# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 1890216'
loop_
_audit_author_name
_audit_author_address
'Ivan Nemec'
;Department of inorganic chemistry, Palacky University
Czech Republic
;
_audit_update_record             
;
2019-01-11 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H27 Fe1 N4 O6'
_chemical_formula_weight         475.3

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   7.3393(6)
_cell_length_b                   13.1519(18)
_cell_length_c                   21.8069(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2104.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5223
_cell_measurement_theta_min      2.922
_cell_measurement_theta_max      26.126

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_F_000             996
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    0.762
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8224
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   multi-scan
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
'Goniometer KM4/Xcalibur detector: Sapphire2 (large Be window)'
_diffrn_measurement_method       
;Rotation method data acquisition using omega and phi scans
;
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4821
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.928
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3364
_reflns_number_gt                2390
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.733
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_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          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0627P)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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.55(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3364
_refine_ls_number_parameters     292
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1141
_refine_ls_wR_factor_gt          0.1063
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      1.010
_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
C1 C 0.7596(8) 0.8241(6) 0.3459(3) 0.0428(17) Uani 1 1 d . . . . .
C2 C 0.7597(8) 0.7213(6) 0.3310(3) 0.0454(18) Uani 1 1 d . . . . .
H2 H 0.7185 0.6743 0.3596 0.054 Uiso 1 1 calc R U . . .
C3 C 0.8199(8) 0.6872(6) 0.2741(3) 0.0490(19) Uani 1 1 d . . . . .
C4 C 0.8798(11) 0.7586(7) 0.2313(3) 0.061(2) Uani 1 1 d . . . . .
H4 H 0.9205 0.7370 0.1931 0.073 Uiso 1 1 calc R U . . .
C5 C 0.8792(11) 0.8596(7) 0.2450(3) 0.059(2) Uani 1 1 d . . . . .
H5 H 0.9214 0.9057 0.2159 0.070 Uiso 1 1 calc R U . . .
C6 C 0.8167(8) 0.8962(6) 0.3019(3) 0.0486(19) Uani 1 1 d . . . . .
C7 C 0.8019(8) 1.0018(6) 0.3105(3) 0.0484(14) Uani 1 1 d . . . . .
H7 H 0.8489 1.0435 0.2799 0.058 Uiso 1 1 calc R U . . .
C8A C 0.7118(12) 1.1558(6) 0.3585(4) 0.071(2) Uani 0.5 1 d . . P A 1
H8A1 H 0.7398 1.1833 0.3183 0.085 Uiso 0.5 1 calc R U P A 1
H8A2 H 0.7971 1.1844 0.3878 0.085 Uiso 0.5 1 calc R U P A 1
C8B C 0.7118(12) 1.1558(6) 0.3585(4) 0.071(2) Uani 0.5 1 d . . P A 2
H8B1 H 0.6384 1.1777 0.3239 0.085 Uiso 0.5 1 calc R U P A 2
H8B2 H 0.8319 1.1858 0.3541 0.085 Uiso 0.5 1 calc R U P A 2
C9A C 0.526(2) 1.1822(11) 0.3757(7) 0.071(3) Uani 0.611(11) 1 d . . P A 1
H9A1 H 0.4429 1.1646 0.3428 0.085 Uiso 0.611(11) 1 calc R U P A 1
H9A2 H 0.5171 1.2547 0.3832 0.085 Uiso 0.611(11) 1 calc R U P A 1
C9B C 0.621(3) 1.1954(15) 0.4206(10) 0.071(3) Uani 0.389(11) 1 d . . P A 2
H9B1 H 0.7101 1.1976 0.4534 0.085 Uiso 0.389(11) 1 calc R U P A 2
H9B2 H 0.5702 1.2629 0.4151 0.085 Uiso 0.389(11) 1 calc R U P A 2
C10A C 0.324(4) 1.118(2) 0.3999(18) 0.071(3) Uani 0.315(19) 1 d . . P A 2
H10A H 0.3580 1.1372 0.3584 0.085 Uiso 0.315(19) 1 calc R U P A 2
H10B H 0.2431 1.1711 0.4149 0.085 Uiso 0.315(19) 1 calc R U P A 2
C10B C 0.2787(18) 1.1076(11) 0.4349(8) 0.071(3) Uani 0.685(19) 1 d . . P A 1
H10C H 0.2396 1.0934 0.4765 0.085 Uiso 0.685(19) 1 calc R U P A 1
H10D H 0.2203 1.1702 0.4220 0.085 Uiso 0.685(19) 1 calc R U P A 1
C11A C 0.2203(12) 1.0269(8) 0.3960(5) 0.092(3) Uani 0.315(19) 1 d . . P A 2
H11A H 0.1431 1.0288 0.3599 0.111 Uiso 0.315(19) 1 calc R U P A 2
H11B H 0.1428 1.0205 0.4318 0.111 Uiso 0.315(19) 1 calc R U P A 2
C11B C 0.2203(12) 1.0269(8) 0.3960(5) 0.092(3) Uani 0.685(19) 1 d . . P A 1
H11C H 0.2034 1.0538 0.3549 0.111 Uiso 0.685(19) 1 calc R U P A 1
H11D H 0.1026 1.0031 0.4103 0.111 Uiso 0.685(19) 1 calc R U P A 1
C12 C 0.2784(11) 0.8466(7) 0.4221(4) 0.080(3) Uani 1 1 d . . . . .
H12A H 0.3449 0.7888 0.4060 0.095 Uiso 1 1 calc R U . . .
H12B H 0.1502 0.8368 0.4131 0.095 Uiso 1 1 calc R U . . .
C13 C 0.3049(10) 0.8524(7) 0.4894(3) 0.071(2) Uani 1 1 d . . . . .
H13A H 0.2068 0.8918 0.5075 0.085 Uiso 1 1 calc R U . . .
H13B H 0.3007 0.7845 0.5067 0.085 Uiso 1 1 calc R U . . .
C14 C 0.5445(8) 0.8863(6) 0.5578(3) 0.0484(14) Uani 1 1 d . . . . .
H14 H 0.4794 0.8439 0.5840 0.058 Uiso 1 1 calc R U . . .
C15 C 0.7074(9) 0.9292(5) 0.5821(3) 0.0466(18) Uani 1 1 d . . . . .
C16 C 0.7559(9) 0.9060(6) 0.6429(3) 0.056(2) Uani 1 1 d . . . . .
H16 H 0.6792 0.8643 0.6657 0.068 Uiso 1 1 calc R U . . .
C17 C 0.9101(10) 0.9418(6) 0.6698(3) 0.060(2) Uani 1 1 d . . . . .
H17 H 0.9372 0.9252 0.7102 0.073 Uiso 1 1 calc R U . . .
C18 C 1.0293(9) 1.0049(6) 0.6354(3) 0.052(2) Uani 1 1 d . . . . .
C19 C 0.9825(8) 1.0294(6) 0.5766(3) 0.0488(16) Uani 1 1 d . . . . .
H19 H 1.0595 1.0717 0.5543 0.059 Uiso 1 1 calc R U . . .
C20 C 0.8237(8) 0.9936(5) 0.5485(3) 0.0450(19) Uani 1 1 d . . . . .
N1 N 0.7279(7) 1.0457(5) 0.3576(2) 0.0495(15) Uani 1 1 d . . . . .
N2 N 0.4778(8) 1.1223(5) 0.4344(3) 0.0633(17) Uani 1 1 d D . . . .
H1N2 H 0.5158 1.1606 0.4708 0.076 Uiso 1 1 calc DR U . A 1
N3 N 0.3428(8) 0.9403(5) 0.3924(3) 0.0625(19) Uani 1 1 d D . . . .
H1N3 H 0.3623 0.9250 0.3489 0.075 Uiso 1 1 calc DR U . A 1
N4 N 0.4771(7) 0.8991(4) 0.5042(2) 0.0470(15) Uani 1 1 d . . . . .
O1 O 0.7102(6) 0.8501(4) 0.40139(18) 0.0534(13) Uani 1 1 d . . . . .
O1S O 0.3760(9) 0.8458(5) 0.2666(3) 0.0887(19) Uani 1 1 d D . . . .
O2 O 0.7898(6) 1.0181(4) 0.49078(18) 0.0556(12) Uani 1 1 d . . . . .
O2S O 1.4382(8) 1.1376(4) 0.5874(3) 0.0856(19) Uani 1 1 d D . . . .
O3 O 0.8181(6) 0.5880(4) 0.2588(2) 0.0624(15) Uani 1 1 d . . . . .
O4 O 1.1842(6) 1.0364(5) 0.6598(2) 0.0653(14) Uani 1 1 d D . . . .
Fe1 Fe 0.61039(13) 0.97382(8) 0.43320(4) 0.0467(3) Uani 1 1 d . . . . .
H1S1 H 0.279(5) 0.814(5) 0.276(3) 0.056 Uiso 1 1 d D U . . .
H1S2 H 1.525(5) 1.096(3) 0.584(3) 0.056 Uiso 1 1 d D U . . .
H2S2 H 1.347(5) 1.106(4) 0.602(3) 0.056 Uiso 1 1 d D U . . .
H2S1 H 0.349(7) 0.882(4) 0.236(2) 0.056 Uiso 1 1 d D U . . .
H1O4 H 1.235(8) 0.996(4) 0.685(2) 0.056 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
C1 O1 1.308(7) . ?
C1 C2 1.391(9) . ?
C1 C6 1.413(9) . ?
C2 C3 1.390(9) . ?
C3 O3 1.348(9) . ?
C3 C4 1.394(10) . ?
C4 C5 1.362(10) . ?
C5 C6 1.408(9) . ?
C6 C7 1.404(10) . ?
C7 N1 1.298(8) . ?
C8A N1 1.454(9) . ?
C8A C9A 1.454(14) . ?
C8B N1 1.454(9) . ?
C8B C9B 1.60(2) . ?
C9A N2 1.546(14) . ?
C9B N2 1.46(2) . ?
C10A N2 1.36(3) . ?
C10A C11A 1.43(3) . ?
C10B C11B 1.426(17) . ?
C10B N2 1.474(14) . ?
C11A N3 1.453(10) . ?
C11B N3 1.453(10) . ?
C12 N3 1.470(10) . ?
C12 C13 1.482(10) . ?
C13 N4 1.441(8) . ?
C14 N4 1.281(8) . ?
C14 C15 1.424(9) . ?
C15 C16 1.407(8) . ?
C15 C20 1.408(9) . ?
C16 C17 1.359(9) . ?
C17 C18 1.420(9) . ?
C18 O4 1.322(8) . ?
C18 C19 1.368(8) . ?
C19 C20 1.398(9) . ?
C20 O2 1.322(7) . ?
N1 Fe1 2.087(5) . ?
N2 Fe1 2.182(6) . ?
N3 Fe1 2.201(6) . ?
N4 Fe1 2.078(5) . ?
O1 Fe1 1.915(5) . ?
O2 Fe1 1.911(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 118.1(6) . . ?
O1 C1 C6 122.4(7) . . ?
C2 C1 C6 119.5(6) . . ?
C3 C2 C1 121.5(7) . . ?
O3 C3 C2 122.0(7) . . ?
O3 C3 C4 119.3(6) . . ?
C2 C3 C4 118.7(7) . . ?
C5 C4 C3 120.7(7) . . ?
C4 C5 C6 121.8(7) . . ?
C7 C6 C5 118.7(7) . . ?
C7 C6 C1 123.3(6) . . ?
C5 C6 C1 117.8(7) . . ?
N1 C7 C6 125.3(6) . . ?
N1 C8A C9A 108.5(9) . . ?
N1 C8B C9B 111.7(9) . . ?
C8A C9A N2 107.9(10) . . ?
N2 C9B C8B 105.2(14) . . ?
N2 C10A C11A 121(2) . . ?
C11B C10B N2 113.0(12) . . ?
C10A C11A N3 109.5(13) . . ?
C10B C11B N3 115.4(8) . . ?
N3 C12 C13 110.6(7) . . ?
N4 C13 C12 110.9(6) . . ?
N4 C14 C15 127.7(6) . . ?
C16 C15 C20 117.9(6) . . ?
C16 C15 C14 118.5(6) . . ?
C20 C15 C14 123.6(6) . . ?
C17 C16 C15 122.9(7) . . ?
C16 C17 C18 119.1(6) . . ?
O4 C18 C19 121.3(7) . . ?
O4 C18 C17 120.1(6) . . ?
C19 C18 C17 118.6(7) . . ?
C18 C19 C20 122.7(7) . . ?
O2 C20 C19 119.4(6) . . ?
O2 C20 C15 121.9(6) . . ?
C19 C20 C15 118.7(6) . . ?
C7 N1 C8B 119.2(6) . . ?
C7 N1 C8A 119.2(6) . . ?
C7 N1 Fe1 126.6(5) . . ?
C8B N1 Fe1 114.0(5) . . ?
C8A N1 Fe1 114.0(5) . . ?
C10A N2 C9B 120.6(19) . . ?
C10B N2 C9A 107.5(10) . . ?
C10A N2 Fe1 109.3(13) . . ?
C9B N2 Fe1 105.5(9) . . ?
C10B N2 Fe1 109.0(7) . . ?
C9A N2 Fe1 110.1(6) . . ?
C11B N3 C12 115.7(7) . . ?
C11A N3 C12 115.7(7) . . ?
C11B N3 Fe1 111.9(5) . . ?
C11A N3 Fe1 111.9(5) . . ?
C12 N3 Fe1 106.0(4) . . ?
C14 N4 C13 119.1(6) . . ?
C14 N4 Fe1 124.1(5) . . ?
C13 N4 Fe1 116.6(4) . . ?
C1 O1 Fe1 131.5(4) . . ?
C20 O2 Fe1 132.9(4) . . ?
O2 Fe1 O1 103.5(2) . . ?
O2 Fe1 N4 88.81(19) . . ?
O1 Fe1 N4 92.7(2) . . ?
O2 Fe1 N1 95.52(19) . . ?
O1 Fe1 N1 86.6(2) . . ?
N4 Fe1 N1 175.6(2) . . ?
O2 Fe1 N2 91.5(2) . . ?
O1 Fe1 N2 159.3(2) . . ?
N4 Fe1 N2 101.8(2) . . ?
N1 Fe1 N2 77.8(2) . . ?
O2 Fe1 N3 160.4(2) . . ?
O1 Fe1 N3 91.4(2) . . ?
N4 Fe1 N3 77.7(2) . . ?
N1 Fe1 N3 98.0(2) . . ?
N2 Fe1 N3 77.7(2) . . ?

