#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:57:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179163 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/24/4312418.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_4312418
loop_
_publ_author_name
'Wenbin Yang'
'Canzhong Lu'
'Quanzheng Zhang'
'Shumei Chen'
'Xiaoping Zhan'
'Jiuhui Liu'
_publ_contact_author_address
;
     Fujian Institute of Research  
        on the Structure of Matter,
        Chinese Academy of Sciences,
        Fuzhou, Fujian 350002, 
    P.R.China
;
_publ_contact_author_email       czlu@ms.fjirsm.ac.cn
_publ_contact_author_fax         0086-0591-3714946
_publ_contact_author_name        'Dr. Canzhong Lu'
_publ_contact_author_phone       0086-0591-3705794
_publ_section_title
;
 Structure and Properties of a Novel 3D Straight-Channel Polyoxovanadate
 and an Unexpected Trimeric Barbiturate Obtained by Hydrothermal Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7309
_journal_page_last               7314
_journal_paper_doi               10.1021/ic034554p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C12 H20 N6 Na2 O16'
_chemical_formula_weight         550.32
_chemical_name_systematic
; 
 ? 
;
_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                106.028(2)
_cell_angle_beta                 103.547(2)
_cell_angle_gamma                93.244(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0888(5)
_cell_length_b                   10.5501(7)
_cell_length_c                   13.2798(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1049.95(12)
_computing_cell_refinement       'Simens CCD SAINT'
_computing_data_collection       'Simens SMART CCD'
_computing_data_reduction        'Simens CCD SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Siemens CCD SMART'
_diffrn_measurement_method       omega-scan
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5424
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.861968
_exptl_absorpt_correction_T_min  0.484943
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         3639
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0714
_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)+(0.1318P)²+0.5435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.2205
_reflns_number_gt                2310
_reflns_number_total             3639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034554psi20030523_062536.cif
_cod_data_source_block           C12
_cod_database_code               4312418
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
Na1 Na 0.7407(3) -0.15406(19) 0.65752(15) 0.0389(5) Uani 1 1 d . . .
Na2 Na 0.7483(4) -0.4655(3) 0.5291(2) 0.0897(11) Uani 1 1 d . . .
O1 O 0.8101(4) -0.0104(3) 0.8346(2) 0.0306(8) Uani 1 1 d . . .
O2 O 0.9919(5) 0.3087(4) 1.1533(3) 0.0422(9) Uani 1 1 d . . .
O3 O 1.1227(5) 0.4032(3) 0.8695(3) 0.0377(9) Uani 1 1 d . . .
O4 O 1.1868(4) 0.0454(3) 0.9256(2) 0.0286(8) Uani 1 1 d . . .
O5 O 1.4467(4) -0.0883(3) 0.6526(2) 0.0328(8) Uani 1 1 d D . .
O6 O 1.0689(4) 0.2115(3) 0.6252(3) 0.0339(8) Uani 1 1 d . . .
O7 O 0.7753(4) 0.0184(3) 0.5926(2) 0.0267(7) Uani 1 1 d . . .
O8 O 0.4280(5) 0.3247(4) 0.5303(3) 0.0538(11) Uani 1 1 d D . .
O9 O 0.7495(4) 0.3959(3) 0.8771(2) 0.0304(8) Uani 1 1 d . . .
O11 O 0.6778(6) -0.3388(5) 0.7146(4) 0.0622(12) Uani 1 1 d D . .
H11A H 0.609(9) -0.298(7) 0.766(5) 0.08(2) Uiso 1 1 d D . .
H11B H 0.792(8) -0.342(7) 0.769(5) 0.09(2) Uiso 1 1 d D . .
O12 O 0.9451(6) -0.2633(4) 0.5748(3) 0.0530(11) Uani 1 1 d D . .
H12A H 0.945(12) -0.247(9) 0.505(5) 0.12(3) Uiso 1 1 d D . .
H12B H 1.063(7) -0.282(9) 0.593(7) 0.11(3) Uiso 1 1 d D . .
O13 O 0.9486(6) -0.5406(4) 0.6465(3) 0.0579(12) Uani 1 1 d D . .
H13A H 0.986(9) -0.491(7) 0.727(4) 0.08(2) Uiso 1 1 d D . .
H13B H 0.984(10) -0.626(6) 0.646(6) 0.10(3) Uiso 1 1 d D . .
O14 O 0.7260(6) -0.6485(5) 0.3769(4) 0.0571(11) Uani 1 1 d D . .
H14A H 0.718(11) -0.626(8) 0.307(5) 0.10(3) Uiso 1 1 d D . .
H14B H 0.611(10) -0.703(11) 0.346(10) 0.20(6) Uiso 1 1 d D . .
O15 O 1.5404(5) -0.1757(4) 0.8886(4) 0.0549(11) Uani 1 1 d D . .
H15A H 1.515(12) -0.197(9) 0.946(6) 0.12(3) Uiso 1 1 d D . .
H15B H 1.53(3) -0.088(12) 0.865(15) 0.33(10) Uiso 1 1 d D . .
O16 O 1.3547(6) 0.5282(5) 0.7897(4) 0.0578(12) Uani 1 1 d D . .
H16A H 1.246(10) 0.459(9) 0.777(9) 0.15(4) Uiso 1 1 d D . .
H16B H 1.366(19) 0.578(13) 0.875(6) 0.23(6) Uiso 1 1 d D . .
