Bis[tris(bipyridine)nickel(II)] tris[dicyanoargentate(I)] chloride <i>n</i>-hydrate (<i>n</i> = 9)
Černák, Juraj; Kaňuchová, Mária; Chomič, Jozef; Potočňák, Ivan; Kameníček, Jiří; Žák, Zdirad; Acta Crystallographica Section C 50 (1994) 1563–1566; doi:10.1107/S0108270194005500

data_2010110
_publ_section_title
;
 Bis[tris(bipyridine)nickel(II)] tris[dicyanoargentate(I)] chloride
 <i>n</i>-hydrate (<i>n</i> = 9)
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1563
_journal_page_last               1566
_journal_paper_doi               10.1107/S0108270194005500
_journal_volume                  50
_journal_year                    1994
_chemical_formula_analytical
'2[Ni(C~10~H~8~N~2~)~3~] , 3[AgC~4~N~4~] , Cl , 9(H~2~O)'
_chemical_formula_moiety
'2[Ni (C10 H8 N2 )3 ] 2+ , 3Ag (C N )2 1- , Cl 1- , 9H2 O'
_chemical_formula_structural     '[Ni(bpy)~3~]~2~[Ag(CN)~2~]~3~.Cl.9H~2~O'
_chemical_formula_sum            'C66 H66 Ag3 Cl N18 Ni2 O9'
_chemical_formula_weight         1731.84
_chemical_name_systematic
;
Bis[tris(2,2'-bipyridine)nickel(II)] tris(dicyanoargentate(I)
chloride nonahydrate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3*'
_symmetry_space_group_name_H-M   'R -3 :R'
_audit_creation_method           SHELXL
_cell_angle_alpha                86.010(10)
_cell_angle_beta                 86.010(10)
_cell_angle_gamma                86.010(10)
_cell_formula_units_Z            1
_cell_length_a                   12.218(2)
_cell_length_b                   12.218(2)
_cell_length_c                   12.218(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.66
_cell_measurement_theta_min      9.47
_cell_volume                     1811.2(5)
_computing_cell_refinement       'KM-4 software'
_computing_data_collection       'KM-4 software'
_computing_data_reduction        'KM-4 software'
_computing_molecular_graphics
'ORTEP (Johnson, 1965); MOLDRAW (Ugliengo, Borzani & Viterbo, 1988)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'KUMA KM-4 \k-axis diffractometer'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5989
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'reddish violet'
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_meas      1.56
_exptl_crystal_density_method    'flotation in bromoform/acetone'
_exptl_crystal_description       pseudocube
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.943
_refine_ls_goodness_of_fit_obs   1.164
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_obs          0.0383
_refine_ls_shift/esd_max         0.024
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w=1/[\s^2^(F~o~^2^)+(0.0717P)^2^+0.0000P]
 where P=(F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1318
_refine_ls_wR_factor_obs         0.1121
_reflns_number_observed          1737
_reflns_number_total             3526
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ka1082.cif
_cod_data_source_block           niagall
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C66 H66 Ag3 Cl1 N18 Ni2 O9'
_cod_database_code               2010110