# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_kaz11_tccl6caf_lt_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2298414'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Tc, 2(C8 H11 N4 O2)'
_chemical_formula_sum            'C16 H22 Cl6 N8 O4 Tc'
_chemical_formula_weight         701.11
_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'
Cl Cl 0.1484 0.1585 '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'
Tc Tc -1.4390 0.7593 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.898(3)
_cell_length_b                   8.106(3)
_cell_length_c                   10.452(4)
_cell_angle_alpha                96.572(16)
_cell_angle_beta                 91.809(15)
_cell_angle_gamma                112.382(14)
_cell_volume                     612.7(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.429
_cell_measurement_theta_min      3.068
_shelx_estimated_absorpt_T_max   0.939
_shelx_estimated_absorpt_T_min   0.882
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1012 before and 0.0832 after correction.
The Ratio of minimum to maximum transmission is 0.6862.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             351
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_unetI/netI     0.1230
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10321
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         4.482
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_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                2453
_reflns_number_total             3569
_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 V8.40B (Bruker, 2020)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.213
_refine_diff_density_min         -2.617
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3569
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0585
_refine_ls_restrained_S_all      0.969
_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)+(0.0619P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1417
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C8(H8)
1.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C)
;
_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
Tc1 Tc 1.000000 1.000000 0.500000 0.01345(15) Uani 1 2 d S . P . .
Cl3 Cl 1.04968(14) 0.98737(15) 0.28042(10) 0.0191(3) Uani 1 1 d . . . . .
Cl2 Cl 0.69412(13) 0.96079(15) 0.44895(11) 0.0196(3) Uani 1 1 d . . . . .
Cl1 Cl 0.90544(14) 0.68329(14) 0.48369(11) 0.0195(3) Uani 1 1 d . . . . .
O1 O 0.5416(4) 0.1194(5) 0.8696(3) 0.0255(8) Uani 1 1 d . . . . .
O2 O 0.1532(4) 0.4060(5) 0.9675(3) 0.0265(8) Uani 1 1 d . . . . .
N3 N 0.5787(5) 0.3641(5) 0.7715(4) 0.0171(8) Uani 1 1 d . . . . .
N1 N 0.3503(5) 0.2657(5) 0.9203(4) 0.0180(8) Uani 1 1 d . . . . .
N9 N 0.5684(5) 0.6196(5) 0.6716(4) 0.0191(8) Uani 1 1 d . . . . .
H9 H 0.643(7) 0.622(7) 0.615(5) 0.023 Uiso 1 1 d . U . . .
N7 N 0.3419(5) 0.6520(5) 0.7692(4) 0.0187(8) Uani 1 1 d . . . . .
C4 C 0.5121(5) 0.4890(6) 0.7507(4) 0.0171(9) Uani 1 1 d . . . . .
C2 C 0.4932(6) 0.2394(6) 0.8538(5) 0.0185(10) Uani 1 1 d . . . . .
C6 C 0.2775(6) 0.3947(6) 0.9055(4) 0.0190(10) Uani 1 1 d . . . . .
C5 C 0.3697(5) 0.5089(6) 0.8117(4) 0.0171(9) Uani 1 1 d . . . . .
C8 C 0.4652(6) 0.7172(6) 0.6843(4) 0.0201(10) Uani 1 1 d . . . . .
H8 H 0.477383 0.816792 0.640211 0.024 Uiso 1 1 calc R U . . .
C11 C 0.7346(6) 0.3451(6) 0.7072(5) 0.0222(10) Uani 1 1 d . . . . .
H11A H 0.795084 0.450198 0.663160 0.033 Uiso 1 1 calc R U . . .
H11B H 0.689975 0.235779 0.643897 0.033 Uiso 1 1 calc R U . . .
H11C H 0.822545 0.336552 0.771794 0.033 Uiso 1 1 calc R U . . .
C12 C 0.2024(6) 0.7223(6) 0.8095(6) 0.0275(12) Uani 1 1 d . . . . .
H12A H 0.198385 0.809849 0.753368 0.041 Uiso 1 1 calc R U . . .
H12B H 0.234148 0.781079 0.899170 0.041 Uiso 1 1 calc R U . . .
H12C H 0.081877 0.622707 0.802787 0.041 Uiso 1 1 calc R U . . .
C10 C 0.2644(6) 0.1380(6) 1.0103(5) 0.0223(10) Uani 1 1 d . . . . .
H10A H 0.226534 0.199456 1.083303 0.033 Uiso 1 1 calc R U . . .
H10B H 0.352679 0.090875 1.042090 0.033 Uiso 1 1 calc R U . . .
H10C H 0.156509 0.038377 0.965719 0.033 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 Cl3 2.3380(14) . ?
Tc1 Cl3 2.3380(14) 2_776 ?
Tc1 Cl2 2.3490(14) 2_776 ?
Tc1 Cl2 2.3490(14) . ?
Tc1 Cl1 2.3684(14) . ?
Tc1 Cl1 2.3684(14) 2_776 ?
O1 C2 1.199(6) . ?
O2 C6 1.219(5) . ?
N3 C4 1.341(6) . ?
N3 C2 1.390(5) . ?
N3 C11 1.471(6) . ?
N1 C2 1.415(6) . ?
N1 C6 1.391(6) . ?
N1 C10 1.465(5) . ?
N9 H9 0.84(5) . ?
N9 C4 1.367(5) . ?
N9 C8 1.335(6) . ?
N7 C5 1.377(6) . ?
N7 C8 1.336(6) . ?
N7 C12 1.473(6) . ?
C4 C5 1.363(6) . ?
C6 C5 1.445(6) . ?
C8 H8 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

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
Cl3 Tc1 Cl3 180.0 . 2_776 ?
Cl3 Tc1 Cl2 90.04(4) 2_776 . ?
Cl3 Tc1 Cl2 89.96(4) . . ?
Cl3 Tc1 Cl2 89.96(4) 2_776 2_776 ?
Cl3 Tc1 Cl2 90.04(4) . 2_776 ?
Cl3 Tc1 Cl1 89.87(4) 2_776 . ?
Cl3 Tc1 Cl1 90.13(4) . . ?
Cl3 Tc1 Cl1 89.87(4) . 2_776 ?
Cl3 Tc1 Cl1 90.13(4) 2_776 2_776 ?
Cl2 Tc1 Cl2 180.00(6) 2_776 . ?
Cl2 Tc1 Cl1 90.73(4) 2_776 . ?
Cl2 Tc1 Cl1 89.27(4) . . ?
Cl2 Tc1 Cl1 90.73(4) . 2_776 ?
Cl2 Tc1 Cl1 89.27(4) 2_776 2_776 ?
Cl1 Tc1 Cl1 180.0 . 2_776 ?
C4 N3 C2 119.3(4) . . ?
C4 N3 C11 123.6(4) . . ?
C2 N3 C11 117.1(4) . . ?
C2 N1 C10 116.3(4) . . ?
C6 N1 C2 127.1(4) . . ?
C6 N1 C10 116.5(4) . . ?
C4 N9 H9 123(4) . . ?
C8 N9 H9 127(4) . . ?
C8 N9 C4 109.0(4) . . ?
C5 N7 C12 126.6(4) . . ?
C8 N7 C5 107.7(4) . . ?
C8 N7 C12 125.6(4) . . ?
N3 C4 N9 129.7(4) . . ?
N3 C4 C5 123.8(4) . . ?
C5 C4 N9 106.5(4) . . ?
O1 C2 N3 121.6(4) . . ?
O1 C2 N1 122.2(4) . . ?
N3 C2 N1 116.3(4) . . ?
O2 C6 N1 122.1(4) . . ?
O2 C6 C5 126.5(5) . . ?
N1 C6 C5 111.4(4) . . ?
N7 C5 C6 130.3(4) . . ?
C4 C5 N7 107.8(4) . . ?
C4 C5 C6 121.9(4) . . ?
N9 C8 N7 108.9(4) . . ?
N9 C8 H8 125.6 . . ?
N7 C8 H8 125.6 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N7 C12 H12A 109.5 . . ?
N7 C12 H12B 109.5 . . ?
N7 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N9 H9 Cl1 0.84(5) 2.45(5) 3.275(4) 168(5) . yes
C10 H10B O1 0.98 2.42 3.345(6) 157.6 2_657 yes

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
O2 C6 C5 N7 -0.5(8) . . . . ?
O2 C6 C5 C4 177.6(4) . . . . ?
N3 C4 C5 N7 178.6(4) . . . . ?
N3 C4 C5 C6 0.1(7) . . . . ?
N1 C6 C5 N7 -179.6(4) . . . . ?
N1 C6 C5 C4 -1.5(6) . . . . ?
N9 C4 C5 N7 -0.3(5) . . . . ?
N9 C4 C5 C6 -178.8(4) . . . . ?
C4 N3 C2 O1 175.8(4) . . . . ?
C4 N3 C2 N1 -6.1(6) . . . . ?
C4 N9 C8 N7 -0.5(5) . . . . ?
C2 N3 C4 N9 -177.5(4) . . . . ?
C2 N3 C4 C5 3.9(6) . . . . ?
C2 N1 C6 O2 179.7(4) . . . . ?
C2 N1 C6 C5 -1.1(6) . . . . ?
C6 N1 C2 O1 -177.0(4) . . . . ?
C6 N1 C2 N3 4.9(6) . . . . ?
C5 N7 C8 N9 0.3(5) . . . . ?
C8 N9 C4 N3 -178.3(4) . . . . ?
C8 N9 C4 C5 0.5(5) . . . . ?
C8 N7 C5 C4 0.0(5) . . . . ?
C8 N7 C5 C6 178.3(4) . . . . ?
C11 N3 C4 N9 -0.3(7) . . . . ?
C11 N3 C4 C5 -178.9(4) . . . . ?
C11 N3 C2 O1 -1.5(6) . . . . ?
C11 N3 C2 N1 176.6(4) . . . . ?
C12 N7 C5 C4 -179.8(4) . . . . ?
C12 N7 C5 C6 -1.5(7) . . . . ?
C12 N7 C8 N9 -179.8(4) . . . . ?
C10 N1 C2 O1 0.2(6) . . . . ?
C10 N1 C2 N3 -178.0(4) . . . . ?
C10 N1 C6 O2 2.6(6) . . . . ?
C10 N1 C6 C5 -178.2(4) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_kaz11_tccl6caf_lt_0m_a 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 11 Note
RESPONSE: Closed by beamstop.
;
####################################################################### 
# 
# 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_kazetf6_lt_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2298415'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Tc, 2(C7 H6 N S), 2(H2 O)'
_chemical_formula_sum            'C14 H16 Cl6 N2 O2 S2 Tc'
_chemical_formula_weight         619.11
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.2136(5)
_cell_length_b                   8.0612(6)
_cell_length_c                   9.8742(7)
_cell_angle_alpha                98.062(3)
_cell_angle_beta                 100.830(3)
_cell_angle_gamma                92.071(3)
_cell_volume                     557.23(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3441
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.447
_cell_measurement_theta_min      2.557
_shelx_estimated_absorpt_T_max   0.940
_shelx_estimated_absorpt_T_min   0.822
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0582 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.8920.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             307
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11493
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         4.203
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2587
_reflns_number_total             3237
_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 V8.40B (Bruker, 2020)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3237
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0364
_refine_ls_restrained_S_all      1.023
_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)+(0.0408P)²+0.1154P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0827
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.02
 H1WA-H1WB
 1.35 with sigma of 0.02
 N3-H3
 0.88 with sigma of 0.05
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8)
;
_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
Tc1 Tc 1.000000 0.500000 0.500000 0.01855(9) Uani 1 2 d S . P . .
Cl1 Cl 0.70238(8) 0.48985(9) 0.34709(7) 0.02544(15) Uani 1 1 d . . . . .
Cl2 Cl 0.85440(9) 0.54714(9) 0.69506(7) 0.02500(15) Uani 1 1 d . . . . .
Cl3 Cl 1.03034(9) 0.78868(8) 0.50078(7) 0.02433(15) Uani 1 1 d . . . . .
S1 S 0.18659(9) -0.27386(9) 0.06958(8) 0.02623(16) Uani 1 1 d . . . . .
O1W O 0.4767(3) 0.2031(3) 0.4672(2) 0.0263(4) Uani 1 1 d D . . . .
H1WA H 0.380(3) 0.238(4) 0.481(4) 0.039 Uiso 1 1 d D U . . .
H1WB H 0.553(3) 0.268(4) 0.451(4) 0.039 Uiso 1 1 d D U . . .
N3 N 0.3279(3) -0.0107(3) 0.2314(2) 0.0228(5) Uani 1 1 d D . . . .
H3 H 0.367(4) 0.052(4) 0.302(3) 0.027 Uiso 1 1 d D U . . .
C2 C 0.2763(4) -0.1685(4) 0.2306(3) 0.0274(6) Uani 1 1 d . . . . .
H2 H 0.288291 -0.219013 0.312891 0.033 Uiso 1 1 calc R U . . .
C4 C 0.3003(3) 0.0397(3) 0.1008(3) 0.0186(5) Uani 1 1 d . . . . .
C5 C 0.3439(3) 0.1980(3) 0.0690(3) 0.0218(5) Uani 1 1 d . . . . .
H5 H 0.398984 0.287847 0.139762 0.026 Uiso 1 1 calc R U . . .
C6 C 0.3033(4) 0.2185(4) -0.0707(3) 0.0258(6) Uani 1 1 d . . . . .
H6 H 0.330335 0.324847 -0.096142 0.031 Uiso 1 1 calc R U . . .
C7 C 0.2234(4) 0.0860(4) -0.1743(3) 0.0270(6) Uani 1 1 d . . . . .
H7 H 0.197681 0.104648 -0.268706 0.032 Uiso 1 1 calc R U . . .
C8 C 0.1806(3) -0.0711(4) -0.1442(3) 0.0229(6) Uani 1 1 d . . . . .
H8 H 0.126350 -0.160582 -0.215505 0.027 Uiso 1 1 calc R U . . .
C9 C 0.2209(3) -0.0929(3) -0.0034(3) 0.0186(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
Tc1 Cl1 2.3728(6) . ?
Tc1 Cl1 2.3728(6) 2_766 ?
Tc1 Cl2 2.3539(6) 2_766 ?
Tc1 Cl2 2.3539(6) . ?
Tc1 Cl3 2.3283(7) . ?
Tc1 Cl3 2.3283(7) 2_766 ?
S1 C2 1.692(3) . ?
S1 C9 1.745(3) . ?
O1W H1WA 0.788(17) . ?
O1W H1WB 0.799(17) . ?
N3 H3 0.80(3) . ?
N3 C2 1.311(4) . ?
N3 C4 1.387(3) . ?
C2 H2 0.9500 . ?
C4 C5 1.395(4) . ?
C4 C9 1.398(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.396(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.378(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.403(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
Cl1 Tc1 Cl1 180.0 . 2_766 ?
Cl2 Tc1 Cl1 90.78(2) . . ?
Cl2 Tc1 Cl1 89.22(2) . 2_766 ?
Cl2 Tc1 Cl1 90.78(2) 2_766 2_766 ?
Cl2 Tc1 Cl1 89.22(2) 2_766 . ?
Cl2 Tc1 Cl2 180.0 . 2_766 ?
Cl3 Tc1 Cl1 89.30(2) . . ?
Cl3 Tc1 Cl1 90.70(2) 2_766 . ?
Cl3 Tc1 Cl1 89.30(2) 2_766 2_766 ?
Cl3 Tc1 Cl1 90.70(2) . 2_766 ?
Cl3 Tc1 Cl2 89.50(2) . . ?
Cl3 Tc1 Cl2 89.50(2) 2_766 2_766 ?
Cl3 Tc1 Cl2 90.50(2) 2_766 . ?
Cl3 Tc1 Cl2 90.50(2) . 2_766 ?
Cl3 Tc1 Cl3 180.0 . 2_766 ?
C2 S1 C9 90.27(14) . . ?
H1WA O1W H1WB 117(3) . . ?
C2 N3 H3 122(2) . . ?
C2 N3 C4 114.6(2) . . ?
C4 N3 H3 123(2) . . ?
S1 C2 H2 123.1 . . ?
N3 C2 S1 113.8(2) . . ?
N3 C2 H2 123.1 . . ?
N3 C4 C5 127.5(2) . . ?
N3 C4 C9 111.0(2) . . ?
C5 C4 C9 121.5(2) . . ?
C4 C5 H5 121.5 . . ?
C6 C5 C4 117.0(3) . . ?
C6 C5 H5 121.5 . . ?
C5 C6 H6 119.4 . . ?
C5 C6 C7 121.3(3) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 H7 118.9 . . ?
C8 C7 C6 122.2(3) . . ?
C8 C7 H7 118.9 . . ?
C7 C8 H8 121.5 . . ?
C7 C8 C9 116.9(3) . . ?
C9 C8 H8 121.5 . . ?
C4 C9 S1 110.29(19) . . ?
C4 C9 C8 121.1(3) . . ?
C8 C9 S1 128.6(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1WB Cl1 0.799(17) 2.49(2) 3.259(2) 162(3) . yes
N3 H3 O1W 0.80(3) 1.91(3) 2.711(3) 176(3) . yes

