#------------------------------------------------------------------------------
#$Date: 2026-03-05 13:57:32 +0100 (Thu 05 de Mar de 2026) $
#$Revision: 304928 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/01/7720152.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_7720152
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         'Br6 Tc, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br6 N4 Tc'
_chemical_formula_weight         715.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 98.133(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7038(5)
_cell_length_b                   8.3595(5)
_cell_length_c                   12.6218(8)
_cell_measurement_reflns_used    2870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.767
_cell_measurement_theta_min      2.932
_cell_volume                     804.67(9)
_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)'
_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 0.991
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8718
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.988
_diffrn_reflns_theta_min         4.120
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    15.776
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0425 after correction.
The Ratio of minimum to maximum transmission is 0.6748.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.954
_exptl_crystal_description       fragment
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.727
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         2318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0267
_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)+(0.0215P)²+1.8578P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1968
_reflns_number_total             2318
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt03046c2.cif
_cod_data_source_block           imtcbr_lt_0m
_cod_depositor_comments
'Adding full bibliography for 7720152--7720155.cif.'
_cod_database_code               7720152
_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   0.276
_shelx_estimated_absorpt_t_min   0.032
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C5(H5), C4(H4), C2(H2)
;
_shelx_res_file
;
TITL imtcbr_lt_0m_a.res in P2(1)/c
    imtcbr_lt_0m.res
    created by SHELXL-2018/3 at 13:58:00 on 07-Jun-2021
REM Old TITL ImTcBr_LT_0m in P21/c #14
REM SHELXT solution in P2(1)/c: R1 0.066, Rweak 0.003, Alpha 0.017
REM <I/s> 0.358 for 124 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 Br7
CELL 0.71073 7.7038 8.3595 12.6218 90 98.133 90
ZERR 2 0.0005 0.0005 0.0008 0 0.003 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br N Tc
UNIT 12 20 12 8 2
EQIV $1 1+X,0.5-Y,0.5+Z
EQIV $2 +X,0.5-Y,0.5+Z

L.S. 4 0 0
PLAN  4
SIZE 0.7 0.11 0.41
TEMP -173.15
CONF
HTAB N1 Br2_$1
HTAB N3 Br2_$2
HTAB N3 Br3
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
SHEL 5 0.5
OMIT -2 60
REM <olex2.extras>
REM <HklSrc "%.\\ImTcBr_LT_0m.hkl">
REM </olex2.extras>

WGHT    0.021500    1.857800
FVAR       0.23536
TC1   5    0.500000    0.500000    0.500000    10.50000    0.00550    0.00644 =
         0.00781    0.00039    0.00100    0.00027
BR1   3    0.818112    0.473530    0.581195    11.00000    0.01057    0.01512 =
         0.01473    0.00044    0.00088    0.00078
BR2   3    0.475769    0.200178    0.482177    11.00000    0.01256    0.01150 =
         0.02047   -0.00077    0.00216    0.00047
BR3   3    0.402344    0.478887    0.684846    11.00000    0.01191    0.01905 =
         0.01164    0.00114    0.00198    0.00090
N1    4    1.053105    0.374874    0.870060    11.00000    0.01872    0.01920 =
         0.01528    0.00035    0.00128    0.00680
AFIX  43
H1    2    1.138466    0.304102    0.875496    11.00000   -1.20000
AFIX   0
N3    4    0.796504    0.477389    0.852537    11.00000    0.01057    0.03500 =
         0.01569    0.00143   -0.00050   -0.00066
AFIX  43
H3    2    0.681561    0.486039    0.844786    11.00000   -1.20000
AFIX   0
C5    1    1.075278    0.538531    0.874738    11.00000    0.01474    0.01888 =
         0.01540   -0.00349    0.00226   -0.00651
AFIX  43
H5    2    1.183642    0.594577    0.884492    11.00000   -1.20000
AFIX   0
C4    1    0.912514    0.604153    0.862726    11.00000    0.01954    0.01967 =
         0.01506    0.00215    0.00261    0.00073
AFIX  43
H4    2    0.884193    0.714803    0.861567    11.00000   -1.20000
AFIX   0
C2    1    0.884271    0.340745    0.856184    11.00000    0.02328    0.02221 =
         0.01631   -0.00186    0.00220   -0.00796
AFIX  43
H2    2    0.834426    0.236638    0.849914    11.00000   -1.20000
AFIX   0
HKLF 4




REM  imtcbr_lt_0m_a.res in P2(1)/c
REM wR2 = 0.0585, GooF = S = 1.042, Restrained GooF = 1.042 for all data
REM R1 = 0.0267 for 1968 Fo > 4sig(Fo) and 0.0369 for all 2318 data
REM 79 parameters refined using 0 restraints

