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#$Date: 2023-04-20 21:15:05 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282778 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/48/1564823.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_1564823
loop_
_publ_author_name
'Somov, N.V.'
'Chausov, F.F.'
'Zakirova, R.M.'
'Petrov, V.G.'
'Shumilova, M.A.'
_publ_section_title
;
 Kristallicheskaya struktura tetra- i penta natriyevykh soley nitrilo
 trismetilen fosfonovoy kisloty
;
_journal_issue                   1
_journal_name_full               'Zhurnal neorganicheskoy khimii'
_journal_page_first              46
_journal_page_last               53
_journal_paper_doi               10.7868/S0044457X18010063
_journal_year                    2018
_chemical_formula_sum            'C6 H42 N2 Na8 O31 P6'
_chemical_formula_weight         1008.15
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2015-09-14T09:04:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                92.077(2)
_cell_angle_beta                 106.145(2)
_cell_angle_gamma                95.628(2)
_cell_formula_units_Z            1
_cell_length_a                   7.1515(2)
_cell_length_b                   11.1590(3)
_cell_length_c                   12.0583(3)
_cell_measurement_reflns_used    12768
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.902
_cell_measurement_theta_min      3.909
_cell_volume                     917.86(4)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0302
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0165792
_diffrn_orient_matrix_UB_12      0.0336532
_diffrn_orient_matrix_UB_13      0.0535464
_diffrn_orient_matrix_UB_21      -0.1020613
_diffrn_orient_matrix_UB_22      -0.0073468
_diffrn_orient_matrix_UB_23      -0.0060176
_diffrn_orient_matrix_UB_31      0.0103482
_diffrn_orient_matrix_UB_32      -0.0539542
_diffrn_orient_matrix_UB_33      0.0293807
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17907
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.324
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       prism
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1461
_exptl_crystal_size_min          0.0852
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5585
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0314P)²+0.3635P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0
_reflns_number_gt                5196
_reflns_number_total             5585
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            tmpkcyu3mwl
_cod_data_source_block           naatmp_2
_cod_database_code               1564823
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.21116(16) 0.07175(10) 0.62875(9) 0.01681(19) Uani 1 1 d . . . . .
C2 C 1.12608(17) 0.17725(10) 0.79110(9) 0.01733(19) Uani 1 1 d . . . . .
C3 C 1.04440(16) 0.02662(10) 1.28741(10) 0.0179(2) Uani 1 1 d . . . . .
N1 N 1.14121(13) 0.05794(8) 0.73476(8) 0.01356(16) Uani 1 1 d . . . . .
O1 O 0.5392 0.0914 0.5622 0.02735(19) Uani 1 1 d D . . . .
O2 O 0.55273(13) 0.03744(8) 0.76959(7) 0.02112(16) Uani 1 1 d . . . . .
O3 O 0.51675(14) 0.25023(8) 0.70545(8) 0.02408(18) Uani 1 1 d . . . . .
O4 O 1.34677(12) 0.10676(8) 0.99205(7) 0.02031(16) Uani 1 1 d . . . . .
O5 O 1.19520(15) 0.30531(8) 0.98862(8) 0.02590(19) Uani 1 1 d . . . . .
O6 O 0.98818(12) 0.10639(8) 0.97124(8) 0.02161(17) Uani 1 1 d D . . . .
O7 O 1.16015(13) 0.25209(8) 1.25054(8) 0.02349(17) Uani 1 1 d . . . . .
O8 O 0.79755(12) 0.17618(8) 1.18390(7) 0.02134(16) Uani 1 1 d . . . . .
O9 O 0.96859(15) 0.22325(9) 1.39828(8) 0.02650(19) Uani 1 1 d . . . . .
O10 O 0.6652(2) 0.31961(11) 0.93154(10) 0.0459(3) Uani 1 1 d D . . . .
O11 O 0.86546(18) 0.50522(9) 1.15145(10) 0.0391(2) Uani 1 1 d . . . . .
O12 O 1.49247(19) 0.40781(14) 1.18410(11) 0.0490(3) Uani 1 1 d . . . . .
O13 O 1.1997(2) 0.57941(11) 1.33126(11) 0.0448(3) Uani 1 1 d . . . . .
O14 O 1.60928(19) 0.25679(12) 1.40889(11) 0.0444(3) Uani 1 1 d . . . . .
O15 O 1.6230(3) 0.57532(19) 1.44302(18) 0.0284(4) Uani 0.5 1 d . . P . .
O16 O 1.2739(4) 0.3841(2) 1.53260(19) 0.0321(4) Uani 0.5 1 d . . P . .
O17 O 0.9832(3) 0.4414(2) 1.4972(2) 0.0441(6) Uani 0.5 1 d . . P . .
Na1 Na 0.53054(8) -0.17583(5) 0.79089(5) 0.02697(11) Uani 1 1 d . . . . .
