# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Linfeng Rao'
_publ_contact_author_address     
;
Glenn T Seaborg Center
Lawrence Berkeley National Laboratory
Chemical Sciences Division
MS 70A-1150
Berkeley
CA
94720
UNITED STATES OF AMERICA
;

_publ_contact_author_email       LRAO@LBL.GOV

_publ_section_title              
;
Symmetry and optical spectra: a missing 1:2
Np(V)/oxydiacetate complex
;
loop_
_publ_author_name
'Linfeng Rao'
'Allen Oliver'
'Guoxin Tian'

data_npoda
_database_code_depnum_ccdc_archive 'CCDC 646382'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H8 O12 Np, Na3, 2(H2 O)'
_chemical_formula_sum            'C8 H16 Na3 Np O16'
_chemical_formula_weight         674.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0043 0.0021 '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'
O O 0.0139 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0439 0.0308 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Np Np -6.8138 4.9109 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.256(2)
_cell_length_b                   7.399(2)
_cell_length_c                   9.699(3)
_cell_angle_alpha                67.888(6)
_cell_angle_beta                 87.284(7)
_cell_angle_gamma                67.771(5)
_cell_volume                     443.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    2222
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      29.23

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             318
_exptl_absorpt_coefficient_mu    6.010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6784
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_process_details   'Sheldrik, 2005'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.77500
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  'channel-cut Si-<111> crystal'
_diffrn_measurement_device_type  'Bruker, PLlatinum 200'
_diffrn_measurement_method       \w/2\q-scans
_diffrn_detector_area_resol_mean 36.23
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3040
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         29.23
_reflns_number_total             1766
_reflns_number_gt                1766
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-2 v1.0.27 (Bruker AXS Inc, 2005)'
_computing_cell_refinement       'SAINT v7.06 (Bruker AXS Inc, 2005)'
_computing_data_reduction        'SAINT v7.06 (Bruker AXS Inc 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

The water hydrogen's, though located from a difference Fourier map, were
given a restrained bond distance of 0.83 (DFIX 0.83) to the oxygens to
which they are bonded. This restraint was applied to ensure a reasonable
and stable refinement.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0067P)^2^+4.3565P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1766
_refine_ls_number_parameters     142
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0779
_refine_ls_wR_factor_gt          0.0779
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Np1 Np 0.5000 0.5000 0.5000 0.01146(12) Uani 1 2 d S . .
Na1 Na 0.7943(4) 0.9919(4) 0.8695(3) 0.0215(6) Uani 1 1 d . . .
Na2 Na 1.0000 0.5000 1.0000 0.0196(8) Uani 1 2 d S . .
O1 O 0.7397(7) 0.5329(8) 0.3008(6) 0.0214(10) Uani 1 1 d . . .
O2 O 0.8831(8) 0.7232(8) 0.1274(6) 0.0248(11) Uani 1 1 d . . .
O3 O 0.7270(7) 0.7158(8) 0.4800(5) 0.0206(10) Uani 1 1 d . . .
O4 O 0.5350(7) 0.6254(8) 0.7082(6) 0.0215(10) Uani 1 1 d . . .
O5 O 0.6754(7) 0.7492(8) 0.8353(5) 0.0191(10) Uani 1 1 d . . .
O6 O 0.6932(7) 0.2448(7) 0.6206(5) 0.0192(10) Uani 1 1 d . . .
O10 O 1.1176(7) 0.7559(8) 0.8497(6) 0.0208(10) Uani 1 1 d D . .
H10A H 1.164(12) 0.709(14) 0.785(7) 0.025 Uiso 1 1 d D . .
H10B H 1.198(10) 0.769(14) 0.900(9) 0.025 Uiso 1 1 d D . .
O11 O 0.6054(7) 1.2493(8) 0.9625(6) 0.0213(10) Uani 1 1 d D . .
H11A H 0.587(13) 1.358(8) 0.888(6) 0.026 Uiso 1 1 d D . .
H11B H 0.513(9) 1.243(14) 1.016(8) 0.026 Uiso 1 1 d D . .
C1 C 0.8106(9) 0.6743(10) 0.2499(7) 0.0142(12) Uani 1 1 d . . .
