# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_a21042303a0249_250k
_database_code_depnum_ccdc_archive 'CCDC 2160467'
loop_
_audit_author_name
_audit_author_address
'Qi-Yao Li'
;Sun Yat sen University
China
;
_audit_update_record             
;
2022-03-21 deposited with the CCDC.	2022-06-16 downloaded from the CCDC.
;
_audit_creation_date             2022-03-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C5 Cs Fe N6 O, C2 H8 N'
_chemical_formula_sum            'C7 H8 Cs Fe N7 O'
_chemical_formula_weight         394.96
_chemical_absolute_configuration ?
_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'
Cs Cs -0.3680 2.1192 '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'

_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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.3288(3)
_cell_length_b                   8.9675(3)
_cell_length_c                   17.7852(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1328.35(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8044
_cell_measurement_temperature    249.99(13)
_cell_measurement_theta_max      30.0960
_cell_measurement_theta_min      3.3040
_shelx_estimated_absorpt_T_max   0.701
_shelx_estimated_absorpt_T_min   0.701
_exptl_absorpt_coefficient_mu    3.832
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12283
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.660
_diffrn_reflns_theta_min         3.226
_diffrn_ambient_temperature      249.99(13)
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00  17.00   1.00   13.59    --  -12.93 -77.00 -60.00   58
  2  ω    -43.00  18.00   1.00   13.59    --  -12.93  77.00  60.00   61
  3  ω      4.00  87.00   1.00   13.59    --   14.02  38.00 -60.00   83
  4  ω    -39.00  36.00   1.00   13.59    --   14.02 -77.00-180.00   75
  5  ω    -50.00  -2.00   1.00   13.59    --   14.02 -38.00 120.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                3382
_reflns_number_total             3607
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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         0.514
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_coef       0.00153(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3607
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0204
_refine_ls_restrained_S_all      1.043
_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)+(0.0186P)²+0.3353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0443
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H7A(0.056) H7B(0.056) H6A(0.073) H6B(0.073) H6C(0.073) H7C(0.103)
 H7D(0.103) H7E(0.103)
 Fixed X: H7A(0.3697) H7B(0.3678) H6A(0.4931) H6B(0.3243) H6C(0.4804)
 H7C(0.6369) H7D(0.6344) H7E(0.561)
 Fixed Y: H7A(0.0577) H7B(0.0428) H6A(-0.1642) H6B(-0.1782) H6C(-0.1809)
 H7C(0.0733) H7D(0.0576) H7E(0.1995)
 Fixed Z: H7A(0.4664) H7B(0.5468) H6A(0.4543) H6B(0.4927) H6C(0.5419)
 H7C(0.4649) H7D(0.5527) H7E(0.5144)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cs1 Cs 1.01652(2) 0.98948(2) 0.30591(2) 0.03010(7) Uani 1 1 d . . . . .
Fe1 Fe 0.51271(5) 0.47157(4) 0.33598(2) 0.02041(9) Uani 1 1 d . . . . .
C5 C 0.6639(4) 0.6374(4) 0.3335(2) 0.0263(8) Uani 1 1 d . . . . .
O1 O 0.4920(4) 0.4555(3) 0.17969(14) 0.0614(9) Uani 1 1 d . . . . .
N5 N 0.7587(4) 0.7276(4) 0.3317(2) 0.0450(10) Uani 1 1 d . . . . .
N6 N 0.5018(3) 0.4583(3) 0.24336(15) 0.0293(5) Uani 1 1 d . . . . .
N3 N 0.5288(4) 0.5067(3) 0.50870(16) 0.0402(7) Uani 1 1 d . . . . .
N2 N 0.3045(4) 0.1961(3) 0.37269(18) 0.0371(8) Uani 1 1 d . . . . .
N1 N 0.8156(5) 0.2770(4) 0.3553(2) 0.0484(9) Uani 1 1 d . . . . .
C2 C 0.3778(4) 0.2998(4) 0.35740(19) 0.0260(7) Uani 1 1 d . . . . .
C3 C 0.5210(3) 0.4938(3) 0.44462(17) 0.0256(6) Uani 1 1 d . . . . .
N7 N 0.4234(4) 0.0209(4) 0.50548(19) 0.0467(8) Uani 1 1 d . . . . .
H7A H 0.3697 0.0577 0.4664 0.056 Uiso 1 1 calc R . . . .
H7B H 0.3678 0.0428 0.5468 0.056 Uiso 1 1 calc R . . . .