Na2 Na 1.39093(8) 0.40413(5) 1.35855(5) 0.02807(12) Uani 1 1 d . . . . .
Na3 Na 0.95513(8) 0.32805(5) 1.08326(5) 0.02734(11) Uani 1 1 d . . . . .
Na4 Na 0.65991(7) 0.10236(4) 0.97299(4) 0.02114(10) Uani 1 1 d D . . . .
P1 P 0.47636(4) 0.11607(3) 0.67238(2) 0.01536(6) Uani 1 1 d D . . . .
P2 P 1.17134(4) 0.17386(2) 0.94770(2) 0.01383(6) Uani 1 1 d D . . . .
P3 P 0.98933(4) 0.18363(3) 1.28074(2) 0.01635(6) Uani 1 1 d . . . . .
H1 H 0.185(2) -0.0078(15) 0.5855(14) 0.024(4) Uiso 1 1 d . . . . .
H2 H 0.138(2) 0.1274(15) 0.5840(14) 0.022(4) Uiso 1 1 d . . . . .
H3 H 0.995(3) 0.1996(16) 0.7540(15) 0.032(4) Uiso 1 1 d D . . . .
H4 H 1.223(3) 0.2344(16) 0.7795(14) 0.027(4) Uiso 1 1 d . . . . .
H5 H 1.103(3) 0.0118(15) 1.2243(15) 0.026(4) Uiso 1 1 d . . . . .
H6 H 1.127(2) 0.0092(15) 1.3583(14) 0.022(4) Uiso 1 1 d . . . . .
H7 H 1.236(2) 0.0235(14) 0.7836(13) 0.018(4) Uiso 1 1 d . . . . .
H8 H 0.592(3) 0.3687(18) 0.948(2) 0.075(2) Uiso 1 1 d D . . . .
H9 H 0.6203 0.2999 0.8565 0.075(2) Uiso 1 1 d . . . . .
H10 H 0.8459 0.5595 1.1118 0.075(2) Uiso 1 1 d . . . . .
H11 H 0.9649 0.539 1.2064 0.075(2) Uiso 1 1 d . . . . .
H12 H 1.1715 0.5954 1.3975 0.075(2) Uiso 1 1 d . . . . .
H13 H 1.2731 0.637 1.3257 0.075(2) Uiso 1 1 d . . . . .
H14 H 1.4077 0.3907 1.117 0.075(2) Uiso 1 1 d . . . . .
H15 H 1.5876 0.4341 1.1634 0.075(2) Uiso 1 1 d . . . . .
H16 H 1.5843 0.2099 1.4558 0.075(2) Uiso 1 1 d . . . . .
H17 H 1.7219 0.2458 1.4037 0.075(2) Uiso 1 1 d . . . . .
H18 H 1.2599 0.4398 1.5578 0.075(2) Uiso 0.5 1 d . . P . .
H19 H 1.1814 0.3271 1.5048 0.075(2) Uiso 0.5 1 d . . P . .
H20 H 0.9028 0.4938 1.461 0.075(2) Uiso 0.5 1 d . . P . .
H21 H 0.9748 0.3801 1.4524 0.075(2) Uiso 0.5 1 d . . P . .
H22 H 1.6222 0.6413 1.4003 0.075(2) Uiso 1 1 d . . . . .
H23 H 1.011(9) 0.037(2) 0.995(5) 0.075(2) Uiso 0.5 1 d D . P . .
H24 H 0.500(9) 0.026(2) 0.520(3) 0.075(2) Uiso 0.5 1 d D . P . .
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 0 '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 0.006 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -2 16 0.0662
0 0 -16 0.0771
1 -16 0 0.0362
0 15 2 0.0296
10 0 -7 0.1026
-9 5 0 0.1123
-3 -8 15 0.0661
-8 11 4 0.08
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
N1 C1 P1 109.50(7) 1_455 . ?
N1 C1 H1 107.8(10) 1_455 . ?
P1 C1 H1 108.0(10) . . ?
N1 C1 H2 107.4(10) 1_455 . ?
P1 C1 H2 114.0(10) . . ?
H1 C1 H2 110.0(14) . . ?
N1 C2 P2 112.76(7) . . ?
N1 C2 H3 107.1(11) . . ?
P2 C2 H3 111.5(10) . . ?
N1 C2 H4 108.8(10) . . ?
P2 C2 H4 106.2(10) . . ?
H3 C2 H4 110.5(15) . . ?
N1 C3 P3 110.42(7) 2_757 . ?
N1 C3 H5 108.0(10) 2_757 . ?
P3 C3 H5 106.1(10) . . ?
N1 C3 H6 107.2(10) 2_757 . ?
P3 C3 H6 114.1(10) . . ?
H5 C3 H6 110.9(14) . . ?
C2 N1 C3 112.19(8) . 2_757 ?