O17 O 0.5104(7) 0.3419(6) 0.9830(4) 0.0724(15) Uani 1 1 d D . .
H17A H 0.590(8) 0.368(7) 0.948(5) 0.08(2) Uiso 1 1 d D . .
C1 C 0.9553(5) 0.1898(4) 0.8236(3) 0.0211(9) Uani 1 1 d . . .
C2 C 0.8819(6) 0.1029(4) 0.8820(3) 0.0242(10) Uani 1 1 d . . .
C3 C 0.9823(6) 0.2740(5) 1.0560(3) 0.0276(11) Uani 1 1 d . . .
C4 C 1.0526(6) 0.3233(4) 0.9018(4) 0.0242(10) Uani 1 1 d . . .
C5 C 1.0905(6) 0.1206(4) 0.7732(3) 0.0250(10) Uani 1 1 d . . .
C6 C 1.1956(6) 0.0505(4) 0.8336(3) 0.0233(10) Uani 1 1 d . . .
C7 C 1.3383(5) -0.0152(4) 0.6935(3) 0.0263(10) Uani 1 1 d D . .
C8 C 1.1292(6) 0.1370(5) 0.6788(3) 0.0260(10) Uani 1 1 d . . .
C9 C 0.8011(6) 0.2146(4) 0.7428(3) 0.0222(10) Uani 1 1 d . . .
C10 C 0.7350(6) 0.1288(4) 0.6353(3) 0.0232(10) Uani 1 1 d . . .
C11 C 0.5394(6) 0.2861(5) 0.6016(3) 0.0334(12) Uani 1 1 d D . .
C12 C 0.7159(6) 0.3224(4) 0.7795(4) 0.0263(10) Uani 1 1 d . . .
N1 N 0.8827(5) 0.1585(4) 0.9888(3) 0.0268(9) Uani 1 1 d D . .
N2 N 1.0713(5) 0.3459(4) 1.0104(3) 0.0280(9) Uani 1 1 d D . .
N3 N 1.3183(5) -0.0152(4) 0.7898(3) 0.0294(9) Uani 1 1 d . . .
N4 N 1.2485(5) 0.0576(4) 0.6395(3) 0.0269(9) Uani 1 1 d D . .
N5 N 0.6086(5) 0.1759(4) 0.5680(3) 0.0308(9) Uani 1 1 d . . .
N6 N 0.5824(5) 0.3524(4) 0.7059(3) 0.0302(9) Uani 1 1 d D . .
H1 H 0.848(6) 0.098(4) 1.026(4) 0.038(14) Uiso 1 1 d D . .
H4 H 1.250(7) 0.045(5) 0.565(2) 0.047(15) Uiso 1 1 d D . .
H2 H 1.125(8) 0.434(3) 1.057(4) 0.07(2) Uiso 1 1 d D . .
H6 H 0.516(7) 0.421(5) 0.734(5) 0.060(18) Uiso 1 1 d D . .
H17B H 0.383(10) 0.356(17) 0.971(16) 0.32(10) Uiso 1 1 d 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'
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
O7 Na1 O1 90.60(12) . . ?
O7 Na1 O11 174.56(17) . . ?
O1 Na1 O11 92.32(16) . . ?
O7 Na1 O12 91.67(14) . . ?
O1 Na1 O12 123.54(16) . . ?
O11 Na1 O12 90.54(17) . . ?
O7 Na1 O5 83.80(12) . 1_455 ?
O1 Na1 O5 83.72(12) . 1_455 ?
O11 Na1 O5 91.95(16) . 1_455 ?
O12 Na1 O5 152.51(16) . 1_455 ?
O7 Na1 O8 96.05(13) . 2_656 ?
O1 Na1 O8 162.81(15) . 2_656 ?
O11 Na1 O8 79.89(16) . 2_656 ?
O12 Na1 O8 72.23(15) . 2_656 ?
O5 Na1 O8 81.27(12) 1_455 2_656 ?
O7 Na1 C10 20.25(10) . . ?
O1 Na1 C10 74.18(12) . . ?
O11 Na1 C10 158.81(17) . . ?
O12 Na1 C10 110.48(15) . . ?
O5 Na1 C10 70.73(12) 1_455 . ?
O8 Na1 C10 108.34(12) 2_656 . ?
O7 Na1 Na2 125.30(12) . . ?
O1 Na1 Na2 139.63(12) . . ?
O11 Na1 Na2 53.68(15) . . ?
O12 Na1 Na2 47.83(14) . . ?
O5 Na1 Na2 114.85(12) 1_455 . ?
O8 Na1 Na2 43.92(8) 2_656 . ?
C10 Na1 Na2 144.52(11) . . ?
O8 Na2 O13 158.6(2) 2_656 . ?
O8 Na2 O14 105.79(18) 2_656 . ?
O13 Na2 O14 95.56(18) . . ?
O8 Na2 O12 77.82(17) 2_656 . ?
O13 Na2 O12 88.85(18) . . ?
O14 Na2 O12 123.6(2) . . ?
O8 Na2 O11 80.46(16) 2_656 . ?
O13 Na2 O11 81.15(17) . . ?
O14 Na2 O11 154.1(2) . . ?
O12 Na2 O11 82.22(16) . . ?
O8 Na2 Na1 53.27(11) 2_656 . ?
