#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/54/2015470.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2015470
loop_
_publ_author_name
'Juraj Kuchár'
'Juraj Černák'
'Werner Massa'
_publ_section_title
;
 Hexakis[tris(ethylenediamine-κ²N,N')nickel(II)]
 tricyanocuprate(I) bis{μ-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-κ²N,N')nickel(II)] tricyanocuprate(I)
bis{μ-cyano-bis[tricyanocuprate(I)]} nonahydrate,
[Ni(C₂H₈N₂)₃]₆[Cu₂(CN)₇]₂[Cu(CN)₃].9H₂O
;
_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       φ
_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/[σ²(Fo²)+(0.0446P)²] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'y, x, -z'
'-x+y, -x, z'
'-x, -x+y, -z'
'x-y, -y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.0000 0.0000 0.119160(15) 0.02724(15) Uani d S 1 . .
Ni Ni2 0.0000 0.0000 0.5000 0.0270(2) Uani d S 1 . .
Ni Ni3 0.15322(4) 0.3333 0.3333 0.02197(13) Uani d S 1 . .
Cu Cu4 0.0000 0.0000 0.0000 0.0300(2) Uani d S 1 . .
Cu Cu5 0.0000 0.0000 0.239944(16) 0.03580(17) Uani d S 1 . .
Cu Cu6 0.0000 0.0000 0.378175(14) 0.02865(15) Uani d S 1 . .
N N1 0.0000 0.0000 0.29620(10) 0.0272(9) Uani d S 1 . .
C C1 0.0000 0.0000 0.32615(12) 0.0261(10) Uani d S 1 . .
N N11 0.0259(4) 0.1258(3) 0.15069(10) 0.0667(13) Uani d . 1 . .
H H11A 0.0192 0.1086 0.1740 0.080 Uiso calc R 1 . .
H H11B 0.0901 0.1788 0.1470 0.080 Uiso calc R 1 . .
N N12 -0.0829(4) 0.0510(5) 0.08920(10) 0.0732(15) Uani d . 1 . .
H H12A -0.0667 0.0537 0.0659 0.088 Uiso calc R 1 . .
H H12B -0.1510 0.0071 0.0917 0.088 Uiso calc R 1 . .
C C11 -0.0480(7) 0.1545(5) 0.14094(17) 0.096(3) Uani d . 1 . .
H H11C -0.0262 0.2235 0.1495 0.116 Uiso calc R 1 . .
H H11D -0.1141 0.1076 0.1516 0.116 Uiso calc R 1 . .
C C12 -0.0575(7) 0.1510(6) 0.10155(19) 0.106(3) Uani d . 1 . .
H H12C -0.1108 0.1661 0.0945 0.128 Uiso calc R 1 . .
H H12D 0.0070 0.2025 0.0910 0.128 Uiso calc R 1 . .
N N31 0.2078(2) 0.2316(2) 0.32425(9) 0.0287(7) Uani d . 1 . .
H H31A 0.1914 0.1879 0.3428 0.034 Uiso calc R 1 . .
H H31B 0.1788 0.1945 0.3044 0.034 Uiso calc R 1 . .
N N32 0.1280(2) 0.3066(2) 0.38853(7) 0.0315(6) Uiso d . 1 . .
H H32A 0.0941 0.2384 0.3931 0.038 Uiso calc R 1 . .
H H32B 0.1885 0.3359 0.4003 0.038 Uiso calc R 1 . .
N N33 0.1097(2) 0.4419(2) 0.34390(9) 0.0287(7) Uani d . 1 . .
H H33A 0.1552 0.5028 0.3340 0.034 Uiso calc R 1 . .
H H33B 0.0471 0.4215 0.3345 0.034 Uiso calc R 1 . .
C C31 0.3179(3) 0.2906(3) 0.32012(11) 0.0373(9) Uani d . 1 . .
H H31C 0.3344 0.3179 0.2969 0.045 Uiso d R 1 . .