C2 N1 C1 112.30(8) . 1_655 ?
C3 N1 C1 112.84(8) 2_757 1_655 ?
C2 N1 H7 107.6(10) . . ?
C3 N1 H7 107.1(10) 2_757 . ?
C1 N1 H7 104.2(10) 1_655 . ?
P1 O1 H24 122(4) . . ?
P1 O2 Na1 134.84(5) . . ?
P1 O2 Na4 125.53(5) . . ?
Na1 O2 Na4 97.61(3) . . ?
P2 O4 Na4 139.11(5) . 1_655 ?
P2 O4 Na4 126.11(5) . 2_757 ?
Na4 O4 Na4 88.56(3) 1_655 2_757 ?
P2 O4 Na1 103.50(4) . 2_757 ?
Na4 O4 Na1 93.85(3) 1_655 2_757 ?
Na4 O4 Na1 93.65(3) 2_757 2_757 ?
P2 O5 Na3 106.49(5) . . ?
P2 O6 Na4 149.46(5) . . ?
P2 O6 Na3 85.47(4) . . ?
Na4 O6 Na3 73.22(3) . . ?
P2 O6 H23 111(4) . . ?
Na4 O6 H23 99(4) . . ?
Na3 O6 H23 133(4) . . ?
P3 O7 Na2 129.19(5) . . ?
P3 O7 Na3 93.23(4) . . ?
Na2 O7 Na3 110.79(4) . . ?
P3 O7 Na1 130.47(5) . 2_757 ?
Na2 O7 Na1 82.18(3) . 2_757 ?
Na3 O7 Na1 111.46(4) . 2_757 ?
P3 O8 Na1 126.03(5) . 2_657 ?
P3 O8 Na3 89.07(4) . . ?
Na1 O8 Na3 125.61(4) 2_657 . ?
P3 O8 Na4 139.44(5) . . ?
Na1 O8 Na4 92.01(3) 2_657 . ?
Na3 O8 Na4 76.93(3) . . ?
Na3 O10 Na4 80.23(4) . . ?
Na3 O10 H8 109.5(17) . . ?
Na4 O10 H8 126.2(18) . . ?
Na3 O10 H9 140.22(12) . . ?
Na4 O10 H9 90.63(9) . . ?
H8 O10 H9 107.1(18) . . ?
Na3 O11 H10 120.33(11) . . ?
Na3 O11 H11 107.76(9) . . ?
H10 O11 H11 99.51(11) . . ?
Na2 O12 Na1 80.58(4) . 2_757 ?
Na2 O12 H14 120.66(10) . . ?
Na1 O12 H14 86.63(10) 2_757 . ?
Na2 O12 H15 138.49(11) . . ?
Na1 O12 H15 113.79(12) 2_757 . ?
H14 O12 H15 99.59(13) . . ?
Na2 O13 H12 107.26(10) . . ?
Na2 O13 H13 106.96(11) . . ?
H12 O13 H13 104.46(14) . . ?
Na2 O14 Na1 85.31(4) . 2_757 ?
Na2 O14 H16 114.39(9) . . ?
Na1 O14 H16 112.37(12) 2_757 . ?
Na2 O14 H17 137.11(10) . . ?
Na1 O14 H17 89.31(9) 2_757 . ?
H16 O14 H17 106.98(12) . . ?
O16 O15 Na2 159.5(3) 2_868 . ?
O16 O15 Na2 84.2(2) 2_868 2_868 ?
Na2 O15 Na2 104.36(8) . 2_868 ?
O16 O15 H22 71.5(2) 2_868 . ?
Na2 O15 H22 117.25(17) . . ?
Na2 O15 H22 120.54(17) 2_868 . ?
O15 O16 Na2 77.1(2) 2_868 . ?
O15 O16 H18 70.4(3) 2_868 . ?
Na2 O16 H18 114.1(2) . . ?
O15 O16 H19 165.8(3) 2_868 . ?
Na2 O16 H19 97.57(16) . . ?
H18 O16 H19 123.5(3) . . ?
O17 O17 H20 52.28(18) 2_768 . ?
O17 O17 H21 141.4(4) 2_768 . ?
H20 O17 H21 109.9(3) . . ?
O2 Na1 O14 101.93(4) . 2_757 ?
O2 Na1 O8 91.17(3) . 2_657 ?
O14 Na1 O8 90.66(4) 2_757 2_657 ?
O2 Na1 O4 82.45(3) . 2_757 ?
O14 Na1 O4 174.00(4) 2_757 2_757 ?
O8 Na1 O4 85.12(3) 2_657 2_757 ?
O2 Na1 O7 107.03(3) . 2_757 ?
O14 Na1 O7 79.82(4) 2_757 2_757 ?
O8 Na1 O7 160.80(4) 2_657 2_757 ?
O4 Na1 O7 102.95(3) 2_757 2_757 ?
