# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_H2O@150K
_database_code_depnum_ccdc_archive 'CCDC 1965898'
loop_
_audit_author_name
_audit_author_address
'Jun Tao'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2019-11-15 deposited with the CCDC.	2019-12-30 downloaded from the CCDC.
;
_audit_creation_date             2019-11-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        H2O
_chemical_formula_moiety         'C56 H32 Fe N10 S2, 2(H2 O)'
_chemical_formula_sum            'C56 H36 Fe N10 O2 S2'
_chemical_formula_weight         1000.92
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Co1 S1 O4 N6 C6 H12'
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   12.3848(11)
_cell_length_b                   23.950(3)
_cell_length_c                   16.0358(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4756.4(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2737
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      27.1450
_cell_measurement_theta_min      3.6180
_shelx_estimated_absorpt_T_max   0.913
_shelx_estimated_absorpt_T_min   0.682
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_preparation       'Absorb water after solvent removal'
_exptl_crystal_recrystallization_method 'Reddish black crystals'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1391
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29555
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.472
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -58.00 -33.00   0.25   80.00    --    0.00 -53.00-118.00  100
  2  ω     10.00  35.00   0.25   80.00    --    0.00  53.00  26.00  100
  3  ω    -63.00 -34.00   0.25   80.00    --    0.00 -82.00-150.00  116
  4  ω     -5.00   7.50   0.25   80.00    --    0.00 -82.00-150.00   50
  5  ω    -28.00  11.00   0.25   80.00    --    0.00 -57.00   0.00  156
  6  ω      5.00  31.00   0.25   80.00    --    0.00 -82.00  90.00  104
  7  ω    -18.00  26.00   0.25   80.00    --    0.00  19.00  30.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0503711000
_diffrn_orient_matrix_UB_12      0.0050657000
_diffrn_orient_matrix_UB_13      0.0196497000
_diffrn_orient_matrix_UB_21      -0.0035578000
_diffrn_orient_matrix_UB_22      0.0262034000
_diffrn_orient_matrix_UB_23      -0.0204105000
_diffrn_orient_matrix_UB_31      -0.0269948000
_diffrn_orient_matrix_UB_32      -0.0127947000
_diffrn_orient_matrix_UB_33      -0.0340267000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3164
_reflns_number_total             4831
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4831
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0876
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0691P)²+20.3494P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.2108
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.250000 0.250000 0.51676(6) 0.0272(3) Uani 1 2 d S T P . .
S1 S 0.02514(15) 0.32628(7) 0.30901(10) 0.0499(5) Uani 1 1 d . . . . .
N1 N 0.1696(4) 0.29036(18) 0.4309(3) 0.0317(10) Uani 1 1 d . . . . .
N2 N 0.1839(3) 0.29486(17) 0.6071(2) 0.0246(9) Uani 1 1 d . . . . .
N3 N 0.3597(3) 0.31007(17) 0.5207(3) 0.0262(9) Uani 1 1 d . . . . .
N4 N 0.4421(3) 0.47320(17) 0.6996(2) 0.0244(9) Uani 1 1 d . . . . .
N5 N 0.2955(3) 0.45838(17) 0.7770(3) 0.0254(9) Uani 1 1 d . . . . .
H5 H 0.248332 0.462322 0.815953 0.030 Uiso 1 1 calc R . . . .
C1 C 0.1116(5) 0.3057(2) 0.3794(3) 0.0305(12) Uani 1 1 d . . . . .
C2 C 0.0959(4) 0.2843(2) 0.6517(3) 0.0294(12) Uani 1 1 d . . . . .
H2 H 0.053716 0.253735 0.637193 0.035 Uiso 1 1 calc R . . . .
C3 C 0.0634(4) 0.3174(2) 0.7201(3) 0.0295(12) Uani 1 1 d . . . . .
H3 H 0.000823 0.308553 0.749218 0.035 Uiso 1 1 calc R . . . .
C4 C 0.1234(4) 0.3621(2) 0.7433(3) 0.0280(11) Uani 1 1 d . . . . .
H4 H 0.102450 0.384080 0.788321 0.034 Uiso 1 1 calc R . . . .
C5 C 0.2184(4) 0.3750(2) 0.6980(3) 0.0237(11) Uani 1 1 d . . . . .
C6 C 0.2457(4) 0.33974(19) 0.6304(3) 0.0229(10) Uani 1 1 d . . . . .
C7 C 0.2925(4) 0.4197(2) 0.7134(3) 0.0238(10) Uani 1 1 d . . . . .
C8 C 0.3832(4) 0.4297(2) 0.6656(3) 0.0242(10) Uani 1 1 d . . . . .
C9 C 0.4114(4) 0.3941(2) 0.5966(3) 0.0230(10) Uani 1 1 d . . . . .
C10 C 0.3409(4) 0.3494(2) 0.5810(3) 0.0254(11) Uani 1 1 d . . . . .
C11 C 0.5024(4) 0.3997(2) 0.5460(3) 0.0294(12) Uani 1 1 d . . . . .
H11 H 0.550754 0.428908 0.554356 0.035 Uiso 1 1 calc R . . . .
C12 C 0.5191(5) 0.3613(2) 0.4836(3) 0.0358(13) Uani 1 1 d . . . . .
H12 H 0.578826 0.364673 0.448840 0.043 Uiso 1 1 calc R . . . .
C13 C 0.4466(4) 0.3172(2) 0.4723(3) 0.0341(13) Uani 1 1 d . . . . .
H13 H 0.459272 0.291787 0.429525 0.041 Uiso 1 1 calc R . . . .
C14 C 0.6469(5) 0.5478(3) 0.9863(3) 0.0390(14) Uani 1 1 d . . . . .
H14 H 0.668400 0.572619 1.027657 0.047 Uiso 1 1 calc R . . . .
C15 C 0.7067(5) 0.5017(3) 0.9716(4) 0.0423(15) Uani 1 1 d . . . . .
H15 H 0.768974 0.495166 1.002563 0.051 Uiso 1 1 calc R . . . .
C16 C 0.6748(4) 0.4632(3) 0.9092(3) 0.0374(14) Uani 1 1 d . . . . .
H16 H 0.715799 0.431165 0.900421 0.045 Uiso 1 1 calc R . . . .
C17 C 0.5852(4) 0.4721(2) 0.8619(3) 0.0318(12) Uani 1 1 d . . . . .
H17 H 0.566353 0.446440 0.820863 0.038 Uiso 1 1 calc R . . . .
C18 C 0.5194(4) 0.5207(2) 0.8745(3) 0.0249(11) Uani 1 1 d . . . . .
C19 C 0.5505(4) 0.5592(2) 0.9391(3) 0.0312(12) Uani 1 1 d . . . . .
C20 C 0.4854(5) 0.6050(2) 0.9564(3) 0.0335(13) Uani 1 1 d . . . . .
H20 H 0.505204 0.629005 0.999403 0.040 Uiso 1 1 calc R . . . .
C21 C 0.3927(5) 0.6161(2) 0.9121(3) 0.0330(13) Uani 1 1 d . . . . .
C22 C 0.3592(4) 0.5784(2) 0.8459(3) 0.0290(11) Uani 1 1 d . . . . .
C23 C 0.4238(4) 0.5309(2) 0.8294(3) 0.0260(11) Uani 1 1 d . . . . .
C24 C 0.3256(5) 0.6632(3) 0.9294(4) 0.0469(16) Uani 1 1 d . . . . .
H24 H 0.345131 0.687221 0.972325 0.056 Uiso 1 1 calc R . . . .
C25 C 0.2360(6) 0.6739(3) 0.8863(5) 0.0569(19) Uani 1 1 d . . . . .
H25 H 0.193995 0.704956 0.899116 0.068 Uiso 1 1 calc R . . . .
C26 C 0.2055(5) 0.6375(3) 0.8206(4) 0.0521(17) Uani 1 1 d . . . . .
H26 H 0.143485 0.645373 0.790136 0.063 Uiso 1 1 calc R . . . .
C27 C 0.2645(4) 0.5916(2) 0.8011(4) 0.0371(13) Uani 1 1 d . . . . .
H27 H 0.242151 0.568499 0.757776 0.045 Uiso 1 1 calc R . . . .
C28 C 0.3872(4) 0.4892(2) 0.7666(3) 0.0250(11) Uani 1 1 d . . . . .
O1 O 0.6108(3) 0.52767(17) 0.6212(2) 0.0345(9) Uani 1 1 d . . . . .
H1A H 0.583288 0.549449 0.585131 0.052 Uiso 1 1 d G . . . .
H1B H 0.556913 0.514692 0.647716 0.052 Uiso 1 1 d G . . . .


_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 1.955(5) 2 ?
Fe1 N1 1.955(5) . ?
Fe1 N2 1.981(4) . ?
Fe1 N2 1.981(4) 2 ?
Fe1 N3 1.980(4) 2 ?
Fe1 N3 1.980(4) . ?
S1 C1 1.632(6) . ?
N1 C1 1.154(7) . ?
N2 C2 1.327(7) . ?
N2 C6 1.371(6) . ?
N3 C10 1.369(6) . ?
N3 C13 1.338(7) . ?
N4 C8 1.384(6) . ?
N4 C28 1.329(6) . ?
N5 H5 0.8600 . ?
N5 C7 1.378(6) . ?
N5 C28 1.365(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.412(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.355(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.417(7) . ?
C5 C6 1.415(7) . ?
C5 C7 1.432(7) . ?
C6 C10 1.439(7) . ?
C7 C8 1.381(7) . ?
C8 C9 1.440(7) . ?
C9 C10 1.404(7) . ?
C9 C11 1.395(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.375(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.399(8) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.350(9) . ?
C14 C19 1.440(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.418(8) . ?
C16 H16 0.9300 . ?
C16 C17 1.362(7) . ?
C17 H17 0.9300 . ?
C17 C18 1.434(7) . ?
C18 C19 1.439(7) . ?
C18 C23 1.410(7) . ?
C19 C20 1.390(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.377(8) . ?
C21 C22 1.454(7) . ?
C21 C24 1.428(8) . ?
C22 C23 1.415(7) . ?
C22 C27 1.412(7) . ?
C23 C28 1.489(7) . ?
C24 H24 0.9300 . ?
C24 C25 1.332(9) . ?
C25 H25 0.9300 . ?
C25 C26 1.418(9) . ?
C26 H26 0.9300 . ?
C26 C27 1.358(8) . ?
C27 H27 0.9300 . ?
O1 H1A 0.8499 . ?
O1 H1B 0.8499 . ?

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 N1 90.5(3) 2 . ?
N1 Fe1 N2 173.63(18) 2 . ?
N1 Fe1 N2 92.10(17) . . ?
N1 Fe1 N2 92.10(17) 2 2 ?
N1 Fe1 N2 173.63(18) . 2 ?
N1 Fe1 N3 90.75(18) 2 2 ?
N1 Fe1 N3 91.85(18) 2 . ?
N1 Fe1 N3 91.85(18) . 2 ?
N1 Fe1 N3 90.75(18) . . ?
N2 Fe1 N2 86.0(2) 2 . ?
N3 Fe1 N2 95.00(17) 2 . ?
N3 Fe1 N2 82.29(17) 2 2 ?
N3 Fe1 N2 95.00(17) . 2 ?
N3 Fe1 N2 82.29(17) . . ?
N3 Fe1 N3 176.3(2) 2 . ?
C1 N1 Fe1 168.0(4) . . ?
C2 N2 Fe1 129.1(4) . . ?
C2 N2 C6 117.4(4) . . ?
C6 N2 Fe1 113.2(3) . . ?
C10 N3 Fe1 114.0(3) . . ?
C13 N3 Fe1 128.7(4) . . ?
C13 N3 C10 117.3(4) . . ?
C28 N4 C8 105.4(4) . . ?
C7 N5 H5 126.4 . . ?
C28 N5 H5 126.4 . . ?
C28 N5 C7 107.2(4) . . ?
N1 C1 S1 177.4(5) . . ?
N2 C2 H2 118.5 . . ?
N2 C2 C3 123.1(5) . . ?
C3 C2 H2 118.5 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0(5) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.1(5) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 C7 127.3(5) . . ?
C6 C5 C4 117.5(4) . . ?
C6 C5 C7 115.2(4) . . ?
N2 C6 C5 122.9(4) . . ?
N2 C6 C10 115.7(4) . . ?
C5 C6 C10 121.4(4) . . ?
N5 C7 C5 130.4(4) . . ?
N5 C7 C8 105.8(4) . . ?
C8 C7 C5 123.7(4) . . ?
N4 C8 C9 128.4(4) . . ?
C7 C8 N4 109.9(4) . . ?
C7 C8 C9 121.4(4) . . ?
C10 C9 C8 116.0(4) . . ?
C11 C9 C8 125.8(5) . . ?
C11 C9 C10 118.2(5) . . ?
N3 C10 C6 114.6(4) . . ?
N3 C10 C9 123.0(5) . . ?
C9 C10 C6 122.2(4) . . ?
C9 C11 H11 120.7 . . ?
C12 C11 C9 118.7(5) . . ?
C12 C11 H11 120.7 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.2(5) . . ?
C13 C12 H12 119.9 . . ?
N3 C13 C12 122.5(5) . . ?
N3 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C15 C14 H14 119.4 . . ?
C15 C14 C19 121.2(5) . . ?
C19 C14 H14 119.4 . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.1(5) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 119.4 . . ?
C17 C16 C15 121.2(6) . . ?
C17 C16 H16 119.4 . . ?
C16 C17 H17 119.6 . . ?
C16 C17 C18 120.8(5) . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C19 118.0(5) . . ?
C23 C18 C17 123.1(5) . . ?
C23 C18 C19 118.8(5) . . ?
C18 C19 C14 118.5(5) . . ?
C20 C19 C14 121.7(5) . . ?
C20 C19 C18 119.7(5) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 C19 122.2(5) . . ?
C21 C20 H20 118.9 . . ?
C20 C21 C22 119.7(5) . . ?
C20 C21 C24 122.5(5) . . ?
C24 C21 C22 117.8(5) . . ?
C23 C22 C21 118.3(5) . . ?
C27 C22 C21 118.0(5) . . ?
C27 C22 C23 123.7(5) . . ?
C18 C23 C22 121.3(5) . . ?
C18 C23 C28 119.1(5) . . ?
C22 C23 C28 119.5(4) . . ?
C21 C24 H24 118.8 . . ?
C25 C24 C21 122.5(6) . . ?
C25 C24 H24 118.8 . . ?
C24 C25 H25 120.4 . . ?
C24 C25 C26 119.2(6) . . ?
C26 C25 H25 120.4 . . ?
C25 C26 H26 119.1 . . ?
C27 C26 C25 121.8(6) . . ?
C27 C26 H26 119.1 . . ?
C22 C27 H27 119.6 . . ?
C26 C27 C22 120.7(6) . . ?
C26 C27 H27 119.6 . . ?
N4 C28 N5 111.6(4) . . ?
N4 C28 C23 125.8(4) . . ?
N5 C28 C23 122.3(4) . . ?
H1A O1 H1B 104.5 . . ?

