# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_Comp1
_database_code_depnum_ccdc_archive 'CCDC 1847517'
_audit_update_record             
;
2018-07-25 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H17 Fe K N12 O4, 3(H2 O)'
_chemical_formula_sum            'C18 H23 Fe K N12 O7'
_chemical_formula_weight         614.43

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'
K K 0.2009 0.2494 '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'

_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                   8.3483(11)
_cell_length_b                   12.6991(16)
_cell_length_c                   12.8859(16)
_cell_angle_alpha                110.674(2)
_cell_angle_beta                 91.693(2)
_cell_angle_gamma                97.884(2)
_cell_volume                     1261.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4371
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.54

_exptl_crystal_description       needle
_exptl_crystal_colour            'reddish purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_F_000             632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.828
_shelx_estimated_absorpt_T_min   0.712
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6409
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            7294
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.695
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             5562
_reflns_number_gt                4866
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0956P)²+3.5991P] 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         5562
_refine_ls_number_parameters     394
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1695
_refine_ls_wR_factor_gt          0.1620
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_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
Fe1 Fe 0.88663(5) 0.11179(3) 0.75223(4) 0.01420(15) Uani 1 1 d . . . . .
K1 K 0.39868(9) 0.40782(6) 0.64215(6) 0.02416(19) Uani 1 1 d . . . . .
N1 N 0.7621(3) 0.1072(2) 0.6164(2) 0.0153(5) Uani 1 1 d . . . . .
N2 N 0.5890(3) 0.2139(2) 0.5544(2) 0.0180(5) Uani 1 1 d . . . . .
N3 N 0.8143(3) 0.2517(2) 0.8075(2) 0.0149(5) Uani 1 1 d . . . . .
N4 N 0.6537(3) 0.3797(2) 0.7800(2) 0.0164(5) Uani 1 1 d . . . . .
N5 N 0.8007(3) 0.4228(2) 0.9563(2) 0.0161(5) Uani 1 1 d . . . . .
N6 N 0.9827(3) 0.1688(2) 0.9097(2) 0.0164(5) Uani 1 1 d . . . . .
N7 N 0.9927(3) 0.3262(2) 1.0822(2) 0.0193(5) Uani 1 1 d . . . . .
N8 N 0.5322(3) 0.5753(2) 0.8603(2) 0.0209(6) Uani 1 1 d . . . . .
N9 N 0.6781(3) 0.6221(2) 1.0377(2) 0.0180(5) Uani 1 1 d . . . . .
C1 C 0.6834(4) 0.1980(3) 0.6304(3) 0.0156(6) Uani 1 1 d . . . . .
C2 C 0.7492(4) 0.0288(3) 0.5125(3) 0.0175(6) Uani 1 1 d . . . . .
H1 H 0.803908 -0.035196 0.497684 0.021 Uiso 1 1 calc R U . . .
C3 C 0.6574(4) 0.0403(3) 0.4271(3) 0.0195(6) Uani 1 1 d . . . . .
H2 H 0.649822 -0.014147 0.353533 0.023 Uiso 1 1 calc R U . . .
C4 C 0.5763(4) 0.1339(3) 0.4520(3) 0.0202(6) Uani 1 1 d . . . . .
H3 H 0.509876 0.141442 0.394661 0.024 Uiso 1 1 calc R U . . .
C5 C 0.7141(4) 0.2835(3) 0.7432(3) 0.0158(6) Uani 1 1 d . . . . .
C6 C 0.7020(4) 0.4472(3) 0.8865(3) 0.0166(6) Uani 1 1 d . . . . .
C7 C 0.8516(4) 0.3231(3) 0.9132(3) 0.0155(6) Uani 1 1 d . . . . .
C8 C 0.9499(4) 0.2723(3) 0.9744(3) 0.0160(6) Uani 1 1 d . . . . .
C9 C 1.0715(4) 0.1173(3) 0.9609(3) 0.0199(6) Uani 1 1 d . . . . .
H4 H 1.099616 0.045224 0.919070 0.024 Uiso 1 1 calc R U . . .
C10 C 1.1222(4) 0.1672(3) 1.0727(3) 0.0224(7) Uani 1 1 d . . . . .
H5 H 1.184594 0.130568 1.108358 0.027 Uiso 1 1 calc R U . . .
C11 C 1.0793(4) 0.2727(3) 1.1317(3) 0.0224(7) Uani 1 1 d . . . . .
H6 H 1.111877 0.307842 1.209019 0.027 Uiso 1 1 calc R U . . .
C12 C 0.6335(4) 0.5558(3) 0.9309(3) 0.0166(6) Uani 1 1 d . . . . .
C13 C 0.4702(4) 0.6724(3) 0.9000(3) 0.0238(7) Uani 1 1 d . . . . .
H7 H 0.396816 0.689459 0.852600 0.029 Uiso 1 1 calc R U . . .
C14 C 0.5100(4) 0.7488(3) 1.0081(3) 0.0228(7) Uani 1 1 d . . . . .
H8 H 0.467498 0.818265 1.035088 0.027 Uiso 1 1 calc R U . . .
C15 C 0.6148(4) 0.7192(3) 1.0752(3) 0.0205(7) Uani 1 1 d . . . . .
H9 H 0.642600 0.769243 1.150092 0.025 Uiso 1 1 calc R U . . .
C16 C 0.6966(4) 0.0335(3) 0.7946(3) 0.0177(6) Uani 1 1 d . . . . .
N10 N 0.5853(4) -0.0113(3) 0.8222(2) 0.0240(6) Uani 1 1 d . . . . .
C17 C 0.9548(4) -0.0355(3) 0.6932(3) 0.0207(6) Uani 1 1 d . . . . .
N11 N 0.9885(4) -0.1259(3) 0.6553(3) 0.0354(8) Uani 1 1 d . . . . .
C18 C 1.0856(4) 0.1732(2) 0.7033(2) 0.0162(6) Uani 1 1 d . . . . .
N12 N 1.2019(4) 0.2094(2) 0.6734(2) 0.0214(6) Uani 1 1 d . . . . .
O1 O 0.7255(6) 0.4731(4) 0.5759(4) 0.0636(11) Uani 1 1 d D . . . .
H11 H 0.8002(19) 0.497(2) 0.537(2) 0.076 Uiso 1 1 d D U . . .
H12 H 0.808(5) 0.448(6) 0.602(5) 0.076 Uiso 1 1 d D U . . .
O2 O 0.2897(4) 0.3123(3) 0.4114(3) 0.0429(7) Uani 1 1 d D . . . .
H21 H 0.210(5) 0.259(3) 0.398(5) 0.051 Uiso 1 1 d D U . . .
H22 H 0.262(6) 0.352(4) 0.376(4) 0.051 Uiso 1 1 d D U . . .
O3 O 0.3994(5) 0.6294(4) 0.6340(4) 0.0618(11) Uani 1 1 d D . . . .
H31 H 0.340(5) 0.622(4) 0.5777(18) 0.074 Uiso 1 1 d D U . . .
H32 H 0.478(3) 0.681(2) 0.641(4) 0.074 Uiso 1 1 d D U . . .
O4 O 0.1287(4) 0.4530(2) 0.7922(2) 0.0325(6) Uani 1 1 d D . . . .
H41 H 0.171(6) 0.436(4) 0.842(3) 0.039 Uiso 1 1 d D U . . .
H42 H 0.093(6) 0.512(3) 0.826(3) 0.039 Uiso 1 1 d D U . . .
O5 O -0.0274(5) 0.3443(3) 0.5797(3) 0.0504(9) Uani 1 1 d D . . . .
H51 H 0.061(4) 0.382(4) 0.575(5) 0.060 Uiso 1 1 d D U . . .
H52 H -0.013(7) 0.280(3) 0.533(4) 0.060 Uiso 1 1 d D U . . .
O6 O 0.2339(10) 0.7936(9) 0.7579(8) 0.192(5) Uani 1 1 d D . . . .
H61 H 0.161(6) 0.784(5) 0.706(4) 0.231 Uiso 1 1 d D U . . .
H62 H 0.279(6) 0.861(3) 0.775(6) 0.231 Uiso 1 1 d D U . . .
O7 O 0.3151(9) 0.9388(7) 0.9271(7) 0.120(3) Uani 1 1 d D . . . .
H71 H 0.311(11) 0.915(9) 0.984(6) 0.144 Uiso 1 1 d D U . . .
H72 H 0.415(6) 0.926(9) 0.909(8) 0.144 Uiso 1 1 d D 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
Fe1 N3 1.859(3) . ?
Fe1 C17 1.927(3) . ?
Fe1 C16 1.951(3) . ?
Fe1 C18 1.954(3) . ?
Fe1 N1 1.988(3) . ?
Fe1 N6 1.998(3) . ?
K1 O3 2.852(4) . ?
K1 O2 2.852(3) . ?
K1 N4 2.872(3) . ?
K1 N8 2.935(3) . ?
K1 N12 2.971(3) 1_455 ?
K1 O1 2.980(4) . ?
K1 O4 2.996(3) . ?
K1 N2 3.014(3) . ?
K1 H51 2.86(4) . ?
N1 C2 1.348(4) . ?
N1 C1 1.364(4) . ?
N2 C1 1.325(4) . ?
N2 C4 1.341(4) . ?
N3 C7 1.342(4) . ?
N3 C5 1.355(4) . ?
N4 C5 1.321(4) . ?
N4 C6 1.351(4) . ?
N5 C7 1.326(4) . ?
N5 C6 1.343(4) . ?
N6 C9 1.349(4) . ?
N6 C8 1.355(4) . ?
N7 C8 1.325(4) . ?
N7 C11 1.344(4) . ?
N8 C12 1.332(4) . ?
N8 C13 1.340(4) . ?
N9 C15 1.344(4) . ?
N9 C12 1.344(4) . ?
C1 C5 1.465(4) . ?
C2 C3 1.384(5) . ?
C2 H1 0.9500 . ?
C3 C4 1.392(5) . ?
C3 H2 0.9500 . ?
C4 H3 0.9500 . ?
C6 C12 1.495(4) . ?
C7 C8 1.475(4) . ?
C9 C10 1.380(5) . ?
C9 H4 0.9500 . ?
C10 C11 1.388(5) . ?
C10 H5 0.9500 . ?
C11 H6 0.9500 . ?
C13 C14 1.386(5) . ?
C13 H7 0.9500 . ?
C14 C15 1.388(5) . ?
C14 H8 0.9500 . ?
C15 H9 0.9500 . ?
C16 N10 1.154(5) . ?
C17 N11 1.157(5) . ?
C18 N12 1.152(4) . ?
O1 H11 0.897(19) . ?
O1 H12 0.90(2) . ?
O2 H21 0.847(19) . ?
O2 H22 0.833(19) . ?
O3 H31 0.834(19) . ?
O3 H32 0.84(2) . ?
O4 H41 0.829(19) . ?
O4 H42 0.825(19) . ?
O5 H51 0.84(2) . ?
O5 H52 0.853(19) . ?
O6 H61 0.85(2) . ?
O6 H62 0.83(2) . ?
O7 H71 0.89(2) . ?
O7 H72 0.90(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
N3 Fe1 C17 178.23(13) . . ?
N3 Fe1 C16 92.61(12) . . ?
C17 Fe1 C16 86.03(13) . . ?
N3 Fe1 C18 93.98(12) . . ?
C17 Fe1 C18 87.38(13) . . ?
C16 Fe1 C18 173.41(13) . . ?
N3 Fe1 N1 80.18(11) . . ?
C17 Fe1 N1 98.70(13) . . ?
C16 Fe1 N1 91.04(12) . . ?
C18 Fe1 N1 90.14(12) . . ?
N3 Fe1 N6 79.52(11) . . ?
C17 Fe1 N6 101.59(13) . . ?
C16 Fe1 N6 89.46(12) . . ?
C18 Fe1 N6 91.68(12) . . ?
N1 Fe1 N6 159.69(11) . . ?
O3 K1 O2 88.93(12) . . ?
O3 K1 N4 117.42(10) . . ?
O2 K1 N4 135.63(9) . . ?
O3 K1 N8 72.24(11) . . ?
O2 K1 N8 160.59(9) . . ?
N4 K1 N8 55.08(8) . . ?
O3 K1 N12 145.76(10) . 1_455 ?
O2 K1 N12 88.92(9) . 1_455 ?
N4 K1 N12 86.88(8) . 1_455 ?
N8 K1 N12 109.22(8) . 1_455 ?
O3 K1 O1 74.49(11) . . ?
O2 K1 O1 87.78(12) . . ?
N4 K1 O1 68.24(10) . . ?
N8 K1 O1 82.77(11) . . ?
N12 K1 O1 139.54(10) 1_455 . ?
O3 K1 O4 87.59(10) . . ?
O2 K1 O4 113.55(9) . . ?
N4 K1 O4 103.22(8) . . ?
N8 K1 O4 71.32(8) . . ?
N12 K1 O4 62.25(8) 1_455 . ?
O1 K1 O4 152.10(11) . . ?
O3 K1 N2 137.89(10) . . ?
O2 K1 N2 77.23(9) . . ?
N4 K1 N2 59.11(7) . . ?
N8 K1 N2 113.55(8) . . ?
N12 K1 N2 74.42(8) 1_455 . ?
O1 K1 N2 65.52(9) . . ?
O4 K1 N2 134.45(8) . . ?
O3 K1 H51 82.4(10) . . ?
O2 K1 H51 60.4(12) . . ?
N4 K1 H51 150.5(10) . . ?
N8 K1 H51 119.6(11) . . ?
N12 K1 H51 66.9(10) 1_455 . ?
O1 K1 H51 141.0(11) . . ?
O4 K1 H51 53.3(12) . . ?
N2 K1 H51 121.6(11) . . ?
C2 N1 C1 116.1(3) . . ?
C2 N1 Fe1 128.9(2) . . ?
C1 N1 Fe1 115.0(2) . . ?
C1 N2 C4 115.8(3) . . ?
C1 N2 K1 115.2(2) . . ?
C4 N2 K1 128.4(2) . . ?
C7 N3 C5 116.9(3) . . ?
C7 N3 Fe1 122.1(2) . . ?
C5 N3 Fe1 120.8(2) . . ?
C5 N4 C6 115.4(3) . . ?
C5 N4 K1 117.7(2) . . ?
C6 N4 K1 126.2(2) . . ?
C7 N5 C6 114.9(3) . . ?
C9 N6 C8 115.9(3) . . ?
C9 N6 Fe1 129.0(2) . . ?
C8 N6 Fe1 115.1(2) . . ?
C8 N7 C11 116.2(3) . . ?
C12 N8 C13 116.3(3) . . ?
C12 N8 K1 124.7(2) . . ?
C13 N8 K1 118.3(2) . . ?
C15 N9 C12 115.6(3) . . ?
N2 C1 N1 127.0(3) . . ?
N2 C1 C5 120.4(3) . . ?
N1 C1 C5 112.6(3) . . ?
N1 C2 C3 120.8(3) . . ?
N1 C2 H1 119.6 . . ?
C3 C2 H1 119.6 . . ?
C2 C3 C4 118.2(3) . . ?
C2 C3 H2 120.9 . . ?
C4 C3 H2 120.9 . . ?
N2 C4 C3 122.1(3) . . ?
N2 C4 H3 119.0 . . ?
C3 C4 H3 119.0 . . ?
N4 C5 N3 123.2(3) . . ?
N4 C5 C1 125.6(3) . . ?
N3 C5 C1 111.2(3) . . ?
N5 C6 N4 125.6(3) . . ?
N5 C6 C12 117.8(3) . . ?
N4 C6 C12 116.5(3) . . ?
N5 C7 N3 124.0(3) . . ?
N5 C7 C8 125.6(3) . . ?
N3 C7 C8 110.3(3) . . ?
N7 C8 N6 126.8(3) . . ?
N7 C8 C7 120.2(3) . . ?
N6 C8 C7 112.9(3) . . ?
N6 C9 C10 121.4(3) . . ?
N6 C9 H4 119.3 . . ?
C10 C9 H4 119.3 . . ?
C9 C10 C11 118.0(3) . . ?
C9 C10 H5 121.0 . . ?
C11 C10 H5 121.0 . . ?
N7 C11 C10 121.6(3) . . ?
N7 C11 H6 119.2 . . ?
C10 C11 H6 119.2 . . ?
N8 C12 N9 127.0(3) . . ?
N8 C12 C6 116.1(3) . . ?
N9 C12 C6 116.9(3) . . ?
N8 C13 C14 121.9(3) . . ?
N8 C13 H7 119.0 . . ?
C14 C13 H7 119.0 . . ?
C13 C14 C15 117.1(3) . . ?
C13 C14 H8 121.5 . . ?
C15 C14 H8 121.5 . . ?
N9 C15 C14 122.2(3) . . ?
N9 C15 H9 118.9 . . ?
C14 C15 H9 118.9 . . ?
N10 C16 Fe1 178.4(3) . . ?
N11 C17 Fe1 176.8(3) . . ?
N12 C18 Fe1 179.2(3) . . ?
C18 N12 K1 148.1(2) . 1_655 ?
K1 O1 H11 158.6(17) . . ?
K1 O1 H12 116(3) . . ?
H11 O1 H12 84(3) . . ?
K1 O2 H21 112(4) . . ?
K1 O2 H22 122(4) . . ?
H21 O2 H22 104(4) . . ?
K1 O3 H31 107(4) . . ?
K1 O3 H32 129(3) . . ?
H31 O3 H32 107(4) . . ?
K1 O4 H41 96(3) . . ?
K1 O4 H42 132(4) . . ?
H41 O4 H42 104(4) . . ?
H51 O5 H52 98(4) . . ?
H61 O6 H62 105(2) . . ?
H71 O7 H72 99(4) . . ?

