# Supplementary Information (SI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

####################################################################### 
# 
# 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_Desolvation-C2Cl4
_database_code_depnum_ccdc_archive 'CCDC 2341652'
loop_
_audit_author_name
_audit_author_address
'Yu-Ting Yang'
;Ningbo University
China
;
_audit_update_record             
;
2024-03-20 deposited with the CCDC.	2024-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-10-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H22 B2 Fe N6'
_chemical_formula_sum            'C24 H22 B2 Fe N6'
_chemical_formula_weight         471.94
_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'
B B 0.0013 0.0007 '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'

_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      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   9.8528(18)
_cell_length_b                   9.8528(18)
_cell_length_c                   17.332(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1682.6(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3835
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      26.186
_cell_measurement_theta_min      2.373
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.2810
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1171 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.3770.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.932
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4743
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.452
_diffrn_reflns_theta_min         2.378
_diffrn_ambient_temperature      298.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_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                522
_reflns_number_total             542
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         542
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0850
_refine_ls_restrained_S_all      1.099
_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)+(0.1451P)²+5.1883P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2422
_refine_ls_wR_factor_ref         0.2437
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H) groups
2. Restrained distances
 C1-B1
 1.6 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(B1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C5(0.125) C2(0.5) H2(0.5) C3(0.5) H3(0.5) H1A(0.125) H1B(0.125)
 H1C(0.125)
5.a Riding coordinates:
 B1(H1A,H1B,H1C)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
;
_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 0.500000 0.500000 0.500000 0.0399(7) Uani 1 16 d S T P A .
N2 N 0.3406(4) 0.3406(4) 0.500000 0.0477(14) Uani 1 4 d S T P . .
C4 C 0.1405(5) 0.1405(5) 0.500000 0.0554(19) Uani 1 4 d S T P . .
C5 C 0.000000 0.0712(13) 0.500000 0.041(3) Uani 0.5 4 d S T P . .
C2 C 0.2446(8) 0.3343(9) 0.4444(5) 0.059(2) Uani 0.5 1 d . . P A -1
H2 H 0.245703 0.398913 0.405328 0.071 Uiso 0.5 1 calc R U P A -1
C3 C 0.1456(8) 0.2365(10) 0.4433(5) 0.063(2) Uani 0.5 1 d . . P A -1
H3 H 0.081799 0.235554 0.403773 0.076 Uiso 0.5 1 calc R U P A -1
B1 B 0.500000 0.500000 0.7785(11) 0.136(10) Uani 1 8 d DS TU P . .
H1A H 0.475210 0.411550 0.796942 0.204 Uiso 0.125 1 d R U P B -1
H1B H 0.435790 0.565690 0.796942 0.204 Uiso 0.125 1 d R U P B -1
H1C H 0.589000 0.522760 0.796942 0.204 Uiso 0.125 1 d R U P B -1
N1 N 0.500000 0.500000 0.6289(7) 0.050(2) Uani 1 8 d S T P . .
C1 C 0.500000 0.500000 0.6847(10) 0.075(4) Uani 1 8 d DS TU P A .


_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 N2 2.222(6) . ?
Fe1 N2 2.222(6) 3_655 ?
Fe1 N2 2.222(6) 17_666 ?
Fe1 N2 2.222(6) 19_566 ?
Fe1 N1 2.234(12) 17_666 ?
Fe1 N1 2.234(12) . ?
N2 C2 1.351(8) . ?
C4 C5 1.544(9) 19_556 ?
C4 C5 1.544(9) . ?
C4 C3 1.365(10) . ?
C5 C5 1.40(3) 17_556 ?
C5 C5 0.992(18) 19_556 ?
C5 C5 0.992(19) 3 ?
C2 H2 0.9300 . ?
C2 C3 1.371(12) . ?
C3 H3 0.9300 . ?
B1 H1A 0.9600 . ?
B1 H1B 0.9600 . ?
B1 H1C 0.9601 . ?
B1 C1 1.625(10) . ?
N1 C1 0.968(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 180.0 . 17_666 ?
N2 Fe1 N2 90.0 17_666 3_655 ?
N2 Fe1 N2 90.0 . 3_655 ?
N2 Fe1 N2 90.0 . 19_566 ?
N2 Fe1 N2 90.0 17_666 19_566 ?
N2 Fe1 N2 180.0 19_566 3_655 ?
N2 Fe1 N1 90.0 19_566 . ?
N2 Fe1 N1 90.000(1) . . ?
N2 Fe1 N1 90.0 3_655 17_666 ?
N2 Fe1 N1 90.000(1) 17_666 17_666 ?
N2 Fe1 N1 90.000(1) 17_666 . ?
N2 Fe1 N1 90.0 19_566 17_666 ?
N2 Fe1 N1 90.000(1) . 17_666 ?
N2 Fe1 N1 90.0 3_655 . ?
N1 Fe1 N1 180.0 17_666 . ?
C2 N2 Fe1 121.8(4) . . ?
C5 C4 C5 37.5(9) . 19_556 ?
C3 C4 C5 129.6(5) . 19_556 ?
C3 C4 C5 109.9(5) . . ?
C4 C5 C4 127.5(9) . 3 ?
C5 C5 C4 116.3(4) 17_556 3 ?
C5 C5 C4 161.3(4) 19_556 3 ?
C5 C5 C4 71.3(4) 3 3 ?
C5 C5 C4 161.3(4) 3 . ?
C5 C5 C4 71.3(4) 19_556 . ?
C5 C5 C4 116.3(4) 17_556 . ?
C5 C5 C5 90.000(2) 3 19_556 ?