_refine_diff_density_max         0.502
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.055


# start Validation Reply Form
_vrf_PLAT414_1b                  
;
RESPONSE: All reported problems with short contacts involving H1N2  
arose from disorder of alifatic chain, which was not possible  
to model over two positions in the case of nitrogen atom.
;
_vrf_PLAT417_1b                  
;
RESPONSE: This is due to specific arrangement of the lattice solvent molecules. 
;
_vrf_PLAT420_1b                  
;
RESPONSE: For both oxygen atoms of the lattice water molecules the second
 hydrogen atoms form O-H..pi interactions. 
;
####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 1890217'
loop_
_audit_author_name
_audit_author_address
'Ivan Nemec'
;Department of inorganic chemistry, Palacky University
Czech Republic
;
_audit_update_record             
;
2019-01-11 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C92 H88 Cr2 Fe2 N12 O17'
_chemical_formula_weight         1848.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Cr Cr 0.3210 0.6240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 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                   11.2435(6)
_cell_length_b                   13.6516(7)
_cell_length_c                   14.4148(6)
_cell_angle_alpha                96.464(4)
_cell_angle_beta                 106.508(4)
_cell_angle_gamma                93.240(4)
_cell_volume                     2098.75(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    14833
_cell_measurement_theta_min      2.514
_cell_measurement_theta_max      25.612