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
C16 Fe1 N3 C7 89.6(2) . . . . ?
C18 Fe1 N3 C7 -90.3(2) . . . . ?
N1 Fe1 N3 C7 -179.8(3) . . . . ?
N6 Fe1 N3 C7 0.7(2) . . . . ?
C16 Fe1 N3 C5 -87.1(2) . . . . ?
C18 Fe1 N3 C5 93.0(2) . . . . ?
N1 Fe1 N3 C5 3.5(2) . . . . ?
N6 Fe1 N3 C5 -176.0(2) . . . . ?
C4 N2 C1 N1 -3.1(5) . . . . ?
K1 N2 C1 N1 169.3(2) . . . . ?
C4 N2 C1 C5 176.2(3) . . . . ?
K1 N2 C1 C5 -11.4(4) . . . . ?
C2 N1 C1 N2 4.0(5) . . . . ?
Fe1 N1 C1 N2 -177.9(3) . . . . ?
C2 N1 C1 C5 -175.4(3) . . . . ?
Fe1 N1 C1 C5 2.7(3) . . . . ?
C1 N1 C2 C3 -1.6(4) . . . . ?
Fe1 N1 C2 C3 -179.3(2) . . . . ?
N1 C2 C3 C4 -1.2(5) . . . . ?
C1 N2 C4 C3 -0.1(5) . . . . ?
K1 N2 C4 C3 -171.3(2) . . . . ?
C2 C3 C4 N2 2.1(5) . . . . ?
C6 N4 C5 N3 1.7(4) . . . . ?
K1 N4 C5 N3 -168.6(2) . . . . ?
C6 N4 C5 C1 -178.4(3) . . . . ?
K1 N4 C5 C1 11.3(4) . . . . ?
C7 N3 C5 N4 0.1(4) . . . . ?
Fe1 N3 C5 N4 176.9(2) . . . . ?
C7 N3 C5 C1 -179.9(3) . . . . ?
Fe1 N3 C5 C1 -3.0(3) . . . . ?
N2 C1 C5 N4 0.6(5) . . . . ?
N1 C1 C5 N4 -179.9(3) . . . . ?
N2 C1 C5 N3 -179.5(3) . . . . ?
N1 C1 C5 N3 0.0(4) . . . . ?
C7 N5 C6 N4 -0.2(4) . . . . ?
C7 N5 C6 C12 177.2(3) . . . . ?
C5 N4 C6 N5 -1.7(5) . . . . ?
K1 N4 C6 N5 167.6(2) . . . . ?
C5 N4 C6 C12 -179.1(3) . . . . ?
K1 N4 C6 C12 -9.8(4) . . . . ?
C6 N5 C7 N3 2.2(4) . . . . ?
C6 N5 C7 C8 -174.9(3) . . . . ?
C5 N3 C7 N5 -2.2(4) . . . . ?
Fe1 N3 C7 N5 -179.0(2) . . . . ?
C5 N3 C7 C8 175.3(2) . . . . ?
Fe1 N3 C7 C8 -1.5(3) . . . . ?
C11 N7 C8 N6 0.7(5) . . . . ?
C11 N7 C8 C7 178.7(3) . . . . ?
C9 N6 C8 N7 -1.5(5) . . . . ?
Fe1 N6 C8 N7 176.7(3) . . . . ?
C9 N6 C8 C7 -179.6(3) . . . . ?
Fe1 N6 C8 C7 -1.4(3) . . . . ?
N5 C7 C8 N7 1.0(5) . . . . ?
N3 C7 C8 N7 -176.4(3) . . . . ?
N5 C7 C8 N6 179.2(3) . . . . ?
N3 C7 C8 N6 1.8(4) . . . . ?
C8 N6 C9 C10 1.1(4) . . . . ?
Fe1 N6 C9 C10 -176.8(2) . . . . ?
N6 C9 C10 C11 0.0(5) . . . . ?
C8 N7 C11 C10 0.5(5) . . . . ?
C9 C10 C11 N7 -0.8(5) . . . . ?
C13 N8 C12 N9 1.1(5) . . . . ?
K1 N8 C12 N9 -168.8(2) . . . . ?
C13 N8 C12 C6 179.8(3) . . . . ?
K1 N8 C12 C6 9.9(4) . . . . ?
C15 N9 C12 N8 -1.3(5) . . . . ?
C15 N9 C12 C6 180.0(3) . . . . ?
N5 C6 C12 N8 -177.9(3) . . . . ?
N4 C6 C12 N8 -0.3(4) . . . . ?
N5 C6 C12 N9 0.9(4) . . . . ?
N4 C6 C12 N9 178.5(3) . . . . ?
C12 N8 C13 C14 0.4(5) . . . . ?
K1 N8 C13 C14 171.0(3) . . . . ?
N8 C13 C14 C15 -1.4(5) . . . . ?
C12 N9 C15 C14 0.1(5) . . . . ?
C13 C14 C15 N9 1.2(5) . . . . ?