C5 C5 C5 45.000(2) 3 17_556 ?
C5 C5 C5 45.0 19_556 17_556 ?
N2 C2 H2 118.7 . . ?
N2 C2 C3 122.7(7) . . ?
C3 C2 H2 118.7 . . ?
C4 C3 C2 120.2(7) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
H1A B1 H1B 109.5 . . ?
H1A B1 H1C 109.5 . . ?
H1B B1 H1C 109.5 . . ?
C1 B1 H1A 109.5 . . ?
C1 B1 H1B 109.5 . . ?
C1 B1 H1C 109.5 . . ?
C1 N1 Fe1 180.0 . . ?
N1 C1 B1 180.0 . . ?

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 N2 C2 C3 179.8(7) . . . . ?
N2 C2 C3 C4 0.4(14) . . . . ?
C5 C4 C5 C4 180.0 19_556 . . 3 ?
C5 C4 C5 C5 0.0 19_556 . . 3 ?
C5 C4 C5 C5 0.0 19_556 . . 17_556 ?
C5 C4 C3 C2 163.1(8) . . . . ?
C5 C4 C3 C2 -159.7(8) 19_556 . . . ?
C3 C4 C5 C4 -50.0(5) . . . 3 ?
C3 C4 C5 C5 130.0(5) . . . 19_556 ?
C3 C4 C5 C5 130.0(5) . . . 3 ?
C3 C4 C5 C5 130.0(5) . . . 17_556 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.525 -0.400 -0.336 600.7 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_tpe-meoh-rt
_database_code_depnum_ccdc_archive 'CCDC 2341653'
loop_
_audit_author_name
_audit_author_address
'Yu-Ting Yang'
;Ningbo University
China
;
_audit_update_record             
;
2024-03-20 deposited with the CCDC.	2024-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-04-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H22 B2 Fe N6'
_chemical_formula_sum            'C24 H22 B2 Fe N6'
_chemical_formula_weight         471.94
_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'
B B 0.0013 0.0007 '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'

_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      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   9.8237(5)
_cell_length_b                   9.8237(5)
_cell_length_c                   17.274(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1667.0(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1728
_cell_measurement_temperature    301.11(10)
_cell_measurement_theta_max      24.9810
_cell_measurement_theta_min      3.7790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.940
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5015
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.064
_diffrn_reflns_theta_min         3.764
_diffrn_ambient_temperature      301.11(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       ?
_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                514
_reflns_number_total             639
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         639
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0462
_refine_ls_restrained_S_all      1.162
_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)+(0.0775P)²+0.2339P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1262
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
B1 \\sim C1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
3. Others
 Fixed Sof: C5(0.125) C2(0.5) H2(0.5) C3(0.5) H3(0.5) H1C(0.125) H1B(0.125)
 H1A(0.125)
4.a Riding coordinates:
 B1(H1C,H1B,H1A)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe1 Fe 0.500000 0.500000 0.500000 0.0309(4) Uani 1 16 d S T P A .
N1 N 0.500000 0.500000 0.6226(3) 0.0433(10) Uani 1 8 d S T P . .
N2 N 0.34028(19) 0.34028(19) 0.500000 0.0399(7) Uani 1 4 d S T P . .
C4 C 0.1400(2) 0.1400(2) 0.500000 0.0484(9) Uani 1 4 d S T P . .
C1 C 0.500000 0.500000 0.6863(4) 0.0631(16) Uani 1 8 d S TU P . .
C5 C 0.0685(6) 0.000000 0.500000 0.0353(14) Uani 0.5 4 d S T P . .
C2 C 0.3330(4) 0.2458(4) 0.4442(2) 0.0474(9) Uani 0.5 1 d . . P A -1
H2 H 0.397031 0.248479 0.404547 0.057 Uiso 0.5 1 calc R U P A -1
C3 C 0.2365(4) 0.1459(4) 0.4424(2) 0.0496(9) Uani 0.5 1 d . . P A -1
H3 H 0.236073 0.082227 0.402598 0.060 Uiso 0.5 1 calc R U P A -1
B1 B 0.500000 0.500000 0.7781(8) 0.165(6) Uani 1 8 d S TU P . .
H1C H 0.586500 0.468280 0.796574 0.248 Uiso 0.125 1 d R U P B -1
H1B H 0.429280 0.440950 0.796574 0.248 Uiso 0.125 1 d R U P B -1
H1A H 0.484220 0.590770 0.796574 0.248 Uiso 0.125 1 d R U P 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 2.118(5) 17_666 ?
Fe1 N1 2.118(5) . ?
Fe1 N2 2.219(3) . ?
Fe1 N2 2.219(3) 19_566 ?
Fe1 N2 2.219(3) 17_666 ?
Fe1 N2 2.219(3) 3_655 ?
N1 C1 1.101(8) . ?
N2 C2 1.340(4) . ?
C4 C5 1.544(5) . ?
C4 C5 1.544(5) 3 ?
C4 C3 1.375(4) . ?
C1 B1 1.585(15) . ?
C5 C5 1.346(12) 17_556 ?
C5 C5 0.952(9) 19_556 ?
C5 C5 0.952(9) 3 ?
C2 H2 0.9300 . ?
C2 C3 1.365(5) . ?
C3 H3 0.9300 . ?
B1 H1C 0.9600 . ?
B1 H1B 0.9599 . ?
B1 H1A 0.9599 . ?

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 180.0 17_666 . ?
N1 Fe1 N2 90.0 . 19_566 ?
N1 Fe1 N2 90.000(1) 17_666 . ?