C2 C 0.8144(10) 0.7922(12) 0.3479(8) 0.0199(14) Uani 1 1 d . . .
H2A H 0.9528 0.7688 0.3737 0.024 Uiso 1 1 calc R . .
H2B H 0.7389 0.9446 0.2941 0.024 Uiso 1 1 calc R . .
C3 C 0.7520(10) 0.7964(11) 0.5866(7) 0.0175(13) Uani 1 1 d . . .
H3A H 0.6951 0.9516 0.5422 0.021 Uiso 1 1 calc R . .
H3B H 0.8947 0.7477 0.6180 0.021 Uiso 1 1 calc R . .
C4 C 0.6456(9) 0.7176(10) 0.7204(7) 0.0152(12) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Np1 0.01432(17) 0.00953(17) 0.00933(17) -0.00311(12) -0.00146(10) -0.00360(12)
Na1 0.0274(14) 0.0157(13) 0.0182(13) -0.0060(11) -0.0012(11) -0.0052(11)
Na2 0.0267(19) 0.0165(19) 0.0163(18) -0.0065(16) 0.0027(14) -0.0089(15)
O1 0.026(2) 0.025(3) 0.018(2) -0.012(2) 0.0072(19) -0.012(2)
O2 0.031(3) 0.019(3) 0.022(3) -0.009(2) 0.006(2) -0.007(2)
O3 0.031(3) 0.028(3) 0.017(2) -0.014(2) 0.0071(19) -0.021(2)
O4 0.029(2) 0.026(3) 0.017(2) -0.011(2) 0.0049(19) -0.016(2)
O5 0.025(2) 0.025(3) 0.014(2) -0.010(2) 0.0008(18) -0.013(2)
O6 0.022(2) 0.011(2) 0.019(2) -0.0038(19) -0.0059(18) -0.0024(18)
O10 0.021(2) 0.024(3) 0.022(3) -0.012(2) 0.0040(19) -0.011(2)
O11 0.023(2) 0.019(3) 0.014(2) 0.000(2) 0.0027(18) -0.006(2)
C1 0.015(3) 0.014(3) 0.007(3) 0.000(2) 0.003(2) -0.002(2)
C2 0.025(3) 0.023(4) 0.013(3) -0.005(3) 0.007(3) -0.014(3)
C3 0.022(3) 0.020(3) 0.016(3) -0.009(3) 0.004(2) -0.012(3)
C4 0.015(3) 0.016(3) 0.012(3) -0.004(2) -0.003(2) -0.005(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Np1 O6 1.841(5) 2_666 ?
Np1 O6 1.841(5) . ?
Np1 O1 2.543(5) . ?
Np1 O1 2.543(5) 2_666 ?
Np1 O4 2.577(5) 2_666 ?
Np1 O4 2.577(5) . ?
Np1 O3 2.650(5) . ?
Np1 O3 2.650(5) 2_666 ?
Np1 Na1 4.005(3) 2_676 ?
Np1 Na1 4.005(3) 1_545 ?
Na1 O11 2.350(6) . ?
Na1 O6 2.365(6) 1_565 ?
Na1 O10 2.387(6) . ?
Na1 O5 2.392(5) . ?
Na1 O2 2.463(6) 1_556 ?
Na1 Na2 3.111(3) . ?
Na1 Np1 4.005(3) 1_565 ?
Na1 Na1 4.069(6) 2_777 ?
Na1 H11A 2.63(8) . ?
Na2 O2 2.313(5) 2_766 ?
Na2 O2 2.313(5) 1_556 ?
Na2 O10 2.337(5) . ?
Na2 O10 2.337(5) 2_767 ?
Na2 O5 2.520(5) . ?
Na2 O5 2.520(5) 2_767 ?
Na2 Na1 3.111(3) 2_767 ?
Na2 H10A 2.63(8) . ?
O1 C1 1.264(8) . ?
O2 C1 1.257(8) . ?
O2 Na2 2.313(5) 1_554 ?
O2 Na1 2.463(6) 1_554 ?
O3 C2 1.418(8) . ?
O3 C3 1.422(8) . ?
O4 C4 1.267(8) . ?