_refine_diff_density_max         2.019
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.120

####################################################################### 
# 
# 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_Comp4
_database_code_depnum_ccdc_archive 'CCDC 1847520'
_audit_update_record             
;
2018-06-06 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C18 H15 Fe Gd N14 O9), 4(C H4 O), H4 O '
_chemical_formula_sum            'C20 H25 Fe Gd N14 O11.50'
_chemical_formula_weight         858.64

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'
Gd Gd -0.1653 3.9035 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_H-M_alt        'P b c m'
_space_group_name_Hall           '-P 2c 2b'

_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+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.142(3)
_cell_length_b                   10.635(2)
_cell_length_c                   19.470(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3135.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    98(2)
_cell_measurement_reflns_used    3259
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.98

_exptl_crystal_description       needle
_exptl_crystal_colour            'reddish purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_F_000             1700
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.002
_exptl_absorpt_coefficient_mu    2.639
_shelx_estimated_absorpt_T_min   0.620
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6386
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      98(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            17194
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.345
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3706
_reflns_number_gt                2704
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0528P)²+27.5077P] 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         3706
_refine_ls_number_parameters     245
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1429
_refine_ls_wR_factor_gt          0.1277
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.110
_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
Fe1 Fe 0.27991(10) 0.750000 0.500000 0.0209(3) Uani 1 2 d S T P . .
Gd1 Gd 0.29179(3) 0.52988(5) 0.250000 0.01638(15) Uani 1 2 d S T P . .
N1 N 0.4026(6) 0.750000 0.500000 0.0214(19) Uani 1 2 d S T P . .
N2 N 0.5357(5) 0.8384(7) 0.4618(3) 0.0320(16) Uani 1 1 d . . . . .
N3 N 0.3031(4) 0.8940(6) 0.4386(3) 0.0256(14) Uani 1 1 d . . . . .
N4 N 0.4222(5) 1.0072(8) 0.3847(4) 0.047(2) Uani 1 1 d . . . . .
N5 N 0.7128(5) 0.8288(7) 0.4557(3) 0.0360(17) Uani 1 1 d . . . . .
N6 N 0.2694(6) 0.5983(7) 0.3670(4) 0.050(2) Uani 1 1 d . . . . .
N7 N 0.0808(9) 0.750000 0.500000 0.073(4) Uani 1 2 d S T P . .
N8 N 0.1759(6) 0.3119(9) 0.250000 0.0228(19) Uani 1 2 d S T P . .
N9 N 0.4047(6) 0.7521(10) 0.250000 0.031(2) Uani 1 2 d S T P . .
C1 C 0.4484(5) 0.8346(8) 0.4638(4) 0.0291(18) Uani 1 1 d . . . . .
C2 C 0.5758(8) 0.750000 0.500000 0.030(3) Uani 1 2 d S T P . .
C3 C 0.3888(6) 0.9192(8) 0.4261(4) 0.0325(19) Uani 1 1 d . . . . .
C4 C 0.2446(6) 0.9663(9) 0.4036(4) 0.0359(19) Uani 1 1 d . . . . .
H1 H 0.183140 0.951888 0.409385 0.043 Uiso 1 1 calc R U . . .
C5 C 0.2725(7) 1.0606(9) 0.3596(5) 0.049(3) Uani 1 1 d . . . . .
H2 H 0.231130 1.112879 0.336507 0.059 Uiso 1 1 calc R U . . .
C6 C 0.3628(7) 1.0764(11) 0.3503(6) 0.056(3) Uani 1 1 d . . . . .
H3 H 0.383043 1.137857 0.318589 0.067 Uiso 1 1 calc R U . . .
C7 C 0.6757(8) 0.750000 0.500000 0.030(3) Uani 1 2 d S T P . .
C8 C 0.8012(6) 0.8293(8) 0.4572(4) 0.0337(19) Uani 1 1 d . . . . .
H4 H 0.832288 0.885637 0.428095 0.040 Uiso 1 1 calc R U . . .
C9 C 0.8489(8) 0.750000 0.500000 0.037(3) Uani 1 2 d S T P . .
H5 H 0.911636 0.750000 0.500001 0.045 Uiso 1 2 calc R U P . .
C10 C 0.2733(6) 0.6496(8) 0.4188(4) 0.033(2) Uani 1 1 d . . . . .
C11 C 0.1553(10) 0.750000 0.500000 0.050(4) Uani 1 2 d S T P . .
O1 O 0.2021(7) 0.3605(9) 0.1981(3) 0.101(4) Uani 1 1 d . . . . .
O2 O 0.1306(6) 0.2170(8) 0.250000 0.039(2) Uani 1 2 d S T P . .
O3 O 0.4365(5) 0.6409(9) 0.250000 0.048(3) Uani 1 2 d S T P . .
O4 O 0.3256(6) 0.7593(8) 0.250000 0.046(3) Uani 1 2 d S T P . .
O5 O 0.4492(7) 0.8465(10) 0.250000 0.094(5) Uani 1 2 d S T P . .
O6 O 0.3848(5) 0.4032(10) 0.3225(4) 0.081(3) Uani 1 1 d D . . . .
H61 H 0.421(8) 0.462(9) 0.326(6) 0.097 Uiso 1 1 d D U . . .
H62 H 0.372(8) 0.386(11) 0.363(2) 0.097 Uiso 1 1 d D U . . .
O7 O 0.1498(5) 0.6318(9) 0.250000 0.043(2) Uani 1 2 d DS T P . .
H71 H 0.104(3) 0.590(4) 0.250000 0.051 Uiso 1 2 d DS U P . .
H72 H 0.121997 0.710237 0.250000 0.051 Uiso 1 2 d DS U P . .
O8 O 0.0208(18) 0.000(3) 0.3567(18) 0.39(2) Uani 1 1 d D . . . .
H9 H 0.051444 -0.010626 0.392212 0.587 Uiso 1 1 calc DR U . . .
C12 C -0.0390(18) 0.096(3) 0.3681(10) 0.46(5) Uani 1 1 d D . . . .
H10 H -0.027291 0.165347 0.336020 0.695 Uiso 1 1 calc DR U . . .
H11 H -0.032912 0.126806 0.415351 0.695 Uiso 1 1 calc R U . . .
H12 H -0.099080 0.064780 0.360945 0.695 Uiso 1 1 calc DR U . . .
O9 O 0.2865(12) 0.9729(18) 0.2762(8) 0.013(3) Uiso 0.25 1 d D . P . .
H91 H 0.331(2) 0.979(10) 0.250000 0.016 Uiso 1 2 d DS U P . .
H92 H 0.244(3) 0.956(9) 0.250000 0.016 Uiso 1 2 d DS U 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
Fe1 N1 1.858(9) . ?
Fe1 C11 1.887(15) . ?
Fe1 C10 1.910(8) 3_566 ?
Fe1 C10 1.910(8) . ?
Fe1 N3 1.974(6) . ?
Fe1 N3 1.974(6) 3_566 ?
Gd1 O6 2.407(7) . ?
Gd1 O6 2.407(7) 6_556 ?
Gd1 O7 2.408(8) . ?
Gd1 N6 2.416(7) . ?
Gd1 N6 2.416(7) 6_556 ?
Gd1 O1 2.471(7) . ?
Gd1 O1 2.472(7) 6_556 ?
Gd1 O3 2.489(8) . ?
Gd1 O4 2.493(8) . ?
Gd1 N8 2.907(9) . ?
Gd1 N9 2.917(10) . ?
Gd1 H61 2.55(13) . ?
N1 C1 1.336(9) . ?
N1 C1 1.336(9) 3_566 ?
N2 C1 1.323(10) . ?
N2 C2 1.344(8) . ?
N3 C3 1.348(11) . ?
N3 C4 1.356(10) . ?
N4 C3 1.335(11) . ?
N4 C6 1.342(12) . ?
N5 C7 1.328(8) . ?
N5 C8 1.338(10) . ?
N6 C10 1.149(10) . ?
N7 C11 1.128(17) . ?
N8 O1 1.203(8) . ?
N8 O1 1.203(8) 6_556 ?
N8 O2 1.221(12) . ?
N9 O4 1.201(12) . ?
N9 O5 1.208(13) . ?
N9 O3 1.277(13) . ?
C1 C3 1.470(11) . ?
C2 C7 1.513(16) . ?
C4 C5 1.385(13) . ?
C4 H1 0.9500 . ?
C5 C6 1.390(14) . ?
C5 H2 0.9500 . ?
C6 H3 0.9500 . ?
C8 C9 1.388(10) . ?
C8 H4 0.9500 . ?
C9 H5 0.9500 . ?
O6 H61 0.83(2) . ?
O6 H62 0.83(2) . ?
O7 H71 0.82(2) . ?
O7 H72 0.934(9) . ?
O8 C12 1.381(18) . ?
O8 H9 0.8400 . ?
C12 H10 0.9800 . ?
C12 H11 0.9800 . ?
C12 H12 0.9800 . ?
O9 O9 1.02(3) 6_556 ?
O9 H91 0.845(18) . ?
O9 H92 0.844(18) . ?

