#------------------------------------------------------------------------------
#$Date: 2026-03-05 13:57:32 +0100 (Thu 05 de Mar de 2026) $
#$Revision: 304928 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/01/7720155.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_7720155
loop_
_publ_author_name
'Novikov, Anton P.'
'Volkov, Mikhail A.'
'Grigoriev, Mikhail S.'
_publ_section_title
;
 Crystallographic insights into (ImHR)₂[TcBr₆] (Im =
 imidazole, R = H, Me, Et): non-covalent interactions and mass
 spectrometry.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3990
_journal_page_last               3999
_journal_paper_doi               10.1039/d5dt03046c
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'Br3 Tc0.5, C4 H7 N2'
_chemical_formula_sum            'C4 H7 Br3 N2 Tc0.5'
_chemical_formula_weight         371.85
_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   geom
_audit_creation_date             2025-07-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-12-02 deposited with the CCDC.	2026-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                79.107(5)
_cell_angle_beta                 86.065(5)
_cell_angle_gamma                66.969(5)
_cell_formula_units_Z            2
_cell_length_a                   7.7095(8)
_cell_length_b                   7.9065(8)
_cell_length_c                   8.0783(8)
_cell_measurement_reflns_used    8224
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.976
_cell_measurement_theta_min      2.844
_cell_volume                     444.99(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18576
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         39.996
_diffrn_reflns_theta_min         4.157
_exptl_absorpt_coefficient_mu    14.270
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.5018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0949 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.6709.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.775
_exptl_crystal_description       fragment
_exptl_crystal_F_000             343
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.264
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0282
_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)+(0.0312P)²+0.3930P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4696
_reflns_number_total             5509
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt03046c2.cif
_cod_data_source_block           tcm
_cod_depositor_comments
'Adding full bibliography for 7720152--7720155.cif.'
_cod_original_formula_sum        'C4 H7 Br3 N2 Tc0.50'
_cod_database_code               7720155
_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   0.183
_shelx_estimated_absorpt_t_min   0.079
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C3(H3), C4(H4)
1.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_shelx_res_file
;
TITL TcNaMeIm_LT_0m in P-1
    tcm.res
    created by SHELXL-2018/3 at 13:00:50 on 23-Aug-2021
CELL 0.71073 7.7095 7.9065 8.0783 79.107 86.065 66.969
ZERR 2 0.0008 0.0008 0.0008 0.005 0.005 0.005
LATT 1
SFAC C H Br N Tc
UNIT 8 14 6 4 1
EQIV $1 1+X,+Y,+Z
EQIV $2 -X,1-Y,-Z
EQIV $3 1-X,-Y,1-Z

L.S. 8
PLAN  5
SIZE 0.36 0.2 0.18
TEMP -173(2)
HTAB N1 Br1_$1
HTAB N1 Br3
HTAB N2 Br1_$2
CONF
HTAB C3 Br3_$3
BOND $H
HTAB
MORE -1
fmap 2
acta
SHEL 5 0.5
OMIT -2 80
OMIT -1 -2 2
OMIT 2 0 3
OMIT -3 1 1
OMIT 0 3 2
OMIT -1 1 1
OMIT 2 -1 2
OMIT 3 2 3
OMIT 5 6 4
REM <olex2.extras>
REM <HklSrc "%.\\tcm.hkl">
REM </olex2.extras>

WGHT    0.031200    0.393000
FVAR       0.15476
TC1   5    0.000000    0.000000    0.500000    10.50000    0.00836    0.00815 =
         0.00675   -0.00078    0.00040   -0.00204
BR1   3   -0.286131    0.296720    0.485456    11.00000    0.01219    0.01112 =
         0.01137   -0.00226   -0.00092    0.00093
BR2   3    0.058806    0.091832    0.192483    11.00000    0.01416    0.01349 =
         0.00758   -0.00011    0.00158   -0.00431
BR3   3    0.197570    0.160048    0.583845    11.00000    0.01394    0.01337 =
         0.01262   -0.00117   -0.00079   -0.00694
N1    4    0.440149    0.246359    0.188427    11.00000    0.01979    0.02462 =
         0.01984    0.00294   -0.00312   -0.00928
AFIX  43
H1    2    0.446566    0.206337    0.298031    11.00000   -1.20000
AFIX   0
N2    4    0.344337    0.414342   -0.063486    11.00000    0.02021    0.02187 =
         0.01452    0.00018   -0.00062   -0.00732
AFIX  43
H2    2    0.276598    0.503129   -0.143848    11.00000   -1.20000
AFIX   0
C1    1    0.304911    0.397267    0.106864    11.00000    0.00785    0.00977 =
         0.00871   -0.00017   -0.00074   -0.00457
C2    1    0.141504    0.524917    0.185217    11.00000    0.01635    0.01874 =
         0.01727   -0.00509    0.00308   -0.00705
AFIX 137
H2A   2    0.118508    0.653987    0.132085    11.00000   -1.50000
H2B   2    0.166192    0.508258    0.305839    11.00000   -1.50000
H2C   2    0.030434    0.497950    0.170176    11.00000   -1.50000
AFIX   0
C3    1    0.563801    0.166580    0.075735    11.00000    0.00936    0.01341 =
         0.01917    0.00058   -0.00110   -0.00265
AFIX  43
H3    2    0.674337    0.056340    0.100667    11.00000   -1.20000
AFIX   0
C4    1    0.506533    0.269030   -0.083562    11.00000    0.01712    0.02060 =
         0.01623   -0.00404    0.00329   -0.00777
AFIX  43
H4    2    0.568859    0.242555   -0.186799    11.00000   -1.20000
AFIX   0
HKLF 4