N1 Fe1 N2 90.000(1) 17_666 17_666 ?
N1 Fe1 N2 90.0 . 3_655 ?
N1 Fe1 N2 90.000(1) . 17_666 ?
N1 Fe1 N2 90.000(1) . . ?
N1 Fe1 N2 90.0 17_666 19_566 ?
N1 Fe1 N2 90.0 17_666 3_655 ?
N2 Fe1 N2 180.0 19_566 3_655 ?
N2 Fe1 N2 90.0 17_666 3_655 ?
N2 Fe1 N2 180.0 17_666 . ?
N2 Fe1 N2 90.0 19_566 . ?
N2 Fe1 N2 90.0 17_666 19_566 ?
N2 Fe1 N2 90.0 3_655 . ?
C1 N1 Fe1 180.0 . . ?
C2 N2 Fe1 121.83(18) . . ?
C5 C4 C5 35.9(4) . 3 ?
C3 C4 C5 110.6(2) . . ?
C3 C4 C5 129.3(2) . 3 ?
N1 C1 B1 180.0 . . ?
C4 C5 C4 125.9(4) 19_556 . ?
C5 C5 C4 117.0(2) 17_556 19_556 ?
C5 C5 C4 72.1(2) 3 . ?
C5 C5 C4 162.0(2) 19_556 . ?
C5 C5 C4 72.1(2) 19_556 19_556 ?
C5 C5 C4 117.0(2) 17_556 . ?
C5 C5 C4 162.0(2) 3 19_556 ?
C5 C5 C5 44.999(1) 19_556 17_556 ?
C5 C5 C5 45.0 3 17_556 ?
C5 C5 C5 89.997(1) 19_556 3 ?
N2 C2 H2 118.3 . . ?
N2 C2 C3 123.4(3) . . ?
C3 C2 H2 118.3 . . ?
C4 C3 H3 120.2 . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 H3 120.2 . . ?
C1 B1 H1C 109.5 . . ?
C1 B1 H1B 109.5 . . ?
C1 B1 H1A 109.5 . . ?
H1C B1 H1B 109.5 . . ?
H1C B1 H1A 109.5 . . ?
H1B B1 H1A 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 N2 C2 C3 179.8(3) . . . . ?
N2 C2 C3 C4 0.4(6) . . . . ?
C5 C4 C5 C4 180.0 3 . . 19_556 ?
C5 C4 C5 C5 0.0 3 . . 17_556 ?
C5 C4 C5 C5 0.0 3 . . 19_556 ?
C5 C4 C3 C2 -164.1(4) . . . . ?
C5 C4 C3 C2 160.1(4) 3 . . . ?
C3 C4 C5 C4 50.5(2) . . . 19_556 ?
C3 C4 C5 C5 -129.5(2) . . . 3 ?
C3 C4 C5 C5 -129.5(2) . . . 19_556 ?
C3 C4 C5 C5 -129.5(2) . . . 17_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_tpe-c2cl4
_database_code_depnum_ccdc_archive 'CCDC 2341656'
loop_
_audit_author_name
_audit_author_address
'Yu-Ting Yang'
;Ningbo University
China
;
_audit_update_record             
;
2024-03-20 deposited with the CCDC.	2024-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-04-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H22 B2 Fe N6, 2(C2 Cl4)'
_chemical_formula_sum            'C28 H22 B2 Cl8 Fe N6'
_chemical_formula_weight         803.58
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_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           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   17.9178(8)
_cell_length_b                   13.9608(6)
_cell_length_c                   13.9443(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3488.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5201
_cell_measurement_temperature    200.02(10)
_cell_measurement_theta_max      29.2290
_cell_measurement_theta_min      3.9630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20307
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.227
_diffrn_reflns_theta_min         3.456
_diffrn_ambient_temperature      200.02(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'CCD plate'
_diffrn_measurement_method       ?
_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                3171
_reflns_number_total             4291
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4291
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0487
_refine_ls_restrained_S_all      1.052
_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)+(0.0717P)²+0.3352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1281
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.8887(9)
 0.1113(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H) groups
3. Others
 Sof(C16A)=Sof(C15A)=1-FVAR(1)
 Sof(C16B)=Sof(C15B)=FVAR(1)
 Fixed Sof: C6(0.5) C5(0.5)
4.a Riding coordinates:
 B(HA,HB,HC)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C9(H9), C8(H8), C2(H2), C13(H13), C10(H10), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe1 Fe 0.500000 0.23813(3) 0.250000 0.01464(14) Uani 1 2 d S T P . .
Cl4 Cl 0.87308(5) 0.52261(7) 0.45168(8) 0.0616(3) Uani 1 1 d . . . . .
Cl1 Cl 0.63602(5) 0.51192(7) 0.48138(10) 0.0715(3) Uani 1 1 d . . . . .
Cl3 Cl 0.75577(6) 0.39755(8) 0.37223(11) 0.0871(4) Uani 1 1 d . . . . .
Cl2 Cl 0.75260(6) 0.63469(10) 0.56353(11) 0.0871(4) Uani 1 1 d . . . . .
N2 N 0.500000 0.39655(19) 0.250000 0.0196(6) Uani 1 2 d S T P . .
N4 N 0.500000 1.07637(19) 0.250000 0.0235(7) Uani 1 2 d S T P . .
N1 N 0.38152(10) 0.23191(14) 0.24867(15) 0.0208(4) Uani 1 1 d . . . . .
N3 N 0.50249(10) 0.75387(12) 0.58921(18) 0.0212(5) Uani 1 1 d . . . . .