_olex2_exptl_crystal_mounting_method 'coordinate bond'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.073
_oxdiff_exptl_absorpt_empirical_full_min 0.493
####################################################################### 
# 
# 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_desol@150K
_database_code_depnum_ccdc_archive 'CCDC 1965901'
loop_
_audit_author_name
_audit_author_address
'Jun Tao'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2019-11-15 deposited with the CCDC.	2019-12-30 downloaded from the CCDC.
;
_audit_creation_date             2019-11-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        C28H16Fe0.5N5S
_chemical_formula_moiety         'C56 H32 Fe N10 S2'
_chemical_formula_sum            'C56 H32 Fe N10 S2'
_chemical_formula_weight         964.88
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   12.0479(17)
_cell_length_b                   25.4757(15)
_cell_length_c                   14.6834(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4506.8(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4359
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      28.8960
_cell_measurement_theta_min      3.7150
_shelx_estimated_absorpt_T_max   0.795
_shelx_estimated_absorpt_T_min   0.672
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dull pinkish red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_preparation       'disolvent craystal'
_exptl_crystal_recrystallization_method 'reddish black crystal'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2275
_diffrn_reflns_av_unetI/netI     0.1350
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38906
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.867
_diffrn_reflns_theta_min         3.622
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00   1.00   0.50   70.00    --    0.00  -3.00  19.00   50
  2  ω    -24.00   1.00   0.50   70.00    --    0.00   3.00-163.00   50
  3  ω    -89.00  16.00   0.50   70.00    --    0.00 -38.00  60.00  210
  4  ω    -41.00   6.00   0.50   70.00    --    0.00 -82.00-120.00   94
  5  ω    -12.00  15.00   0.50   70.00    --    0.00  57.00-120.00   54
  6  ω    -44.00 -11.00   0.50   70.00    --    0.00 -82.00 -30.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0572643000
_diffrn_orient_matrix_UB_12      -0.0064098000
_diffrn_orient_matrix_UB_13      -0.0008663000
_diffrn_orient_matrix_UB_21      -0.0135503000
_diffrn_orient_matrix_UB_22      -0.0270593000
_diffrn_orient_matrix_UB_23      0.0022278000
_diffrn_orient_matrix_UB_31      -0.0015867000
_diffrn_orient_matrix_UB_32      -0.0010891000
_diffrn_orient_matrix_UB_33      -0.0482601000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3620
_reflns_number_total             5967
_reflns_odcompleteness_completeness 99.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5967
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2009
_refine_ls_R_factor_gt           0.1308
_refine_ls_restrained_S_all      1.169
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0767P)²+27.7149P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2657
_refine_ls_wR_factor_ref         0.2924
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N5(H5), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.750000 0.250000 0.51479(9) 0.0244(3) Uani 1 2 d S T P . .
S1 S 0.47550(17) 0.19010(7) 0.30694(14) 0.0402(5) Uani 1 1 d . . . . .
N1 N 0.6604(5) 0.20825(19) 0.4163(4) 0.0304(13) Uani 1 1 d . . . . .
N2 N 0.7987(4) 0.30144(18) 0.6295(3) 0.0227(11) Uani 1 1 d . . . . .
N3 N 0.6115(5) 0.30605(18) 0.5315(3) 0.0237(11) Uani 1 1 d . . . . .
N4 N 0.5019(5) 0.46129(19) 0.7106(4) 0.0266(12) Uani 1 1 d . . . . .
N5 N 0.6558(5) 0.45659(18) 0.7954(4) 0.0273(12) Uani 1 1 d . . . . .
H5 H 0.703201 0.464177 0.837187 0.033 Uiso 1 1 calc R . . . .
C1 C 0.5852(6) 0.2000(2) 0.3689(5) 0.0294(15) Uani 1 1 d . . . . .
C2 C 0.8903(5) 0.2975(2) 0.6794(4) 0.0241(13) Uani 1 1 d . . . . .
H2 H 0.939384 0.270315 0.666632 0.029 Uiso 1 1 calc R . . . .
C3 C 0.9166(5) 0.3319(2) 0.7496(4) 0.0264(13) Uani 1 1 d . . . . .
H3 H 0.981186 0.327168 0.783291 0.032 Uiso 1 1 calc R . . . .
C4 C 0.8466(5) 0.3727(2) 0.7689(4) 0.0247(13) Uani 1 1 d . . . . .
H4 H 0.863691 0.396406 0.814896 0.030 Uiso 1 1 calc R . . . .
C5 C 0.7483(6) 0.3782(2) 0.7180(4) 0.0216(11) Uani 1 1 d . . . . .
C6 C 0.7273(5) 0.3414(2) 0.6485(4) 0.0184(12) Uani 1 1 d . . . . .
C7 C 0.6656(5) 0.4177(2) 0.7309(4) 0.0218(12) Uani 1 1 d . . . . .
C8 C 0.5693(5) 0.4213(2) 0.6799(4) 0.0230(13) Uani 1 1 d . . . . .
C9 C 0.5489(5) 0.3845(2) 0.6083(4) 0.0239(13) Uani 1 1 d . . . . .
C10 C 0.6265(5) 0.3442(2) 0.5944(4) 0.0210(12) Uani 1 1 d . . . . .
C11 C 0.4533(6) 0.3844(3) 0.5553(5) 0.0313(15) Uani 1 1 d . . . . .
H11 H 0.399215 0.410039 0.563603 0.038 Uiso 1 1 calc R . . . .
C12 C 0.4396(6) 0.3463(3) 0.4907(5) 0.0368(16) Uani 1 1 d . . . . .
H12 H 0.377117 0.346491 0.453514 0.044 Uiso 1 1 calc R . . . .
C13 C 0.5190(6) 0.3076(2) 0.4809(5) 0.0316(14) Uani 1 1 d . . . . .
H13 H 0.507776 0.281557 0.437492 0.038 Uiso 1 1 calc R . . . .
C14 C 0.6123(7) 0.6537(3) 0.9287(6) 0.049(2) Uani 1 1 d . . . . .
H14 H 0.593096 0.677935 0.973314 0.059 Uiso 1 1 calc R . . . .
C15 C 0.6996(8) 0.6631(3) 0.8761(8) 0.059(3) Uani 1 1 d . . . . .
H15 H 0.739073 0.694262 0.882508 0.070 Uiso 1 1 calc R . . . .
C16 C 0.7326(7) 0.6255(3) 0.8097(7) 0.055(2) Uani 1 1 d . . . . .
H16 H 0.793854 0.632462 0.773113 0.066 Uiso 1 1 calc R . . . .
C17 C 0.6765(6) 0.5795(3) 0.7986(6) 0.0382(17) Uani 1 1 d . . . . .
H17 H 0.699980 0.555149 0.755594 0.046 Uiso 1 1 calc R . . . .
C18 C 0.5815(6) 0.5692(2) 0.8533(5) 0.0336(16) Uani 1 1 d . . . . .
C19 C 0.5470(7) 0.6070(3) 0.9187(5) 0.0368(18) Uani 1 1 d . . . . .
C20 C 0.4472(7) 0.6005(3) 0.9649(5) 0.0376(18) Uani 1 1 d . . . . .
H20 H 0.424063 0.626367 1.005424 0.045 Uiso 1 1 calc R . . . .
C21 C 0.3818(6) 0.5568(3) 0.9522(4) 0.0315(16) Uani 1 1 d . . . . .
C22 C 0.4184(6) 0.5160(2) 0.8918(4) 0.0281(14) Uani 1 1 d . . . . .
C23 C 0.5174(6) 0.5232(2) 0.8435(4) 0.0270(13) Uani 1 1 d . . . . .
C24 C 0.2758(6) 0.5513(3) 0.9954(5) 0.0415(19) Uani 1 1 d . . . . .
H24 H 0.249483 0.578487 1.031642 0.050 Uiso 1 1 calc R . . . .
C25 C 0.2134(7) 0.5081(3) 0.9852(5) 0.0443(19) Uani 1 1 d . . . . .
H25 H 0.143837 0.505963 1.012419 0.053 Uiso 1 1 calc R . . . .
C26 C 0.2545(8) 0.4662(3) 0.9329(5) 0.0450(18) Uani 1 1 d . . . . .
H26 H 0.214198 0.435109 0.929651 0.054 Uiso 1 1 calc R . . . .
C27 C 0.3529(6) 0.4703(3) 0.8866(5) 0.0345(16) Uani 1 1 d . . . . .
H27 H 0.376938 0.442307 0.850994 0.041 Uiso 1 1 calc R . . . .
C28 C 0.5565(6) 0.4808(2) 0.7804(4) 0.0274(14) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.094(6) 2_655 ?
Fe1 N1 2.094(6) . ?
Fe1 N2 2.213(5) . ?
Fe1 N2 2.213(5) 2_655 ?
Fe1 N3 2.210(5) . ?
Fe1 N3 2.210(5) 2_655 ?
S1 C1 1.624(8) . ?
N1 C1 1.162(9) . ?
N2 C2 1.329(8) . ?
N2 C6 1.362(7) . ?
N3 C10 1.354(7) . ?
N3 C13 1.339(9) . ?
N4 C8 1.378(8) . ?
N4 C28 1.315(9) . ?
N5 H5 0.8600 . ?
N5 C7 1.375(7) . ?
N5 C28 1.364(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.389(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.368(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.406(9) . ?
C5 C6 1.409(8) . ?
C5 C7 1.429(8) . ?
C6 C10 1.452(8) . ?
C7 C8 1.384(9) . ?
C8 C9 1.430(8) . ?
C9 C10 1.404(8) . ?
C9 C11 1.391(9) . ?
C11 H11 0.9300 . ?
C11 C12 1.366(9) . ?
C12 H12 0.9300 . ?
C12 C13 1.382(9) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.327(13) . ?
C14 C19 1.434(11) . ?
C15 H15 0.9300 . ?
C15 C16 1.423(12) . ?
C16 H16 0.9300 . ?
C16 C17 1.362(10) . ?
C17 H17 0.9300 . ?
C17 C18 1.423(11) . ?
C18 C19 1.422(9) . ?
C18 C23 1.411(9) . ?
C19 C20 1.390(11) . ?
C20 H20 0.9300 . ?
C20 C21 1.377(11) . ?
C21 C22 1.435(8) . ?
C21 C24 1.433(11) . ?
C22 C23 1.400(10) . ?
C22 C27 1.409(10) . ?
C23 C28 1.498(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.340(12) . ?
C25 H25 0.9300 . ?
C25 C26 1.406(11) . ?
C26 H26 0.9300 . ?
C26 C27 1.371(11) . ?
C27 H27 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
N1 Fe1 N1 92.7(3) 2_655 . ?
N1 Fe1 N2 95.0(2) 2_655 . ?
N1 Fe1 N2 164.3(2) . . ?
N1 Fe1 N2 164.3(2) 2_655 2_655 ?
N1 Fe1 N2 95.0(2) . 2_655 ?
N1 Fe1 N3 97.9(2) 2_655 . ?
N1 Fe1 N3 90.9(2) 2_655 2_655 ?
N1 Fe1 N3 90.9(2) . . ?
N1 Fe1 N3 97.9(2) . 2_655 ?
N2 Fe1 N2 80.9(2) 2_655 . ?
N3 Fe1 N2 95.64(19) 2_655 . ?
N3 Fe1 N2 95.64(19) . 2_655 ?
N3 Fe1 N2 74.52(19) 2_655 2_655 ?
N3 Fe1 N2 74.52(19) . . ?
N3 Fe1 N3 167.3(3) . 2_655 ?
C1 N1 Fe1 155.1(5) . . ?
C2 N2 Fe1 126.5(4) . . ?
C2 N2 C6 117.9(5) . . ?
C6 N2 Fe1 115.6(4) . . ?
C10 N3 Fe1 116.0(4) . . ?
C13 N3 Fe1 125.9(4) . . ?
C13 N3 C10 118.0(5) . . ?
C28 N4 C8 103.8(5) . . ?
C7 N5 H5 126.6 . . ?
C28 N5 H5 126.6 . . ?
C28 N5 C7 106.8(5) . . ?
N1 C1 S1 176.8(6) . . ?
N2 C2 H2 118.3 . . ?
N2 C2 C3 123.5(5) . . ?
C3 C2 H2 118.3 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(6) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(6) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 C6 118.0(5) . . ?
C4 C5 C7 126.0(5) . . ?
C6 C5 C7 116.0(6) . . ?
N2 C6 C5 122.2(5) . . ?
N2 C6 C10 116.9(5) . . ?
C5 C6 C10 120.9(5) . . ?
N5 C7 C5 131.1(6) . . ?
N5 C7 C8 104.7(5) . . ?
C8 C7 C5 124.1(5) . . ?
N4 C8 C7 111.5(5) . . ?
N4 C8 C9 128.5(6) . . ?
C7 C8 C9 119.9(5) . . ?
C10 C9 C8 118.2(6) . . ?
C11 C9 C8 123.8(6) . . ?
C11 C9 C10 118.0(6) . . ?
N3 C10 C6 116.8(5) . . ?
N3 C10 C9 122.4(6) . . ?
C9 C10 C6 120.9(5) . . ?
C9 C11 H11 120.3 . . ?
C12 C11 C9 119.3(6) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.7(7) . . ?
C13 C12 H12 120.1 . . ?
N3 C13 C12 122.6(6) . . ?
N3 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
C15 C14 H14 119.1 . . ?
C15 C14 C19 121.7(7) . . ?
C19 C14 H14 119.1 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.9(7) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 119.3 . . ?
C17 C16 C15 121.5(9) . . ?
C17 C16 H16 119.3 . . ?
C16 C17 H17 120.3 . . ?
C16 C17 C18 119.4(7) . . ?
C18 C17 H17 120.3 . . ?
C19 C18 C17 119.4(7) . . ?
C23 C18 C17 122.4(6) . . ?
C23 C18 C19 118.2(7) . . ?
C18 C19 C14 118.1(8) . . ?
C20 C19 C14 121.5(7) . . ?
C20 C19 C18 120.2(7) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 121.6(6) . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C22 119.6(7) . . ?
C20 C21 C24 122.0(6) . . ?
C24 C21 C22 118.4(7) . . ?
C23 C22 C21 118.7(6) . . ?
C23 C22 C27 123.8(6) . . ?
C27 C22 C21 117.4(6) . . ?
C18 C23 C28 119.3(6) . . ?
C22 C23 C18 121.5(6) . . ?
C22 C23 C28 119.2(6) . . ?
C21 C24 H24 118.9 . . ?
C25 C24 C21 122.1(7) . . ?
C25 C24 H24 118.9 . . ?
C24 C25 H25 120.4 . . ?
C24 C25 C26 119.1(8) . . ?
C26 C25 H25 120.4 . . ?
C25 C26 H26 119.4 . . ?
C27 C26 C25 121.2(8) . . ?
C27 C26 H26 119.4 . . ?
C22 C27 H27 119.3 . . ?
C26 C27 C22 121.3(6) . . ?
C26 C27 H27 119.3 . . ?
N4 C28 N5 113.3(5) . . ?
N4 C28 C23 126.6(6) . . ?
N5 C28 C23 120.1(6) . . ?

