Tricarbonyl (99m)Tc(i) and Re(i)-thiosemicarbazone complexes: synthesis, characterization and biological evaluation for targeting bacterial infection.
Nayak, Dipak Kumar; Baishya, Rinku; Natarajan, Ramalingam; Sen, Tuhinadri; Debnath, Mita Chatterjee; Dalton transactions (Cambridge, England : 2003) 44 (2015) 16136–16148; doi:10.1039/c5dt02264a

data_7036227
_publ_section_title
;
 Tricarbonyl (99m)Tc(i) and Re(i)-thiosemicarbazone complexes: synthesis,
 characterization and biological evaluation for targeting bacterial
 infection.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16136
_journal_page_last               16148
_journal_paper_doi               10.1039/c5dt02264a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C10 H8 Br N4 O6 Re S, 0.5(C7 H8)'
_chemical_formula_sum            'C13.5 H12 Br N4 O6 Re S'
_chemical_formula_weight         624.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-05-25 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                94.519(5)
_cell_angle_beta                 97.975(5)
_cell_angle_gamma                90.201(4)
_cell_formula_units_Z            2
_cell_length_a                   7.5512(7)
_cell_length_b                   10.6017(9)
_cell_length_c                   12.8522(12)
_cell_measurement_reflns_used    9633
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.056
_cell_measurement_theta_min      2.409
_cell_volume                     1015.66(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18391
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.255
_diffrn_reflns_theta_min         1.927
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.087
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1506 before and 0.0903 after correction.
The Ratio of minimum to maximum transmission is 0.4665.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_description       block
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.973
_refine_diff_density_min         -1.786
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4491
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0689P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3956
_reflns_number_total             4491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02264a2.cif
_cod_data_source_block           mcd_msc2_020315_0m_a
_cod_depositor_comments
'Adding full bibliography for 7036222--7036227.cif.'
_cod_original_formula_sum        'C13.50 H12 Br N4 O6 Re S'
_cod_database_code               7036227
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C11 \\sim C17-C13
 with sigma of 0.02
3. Rigid bond restraints
 C17, C11, C12, C16, C13, C15, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim C16 \\sim C13 \\sim C17 \\sim C15 \\sim C14: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O5) = Uanis(O6)
5. Rigid body (RIGU) restrains
 C17, C11, C12, C16, C13, C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C11(0.5) H11(0.5) C12(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5)
 C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5)
7.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C)
7.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C5(H5), C7(H7), C8(H8), C11(H11), C13(H13), C14(H14),
 C15(H15), C16(H16)
7.c Fitted hexagon refined as free rotating group:
 C11(C12,C13,C14,C15,C16)
7.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              11258
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'