C7 C 0.500000 0.8754(2) 0.250000 0.0330(10) Uani 1 2 d S T P . .
C4 C 0.500000 0.5965(2) 0.250000 0.0350(10) Uani 1 2 d S T P . .
C11 C 0.44083(14) 0.7297(2) 0.5414(2) 0.0314(6) Uani 1 1 d . . . . .
H11 H 0.396906 0.717322 0.577480 0.038 Uiso 1 1 calc R U . . .
C12 C 0.49992(14) 0.7377(2) 0.3891(2) 0.0303(6) Uani 1 1 d . . . . .
C14 C 0.56355(14) 0.7676(2) 0.5352(2) 0.0313(6) Uani 1 1 d . . . . .
H14 H 0.608949 0.782920 0.566858 0.038 Uiso 1 1 calc R U . . .
C9 C 0.55360(14) 1.02568(18) 0.2064(2) 0.0302(6) Uani 1 1 d . . . . .
H9 H 0.592609 1.059581 0.175169 0.036 Uiso 1 1 calc R U . . .
C8 C 0.55528(15) 0.92632(18) 0.2044(2) 0.0336(7) Uani 1 1 d . . . . .
H8 H 0.594312 0.893743 0.171847 0.040 Uiso 1 1 calc R U . . .
C2 C 0.56137(14) 0.44660(19) 0.2320(3) 0.0376(8) Uani 1 1 d . . . . .
H2 H 0.606000 0.412484 0.218367 0.045 Uiso 1 1 calc R U . . .
C13 C 0.56445(15) 0.7608(2) 0.4369(2) 0.0318(6) Uani 1 1 d . . . . .
H13 H 0.609298 0.771975 0.402293 0.038 Uiso 1 1 calc R U . . .
C10 C 0.43668(15) 0.7214(2) 0.4432(2) 0.0350(7) Uani 1 1 d . . . . .
H10 H 0.390943 0.704684 0.413102 0.042 Uiso 1 1 calc R U . . .
C3 C 0.56407(15) 0.54563(19) 0.2320(3) 0.0451(9) Uani 1 1 d . . . . .
H3 H 0.609699 0.578053 0.219762 0.054 Uiso 1 1 calc R U . . .
C6 C 0.5018(3) 0.7704(3) 0.2177(4) 0.0187(10) Uani 0.5 1 d . . P A -1
B B 0.23642(18) 0.1771(3) 0.2672(3) 0.0500(11) Uani 1 1 d . . . . .
HA H 0.219095 0.139086 0.200869 0.075 Uiso 1 1 d R U . . .
HB H 0.201215 0.238206 0.280049 0.075 Uiso 1 1 d R U . . .
HC H 0.230865 0.127296 0.325669 0.075 Uiso 1 1 d R U . . .
C5 C 0.4990(3) 0.7026(4) 0.2853(4) 0.0172(9) Uani 0.5 1 d . . P A -1
C16B C 0.7797(4) 0.4925(5) 0.4435(5) 0.051(2) Uani 0.756(18) 1 d . . P B 1
C15B C 0.7282(4) 0.5389(5) 0.4905(5) 0.050(2) Uani 0.756(18) 1 d . . P B 1
C16A C 0.7855(11) 0.5457(15) 0.4815(14) 0.048(6) Uani 0.244(18) 1 d . . P B 2
C15A C 0.7275(12) 0.4902(14) 0.4518(14) 0.047(6) Uani 0.244(18) 1 d . . P B 2
C1 C 0.31982(14) 0.21047(17) 0.2550(2) 0.0248(5) 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 N2 2.212(3) . ?
Fe1 N4 2.258(3) 1_545 ?
Fe1 N1 2.1246(18) 3_655 ?
Fe1 N1 2.1247(18) . ?
Fe1 N3 2.245(2) 5_666 ?
Fe1 N3 2.245(2) 7_565 ?
Cl4 C16B 1.729(7) . ?
Cl4 C16A 1.656(19) . ?
Cl1 C15B 1.698(7) . ?
Cl1 C15A 1.72(2) . ?
Cl3 C16B 1.711(8) . ?
Cl3 C15A 1.78(2) . ?
Cl2 C15B 1.737(8) . ?
Cl2 C16A 1.79(2) . ?
N2 C2 1.327(3) . ?
N2 C2 1.327(3) 3_655 ?
N4 C9 1.339(3) 3_655 ?
N4 C9 1.339(3) . ?
N1 C1 1.149(3) . ?
N3 C11 1.334(3) . ?
N3 C14 1.342(3) . ?
C7 C8 1.375(3) 3_655 ?
C7 C8 1.375(3) . ?
C7 C6 1.535(5) . ?
C4 C3 1.373(3) 3_655 ?
C4 C3 1.373(3) . ?
C4 C5 1.562(6) . ?
C11 H11 0.9500 . ?
C11 C10 1.376(4) . ?
C12 C13 1.373(4) . ?
C12 C10 1.380(4) . ?
C12 C5 1.528(6) . ?
C14 H14 0.9500 . ?
C14 C13 1.374(4) . ?
C9 H9 0.9500 . ?
C9 C8 1.388(3) . ?
C8 H8 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.383(4) . ?
C13 H13 0.9500 . ?
C10 H10 0.9500 . ?
C3 H3 0.9500 . ?
C6 C5 1.337(6) . ?
B HA 1.1105 . ?
B HB 1.0761 . ?
B HC 1.0762 . ?
B C1 1.575(4) . ?
C16B C15B 1.304(13) . ?
C16A C15A 1.36(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N4 180.0 . 1_545 ?
N2 Fe1 N3 87.15(5) . 7_565 ?