_olex2_exptl_crystal_mounting_method 'coordinate bond'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.937
_oxdiff_exptl_absorpt_empirical_full_min 0.257
####################################################################### 
# 
# 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_MeOH@300K
_database_code_depnum_ccdc_archive 'CCDC 1965899'
loop_
_audit_author_name
_audit_author_address
'Jun Tao'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2019-11-15 deposited with the CCDC.	2019-12-30 downloaded from the CCDC.
;
_audit_creation_date             2019-11-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        C59H38FeN10O3S2
_chemical_formula_moiety         'C56 H32 Fe N10 S2, 3(C H4 O)'
_chemical_formula_sum            'C59 H44 Fe N10 O3 S2'
_chemical_formula_weight         1061.01
_chemical_melting_point          ?
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   12.1817(8)
_cell_length_b                   25.0030(17)
_cell_length_c                   17.0415(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5190.5(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5588
_cell_measurement_temperature    299.96(10)
_cell_measurement_theta_max      26.1190
_cell_measurement_theta_min      3.6400
_shelx_estimated_absorpt_T_max   0.814
_shelx_estimated_absorpt_T_min   0.699
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_preparation       
'FeCl2.6H2O (0.8 g, 0.003mol) and enough ascorbic acid was dissolved by MeOH(100 ml).Then the mixed solution was filtered. Pyridine (40 ml) was added when the filtrate was stirred. Yellow precipitate was collected.'
_exptl_crystal_recrystallization_method 'Reddish black crystals'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33916
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.622
_diffrn_reflns_theta_min         3.645
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.96(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00 -19.00   0.50   60.00    --    0.00 -42.00   1.00   50
  2  ω      1.00  36.00   0.50   60.00    --    0.00  42.00 153.00   70
  3  ω    -22.00   8.00   0.50   60.00    --    0.00  57.00  60.00   60
  4  ω     28.00  54.00   0.50   60.00    --    0.00  57.00  60.00   52
  5  ω    -47.00   8.00   0.50   60.00    --    0.00 -82.00 -60.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0356536000
_diffrn_orient_matrix_UB_12      -0.0222343000
_diffrn_orient_matrix_UB_13      -0.0044031000
_diffrn_orient_matrix_UB_21      0.0370908000
_diffrn_orient_matrix_UB_22      0.0161003000
_diffrn_orient_matrix_UB_23      -0.0216046000
_diffrn_orient_matrix_UB_31      0.0271830000
_diffrn_orient_matrix_UB_32      0.0071446000
_diffrn_orient_matrix_UB_33      0.0353372000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4543
_reflns_number_total             6462
_reflns_odcompleteness_completeness 98.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6462
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0517
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0578P)²+2.5630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1399
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.05
3. Others
 Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) O2(0.5) H2A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N5(H5), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27)
4.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.750000 0.750000 0.52606(3) 0.05057(15) Uani 1 2 d S T P . .
S1 S 0.52411(9) 0.67869(4) 0.32077(6) 0.1036(3) Uani 1 1 d . . . . .
O1 O 1.12417(12) 0.47970(7) 0.63688(9) 0.0539(4) Uani 1 1 d . . . . .
H1 H 1.084414 0.499093 0.663295 0.081 Uiso 1 1 calc GR . . . .
N1 N 0.6604(2) 0.70826(9) 0.44388(15) 0.0738(6) Uani 1 1 d . . . . .
N2 N 0.68963(14) 0.70147(6) 0.62254(10) 0.0422(4) Uani 1 1 d . . . . .
N3 N 0.87655(15) 0.69158(7) 0.54178(10) 0.0463(4) Uani 1 1 d . . . . .
N4 N 0.96768(14) 0.53731(7) 0.71127(9) 0.0435(4) Uani 1 1 d . . . . .
N5 N 0.81057(14) 0.54509(7) 0.77727(9) 0.0420(4) Uani 1 1 d . . . . .
H5 H 0.759988 0.538949 0.811300 0.050 Uiso 1 1 calc R . . . .
C1 C 0.6041(2) 0.69576(9) 0.39195(17) 0.0637(7) Uani 1 1 d . . . . .
C2 C 0.60077(18) 0.70994(9) 0.66589(13) 0.0508(5) Uani 1 1 d . . . . .
H2 H 0.555768 0.738689 0.653067 0.061 Uiso 1 1 calc R . . . .
C3 C 0.57133(19) 0.67810(10) 0.72953(15) 0.0568(6) Uani 1 1 d . . . . .
H3 H 0.508917 0.685944 0.758770 0.068 Uiso 1 1 calc R . . . .
C4 C 0.63572(18) 0.63502(9) 0.74844(14) 0.0516(5) Uani 1 1 d . . . . .
H4 H 0.616499 0.612702 0.789882 0.062 Uiso 1 1 calc R . . . .
C5 C 0.73089(16) 0.62501(8) 0.70458(12) 0.0397(4) Uani 1 1 d . . . . .
C6 C 0.75598(16) 0.65981(7) 0.64241(11) 0.0376(4) Uani 1 1 d . . . . .
C7 C 0.80861(16) 0.58345(8) 0.71960(11) 0.0391(4) Uani 1 1 d . . . . .
C8 C 0.90580(16) 0.57814(7) 0.67935(11) 0.0385(4) Uani 1 1 d . . . . .
C9 C 0.93477(16) 0.61425(8) 0.61715(11) 0.0397(4) Uani 1 1 d . . . . .
C10 C 0.85755(16) 0.65453(7) 0.59871(11) 0.0385(4) Uani 1 1 d . . . . .
C11 C 1.03482(19) 0.61384(9) 0.57632(13) 0.0503(5) Uani 1 1 d . . . . .
H11 H 1.088149 0.588352 0.587539 0.060 Uiso 1 1 calc R . . . .
C12 C 1.0524(2) 0.65173(10) 0.51958(14) 0.0585(6) Uani 1 1 d . . . . .
H12 H 1.118226 0.652163 0.491921 0.070 Uiso 1 1 calc R . . . .
C13 C 0.9722(2) 0.68938(9) 0.50349(14) 0.0561(6) Uani 1 1 d . . . . .
H13 H 0.985431 0.714324 0.464136 0.067 Uiso 1 1 calc R . . . .
C14 C 0.8442(3) 0.34088(12) 0.8912(2) 0.0891(10) Uani 1 1 d . . . . .
H14 H 0.859421 0.315587 0.929732 0.107 Uiso 1 1 calc R . . . .
C15 C 0.7639(3) 0.33121(12) 0.8396(3) 0.0994(12) Uani 1 1 d . . . . .
H15 H 0.724331 0.299470 0.842707 0.119 Uiso 1 1 calc R . . . .
C16 C 0.7387(3) 0.36867(12) 0.7805(2) 0.0887(10) Uani 1 1 d . . . . .
H16 H 0.683628 0.361141 0.744313 0.106 Uiso 1 1 calc R . . . .
C17 C 0.7940(2) 0.41554(10) 0.77601(17) 0.0646(6) Uani 1 1 d . . . . .
H17 H 0.775404 0.440035 0.737138 0.078 Uiso 1 1 calc R . . . .
C18 C 0.88016(19) 0.42818(9) 0.82969(13) 0.0517(5) Uani 1 1 d . . . . .
C19 C 0.9075(2) 0.38929(10) 0.88874(16) 0.0645(7) Uani 1 1 d . . . . .
C20 C 0.9947(3) 0.39908(12) 0.93851(15) 0.0731(8) Uani 1 1 d . . . . .
H20 H 1.011749 0.373861 0.976732 0.088 Uiso 1 1 calc R . . . .
C21 C 1.0583(2) 0.44547(12) 0.93353(13) 0.0644(7) Uani 1 1 d . . . . .
C22 C 1.03063(18) 0.48530(10) 0.87640(12) 0.0502(5) Uani 1 1 d . . . . .
C23 C 0.94078(17) 0.47602(8) 0.82588(11) 0.0450(5) Uani 1 1 d . . . . .
C24 C 1.1490(3) 0.45545(18) 0.98449(16) 0.0866(10) Uani 1 1 d . . . . .
H24 H 1.169205 0.429554 1.020905 0.104 Uiso 1 1 calc R . . . .
C25 C 1.2057(3) 0.5013(2) 0.98102(18) 0.0952(11) Uani 1 1 d . . . . .
H25 H 1.263865 0.507049 1.015367 0.114 Uiso 1 1 calc R . . . .
C26 C 1.1778(2) 0.54059(15) 0.92579(17) 0.0831(9) Uani 1 1 d . . . . .
H26 H 1.218325 0.572084 0.923750 0.100 Uiso 1 1 calc R . . . .
C27 C 1.0928(2) 0.53360(12) 0.87526(14) 0.0624(6) Uani 1 1 d . . . . .
H27 H 1.075121 0.560460 0.839700 0.075 Uiso 1 1 calc R . . . .
C28 C 0.90779(17) 0.51860(8) 0.77033(11) 0.0427(4) Uani 1 1 d . . . . .
C29 C 1.0596(3) 0.44943(11) 0.58506(15) 0.0702(7) Uani 1 1 d . . . . .
H29A H 1.038406 0.471251 0.541257 0.105 Uiso 1 1 calc GR . . . .
H29B H 0.995123 0.437025 0.611851 0.105 Uiso 1 1 calc GR . . . .
H29C H 1.101133 0.419308 0.566636 0.105 Uiso 1 1 calc GR . . . .
C30 C 0.250000 0.750000 0.3800(6) 0.171(4) Uani 1 2 d S TU P . .
H30A H 0.201446 0.732169 0.344152 0.256 Uiso 0.5 1 calc GR . . A -1
H30B H 0.287164 0.723935 0.411695 0.256 Uiso 0.5 1 calc GR . . A -1
H30C H 0.303008 0.770394 0.350967 0.256 Uiso 0.5 1 calc GR . . A -1
O2 O 0.1936(10) 0.7819(7) 0.4249(5) 0.235(6) Uani 0.5 1 d . U . B -1
H2A H 0.140400 0.793280 0.400658 0.353 Uiso 0.5 1 calc GR . . B -1


_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 2.060(3) . ?
Fe1 N1 2.060(3) 2_665 ?
Fe1 N2 2.1718(17) 2_665 ?
Fe1 N2 2.1717(17) . ?
Fe1 N3 2.1405(19) 2_665 ?
Fe1 N3 2.1406(19) . ?
S1 C1 1.613(3) . ?
O1 H1 0.8200 . ?
O1 C29 1.404(3) . ?
N1 C1 1.162(4) . ?
N2 C2 1.328(3) . ?
N2 C6 1.361(2) . ?
N3 C10 1.361(2) . ?
N3 C13 1.336(3) . ?
N4 C8 1.381(2) . ?
N4 C28 1.328(3) . ?
N5 H5 0.8600 . ?
N5 C7 1.373(2) . ?
N5 C28 1.362(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.392(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.371(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.402(3) . ?
C5 C6 1.405(3) . ?
C5 C7 1.429(3) . ?
C6 C10 1.450(3) . ?
C7 C8 1.375(3) . ?
C8 C9 1.436(3) . ?
C9 C10 1.413(3) . ?
C9 C11 1.404(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.370(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.385(3) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.338(5) . ?
C14 C19 1.436(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.409(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.354(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.428(4) . ?
C18 C19 1.438(3) . ?
C18 C23 1.407(3) . ?
C19 C20 1.381(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.397(4) . ?
C21 C22 1.433(3) . ?
C21 C24 1.428(4) . ?
C22 C23 1.412(3) . ?
C22 C27 1.426(4) . ?
C23 C28 1.480(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.339(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.403(5) . ?
C26 H26 0.9300 . ?
C26 C27 1.358(4) . ?
C27 H27 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30 O2 1.301(9) . ?
O2 H2A 0.8200 . ?

