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#$Date: 2023-11-05 02:13:17 +0200 (Sun, 05 Nov 2023) $
#$Revision: 287267 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/43/7714384.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7714384
loop_
_publ_author_name
'Novikov, Anton P.'
'Zagidullin, Karim A.'
'Volkov, Mikhail A.'
'German, Konstantin E.'
'Nevolin, Iurii'
'Grigoriev , Mikhail'
_publ_section_title
;
 Influence of organic cation on the formation of hexahalotechnetates:
 X-ray, thermal and comparative analysis of non-covalent interactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03235C
_journal_year                    2023
_chemical_formula_moiety         'Cl6 Tc, 2(C8 H11 N4 O2)'
_chemical_formula_sum            'C16 H22 Cl6 N8 O4 Tc'
_chemical_formula_weight         701.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-07-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-29 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                96.572(16)
_cell_angle_beta                 91.809(15)
_cell_angle_gamma                112.382(14)
_cell_formula_units_Z            1
_cell_length_a                   7.898(3)
_cell_length_b                   8.106(3)
_cell_length_c                   10.452(4)
_cell_measurement_reflns_used    2103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.429
_cell_measurement_theta_min      3.068
_cell_volume                     612.6(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_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)'
_diffrn_ambient_temperature      100(2)
_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_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_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
_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_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.900
_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
_refine_diff_density_max         1.213
_refine_diff_density_min         -2.617
_refine_diff_density_rms         0.194
_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_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0585
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2453
_reflns_number_total             3569
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03235c2.cif
_cod_data_source_block           kaz11_tccl6caf_lt_0m_a
_cod_original_cell_volume        612.7(4)
_cod_database_code               7714384
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.882
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 . . .
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'
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_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_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) . . . . ?