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
N1 Fe1 C11 180.0 . . ?
N1 Fe1 C10 93.0(3) . 3_566 ?
C11 Fe1 C10 87.0(3) . 3_566 ?
N1 Fe1 C10 93.0(3) . . ?
C11 Fe1 C10 87.0(3) . . ?
C10 Fe1 C10 174.0(6) 3_566 . ?
N1 Fe1 N3 79.77(19) . . ?
C11 Fe1 N3 100.23(19) . . ?
C10 Fe1 N3 94.4(3) 3_566 . ?
C10 Fe1 N3 86.7(3) . . ?
N1 Fe1 N3 79.77(19) . 3_566 ?
C11 Fe1 N3 100.23(19) . 3_566 ?
C10 Fe1 N3 86.7(3) 3_566 3_566 ?
C10 Fe1 N3 94.4(3) . 3_566 ?
N3 Fe1 N3 159.5(4) . 3_566 ?
O6 Gd1 O6 71.8(4) . 6_556 ?
O6 Gd1 O7 140.78(19) . . ?
O6 Gd1 O7 140.78(19) 6_556 . ?
O6 Gd1 N6 72.4(3) . . ?
O6 Gd1 N6 143.5(3) 6_556 . ?
O7 Gd1 N6 74.9(2) . . ?
O6 Gd1 N6 143.5(3) . 6_556 ?
O6 Gd1 N6 72.4(3) 6_556 6_556 ?
O7 Gd1 N6 74.9(2) . 6_556 ?
N6 Gd1 N6 141.2(4) . 6_556 ?
O6 Gd1 O1 98.8(4) . . ?
O6 Gd1 O1 71.0(3) 6_556 . ?
O7 Gd1 O1 80.7(4) . . ?
N6 Gd1 O1 121.9(3) . . ?
N6 Gd1 O1 75.9(3) 6_556 . ?
O6 Gd1 O1 70.9(3) . 6_556 ?
O6 Gd1 O1 98.8(4) 6_556 6_556 ?
O7 Gd1 O1 80.7(4) . 6_556 ?
N6 Gd1 O1 75.9(3) . 6_556 ?
N6 Gd1 O1 121.9(3) 6_556 6_556 ?
O1 Gd1 O1 48.3(3) . 6_556 ?
O6 Gd1 O3 75.5(3) . . ?
O6 Gd1 O3 75.5(3) 6_556 . ?
O7 Gd1 O3 124.9(3) . . ?
N6 Gd1 O3 88.9(2) . . ?
N6 Gd1 O3 88.9(2) 6_556 . ?
O1 Gd1 O3 146.0(3) . . ?
O1 Gd1 O3 146.0(3) 6_556 . ?
O6 Gd1 O4 115.3(3) . . ?
O6 Gd1 O4 115.3(3) 6_556 . ?
O7 Gd1 O4 75.1(3) . . ?
N6 Gd1 O4 74.6(2) . . ?
N6 Gd1 O4 74.6(2) 6_556 . ?
O1 Gd1 O4 145.7(3) . . ?
O1 Gd1 O4 145.7(3) 6_556 . ?
O3 Gd1 O4 49.8(3) . . ?
O6 Gd1 N8 84.6(3) . . ?
O6 Gd1 N8 84.6(3) 6_556 . ?
O7 Gd1 N8 79.6(3) . . ?
N6 Gd1 N8 98.9(2) . . ?
N6 Gd1 N8 98.9(2) 6_556 . ?
O1 Gd1 N8 24.14(16) . . ?
O1 Gd1 N8 24.14(16) 6_556 . ?
O3 Gd1 N8 155.4(3) . . ?
O4 Gd1 N8 154.7(3) . . ?
O6 Gd1 N9 96.3(3) . . ?
O6 Gd1 N9 96.3(3) 6_556 . ?
O7 Gd1 N9 99.1(3) . . ?
N6 Gd1 N9 80.7(2) . . ?
N6 Gd1 N9 80.7(2) 6_556 . ?
O1 Gd1 N9 155.84(16) . . ?
O1 Gd1 N9 155.84(16) 6_556 . ?
O3 Gd1 N9 25.8(3) . . ?
O4 Gd1 N9 24.0(3) . . ?
N8 Gd1 N9 178.8(3) . . ?
O6 Gd1 H61 19.1(11) . . ?
O6 Gd1 H61 75(3) 6_556 . ?
O7 Gd1 H61 144(3) . . ?
N6 Gd1 H61 69(3) . . ?
N6 Gd1 H61 138(2) 6_556 . ?
O1 Gd1 H61 116.9(16) . . ?
O1 Gd1 H61 88.7(13) 6_556 . ?
O3 Gd1 H61 57.4(12) . . ?
O4 Gd1 H61 96.8(14) . . ?
N8 Gd1 H61 103.7(11) . . ?
N9 Gd1 H61 77.3(11) . . ?
C1 N1 C1 117.5(9) . 3_566 ?
C1 N1 Fe1 121.2(5) . . ?
C1 N1 Fe1 121.2(5) 3_566 . ?
C1 N2 C2 114.5(8) . . ?
C3 N3 C4 115.1(7) . . ?
C3 N3 Fe1 115.8(5) . . ?
C4 N3 Fe1 128.9(6) . . ?
C3 N4 C6 115.6(8) . . ?
C7 N5 C8 114.3(8) . . ?
C10 N6 Gd1 164.6(8) . . ?
O1 N8 O1 114.4(10) . 6_556 ?
O1 N8 O2 122.8(5) . . ?
O1 N8 O2 122.8(5) 6_556 . ?
O1 N8 Gd1 57.2(5) . . ?
O1 N8 Gd1 57.2(5) 6_556 . ?
O2 N8 Gd1 177.1(7) . . ?
O4 N9 O5 120.1(12) . . ?
O4 N9 O3 115.8(10) . . ?
O5 N9 O3 124.1(10) . . ?
O4 N9 Gd1 57.8(6) . . ?
O5 N9 Gd1 177.9(9) . . ?
O3 N9 Gd1 58.0(5) . . ?
N2 C1 N1 123.7(7) . . ?
N2 C1 C3 125.4(7) . . ?
N1 C1 C3 110.9(7) . . ?
N2 C2 N2 126.2(11) . 3_566 ?
N2 C2 C7 116.9(6) . . ?
N2 C2 C7 116.9(6) 3_566 . ?
N4 C3 N3 127.9(8) . . ?
N4 C3 C1 119.9(8) . . ?
N3 C3 C1 112.2(7) . . ?
N3 C4 C5 121.5(9) . . ?
N3 C4 H1 119.2 . . ?
C5 C4 H1 119.2 . . ?
C4 C5 C6 117.9(9) . . ?
C4 C5 H2 121.1 . . ?
C6 C5 H2 121.1 . . ?
N4 C6 C5 121.9(9) . . ?
N4 C6 H3 119.0 . . ?
C5 C6 H3 119.0 . . ?
N5 C7 N5 129.9(11) . 3_566 ?
N5 C7 C2 115.1(6) . . ?
N5 C7 C2 115.1(6) 3_566 . ?
N5 C8 C9 122.1(8) . . ?
N5 C8 H4 119.0 . . ?
C9 C8 H4 119.0 . . ?
C8 C9 C8 117.3(11) . 3_566 ?
C8 C9 H5 121.4 . . ?
C8 C9 H5 121.4 3_566 . ?
N6 C10 Fe1 174.3(7) . . ?
N7 C11 Fe1 180.0 . . ?
N8 O1 Gd1 98.7(5) . . ?
N9 O3 Gd1 96.2(6) . . ?
N9 O4 Gd1 98.2(7) . . ?
Gd1 O6 H61 90(10) . . ?
Gd1 O6 H62 123(10) . . ?
H61 O6 H62 103(5) . . ?
Gd1 O7 H71 120(4) . . ?
Gd1 O7 H72 143.6(7) . . ?
H71 O7 H72 96(4) . . ?
C12 O8 H9 109.5 . . ?
O8 C12 H10 109.5 . . ?
O8 C12 H11 109.5 . . ?
H10 C12 H11 109.5 . . ?
O8 C12 H12 109.5 . . ?
H10 C12 H12 109.5 . . ?
H11 C12 H12 109.5 . . ?
O9 O9 H91 52.9(15) 6_556 . ?
O9 O9 H92 52.9(15) 6_556 . ?
H91 O9 H92 105(3) . . ?

