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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tu62_200k_sq
_database_code_depnum_ccdc_archive 'CCDC 1564873'
_audit_update_record             
;
2017-07-26 deposited with the CCDC.
2018-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4.50 H6 B0.33 F1.33 Fe0.17 N4'
_chemical_formula_weight         154.38

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   11.3101(16)
_cell_length_b                   11.3101(16)
_cell_length_c                   19.393(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2148.4(7)
_cell_formula_units_Z            12
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_F_000             948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.439
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6781
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16410
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.603
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1781
_reflns_number_gt                1479
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0550P)²+1.8861P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1781
_refine_ls_number_parameters     108
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1393
_refine_ls_wR_factor_gt          0.1324
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
FE1 Fe 0.000000 0.000000 0.500000 0.0265(2) Uani 1 6 d S T P . .
N1 N 0.2925(2) 0.3658(2) 0.39591(10) 0.0340(5) Uani 1 1 d . . . . .
N2 N 0.1751(2) 0.3656(2) 0.38377(13) 0.0477(6) Uani 1 1 d . . . . .
N3 N 0.0780(2) 0.2530(2) 0.40888(12) 0.0431(5) Uani 1 1 d . . . . .
N4 N 0.1305(2) 0.1796(2) 0.43742(9) 0.0325(4) Uani 1 1 d . . . . .
C1 C 0.2631(2) 0.2514(2) 0.42828(12) 0.0342(5) Uani 1 1 d . . . . .
H1 H 0.327294 0.225448 0.442546 0.041 Uiso 1 1 calc R U . . .
C2 C 0.4235(3) 0.4795(2) 0.37222(13) 0.0411(6) Uani 1 1 d . . . . .
H2A H 0.499168 0.480507 0.398430 0.049 Uiso 1 1 calc R U . . .
H2B H 0.426093 0.567090 0.380469 0.049 Uiso 1 1 calc R U . . .
C3 C 0.4411(2) 0.4636(2) 0.29653(12) 0.0306(5) Uani 1 1 d . . . . .
C4 C 0.4514(2) 0.3451(2) 0.26304(13) 0.0359(5) Uani 1 1 d . . . . .
H4A H 0.534736 0.340749 0.273826 0.043 Uiso 1 1 calc R U . . .
H4B H 0.367250 0.254521 0.263804 0.043 Uiso 1 1 calc R U . . .
C5 C 0.5620(3) 0.5620(3) 0.250000 0.0354(7) Uani 1 2 d S T P . .
H5A H 0.569224 0.651173 0.239893 0.042 Uiso 0.5 1 calc R U P . .
H5B H 0.651174 0.569227 0.260107 0.042 Uiso 0.5 1 calc R U P . .
B1 B 0.666667 0.333333 0.4581(3) 0.0464(12) Uani 1 3 d S T P . .
F2 F 0.666667 0.333333 0.5270(6) 0.151(5) Uani 0.500(0) 3 d S T P . .
F3 F 0.666667 0.333333 0.3928(5) 0.219(9) Uani 0.500(0) 3 d S T P . .
F1A F 0.5455(8) 0.2710(12) 0.4833(5) 0.175(5) Uani 0.500(0) 1 d . . P . .
F1B F 0.5390(7) 0.2483(7) 0.4374(5) 0.118(3) Uani 0.500(0) 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
FE1 N4 2.1858(19) . ?
FE1 N4 2.1858(19) 8_556 ?
FE1 N4 2.1858(19) 2 ?
FE1 N4 2.1858(19) 9_556 ?
FE1 N4 2.1858(19) 3 ?
FE1 N4 2.1858(19) 7_556 ?
N1 C1 1.322(3) . ?
N1 N2 1.348(3) . ?
N1 C2 1.468(3) . ?
N2 N3 1.291(3) . ?
N3 N4 1.357(3) . ?
N4 C1 1.313(3) . ?
C2 C3 1.504(3) . ?
C3 C4 1.544(3) 4 ?
C3 C4 1.546(3) . ?
C3 C5 1.549(3) . ?
C3 C3 1.858(5) 4 ?
C4 C3 1.544(3) 4 ?
C5 C3 1.549(3) 4 ?
B1 F3 1.265(11) . ?
B1 F1A 1.284(8) 3_665 ?
B1 F1A 1.284(8) . ?
B1 F1A 1.284(8) 2_655 ?
B1 F1B 1.335(6) 3_665 ?
B1 F1B 1.335(6) . ?
B1 F1B 1.335(6) 2_655 ?
B1 F2 1.337(12) . ?
F2 F1A 1.458(11) 3_665 ?
F2 F1A 1.458(11) . ?
F2 F1A 1.458(11) 2_655 ?
F3 F1B 1.539(10) 3_665 ?
F3 F1B 1.539(10) . ?
F3 F1B 1.539(10) 2_655 ?
F1A F1B 0.920(11) . ?

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
N4 FE1 N4 87.84(7) . 8_556 ?
N4 FE1 N4 92.16(7) . 2 ?