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
N3 C4 C5 C6 179.9(2) . . . . ?
N3 C4 C9 S1 -0.3(2) . . . . ?
N3 C4 C9 C8 -179.9(2) . . . . ?
C2 S1 C9 C4 0.07(18) . . . . ?
C2 S1 C9 C8 179.7(2) . . . . ?
C2 N3 C4 C5 -179.0(2) . . . . ?
C2 N3 C4 C9 0.4(3) . . . . ?
C4 N3 C2 S1 -0.4(3) . . . . ?
C4 C5 C6 C7 -0.4(4) . . . . ?
C5 C4 C9 S1 179.15(18) . . . . ?
C5 C4 C9 C8 -0.5(3) . . . . ?
C5 C6 C7 C8 0.1(4) . . . . ?
C6 C7 C8 C9 0.0(4) . . . . ?
C7 C8 C9 S1 -179.41(19) . . . . ?
C7 C8 C9 C4 0.2(3) . . . . ?
C9 S1 C2 N3 0.2(2) . . . . ?
C9 C4 C5 C6 0.6(3) . . . . ?

_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_deatccl6_lt_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2298416'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Tc, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 Cl6 N2 Tc'
_chemical_formula_weight         458.99
_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'
Cl Cl 0.1484 0.1585 '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'
Tc Tc -1.4390 0.7593 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.8583(7)
_cell_length_b                   10.4340(8)
_cell_length_c                   9.6725(8)
_cell_angle_alpha                90
_cell_angle_beta                 92.915(3)
_cell_angle_gamma                90
_cell_volume                     892.85(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.986
_cell_measurement_theta_min      2.873
_shelx_estimated_absorpt_T_max   0.762
_shelx_estimated_absorpt_T_min   0.708
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0672 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.9062.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15015
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.199
_diffrn_reflns_theta_min         3.019
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2227
_reflns_number_total             2620
_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 V8.40B (Bruker, 2020)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2620
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0231
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0148P)²+0.0933P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0485
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_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
Tc1 Tc 0.500000 0.500000 0.500000 0.01090(6) Uani 1 2 d S . P . .
Cl1 Cl 0.34277(5) 0.60373(4) 0.65472(4) 0.01583(9) Uani 1 1 d . . . . .
Cl2 Cl 0.70822(5) 0.61889(4) 0.58911(4) 0.02066(10) Uani 1 1 d . . . . .
Cl3 Cl 0.44622(5) 0.66095(4) 0.33387(4) 0.02102(10) Uani 1 1 d . . . . .
N1 N 0.57536(17) 0.78857(14) 0.84625(15) 0.0155(3) Uani 1 1 d . . . . .
C3 C 0.4704(2) 0.89715(17) 0.80966(18) 0.0178(4) Uani 1 1 d . . . . .
C4 C 0.5129(3) 0.9580(2) 0.6758(2) 0.0251(4) Uani 1 1 d . . . . .
C1 C 0.5399(2) 0.71866(17) 0.97608(17) 0.0164(3) Uani 1 1 d . . . . .
C2 C 0.6489(2) 0.60872(18) 0.9993(2) 0.0207(4) Uani 1 1 d . . . . .
H1C H 0.5511(19) 0.7805(16) 1.0518(18) 0.011(4) Uiso 1 1 d . . . . .
H3A H 0.477(2) 0.9585(17) 0.8860(19) 0.013(5) Uiso 1 1 d . . . . .
H1A H 0.670(2) 0.8181(18) 0.857(2) 0.021(5) Uiso 1 1 d . . . . .
H4A H 0.447(3) 1.022(2) 0.650(2) 0.036(7) Uiso 1 1 d . . . . .
H3B H 0.372(2) 0.8675(17) 0.8016(19) 0.018(5) Uiso 1 1 d . . . . .
H2A H 0.639(2) 0.5510(18) 0.926(2) 0.017(5) Uiso 1 1 d . . . . .
H4B H 0.510(2) 0.8949(19) 0.602(2) 0.031(6) Uiso 1 1 d . . . . .
H4C H 0.610(3) 0.9915(19) 0.687(2) 0.038(7) Uiso 1 1 d . . . . .
H2B H 0.631(2) 0.5700(18) 1.086(2) 0.021(5) Uiso 1 1 d . . . . .
H2C H 0.750(2) 0.6394(16) 1.0023(19) 0.017(5) Uiso 1 1 d . . . . .
H1D H 0.436(2) 0.6913(17) 0.9589(18) 0.015(5) Uiso 1 1 d . . . . .
H1B H 0.575(2) 0.7301(19) 0.774(2) 0.027(5) Uiso 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
Tc1 Cl1 2.3586(4) 3_666 ?
Tc1 Cl1 2.3586(4) . ?
Tc1 Cl2 2.3499(4) . ?
Tc1 Cl2 2.3499(4) 3_666 ?
Tc1 Cl3 2.3562(4) . ?
Tc1 Cl3 2.3562(4) 3_666 ?
N1 C3 1.497(2) . ?
N1 C1 1.499(2) . ?
N1 H1A 0.89(2) . ?
N1 H1B 0.93(2) . ?
C3 C4 1.507(3) . ?
C3 H3A 0.977(18) . ?
C3 H3B 0.93(2) . ?
C4 H4A 0.91(2) . ?
C4 H4B 0.97(2) . ?
C4 H4C 0.93(3) . ?
C1 C2 1.509(2) . ?
C1 H1C 0.977(17) . ?
C1 H1D 0.973(19) . ?
C2 H2A 0.932(19) . ?
C2 H2B 0.95(2) . ?
C2 H2C 0.95(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Tc1 Cl1 180.0 . 3_666 ?
Cl2 Tc1 Cl1 90.164(16) . . ?
Cl2 Tc1 Cl1 89.836(15) 3_666 . ?
Cl2 Tc1 Cl1 90.163(15) 3_666 3_666 ?
Cl2 Tc1 Cl1 89.837(15) . 3_666 ?
Cl2 Tc1 Cl2 180.0 . 3_666 ?
Cl2 Tc1 Cl3 89.907(17) . 3_666 ?
Cl2 Tc1 Cl3 90.093(17) . . ?
Cl2 Tc1 Cl3 90.093(17) 3_666 3_666 ?
Cl2 Tc1 Cl3 89.907(17) 3_666 . ?
Cl3 Tc1 Cl1 89.987(15) 3_666 . ?
Cl3 Tc1 Cl1 89.986(16) . 3_666 ?
Cl3 Tc1 Cl1 90.013(15) . . ?
Cl3 Tc1 Cl1 90.014(16) 3_666 3_666 ?
Cl3 Tc1 Cl3 180.0 3_666 . ?
C3 N1 C1 114.35(14) . . ?
C3 N1 H1A 109.5(12) . . ?
C3 N1 H1B 110.0(12) . . ?
C1 N1 H1A 107.9(12) . . ?
C1 N1 H1B 108.5(12) . . ?
H1A N1 H1B 106.4(17) . . ?
N1 C3 C4 110.05(16) . . ?
N1 C3 H3A 107.8(11) . . ?
N1 C3 H3B 109.9(11) . . ?
C4 C3 H3A 111.5(11) . . ?
C4 C3 H3B 110.1(12) . . ?
H3A C3 H3B 107.5(15) . . ?
C3 C4 H4A 110.9(15) . . ?
C3 C4 H4B 110.4(12) . . ?
C3 C4 H4C 109.0(15) . . ?
H4A C4 H4B 107.6(19) . . ?
H4A C4 H4C 109.4(19) . . ?
H4B C4 H4C 109.6(18) . . ?
N1 C1 C2 109.55(15) . . ?
N1 C1 H1C 106.8(10) . . ?
N1 C1 H1D 103.7(10) . . ?
C2 C1 H1C 110.6(10) . . ?
C2 C1 H1D 113.4(11) . . ?
H1C C1 H1D 112.4(15) . . ?
C1 C2 H2A 110.0(12) . . ?
C1 C2 H2B 108.7(12) . . ?
C1 C2 H2C 110.1(11) . . ?
H2A C2 H2B 112.4(16) . . ?
H2A C2 H2C 107.3(16) . . ?
H2B C2 H2C 108.4(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A Cl3 0.89(2) 2.48(2) 3.3353(16) 160.8(17) 4_676 yes
N1 H1B Cl1 0.93(2) 2.66(2) 3.3179(16) 128.9(16) . yes
N1 H1B Cl2 0.93(2) 2.48(2) 3.3172(15) 150.0(17) . yes

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
C3 N1 C1 C2 177.82(15) . . . . ?
C1 N1 C3 C4 -178.26(15) . . . . ?

_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_ednatcbr_lt_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2298419'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br6 Tc, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 Br6 N2 Tc'
_chemical_formula_weight         725.75
_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'
Br Br -0.2901 2.4595 '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'
Tc Tc -1.4390 0.7593 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.1485(5)
_cell_length_b                   10.7497(6)
_cell_length_c                   9.9767(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.386(2)
_cell_angle_gamma                90
_cell_volume                     980.29(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6240
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.149
_cell_measurement_theta_min      2.787
_shelx_estimated_absorpt_T_max   0.264
_shelx_estimated_absorpt_T_min   0.122
_exptl_absorpt_coefficient_mu    12.948
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1117 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.6414.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20326
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.996
_diffrn_reflns_theta_min         4.089
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_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                2429
_reflns_number_total             2839
_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 V8.40B (Bruker, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         2839
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0218
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0188P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0425
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C3(H3A,H3B)
1.b Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_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
Tc1 Tc 0.500000 0.500000 0.500000 0.01023(6) Uani 1 2 d S . P . .
Br1 Br 0.71868(3) 0.61505(2) 0.59581(2) 0.01793(6) Uani 1 1 d . . . . .
Br2 Br 0.66292(2) 0.39454(2) 0.33784(2) 0.01462(6) Uani 1 1 d . . . . .
Br3 Br 0.54558(3) 0.32753(2) 0.66680(2) 0.01915(6) Uani 1 1 d . . . . .
N1 N 0.5763(2) 0.78849(18) 0.8447(2) 0.0161(4) Uani 1 1 d . . . . .
H1A H 0.670(3) 0.820(2) 0.854(3) 0.019 Uiso 1 1 d . U . . .
H1B H 0.576(3) 0.738(2) 0.780(3) 0.019 Uiso 1 1 d . U . . .
C1 C 0.5418(3) 0.7209(2) 0.9711(2) 0.0170(5) Uani 1 1 d . . . . .
H1C H 0.439579 0.690520 0.964754 0.020 Uiso 1 1 calc R U . . .
H1D H 0.551864 0.778344 1.048497 0.020 Uiso 1 1 calc R U . . .
C2 C 0.6458(3) 0.6118(2) 0.9917(3) 0.0220(5) Uani 1 1 d . . . . .
H2A H 0.623019 0.567786 1.074326 0.033 Uiso 1 1 calc R U . . .
H2B H 0.634664 0.554796 0.915332 0.033 Uiso 1 1 calc R U . . .
H2C H 0.746687 0.642414 0.998879 0.033 Uiso 1 1 calc R U . . .
C3 C 0.4763(3) 0.89423(19) 0.8081(3) 0.0181(5) Uani 1 1 d . . . . .
H3A H 0.486586 0.960143 0.877194 0.022 Uiso 1 1 calc R U . . .
H3B H 0.373649 0.864865 0.805298 0.022 Uiso 1 1 calc R U . . .
C4 C 0.5122(3) 0.9471(2) 0.6726(3) 0.0235(6) Uani 1 1 d . . . . .
H4A H 0.445811 1.016218 0.650086 0.035 Uiso 1 1 calc R U . . .
H4B H 0.613431 0.977187 0.675913 0.035 Uiso 1 1 calc R U . . .
H4C H 0.500676 0.882061 0.604132 0.035 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 Br1 2.5073(2) . ?
Tc1 Br1 2.5073(2) 3_666 ?
Tc1 Br2 2.5149(2) . ?
Tc1 Br2 2.5149(2) 3_666 ?
Tc1 Br3 2.5145(2) 3_666 ?
Tc1 Br3 2.5145(2) . ?
N1 H1A 0.92(3) . ?
N1 H1B 0.84(3) . ?
N1 C1 1.500(3) . ?
N1 C3 1.495(3) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C1 C2 1.519(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.515(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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
Br1 Tc1 Br1 180.0 . 3_666 ?
Br1 Tc1 Br2 90.988(8) 3_666 . ?
Br1 Tc1 Br2 89.012(8) . . ?
Br1 Tc1 Br2 89.012(8) 3_666 3_666 ?
Br1 Tc1 Br2 90.988(8) . 3_666 ?
Br1 Tc1 Br3 90.211(8) . . ?
Br1 Tc1 Br3 89.789(8) 3_666 . ?
Br1 Tc1 Br3 90.211(8) 3_666 3_666 ?
Br1 Tc1 Br3 89.789(9) . 3_666 ?
Br2 Tc1 Br2 180.0 3_666 . ?
Br3 Tc1 Br2 90.400(8) 3_666 3_666 ?
Br3 Tc1 Br2 90.400(8) . . ?
Br3 Tc1 Br2 89.600(8) . 3_666 ?
Br3 Tc1 Br2 89.600(8) 3_666 . ?
Br3 Tc1 Br3 180.0 . 3_666 ?
H1A N1 H1B 107(2) . . ?
C1 N1 H1A 109.0(16) . . ?
C1 N1 H1B 109.5(18) . . ?
C3 N1 H1A 107.2(15) . . ?
C3 N1 H1B 108.7(18) . . ?
C3 N1 C1 115.17(18) . . ?
N1 C1 H1C 109.8 . . ?
N1 C1 H1D 109.8 . . ?
N1 C1 C2 109.6(2) . . ?
H1C C1 H1D 108.2 . . ?
C2 C1 H1C 109.8 . . ?
C2 C1 H1D 109.8 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
N1 C3 C4 110.5(2) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A Br3 0.92(3) 2.62(3) 3.491(2) 157(2) 2_656 yes
N1 H1B Br1 0.84(3) 2.65(3) 3.407(2) 150(2) . yes
N1 H1B Br2 0.84(3) 2.82(3) 3.413(2) 129(2) 3_666 yes
C1 H1D Br2 0.99 3.07 3.740(2) 126.3 2_656 yes
C4 H4B Br1 0.98 3.07 3.766(3) 128.8 2_656 yes