O2 Na1 O12 179.54(4) . 2_757 ?
O14 Na1 O12 78.53(4) 2_757 2_757 ?
O8 Na1 O12 88.82(4) 2_657 2_757 ?
O4 Na1 O12 97.09(4) 2_757 2_757 ?
O7 Na1 O12 73.03(4) 2_757 2_757 ?
O2 Na1 Na2 133.37(3) . 2_757 ?
O14 Na1 Na2 46.30(3) 2_757 2_757 ?
O8 Na1 Na2 117.20(3) 2_657 2_757 ?
O4 Na1 Na2 132.70(3) 2_757 2_757 ?
O7 Na1 Na2 45.07(2) 2_757 2_757 ?
O12 Na1 Na2 46.99(3) 2_757 2_757 ?
O2 Na1 P2 98.61(3) . 2_757 ?
O14 Na1 P2 153.45(3) 2_757 2_757 ?
O8 Na1 P2 105.64(3) 2_657 2_757 ?
O4 Na1 P2 26.507(19) 2_757 2_757 ?
O7 Na1 P2 78.19(2) 2_757 2_757 ?
O12 Na1 P2 80.95(3) 2_757 2_757 ?
Na2 Na1 P2 107.148(19) 2_757 2_757 ?
O2 Na1 Na4 84.33(3) . 2_657 ?
O14 Na1 Na4 135.52(3) 2_757 2_657 ?
O8 Na1 Na4 44.93(2) 2_657 2_657 ?
O4 Na1 Na4 40.22(2) 2_757 2_657 ?
O7 Na1 Na4 140.90(3) 2_757 2_657 ?
O12 Na1 Na4 95.33(3) 2_757 2_657 ?
Na2 Na1 Na4 142.02(2) 2_757 2_657 ?
P2 Na1 Na4 62.990(13) 2_757 2_657 ?
O2 Na1 Na4 41.40(2) . . ?
O14 Na1 Na4 143.05(3) 2_757 . ?
O8 Na1 Na4 86.64(3) 2_657 . ?
O4 Na1 Na4 41.06(2) 2_757 . ?
O7 Na1 Na4 110.97(3) 2_757 . ?
O12 Na1 Na4 138.13(3) 2_757 . ?
Na2 Na1 Na4 156.02(2) 2_757 . ?
P2 Na1 Na4 60.511(13) 2_757 . ?
Na4 Na1 Na4 54.219(16) 2_657 . ?
O2 Na1 Na3 117.92(3) . 2_757 ?
O14 Na1 Na3 106.47(3) 2_757 2_757 ?
O8 Na1 Na3 141.03(3) 2_657 2_757 ?
O4 Na1 Na3 74.59(2) 2_757 2_757 ?
O7 Na1 Na3 32.45(2) 2_757 2_757 ?
O12 Na1 Na3 61.89(3) 2_757 2_757 ?
Na2 Na1 Na3 61.950(15) 2_757 2_757 ?
P2 Na1 Na3 48.227(11) 2_757 2_757 ?
Na4 Na1 Na3 108.991(17) 2_657 2_757 ?
Na4 Na1 Na3 98.366(17) . 2_757 ?
O7 Na2 O14 87.70(5) . . ?
O7 Na2 O15 171.35(6) . . ?
O14 Na2 O15 96.71(6) . . ?
O7 Na2 O12 82.10(4) . . ?
O14 Na2 O12 84.29(5) . . ?
O15 Na2 O12 90.92(6) . . ?
O7 Na2 O15 111.89(6) . 2_868 ?
O14 Na2 O15 90.16(6) . 2_868 ?
O15 Na2 O15 75.64(9) . 2_868 ?
O12 Na2 O15 164.79(7) . 2_868 ?
O7 Na2 O13 101.22(4) . . ?
O14 Na2 O13 170.80(6) . . ?
O15 Na2 O13 74.75(6) . . ?
O12 Na2 O13 99.05(5) . . ?
O15 Na2 O13 84.45(6) 2_868 . ?
O7 Na2 O16 93.69(7) . . ?
O14 Na2 O16 94.00(6) . . ?
O15 Na2 O16 93.41(8) . . ?
O12 Na2 O16 175.51(7) . . ?
O15 Na2 O16 18.74(6) 2_868 . ?
O13 Na2 O16 83.27(6) . . ?
O7 Na2 Na1 52.75(3) . 2_757 ?
O14 Na2 Na1 48.39(4) . 2_757 ?
O15 Na2 Na1 125.94(6) . 2_757 ?
O12 Na2 Na1 52.43(4) . 2_757 ?
O15 Na2 Na1 131.04(5) 2_868 2_757 ?
O13 Na2 Na1 139.80(4) . 2_757 ?
O16 Na2 Na1 123.56(6) . 2_757 ?
O7 Na2 Na2 149.24(4) . 2_868 ?