N4 FE1 N4 180.0 8_556 2 ?
N4 FE1 N4 87.84(7) . 9_556 ?
N4 FE1 N4 92.16(7) 8_556 9_556 ?
N4 FE1 N4 87.84(7) 2 9_556 ?
N4 FE1 N4 92.16(7) . 3 ?
N4 FE1 N4 87.84(7) 8_556 3 ?
N4 FE1 N4 92.16(7) 2 3 ?
N4 FE1 N4 180.0 9_556 3 ?
N4 FE1 N4 180.0 . 7_556 ?
N4 FE1 N4 92.16(7) 8_556 7_556 ?
N4 FE1 N4 87.84(7) 2 7_556 ?
N4 FE1 N4 92.16(7) 9_556 7_556 ?
N4 FE1 N4 87.84(7) 3 7_556 ?
C1 N1 N2 108.4(2) . . ?
C1 N1 C2 131.0(2) . . ?
N2 N1 C2 120.6(2) . . ?
N3 N2 N1 106.6(2) . . ?
N2 N3 N4 110.0(2) . . ?
C1 N4 N3 106.27(19) . . ?
C1 N4 FE1 132.97(16) . . ?
N3 N4 FE1 119.78(15) . . ?
N4 C1 N1 108.7(2) . . ?
N1 C2 C3 109.68(19) . . ?
C2 C3 C4 127.7(2) . 4 ?
C2 C3 C4 125.8(2) . . ?
C4 C3 C4 87.88(19) 4 . ?
C2 C3 C5 127.20(19) . . ?
C4 C3 C5 87.54(16) 4 . ?
C4 C3 C5 87.48(16) . . ?
C2 C3 C3 178.8(2) . 4 ?
C4 C3 C3 53.09(14) 4 4 ?
C4 C3 C3 53.00(14) . 4 ?
C5 C3 C3 53.16(11) . 4 ?
C3 C4 C3 73.92(18) 4 . ?
C3 C5 C3 73.7(2) 4 . ?
F3 B1 F1A 112.4(5) . 3_665 ?
F3 B1 F1A 112.4(6) . . ?
F1A B1 F1A 106.4(6) 3_665 . ?
F3 B1 F1A 112.4(5) . 2_655 ?
F1A B1 F1A 106.4(6) 3_665 2_655 ?
F1A B1 F1A 106.4(6) . 2_655 ?
F3 B1 F1B 72.5(5) . 3_665 ?
F1A B1 F1B 41.1(5) 3_665 3_665 ?
F1A B1 F1B 114.7(8) . 3_665 ?
F1A B1 F1B 132.8(8) 2_655 3_665 ?
F3 B1 F1B 72.5(5) . . ?
F1A B1 F1B 132.8(8) 3_665 . ?
F1A B1 F1B 41.1(5) . . ?
F1A B1 F1B 114.7(8) 2_655 . ?
F1B B1 F1B 111.4(5) 3_665 . ?
F3 B1 F1B 72.5(5) . 2_655 ?
F1A B1 F1B 114.7(8) 3_665 2_655 ?
F1A B1 F1B 132.8(8) . 2_655 ?
F1A B1 F1B 41.1(5) 2_655 2_655 ?
F1B B1 F1B 111.4(5) 3_665 2_655 ?
F1B B1 F1B 111.4(5) . 2_655 ?
F3 B1 F2 180.0 . . ?
F1A B1 F2 67.6(5) 3_665 . ?
F1A B1 F2 67.6(5) . . ?
F1A B1 F2 67.6(5) 2_655 . ?
F1B B1 F2 107.5(5) 3_665 . ?
F1B B1 F2 107.5(5) . . ?
F1B B1 F2 107.5(5) 2_655 . ?
B1 F2 F1A 54.5(5) . 3_665 ?
B1 F2 F1A 54.5(5) . . ?
F1A F2 F1A 89.6(6) 3_665 . ?
B1 F2 F1A 54.5(5) . 2_655 ?
F1A F2 F1A 89.6(6) 3_665 2_655 ?
F1A F2 F1A 89.7(6) . 2_655 ?
B1 F3 F1B 55.9(4) . 3_665 ?
B1 F3 F1B 55.9(4) . . ?
F1B F3 F1B 91.6(5) 3_665 . ?
B1 F3 F1B 55.9(4) . 2_655 ?
F1B F3 F1B 91.6(5) 3_665 2_655 ?
F1B F3 F1B 91.6(5) . 2_655 ?
F1B F1A B1 72.5(8) . . ?
F1B F1A F2 128.5(11) . . ?
B1 F1A F2 57.9(6) . . ?
F1A F1B B1 66.5(7) . . ?
F1A F1B F3 116.7(10) . . ?
B1 F1B F3 51.6(5) . . ?

_refine_diff_density_max         0.308
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.053



####################################################################### 
# 
# 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_tu65_100k_sq
_database_code_depnum_ccdc_archive 'CCDC 1564876'
_audit_update_record             
;
2017-07-26 deposited with the CCDC.