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 N1 94.33(13) . 2_665 ?
N1 Fe1 N2 167.78(8) . 2_665 ?
N1 Fe1 N2 92.99(8) 2_665 2_665 ?
N1 Fe1 N2 92.99(8) . . ?
N1 Fe1 N2 167.78(8) 2_665 . ?
N1 Fe1 N3 92.81(8) . 2_665 ?
N1 Fe1 N3 96.95(8) . . ?
N1 Fe1 N3 96.95(8) 2_665 2_665 ?
N1 Fe1 N3 92.81(8) 2_665 . ?
N2 Fe1 N2 81.58(9) . 2_665 ?
N3 Fe1 N2 76.58(6) 2_665 2_665 ?
N3 Fe1 N2 92.44(7) 2_665 . ?
N3 Fe1 N2 76.58(6) . . ?
N3 Fe1 N2 92.44(7) . 2_665 ?
N3 Fe1 N3 165.62(9) 2_665 . ?
C29 O1 H1 109.5 . . ?
C1 N1 Fe1 165.1(2) . . ?
C2 N2 Fe1 127.47(14) . . ?
C2 N2 C6 117.89(17) . . ?
C6 N2 Fe1 114.51(13) . . ?
C10 N3 Fe1 115.54(13) . . ?
C13 N3 Fe1 126.49(15) . . ?
C13 N3 C10 117.92(19) . . ?
C28 N4 C8 105.02(16) . . ?
C7 N5 H5 126.5 . . ?
C28 N5 H5 126.5 . . ?
C28 N5 C7 107.01(16) . . ?
N1 C1 S1 179.0(3) . . ?
N2 C2 H2 118.2 . . ?
N2 C2 C3 123.52(19) . . ?
C3 C2 H2 118.2 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.0(2) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(2) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 118.14(18) . . ?
C4 C5 C7 125.61(18) . . ?
C6 C5 C7 116.19(17) . . ?
N2 C6 C5 122.17(18) . . ?
N2 C6 C10 116.65(17) . . ?
C5 C6 C10 121.11(17) . . ?
N5 C7 C5 130.36(18) . . ?
N5 C7 C8 105.94(16) . . ?
C8 C7 C5 123.47(18) . . ?
N4 C8 C9 128.42(18) . . ?
C7 C8 N4 110.18(17) . . ?
C7 C8 C9 121.27(17) . . ?
C10 C9 C8 116.64(17) . . ?
C11 C9 C8 125.08(19) . . ?
C11 C9 C10 118.22(18) . . ?
N3 C10 C6 116.69(17) . . ?
N3 C10 C9 122.02(18) . . ?
C9 C10 C6 121.23(17) . . ?
C9 C11 H11 120.6 . . ?
C12 C11 C9 118.7(2) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 119.9(2) . . ?
C13 C12 H12 120.0 . . ?
N3 C13 C12 123.1(2) . . ?
N3 C13 H13 118.4 . . ?
C12 C13 H13 118.4 . . ?
C15 C14 H14 119.1 . . ?
C15 C14 C19 121.7(3) . . ?
C19 C14 H14 119.1 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.6(3) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 119.3 . . ?
C16 C17 C18 121.4(3) . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C19 118.0(2) . . ?
C23 C18 C17 123.0(2) . . ?
C23 C18 C19 119.0(2) . . ?
C14 C19 C18 117.8(3) . . ?
C20 C19 C14 123.0(3) . . ?
C20 C19 C18 119.2(3) . . ?
C19 C20 H20 118.8 . . ?
C19 C20 C21 122.4(2) . . ?
C21 C20 H20 118.8 . . ?
C20 C21 C22 119.2(2) . . ?
C20 C21 C24 122.5(3) . . ?
C24 C21 C22 118.3(3) . . ?
C23 C22 C21 118.8(2) . . ?
C23 C22 C27 122.9(2) . . ?
C27 C22 C21 118.2(2) . . ?
C18 C23 C22 121.22(19) . . ?
C18 C23 C28 119.90(19) . . ?
C22 C23 C28 118.8(2) . . ?
C21 C24 H24 119.3 . . ?
C25 C24 C21 121.5(3) . . ?
C25 C24 H24 119.3 . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.3(3) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 119.3 . . ?
C27 C26 C25 121.3(3) . . ?
C27 C26 H26 119.3 . . ?
C22 C27 H27 119.8 . . ?
C26 C27 C22 120.4(3) . . ?
C26 C27 H27 119.8 . . ?
N4 C28 N5 111.85(17) . . ?
N4 C28 C23 126.07(18) . . ?
N5 C28 C23 122.02(18) . . ?
O1 C29 H29A 109.5 . . ?
O1 C29 H29B 109.5 . . ?
O1 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O2 C30 H30A 109.5 . . ?
O2 C30 H30B 109.5 . . ?
O2 C30 H30C 109.5 . . ?
C30 O2 H2A 109.5 . . ?

_olex2_exptl_crystal_mounting_method 'coordinate bond'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.699
####################################################################### 
# 
# 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_MeOH@150K
_database_code_depnum_ccdc_archive 'CCDC 1965902'
loop_
_audit_author_name
_audit_author_address
'Jun Tao'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2019-11-15 deposited with the CCDC.	2019-12-30 downloaded from the CCDC.
;
_audit_creation_date             2019-11-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        C59H38FeN10O3S2
_chemical_formula_moiety         'C56 H32 Fe N10 S2, 3(C H4 O)'
_chemical_formula_sum            'C59 H44 Fe N10 O3 S2'
_chemical_formula_weight         1061.01
_chemical_melting_point          ?
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   11.9880(3)
_cell_length_b                   24.7721(7)
_cell_length_c                   16.8246(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4996.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15987
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.8950
_cell_measurement_theta_min      3.8990
_shelx_estimated_absorpt_T_max   0.808
_shelx_estimated_absorpt_T_min   0.690
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dull pinkish red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2200
_exptl_crystal_preparation       
'FeCl2.6H2O (0.8 g, 0.003mol) and enough ascorbic acid was dissolved by MeOH(100 ml).Then the mixed solution was filtered. Pyridine (40 ml) was added when the filtrate was stirred. Yellow precipitate was collected.'
_exptl_crystal_recrystallization_method 'Reddish black crystals'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35135
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         3.701
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00  60.00   0.50   90.00    --    0.00  47.00  65.00   50
  2  ω    -50.00  -2.00   0.50   90.00    --    0.00 -82.00   0.00   96
  3  ω      3.00  28.00   0.50   90.00    --    0.00 -82.00   0.00   50
  4  ω    -60.00 -34.00   0.50   90.00    --    0.00 -82.00-150.00   52
  5  ω    -56.00 -28.00   0.50   90.00    --    0.00 -82.00 -30.00   56
  6  ω    -18.00  23.00   0.50   90.00    --    0.00 -77.00 -90.00   82
  7  ω    -50.00 -20.00   0.50   90.00    --    0.00 -82.00-120.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0378370000
_diffrn_orient_matrix_UB_12      0.0145526000
_diffrn_orient_matrix_UB_13      0.0242888000
_diffrn_orient_matrix_UB_21      0.0339293000
_diffrn_orient_matrix_UB_22      0.0233662000
_diffrn_orient_matrix_UB_23      -0.0035026000
_diffrn_orient_matrix_UB_31      -0.0302331000
_diffrn_orient_matrix_UB_32      0.0079364000
_diffrn_orient_matrix_UB_33      -0.0342900000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4289
_reflns_number_total             4644
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4644
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0299
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0395P)²+3.2344P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0816
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) O2(0.5) H2A(0.5)
3.a Riding coordinates:
 O1(H1), C29(H29A,H29B,H29C), O2(H2A)
3.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.250000 0.250000 0.46305(2) 0.01881(9) Uani 1 2 d S T P . .
S1 S 0.46194(4) 0.32562(2) 0.67152(3) 0.03859(13) Uani 1 1 d . . . . .
N1 N 0.32733(11) 0.29074(5) 0.54540(7) 0.0245(3) Uani 1 1 d . . . . .
N2 N 0.31423(10) 0.29482(5) 0.37779(7) 0.0190(2) Uani 1 1 d . . . . .
N3 N 0.12903(11) 0.30405(5) 0.45770(7) 0.0204(3) Uani 1 1 d . . . . .
N4 N 0.03652(10) 0.46266(5) 0.29133(7) 0.0207(3) Uani 1 1 d . . . . .
N5 N 0.19610(10) 0.45536(5) 0.22491(7) 0.0202(3) Uani 1 1 d . . . . .
H5 H 0.247538 0.461830 0.190571 0.024 Uiso 1 1 calc R . . . .
C1 C 0.38155(13) 0.30567(6) 0.59833(9) 0.0233(3) Uani 1 1 d . . . . .
C2 C 0.40495(12) 0.28576(6) 0.33383(9) 0.0233(3) Uani 1 1 d . . . . .
H2 H 0.449270 0.256076 0.345972 0.028 Uiso 1 1 calc R . . . .
C3 C 0.43637(13) 0.31873(7) 0.27056(10) 0.0268(3) Uani 1 1 d . . . . .
H3 H 0.499588 0.310453 0.240925 0.032 Uiso 1 1 calc R . . . .
C4 C 0.37387(13) 0.36349(6) 0.25199(9) 0.0244(3) Uani 1 1 d . . . . .
H4 H 0.395240 0.386364 0.210895 0.029 Uiso 1 1 calc R . . . .
C5 C 0.27703(12) 0.37397(6) 0.29637(8) 0.0193(3) Uani 1 1 d . . . . .
C6 C 0.24942(12) 0.33824(6) 0.35825(8) 0.0182(3) Uani 1 1 d . . . . .
C7 C 0.19844(12) 0.41621(6) 0.28255(8) 0.0192(3) Uani 1 1 d . . . . .
C8 C 0.09895(12) 0.42130(6) 0.32342(8) 0.0194(3) Uani 1 1 d . . . . .
C9 C 0.06870(12) 0.38420(6) 0.38522(8) 0.0194(3) Uani 1 1 d . . . . .
C10 C 0.14714(12) 0.34335(6) 0.40216(8) 0.0185(3) Uani 1 1 d . . . . .
C11 C -0.03295(13) 0.38344(6) 0.42661(9) 0.0239(3) Uani 1 1 d . . . . .
H11 H -0.087595 0.409172 0.416389 0.029 Uiso 1 1 calc R . . . .
C12 C -0.05006(13) 0.34379(6) 0.48265(9) 0.0273(3) Uani 1 1 d . . . . .
H12 H -0.116758 0.342709 0.510838 0.033 Uiso 1 1 calc R . . . .
C13 C 0.03236(13) 0.30517(6) 0.49736(9) 0.0252(3) Uani 1 1 d . . . . .
H13 H 0.019499 0.279224 0.536251 0.030 Uiso 1 1 calc R . . . .
C14 C -0.14585(16) 0.54660(9) 0.01383(10) 0.0399(4) Uani 1 1 d . . . . .
H14 H -0.165389 0.572681 -0.023421 0.048 Uiso 1 1 calc R . . . .
C15 C -0.20461(16) 0.50023(10) 0.01742(11) 0.0446(5) Uani 1 1 d . . . . .
H15 H -0.264001 0.494696 -0.017192 0.054 Uiso 1 1 calc R . . . .
C16 C -0.17632(15) 0.45989(8) 0.07367(10) 0.0388(4) Uani 1 1 d . . . . .
H16 H -0.217026 0.427954 0.075317 0.047 Uiso 1 1 calc R . . . .
C17 C -0.09023(13) 0.46735(7) 0.12534(10) 0.0294(4) Uani 1 1 d . . . . .
H17 H -0.072687 0.440373 0.161687 0.035 Uiso 1 1 calc R . . . .
C18 C -0.02665(13) 0.51599(6) 0.12442(9) 0.0244(3) Uani 1 1 d . . . . .
C19 C -0.05423(14) 0.55643(7) 0.06611(9) 0.0301(4) Uani 1 1 d . . . . .
C20 C 0.01047(15) 0.60306(7) 0.06108(10) 0.0340(4) Uani 1 1 d . . . . .
H20 H -0.006369 0.628510 0.022254 0.041 Uiso 1 1 calc R . . . .
C21 C 0.09932(14) 0.61276(6) 0.11219(10) 0.0301(4) Uani 1 1 d . . . . .
C22 C 0.12610(13) 0.57345(6) 0.17209(9) 0.0252(3) Uani 1 1 d . . . . .
C23 C 0.06435(13) 0.52531(6) 0.17586(9) 0.0222(3) Uani 1 1 d . . . . .
C24 C 0.16353(16) 0.66141(7) 0.10897(12) 0.0409(5) Uani 1 1 d . . . . .
H24 H 0.148616 0.686650 0.069459 0.049 Uiso 1 1 calc R . . . .
C25 C 0.24533(17) 0.67141(7) 0.16215(14) 0.0458(5) Uani 1 1 d . . . . .
H25 H 0.285606 0.703426 0.159103 0.055 Uiso 1 1 calc R . . . .
C26 C 0.27016(16) 0.63341(7) 0.22256(13) 0.0416(5) Uani 1 1 d . . . . .
H26 H 0.325562 0.641022 0.259590 0.050 Uiso 1 1 calc R . . . .
C27 C 0.21353(14) 0.58582(7) 0.22683(11) 0.0318(4) Uani 1 1 d . . . . .
H27 H 0.232115 0.560954 0.266067 0.038 Uiso 1 1 calc R . . . .
C28 C 0.09770(12) 0.48202(6) 0.23203(9) 0.0204(3) Uani 1 1 d . . . . .
O1 O 0.37795(9) 0.48040(4) 0.13456(6) 0.0269(2) Uani 1 1 d . . . . .
H1 H 0.422772 0.495767 0.166501 0.032 Uiso 1 1 d R . . . .
C29 C 0.44043(16) 0.44735(7) 0.08240(10) 0.0350(4) Uani 1 1 d . . . . .
H29A H 0.393864 0.414657 0.071055 0.057(7) Uiso 1 1 d R . . . .
H29B H 0.511564 0.435127 0.109245 0.071(8) Uiso 1 1 d R . . . .
H29C H 0.456434 0.465657 0.034695 0.059(7) Uiso 1 1 d R . . . .
C30 C 0.750000 0.250000 0.6250(2) 0.0742(11) Uani 1 2 d S T P . .
H30A H 0.806602 0.231672 0.594960 0.111 Uiso 0.5 1 calc GR . . A .
H30B H 0.698766 0.224033 0.646455 0.111 Uiso 0.5 1 calc GR . . . .
H30C H 0.784108 0.269781 0.667601 0.111 Uiso 0.5 1 calc GR . . . .
O2 O 0.6921(4) 0.2860(2) 0.5750(2) 0.0962(16) Uani 0.5 1 d . . . A -1
H2A H 0.633303 0.296623 0.598436 0.115 Uiso 0.5 1 d R . . A -1


_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 1.9487(13) . ?
Fe1 N1 1.9487(13) 2 ?
Fe1 N2 1.9706(12) . ?
Fe1 N2 1.9707(12) 2 ?
Fe1 N3 1.9758(12) 2 ?
Fe1 N3 1.9758(12) . ?
S1 C1 1.6399(16) . ?
N1 C1 1.163(2) . ?
N2 C2 1.3342(19) . ?
N2 C6 1.3671(18) . ?
N3 C10 1.3667(18) . ?
N3 C13 1.337(2) . ?
N4 C8 1.3789(18) . ?
N4 C28 1.3279(19) . ?
N5 H5 0.8600 . ?
N5 C7 1.3718(18) . ?
N5 C28 1.3572(19) . ?
C2 H2 0.9300 . ?
C2 C3 1.394(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.374(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.404(2) . ?
C5 C6 1.406(2) . ?
C5 C7 1.427(2) . ?
C6 C10 1.437(2) . ?
C7 C8 1.382(2) . ?
C8 C9 1.434(2) . ?
C9 C10 1.411(2) . ?
C9 C11 1.404(2) . ?
C11 H11 0.9300 . ?
C11 C12 1.377(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.398(2) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.349(3) . ?
C14 C19 1.428(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.417(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.362(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.426(2) . ?
C18 C19 1.441(2) . ?
C18 C23 1.412(2) . ?
C19 C20 1.394(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.390(3) . ?
C21 C22 1.438(2) . ?
C21 C24 1.431(3) . ?
C22 C23 1.405(2) . ?
C22 C27 1.429(2) . ?
C23 C28 1.484(2) . ?
C24 H24 0.9300 . ?
C24 C25 1.350(3) . ?
C25 H25 0.9300 . ?
C25 C26 1.417(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.362(3) . ?
C27 H27 0.9300 . ?
O1 H1 0.8500 . ?
O1 C29 1.415(2) . ?
C29 H29A 1.0019 . ?
C29 H29B 1.0113 . ?
C29 H29C 0.9416 . ?
C30 H30A 0.96(4) 2_655 ?
C30 H30A 0.9600 . ?
C30 H30B 0.96(3) 2_655 ?
C30 H30B 0.9600 . ?
C30 H30C 0.96(5) 2_655 ?
C30 H30C 0.9600 . ?
C30 O2 1.408(4) . ?
O2 H2A 0.8499 . ?