O5 C4 1.265(8) . ?
O6 Na1 2.365(6) 1_545 ?
O10 H10A 0.83(2) . ?
O10 H10B 0.83(2) . ?
O11 H11A 0.82(2) . ?
O11 H11B 0.83(2) . ?
C1 C2 1.520(9) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 C4 1.515(9) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?

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
O6 Np1 O6 180.0 2_666 . ?
O6 Np1 O1 90.6(2) 2_666 . ?
O6 Np1 O1 89.4(2) . . ?
O6 Np1 O1 89.4(2) 2_666 2_666 ?
O6 Np1 O1 90.6(2) . 2_666 ?
O1 Np1 O1 180.0 . 2_666 ?
O6 Np1 O4 85.17(19) 2_666 2_666 ?
O6 Np1 O4 94.83(19) . 2_666 ?
O1 Np1 O4 63.27(16) . 2_666 ?
O1 Np1 O4 116.72(16) 2_666 2_666 ?
O6 Np1 O4 94.83(19) 2_666 . ?
O6 Np1 O4 85.17(19) . . ?
O1 Np1 O4 116.73(16) . . ?
O1 Np1 O4 63.28(16) 2_666 . ?
O4 Np1 O4 180.0 2_666 . ?
O6 Np1 O3 85.96(19) 2_666 . ?
O6 Np1 O3 94.04(19) . . ?
O1 Np1 O3 58.86(15) . . ?
O1 Np1 O3 121.14(15) 2_666 . ?
O4 Np1 O3 121.22(15) 2_666 . ?
O4 Np1 O3 58.78(15) . . ?
O6 Np1 O3 94.04(19) 2_666 2_666 ?
O6 Np1 O3 85.96(19) . 2_666 ?
O1 Np1 O3 121.14(15) . 2_666 ?
O1 Np1 O3 58.86(15) 2_666 2_666 ?
O4 Np1 O3 58.78(15) 2_666 2_666 ?
O4 Np1 O3 121.22(15) . 2_666 ?
O3 Np1 O3 180.0 . 2_666 ?
O6 Np1 Na1 20.22(16) 2_666 2_676 ?
O6 Np1 Na1 159.78(16) . 2_676 ?
O1 Np1 Na1 71.45(12) . 2_676 ?
O1 Np1 Na1 108.55(12) 2_666 2_676 ?
O4 Np1 Na1 71.24(12) 2_666 2_676 ?
O4 Np1 Na1 108.76(12) . 2_676 ?
O3 Np1 Na1 81.63(12) . 2_676 ?
O3 Np1 Na1 98.37(12) 2_666 2_676 ?
O6 Np1 Na1 159.78(16) 2_666 1_545 ?
O6 Np1 Na1 20.22(16) . 1_545 ?
O1 Np1 Na1 108.55(12) . 1_545 ?
O1 Np1 Na1 71.45(12) 2_666 1_545 ?
O4 Np1 Na1 108.76(12) 2_666 1_545 ?
O4 Np1 Na1 71.24(12) . 1_545 ?
O3 Np1 Na1 98.37(12) . 1_545 ?
O3 Np1 Na1 81.63(12) 2_666 1_545 ?
Na1 Np1 Na1 180.0 2_676 1_545 ?
O11 Na1 O6 90.79(19) . 1_565 ?
O11 Na1 O10 147.6(2) . . ?
O6 Na1 O10 102.2(2) 1_565 . ?
O11 Na1 O5 123.3(2) . . ?
O6 Na1 O5 95.40(19) 1_565 . ?
O10 Na1 O5 85.29(19) . . ?
O11 Na1 O2 89.34(19) . 1_556 ?
O6 Na1 O2 176.7(2) 1_565 1_556 ?
O10 Na1 O2 79.35(19) . 1_556 ?
O5 Na1 O2 81.80(19) . 1_556 ?
O11 Na1 Na2 135.57(17) . . ?
O6 Na1 Na2 131.88(16) 1_565 . ?
O10 Na1 Na2 48.13(13) . . ?
O5 Na1 Na2 52.56(13) . . ?
O2 Na1 Na2 47.30(13) 1_556 . ?
O11 Na1 Np1 76.39(14) . 1_565 ?
