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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/1/56/48/1564829.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_1564829
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            'C3 H33 N Na5 O22 P3'
_chemical_formula_weight         643.16
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2016-01-16T18:16:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.261(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3024(2)
_cell_length_b                   21.5639(7)
_cell_length_c                   18.1608(6)
_cell_measurement_reflns_used    7378
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.988
_cell_measurement_theta_min      3.737
_cell_volume                     2467.53(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0108756
_diffrn_orient_matrix_UB_12      -0.0073675
_diffrn_orient_matrix_UB_13      0.0377986
_diffrn_orient_matrix_UB_21      -0.0713124
_diffrn_orient_matrix_UB_22      -0.0242768
_diffrn_orient_matrix_UB_23      -0.0096599
_diffrn_orient_matrix_UB_31      0.0863915
_diffrn_orient_matrix_UB_32      -0.0209421
_diffrn_orient_matrix_UB_33      -0.0020879
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35238
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.369
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.731
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0394P)²+3.0692P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0
_reflns_number_gt                4486
_reflns_number_total             5031
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            tmp6v4_n1ew
_cod_data_source_block           mgnaatmp
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1564829
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.8724(5) 0.20733(14) 0.23257(17) 0.0197(7) Uani 1 1 d . . . . .
C2 C 0.8522(5) 0.15474(14) 0.11141(17) 0.0183(7) Uani 1 1 d . . . . .
C3 C 0.9373(5) 0.26702(14) 0.11815(17) 0.0184(7) Uani 1 1 d . . . . .
O1 O 1.2100(4) 0.14010(11) 0.26847(13) 0.0243(5) Uani 1 1 d . . . . .
O2 O 0.9588(4) 0.17510(10) 0.36916(12) 0.0213(5) Uani 1 1 d . . . . .
O3 O 0.8601(4) 0.08694(10) 0.28370(13) 0.0247(5) Uani 1 1 d D . . . .
O4 O 1.2262(4) 0.13312(11) 0.05293(13) 0.0263(5) Uani 1 1 d . . . . .
O5 O 0.9489(3) 0.18063(10) -0.03159(12) 0.0204(5) Uani 1 1 d . . . . .
O6 O 0.9088(4) 0.06950(10) 0.01019(12) 0.0240(5) Uani 1 1 d . . . . .
O7 O 1.3309(4) 0.29149(11) 0.16439(13) 0.0268(5) Uani 1 1 d . . . . .
O8 O 1.0399(4) 0.35594(11) 0.22108(12) 0.0247(5) Uani 1 1 d . . . . .
O9 O 1.1302(4) 0.37199(11) 0.08813(13) 0.0257(5) Uani 1 1 d . . . . .
O11 O 0.4308(4) 0.24163(13) 0.02117(15) 0.0292(6) Uani 1 1 d . . . . .
O12 O 0.4182(4) 0.24584(13) 0.31354(15) 0.0289(6) Uani 1 1 d . . . . .
O13 O 0.4597(4) 0.16902(11) 0.45537(15) 0.0282(6) Uani 1 1 d . . . . .
O14 O 0.9484(4) 0.32165(12) 0.36736(15) 0.0292(6) Uani 1 1 d . . . . .
O15 O 1.4309(5) 0.40129(12) 0.34607(15) 0.0322(6) Uani 1 1 d . . . . .
O16 O 1.2427(5) 0.54712(14) 0.33826(17) 0.0435(8) Uani 1 1 d . . . . .
O17 O 1.3765(4) 0.48233(12) 0.18088(17) 0.0379(7) Uani 1 1 d D . . . .
O18 O 1.0102(4) 0.57126(13) 0.14661(16) 0.0340(6) Uani 1 1 d . . . . .
O19 O 0.7679(5) 0.48430(15) 0.02575(18) 0.0398(7) Uani 1 1 d . . . . .
O20 O 0.6838(5) 0.00551(15) 0.18628(17) 0.0499(8) Uani 1 1 d D . . . .