O13 Na2 Na1 105.49(14) . . ?
O14 Na2 Na1 155.57(16) . . ?
O12 Na2 Na1 46.40(11) . . ?
O11 Na2 Na1 45.21(11) . . ?
O8 Na2 Na2 58.17(14) 2_656 2_646 ?
O13 Na2 Na2 126.5(2) . 2_646 ?
O14 Na2 Na2 86.89(15) . 2_646 ?
O12 Na2 Na2 132.81(15) . 2_646 ?
O11 Na2 Na2 74.99(16) . 2_646 ?
Na1 Na2 Na2 90.36(11) . 2_646 ?
C2 O1 Na1 136.9(3) . . ?
C4 O3 H16A 156(3) . . ?
C4 O3 O16 162.2(3) . . ?
H16A O3 O16 15(3) . . ?
C7 O5 Na1 152.5(3) . 1_655 ?
C10 O7 Na1 121.1(3) . . ?
C11 O8 Na2 155.7(3) . 2_656 ?
C11 O8 Na1 120.8(3) . 2_656 ?
Na2 O8 Na1 82.81(13) 2_656 2_656 ?
C12 O9 H17A 114(2) . . ?
C12 O9 O17 112.6(3) . . ?
H17A O9 O17 2(2) . . ?
Na1 O11 Na2 81.11(16) . . ?
Na1 O11 O2 92.38(17) . 2_757 ?
Na2 O11 O2 96.67(18) . 2_757 ?
Na1 O11 O15 92.04(18) . 1_455 ?
Na2 O11 O15 167.2(2) . 1_455 ?
O2 O11 O15 94.43(18) 2_757 1_455 ?
Na1 O11 H11A 99(4) . . ?
Na2 O11 H11A 159(4) . . ?
O2 O11 H11A 104(4) 2_757 . ?
O15 O11 H11A 12(4) 1_455 . ?
Na1 O11 H11B 104(4) . . ?
Na2 O11 H11B 100(4) . . ?
O2 O11 H11B 11(4) 2_757 . ?
O15 O11 H11B 92(4) 1_455 . ?
H11A O11 H11B 100(6) . . ?
Na1 O12 Na2 85.77(17) . . ?
Na1 O12 O6 110.56(16) . 2_756 ?
Na2 O12 O6 105.29(19) . 2_756 ?
Na1 O12 O14 142.6(2) . 2_746 ?
Na2 O12 O14 103.01(18) . 2_746 ?
O6 O12 O14 102.16(16) 2_756 2_746 ?
Na1 O12 H12A 113(5) . . ?
Na2 O12 H12A 105(6) . . ?
O6 O12 H12A 3(5) 2_756 . ?
O14 O12 H12A 100(5) 2_746 . ?
Na1 O12 H12B 141(5) . . ?
Na2 O12 H12B 110(5) . . ?
O6 O12 H12B 99(5) 2_756 . ?
O14 O12 H12B 7(5) 2_746 . ?
H12A O12 H12B 97(6) . . ?
Na2 O13 O6 131.7(2) . 1_545 ?
Na2 O13 O2 99.39(17) . 2_757 ?
O6 O13 O2 128.33(17) 1_545 2_757 ?
Na2 O13 H13A 121(4) . . ?
O6 O13 H13A 106(4) 1_545 . ?
O2 O13 H13A 23(4) 2_757 . ?
Na2 O13 H13B 134(5) . . ?
O6 O13 H13B 7(5) 1_545 . ?
O2 O13 H13B 124(5) 2_757 . ?
H13A O13 H13B 102(6) . . ?
Na2 O14 O16 100.57(19) . 2_756 ?
Na2 O14 H14A 115(5) . . ?
O16 O14 H14A 17(4) 2_756 . ?
Na2 O14 H14B 116(8) . . ?
O16 O14 H14B 88(7) 2_756 . ?
H14A O14 H14B 91(8) . . ?
O17 O15 O4 82.56(17) 2_757 2_857 ?
O17 O15 H15A 23(6) 2_757 . ?
O4 O15 H15A 73(6) 2_857 . ?
O17 O15 H15B 153(10) 2_757 . ?
O4 O15 H15B 93(10) 2_857 . ?
H15A O15 H15B 130(10) . . ?
O3 O16 H16A 29(6) . . ?
O3 O16 H16B 68(8) . . ?
H16A O16 H16B 96(9) . . ?
O9 O17 H17A 5(4) . . ?
O9 O17 H17B 130(10) . . ?
H17A O17 H17B 128(10) . . ?
C5 C1 C9 115.1(3) . . ?
C5 C1 C2 109.3(3) . . ?
C9 C1 C2 105.8(3) . . ?
C5 C1 C4 104.6(3) . . ?
C9 C1 C4 109.8(3) . . ?
C2 C1 C4 112.5(3) . . ?
O1 C2 N1 118.9(4) . . ?
O1 C2 C1 122.2(4) . . ?
N1 C2 C1 118.6(4) . . ?
O2 C3 N2 121.9(4) . . ?
O2 C3 N1 120.7(4) . . ?
N2 C3 N1 117.4(4) . . ?
O3 C4 N2 120.1(4) . . ?
O3 C4 C1 121.3(4) . . ?
N2 C4 C1 118.4(4) . . ?
C6 C5 C8 118.9(4) . . ?
C6 C5 C1 116.6(4) . . ?