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_F_000             960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_absorpt_coefficient_mu    0.669
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7822
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
'CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET)
(compiled Apr 18 2008,18:17:43)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm'
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
'Goniometer KM4/Xcalibur detector: Sapphire2 (large Be window)'
_diffrn_measurement_method       
;Rotation method data acquisition using omega and phi scans
;
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14368
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.522
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7393
_reflns_number_gt                4316
_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)+(0.0656P)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         7393
_refine_ls_number_parameters     588
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1356
_refine_ls_wR_factor_gt          0.1212
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.999
_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
C1 C 0.1391(4) 0.3749(3) 0.7646(3) 0.0408(10) Uani 1 1 d . . . . .
C2 C 0.2408(4) 0.3907(3) 0.7288(3) 0.0425(10) Uani 1 1 d . . . . .
H2 H 0.2701 0.3369 0.6994 0.051 Uiso 1 1 calc R U . . .
C3 C 0.2985(4) 0.4837(3) 0.7360(3) 0.0456(11) Uani 1 1 d . . . . .
C4 C 0.2553(4) 0.5662(3) 0.7777(3) 0.0553(12) Uani 1 1 d . . . . .
H4 H 0.2924 0.6296 0.7808 0.066 Uiso 1 1 calc R U . . .
C5 C 0.1568(4) 0.5513(3) 0.8140(3) 0.0570(12) Uani 1 1 d . . . . .
H5 H 0.1284 0.6061 0.8428 0.068 Uiso 1 1 calc R U . . .
C6 C 0.0968(4) 0.4579(3) 0.8098(3) 0.0405(10) Uani 1 1 d . . . . .
C7 C -0.0055(4) 0.4494(3) 0.8480(3) 0.0485(11) Uani 1 1 d . . . . .
H7 H -0.0252 0.5077 0.8779 0.058 Uiso 1 1 calc R U . . .
C8 C -0.1812(4) 0.3810(3) 0.8850(3) 0.0559(12) Uani 1 1 d . . . . .
H8A H -0.2476 0.4079 0.8386 0.067 Uiso 1 1 calc R U . . .
H8B H -0.1565 0.4262 0.9456 0.067 Uiso 1 1 calc R U . . .
C9 C -0.2265(4) 0.2800(4) 0.9030(4) 0.0619(13) Uani 1 1 d . . . . .
H9A H -0.1703 0.2615 0.9617 0.074 Uiso 1 1 calc R U . . .
H9B H -0.3087 0.2818 0.9118 0.074 Uiso 1 1 calc R U . . .
C10 C -0.3361(4) 0.2135(4) 0.7301(4) 0.0664(14) Uani 1 1 d . . . . .
H10A H -0.3504 0.2822 0.7243 0.080 Uiso 1 1 calc R U . . .
H10B H -0.4114 0.1792 0.7352 0.080 Uiso 1 1 calc R U . . .
C11 C -0.3030(4) 0.1668(4) 0.6429(4) 0.0663(14) Uani 1 1 d . . . . .
H11A H -0.2982 0.0963 0.6451 0.080 Uiso 1 1 calc R U . . .
H11B H -0.3663 0.1757 0.5835 0.080 Uiso 1 1 calc R U . . .
C12 C -0.1219(4) 0.1613(4) 0.5765(3) 0.0614(13) Uani 1 1 d . . . . .
H12A H -0.0529 0.2033 0.5702 0.074 Uiso 1 1 calc R U . . .
H12B H -0.1818 0.1446 0.5124 0.074 Uiso 1 1 calc R U . . .
C13 C -0.0749(4) 0.0672(4) 0.6155(3) 0.0619(13) Uani 1 1 d . . . . .
H13A H -0.1426 0.0149 0.5978 0.074 Uiso 1 1 calc R U . . .
H13B H -0.0104 0.0455 0.5876 0.074 Uiso 1 1 calc R U . . .
C14 C 0.0481(4) 0.0274(3) 0.7656(3) 0.0458(11) Uani 1 1 d . . . . .
H14 H 0.0667 -0.0243 0.7257 0.055 Uiso 1 1 calc R U . . .
C15 C 0.1034(4) 0.0310(3) 0.8687(3) 0.0400(10) Uani 1 1 d . . . . .
C16 C 0.1743(4) -0.0464(3) 0.9017(3) 0.0490(11) Uani 1 1 d . . . . .
H16 H 0.1845 -0.0965 0.8561 0.059 Uiso 1 1 calc R U . . .
C17 C 0.2289(4) -0.0503(3) 0.9986(3) 0.0462(11) Uani 1 1 d . . . . .
H17 H 0.2763 -0.1020 1.0184 0.055 Uiso 1 1 calc R U . . .
C18 C 0.2128(4) 0.0239(3) 1.0676(3) 0.0425(10) Uani 1 1 d . . . . .
C19 C 0.1442(4) 0.1005(3) 1.0374(3) 0.0429(10) Uani 1 1 d . . . . .
H19 H 0.1345 0.1500 1.0839 0.051 Uiso 1 1 calc R U . . .
C20 C 0.0887(4) 0.1061(3) 0.9387(3) 0.0406(10) Uani 1 1 d . . . . .
C67 C 0.5728(4) 0.0453(3) 0.3641(3) 0.0440(11) Uani 1 1 d . . . . .
C68 C 0.6151(4) -0.0276(3) 0.4233(3) 0.0492(11) Uani 1 1 d . . . . .
H68 H 0.6015 -0.0249 0.4841 0.059 Uiso 1 1 calc R U . . .
C69 C 0.6756(4) -0.1019(3) 0.3931(4) 0.0619(13) Uani 1 1 d . . . . .
H69 H 0.7048 -0.1486 0.4343 0.074 Uiso 1 1 calc R U . . .
C70 C 0.6946(5) -0.1099(4) 0.3027(5) 0.0714(15) Uani 1 1 d . . . . .
H70 H 0.7375 -0.1607 0.2831 0.086 Uiso 1 1 calc R U . . .
C71 C 0.6499(4) -0.0423(4) 0.2425(4) 0.0646(14) Uani 1 1 d . . . . .
H71 H 0.6594 -0.0491 0.1801 0.078 Uiso 1 1 calc R U . . .
C72 C 0.5907(4) 0.0362(3) 0.2715(3) 0.0484(11) Uani 1 1 d . . . . .
C73A C 0.5199(10) 0.1347(8) 0.1439(9) 0.045(2) Uani 0.466(6) 1 d . . P A 1
H73A H 0.5340 0.0827 0.1020 0.054 Uiso 0.466(6) 1 calc R U P A 1
C73B C 0.5540(8) 0.0887(8) 0.1890(7) 0.045(2) Uani 0.534(6) 1 d . . P A 2
H73B H 0.5646 0.0622 0.1298 0.054 Uiso 0.534(6) 1 calc R U P A 2
C74 C 0.4716(4) 0.2255(4) 0.1088(3) 0.0521(12) Uani 1 1 d . . . . .
C75 C 0.4588(5) 0.2059(4) 0.0097(4) 0.0764(15) Uani 1 1 d . . . . .
H75 H 0.4743 0.1440 -0.0159 0.092 Uiso 1 1 calc R U . . .
C76 C 0.4239(6) 0.2757(5) -0.0510(4) 0.0925(19) Uani 1 1 d . . . . .
H76 H 0.4156 0.2615 -0.1173 0.111 Uiso 1 1 calc R U . . .
C77 C 0.4013(5) 0.3669(5) -0.0129(4) 0.0862(18) Uani 1 1 d . . . . .
H77 H 0.3778 0.4149 -0.0539 0.103 Uiso 1 1 calc R U . . .
C78 C 0.4128(4) 0.3884(4) 0.0843(3) 0.0646(14) Uani 1 1 d . . . . .
H78 H 0.3976 0.4508 0.1089 0.078 Uiso 1 1 calc R U . . .
C79 C 0.4474(4) 0.3170(3) 0.1475(3) 0.0484(11) Uani 1 1 d . . . . .
C80 C 0.2388(4) 0.2200(3) 0.3318(3) 0.0419(10) Uani 1 1 d . . . . .
C81 C 0.1103(4) 0.1963(4) 0.3057(4) 0.0660(14) Uani 1 1 d . . . . .
H81 H 0.0690 0.1573 0.2469 0.079 Uiso 1 1 calc R U . . .
C82 C 0.0442(5) 0.2321(4) 0.3694(5) 0.0745(16) Uani 1 1 d . . . . .
H82 H -0.0415 0.2165 0.3534 0.089 Uiso 1 1 calc R U . . .
C83 C 0.1071(5) 0.2907(4) 0.4561(4) 0.0639(14) Uani 1 1 d . . . . .
H83 H 0.0635 0.3121 0.4995 0.077 Uiso 1 1 calc R U . . .
C84 C 0.2304(5) 0.3175(3) 0.4791(3) 0.0567(12) Uani 1 1 d . . . . .
H84 H 0.2702 0.3595 0.5364 0.068 Uiso 1 1 calc R U . . .
C85 C 0.2963(4) 0.2832(3) 0.4189(3) 0.0401(10) Uani 1 1 d D . . . .
C86A C 0.4980(4) 0.3655(4) 0.5073(4) 0.0449(14) Uani 0.901(7) 1 d D . P A 1
H86A H 0.4602 0.3931 0.5524 0.054 Uiso 0.901(7) 1 calc R U P A 1
C87 C 0.6254(4) 0.3907(3) 0.5238(3) 0.0493(12) Uani 1 1 d D . . . .
C88 C 0.6867(5) 0.4587(3) 0.6090(3) 0.0604(13) Uani 1 1 d . . . . .
H88 H 0.6412 0.4824 0.6501 0.072 Uiso 1 1 calc R U . . .
C89 C 0.8088(5) 0.4896(4) 0.6316(4) 0.0710(15) Uani 1 1 d . . . . .
H89 H 0.8466 0.5331 0.6882 0.085 Uiso 1 1 calc R U . . .
C90 C 0.8763(5) 0.4574(4) 0.5722(4) 0.0667(14) Uani 1 1 d . . . . .
H90 H 0.9603 0.4795 0.5879 0.080 Uiso 1 1 calc R U . . .
C91 C 0.8227(4) 0.3934(3) 0.4900(4) 0.0546(12) Uani 1 1 d . . . . .
H91 H 0.8714 0.3738 0.4500 0.065 Uiso 1 1 calc R U . . .
C92 C 0.6976(4) 0.3552(3) 0.4624(3) 0.0453(11) Uani 1 1 d . . . . .
Cr1 Cr 0.48643(6) 0.23258(5) 0.32554(5) 0.0417(2) Uani 1 1 d . . . . .
Fe1 Fe -0.05025(5) 0.22682(4) 0.79022(4) 0.0436(2) Uani 1 1 d . . . . .
N1 N -0.0748(3) 0.3700(3) 0.8463(2) 0.0456(9) Uani 1 1 d . . . . .
N3 N -0.2308(3) 0.2068(3) 0.8177(3) 0.0516(10) Uani 1 1 d . . . . .
H1N3 H -0.2393 0.1405 0.8363 0.062 Uiso 1 1 calc R U . . .
N2 N -0.1807(3) 0.2144(3) 0.6436(2) 0.0518(10) Uani 1 1 d . . . . .
H1N2 H -0.1925 0.2812 0.6260 0.062 Uiso 1 1 calc R U . . .
N4 N -0.0245(3) 0.0883(3) 0.7229(2) 0.0464(9) Uani 1 1 d . . . . .
N11A N 0.5417(8) 0.1309(6) 0.2357(8) 0.0357(14) Uani 0.466(6) 1 d . . P A 1
N11B N 0.5069(7) 0.1713(6) 0.1951(5) 0.0357(14) Uani 0.534(6) 1 d . . P A 2
N12A N 0.4307(3) 0.3061(3) 0.4329(3) 0.0365(12) Uani 0.901(7) 1 d D . P A 1
O2 O 0.0860(3) 0.2847(2) 0.7547(2) 0.0516(8) Uani 1 1 d . . . . .
O1 O 0.0249(3) 0.1826(2) 0.91364(19) 0.0514(8) Uani 1 1 d D . . . .
O3 O 0.3972(3) 0.4899(2) 0.7004(2) 0.0567(8) Uani 1 1 d . . . . .
H1O3 H 0.4331 0.5458 0.7166 0.085 Uiso 1 1 calc R U . . .
O4 O 0.2658(2) 0.0148(2) 1.1627(2) 0.0525(8) Uani 1 1 d . . . . .
H1O4 H 0.2701 0.0683 1.1963 0.079 Uiso 1 1 calc R U . . .
O7 O 0.5193(3) 0.1196(2) 0.3953(2) 0.0639(9) Uani 1 1 d . . . . .
O9 O 0.4591(3) 0.3387(2) 0.2423(2) 0.0590(8) Uani 1 1 d . . . . .
O6 O 0.3081(2) 0.1861(2) 0.2759(2) 0.0491(7) Uani 1 1 d . . . . .
O8 O 0.6554(2) 0.2905(2) 0.3834(2) 0.0542(8) Uani 1 1 d . . . . .
O1S O 0.0999(11) 0.3406(5) 1.0885(7) 0.124(4) Uani 0.5 1 d D . P . .
C86B C 0.402(2) 0.332(3) 0.482(2) 0.0449(14) Uani 0.099(7) 1 d D . P A 2
H86B H 0.4000 0.3655 0.5414 0.054 Uiso 0.099(7) 1 calc R U P A 2
N12B N 0.505(2) 0.330(3) 0.460(2) 0.0365(12) Uani 0.099(7) 1 d D . P A 2
H2S1 H 0.050(3) 0.296(2) 1.0433(19) 0.044 Uiso 1 1 d D U . . .
H1S1 H 0.142(3) 0.366(3) 1.063(3) 0.044 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
C1 O2 1.312(5) . ?
C1 C2 1.397(5) . ?
C1 C6 1.417(5) . ?
C2 C3 1.372(5) . ?
C2 H2 0.9300 . ?
C3 O3 1.351(5) . ?
C3 C4 1.394(6) . ?
C4 C5 1.367(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.413(5) . ?
C7 N1 1.293(5) . ?