O21 O 0.5265(5) -0.07102(14) 0.04622(18) 0.0419(7) Uani 1 1 d . . . . .
O22 O 0.6159(4) 0.37833(12) 0.21333(16) 0.0350(6) Uani 1 1 d D . . . .
O23 O 0.9492(5) 0.09842(14) 0.49024(18) 0.0398(7) Uani 1 1 d . . . . .
Na1 Na 0.6920(2) 0.24800(6) 0.40878(7) 0.0242(3) Uani 1 1 d . . . . .
Na2 Na 1.1486(3) 0.44929(7) 0.28222(10) 0.0428(4) Uani 1 1 d . . . . .
Na3 Na 1.0940(2) 0.47883(6) 0.08965(8) 0.0323(4) Uani 1 1 d . . . . .
Na4 Na 0.6936(2) 0.25296(6) -0.07274(7) 0.0239(3) Uani 1 1 d . . . . .
Na5 Na 0.9043(3) -0.01714(7) 0.08610(9) 0.0438(4) Uani 1 1 d D . . . .
P1 P 0.98175(13) 0.14707(4) 0.29391(4) 0.01629(18) Uani 1 1 d . . . . .
P2 P 0.99273(13) 0.13344(4) 0.02792(4) 0.01685(19) Uani 1 1 d . . . . .
P3 P 1.12565(13) 0.32680(4) 0.15156(5) 0.01693(19) Uani 1 1 d . . . . .
N1 N 0.9554(4) 0.20568(11) 0.15594(14) 0.0150(5) Uani 1 1 d . . . . .
H1 H 0.7311 0.2055 0.2309 0.036(11) Uiso 1 1 d . . . . .
H2 H 0.9067 0.2479 0.253 0.035(11) Uiso 1 1 d . . . . .
H3 H 0.7252 0.1684 0.102 0.022(9) Uiso 1 1 d . . . . .
H4 H 0.8528 0.1203 0.1461 0.027(10) Uiso 1 1 d . . . . .
H5 H 0.9692 0.2599 0.0691 0.013(8) Uiso 1 1 d . . . . .
H6 H 0.8125 0.2808 0.1204 0.030(11) Uiso 1 1 d . . . . .
H7 H 1.0744 0.1931 0.1604 0.022(10) Uiso 1 1 d . . . . .
H8 H 0.409(8) 0.260(2) 0.059(3) 0.058(3) Uiso 1 1 d . U . . .
H9 H 0.376(8) 0.205(2) 0.034(3) 0.058(3) Uiso 1 1 d . U . . .
H10 H 0.703(8) 0.513(2) 0.026(3) 0.058(3) Uiso 1 1 d . U . . .
H11 H 0.685(8) 0.455(2) 0.017(3) 0.058(3) Uiso 1 1 d . U . . .
H12 H 0.901(8) 0.573(2) 0.166(3) 0.058(3) Uiso 1 1 d . U . . .
H13 H 1.096(8) 0.591(2) 0.175(3) 0.058(3) Uiso 1 1 d . U . . .
H14 H 1.257(8) 0.570(2) 0.305(3) 0.058(3) Uiso 1 1 d . U . . .
H15 H 1.231(7) 0.576(2) 0.377(3) 0.058(3) Uiso 1 1 d . U . . .
H16 H 1.501(8) 0.387(2) 0.308(3) 0.058(3) Uiso 1 1 d . U . . .
H17 H 1.427(8) 0.374(2) 0.377(3) 0.058(3) Uiso 1 1 d . U . . .
H18 H 0.961(8) 0.355(2) 0.390(3) 0.058(3) Uiso 1 1 d . U . . .
H19 H 0.464(8) 0.135(2) 0.4262(19) 0.058(3) Uiso 1 1 d D U . . .
H20 H 0.495(8) 0.156(2) 0.501(2) 0.058(3) Uiso 1 1 d D U . . .
H21 H 0.401(8) 0.266(2) 0.277(3) 0.058(3) Uiso 1 1 d . U . . .
H22 H 0.375(8) 0.212(2) 0.303(3) 0.058(3) Uiso 1 1 d . U . . .
