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_7714391
_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, 4(Cl), 1.5(H2 O), 6(C4 H5 N2)'
_chemical_formula_sum            'C24 H33 Cl10 N12 O1.5 Tc'
_chemical_formula_weight         966.12
_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   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                 108.1910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.5623(9)
_cell_length_b                   12.8616(4)
_cell_length_c                   22.0923(7)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.43
_cell_measurement_theta_min      3.22
_cell_volume                     7710.1(4)
_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, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.972
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            205070
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.996
_diffrn_reflns_theta_min         4.148
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         33002
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+3.5907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23824
_reflns_number_total             33002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03235c2.cif
_cod_data_source_block           MV19
_cod_depositor_comments
;

2024-11-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H66 Cl20 N24 O3 Tc2'
_cod_original_formula_weight         1932.24
_cod_original_formula_moiety         '2(Cl6 Tc), 8(Cl), 3(H2 O), 12(C4 H5 N2)'
_cod_original_formula_units_Z            4
_cod_database_code               7714391
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Restrained distances
 O1W-H1A = O1W-H1B = O2W-H2A = O2W-H2B = O3W-H3A = O3W-H3B
 0.85 with sigma of 0.02
 H1A-H1B = H2A-H2B = H3A-H3B
 1.35 with sigma of 0.02
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N5(H5), N7(H7), N9(H9), N11(H11), N13(H13), N15(H15),
 N17(H17), N19(H19), N21(H21), N23(H23), C1(H1C), C2(H2C), C3(H3C), C4(H4A),
 C5(H5A), C6(H6A), C7(H7A), C8(H8A), C9(H9A), C10(H10A), C11(H11A), C12(H12A),
 C13(H13A), C14(H14A), C15(H15A), C16(H16A), C17(H17A), C18(H18A), C19(H19A),
 C20(H20A), C21(H21A), C22(H22A), C23(H23A), C24(H24A), C25(H25A), C26(H26A),
 C27(H27A), C28(H28A), C29(H29A), C30(H30A), C31(H31A), C32(H32A), C33(H33A),
 C34(H34A), C35(H35A), C36(H36A), C37(H37A), C38(H38A), C39(H39A), C40(H40A),
 C41(H41A), C42(H42A), C43(H43A), C44(H44A), C45(H45A), C46(H46A), C47(H47A),
 C48(H48A)
;
_shelx_res_checksum              16774
_olex2_submission_special_instructions 'No special instructions were received'