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_7036225
_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         'C11 H10 Br N4 O6 Re S, 1(C7 H8)'
_chemical_formula_sum            'C18 H18 Br N4 O6 Re S'
_chemical_formula_weight         684.53
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-05-23 deposited with the CCDC.
2015-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.055(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1341(6)
_cell_length_b                   18.3725(10)
_cell_length_c                   11.6288(6)
_cell_measurement_reflns_used    9162
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      2.17
_cell_volume                     2334.7(2)
_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      296.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19069
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.168
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.046
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.2969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1463 before and 0.0742 after correction. The Ratio of minimum to maximum transmission is 0.3981. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.353
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4570
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0570P)^2^+16.3538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3411
_reflns_number_total             4570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02264a2.cif
_cod_data_source_block           mcd_esc_re_jan14_0m
_cod_depositor_comments
'Adding full bibliography for 7036222--7036227.cif.'
_cod_database_code               7036225
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C18
 1.47 with sigma of 0.04
 C13A-C18A
 1.47 with sigma of 0.04
 C18-C14 \\sim C18-C12 \\sim C18A-C14A \\sim C18A-C12A
 with sigma of 0.04
3. Rigid bond restraints
 C18, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
C13A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C18) = Uanis(C18A)
5. Rigid body (RIGU) restrains
 C13, C14, C15, C16, C17, C12, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C14A, C15A, C16A, C17A, C12A, C18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C13A)=Sof(C12A)=Sof(H12A)=
 Sof(C17A)=Sof(H17A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=Sof(C14A)=
 Sof(H14A)=1-FVAR(1)
 Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=
 Sof(H17)=Sof(C12)=Sof(H12)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
7.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F)
7.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), N4(H4), N2(H2), C14(H14), C15(H15), C16(H16),
 C17(H17), C12(H12), C12A(H12A), C17A(H17A), C16A(H16A), C15A(H15A), C14A(H14A)
7.d Fitted hexagon refined as free rotating group:
 C13(C14,C15,C16,C17,C12), C13A(C12A,C17A,C16A,C15A,C14A)
7.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              96273
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'