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_7036224
_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         'C22 H18 N8 O12 Re2 S2, C H4 O, C3 H6 O'
_chemical_formula_sum            'C26 H28 N8 O14 Re2 S2'
_chemical_formula_weight         1113.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-20
_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                 99.338(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2120(8)
_cell_length_b                   41.834(4)
_cell_length_c                   9.7296(9)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      2.29
_cell_volume                     3699.9(6)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            32654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.947
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.724
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1226 before and 0.0666 after correction. The Ratio of minimum to maximum transmission is 0.4909. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.509
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.179(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         14131
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0294P)^2^+7.1922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.971
_reflns_friedel_fraction_full    0.999
_reflns_friedel_fraction_max     0.999
_reflns_number_gt                13055
_reflns_number_total             14131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02264a2.cif
_cod_data_source_block           mcd_reesc_14mar14_0m
_cod_depositor_comments
'Adding full bibliography for 7036222--7036227.cif.'
_cod_database_code               7036224
_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, All O(H) groups
2. Restrained distances
 C57B-C56B \\sim C56B-C55B \\sim C53B-C52B \\sim C52B-C51B
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10A(H10A,H10B), C30A(H30A,H30B), C10B(H10C,H10D), C30B(H30C,H30D)
3.b Aromatic/amide H refined with riding coordinates:
 N4A(H4A), N8A(H8A), C5A(H5A), C7A(H7A), C8A(H8AA), C25A(H25A), C27A(H27A),
 C28A(H28A), N4B(H4B), N8B(H8B), C5B(H5B), C7B(H7B), C8B(H8BA), C25B(H25B),
 C27B(H27B), C28B(H28B)
3.c Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C31A(H31A,H31B,H31C), C11B(H11D,H11E,H11F), C31B(H31D,
 H31E,H31F), C50B(H50A,H50C,H50D), C51B(H51A,H51B,H51C), C53B(H53A,H53B,H53C),
 C54B(H54A,H54B,H54C), C55B(H55A,H55B,H55C), C57B(H57A,H57B,H57C)
3.d Idealised tetrahedral OH refined as rotating group:
 O50B(H50B), O53B(H53D)
;
_shelx_res_checksum              12863
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'