Functionalized Thiosemicarbazone Clusters of Copper(I) and Silver(I)
Laura J. Ashfield; Andrew R. Cowley; Jonathan R. Dilworth; Paul S. Donnelly; Inorganic Chemistry 43 (2004) 4121–4123; doi:10.1021/ic035451+

data_4327378
_publ_contact_author_address
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Inorganic Chemistry Laboratory 
University of Oxford
South Parks Road                        
Oxford OX1 3QR, UK                      
;
_publ_contact_author_name        'Dilworth, Jonathan R.'
_publ_section_title
;
 Functionalized Thiosemicarbazone Clusters of Copper(I) and Silver(I)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4121
_journal_page_last               4123
_journal_paper_doi               10.1021/ic035451+
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety
' C48 H48 Cu4 Fe4 N12 S4, 3(C4 H10 O), C3 H7 N O '
_chemical_formula_sum            'C63 H85 Cu4 Fe4 N13 O4 S4'
_chemical_formula_weight         1694.25
_chemical_name_systematic
;                                                             
?                                                             
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.4412(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4351(2)
_cell_length_b                   12.3172(2)
_cell_length_c                   46.2731(3)
_cell_measurement_reflns_used    68643
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     7066.17(17)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.056
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            68643
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         5.11
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.149
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' orange-brown '
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             3490.924
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0430
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         10001
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.022200
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979,
0.497    0.131    0.271   
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0389
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              59
_reflns_limit_l_min              0
_reflns_number_gt                10001
_reflns_number_total             15934
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ic0354512Bsi20031218_101248_1.cif
_cod_data_source_block           Compound_6
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C63 H85 Cu4 Fe4 N13 O4 S4 '
_cod_database_code               4327378