C7 H7 0.9300 . ?
C8 N1 1.466(5) . ?
C8 C9 1.518(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N3 1.482(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N3 1.480(5) . ?
C10 C11 1.497(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.484(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N2 1.469(6) . ?
C12 C13 1.522(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N4 1.477(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 N4 1.282(5) . ?
C14 C15 1.433(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.404(5) . ?
C15 C20 1.405(5) . ?
C16 C17 1.366(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.395(6) . ?
C17 H17 0.9300 . ?
C18 O4 1.353(4) . ?
C18 C19 1.372(5) . ?
C19 C20 1.395(5) . ?
C19 H19 0.9300 . ?
C20 O1 1.326(5) . ?
C67 O7 1.309(5) . ?
C67 C72 1.399(6) . ?
C67 C68 1.399(5) . ?
C68 C69 1.351(6) . ?
C68 H68 0.9300 . ?
C69 C70 1.373(6) . ?
C69 H69 0.9300 . ?
C70 C71 1.357(6) . ?
C70 H70 0.9300 . ?
C71 C72 1.381(6) . ?
C71 H71 0.9300 . ?
C72 C73B 1.429(11) . ?
C72 N11A 1.519(10) . ?
C73A N11A 1.282(19) . ?
C73A C74 1.465(12) . ?
C73A H73A 0.9300 . ?
C73B N11B 1.277(17) . ?
C73B H73B 0.9300 . ?
C74 C79 1.384(6) . ?
C74 C75 1.387(7) . ?
C74 N11B 1.487(8) . ?
C75 C76 1.364(7) . ?
C75 H75 0.9300 . ?
C76 C77 1.370(8) . ?
C76 H76 0.9300 . ?
C77 C78 1.367(7) . ?
C77 H77 0.9300 . ?
C78 C79 1.404(6) . ?
C78 H78 0.9300 . ?
C79 O9 1.332(5) . ?
C80 O6 1.336(5) . ?
C80 C81 1.395(6) . ?
C80 C85 1.404(6) . ?
C81 C82 1.400(6) . ?
C81 H81 0.9300 . ?
C82 C83 1.383(7) . ?
C82 H82 0.9300 . ?
C83 C84 1.349(6) . ?
C83 H83 0.9300 . ?
C84 C85 1.354(6) . ?
C84 H84 0.9300 . ?
C85 C86B 1.36(2) . ?
C85 N12A 1.476(5) . ?
C86A N12A 1.287(6) . ?
C86A C87 1.399(6) . ?
C86A H86A 0.9300 . ?
C87 C88 1.426(6) . ?
C87 C92 1.427(6) . ?
C87 N12B 1.538(19) . ?
C88 C89 1.348(6) . ?
C88 H88 0.9300 . ?
C89 C90 1.350(7) . ?
C89 H89 0.9300 . ?
C90 C91 1.354(6) . ?
C90 H90 0.9300 . ?
C91 C92 1.400(6) . ?
C91 H91 0.9300 . ?
C92 O8 1.311(5) . ?
Cr1 O8 1.927(3) . ?
Cr1 O7 1.931(3) . ?
Cr1 O9 1.966(3) . ?
Cr1 O6 1.968(3) . ?
Cr1 N12A 2.017(4) . ?
Cr1 N11A 2.035(9) . ?
Cr1 N11B 2.050(8) . ?
Cr1 N12B 2.17(3) . ?
Fe1 O2 1.906(3) . ?
Fe1 O1 1.921(3) . ?
Fe1 N1 2.093(4) . ?
Fe1 N4 2.100(4) . ?
Fe1 N3 2.184(3) . ?
Fe1 N2 2.186(3) . ?
N3 H1N3 0.9800 . ?
N2 H1N2 0.9800 . ?
O3 H1O3 0.8200 . ?
O4 H1O4 0.8200 . ?
O1S H2S1 0.884(16) . ?
O1S H1S1 0.770(18) . ?
C86B N12B 1.286(19) . ?
C86B H86B 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
O2 C1 C2 119.3(4) . . ?
O2 C1 C6 122.5(4) . . ?
C2 C1 C6 118.2(4) . . ?
C3 C2 C1 121.7(4) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
O3 C3 C2 116.5(4) . . ?
O3 C3 C4 122.9(4) . . ?
C2 C3 C4 120.6(4) . . ?
C5 C4 C3 118.1(4) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
C4 C5 C6 123.1(4) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C5 C6 C7 119.4(4) . . ?
C5 C6 C1 118.3(4) . . ?
C7 C6 C1 122.3(4) . . ?
N1 C7 C6 127.5(4) . . ?
N1 C7 H7 116.2 . . ?
C6 C7 H7 116.2 . . ?
N1 C8 C9 108.5(4) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
N3 C9 C8 108.6(4) . . ?
N3 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
N3 C9 H9B 110.0 . . ?
C8 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
N3 C10 C11 107.8(4) . . ?
N3 C10 H10A 110.2 . . ?
C11 C10 H10A 110.2 . . ?
N3 C10 H10B 110.2 . . ?
C11 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
N2 C11 C10 108.4(4) . . ?
N2 C11 H11A 110.0 . . ?
C10 C11 H11A 110.0 . . ?
N2 C11 H11B 110.0 . . ?
C10 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
N2 C12 C13 109.7(3) . . ?
N2 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
N2 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N4 C13 C12 108.5(4) . . ?
N4 C13 H13A 110.0 . . ?
C12 C13 H13A 110.0 . . ?
N4 C13 H13B 110.0 . . ?
C12 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
N4 C14 C15 126.4(4) . . ?
N4 C14 H14 116.8 . . ?
C15 C14 H14 116.8 . . ?
C16 C15 C20 118.2(4) . . ?
C16 C15 C14 117.8(4) . . ?
C20 C15 C14 124.0(4) . . ?
C17 C16 C15 122.1(4) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C16 C17 C18 119.4(4) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
O4 C18 C19 123.3(4) . . ?
O4 C18 C17 116.9(4) . . ?
C19 C18 C17 119.7(4) . . ?
C18 C19 C20 121.6(4) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
O1 C20 C19 119.0(4) . . ?
O1 C20 C15 122.0(4) . . ?
C19 C20 C15 119.0(4) . . ?
O7 C67 C72 121.5(4) . . ?
O7 C67 C68 120.7(4) . . ?
C72 C67 C68 117.7(4) . . ?
C69 C68 C67 120.9(4) . . ?
C69 C68 H68 119.6 . . ?
C67 C68 H68 119.6 . . ?
C68 C69 C70 121.3(4) . . ?
C68 C69 H69 119.4 . . ?
C70 C69 H69 119.4 . . ?
C71 C70 C69 118.9(5) . . ?
C71 C70 H70 120.6 . . ?
C69 C70 H70 120.6 . . ?
C70 C71 C72 121.6(5) . . ?
C70 C71 H71 119.2 . . ?
C72 C71 H71 119.2 . . ?
C71 C72 C67 119.5(4) . . ?
C71 C72 C73B 105.6(6) . . ?
C67 C72 C73B 134.8(6) . . ?
C71 C72 N11A 139.2(6) . . ?
C67 C72 N11A 101.1(5) . . ?
N11A C73A C74 116.4(10) . . ?
N11A C73A H73A 121.8 . . ?
C74 C73A H73A 121.8 . . ?
N11B C73B C72 121.1(9) . . ?
N11B C73B H73B 119.4 . . ?
C72 C73B H73B 119.4 . . ?
C79 C74 C75 119.8(4) . . ?
C79 C74 C73A 138.2(6) . . ?
C75 C74 C73A 101.8(6) . . ?
C79 C74 N11B 103.3(5) . . ?
C75 C74 N11B 136.9(6) . . ?
C76 C75 C74 121.4(5) . . ?
C76 C75 H75 119.3 . . ?
C74 C75 H75 119.3 . . ?
C75 C76 C77 119.1(5) . . ?
C75 C76 H76 120.5 . . ?
C77 C76 H76 120.5 . . ?
C78 C77 C76 120.9(5) . . ?
C78 C77 H77 119.5 . . ?
C76 C77 H77 119.5 . . ?
C77 C78 C79 120.6(5) . . ?
C77 C78 H78 119.7 . . ?
C79 C78 H78 119.7 . . ?
O9 C79 C74 121.6(4) . . ?
O9 C79 C78 120.3(4) . . ?
C74 C79 C78 118.1(4) . . ?
O6 C80 C81 122.2(4) . . ?
O6 C80 C85 119.2(4) . . ?
C81 C80 C85 118.5(4) . . ?
C80 C81 C82 119.1(5) . . ?
C80 C81 H81 120.5 . . ?
C82 C81 H81 120.5 . . ?
C83 C82 C81 119.6(5) . . ?
C83 C82 H82 120.2 . . ?
C81 C82 H82 120.2 . . ?
C84 C83 C82 121.3(5) . . ?
C84 C83 H83 119.4 . . ?
C82 C83 H83 119.4 . . ?
C83 C84 C85 120.1(5) . . ?
C83 C84 H84 119.9 . . ?
C85 C84 H84 119.9 . . ?
C84 C85 C86B 89.9(15) . . ?
C84 C85 C80 121.3(4) . . ?
C86B C85 C80 148.8(15) . . ?
C84 C85 N12A 126.8(4) . . ?
C80 C85 N12A 111.9(3) . . ?
N12A C86A C87 123.2(5) . . ?
N12A C86A H86A 118.4 . . ?
C87 C86A H86A 118.4 . . ?
C86A C87 C88 116.5(4) . . ?
C86A C87 C92 125.6(5) . . ?
C88 C87 C92 117.9(4) . . ?
C88 C87 N12B 148.3(13) . . ?
C92 C87 N12B 93.8(13) . . ?
C89 C88 C87 121.8(5) . . ?
C89 C88 H88 119.1 . . ?
C87 C88 H88 119.1 . . ?
C88 C89 C90 120.2(5) . . ?
C88 C89 H89 119.9 . . ?
C90 C89 H89 119.9 . . ?
C89 C90 C91 120.6(5) . . ?
C89 C90 H90 119.7 . . ?
C91 C90 H90 119.7 . . ?
C90 C91 C92 123.1(5) . . ?
C90 C91 H91 118.4 . . ?
C92 C91 H91 118.4 . . ?
O8 C92 C91 118.7(4) . . ?
O8 C92 C87 124.9(4) . . ?
C91 C92 C87 116.4(4) . . ?
O8 Cr1 O7 91.61(13) . . ?
O8 Cr1 O9 88.34(12) . . ?
O7 Cr1 O9 173.25(13) . . ?
O8 Cr1 O6 173.26(13) . . ?
O7 Cr1 O6 90.70(12) . . ?
O9 Cr1 O6 90.12(12) . . ?
O8 Cr1 N12A 91.54(14) . . ?
O7 Cr1 N12A 91.86(13) . . ?
O9 Cr1 N12A 94.89(14) . . ?
O6 Cr1 N12A 82.05(13) . . ?
O8 Cr1 N11A 91.2(2) . . ?
O7 Cr1 N11A 74.6(3) . . ?
O9 Cr1 N11A 98.6(3) . . ?
O6 Cr1 N11A 95.6(2) . . ?
N12A Cr1 N11A 166.3(3) . . ?
O8 Cr1 N11B 97.4(2) . . ?
O7 Cr1 N11B 98.4(2) . . ?
O9 Cr1 N11B 74.9(2) . . ?
O6 Cr1 N11B 88.5(2) . . ?
O8 Cr1 N12B 68.8(6) . . ?
O7 Cr1 N12B 91.6(10) . . ?
O9 Cr1 N12B 94.7(10) . . ?
O6 Cr1 N12B 104.8(6) . . ?
N11B Cr1 N12B 163.3(8) . . ?
O2 Fe1 O1 104.64(13) . . ?
O2 Fe1 N1 87.15(12) . . ?
O1 Fe1 N1 96.71(13) . . ?
O2 Fe1 N4 89.41(12) . . ?
O1 Fe1 N4 87.75(13) . . ?
N1 Fe1 N4 174.94(13) . . ?
O2 Fe1 N3 160.86(13) . . ?
O1 Fe1 N3 88.48(12) . . ?
N1 Fe1 N3 77.37(13) . . ?
N4 Fe1 N3 105.24(14) . . ?
O2 Fe1 N2 94.59(13) . . ?
O1 Fe1 N2 154.84(13) . . ?
N1 Fe1 N2 100.37(14) . . ?
N4 Fe1 N2 76.21(14) . . ?
N3 Fe1 N2 77.48(13) . . ?
C7 N1 C8 117.4(4) . . ?
C7 N1 Fe1 125.6(3) . . ?
C8 N1 Fe1 117.0(3) . . ?
C10 N3 C9 113.9(4) . . ?
C10 N3 Fe1 112.4(3) . . ?
C9 N3 Fe1 106.6(3) . . ?
C10 N3 H1N3 107.9 . . ?
C9 N3 H1N3 107.9 . . ?
Fe1 N3 H1N3 107.9 . . ?
C12 N2 C11 114.6(4) . . ?
C12 N2 Fe1 107.1(3) . . ?
C11 N2 Fe1 109.8(3) . . ?
C12 N2 H1N2 108.4 . . ?
C11 N2 H1N2 108.4 . . ?
Fe1 N2 H1N2 108.4 . . ?
C14 N4 C13 116.9(4) . . ?
C14 N4 Fe1 124.5(3) . . ?
C13 N4 Fe1 117.6(3) . . ?
C73A N11A C72 116.1(9) . . ?
C73A N11A Cr1 122.7(8) . . ?
C72 N11A Cr1 120.3(6) . . ?
C73B N11B C74 120.2(8) . . ?
C73B N11B Cr1 120.1(7) . . ?
C74 N11B Cr1 119.6(5) . . ?
C86A N12A C85 120.7(4) . . ?
C86A N12A Cr1 127.5(3) . . ?
C85 N12A Cr1 111.8(3) . . ?
C1 O2 Fe1 134.8(3) . . ?
C20 O1 Fe1 133.0(3) . . ?
C3 O3 H1O3 109.5 . . ?
C18 O4 H1O4 109.5 . . ?
C67 O7 Cr1 121.5(3) . . ?
C79 O9 Cr1 119.1(3) . . ?
C80 O6 Cr1 115.0(3) . . ?
C92 O8 Cr1 127.1(3) . . ?
H2S1 O1S H1S1 106(3) . . ?
N12B C86B C85 120(2) . . ?
N12B C86B H86B 120.2 . . ?
C85 C86B H86B 120.2 . . ?
C86B N12B C87 122(2) . . ?
C86B N12B Cr1 112.4(16) . . ?
C87 N12B Cr1 125.3(18) . . ?