H23 H 0.576(8) -0.088(2) 0.010(3) 0.058(3) Uiso 1 1 d . U . . .
H24 H 0.408(8) -0.068(2) 0.037(3) 0.058(3) Uiso 1 1 d . U . . .
H25 H 1.449(8) 0.5169(10) 0.185(3) 0.058(3) Uiso 1 1 d D U . . .
H26 H 1.451(5) 0.4497(10) 0.185(3) 0.058(3) Uiso 1 1 d D U . . .
H27 H 0.7477(14) 0.3705(16) 0.218(2) 0.058(3) Uiso 1 1 d D U . . .
H28 H 0.538(4) 0.3501(12) 0.194(2) 0.058(3) Uiso 1 1 d D U . . .
H29 H 0.975(8) 0.329(2) 0.324(3) 0.058(3) Uiso 1 1 d . U . . .
H30 H 0.960(8) 0.120(2) 0.451(3) 0.058(3) Uiso 1 1 d . U . . .
H31 H 0.889(8) 0.115(2) 0.523(3) 0.058(3) Uiso 1 1 d . U . . .
H32 H 0.692(5) -0.0303(5) 0.2059(10) 0.058(3) Uiso 1 1 d D U . . .
H33 H 0.730(7) 0.0359(9) 0.2119(16) 0.058(3) Uiso 1 1 d D U . . .
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'
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'
N N 0.0061 0.0033 '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 30 -1 0.0108
0 -30 1 0.0267
-8 -7 -8 0.0472
8 0 -8 0.0317
2 -8 24 0.0741
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 114.4(2) . . ?
N1 C1 H1 109.6(3) . . ?
P1 C1 H1 110.5(3) . . ?
N1 C1 H2 107.3(3) . . ?
P1 C1 H2 109.1(2) . . ?
H1 C1 H2 105.5(3) . . ?
N1 C2 P2 114.7(2) . . ?
N1 C2 H3 104.1(3) . . ?
P2 C2 H3 112.6(3) . . ?
N1 C2 H4 102.3(3) . . ?
P2 C2 H4 110.4(2) . . ?
H3 C2 H4 112.2(3) . . ?
N1 C3 P3 115.2(2) . . ?
N1 C3 H5 106.1(3) . . ?
P3 C3 H5 106.2(2) . . ?
N1 C3 H6 110.7(3) . . ?
P3 C3 H6 109.3(3) . . ?
H5 C3 H6 109.1(3) . . ?
P1 O2 Na4 126.48(13) . 4_666 ?
P1 O2 Na1 127.72(13) . . ?
Na4 O2 Na1 82.77(8) 4_666 . ?
P2 O5 Na4 142.20(14) . . ?
P2 O5 Na1 129.60(13) . 4_665 ?
Na4 O5 Na1 82.68(8) . 4_665 ?
P2 O6 Na5 128.10(14) . . ?
P2 O6 Na5 114.08(13) . 3_755 ?
Na5 O6 Na5 93.81(9) . 3_755 ?
P3 O8 Na2 129.07(14) . . ?
P3 O9 Na3 129.03(14) . . ?
Na4 O11 Na1 79.96(9) . 4_565 ?
Na4 O11 H8 133(4) . . ?
Na1 O11 H8 122(4) 4_565 . ?
Na4 O11 H9 123(3) . . ?
Na1 O11 H9 93(3) 4_565 . ?
H8 O11 H9 99(5) . . ?
Na1 O12 Na4 79.57(9) . 4_566 ?
Na1 O12 H21 132(4) . . ?
Na4 O12 H21 127(4) 4_566 . ?
Na1 O12 H22 115(4) . . ?
Na4 O12 H22 91(4) 4_566 . ?
H21 O12 H22 105(5) . . ?
Na1 O13 Na4 81.85(9) . 4_566 ?
Na1 O13 H19 110(3) . . ?
Na4 O13 H19 118(3) 4_566 . ?
Na1 O13 H20 114(3) . . ?