O6 Na1 Np1 15.60(12) 1_565 1_565 ?
O10 Na1 Np1 117.64(16) . 1_565 ?
O5 Na1 Np1 98.19(14) . 1_565 ?
O2 Na1 Np1 162.99(16) 1_556 1_565 ?
Na2 Na1 Np1 143.57(9) . 1_565 ?
O11 Na1 Na1 75.89(15) . 2_777 ?
O6 Na1 Na1 119.58(18) 1_565 2_777 ?
O10 Na1 Na1 71.85(15) . 2_777 ?
O5 Na1 Na1 141.08(18) . 2_777 ?
O2 Na1 Na1 63.61(15) 1_556 2_777 ?
Na2 Na1 Na1 89.42(9) . 2_777 ?
Np1 Na1 Na1 120.16(11) 1_565 2_777 ?
O11 Na1 H11A 18.0(10) . . ?
O6 Na1 H11A 73.6(12) 1_565 . ?
O10 Na1 H11A 145.7(18) . . ?
O5 Na1 H11A 128.7(19) . . ?
O2 Na1 H11A 106.8(11) 1_556 . ?
Na2 Na1 H11A 153.5(10) . . ?
Np1 Na1 H11A 60.0(13) 1_565 . ?
Na1 Na1 H11A 80.8(19) 2_777 . ?
O2 Na2 O2 180.0 2_766 1_556 ?
O2 Na2 O10 96.50(18) 2_766 . ?
O2 Na2 O10 83.50(18) 1_556 . ?
O2 Na2 O10 83.50(18) 2_766 2_767 ?
O2 Na2 O10 96.50(18) 1_556 2_767 ?
O10 Na2 O10 180.0 . 2_767 ?
O2 Na2 O5 97.86(17) 2_766 . ?
O2 Na2 O5 82.14(17) 1_556 . ?
O10 Na2 O5 83.51(16) . . ?
O10 Na2 O5 96.49(17) 2_767 . ?
O2 Na2 O5 82.14(17) 2_766 2_767 ?
O2 Na2 O5 97.86(17) 1_556 2_767 ?
O10 Na2 O5 96.49(17) . 2_767 ?
O10 Na2 O5 83.50(16) 2_767 2_767 ?
O5 Na2 O5 180.0 . 2_767 ?
O2 Na2 Na1 128.52(14) 2_766 . ?
O2 Na2 Na1 51.48(14) 1_556 . ?
O10 Na2 Na1 49.51(13) . . ?
O10 Na2 Na1 130.49(13) 2_767 . ?
O5 Na2 Na1 48.91(12) . . ?
O5 Na2 Na1 131.09(12) 2_767 . ?
O2 Na2 Na1 51.48(14) 2_766 2_767 ?
O2 Na2 Na1 128.52(14) 1_556 2_767 ?
O10 Na2 Na1 130.49(13) . 2_767 ?
O10 Na2 Na1 49.51(13) 2_767 2_767 ?
O5 Na2 Na1 131.09(12) . 2_767 ?
O5 Na2 Na1 48.91(12) 2_767 2_767 ?
Na1 Na2 Na1 180.0 . 2_767 ?
O2 Na2 H10A 78.5(11) 2_766 . ?
O2 Na2 H10A 101.5(11) 1_556 . ?
O10 Na2 H10A 18.0(11) . . ?
O10 Na2 H10A 162.0(11) 2_767 . ?
O5 Na2 H10A 84.8(19) . . ?
O5 Na2 H10A 95.2(19) 2_767 . ?
Na1 Na2 H10A 62.8(15) . . ?
Na1 Na2 H10A 117.2(15) 2_767 . ?
C1 O1 Np1 127.3(4) . . ?
C1 O2 Na2 123.3(4) . 1_554 ?
C1 O2 Na1 140.9(4) . 1_554 ?
Na2 O2 Na1 81.22(18) 1_554 1_554 ?
C2 O3 C3 111.5(5) . . ?
C2 O3 Np1 122.4(4) . . ?
C3 O3 Np1 125.5(4) . . ?
C4 O4 Np1 129.1(4) . . ?
C4 O5 Na1 132.1(4) . . ?