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
C10 Fe1 N1 C1 -94.0(5) 3_566 . . . ?
C10 Fe1 N1 C1 86.0(5) . . . . ?
N3 Fe1 N1 C1 -0.1(5) . . . . ?
N3 Fe1 N1 C1 179.9(5) 3_566 . . . ?
C10 Fe1 N1 C1 86.0(5) 3_566 . . 3_566 ?
C10 Fe1 N1 C1 -94.0(5) . . . 3_566 ?
N3 Fe1 N1 C1 179.9(5) . . . 3_566 ?
N3 Fe1 N1 C1 -0.1(5) 3_566 . . 3_566 ?
C2 N2 C1 N1 -0.6(11) . . . . ?
C2 N2 C1 C3 -179.1(7) . . . . ?
C1 N1 C1 N2 0.3(6) 3_566 . . . ?
Fe1 N1 C1 N2 -179.7(6) . . . . ?
C1 N1 C1 C3 179.0(8) 3_566 . . . ?
Fe1 N1 C1 C3 -1.0(8) . . . . ?
C1 N2 C2 N2 0.3(5) . . . 3_566 ?
C1 N2 C2 C7 -179.7(5) . . . . ?
C6 N4 C3 N3 -1.9(15) . . . . ?
C6 N4 C3 C1 177.2(9) . . . . ?
C4 N3 C3 N4 1.2(13) . . . . ?
Fe1 N3 C3 N4 177.1(8) . . . . ?
C4 N3 C3 C1 -178.0(7) . . . . ?
Fe1 N3 C3 C1 -2.1(9) . . . . ?
N2 C1 C3 N4 1.3(14) . . . . ?
N1 C1 C3 N4 -177.3(7) . . . . ?
N2 C1 C3 N3 -179.4(8) . . . . ?
N1 C1 C3 N3 1.9(10) . . . . ?
C3 N3 C4 C5 -1.4(13) . . . . ?
Fe1 N3 C4 C5 -176.6(7) . . . . ?
N3 C4 C5 C6 2.3(15) . . . . ?
C3 N4 C6 C5 2.7(16) . . . . ?
C4 C5 C6 N4 -3.0(17) . . . . ?
C8 N5 C7 N5 -1.1(6) . . . 3_566 ?
C8 N5 C7 C2 178.9(6) . . . . ?
N2 C2 C7 N5 -7.4(5) . . . . ?
N2 C2 C7 N5 172.6(5) 3_566 . . . ?
N2 C2 C7 N5 172.6(5) . . . 3_566 ?
N2 C2 C7 N5 -7.4(5) 3_566 . . 3_566 ?
C7 N5 C8 C9 2.3(11) . . . . ?
N5 C8 C9 C8 -1.2(6) . . . 3_566 ?
O1 N8 O1 Gd1 -0.5(15) 6_556 . . . ?
O2 N8 O1 Gd1 -176.5(9) . . . . ?
O4 N9 O3 Gd1 0.0 . . . . ?
O5 N9 O3 Gd1 180.0 . . . . ?
O5 N9 O4 Gd1 180.0 . . . . ?
O3 N9 O4 Gd1 0.0 . . . . ?

_refine_diff_density_max         2.055
_refine_diff_density_min         -1.890
_refine_diff_density_rms         0.195

####################################################################### 
# 
# 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_Comp3
_database_code_depnum_ccdc_archive 'CCDC 1847519'
_audit_update_record             
;
2018-06-06 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H22 Fe2 Mn N24 O2, 6(H2 O)'
_chemical_formula_sum            'C18 H17 Fe Mn0.50 N12 O4'
_chemical_formula_weight         548.75

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'
Mn Mn 0.3368 0.7283 '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                   7.096(2)
_cell_length_b                   12.045(4)
_cell_length_c                   13.365(5)
_cell_angle_alpha                75.886(4)
_cell_angle_beta                 83.782(5)
_cell_angle_gamma                75.639(4)
_cell_volume                     1071.8(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    946
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      26.61

_exptl_crystal_description       needle
_exptl_crystal_colour            'reddish purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_F_000             559
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.042
_shelx_estimated_absorpt_T_min   0.894
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6624
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            6137
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.573
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             4653
_reflns_number_gt                3212
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0404P)²+1.6880P] 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         4653
_refine_ls_number_parameters     347
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1304
_refine_ls_wR_factor_gt          0.1122
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.005
_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
Fe1 Fe 0.37735(9) 0.20584(5) 0.19006(5) 0.01151(16) Uani 1 1 d . . . . .
Mn2 Mn 0.000000 0.000000 0.000000 0.0127(2) Uani 1 2 d S . P . .
N1 N 0.1899(5) 0.2676(3) 0.2825(3) 0.0115(7) Uani 1 1 d . . . . .
N2 N 0.0392(5) 0.2441(3) 0.4497(3) 0.0143(8) Uani 1 1 d . . . . .
N3 N -0.0175(5) 0.4335(3) 0.3322(3) 0.0148(8) Uani 1 1 d . . . . .
N4 N 0.3919(5) 0.0649(3) 0.3044(3) 0.0132(8) Uani 1 1 d . . . . .
N5 N 0.2554(5) -0.0001(3) 0.4753(3) 0.0161(8) Uani 1 1 d . . . . .
N6 N 0.2856(5) 0.3688(3) 0.1081(3) 0.0140(8) Uani 1 1 d . . . . .
N7 N 0.0913(5) 0.5580(3) 0.1256(3) 0.0180(8) Uani 1 1 d . . . . .
N8 N -0.2489(5) 0.5250(3) 0.4868(3) 0.0176(8) Uani 1 1 d . . . . .
N9 N -0.2100(5) 0.3296(3) 0.5913(3) 0.0203(9) Uani 1 1 d . . . . .
N10 N 0.1380(5) 0.1140(3) 0.0620(3) 0.0178(8) Uani 1 1 d . . . . .
N11 N 0.7198(6) 0.0859(3) 0.0637(3) 0.0223(9) Uani 1 1 d . . . . .
N12 N 0.7015(6) 0.2785(3) 0.2809(3) 0.0185(8) Uani 1 1 d . . . . .
C1 C 0.1553(6) 0.2014(3) 0.3772(3) 0.0122(9) Uani 1 1 d . . . . .
C2 C -0.0452(6) 0.3600(4) 0.4236(3) 0.0143(9) Uani 1 1 d . . . . .
C3 C 0.1000(6) 0.3830(3) 0.2645(3) 0.0125(9) Uani 1 1 d . . . . .
C4 C 0.2717(6) 0.0809(3) 0.3891(3) 0.0132(9) Uani 1 1 d . . . . .
C5 C 0.5051(6) -0.0437(4) 0.3094(3) 0.0159(9) Uani 1 1 d . . . . .
H5 H 0.591956 -0.059182 0.252569 0.019 Uiso 1 1 calc R U . . .
C6 C 0.4971(6) -0.1334(4) 0.3964(3) 0.0178(10) Uani 1 1 d . . . . .
H6 H 0.577258 -0.210158 0.400369 0.021 Uiso 1 1 calc R U . . .
C7 C 0.3675(6) -0.1069(4) 0.4774(3) 0.0167(9) Uani 1 1 d . . . . .
H7 H 0.358537 -0.167772 0.536933 0.020 Uiso 1 1 calc R U . . .
C8 C 0.1606(6) 0.4430(4) 0.1600(3) 0.0139(9) Uani 1 1 d . . . . .
C9 C 0.3286(6) 0.4146(4) 0.0080(3) 0.0182(10) Uani 1 1 d . . . . .
H9 H 0.408849 0.365193 -0.033061 0.022 Uiso 1 1 calc R U . . .
C10 C 0.2572(7) 0.5325(4) -0.0357(4) 0.0212(10) Uani 1 1 d . . . . .
H10 H 0.285694 0.564380 -0.106492 0.025 Uiso 1 1 calc R U . . .
C11 C 0.1432(6) 0.6027(4) 0.0264(4) 0.0207(10) Uani 1 1 d . . . . .
H11 H 0.100265 0.684663 -0.001420 0.025 Uiso 1 1 calc R U . . .
C12 C -0.1761(6) 0.4084(4) 0.5053(3) 0.0166(9) Uani 1 1 d . . . . .
C13 C -0.3684(6) 0.5629(4) 0.5627(4) 0.0184(10) Uani 1 1 d . . . . .
H13 H -0.424170 0.644868 0.553241 0.022 Uiso 1 1 calc R U . . .
C14 C -0.4148(6) 0.4888(4) 0.6541(4) 0.0198(10) Uani 1 1 d . . . . .
H14 H -0.500187 0.517709 0.706572 0.024 Uiso 1 1 calc R U . . .
C15 C -0.3297(7) 0.3707(4) 0.6644(4) 0.0211(10) Uani 1 1 d . . . . .
H15 H -0.357471 0.316941 0.725865 0.025 Uiso 1 1 calc R U . . .
C16 C 0.2176(6) 0.1499(3) 0.1144(3) 0.0116(9) Uani 1 1 d . . . . .
C17 C 0.5889(6) 0.1358(4) 0.1069(3) 0.0151(9) Uani 1 1 d . . . . .
C18 C 0.5785(6) 0.2517(3) 0.2477(3) 0.0147(9) Uani 1 1 d . . . . .
O1 O 0.0728(6) -0.1343(3) 0.1477(3) 0.0295(8) Uani 1 1 d D . . . .
H21 H 0.010(6) -0.106(4) 0.197(3) 0.035 Uiso 1 1 d D U . . .
H22 H 0.192(3) -0.150(5) 0.154(4) 0.035 Uiso 1 1 d D U . . .
O2 O -0.2019(6) 0.7034(3) 0.2618(3) 0.0419(10) Uani 1 1 d D . . . .
H31 H -0.179(8) 0.636(3) 0.302(3) 0.050 Uiso 1 1 d D U . . .
H32 H -0.130(7) 0.690(5) 0.210(3) 0.050 Uiso 1 1 d D U . . .
O3 O -0.5018(6) 0.7945(4) 0.1324(3) 0.0391(10) Uani 1 1 d D . . . .
H41 H -0.481(8) 0.849(4) 0.080(3) 0.047 Uiso 1 1 d D U . . .
H42 H -0.398(5) 0.767(4) 0.168(4) 0.047 Uiso 1 1 d D U . . .
O4 O 0.0021(6) 0.9196(3) 0.3357(3) 0.0353(9) Uani 1 1 d D . . . .
H51 H -0.056(7) 0.9950(19) 0.328(4) 0.042 Uiso 1 1 d D U . . .
H52 H -0.029(8) 0.874(3) 0.388(3) 0.042 Uiso 1 1 d D 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
Fe1 N1 1.857(4) . ?
Fe1 C17 1.915(5) . ?
Fe1 C16 1.929(4) . ?
Fe1 C18 1.943(5) . ?
Fe1 N4 1.978(3) . ?
Fe1 N6 1.987(3) . ?
Mn2 N11 2.189(4) 2_655 ?
Mn2 N11 2.189(4) 1_455 ?
Mn2 N10 2.220(4) 2 ?
Mn2 N10 2.220(4) . ?
Mn2 O1 2.243(3) . ?
Mn2 O1 2.243(3) 2 ?
N1 C3 1.352(5) . ?
N1 C1 1.355(5) . ?
N2 C1 1.321(5) . ?
N2 C2 1.350(5) . ?
N3 C3 1.318(5) . ?
N3 C2 1.350(5) . ?
N4 C5 1.345(5) . ?
N4 C4 1.364(5) . ?
N5 C4 1.330(5) . ?
N5 C7 1.330(5) . ?
N6 C9 1.350(5) . ?
N6 C8 1.357(5) . ?
N7 C8 1.332(5) . ?
N7 C11 1.351(6) . ?
N8 C12 1.341(5) . ?
N8 C13 1.343(6) . ?
N9 C15 1.330(6) . ?
N9 C12 1.342(5) . ?
N10 C16 1.163(5) . ?
N11 C17 1.155(6) . ?
N12 C18 1.165(5) . ?
C1 C4 1.461(6) . ?
C2 C12 1.489(6) . ?
C3 C8 1.480(6) . ?
C5 C6 1.388(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.387(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C9 C10 1.385(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(7) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C13 C14 1.387(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O1 H21 0.846(19) . ?
O1 H22 0.829(19) . ?
O2 H31 0.845(19) . ?
O2 H32 0.837(19) . ?
O3 H41 0.864(19) . ?
O3 H42 0.870(19) . ?
O4 H51 0.885(19) . ?
O4 H52 0.822(19) . ?

