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_7717435
_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         'C9 H6 Br N6 O5 Re S, C3 H6 O'
_chemical_formula_sum            'C12 H12 Br N6 O6 Re S'
_chemical_formula_weight         634.45
_chemical_name_common            '[ReBr(CO)3(LH,H)]'
_chemical_name_systematic
'(5-(1-methyl-5-nitro-1H-imidazol-2-yl)-1,3,4-thiadiazol-2-amine)bromotricarbonylrhenium(I) acetone solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-06-23
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8493(2)
_cell_length_b                   11.36270(10)
_cell_length_c                   11.34830(10)
_cell_measurement_reflns_used    15740
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      78.1750
_cell_measurement_theta_min      3.8990
_cell_volume                     1914.78(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      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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    -61.00  25.00   0.50   10.00    --  -51.66  38.00 120.00  172
  2  \w     -6.00  80.00   0.50   10.00    --    8.00  59.00 148.61  172
  3  \w     12.00  98.00   0.50   20.00    --   84.00 -59.00  47.95  172
  4  \w     28.00  69.00   0.50   20.00    --  105.75 -30.00 -60.00   82
  5  \w     30.00  77.00   0.50   20.00    --  105.75 -45.00-120.00   94
  6  \w     33.00  93.00   0.50   20.00    --  105.75 -56.00-138.50  120
  7  \w     28.00  69.00   0.50   20.00    --  105.75 -30.00 -90.00   82
  8  \w     28.00  69.00   0.50   20.00    --  105.75 -30.00 -30.00   82
  9  \w     34.00 121.00   0.50   20.00    --  105.75 -60.00  27.82  174
 10  \w     33.00  91.00   0.50   20.00    --  105.75 -55.00 112.00  116
 11  \w     34.00 121.00   0.50   20.00    --  105.75 -60.00  10.11  174
 12  \w     30.00  77.00   0.50   20.00    --  105.75 -45.00 -90.00   94
 13  \w     34.00  98.00   0.50   20.00    --  105.75 -58.00 -32.13  128
 14  \w     28.00  69.00   0.50   20.00    --  105.75 -30.00  30.00   82
 15  \w     28.00  69.00   0.50   20.00    --  105.75 -30.00  90.00   82
 16  \w     26.00 116.00   0.50   20.00    --  105.75 -15.00 150.00  180
 17  \w     34.00 121.00   0.50   20.00    --  105.75 -60.00  65.48  174
 18  \w     34.00 121.00   0.50   20.00    --  105.75 -60.00  89.06  174
 19  \w     53.00 139.00   0.50   10.00    --   68.00  60.00-177.66  172
 20  \w   -132.00 -46.00   0.50   10.00    --  -60.00 -59.00 -31.09  172
 21  \w   -137.00 -51.00   0.50   10.00    --  -64.00 -55.00  69.78  172
;
_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      0.0116834000
_diffrn_orient_matrix_UB_12      0.1346046000
_diffrn_orient_matrix_UB_13      -0.0056597000
_diffrn_orient_matrix_UB_21      -0.0256483000
_diffrn_orient_matrix_UB_22      -0.0018000000
_diffrn_orient_matrix_UB_23      -0.1315295000
_diffrn_orient_matrix_UB_31      -0.0998359000
_diffrn_orient_matrix_UB_32      0.0162792000
_diffrn_orient_matrix_UB_33      0.0330971000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17726
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         4.901
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.277
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.274
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.561
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 1370 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3301
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0211
_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^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0558
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    0.885
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                3187
_reflns_number_total             3301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02714k2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7717431--7717436.cif.'
_cod_database_code               7717435
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C12 H12 Br N6 O6 Re S'
_chemical_oxdiff_usercomment     'EB04 complex yellow crystal'
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.226
_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
C22 \\sim C21 \\sim C23: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              98974
_shelx_hkl_checksum              98095
_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 1.518
_oxdiff_exptl_absorpt_empirical_full_min 0.626