O14 Na2 Na2 94.31(4) . 2_868 ?
O15 Na2 Na2 38.10(5) . 2_868 ?
O12 Na2 Na2 128.66(4) . 2_868 ?
O15 Na2 Na2 37.54(6) 2_868 2_868 ?
O13 Na2 Na2 76.88(4) . 2_868 ?
O16 Na2 Na2 55.54(6) . 2_868 ?
Na1 Na2 Na2 141.94(3) 2_757 2_868 ?
O7 Na2 Na3 35.08(3) . . ?
O14 Na2 Na3 116.49(4) . . ?
O15 Na2 Na3 136.98(5) . . ?
O12 Na2 Na3 67.65(3) . . ?
O15 Na2 Na3 127.25(6) 2_868 . ?
O13 Na2 Na3 72.65(4) . . ?
O16 Na2 Na3 109.66(6) . . ?
Na1 Na2 Na3 70.215(16) 2_757 . ?
Na2 Na2 Na3 147.71(3) 2_868 . ?
O11 Na3 O5 128.60(4) . . ?
O11 Na3 O10 86.67(5) . . ?
O5 Na3 O10 103.60(5) . . ?
O11 Na3 O7 104.53(4) . . ?
O5 Na3 O7 89.02(4) . . ?
O10 Na3 O7 152.58(5) . . ?
O11 Na3 O8 100.78(4) . . ?
O5 Na3 O8 128.73(4) . . ?
O10 Na3 O8 90.60(5) . . ?
O7 Na3 O8 62.98(3) . . ?
O11 Na3 O6 168.76(4) . . ?
O5 Na3 O6 57.11(3) . . ?
O10 Na3 O6 82.34(4) . . ?
O7 Na3 O6 84.46(3) . . ?
O8 Na3 O6 77.07(3) . . ?
O11 Na3 P3 101.03(3) . . ?
O5 Na3 P3 113.68(3) . . ?
O10 Na3 P3 122.48(4) . . ?
O7 Na3 P3 31.53(2) . . ?
O8 Na3 P3 31.87(2) . . ?
O6 Na3 P3 83.04(2) . . ?
O11 Na3 Na4 123.93(4) . . ?
O5 Na3 Na4 99.86(3) . . ?
O10 Na3 Na4 51.96(4) . . ?
O7 Na3 Na4 102.35(3) . . ?
O8 Na3 Na4 52.29(2) . . ?
O6 Na3 Na4 46.18(2) . . ?
P3 Na3 Na4 78.931(17) . . ?
O11 Na3 P2 155.65(4) . . ?
O5 Na3 P2 27.60(2) . . ?
O10 Na3 P2 95.21(4) . . ?
O7 Na3 P2 84.76(3) . . ?
O8 Na3 P2 103.46(3) . . ?
O6 Na3 P2 29.593(18) . . ?
P3 Na3 P2 98.382(18) . . ?
Na4 Na3 P2 74.216(16) . . ?
O11 Na3 Na2 80.58(3) . . ?
O5 Na3 Na2 85.24(3) . . ?
O10 Na3 Na2 167.22(4) . . ?
O7 Na3 Na2 34.13(2) . . ?
O8 Na3 Na2 90.93(3) . . ?
O6 Na3 Na2 110.36(2) . . ?
P3 Na3 Na2 59.956(14) . . ?
Na4 Na3 Na2 136.43(2) . . ?
P2 Na3 Na2 96.770(17) . . ?
O11 Na3 Na1 128.03(4) . 2_757 ?
O5 Na3 Na1 53.21(3) . 2_757 ?
O10 Na3 Na1 144.93(4) . 2_757 ?
O7 Na3 Na1 36.09(2) . 2_757 ?
O8 Na3 Na1 87.76(3) . 2_757 ?
O6 Na3 Na1 63.15(2) . 2_757 ?
P3 Na3 Na1 62.173(14) . 2_757 ?
Na4 Na3 Na1 101.849(18) . 2_757 ?
P2 Na3 Na1 51.490(12) . 2_757 ?
Na2 Na3 Na1 47.834(13) . 2_757 ?
O4 Na4 O6 174.66(4) 1_455 . ?
O4 Na4 O4 91.44(3) 1_455 2_757 ?
O6 Na4 O4 89.66(3) . 2_757 ?
O4 Na4 O2 95.18(3) 1_455 . ?
O6 Na4 O2 90.10(3) . . ?
O4 Na4 O2 86.27(3) 2_757 . ?
O4 Na4 O10 88.82(4) 1_455 . ?
O6 Na4 O10 90.20(4) . . ?
O4 Na4 O10 178.67(4) 2_757 . ?
O2 Na4 O10 92.41(4) . . ?
O4 Na4 O8 88.96(3) 1_455 . ?
O6 Na4 O8 85.74(3) . . ?
O4 Na4 O8 95.20(3) 2_757 . ?