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
N1 Fe1 C17 173.82(17) . . ?
N1 Fe1 C16 99.96(16) . . ?
C17 Fe1 C16 84.76(18) . . ?
N1 Fe1 C18 91.10(17) . . ?
C17 Fe1 C18 84.24(18) . . ?
C16 Fe1 C18 168.92(18) . . ?
N1 Fe1 N4 80.17(14) . . ?
C17 Fe1 N4 95.82(16) . . ?
C16 Fe1 N4 91.36(15) . . ?
C18 Fe1 N4 91.01(15) . . ?
N1 Fe1 N6 79.56(14) . . ?
C17 Fe1 N6 104.54(16) . . ?
C16 Fe1 N6 90.27(15) . . ?
C18 Fe1 N6 91.27(15) . . ?
N4 Fe1 N6 159.63(15) . . ?
N11 Mn2 N11 180.0(3) 2_655 1_455 ?
N11 Mn2 N10 88.11(14) 2_655 2 ?
N11 Mn2 N10 91.89(14) 1_455 2 ?
N11 Mn2 N10 91.89(14) 2_655 . ?
N11 Mn2 N10 88.11(14) 1_455 . ?
N10 Mn2 N10 180.0 2 . ?
N11 Mn2 O1 86.43(14) 2_655 . ?
N11 Mn2 O1 93.57(14) 1_455 . ?
N10 Mn2 O1 93.39(13) 2 . ?
N10 Mn2 O1 86.61(13) . . ?
N11 Mn2 O1 93.57(14) 2_655 2 ?
N11 Mn2 O1 86.43(14) 1_455 2 ?
N10 Mn2 O1 86.61(13) 2 2 ?
N10 Mn2 O1 93.39(13) . 2 ?
O1 Mn2 O1 180.0 . 2 ?
C3 N1 C1 116.6(4) . . ?
C3 N1 Fe1 122.1(3) . . ?
C1 N1 Fe1 120.8(3) . . ?
C1 N2 C2 115.4(4) . . ?
C3 N3 C2 114.6(4) . . ?
C5 N4 C4 116.3(4) . . ?
C5 N4 Fe1 128.4(3) . . ?
C4 N4 Fe1 115.3(3) . . ?
C4 N5 C7 115.8(4) . . ?
C9 N6 C8 116.1(4) . . ?
C9 N6 Fe1 128.7(3) . . ?
C8 N6 Fe1 115.1(3) . . ?
C8 N7 C11 115.6(4) . . ?
C12 N8 C13 115.0(4) . . ?
C15 N9 C12 116.9(4) . . ?
C16 N10 Mn2 163.3(3) . . ?
C17 N11 Mn2 169.6(4) . 1_655 ?
N2 C1 N1 123.3(4) . . ?
N2 C1 C4 125.5(4) . . ?
N1 C1 C4 111.1(4) . . ?
N3 C2 N2 125.6(4) . . ?
N3 C2 C12 118.8(4) . . ?
N2 C2 C12 115.6(4) . . ?
N3 C3 N1 124.4(4) . . ?
N3 C3 C8 126.0(4) . . ?
N1 C3 C8 109.5(4) . . ?
N5 C4 N4 126.5(4) . . ?
N5 C4 C1 121.0(4) . . ?
N4 C4 C1 112.5(3) . . ?
N4 C5 C6 121.0(4) . . ?
N4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 117.5(4) . . ?
C7 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
N5 C7 C6 122.9(4) . . ?
N5 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
N7 C8 N6 126.8(4) . . ?
N7 C8 C3 120.2(4) . . ?
N6 C8 C3 113.0(3) . . ?
N6 C9 C10 120.9(4) . . ?
N6 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 118.2(4) . . ?
C11 C10 H10 120.9 . . ?
C9 C10 H10 120.9 . . ?
N7 C11 C10 121.9(4) . . ?
N7 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
N8 C12 N9 126.2(4) . . ?
N8 C12 C2 117.9(4) . . ?
N9 C12 C2 115.9(4) . . ?
N8 C13 C14 123.5(4) . . ?
N8 C13 H13 118.3 . . ?
C14 C13 H13 118.3 . . ?
C15 C14 C13 116.1(4) . . ?
C15 C14 H14 121.9 . . ?
C13 C14 H14 121.9 . . ?
N9 C15 C14 122.3(4) . . ?
N9 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
N10 C16 Fe1 172.9(4) . . ?
N11 C17 Fe1 174.4(4) . . ?
N12 C18 Fe1 178.8(4) . . ?
Mn2 O1 H21 108(4) . . ?
Mn2 O1 H22 109(4) . . ?
H21 O1 H22 112(4) . . ?
H31 O2 H32 101(4) . . ?
H41 O3 H42 109(4) . . ?
H51 O4 H52 118(4) . . ?

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
C16 Fe1 N1 C3 -95.8(3) . . . . ?
C18 Fe1 N1 C3 83.7(3) . . . . ?
N4 Fe1 N1 C3 174.6(3) . . . . ?
N6 Fe1 N1 C3 -7.4(3) . . . . ?
C16 Fe1 N1 C1 92.8(3) . . . . ?
C18 Fe1 N1 C1 -87.7(3) . . . . ?
N4 Fe1 N1 C1 3.1(3) . . . . ?
N6 Fe1 N1 C1 -178.8(3) . . . . ?
C2 N2 C1 N1 0.1(6) . . . . ?
C2 N2 C1 C4 176.1(4) . . . . ?
C3 N1 C1 N2 0.7(6) . . . . ?
Fe1 N1 C1 N2 172.5(3) . . . . ?
C3 N1 C1 C4 -175.8(3) . . . . ?
Fe1 N1 C1 C4 -3.9(5) . . . . ?
C3 N3 C2 N2 1.5(6) . . . . ?
C3 N3 C2 C12 -179.8(4) . . . . ?
C1 N2 C2 N3 -1.3(6) . . . . ?
C1 N2 C2 C12 180.0(4) . . . . ?
C2 N3 C3 N1 -0.6(6) . . . . ?
C2 N3 C3 C8 -178.0(4) . . . . ?
C1 N1 C3 N3 -0.4(6) . . . . ?
Fe1 N1 C3 N3 -172.1(3) . . . . ?
C1 N1 C3 C8 177.3(3) . . . . ?
Fe1 N1 C3 C8 5.6(5) . . . . ?
C7 N5 C4 N4 -0.5(6) . . . . ?
C7 N5 C4 C1 179.6(4) . . . . ?
C5 N4 C4 N5 -0.3(6) . . . . ?
Fe1 N4 C4 N5 -179.9(3) . . . . ?
C5 N4 C4 C1 179.6(3) . . . . ?
Fe1 N4 C4 C1 -0.1(4) . . . . ?
N2 C1 C4 N5 5.8(7) . . . . ?
N1 C1 C4 N5 -177.8(4) . . . . ?
N2 C1 C4 N4 -174.0(4) . . . . ?
N1 C1 C4 N4 2.4(5) . . . . ?
C4 N4 C5 C6 0.4(6) . . . . ?
Fe1 N4 C5 C6 180.0(3) . . . . ?
N4 C5 C6 C7 0.3(6) . . . . ?
C4 N5 C7 C6 1.2(6) . . . . ?
C5 C6 C7 N5 -1.2(7) . . . . ?
C11 N7 C8 N6 4.3(6) . . . . ?
C11 N7 C8 C3 -175.0(4) . . . . ?
C9 N6 C8 N7 -7.0(6) . . . . ?
Fe1 N6 C8 N7 174.0(3) . . . . ?
C9 N6 C8 C3 172.3(4) . . . . ?
Fe1 N6 C8 C3 -6.7(4) . . . . ?
N3 C3 C8 N7 -1.8(6) . . . . ?
N1 C3 C8 N7 -179.4(4) . . . . ?
N3 C3 C8 N6 178.9(4) . . . . ?
N1 C3 C8 N6 1.2(5) . . . . ?
C8 N6 C9 C10 3.9(6) . . . . ?
Fe1 N6 C9 C10 -177.2(3) . . . . ?
N6 C9 C10 C11 1.1(6) . . . . ?
C8 N7 C11 C10 1.5(6) . . . . ?
C9 C10 C11 N7 -4.0(6) . . . . ?
C13 N8 C12 N9 -1.0(6) . . . . ?
C13 N8 C12 C2 179.0(4) . . . . ?
C15 N9 C12 N8 1.2(7) . . . . ?
C15 N9 C12 C2 -178.7(4) . . . . ?
N3 C2 C12 N8 -5.0(6) . . . . ?
N2 C2 C12 N8 173.8(4) . . . . ?
N3 C2 C12 N9 174.9(4) . . . . ?
N2 C2 C12 N9 -6.3(6) . . . . ?
C12 N8 C13 C14 0.2(6) . . . . ?
N8 C13 C14 C15 0.3(7) . . . . ?
C12 N9 C15 C14 -0.6(7) . . . . ?
C13 C14 C15 N9 0.0(7) . . . . ?