REM  TcNaMeIm_LT_0m in P-1
REM wR2 = 0.0705, GooF = S = 1.041, Restrained GooF = 1.041 for all data
REM R1 = 0.0282 for 4696 Fo > 4sig(Fo) and 0.0368 for all 5509 data
REM 89 parameters refined using 0 restraints

END

WGHT      0.0312      0.3928

REM Instructions for potential hydrogen bonds
HTAB N1 Br1_$1
HTAB N1 Br3
HTAB N2 Br1_$2
HTAB C2 Br2_$2
EQIV $5 -x, -y+1, -z+1
HTAB C2 Br1_$5
HTAB C2 Br2
EQIV $6 -x+1, -y, -z
HTAB C3 Br2_$6
HTAB C3 Br3_$3
EQIV $7 x+1, y, z-1
HTAB C4 Br1_$7
HTAB C4 Br2_$6

REM Highest difference peak  1.264,  deepest hole -1.307,  1-sigma level  0.204
Q1    1   0.3047  0.4013  0.0598  11.00000  0.05    1.26
Q2    1   0.2675  0.4264  0.1201  11.00000  0.05    1.23
Q3    1   0.3044  0.4390  0.1113  11.00000  0.05    1.19
Q4    1   0.3603  0.3598  0.1280  11.00000  0.05    1.18
Q5    1   0.5624  0.1236  0.0758  11.00000  0.05    1.07
;
_shelx_res_checksum              58945
_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 0.000000 0.000000 0.500000 0.00821(4) Uani 1 2 d S . P . .
Br1 Br -0.28613(3) 0.29672(3) 0.48546(2) 0.01317(4) Uani 1 1 d . . . . .
Br2 Br 0.05881(3) 0.09183(3) 0.19248(2) 0.01238(4) Uani 1 1 d . . . . .
Br3 Br 0.19757(3) 0.16005(3) 0.58385(2) 0.01290(4) Uani 1 1 d . . . . .
N1 N 0.4401(3) 0.2464(3) 0.1884(3) 0.0220(4) Uani 1 1 d . . . . .
H1 H 0.446566 0.206337 0.298031 0.026 Uiso 1 1 calc R U . . .
N2 N 0.3443(3) 0.4143(3) -0.0635(2) 0.0196(3) Uani 1 1 d . . . . .
H2 H 0.276598 0.503129 -0.143848 0.023 Uiso 1 1 calc R U . . .
C1 C 0.3049(2) 0.3973(2) 0.1069(2) 0.0086(2) Uani 1 1 d . . . . .
C2 C 0.1415(3) 0.5249(3) 0.1852(3) 0.0172(3) Uani 1 1 d . . . . .
H2A H 0.118508 0.653987 0.132085 0.026 Uiso 1 1 calc R U . . .
H2B H 0.166192 0.508258 0.305839 0.026 Uiso 1 1 calc R U . . .
H2C H 0.030434 0.497950 0.170176 0.026 Uiso 1 1 calc R U . . .
C3 C 0.5638(3) 0.1666(3) 0.0757(3) 0.0150(3) Uani 1 1 d . . . . .
H3 H 0.674337 0.056340 0.100667 0.018 Uiso 1 1 calc R U . . .
C4 C 0.5065(3) 0.2690(3) -0.0836(3) 0.0179(4) Uani 1 1 d . . . . .
H4 H 0.568859 0.242555 -0.186799 0.021 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Tc1 0.00836(8) 0.00815(8) 0.00675(7) -0.00078(6) 0.00040(6) -0.00204(6)
Br1 0.01219(8) 0.01112(8) 0.01137(8) -0.00226(6) -0.00092(6) 0.00093(6)
Br2 0.01416(8) 0.01349(8) 0.00758(7) -0.00011(5) 0.00158(6) -0.00431(6)