H H31D 0.3465 0.2479 0.3236 0.045 Uiso d R 1 . .
C C32 0.0668(3) 0.3522(3) 0.39954(10) 0.0354(8) Uiso d . 1 . .
H H32C 0.0704 0.3608 0.4252 0.042 Uiso calc R 1 . .
H H32D -0.0046 0.3072 0.3929 0.042 Uiso calc R 1 . .
C C33 0.1067(3) 0.4529(3) 0.38199(10) 0.0320(8) Uani d . 1 . .
H H33C 0.0628 0.4814 0.3877 0.038 Uiso calc R 1 . .
H H33D 0.1754 0.5002 0.3907 0.038 Uiso calc R 1 . .
C C41 -0.1279(4) -0.1279(4) 0.0000 0.0381(13) Uani d S 1 . .
N N41 -0.2020(4) -0.2020(4) 0.0000 0.0603(16) Uani d S 1 . .
C C51 0.1243(4) 0.1285(4) 0.23033(10) 0.0425(10) Uani d . 1 . .
N N51 0.1977(4) 0.2062(3) 0.22805(11) 0.0646(12) Uani d . 1 . .
C C61 -0.0811(3) 0.0608(3) 0.39484(8) 0.0293(7) Uani d . 1 . .
N N61 -0.1299(3) 0.0930(3) 0.40382(9) 0.0472(9) Uani d . 1 . .
N N21A 0.0576(4) 0.1337(2) 0.46966(7) 0.0500(9) Uani d PD 0.50 A 1
H H21A 0.1235 0.1557 0.4635 0.060 Uiso calc PR 0.255(15) B 1
H H21B 0.0204 0.1213 0.4495 0.060 Uiso calc PR 0.255(15) B 1
N N21B 0.0576(4) 0.1337(2) 0.46966(7) 0.0500(9) Uani d PD 0.50 A 2
H H21C 0.1259 0.1734 0.4733 0.060 Uiso calc PR 0.745(15) B 2
H H21D 0.0470 0.1176 0.4463 0.060 Uiso calc PR 0.745(15) B 2
C C21A 0.0516(8) 0.2125(7) 0.4910(5) 0.071(3) Uani d PDU 0.255(15) . 1
H H21E 0.0584 0.2679 0.4757 0.106 Uiso calc PR 0.255(15) B 1
H H21F 0.1063 0.2411 0.5086 0.106 Uiso calc PR 0.255(15) B 1
C C21B 0.0050(9) 0.1901(7) 0.48008(16) 0.071(3) Uani d PD 0.745(15) . 2
H H21G -0.0625 0.1591 0.4691 0.106 Uiso calc PR 0.745(15) B 2
H H21H 0.0446 0.2612 0.4723 0.106 Uiso calc PR 0.745(15) B 2
O O1 0.2642(5) 0.2979(5) 0.11186(12) 0.0457(15) Uani d PG 0.50 . .
H H1O1 0.2954 0.3396 0.0955 0.069 Uiso d PG 0.50 . .
H H2O1 0.2790 0.2513 0.1106 0.069 Uiso d PG 0.50 . .
O O2 0.2950(8) 0.3651(6) 0.18142(13) 0.105(4) Uani d PG 0.50 . .
H H1O2 0.2607 0.3728 0.1655 0.157 Uiso d PG 0.50 . .
H H2O2 0.2607 0.3050 0.1890 0.157 Uiso d PG 0.50 . .
O O3 0.2018(5) 0.2905(8) 0.11546(17) 0.136(4) Uani d PGU 0.50 . .
H H1O3 0.1935 0.3026 0.1365 0.204 Uiso d PG 0.50 . .
H H2O3 0.1526 0.2857 0.1036 0.204 Uiso d PG 0.50 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N12 Ni1 N12 2 . 93.68(16) ?
N12 Ni1 N12 2 4 93.68(16) ?
