A mixed-valence Cu^II^/Cu^I^ anion–cation complex: bis[μ-5-sulfosalicylato(3–)]bis[(di-2-pyridylamine)copper(II)] bis[bis(di-2-pyridylamine)copper(I)] dihydrate
Fan, Sai-Rong; Cai, Guo-Qiang; Zhu, Long-Guan; Xiao, Hong-Ping; Acta Crystallographica Section C 61 (2005) m177–m179; doi:10.1107/S0108270105004580

data_2014878
_publ_section_title
;
 A mixed-valence Cu^II^/Cu^I^ anion--cation complex:
 bis[\m-5-sulfosalicylato(3--)]bis[(di-2-pyridylamine)copper(II)]
 bis[bis(di-2-pyridylamine)copper(I)] dihydrate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m177
_journal_page_last               m179
_journal_paper_doi               10.1107/S0108270105004580
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'[Cu2 (C7 H3 O6 S)2 (C10 H9 N3)2] [Cu (C10 H9 N3)2]2, 2H2 O'
_chemical_formula_moiety
'C34 H24 Cu2 N6 O12 S2 2-, 2C20 H18 Cu N6 +, 2H2 O'
_chemical_formula_sum            'C74 H64 Cu4 N18 O14 S2'
_chemical_formula_weight         1747.71
_chemical_name_systematic
;
bis[\m-5-sulfosalicylato(3-)]bis[(di-2-pyridylamine)copper(II)]
bis[bis(di-2-pyridylamine)copper(I)] dihydrate
;
_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-97
_cell_angle_alpha                82.428(4)
_cell_angle_beta                 80.697(4)
_cell_angle_gamma                86.409(4)
_cell_formula_units_Z            1
_cell_length_a                   7.258(2)
_cell_length_b                   14.422(4)
_cell_length_c                   18.312(5)
_cell_measurement_reflns_used    4694
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.22
_cell_measurement_theta_min      2.53
_cell_volume                     1873.4(9)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
'Bruker SMART APEX area-detector diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13648
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.414
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6582
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+3.6691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                6078
_reflns_number_total             6582
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1813.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1873.5(9)
_cod_database_code               2014878
_cod_database_fobs_code          2014878