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
C1 N1 C3 C4 -174.4(2) . . . . ?
C3 N1 C1 C2 176.71(19) . . . . ?

_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_tctunicbr_lt_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2298418'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br6 Tc, 2(C6 H7 N2 O)'
_chemical_formula_sum            'C12 H14 Br6 N4 O2 Tc'
_chemical_formula_weight         823.73
_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'
Br Br -0.2901 2.4595 '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'
Tc Tc -1.4390 0.7593 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.3100(11)
_cell_length_b                   10.8013(15)
_cell_length_c                   11.8992(16)
_cell_angle_alpha                90
_cell_angle_beta                 101.549(6)
_cell_angle_gamma                90
_cell_volume                     1046.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1525
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.820
_cell_measurement_theta_min      3.326
_shelx_estimated_absorpt_T_max   0.407
_shelx_estimated_absorpt_T_min   0.323
_exptl_absorpt_coefficient_mu    12.158
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0987 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.7550.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.614
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1211
_diffrn_reflns_av_unetI/netI     0.1010
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18373
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         4.159
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_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                1867
_reflns_number_total             3039
_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 V8.40B (Bruker, 2020)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.977
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         3039
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0454
_refine_ls_restrained_S_all      0.997
_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)+(0.0227P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0792
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N1-H1 = N2-H2B = N2-H2A
 0.86 with sigma of 0.05
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C2(H2)
;
_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
Tc1 Tc 0.500000 0.500000 0.500000 0.01482(17) Uani 1 2 d S . P . .
Br3 Br 0.78115(6) 0.52172(6) 0.45863(5) 0.02073(16) Uani 1 1 d . . . . .
Br1 Br 0.49242(7) 0.27507(6) 0.44115(6) 0.02299(16) Uani 1 1 d . . . . .
Br2 Br 0.61932(7) 0.43904(6) 0.70318(5) 0.02366(17) Uani 1 1 d . . . . .
O1 O 1.0096(5) 0.8483(4) 0.5303(4) 0.0293(11) Uani 1 1 d . . . . .
N1 N 0.5887(6) 0.8008(5) 0.2121(5) 0.0218(12) Uani 1 1 d D . . . .
H1 H 0.566(7) 0.759(6) 0.152(4) 0.026 Uiso 1 1 d D U . . .
N2 N 1.0879(6) 0.7769(6) 0.3698(5) 0.0309(14) Uani 1 1 d D . . . .
H2A H 1.180(6) 0.760(6) 0.410(5) 0.037 Uiso 1 1 d D U . . .
H2B H 1.066(8) 0.744(6) 0.306(4) 0.037 Uiso 1 1 d D U . . .
C4 C 0.7146(7) 0.9409(6) 0.3964(6) 0.0261(15) Uani 1 1 d . . . . .
H4 H 0.757549 0.988690 0.462641 0.031 Uiso 1 1 calc R U . . .
C3 C 0.8113(7) 0.8516(6) 0.3589(5) 0.0173(13) Uani 1 1 d . . . . .
C5 C 0.5564(7) 0.9603(6) 0.3378(6) 0.0261(15) Uani 1 1 d . . . . .
H5 H 0.491050 1.023627 0.361358 0.031 Uiso 1 1 calc R U . . .
C7 C 0.9795(7) 0.8235(6) 0.4265(6) 0.0247(15) Uani 1 1 d . . . . .
C6 C 0.4938(7) 0.8870(6) 0.2447(6) 0.0243(15) Uani 1 1 d . . . . .
H6 H 0.383959 0.897892 0.204283 0.029 Uiso 1 1 calc R U . . .
C2 C 0.7441(7) 0.7801(6) 0.2655(5) 0.0206(14) Uani 1 1 d . . . . .
H2 H 0.807086 0.716924 0.239377 0.025 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 Br3 2.4932(6) 3_666 ?
Tc1 Br3 2.4933(6) . ?
Tc1 Br1 2.5258(7) 3_666 ?
Tc1 Br1 2.5258(7) . ?
Tc1 Br2 2.5103(7) . ?
Tc1 Br2 2.5103(7) 3_666 ?
O1 C7 1.239(7) . ?
N1 H1 0.83(4) . ?
N1 C6 1.328(8) . ?
N1 C2 1.339(7) . ?
N2 H2A 0.84(4) . ?
N2 H2B 0.83(4) . ?
N2 C7 1.327(8) . ?
C4 H4 0.9500 . ?
C4 C3 1.385(8) . ?
C4 C5 1.375(8) . ?
C3 C7 1.498(8) . ?
C3 C2 1.376(8) . ?
C5 H5 0.9500 . ?
C5 C6 1.377(9) . ?
C6 H6 0.9500 . ?
C2 H2 0.9500 . ?

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
Br3 Tc1 Br3 180.0 3_666 . ?
Br3 Tc1 Br1 89.536(19) . 3_666 ?
Br3 Tc1 Br1 89.536(19) 3_666 . ?
Br3 Tc1 Br1 90.465(19) 3_666 3_666 ?
Br3 Tc1 Br1 90.464(19) . . ?
Br3 Tc1 Br2 90.56(2) 3_666 3_666 ?
Br3 Tc1 Br2 90.56(2) . . ?
Br3 Tc1 Br2 89.44(2) . 3_666 ?
Br3 Tc1 Br2 89.44(2) 3_666 . ?
Br1 Tc1 Br1 180.0 . 3_666 ?
Br2 Tc1 Br1 90.12(2) . 3_666 ?
Br2 Tc1 Br1 89.88(2) 3_666 3_666 ?
Br2 Tc1 Br1 89.88(2) . . ?
Br2 Tc1 Br1 90.12(2) 3_666 . ?
Br2 Tc1 Br2 180.00(3) 3_666 . ?
C6 N1 H1 126(4) . . ?
C6 N1 C2 123.4(6) . . ?
C2 N1 H1 110(4) . . ?
H2A N2 H2B 116(7) . . ?
C7 N2 H2A 116(5) . . ?
C7 N2 H2B 125(5) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C5 C4 C3 120.0(6) . . ?
C4 C3 C7 120.5(5) . . ?
C2 C3 C4 118.9(5) . . ?
C2 C3 C7 120.3(6) . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.3(6) . . ?
C6 C5 H5 120.4 . . ?
O1 C7 N2 124.5(6) . . ?
O1 C7 C3 118.2(6) . . ?
N2 C7 C3 117.3(6) . . ?
N1 C6 C5 119.2(6) . . ?
N1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
N1 C2 C3 119.2(6) . . ?
N1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O1 0.83(4) 1.85(4) 2.671(7) 173(7) 4_575 yes
C4 H4 O1 0.95 2.61 3.225(7) 123.2 3_776 yes

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
C4 C3 C7 O1 23.5(9) . . . . ?
C4 C3 C7 N2 -154.5(6) . . . . ?
C4 C3 C2 N1 1.6(9) . . . . ?
C4 C5 C6 N1 -1.4(9) . . . . ?
C3 C4 C5 C6 2.5(10) . . . . ?
C5 C4 C3 C7 -175.8(6) . . . . ?
C5 C4 C3 C2 -2.6(9) . . . . ?
C7 C3 C2 N1 174.7(5) . . . . ?
C6 N1 C2 C3 -0.5(9) . . . . ?
C2 N1 C6 C5 0.4(9) . . . . ?
C2 C3 C7 O1 -149.5(6) . . . . ?
C2 C3 C7 N2 32.5(9) . . . . ?

_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_kazt6_lt_1_0m
_database_code_depnum_ccdc_archive 'CCDC 2298417'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Tc, 2(Cl), 4(C7 H6 N S), 4(H2 O)'
_chemical_formula_sum            'C28 H32 Cl8 N4 O4 S4 Tc'
_chemical_formula_weight         998.41
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.1584(4)
_cell_length_b                   9.3884(5)
_cell_length_c                   15.4846(8)
_cell_angle_alpha                76.369(2)
_cell_angle_beta                 79.704(2)
_cell_angle_gamma                81.477(2)
_cell_volume                     988.92(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9330
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.198
_cell_measurement_theta_min      2.246
_shelx_estimated_absorpt_T_max   0.924
_shelx_estimated_absorpt_T_min   0.802
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0473 before and 0.0391 after correction.
The Ratio of minimum to maximum transmission is 0.9119.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             503
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19290
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.995
_diffrn_reflns_theta_min         4.089
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_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                5023
_reflns_number_total             5751
_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 V8.40B (Bruker, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         5751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0230
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0200P)²+0.2965P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0516
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C15(H15), C16(H16), C17(H17), C5(H5), C2(H2), C18(H18),
 C7(H7), C6(H6)
;
_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
Tc1 Tc 0.500000 1.000000 0.000000 0.01108(4) Uani 1 2 d S . P . .
Cl1 Cl 0.62106(5) 0.74762(4) 0.02726(2) 0.01549(7) Uani 1 1 d . . . . .
Cl2 Cl 0.25155(5) 0.94030(4) -0.06316(2) 0.01609(7) Uani 1 1 d . . . . .
Cl3 Cl 0.68970(5) 1.03788(4) -0.14278(2) 0.01581(7) Uani 1 1 d . . . . .
Cl4 Cl 0.65467(5) 1.10172(4) 0.54905(2) 0.02137(8) Uani 1 1 d . . . . .
S13 S 1.12136(5) 0.58437(4) 0.06720(2) 0.01667(7) Uani 1 1 d . . . . .
S3 S 0.45861(5) 0.65466(4) 0.82882(2) 0.01799(8) Uani 1 1 d . . . . .
O1 O 0.91434(19) 0.89431(15) 0.42945(9) 0.0299(3) Uani 1 1 d . . . . .
H1A H 1.028(3) 0.892(2) 0.4356(15) 0.045 Uiso 1 1 d . U . . .
H1B H 0.856(3) 0.949(3) 0.4623(15) 0.045 Uiso 1 1 d . U . . .
O2 O 0.72118(18) 0.84235(14) 0.30947(9) 0.0279(3) Uani 1 1 d . . . . .
H2A H 0.620(3) 0.830(2) 0.3403(15) 0.042 Uiso 1 1 d . U . . .
H2B H 0.786(3) 0.855(2) 0.3428(15) 0.042 Uiso 1 1 d . U . . .
N1 N 0.56042(17) 0.80633(14) 0.67397(9) 0.0179(2) Uani 1 1 d . . . . .
H1 H 0.580(2) 0.886(2) 0.6317(12) 0.022 Uiso 1 1 d . U . . .
N11 N 0.91625(17) 0.67964(14) 0.19710(9) 0.0158(2) Uani 1 1 d . . . . .
H11 H 0.852(2) 0.740(2) 0.2288(12) 0.019 Uiso 1 1 d . U . . .
C12 C 1.00888(19) 0.72390(16) 0.11651(10) 0.0172(3) Uani 1 1 d . . . . .
H12 H 1.012895 0.825032 0.088098 0.021 Uiso 1 1 calc R U . . .
C9 C 0.61550(19) 0.66213(16) 0.66409(10) 0.0157(3) Uani 1 1 d . . . . .
C8 C 0.7041(2) 0.61513(17) 0.58607(10) 0.0215(3) Uani 1 1 d . . . . .
H8 H 0.734660 0.683523 0.531081 0.026 Uiso 1 1 calc R U . . .
C14 C 1.03466(18) 0.45504(15) 0.16135(9) 0.0137(3) Uani 1 1 d . . . . .
C15 C 1.06485(19) 0.30145(16) 0.17701(10) 0.0171(3) Uani 1 1 d . . . . .
H15 H 1.134244 0.252136 0.132201 0.021 Uiso 1 1 calc R U . . .
C16 C 0.9894(2) 0.22371(17) 0.26065(11) 0.0206(3) Uani 1 1 d . . . . .
H16 H 1.008821 0.118998 0.273595 0.025 Uiso 1 1 calc R U . . .
C17 C 0.8849(2) 0.29640(17) 0.32669(10) 0.0207(3) Uani 1 1 d . . . . .
H17 H 0.835989 0.239870 0.383486 0.025 Uiso 1 1 calc R U . . .
C5 C 0.6113(2) 0.41028(16) 0.75064(10) 0.0174(3) Uani 1 1 d . . . . .
H5 H 0.580182 0.341628 0.805454 0.021 Uiso 1 1 calc R U . . .
C4 C 0.56916(19) 0.56148(16) 0.74493(10) 0.0149(3) Uani 1 1 d . . . . .
C2 C 0.4783(2) 0.81866(17) 0.75523(10) 0.0192(3) Uani 1 1 d . . . . .
H2 H 0.434087 0.910872 0.771208 0.023 Uiso 1 1 calc R U . . .
C19 C 0.92859(18) 0.52688(15) 0.22676(9) 0.0138(3) Uani 1 1 d . . . . .
C18 C 0.8518(2) 0.44823(17) 0.31068(10) 0.0190(3) Uani 1 1 d . . . . .
H18 H 0.779624 0.497318 0.355022 0.023 Uiso 1 1 calc R U . . .
C7 C 0.7454(2) 0.46503(18) 0.59233(11) 0.0247(3) Uani 1 1 d . . . . .
H7 H 0.805857 0.429274 0.540558 0.030 Uiso 1 1 calc R U . . .
C6 C 0.6997(2) 0.36384(17) 0.67379(11) 0.0207(3) Uani 1 1 d . . . . .
H6 H 0.730521 0.261236 0.675867 0.025 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 Cl1 2.3652(4) . ?
Tc1 Cl1 2.3652(4) 2_675 ?
Tc1 Cl2 2.3684(3) 2_675 ?
Tc1 Cl2 2.3684(3) . ?
Tc1 Cl3 2.3574(3) 2_675 ?
Tc1 Cl3 2.3575(3) . ?
S13 C12 1.6990(16) . ?
S13 C14 1.7466(14) . ?
S3 C4 1.7441(15) . ?
S3 C2 1.6938(16) . ?
O1 H1A 0.83(2) . ?
O1 H1B 0.83(2) . ?
O2 H2A 0.80(2) . ?
O2 H2B 0.79(2) . ?
N1 H1 0.877(18) . ?
N1 C9 1.3891(19) . ?
N1 C2 1.3140(19) . ?
N11 H11 0.861(18) . ?
N11 C12 1.3081(19) . ?
N11 C19 1.3936(18) . ?
C12 H12 0.9500 . ?
C9 C8 1.397(2) . ?
C9 C4 1.3989(19) . ?
C8 H8 0.9500 . ?
C8 C7 1.380(2) . ?
C14 C15 1.3951(19) . ?
C14 C19 1.3973(19) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.406(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.380(2) . ?
C5 H5 0.9500 . ?
C5 C4 1.392(2) . ?
C5 C6 1.379(2) . ?
C2 H2 0.9500 . ?
C19 C18 1.3959(19) . ?
C18 H18 0.9500 . ?
C7 H7 0.9500 . ?
C7 C6 1.407(2) . ?
C6 H6 0.9500 . ?

