Crystallographic insights into (ImHR)<sub>2</sub>[TcBr<sub>6</sub>] (Im = imidazole, R = H, Me, Et): non-covalent interactions and mass spectrometry.
Novikov, Anton P.; Volkov, Mikhail A.; Grigoriev, Mikhail S.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3990–3999; doi:10.1039/d5dt03046c

data_7720153
_publ_section_title
;
 Crystallographic insights into (ImHR)<sub>2</sub>[TcBr<sub>6</sub>] (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(C4 H7 N2)'
_chemical_formula_sum            'C8 H14 Br6 N4 Tc'
_chemical_formula_weight         743.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8599(6)
_cell_length_b                   16.0412(13)
_cell_length_c                   7.2519(6)
_cell_measurement_reflns_used    2456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.057
_cell_measurement_theta_min      3.082
_cell_volume                     914.34(13)
_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 0.988
_diffrn_measured_fraction_theta_max 0.992
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8987
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.992
_diffrn_reflns_theta_min         4.592
_exptl_absorpt_coefficient_mu    13.890
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1256 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.5153.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.701
_exptl_crystal_description       fragment
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.6491
_refine_diff_density_max         2.647
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.198
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         2645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0359
_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/[\s^2^(Fo^2^)+(0.0291P)^2^+3.2821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.715
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2259
_reflns_number_total             2645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03046c2.cif
_cod_data_source_block           tcb
_cod_depositor_comments
'Adding full bibliography for 7720152--7720155.cif.'
_cod_database_code               7720153
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.215
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5205
 0.4795
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1A), N2(H2A), C3(H3A), C4(H4A)
2.b Idealised Me refined as rotating group:
 C2(H2B,H2C,H2D)
;
_shelx_res_checksum              25733
_olex2_submission_special_instructions 'No special instructions were received'