2018-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H36 Cl2 Fe N24 O8'
_chemical_formula_weight         951.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'

_cell_length_a                   11.1004(7)
_cell_length_b                   11.1004(7)
_cell_length_c                   19.4074(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2071.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_F_000             980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.571
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48146
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.671
_diffrn_reflns_theta_max         30.566
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2123
_reflns_number_gt                1949
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+14.0542P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2123
_refine_ls_number_parameters     108
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0953
_refine_ls_wR_factor_ref         0.1876
_refine_ls_wR_factor_gt          0.1857
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_restrained_S_all      1.264
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
FE Fe 0.000000 0.000000 0.500000 0.0153(3) Uani 1 6 d S T P . .
N1 N 0.2741(4) 0.3591(4) 0.39569(18) 0.0235(7) Uani 1 1 d . . . . .
N2 N 0.1505(4) 0.3522(4) 0.3823(2) 0.0286(8) Uani 1 1 d . . . . .
N3 N 0.0548(4) 0.2388(4) 0.40987(19) 0.0250(7) Uani 1 1 d . . . . .
N4 N 0.1136(3) 0.1709(4) 0.44110(16) 0.0183(6) Uani 1 1 d . . . . .
C1 C 0.2490(4) 0.2469(4) 0.4312(2) 0.0232(8) Uani 1 1 d . . . . .
H1 H 0.316887 0.224945 0.446925 0.028 Uiso 1 1 calc R U . . .
C2 C 0.4050(5) 0.4740(4) 0.3706(2) 0.0287(9) Uani 1 1 d . . . . .
H2A H 0.482883 0.480115 0.398183 0.034 Uiso 1 1 calc R U . . .
H2B H 0.404489 0.562403 0.376186 0.034 Uiso 1 1 calc R U . . .
C3 C 0.4261(4) 0.4534(4) 0.2959(2) 0.0195(7) Uani 1 1 d . . . . .
C4 C 0.4370(4) 0.3297(4) 0.2655(2) 0.0238(8) Uani 1 1 d . . . . .
H4A H 0.520876 0.325016 0.278336 0.029 Uiso 1 1 calc R U . . .
H4B H 0.350718 0.237888 0.266206 0.029 Uiso 1 1 calc R U . . .
C5 C 0.5509(5) 0.5509(5) 0.250000 0.0216(11) Uani 1 2 d S T P . .
H5A H 0.558851 0.641275 0.237958 0.026 Uiso 0.5 1 calc R U P . .
H5B H 0.641273 0.558848 0.262042 0.026 Uiso 0.5 1 calc R U P . .
CL1 Cl 0.666667 0.333333 0.45903(8) 0.0235(3) Uani 1 3 d S T P . .
O2 O 0.666667 0.333333 0.5266(10) 0.154(14) Uani 0.500(0) 3 d S T P . .
O3 O 0.666667 0.333333 0.3942(11) 0.20(2) Uani 0.500(0) 3 d S T P . .
O1A O 0.5378(17) 0.254(2) 0.4815(13) 0.180(12) Uani 0.500(0) 1 d . . P . .
O1B O 0.5359(13) 0.2359(13) 0.4363(10) 0.119(9) Uani 0.500(0) 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
FE N4 2.026(3) 9_556 ?
FE N4 2.026(3) 3 ?
FE N4 2.026(3) . ?
FE N4 2.026(3) 7_556 ?
FE N4 2.026(3) 2 ?
FE N4 2.026(3) 8_556 ?
N1 C1 1.327(5) . ?
N1 N2 1.361(5) . ?
N1 C2 1.456(5) . ?
N2 N3 1.290(5) . ?
N3 N4 1.361(5) . ?
N4 C1 1.319(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.505(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.544(6) . ?
C3 C4 1.549(5) 4 ?
C3 C4 1.554(5) . ?
C3 C3 1.856(8) 4 ?
C4 C3 1.549(5) 4 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C3 1.544(6) 4 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
CL1 O3 1.26(2) . ?
CL1 O2 1.31(2) . ?
CL1 O1A 1.324(13) 2_655 ?
CL1 O1A 1.324(13) 3_665 ?
CL1 O1A 1.324(13) . ?
CL1 O1B 1.379(9) 2_655 ?
CL1 O1B 1.379(9) . ?
CL1 O1B 1.379(9) 3_665 ?
O2 O1A 1.53(2) 2_655 ?
O2 O1A 1.53(2) 3_665 ?
O2 O1A 1.53(2) . ?
O3 O1B 1.54(2) 2_655 ?
O3 O1B 1.54(2) 3_665 ?
O3 O1B 1.54(2) . ?
O1A O1B 0.90(3) . ?

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
N4 FE N4 180.00(15) 9_556 3 ?
N4 FE N4 88.73(13) 9_556 . ?
N4 FE N4 91.27(13) 3 . ?
N4 FE N4 91.27(13) 9_556 7_556 ?
N4 FE N4 88.73(13) 3 7_556 ?
N4 FE N4 180.0 . 7_556 ?
N4 FE N4 88.73(13) 9_556 2 ?