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
Cl1 Tc1 Cl1 180.0 . 2_675 ?
Cl1 Tc1 Cl2 88.657(12) 2_675 2_675 ?
Cl1 Tc1 Cl2 91.343(12) 2_675 . ?
Cl1 Tc1 Cl2 88.657(12) . . ?
Cl1 Tc1 Cl2 91.343(12) . 2_675 ?
Cl2 Tc1 Cl2 180.0 2_675 . ?
Cl3 Tc1 Cl1 90.001(12) 2_675 2_675 ?
Cl3 Tc1 Cl1 89.999(12) . 2_675 ?
Cl3 Tc1 Cl1 90.001(12) . . ?
Cl3 Tc1 Cl1 89.998(12) 2_675 . ?
Cl3 Tc1 Cl2 89.828(12) . . ?
Cl3 Tc1 Cl2 90.171(12) . 2_675 ?
Cl3 Tc1 Cl2 89.829(12) 2_675 2_675 ?
Cl3 Tc1 Cl2 90.172(12) 2_675 . ?
Cl3 Tc1 Cl3 180.000(17) 2_675 . ?
C12 S13 C14 90.31(7) . . ?
C2 S3 C4 90.45(7) . . ?
H1A O1 H1B 103(2) . . ?
H2A O2 H2B 104(2) . . ?
C9 N1 H1 125.4(12) . . ?
C2 N1 H1 120.1(12) . . ?
C2 N1 C9 114.51(13) . . ?
C12 N11 H11 123.0(12) . . ?
C12 N11 C19 114.11(13) . . ?
C19 N11 H11 122.9(12) . . ?
S13 C12 H12 123.0 . . ?
N11 C12 S13 113.99(11) . . ?
N11 C12 H12 123.0 . . ?
N1 C9 C8 127.38(13) . . ?
N1 C9 C4 111.13(13) . . ?
C8 C9 C4 121.49(14) . . ?
C9 C8 H8 121.4 . . ?
C7 C8 C9 117.11(14) . . ?
C7 C8 H8 121.4 . . ?
C15 C14 S13 128.85(11) . . ?
C15 C14 C19 121.09(12) . . ?
C19 C14 S13 110.01(10) . . ?
C14 C15 H15 121.4 . . ?
C16 C15 C14 117.27(14) . . ?
C16 C15 H15 121.4 . . ?
C15 C16 H16 119.3 . . ?
C15 C16 C17 121.46(14) . . ?
C17 C16 H16 119.3 . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.31(13) . . ?
C18 C17 H17 119.3 . . ?
C4 C5 H5 121.2 . . ?
C6 C5 H5 121.2 . . ?
C6 C5 C4 117.53(13) . . ?
C9 C4 S3 110.25(11) . . ?
C5 C4 S3 128.73(11) . . ?
C5 C4 C9 121.02(13) . . ?
S3 C2 H2 123.2 . . ?
N1 C2 S3 113.66(12) . . ?
N1 C2 H2 123.2 . . ?
N11 C19 C14 111.53(12) . . ?
N11 C19 C18 126.99(14) . . ?
C18 C19 C14 121.46(13) . . ?
C17 C18 C19 117.38(14) . . ?
C17 C18 H18 121.3 . . ?
C19 C18 H18 121.3 . . ?
C8 C7 H7 119.3 . . ?
C8 C7 C6 121.38(14) . . ?
C6 C7 H7 119.3 . . ?
C5 C6 C7 121.47(14) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A Cl4 0.83(2) 2.34(2) 3.1683(14) 178(2) 2_776 yes
O1 H1B Cl4 0.83(2) 2.35(2) 3.1738(14) 173(2) . yes
O2 H2A Cl4 0.80(2) 2.48(2) 3.2141(13) 153(2) 2_676 yes
O2 H2B O1 0.79(2) 1.88(2) 2.6732(18) 173(2) . yes
N1 H1 Cl4 0.877(18) 2.213(18) 3.0736(13) 166.8(16) . yes
N11 H11 O2 0.861(18) 1.803(19) 2.6577(17) 171.3(17) . yes
C12 H12 Cl2 0.95 2.74 3.3970(15) 127.1 1_655 yes
C2 H2 Cl2 0.95 2.72 3.3435(16) 124.0 1_556 yes
C2 H2 O2 0.95 2.56 3.291(2) 134.4 2_676 yes

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
S13 C14 C15 C16 175.74(11) . . . . ?
S13 C14 C19 N11 2.29(14) . . . . ?
S13 C14 C19 C18 -176.56(11) . . . . ?
N1 C9 C8 C7 -179.85(14) . . . . ?
N1 C9 C4 S3 0.02(14) . . . . ?
N1 C9 C4 C5 179.95(12) . . . . ?
N11 C19 C18 C17 -178.60(13) . . . . ?
C12 S13 C14 C15 -179.36(13) . . . . ?
C12 S13 C14 C19 -1.84(10) . . . . ?
C12 N11 C19 C14 -1.66(17) . . . . ?
C12 N11 C19 C18 177.11(13) . . . . ?
C9 N1 C2 S3 -0.16(16) . . . . ?
C9 C8 C7 C6 0.1(2) . . . . ?
C8 C9 C4 S3 -179.45(11) . . . . ?
C8 C9 C4 C5 0.5(2) . . . . ?
C8 C7 C6 C5 0.3(2) . . . . ?
C14 S13 C12 N11 0.96(11) . . . . ?
C14 C15 C16 C17 0.7(2) . . . . ?
C14 C19 C18 C17 0.1(2) . . . . ?
C15 C14 C19 N11 -179.96(12) . . . . ?
C15 C14 C19 C18 1.2(2) . . . . ?
C15 C16 C17 C18 0.5(2) . . . . ?
C16 C17 C18 C19 -0.9(2) . . . . ?
C4 S3 C2 N1 0.14(12) . . . . ?
C4 C9 C8 C7 -0.5(2) . . . . ?
C4 C5 C6 C7 -0.3(2) . . . . ?
C2 S3 C4 C9 -0.09(11) . . . . ?
C2 S3 C4 C5 179.98(13) . . . . ?
C2 N1 C9 C8 179.51(15) . . . . ?
C2 N1 C9 C4 0.09(17) . . . . ?
C19 N11 C12 S13 0.21(16) . . . . ?
C19 C14 C15 C16 -1.5(2) . . . . ?
C6 C5 C4 S3 179.82(11) . . . . ?
C6 C5 C4 C9 -0.1(2) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_kazt6_lt_1_0m       
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 16 Note
RESPONSE: Closed by beamstop.
;
####################################################################### 
# 
# 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_kaz12_lt_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2298420'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br6 Tc, 2(C8 H11 N4 O2), H2 O'
_chemical_formula_sum            'C16 H24 Br6 N8 O5 Tc'
_chemical_formula_weight         985.89
_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'
Br Br -0.2901 2.4595 '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'
Tc Tc -1.4390 0.7593 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.428(2)
_cell_length_b                   14.292(3)
_cell_length_c                   15.242(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.823(7)
_cell_angle_gamma                90
_cell_volume                     2800.0(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.096
_cell_measurement_theta_min      2.788
_shelx_estimated_absorpt_T_max   0.772
_shelx_estimated_absorpt_T_min   0.462
_exptl_absorpt_coefficient_mu    9.120
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1103 before and 0.0764 after correction.
The Ratio of minimum to maximum transmission is 0.6617.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1817
_diffrn_reflns_av_unetI/netI     0.1617
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43761
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         4.192
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_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                3939
_reflns_number_total             8150
_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 V8.40B (Bruker, 2020)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.545
_refine_diff_density_min         -1.921
_refine_diff_density_rms         0.256
_refine_ls_extinction_coef       0.00085(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         8150
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_gt           0.0610
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0416P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1380
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N9-H9
 0.86 with sigma of 0.02
 O1-H1A = O1-H1B
 0.85 with sigma of 0.02
 N29-H29
 0.88 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(N27) = Uanis(C28)
Uanis(O33) = Uanis(O31)
Uanis(C22) = Uanis(C26)
3.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C8(H8)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C34(H34A,H34B,H34C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C10(H10A,H10B,H10C)
;
_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
Tc1 Tc 0.99322(5) 0.72203(5) 0.73113(5) 0.01588(17) Uani 1 1 d . . . . .
Br1 Br 0.99985(6) 0.89440(6) 0.75449(7) 0.0238(2) Uani 1 1 d . . . . .
Br2 Br 1.16427(6) 0.70712(6) 0.85338(6) 0.0245(2) Uani 1 1 d . . . . .
Br3 Br 0.90210(6) 0.70639(6) 0.85454(7) 0.0269(2) Uani 1 1 d . . . . .
Br4 Br 0.82116(6) 0.73862(7) 0.61189(7) 0.0288(2) Uani 1 1 d . . . . .
Br5 Br 1.08733(7) 0.73912(7) 0.61128(7) 0.0317(2) Uani 1 1 d . . . . .
Br6 Br 0.98702(7) 0.54840(6) 0.70831(8) 0.0363(3) Uani 1 1 d . . . . .
O13 O 0.6770(4) 0.4763(4) 0.4909(4) 0.0261(15) Uani 1 1 d . . . . .
O31 O 1.0725(5) 0.2997(5) 0.7134(4) 0.0384(12) Uani 1 1 d . . . . .
O11 O 0.5668(4) 0.6587(4) 0.6924(4) 0.0245(14) Uani 1 1 d . . . . .
N7 N 0.8087(5) 0.3723(5) 0.6599(5) 0.0247(18) Uani 1 1 d . . . . .
N21 N 1.1762(5) 0.3769(4) 0.8359(5) 0.0192(16) Uani 1 1 d . . . . .
N29 N 1.2987(5) 0.5391(4) 0.6793(5) 0.0170(15) Uani 1 1 d D . . . .
H29 H 1.284(6) 0.543(5) 0.6198(15) 0.020 Uiso 1 1 d D U . . .
N1 N 0.6237(5) 0.5675(4) 0.5924(5) 0.0185(15) Uani 1 1 d . . . . .
N3 N 0.6859(5) 0.5460(4) 0.7534(5) 0.0165(15) Uani 1 1 d . . . . .
N23 N 1.1813(5) 0.4099(4) 0.6854(5) 0.0169(15) Uani 1 1 d . . . . .
O1 O 0.9008(5) 0.4369(5) 0.9830(5) 0.0432(18) Uani 1 1 d D . . . .
H1A H 0.921(8) 0.407(7) 1.033(4) 0.065 Uiso 1 1 d D U . . .
H1B H 0.960(4) 0.442(7) 0.974(8) 0.065 Uiso 1 1 d D U . . .
N9 N 0.8101(5) 0.4172(5) 0.7972(5) 0.0209(16) Uani 1 1 d D . . . .
H9 H 0.820(6) 0.417(6) 0.8562(17) 0.025 Uiso 1 1 d D U . . .
N27 N 1.3600(5) 0.5667(4) 0.8257(5) 0.0185(12) Uani 1 1 d . . . . .
O33 O 1.2794(5) 0.4541(4) 0.9620(4) 0.0384(12) Uani 1 1 d . . . . .
C5 C 0.7431(6) 0.4483(5) 0.6513(6) 0.0182(18) Uani 1 1 d . . . . .
C12 C 0.6825(6) 0.5631(6) 0.8475(5) 0.023(2) Uani 1 1 d . . . . .
H12A H 0.670961 0.503854 0.875388 0.034 Uiso 1 1 calc R U . . .
H12B H 0.625565 0.606449 0.846389 0.034 Uiso 1 1 calc R U . . .
H12C H 0.748615 0.590479 0.883442 0.034 Uiso 1 1 calc R U . . .
C6 C 0.6827(6) 0.4945(6) 0.5711(6) 0.0207(19) Uani 1 1 d . . . . .
C25 C 1.2886(6) 0.4950(5) 0.8143(6) 0.0177(18) Uani 1 1 d . . . . .
C24 C 1.2520(6) 0.4771(5) 0.7233(6) 0.0162(18) Uani 1 1 d . . . . .
C26 C 1.2526(6) 0.4433(6) 0.8774(6) 0.0221(14) Uani 1 1 d . . . . .
C4 C 0.7436(6) 0.4749(5) 0.7366(6) 0.0172(18) Uani 1 1 d . . . . .
C2 C 0.6226(6) 0.5951(5) 0.6812(6) 0.0190(19) Uani 1 1 d . . . . .
C14 C 0.8365(7) 0.3240(7) 0.5871(7) 0.036(3) Uani 1 1 d . . . . .
H14A H 0.775623 0.290467 0.548974 0.054 Uiso 1 1 calc R U . . .
H14B H 0.892390 0.279243 0.613636 0.054 Uiso 1 1 calc R U . . .
H14C H 0.860252 0.369459 0.549466 0.054 Uiso 1 1 calc R U . . .
C28 C 1.3642(6) 0.5910(6) 0.7434(6) 0.0185(12) Uani 1 1 d . . . . .
H28 H 1.407673 0.638803 0.731399 0.022 Uiso 1 1 calc R U . . .
C22 C 1.1391(6) 0.3584(6) 0.7431(6) 0.0221(14) Uani 1 1 d . . . . .
C34 C 1.4221(6) 0.6095(6) 0.9127(6) 0.027(2) Uani 1 1 d . . . . .
H34A H 1.376678 0.623648 0.951057 0.040 Uiso 1 1 calc R U . . .
H34B H 1.454110 0.667450 0.899575 0.040 Uiso 1 1 calc R U . . .
H34C H 1.476572 0.565821 0.945099 0.040 Uiso 1 1 calc R U . . .
C30 C 1.1327(7) 0.3214(7) 0.8979(6) 0.038(3) Uani 1 1 d . . . . .
H30A H 1.177274 0.267016 0.920221 0.057 Uiso 1 1 calc R U . . .
H30B H 1.062549 0.300254 0.864647 0.057 Uiso 1 1 calc R U . . .
H30C H 1.129529 0.360206 0.950086 0.057 Uiso 1 1 calc R U . . .
C8 C 0.8477(6) 0.3552(6) 0.7490(7) 0.027(2) Uani 1 1 d . . . . .
H8 H 0.895165 0.306273 0.774648 0.032 Uiso 1 1 calc R U . . .
C32 C 1.1404(6) 0.3998(5) 0.5851(6) 0.022(2) Uani 1 1 d . . . . .
H32A H 1.110816 0.459576 0.558152 0.033 Uiso 1 1 calc R U . . .
H32B H 1.086128 0.351631 0.570449 0.033 Uiso 1 1 calc R U . . .
H32C H 1.196908 0.381613 0.559880 0.033 Uiso 1 1 calc R U . . .
C10 C 0.5589(6) 0.6265(6) 0.5167(6) 0.028(2) Uani 1 1 d . . . . .
H10A H 0.592344 0.687517 0.517276 0.042 Uiso 1 1 calc R U . . .
H10B H 0.489888 0.635335 0.525286 0.042 Uiso 1 1 calc R U . . .
H10C H 0.551668 0.595502 0.457885 0.042 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 Br1 2.4871(12) . ?
Tc1 Br2 2.5132(11) . ?
Tc1 Br3 2.5334(12) . ?
Tc1 Br4 2.5034(12) . ?
Tc1 Br5 2.5159(12) . ?
Tc1 Br6 2.5038(12) . ?
O13 C6 1.230(9) . ?
O31 C22 1.213(10) . ?
O11 C2 1.221(9) . ?
N7 C5 1.380(9) . ?
N7 C14 1.444(10) . ?
N7 C8 1.330(11) . ?
N21 C26 1.406(10) . ?
N21 C22 1.384(11) . ?
N21 C30 1.477(10) . ?
N29 H29 0.87(2) . ?
N29 C24 1.369(9) . ?
N29 C28 1.334(10) . ?
N1 C6 1.405(10) . ?
N1 C2 1.414(10) . ?
N1 C10 1.489(10) . ?
N3 C12 1.469(10) . ?
N3 C4 1.346(9) . ?
N3 C2 1.373(10) . ?
N23 C24 1.356(10) . ?
N23 C22 1.387(10) . ?
N23 C32 1.475(10) . ?
O1 H1A 0.85(2) . ?
O1 H1B 0.84(2) . ?
N9 H9 0.87(2) . ?
N9 C4 1.361(10) . ?
N9 C8 1.341(11) . ?
N27 C25 1.380(9) . ?
N27 C28 1.319(10) . ?
N27 C34 1.479(10) . ?
O33 C26 1.244(10) . ?
C5 C6 1.419(11) . ?
C5 C4 1.354(11) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C25 C24 1.354(11) . ?
C25 C26 1.405(11) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C28 H28 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C8 H8 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