Na4 O13 H20 125(3) 4_566 . ?
H19 O13 H20 106(3) . . ?
Na1 O14 Na4 81.36(9) . 4_666 ?
Na1 O14 H18 119(4) . . ?
Na4 O14 H18 107(3) 4_666 . ?
Na1 O14 H29 126(3) . . ?
Na4 O14 H29 114(3) 4_666 . ?
H18 O14 H29 106(5) . . ?
Na2 O15 Na5 104.38(12) . 2_755 ?
Na2 O15 H16 99(3) . . ?
Na5 O15 H16 116(3) 2_755 . ?
Na2 O15 H17 129(4) . . ?
Na5 O15 H17 101(4) 2_755 . ?
H16 O15 H17 108(5) . . ?
Na2 O16 Na5 87.78(11) . 2_755 ?
Na2 O16 H14 104(4) . . ?
Na5 O16 H14 124(4) 2_755 . ?
Na2 O16 H15 150(3) . . ?
Na5 O16 H15 92(3) 2_755 . ?
H14 O16 H15 101(5) . . ?
Na3 O17 Na2 94.04(11) . . ?
Na3 O17 H25 117(3) . . ?
Na2 O17 H25 120(3) . . ?
Na3 O17 H26 116(3) . . ?
Na2 O17 H26 92(3) . . ?
H25 O17 H26 114(3) . . ?
Na3 O18 H12 118(4) . . ?
Na3 O18 H13 123(3) . . ?
H12 O18 H13 105(5) . . ?
Na3 O19 Na3 96.74(12) . 3_765 ?
Na3 O19 H10 121(4) . . ?
Na3 O19 H10 87(4) 3_765 . ?
Na3 O19 H11 126(3) . . ?
Na3 O19 H11 109(3) 3_765 . ?
H10 O19 H11 107(5) . . ?
Na5 O20 Na2 125.88(13) . 2_645 ?
Na5 O20 H32 95.8(8) . . ?
Na2 O20 H32 60.7(19) 2_645 . ?
Na5 O20 H33 112(3) . . ?
Na2 O20 H33 122(3) 2_645 . ?
H32 O20 H33 116.8(4) . . ?
Na5 O21 H23 93(4) . . ?
Na5 O21 H24 149(4) . . ?
H23 O21 H24 105(5) . . ?
H27 O22 H28 117.0(4) . . ?
H30 O23 H31 115(5) . . ?
O14 Na1 O13 174.97(11) . . ?
O14 Na1 O12 105.29(11) . . ?
O13 Na1 O12 78.94(10) . . ?
O14 Na1 O2 81.93(9) . . ?
O13 Na1 O2 94.39(9) . . ?
O12 Na1 O2 105.32(10) . . ?
O14 Na1 O5 98.94(9) . 4_566 ?
O13 Na1 O5 84.14(9) . 4_566 ?
O12 Na1 O5 83.38(9) . 4_566 ?
O2 Na1 O5 170.78(10) . 4_566 ?
O14 Na1 O11 78.50(10) . 4_666 ?
O13 Na1 O11 97.75(10) . 4_666 ?
O12 Na1 O11 170.43(11) . 4_666 ?
O2 Na1 O11 83.80(9) . 4_666 ?
O5 Na1 O11 87.37(9) 4_566 4_666 ?
O14 Na1 Na4 135.59(9) . 4_566 ?
O13 Na1 Na4 49.22(7) . 4_566 ?
O12 Na1 Na4 51.79(7) . 4_566 ?
O2 Na1 Na4 136.38(8) . 4_566 ?
O5 Na1 Na4 47.43(6) 4_566 4_566 ?
O11 Na1 Na4 119.41(8) 4_666 4_566 ?
O14 Na1 Na4 50.25(7) . 4_666 ?
O13 Na1 Na4 124.73(8) . 4_666 ?
O12 Na1 Na4 140.34(9) . 4_666 ?
O2 Na1 Na4 47.97(6) . 4_666 ?
O5 Na1 Na4 126.21(7) 4_566 4_666 ?