N4 FE N4 91.27(13) 3 2 ?
N4 FE N4 91.27(13) . 2 ?
N4 FE N4 88.73(13) 7_556 2 ?
N4 FE N4 91.27(13) 9_556 8_556 ?
N4 FE N4 88.73(13) 3 8_556 ?
N4 FE N4 88.73(13) . 8_556 ?
N4 FE N4 91.27(13) 7_556 8_556 ?
N4 FE N4 180.00(14) 2 8_556 ?
C1 N1 N2 108.3(4) . . ?
C1 N1 C2 130.2(4) . . ?
N2 N1 C2 121.4(4) . . ?
N3 N2 N1 106.9(3) . . ?
N2 N3 N4 109.7(3) . . ?
C1 N4 N3 106.9(3) . . ?
C1 N4 FE 131.1(3) . . ?
N3 N4 FE 121.6(2) . . ?
N4 C1 N1 108.2(4) . . ?
N4 C1 H1 125.9 . . ?
N1 C1 H1 125.9 . . ?
N1 C2 C3 110.6(3) . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C5 127.1(3) . . ?
C2 C3 C4 127.4(4) . 4 ?
C5 C3 C4 88.0(3) . 4 ?
C2 C3 C4 125.9(3) . . ?
C5 C3 C4 87.8(3) . . ?
C4 C3 C4 87.6(3) 4 . ?
C2 C3 C3 179.0(4) . 4 ?
C5 C3 C3 53.04(19) . 4 ?
C4 C3 C3 53.4(2) 4 4 ?
C4 C3 C3 53.1(2) . 4 ?
C3 C4 C3 73.5(3) 4 . ?
C3 C4 H4A 116.2 4 . ?
C3 C4 H4A 116.2 . . ?
C3 C4 H4B 116.2 4 . ?
C3 C4 H4B 116.2 . . ?
H4A C4 H4B 113.2 . . ?
C3 C5 C3 73.9(4) 4 . ?
C3 C5 H5A 116.1 4 . ?
C3 C5 H5A 116.1 . . ?
C3 C5 H5B 116.1 4 . ?
C3 C5 H5B 116.1 . . ?
H5A C5 H5B 113.1 . . ?
O3 CL1 O2 180.0 . . ?
O3 CL1 O1A 109.2(11) . 2_655 ?
O2 CL1 O1A 70.8(11) . 2_655 ?
O3 CL1 O1A 109.2(11) . 3_665 ?
O2 CL1 O1A 70.8(11) . 3_665 ?
O1A CL1 O1A 109.7(11) 2_655 3_665 ?
O3 CL1 O1A 109.2(11) . . ?
O2 CL1 O1A 70.8(11) . . ?
O1A CL1 O1A 109.7(11) 2_655 . ?
O1A CL1 O1A 109.7(11) 3_665 . ?
O3 CL1 O1B 71.3(9) . 2_655 ?
O2 CL1 O1B 108.7(9) . 2_655 ?
O1A CL1 O1B 38.7(13) 2_655 2_655 ?
O1A CL1 O1B 116.0(14) 3_665 2_655 ?
O1A CL1 O1B 131.2(15) . 2_655 ?
O3 CL1 O1B 71.3(9) . . ?
O2 CL1 O1B 108.7(9) . . ?
O1A CL1 O1B 116.0(14) 2_655 . ?
O1A CL1 O1B 131.2(15) 3_665 . ?
O1A CL1 O1B 38.7(13) . . ?
O1B CL1 O1B 110.3(9) 2_655 . ?
O3 CL1 O1B 71.3(9) . 3_665 ?
O2 CL1 O1B 108.7(9) . 3_665 ?
O1A CL1 O1B 131.2(15) 2_655 3_665 ?
O1A CL1 O1B 38.7(13) 3_665 3_665 ?
O1A CL1 O1B 116.0(14) . 3_665 ?
O1B CL1 O1B 110.3(9) 2_655 3_665 ?
O1B CL1 O1B 110.3(9) . 3_665 ?
CL1 O2 O1A 55.0(8) . 2_655 ?
CL1 O2 O1A 55.0(8) . 3_665 ?
O1A O2 O1A 90.3(12) 2_655 3_665 ?
CL1 O2 O1A 55.0(8) . . ?
O1A O2 O1A 90.3(12) 2_655 . ?
O1A O2 O1A 90.3(12) 3_665 . ?
CL1 O3 O1B 58.0(8) . 2_655 ?
CL1 O3 O1B 58.0(8) . 3_665 ?
O1B O3 O1B 94.5(11) 2_655 3_665 ?
CL1 O3 O1B 58.0(8) . . ?
O1B O3 O1B 94.5(11) 2_655 . ?
O1B O3 O1B 94.5(11) 3_665 . ?
O1B O1A CL1 74.0(14) . . ?
O1B O1A O2 126.9(19) . . ?
CL1 O1A O2 54.2(10) . . ?
O1A O1B CL1 67.3(12) . . ?
O1A O1B O3 116.9(18) . . ?
