Functionalized Bis(thiosemicarbazonato) Complexes of Zinc and Copper: Synthetic Platforms Toward Site-Specific Radiopharmaceuticals
Jason P. Holland; Franklin I. Aigbirhio; Helen M. Betts; Paul D. Bonnitcha; Paul Burke; Martin Christlieb; Grant C. Churchill; Andrew R. Cowley; Jonathan R. Dilworth; Paul S. Donnelly; Jennifer C. Green; Josephine M. Peach; Sridhar R. Vasudevan; John E. Warren; Inorganic Chemistry 46 (2007) 465–485; doi:10.1021/ic0615628

data_4307065
_publ_contact_author
;
'Jonathan R. Dilworth'
;
_publ_contact_author_address
;
Chemistry Research Laboratory,
Department of Chemistry,
University of Oxford,
12 Mansfield Road,
Oxford,
UK,
OX1 3TA
;
_publ_contact_author_email
;
'jon.dilworth@chem.ox.ac.uk'
;
_publ_contact_author_phone
;
'01865 285151'
;
_publ_section_title
;
Functionalized Bis(thiosemicarbazonato) Complexes of Zinc and Copper:
Synthetic Platforms Toward Site-Specific Radiopharmaceuticals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              465
_journal_page_last               485
_journal_paper_doi               10.1021/ic0615628
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'synthesis as discussed'
_chemical_formula_moiety         'C7 H13 N7 S2 Zn '
_chemical_formula_sum            'C7 H13 N7 S2 Zn'
_chemical_formula_weight         324.77
_chemical_name_systematic
;
diacetyl-2-(4-N-methyl-3-thiosemicarbazonato)-
3-(4-N-amino-3-thiosemicarbazonato) zinc(II)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-12-08
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.8643(14)
_cell_length_b                   14.627(2)
_cell_length_c                   17.117(2)
_cell_measurement_reflns_used    16526
_cell_measurement_temperature    150
_cell_measurement_theta_max      32
_cell_measurement_theta_min      1
_cell_volume                     2469.7(6)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.84570
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16526
_diffrn_reflns_theta_full        32
_diffrn_reflns_theta_max         31.632
_diffrn_reflns_theta_min         2.964
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.316
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Correction applied by SADABS 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1044
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         2920
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.004054
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.404 0.295 0.232 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0607
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0433
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -21
_reflns_number_gt                2920
_reflns_number_total             4611
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_cod_data_source_file            ic0615628si20060817_104225_4.cif
_cod_data_source_block           Compound12
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C7 H13 N7 S2 Zn '
_cod_database_code               4307065