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
Br1 Tc1 Br2 89.47(4) . . ?
Br1 Tc1 Br3 89.20(4) . . ?
Br1 Tc1 Br4 89.85(4) . . ?
Br1 Tc1 Br5 90.18(4) . . ?
Br1 Tc1 Br6 179.75(5) . . ?
Br2 Tc1 Br3 88.63(4) . . ?
Br2 Tc1 Br5 90.19(4) . . ?
Br4 Tc1 Br2 178.72(4) . . ?
Br4 Tc1 Br3 90.28(4) . . ?
Br4 Tc1 Br5 90.90(4) . . ?
Br4 Tc1 Br6 90.37(4) . . ?
Br5 Tc1 Br3 178.67(4) . . ?
Br6 Tc1 Br2 90.31(4) . . ?
Br6 Tc1 Br3 90.68(4) . . ?
Br6 Tc1 Br5 89.93(4) . . ?
C5 N7 C14 127.1(8) . . ?
C8 N7 C5 107.1(7) . . ?
C8 N7 C14 125.7(8) . . ?
C26 N21 C30 116.5(7) . . ?
C22 N21 C26 126.1(7) . . ?
C22 N21 C30 117.4(7) . . ?
C24 N29 H29 123(5) . . ?
C28 N29 H29 129(5) . . ?
C28 N29 C24 107.5(7) . . ?
C6 N1 C2 126.3(7) . . ?
C6 N1 C10 119.0(7) . . ?
C2 N1 C10 114.6(7) . . ?
C4 N3 C12 119.5(7) . . ?
C4 N3 C2 119.4(7) . . ?
C2 N3 C12 120.7(7) . . ?
C24 N23 C22 118.0(7) . . ?
C24 N23 C32 121.0(6) . . ?
C22 N23 C32 120.5(7) . . ?
H1A O1 H1B 97(10) . . ?
C4 N9 H9 125(5) . . ?
C8 N9 H9 127(6) . . ?
C8 N9 C4 107.8(8) . . ?
C25 N27 C34 127.7(7) . . ?
C28 N27 C25 107.2(7) . . ?
C28 N27 C34 125.1(7) . . ?
N7 C5 C6 129.6(8) . . ?
C4 C5 N7 107.7(7) . . ?
C4 C5 C6 122.7(7) . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O13 C6 N1 120.7(8) . . ?
O13 C6 C5 127.9(8) . . ?
N1 C6 C5 111.5(7) . . ?
N27 C25 C26 131.9(8) . . ?
C24 C25 N27 107.7(7) . . ?
C24 C25 C26 120.4(7) . . ?
N23 C24 N29 127.8(8) . . ?
C25 C24 N29 107.3(7) . . ?
C25 C24 N23 124.9(7) . . ?
O33 C26 N21 120.3(7) . . ?
O33 C26 C25 126.2(8) . . ?
C25 C26 N21 113.4(8) . . ?
N3 C4 N9 129.0(8) . . ?
N3 C4 C5 123.4(7) . . ?
C5 C4 N9 107.6(7) . . ?
O11 C2 N1 121.2(8) . . ?
O11 C2 N3 122.1(8) . . ?
N3 C2 N1 116.6(7) . . ?
N7 C14 H14A 109.5 . . ?
N7 C14 H14B 109.5 . . ?
N7 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N29 C28 H28 124.8 . . ?
N27 C28 N29 110.4(7) . . ?
N27 C28 H28 124.8 . . ?
O31 C22 N21 121.5(8) . . ?
O31 C22 N23 121.5(8) . . ?
N21 C22 N23 117.0(8) . . ?
N27 C34 H34A 109.5 . . ?
N27 C34 H34B 109.5 . . ?
N27 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N21 C30 H30A 109.5 . . ?
N21 C30 H30B 109.5 . . ?
N21 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N7 C8 N9 109.8(7) . . ?
N7 C8 H8 125.1 . . ?
N9 C8 H8 125.1 . . ?
N23 C32 H32A 109.5 . . ?
N23 C32 H32B 109.5 . . ?
N23 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N29 H29 O13 0.87(2) 1.93(4) 2.716(9) 150(7) 3_766 yes
O1 H1B O1 0.84(2) 2.50(8) 3.134(15) 133(9) 3_767 yes
N9 H9 O1 0.87(2) 1.94(4) 2.754(10) 154(7) . yes
C14 H14B O31 0.98 2.47 3.216(11) 132.2 . yes
C28 H28 O31 0.95 2.44 3.119(10) 128.6 2_756 yes
C28 H28 O11 0.95 2.40 3.189(9) 140.9 1_655 yes
C34 H34B O31 0.98 2.51 3.343(11) 142.4 2_756 yes
C8 H8 O11 0.95 2.19 3.066(10) 152.3 2_646 yes