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 N1 89.37(8) . 2 ?
N1 Fe1 N2 174.39(5) 2 . ?
N1 Fe1 N2 92.29(5) 2 2 ?
N1 Fe1 N2 92.29(5) . . ?
N1 Fe1 N2 174.39(5) . 2 ?
N1 Fe1 N3 91.76(5) 2 2 ?
N1 Fe1 N3 91.96(5) 2 . ?
N1 Fe1 N3 91.76(5) . . ?
N1 Fe1 N3 91.95(5) . 2 ?
N2 Fe1 N2 86.57(7) . 2 ?
N2 Fe1 N3 82.64(5) 2 2 ?
N2 Fe1 N3 93.54(5) 2 . ?
N2 Fe1 N3 82.64(5) . . ?
N2 Fe1 N3 93.54(5) . 2 ?
N3 Fe1 N3 174.77(7) 2 . ?
C1 N1 Fe1 167.18(12) . . ?
C2 N2 Fe1 128.85(10) . . ?
C2 N2 C6 117.53(12) . . ?
C6 N2 Fe1 113.35(9) . . ?
C10 N3 Fe1 113.41(9) . . ?
C13 N3 Fe1 128.84(10) . . ?
C13 N3 C10 117.65(13) . . ?
C28 N4 C8 105.24(12) . . ?
C7 N5 H5 126.3 . . ?
C28 N5 H5 126.3 . . ?
C28 N5 C7 107.41(12) . . ?
N1 C1 S1 177.91(15) . . ?
N2 C2 H2 118.5 . . ?
N2 C2 C3 123.04(14) . . ?
C3 C2 H2 118.5 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 119.94(14) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.7 . . ?
C3 C4 C5 118.62(14) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 C6 118.16(13) . . ?
C4 C5 C7 126.48(14) . . ?
C6 C5 C7 115.26(13) . . ?
N2 C6 C5 122.65(13) . . ?
N2 C6 C10 115.50(12) . . ?
C5 C6 C10 121.75(13) . . ?
N5 C7 C5 130.32(13) . . ?
N5 C7 C8 105.64(12) . . ?
C8 C7 C5 123.73(13) . . ?
N4 C8 C7 109.95(12) . . ?
N4 C8 C9 128.51(13) . . ?
C7 C8 C9 121.36(13) . . ?
C10 C9 C8 115.95(13) . . ?
C11 C9 C8 126.00(13) . . ?
C11 C9 C10 117.96(13) . . ?
N3 C10 C6 115.11(12) . . ?
N3 C10 C9 122.91(13) . . ?
C9 C10 C6 121.87(13) . . ?
C9 C11 H11 120.7 . . ?
C12 C11 C9 118.59(14) . . ?
C12 C11 H11 120.7 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.29(14) . . ?
C13 C12 H12 119.9 . . ?
N3 C13 C12 122.57(14) . . ?
N3 C13 H13 118.7 . . ?
C12 C13 H13 118.7 . . ?
C15 C14 H14 119.4 . . ?
C15 C14 C19 121.28(17) . . ?
C19 C14 H14 119.4 . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C16 120.36(17) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 119.6 . . ?
C17 C16 C15 120.78(19) . . ?
C17 C16 H16 119.6 . . ?
C16 C17 H17 119.6 . . ?
C16 C17 C18 120.85(16) . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C19 118.19(15) . . ?
C23 C18 C17 123.00(14) . . ?
C23 C18 C19 118.77(15) . . ?
C14 C19 C18 118.52(17) . . ?
C20 C19 C14 122.13(16) . . ?
C20 C19 C18 119.33(15) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 C19 122.15(15) . . ?
C21 C20 H20 118.9 . . ?
C20 C21 C22 119.19(16) . . ?
C20 C21 C24 122.30(16) . . ?
C24 C21 C22 118.48(16) . . ?
C23 C22 C21 119.27(15) . . ?
C23 C22 C27 122.65(14) . . ?
C27 C22 C21 118.07(15) . . ?
C18 C23 C28 118.71(14) . . ?
C22 C23 C18 121.22(14) . . ?
C22 C23 C28 120.01(14) . . ?
C21 C24 H24 119.3 . . ?
C25 C24 C21 121.33(17) . . ?
C25 C24 H24 119.3 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.40(17) . . ?
C26 C25 H25 119.8 . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.53(19) . . ?
C27 C26 H26 119.7 . . ?
C22 C27 H27 119.4 . . ?
C26 C27 C22 121.14(17) . . ?
C26 C27 H27 119.4 . . ?
N4 C28 N5 111.76(13) . . ?
N4 C28 C23 126.20(13) . . ?
N5 C28 C23 121.96(13) . . ?
C29 O1 H1 108.5 . . ?
O1 C29 H29A 106.9 . . ?
O1 C29 H29B 110.0 . . ?
O1 C29 H29C 111.0 . . ?
H29A C29 H29B 108.2 . . ?
H29A C29 H29C 109.9 . . ?
H29B C29 H29C 110.7 . . ?
H30A C30 H30A 116.5 . 2_655 ?
H30A C30 H30B 93.6 . 2_655 ?
H30A C30 H30B 109.5 2_655 2_655 ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 2_655 2_655 ?
H30A C30 H30C 116.9 . 2_655 ?
H30B C30 H30A 93.6 . 2_655 ?
H30B C30 H30B 135.8 . 2_655 ?
H30B C30 H30C 109.5 2_655 2_655 ?
H30B C30 H30C 26.4 . 2_655 ?
H30B C30 H30C 109.5 . . ?
H30C C30 H30A 116.9 . 2_655 ?
H30C C30 H30B 26.4 . 2_655 ?
H30C C30 H30C 83.3 . 2_655 ?
O2 C30 H30A 15.9(15) . 2_655 ?
O2 C30 H30A 109.5 . . ?
O2 C30 H30B 97(2) . 2_655 ?
O2 C30 H30B 109.5 . . ?
O2 C30 H30C 124.0(8) . 2_655 ?
O2 C30 H30C 109.5 . . ?
C30 O2 H30A 28.5(11) . 2_655 ?
C30 O2 H2A 109.2 . . ?
H2A O2 H30A 89.2 . 2_655 ?

_olex2_exptl_crystal_mounting_method 'coordinate bond'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.621
####################################################################### 
# 
# 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_NewMeOH@293K
_database_code_depnum_ccdc_archive 'CCDC 1965903'
loop_
_audit_author_name
_audit_author_address
'Jun Tao'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2019-11-15 deposited with the CCDC.	2019-12-30 downloaded from the CCDC.
;
_audit_creation_date             2019-11-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        C59H44FeN10O3S2
_chemical_formula_moiety         'C56 H32 Fe N10 S2, 3(C H4 O)'
_chemical_formula_sum            'C59 H44 Fe N10 O3 S2'
_chemical_formula_weight         1061.01
_chemical_melting_point          ?
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   12.1381(13)
_cell_length_b                   24.950(3)
_cell_length_c                   16.8691(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5108.7(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4099
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.9990
_cell_measurement_theta_min      3.8240
_shelx_estimated_absorpt_T_max   0.918
_shelx_estimated_absorpt_T_min   0.881
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_preparation       '1 absorbed methnol molecules.'
_exptl_crystal_recrystallization_method 'Reddish black crystals'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1737
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32666
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.149
_diffrn_reflns_theta_max         25.149
_diffrn_reflns_theta_min         3.660
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00 -18.00   0.50  160.00    --    0.10  -6.00 117.00   52
  2  ω     10.00  35.00   0.50  160.00    --    0.10   6.00 -66.00   50
  3  ω    -46.00 -19.00   0.50  160.00    --    0.10 -82.00-180.00   54
  4  ω    -65.00   7.00   0.50  160.00    --    0.10 -38.00 -30.00  144
  5  ω    -62.00  19.00   0.50  160.00    --    0.10 -82.00 -60.00  162
  6  ω      4.00  29.00   0.50  160.00    --    0.10  57.00   0.00   50
  7  ω    -41.00 -16.00   0.50  160.00    --    0.10 -82.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0426747000
_diffrn_orient_matrix_UB_12      -0.0023789000
_diffrn_orient_matrix_UB_13      0.0285071000
_diffrn_orient_matrix_UB_21      -0.0398548000
_diffrn_orient_matrix_UB_22      -0.0015048000
_diffrn_orient_matrix_UB_23      0.0306379000
_diffrn_orient_matrix_UB_31      -0.0014646000
_diffrn_orient_matrix_UB_32      -0.0283050000
_diffrn_orient_matrix_UB_33      -0.0040450000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2609
_reflns_number_total             4494
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4494
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2312
_refine_ls_R_factor_gt           0.1429
_refine_ls_restrained_S_all      1.224
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+61.8028P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2453
_refine_ls_wR_factor_ref         0.3116
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) O2(0.5) H2A(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N5(H5), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27)
3.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.750000 0.750000 0.52530(16) 0.0602(7) Uani 1 2 d S T P . .
S1 S 0.5215(4) 0.67898(19) 0.3211(3) 0.1149(16) Uani 1 1 d . . . . .
O1 O 1.1232(6) 0.4790(3) 0.6363(5) 0.065(2) Uani 1 1 d . . . . .
H1 H 1.083403 0.496995 0.665186 0.098 Uiso 1 1 calc GR . . . .
N1 N 0.6607(10) 0.7089(4) 0.4420(7) 0.074(3) Uani 1 1 d . . . . .
N2 N 0.6895(6) 0.7020(3) 0.6225(5) 0.0409(19) Uani 1 1 d . . . . .
N3 N 0.8764(7) 0.6914(3) 0.5403(5) 0.049(2) Uani 1 1 d . . . . .
N4 N 0.9659(7) 0.5366(3) 0.7104(5) 0.053(2) Uani 1 1 d . . . . .
N5 N 0.8093(7) 0.5447(3) 0.7778(5) 0.048(2) Uani 1 1 d . . . . .
H5 H 0.758637 0.538140 0.812113 0.057 Uiso 1 1 calc R . . . .
C1 C 0.6025(11) 0.6966(5) 0.3923(9) 0.068(4) Uani 1 1 d . . . . .
C2 C 0.6008(8) 0.7097(4) 0.6648(7) 0.055(3) Uani 1 1 d . . . . .
H2 H 0.554634 0.737763 0.650292 0.065 Uiso 1 1 calc R . . . .
C3 C 0.5695(9) 0.6783(4) 0.7312(6) 0.054(3) Uani 1 1 d . . . . .
H3 H 0.507277 0.686338 0.761072 0.065 Uiso 1 1 calc R . . . .
C4 C 0.6362(8) 0.6352(4) 0.7491(6) 0.053(3) Uani 1 1 d . . . . .
H4 H 0.617427 0.612540 0.790713 0.064 Uiso 1 1 calc R . . . .
C5 C 0.7323(7) 0.6252(3) 0.7051(5) 0.038(2) Uani 1 1 d . . . . .
C6 C 0.7553(8) 0.6596(3) 0.6420(5) 0.035(2) Uani 1 1 d . . . . .
C7 C 0.8071(8) 0.5835(4) 0.7201(6) 0.041(2) Uani 1 1 d . . . . .
C8 C 0.9041(8) 0.5780(4) 0.6794(6) 0.043(2) Uani 1 1 d . . . . .
C9 C 0.9336(7) 0.6141(4) 0.6162(6) 0.041(2) Uani 1 1 d . . . . .
C10 C 0.8561(8) 0.6545(4) 0.5972(6) 0.040(2) Uani 1 1 d . . . . .
C11 C 1.0331(10) 0.6133(4) 0.5746(7) 0.061(3) Uani 1 1 d . . . . .
H11 H 1.085845 0.587227 0.585338 0.073 Uiso 1 1 calc R . . . .
C12 C 1.0517(10) 0.6515(5) 0.5176(7) 0.066(3) Uani 1 1 d . . . . .
H12 H 1.118117 0.652077 0.490105 0.079 Uiso 1 1 calc R . . . .
C13 C 0.9709(11) 0.6891(4) 0.5015(6) 0.063(3) Uani 1 1 d . . . . .
H13 H 0.983757 0.713945 0.461433 0.076 Uiso 1 1 calc R . . . .
C14 C 0.8444(13) 0.3404(5) 0.8927(10) 0.089(5) Uani 1 1 d . . . . .
H14 H 0.860814 0.314844 0.931100 0.107 Uiso 1 1 calc R . . . .
C15 C 0.7617(15) 0.3311(5) 0.8410(12) 0.107(6) Uani 1 1 d . . . . .
H15 H 0.721078 0.299631 0.844655 0.129 Uiso 1 1 calc R . . . .
C16 C 0.7365(12) 0.3686(5) 0.7820(10) 0.092(5) Uani 1 1 d . . . . .
H16 H 0.681113 0.361158 0.745490 0.111 Uiso 1 1 calc R . . . .
C17 C 0.7924(9) 0.4159(4) 0.7775(8) 0.067(3) Uani 1 1 d . . . . .
H17 H 0.772952 0.440650 0.738779 0.081 Uiso 1 1 calc R . . . .
C18 C 0.8788(8) 0.4281(4) 0.8302(7) 0.049(3) Uani 1 1 d . . . . .
C19 C 0.9074(10) 0.3889(4) 0.8892(8) 0.062(3) Uani 1 1 d . . . . .
C20 C 0.9956(11) 0.3983(5) 0.9382(7) 0.070(4) Uani 1 1 d . . . . .
H20 H 1.014105 0.372683 0.975934 0.084 Uiso 1 1 calc R . . . .
C21 C 1.0581(10) 0.4450(5) 0.9333(7) 0.061(3) Uani 1 1 d . . . . .
C22 C 1.0308(8) 0.4853(4) 0.8768(6) 0.048(3) Uani 1 1 d . . . . .
C23 C 0.9395(8) 0.4759(4) 0.8260(6) 0.045(2) Uani 1 1 d . . . . .
C24 C 1.1497(12) 0.4544(7) 0.9843(8) 0.083(4) Uani 1 1 d . . . . .
H24 H 1.169991 0.428231 1.020778 0.100 Uiso 1 1 calc R . . . .
C25 C 1.2078(12) 0.5007(8) 0.9806(8) 0.093(5) Uani 1 1 d . . . . .
H25 H 1.266943 0.506314 1.014689 0.111 Uiso 1 1 calc R . . . .
C26 C 1.1782(10) 0.5403(6) 0.9249(7) 0.076(4) Uani 1 1 d . . . . .
H26 H 1.218492 0.571922 0.921981 0.091 Uiso 1 1 calc R . . . .
C27 C 1.0916(9) 0.5327(5) 0.8756(7) 0.064(3) Uani 1 1 d . . . . .
H27 H 1.072210 0.559689 0.840158 0.077 Uiso 1 1 calc R . . . .
C28 C 0.9072(9) 0.5184(4) 0.7701(7) 0.051(3) Uani 1 1 d . . . . .
C29 C 1.0590(13) 0.4505(6) 0.5836(8) 0.093(5) Uani 1 1 d . . . . .
H29A H 1.044149 0.472140 0.537840 0.140 Uiso 1 1 calc GR . . . .
H29B H 0.990831 0.440775 0.608638 0.140 Uiso 1 1 calc GR . . . .
H29C H 1.097438 0.418587 0.567710 0.140 Uiso 1 1 calc GR . . . .
C30 C 1.250000 0.750000 0.373(4) 0.48(9) Uani 1 2 d S T P . .
H30A H 1.228708 0.733982 0.323765 0.721 Uiso 0.5 1 calc GR . . A -1
H30B H 1.299663 0.779184 0.363263 0.721 Uiso 0.5 1 calc GR . . A -1
H30C H 1.185725 0.763153 0.400043 0.721 Uiso 0.5 1 calc GR . . A -1
O2 O 1.298(4) 0.715(3) 0.417(3) 0.36(4) Uani 0.5 1 d . . . B -1
H2A H 1.269775 0.714186 0.460981 0.535 Uiso 0.5 1 calc GR . . B -1


