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_7714390
_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         'Br6 Tc, 2(C8 H11 N4 O2), H2 O'
_chemical_formula_sum            'C16 H24 Br6 N8 O5 Tc'
_chemical_formula_weight         985.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 106.823(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.428(2)
_cell_length_b                   14.292(3)
_cell_length_c                   15.242(3)
_cell_measurement_reflns_used    1946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.096
_cell_measurement_theta_min      2.788
_cell_volume                     2800.0(9)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_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 0.997
_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  0.1817
_diffrn_reflns_av_unetI/netI     0.1617
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43761
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         4.192
_exptl_absorpt_coefficient_mu    9.120
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1103 before and 0.0764 after correction.
The Ratio of minimum to maximum transmission is 0.6617.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.339
_exptl_crystal_description       plate
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.545
_refine_diff_density_min         -1.921
_refine_diff_density_rms         0.256
_refine_ls_extinction_coef       0.00085(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         8150
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0416P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3939
_reflns_number_total             8150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03235c2.cif
_cod_data_source_block           kaz12_lt_0m_a
_cod_database_code               7714390
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.462
_olex2_refinement_description
;
1. Restrained distances
 N9-H9
 0.86 with sigma of 0.02
 O1-H1A = O1-H1B
 0.85 with sigma of 0.02
 N29-H29
 0.88 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(N27) = Uanis(C28)
Uanis(O33) = Uanis(O31)
Uanis(C22) = Uanis(C26)
3.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C8(H8)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C34(H34A,H34B,H34C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              35507
_olex2_submission_special_instructions 'No special instructions were received'