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
N7 C5 C6 O13 -0.7(13) . . . . ?
N7 C5 C6 N1 178.1(7) . . . . ?
N7 C5 C4 N3 -178.4(7) . . . . ?
N7 C5 C4 N9 1.2(9) . . . . ?
N27 C25 C24 N29 -1.5(8) . . . . ?
N27 C25 C24 N23 179.0(7) . . . . ?
N27 C25 C26 N21 178.4(7) . . . . ?
N27 C25 C26 O33 1.1(14) . . . . ?
C5 N7 C8 N9 -0.2(9) . . . . ?
C12 N3 C4 N9 -6.3(11) . . . . ?
C12 N3 C4 C5 173.2(7) . . . . ?
C12 N3 C2 O11 5.2(11) . . . . ?
C12 N3 C2 N1 -173.9(6) . . . . ?
C6 N1 C2 O11 -178.6(7) . . . . ?
C6 N1 C2 N3 0.4(10) . . . . ?
C6 C5 C4 N3 1.2(12) . . . . ?
C6 C5 C4 N9 -179.2(7) . . . . ?
C25 N27 C28 N29 0.4(8) . . . . ?
C24 N29 C28 N27 -1.4(8) . . . . ?
C24 N23 C22 O31 177.1(7) . . . . ?
C24 N23 C22 N21 -2.8(10) . . . . ?
C24 C25 C26 N21 -1.8(11) . . . . ?
C24 C25 C26 O33 -179.1(8) . . . . ?
C26 N21 C22 O31 -179.8(8) . . . . ?
C26 N21 C22 N23 0.1(11) . . . . ?
C26 C25 C24 N29 178.6(7) . . . . ?
C26 C25 C24 N23 -0.9(12) . . . . ?
C4 N3 C2 O11 178.2(7) . . . . ?
C4 N3 C2 N1 -0.8(10) . . . . ?
C4 N9 C8 N7 1.0(9) . . . . ?
C4 C5 C6 O13 179.8(7) . . . . ?
C4 C5 C6 N1 -1.5(10) . . . . ?
C2 N1 C6 O13 179.6(7) . . . . ?
C2 N1 C6 C5 0.7(10) . . . . ?
C2 N3 C4 N9 -179.4(7) . . . . ?
C2 N3 C4 C5 0.1(11) . . . . ?
C14 N7 C5 C6 4.0(13) . . . . ?
C14 N7 C5 C4 -176.4(7) . . . . ?
C14 N7 C8 N9 175.7(7) . . . . ?
C28 N29 C24 N23 -178.8(7) . . . . ?
C28 N29 C24 C25 1.8(8) . . . . ?
C28 N27 C25 C24 0.7(8) . . . . ?
C28 N27 C25 C26 -179.4(8) . . . . ?
C22 N21 C26 O33 179.7(8) . . . . ?
C22 N21 C26 C25 2.2(11) . . . . ?
C22 N23 C24 N29 -176.0(7) . . . . ?
C22 N23 C24 C25 3.4(11) . . . . ?
C34 N27 C25 C24 -178.8(7) . . . . ?
C34 N27 C25 C26 1.1(13) . . . . ?
C34 N27 C28 N29 180.0(7) . . . . ?
C30 N21 C26 O33 -1.1(11) . . . . ?
C30 N21 C26 C25 -178.5(7) . . . . ?
C30 N21 C22 O31 0.9(12) . . . . ?
C30 N21 C22 N23 -179.1(7) . . . . ?
C8 N7 C5 C6 179.8(8) . . . . ?
C8 N7 C5 C4 -0.6(9) . . . . ?
C8 N9 C4 N3 178.3(7) . . . . ?
C8 N9 C4 C5 -1.3(9) . . . . ?
C32 N23 C24 N29 -3.8(11) . . . . ?
C32 N23 C24 C25 175.6(7) . . . . ?
C32 N23 C22 O31 4.8(12) . . . . ?
C32 N23 C22 N21 -175.1(7) . . . . ?
C10 N1 C6 O13 -3.7(10) . . . . ?
C10 N1 C6 C5 177.4(6) . . . . ?
C10 N1 C2 O11 4.5(10) . . . . ?
C10 N1 C2 N3 -176.4(6) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT417_kaz12_lt_0m_a       
;
PROBLEM: Short Inter D-H..H-D H1B ..H1B . 2.01 Ang.
RESPONSE: The hydrogen atoms have been refined and this is their position 
after the refinement.
;
_vrf_PLAT910_kaz12_lt_0m_a       
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 24 Note
RESPONSE: Closed by beamstop.
;
# start Validation Reply Form
_vrf_RINTA01_kaz12_lt_0m_a       
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Small crystal.
;
####################################################################### 
# 
# 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_MV19
_database_code_depnum_ccdc_archive 'CCDC 2298421'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_audit_creation_date             2023-07-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Cl6 Tc), 8(Cl), 3(H2 O), 12(C4 H5 N2)'
_chemical_formula_sum            'C48 H66 Cl20 N24 O3 Tc2'
_chemical_formula_weight         1932.24
_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'
Cl Cl 0.1484 0.1585 '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'
Tc Tc -1.4390 0.7593 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   28.5623(9)
_cell_length_b                   12.8616(4)
_cell_length_c                   22.0923(7)
_cell_angle_alpha                90
_cell_angle_beta                 108.1910(10)
_cell_angle_gamma                90
_cell_volume                     7710.1(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.43
_cell_measurement_theta_min      3.22
_shelx_estimated_absorpt_T_max   0.809
_shelx_estimated_absorpt_T_min   0.732
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_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   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            205070
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.996
_diffrn_reflns_theta_min         4.148
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_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                23824
_reflns_number_total             33002
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    ?
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         33002
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0216P)²+3.5907P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0735
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O1W-H1A = O1W-H1B = O2W-H2A = O2W-H2B = O3W-H3A = O3W-H3B
 0.85 with sigma of 0.02
 H1A-H1B = H2A-H2B = H3A-H3B
 1.35 with sigma of 0.02
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N5(H5), N7(H7), N9(H9), N11(H11), N13(H13), N15(H15),
 N17(H17), N19(H19), N21(H21), N23(H23), C1(H1C), C2(H2C), C3(H3C), C4(H4A),
 C5(H5A), C6(H6A), C7(H7A), C8(H8A), C9(H9A), C10(H10A), C11(H11A), C12(H12A),
 C13(H13A), C14(H14A), C15(H15A), C16(H16A), C17(H17A), C18(H18A), C19(H19A),
 C20(H20A), C21(H21A), C22(H22A), C23(H23A), C24(H24A), C25(H25A), C26(H26A),
 C27(H27A), C28(H28A), C29(H29A), C30(H30A), C31(H31A), C32(H32A), C33(H33A),
 C34(H34A), C35(H35A), C36(H36A), C37(H37A), C38(H38A), C39(H39A), C40(H40A),
 C41(H41A), C42(H42A), C43(H43A), C44(H44A), C45(H45A), C46(H46A), C47(H47A),
 C48(H48A)
;
_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
Tc1 Tc 0.62908(2) 0.86988(2) 0.25649(2) 0.00818(3) Uani 1 1 d . . . . .
Tc2 Tc 0.87696(2) 0.10999(2) 0.75457(2) 0.00813(3) Uani 1 1 d . . . . .
Cl1 Cl 0.56068(2) 0.33573(4) 0.16484(2) 0.02475(9) Uani 1 1 d . . . . .
Cl2 Cl 0.68816(2) 0.40432(4) 0.33650(2) 0.02166(9) Uani 1 1 d . . . . .
Cl3 Cl 0.79938(2) 0.63040(3) 0.44361(2) 0.01255(7) Uani 1 1 d . . . . .
Cl4 Cl 0.84485(2) 0.63668(3) 0.61887(2) 0.01783(8) Uani 1 1 d . . . . .
Cl5 Cl 0.69948(2) 0.37483(3) 0.57146(2) 0.01497(7) Uani 1 1 d . . . . .
Cl6 Cl 0.54973(2) 0.11190(3) 0.42833(2) 0.01463(7) Uani 1 1 d . . . . .
Cl7 Cl 0.90584(2) 0.62933(3) 0.88770(2) 0.01767(8) Uani 1 1 d . . . . .
Cl8 Cl 0.95437(2) 0.63293(3) 1.06321(2) 0.01307(7) Uani 1 1 d . . . . .
Cl11 Cl 0.54678(2) 0.85196(3) 0.25719(2) 0.01296(7) Uani 1 1 d . . . . .
Cl12 Cl 0.65540(2) 0.74713(3) 0.33912(2) 0.01353(7) Uani 1 1 d . . . . .
Cl13 Cl 0.63983(2) 1.00497(3) 0.33112(2) 0.01287(7) Uani 1 1 d . . . . .
Cl14 Cl 0.60628(2) 0.99305(3) 0.17386(2) 0.01331(7) Uani 1 1 d . . . . .
Cl15 Cl 0.61441(2) 0.73554(3) 0.18072(2) 0.01354(7) Uani 1 1 d . . . . .
Cl16 Cl 0.71161(2) 0.88545(3) 0.25670(2) 0.01211(7) Uani 1 1 d . . . . .
Cl21 Cl 0.79441(2) 0.12098(3) 0.75512(2) 0.01448(7) Uani 1 1 d . . . . .
Cl22 Cl 0.90160(2) 0.23772(3) 0.83474(2) 0.01345(7) Uani 1 1 d . . . . .
Cl23 Cl 0.89082(2) -0.02012(3) 0.83309(2) 0.01342(7) Uani 1 1 d . . . . .
Cl24 Cl 0.85485(2) -0.01710(3) 0.67456(2) 0.01388(7) Uani 1 1 d . . . . .
Cl25 Cl 0.85977(2) 0.24109(3) 0.67703(2) 0.01343(7) Uani 1 1 d . . . . .
Cl26 Cl 0.95928(2) 0.09744(3) 0.75345(2) 0.01266(7) Uani 1 1 d . . . . .
O1W O 0.66742(5) 0.39899(13) 0.18327(6) 0.0302(3) Uani 1 1 d D . . . .
H1A H 0.6385(5) 0.3938(19) 0.1731(11) 0.045 Uiso 1 1 d D U . . .
H1B H 0.6800(8) 0.3950(19) 0.2224(7) 0.045 Uiso 1 1 d D U . . .
O2W O 0.89101(7) 0.52547(13) 0.75172(8) 0.0460(4) Uani 1 1 d D . . . .
H2A H 0.8945(10) 0.5684(19) 0.7838(9) 0.069 Uiso 1 1 d D U . . .
H2B H 0.8775(10) 0.5665(19) 0.7183(9) 0.069 Uiso 1 1 d D U . . .
O3W O 0.58294(5) 0.31710(11) 0.31809(6) 0.0221(3) Uani 1 1 d D . . . .
H3A H 0.6121(5) 0.3268(18) 0.3277(10) 0.033 Uiso 1 1 d D U . . .
H3B H 0.5701(7) 0.3269(17) 0.2797(7) 0.033 Uiso 1 1 d D U . . .
N1 N 0.70100(5) 0.38309(10) 0.08339(7) 0.0156(3) Uani 1 1 d . . . . .
H1 H 0.692839 0.393277 0.118186 0.019 Uiso 1 1 calc R U . . .
N2 N 0.72620(5) 0.35180(11) -0.02486(7) 0.0198(3) Uani 1 1 d . . . . .
N3 N 0.54739(5) 0.36063(10) 0.41470(7) 0.0157(3) Uani 1 1 d . . . . .
H3 H 0.556620 0.357032 0.380300 0.019 Uiso 1 1 calc R U . . .
N4 N 0.51845(6) 0.37247(12) 0.52132(7) 0.0215(3) Uani 1 1 d . . . . .
N5 N 0.46137(5) 0.35473(11) 0.06409(7) 0.0179(3) Uani 1 1 d . . . . .
H5 H 0.488079 0.339344 0.095614 0.021 Uiso 1 1 calc R U . . .
N6 N 0.37848(6) 0.40004(12) -0.03396(7) 0.0223(3) Uani 1 1 d . . . . .
N7 N 0.78764(5) 0.37144(10) 0.43395(7) 0.0155(3) Uani 1 1 d . . . . .
H7 H 0.760299 0.365682 0.401754 0.019 Uiso 1 1 calc R U . . .
N8 N 0.87220(5) 0.38792(11) 0.53374(7) 0.0192(3) Uani 1 1 d . . . . .
N9 N 0.91251(5) 0.62042(10) 0.53193(7) 0.0137(3) Uani 1 1 d . . . . .
H9 H 0.882506 0.620543 0.534935 0.016 Uiso 1 1 calc R U . . .
N10 N 1.00548(5) 0.61835(11) 0.52248(7) 0.0162(3) Uani 1 1 d . . . . .
N11 N 0.72867(5) 0.61730(10) 0.52508(7) 0.0163(3) Uani 1 1 d . . . . .
H11 H 0.759394 0.618797 0.524756 0.020 Uiso 1 1 calc R U . . .
N12 N 0.63323(5) 0.62036(11) 0.52520(7) 0.0182(3) Uani 1 1 d . . . . .
N13 N 0.76625(5) 0.64743(11) 0.30059(6) 0.0157(3) Uani 1 1 d . . . . .
H13 H 0.769050 0.636624 0.340905 0.019 Uiso 1 1 calc R U . . .
N14 N 0.75798(5) 0.67859(11) 0.17595(6) 0.0169(3) Uani 1 1 d . . . . .
N15 N 0.73471(6) 0.37147(11) 0.71293(7) 0.0213(3) Uani 1 1 d . . . . .
H15 H 0.718095 0.367979 0.672080 0.026 Uiso 1 1 calc R U . . .
N16 N 0.78636(6) 0.38062(12) 0.83927(7) 0.0230(3) Uani 1 1 d . . . . .
N17 N 1.02140(5) 0.62213(10) 0.97212(7) 0.0173(3) Uani 1 1 d . . . . .
H17 H 0.990533 0.624730 0.971774 0.021 Uiso 1 1 calc R U . . .
N18 N 1.11720(5) 0.61818(11) 0.97339(7) 0.0159(3) Uani 1 1 d . . . . .
N19 N 0.98570(5) 0.65836(11) 1.20610(6) 0.0160(3) Uani 1 1 d . . . . .
H19 H 0.982436 0.650427 1.165424 0.019 Uiso 1 1 calc R U . . .
N20 N 0.99535(5) 0.68078(12) 1.33179(7) 0.0197(3) Uani 1 1 d . . . . .
N21 N 0.83853(5) 0.61853(10) 0.97495(7) 0.0137(3) Uani 1 1 d . . . . .
H21 H 0.868394 0.618383 0.971475 0.016 Uiso 1 1 calc R U . . .
N22 N 0.74596(5) 0.61710(11) 0.98573(7) 0.0162(3) Uani 1 1 d . . . . .
N23 N 0.51218(5) 0.10173(10) 0.28596(7) 0.0165(3) Uani 1 1 d . . . . .
H23 H 0.532138 0.109281 0.325103 0.020 Uiso 1 1 calc R U . . .
N24 N 0.45037(5) 0.07829(11) 0.16500(7) 0.0175(3) Uani 1 1 d . . . . .
C1 C 0.66573(6) 0.37040(13) 0.02803(8) 0.0178(3) Uani 1 1 d . . . . .
H1C H 0.631975 0.371711 0.025801 0.021 Uiso 1 1 calc R U . . .
C2 C 0.67918(6) 0.35530(14) -0.02601(8) 0.0199(3) Uani 1 1 d . . . . .
H2C H 0.654021 0.347043 -0.065685 0.024 Uiso 1 1 calc R U . . .
C3 C 0.76049(6) 0.36477(13) 0.03206(8) 0.0174(3) Uani 1 1 d . . . . .
H3C H 0.794276 0.362909 0.034466 0.021 Uiso 1 1 calc R U . . .
C4 C 0.74859(6) 0.38068(12) 0.08719(8) 0.0163(3) Uani 1 1 d . . . . .
H4A H 0.773609 0.389710 0.126905 0.020 Uiso 1 1 calc R U . . .
C5 C 0.58153(6) 0.36613(13) 0.47167(8) 0.0191(3) Uani 1 1 d . . . . .
H5A H 0.615616 0.366216 0.475591 0.023 Uiso 1 1 calc R U . . .
C6 C 0.56605(7) 0.37170(14) 0.52493(9) 0.0233(4) Uani 1 1 d . . . . .
H6A H 0.590203 0.375129 0.565739 0.028 Uiso 1 1 calc R U . . .
C7 C 0.48551(6) 0.36717(13) 0.46304(8) 0.0173(3) Uani 1 1 d . . . . .
H7A H 0.451394 0.368038 0.458911 0.021 Uiso 1 1 calc R U . . .
C8 C 0.49949(6) 0.36048(13) 0.40879(8) 0.0169(3) Uani 1 1 d . . . . .
H8A H 0.475432 0.355853 0.367959 0.020 Uiso 1 1 calc R U . . .
C9 C 0.41791(6) 0.35305(13) 0.07420(8) 0.0174(3) Uani 1 1 d . . . . .
H9A H 0.415432 0.336652 0.115019 0.021 Uiso 1 1 calc R U . . .
C10 C 0.37640(6) 0.37583(13) 0.02370(8) 0.0183(3) Uani 1 1 d . . . . .
H10A H 0.345139 0.374136 0.030427 0.022 Uiso 1 1 calc R U . . .
C11 C 0.42301(7) 0.40185(14) -0.04142(9) 0.0246(4) Uani 1 1 d . . . . .
H11A H 0.425609 0.419500 -0.082004 0.029 Uiso 1 1 calc R U . . .
C12 C 0.46552(7) 0.37913(14) 0.00740(9) 0.0225(4) Uani 1 1 d . . . . .
H12A H 0.496804 0.380854 0.000766 0.027 Uiso 1 1 calc R U . . .
C13 C 0.83075(6) 0.37059(13) 0.42250(8) 0.0165(3) Uani 1 1 d . . . . .
H13A H 0.832311 0.364799 0.380305 0.020 Uiso 1 1 calc R U . . .
C14 C 0.87325(6) 0.37845(12) 0.47417(8) 0.0168(3) Uani 1 1 d . . . . .
H14A H 0.904284 0.377023 0.466798 0.020 Uiso 1 1 calc R U . . .
C15 C 0.82804(7) 0.38916(13) 0.54234(8) 0.0200(3) Uani 1 1 d . . . . .
H15A H 0.826301 0.396126 0.584399 0.024 Uiso 1 1 calc R U . . .
C16 C 0.78471(6) 0.38069(12) 0.49240(8) 0.0181(3) Uani 1 1 d . . . . .
H16A H 0.753668 0.381475 0.499749 0.022 Uiso 1 1 calc R U . . .
C17 C 0.91892(6) 0.64134(12) 0.47594(8) 0.0148(3) Uani 1 1 d . . . . .
H17A H 0.891649 0.656874 0.439530 0.018 Uiso 1 1 calc R U . . .
C18 C 0.96645(6) 0.63979(13) 0.47240(8) 0.0152(3) Uani 1 1 d . . . . .
H18A H 0.971411 0.654593 0.432718 0.018 Uiso 1 1 calc R U . . .
C19 C 0.99724(6) 0.59788(13) 0.57778(8) 0.0164(3) Uani 1 1 d . . . . .
H19A H 1.024481 0.581893 0.614136 0.020 Uiso 1 1 calc R U . . .
C20 C 0.95070(6) 0.59921(12) 0.58371(8) 0.0151(3) Uani 1 1 d . . . . .
H20A H 0.945776 0.585431 0.623537 0.018 Uiso 1 1 calc R U . . .
C21 C 0.71939(6) 0.63112(13) 0.57980(8) 0.0176(3) Uani 1 1 d . . . . .
H21A H 0.745457 0.639594 0.618598 0.021 Uiso 1 1 calc R U . . .
C22 C 0.67065(6) 0.63283(13) 0.57878(8) 0.0179(3) Uani 1 1 d . . . . .
H22A H 0.663624 0.643257 0.617629 0.021 Uiso 1 1 calc R U . . .
C23 C 0.64485(6) 0.60328(13) 0.47184(8) 0.0182(3) Uani 1 1 d . . . . .
H23A H 0.618983 0.592098 0.433161 0.022 Uiso 1 1 calc R U . . .
C24 C 0.69269(6) 0.60127(13) 0.47074(8) 0.0186(3) Uani 1 1 d . . . . .
H24A H 0.699878 0.588762 0.432192 0.022 Uiso 1 1 calc R U . . .
C25 C 0.72680(6) 0.61190(13) 0.25592(8) 0.0175(3) Uani 1 1 d . . . . .
H25A H 0.701611 0.575814 0.266980 0.021 Uiso 1 1 calc R U . . .
C26 C 0.72326(6) 0.62874(13) 0.19280(8) 0.0164(3) Uani 1 1 d . . . . .
H26A H 0.695071 0.603816 0.160453 0.020 Uiso 1 1 calc R U . . .
C27 C 0.79696(6) 0.71397(13) 0.22273(8) 0.0180(3) Uani 1 1 d . . . . .
H27A H 0.822087 0.750530 0.211809 0.022 Uiso 1 1 calc R U . . .
C28 C 0.80177(6) 0.69903(13) 0.28610(8) 0.0167(3) Uani 1 1 d . . . . .
H28A H 0.829650 0.724816 0.318599 0.020 Uiso 1 1 calc R U . . .
C29 C 0.78124(7) 0.40292(15) 0.73060(9) 0.0245(4) Uani 1 1 d . . . . .
H29A H 0.796606 0.422116 0.699813 0.029 Uiso 1 1 calc R U . . .
C30 C 0.80673(7) 0.40702(15) 0.79484(9) 0.0247(4) Uani 1 1 d . . . . .
H30A H 0.840074 0.429533 0.807896 0.030 Uiso 1 1 calc R U . . .
C31 C 0.73966(7) 0.34996(14) 0.81932(8) 0.0217(4) Uani 1 1 d . . . . .
H31A H 0.724237 0.330613 0.850014 0.026 Uiso 1 1 calc R U . . .
C32 C 0.71261(7) 0.34518(13) 0.75520(8) 0.0208(3) Uani 1 1 d . . . . .
H32A H 0.679122 0.323633 0.741970 0.025 Uiso 1 1 calc R U . . .
C33 C 1.03104(6) 0.61840(13) 0.91711(8) 0.0175(3) Uani 1 1 d . . . . .
H33A H 1.005145 0.616817 0.877731 0.021 Uiso 1 1 calc R U . . .
C34 C 1.07992(6) 0.61687(13) 0.91877(8) 0.0176(3) Uani 1 1 d . . . . .
H34A H 1.087217 0.614817 0.879681 0.021 Uiso 1 1 calc R U . . .
C35 C 1.10549(6) 0.61998(13) 1.02733(8) 0.0175(3) Uani 1 1 d . . . . .
H35A H 1.131313 0.619830 1.066792 0.021 Uiso 1 1 calc R U . . .
C36 C 1.05738(7) 0.62205(13) 1.02803(9) 0.0204(3) Uani 1 1 d . . . . .
H36A H 1.050012 0.623380 1.067088 0.024 Uiso 1 1 calc R U . . .
C37 C 1.02731(6) 0.62802(13) 1.24927(8) 0.0181(3) Uani 1 1 d . . . . .
H37A H 1.053459 0.598864 1.236818 0.022 Uiso 1 1 calc R U . . .
C38 C 1.03134(6) 0.64023(13) 1.31293(8) 0.0184(3) Uani 1 1 d . . . . .
H38A H 1.060877 0.618885 1.344302 0.022 Uiso 1 1 calc R U . . .
C39 C 0.95440(6) 0.71069(14) 1.28651(8) 0.0200(3) Uani 1 1 d . . . . .
H39A H 0.928248 0.740052 1.298875 0.024 Uiso 1 1 calc R U . . .
C40 C 0.94875(6) 0.70047(13) 1.22254(8) 0.0173(3) Uani 1 1 d . . . . .
H40A H 0.919426 0.722740 1.191109 0.021 Uiso 1 1 calc R U . . .
C41 C 0.83282(6) 0.63638(12) 1.03140(8) 0.0151(3) Uani 1 1 d . . . . .
H41A H 0.860477 0.649233 1.067850 0.018 Uiso 1 1 calc R U . . .
C42 C 0.78551(6) 0.63577(12) 1.03578(7) 0.0143(3) Uani 1 1 d . . . . .
H42A H 0.781070 0.649154 1.075929 0.017 Uiso 1 1 calc R U . . .
C43 C 0.75363(6) 0.59951(13) 0.93001(8) 0.0170(3) Uani 1 1 d . . . . .
H43A H 0.726071 0.585589 0.893634 0.020 Uiso 1 1 calc R U . . .
C44 C 0.79990(6) 0.60076(13) 0.92328(8) 0.0161(3) Uani 1 1 d . . . . .
H44A H 0.804292 0.589296 0.882912 0.019 Uiso 1 1 calc R U . . .
C45 C 0.46563(6) 0.07352(13) 0.27703(8) 0.0185(3) Uani 1 1 d . . . . .
H45A H 0.453937 0.061223 0.312203 0.022 Uiso 1 1 calc R U . . .
C46 C 0.43483(6) 0.06266(13) 0.21524(8) 0.0192(3) Uani 1 1 d . . . . .
H46A H 0.401449 0.043392 0.208312 0.023 Uiso 1 1 calc R U . . .
C47 C 0.49711(6) 0.10680(12) 0.17629(8) 0.0161(3) Uani 1 1 d . . . . .
H47A H 0.508849 0.119407 0.141186 0.019 Uiso 1 1 calc R U . . .
C48 C 0.52926(6) 0.11872(12) 0.23757(8) 0.0160(3) Uani 1 1 d . . . . .
H48A H 0.562591 0.138501 0.244640 0.019 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 Cl11 2.3668(4) . ?
Tc1 Cl12 2.3523(4) . ?
Tc1 Cl13 2.3485(4) . ?
Tc1 Cl14 2.3503(4) . ?
Tc1 Cl15 2.3505(4) . ?
Tc1 Cl16 2.3641(4) . ?
Tc2 Cl21 2.3658(4) . ?
Tc2 Cl22 2.3564(4) . ?
Tc2 Cl23 2.3531(4) . ?
Tc2 Cl24 2.3448(4) . ?
Tc2 Cl25 2.3438(4) . ?
Tc2 Cl26 2.3647(4) . ?
O1W H1A 0.789(15) . ?
O1W H1B 0.828(15) . ?
O2W H2A 0.879(16) . ?
O2W H2B 0.891(16) . ?
O3W H3A 0.801(14) . ?
O3W H3B 0.822(14) . ?
N1 H1 0.8800 . ?
N1 C1 1.330(2) . ?
N1 C4 1.336(2) . ?
N2 C2 1.336(2) . ?
N2 C3 1.342(2) . ?
N3 H3 0.8800 . ?
N3 C5 1.332(2) . ?
N3 C8 1.333(2) . ?
N4 C6 1.337(2) . ?
N4 C7 1.338(2) . ?
N5 H5 0.8800 . ?
N5 C9 1.328(2) . ?
N5 C12 1.332(2) . ?
N6 C10 1.331(2) . ?
N6 C11 1.333(2) . ?
N7 H7 0.8800 . ?
N7 C13 1.332(2) . ?
N7 C16 1.325(2) . ?
N8 C14 1.331(2) . ?
N8 C15 1.333(2) . ?
N9 H9 0.8800 . ?
N9 C17 1.333(2) . ?
N9 C20 1.339(2) . ?
N10 C18 1.331(2) . ?
N10 C19 1.340(2) . ?
N11 H11 0.8800 . ?
N11 C21 1.328(2) . ?
N11 C24 1.330(2) . ?
N12 C22 1.334(2) . ?
N12 C23 1.339(2) . ?
N13 H13 0.8800 . ?
N13 C25 1.326(2) . ?
N13 C28 1.332(2) . ?
N14 C26 1.328(2) . ?
N14 C27 1.340(2) . ?
N15 H15 0.8800 . ?
N15 C29 1.326(2) . ?
N15 C32 1.324(2) . ?
N16 C30 1.332(2) . ?
N16 C31 1.327(2) . ?
N17 H17 0.8800 . ?
N17 C33 1.328(2) . ?
N17 C36 1.338(2) . ?
N18 C34 1.337(2) . ?
N18 C35 1.335(2) . ?
N19 H19 0.8800 . ?
N19 C37 1.329(2) . ?
N19 C40 1.334(2) . ?
N20 C38 1.330(2) . ?
N20 C39 1.337(2) . ?
N21 H21 0.8800 . ?
N21 C41 1.327(2) . ?
N21 C44 1.337(2) . ?
N22 C42 1.333(2) . ?
N22 C43 1.335(2) . ?
N23 H23 0.8800 . ?
N23 C45 1.332(2) . ?
N23 C48 1.325(2) . ?
N24 C46 1.333(2) . ?
N24 C47 1.331(2) . ?
C1 H1C 0.9500 . ?
C1 C2 1.377(2) . ?
C2 H2C 0.9500 . ?
C3 H3C 0.9500 . ?
C3 C4 1.378(2) . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
C5 C6 1.382(3) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C7 C8 1.379(2) . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?
C9 C10 1.382(2) . ?
C10 H10A 0.9500 . ?
C11 H11A 0.9500 . ?
C11 C12 1.380(3) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C13 C14 1.386(2) . ?
C14 H14A 0.9500 . ?
C15 H15A 0.9500 . ?
C15 C16 1.382(2) . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9500 . ?
C17 C18 1.384(2) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C19 C20 1.376(2) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
C21 C22 1.385(2) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C23 C24 1.374(2) . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9500 . ?
C25 C26 1.383(2) . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9500 . ?
C27 C28 1.377(2) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C29 C30 1.379(3) . ?
C30 H30A 0.9500 . ?
C31 H31A 0.9500 . ?
C31 C32 1.387(2) . ?
C32 H32A 0.9500 . ?
C33 H33A 0.9500 . ?
C33 C34 1.385(2) . ?
C34 H34A 0.9500 . ?
C35 H35A 0.9500 . ?
C35 C36 1.379(2) . ?
C36 H36A 0.9500 . ?
C37 H37A 0.9500 . ?
C37 C38 1.384(2) . ?
C38 H38A 0.9500 . ?
C39 H39A 0.9500 . ?
C39 C40 1.378(2) . ?
C40 H40A 0.9500 . ?
C41 H41A 0.9500 . ?
C41 C42 1.385(2) . ?
C42 H42A 0.9500 . ?
C43 H43A 0.9500 . ?
C43 C44 1.376(2) . ?
C44 H44A 0.9500 . ?
C45 H45A 0.9500 . ?
C45 C46 1.381(2) . ?
C46 H46A 0.9500 . ?
C47 H47A 0.9500 . ?
C47 C48 1.387(2) . ?
C48 H48A 0.9500 . ?