_refine_diff_density_max         0.788
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.115

####################################################################### 
# 
# 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_Comp2
_database_code_depnum_ccdc_archive 'CCDC 1847518'
_audit_update_record             
;
2018-06-06 deposited with the CCDC.
2018-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H22 Fe3 N24 O2, 6(H2 O)'
_chemical_formula_sum            'C18 H17 Fe1.50 N12 O4'
_chemical_formula_weight         549.21

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'

_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                   7.036(3)
_cell_length_b                   12.005(4)
_cell_length_c                   13.309(5)
_cell_angle_alpha                76.130(4)
_cell_angle_beta                 83.693(4)
_cell_angle_gamma                75.671(5)
_cell_volume                     1055.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3252
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.47

_exptl_crystal_description       needle
_exptl_crystal_colour            'reddish purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_F_000             560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.102
_shelx_estimated_absorpt_T_min   0.667
_shelx_estimated_absorpt_T_max   0.852
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4481
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            5911
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.578
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             4538
_reflns_number_gt                3875
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.1000P)²] 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         4538
_refine_ls_number_parameters     346
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.1305
_refine_ls_wR_factor_gt          0.1229
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      0.953
_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
Fe1 Fe 0.37741(4) 0.20378(3) 0.18922(2) 0.01192(13) Uani 1 1 d . . . . .
Fe2 Fe 0.000000 0.000000 0.000000 0.01235(15) Uani 1 2 d S . P . .
N1 N 0.1862(3) 0.26683(17) 0.28162(13) 0.0141(4) Uani 1 1 d . . . . .
N2 N 0.0373(3) 0.24389(17) 0.44930(13) 0.0150(4) Uani 1 1 d . . . . .
N3 N -0.0179(3) 0.43330(18) 0.33236(14) 0.0154(4) Uani 1 1 d . . . . .
N4 N 0.3923(3) 0.06316(17) 0.30398(13) 0.0140(4) Uani 1 1 d . . . . .
N5 N 0.2547(3) -0.00082(17) 0.47532(13) 0.0161(4) Uani 1 1 d . . . . .
N6 N 0.2861(3) 0.36669(17) 0.10689(14) 0.0142(4) Uani 1 1 d . . . . .
N7 N 0.0930(3) 0.55766(18) 0.12560(14) 0.0184(5) Uani 1 1 d . . . . .
N8 N -0.2513(3) 0.52510(18) 0.48700(14) 0.0175(4) Uani 1 1 d . . . . .
N9 N -0.2065(3) 0.32988(19) 0.59189(14) 0.0196(5) Uani 1 1 d . . . . .
N10 N 0.1386(3) 0.10994(19) 0.06059(15) 0.0184(4) Uani 1 1 d . . . . .
N11 N 0.7270(3) 0.08177(19) 0.06563(15) 0.0177(5) Uani 1 1 d . . . . .
N12 N 0.7029(3) 0.27732(18) 0.28031(14) 0.0198(5) Uani 1 1 d . . . . .
C1 C 0.1536(3) 0.2001(2) 0.37618(16) 0.0146(5) Uani 1 1 d . . . . .
C2 C -0.0459(3) 0.3591(2) 0.42364(16) 0.0150(5) Uani 1 1 d . . . . .
C3 C 0.1009(3) 0.3814(2) 0.26377(16) 0.0144(5) Uani 1 1 d . . . . .
C4 C 0.2695(3) 0.0802(2) 0.38829(16) 0.0135(5) Uani 1 1 d . . . . .
C5 C 0.5079(3) -0.0450(2) 0.30974(16) 0.0162(5) Uani 1 1 d . . . . .
H5 H 0.597615 -0.060516 0.253289 0.019 Uiso 1 1 calc R U . . .
C6 C 0.4986(3) -0.1348(2) 0.39672(17) 0.0179(5) Uani 1 1 d . . . . .
H6 H 0.579508 -0.211717 0.400607 0.021 Uiso 1 1 calc R U . . .
C7 C 0.3663(3) -0.1079(2) 0.47822(16) 0.0188(5) Uani 1 1 d . . . . .
H7 H 0.355794 -0.168577 0.537884 0.023 Uiso 1 1 calc R U . . .
C8 C 0.1605(3) 0.4427(2) 0.15945(16) 0.0144(5) Uani 1 1 d . . . . .
C9 C 0.3295(3) 0.4132(2) 0.00693(16) 0.0168(5) Uani 1 1 d . . . . .
H9 H 0.410533 0.363984 -0.034737 0.020 Uiso 1 1 calc R U . . .
C10 C 0.2581(3) 0.5315(2) -0.03622(17) 0.0203(6) Uani 1 1 d . . . . .
H10 H 0.285542 0.563191 -0.107388 0.024 Uiso 1 1 calc R U . . .
C11 C 0.1456(3) 0.6027(2) 0.02677(17) 0.0213(6) Uani 1 1 d . . . . .
H11 H 0.104864 0.685135 -0.000432 0.026 Uiso 1 1 calc R U . . .
C12 C -0.1775(3) 0.4095(2) 0.50560(16) 0.0155(5) Uani 1 1 d . . . . .
C13 C -0.3712(3) 0.5646(2) 0.56241(17) 0.0182(5) Uani 1 1 d . . . . .
H13 H -0.428705 0.646572 0.552742 0.022 Uiso 1 1 calc R U . . .
C14 C -0.4143(3) 0.4892(2) 0.65479(17) 0.0198(5) Uani 1 1 d . . . . .
H14 H -0.500715 0.518078 0.707601 0.024 Uiso 1 1 calc R U . . .
C15 C -0.3269(4) 0.3718(2) 0.66628(17) 0.0216(6) Uani 1 1 d . . . . .
H15 H -0.352336 0.318534 0.728829 0.026 Uiso 1 1 calc R U . . .
C16 C 0.2188(3) 0.1463(2) 0.11233(16) 0.0141(5) Uani 1 1 d . . . . .
C17 C 0.5943(3) 0.1332(2) 0.10669(16) 0.0157(5) Uani 1 1 d . . . . .
C18 C 0.5814(3) 0.2500(2) 0.24745(15) 0.0151(5) Uani 1 1 d . . . . .
O1 O 0.0745(3) -0.13169(17) 0.14187(13) 0.0230(4) Uani 1 1 d D . . . .
H21 H 0.032(4) -0.098(3) 0.1908(18) 0.028 Uiso 1 1 d D U . . .
H22 H 0.197(3) -0.143(3) 0.140(2) 0.028 Uiso 1 1 d D U . . .
O2 O -0.2024(3) 0.7006(2) 0.26242(15) 0.0377(6) Uani 1 1 d D . . . .
H31 H -0.169(5) 0.631(2) 0.298(2) 0.045 Uiso 1 1 d D U . . .
H32 H -0.107(4) 0.704(3) 0.217(2) 0.045 Uiso 1 1 d D U . . .
O3 O -0.5031(3) 0.79810(19) 0.13105(14) 0.0306(5) Uani 1 1 d D . . . .
H41 H -0.463(4) 0.839(3) 0.0720(17) 0.037 Uiso 1 1 d D U . . .
H42 H -0.393(3) 0.770(3) 0.165(2) 0.037 Uiso 1 1 d D U . . .
O4 O -0.0010(3) 0.91897(19) 0.33303(13) 0.0279(5) Uani 1 1 d D . . . .
H51 H -0.083(4) 0.963(2) 0.364(2) 0.033 Uiso 1 1 d D U . . .
H52 H 0.036(4) 0.8550(19) 0.371(2) 0.033 Uiso 1 1 d D 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
Fe1 N1 1.8638(18) . ?
Fe1 C17 1.921(2) . ?
Fe1 C16 1.934(3) . ?
Fe1 C18 1.953(3) . ?
Fe1 N4 1.9762(18) . ?
Fe1 N6 1.986(2) . ?
Fe2 N11 2.127(2) 2_655 ?
Fe2 N11 2.127(2) 1_455 ?
Fe2 N10 2.159(2) . ?
Fe2 N10 2.159(2) 2 ?
Fe2 O1 2.1715(18) 2 ?
Fe2 O1 2.1715(18) . ?
N1 C3 1.332(3) . ?
N1 C1 1.350(2) . ?
N2 C1 1.323(3) . ?
N2 C2 1.337(3) . ?
N3 C3 1.330(3) . ?
N3 C2 1.350(3) . ?
N4 C5 1.340(3) . ?
N4 C4 1.363(2) . ?
N5 C7 1.325(3) . ?
N5 C4 1.335(3) . ?
N6 C9 1.347(3) . ?
N6 C8 1.369(3) . ?
N7 C8 1.325(3) . ?
N7 C11 1.346(3) . ?
N8 C12 1.328(3) . ?
N8 C13 1.337(3) . ?
N9 C12 1.339(3) . ?
N9 C15 1.339(3) . ?
N10 C16 1.155(3) . ?
N11 C17 1.147(3) . ?
N12 C18 1.149(3) . ?
C1 C4 1.449(3) . ?
C2 C12 1.494(3) . ?
C3 C8 1.477(2) . ?
C5 C6 1.388(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.394(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C9 C10 1.385(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C13 C14 1.394(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.370(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O1 H21 0.835(17) . ?
O1 H22 0.837(17) . ?
O2 H31 0.843(18) . ?
O2 H32 0.850(17) . ?
O3 H41 0.881(17) . ?
O3 H42 0.890(18) . ?
O4 H51 0.822(17) . ?
O4 H52 0.808(17) . ?