N12 Ni1 N12 . 4 93.68(16) ?
N12 Ni1 N11 2 . 170.7(2) ?
N12 Ni1 N11 . . 81.33(18) y
N12 Ni1 N11 4 . 94.4(2) ?
N12 Ni1 N11 2 4 94.4(2) ?
N12 Ni1 N11 . 4 170.7(2) ?
N12 Ni1 N11 4 4 81.33(18) ?
N11 Ni1 N11 . 4 91.22(15) ?
N12 Ni1 N11 2 2 81.33(18) ?
N12 Ni1 N11 . 2 94.4(2) ?
N12 Ni1 N11 4 2 170.7(2) ?
N11 Ni1 N11 . 2 91.22(15) ?
N11 Ni1 N11 4 2 91.22(15) ?
N21B Ni2 N21A 2 2 0.0(4) ?
N21B Ni2 N21B 2 4 92.97(11) ?
N21A Ni2 N21B 2 4 92.97(11) ?
N21B Ni2 N21A 2 4 92.97(11) ?
N21A Ni2 N21A 2 4 92.97(11) ?
N21B Ni2 N21A 4 4 0.0(3) ?
N21B Ni2 N21B 2 3_556 172.3(3) ?
N21A Ni2 N21B 2 3_556 172.3(3) ?
N21B Ni2 N21B 4 3_556 81.7(2) ?
N21A Ni2 N21B 4 3_556 81.7(2) ?
N21B Ni2 N21A 2 3_556 172.3(3) ?
N21A Ni2 N21A 2 3_556 172.3(3) ?
N21B Ni2 N21A 4 3_556 81.7(2) ?
N21A Ni2 N21A 4 3_556 81.7(2) ?
N21B Ni2 N21A 3_556 3_556 0.0(3) ?
N21B Ni2 N21A 2 . 92.97(11) ?
N21A Ni2 N21A 2 . 92.97(11) ?
N21B Ni2 N21A 4 . 92.97(11) ?
N21A Ni2 N21A 4 . 92.97(11) ?
N21B Ni2 N21A 3_556 . 92.8(3) ?
N21A Ni2 N21A 3_556 . 92.8(3) ?
N21B Ni2 N21B 2 5_556 92.8(3) ?
N21A Ni2 N21B 2 5_556 92.8(3) ?
N21B Ni2 N21B 4 5_556 172.3(3) ?
N21A Ni2 N21B 4 5_556 172.3(3) ?
N21B Ni2 N21B 3_556 5_556 92.97(11) ?
N21A Ni2 N21B 3_556 5_556 92.97(11) ?
N21A Ni2 N21B . 5_556 81.7(2) ?
N21B Ni2 N21A 2 5_556 92.8(3) ?
N21A Ni2 N21A 2 5_556 92.8(3) ?
N21B Ni2 N21A 4 5_556 172.3(3) ?
N21A Ni2 N21A 4 5_556 172.3(3) ?
N21B Ni2 N21A 3_556 5_556 92.97(11) ?
N21A Ni2 N21A 3_556 5_556 92.97(11) ?
N21A Ni2 N21A . 5_556 81.7(2) ?
N21B Ni2 N21A 5_556 5_556 0.0(3) ?
N21B Ni2 N21B 2 6_556 81.7(2) ?
N21A Ni2 N21B 2 6_556 81.7(2) ?
N21B Ni2 N21B 4 6_556 92.8(3) ?
N21A Ni2 N21B 4 6_556 92.8(3) ?
N21B Ni2 N21B 3_556 6_556 92.97(11) ?
N21A Ni2 N21B 3_556 6_556 92.97(11) ?
N21A Ni2 N21B . 6_556 172.3(3) ?
N21B Ni2 N21B 5_556 6_556 92.97(11) ?
N21A Ni2 N21B 5_556 6_556 92.97(11) ?
N21B Ni2 N21A 2 6_556 81.7(2) ?