N2 Fe1 N3 87.15(5) . 5_666 ?
N1 Fe1 N2 92.34(5) 3_655 . ?
N1 Fe1 N2 92.34(5) . . ?
N1 Fe1 N4 87.66(5) 3_655 1_545 ?
N1 Fe1 N4 87.66(5) . 1_545 ?
N1 Fe1 N1 175.31(10) 3_655 . ?
N1 Fe1 N3 89.48(7) . 5_666 ?
N1 Fe1 N3 90.75(7) 3_655 5_666 ?
N1 Fe1 N3 90.75(7) . 7_565 ?
N1 Fe1 N3 89.48(7) 3_655 7_565 ?
N3 Fe1 N4 92.85(5) 5_666 1_545 ?
N3 Fe1 N4 92.85(5) 7_565 1_545 ?
N3 Fe1 N3 174.30(9) 5_666 7_565 ?
C2 N2 Fe1 121.78(15) 3_655 . ?
C2 N2 Fe1 121.78(15) . . ?
C2 N2 C2 116.4(3) . 3_655 ?
C9 N4 Fe1 121.91(15) 3_655 1_565 ?
C9 N4 Fe1 121.91(15) . 1_565 ?
C9 N4 C9 116.2(3) 3_655 . ?
C1 N1 Fe1 166.30(19) . . ?
C11 N3 Fe1 119.70(17) . 5_666 ?
C11 N3 C14 115.5(3) . . ?
C14 N3 Fe1 124.72(17) . 5_666 ?
C8 C7 C8 117.7(3) . 3_655 ?
C8 C7 C6 130.2(2) 3_655 . ?
C8 C7 C6 110.0(2) . . ?
C3 C4 C3 117.7(3) . 3_655 ?
C3 C4 C5 123.9(2) . . ?
C3 C4 C5 115.1(2) 3_655 . ?
N3 C11 H11 117.9 . . ?
N3 C11 C10 124.3(2) . . ?
C10 C11 H11 117.9 . . ?
C13 C12 C10 117.7(3) . . ?
C13 C12 C5 122.9(3) . . ?
C10 C12 C5 117.1(3) . . ?
N3 C14 H14 118.0 . . ?
N3 C14 C13 124.0(3) . . ?
C13 C14 H14 118.0 . . ?
N4 C9 H9 118.2 . . ?
N4 C9 C8 123.6(3) . . ?
C8 C9 H9 118.2 . . ?
C7 C8 C9 119.5(3) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
N2 C2 H2 118.1 . . ?
N2 C2 C3 123.7(2) . . ?
C3 C2 H2 118.1 . . ?
C12 C13 C14 119.4(3) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C11 C10 C12 119.1(3) . . ?
C11 C10 H10 120.5 . . ?
C12 C10 H10 120.5 . . ?
C4 C3 C2 119.2(3) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C6 C7 117.9(4) . . ?
HA B HB 110.7 . . ?
HA B HC 107.2 . . ?
HB B HC 109.4 . . ?
C1 B HA 108.5 . . ?
C1 B HB 109.9 . . ?
C1 B HC 111.2 . . ?
C12 C5 C4 127.1(3) . . ?
C6 C5 C4 116.6(4) . . ?
C6 C5 C12 116.2(4) . . ?
Cl3 C16B Cl4 118.0(5) . . ?
C15B C16B Cl4 122.1(7) . . ?
C15B C16B Cl3 120.0(7) . . ?
Cl1 C15B Cl2 117.4(4) . . ?
C16B C15B Cl1 122.7(7) . . ?
C16B C15B Cl2 119.9(7) . . ?
Cl4 C16A Cl2 127.4(15) . . ?
C15A C16A Cl4 122(2) . . ?
C15A C16A Cl2 109.8(17) . . ?
Cl1 C15A Cl3 123.4(13) . . ?
C16A C15A Cl1 123.7(19) . . ?
C16A C15A Cl3 112.8(18) . . ?
N1 C1 B 177.2(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C2 C3 -179.5(3) . . . . ?
Fe1 N4 C9 C8 -179.6(2) 1_565 . . . ?
Fe1 N3 C11 C10 -179.1(2) 5_666 . . . ?
Fe1 N3 C14 C13 178.8(2) 5_666 . . . ?
Cl4 C16B C15B Cl1 178.6(3) . . . . ?
Cl4 C16B C15B Cl2 0.4(7) . . . . ?
Cl4 C16A C15A Cl1 179.9(9) . . . . ?
Cl4 C16A C15A Cl3 -4.2(19) . . . . ?
Cl3 C16B C15B Cl1 -2.3(7) . . . . ?
Cl3 C16B C15B Cl2 179.5(3) . . . . ?
Cl2 C16A C15A Cl1 5.7(19) . . . . ?
Cl2 C16A C15A Cl3 -178.4(8) . . . . ?
N2 C2 C3 C4 -1.1(5) . . . . ?
N4 C9 C8 C7 -0.7(5) . . . . ?
N3 C11 C10 C12 0.8(5) . . . . ?
N3 C14 C13 C12 -0.7(5) . . . . ?
C7 C6 C5 C4 179.3(3) . . . . ?
C7 C6 C5 C12 -4.2(6) . . . . ?
C11 N3 C14 C13 2.0(4) . . . . ?
C14 N3 C11 C10 -2.0(4) . . . . ?
C9 N4 C9 C8 0.4(2) 3_655 . . . ?
C8 C7 C8 C9 0.3(2) 3_655 . . . ?
C8 C7 C6 C5 -64.6(5) 3_655 . . . ?