C4 C 0.3284(4) 0.6038(4) 0.3405(2) 0.0279(7) Uani 1 1 d . . . . .
N4 N 0.2182(4) 0.6803(5) 0.3407(2) 0.0478(9) Uani 1 1 d . . . . .
C1 C 0.6995(5) 0.3452(4) 0.3478(2) 0.0303(8) Uani 1 1 d . . . . .
C6 C 0.4309(6) -0.1389(5) 0.4980(3) 0.0488(11) Uani 1 1 d . . . . .
H6A H 0.4931 -0.1642 0.4543 0.073 Uiso 1 1 calc GR . . . .
H6B H 0.3243 -0.1782 0.4927 0.073 Uiso 1 1 calc GR . . . .
H6C H 0.4804 -0.1809 0.5419 0.073 Uiso 1 1 calc GR . . . .
C7 C 0.5766(7) 0.0939(6) 0.5097(3) 0.0689(17) Uani 1 1 d . . . . .
H7C H 0.6369 0.0733 0.4649 0.103 Uiso 1 1 calc GR . . . .
H7D H 0.6344 0.0576 0.5527 0.103 Uiso 1 1 calc GR . . . .
H7E H 0.5610 0.1995 0.5144 0.103 Uiso 1 1 calc GR . . . .


_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
Cs1 Cs1 4.9127(2) 3_745 ?
Cs1 Cs1 4.9127(2) 3_755 ?
Cs1 C5 3.872(4) 3_755 ?
Cs1 N5 3.749(4) 3_755 ?
Cs1 N5 3.215(3) . ?
Cs1 N3 3.299(3) 4_566 ?
Cs1 N2 3.255(3) 1_665 ?
Cs1 N1 3.197(3) 1_565 ?
Cs1 N1 3.715(4) 3_755 ?
Cs1 N4 3.300(4) 1_655 ?
Cs1 N4 3.680(4) 3_655 ?
Cs1 C1 3.840(4) 3_755 ?
Fe1 C5 1.949(3) . ?
Fe1 N6 1.654(3) . ?
Fe1 C2 1.945(3) . ?
Fe1 C3 1.944(3) . ?
Fe1 C4 1.941(3) . ?
Fe1 C1 1.937(4) . ?
C5 Cs1 3.872(4) 3_745 ?
C5 N5 1.132(5) . ?
O1 N6 1.136(3) . ?
N5 Cs1 3.749(4) 3_745 ?
N3 Cs1 3.299(3) 4_466 ?
N3 C3 1.147(4) . ?
N2 Cs1 3.255(3) 1_445 ?
N2 C2 1.145(4) . ?
N1 Cs1 3.197(3) 1_545 ?
N1 Cs1 3.715(4) 3_745 ?
N1 C1 1.151(5) . ?
N7 C6 1.441(5) . ?
N7 C7 1.436(6) . ?
C4 N4 1.146(5) . ?
N4 Cs1 3.300(4) 1_455 ?
N4 Cs1 3.680(4) 3_645 ?
C1 Cs1 3.840(4) 3_745 ?

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
Cs1 Cs1 Cs1 131.758(9) 3_755 3_745 ?
C5 Cs1 Cs1 57.77(5) 3_755 3_755 ?
C5 Cs1 Cs1 95.27(5) 3_755 3_745 ?
N5 Cs1 Cs1 40.87(5) 3_755 3_755 ?
N5 Cs1 Cs1 133.40(7) . 3_755 ?
N5 Cs1 Cs1 49.74(7) . 3_745 ?
N5 Cs1 Cs1 106.47(6) 3_755 3_745 ?
N5 Cs1 C5 143.20(9) . 3_755 ?
N5 Cs1 C5 16.98(7) 3_755 3_755 ?
N5 Cs1 N5 147.43(5) . 3_755 ?
N5 Cs1 N3 83.42(9) . 4_566 ?
N5 Cs1 N2 148.84(9) . 1_665 ?
N5 Cs1 N1 89.25(9) . 3_755 ?
N5 Cs1 N4 72.51(10) . 1_655 ?
N5 Cs1 N4 94.94(8) . 3_655 ?
N5 Cs1 C1 54.52(8) 3_755 3_755 ?
N5 Cs1 C1 105.48(9) . 3_755 ?
N3 Cs1 Cs1 114.57(5) 4_566 3_745 ?
N3 Cs1 Cs1 113.38(5) 4_566 3_755 ?
