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_4307062
_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 described
;
_chemical_formula_moiety         ' C12 H22 N6 O1 S2 Zn1 '
_chemical_formula_sum            'C12 H22 N6 O S2 Zn'
_chemical_formula_weight         395.86
_chemical_name_systematic
; 
diacetyl-2-(4-N-ethyl-3-thiosemicarbazonato)-
3-(4-N-allyl-3-thiosemicarbazonato) zinc(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90
_cell_angle_beta                 99.5855(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4508(2)
_cell_length_b                   14.7225(3)
_cell_length_c                   16.3562(3)
_cell_measurement_reflns_used    18591
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1769.13(7)
_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_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.063
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18591
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         5.123
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_thermal_history
; 
The material was crystallised at ambient temperature. A suitable crystal 
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. 
;
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1280
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         2537
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.029709
_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: 
 0.819 0.484 0.612 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0610
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0453
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2537
_reflns_number_total             4006
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic0615628si20060817_104225_1.cif
_cod_data_source_block           Compound17
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1 21/n 1 '
_cod_original_formula_sum        ' C12 H22 N6 O1 S2 Zn1 '
_cod_database_code               4307062