#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/24/8102448.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8102448
loop_
_publ_author_name
'Meng Guo'
'Fang-Fang Jian'
_publ_section_title
;
 Crystal structure of
 catena-(hexaaqua-tetrakis(isocyanurato)nickel-disodium),
 Na2Ni(H2O)6(C3N3O3)4
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              573
_journal_volume                  224
_journal_year                    2009
_chemical_formula_moiety         'C12 H20 N12 Na2 Ni O18'
_chemical_formula_sum            'C12 H20 N12 Na2 Ni O18'
_chemical_formula_weight         725.11
_chemical_name_systematic
; 
catena-(Hexa-aqua-tetrakis(isocyanurato)-nickel-di-sodium), 
C₁₂H₂₀N₁₂Na₂Ni₁O₁₈
;
_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                62.83(3)
_cell_angle_beta                 83.72(3)
_cell_angle_gamma                71.82(3)
_cell_formula_units_Z            1
_cell_length_a                   6.7600(14)
_cell_length_b                   10.443(2)
_cell_length_c                   10.455(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.30
_cell_volume                     623.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0127
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3471
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0273
_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)+(0.0453P)²+0.2840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                2143
_reflns_number_total             2305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2624.cff
_cod_data_source_block           wf0886
_cod_original_cell_volume        623.4(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8102448
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.5000 0.01716(12) Uani 1 2 d S . .
Na1 Na 0.25919(13) 0.53018(10) 0.90125(9) 0.0339(2) Uani 1 1 d . . .
O9 O -0.2843(2) 1.06459(16) 1.04349(16) 0.0311(3) Uani 1 1 d . . .
O3 O 0.7041(2) -0.04644(16) 0.76356(15) 0.0317(3) Uani 1 1 d . . .
O8 O 0.1067(2) 0.67474(16) 1.43179(15) 0.0290(3) Uani 1 1 d . . .
O4 O 0.4113(2) 0.41017(17) 0.75972(16) 0.0318(3) Uani 1 1 d . . .
N3 N 0.5110(2) 0.14377(18) 0.56727(17) 0.0212(3) Uani 1 1 d . . .
O7 O 0.0174(2) 0.61214(17) 1.04366(16) 0.0327(4) Uani 1 1 d . . .
N6 N -0.0914(2) 0.87669(18) 1.24220(17) 0.0230(4) Uani 1 1 d . . .
N2 N 0.5610(3) 0.18105(18) 0.76417(17) 0.0233(4) Uani 1 1 d . . .
H2A H 0.6140 0.1448 0.8492 0.028 Uiso 1 1 calc R . .
N1 N 0.3676(3) 0.37931(18) 0.56479(17) 0.0233(4) Uani 1 1 d . . .
H1A H 0.2968 0.4726 0.5194 0.028 Uiso 1 1 calc R . .
O6W O 0.5020(3) 0.3313(2) 1.1026(2) 0.0414(4) Uani 1 1 d . . .
C3 C 0.4450(3) 0.3288(2) 0.7006(2) 0.0220(4) Uani 1 1 d . . .
O5W O 0.0737(3) 0.7453(2) 0.6787(2) 0.0388(4) Uani 1 1 d . . .
N5 N -0.1343(3) 0.83907(19) 1.04290(17) 0.0247(4) Uani 1 1 d . . .
H5A H -0.1905 0.8753 0.9588 0.030 Uiso 1 1 calc R . .
C6 C -0.0130(3) 0.6938(2) 1.1031(2) 0.0241(4) Uani 1 1 d . . .
C5 C 0.0297(3) 0.7324(2) 1.3085(2) 0.0214(4) Uani 1 1 d . . .
N4 N 0.0695(3) 0.64439(19) 1.23638(18) 0.0260(4) Uani 1 1 d . . .
H4A H 0.1508 0.5537 1.2781 0.031 Uiso 1 1 calc R . .
C4 C -0.1730(3) 0.9325(2) 1.1090(2) 0.0221(4) Uani 1 1 d . . .