O2 Na4 O8 175.57(4) . . ?
O10 Na4 O8 86.11(4) . . ?
O4 Na4 Na3 115.27(3) 1_455 . ?
O6 Na4 Na3 60.60(3) . . ?
O4 Na4 Na3 133.08(3) 2_757 . ?
O2 Na4 Na3 125.55(3) . . ?
O10 Na4 Na3 47.81(3) . . ?
O8 Na4 Na3 50.78(2) . . ?
O4 Na4 Na4 46.54(2) 1_455 2_657 ?
O6 Na4 Na4 134.32(3) . 2_657 ?
O4 Na4 Na4 44.90(2) 2_757 2_657 ?
O2 Na4 Na4 90.94(3) . 2_657 ?
O10 Na4 Na4 135.35(4) . 2_657 ?
O8 Na4 Na4 93.04(3) . 2_657 ?
Na3 Na4 Na4 142.87(3) . 2_657 ?
O4 Na4 Na1 45.93(3) 1_455 2_657 ?
O6 Na4 Na1 128.79(3) . 2_657 ?
O4 Na4 Na1 93.56(3) 2_757 2_657 ?
O2 Na4 Na1 141.11(3) . 2_657 ?
O10 Na4 Na1 87.56(4) . 2_657 ?
O8 Na4 Na1 43.06(2) . 2_657 ?
Na3 Na4 Na1 81.379(18) . 2_657 ?
Na4 Na4 Na1 63.509(18) 2_657 2_657 ?
O4 Na4 Na1 93.69(3) 1_455 . ?
O6 Na4 Na1 90.79(3) . . ?
O4 Na4 Na1 45.30(2) 2_757 . ?
O2 Na4 Na1 40.99(2) . . ?
O10 Na4 Na1 133.38(3) . . ?
O8 Na4 Na1 140.42(3) . . ?
Na3 Na4 Na1 150.57(2) . . ?
Na4 Na4 Na1 62.272(18) 2_657 . ?
Na1 Na4 Na1 125.781(16) 2_657 . ?
O4 Na4 H9 89.70(3) 1_455 . ?
O6 Na4 H9 91.13(3) . . ?
O4 Na4 H9 159.23(3) 2_757 . ?
O2 Na4 H9 72.98(2) . . ?
O10 Na4 H9 19.45(3) . . ?
O8 Na4 H9 105.55(3) . . ?
Na3 Na4 H9 63.809(14) . . ?
Na4 Na4 H9 132.47(2) 2_657 . ?
Na1 Na4 H9 102.037(17) 2_657 . ?
Na1 Na4 H9 113.936(18) . . ?
O4 Na4 H23 160.8(8) 1_455 . ?
O6 Na4 H23 18.6(7) . . ?
O4 Na4 H23 71.3(7) 2_757 . ?
O2 Na4 H23 92.0(13) . . ?
O10 Na4 H23 108.6(7) . . ?
O8 Na4 H23 84.6(13) . . ?
Na3 Na4 H23 73.9(10) . . ?
Na4 Na4 H23 115.7(7) 2_657 . ?
Na1 Na4 H23 124.8(13) 2_657 . ?
Na1 Na4 H23 80.2(11) . . ?
H9 Na4 H23 109.4(7) . . ?
O2 P1 O3 114.69(5) . . ?
O2 P1 O1 115.41(4) . . ?
O3 P1 O1 108.43(4) . . ?
O2 P1 C1 103.72(5) . . ?
O3 P1 C1 109.30(5) . . ?
O1 P1 C1 104.56(4) . . ?
O4 P2 O5 116.18(6) . . ?
O4 P2 O6 110.47(5) . . ?
O5 P2 O6 110.63(5) . . ?
O4 P2 C2 107.32(5) . . ?
O5 P2 C2 103.67(5) . . ?
O6 P2 C2 108.01(5) . . ?
O4 P2 Na3 129.86(4) . . ?
O5 P2 Na3 45.91(4) . . ?
O6 P2 Na3 64.94(4) . . ?
C2 P2 Na3 121.84(4) . . ?
O4 P2 Na1 49.99(4) . 2_757 ?
O5 P2 Na1 77.92(4) . 2_757 ?
O6 P2 Na1 97.81(4) . 2_757 ?
C2 P2 Na1 151.25(4) . 2_757 ?
Na3 P2 Na1 80.283(15) . 2_757 ?
O7 P3 O9 113.87(5) . . ?
O7 P3 O8 113.23(5) . . ?
O9 P3 O8 113.21(5) . . ?
O7 P3 C3 105.01(5) . . ?
O9 P3 C3 107.22(5) . . ?
O8 P3 C3 103.14(5) . . ?
O7 P3 Na3 55.24(4) . . ?
O9 P3 Na3 126.90(4) . . ?
O8 P3 Na3 59.05(4) . . ?
C3 P3 Na3 125.88(4) . . ?