N3 Cs1 C5 127.97(8) 4_566 3_755 ?
N3 Cs1 N5 129.14(8) 4_566 3_755 ?
N3 Cs1 N1 139.89(8) 4_566 3_755 ?
N3 Cs1 N4 136.02(8) 4_566 3_655 ?
N3 Cs1 N4 78.80(9) 4_566 1_655 ?
N3 Cs1 C1 134.12(8) 4_566 3_755 ?
N2 Cs1 Cs1 135.11(6) 1_665 3_745 ?
N2 Cs1 Cs1 70.70(6) 1_665 3_755 ?
N2 Cs1 C5 62.11(8) 1_665 3_755 ?
N2 Cs1 N5 63.01(8) 1_665 3_755 ?
N2 Cs1 N3 66.84(8) 1_665 4_566 ?
N2 Cs1 N1 107.22(8) 1_665 3_755 ?
N2 Cs1 N4 112.65(8) 1_665 3_655 ?
N2 Cs1 N4 92.00(9) 1_665 1_655 ?
N2 Cs1 C1 89.88(8) 1_665 3_755 ?
N1 Cs1 Cs1 40.59(5) 3_755 3_745 ?
N1 Cs1 Cs1 144.88(7) 1_565 3_745 ?
N1 Cs1 Cs1 100.19(6) 3_755 3_755 ?
N1 Cs1 Cs1 49.13(7) 1_565 3_755 ?
N1 Cs1 C5 105.04(9) 1_565 3_755 ?
N1 Cs1 C5 54.75(8) 3_755 3_755 ?
N1 Cs1 N5 88.93(9) 1_565 3_755 ?
N1 Cs1 N5 66.45(8) 3_755 3_755 ?
N1 Cs1 N5 101.56(9) 1_565 . ?
N1 Cs1 N3 74.54(9) 1_565 4_566 ?
N1 Cs1 N2 80.01(10) 1_565 1_665 ?
N1 Cs1 N1 145.34(7) 1_565 3_755 ?
N1 Cs1 N4 153.21(10) 1_565 1_655 ?
N1 Cs1 N4 62.70(10) 1_565 3_655 ?
N1 Cs1 C1 142.16(9) 1_565 3_755 ?
N1 Cs1 C1 17.43(8) 3_755 3_755 ?
N4 Cs1 Cs1 96.19(6) 3_655 3_745 ?
N4 Cs1 Cs1 48.51(7) 1_655 3_745 ?
N4 Cs1 Cs1 150.59(7) 1_655 3_755 ?
N4 Cs1 Cs1 42.20(6) 3_655 3_755 ?
N4 Cs1 C5 75.66(8) 3_655 3_755 ?
N4 Cs1 C5 93.32(8) 1_655 3_755 ?
N4 Cs1 N5 62.48(7) 3_655 3_755 ?
N4 Cs1 N5 110.29(8) 1_655 3_755 ?
N4 Cs1 N1 83.79(10) 3_655 3_755 ?
N4 Cs1 N1 61.45(10) 1_655 3_755 ?
N4 Cs1 N4 142.52(8) 1_655 3_655 ?
N4 Cs1 C1 88.82(9) 3_655 3_755 ?
N4 Cs1 C1 62.40(9) 1_655 3_755 ?
C1 Cs1 Cs1 55.85(5) 3_755 3_745 ?
C1 Cs1 Cs1 93.09(5) 3_755 3_755 ?
C1 Cs1 C5 40.18(7) 3_755 3_755 ?
N6 Fe1 C5 93.91(14) . . ?
N6 Fe1 C2 96.10(13) . . ?
N6 Fe1 C3 177.92(12) . . ?
N6 Fe1 C4 92.39(15) . . ?
N6 Fe1 C1 96.34(15) . . ?
C2 Fe1 C5 169.16(15) . . ?
C3 Fe1 C5 85.46(14) . . ?
C3 Fe1 C2 84.67(13) . . ?
C4 Fe1 C5 92.63(14) . . ?
C4 Fe1 C2 91.08(15) . . ?
C4 Fe1 C3 85.66(14) . . ?
C1 Fe1 C5 85.98(14) . . ?
C1 Fe1 C2 88.81(16) . . ?
C1 Fe1 C3 85.60(14) . . ?
C1 Fe1 C4 171.24(18) . . ?
Fe1 C5 Cs1 101.37(13) . 3_745 ?
N5 C5 Cs1 75.3(3) . 3_745 ?
N5 C5 Fe1 175.9(3) . . ?