_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 2.049(12) . ?
Fe1 N1 2.049(12) 2_665 ?
Fe1 N2 2.158(8) 2_665 ?
Fe1 N2 2.158(8) . ?
Fe1 N3 2.135(8) 2_665 ?
Fe1 N3 2.135(8) . ?
S1 C1 1.612(16) . ?
O1 H1 0.8200 . ?
O1 C29 1.379(14) . ?
N1 C1 1.139(16) . ?
N2 C2 1.307(13) . ?
N2 C6 1.367(11) . ?
N3 C10 1.351(11) . ?
N3 C13 1.323(13) . ?
N4 C8 1.379(12) . ?
N4 C28 1.315(13) . ?
N5 H5 0.8600 . ?
N5 C7 1.375(12) . ?
N5 C28 1.363(12) . ?
C2 H2 0.9300 . ?
C2 C3 1.418(14) . ?
C3 H3 0.9300 . ?
C3 C4 1.379(13) . ?
C4 H4 0.9300 . ?
C4 C5 1.405(13) . ?
C5 C6 1.394(12) . ?
C5 C7 1.404(12) . ?
C6 C10 1.444(13) . ?
C7 C8 1.368(13) . ?
C8 C9 1.441(13) . ?
C9 C10 1.416(12) . ?
C9 C11 1.397(14) . ?
C11 H11 0.9300 . ?
C11 C12 1.372(14) . ?
C12 H12 0.9300 . ?
C12 C13 1.385(15) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.35(2) . ?
C14 C19 1.434(17) . ?
C15 H15 0.9300 . ?
C15 C16 1.40(2) . ?
C16 H16 0.9300 . ?
C16 C17 1.363(15) . ?
C17 H17 0.9300 . ?
C17 C18 1.408(15) . ?
C18 C19 1.437(15) . ?
C18 C23 1.404(13) . ?
C19 C20 1.373(17) . ?
C20 H20 0.9300 . ?
C20 C21 1.392(17) . ?
C21 C22 1.425(14) . ?
C21 C24 1.426(17) . ?
C22 C23 1.420(14) . ?
C22 C27 1.395(15) . ?
C23 C28 1.473(14) . ?
C24 H24 0.9300 . ?
C24 C25 1.355(19) . ?
C25 H25 0.9300 . ?
C25 C26 1.411(19) . ?
C26 H26 0.9300 . ?
C26 C27 1.354(15) . ?
C27 H27 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30 O2 1.29(6) . ?
O2 H2A 0.8200 . ?

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 N1 93.4(6) . 2_665 ?
N1 Fe1 N2 168.0(4) . 2_665 ?
N1 Fe1 N2 93.6(3) 2_665 2_665 ?
N1 Fe1 N2 93.6(3) . . ?
N1 Fe1 N2 168.0(4) 2_665 . ?
N1 Fe1 N3 92.5(4) . 2_665 ?
N1 Fe1 N3 96.8(4) . . ?
N1 Fe1 N3 96.8(4) 2_665 2_665 ?
N1 Fe1 N3 92.5(4) 2_665 . ?
N2 Fe1 N2 81.2(4) . 2_665 ?
N3 Fe1 N2 77.0(3) 2_665 2_665 ?
N3 Fe1 N2 92.6(3) 2_665 . ?
N3 Fe1 N2 77.0(3) . . ?
N3 Fe1 N2 92.6(3) . 2_665 ?
N3 Fe1 N3 166.3(5) 2_665 . ?
C29 O1 H1 109.5 . . ?
C1 N1 Fe1 165.5(11) . . ?
C2 N2 Fe1 127.9(7) . . ?
C2 N2 C6 117.5(8) . . ?
C6 N2 Fe1 114.5(6) . . ?
C10 N3 Fe1 114.8(7) . . ?
C13 N3 Fe1 126.5(7) . . ?
C13 N3 C10 118.7(9) . . ?
C28 N4 C8 104.7(8) . . ?
C7 N5 H5 126.6 . . ?
C28 N5 H5 126.6 . . ?
C28 N5 C7 106.7(9) . . ?
N1 C1 S1 179.2(13) . . ?
N2 C2 H2 117.6 . . ?
N2 C2 C3 124.9(9) . . ?
C3 C2 H2 117.6 . . ?
C2 C3 H3 121.8 . . ?
C4 C3 C2 116.5(10) . . ?
C4 C3 H3 121.8 . . ?
C3 C4 H4 119.7 . . ?
C3 C4 C5 120.7(9) . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 117.4(9) . . ?
C6 C5 C7 117.6(9) . . ?
C7 C5 C4 125.0(9) . . ?
N2 C6 C5 122.9(9) . . ?
N2 C6 C10 115.8(8) . . ?
C5 C6 C10 121.1(8) . . ?
N5 C7 C5 131.5(9) . . ?
C8 C7 N5 105.5(8) . . ?
C8 C7 C5 122.7(9) . . ?
N4 C8 C9 127.8(9) . . ?
C7 C8 N4 110.7(9) . . ?
C7 C8 C9 121.4(9) . . ?
C10 C9 C8 116.6(8) . . ?
C11 C9 C8 125.3(9) . . ?
C11 C9 C10 118.0(9) . . ?
N3 C10 C6 117.8(8) . . ?
N3 C10 C9 121.7(9) . . ?
C9 C10 C6 120.4(8) . . ?
C9 C11 H11 120.5 . . ?
C12 C11 C9 119.0(10) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 H12 120.3 . . ?
C11 C12 C13 119.5(11) . . ?
C13 C12 H12 120.3 . . ?
N3 C13 C12 123.1(10) . . ?
N3 C13 H13 118.4 . . ?
C12 C13 H13 118.4 . . ?
C15 C14 H14 119.5 . . ?
C15 C14 C19 120.9(14) . . ?
C19 C14 H14 119.5 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.6(14) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.7 . . ?
C17 C16 C15 120.6(15) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 H17 119.2 . . ?
C16 C17 C18 121.6(13) . . ?
C18 C17 H17 119.2 . . ?
C17 C18 C19 118.0(10) . . ?
C23 C18 C17 122.9(10) . . ?
C23 C18 C19 119.0(10) . . ?
C14 C19 C18 118.3(13) . . ?
C20 C19 C14 122.3(13) . . ?
C20 C19 C18 119.3(11) . . ?
C19 C20 H20 118.9 . . ?
C19 C20 C21 122.1(11) . . ?
C21 C20 H20 118.9 . . ?
C20 C21 C22 120.3(11) . . ?
C20 C21 C24 121.8(12) . . ?
C22 C21 C24 117.9(12) . . ?
C23 C22 C21 117.9(10) . . ?
C27 C22 C21 119.1(11) . . ?
C27 C22 C23 122.9(10) . . ?
C18 C23 C22 121.3(9) . . ?
C18 C23 C28 120.3(10) . . ?
C22 C23 C28 118.4(9) . . ?
C21 C24 H24 119.4 . . ?
C25 C24 C21 121.3(13) . . ?
C25 C24 H24 119.4 . . ?
C24 C25 H25 120.2 . . ?
C24 C25 C26 119.7(14) . . ?
C26 C25 H25 120.2 . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.7(14) . . ?
C27 C26 H26 119.7 . . ?
C22 C27 H27 119.3 . . ?
C26 C27 C22 121.3(12) . . ?
C26 C27 H27 119.3 . . ?
N4 C28 N5 112.3(9) . . ?
N4 C28 C23 126.5(9) . . ?
N5 C28 C23 121.1(10) . . ?
O1 C29 H29A 109.5 . . ?
O1 C29 H29B 109.5 . . ?
O1 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O2 C30 H30A 109.5 . . ?
O2 C30 H30B 109.5 . . ?
O2 C30 H30C 109.5 . . ?
C30 O2 H2A 109.5 . . ?