C8 C7 C6 C5 132.3(4) . . . . ?
C2 N2 C2 C3 0.5(3) 3_655 . . . ?
C13 C12 C10 C11 0.6(4) . . . . ?
C13 C12 C5 C4 93.3(4) . . . . ?
C13 C12 C5 C6 -82.8(5) . . . . ?
C10 C12 C13 C14 -0.6(4) . . . . ?
C10 C12 C5 C4 -69.3(5) . . . . ?
C10 C12 C5 C6 114.6(4) . . . . ?
C3 C4 C3 C2 0.5(2) 3_655 . . . ?
C3 C4 C5 C12 69.4(4) 3_655 . . . ?
C3 C4 C5 C12 -89.5(4) . . . . ?
C3 C4 C5 C6 86.6(5) . . . . ?
C3 C4 C5 C6 -114.5(4) 3_655 . . . ?
C6 C7 C8 C9 165.8(3) . . . . ?
C5 C4 C3 C2 158.9(3) . . . . ?
C5 C12 C13 C14 -163.2(3) . . . . ?
C5 C12 C10 C11 164.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.8887(9)
2 0.1113(9)

####################################################################### 
# 
# 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_tpe-meoh-200k
_database_code_depnum_ccdc_archive 'CCDC 2341654'
loop_
_audit_author_name
_audit_author_address
'Yu-Ting Yang'
;Ningbo University
China
;
_audit_update_record             
;
2024-03-20 deposited with the CCDC.	2024-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-04-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H28 B2 Fe N6'
_chemical_formula_sum            'C24 H28 B2 Fe N6'
_chemical_formula_weight         477.99
_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'
B B 0.0013 0.0007 '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'

_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      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'y, x, -z'
'-x, y, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z'
'-y, -x, z'
'x, -y, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   9.5534(5)
_cell_length_b                   9.5534(5)
_cell_length_c                   16.771(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1530.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1473
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      27.7390
_cell_measurement_theta_min      4.2340
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3489
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.013
_diffrn_reflns_theta_min         3.873
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'CCD plate'
_diffrn_measurement_method       ?
_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                514
_reflns_number_total             580
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         580
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0417
_refine_ls_restrained_S_all      1.174
_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)+(0.0520P)²+1.6565P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1151
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H) groups, All C(H) groups
2. Others
 Fixed Sof: C2(0.5) H2(0.5) C3(0.5) H3(0.5) H1B(0.25) H1A(0.25) H1C(0.25)
 C5(0.125)
3.a Riding coordinates:
 B1(H1B,H1A,H1C)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_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
Fe1 Fe -0.500000 -0.500000 0.500000 0.0165(3) Uani 1 16 d S T P A .
N2 N -0.3515(2) -0.3515(2) 0.500000 0.0192(6) Uani 1 4 d S T P . .
N1 N -0.500000 -0.500000 0.3841(2) 0.0221(8) Uani 1 8 d S T P . .
C1 C -0.500000 -0.500000 0.3162(3) 0.0333(12) Uani 1 8 d S T P A .
C4 C -0.1439(3) -0.1439(3) 0.500000 0.0355(10) Uani 1 4 d S T P . .
C2 C -0.3505(4) -0.2473(4) 0.4456(2) 0.0235(7) Uani 0.5 1 d . . P A -1
H2 H -0.422361 -0.245276 0.406522 0.028 Uiso 0.5 1 calc R U P A -1
C3 C -0.2500(4) -0.1436(4) 0.4441(2) 0.0299(8) Uani 0.5 1 d . . P A -1
H3 H -0.253782 -0.072277 0.404744 0.036 Uiso 0.5 1 calc R U P A -1
B1 B -0.500000 -0.500000 0.2236(5) 0.099(5) Uani 1 8 d S T P . .
H1B H -0.529950 -0.410120 0.204499 0.118 Uiso 0.25 1 d R U P A -1
H1A H -0.562860 -0.570880 0.204499 0.118 Uiso 0.25 1 d R U P A -1
H1C H -0.407180 -0.519000 0.204499 0.118 Uiso 0.25 1 d R U P A -1
C5 C -0.0717(7) 0.000000 0.500000 0.0197(12) Uani 0.5 4 d S T P A .


_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 N2 2.006(3) . ?
Fe1 N2 2.006(3) 2_455 ?
Fe1 N2 2.006(3) 17_446 ?
Fe1 N2 2.006(3) 18_546 ?
Fe1 N1 1.944(4) 17_446 ?
Fe1 N1 1.944(4) . ?
N2 C2 1.350(4) . ?
N1 C1 1.139(7) . ?
C1 B1 1.552(10) . ?
C4 C3 1.380(4) . ?
C4 C5 1.538(4) . ?
C4 C5 1.538(4) 2 ?
C2 H2 0.9500 . ?
C2 C3 1.379(5) . ?
C3 H3 0.9500 . ?
B1 H1B 0.9602 . ?
B1 H1A 0.9602 . ?
B1 H1C 0.9603 . ?
C5 C5 0.968(9) 2 ?
C5 C5 1.369(13) 17_556 ?
C5 C5 0.968(9) 18_556 ?

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 Fe1 N2 180.0 . 17_446 ?
N2 Fe1 N2 90.0 17_446 2_455 ?
N2 Fe1 N2 90.0 . 2_455 ?
N2 Fe1 N2 90.0 . 18_546 ?
N2 Fe1 N2 180.0 2_455 18_546 ?
N2 Fe1 N2 90.0 17_446 18_546 ?
N1 Fe1 N2 90.0 17_446 17_446 ?