Cs1 N5 Cs1 89.39(8) . 3_745 ?
C5 N5 Cs1 87.7(3) . 3_745 ?
C5 N5 Cs1 173.2(3) . . ?
O1 N6 Fe1 177.0(3) . . ?
C3 N3 Cs1 172.8(2) . 4_466 ?
C2 N2 Cs1 140.2(3) . 1_445 ?
Cs1 N1 Cs1 90.28(9) 1_545 3_745 ?
C1 N1 Cs1 87.4(3) . 3_745 ?
C1 N1 Cs1 146.8(3) . 1_545 ?
N2 C2 Fe1 176.3(3) . . ?
N3 C3 Fe1 178.8(3) . . ?
C7 N7 C6 114.8(4) . . ?
N4 C4 Fe1 177.6(4) . . ?
Cs1 N4 Cs1 89.29(8) 1_455 3_645 ?
C4 N4 Cs1 155.5(3) . 1_455 ?
C4 N4 Cs1 98.3(3) . 3_645 ?
Fe1 C1 Cs1 102.71(14) . 3_745 ?
N1 C1 Cs1 75.1(3) . 3_745 ?
N1 C1 Fe1 176.2(4) . . ?

_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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.91(3)
2 0.09(3)

####################################################################### 
# 
# 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_new
_database_code_depnum_ccdc_archive 'CCDC 2160468'
loop_
_audit_author_name
_audit_author_address
'Qi-Yao Li'
;Sun Yat sen University
China
;
_audit_update_record             
;
2022-06-15 deposited with the CCDC.	2022-06-16 downloaded from the CCDC.
;
_audit_creation_date             2022-06-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C20 Cs4 Fe4 N24 O4), C2 H8 N'
_chemical_formula_sum            'C7 H8 Cs Fe N7 O'
_chemical_formula_weight         394.96
_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'
Cs Cs -0.3680 2.1192 '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'

_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           63
_space_group_name_H-M_alt        'B m m b'
_space_group_name_Hall           '-B 2b 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'-x+1/2, -y, -z+1/2'
'x+1/2, y-1/2, -z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y-1/2, z+1/2'

_cell_length_a                   8.2860(3)
_cell_length_b                   9.0586(4)
_cell_length_c                   18.0168(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1352.33(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8044
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0960
_cell_measurement_theta_min      3.3040
_shelx_estimated_absorpt_T_max   0.705
_shelx_estimated_absorpt_T_min   0.705
_exptl_absorpt_coefficient_mu    3.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6738
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.995
_diffrn_reflns_theta_min         2.706
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1005
_reflns_number_total             1108
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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         0.806
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1108
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0263
_refine_ls_restrained_S_all      1.128
_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)+(0.0388P)²+0.9483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0712
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C4 = N4-C3
 1.5 with sigma of 0.02
 C4-C3
 2.55 with sigma of 0.02
 C1-N1 \\sim C1'-N1'
 with sigma of 0.02
 Fe1-N1 \\sim Fe1-N1'
 with sigma of 0.04
 Cs1-N1 \\sim Cs1-N1'
 with sigma of 0.02
 Cs1-C1 \\sim Cs1-C1'
 with sigma of 0.04
 Fe1-C1 \\sim Fe1-C1'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3 \\sim N4 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(N1') \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C1') \\sim Ueq, Uanis(N1)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C1, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1', C1'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C1')=Sof(N1')=1-FVAR(1)
 Sof(C1)=Sof(N1)=FVAR(1)
 Fixed Sof: C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25) N4(0.25) H4A(0.25)
 H4B(0.25) C4(0.25) H4C(0.25) H4D(0.25) H4E(0.25)
6.a Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B)
6.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4C,H4D,H4E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cs1 Cs 0.0000 -0.2500 0.55922(2) 0.04807(14) Uani 1 4 d DS T P . .
Fe1 Fe 0.5000 0.2500 0.58570(3) 0.03355(16) Uani 1 4 d DS T P . .
O1 O 0.5000 0.2500 0.4315(2) 0.097(2) Uani 1 4 d S T P . .
C2 C 0.5000 0.2500 0.6933(3) 0.0447(10) Uani 1 4 d S T P A .
N3 N 0.5000 0.2500 0.4945(2) 0.0520(10) Uani 1 4 d S T P A .
C1 C 0.3495(11) 0.0870(10) 0.5910(8) 0.057(2) Uani 0.529(18) 1 d D U . A 1
N2 N 0.5000 0.2500 0.7569(3) 0.0789(19) Uani 1 4 d S T P . .