Br3 0.01394(8) 0.01337(8) 0.01262(8) -0.00117(6) -0.00079(6) -0.00694(6)
N1 0.0198(8) 0.0246(9) 0.0198(8) 0.0029(7) -0.0031(7) -0.0093(7)
N2 0.0202(8) 0.0219(8) 0.0145(7) 0.0002(6) -0.0006(6) -0.0073(7)
C1 0.0078(6) 0.0098(6) 0.0087(6) -0.0002(5) -0.0007(5) -0.0046(5)
C2 0.0163(8) 0.0187(9) 0.0173(8) -0.0051(7) 0.0031(7) -0.0070(7)
C3 0.0094(7) 0.0134(7) 0.0192(8) 0.0006(6) -0.0011(6) -0.0027(6)
C4 0.0171(8) 0.0206(9) 0.0162(8) -0.0040(7) 0.0033(7) -0.0078(7)
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'
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 . 2_556 ?
Br1 Tc1 Br2 90.361(10) 2_556 . ?
Br1 Tc1 Br2 89.640(9) . . ?
Br1 Tc1 Br2 89.639(9) 2_556 2_556 ?
Br1 Tc1 Br2 90.360(9) . 2_556 ?
Br1 Tc1 Br3 90.069(11) . . ?
Br1 Tc1 Br3 89.931(11) . 2_556 ?
Br1 Tc1 Br3 90.069(11) 2_556 2_556 ?
Br1 Tc1 Br3 89.931(11) 2_556 . ?
Br2 Tc1 Br2 180.0 2_556 . ?
Br2 Tc1 Br3 91.409(9) . . ?
Br2 Tc1 Br3 88.590(9) 2_556 . ?
Br2 Tc1 Br3 91.410(9) 2_556 2_556 ?
Br2 Tc1 Br3 88.591(8) . 2_556 ?
Br3 Tc1 Br3 180.0 . 2_556 ?
C1 N1 H1 125.9 . . ?
C3 N1 H1 125.9 . . ?
C3 N1 C1 108.12(19) . . ?
C1 N2 H2 126.4 . . ?
C4 N2 H2 126.4 . . ?
C4 N2 C1 107.15(18) . . ?
N1 C1 N2 108.91(18) . . ?
N1 C1 C2 125.46(19) . . ?
N2 C1 C2 125.63(18) . . ?
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 H3 125.3 . . ?
N1 C3 C4 109.35(19) . . ?
C4 C3 H3 125.3 . . ?
N2 C4 C3 106.48(19) . . ?
N2 C4 H4 126.8 . . ?
C3 C4 H4 126.8 . . ?
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 2.5032(3) . ?
Tc1 Br1 2.5032(3) 2_556 ?
Tc1 Br2 2.5150(3) 2_556 ?
Tc1 Br2 2.5150(3) . ?
Tc1 Br3 2.5207(3) 2_556 ?
Tc1 Br3 2.5207(3) . ?
N1 H1 0.8800 . ?
N1 C1 1.330(3) . ?
N1 C3 1.328(3) . ?
N2 H2 0.8800 . ?
N2 C1 1.382(3) . ?
N2 C4 1.352(3) . ?
C1 C2 1.464(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 0.9500 . ?
C3 C4 1.382(3) . ?
C4 H4 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
N1 H1 Br1 0.88 3.01 3.476(2) 115.4 1_655 yes
N1 H1 Br3 0.88 2.96 3.677(2) 139.7 . yes
N2 H2 Br1 0.88 2.92 3.675(2) 144.6 2_565 yes
C3 H3 Br3 0.95 2.79 3.451(2) 127.6 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
N1 C3 C4 N2 0.3(3) . . . . ?
C1 N1 C3 C4 -0.1(3) . . . . ?
C1 N2 C4 C3 -0.4(2) . . . . ?
C3 N1 C1 N2 -0.2(2) . . . . ?
C3 N1 C1 C2 -179.91(19) . . . . ?
C4 N2 C1 N1 0.4(2) . . . . ?
C4 N2 C1 C2 -179.9(2) . . . . ?