C8 C5 C1 124.0(4) . . ?
O4 C6 N3 117.8(4) . . ?
O4 C6 C5 123.9(4) . . ?
N3 C6 C5 118.3(4) . . ?
O5 C7 N4 120.8(4) . . ?
O5 C7 N3 119.4(4) . . ?
N4 C7 N3 119.8(3) . . ?
O6 C8 N4 116.1(4) . . ?
O6 C8 C5 127.8(4) . . ?
N4 C8 C5 116.0(4) . . ?
C12 C9 C10 118.9(4) . . ?
C12 C9 C1 117.8(4) . . ?
C10 C9 C1 123.2(4) . . ?
O7 C10 N5 115.8(4) . . ?
O7 C10 C9 128.8(4) . . ?
N5 C10 C9 115.4(4) . . ?
O7 C10 Na1 38.7(2) . . ?
N5 C10 Na1 128.1(3) . . ?
C9 C10 Na1 104.8(3) . . ?
O8 C11 N6 121.9(4) . . ?
O8 C11 N5 119.1(4) . . ?
N6 C11 N5 119.0(3) . . ?
O9 C12 N6 116.5(4) . . ?
O9 C12 C9 124.6(4) . . ?
N6 C12 C9 118.9(4) . . ?
C3 N1 C2 124.5(4) . . ?
C3 N1 O4 119.3(3) . 2_757 ?
C2 N1 O4 108.4(3) . 2_757 ?
C3 N1 H1 115(3) . . ?
C2 N1 H1 117(3) . . ?
O4 N1 H1 10(3) 2_757 . ?
C3 N2 C4 125.6(4) . . ?
C3 N2 O9 123.4(3) . 2_767 ?
C4 N2 O9 108.9(3) . 2_767 ?
C3 N2 H2 116(4) . . ?
C4 N2 H2 116(4) . . ?
O9 N2 H2 8(4) 2_767 . ?
C7 N3 C6 122.3(3) . . ?
C7 N4 C8 123.3(3) . . ?
C7 N4 O7 115.3(2) . 2_756 ?
C8 N4 O7 118.6(3) . 2_756 ?
C7 N4 H4 119(3) . . ?
C8 N4 H4 117(3) . . ?
O7 N4 H4 8(3) 2_756 . ?
C11 N5 C10 124.3(4) . . ?
C11 N6 C12 122.1(4) . . ?
C11 N6 O16 118.6(3) . 1_455 ?
C12 N6 O16 118.3(3) . 1_455 ?
C11 N6 H6 120(4) . . ?
C12 N6 H6 118(4) . . ?
O16 N6 H6 7(4) 1_455 . ?
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
Na1 O7 2.247(3) . ?
Na1 O1 2.336(4) . ?
Na1 O11 2.348(5) . ?
Na1 O12 2.374(4) . ?
Na1 O5 2.506(3) 1_455 ?
Na1 O8 2.641(4) 2_656 ?
Na1 C10 3.080(5) . ?
Na1 Na2 3.269(3) . ?
Na2 O8 2.286(4) 2_656 ?
Na2 O13 2.308(5) . ?
Na2 O14 2.341(5) . ?
Na2 O12 2.429(6) . ?
Na2 O11 2.666(6) . ?
Na2 Na2 3.895(7) 2_646 ?
O1 C2 1.223(5) . ?
O2 C3 1.223(5) . ?
O3 C4 1.216(5) . ?
O3 H16A 1.93(8) . ?
O3 O16 2.793(5) . ?
O4 C6 1.257(5) . ?
O5 C7 1.314(2) . ?
O5 Na1 2.506(3) 1_655 ?
O6 C8 1.246(5) . ?
O7 C10 1.245(5) . ?
O8 C11 1.315(2) . ?
O8 Na2 2.286(4) 2_656 ?
O8 Na1 2.641(4) 2_656 ?
O9 C12 1.268(5) . ?
O9 H17A 1.82(5) . ?
O9 O17 2.763(5) . ?
O11 O2 2.778(6) 2_757 ?
O11 O15 2.959(7) 1_455 ?
O11 H11A 1.01(5) . ?
O11 H11B 1.04(5) . ?
O12 O6 2.834(5) 2_756 ?
O12 O14 2.858(6) 2_746 ?
O12 H12A 0.98(5) . ?
O12 H12B 0.97(5) . ?
O13 O6 2.806(5) 1_545 ?
O13 O2 2.993(5) 2_757 ?
O13 H13A 1.02(5) . ?
O13 H13B 0.96(5) . ?
O14 O16 2.811(6) 2_756 ?
O14 H14A 1.01(5) . ?
O14 H14B 1.00(6) . ?
O15 O17 2.837(6) 2_757 ?
O15 O4 2.842(5) 2_857 ?
O15 H15A 0.92(5) . ?
O15 H15B 1.06(6) . ?
O16 H16A 1.06(6) . ?
O16 H16B 1.09(6) . ?
O17 H17A 0.95(5) . ?
O17 H17B 1.03(6) . ?
C1 C5 1.530(6) . ?
C1 C9 1.530(6) . ?
C1 C2 1.530(6) . ?
C1 C4 1.538(6) . ?
C2 N1 1.375(5) . ?
C3 N2 1.364(6) . ?
C3 N1 1.372(6) . ?
C4 N2 1.364(6) . ?
