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_7717436
_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         'C11 H10 Br N6 O5 Re S'
_chemical_formula_sum            'C11 H10 Br N6 O5 Re S'
_chemical_formula_weight         604.42
_chemical_name_common            '[ReBr(CO)3(LMe,Me)]'
_chemical_name_systematic
(N,N-dimethyl-5-(1-methyl-5-nitro-1H-imidazol-2-yl)-1,3,4-thiadiazol-2-amine)bromotricarbonylrhenium(I)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.8669(5)
_cell_length_b                   8.9140(3)
_cell_length_c                   29.5706(12)
_cell_measurement_reflns_used    9190
_cell_measurement_temperature    159.95(10)
_cell_measurement_theta_max      32.8740
_cell_measurement_theta_min      3.0400
_cell_volume                     3391.6(2)
_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      159.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -95.00  13.00   0.80   40.00    --  -18.46 -77.00  90.00  135
  2  \w     -9.00  91.00   0.80   40.00    --   19.40  57.00-150.00  125
  3  \w     35.00 102.20   0.80   40.00    --   19.40 178.00-120.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0113154000
_diffrn_orient_matrix_UB_12      -0.0023558000
_diffrn_orient_matrix_UB_13      0.0234635000
_diffrn_orient_matrix_UB_21      -0.0529122000
_diffrn_orient_matrix_UB_22      0.0160579000
_diffrn_orient_matrix_UB_23      -0.0046738000
_diffrn_orient_matrix_UB_31      -0.0105877000
_diffrn_orient_matrix_UB_32      -0.0778798000
_diffrn_orient_matrix_UB_33      -0.0016501000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            26767
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.516
_diffrn_reflns_theta_min         2.755
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.681
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_correction_T_min  0.286
_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    2.367
_exptl_crystal_description       prism
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.371
_refine_diff_density_min         -1.623
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         5186
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0030P)^2^+12.4278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4347
_reflns_number_total             5186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02714k2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7717431--7717436.cif.'
_cod_database_code               7717436
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C11 H10 Br N6 O5 Re S'
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.214
_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. Restrained distances
 Re1-Br1B \\sim Re1-Br1A
 with sigma of 0.005
 Re1-C13B \\sim Re1-C13A
 with sigma of 0.005
 O13B-C13B \\sim O13A-C13A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C13A) = Uanis(C13B)
Uanis(O13A) = Uanis(O13B)
Uanis(Br1B) = Uanis(Br1A)
4. Others
 Sof(Br1B)=Sof(C13B)=Sof(O13B)=1-FVAR(1)
 Sof(Br1A)=Sof(C13A)=Sof(O13A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              23191
_shelx_hkl_checksum              12910
_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 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.827