CL1 O1B O3 50.7(9) . . ?

_refine_diff_density_max         0.557
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.121



####################################################################### 
# 
# 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_tu62_100k_sq
_database_code_depnum_ccdc_archive 'CCDC 1564874'
_audit_update_record             
;
2017-07-26 deposited with the CCDC.
2018-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4.50 H6 B0.33 F1.33 Fe0.17 N4'
_chemical_formula_weight         154.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   11.1171(16)
_cell_length_b                   11.1171(16)
_cell_length_c                   19.268(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2062.3(7)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_F_000             948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.458
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6755
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21198
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.665
_diffrn_reflns_theta_max         28.317
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1722
_reflns_number_gt                1271
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0332P)²+3.8643P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1722
_refine_ls_number_parameters     109
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.1276
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
FE1 Fe 0.000000 0.000000 0.500000 0.0150(2) Uani 1 6 d S T P . .
N1 N 0.2790(3) 0.3582(2) 0.39637(12) 0.0234(5) Uani 1 1 d . . . . .
N2 N 0.1568(2) 0.3536(3) 0.38265(13) 0.0276(6) Uani 1 1 d . . . . .
N3 N 0.0603(3) 0.2405(3) 0.40925(13) 0.0260(6) Uani 1 1 d . . . . .
N4 N 0.1165(2) 0.1698(2) 0.44116(12) 0.0203(5) Uani 1 1 d . . . . .
C1 C 0.2525(3) 0.2450(3) 0.43192(15) 0.0221(6) Uani 1 1 d . . . . .
H1 H 0.319383 0.222093 0.447888 0.026 Uiso 1 1 calc R U . . .
C2 C 0.4116(3) 0.4747(3) 0.37252(16) 0.0277(7) Uani 1 1 d . . . . .
H2A H 0.488837 0.478390 0.399813 0.033 Uiso 1 1 calc R U . . .
H2B H 0.412078 0.563141 0.379457 0.033 Uiso 1 1 calc R U . . .
C3 C 0.4311(3) 0.4560(3) 0.29691(15) 0.0204(6) Uani 1 1 d . . . . .
C4 C 0.4413(3) 0.3339(3) 0.26446(15) 0.0238(6) Uani 1 1 d . . . . .
H4A H 0.355194 0.242138 0.265276 0.029 Uiso 1 1 calc R U . . .
H4B H 0.525341 0.328923 0.276318 0.029 Uiso 1 1 calc R U . . .
C5 C 0.5548(3) 0.5548(3) 0.250000 0.0234(9) Uani 1 2 d S T P . .
H5A H 0.645382 0.562459 0.260985 0.028 Uiso 0.5 1 calc R U P . .
H5B H 0.562458 0.645381 0.239015 0.028 Uiso 0.5 1 calc R U P . .
B1 B 0.666667 0.333333 0.4605(3) 0.0265(12) Uani 1 3 d S T P . .
F2 F 0.666667 0.333333 0.5304(5) 0.119(5) Uani 0.500(0) 3 d S T P . .
F3 F 0.666667 0.333333 0.3917(4) 0.116(5) Uani 0.500(0) 3 d S T P . .
F1A F 0.5377(6) 0.2753(8) 0.4853(4) 0.091(2) Uani 0.500(0) 1 d . . P . .
F1B F 0.5348(7) 0.2426(7) 0.4402(5) 0.100(3) Uani 0.500(0) 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
FE1 N4 2.021(2) 8_556 ?
FE1 N4 2.021(2) 2 ?
FE1 N4 2.021(2) 9_556 ?
FE1 N4 2.021(2) 3 ?
FE1 N4 2.021(2) 7_556 ?
FE1 N4 2.021(2) . ?
N1 C1 1.330(4) . ?
N1 N2 1.360(3) . ?
N1 C2 1.466(4) . ?
N2 N3 1.283(3) . ?
N3 N4 1.370(3) . ?
N4 C1 1.323(4) . ?
C2 C3 1.503(4) . ?
C3 C4 1.549(4) . ?
C3 C5 1.550(4) . ?
C3 C4 1.555(4) 4 ?
C3 C3 1.870(6) 4 ?
C4 C3 1.555(4) 4 ?
C5 C3 1.550(4) 4 ?
B1 F3 1.326(9) . ?
B1 F1A 1.333(6) . ?
B1 F1A 1.333(6) 2_655 ?
B1 F1A 1.333(6) 3_665 ?
B1 F2 1.348(11) . ?
B1 F1B 1.356(6) 2_655 ?
B1 F1B 1.356(6) . ?
B1 F1B 1.356(6) 3_665 ?
F2 F1A 1.517(9) . ?
F2 F1A 1.517(9) 2_655 ?
F2 F1A 1.517(9) 3_665 ?
F3 F1B 1.601(10) 2_655 ?
F3 F1B 1.601(10) 3_665 ?
F3 F1B 1.601(10) . ?
F1A F1B 0.936(9) . ?

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
N4 FE1 N4 180.00(9) 8_556 2 ?