N1 N 0.2011(10) 0.0495(13) 0.5979(4) 0.078(3) Uani 0.529(18) 1 d D U . A 1
C3 C 0.438(3) -0.355(4) 0.7545(12) 0.083(6) Uani 0.25 1 d D U . B -1
H3A H 0.5032 -0.4177 0.7238 0.124 Uiso 0.25 1 calc GR . . B -1
H3B H 0.3508 -0.3152 0.7257 0.124 Uiso 0.25 1 calc GR . . B -1
H3C H 0.3949 -0.4116 0.7951 0.124 Uiso 0.25 1 calc GR . . B -1
C1' C 0.3169(11) 0.1231(11) 0.5974(8) 0.052(2) Uani 0.471(18) 1 d D U . A 2
N1' N 0.2693(14) -0.0112(10) 0.6008(6) 0.082(3) Uani 0.471(18) 1 d D U . A 2
N4 N 0.535(2) -0.236(3) 0.7832(6) 0.111(6) Uani 0.25 1 d D U . B -1
H4A H 0.4766 -0.1923 0.8182 0.133 Uiso 0.25 1 calc R . . B -1
H4B H 0.6187 -0.2780 0.8061 0.133 Uiso 0.25 1 calc R . . B -1
C4 C 0.599(4) -0.122(4) 0.7377(15) 0.102(8) Uani 0.25 1 d D U . B -1
H4C H 0.5624 -0.1352 0.6876 0.152 Uiso 0.25 1 calc GR . . B -1
H4D H 0.7149 -0.1260 0.7389 0.152 Uiso 0.25 1 calc GR . . B -1
H4E H 0.5633 -0.0281 0.7559 0.152 Uiso 0.25 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
Cs1 N2 3.314(5) 13_556 y
Cs1 N1 3.259(7) . y
Cs1 N1 3.753(10) 4_546 y
Cs1 N1 3.259(7) 12 y
Cs1 N1 3.259(7) 2_545 y
Cs1 N1 3.753(10) 10_556 y
Cs1 N1 3.259(7) 11 y
Cs1 N1 3.753(10) 9_556 y
Cs1 N1' 3.196(7) 12 y
Cs1 N1' 3.196(7) . y
Cs1 N1' 3.196(7) 2_545 y
Cs1 N1' 3.196(7) 11 y
Fe1 C2 1.939(5) . y
Fe1 N3 1.643(4) . y
Fe1 C1 1.935(7) 12_565 y
Fe1 C1 1.935(7) 2_655 y
Fe1 C1 1.935(7) . y
Fe1 C1 1.935(7) 11_655 y
Fe1 C1' 1.915(7) 11_655 y
Fe1 C1' 1.915(7) 2_655 y
Fe1 C1' 1.915(7) 12_565 y
Fe1 C1' 1.915(7) . y
O1 N3 1.136(6) . ?
C2 N2 1.145(7) . ?
C1 N1 1.282(10) . ?
N2 Cs1 3.314(5) 13_556 y
N1 Cs1 3.753(10) 9_556 y
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 N4 1.439(16) . ?
C1' N1' 1.280(11) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C4 1.423(16) . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?

