . ?
C5 O12 Fe2 129.3(13) . . ?
C4 O20 Fe1 133.8(15) . . ?
C10 O2 Fe2 129.6(13) . . ?
C7 O6 Fe3 131.5(13) . . ?
C8 O8 Fe1 133.6(13) . . ?
C8 O9 Fe3 131.1(13) . . ?
C10 O3 Fe3 132.2(13) . . ?
C3 O5 Fe2 133.1(13) . . ?
C6 O14 Fe3 132.1(12) . . ?
C6 O15 Mn1 125.4(11) . . ?
O4 C3 O5 129.0(17) . . ?
O4 C3 H3A 115.5 . . ?
O5 C3 H3A 115.5 . . ?
Mn1 O1W H1WA 117.6 . . ?
Mn1 O1W H1WB 85.4 . . ?
H1WA O1W H1WB 86.5 . . ?
C7 O7 Fe1 131.0(13) . . ?
C1 O17 Fe2 123.4(12) . . ?
O20 C4 O18 134(2) . . ?
O20 C4 H4A 113.1 . . ?
O18 C4 H4A 113.1 . . ?
O13 C5 O12 126.7(19) . . ?
O13 C5 H5A 116.6 . . ?
O12 C5 H5A 116.6 . . ?
O15 C6 O14 125.0(16) . . ?
O15 C6 H6A 117.5 . . ?
O14 C6 H6A 117.5 . . ?
C9 O11 Fe2 128.9(13) . . ?
O7 C7 O6 129.0(18) . . ?
O7 C7 H7A 115.5 . . ?
O6 C7 H7A 115.5 . . ?
O9 C8 O8 127.1(18) . . ?
O9 C8 H8A 116.5 . . ?
O8 C8 H8A 116.5 . . ?
C5 O13 Fe1 133.5(13) . . ?
O11 C9 O10 129.5(18) . . ?
O11 C9 H9A 115.3 . . ?
O10 C9 H9A 115.3 . . ?
O3 C10 O2 128.0(18) . . ?
O3 C10 H10A 116.0 . . ?
O2 C10 H10A 116.0 . . ?
H21A N1 H21B 109.5 . . ?
H21A N1 H21C 109.5 . . ?
H21B N1 H21C 109.5 . . ?
H21A N1 H21D 109.5 . . ?
H21B N1 H21D 109.5 . . ?
H21C N1 H21D 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn1 O16 C1 O17 11(3) 1_665 . . . ?
O9 Fe3 O1 Fe2 -134.2(7) . . . . ?
O6 Fe3 O1 Fe2 136.3(7) . . . . ?
O3 Fe3 O1 Fe2 -47.7(7) . . . . ?
O4 Fe3 O1 Fe2 47.5(7) . . . . ?
O9 Fe3 O1 Fe1 49.5(7) . . . . ?
O6 Fe3 O1 Fe1 -40.0(8) . . . . ?
O3 Fe3 O1 Fe1 136.0(7) . . . . ?
O4 Fe3 O1 Fe1 -128.8(7) . . . . ?
Fe3 O4 C3 O5 11(3) . . . . ?
Fe2 O5 C3 O4 6(3) . . . . ?
O16 C1 O17 Fe2 155.1(17) . . . . ?
Fe1 O20 C4 O18 169.3(19) . . . . ?
Fe2 O12 C5 O13 16(3) . . . . ?
Mn1 O15 C6 O14 144.4(15) . . . . ?
Fe3 O14 C6 O15 -168.6(13) . . . . ?
Fe1 O7 C7 O6 8(3) . . . . ?
Fe3 O6 C7 O7 0(3) . . . . ?
Fe3 O9 C8 O8 1(3) . . . . ?
Fe1 O8 C8 O9 2(4) . . . . ?
O12 C5 O13 Fe1 -2(3) . . . . ?
Fe2 O11 C9 O10 9(3) . . . . ?
Fe1 O10 C9 O11 2(4) . . . . ?
Fe3 O3 C10 O2 18(3) . . . . ?
Fe2 O2 C10 O3 -4(3) . . . . ?

_refine_diff_density_max         1.396
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.244
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1402022'
_audit_update_record             
;
2015-05-20 deposited with the CCDC.