N4 FE1 N4 91.59(9) 8_556 9_556 ?
N4 FE1 N4 88.41(9) 2 9_556 ?
N4 FE1 N4 88.41(9) 8_556 3 ?
N4 FE1 N4 91.59(9) 2 3 ?
N4 FE1 N4 180.00(11) 9_556 3 ?
N4 FE1 N4 91.59(9) 8_556 7_556 ?
N4 FE1 N4 88.41(9) 2 7_556 ?
N4 FE1 N4 91.59(9) 9_556 7_556 ?
N4 FE1 N4 88.41(9) 3 7_556 ?
N4 FE1 N4 88.41(9) 8_556 . ?
N4 FE1 N4 91.59(9) 2 . ?
N4 FE1 N4 88.41(9) 9_556 . ?
N4 FE1 N4 91.59(9) 3 . ?
N4 FE1 N4 180.0 7_556 . ?
C1 N1 N2 108.6(2) . . ?
C1 N1 C2 130.3(3) . . ?
N2 N1 C2 121.1(2) . . ?
N3 N2 N1 106.8(2) . . ?
N2 N3 N4 110.1(2) . . ?
C1 N4 N3 106.4(2) . . ?
C1 N4 FE1 131.44(19) . . ?
N3 N4 FE1 121.62(17) . . ?
N4 C1 N1 108.1(2) . . ?
N1 C2 C3 109.4(2) . . ?
C2 C3 C4 126.2(2) . . ?
C2 C3 C5 127.3(2) . . ?
C4 C3 C5 87.61(19) . . ?
C2 C3 C4 127.7(2) . 4 ?
C4 C3 C4 87.3(2) . 4 ?
C5 C3 C4 87.43(19) . 4 ?
C2 C3 C3 179.3(3) . 4 ?
C4 C3 C3 53.08(17) . 4 ?
C5 C3 C3 52.91(13) . 4 ?
C4 C3 C3 52.83(16) 4 4 ?
C3 C4 C3 74.1(2) . 4 ?
C3 C5 C3 74.2(3) . 4 ?
F3 B1 F1A 111.1(4) . . ?
F3 B1 F1A 111.1(4) . 2_655 ?
F1A B1 F1A 107.8(4) . 2_655 ?
F3 B1 F1A 111.1(4) . 3_665 ?
F1A B1 F1A 107.8(4) . 3_665 ?
F1A B1 F1A 107.8(4) 2_655 3_665 ?
F3 B1 F2 180.0 . . ?
F1A B1 F2 68.9(4) . . ?
F1A B1 F2 68.9(4) 2_655 . ?
F1A B1 F2 68.9(4) 3_665 . ?
F3 B1 F1B 73.3(5) . 2_655 ?
F1A B1 F1B 137.9(5) . 2_655 ?
F1A B1 F1B 40.7(4) 2_655 2_655 ?
F1A B1 F1B 109.0(6) 3_665 2_655 ?
F2 B1 F1B 106.7(5) . 2_655 ?
F3 B1 F1B 73.3(5) . . ?
F1A B1 F1B 40.7(4) . . ?
F1A B1 F1B 109.0(6) 2_655 . ?
F1A B1 F1B 137.9(5) 3_665 . ?
F2 B1 F1B 106.7(5) . . ?
F1B B1 F1B 112.1(4) 2_655 . ?
F3 B1 F1B 73.3(5) . 3_665 ?
F1A B1 F1B 109.0(6) . 3_665 ?
F1A B1 F1B 137.9(5) 2_655 3_665 ?
F1A B1 F1B 40.7(4) 3_665 3_665 ?
F2 B1 F1B 106.7(5) . 3_665 ?
F1B B1 F1B 112.1(4) 2_655 3_665 ?
F1B B1 F1B 112.1(4) . 3_665 ?
B1 F2 F1A 55.1(4) . . ?
B1 F2 F1A 55.1(4) . 2_655 ?
F1A F2 F1A 90.4(5) . 2_655 ?
B1 F2 F1A 55.1(4) . 3_665 ?
F1A F2 F1A 90.4(5) . 3_665 ?
F1A F2 F1A 90.4(5) 2_655 3_665 ?
B1 F3 F1B 54.2(3) . 2_655 ?
B1 F3 F1B 54.2(3) . 3_665 ?
F1B F3 F1B 89.3(4) 2_655 3_665 ?
B1 F3 F1B 54.2(3) . . ?
F1B F3 F1B 89.3(4) 2_655 . ?
F1B F3 F1B 89.3(4) 3_665 . ?
F1B F1A B1 71.0(7) . . ?
F1B F1A F2 122.6(9) . . ?
B1 F1A F2 56.0(5) . . ?
F1A F1B B1 68.3(6) . . ?
F1A F1B F3 117.1(8) . . ?
B1 F1B F3 52.5(5) . . ?

_refine_diff_density_max         0.379
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.073



####################################################################### 
# 
# 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_tu65_250k_sq
_database_code_depnum_ccdc_archive 'CCDC 1564875'
_audit_update_record             
;
2017-07-26 deposited with the CCDC.