N1 Fe1 N2 90.0 . . ?
N1 Fe1 N2 90.0 . 18_546 ?
N1 Fe1 N2 90.0 . 17_446 ?
N1 Fe1 N2 90.0 17_446 . ?
N1 Fe1 N2 90.0 17_446 2_455 ?
N1 Fe1 N2 90.0 . 2_455 ?
N1 Fe1 N2 90.0 17_446 18_546 ?
N1 Fe1 N1 180.0 17_446 . ?
C2 N2 Fe1 121.78(18) . . ?
C1 N1 Fe1 180.0 . . ?
N1 C1 B1 180.0 . . ?
C3 C4 C5 131.0(2) . 2 ?
C3 C4 C5 109.1(2) . . ?
C5 C4 C5 36.7(4) 2 . ?
N2 C2 H2 118.4 . . ?
N2 C2 C3 123.2(3) . . ?
C3 C2 H2 118.4 . . ?
C4 C3 H3 120.1 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C1 B1 H1B 109.5 . . ?
C1 B1 H1A 109.5 . . ?
C1 B1 H1C 109.5 . . ?
H1B B1 H1A 109.4 . . ?
H1B B1 H1C 109.4 . . ?
H1A B1 H1C 109.4 . . ?
C4 C5 C4 126.7(4) 18_556 . ?
C5 C5 C4 161.7(2) 18_556 . ?
C5 C5 C4 71.6(2) 18_556 18_556 ?
C5 C5 C4 71.6(2) 2 . ?
C5 C5 C4 116.7(2) 17_556 . ?
C5 C5 C4 116.7(2) 17_556 18_556 ?
C5 C5 C4 161.7(2) 2 18_556 ?
C5 C5 C5 45.001(1) 18_556 17_556 ?
C5 C5 C5 90.002(1) 18_556 2 ?
C5 C5 C5 45.001(1) 2 17_556 ?

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 N2 C2 C3 179.9(3) . . . . ?
N2 C2 C3 C4 0.2(5) . . . . ?
C3 C4 C5 C4 45.94(18) . . . 18_556 ?
C3 C4 C5 C5 -134.06(18) . . . 2 ?
C3 C4 C5 C5 -134.06(18) . . . 18_556 ?
C3 C4 C5 C5 -134.06(18) . . . 17_556 ?
C5 C4 C3 C2 -164.7(3) . . . . ?
C5 C4 C3 C2 160.6(4) 2 . . . ?
C5 C4 C5 C4 180.0 2 . . 18_556 ?
C5 C4 C5 C5 0.0 2 . . 18_556 ?
C5 C4 C5 C5 0.0 2 . . 17_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_Desolvation-C2Cl4-448K
_database_code_depnum_ccdc_archive 'CCDC 2341655'
loop_
_audit_author_name
_audit_author_address
'Yu-Ting Yang'
;Ningbo University
China
;
_audit_update_record             
;
2024-03-20 deposited with the CCDC.	2024-07-24 downloaded from the CCDC.
;
_audit_creation_date             2023-10-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H22 B2 Fe N6'
_chemical_formula_sum            'C24 H22 B2 Fe N6'
_chemical_formula_weight         471.94
_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'
B B 0.0013 0.0007 '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'

_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      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   9.856(3)
_cell_length_b                   9.856(3)
_cell_length_c                   17.199(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1670.8(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1954
_cell_measurement_temperature    448.1
_cell_measurement_theta_max      38.523
_cell_measurement_theta_min      2.376
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.7477
_exptl_absorpt_correction_T_min  0.2927
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1783 before and 0.0975 after correction.
The Ratio of minimum to maximum transmission is 0.3915.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.938
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.4123
_diffrn_reflns_av_unetI/netI     0.1620
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3842
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.382
_diffrn_ambient_temperature      448.1
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                338
_reflns_number_total             460
_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       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.444
_refine_diff_density_min         -1.931
_refine_diff_density_rms         0.360
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.467
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         460
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.3546
_refine_ls_R_factor_gt           0.3234
_refine_ls_restrained_S_all      2.366
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5982
_refine_ls_wR_factor_ref         0.6124
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim N1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: C5(0.125) C2(0.5) H2(0.5) C3(0.5) H3(0.5) H1C(0.125) H1A(0.125)
 H1B(0.125)
5.a Riding coordinates:
 B1(H1C,H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
;
_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 0.500000 0.500000 0.500000 0.013(3) Uani 1 16 d S T P A .
N2 N 0.3469(17) 0.3469(17) 0.500000 0.038(5) Uani 1 4 d S TU P . .
C4 C 0.147(3) 0.147(3) 0.500000 0.050(7) Uani 1 4 d S T P . .
C5 C 0.000000 0.078(7) 0.500000 0.046(11) Uani 0.5 4 d S T P . .
C2 C 0.257(4) 0.335(4) 0.446(2) 0.048(7) Uani 0.5 1 d . U P A -1
H2 H 0.261568 0.396306 0.405056 0.058 Uiso 0.5 1 calc R U P A -1
C3 C 0.145(4) 0.232(4) 0.444(2) 0.047(6) Uani 0.5 1 d . U P A -1
H3 H 0.079025 0.229911 0.405208 0.057 Uiso 0.5 1 calc R U P A -1
N1 N 0.500000 0.500000 0.624(3) 0.045(7) Uani 1 8 d S TU P . .
C1 C 0.500000 0.500000 0.691(3) 0.049(8) Uani 1 8 d S TU P A .
B1 B 0.500000 0.500000 0.777(4) 0.11(4) Uani 1 8 d S T P . .
