Hexakis[tris(ethylenediamine-κ^2^<i>N</i>,<i>N</i>')nickel(II)] tricyanocuprate(I) bis{μ-cyano-bis[tricyanocuprate(I)]} nonahydrate
Juraj Kuchár; Juraj Černák; Werner Massa; Acta Crystallographica Section C 62 (2006) m337–m339; doi:10.1107/S0108270106015769

data_2015470
_publ_section_title
;
 Hexakis[tris(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')nickel(II)]
 tricyanocuprate(I) bis{\m-cyano-bis[tricyanocuprate(I)]} nonahydrate
;
_journal_coeditor_code           DN3005
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m337
_journal_page_last               m339
_journal_paper_doi               10.1107/S0108270106015769
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Ni (C2 H8 N2)3]6 [Cu2 (C N)7]2 [Cu (C N)3], 9H2 O'
_chemical_formula_moiety
'6C6 H24 N6 Ni1 2+, 2C7 Cu2 N7 5-, C3 Cu1 N3 2-, 9H2 O'
_chemical_formula_sum            'C53 H162 Cu5 N53 Ni6 O9'
_chemical_formula_weight         2356.32
_chemical_name_systematic
;
hexakis[tris(ethylenediamine-\k^2^N,N')nickel(II)] tricyanocuprate(I)
bis{\m-cyano-bis[tricyanocuprate(I)]} nonahydrate,
[Ni(C~2~H~8~N~2~)~3~]~6~[Cu~2~(CN)~7~]~2~[Cu(CN)~3~].9H~2~O
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.3025(5)
_cell_length_b                   15.3025(5)
_cell_length_c                   38.2467(17)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30.3
_cell_measurement_theta_min      2.6
_cell_volume                     7756.2(5)
_computing_cell_refinement       'CELL in IPDS'
_computing_data_collection       'EXPOSE in IPDS (Stoe & Cie, 1999)'
_computing_data_reduction        'INTEGRATE in IPDS'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2001)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            27795
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(WinGX; Farrugia, 1999; Spek, 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3708
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.617
_refine_ls_abs_structure_details 'Flack (1983), 2050 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         4597
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                3287
_reflns_number_total             4597
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn3005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'R 3 2'
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               2015470