_olex2_exptl_crystal_mounting_method 'coordinate bond'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.573
_oxdiff_exptl_absorpt_empirical_full_min 0.641
####################################################################### 
# 
# 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_NewMeOH@150K
_database_code_depnum_ccdc_archive 'CCDC 1965900'
loop_
_audit_author_name
_audit_author_address
'Jun Tao'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2019-11-15 deposited with the CCDC.	2019-12-30 downloaded from the CCDC.
;
_audit_creation_date             2019-11-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        C59H42FeN10O3S2
_chemical_formula_moiety         'C56 H32 Fe N10 S2, 3(C H4 O)'
_chemical_formula_sum            'C59 H44 Fe N10 O3 S2'
_chemical_formula_weight         1061.01
_chemical_melting_point          ?
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   11.9693(13)
_cell_length_b                   24.7798(13)
_cell_length_c                   16.7667(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4973.0(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6842
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      29.3340
_cell_measurement_theta_min      3.8820
_shelx_estimated_absorpt_T_max   0.916
_shelx_estimated_absorpt_T_min   0.877
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_preparation       '1 absorbed methnol molecules.'
_exptl_crystal_recrystallization_method 'Reddish black crystals'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34594
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.707
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      3.00  32.00   0.50  110.00    --    0.10  32.00-121.00   58
  2  ω    -46.00 -18.00   0.50  110.00    --    0.10 -32.00  79.00   56
  3  ω      8.00  35.00   0.50  110.00    --    0.10  38.00 120.00   54
  4  ω     49.00  90.00   0.50  110.00    --    0.10  38.00 120.00   82
  5  ω    -75.00  28.00   0.50  110.00    --    0.10 -77.00-120.00  206
  6  ω      1.00  28.00   0.50  110.00    --    0.10 -82.00  30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0229220000
_diffrn_orient_matrix_UB_12      -0.0262769000
_diffrn_orient_matrix_UB_13      0.0037267000
_diffrn_orient_matrix_UB_21      -0.0088865000
_diffrn_orient_matrix_UB_22      -0.0044875000
_diffrn_orient_matrix_UB_23      -0.0412985000
_diffrn_orient_matrix_UB_31      0.0539010000
_diffrn_orient_matrix_UB_32      0.0104752000
_diffrn_orient_matrix_UB_33      -0.0084014000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3507
_reflns_number_total             5011
_reflns_odcompleteness_completeness 99.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5011
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.1401
_refine_ls_restrained_S_all      1.214
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+102.5649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2793
_refine_ls_wR_factor_ref         0.3159
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) O2(0.5) H2A(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N5(H5), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27)
3.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.250000 0.250000 0.53682(11) 0.0258(4) Uani 1 2 d S T P . .
S1 S 0.4625(2) 0.17456(11) 0.32818(17) 0.0442(7) Uani 1 1 d . . . . .
N1 N 0.3268(7) 0.2093(3) 0.4535(5) 0.0308(17) Uani 1 1 d . . . . .
N2 N 0.3693(7) 0.3041(3) 0.5425(4) 0.0267(16) Uani 1 1 d . . . . .
N3 N 0.1851(6) 0.2941(3) 0.6218(4) 0.0227(15) Uani 1 1 d . . . . .
N4 N 0.4618(6) 0.4634(3) 0.7081(4) 0.0264(16) Uani 1 1 d . . . . .
N5 N 0.3031(6) 0.4555(3) 0.7759(4) 0.0263(16) Uani 1 1 d . . . . .
H5 H 0.251541 0.461902 0.810417 0.032 Uiso 1 1 calc R . . . .
C1 C 0.3814(7) 0.1944(4) 0.4015(5) 0.0283(19) Uani 1 1 d . . . . .
C2 C 0.4648(9) 0.3059(4) 0.5016(5) 0.033(2) Uani 1 1 d . . . . .
H2 H 0.475815 0.280886 0.460930 0.040 Uiso 1 1 calc R . . . .
C3 C 0.5503(8) 0.3442(4) 0.5172(6) 0.035(2) Uani 1 1 d . . . . .
H3 H 0.618290 0.342314 0.490423 0.042 Uiso 1 1 calc R . . . .
C4 C 0.5310(8) 0.3842(4) 0.5728(5) 0.029(2) Uani 1 1 d . . . . .
H4 H 0.584708 0.410547 0.582451 0.035 Uiso 1 1 calc R . . . .
C5 C 0.4302(7) 0.3848(3) 0.6142(5) 0.0233(18) Uani 1 1 d . . . . .
C6 C 0.3512(8) 0.3431(3) 0.5978(5) 0.0227(18) Uani 1 1 d . . . . .
C7 C 0.2515(7) 0.3381(3) 0.6419(4) 0.0194(16) Uani 1 1 d . . . . .
C8 C 0.2235(7) 0.3737(3) 0.7034(5) 0.0219(18) Uani 1 1 d . . . . .
C9 C 0.3009(7) 0.4161(3) 0.7179(5) 0.0218(17) Uani 1 1 d . . . . .
C10 C 0.3994(7) 0.4216(3) 0.6770(5) 0.0226(17) Uani 1 1 d . . . . .
C11 C 0.1257(7) 0.3634(4) 0.7487(5) 0.0289(19) Uani 1 1 d . . . . .
H11 H 0.105103 0.386766 0.789532 0.035 Uiso 1 1 calc R . . . .
C12 C 0.0610(7) 0.3184(3) 0.7319(5) 0.0262(19) Uani 1 1 d . . . . .
H12 H -0.001850 0.309797 0.761948 0.031 Uiso 1 1 calc R . . . .
C13 C 0.0960(8) 0.2857(4) 0.6657(5) 0.030(2) Uani 1 1 d . . . . .
H13 H 0.051843 0.256041 0.652930 0.036 Uiso 1 1 calc R . . . .
C14 C 0.4018(7) 0.4824(4) 0.7687(5) 0.0256(18) Uani 1 1 d . . . . .
C15 C 0.4351(7) 0.5258(3) 0.8240(5) 0.0238(17) Uani 1 1 d . . . . .
C16 C 0.3722(8) 0.5737(3) 0.8287(6) 0.030(2) Uani 1 1 d . . . . .
C17 C 0.2846(8) 0.5860(4) 0.7746(6) 0.038(2) Uani 1 1 d . . . . .
H17 H 0.265681 0.561057 0.735343 0.045 Uiso 1 1 calc R . . . .
C18 C 0.2281(10) 0.6332(4) 0.7788(8) 0.050(3) Uani 1 1 d . . . . .
H18 H 0.172074 0.640491 0.741876 0.060 Uiso 1 1 calc R . . . .
C19 C 0.2530(9) 0.6715(4) 0.8384(7) 0.046(3) Uani 1 1 d . . . . .
H19 H 0.212534 0.703455 0.841169 0.055 Uiso 1 1 calc R . . . .
C20 C 0.3358(9) 0.6617(4) 0.8916(7) 0.043(3) Uani 1 1 d . . . . .
H20 H 0.351221 0.686966 0.931157 0.051 Uiso 1 1 calc R . . . .
C21 C 0.3998(7) 0.6130(3) 0.8875(6) 0.0277(19) Uani 1 1 d . . . . .
C22 C 0.4884(9) 0.6037(4) 0.9392(5) 0.036(2) Uani 1 1 d . . . . .
H22 H 0.504768 0.629320 0.978037 0.043 Uiso 1 1 calc R . . . .
C23 C 0.5544(8) 0.5566(4) 0.9343(5) 0.031(2) Uani 1 1 d . . . . .
C24 C 0.6473(8) 0.5470(5) 0.9861(5) 0.038(2) Uani 1 1 d . . . . .
H24 H 0.668187 0.573326 1.022782 0.046 Uiso 1 1 calc R . . . .
C25 C 0.7052(8) 0.5002(5) 0.9823(6) 0.042(3) Uani 1 1 d . . . . .
H25 H 0.764311 0.494288 1.017294 0.051 Uiso 1 1 calc R . . . .
C26 C 0.6768(9) 0.4601(5) 0.9258(6) 0.040(2) Uani 1 1 d . . . . .
H26 H 0.717898 0.428306 0.923297 0.048 Uiso 1 1 calc R . . . .
C27 C 0.5892(7) 0.4678(4) 0.8747(5) 0.030(2) Uani 1 1 d . . . . .
H27 H 0.570535 0.440679 0.838825 0.036 Uiso 1 1 calc R . . . .
C28 C 0.5261(7) 0.5164(3) 0.8752(5) 0.0235(17) Uani 1 1 d . . . . .
O1 O 0.6203(6) 0.5201(3) 0.6335(4) 0.0346(15) Uani 1 1 d . . . . .
H1 H 0.579843 0.508998 0.669344 0.052 Uiso 1 1 calc GR . . . .
C29 C 0.5584(10) 0.5525(4) 0.5820(6) 0.044(3) Uani 1 1 d . . . . .
H29A H 0.547682 0.534021 0.532314 0.066 Uiso 1 1 calc GR . . . .
H29B H 0.597708 0.585703 0.572720 0.066 Uiso 1 1 calc GR . . . .
H29C H 0.487021 0.560217 0.605580 0.066 Uiso 1 1 calc GR . . . .
C30 C 0.750000 0.250000 0.3743(12) 0.078(6) Uani 1 2 d S T P . .
H30A H 0.783726 0.249391 0.322315 0.117 Uiso 0.5 1 calc GR . . A -1
H30B H 0.674879 0.263279 0.370097 0.117 Uiso 0.5 1 calc GR . . A -1
H30C H 0.749020 0.214133 0.395888 0.117 Uiso 0.5 1 calc GR . . A -1
O2 O 0.8124(17) 0.2842(12) 0.4250(12) 0.104(9) Uani 0.5 1 d . . . B -1
H2A H 0.863359 0.298113 0.399651 0.156 Uiso 0.5 1 calc GR . . B -1


_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 1.954(8) . ?
Fe1 N1 1.954(8) 2 ?
Fe1 N2 1.962(7) 2 ?
Fe1 N2 1.962(7) . ?
Fe1 N3 1.956(7) . ?
Fe1 N3 1.956(7) 2 ?
S1 C1 1.642(9) . ?
N1 C1 1.150(11) . ?
N2 C2 1.334(12) . ?
N2 C6 1.355(10) . ?
N3 C7 1.390(10) . ?
N3 C13 1.313(11) . ?
N4 C10 1.378(10) . ?
N4 C14 1.330(11) . ?
N5 C9 1.379(10) . ?
N5 C14 1.362(11) . ?
C2 C3 1.421(13) . ?
C3 C4 1.381(12) . ?
C4 C5 1.391(12) . ?
C5 C6 1.428(12) . ?
C5 C10 1.442(11) . ?
C6 C7 1.409(12) . ?
C7 C8 1.399(11) . ?
C8 C9 1.421(11) . ?
C8 C11 1.418(12) . ?
C9 C10 1.371(12) . ?
C11 C12 1.388(12) . ?
C12 C13 1.436(12) . ?
C14 C15 1.477(11) . ?
C15 C16 1.407(12) . ?
C15 C28 1.406(12) . ?
C16 C17 1.420(13) . ?
C16 C21 1.424(12) . ?
C17 C18 1.354(14) . ?
C18 C19 1.409(15) . ?
C19 C20 1.355(16) . ?
C20 C21 1.433(13) . ?
C21 C22 1.388(13) . ?
C22 C23 1.412(14) . ?
C23 C24 1.431(13) . ?
C23 C28 1.446(12) . ?
C24 C25 1.353(16) . ?
C25 C26 1.415(14) . ?
C26 C27 1.366(13) . ?
C27 C28 1.420(12) . ?
O1 C29 1.393(12) . ?
C30 O2 1.41(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
N1 Fe1 N1 88.6(4) . 2 ?
N1 Fe1 N2 91.4(3) . 2 ?
N1 Fe1 N2 92.6(3) 2 2 ?
N1 Fe1 N2 92.6(3) . . ?
N1 Fe1 N2 91.4(3) 2 . ?
N1 Fe1 N3 175.1(3) . . ?
N1 Fe1 N3 92.6(3) . 2 ?
N1 Fe1 N3 175.1(3) 2 2 ?
N1 Fe1 N3 92.6(3) 2 . ?
N2 Fe1 N2 174.4(4) . 2 ?
N3 Fe1 N2 82.6(3) 2 2 ?
N3 Fe1 N2 93.3(3) 2 . ?
N3 Fe1 N2 93.3(3) . 2 ?
N3 Fe1 N2 82.6(3) . . ?
N3 Fe1 N3 86.5(4) . 2 ?
C1 N1 Fe1 167.2(8) . . ?
C2 N2 Fe1 128.4(6) . . ?
C2 N2 C6 117.8(8) . . ?
C6 N2 Fe1 113.8(6) . . ?
C7 N3 Fe1 112.8(6) . . ?
C13 N3 Fe1 130.0(6) . . ?
C13 N3 C7 116.9(7) . . ?
C14 N4 C10 105.2(7) . . ?
C14 N5 C9 107.4(7) . . ?
N1 C1 S1 178.1(9) . . ?
N2 C2 C3 123.0(8) . . ?
C4 C3 C2 118.9(9) . . ?
C3 C4 C5 119.3(8) . . ?
C4 C5 C6 118.1(8) . . ?
C4 C5 C10 126.4(8) . . ?
C6 C5 C10 115.4(8) . . ?
N2 C6 C5 122.8(8) . . ?
N2 C6 C7 115.5(7) . . ?
C7 C6 C5 121.6(7) . . ?
N3 C7 C6 115.2(7) . . ?
N3 C7 C8 122.5(8) . . ?
C8 C7 C6 122.3(7) . . ?
C7 C8 C9 115.9(8) . . ?
C7 C8 C11 118.6(8) . . ?
C11 C8 C9 125.4(8) . . ?
N5 C9 C8 131.0(8) . . ?
C10 C9 N5 105.4(7) . . ?
C10 C9 C8 123.3(7) . . ?
N4 C10 C5 127.8(8) . . ?
C9 C10 N4 110.6(7) . . ?
C9 C10 C5 121.5(7) . . ?
C12 C11 C8 119.8(8) . . ?
C11 C12 C13 116.6(8) . . ?
N3 C13 C12 125.5(8) . . ?
N4 C14 N5 111.3(8) . . ?
N4 C14 C15 126.3(8) . . ?
N5 C14 C15 122.3(8) . . ?
C16 C15 C14 120.3(8) . . ?
C28 C15 C14 118.1(7) . . ?
C28 C15 C16 121.4(8) . . ?
C15 C16 C17 122.7(8) . . ?
C15 C16 C21 119.4(8) . . ?
C17 C16 C21 117.9(8) . . ?
C18 C17 C16 121.4(10) . . ?
C17 C18 C19 120.9(11) . . ?
C20 C19 C18 120.1(10) . . ?
C19 C20 C21 120.6(9) . . ?
C16 C21 C20 119.0(9) . . ?
C22 C21 C16 119.8(8) . . ?
C22 C21 C20 121.2(9) . . ?
C21 C22 C23 121.8(8) . . ?
C22 C23 C24 122.4(9) . . ?
C22 C23 C28 118.6(8) . . ?
C24 C23 C28 118.9(9) . . ?
C25 C24 C23 120.8(9) . . ?
C24 C25 C26 120.7(9) . . ?
C27 C26 C25 120.4(10) . . ?
C26 C27 C28 121.6(9) . . ?
C15 C28 C23 119.0(8) . . ?
C15 C28 C27 123.4(8) . . ?
C27 C28 C23 117.6(8) . . ?

