Influence of organic cation on the formation of hexahalotechnetates: X-ray, thermal and comparative analysis of non-covalent interactions
Novikov, Anton P.; Zagidullin, Karim A.; Volkov, Mikhail A.; German, Konstantin E.; Nevolin, Iurii; Grigoriev , Mikhail; Dalton Transactions  (2023) –; doi:10.1039/D3DT03235C

data_7714389
_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 \l/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/[\s^2^(Fo^2^)+(0.0200P)^2^+0.2965P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              60897
_olex2_submission_special_instructions 'No special instructions were received'