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
C1 N1 1.5042(13) 1_455 ?
C1 P1 1.8332(11) . ?
C1 H1 0.988(17) . ?
C1 H2 0.938(16) . ?
C2 N1 1.4999(14) . ?
C2 P2 1.8274(11) . ?
C2 H3 0.979(18) . ?
C2 H4 0.936(18) . ?
C3 N1 1.5041(14) 2_757 ?
C3 P3 1.8329(12) . ?
C3 H5 0.981(17) . ?
C3 H6 0.935(16) . ?
N1 C3 1.5041(14) 2_757 ?
N1 C1 1.5043(13) 1_655 ?
N1 H7 0.893(16) . ?
O1 P1 1.5408(3) . ?
O1 H24 0.8500(11) . ?
O2 P1 1.5016(8) . ?
O2 Na1 2.3974(10) . ?
O2 Na4 2.4175(10) . ?
O3 P1 1.5137(9) . ?
O4 P2 1.5035(8) . ?
O4 Na4 2.3189(9) 1_655 ?
O4 Na4 2.3846(10) 2_757 ?
O4 Na1 2.5804(10) 2_757 ?
O5 P2 1.5086(9) . ?
O5 Na3 2.3385(11) . ?
O6 P2 1.5466(9) . ?
O6 Na4 2.3496(9) . ?
O6 Na3 2.8370(11) . ?
O6 H23 0.850(2) . ?
O7 P3 1.5143(9) . ?
O7 Na2 2.3225(10) . ?
O7 Na3 2.3790(11) . ?
O7 Na1 2.6115(11) 2_757 ?
O8 P3 1.5269(9) . ?
O8 Na1 2.4480(10) 2_657 ?
O8 Na3 2.4798(10) . ?
O8 Na4 2.5323(10) . ?
O9 P3 1.5201(9) . ?
O10 Na3 2.3440(13) . ?
O10 Na4 2.4918(14) . ?
O10 H8 0.8498(10) . ?
O10 H9 0.8834(12) . ?
O11 Na3 2.3282(13) . ?
O11 H10 0.7845(11) . ?
O11 H11 0.8683(12) . ?
O12 Na2 2.4091(13) . ?
O12 Na1 2.6114(16) 2_757 ?
O12 H14 0.8672(13) . ?
O12 H15 0.8195(12) . ?
O13 Na2 2.4749(14) . ?
O13 H12 0.8927(12) . ?
O13 H13 0.8059(12) . ?
O14 Na2 2.3577(12) . ?
O14 Na1 2.4382(15) 2_757 ?
O14 H16 0.8277(11) . ?
O14 H17 0.8453(11) . ?
O15 O16 0.799(3) 2_868 ?
O15 Na2 2.395(2) . ?
O15 Na2 2.426(2) 2_868 ?
O15 H22 0.914(2) . ?
O16 O15 0.799(3) 2_868 ?
O16 Na2 2.476(2) . ?
O16 H18 0.709(2) . ?
O16 H19 0.857(2) . ?
O17 O17 1.302(5) 2_768 ?
O17 H20 0.899(3) . ?
O17 H21 0.843(2) . ?
Na1 O14 2.4382(15) 2_757 ?
Na1 O8 2.4480(10) 2_657 ?
Na1 O4 2.5804(10) 2_757 ?
Na1 O7 2.6114(11) 2_757 ?
Na1 O12 2.6115(16) 2_757 ?
Na1 Na2 3.2502(8) 2_757 ?
Na1 P2 3.2757(6) 2_757 ?
Na1 Na4 3.5833(7) 2_657 ?
Na1 Na4 3.6231(8) . ?
Na1 Na3 4.1262(8) 2_757 ?
Na2 O15 2.426(2) 2_868 ?
Na2 Na1 3.2502(8) 2_757 ?
Na2 Na2 3.8085(11) 2_868 ?
Na2 Na3 3.8699(8) . ?
Na3 P3 2.8911(6) . ?
Na3 Na4 3.1179(8) . ?
Na3 P2 3.1220(6) . ?
Na3 Na1 4.1261(8) 2_757 ?
Na4 O4 2.3189(9) 1_455 ?
Na4 O4 2.3846(10) 2_757 ?
Na4 Na4 3.2841(10) 2_657 ?
Na4 Na1 3.5833(7) 2_657 ?
Na4 H9 2.6530(5) . ?
Na4 H23 2.62(6) . ?
P2 Na1 3.2757(6) 2_757 ?
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
C1 H1 O9 0.988(17) 2.582(17) 3.3845(15) 138.4(12) 2_657
C1 H2 O9 0.938(16) 2.559(16) 3.4388(15) 156.3(13) 1_454
C2 H4 O3 0.936(18) 2.497(18) 3.2795(15) 141.2(14) 1_655
C3 H5 O2 0.981(17) 2.558(17) 3.2793(14) 130.3(13) 2_757
C3 H5 O6 0.981(17) 2.545(17) 3.3432(15) 138.5(13) 2_757
N1 H7 O2 0.893(16) 2.311(16) 2.8882(12) 122.3(12) 1_655
N1 H7 O4 0.893(16) 2.527(15) 3.0443(12) 117.5(12) .