C5 C6 1.412(6) . ?
C5 C8 1.414(6) . ?
C6 N3 1.388(6) . ?
C7 N4 1.325(5) . ?
C7 N3 1.326(5) . ?
C8 N4 1.411(6) . ?
C9 C12 1.395(6) . ?
C9 C10 1.421(6) . ?
C10 N5 1.402(6) . ?
C11 N6 1.319(6) . ?
C11 N5 1.330(6) . ?
C12 N6 1.391(6) . ?
N1 O4 2.783(5) 2_757 ?
N1 H1 0.98(2) . ?
N2 O9 2.837(5) 2_767 ?
N2 H2 0.97(2) . ?
N4 O7 2.919(4) 2_756 ?
N4 H4 0.97(2) . ?
N6 O16 2.877(5) 1_455 ?
N6 H6 0.97(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O16 H16A O3 1.06(6) 1.93(8) 2.793(5) 136(8) .
O17 H17A O9 0.95(5) 1.82(5) 2.763(5) 173(6) .
N6 H6 O16 0.97(2) 1.92(2) 2.877(5) 169(5) 1_455
O11 H11A O15 1.01(5) 1.99(5) 2.959(7) 162(6) 1_455
O13 H13B O6 0.96(5) 1.86(5) 2.806(5) 170(7) 1_545
O12 H12B O14 0.97(5) 1.90(5) 2.858(6) 169(8) 2_746
N4 H4 O7 0.97(2) 1.96(2) 2.919(4) 167(5) 2_756
O12 H12A O6 0.98(5) 1.85(5) 2.834(5) 176(8) 2_756
N1 H1 O4 0.98(2) 1.82(2) 2.783(5) 165(4) 2_757
O11 H11B O2 1.04(5) 1.77(6) 2.778(6) 162(6) 2_757
O13 H13A O2 1.02(5) 2.09(6) 2.993(5) 146(6) 2_757
O15 H15A O17 0.92(5) 2.03(7) 2.837(6) 146(8) 2_757
N2 H2 O9 0.97(2) 1.88(2) 2.837(5) 168(6) 2_767
O15 H15A O4 0.92(5) 2.72(10) 2.842(5) 88(6) 2_857
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 Na1 Na2 O8 -56.7(2) . . . 2_656 ?
O1 Na1 Na2 O8 154.8(2) . . . 2_656 ?
O11 Na1 Na2 O8 116.7(2) . . . 2_656 ?
O12 Na1 Na2 O8 -110.3(2) . . . 2_656 ?
O5 Na1 Na2 O8 43.79(19) 1_455 . . 2_656 ?
C10 Na1 Na2 O8 -47.5(3) . . . 2_656 ?
O7 Na1 Na2 O13 126.6(2) . . . . ?
O1 Na1 Na2 O13 -21.9(3) . . . . ?
O11 Na1 Na2 O13 -60.0(2) . . . . ?
O12 Na1 Na2 O13 73.0(2) . . . . ?
O5 Na1 Na2 O13 -132.92(19) 1_455 . . . ?
O8 Na1 Na2 O13 -176.7(3) 2_656 . . . ?
C10 Na1 Na2 O13 135.8(2) . . . . ?
O7 Na1 Na2 O14 -21.9(5) . . . . ?
O1 Na1 Na2 O14 -170.4(4) . . . . ?
O11 Na1 Na2 O14 151.5(5) . . . . ?
O12 Na1 Na2 O14 -75.5(5) . . . . ?
O5 Na1 Na2 O14 78.6(5) 1_455 . . . ?
O8 Na1 Na2 O14 34.8(4) 2_656 . . . ?
C10 Na1 Na2 O14 -12.8(6) . . . . ?
O7 Na1 Na2 O12 53.61(19) . . . . ?
O1 Na1 Na2 O12 -94.9(2) . . . . ?
O11 Na1 Na2 O12 -133.0(2) . . . . ?
O5 Na1 Na2 O12 154.10(18) 1_455 . . . ?
O8 Na1 Na2 O12 110.3(2) 2_656 . . . ?
C10 Na1 Na2 O12 62.8(2) . . . . ?
O7 Na1 Na2 O11 -173.4(2) . . . . ?
O1 Na1 Na2 O11 38.1(2) . . . . ?
O12 Na1 Na2 O11 133.0(2) . . . . ?
O5 Na1 Na2 O11 -72.92(18) 1_455 . . . ?
O8 Na1 Na2 O11 -116.7(2) 2_656 . . . ?
C10 Na1 Na2 O11 -164.2(3) . . . . ?
O7 Na1 Na2 Na2 -105.19(17) . . . 2_646 ?
O1 Na1 Na2 Na2 106.30(19) . . . 2_646 ?
O11 Na1 Na2 Na2 68.22(18) . . . 2_646 ?
O12 Na1 Na2 Na2 -158.80(19) . . . 2_646 ?
O5 Na1 Na2 Na2 -4.70(16) 1_455 . . 2_646 ?
O8 Na1 Na2 Na2 -48.49(15) 2_656 . . 2_646 ?
C10 Na1 Na2 Na2 -96.0(2) . . . 2_646 ?
O7 Na1 O1 C2 -18.5(4) . . . . ?
O11 Na1 O1 C2 166.1(4) . . . . ?
O12 Na1 O1 C2 73.9(5) . . . . ?
