An Unusual Dimeric Structure of a Cu(I) Bis(thiosemicarbazone) Complex: Implications for the Mechanism of Hypoxic Selectivity of the Cu(II) Derivatives
Andrew R. Cowley; Jonathan R. Dilworth; Paul S. Donnelly; Elena Labisbal; Antonio Sousa; Journal of the American Chemical Society 124 (2002) 5270–5271; doi:10.1021/ja012668z

data_4114797
_publ_section_title
;
 An Unusual Dimeric Structure of a Cu(I) Bis(thiosemicarbazone) Complex:
 Implications for the Mechanism of Hypoxic Selectivity of the Cu(II)
 Derivatives
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5270
_journal_page_last               5271
_journal_paper_doi               10.1021/ja012668z
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C8 H14 N6 S2 Zn1 '
_chemical_formula_sum            'C8 H14 N6 S2 Zn'
_chemical_formula_weight         323.74
_chemical_name_systematic
;                                                                          
?                                                                          
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             01-13-06
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                99.1702(8)
_cell_angle_beta                 107.5031(8)
_cell_angle_gamma                105.033(1)
_cell_formula_units_Z            2
_cell_length_a                   7.3522(1)
_cell_length_b                   9.9455(2)
_cell_length_c                   10.0514(3)
_cell_measurement_reflns_used    45757
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     654.09(3)
_computing_cell_refinement
;                                                                          
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)                       
;
_computing_data_collection
;                                                                          
KappaCCD software 'Collect' (Nonius, 2000)                                 
;
_computing_data_reduction
;                                                                          
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)                       
;
_computing_publication_material
;                                                                          
CRYSTALS (Watkin et al, 2001)                                              
;
_computing_structure_refinement
;                                                                          
CRYSTALS (Watkin et al, 2001)                                              
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
;                                                                          
Nonius KappaCCD                                                            
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11099
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         5.36
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.184
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             332.873
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0068
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2697
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.004714
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
 1.80    -.147     1.03    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0243
_reflns_limit_h_max              8
_reflns_limit_h_min              -9
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2697
_reflns_number_total             2956
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ja012668z_2.cif
_cod_data_source_block           Zn(II)_thiosemicarbazone
_cod_original_cell_volume        654.1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C8 H14 N6 S2 Zn1 '
_cod_database_code               4114797