2015-08-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H30 Fe6 Mg N2 O40'
_chemical_formula_weight         1273.85

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'
Mg Mg 0.0486 0.0363 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   6.8025(14)
_cell_length_b                   10.887(2)
_cell_length_c                   14.826(3)
_cell_angle_alpha                111.43(3)
_cell_angle_beta                 97.52(3)
_cell_angle_gamma                92.24(3)
_cell_volume                     1008.8(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_F_000             640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    2.247
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8751
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.034
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_full        25.007
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             3510
_reflns_number_gt                3146
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0423P)²+1.4728P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3510
_refine_ls_number_parameters     316
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.002

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 0.33418(7) 0.30223(5) 0.06940(3) 0.01892(14) Uani 1 1 d . . . . .
Fe2 Fe 0.19961(7) 0.24986(5) 0.26152(3) 0.01766(13) Uani 1 1 d . . . . .
Fe3 Fe 0.41351(7) 0.54375(5) 0.28954(3) 0.01706(13) Uani 1 1 d . . . . .
Mg1 Mg 0.0000 0.0000 0.5000 0.0009(2) Uani 1 2 d S U P . .
O1 O 0.3122(3) 0.3670(2) 0.20770(16) 0.0170(5) Uani 1 1 d . . . . .
O19 O 0.4980(4) 0.2680(2) 0.61703(18) 0.0258(6) Uani 1 1 d . . . . .
O9 O 0.1609(4) 0.5855(2) 0.35302(19) 0.0250(6) Uani 1 1 d . . . . .
O18 O 0.2841(3) 0.0969(2) 0.52580(17) 0.0221(5) Uani 1 1 d . . . . .
O7 O 0.5556(4) 0.4884(2) 0.39647(17) 0.0260(6) Uani 1 1 d . . . . .
O17 O -0.1306(4) 0.1009(3) 0.41673(19) 0.0269(6) Uani 1 1 d . . . . .
O11 O 0.6182(4) 0.3823(3) 0.09084(19) 0.0315(6) Uani 1 1 d . . . . .
O6 O 0.4398(4) 0.2814(3) 0.36647(19) 0.0292(6) Uani 1 1 d . . . . .
O16 O 0.0899(4) 0.1345(2) 0.32762(19) 0.0262(6) Uani 1 1 d . . . . .
O3 O 0.3329(4) 0.0882(2) 0.18852(19) 0.0311(6) Uani 1 1 d . . . . .
O4 O 0.0528(4) 0.2105(3) 0.02913(19) 0.0368(7) Uani 1 1 d . . . . .
O2 O 0.4532(4) 0.1358(3) 0.07175(18) 0.0294(6) Uani 1 1 d . . . . .
O13 O 0.3016(4) 0.6281(3) 0.19514(19) 0.0320(6) Uani 1 1 d . . . . .
O15 O 0.2401(4) 0.1609(3) -0.23120(19) 0.0392(7) Uani 1 1 d . . . . .
O1W O 0.0653(4) -0.1455(3) 0.3716(2) 0.0262(6) Uani 1 1 d . . . . .
O8 O 0.0524(4) 0.3906(3) 0.3536(2) 0.0322(6) Uani 1 1 d . . . . .
O12 O 0.2294(4) 0.4626(3) 0.04960(19) 0.0360(7) Uani 1 1 d . . . . .
C5 C 0.2417(6) 0.5802(4) 0.1043(3) 0.0262(8) Uani 1 1 d . . . . .
H5A H 0.2024 0.6398 0.0753 0.031 Uiso 1 1 calc R U . . .
O14 O 0.3592(4) 0.2278(3) -0.07416(18) 0.0295(6) Uani 1 1 d . . . . .
O5 O -0.0471(4) 0.1909(3) 0.1608(2) 0.0336(6) Uani 1 1 d . . . . .
N1 N 0.5589(6) 0.0335(4) 0.6673(3) 0.0352(9) Uani 1 1 d . . . . .
H24 H 0.6869 0.0097 0.6496 0.042 Uiso 1 1 d R U . . .
H23 H 0.5369 0.1251 0.6829 0.042 Uiso 1 1 d R U . . .