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
Cl12 Tc1 Cl11 90.398(14) . . ?
Cl12 Tc1 Cl16 88.765(13) . . ?
Cl13 Tc1 Cl11 88.847(13) . . ?
Cl13 Tc1 Cl12 90.669(14) . . ?
Cl13 Tc1 Cl14 89.450(14) . . ?
Cl13 Tc1 Cl15 177.378(14) . . ?
Cl13 Tc1 Cl16 91.388(13) . . ?
Cl14 Tc1 Cl11 92.050(14) . . ?
Cl14 Tc1 Cl12 177.551(14) . . ?
Cl14 Tc1 Cl15 89.875(14) . . ?
Cl14 Tc1 Cl16 88.786(13) . . ?
Cl15 Tc1 Cl11 88.646(13) . . ?
Cl15 Tc1 Cl12 90.115(14) . . ?
Cl15 Tc1 Cl16 91.130(13) . . ?
Cl16 Tc1 Cl11 179.134(15) . . ?
Cl22 Tc2 Cl21 91.080(14) . . ?
Cl22 Tc2 Cl26 89.472(14) . . ?
Cl23 Tc2 Cl21 88.706(14) . . ?
Cl23 Tc2 Cl22 89.985(14) . . ?
Cl23 Tc2 Cl26 91.153(14) . . ?
Cl24 Tc2 Cl21 90.643(14) . . ?
Cl24 Tc2 Cl22 178.270(14) . . ?
Cl24 Tc2 Cl23 90.212(14) . . ?
Cl24 Tc2 Cl26 88.806(14) . . ?
Cl25 Tc2 Cl21 88.798(14) . . ?
Cl25 Tc2 Cl22 89.599(14) . . ?
Cl25 Tc2 Cl23 177.462(14) . . ?
Cl25 Tc2 Cl24 90.279(14) . . ?
Cl25 Tc2 Cl26 91.346(14) . . ?
Cl26 Tc2 Cl21 179.431(15) . . ?
H1A O1W H1B 112(2) . . ?
H2A O2W H2B 101.9(19) . . ?
H3A O3W H3B 109.9(18) . . ?
C1 N1 H1 119.4 . . ?
C1 N1 C4 121.26(15) . . ?
C4 N1 H1 119.4 . . ?
C2 N2 C3 116.68(15) . . ?
C5 N3 H3 119.4 . . ?
C5 N3 C8 121.26(15) . . ?
C8 N3 H3 119.4 . . ?
C6 N4 C7 116.96(15) . . ?
C9 N5 H5 119.2 . . ?
C9 N5 C12 121.61(15) . . ?
C12 N5 H5 119.2 . . ?
C10 N6 C11 116.88(16) . . ?
C13 N7 H7 119.0 . . ?
C16 N7 H7 119.0 . . ?
C16 N7 C13 121.94(15) . . ?
C14 N8 C15 117.16(15) . . ?
C17 N9 H9 119.2 . . ?
C17 N9 C20 121.51(14) . . ?
C20 N9 H9 119.2 . . ?
C18 N10 C19 117.28(14) . . ?
C21 N11 H11 119.2 . . ?
C21 N11 C24 121.65(14) . . ?
C24 N11 H11 119.2 . . ?
C22 N12 C23 116.79(14) . . ?
C25 N13 H13 119.1 . . ?
C25 N13 C28 121.79(14) . . ?
C28 N13 H13 119.1 . . ?
C26 N14 C27 117.46(14) . . ?
C29 N15 H15 119.2 . . ?
C32 N15 H15 119.2 . . ?
C32 N15 C29 121.68(16) . . ?
C31 N16 C30 117.13(16) . . ?
C33 N17 H17 119.1 . . ?
C33 N17 C36 121.74(15) . . ?
C36 N17 H17 119.1 . . ?
C35 N18 C34 117.07(14) . . ?
C37 N19 H19 119.0 . . ?
C37 N19 C40 122.02(15) . . ?
C40 N19 H19 119.0 . . ?
C38 N20 C39 117.37(15) . . ?
C41 N21 H21 119.3 . . ?
C41 N21 C44 121.43(14) . . ?
C44 N21 H21 119.3 . . ?
C42 N22 C43 117.07(14) . . ?
C45 N23 H23 119.1 . . ?
C48 N23 H23 119.1 . . ?
C48 N23 C45 121.83(15) . . ?
C47 N24 C46 117.44(14) . . ?
N1 C1 H1C 120.7 . . ?
N1 C1 C2 118.57(15) . . ?
C2 C1 H1C 120.7 . . ?
N2 C2 C1 122.61(15) . . ?
N2 C2 H2C 118.7 . . ?
C1 C2 H2C 118.7 . . ?
N2 C3 H3C 118.7 . . ?
N2 C3 C4 122.52(15) . . ?
C4 C3 H3C 118.7 . . ?
N1 C4 C3 118.35(15) . . ?
N1 C4 H4A 120.8 . . ?
C3 C4 H4A 120.8 . . ?
N3 C5 H5A 120.9 . . ?
N3 C5 C6 118.21(16) . . ?
C6 C5 H5A 120.9 . . ?
N4 C6 C5 122.65(16) . . ?
N4 C6 H6A 118.7 . . ?
C5 C6 H6A 118.7 . . ?
N4 C7 H7A 118.9 . . ?
N4 C7 C8 122.13(15) . . ?
C8 C7 H7A 118.9 . . ?
N3 C8 C7 118.78(15) . . ?
N3 C8 H8A 120.6 . . ?
C7 C8 H8A 120.6 . . ?
N5 C9 H9A 120.9 . . ?
N5 C9 C10 118.16(16) . . ?
C10 C9 H9A 120.9 . . ?
N6 C10 C9 122.60(16) . . ?
N6 C10 H10A 118.7 . . ?
C9 C10 H10A 118.7 . . ?
N6 C11 H11A 118.7 . . ?
N6 C11 C12 122.70(17) . . ?
C12 C11 H11A 118.7 . . ?
N5 C12 C11 118.04(16) . . ?
N5 C12 H12A 121.0 . . ?
C11 C12 H12A 121.0 . . ?
N7 C13 H13A 121.1 . . ?
N7 C13 C14 117.83(15) . . ?
C14 C13 H13A 121.1 . . ?
N8 C14 C13 122.43(15) . . ?
N8 C14 H14A 118.8 . . ?
C13 C14 H14A 118.8 . . ?
N8 C15 H15A 118.8 . . ?
N8 C15 C16 122.46(16) . . ?
C16 C15 H15A 118.8 . . ?
N7 C16 C15 118.17(15) . . ?
N7 C16 H16A 120.9 . . ?
C15 C16 H16A 120.9 . . ?
N9 C17 H17A 121.0 . . ?
N9 C17 C18 118.08(14) . . ?
C18 C17 H17A 121.0 . . ?
N10 C18 C17 122.52(15) . . ?
N10 C18 H18A 118.7 . . ?
C17 C18 H18A 118.7 . . ?
N10 C19 H19A 118.9 . . ?
N10 C19 C20 122.28(15) . . ?
C20 C19 H19A 118.9 . . ?
N9 C20 C19 118.33(15) . . ?
N9 C20 H20A 120.8 . . ?
C19 C20 H20A 120.8 . . ?
N11 C21 H21A 120.9 . . ?
N11 C21 C22 118.19(15) . . ?
C22 C21 H21A 120.9 . . ?
N12 C22 C21 122.37(16) . . ?
N12 C22 H22A 118.8 . . ?
C21 C22 H22A 118.8 . . ?
N12 C23 H23A 118.7 . . ?
N12 C23 C24 122.66(16) . . ?
C24 C23 H23A 118.7 . . ?
N11 C24 C23 118.26(15) . . ?
N11 C24 H24A 120.9 . . ?
C23 C24 H24A 120.9 . . ?
N13 C25 H25A 120.9 . . ?
N13 C25 C26 118.30(15) . . ?
C26 C25 H25A 120.9 . . ?
N14 C26 C25 122.15(16) . . ?
N14 C26 H26A 118.9 . . ?
C25 C26 H26A 118.9 . . ?
N14 C27 H27A 118.9 . . ?
N14 C27 C28 122.13(16) . . ?
C28 C27 H27A 118.9 . . ?
N13 C28 C27 118.17(15) . . ?
N13 C28 H28A 120.9 . . ?
C27 C28 H28A 120.9 . . ?
N15 C29 H29A 120.9 . . ?
N15 C29 C30 118.24(18) . . ?
C30 C29 H29A 120.9 . . ?
N16 C30 C29 122.47(18) . . ?
N16 C30 H30A 118.8 . . ?
C29 C30 H30A 118.8 . . ?
N16 C31 H31A 118.9 . . ?
N16 C31 C32 122.28(17) . . ?
C32 C31 H31A 118.9 . . ?
N15 C32 C31 118.21(17) . . ?
N15 C32 H32A 120.9 . . ?
C31 C32 H32A 120.9 . . ?
N17 C33 H33A 120.9 . . ?
N17 C33 C34 118.12(15) . . ?
C34 C33 H33A 120.9 . . ?
N18 C34 C33 122.41(15) . . ?
N18 C34 H34A 118.8 . . ?
C33 C34 H34A 118.8 . . ?
N18 C35 H35A 118.7 . . ?
N18 C35 C36 122.58(16) . . ?
C36 C35 H35A 118.7 . . ?
N17 C36 C35 118.07(16) . . ?
N17 C36 H36A 121.0 . . ?
C35 C36 H36A 121.0 . . ?
N19 C37 H37A 121.0 . . ?
N19 C37 C38 117.91(16) . . ?
C38 C37 H37A 121.0 . . ?
N20 C38 C37 122.39(16) . . ?
N20 C38 H38A 118.8 . . ?
C37 C38 H38A 118.8 . . ?
N20 C39 H39A 118.8 . . ?
N20 C39 C40 122.36(16) . . ?
C40 C39 H39A 118.8 . . ?
N19 C40 C39 117.96(16) . . ?
N19 C40 H40A 121.0 . . ?
C39 C40 H40A 121.0 . . ?
N21 C41 H41A 120.9 . . ?
N21 C41 C42 118.26(15) . . ?
C42 C41 H41A 120.9 . . ?
N22 C42 C41 122.40(15) . . ?
N22 C42 H42A 118.8 . . ?
C41 C42 H42A 118.8 . . ?
N22 C43 H43A 118.7 . . ?
N22 C43 C44 122.51(15) . . ?
C44 C43 H43A 118.7 . . ?
N21 C44 C43 118.32(15) . . ?
N21 C44 H44A 120.8 . . ?
C43 C44 H44A 120.8 . . ?
N23 C45 H45A 120.9 . . ?
N23 C45 C46 118.19(16) . . ?
C46 C45 H45A 120.9 . . ?
N24 C46 C45 122.19(16) . . ?
N24 C46 H46A 118.9 . . ?
C45 C46 H46A 118.9 . . ?
N24 C47 H47A 118.9 . . ?
N24 C47 C48 122.22(16) . . ?
C48 C47 H47A 118.9 . . ?
N23 C48 C47 118.11(15) . . ?
N23 C48 H48A 120.9 . . ?
C47 C48 H48A 120.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1A Cl1 0.789(15) 2.297(17) 3.0572(14) 162(2) . yes
O1W H1B Cl2 0.828(15) 2.461(17) 3.2502(14) 160(2) . yes
O2W H2A Cl7 0.879(16) 2.350(16) 3.1927(17) 161(2) . yes
O2W H2B Cl4 0.891(16) 2.287(16) 3.1593(16) 166(2) . yes
O3W H3A Cl2 0.801(14) 2.344(16) 3.1135(13) 161(2) . yes
O3W H3B Cl1 0.822(14) 2.469(16) 3.2528(14) 159.7(19) . yes
N1 H1 O1W 0.88 1.80 2.6743(19) 170.1 . yes
N3 H3 O3W 0.88 1.83 2.6931(19) 164.9 . yes
N5 H5 Cl1 0.88 2.16 3.0196(15) 165.7 . yes
N7 H7 Cl2 0.88 2.17 3.0112(14) 159.4 . yes
N9 H9 Cl3 0.88 2.59 3.2138(13) 128.2 . yes
N9 H9 Cl4 0.88 2.43 3.1282(14) 137.1 . yes
N11 H11 Cl3 0.88 2.41 3.1009(14) 135.4 . yes
N11 H11 Cl4 0.88 2.68 3.3277(14) 131.7 . yes
N13 H13 Cl3 0.88 2.16 3.0100(14) 161.4 . yes
N15 H15 Cl5 0.88 2.12 2.9697(15) 162.1 . yes
N17 H17 Cl7 0.88 2.55 3.2463(15) 136.7 . yes
N17 H17 Cl8 0.88 2.54 3.1845(14) 130.5 . yes
N19 H19 Cl8 0.88 2.16 3.0182(14) 165.1 . yes
N21 H21 Cl7 0.88 2.41 3.1217(14) 137.8 . yes
N21 H21 Cl8 0.88 2.66 3.2794(14) 128.5 . yes
N23 H23 Cl6 0.88 2.18 2.9922(14) 153.9 . yes