C4 O5 Na2 116.5(4) . . ?
Na1 O5 Na2 78.52(15) . . ?
Np1 O6 Na1 144.2(3) . 1_545 ?
Na2 O10 Na1 82.35(17) . . ?
Na2 O10 H10A 101(6) . . ?
Na1 O10 H10A 133(6) . . ?
Na2 O10 H10B 111(6) . . ?
Na1 O10 H10B 105(6) . . ?
H10A O10 H10B 116(9) . . ?
Na1 O11 H11A 100(6) . . ?
Na1 O11 H11B 125(6) . . ?
H11A O11 H11B 119(9) . . ?
O2 C1 O1 126.2(6) . . ?
O2 C1 C2 116.8(6) . . ?
O1 C1 C2 117.0(5) . . ?
O3 C2 C1 108.5(5) . . ?
O3 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
O3 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
O3 C3 C4 108.3(5) . . ?
O3 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
O3 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
O5 C4 O4 125.5(6) . . ?
O5 C4 C3 116.9(6) . . ?
O4 C4 C3 117.5(6) . . ?

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
O11 Na1 Na2 O2 164.5(3) . . . 2_766 ?
O6 Na1 Na2 O2 4.3(3) 1_565 . . 2_766 ?
O10 Na1 Na2 O2 -60.7(2) . . . 2_766 ?
O5 Na1 Na2 O2 62.5(2) . . . 2_766 ?
O2 Na1 Na2 O2 180.0 1_556 . . 2_766 ?
Np1 Na1 Na2 O2 19.8(2) 1_565 . . 2_766 ?
Na1 Na1 Na2 O2 -126.54(18) 2_777 . . 2_766 ?
O11 Na1 Na2 O2 -15.5(3) . . . 1_556 ?
O6 Na1 Na2 O2 -175.7(3) 1_565 . . 1_556 ?
O10 Na1 Na2 O2 119.3(2) . . . 1_556 ?
O5 Na1 Na2 O2 -117.5(2) . . . 1_556 ?
Np1 Na1 Na2 O2 -160.2(2) 1_565 . . 1_556 ?
Na1 Na1 Na2 O2 53.46(18) 2_777 . . 1_556 ?
O11 Na1 Na2 O10 -134.8(3) . . . . ?
O6 Na1 Na2 O10 65.0(3) 1_565 . . . ?
O5 Na1 Na2 O10 123.2(2) . . . . ?
O2 Na1 Na2 O10 -119.3(2) 1_556 . . . ?
Np1 Na1 Na2 O10 80.5(2) 1_565 . . . ?
Na1 Na1 Na2 O10 -65.85(18) 2_777 . . . ?
O11 Na1 Na2 O10 45.2(3) . . . 2_767 ?
O6 Na1 Na2 O10 -115.0(3) 1_565 . . 2_767 ?
O10 Na1 Na2 O10 180.0 . . . 2_767 ?
O5 Na1 Na2 O10 -56.8(2) . . . 2_767 ?
O2 Na1 Na2 O10 60.7(2) 1_556 . . 2_767 ?
Np1 Na1 Na2 O10 -99.5(2) 1_565 . . 2_767 ?
Na1 Na1 Na2 O10 114.15(18) 2_777 . . 2_767 ?
O11 Na1 Na2 O5 102.0(3) . . . . ?
O6 Na1 Na2 O5 -58.2(2) 1_565 . . . ?
O10 Na1 Na2 O5 -123.2(2) . . . . ?
O2 Na1 Na2 O5 117.5(2) 1_556 . . . ?
Np1 Na1 Na2 O5 -42.67(18) 1_565 . . . ?
Na1 Na1 Na2 O5 170.99(19) 2_777 . . . ?
O11 Na1 Na2 O5 -78.0(3) . . . 2_767 ?
O6 Na1 Na2 O5 121.8(2) 1_565 . . 2_767 ?
O10 Na1 Na2 O5 56.8(2) . . . 2_767 ?
O5 Na1 Na2 O5 180.0 . . . 2_767 ?
O2 Na1 Na2 O5 -62.5(2) 1_556 . . 2_767 ?
Np1 Na1 Na2 O5 137.33(18) 1_565 . . 2_767 ?