H22 H 0.4501 0.0078 0.6138 0.042 Uiso 1 1 d R U . . .
O10 O 0.6788(4) 0.5376(3) 0.24143(19) 0.0304(6) Uani 1 1 d . . . . .
C8 C 0.3369(5) 0.2174(3) 0.5636(3) 0.0245(8) Uani 1 1 d . . . . .
H8A H 0.2487 0.2743 0.5509 0.029 Uiso 1 1 calc R U . . .
C7 C -0.0807(5) 0.1354(4) 0.3506(3) 0.0243(8) Uani 1 1 d . . . . .
H7A H -0.1792 0.1642 0.3153 0.029 Uiso 1 1 calc R U . . .
C3 C 0.5610(5) 0.3804(4) 0.4074(3) 0.0229(8) Uani 1 1 d . . . . .
H3A H 0.6675 0.3734 0.4509 0.027 Uiso 1 1 calc R U . . .
C9 C 0.0477(5) 0.5119(4) 0.3743(3) 0.0227(8) Uani 1 1 d . . . . .
H9A H -0.0515 0.5516 0.4095 0.027 Uiso 1 1 calc R U . . .
C1 C 0.4376(5) 0.0690(4) 0.1224(3) 0.0244(8) Uani 1 1 d . . . . .
H1A H 0.5120 -0.0037 0.1099 0.029 Uiso 1 1 calc R U . . .
C4 C 0.7257(6) 0.4672(4) 0.1618(3) 0.0290(9) Uani 1 1 d . . . . .
H4A H 0.8579 0.4797 0.1546 0.035 Uiso 1 1 calc R U . . .
C2 C -0.0702(5) 0.1792(4) 0.0730(3) 0.0283(8) Uani 1 1 d . . . . .
H2A H -0.1947 0.1427 0.0364 0.034 Uiso 1 1 calc R U . . .
C6 C 0.2285(6) 0.2151(4) -0.1451(3) 0.0334(9) Uani 1 1 d . . . . .
H6A H 0.1096 0.2510 -0.1303 0.040 Uiso 1 1 calc R U . . .
H1WB H 0.090(7) -0.220(5) 0.379(3) 0.040(13) Uiso 1 1 d . . . . .
H1WA H -0.009(9) -0.144(6) 0.328(4) 0.07(2) Uiso 1 1 d . . . . .
H21 H 0.583(10) 0.007(7) 0.695(5) 0.07(2) Uiso 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 O1 1.938(2) . ?
Fe1 O12 2.015(3) . ?
Fe1 O14 2.015(3) . ?
Fe1 O2 2.024(3) . ?
Fe1 O11 2.025(3) . ?
Fe1 O4 2.033(3) . ?
Fe2 O1 1.917(2) . ?
Fe2 O5 2.004(3) . ?
Fe2 O3 2.020(3) . ?
Fe2 O6 2.027(3) . ?
Fe2 O16 2.028(2) . ?
Fe2 O8 2.041(3) . ?
Fe3 O1 1.903(2) . ?
Fe3 O10 2.020(3) . ?
Fe3 O19 2.023(3) 2_666 ?
Fe3 O13 2.025(3) . ?
Fe3 O7 2.038(2) . ?
Fe3 O9 2.054(2) . ?
Mg1 O17 2.074(2) 2_556 ?
Mg1 O17 2.074(2) . ?
Mg1 O18 2.084(2) 2_556 ?
Mg1 O18 2.084(2) . ?
Mg1 O1W 2.098(3) . ?
Mg1 O1W 2.098(3) 2_556 ?
O19 C8 1.240(4) . ?
O19 Fe3 2.023(3) 2_666 ?
O9 C9 1.239(4) . ?
O18 C8 1.240(4) . ?
O7 C3 1.246(4) . ?
O17 C7 1.251(4) . ?
O11 C4 1.237(5) . ?
O6 C3 1.237(4) . ?
O16 C7 1.251(4) . ?
O3 C1 1.248(4) . ?
O4 C2 1.234(5) . ?
O2 C1 1.231(4) . ?
O13 C5 1.256(4) . ?
O15 C6 1.210(5) . ?
O1W H1WB 0.88(5) . ?