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
N2 Cs1 N1 138.94(18) 13_556 10_556 y
N2 Cs1 N1 138.94(18) 13_556 4_546 y
N2 Cs1 N1 138.94(18) 13_556 9_556 y
N1 Cs1 N2 77.67(13) 11 13_556 y
N1 Cs1 N2 77.67(14) . 13_556 y
N1 Cs1 N2 77.67(13) 2_545 13_556 y
N1 Cs1 N2 77.67(13) 12 13_556 y
N1 Cs1 N1 112.7(4) 2_545 11 y
N1 Cs1 N1 109.69(16) . 10_556 y
N1 Cs1 N1 82.1(4) 10_556 9_556 y
N1 Cs1 N1 112.7(4) . 12 y
N1 Cs1 N1 142.3(2) 11 10_556 y
N1 Cs1 N1 62.0(3) 12 10_556 y
N1 Cs1 N1 155.3(3) . 2_545 y
N1 Cs1 N1 52.71(19) 4_546 10_556 y
N1 Cs1 N1 89.15(16) 2_545 10_556 y
N1 Cs1 N1 62.0(3) 11 9_556 y
N1 Cs1 N1 61.5(4) . 11 y
N1 Cs1 N1 61.5(4) 2_545 12 y
N1 Cs1 N1 155.3(3) 11 12 y
N1 Cs1 N1 89.15(16) . 9_556 y
N1 Cs1 N1 142.3(2) . 4_546 y
N1 Cs1 N1 142.3(2) 12 9_556 y
N1 Cs1 N1 62.0(3) 2_545 4_546 y
N1 Cs1 N1 57.9(3) 4_546 9_556 y
N1 Cs1 N1 109.69(16) 11 4_546 y
N1 Cs1 N1 89.15(16) 12 4_546 y
N1 Cs1 N1 109.69(16) 2_545 9_556 y
N1' Cs1 N2 76.46(18) 2_545 13_556 y
N1' Cs1 N2 76.46(18) 11 13_556 y
N1' Cs1 N2 76.46(18) 12 13_556 y
N1' Cs1 N2 76.46(18) . 13_556 y
N1' Cs1 N1' 152.9(4) . 2_545 y
N1' Cs1 N1' 152.9(4) 12 11 y
N1' Cs1 N1' 85.2(5) 2_545 11 y
N1' Cs1 N1' 88.5(5) 2_545 12 y
N1' Cs1 N1' 88.5(5) . 11 y
N1' Cs1 N1' 85.2(5) . 12 y
N3 Fe1 C2 180.0 . . y
N3 Fe1 C1 92.8(4) . . y
N3 Fe1 C1 92.8(4) . 2_655 y
N3 Fe1 C1 92.8(4) . 11_655 y
N3 Fe1 C1 92.8(4) . 12_565 y
N3 Fe1 C1' 96.3(4) . 2_655 y
N3 Fe1 C1' 96.3(4) . . y
N3 Fe1 C1' 96.3(4) . 11_655 y
N3 Fe1 C1' 96.3(4) . 12_565 y
C1 Fe1 C2 87.2(4) . . y
C1 Fe1 C2 87.2(4) 2_655 . y
C1 Fe1 C2 87.2(4) 12_565 . y
C1 Fe1 C2 87.2(4) 11_655 . y
C1 Fe1 C1 174.4(8) 11_655 12_565 y
C1 Fe1 C1 99.5(7) 2_655 11_655 y
C1 Fe1 C1 174.4(8) 2_655 . y
C1 Fe1 C1 99.5(7) 12_565 . y
C1 Fe1 C1 80.3(7) 11_655 . y
C1 Fe1 C1 80.3(7) 2_655 12_565 y
C1' Fe1 C2 83.7(4) 2_655 . y
C1' Fe1 C2 83.7(4) . . y
C1' Fe1 C2 83.7(4) 11_655 . y
C1' Fe1 C2 83.7(4) 12_565 . y
C1' Fe1 C1' 167.4(8) 2_655 . y
C1' Fe1 C1' 167.4(8) 11_655 12_565 y
C1' Fe1 C1' 73.8(7) 2_655 11_655 y
C1' Fe1 C1' 104.8(7) 2_655 12_565 y
C1' Fe1 C1' 73.8(7) 12_565 . y
C1' Fe1 C1' 104.8(7) 11_655 . y
N2 C2 Fe1 180.0 . . ?
O1 N3 Fe1 180.0 . . ?
N1 C1 Fe1 145.6(12) . . ?
C2 N2 Cs1 180.0 . 13_556 ?
Cs1 N1 Cs1 90.85(16) . 9_556 ?
C1 N1 Cs1 103.0(9) . 9_556 ?
C1 N1 Cs1 133.7(10) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N4 C3 H3A 109.5 . . ?
N4 C3 H3B 109.5 . . ?
N4 C3 H3C 109.5 . . ?
N1' C1' Fe1 145.1(12) . . ?
C1' N1' Cs1 147.9(11) . . ?
C3 N4 H4A 106.6 . . ?
C3 N4 H4B 106.6 . . ?
H4A N4 H4B 106.5 . . ?
C4 N4 C3 123.1(13) . . ?
C4 N4 H4A 106.6 . . ?
C4 N4 H4B 106.6 . . ?
N4 C4 H4C 109.5 . . ?
N4 C4 H4D 109.5 . . ?
N4 C4 H4E 109.5 . . ?
H4C C4 H4D 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 C1 N1 Cs1 160.2(11) . . . . ?
Fe1 C1 N1 Cs1 56(2) . . . 9_556 ?
Fe1 C1' N1' Cs1 -141.8(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