O11 Na1 Na4 48.59(7) 4_666 4_666 ?
Na4 Na1 Na4 167.82(7) 4_566 4_666 ?
O15 Na2 O8 93.69(11) . . ?
O15 Na2 O16 90.04(12) . . ?
O8 Na2 O16 176.18(13) . . ?
O15 Na2 O17 92.78(11) . . ?
O8 Na2 O17 93.57(10) . . ?
O16 Na2 O17 85.43(11) . . ?
O15 Na2 O20 137.10(12) . 2_655 ?
O8 Na2 O20 106.38(12) . 2_655 ?
O16 Na2 O20 71.23(12) . 2_655 ?
O17 Na2 O20 122.43(11) . 2_655 ?
O15 Na2 Na3 128.34(10) . . ?
O8 Na2 Na3 71.00(7) . . ?
O16 Na2 Na3 105.98(9) . . ?
O17 Na2 Na3 42.34(7) . . ?
O20 Na2 Na3 94.29(9) 2_655 . ?
O15 Na2 Na5 38.10(7) . 2_755 ?
O8 Na2 Na5 131.77(9) . 2_755 ?
O16 Na2 Na5 51.95(9) . 2_755 ?
O17 Na2 Na5 88.74(8) . 2_755 ?
O20 Na2 Na5 112.64(10) 2_655 2_755 ?
Na3 Na2 Na5 130.56(6) . 2_755 ?
O15 Na2 H16 19.3(11) . . ?
O8 Na2 H16 83.4(11) . . ?
O16 Na2 H16 99.9(11) . . ?
O17 Na2 H16 77.2(11) . . ?
O20 Na2 H16 156.4(11) 2_655 . ?
Na3 Na2 H16 109.3(11) . . ?
Na5 Na2 H16 50.2(11) 2_755 . ?
O15 Na2 H26 77.3(7) . . ?
O8 Na2 H26 84.0(8) . . ?
O16 Na2 H26 96.1(8) . . ?
O17 Na2 H26 18.9(3) . . ?
O20 Na2 H26 141.0(4) 2_655 . ?
Na3 Na2 H26 52.8(8) . . ?
Na5 Na2 H26 83.2(9) 2_755 . ?
H16 Na2 H26 60.0(13) . . ?
O18 Na3 O9 152.46(12) . . ?
O18 Na3 O19 88.37(12) . . ?
O9 Na3 O19 97.46(11) . . ?
O18 Na3 O17 80.67(11) . . ?
O9 Na3 O17 88.16(10) . . ?
O19 Na3 O17 165.46(13) . . ?
O18 Na3 O19 101.20(12) . 3_765 ?
O9 Na3 O19 106.21(11) . 3_765 ?
O19 Na3 O19 83.26(12) . 3_765 ?
O17 Na3 O19 108.14(12) . 3_765 ?
O18 Na3 Na3 96.51(9) . 3_765 ?
O9 Na3 Na3 105.97(9) . 3_765 ?
O19 Na3 Na3 42.49(9) . 3_765 ?
O17 Na3 Na3 148.02(11) . 3_765 ?
O19 Na3 Na3 40.77(8) 3_765 3_765 ?
O18 Na3 Na2 74.53(9) . . ?
O9 Na3 Na2 80.01(7) . . ?
O19 Na3 Na2 124.06(10) . . ?
O17 Na3 Na2 43.62(8) . . ?
O19 Na3 Na2 151.58(9) 3_765 . ?
Na3 Na3 Na2 165.11(8) 3_765 . ?
O5 Na4 O2 171.86(10) . 4_565 ?
O5 Na4 O11 100.58(10) . . ?
O2 Na4 O11 87.10(9) 4_565 . ?
O5 Na4 O13 85.87(9) . 4_665 ?
O2 Na4 O13 93.54(9) 4_565 4_665 ?
O11 Na4 O13 113.82(11) . 4_665 ?
O5 Na4 O14 97.19(9) . 4_565 ?
O2 Na4 O14 81.49(9) 4_565 4_565 ?