_refine_diff_density_max         0.551
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.062


# start Validation Reply Form
_vrf_PLAT245_3b                  
;
RESPONSE: The water molecule is placed in the cavity
and its second hydrogen atom forms only weak OH...pi 
contact and furthermore, it executes significant 
thermal motion resulting in enlarged thermal ellipsoid. 
;
_vrf_PLAT410_3b                  
;
RESPONSE: This alert is due to disorder of imino part of 
the ligand which was possible to model only for imino fragment.
;
_vrf_PLAT420_3b                  
;
RESPONSE: The second hydrogen atom forms only weak
 OH...pi contact.
;
####################################################################### 
# 
# 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_3d
_database_code_depnum_ccdc_archive 'CCDC 1890219'
loop_
_audit_author_name
_audit_author_address
'Ivan Nemec'
;Department of inorganic chemistry, Palacky University
Czech Republic
;
_audit_update_record             
;
2019-01-11 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H24 Ag Fe N6 O4'
_chemical_formula_weight         600.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Ag Ag -0.8970 1.1020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 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           45
_space_group_name_H-M_alt        'I b a 2'
_space_group_name_Hall           'I 2 -2c'

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

_cell_length_a                   12.8506(6)
_cell_length_b                   12.7677(6)
_cell_length_c                   14.4195(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2365.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7422
_cell_measurement_theta_min      3.160
_cell_measurement_theta_max      26.112

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_F_000             1212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    1.482
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
'CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET)
(compiled Apr 18 2008,18:17:43)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm'
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
'Goniometer KM4/Xcalibur detector: Sapphire2 (large Be window)'
_diffrn_measurement_method       
;Rotation method data acquisition using omega and phi scans
;
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6901
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.170
_diffrn_reflns_theta_max         25.988
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_point_group_measured_fraction_full 0.809
_reflns_number_total             1886
_reflns_number_gt                1698
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.554
_reflns_Friedel_fraction_max     0.604
_reflns_Friedel_fraction_full    0.600