N21A Ni2 N21A 2 6_556 81.7(2) y
N21B Ni2 N21A 4 6_556 92.8(3) ?
N21A Ni2 N21A 4 6_556 92.8(3) ?
N21B Ni2 N21A 3_556 6_556 92.97(11) ?
N21A Ni2 N21A 3_556 6_556 92.97(11) ?
N21A Ni2 N21A . 6_556 172.3(3) ?
N21B Ni2 N21A 5_556 6_556 92.97(11) ?
N21A Ni2 N21A 5_556 6_556 92.97(11) ?
N21B Ni2 N21A 6_556 6_556 0.0(4) ?
N33 Ni3 N33 18 . 89.92(17) ?
N33 Ni3 N31 18 . 94.26(10) ?
N33 Ni3 N31 . . 175.74(14) y
N33 Ni3 N31 18 18 175.73(14) ?
N33 Ni3 N31 . 18 94.27(10) ?
N31 Ni3 N31 . 18 81.56(16) ?
N33 Ni3 N32 18 . 90.91(12) ?
N33 Ni3 N32 . . 82.23(12) y
N31 Ni3 N32 . . 96.88(12) y
N31 Ni3 N32 18 . 90.46(12) ?
N33 Ni3 N32 18 18 82.23(12) ?
N33 Ni3 N32 . 18 90.91(12) ?
N31 Ni3 N32 . 18 90.45(12) ?
N31 Ni3 N32 18 18 96.87(12) ?
N32 Ni3 N32 . 18 170.33(15) ?
C41 Cu4 C41 4 2 120.0 ?
C41 Cu4 C41 4 . 120.0 ?
C41 Cu4 C41 2 . 120.0 ?
C51 Cu5 C51 . 4 116.60(7) ?
C51 Cu5 C51 . 2 116.60(7) ?
C51 Cu5 C51 4 2 116.60(7) ?
C51 Cu5 N1 . . 100.75(12) ?
C51 Cu5 N1 4 . 100.75(12) ?
C51 Cu5 N1 2 . 100.75(12) ?
C1 Cu6 C61 . 4 108.67(9) ?
C1 Cu6 C61 . . 108.67(9) ?
C61 Cu6 C61 4 . 110.26(8) ?
C1 Cu6 C61 . 2 108.67(9) ?
C61 Cu6 C61 4 2 110.26(8) ?
C61 Cu6 C61 . 2 110.26(8) ?
C1 N1 Cu5 . . 180.0000(10) ?
N1 C1 Cu6 . . 180.0 ?
C11 N11 Ni1 . . 107.9(3) ?
C11 N11 H11A . . 110.1 ?
Ni1 N11 H11A . . 110.1 ?
C11 N11 H11B . . 110.1 ?
Ni1 N11 H11B . . 110.1 ?
H11A N11 H11B . . 108.4 ?
C12 N12 Ni1 . . 108.4(4) ?
C12 N12 H12A . . 110.0 ?
Ni1 N12 H12A . . 110.0 ?
C12 N12 H12B . . 110.0 ?
Ni1 N12 H12B . . 110.0 ?
H12A N12 H12B . . 108.4 ?
N11 C11 C12 . . 108.7(5) ?
N11 C11 H11C . . 109.9 ?
C12 C11 H11C . . 109.9 ?
N11 C11 H11D . . 109.9 ?
C12 C11 H11D . . 109.9 ?
H11C C11 H11D . . 108.3 ?
N12 C12 C11 . . 109.3(4) ?
N12 C12 H12C . . 109.8 ?
C11 C12 H12C . . 109.8 ?
N12 C12 H12D . . 109.8 ?
C11 C12 H12D . . 109.8 ?
H12C C12 H12D . . 108.3 ?
C31 N31 Ni3 . . 108.5(2) ?
C31 N31 H31A . . 110.0 ?
Ni3 N31 H31A . . 110.0 ?
