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_4307063
_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         ' C8 H13 N3 O S '
_chemical_formula_sum            'C8 H13 N3 O S'
_chemical_formula_weight         199.28
_chemical_name_systematic
; 
diacetyl-2-(4-N-allyl-3-thiosemicarbazone) 
;
_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                 90.1257(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8603(2)
_cell_length_b                   17.3868(4)
_cell_length_c                   8.5281(2)
_cell_measurement_reflns_used    11561
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1017.22(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.054
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11561
_diffrn_reflns_theta_full        27.493
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         5.186
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_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         0.29
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1562
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.028447
_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: 
 0.376 0.156 0.151 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0619
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0381
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                1562
_reflns_number_total             2301
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic0615628si20060817_104225_2.cif
_cod_data_source_block           Compound5
_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        ' C8 H13 N3 O S '
_cod_database_code               4307063