O11 Na4 O14 79.21(10) . 4_565 ?
O13 Na4 O14 165.95(11) 4_665 4_565 ?
O5 Na4 O12 82.82(9) . 4_665 ?
O2 Na4 O12 89.15(9) 4_565 4_665 ?
O11 Na4 O12 169.16(11) . 4_665 ?
O13 Na4 O12 76.56(10) 4_665 4_665 ?
O14 Na4 O12 90.18(10) 4_565 4_665 ?
O5 Na4 Na1 49.89(6) . 4_665 ?
O2 Na4 Na1 124.55(8) 4_565 4_665 ?
O11 Na4 Na1 140.48(9) . 4_665 ?
O13 Na4 Na1 48.93(7) 4_665 4_665 ?
O14 Na4 Na1 124.21(8) 4_565 4_665 ?
O12 Na4 Na1 48.64(7) 4_665 4_665 ?
O5 Na4 Na1 134.66(8) . 4_565 ?
O2 Na4 Na1 49.26(6) 4_565 4_565 ?
O11 Na4 Na1 51.45(7) . 4_565 ?
O13 Na4 Na1 135.30(8) 4_665 4_565 ?
O14 Na4 Na1 48.39(7) 4_565 4_565 ?
O12 Na4 Na1 119.22(8) 4_665 4_565 ?
Na1 Na4 Na1 167.82(7) 4_665 4_565 ?
O6 Na5 O20 107.79(12) . . ?
O6 Na5 O15 153.29(13) . 2_745 ?
O20 Na5 O15 90.68(12) . 2_745 ?
O6 Na5 O6 86.19(9) . 3_755 ?
O20 Na5 O6 163.70(12) . 3_755 ?
O15 Na5 O6 79.29(10) 2_745 3_755 ?
O6 Na5 O21 101.92(11) . . ?
O20 Na5 O21 76.60(11) . . ?
O15 Na5 O21 101.03(11) 2_745 . ?
O6 Na5 O21 92.61(11) 3_755 . ?
O6 Na5 O16 83.05(10) . 2_745 ?
O20 Na5 O16 89.70(10) . 2_745 ?
O15 Na5 O16 77.79(10) 2_745 2_745 ?
O6 Na5 O16 100.54(10) 3_755 2_745 ?
O21 Na5 O16 166.26(11) . 2_745 ?
O6 Na5 P2 103.41(8) . 3_755 ?
O20 Na5 P2 139.55(10) . 3_755 ?
O15 Na5 P2 71.04(8) 2_745 3_755 ?
O6 Na5 P2 24.48(6) 3_755 3_755 ?
O21 Na5 P2 72.25(8) . 3_755 ?
O16 Na5 P2 119.40(8) 2_745 3_755 ?
O6 Na5 Na5 44.10(6) . 3_755 ?
O20 Na5 Na5 151.00(12) . 3_755 ?
O15 Na5 Na5 118.07(10) 2_745 3_755 ?
O6 Na5 Na5 42.10(6) 3_755 3_755 ?
O21 Na5 Na5 99.82(10) . 3_755 ?
O16 Na5 Na5 92.66(9) 2_745 3_755 ?
P2 Na5 Na5 61.39(5) 3_755 3_755 ?
O6 Na5 Na2 121.22(9) . 2_745 ?
O20 Na5 Na2 89.74(10) . 2_745 ?
O15 Na5 Na2 37.52(8) 2_745 2_745 ?
O6 Na5 Na2 89.99(8) 3_755 2_745 ?
O21 Na5 Na2 136.86(9) . 2_745 ?
O16 Na5 Na2 40.27(6) 2_745 2_745 ?
P2 Na5 Na2 95.62(5) 3_755 2_745 ?
Na5 Na5 Na2 110.37(8) 3_755 2_745 ?
O6 Na5 H32 126.79(18) . . ?
O20 Na5 H32 19.05(12) . . ?
O15 Na5 H32 73.2(4) 2_745 . ?
O6 Na5 H32 145.7(2) 3_755 . ?