C31 N31 H31B . . 110.0 ?
Ni3 N31 H31B . . 110.0 ?
H31A N31 H31B . . 108.4 ?
C32 N32 Ni3 . . 106.6(2) ?
C32 N32 H32A . . 110.4 ?
Ni3 N32 H32A . . 110.4 ?
C32 N32 H32B . . 110.4 ?
Ni3 N32 H32B . . 110.4 ?
H32A N32 H32B . . 108.6 ?
C33 N33 Ni3 . . 108.6(2) ?
C33 N33 H33A . . 110.0 ?
Ni3 N33 H33A . . 110.0 ?
C33 N33 H33B . . 110.0 ?
Ni3 N33 H33B . . 110.0 ?
H33A N33 H33B . . 108.3 ?
N31 C31 C31 . 18 109.0(3) ?
N31 C31 H31C . . 109.7 ?
C31 C31 H31C 18 . 109.6 ?
N31 C31 H31D . . 109.9 ?
C31 C31 H31D 18 . 110.3 ?
H31C C31 H31D . . 108.4 ?
N32 C32 C33 . . 109.2(3) ?
N32 C32 H32C . . 109.8 ?
C33 C32 H32C . . 109.8 ?
N32 C32 H32D . . 109.8 ?
C33 C32 H32D . . 109.8 ?
H32C C32 H32D . . 108.3 ?
N33 C33 C32 . . 110.2(3) ?
N33 C33 H33C . . 109.6 ?
C32 C33 H33C . . 109.6 ?
N33 C33 H33D . . 109.6 ?
C32 C33 H33D . . 109.6 ?
H33C C33 H33D . . 108.1 ?
N41 C41 Cu4 . . 180.0(9) ?
N51 C51 Cu5 . . 173.5(4) ?
N61 C61 Cu6 . . 177.8(4) ?
C21A N21A Ni2 . . 108.4(7) ?
C21A N21A H21A . . 110.0 ?
Ni2 N21A H21A . . 110.0 ?
C21A N21A H21B . . 110.0 ?
Ni2 N21A H21B . . 110.0 ?
H21A N21A H21B . . 108.4 ?
N21A C21A C21A . 5_556 107.1(8) ?
N21A C21A H21E . . 110.3 ?
C21A C21A H21E 5_556 . 110.3 ?
N21A C21A H21F . . 110.3 ?
C21A C21A H21F 5_556 . 110.3 ?
H21E C21A H21F . . 108.6 ?
C21B C21B H21G 5_556 . 110.1 ?
C21B C21B H21H 5_556 . 110.1 ?
H21G C21B H21H . . 108.5 ?
H1O1 O1 H2O1 . . 107.7 ?
H1O1 O1 H1O3 . . 126.1 ?
H2O1 O1 H1O3 . . 126.1 ?
O2 O2 H1O2 11 . 80.0 ?
O2 O2 H2O2 11 . 127.6 ?
H1O2 O2 H2O2 . . 107.7 ?
H1O1 O3 H1O3 . . 126.8 ?
H1O1 O3 H2O3 . . 111.4 ?
H1O3 O3 H2O3 . . 107.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N12 2 2.126(4) ?
Ni1 N12 . 2.126(4) y
Ni1 N12 4 2.126(4) ?
Ni1 N11 . 2.134(4) y
Ni1 N11 4 2.134(4) ?
Ni1 N11 2 2.134(4) ?
Ni2 N21B 2 2.123(3) ?
Ni2 N21A 2 2.123(3) ?
Ni2 N21B 4 2.123(3) ?
Ni2 N21A 4 2.123(3) ?
Ni2 N21B 3_556 2.123(3) ?
Ni2 N21A 3_556 2.123(3) ?
Ni2 N21A . 2.123(3) y
Ni2 N21B 5_556 2.123(3) ?
Ni2 N21A 5_556 2.123(3) ?
Ni2 N21B 6_556 2.123(3) ?