H1C H 0.421860 0.548250 0.796045 0.159 Uiso 0.125 1 d R U P A -1
H1A H 0.580850 0.543540 0.796045 0.159 Uiso 0.125 1 d R U P A -1
H1B H 0.497280 0.408210 0.796045 0.159 Uiso 0.125 1 d R U P 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 N2 2.13(2) 17_666 ?
Fe1 N2 2.13(2) 3_655 ?
Fe1 N2 2.13(2) 19_566 ?
Fe1 N2 2.13(2) . ?
Fe1 N1 2.13(4) 17_666 ?
Fe1 N1 2.13(4) . ?
N2 C2 1.29(4) . ?
C4 C5 1.60(5) 19_556 ?
C4 C5 1.60(5) . ?
C4 C3 1.27(4) . ?
C5 C5 1.09(10) 19_556 ?
C5 C5 1.54(14) 17_556 ?
C5 C5 1.09(10) 3 ?
C2 H2 0.9300 . ?
C2 C3 1.50(5) . ?
C3 H3 0.9300 . ?
N1 C1 1.16(6) . ?
C1 B1 1.48(10) . ?
B1 H1C 0.9600 . ?
B1 H1A 0.9599 . ?
B1 H1B 0.9599 . ?

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 Fe1 N2 90.0 17_666 19_566 ?
N2 Fe1 N2 90.000(2) 3_655 . ?
N2 Fe1 N2 180.0 17_666 . ?
N2 Fe1 N2 90.000(1) 17_666 3_655 ?
N2 Fe1 N2 180.0 19_566 3_655 ?
N2 Fe1 N2 90.000(1) 19_566 . ?
N1 Fe1 N2 90.000(1) 17_666 3_655 ?
N1 Fe1 N2 90.000(6) 17_666 . ?
N1 Fe1 N2 90.000(1) . 19_566 ?
N1 Fe1 N2 90.000(1) . 3_655 ?
N1 Fe1 N2 90.000(1) 17_666 19_566 ?
N1 Fe1 N2 90.000(6) 17_666 17_666 ?
N1 Fe1 N2 90.000(6) . 17_666 ?
N1 Fe1 N2 90.000(6) . . ?
N1 Fe1 N1 180.0 17_666 . ?
C2 N2 Fe1 123.4(19) . . ?
C5 C4 C5 40(5) . 19_556 ?
C3 C4 C5 126(3) . 19_556 ?
C3 C4 C5 105(2) . . ?
C4 C5 C4 130(5) 3 . ?
C5 C5 C4 160(2) 19_556 3 ?
C5 C5 C4 70(2) 3 3 ?
C5 C5 C4 70(2) 19_556 . ?
C5 C5 C4 115(2) 17_556 . ?
C5 C5 C4 160(2) 3 . ?
C5 C5 C4 115(2) 17_556 3 ?
C5 C5 C5 44.999(7) 3 17_556 ?
C5 C5 C5 89.998(9) 3 19_556 ?
C5 C5 C5 45.0 19_556 17_556 ?
N2 C2 H2 117.1 . . ?
N2 C2 C3 126(3) . . ?
C3 C2 H2 117.1 . . ?
C4 C3 C2 114(4) . . ?
C4 C3 H3 122.9 . . ?
C2 C3 H3 122.9 . . ?
C1 N1 Fe1 180.000(11) . . ?
N1 C1 B1 180.00(3) . . ?
C1 B1 H1C 109.5 . . ?
C1 B1 H1A 109.5 . . ?
C1 B1 H1B 109.5 . . ?
H1C B1 H1A 109.5 . . ?
H1C B1 H1B 109.5 . . ?
H1A B1 H1B 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 N2 C2 C3 -178(3) . . . . ?
N2 C2 C3 C4 -3(6) . . . . ?
C5 C4 C5 C4 180.0 19_556 . . 3 ?
C5 C4 C5 C5 0.0 19_556 . . 3 ?
C5 C4 C5 C5 0.0 19_556 . . 17_556 ?
C5 C4 C3 C2 164(3) . . . . ?
C5 C4 C3 C2 -158(4) 19_556 . . . ?
C3 C4 C5 C4 -51(2) . . . 3 ?
C3 C4 C5 C5 129(2) . . . 19_556 ?
C3 C4 C5 C5 129(2) . . . 3 ?
C3 C4 C5 C5 129(2) . . . 17_556 ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_RINTA01_Desolvation-C2Cl4-448K 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The spot quality of this crystal was not ideal at high temperature 
(448 K), but the data of this crystal cooled in situ to room temperature is of 
good quality and can be used to illustrate the single-crystal-to-single-crystal 
transformation. The data reported here is to establish the structure of 
desolventized state at high temperature.
;
_vrf_PLAT020_Desolvation-C2Cl4-448K 
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.412 Report
RESPONSE: For the same reasons as above.
;
_vrf_PLAT082_Desolvation-C2Cl4-448K 
;
PROBLEM: High R1 Value ..................................       0.32 Report
RESPONSE: For the same reasons as above.
;
_vrf_PLAT084_Desolvation-C2Cl4-448K 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.61 Report
RESPONSE: For the same reasons as above.
;
_vrf_PLAT601_Desolvation-C2Cl4-448K 
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        590 Ang**3
RESPONSE: For the same reasons as above.
;
_vrf_PLAT049_Desolvation-C2Cl4-448K 
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.9382 Check 
RESPONSE: For the same reasons as above.
;
_vrf_PLAT097_Desolvation-C2Cl4-448K 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       4.44 eA-3  
RESPONSE: For the same reasons as above.
;
# end Validation Reply Form