N1 H7 O8 0.893(16) 2.278(15) 2.8549(12) 122.2(12) 2_757
O10 H9 O3 0.8834(12) 1.8082(9) 2.6899(14) 175.67(10) .
O11 H10 O5 0.7845(11) 1.9622(9) 2.7464(14) 178.16(10) 2_767
O11 H11 O13 0.8683(12) 1.9200(14) 2.7748(19) 167.81(8) .
O13 H12 O17 0.8927(12) 2.609(3) 3.201(3) 124.62(9) .
O13 H12 O17 0.8927(12) 1.933(3) 2.743(3) 150.13(11) 2_768
O13 H13 O3 0.8059(12) 1.9902(9) 2.7795(15) 166.24(10) 2_767
O12 H14 O5 0.8672(13) 1.9786(10) 2.8152(16) 161.73(10) .
O12 H15 O11 0.8195(12) 2.1114(12) 2.9151(17) 166.75(10) 1_655
O14 H16 O1 0.8277(11) 1.94080(10) 2.7666(11) 175.41(8) 1_656
O14 H17 O9 0.8453(11) 1.8247(10) 2.6697(15) 177.88(10) 1_655
O16 H18 O17 0.709(2) 2.257(2) 2.772(3) 130.7(2) 2_768
O16 H19 O9 0.857(2) 1.9411(10) 2.769(3) 162.18(14) .
O17 H20 O15 0.899(3) 2.238(2) 3.031(3) 146.90(18) 1_455
O17 H20 O16 0.899(3) 1.960(2) 2.772(3) 149.49(17) 2_768
O17 H21 O9 0.843(2) 1.8377(9) 2.651(2) 161.8(2) .
O15 H22 O3 0.914(2) 1.9291(9) 2.763(2) 150.81(15) 2_767
O6 H23 O6 0.850(2) 1.666(11) 2.5061(18) 170(6) 2_757
C1 H1 O9 0.988(17) 2.582(17) 3.3845(15) 138.4(12) 2_657
C1 H2 O9 0.938(16) 2.559(16) 3.4388(15) 156.3(13) 1_454
C2 H4 O3 0.936(18) 2.497(18) 3.2795(15) 141.2(14) 1_655
C3 H5 O2 0.981(17) 2.558(17) 3.2793(14) 130.3(13) 2_757
C3 H5 O6 0.981(17) 2.545(17) 3.3432(15) 138.5(13) 2_757
N1 H7 O2 0.893(16) 2.311(16) 2.8882(12) 122.3(12) 1_655
N1 H7 O4 0.893(16) 2.527(15) 3.0443(12) 117.5(12) .
N1 H7 O8 0.893(16) 2.278(15) 2.8549(12) 122.2(12) 2_757
O10 H9 O3 0.8834(12) 1.8082(9) 2.6899(14) 175.67(10) .
O11 H10 O5 0.7845(11) 1.9622(9) 2.7464(14) 178.16(10) 2_767
O11 H11 O13 0.8683(12) 1.9200(14) 2.7748(19) 167.81(8) .
O13 H12 O17 0.8927(12) 2.609(3) 3.201(3) 124.62(9) .
O13 H12 O17 0.8927(12) 1.933(3) 2.743(3) 150.13(11) 2_768
O13 H13 O3 0.8059(12) 1.9902(9) 2.7795(15) 166.24(10) 2_767
O12 H14 O5 0.8672(13) 1.9786(10) 2.8152(16) 161.73(10) .
O12 H15 O11 0.8195(12) 2.1114(12) 2.9151(17) 166.75(10) 1_655
O14 H16 O1 0.8277(11) 1.94080(10) 2.7666(11) 175.41(8) 1_656
O14 H17 O9 0.8453(11) 1.8247(10) 2.6697(15) 177.88(10) 1_655
O16 H18 O17 0.709(2) 2.257(2) 2.772(3) 130.7(2) 2_768
O16 H19 O9 0.857(2) 1.9411(10) 2.769(3) 162.18(14) .
O17 H20 O15 0.899(3) 2.238(2) 3.031(3) 146.90(18) 1_455
O17 H20 O16 0.899(3) 1.960(2) 2.772(3) 149.49(17) 2_768
O17 H21 O9 0.843(2) 1.8377(9) 2.651(2) 161.8(2) .
O15 H22 O3 0.914(2) 1.9291(9) 2.763(2) 150.81(15) 2_767
O6 H23 O6 0.850(2) 1.666(11) 2.5061(18) 170(6) 2_757