_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)+(0.0253P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 539 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1886
_refine_ls_number_parameters     155
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0436
_refine_ls_wR_factor_gt          0.0429
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.091
_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
C1 C 1.0938(2) 0.6813(2) 0.4167(2) 0.0152(6) Uani 1 1 d . . . . .
C2 C 1.1783(2) 0.7175(2) 0.4694(2) 0.0184(6) Uani 1 1 d . . . . .
H2 H 1.2267 0.6699 0.4924 0.022 Uiso 1 1 calc R U . . .
C3 C 1.1904(2) 0.8231(2) 0.4875(2) 0.0199(7) Uani 1 1 d . . . . .
C4 C 1.1196(2) 0.8971(2) 0.4527(2) 0.0216(7) Uani 1 1 d . . . . .
H4 H 1.1287 0.9682 0.4640 0.026 Uiso 1 1 calc R U . . .
C5 C 1.0373(2) 0.8622(2) 0.4020(3) 0.0207(6) Uani 1 1 d . . . . .
H5 H 0.9904 0.9109 0.3785 0.025 Uiso 1 1 calc R U . . .
C6 C 1.0206(2) 0.7552(2) 0.3839(2) 0.0162(6) Uani 1 1 d . . . . .
C7 C 0.9295(2) 0.7265(2) 0.3329(2) 0.0176(6) Uani 1 1 d . . . . .
H7 H 0.8845 0.7805 0.3165 0.021 Uiso 1 1 calc R U . . .
C8 C 0.8061(2) 0.6231(2) 0.2543(2) 0.0204(7) Uani 1 1 d . . . . .
H8A H 0.8082 0.6678 0.2000 0.024 Uiso 1 1 calc R U . . .
H8B H 0.7474 0.6442 0.2923 0.024 Uiso 1 1 calc R U . . .
C9 C 0.7939(2) 0.5090(2) 0.2251(3) 0.0185(6) Uani 1 1 d . . . . .
H9A H 0.7635 0.4688 0.2754 0.022 Uiso 1 1 calc R U . . .
H9B H 0.7480 0.5043 0.1718 0.022 Uiso 1 1 calc R U . . .
C10 C 0.9424(2) 0.5120(2) 0.1155(2) 0.0168(7) Uani 1 1 d . . . . .
H10A H 0.9311 0.5871 0.1143 0.020 Uiso 1 1 calc R U . . .
H10B H 0.9095 0.4815 0.0613 0.020 Uiso 1 1 calc R U . . .
Fe1 Fe 1.0000 0.5000 0.31794(4) 0.01181(14) Uani 1 2 d S T P . .
N1 N 0.90357(19) 0.63383(18) 0.30747(18) 0.0156(5) Uani 1 1 d . . . . .
N2 N 0.89766(17) 0.46630(18) 0.20133(17) 0.0140(5) Uani 1 1 d . . . . .
H1N2 H 0.8921 0.3902 0.1938 0.017 Uiso 1 1 calc R U . . .
O1 O 1.08527(15) 0.58031(12) 0.39999(16) 0.0184(4) Uani 1 1 d . . . . .
O2 O 1.26861(17) 0.86177(17) 0.53967(17) 0.0279(5) Uani 1 1 d . . . . .
H1O2 H 1.3077 0.8140 0.5548 0.033 Uiso 1 1 calc R U . . .
Ag1 Ag 1.0000 1.0000 0.64145(2) 0.02505(11) Uani 1 2 d S T P . .
C11 C 0.9390(2) 0.8513(2) 0.6398(3) 0.0241(7) Uani 1 1 d . . . . .
N3 N 0.9030(2) 0.7698(2) 0.6321(2) 0.0291(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.317(3) . ?
C1 C2 1.404(4) . ?
C1 C6 1.414(4) . ?
C2 C3 1.382(4) . ?
C2 H2 0.9300 . ?
C3 O2 1.349(4) . ?
C3 C4 1.405(4) . ?
C4 C5 1.360(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.408(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.430(4) . ?
C7 N1 1.283(3) . ?
C7 H7 0.9300 . ?
C8 N1 1.475(3) . ?
C8 C9 1.524(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.481(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.484(4) . ?
C10 C10 1.513(6) 2_765 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
Fe1 O1 1.911(2) 2_765 ?
Fe1 O1 1.911(2) . ?
Fe1 N1 2.116(2) 2_765 ?
Fe1 N1 2.116(2) . ?
Fe1 N2 2.178(2) . ?
Fe1 N2 2.178(2) 2_765 ?
N2 H1N2 0.9800 . ?
O2 H1O2 0.8200 . ?
Ag1 C11 2.054(3) 2_775 ?
Ag1 C11 2.055(3) . ?
C11 N3 1.144(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 119.1(2) . . ?
O1 C1 C6 122.5(2) . . ?
C2 C1 C6 118.5(2) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
O2 C3 C2 123.1(3) . . ?
O2 C3 C4 115.8(3) . . ?
C2 C3 C4 121.1(3) . . ?
C5 C4 C3 118.4(3) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 122.4(3) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C1 118.9(3) . . ?
C5 C6 C7 118.0(3) . . ?
C1 C6 C7 123.1(2) . . ?
N1 C7 C6 126.6(3) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
N1 C8 C9 108.7(2) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.3 . . ?
N2 C9 C8 108.9(2) . . ?
N2 C9 H9A 109.9 . . ?
C8 C9 H9A 109.9 . . ?
N2 C9 H9B 109.9 . . ?
C8 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
N2 C10 C10 107.44(19) . 2_765 ?
N2 C10 H10A 110.2 . . ?
C10 C10 H10A 110.2 2_765 . ?
N2 C10 H10B 110.2 . . ?
C10 C10 H10B 110.2 2_765 . ?
H10A C10 H10B 108.5 . . ?
O1 Fe1 O1 103.50(13) 2_765 . ?
O1 Fe1 N1 86.95(9) 2_765 2_765 ?
O1 Fe1 N1 98.14(9) . 2_765 ?
O1 Fe1 N1 98.14(9) 2_765 . ?
O1 Fe1 N1 86.95(9) . . ?
N1 Fe1 N1 171.82(15) 2_765 . ?
O1 Fe1 N2 91.47(9) 2_765 . ?
O1 Fe1 N2 158.49(9) . . ?
N1 Fe1 N2 97.99(9) 2_765 . ?
N1 Fe1 N2 75.57(9) . . ?
O1 Fe1 N2 158.49(9) 2_765 2_765 ?
O1 Fe1 N2 91.48(9) . 2_765 ?
N1 Fe1 N2 75.57(9) 2_765 2_765 ?
N1 Fe1 N2 97.99(9) . 2_765 ?
N2 Fe1 N2 78.91(12) . 2_765 ?
C7 N1 C8 117.0(2) . . ?
C7 N1 Fe1 124.9(2) . . ?
C8 N1 Fe1 117.35(17) . . ?
C9 N2 C10 113.4(2) . . ?
C9 N2 Fe1 107.00(18) . . ?
C10 N2 Fe1 109.43(15) . . ?
C9 N2 H1N2 109.0 . . ?
C10 N2 H1N2 109.0 . . ?
Fe1 N2 H1N2 109.0 . . ?
C1 O1 Fe1 133.36(18) . . ?
C3 O2 H1O2 109.5 . . ?
C11 Ag1 C11 178.6(2) 2_775 . ?
N3 C11 Ag1 174.9(3) . . ?

_refine_diff_density_max         0.233
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.046

####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1890218'
loop_
_audit_author_name
_audit_author_address
'Ivan Nemec'
;Department of inorganic chemistry, Palacky University
Czech Republic
;
_audit_update_record             
;
2019-01-11 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H44 Co Fe N6 O9'
_chemical_formula_weight         939.65

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'
Co Co 0.3494 0.9721 '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                   11.2605(7)
_cell_length_b                   13.5063(8)
_cell_length_c                   14.1826(9)
_cell_angle_alpha                97.156(5)
_cell_angle_beta                 106.096(5)
_cell_angle_gamma                92.685(5)
_cell_volume                     2048.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15079
_cell_measurement_theta_min      2.518
_cell_measurement_theta_max      25.998