O21 Na5 H32 73.4(7) . . ?
O16 Na5 H32 93.3(7) 2_745 . ?
P2 Na5 H32 123.5(4) 3_755 . ?
Na5 Na5 H32 168.2(5) 3_755 . ?
Na2 Na5 H32 80.6(7) 2_745 . ?
O2 P1 O3 113.35(13) . . ?
O2 P1 O1 115.11(13) . . ?
O3 P1 O1 110.86(13) . . ?
O2 P1 C1 102.97(13) . . ?
O3 P1 C1 110.43(14) . . ?
O1 P1 C1 103.26(14) . . ?
O5 P2 O6 113.98(13) . . ?
O5 P2 O4 112.09(13) . . ?
O6 P2 O4 112.93(14) . . ?
O5 P2 C2 109.89(14) . . ?
O6 P2 C2 103.43(14) . . ?
O4 P2 C2 103.58(14) . . ?
O5 P2 Na5 95.62(9) . 3_755 ?
O6 P2 Na5 41.44(9) . 3_755 ?
O4 P2 Na5 88.96(10) . 3_755 ?
C2 P2 Na5 144.04(11) . 3_755 ?
O9 P3 O7 114.29(14) . . ?
O9 P3 O8 112.33(14) . . ?
O7 P3 O8 113.45(14) . . ?
O9 P3 C3 102.88(14) . . ?
O7 P3 C3 103.92(14) . . ?
O8 P3 C3 108.90(14) . . ?
C3 N1 C1 112.4(2) . . ?
C3 N1 C2 111.9(2) . . ?
C1 N1 C2 111.2(2) . . ?
C3 N1 H7 114.1(3) . . ?
C1 N1 H7 105.1(3) . . ?
C2 N1 H7 101.6(2) . . ?
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 1.498(4) . ?
C1 P1 1.836(3) . ?
C1 H1 0.892(3) . ?
C1 H2 0.972(3) . ?
C2 N1 1.503(4) . ?
C2 P2 1.831(3) . ?
C2 H3 0.867(3) . ?
C2 H4 0.974(3) . ?
C3 N1 1.494(4) . ?
C3 P3 1.846(3) . ?
C3 H5 0.930(3) . ?
C3 H6 0.843(3) . ?
O1 P1 1.528(2) . ?
O2 P1 1.504(2) . ?
O2 Na4 2.375(3) 4_666 ?
O2 Na1 2.423(3) . ?
O3 P1 1.516(2) . ?
O4 P2 1.530(2) . ?
O5 P2 1.506(2) . ?
O5 Na4 2.351(2) . ?
O5 Na1 2.442(2) 4_665 ?
O6 P2 1.509(2) . ?
O6 Na5 2.322(3) . ?
O6 Na5 2.411(3) 3_755 ?
O7 P3 1.515(2) . ?
O8 P3 1.520(2) . ?
O8 Na2 2.392(3) . ?
O9 P3 1.509(2) . ?
O9 Na3 2.315(3) . ?
O11 Na4 2.416(3) . ?
O11 Na1 2.519(3) 4_565 ?
O11 H8 0.81(5) . ?
O11 H9 0.89(5) . ?
O12 Na1 2.416(3) . ?
O12 Na4 2.530(3) 4_566 ?
O12 H21 0.81(5) . ?
O12 H22 0.80(5) . ?
O13 Na1 2.411(3) . ?
O13 Na4 2.422(3) 4_566 ?
O13 H19 0.91(4) . ?
O13 H20 0.91(4) . ?
O14 Na1 2.399(3) . ?
O14 Na4 2.467(3) 4_666 ?
O14 H18 0.82(5) . ?
O14 H29 0.83(5) . ?
O15 Na2 2.343(3) . ?
O15 Na5 2.374(3) 2_755 ?
O15 H16 0.88(5) . ?
O15 H17 0.82(5) . ?
O16 Na2 2.411(3) . ?
O16 Na5 2.936(4) 2_755 ?
O16 H14 0.78(5) . ?
