Rhenium(I) and technetium(I) complexes with megazol derivatives: towards the development of a theranostic platform for Chagas disease.
Gonçalves, Ana C R; Libardi, Silvia H.; Borges, Júlio C; Oliveira, Ronaldo J.; Gotzmann, Carla; Blacque, Olivier; de Albuquerque, Sergio; Lopes, Carla D.; Alberto, Roger; Maia, Pedro I. S.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 19153–19165; doi:10.1039/d4dt02714k

data_7717431
_publ_section_title
;
 Rhenium(I) and technetium(I) complexes with megazol derivatives: towards
 the development of a theranostic platform for Chagas disease.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19153
_journal_page_last               19165
_journal_paper_doi               10.1039/d4dt02714k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C7 H10 N6 O2 S'
_chemical_formula_sum            'C7 H10 N6 O2 S'
_chemical_formula_weight         242.27
_chemical_name_common            TscH,Me
_chemical_name_systematic
(E)-N-methyl-2-((1-methyl-5-nitro-1H-imidazol-2-yl)methylene)hydrazinecarbothioamide
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-28 deposited with the CCDC.	2024-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9473(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.83761(15)
_cell_length_b                   10.32677(19)
_cell_length_c                   13.6972(2)
_cell_measurement_reflns_used    5592
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      76.1790
_cell_measurement_theta_min      3.2450
_cell_volume                     1091.95(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -116.00 -20.00   1.00    1.00    --  -42.74 -37.00   0.00   96
  2  \w    -65.00  30.00   1.00    1.00    --  -42.74  37.00-180.00   95
  3  \w     23.00  98.00   1.00    1.00    --   42.74-125.00 -30.00   75
  4  \w     23.00  98.00   1.00    1.00    --   42.74-125.00-150.00   75
  5  \w     87.00 178.00   1.00    1.00    --  111.00  30.00 -30.00   91
  6  \w     40.00 135.00   1.00    1.00    --  111.00 -45.00-180.00   95
  7  \w     83.00 178.00   1.00    1.00    --  111.00  61.00   0.00   95
  8  \w     36.00 113.00   1.00    1.00    --  111.00-111.00 -90.00   77
  9  \w     30.00 110.00   1.00    1.00    --  111.00 -94.00 -30.00   80
 10  \w    100.00 178.00   1.00    1.00    --  111.00 111.00-150.00   78
 11  \w    100.00 178.00   1.00    1.00    --  111.00 111.00-180.00   78
 12  \w    100.00 178.00   1.00    1.00    --  111.00 111.00-120.00   78
 13  \w     83.00 178.00   1.00    1.00    --  111.00  61.00  30.00   95
 14  \w     83.00 178.00   1.00    1.00    --  111.00  61.00  60.00   95
 15  \w   -113.00 -82.00   1.00    1.00    --  -42.74 -57.00-180.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1427312000
_diffrn_orient_matrix_UB_12      -0.0978529000
_diffrn_orient_matrix_UB_13      -0.0414073000
_diffrn_orient_matrix_UB_21      0.0103347000
_diffrn_orient_matrix_UB_22      -0.0590064000
_diffrn_orient_matrix_UB_23      0.1040601000
_diffrn_orient_matrix_UB_31      -0.1393644000
_diffrn_orient_matrix_UB_32      0.0957683000
_diffrn_orient_matrix_UB_33      0.0219810000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8233
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.477
_diffrn_reflns_theta_min         5.731
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.656
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0487P)^2^+0.6300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2105
_reflns_number_total             2225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02714k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7717431--7717436.cif.'
_cod_original_cell_volume        1091.95(4)
_cod_database_code               7717431
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C7 H10 N6 O2 S'
_chemical_oxdiff_usercomment     AR34
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.523
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(S1) = Uanis(N6)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              96990
_shelx_hkl_checksum              51605
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.542
_oxdiff_exptl_absorpt_empirical_full_min 0.649