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_F_000             974
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.826
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7762
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
'CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET)
(compiled Apr 18 2008,18:17:43)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm'
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
'Goniometer KM4/Xcalibur detector: Sapphire2 (large Be window)'
_diffrn_measurement_method       
;Rotation method data acquisition using omega and phi scans
;
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15079
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.526
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8052
_reflns_number_gt                5655
_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)+(0.0529P)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         8052
_refine_ls_number_parameters     582
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_restrained_S_all      1.001
_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
C1 C 0.0910(2) 0.60299(18) 0.43676(18) 0.0204(5) Uani 1 1 d . . . . .
C2 C 0.1484(2) 0.59676(18) 0.53640(18) 0.0232(6) Uani 1 1 d . . . . .
H2 H 0.1398 0.6477 0.5861 0.028 Uiso 1 1 calc R U . . .
C3 C 0.2177(2) 0.51762(18) 0.56393(18) 0.0218(5) Uani 1 1 d . . . . .
C4 C 0.2321(2) 0.44180(18) 0.49191(19) 0.0242(6) Uani 1 1 d . . . . .
H4 H 0.2815 0.3885 0.5108 0.029 Uiso 1 1 calc R U . . .
C5 C 0.1743(2) 0.44550(18) 0.39420(19) 0.0239(6) Uani 1 1 d . . . . .
H5 H 0.1821 0.3930 0.3456 0.029 Uiso 1 1 calc R U . . .
C6 C 0.1034(2) 0.52527(18) 0.36349(17) 0.0200(5) Uani 1 1 d . . . . .
C7 C 0.0476(2) 0.52296(18) 0.25921(18) 0.0227(6) Uani 1 1 d . . . . .
H7 H 0.0666 0.4702 0.2163 0.027 Uiso 1 1 calc R U . . .
C8 C -0.0780(3) 0.5647(2) 0.10922(18) 0.0284(6) Uani 1 1 d . . . . .
H8A H -0.1481 0.5123 0.0915 0.034 Uiso 1 1 calc R U . . .
H8B H -0.0139 0.5401 0.0787 0.034 Uiso 1 1 calc R U . . .
C9 C -0.1227(2) 0.66018(19) 0.07064(19) 0.0277(6) Uani 1 1 d . . . . .
H9A H -0.0519 0.7019 0.0634 0.033 Uiso 1 1 calc R U . . .
H9B H -0.1844 0.6436 0.0047 0.033 Uiso 1 1 calc R U . . .
C10 C -0.3014(2) 0.6682(2) 0.14120(19) 0.0287(6) Uani 1 1 d . . . . .
H10A H -0.2959 0.5955 0.1432 0.034 Uiso 1 1 calc R U . . .
H10B H -0.3661 0.6773 0.0802 0.034 Uiso 1 1 calc R U . . .
C11 C -0.3340(2) 0.7164(2) 0.2309(2) 0.0305(6) Uani 1 1 d . . . . .
H11A H -0.3481 0.7875 0.2256 0.037 Uiso 1 1 calc R U . . .
H11B H -0.4108 0.6818 0.2363 0.037 Uiso 1 1 calc R U . . .
C12 C -0.2237(3) 0.78515(19) 0.40645(19) 0.0283(6) Uani 1 1 d . . . . .
H12A H -0.1669 0.7661 0.4671 0.034 Uiso 1 1 calc R U . . .
H12B H -0.3071 0.7890 0.4164 0.034 Uiso 1 1 calc R U . . .
C13 C -0.1772(2) 0.88590(19) 0.38739(19) 0.0263(6) Uani 1 1 d . . . . .
H13A H -0.2443 0.9139 0.3395 0.032 Uiso 1 1 calc R U . . .
H13B H -0.1517 0.9333 0.4500 0.032 Uiso 1 1 calc R U . . .
C14 C -0.0015(2) 0.95345(19) 0.34970(18) 0.0247(6) Uani 1 1 d . . . . .
H14 H -0.0209 1.0144 0.3811 0.030 Uiso 1 1 calc R U . . .
C15 C 0.1007(2) 0.95858(18) 0.30954(18) 0.0222(5) Uani 1 1 d . . . . .
C16 C 0.1622(2) 1.05327(19) 0.31493(19) 0.0286(6) Uani 1 1 d . . . . .
H16 H 0.1342 1.1105 0.3457 0.034 Uiso 1 1 calc R U . . .
C17 C 0.2612(2) 1.06616(19) 0.27739(19) 0.0275(6) Uani 1 1 d . . . . .
H17 H 0.3004 1.1310 0.2814 0.033 Uiso 1 1 calc R U . . .
C18 C 0.3031(2) 0.98099(19) 0.23282(17) 0.0227(6) Uani 1 1 d . . . . .
C19 C 0.2443(2) 0.88749(19) 0.22563(17) 0.0232(6) Uani 1 1 d . . . . .
H19 H 0.2738 0.8309 0.1951 0.028 Uiso 1 1 calc R U . . .
C20 C 0.1421(2) 0.87363(18) 0.26218(17) 0.0219(5) Uani 1 1 d . . . . .
C21 C 0.2998(2) 0.15197(19) 0.04943(19) 0.0261(6) Uani 1 1 d . . . . .
C22 C 0.1730(2) 0.11699(19) 0.02454(19) 0.0266(6) Uani 1 1 d . . . . .
H22 H 0.1254 0.1389 0.0678 0.032 Uiso 1 1 calc R U . . .
C23 C 0.1173(2) 0.05247(19) -0.0601(2) 0.0287(6) Uani 1 1 d . . . . .
H23 H 0.0315 0.0317 -0.0753 0.034 Uiso 1 1 calc R U . . .
C24 C 0.1837(3) 0.0165(2) -0.1247(2) 0.0316(6) Uani 1 1 d . . . . .
H24 H 0.1437 -0.0279 -0.1837 0.038 Uiso 1 1 calc R U . . .
C25 C 0.3063(3) 0.0456(2) -0.1024(2) 0.0309(6) Uani 1 1 d D . . . .
H25 H 0.3521 0.0199 -0.1457 0.037 Uiso 1 1 calc R U . . .
C26 C 0.3677(2) 0.11318(19) -0.0165(2) 0.0274(6) Uani 1 1 d D . . . .
C27A C 0.4969(3) 0.1357(2) -0.0018(2) 0.0213(7) Uani 0.888(4) 1 d D . P A 1
H27A H 0.5341 0.1057 -0.0496 0.026 Uiso 0.888(4) 1 calc R U P A 1
C28 C 0.6961(2) 0.21679(18) 0.08475(18) 0.0213(5) Uani 1 1 d D . . . .
C29 C 0.7644(2) 0.18074(19) 0.02256(19) 0.0276(6) Uani 1 1 d D . . . .
H29 H 0.7251 0.1359 -0.0363 0.033 Uiso 1 1 calc R U . . .
C30 C 0.8883(3) 0.20940(19) 0.0456(2) 0.0292(6) Uani 1 1 d . . . . .
H30 H 0.9343 0.1867 0.0014 0.035 Uiso 1 1 calc R U . . .
C31 C 0.9466(2) 0.2717(2) 0.1333(2) 0.0317(6) Uani 1 1 d . . . . .
H31 H 1.0331 0.2902 0.1497 0.038 Uiso 1 1 calc R U . . .
C32 C 0.8796(2) 0.3072(2) 0.1975(2) 0.0324(7) Uani 1 1 d . . . . .
H32 H 0.9207 0.3484 0.2583 0.039 Uiso 1 1 calc R U . . .
C33 C 0.7523(2) 0.28233(18) 0.17253(19) 0.0233(6) Uani 1 1 d . . . . .
C34 C 0.5564(2) 0.1767(2) 0.34852(18) 0.0267(6) Uani 1 1 d . . . . .
C35 C 0.5921(3) 0.1026(2) 0.40928(19) 0.0307(6) Uani 1 1 d . . . . .
H35 H 0.6090 0.0391 0.3812 0.037 Uiso 1 1 calc R U . . .
C36 C 0.6029(3) 0.1209(2) 0.5085(2) 0.0386(7) Uani 1 1 d . . . . .
H36 H 0.6270 0.0696 0.5485 0.046 Uiso 1 1 calc R U . . .
C37 C 0.5795(3) 0.2124(3) 0.5516(2) 0.0477(9) Uani 1 1 d . . . . .
H37 H 0.5888 0.2248 0.6207 0.057 Uiso 1 1 calc R U . . .
C38 C 0.5428(3) 0.2852(2) 0.4931(3) 0.0470(9) Uani 1 1 d . . . . .
H38 H 0.5257 0.3483 0.5219 0.056 Uiso 1 1 calc R U . . .
C39 C 0.5301(2) 0.2677(2) 0.3917(2) 0.0306(5) Uani 1 1 d D . . . .
C40A C 0.4442(5) 0.4101(4) 0.3121(4) 0.0232(8) Uani 0.491(3) 1 d D . P A 1
H40A H 0.4310 0.4379 0.3730 0.028 Uiso 0.491(3) 1 calc R U P A 1
C40B C 0.4780(5) 0.3622(4) 0.3555(4) 0.0232(8) Uani 0.509(3) 1 d D . P A 2
H40B H 0.4588 0.4148 0.3984 0.028 Uiso 0.509(3) 1 calc R U P A 2
C41 C 0.4108(2) 0.4592(2) 0.2281(2) 0.0306(5) Uani 1 1 d D . . . .
C42 C 0.3527(3) 0.5384(2) 0.2600(2) 0.0402(8) Uani 1 1 d D . . . .
H42 H 0.3430 0.5448 0.3248 0.048 Uiso 1 1 calc R U . . .
C43 C 0.3085(3) 0.6083(2) 0.1998(2) 0.0400(8) Uani 1 1 d . . . . .
H43 H 0.2652 0.6612 0.2214 0.048 Uiso 1 1 calc R U . . .
C44 C 0.3279(2) 0.6007(2) 0.1068(2) 0.0322(7) Uani 1 1 d . . . . .
H44 H 0.2993 0.6499 0.0653 0.039 Uiso 1 1 calc R U . . .
C45 C 0.3874(2) 0.52370(19) 0.07405(19) 0.0253(6) Uani 1 1 d . . . . .
H45 H 0.4013 0.5205 0.0107 0.030 Uiso 1 1 calc R U . . .
C46 C 0.4285(2) 0.44892(18) 0.1334(2) 0.0247(6) Uani 1 1 d . . . . .
N1 N -0.02577(19) 0.58530(15) 0.21799(14) 0.0222(5) Uani 1 1 d . . . . .
N2 N -0.17964(19) 0.71631(15) 0.14105(14) 0.0231(5) Uani 1 1 d . . . . .
H1N2 H -0.1915 0.7854 0.1236 0.028 Uiso 1 1 calc R U . . .
N3 N -0.22950(19) 0.70895(15) 0.31947(15) 0.0248(5) Uani 1 1 d . . . . .
H1N3 H -0.2385 0.6410 0.3391 0.030 Uiso 1 1 calc R U . . .
N4 N -0.07108(19) 0.87266(15) 0.34728(15) 0.0226(5) Uani 1 1 d . . . . .
N5A N 0.5653(2) 0.19528(17) 0.07379(17) 0.0195(6) Uani 0.888(4) 1 d D . P A 1
N6A N 0.4951(4) 0.3231(3) 0.3038(3) 0.0180(7) Uani 0.491(3) 1 d D . P A 1
N6B N 0.4619(4) 0.3659(3) 0.2651(3) 0.0180(7) Uani 0.509(3) 1 d D . P A 2
O1 O 0.02691(16) 0.68070(13) 0.41299(12) 0.0261(4) Uani 1 1 d . . . . .
O1S O 0.0994(4) 0.8423(2) 0.5748(2) 0.1078(12) Uani 1 1 d D . . . .
O2 O 0.08752(15) 0.78263(12) 0.25193(13) 0.0250(4) Uani 1 1 d . . . . .
O3 O 0.27430(15) 0.50880(12) 0.65979(12) 0.0259(4) Uani 1 1 d . . . . .
H1O3 H 0.2801 0.5645 0.6952 0.031 Uiso 1 1 calc R U . . .
O4 O 0.40102(16) 0.98614(13) 0.19527(12) 0.0283(4) Uani 1 1 d . . . . .
H1O4 H 0.4396 1.0431 0.2142 0.034 Uiso 1 1 calc R U . . .
O5 O 0.34543(16) 0.21705(13) 0.12965(13) 0.0318(4) Uani 1 1 d . . . . .
O6 O 0.68233(16) 0.31719(13) 0.22937(13) 0.0304(4) Uani 1 1 d . . . . .
O7 O 0.54465(17) 0.15768(14) 0.25130(12) 0.0344(5) Uani 1 1 d . . . . .
O8 O 0.48149(17) 0.37217(13) 0.10034(15) 0.0372(5) Uani 1 1 d . . . . .
Fe1 Fe -0.04959(3) 0.72669(3) 0.28854(3) 0.02076(10) Uani 1 1 d . . . . .
Co1 Co 0.51274(3) 0.26681(3) 0.17699(3) 0.02412(10) Uani 1 1 d . . . . .
N5B N 0.4809(14) 0.1796(13) 0.0554(12) 0.0195(6) Uani 0.112(4) 1 d D . P A 2
C27B C 0.5732(12) 0.1693(17) 0.0284(17) 0.0213(7) Uani 0.112(4) 1 d D . P A 2
H27B H 0.5654 0.1281 -0.0328 0.026 Uiso 0.112(4) 1 calc R U P A 2
H1S1 H 0.1608(19) 0.8364(19) 0.6247(12) 0.032 Uiso 1 1 d D U . . .
H2S1 H 0.094(2) 0.7956(15) 0.5292(12) 0.032 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
C1 O1 1.327(3) . ?
C1 C2 1.397(3) . ?
C1 C6 1.423(3) . ?
C2 C3 1.385(3) . ?
C3 O3 1.355(3) . ?
C3 C4 1.402(3) . ?
C4 C5 1.366(3) . ?
C5 C6 1.412(3) . ?
C6 C7 1.433(3) . ?
C7 N1 1.286(3) . ?
C8 N1 1.476(3) . ?
C8 C9 1.516(3) . ?
C9 N2 1.482(3) . ?
C10 N2 1.490(3) . ?
C10 C11 1.501(4) . ?
C11 N3 1.481(3) . ?
C12 N3 1.489(3) . ?
C12 C13 1.517(3) . ?
C13 N4 1.468(3) . ?
C14 N4 1.304(3) . ?
C14 C15 1.421(3) . ?
C15 C16 1.409(3) . ?
C15 C20 1.420(3) . ?
C16 C17 1.375(3) . ?
C17 C18 1.408(4) . ?
C18 O4 1.353(3) . ?
C18 C19 1.377(3) . ?
C19 C20 1.401(3) . ?
C20 O2 1.321(3) . ?
C21 O5 1.310(3) . ?
C21 C22 1.416(3) . ?
C21 C26 1.430(4) . ?
C22 C23 1.366(4) . ?
C23 C24 1.392(4) . ?
C24 C25 1.355(4) . ?
C25 C26 1.411(4) . ?
C26 C27A 1.424(4) . ?
C26 N5B 1.553(14) . ?
C27A N5A 1.288(3) . ?
C28 C29 1.382(3) . ?
C28 C33 1.403(3) . ?
C28 N5A 1.449(3) . ?
C28 C27B 1.463(15) . ?
C29 C30 1.367(4) . ?
C30 C31 1.386(4) . ?
C31 C32 1.391(4) . ?
C32 C33 1.392(3) . ?
C33 O6 1.336(3) . ?
C34 O7 1.339(3) . ?
C34 C39 1.386(4) . ?
C34 C35 1.402(3) . ?
C35 C36 1.369(4) . ?
C36 C37 1.379(4) . ?
C37 C38 1.370(4) . ?
C38 C39 1.394(4) . ?
C39 N6A 1.501(5) . ?
C39 C40B 1.517(5) . ?
C40A N6A 1.338(7) . ?
C40A C41 1.405(6) . ?
C40B N6B 1.252(7) . ?
C41 C42 1.374(4) . ?
C41 C46 1.402(4) . ?
C41 N6B 1.503(5) . ?
C42 C43 1.370(4) . ?
C43 C44 1.388(4) . ?
C44 C45 1.366(4) . ?
C45 C46 1.408(3) . ?
C46 O8 1.320(3) . ?
N1 Fe1 2.107(2) . ?
N2 Fe1 2.179(2) . ?
N3 Fe1 2.197(2) . ?
N4 Fe1 2.095(2) . ?
N5A Co1 1.900(2) . ?
N6A Co1 1.930(5) . ?
N6B Co1 1.932(4) . ?
O1 Fe1 1.9295(17) . ?
O2 Fe1 1.9124(17) . ?
O5 Co1 1.8760(18) . ?
O6 Co1 1.9046(18) . ?
O7 Co1 1.9076(19) . ?
O8 Co1 1.8843(19) . ?
Co1 N5B 1.898(16) . ?
N5B C27B 1.211(16) . ?