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
N1 C1 C2 N2 0.7(3) . . . . ?
N2 C3 C4 N1 0.1(2) . . . . ?
N3 C5 C6 N4 -0.5(3) . . . . ?
N4 C7 C8 N3 -0.9(3) . . . . ?
N5 C9 C10 N6 -0.6(3) . . . . ?
N6 C11 C12 N5 -0.1(3) . . . . ?
N7 C13 C14 N8 -0.8(2) . . . . ?
N8 C15 C16 N7 -0.3(2) . . . . ?
N9 C17 C18 N10 0.0(2) . . . . ?
N10 C19 C20 N9 0.9(2) . . . . ?
N11 C21 C22 N12 0.5(3) . . . . ?
N12 C23 C24 N11 -0.2(3) . . . . ?
N13 C25 C26 N14 0.2(2) . . . . ?
N14 C27 C28 N13 0.1(2) . . . . ?
N15 C29 C30 N16 0.1(3) . . . . ?
N16 C31 C32 N15 0.6(3) . . . . ?
N17 C33 C34 N18 0.5(3) . . . . ?
N18 C35 C36 N17 0.1(3) . . . . ?
N19 C37 C38 N20 0.0(2) . . . . ?
N20 C39 C40 N19 0.5(3) . . . . ?
N21 C41 C42 N22 0.6(2) . . . . ?
N22 C43 C44 N21 1.2(3) . . . . ?
N23 C45 C46 N24 0.8(3) . . . . ?
N24 C47 C48 N23 -0.6(2) . . . . ?
C1 N1 C4 C3 0.1(2) . . . . ?
C2 N2 C3 C4 0.2(2) . . . . ?
C3 N2 C2 C1 -0.6(2) . . . . ?
C4 N1 C1 C2 -0.5(2) . . . . ?
C5 N3 C8 C7 0.6(2) . . . . ?
C6 N4 C7 C8 0.4(3) . . . . ?
C7 N4 C6 C5 0.2(3) . . . . ?
C8 N3 C5 C6 0.0(2) . . . . ?
C9 N5 C12 C11 -0.7(2) . . . . ?
C10 N6 C11 C12 0.6(3) . . . . ?
C11 N6 C10 C9 -0.2(3) . . . . ?
C12 N5 C9 C10 1.0(2) . . . . ?
C13 N7 C16 C15 -0.3(2) . . . . ?
C14 N8 C15 C16 0.3(2) . . . . ?
C15 N8 C14 C13 0.3(2) . . . . ?
C16 N7 C13 C14 0.8(2) . . . . ?
C17 N9 C20 C19 -1.0(2) . . . . ?
C18 N10 C19 C20 -0.4(2) . . . . ?
C19 N10 C18 C17 0.0(2) . . . . ?
C20 N9 C17 C18 0.5(2) . . . . ?
C21 N11 C24 C23 2.5(2) . . . . ?
C22 N12 C23 C24 -1.8(2) . . . . ?
C23 N12 C22 C21 1.6(2) . . . . ?
C24 N11 C21 C22 -2.7(2) . . . . ?
C25 N13 C28 C27 -0.8(2) . . . . ?
C26 N14 C27 C28 0.7(2) . . . . ?
C27 N14 C26 C25 -0.9(2) . . . . ?
C28 N13 C25 C26 0.6(2) . . . . ?
C29 N15 C32 C31 -0.8(2) . . . . ?
C30 N16 C31 C32 -0.1(3) . . . . ?
C31 N16 C30 C29 -0.3(3) . . . . ?
C32 N15 C29 C30 0.5(3) . . . . ?
C33 N17 C36 C35 1.2(2) . . . . ?
C34 N18 C35 C36 -1.0(2) . . . . ?
C35 N18 C34 C33 0.7(2) . . . . ?
C36 N17 C33 C34 -1.5(2) . . . . ?
C37 N19 C40 C39 -1.0(2) . . . . ?
C38 N20 C39 C40 0.2(3) . . . . ?
C39 N20 C38 C37 -0.4(2) . . . . ?
C40 N19 C37 C38 0.7(2) . . . . ?
C41 N21 C44 C43 -1.1(2) . . . . ?
C42 N22 C43 C44 -0.4(2) . . . . ?
C43 N22 C42 C41 -0.6(2) . . . . ?
C44 N21 C41 C42 0.3(2) . . . . ?
C45 N23 C48 C47 0.3(2) . . . . ?
C46 N24 C47 C48 1.0(2) . . . . ?
C47 N24 C46 C45 -1.0(2) . . . . ?
C48 N23 C45 C46 -0.4(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_MV19                
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 68 Note
RESPONSE: Closed by beamstop.
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