_olex2_exptl_crystal_mounting_method 'coordinate bond'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.673
####################################################################### 
# 
# 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_H2O@293K
_database_code_depnum_ccdc_archive 'CCDC 1965904'
loop_
_audit_author_name
_audit_author_address
'Jun Tao'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2019-11-15 deposited with the CCDC.	2019-12-30 downloaded from the CCDC.
;
_audit_creation_date             2019-11-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        1.2H2O
_chemical_formula_moiety         'C56 H32 Fe N10 S2, 2(H2 O)'
_chemical_formula_sum            'C56 H36 Fe N10 O2 S2'
_chemical_formula_weight         1000.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O Fe1 S1'
_chemical_oxdiff_usercomment     'Co1 S1 O4 N6 C6 H12'
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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   12.5057(19)
_cell_length_b                   24.082(4)
_cell_length_c                   16.140(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4860.6(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1885
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8670
_cell_measurement_theta_min      3.6290
_shelx_estimated_absorpt_T_max   0.915
_shelx_estimated_absorpt_T_min   0.877
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_preparation       'Absord water after  solvent removal'
_exptl_crystal_recrystallization_method 'reddish black crystal'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1996
_diffrn_reflns_av_unetI/netI     0.1610
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24394
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.595
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  36.00   0.50  190.00    --    0.00  54.00 177.00   58
  2  ω    -65.00 -21.00   0.50  190.00    --    0.00 -81.00 -87.00   88
  3  ω     -3.00  30.00   0.50  190.00    --    0.00 -82.00-150.00   66
  4  ω    -46.00 -21.00   0.50  190.00    --    0.00 -82.00   0.00   50
  5  ω    -41.00  28.00   0.50  190.00    --    0.00 -82.00-180.00  138
  6  ω     -4.00  11.50   0.50  190.00    --    0.00  38.00-120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0442349000
_diffrn_orient_matrix_UB_12      -0.0176108000
_diffrn_orient_matrix_UB_13      -0.0080934000
_diffrn_orient_matrix_UB_21      -0.0218235000
_diffrn_orient_matrix_UB_22      -0.0203474000
_diffrn_orient_matrix_UB_23      0.0269431000
_diffrn_orient_matrix_UB_31      -0.0279872000
_diffrn_orient_matrix_UB_32      -0.0119423000
_diffrn_orient_matrix_UB_33      -0.0337939000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2122
_reflns_number_total             4854
_reflns_odcompleteness_completeness 95.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4854
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2636
_refine_ls_R_factor_gt           0.1377
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0217P)²+21.3333P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2281
_refine_ls_wR_factor_ref         0.2870
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.250000 0.750000 0.49875(13) 0.0669(6) Uani 1 2 d S T P . .
S1 S 0.4981(4) 0.81929(17) 0.6954(3) 0.1402(16) Uani 1 1 d . . . . .
N1 N 0.3416(8) 0.7915(4) 0.5833(6) 0.089(3) Uani 1 1 d . . . . .
N2 N 0.1893(5) 0.7011(3) 0.3966(4) 0.0535(18) Uani 1 1 d . . . . .
N3 N 0.3659(5) 0.6849(3) 0.4840(4) 0.0611(19) Uani 1 1 d . . . . .
N4 N 0.4514(5) 0.5273(3) 0.2999(5) 0.0624(19) Uani 1 1 d . . . . .
N5 N 0.3068(5) 0.5428(3) 0.2234(4) 0.0578(18) Uani 1 1 d . . . . .
H5 H 0.260726 0.539167 0.184178 0.069 Uiso 1 1 calc R . . . .
C1 C 0.4054(10) 0.8036(4) 0.6307(7) 0.081(3) Uani 1 1 d . . . . .
C2 C 0.1029(7) 0.7108(4) 0.3507(6) 0.065(2) Uani 1 1 d . . . . .
H2 H 0.058876 0.740176 0.365929 0.078 Uiso 1 1 calc R . . . .
C3 C 0.0740(7) 0.6798(4) 0.2812(5) 0.065(2) Uani 1 1 d . . . . .
H3 H 0.012395 0.688438 0.251613 0.078 Uiso 1 1 calc R . . . .
C4 C 0.1368(6) 0.6369(4) 0.2574(5) 0.056(2) Uani 1 1 d . . . . .
H4 H 0.118911 0.616152 0.210895 0.068 Uiso 1 1 calc R . . . .
C5 C 0.2291(6) 0.6237(3) 0.3029(5) 0.050(2) Uani 1 1 d . . . . .
C6 C 0.2534(6) 0.6577(3) 0.3723(4) 0.0453(17) Uani 1 1 d . . . . .
C7 C 0.3033(6) 0.5808(3) 0.2869(5) 0.050(2) Uani 1 1 d . . . . .
C8 C 0.3936(6) 0.5700(3) 0.3339(5) 0.049(2) Uani 1 1 d . . . . .
C9 C 0.4182(6) 0.6043(4) 0.4044(5) 0.055(2) Uani 1 1 d . . . . .
C10 C 0.3490(6) 0.6475(3) 0.4231(5) 0.0471(19) Uani 1 1 d . . . . .
C11 C 0.5085(7) 0.5982(4) 0.4548(6) 0.067(3) Uani 1 1 d . . . . .
H11 H 0.556953 0.569665 0.444772 0.080 Uiso 1 1 calc R . . . .
C12 C 0.5248(8) 0.6337(5) 0.5175(6) 0.080(3) Uani 1 1 d . . . . .
H12 H 0.584320 0.629528 0.551537 0.096 Uiso 1 1 calc R . . . .
C13 C 0.4523(8) 0.6771(5) 0.5320(6) 0.078(3) Uani 1 1 d . . . . .
H13 H 0.464419 0.701098 0.576096 0.094 Uiso 1 1 calc R . . . .
C14 C 0.6542(9) 0.4565(6) 0.0152(6) 0.086(4) Uani 1 1 d . . . . .
H14 H 0.675908 0.431979 -0.025997 0.104 Uiso 1 1 calc R . . . .
C15 C 0.7130(9) 0.5025(6) 0.0305(7) 0.094(4) Uani 1 1 d . . . . .
H15 H 0.774597 0.509751 0.000044 0.113 Uiso 1 1 calc R . . . .
C16 C 0.6798(9) 0.5387(5) 0.0925(6) 0.086(3) Uani 1 1 d . . . . .
H16 H 0.720838 0.570016 0.103373 0.103 Uiso 1 1 calc R . . . .
C17 C 0.5915(7) 0.5303(4) 0.1370(6) 0.071(3) Uani 1 1 d . . . . .
H17 H 0.571555 0.556377 0.176493 0.085 Uiso 1 1 calc R . . . .
C18 C 0.5273(6) 0.4823(4) 0.1253(5) 0.055(2) Uani 1 1 d . . . . .
C19 C 0.5598(7) 0.4451(4) 0.0610(5) 0.064(3) Uani 1 1 d . . . . .
C20 C 0.4952(9) 0.3986(5) 0.0439(6) 0.078(3) Uani 1 1 d . . . . .
H20 H 0.514359 0.374726 0.001124 0.094 Uiso 1 1 calc R . . . .
C21 C 0.4041(9) 0.3875(4) 0.0893(6) 0.073(3) Uani 1 1 d . . . . .
C22 C 0.3714(7) 0.4238(4) 0.1531(5) 0.061(2) Uani 1 1 d . . . . .
C23 C 0.4336(7) 0.4707(4) 0.1696(5) 0.056(2) Uani 1 1 d . . . . .
C24 C 0.3401(11) 0.3406(5) 0.0704(9) 0.106(4) Uani 1 1 d . . . . .
H24 H 0.361398 0.316664 0.028241 0.127 Uiso 1 1 calc R . . . .
C25 C 0.2500(13) 0.3301(5) 0.1118(10) 0.123(5) Uani 1 1 d . . . . .
H25 H 0.207087 0.300106 0.097008 0.147 Uiso 1 1 calc R . . . .
C26 C 0.2205(10) 0.3651(6) 0.1785(9) 0.118(5) Uani 1 1 d . . . . .
H26 H 0.159802 0.356449 0.209205 0.142 Uiso 1 1 calc R . . . .
C27 C 0.2780(8) 0.4110(5) 0.1989(7) 0.087(3) Uani 1 1 d . . . . .
H27 H 0.256387 0.433633 0.242493 0.105 Uiso 1 1 calc R . . . .
C28 C 0.3981(6) 0.5117(3) 0.2346(6) 0.057(2) Uani 1 1 d . . . . .
O1 O 0.6188(5) 0.4713(3) 0.3752(4) 0.082(2) Uani 1 1 d . . . . .
H1A H 0.564467 0.490080 0.360602 0.123 Uiso 1 1 d G . . . .
H1B H 0.596554 0.451183 0.414924 0.123 Uiso 1 1 d G . . . .


_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 2.042(10) 2_565 ?
Fe1 N1 2.042(10) . ?
Fe1 N2 2.163(7) . ?
Fe1 N2 2.163(7) 2_565 ?
Fe1 N3 2.149(7) . ?
Fe1 N3 2.149(7) 2_565 ?
S1 C1 1.607(14) . ?
N1 C1 1.143(13) . ?
N2 C2 1.332(10) . ?
N2 C6 1.373(9) . ?
N3 C10 1.350(10) . ?
N3 C13 1.343(11) . ?
N4 C8 1.372(10) . ?
N4 C28 1.303(10) . ?
N5 H5 0.8600 . ?
N5 C7 1.374(10) . ?
N5 C28 1.377(10) . ?
C2 H2 0.9300 . ?
C2 C3 1.395(12) . ?
C3 H3 0.9300 . ?
C3 C4 1.353(11) . ?
C4 H4 0.9300 . ?
C4 C5 1.404(10) . ?
C5 C6 1.420(10) . ?
C5 C7 1.414(11) . ?
C6 C10 1.470(10) . ?
C7 C8 1.384(10) . ?
C8 C9 1.439(11) . ?
C9 C10 1.387(11) . ?
C9 C11 1.399(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.341(12) . ?
C12 H12 0.9300 . ?
C12 C13 1.403(13) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.351(15) . ?
C14 C19 1.420(13) . ?
C15 H15 0.9300 . ?
C15 C16 1.391(15) . ?
C16 H16 0.9300 . ?
C16 C17 1.332(12) . ?
C17 H17 0.9300 . ?
C17 C18 1.420(12) . ?
C18 C19 1.430(12) . ?
C18 C23 1.401(11) . ?
C19 C20 1.409(14) . ?
C20 H20 0.9300 . ?
C20 C21 1.380(13) . ?
C21 C22 1.411(13) . ?
C21 C24 1.418(14) . ?
C22 C23 1.397(12) . ?
C22 C27 1.417(13) . ?
C23 C28 1.508(12) . ?
C24 H24 0.9300 . ?
C24 C25 1.335(17) . ?
C25 H25 0.9300 . ?
C25 C26 1.417(18) . ?
C26 H26 0.9300 . ?
C26 C27 1.359(15) . ?
C27 H27 0.9300 . ?
O1 H1A 0.8501 . ?
O1 H1B 0.8502 . ?

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 N1 96.2(5) 2_565 . ?
N1 Fe1 N2 92.6(3) 2_565 . ?
N1 Fe1 N2 166.4(3) . . ?
N1 Fe1 N2 166.4(3) 2_565 2_565 ?
N1 Fe1 N2 92.6(3) . 2_565 ?
N1 Fe1 N3 95.5(3) 2_565 . ?
N1 Fe1 N3 93.0(3) 2_565 2_565 ?
N1 Fe1 N3 93.0(3) . . ?
N1 Fe1 N3 95.5(3) . 2_565 ?
N2 Fe1 N2 80.7(3) 2_565 . ?
N3 Fe1 N2 75.8(3) . . ?
N3 Fe1 N2 94.4(3) . 2_565 ?
N3 Fe1 N2 75.8(3) 2_565 2_565 ?
N3 Fe1 N2 94.4(3) 2_565 . ?
N3 Fe1 N3 167.3(4) . 2_565 ?
C1 N1 Fe1 164.5(10) . . ?
C2 N2 Fe1 127.8(6) . . ?
C2 N2 C6 116.6(7) . . ?
C6 N2 Fe1 115.3(5) . . ?
C10 N3 Fe1 117.5(5) . . ?
C13 N3 Fe1 125.5(7) . . ?
C13 N3 C10 116.9(8) . . ?
C28 N4 C8 105.6(7) . . ?
C7 N5 H5 126.6 . . ?
C7 N5 C28 106.8(7) . . ?
C28 N5 H5 126.6 . . ?
N1 C1 S1 177.9(12) . . ?
N2 C2 H2 117.8 . . ?
N2 C2 C3 124.3(9) . . ?
C3 C2 H2 117.8 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.1(8) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.1(8) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 117.2(7) . . ?
C4 C5 C7 127.5(8) . . ?
C7 C5 C6 115.2(7) . . ?
N2 C6 C5 122.6(7) . . ?
N2 C6 C10 116.3(7) . . ?
C5 C6 C10 121.1(7) . . ?
N5 C7 C5 130.1(8) . . ?
N5 C7 C8 105.0(7) . . ?
C8 C7 C5 124.8(8) . . ?
N4 C8 C7 110.6(7) . . ?
N4 C8 C9 129.3(8) . . ?
C7 C8 C9 120.1(8) . . ?
C10 C9 C8 117.9(7) . . ?
C10 C9 C11 117.1(8) . . ?
C11 C9 C8 124.9(8) . . ?
N3 C10 C6 114.9(7) . . ?
N3 C10 C9 124.1(7) . . ?
C9 C10 C6 120.8(7) . . ?
C9 C11 H11 120.2 . . ?
C12 C11 C9 119.7(9) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.1(9) . . ?
C13 C12 H12 119.9 . . ?
N3 C13 C12 121.9(9) . . ?
N3 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C15 C14 H14 119.5 . . ?
C15 C14 C19 121.1(10) . . ?
C19 C14 H14 119.5 . . ?
C14 C15 H15 120.6 . . ?
C14 C15 C16 118.8(10) . . ?
C16 C15 H15 120.6 . . ?
C15 C16 H16 118.6 . . ?
C17 C16 C15 122.7(12) . . ?
C17 C16 H16 118.6 . . ?
C16 C17 H17 119.3 . . ?
C16 C17 C18 121.4(10) . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C19 116.5(8) . . ?
C23 C18 C17 124.6(8) . . ?
C23 C18 C19 118.9(9) . . ?
C14 C19 C18 119.5(10) . . ?
C20 C19 C14 122.0(10) . . ?
C20 C19 C18 118.5(9) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 121.5(9) . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C22 120.5(10) . . ?
C20 C21 C24 120.3(11) . . ?
C22 C21 C24 119.2(11) . . ?
C21 C22 C27 119.0(10) . . ?
C23 C22 C21 118.6(9) . . ?
C23 C22 C27 122.4(9) . . ?
C18 C23 C28 118.1(8) . . ?
C22 C23 C18 122.0(8) . . ?
C22 C23 C28 119.9(8) . . ?
C21 C24 H24 119.3 . . ?
C25 C24 C21 121.3(12) . . ?
C25 C24 H24 119.3 . . ?
C24 C25 H25 120.4 . . ?
C24 C25 C26 119.2(13) . . ?
C26 C25 H25 120.4 . . ?
C25 C26 H26 119.0 . . ?
C27 C26 C25 122.1(13) . . ?
C27 C26 H26 119.0 . . ?
C22 C27 H27 120.4 . . ?
C26 C27 C22 119.1(11) . . ?
C26 C27 H27 120.4 . . ?
N4 C28 N5 112.0(7) . . ?
N4 C28 C23 126.9(7) . . ?
N5 C28 C23 120.6(8) . . ?
H1A O1 H1B 104.5 . . ?

_olex2_exptl_crystal_mounting_method 'coordination boond'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 10.606
_oxdiff_exptl_absorpt_empirical_full_min 0.248