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
N1 Fe1 C17 173.49(9) . . ?
N1 Fe1 C16 100.36(9) . . ?
C17 Fe1 C16 84.86(10) . . ?
N1 Fe1 C18 91.41(9) . . ?
C17 Fe1 C18 83.43(10) . . ?
C16 Fe1 C18 168.23(8) . . ?
N1 Fe1 N4 80.48(8) . . ?
C17 Fe1 N4 95.58(9) . . ?
C16 Fe1 N4 91.56(9) . . ?
C18 Fe1 N4 90.72(8) . . ?
N1 Fe1 N6 79.44(8) . . ?
C17 Fe1 N6 104.56(8) . . ?
C16 Fe1 N6 90.51(9) . . ?
C18 Fe1 N6 91.32(9) . . ?
N4 Fe1 N6 159.86(8) . . ?
N11 Fe2 N11 180.00(17) 2_655 1_455 ?
N11 Fe2 N10 91.58(8) 2_655 . ?
N11 Fe2 N10 88.42(8) 1_455 . ?
N11 Fe2 N10 88.42(8) 2_655 2 ?
N11 Fe2 N10 91.58(8) 1_455 2 ?
N10 Fe2 N10 180.0 . 2 ?
N11 Fe2 O1 93.29(7) 2_655 2 ?
N11 Fe2 O1 86.71(7) 1_455 2 ?
N10 Fe2 O1 93.39(8) . 2 ?
N10 Fe2 O1 86.61(8) 2 2 ?
N11 Fe2 O1 86.71(7) 2_655 . ?
N11 Fe2 O1 93.29(7) 1_455 . ?
N10 Fe2 O1 86.61(8) . . ?
N10 Fe2 O1 93.39(8) 2 . ?
O1 Fe2 O1 180.0 2 . ?
C3 N1 C1 117.79(18) . . ?
C3 N1 Fe1 121.64(13) . . ?
C1 N1 Fe1 119.76(16) . . ?
C1 N2 C2 115.60(17) . . ?
C3 N3 C2 113.9(2) . . ?
C5 N4 C4 116.51(17) . . ?
C5 N4 Fe1 128.59(13) . . ?
C4 N4 Fe1 114.89(15) . . ?
C7 N5 C4 116.57(17) . . ?
C9 N6 C8 115.3(2) . . ?
C9 N6 Fe1 129.45(17) . . ?
C8 N6 Fe1 115.22(13) . . ?
C8 N7 C11 116.0(2) . . ?
C12 N8 C13 115.65(18) . . ?
C12 N9 C15 116.0(2) . . ?
C16 N10 Fe2 163.94(17) . . ?
C17 N11 Fe2 170.9(2) . 1_655 ?
N2 C1 N1 122.4(2) . . ?
N2 C1 C4 125.46(18) . . ?
N1 C1 C4 111.99(18) . . ?
N2 C2 N3 126.15(18) . . ?
N2 C2 C12 116.07(17) . . ?
N3 C2 C12 117.8(2) . . ?
N3 C3 N1 124.08(17) . . ?
N3 C3 C8 124.9(2) . . ?
N1 C3 C8 111.02(18) . . ?
N5 C4 N4 125.9(2) . . ?
N5 C4 C1 121.38(18) . . ?
N4 C4 C1 112.72(17) . . ?
N4 C5 C6 121.15(19) . . ?
N4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C7 117.5(2) . . ?
C5 C6 H6 121.2 . . ?
C7 C6 H6 121.2 . . ?
N5 C7 C6 122.28(18) . . ?
N5 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
N7 C8 N6 127.10(17) . . ?
N7 C8 C3 121.1(2) . . ?
N6 C8 C3 111.75(19) . . ?
N6 C9 C10 121.2(2) . . ?
N6 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C9 C10 C11 118.53(19) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
N7 C11 C10 121.4(2) . . ?
N7 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
N8 C12 N9 127.10(19) . . ?
N8 C12 C2 118.45(18) . . ?
N9 C12 C2 114.5(2) . . ?
N8 C13 C14 122.0(2) . . ?
N8 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C15 C14 C13 117.25(19) . . ?
C15 C14 H14 121.4 . . ?
C13 C14 H14 121.4 . . ?
N9 C15 C14 121.91(19) . . ?
N9 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
N10 C16 Fe1 173.96(18) . . ?
N11 C17 Fe1 173.2(2) . . ?
N12 C18 Fe1 178.98(17) . . ?
Fe2 O1 H21 107(2) . . ?
Fe2 O1 H22 103(2) . . ?
H21 O1 H22 106(3) . . ?
H31 O2 H32 102(3) . . ?
H41 O3 H42 103(2) . . ?
H51 O4 H52 111(3) . . ?

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
C16 Fe1 N1 C3 -97.23(19) . . . . ?
C18 Fe1 N1 C3 82.4(2) . . . . ?
N4 Fe1 N1 C3 172.9(2) . . . . ?
N6 Fe1 N1 C3 -8.65(19) . . . . ?
C16 Fe1 N1 C1 93.26(19) . . . . ?
C18 Fe1 N1 C1 -87.09(19) . . . . ?
N4 Fe1 N1 C1 3.40(18) . . . . ?
N6 Fe1 N1 C1 -178.2(2) . . . . ?
C2 N2 C1 N1 -0.3(3) . . . . ?
C2 N2 C1 C4 175.6(2) . . . . ?
C3 N1 C1 N2 1.8(3) . . . . ?
Fe1 N1 C1 N2 171.75(18) . . . . ?
C3 N1 C1 C4 -174.5(2) . . . . ?
Fe1 N1 C1 C4 -4.6(3) . . . . ?
C1 N2 C2 N3 -1.7(4) . . . . ?
C1 N2 C2 C12 -180.0(2) . . . . ?
C3 N3 C2 N2 1.8(4) . . . . ?
C3 N3 C2 C12 -179.9(2) . . . . ?
C2 N3 C3 N1 0.0(3) . . . . ?
C2 N3 C3 C8 -178.1(2) . . . . ?
C1 N1 C3 N3 -1.7(3) . . . . ?
Fe1 N1 C3 N3 -171.41(18) . . . . ?
C1 N1 C3 C8 176.6(2) . . . . ?
Fe1 N1 C3 C8 6.9(3) . . . . ?
C7 N5 C4 N4 -1.9(4) . . . . ?
C7 N5 C4 C1 179.6(2) . . . . ?
C5 N4 C4 N5 0.1(4) . . . . ?
Fe1 N4 C4 N5 -179.22(19) . . . . ?
C5 N4 C4 C1 178.7(2) . . . . ?
Fe1 N4 C4 C1 -0.7(3) . . . . ?
N2 C1 C4 N5 5.6(4) . . . . ?
N1 C1 C4 N5 -178.2(2) . . . . ?
N2 C1 C4 N4 -173.1(2) . . . . ?
N1 C1 C4 N4 3.2(3) . . . . ?
C4 N4 C5 C6 1.2(4) . . . . ?
Fe1 N4 C5 C6 -179.59(18) . . . . ?
N4 C5 C6 C7 -0.6(4) . . . . ?
C4 N5 C7 C6 2.5(4) . . . . ?
C5 C6 C7 N5 -1.3(4) . . . . ?
C11 N7 C8 N6 4.0(4) . . . . ?
C11 N7 C8 C3 -175.3(2) . . . . ?
C9 N6 C8 N7 -6.7(4) . . . . ?
Fe1 N6 C8 N7 173.4(2) . . . . ?
C9 N6 C8 C3 172.7(2) . . . . ?
Fe1 N6 C8 C3 -7.2(3) . . . . ?
N3 C3 C8 N7 -1.6(4) . . . . ?
N1 C3 C8 N7 -179.9(2) . . . . ?
N3 C3 C8 N6 179.0(2) . . . . ?
N1 C3 C8 N6 0.8(3) . . . . ?
C8 N6 C9 C10 3.2(3) . . . . ?
Fe1 N6 C9 C10 -176.91(18) . . . . ?
N6 C9 C10 C11 2.2(4) . . . . ?
C8 N7 C11 C10 2.2(4) . . . . ?
C9 C10 C11 N7 -5.1(4) . . . . ?
C13 N8 C12 N9 -1.7(4) . . . . ?
C13 N8 C12 C2 178.7(2) . . . . ?
C15 N9 C12 N8 1.6(4) . . . . ?
C15 N9 C12 C2 -178.8(2) . . . . ?
N2 C2 C12 N8 174.8(2) . . . . ?
N3 C2 C12 N8 -3.7(3) . . . . ?
N2 C2 C12 N9 -4.9(3) . . . . ?
N3 C2 C12 N9 176.7(2) . . . . ?
C12 N8 C13 C14 0.5(4) . . . . ?
N8 C13 C14 C15 0.7(4) . . . . ?
C12 N9 C15 C14 -0.2(4) . . . . ?
C13 C14 C15 N9 -0.8(4) . . . . ?

_refine_diff_density_max         1.019
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.099