O5 Na1 O1 C2 -102.2(4) 1_455 . . . ?
O8 Na1 O1 C2 -131.5(5) 2_656 . . . ?
C10 Na1 O1 C2 -30.5(4) . . . . ?
Na2 Na1 O1 C2 136.3(4) . . . . ?
O1 Na1 O7 C10 -35.3(3) . . . . ?
O11 Na1 O7 C10 87.2(18) . . . . ?
O12 Na1 O7 C10 -158.9(3) . . . . ?
O5 Na1 O7 C10 48.3(3) 1_455 . . . ?
O8 Na1 O7 C10 128.8(3) 2_656 . . . ?
Na2 Na1 O7 C10 164.5(3) . . . . ?
O7 Na1 O11 Na2 81.1(18) . . . . ?
O1 Na1 O11 Na2 -156.43(15) . . . . ?
O12 Na1 O11 Na2 -32.83(16) . . . . ?
O5 Na1 O11 Na2 119.78(14) 1_455 . . . ?
O8 Na1 O11 Na2 39.01(13) 2_656 . . . ?
C10 Na1 O11 Na2 154.1(4) . . . . ?
O7 Na1 O11 O2 177.5(17) . . . 2_757 ?
O1 Na1 O11 O2 -60.05(16) . . . 2_757 ?
O12 Na1 O11 O2 63.55(18) . . . 2_757 ?
O5 Na1 O11 O2 -143.84(15) 1_455 . . 2_757 ?
O8 Na1 O11 O2 135.39(17) 2_656 . . 2_757 ?
C10 Na1 O11 O2 -109.5(4) . . . 2_757 ?
Na2 Na1 O11 O2 96.38(18) . . . 2_757 ?
O7 Na1 O11 O15 -88.0(18) . . . 1_455 ?
O1 Na1 O11 O15 34.48(16) . . . 1_455 ?
O12 Na1 O11 O15 158.07(17) . . . 1_455 ?
O5 Na1 O11 O15 -49.31(15) 1_455 . . 1_455 ?
O8 Na1 O11 O15 -130.09(16) 2_656 . . 1_455 ?
C10 Na1 O11 O15 -15.0(5) . . . 1_455 ?
Na2 Na1 O11 O15 -169.1(2) . . . 1_455 ?
O8 Na2 O11 Na1 -46.55(17) 2_656 . . . ?
O13 Na2 O11 Na1 122.37(18) . . . . ?
O14 Na2 O11 Na1 -153.1(4) . . . . ?
O12 Na2 O11 Na1 32.33(15) . . . . ?
Na2 Na2 O11 Na1 -105.98(14) 2_646 . . . ?
O8 Na2 O11 O2 -137.93(19) 2_656 . . 2_757 ?
O13 Na2 O11 O2 30.99(18) . . . 2_757 ?
O14 Na2 O11 O2 115.5(4) . . . 2_757 ?
O12 Na2 O11 O2 -59.05(16) . . . 2_757 ?
Na1 Na2 O11 O2 -91.38(17) . . . 2_757 ?
Na2 Na2 O11 O2 162.65(15) 2_646 . . 2_757 ?
O8 Na2 O11 O15 11.8(10) 2_656 . . 1_455 ?
O13 Na2 O11 O15 -179.3(10) . . . 1_455 ?
O14 Na2 O11 O15 -94.8(10) . . . 1_455 ?
O12 Na2 O11 O15 90.7(10) . . . 1_455 ?
Na1 Na2 O11 O15 58.4(9) . . . 1_455 ?
Na2 Na2 O11 O15 -47.6(10) 2_646 . . 1_455 ?
O7 Na1 O12 Na2 -138.91(14) . . . . ?
O1 Na1 O12 Na2 129.26(16) . . . . ?
O11 Na1 O12 Na2 36.12(17) . . . . ?
O5 Na1 O12 Na2 -59.2(4) 1_455 . . . ?
O8 Na1 O12 Na2 -43.09(13) 2_656 . . . ?
C10 Na1 O12 Na2 -146.56(14) . . . . ?
O7 Na1 O12 O6 -34.2(2) . . . 2_756 ?
O1 Na1 O12 O6 -125.98(18) . . . 2_756 ?
O11 Na1 O12 O6 140.9(2) . . . 2_756 ?
O5 Na1 O12 O6 45.6(4) 1_455 . . 2_756 ?
O8 Na1 O12 O6 61.67(18) 2_656 . . 2_756 ?
C10 Na1 O12 O6 -41.8(2) . . . 2_756 ?
Na2 Na1 O12 O6 104.8(2) . . . 2_756 ?
O7 Na1 O12 O14 115.2(3) . . . 2_746 ?
O1 Na1 O12 O14 23.3(4) . . . 2_746 ?
O11 Na1 O12 O14 -69.8(4) . . . 2_746 ?
O5 Na1 O12 O14 -165.1(3) 1_455 . . 2_746 ?
O8 Na1 O12 O14 -149.0(4) 2_656 . . 2_746 ?
C10 Na1 O12 O14 107.5(3) . . . 2_746 ?
Na2 Na1 O12 O14 -105.9(4) . . . 2_746 ?
O8 Na2 O12 Na1 50.26(15) 2_656 . . . ?
O13 Na2 O12 Na1 -112.83(18) . . . . ?
O14 Na2 O12 Na1 151.27(18) . . . . ?