END

WGHT      0.0215      1.8579

REM Highest difference peak  1.727,  deepest hole -1.197,  1-sigma level  0.182
Q1    1   0.5023  0.5572  0.4954  11.00000  0.05    1.73
Q2    1   0.4392  0.4993  0.4687  11.00000  0.05    1.57
Q3    1   0.3804  0.1978  0.4395  11.00000  0.05    0.76
Q4    1   0.3230  0.3551  0.6632  11.00000  0.05    0.68
;
_shelx_res_checksum              51161
_olex2_submission_special_instructions 'No special instructions were received'
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'
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 0.00657(9) Uani 1 2 d S . P . .
Br1 Br 0.81811(5) 0.47353(5) 0.58119(3) 0.01356(9) Uani 1 1 d . . . . .
Br2 Br 0.47577(5) 0.20018(5) 0.48218(3) 0.01486(9) Uani 1 1 d . . . . .
Br3 Br 0.40234(5) 0.47889(5) 0.68485(3) 0.01417(9) Uani 1 1 d . . . . .
N1 N 1.0531(4) 0.3749(4) 0.8701(3) 0.0178(7) Uani 1 1 d . . . . .
H1 H 1.138466 0.304102 0.875496 0.021 Uiso 1 1 calc R U . . .
N3 N 0.7965(5) 0.4774(4) 0.8525(3) 0.0207(7) Uani 1 1 d . . . . .
H3 H 0.681561 0.486039 0.844786 0.025 Uiso 1 1 calc R U . . .
C5 C 1.0753(5) 0.5385(5) 0.8747(3) 0.0163(8) Uani 1 1 d . . . . .
H5 H 1.183642 0.594577 0.884492 0.020 Uiso 1 1 calc R U . . .
C4 C 0.9125(5) 0.6042(5) 0.8627(3) 0.0181(8) Uani 1 1 d . . . . .
H4 H 0.884193 0.714803 0.861567 0.022 Uiso 1 1 calc R U . . .
C2 C 0.8843(6) 0.3407(5) 0.8562(3) 0.0207(8) Uani 1 1 d . . . . .
H2 H 0.834426 0.236638 0.849914 0.025 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 0.00550(17) 0.00644(19) 0.00781(17) 0.00039(14) 0.00100(13) 0.00027(14)
Br1 0.01057(17) 0.01512(19) 0.01473(17) 0.00044(13) 0.00088(13) 0.00078(13)
Br2 0.01256(17) 0.01150(18) 0.02047(18) -0.00077(14) 0.00216(13) 0.00047(13)
Br3 0.01191(17) 0.0190(2) 0.01164(16) 0.00114(13) 0.00198(13) 0.00090(14)
N1 0.0187(17) 0.0192(18) 0.0153(15) 0.0003(13) 0.0013(13) 0.0068(14)
N3 0.0106(15) 0.035(2) 0.0157(16) 0.0014(14) -0.0005(12) -0.0007(14)
C5 0.0147(18) 0.019(2) 0.0154(17) -0.0035(14) 0.0023(14) -0.0065(15)
C4 0.020(2) 0.020(2) 0.0151(17) 0.0022(15) 0.0026(15) 0.0007(16)
C2 0.023(2) 0.022(2) 0.0163(18) -0.0019(16) 0.0022(16) -0.0080(18)
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 3_666 . ?
Br1 Tc1 Br3 91.005(12) . . ?
Br1 Tc1 Br3 88.995(12) . 3_666 ?
Br1 Tc1 Br3 88.995(13) 3_666 . ?
Br1 Tc1 Br3 91.005(12) 3_666 3_666 ?
Br2 Tc1 Br1 89.746(12) . 3_666 ?
Br2 Tc1 Br1 90.254(12) 3_666 3_666 ?
Br2 Tc1 Br1 89.745(12) 3_666 . ?
Br2 Tc1 Br1 90.255(12) . . ?
Br2 Tc1 Br2 180.0 . 3_666 ?
Br2 Tc1 Br3 89.150(12) . . ?
Br2 Tc1 Br3 90.850(12) . 3_666 ?
Br2 Tc1 Br3 89.151(12) 3_666 3_666 ?
Br2 Tc1 Br3 90.849(12) 3_666 . ?
Br3 Tc1 Br3 180.0 . 3_666 ?
C5 N1 H1 125.2 . . ?
C2 N1 H1 125.2 . . ?
C2 N1 C5 109.5(3) . . ?
C4 N3 H3 125.1 . . ?
C2 N3 H3 125.1 . . ?
C2 N3 C4 109.8(4) . . ?
N1 C5 H5 126.6 . . ?
C4 C5 N1 106.8(3) . . ?
C4 C5 H5 126.6 . . ?
N3 C4 H4 127.0 . . ?
C5 C4 N3 106.0(4) . . ?
C5 C4 H4 127.0 . . ?
N1 C2 N3 107.9(4) . . ?
N1 C2 H2 126.1 . . ?
N3 C2 H2 126.1 . . ?
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 2.5287(4) 3_666 ?
Tc1 Br1 2.5287(4) . ?
Tc1 Br2 2.5210(4) . ?
Tc1 Br2 2.5210(4) 3_666 ?
Tc1 Br3 2.5568(4) 3_666 ?
Tc1 Br3 2.5568(4) . ?
N1 H1 0.8800 . ?
N1 C5 1.379(5) . ?
N1 C2 1.319(5) . ?
N3 H3 0.8800 . ?
N3 C4 1.380(5) . ?
N3 C2 1.325(6) . ?
C5 H5 0.9500 . ?
C5 C4 1.357(6) . ?
C4 H4 0.9500 . ?
C2 H2 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 Br2 0.88 2.75 3.420(3) 133.6 4_666 yes
N3 H3 Br2 0.88 2.95 3.483(4) 120.4 4_566 yes
N3 H3 Br3 0.88 2.73 3.447(3) 139.0 . 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 C5 C4 N3 0.8(4) . . . . ?
C5 N1 C2 N3 -0.5(4) . . . . ?
C4 N3 C2 N1 1.0(4) . . . . ?
C2 N1 C5 C4 -0.2(4) . . . . ?
C2 N3 C4 C5 -1.1(4) . . . . ?
