#------------------------------------------------------------------------------
#$Date: 2023-11-05 02:13:17 +0200 (Sun, 05 Nov 2023) $
#$Revision: 287267 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/43/7714389.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_7714389
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(Cl), 4(C7 H6 N S), 4(H2 O)'
_chemical_formula_sum            'C28 H32 Cl8 N4 O4 S4 Tc'
_chemical_formula_weight         998.41
_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
_atom_sites_solution_primary     dual
_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                76.369(2)
_cell_angle_beta                 79.704(2)
_cell_angle_gamma                81.477(2)
_cell_formula_units_Z            1
_cell_length_a                   7.1584(4)
_cell_length_b                   9.3884(5)
_cell_length_c                   15.4846(8)
_cell_measurement_reflns_used    9330
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.198
_cell_measurement_theta_min      2.246
_cell_volume                     988.92(9)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_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)'
_diffrn_ambient_temperature      100(2)
_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_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_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
_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_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.676
_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
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.070
_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_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0230
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5023
_reflns_number_total             5751
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03235c2.cif
_cod_data_source_block           kazt6_lt_1_0m
_cod_database_code               7714389
_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   0.924
_shelx_estimated_absorpt_t_min   0.802
_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)
;
_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 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 . . .
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'
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_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_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) . . . . ?