O11 Na2 O12 Na1 -31.60(14) . . . . ?
Na2 Na2 O12 Na1 29.5(3) 2_646 . . . ?
O8 Na2 O12 O6 -59.91(17) 2_656 . . 2_756 ?
O13 Na2 O12 O6 137.00(19) . . . 2_756 ?
O14 Na2 O12 O6 41.1(2) . . . 2_756 ?
O11 Na2 O12 O6 -141.78(16) . . . 2_756 ?
Na1 Na2 O12 O6 -110.17(18) . . . 2_756 ?
Na2 Na2 O12 O6 -80.6(3) 2_646 . . 2_756 ?
O8 Na2 O12 O14 -166.61(19) 2_656 . . 2_746 ?
O13 Na2 O12 O14 30.3(2) . . . 2_746 ?
O14 Na2 O12 O14 -65.6(3) . . . 2_746 ?
O11 Na2 O12 O14 111.53(18) . . . 2_746 ?
Na1 Na2 O12 O14 143.1(2) . . . 2_746 ?
Na2 Na2 O12 O14 172.7(2) 2_646 . . 2_746 ?
O8 Na2 O13 O6 173.9(5) 2_656 . . 1_545 ?
O14 Na2 O13 O6 -11.4(3) . . . 1_545 ?
O12 Na2 O13 O6 -135.0(3) . . . 1_545 ?
O11 Na2 O13 O6 142.6(3) . . . 1_545 ?
Na1 Na2 O13 O6 -178.9(2) . . . 1_545 ?
Na2 Na2 O13 O6 78.8(4) 2_646 . . 1_545 ?
O8 Na2 O13 O2 2.5(8) 2_656 . . 2_757 ?
O14 Na2 O13 O2 177.18(19) . . . 2_757 ?
O12 Na2 O13 O2 53.55(19) . . . 2_757 ?
O11 Na2 O13 O2 -28.76(18) . . . 2_757 ?
Na1 Na2 O13 O2 9.7(2) . . . 2_757 ?
Na2 Na2 O13 O2 -92.6(2) 2_646 . . 2_757 ?
O8 Na2 O14 O16 28.0(3) 2_656 . . 2_756 ?
O13 Na2 O14 O16 -150.0(2) . . . 2_756 ?
O12 Na2 O14 O16 -57.7(2) . . . 2_756 ?
O11 Na2 O14 O16 128.8(4) . . . 2_756 ?
Na1 Na2 O14 O16 -0.3(5) . . . 2_756 ?
Na2 Na2 O14 O16 83.66(17) 2_646 . . 2_756 ?
Na1 O1 C2 N1 173.6(3) . . . . ?
Na1 O1 C2 C1 -0.3(7) . . . . ?
C5 C1 C2 O1 -59.4(5) . . . . ?
C9 C1 C2 O1 65.0(5) . . . . ?
C4 C1 C2 O1 -175.1(4) . . . . ?
C5 C1 C2 N1 126.7(4) . . . . ?
C9 C1 C2 N1 -108.8(4) . . . . ?
C4 C1 C2 N1 11.0(5) . . . . ?
H16A O3 C4 N2 141(7) . . . . ?
O16 O3 C4 N2 101.3(11) . . . . ?
H16A O3 C4 C1 -33(7) . . . . ?
O16 O3 C4 C1 -73.1(12) . . . . ?
C5 C1 C4 O3 59.8(5) . . . . ?
C9 C1 C4 O3 -64.3(5) . . . . ?
C2 C1 C4 O3 178.2(4) . . . . ?
C5 C1 C4 N2 -114.7(4) . . . . ?
C9 C1 C4 N2 121.3(4) . . . . ?
C2 C1 C4 N2 3.7(5) . . . . ?
C9 C1 C5 C6 -156.1(4) . . . . ?
C2 C1 C5 C6 -37.3(5) . . . . ?
C4 C1 C5 C6 83.4(5) . . . . ?
C9 C1 C5 C8 32.3(6) . . . . ?
C2 C1 C5 C8 151.1(4) . . . . ?
C4 C1 C5 C8 -88.3(5) . . . . ?
C8 C5 C6 O4 170.1(4) . . . . ?
C1 C5 C6 O4 -2.0(7) . . . . ?
C8 C5 C6 N3 -8.7(6) . . . . ?
C1 C5 C6 N3 179.2(4) . . . . ?
Na1 O5 C7 N4 120.7(6) 1_655 . . . ?
Na1 O5 C7 N3 -59.7(8) 1_655 . . . ?
C6 C5 C8 O6 -168.1(5) . . . . ?
C1 C5 C8 O6 3.4(8) . . . . ?
C6 C5 C8 N4 13.1(6) . . . . ?
C1 C5 C8 N4 -175.4(4) . . . . ?
C5 C1 C9 C12 -152.2(4) . . . . ?
C2 C1 C9 C12 87.1(5) . . . . ?
C4 C1 C9 C12 -34.5(5) . . . . ?
C5 C1 C9 C10 31.9(6) . . . . ?
C2 C1 C9 C10 -88.8(5) . . . . ?
C4 C1 C9 C10 149.6(4) . . . . ?
Na1 O7 C10 N5 -119.5(3) . . . . ?
Na1 O7 C10 C9 61.3(6) . . . . ?
C12 C9 C10 O7 -168.4(4) . . . . ?