2018-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H36 Cl2 Fe N24 O8'
_chemical_formula_weight         951.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   11.2861(3)
_cell_length_b                   11.2861(3)
_cell_length_c                   19.6585(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2168.55(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_F_000             980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.545
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6916
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51862
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.611
_diffrn_reflns_theta_max         30.531
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2219
_reflns_number_gt                1792
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0631P)²+1.2790P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2219
_refine_ls_number_parameters     108
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1301
_refine_ls_wR_factor_gt          0.1211
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
FE Fe 0.000000 0.000000 0.500000 0.02460(15) Uani 1 6 d S T P . .
N1 N 0.28229(16) 0.36562(15) 0.39355(8) 0.0351(3) Uani 1 1 d . . . . .
N2 N 0.16272(19) 0.35925(18) 0.38003(10) 0.0474(4) Uani 1 1 d . . . . .
N3 N 0.06810(18) 0.24813(18) 0.40670(9) 0.0436(4) Uani 1 1 d . . . . .
N4 N 0.12383(15) 0.18039(15) 0.43781(7) 0.0322(3) Uani 1 1 d . . . . .
C1 C 0.25725(19) 0.25583(19) 0.42856(9) 0.0369(4) Uani 1 1 d . . . . .
H1 H 0.323266 0.234808 0.444286 0.044 Uiso 1 1 calc R U . . .
C2 C 0.4121(2) 0.47967(18) 0.36879(10) 0.0432(5) Uani 1 1 d . . . . .
H2A H 0.487962 0.485683 0.395742 0.052 Uiso 1 1 calc R U . . .
H2B H 0.411586 0.565745 0.374135 0.052 Uiso 1 1 calc R U . . .
C3 C 0.43226(17) 0.45882(16) 0.29536(9) 0.0316(3) Uani 1 1 d . . . . .
C4 C 0.4430(2) 0.33814(18) 0.26537(10) 0.0386(4) Uani 1 1 d . . . . .
H4A H 0.359124 0.248688 0.266221 0.046 Uiso 1 1 calc R U . . .
H4B H 0.524792 0.333722 0.277889 0.046 Uiso 1 1 calc R U . . .
C5 C 0.5551(2) 0.5551(2) 0.250000 0.0368(5) Uani 1 2 d S T P . .
H5A H 0.643086 0.562746 0.261625 0.044 Uiso 0.5 1 calc R U P . .
H5B H 0.562749 0.643087 0.238376 0.044 Uiso 0.5 1 calc R U P . .
CL Cl 0.666667 0.333333 0.45933(5) 0.0490(2) Uani 1 3 d S T P . .
O2 O 0.666667 0.333333 0.5251(7) 0.217(10) Uani 0.500(0) 3 d S T P . .
O3 O 0.666667 0.333333 0.3944(5) 0.200(9) Uani 0.500(0) 3 d S T P . .
O1A O 0.5445(8) 0.2843(14) 0.4894(5) 0.201(6) Uani 0.500(0) 1 d . . P . .
O1B O 0.5371(8) 0.2398(8) 0.4354(5) 0.160(4) Uani 0.500(0) 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
FE N4 2.1788(14) 8_556 ?
FE N4 2.1788(14) 2 ?
FE N4 2.1788(14) 9_556 ?
FE N4 2.1788(14) 3 ?
FE N4 2.1788(14) 7_556 ?
FE N4 2.1788(14) . ?
N1 C1 1.319(2) . ?
N1 N2 1.342(2) . ?
N1 C2 1.468(2) . ?
N2 N3 1.284(2) . ?
N3 N4 1.355(2) . ?
N4 C1 1.320(2) . ?
C1 H1 0.9400 . ?
C2 C3 1.498(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 C4 1.544(2) . ?
C3 C5 1.546(2) . ?
C3 C4 1.548(2) 4 ?
C3 C3 1.858(3) 4 ?
C4 C3 1.548(3) 4 ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 C3 1.546(2) 4 ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
CL O3 1.276(10) . ?
CL O2 1.293(13) . ?
CL O1A 1.339(7) . ?
CL O1A 1.339(7) 2_655 ?
CL O1A 1.339(7) 3_665 ?
CL O1B 1.389(6) 2_655 ?
CL O1B 1.389(6) . ?
CL O1B 1.389(6) 3_665 ?
O2 O1A 1.392(10) . ?
O2 O1A 1.392(10) 2_655 ?
O2 O1A 1.392(10) 3_665 ?
O3 O1B 1.535(11) 2_655 ?
O3 O1B 1.535(11) . ?
O3 O1B 1.535(11) 3_665 ?
O1A O1B 1.160(11) . ?

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
N4 FE N4 180.0 8_556 2 ?
N4 FE N4 91.59(6) 8_556 9_556 ?
N4 FE N4 88.41(6) 2 9_556 ?
N4 FE N4 88.41(6) 8_556 3 ?
N4 FE N4 91.59(6) 2 3 ?