C2 C 0.3966(3) 0.2892(2) 0.4968(2) 0.0215(4) Uani 1 1 d . . .
C1 C 0.5983(3) 0.0866(2) 0.7002(2) 0.0222(4) Uani 1 1 d . . .
O2 O 0.3166(2) 0.34074(16) 0.37560(15) 0.0301(3) Uani 1 1 d . . .
O1W O 0.2451(3) -0.0215(2) 0.60016(19) 0.0426(4) Uani 1 1 d . . .
H1WA H 0.2265 -0.0997 0.6111 0.064 Uiso 1 1 calc R . .
H5WA H 0.061(5) 0.728(4) 0.612(4) 0.077(12) Uiso 1 1 d . . .
H6WA H 0.551(6) 0.239(5) 1.101(4) 0.089(12) Uiso 1 1 d . . .
H5WB H -0.046(6) 0.793(4) 0.692(4) 0.085(13) Uiso 1 1 d . . .
H6WB H 0.453(6) 0.316(4) 1.176(4) 0.091(14) Uiso 1 1 d . . .
H1WB H 0.190(5) 0.029(4) 0.653(3) 0.060(9) Uiso 1 1 d . . .
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'
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'
Na Na 0.0362 0.0249 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1W Ni1 O1W 180.00(5) 2_656 . ?
O1W Ni1 N3 89.72(7) 2_656 . ?
O1W Ni1 N3 90.28(7) . . ?
O1W Ni1 N3 90.28(7) 2_656 2_656 ?
O1W Ni1 N3 89.72(7) . 2_656 ?
N3 Ni1 N3 180.0 . 2_656 ?
O4 Na1 O7 159.65(7) . . ?
O4 Na1 O6W 89.62(7) . . ?
O7 Na1 O6W 95.30(7) . . ?
O4 Na1 O6W 105.01(7) . 2_667 ?
O7 Na1 O6W 95.30(7) . 2_667 ?
O6W Na1 O6W 80.08(7) . 2_667 ?
O4 Na1 O5W 86.97(7) . . ?
O7 Na1 O5W 91.42(7) . . ?
O6W Na1 O5W 169.22(7) . . ?
O6W Na1 O5W 90.92(7) 2_667 . ?
O4 Na1 O7 86.34(6) . 2_567 ?
O7 Na1 O7 73.55(6) . 2_567 ?
O6W Na1 O7 95.56(7) . 2_567 ?
O6W Na1 O7 167.71(7) 2_667 2_567 ?
O5W Na1 O7 94.43(7) . 2_567 ?
O4 Na1 Na1 99.49(6) . 2_667 ?
O7 Na1 Na1 96.93(5) . 2_667 ?
O6W Na1 Na1 40.07(5) . 2_667 ?
O6W Na1 Na1 40.01(5) 2_667 2_667 ?
O5W Na1 Na1 130.67(7) . 2_667 ?
O7 Na1 Na1 134.57(6) 2_567 2_667 ?
O4 Na1 Na1 120.63(6) . 2_567 ?
O7 Na1 Na1 39.20(4) . 2_567 ?
O6W Na1 Na1 96.79(7) . 2_567 ?
O6W Na1 Na1 134.29(6) 2_667 2_567 ?
O5W Na1 Na1 93.75(6) . 2_567 ?
O7 Na1 Na1 34.34(4) 2_567 2_567 ?
Na1 Na1 Na1 122.24(5) 2_667 2_567 ?
C3 O4 Na1 161.22(14) . . ?
C2 N3 C1 121.81(16) . . ?
C2 N3 Ni1 119.55(13) . . ?
C1 N3 Ni1 117.12(13) . . ?
C6 O7 Na1 140.07(14) . . ?
C6 O7 Na1 113.38(13) . 2_567 ?
Na1 O7 Na1 106.45(6) . 2_567 ?
C4 N6 C5 120.11(16) . . ?
C3 N2 C1 123.81(16) . . ?
