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_7717433
_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         'C6 H6 N6 O2 S'
_chemical_formula_sum            'C6 H6 N6 O2 S'
_chemical_formula_weight         226.23
_chemical_name_common            megazol
_chemical_name_systematic
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 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 95.919(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6955(10)
_cell_length_b                   5.6150(5)
_cell_length_c                   14.3386(14)
_cell_measurement_reflns_used    1384
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      72.6000
_cell_measurement_theta_min      6.1910
_cell_volume                     936.60(15)
_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      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_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     29.00 123.20   0.60    5.00    --   50.66  77.00 -30.00  157
  2  \w    115.00 172.60   0.60   13.00    --  105.75  15.00   0.00   96
  3  \w    104.80 177.40   0.60   13.00    --  105.75  45.00 120.00  121
  4  \w     92.00 174.20   0.60   13.00    --  105.75  61.00  30.00  137
  5  \w     84.00 111.00   0.60   13.00    --  105.75-111.00-120.00   45
  6  \w     29.00 111.20   0.60   13.00    --  105.75-111.00-180.00  137
  7  \w     35.00 120.20   0.60   13.00    --  105.75 -61.00-150.00  142
  8  \w     33.00 126.00   0.60   13.00    --  105.75 -77.00-150.00  155
  9  \w     29.00 111.20   0.60   13.00    --  105.75-111.00   0.00  137
 10  \w     28.00  67.60   0.60   13.00    --  105.75 -30.00  90.00   66
 11  \w     28.00  67.60   0.60   13.00    --  105.75 -30.00 150.00   66
 12  \w     94.00 130.00   0.60   13.00    --  105.75-142.00 163.00   60
 13  \w     48.00  76.20   0.60   13.00    --  105.75-142.00 163.00   47
 14  \w     28.00  53.20   0.60   13.00    --  105.75 -30.00-120.00   42
 15  \w     30.00 108.00   0.60   13.00    --  105.75 -94.00-150.00  130
 16  \w    -92.00  -9.80   0.60    5.00    --  -50.66 125.00  60.00  137
 17  \w   -123.00 -37.80   0.60    5.00    --  -50.66 -57.00   0.00  142
 18  \w   -125.00 -71.00   0.60    5.00    --  -50.66-125.00   0.00   90
 19  \w   -125.00 -71.00   0.60    5.00    --  -50.66-125.00 120.00   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      0.0245181000
_diffrn_orient_matrix_UB_12      -0.1963309000
_diffrn_orient_matrix_UB_13      0.0743979000
_diffrn_orient_matrix_UB_21      -0.0263276000
_diffrn_orient_matrix_UB_22      -0.1918038000
_diffrn_orient_matrix_UB_23      -0.0760901000
_diffrn_orient_matrix_UB_31      0.1274159000
_diffrn_orient_matrix_UB_32      -0.0022113000
_diffrn_orient_matrix_UB_33      -0.0184275000
_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  0.0820
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6459
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.442
_diffrn_reflns_theta_min         3.800
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.058
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.788
_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            orange
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0544P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1217
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1324
_reflns_number_total             1882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02714k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7717431--7717436.cif.'
_cod_database_code               7717433
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C6 H6 N6 O2 S'
_chemical_oxdiff_usercomment     EB07-3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.710
_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)
;
_shelx_res_checksum              39412
_shelx_hkl_checksum              47289
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.753