N4 FE N4 180.00(6) 9_556 3 ?
N4 FE N4 91.59(6) 8_556 7_556 ?
N4 FE N4 88.41(6) 2 7_556 ?
N4 FE N4 91.59(6) 9_556 7_556 ?
N4 FE N4 88.41(6) 3 7_556 ?
N4 FE N4 88.41(6) 8_556 . ?
N4 FE N4 91.59(6) 2 . ?
N4 FE N4 88.41(6) 9_556 . ?
N4 FE N4 91.59(6) 3 . ?
N4 FE N4 180.0 7_556 . ?
C1 N1 N2 108.41(15) . . ?
C1 N1 C2 130.41(18) . . ?
N2 N1 C2 121.16(16) . . ?
N3 N2 N1 107.12(15) . . ?
N2 N3 N4 109.97(16) . . ?
C1 N4 N3 105.99(14) . . ?
C1 N4 FE 132.20(12) . . ?
N3 N4 FE 121.25(12) . . ?
N1 C1 N4 108.50(16) . . ?
N1 C1 H1 125.7 . . ?
N4 C1 H1 125.7 . . ?
N1 C2 C3 110.20(15) . . ?
N1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C4 126.29(16) . . ?
C2 C3 C5 126.77(14) . . ?
C4 C3 C5 87.78(12) . . ?
C2 C3 C4 127.71(16) . 4 ?
C4 C3 C4 87.49(15) . 4 ?
C5 C3 C4 87.63(12) . 4 ?
C2 C3 C3 179.3(2) . 4 ?
C4 C3 C3 53.18(11) . 4 ?
C5 C3 C3 53.08(8) . 4 ?
C4 C3 C3 52.97(10) 4 4 ?
C3 C4 C3 73.86(14) . 4 ?
C3 C4 H4A 116.1 . . ?
C3 C4 H4A 116.1 4 . ?
C3 C4 H4B 116.1 . . ?
C3 C4 H4B 116.1 4 . ?
H4A C4 H4B 113.1 . . ?
C3 C5 C3 73.84(17) . 4 ?
C3 C5 H5A 116.1 . . ?
C3 C5 H5A 116.1 4 . ?
C3 C5 H5B 116.1 . . ?
C3 C5 H5B 116.1 4 . ?
H5A C5 H5B 113.1 . . ?
O3 CL O2 180.0 . . ?
O3 CL O1A 116.2(4) . . ?
O2 CL O1A 63.8(4) . . ?
O3 CL O1A 116.2(4) . 2_655 ?
O2 CL O1A 63.8(4) . 2_655 ?
O1A CL O1A 102.0(5) . 2_655 ?
O3 CL O1A 116.2(4) . 3_665 ?
O2 CL O1A 63.8(4) . 3_665 ?
O1A CL O1A 102.0(5) . 3_665 ?
O1A CL O1A 102.0(5) 2_655 3_665 ?
O3 CL O1B 70.2(5) . 2_655 ?
O2 CL O1B 109.8(5) . 2_655 ?
O1A CL O1B 143.6(7) . 2_655 ?
O1A CL O1B 50.3(5) 2_655 2_655 ?
O1A CL O1B 106.5(8) 3_665 2_655 ?
O3 CL O1B 70.2(5) . . ?
O2 CL O1B 109.8(5) . . ?
O1A CL O1B 50.3(5) . . ?
O1A CL O1B 106.5(8) 2_655 . ?
O1A CL O1B 143.6(7) 3_665 . ?
O1B CL O1B 109.1(5) 2_655 . ?
O3 CL O1B 70.2(5) . 3_665 ?
O2 CL O1B 109.8(5) . 3_665 ?
O1A CL O1B 106.5(8) . 3_665 ?
O1A CL O1B 143.6(7) 2_655 3_665 ?
O1A CL O1B 50.3(5) 3_665 3_665 ?
O1B CL O1B 109.1(5) 2_655 3_665 ?
O1B CL O1B 109.1(5) . 3_665 ?
CL O2 O1A 59.7(5) . . ?
CL O2 O1A 59.7(5) . 2_655 ?
O1A O2 O1A 96.8(7) . 2_655 ?
CL O2 O1A 59.7(5) . 3_665 ?
O1A O2 O1A 96.8(7) . 3_665 ?
O1A O2 O1A 96.8(7) 2_655 3_665 ?
CL O3 O1B 58.4(4) . 2_655 ?
CL O3 O1B 58.4(4) . . ?
O1B O3 O1B 95.0(6) 2_655 . ?
CL O3 O1B 58.4(4) . 3_665 ?
O1B O3 O1B 95.0(6) 2_655 3_665 ?
O1B O3 O1B 95.0(6) . 3_665 ?
O1B O1A CL 67.1(6) . . ?
O1B O1A O2 118.5(10) . . ?
CL O1A O2 56.5(6) . . ?
O1A O1B CL 62.6(5) . . ?
O1A O1B O3 110.2(8) . . ?
CL O1B O3 51.4(5) . . ?

_refine_diff_density_max         0.405
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.056