Na1 Na1 Na2 O5 -9.01(19) 2_777 . . 2_767 ?
O11 Na1 Na2 Na1 -50(65) . . . 2_767 ?
O6 Na1 Na2 Na1 150(65) 1_565 . . 2_767 ?
O10 Na1 Na2 Na1 85(65) . . . 2_767 ?
O5 Na1 Na2 Na1 -152(65) . . . 2_767 ?
O2 Na1 Na2 Na1 -35(65) 1_556 . . 2_767 ?
Np1 Na1 Na2 Na1 165(65) 1_565 . . 2_767 ?
Na1 Na1 Na2 Na1 19(65) 2_777 . . 2_767 ?
O6 Np1 O1 C1 62.6(5) 2_666 . . . ?
O6 Np1 O1 C1 -117.4(5) . . . . ?
O1 Np1 O1 C1 142(14) 2_666 . . . ?
O4 Np1 O1 C1 146.8(6) 2_666 . . . ?
O4 Np1 O1 C1 -33.2(6) . . . . ?
O3 Np1 O1 C1 -22.3(5) . . . . ?
O3 Np1 O1 C1 157.7(5) 2_666 . . . ?
Na1 Np1 O1 C1 69.0(5) 2_676 . . . ?
Na1 Np1 O1 C1 -111.0(5) 1_545 . . . ?
O6 Np1 O3 C2 -73.6(5) 2_666 . . . ?
O6 Np1 O3 C2 106.4(5) . . . . ?
O1 Np1 O3 C2 19.6(5) . . . . ?
O1 Np1 O3 C2 -160.4(5) 2_666 . . . ?
O4 Np1 O3 C2 8.3(5) 2_666 . . . ?
O4 Np1 O3 C2 -171.7(5) . . . . ?
O3 Np1 O3 C2 28(73) 2_666 . . . ?
Na1 Np1 O3 C2 -53.7(5) 2_676 . . . ?
Na1 Np1 O3 C2 126.3(5) 1_545 . . . ?
O6 Np1 O3 C3 96.4(5) 2_666 . . . ?
O6 Np1 O3 C3 -83.6(5) . . . . ?
O1 Np1 O3 C3 -170.4(5) . . . . ?
O1 Np1 O3 C3 9.6(5) 2_666 . . . ?
O4 Np1 O3 C3 178.3(5) 2_666 . . . ?
O4 Np1 O3 C3 -1.7(5) . . . . ?
O3 Np1 O3 C3 -162(73) 2_666 . . . ?
Na1 Np1 O3 C3 116.3(5) 2_676 . . . ?
Na1 Np1 O3 C3 -63.7(5) 1_545 . . . ?
O6 Np1 O4 C4 -87.1(6) 2_666 . . . ?
O6 Np1 O4 C4 92.9(6) . . . . ?
O1 Np1 O4 C4 6.1(6) . . . . ?
O1 Np1 O4 C4 -173.9(6) 2_666 . . . ?
O4 Np1 O4 C4 -139(58) 2_666 . . . ?
O3 Np1 O4 C4 -4.8(5) . . . . ?
O3 Np1 O4 C4 175.2(5) 2_666 . . . ?
Na1 Np1 O4 C4 -72.1(6) 2_676 . . . ?
Na1 Np1 O4 C4 107.9(6) 1_545 . . . ?
O11 Na1 O5 C4 119.6(6) . . . . ?
O6 Na1 O5 C4 25.0(6) 1_565 . . . ?
O10 Na1 O5 C4 -76.8(6) . . . . ?
O2 Na1 O5 C4 -156.7(6) 1_556 . . . ?
Na2 Na1 O5 C4 -115.5(6) . . . . ?
Np1 Na1 O5 C4 40.5(6) 1_565 . . . ?
Na1 Na1 O5 C4 -129.9(5) 2_777 . . . ?
O11 Na1 O5 Na2 -124.9(2) . . . . ?
O6 Na1 O5 Na2 140.54(16) 1_565 . . . ?
O10 Na1 O5 Na2 38.72(16) . . . . ?
O2 Na1 O5 Na2 -41.18(15) 1_556 . . . ?