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 C1 C2 119.5(2) . . ?
O1 C1 C6 121.9(2) . . ?
C2 C1 C6 118.6(2) . . ?
C3 C2 C1 121.1(2) . . ?
O3 C3 C2 122.8(2) . . ?
O3 C3 C4 116.7(2) . . ?
C2 C3 C4 120.5(2) . . ?
C5 C4 C3 119.2(2) . . ?
C4 C5 C6 121.8(2) . . ?
C5 C6 C1 118.8(2) . . ?
C5 C6 C7 117.6(2) . . ?
C1 C6 C7 123.7(2) . . ?
N1 C7 C6 126.4(2) . . ?
N1 C8 C9 109.2(2) . . ?
N2 C9 C8 109.3(2) . . ?
N2 C10 C11 108.3(2) . . ?
N3 C11 C10 108.1(2) . . ?
N3 C12 C13 108.7(2) . . ?
N4 C13 C12 109.0(2) . . ?
N4 C14 C15 125.9(2) . . ?
C16 C15 C20 118.3(2) . . ?
C16 C15 C14 118.2(2) . . ?
C20 C15 C14 123.5(2) . . ?
C17 C16 C15 122.6(2) . . ?
C16 C17 C18 118.4(2) . . ?
O4 C18 C19 117.0(2) . . ?
O4 C18 C17 122.6(2) . . ?
C19 C18 C17 120.4(2) . . ?
C18 C19 C20 121.7(2) . . ?
O2 C20 C19 119.4(2) . . ?
O2 C20 C15 122.0(2) . . ?
C19 C20 C15 118.6(2) . . ?
O5 C21 C22 118.1(2) . . ?
O5 C21 C26 125.3(2) . . ?
C22 C21 C26 116.6(2) . . ?
C23 C22 C21 121.6(3) . . ?
C22 C23 C24 121.3(3) . . ?
C25 C24 C23 119.1(3) . . ?
C24 C25 C26 121.7(3) . . ?
C25 C26 C27A 115.4(2) . . ?
C25 C26 C21 119.7(2) . . ?
C27A C26 C21 124.9(2) . . ?
C25 C26 N5B 154.6(6) . . ?
C21 C26 N5B 85.8(6) . . ?
N5A C27A C26 122.5(3) . . ?
C29 C28 C33 121.0(2) . . ?
C29 C28 N5A 128.4(2) . . ?
C33 C28 N5A 110.6(2) . . ?
C29 C28 C27B 99.7(8) . . ?
C33 C28 C27B 139.2(8) . . ?
C30 C29 C28 120.1(2) . . ?
C29 C30 C31 120.0(2) . . ?
C30 C31 C32 120.5(2) . . ?
C31 C32 C33 119.9(2) . . ?
O6 C33 C32 122.6(2) . . ?
O6 C33 C28 119.0(2) . . ?
C32 C33 C28 118.3(2) . . ?
O7 C34 C39 121.8(2) . . ?
O7 C34 C35 120.2(2) . . ?
C39 C34 C35 118.0(2) . . ?
C36 C35 C34 120.7(3) . . ?
C35 C36 C37 121.0(3) . . ?
C38 C37 C36 119.1(3) . . ?
C37 C38 C39 120.7(3) . . ?
C34 C39 C38 120.5(2) . . ?
C34 C39 N6A 101.2(3) . . ?
C38 C39 N6A 138.3(3) . . ?
C34 C39 C40B 136.2(3) . . ?
C38 C39 C40B 103.2(3) . . ?
N6A C40A C41 117.9(5) . . ?
N6B C40B C39 115.4(4) . . ?
C42 C41 C46 120.7(2) . . ?
C42 C41 C40A 102.2(3) . . ?
C46 C41 C40A 137.0(3) . . ?
C42 C41 N6B 137.9(3) . . ?
C46 C41 N6B 101.4(3) . . ?
C43 C42 C41 121.1(3) . . ?
C42 C43 C44 119.0(3) . . ?
C45 C44 C43 121.0(3) . . ?
C44 C45 C46 120.6(2) . . ?
O8 C46 C41 121.7(2) . . ?
O8 C46 C45 120.7(2) . . ?
C41 C46 C45 117.6(2) . . ?
C7 N1 C8 116.9(2) . . ?
C7 N1 Fe1 124.86(17) . . ?
C8 N1 Fe1 117.13(15) . . ?
C9 N2 C10 113.5(2) . . ?
C9 N2 Fe1 107.29(15) . . ?
C10 N2 Fe1 109.37(14) . . ?
C11 N3 C12 114.0(2) . . ?
C11 N3 Fe1 111.63(15) . . ?
C12 N3 Fe1 106.43(15) . . ?
C14 N4 C13 116.6(2) . . ?
C14 N4 Fe1 126.63(17) . . ?
C13 N4 Fe1 116.75(15) . . ?
C27A N5A C28 120.4(2) . . ?
C27A N5A Co1 126.8(2) . . ?
C28 N5A Co1 112.79(17) . . ?
C40A N6A C39 119.4(4) . . ?
C40A N6A Co1 119.4(4) . . ?
C39 N6A Co1 121.1(3) . . ?
C40B N6B C41 116.1(4) . . ?
C40B N6B Co1 124.0(4) . . ?
C41 N6B Co1 119.7(3) . . ?
C1 O1 Fe1 133.28(15) . . ?
C20 O2 Fe1 134.93(15) . . ?
C21 O5 Co1 123.87(17) . . ?
C33 O6 Co1 112.61(16) . . ?
C34 O7 Co1 117.28(17) . . ?
C46 O8 Co1 117.68(17) . . ?
O2 Fe1 O1 103.78(8) . . ?
O2 Fe1 N4 87.04(7) . . ?
O1 Fe1 N4 97.09(7) . . ?
O2 Fe1 N1 89.19(7) . . ?
O1 Fe1 N1 87.38(7) . . ?
N4 Fe1 N1 174.73(8) . . ?
O2 Fe1 N2 94.77(8) . . ?
O1 Fe1 N2 155.23(8) . . ?
N4 Fe1 N2 100.16(8) . . ?
N1 Fe1 N2 76.49(8) . . ?
O2 Fe1 N3 161.46(7) . . ?
O1 Fe1 N3 88.62(8) . . ?
N4 Fe1 N3 77.68(8) . . ?
N1 Fe1 N3 105.32(8) . . ?
N2 Fe1 N3 77.93(8) . . ?
O5 Co1 O8 90.88(8) . . ?
O5 Co1 N5B 68.6(5) . . ?
O8 Co1 N5B 86.8(5) . . ?
O5 Co1 N5A 96.58(9) . . ?
O8 Co1 N5A 88.13(9) . . ?
O5 Co1 O6 178.12(8) . . ?
O8 Co1 O6 90.30(8) . . ?
N5B Co1 O6 112.9(5) . . ?
N5A Co1 O6 84.92(9) . . ?
O5 Co1 O7 88.89(8) . . ?
O8 Co1 O7 178.36(8) . . ?
N5B Co1 O7 91.6(5) . . ?
N5A Co1 O7 90.28(9) . . ?
O6 Co1 O7 89.97(8) . . ?
O5 Co1 N6A 92.63(14) . . ?
O8 Co1 N6A 103.99(14) . . ?
N5A Co1 N6A 164.68(14) . . ?
O6 Co1 N6A 85.67(13) . . ?
O7 Co1 N6A 77.65(14) . . ?
O5 Co1 N6B 86.80(13) . . ?
O8 Co1 N6B 78.63(14) . . ?
N5B Co1 N6B 151.2(5) . . ?
O6 Co1 N6B 92.01(13) . . ?
O7 Co1 N6B 102.98(14) . . ?
C27B N5B C26 111.1(14) . . ?
C27B N5B Co1 112.4(14) . . ?
C26 N5B Co1 136.4(10) . . ?
N5B C27B C28 123.7(19) . . ?

_refine_diff_density_max         0.687
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.073


# start Validation Reply Form
_vrf_PLAT410_3a                  
;
RESPONSE: This alert is due to disorder of imino part of 
the ligand which was possible to model only for imino fragment.
;
_vrf_PLAT420_3a                  
;
RESPONSE: The second hydrogen atom forms only weak OH...pi
contact.
;
_vrf_PLAT230_3a                  
;
RESPONSE: This alert is due to disorder of 
the tridentate 
ligand, which was modelled only for imino fragment. However, 
disorder affected also atoms in proximity of the imino part.  
;
_vrf_PLAT245_3a                  
;
RESPONSE: Lattice water molecule is placed in the cavity
and its second hydrogen atom forms only weak OH...pi 
contact. Therfore, the water molecule executes 
significant thermal motion which 
resulted in enlarged thermal ellipsoid. 
;
