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_7717432
_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 H8 N6 O2 S'
_chemical_formula_sum            'C7 H8 N6 O2 S'
_chemical_formula_weight         240.25
_chemical_name_common            LH,Me
_chemical_name_systematic
N-methyl-5-(1-methyl-5-nitro-1H-imidazol-2-yl)-1,3,4-thiadiazol-2-amine
_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
_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                 95.371(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.67495(16)
_cell_length_b                   9.4303(2)
_cell_length_c                   18.9778(5)
_cell_measurement_reflns_used    5353
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      78.4010
_cell_measurement_theta_min      4.6720
_cell_volume                     1011.17(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.981
_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     42.00 128.00   0.50    0.60    --   51.31  38.00  30.00  172
  2  \w     76.00 162.00   0.50    2.40    --   90.00  57.00 -80.46  172
  3  \w     94.00 178.00   0.50    2.40    --  107.75  58.00-102.59  168
  4  \w     98.00 178.00   0.50    2.40    --  107.75  15.00 120.00  160
  5  \w     34.00  88.00   0.50    2.40    --  107.75 -53.00 123.90  108
  6  \w     33.00  82.00   0.50    2.40    --  107.75 -49.00  69.22   98
  7  \w     34.00  84.00   0.50    2.40    --  107.75 -51.00 -29.00  100
  8  \w     30.00  69.00   0.50    2.40    --  107.75 -30.00 -60.00   78
  9  \w     36.00 102.00   0.50    2.40    --  107.75 -59.00-125.76  132
 10  \w     35.00  91.00   0.50    2.40    --  107.75 -55.00 -91.61  112
 11  \w     30.00  69.00   0.50    2.40    --  107.75 -30.00-180.00   78
 12  \w     30.00  69.00   0.50    2.40    --  107.75 -30.00-150.00   78
 13  \w     32.00  77.00   0.50    2.40    --  107.75 -45.00 -90.00   90
 14  \w     30.00  69.00   0.50    2.40    --  107.75 -30.00   0.00   78
 15  \w     35.00  91.00   0.50    2.40    --  107.75 -55.00  25.27  112
 16  \w     30.00  69.00   0.50    2.40    --  107.75 -30.00  90.00   78
 17  \w     30.00  69.00   0.50    2.40    --  107.75 -30.00 150.00   78
 18  \w     28.00 117.00   0.50    2.40    --  107.75 -15.00  90.00  178
 19  \w     40.00 126.00   0.50    0.60    --   54.00  59.00 113.21  172
 20  \w     55.00 141.00   0.50    0.60    --   70.00  60.00-153.54  172
 21  \w    -65.00  21.00   0.50    0.60    --  -51.31  57.00 -30.00  172
 22  \w   -124.00 -37.00   0.50    0.60    --  -51.31 -57.00-180.00  174
 23  \w   -124.00 -37.00   0.50    0.60    --  -51.31 -57.00 -60.00  174
 24  \w   -146.00 -60.00   0.50    2.40    --  -74.00 -59.00-111.65  172
 25  \w   -158.00-113.00   0.50    2.40    --  -86.25 -58.00  41.90   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2403646000
_diffrn_orient_matrix_UB_12      -0.0423210000
_diffrn_orient_matrix_UB_13      -0.0254188000
_diffrn_orient_matrix_UB_21      -0.0225163000
_diffrn_orient_matrix_UB_22      0.1209071000
_diffrn_orient_matrix_UB_23      -0.0548281000
_diffrn_orient_matrix_UB_31      0.1269005000
_diffrn_orient_matrix_UB_32      0.1013448000
_diffrn_orient_matrix_UB_33      0.0547097000
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9328
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.484
_diffrn_reflns_theta_min         4.681
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.868
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0606P)^2^+0.8433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1862
_reflns_number_total             2026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02714k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7717431--7717436.cif.'
_cod_original_cell_volume        1011.17(5)
_cod_database_code               7717432
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C7 H8 N6 O2 S'
_chemical_oxdiff_usercomment     LB3
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.490
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              147
_shelx_hkl_checksum              82871
_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 1.555
_oxdiff_exptl_absorpt_empirical_full_min 0.570