O1W H1WA 0.77(6) . ?
O8 C9 1.244(4) . ?
O12 C5 1.232(5) . ?
C5 H5A 0.9300 . ?
O14 C6 1.247(5) . ?
O5 C2 1.249(5) . ?
N1 H24 0.9600 . ?
N1 H23 0.9600 . ?
N1 H22 0.9599 . ?
N1 H21 0.60(6) . ?
O10 C4 1.241(5) . ?
C8 H8A 0.9300 . ?
C7 H7A 0.9300 . ?
C3 H3A 0.9300 . ?
C9 H9A 0.9300 . ?
C1 H1A 0.9300 . ?
C4 H4A 0.9300 . ?
C2 H2A 0.9300 . ?
C6 H6A 0.9300 . ?

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
O1 Fe1 O12 94.13(11) . . ?
O1 Fe1 O14 177.70(10) . . ?
O12 Fe1 O14 88.12(11) . . ?
O1 Fe1 O2 93.33(10) . . ?
O12 Fe1 O2 172.22(11) . . ?
O14 Fe1 O2 84.43(11) . . ?
O1 Fe1 O11 94.65(10) . . ?
O12 Fe1 O11 90.86(12) . . ?
O14 Fe1 O11 85.73(11) . . ?
O2 Fe1 O11 86.34(12) . . ?
O1 Fe1 O4 92.78(11) . . ?
O12 Fe1 O4 89.40(13) . . ?
O14 Fe1 O4 86.82(11) . . ?
O2 Fe1 O4 92.44(12) . . ?
O11 Fe1 O4 172.53(11) . . ?
O1 Fe2 O5 94.87(10) . . ?
O1 Fe2 O3 97.18(10) . . ?
O5 Fe2 O3 92.03(12) . . ?
O1 Fe2 O6 93.75(10) . . ?
O5 Fe2 O6 170.66(11) . . ?
O3 Fe2 O6 83.32(12) . . ?
O1 Fe2 O16 176.08(10) . . ?
O5 Fe2 O16 88.47(11) . . ?
O3 Fe2 O16 84.73(10) . . ?
O6 Fe2 O16 83.05(11) . . ?
O1 Fe2 O8 94.81(10) . . ?
O5 Fe2 O8 90.08(12) . . ?
O3 Fe2 O8 167.60(10) . . ?
O6 Fe2 O8 92.78(12) . . ?
O16 Fe2 O8 83.12(10) . . ?
O1 Fe3 O10 96.35(10) . . ?
O1 Fe3 O19 175.16(10) . 2_666 ?
O10 Fe3 O19 88.38(11) . 2_666 ?
O1 Fe3 O13 95.98(10) . . ?
O10 Fe3 O13 90.55(12) . . ?
O19 Fe3 O13 85.00(11) 2_666 . ?
O1 Fe3 O7 93.40(10) . . ?
O10 Fe3 O7 85.89(11) . . ?
O19 Fe3 O7 85.86(11) 2_666 . ?
O13 Fe3 O7 170.28(11) . . ?
O1 Fe3 O9 94.03(10) . . ?
O10 Fe3 O9 169.59(10) . . ?
O19 Fe3 O9 81.26(10) 2_666 . ?
O13 Fe3 O9 87.51(11) . . ?
O7 Fe3 O9 94.37(11) . . ?
O17 Mg1 O17 180.0 2_556 . ?
O17 Mg1 O18 95.29(10) 2_556 2_556 ?
O17 Mg1 O18 84.71(10) . 2_556 ?
O17 Mg1 O18 84.71(10) 2_556 . ?
O17 Mg1 O18 95.29(10) . . ?
O18 Mg1 O18 180.0 2_556 . ?
O17 Mg1 O1W 90.54(12) 2_556 . ?
O17 Mg1 O1W 89.46(12) . . ?
O18 Mg1 O1W 89.67(11) 2_556 . ?
O18 Mg1 O1W 90.32(11) . . ?
O17 Mg1 O1W 89.46(12) 2_556 2_556 ?
O17 Mg1 O1W 90.54(12) . 2_556 ?
O18 Mg1 O1W 90.32(11) 2_556 2_556 ?
O18 Mg1 O1W 89.68(11) . 2_556 ?