C1 C9 C10 O7 7.5(7) . . . . ?
C12 C9 C10 N5 12.5(6) . . . . ?
C1 C9 C10 N5 -171.7(4) . . . . ?
C12 C9 C10 Na1 -133.8(3) . . . . ?
C1 C9 C10 Na1 42.0(4) . . . . ?
O1 Na1 C10 O7 143.1(4) . . . . ?
O11 Na1 C10 O7 -164.8(5) . . . . ?
O12 Na1 C10 O7 22.6(4) . . . . ?
O5 Na1 C10 O7 -128.1(3) 1_455 . . . ?
O8 Na1 C10 O7 -54.7(3) 2_656 . . . ?
Na2 Na1 C10 O7 -22.1(4) . . . . ?
O7 Na1 C10 N5 84.6(5) . . . . ?
O1 Na1 C10 N5 -132.3(4) . . . . ?
O11 Na1 C10 N5 -80.2(6) . . . . ?
O12 Na1 C10 N5 107.2(4) . . . . ?
O5 Na1 C10 N5 -43.5(3) 1_455 . . . ?
O8 Na1 C10 N5 29.9(4) 2_656 . . . ?
Na2 Na1 C10 N5 62.5(4) . . . . ?
O7 Na1 C10 C9 -135.0(5) . . . . ?
O1 Na1 C10 C9 8.1(3) . . . . ?
O11 Na1 C10 C9 60.2(6) . . . . ?
O12 Na1 C10 C9 -112.4(3) . . . . ?
O5 Na1 C10 C9 96.9(3) 1_455 . . . ?
O8 Na1 C10 C9 170.3(3) 2_656 . . . ?
Na2 Na1 C10 C9 -157.1(3) . . . . ?
Na2 O8 C11 N6 8.6(13) 2_656 . . . ?
Na1 O8 C11 N6 -157.2(4) 2_656 . . . ?
Na2 O8 C11 N5 -172.5(7) 2_656 . . . ?
Na1 O8 C11 N5 21.8(6) 2_656 . . . ?
H17A O9 C12 N6 73(2) . . . . ?
O17 O9 C12 N6 74.9(4) . . . . ?
H17A O9 C12 C9 -106(2) . . . . ?
O17 O9 C12 C9 -104.1(4) . . . . ?
C10 C9 C12 O9 170.9(4) . . . . ?
C1 C9 C12 O9 -5.2(7) . . . . ?
C10 C9 C12 N6 -8.1(6) . . . . ?
C1 C9 C12 N6 175.8(4) . . . . ?
O2 C3 N1 C2 -171.0(4) . . . . ?
N2 C3 N1 C2 7.8(6) . . . . ?
O2 C3 N1 O4 -25.3(6) . . . 2_757 ?
N2 C3 N1 O4 153.5(3) . . . 2_757 ?
O1 C2 N1 C3 168.2(4) . . . . ?
C1 C2 N1 C3 -17.7(6) . . . . ?
O1 C2 N1 O4 19.4(5) . . . 2_757 ?
C1 C2 N1 O4 -166.5(3) . . . 2_757 ?
O2 C3 N2 C4 -171.7(4) . . . . ?
N1 C3 N2 C4 9.5(6) . . . . ?
O2 C3 N2 O9 -9.7(6) . . . 2_767 ?
N1 C3 N2 O9 171.4(3) . . . 2_767 ?
O3 C4 N2 C3 170.8(4) . . . . ?
C1 C4 N2 C3 -14.6(6) . . . . ?
O3 C4 N2 O9 6.7(5) . . . 2_767 ?
C1 C4 N2 O9 -178.8(3) . . . 2_767 ?
O5 C7 N3 C6 -174.3(4) . . . . ?
N4 C7 N3 C6 5.3(7) . . . . ?
O4 C6 N3 C7 -179.7(4) . . . . ?
C5 C6 N3 C7 -0.7(7) . . . . ?
O5 C7 N4 C8 179.4(4) . . . . ?
N3 C7 N4 C8 -0.2(7) . . . . ?
O5 C7 N4 O7 18.5(5) . . . 2_756 ?
N3 C7 N4 O7 -161.1(3) . . . 2_756 ?
O6 C8 N4 C7 172.1(4) . . . . ?
C5 C8 N4 C7 -9.0(7) . . . . ?
O6 C8 N4 O7 -27.7(5) . . . 2_756 ?
C5 C8 N4 O7 151.3(3) . . . 2_756 ?
O8 C11 N5 C10 176.5(4) . . . . ?
N6 C11 N5 C10 -4.5(7) . . . . ?
O7 C10 N5 C11 174.2(4) . . . . ?
C9 C10 N5 C11 -6.5(7) . . . . ?
Na1 C10 N5 C11 130.5(4) . . . . ?
O8 C11 N6 C12 -171.4(5) . . . . ?
N5 C11 N6 C12 9.6(7) . . . . ?
O8 C11 N6 O16 20.7(6) . . . 1_455 ?
N5 C11 N6 O16 -158.3(4) . . . 1_455 ?
O9 C12 N6 C11 177.6(4) . . . . ?
C9 C12 N6 C11 -3.3(7) . . . . ?
O9 C12 N6 O16 -14.4(5) . . . 1_455 ?
C9 C12 N6 O16 164.7(3) . . . 1_455 ?
