Copper(II) Complexes of Histamine and Cysteine Produced by Thiosulfate-Assisted Synthesis Using Copper(I) Cyanide. The in Situ Formation of the Thiocyanate Anion and the 2-Amino-2-thiazoline-4-carboxylic Acid Ligand
Fred B. Stocker; Paul Fadden; Spencer Dreher; Doyle Britton; Inorganic Chemistry 38 (1999) 3251–3253; doi:10.1021/ic9814118

data_4322113
_publ_section_title
;
 Copper(II) Complexes of Histamine and Cysteine Produced by
 Thiosulfate-Assisted Synthesis Using Copper(I) Cyanide. The in Situ
 Formation of the Thiocyanate Anion and the
 2-Amino-2-thiazoline-4-carboxylic Acid Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3251
_journal_page_last               3253
_journal_paper_doi               10.1021/ic9814118
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_sum            'C12 H18 Cu N8 S2'
_chemical_formula_weight         402.00
_chemical_name_systematic
;
 bis(histamine)copper(II) thiocyanate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL plus manual editing'
_cell_angle_alpha                87.81(2)
_cell_angle_beta                 85.74(2)
_cell_angle_gamma                66.93(2)
_cell_formula_units_Z            2
_cell_length_a                   8.552(2)
_cell_length_b                   9.254(2)
_cell_length_c                   11.625(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      12
_cell_volume                     844.0(3)
_computing_cell_refinement       'Enraf-Nonius CAD-4 Version 5.0'
_computing_data_collection       'Enraf-Nonius CAD-4 Version 5.0'
_computing_data_reduction        'TEXSAN (Moleular Structure Corp., 1985)'
_computing_molecular_graphics    'SHELXTL V5.0'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution
;
MITHRIL (Gilmore, 1984); DIRDIF(BUERSKENS, 1984)
;
_diffrn_ambient_temperature      297(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'omega-two theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4827
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        'less than 1 %'
_diffrn_standards_interval_time  '100 sec'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.552
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.582(1)
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_hydrogen_treatment    'idealized positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_obs          0.0434
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.2670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1112
_refine_ls_wR_factor_obs         0.1006
_reflns_number_observed          2528
_reflns_number_total             3317
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9814118_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.2670P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.2670P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322113