O1W Mg1 O1W 180.0 . 2_556 ?
Fe3 O1 Fe2 120.79(11) . . ?
Fe3 O1 Fe1 119.54(12) . . ?
Fe2 O1 Fe1 119.61(11) . . ?
C8 O19 Fe3 131.2(2) . 2_666 ?
C9 O9 Fe3 129.1(2) . . ?
C8 O18 Mg1 128.8(2) . . ?
C3 O7 Fe3 133.1(2) . . ?
C7 O17 Mg1 134.7(2) . . ?
C4 O11 Fe1 133.3(2) . . ?
C3 O6 Fe2 129.5(2) . . ?
C7 O16 Fe2 125.3(2) . . ?
C1 O3 Fe2 130.5(2) . . ?
C2 O4 Fe1 134.5(3) . . ?
C1 O2 Fe1 133.0(2) . . ?
C5 O13 Fe3 131.7(2) . . ?
Mg1 O1W H1WB 113(3) . . ?
Mg1 O1W H1WA 108(4) . . ?
H1WB O1W H1WA 122(5) . . ?
C9 O8 Fe2 133.4(2) . . ?
C5 O12 Fe1 132.1(2) . . ?
O12 C5 O13 126.9(3) . . ?
O12 C5 H5A 116.5 . . ?
O13 C5 H5A 116.5 . . ?
C6 O14 Fe1 127.5(3) . . ?
C2 O5 Fe2 129.3(2) . . ?
H24 N1 H23 115.7 . . ?
H24 N1 H22 115.7 . . ?
H23 N1 H22 90.3 . . ?
H24 N1 H21 81.0 . . ?
H23 N1 H21 127.5 . . ?
H22 N1 H21 128.7 . . ?
C4 O10 Fe3 129.8(2) . . ?
O18 C8 O19 125.2(3) . . ?
O18 C8 H8A 117.4 . . ?
O19 C8 H8A 117.4 . . ?
O17 C7 O16 125.8(3) . . ?
O17 C7 H7A 117.1 . . ?
O16 C7 H7A 117.1 . . ?
O6 C3 O7 126.9(3) . . ?
O6 C3 H3A 116.5 . . ?
O7 C3 H3A 116.5 . . ?
O9 C9 O8 127.0(3) . . ?
O9 C9 H9A 116.5 . . ?
O8 C9 H9A 116.5 . . ?
O2 C1 O3 127.1(3) . . ?
O2 C1 H1A 116.5 . . ?
O3 C1 H1A 116.5 . . ?
O11 C4 O10 128.0(3) . . ?
O11 C4 H4A 116.0 . . ?
O10 C4 H4A 116.0 . . ?
O4 C2 O5 127.5(3) . . ?
O4 C2 H2A 116.2 . . ?
O5 C2 H2A 116.2 . . ?
O15 C6 O14 126.9(4) . . ?
O15 C6 H6A 116.6 . . ?
O14 C6 H6A 116.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 O12 C5 O13 -11.6(6) . . . . ?
Fe3 O13 C5 O12 3.4(6) . . . . ?
Mg1 O18 C8 O19 144.7(3) . . . . ?
Fe3 O19 C8 O18 -163.2(3) 2_666 . . . ?
Mg1 O17 C7 O16 -13.0(6) . . . . ?
Fe2 O16 C7 O17 -155.3(3) . . . . ?
Fe2 O6 C3 O7 4.3(6) . . . . ?
Fe3 O7 C3 O6 -19.8(6) . . . . ?
Fe3 O9 C9 O8 -7.0(6) . . . . ?
Fe2 O8 C9 O9 -12.0(6) . . . . ?
Fe1 O2 C1 O3 1.7(6) . . . . ?
Fe2 O3 C1 O2 -15.6(6) . . . . ?
Fe1 O11 C4 O10 -6.6(7) . . . . ?
Fe3 O10 C4 O11 0.5(6) . . . . ?
Fe1 O4 C2 O5 -4.5(7) . . . . ?
Fe2 O5 C2 O4 -5.5(6) . . . . ?
Fe1 O14 C6 O15 -173.8(3) . . . . ?

_refine_diff_density_max         1.531
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.090