Np1 Na1 O5 Na2 156.00(10) 1_565 . . . ?
Na1 Na1 O5 Na2 -14.4(3) 2_777 . . . ?
O2 Na2 O5 C4 -4.0(5) 2_766 . . . ?
O2 Na2 O5 C4 176.0(5) 1_556 . . . ?
O10 Na2 O5 C4 91.7(5) . . . . ?
O10 Na2 O5 C4 -88.3(5) 2_767 . . . ?
O5 Na2 O5 C4 -172(22) 2_767 . . . ?
Na1 Na2 O5 C4 131.6(5) . . . . ?
Na1 Na2 O5 C4 -48.4(5) 2_767 . . . ?
O2 Na2 O5 Na1 -135.54(17) 2_766 . . . ?
O2 Na2 O5 Na1 44.46(17) 1_556 . . . ?
O10 Na2 O5 Na1 -39.85(17) . . . . ?
O10 Na2 O5 Na1 140.15(17) 2_767 . . . ?
O5 Na2 O5 Na1 56(21) 2_767 . . . ?
Na1 Na2 O5 Na1 180.0 2_767 . . . ?
O6 Np1 O6 Na1 90(38) 2_666 . . 1_545 ?
O1 Np1 O6 Na1 162.1(4) . . . 1_545 ?
O1 Np1 O6 Na1 -17.9(4) 2_666 . . 1_545 ?
O4 Np1 O6 Na1 -134.8(4) 2_666 . . 1_545 ?
O4 Np1 O6 Na1 45.2(4) . . . 1_545 ?
O3 Np1 O6 Na1 103.4(4) . . . 1_545 ?
O3 Np1 O6 Na1 -76.6(4) 2_666 . . 1_545 ?
Na1 Np1 O6 Na1 180.0 2_676 . . 1_545 ?
O2 Na2 O10 Na1 136.63(17) 2_766 . . . ?
O2 Na2 O10 Na1 -43.37(17) 1_556 . . . ?
O10 Na2 O10 Na1 -105(23) 2_767 . . . ?
O5 Na2 O10 Na1 39.42(16) . . . . ?
O5 Na2 O10 Na1 -140.58(16) 2_767 . . . ?
Na1 Na2 O10 Na1 180.00 2_767 . . . ?
O11 Na1 O10 Na2 112.2(4) . . . . ?
O6 Na1 O10 Na2 -136.35(17) 1_565 . . . ?
O5 Na1 O10 Na2 -41.83(16) . . . . ?
O2 Na1 O10 Na2 40.70(16) 1_556 . . . ?
Np1 Na1 O10 Na2 -138.61(12) 1_565 . . . ?
Na1 Na1 O10 Na2 106.22(14) 2_777 . . . ?
Na2 O2 C1 O1 -20.8(9) 1_554 . . . ?
Na1 O2 C1 O1 100.4(8) 1_554 . . . ?
Na2 O2 C1 C2 157.3(4) 1_554 . . . ?
Na1 O2 C1 C2 -81.5(8) 1_554 . . . ?
Np1 O1 C1 O2 -159.6(5) . . . . ?
Np1 O1 C1 C2 22.3(8) . . . . ?
C3 O3 C2 C1 171.4(5) . . . . ?
Np1 O3 C2 C1 -17.4(7) . . . . ?
O2 C1 C2 O3 -180.0(5) . . . . ?
O1 C1 C2 O3 -1.7(8) . . . . ?
C2 O3 C3 C4 177.0(5) . . . . ?
Np1 O3 C3 C4 6.1(7) . . . . ?
Na1 O5 C4 O4 -160.4(5) . . . . ?
Na2 O5 C4 O4 100.9(7) . . . . ?
Na1 O5 C4 C3 19.8(9) . . . . ?
Na2 O5 C4 C3 -78.9(6) . . . . ?
Np1 O4 C4 O5 -169.9(5) . . . . ?
Np1 O4 C4 C3 9.9(9) . . . . ?
O3 C3 C4 O5 170.4(5) . . . . ?
O3 C3 C4 O4 -9.4(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        29.23
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         2.687
_refine_diff_density_min         -2.478
_refine_diff_density_rms         0.223