Ni2 N21A 6_556 2.123(3) ?
Ni3 N33 18 2.115(3) ?
Ni3 N33 . 2.115(3) y
Ni3 N31 . 2.131(3) y
Ni3 N31 18 2.131(3) ?
Ni3 N32 . 2.148(3) y
Ni3 N32 18 2.148(3) ?
Cu4 C41 4 1.958(6) ?
Cu4 C41 2 1.958(6) ?
Cu4 C41 . 1.958(6) y
Cu5 C51 . 1.970(5) y
Cu5 C51 4 1.970(5) ?
Cu5 C51 2 1.970(5) ?
Cu5 N1 . 2.152(4) y
Cu6 C1 . 1.990(5) y
Cu6 C61 4 1.991(4) ?
Cu6 C61 . 1.991(4) y
Cu6 C61 2 1.991(4) ?
N1 C1 . 1.145(6) y
N11 C11 . 1.451(8) ?
N11 H11A . 0.9200 ?
N11 H11B . 0.9200 ?
N12 C12 . 1.457(8) ?
N12 H12A . 0.9200 ?
N12 H12B . 0.9200 ?
C11 C12 . 1.512(9) ?
C11 H11C . 0.9900 ?
C11 H11D . 0.9900 ?
C12 H12C . 0.9900 ?
C12 H12D . 0.9900 ?
N31 C31 . 1.469(5) ?
N31 H31A . 0.9200 ?
N31 H31B . 0.9200 ?
N32 C32 . 1.481(5) ?
N32 H32A . 0.9200 ?
N32 H32B . 0.9200 ?
N33 C33 . 1.470(5) ?
N33 H33A . 0.9200 ?
N33 H33B . 0.9200 ?
C31 C31 18 1.519(8) ?
C31 H31C . 0.9599 ?
C31 H31D . 0.9600 ?
C32 C33 . 1.503(5) ?
C32 H32C . 0.9900 ?
C32 H32D . 0.9900 ?
C33 H33C . 0.9900 ?
C33 H33D . 0.9900 ?
C41 N41 . 1.133(7) ?
C51 N51 . 1.161(6) ?
C61 N61 . 1.135(5) ?
N21A C21A . 1.496(9) ?
N21A H21A . 0.9200 ?
N21A H21B . 0.9200 ?
C21A C21A 5_556 1.531(13) ?
C21A H21E . 0.9900 ?
C21A H21F . 0.9900 ?
C21B C21B 5_556 1.529(12) ?
C21B H21G . 0.9900 ?
C21B H21H . 0.9900 ?
O1 H1O1 . 0.8499 ?
O1 H2O1 . 0.8499 ?
O1 H1O3 . 1.4639 ?
O2 O2 11 1.519(17) ?
O2 H1O2 . 0.8501 ?
O2 H2O2 . 0.8500 ?
O3 H1O1 . 1.4576 ?
O3 H1O3 . 0.8500 ?
O3 H2O3 . 0.8500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N11 H11B O3 . 0.92 2.09 2.937(11) 152.1
N12 H12B O3 2 0.92 2.10 2.98(8) 160.2
N12 H12B O1 2 0.92 2.15 2.998(8) 152.5
N31 H31A N61 4 0.92 2.63 3.478(5) 154.4
N32 H32B N51 18 0.92 2.48 3.346(5) 156.8
N33 H33B N41 8_455 0.92 2.37 3.225(6) 155.5
N21A H21A O2 18 0.92 2.34 2.96(7) 124.8
O1 H1O1 N61 14_554 0.85 2.35 2.905(7) 123.6
O1 H2O1 N12 4 0.85 2.55 2.998(8) 113.7
O2 H1O2 O3 . 0.85 2.22 2.842 130.0
O2 H1O2 O1 . 0.85 2.36 2.806 112.8
O2 H2O2 N51 . 0.85 2.00 2.773(9) 151.2