C3 N2 H2A 118.1 . . ?
C1 N2 H2A 118.1 . . ?
C3 N1 C2 123.68(17) . . ?
C3 N1 H1A 118.2 . . ?
C2 N1 H1A 118.2 . . ?
Na1 O6W Na1 99.92(7) . 2_667 ?
Na1 O6W H6WA 115(2) . . ?
Na1 O6W H6WA 121(2) 2_667 . ?
Na1 O6W H6WB 112(3) . . ?
Na1 O6W H6WB 102(3) 2_667 . ?
H6WA O6W H6WB 106(4) . . ?
O4 C3 N2 122.88(18) . . ?
O4 C3 N1 122.20(18) . . ?
N2 C3 N1 114.92(16) . . ?
Na1 O5W H5WA 117(3) . . ?
Na1 O5W H5WB 114(3) . . ?
H5WA O5W H5WB 107(3) . . ?
C6 N5 C4 123.73(17) . . ?
C6 N5 H5A 118.1 . . ?
C4 N5 H5A 118.1 . . ?
O7 C6 N5 122.81(18) . . ?
O7 C6 N4 122.48(19) . . ?
N5 C6 N4 114.70(17) . . ?
O8 C5 N6 122.78(17) . . ?
O8 C5 N4 118.37(17) . . ?
N6 C5 N4 118.85(17) . . ?
C6 N4 C5 123.53(17) . . ?
C6 N4 H4A 118.2 . . ?
C5 N4 H4A 118.2 . . ?
O9 C4 N6 122.41(18) . . ?
O9 C4 N5 118.54(17) . . ?
N6 C4 N5 119.04(17) . . ?
O2 C2 N3 121.53(17) . . ?
O2 C2 N1 120.50(18) . . ?
N3 C2 N1 117.97(17) . . ?
O3 C1 N3 121.45(17) . . ?
O3 C1 N2 120.78(17) . . ?
N3 C1 N2 117.75(17) . . ?
Ni1 O1W H1WA 109.5 . . ?
Ni1 O1W H1WB 121.0(19) . . ?
H1WA O1W H1WB 125.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1W 1.9359(16) 2_656 ?
Ni1 O1W 1.9359(16) . ?
Ni1 N3 1.9493(16) . ?
Ni1 N3 1.9493(16) 2_656 ?
Na1 O4 2.3183(17) . ?
Na1 O7 2.3194(18) . ?
Na1 O6W 2.465(2) . ?
Na1 O6W 2.468(2) 2_667 ?
Na1 O5W 2.478(2) . ?
Na1 O7 2.5987(19) 2_567 ?
Na1 Na1 3.777(2) 2_667 ?
Na1 Na1 3.943(2) 2_567 ?
O9 C4 1.241(3) . ?
O3 C1 1.234(2) . ?
O8 C5 1.240(2) . ?
O4 C3 1.218(2) . ?
N3 C2 1.348(3) . ?
N3 C1 1.355(3) . ?
O7 C6 1.225(2) . ?
O7 Na1 2.5987(19) 2_567 ?
N6 C4 1.345(3) . ?
N6 C5 1.350(3) . ?
N2 C3 1.364(3) . ?
N2 C1 1.377(2) . ?
N2 H2A 0.8600 . ?
N1 C3 1.369(3) . ?
N1 C2 1.376(2) . ?
N1 H1A 0.8600 . ?
O6W Na1 2.468(2) 2_667 ?
O6W H6WA 0.92(4) . ?
O6W H6WB 0.77(4) . ?
O5W H5WA 0.81(4) . ?
O5W H5WB 0.85(4) . ?
N5 C6 1.355(3) . ?
N5 C4 1.384(2) . ?
N5 H5A 0.8600 . ?
C6 N4 1.361(3) . ?
C5 N4 1.386(2) . ?
N4 H4A 0.8600 . ?
C2 O2 1.239(2) . ?
O1W H1WA 0.8200 . ?
O1W H1WB 0.91(3) . ?