O16 H15 0.95(5) . ?
O17 Na3 2.406(3) . ?
O17 Na2 2.465(4) . ?
O17 H25 0.88(3) . ?
O17 H26 0.850(2) . ?
O18 Na3 2.312(3) . ?
O18 H12 0.78(5) . ?
O18 H13 0.85(5) . ?
O19 Na3 2.341(3) . ?
O19 Na3 2.421(4) 3_765 ?
O19 H10 0.75(5) . ?
O19 H11 0.83(5) . ?
O20 Na5 2.365(3) . ?
O20 Na2 2.497(3) 2_645 ?
O20 H32 0.851(2) . ?
O20 H33 0.851(2) . ?
O21 Na5 2.733(4) . ?
O21 H23 0.81(5) . ?
O21 H24 0.77(5) . ?
O22 H27 0.850(2) . ?
O22 H28 0.850(2) . ?
O23 H30 0.85(5) . ?
O23 H31 0.80(5) . ?
Na1 O5 2.442(2) 4_566 ?
Na1 O11 2.519(3) 4_666 ?
Na1 Na4 3.1661(18) 4_566 ?
Na1 Na4 3.1720(17) 4_666 ?
Na2 O20 2.497(3) 2_655 ?
Na2 Na3 3.564(2) . ?
Na2 Na5 3.726(2) 2_755 ?
Na2 H16 2.63(5) . ?
Na2 H26 2.63(4) . ?
Na3 O19 2.421(4) 3_765 ?
Na3 Na3 3.560(3) 3_765 ?
Na4 O2 2.375(3) 4_565 ?
Na4 O13 2.422(3) 4_665 ?
Na4 O14 2.467(3) 4_565 ?
Na4 O12 2.530(3) 4_665 ?
Na4 Na1 3.1661(17) 4_665 ?
Na4 Na1 3.1721(17) 4_565 ?
Na5 O15 2.374(3) 2_745 ?
Na5 O6 2.411(3) 3_755 ?
Na5 O16 2.937(4) 2_745 ?
Na5 P2 3.3252(17) 3_755 ?
Na5 Na5 3.457(3) 3_755 ?
Na5 Na2 3.726(2) 2_745 ?
Na5 H32 2.593(10) . ?
P2 Na5 3.3253(17) 3_755 ?
N1 H7 0.800(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
C1 H1 O12 0.892(3) 2.651(3) 3.351(4) 136.1(2) .
C1 H2 O8 0.972(3) 2.548(2) 3.382(4) 143.82(19) .
C1 H2 O14 0.972(3) 2.625(3) 3.500(4) 149.84(19) .
C2 H4 O3 0.974(3) 2.600(2) 3.453(4) 146.33(19) .
C3 H5 O5 0.930(3) 2.504(2) 3.298(4) 143.5(2) .
C3 H5 O13 0.930(3) 2.573(3) 3.268(4) 131.9(2) 4_665
N1 H7 O1 0.800(2) 2.412(2) 2.934(3) 123.87(18) .
N1 H7 O4 0.800(2) 2.546(2) 3.000(3) 117.50(18) .
O11 H8 O7 0.81(5) 2.10(5) 2.896(4) 168(5) 1_455
O11 H9 O4 0.89(5) 1.86(5) 2.739(4) 172(5) 1_455
O19 H10 O23 0.75(5) 2.09(5) 2.828(4) 170(6) 2_655
O19 H11 O23 0.83(5) 1.93(5) 2.752(4) 167(5) 4_565
O18 H12 O3 0.78(5) 1.92(5) 2.700(4) 174(5) 2_655
O18 H13 O1 0.85(5) 1.90(5) 2.752(4) 174(5) 2_755
O16 H14 O1 0.78(5) 2.04(5) 2.809(4) 170(5) 2_755
O16 H15 O4 0.95(5) 1.78(5) 2.714(4) 167(4) 2_755
O15 H16 O22 0.88(5) 1.89(5) 2.746(4) 162(5) 1_655
O15 H17 O5 0.82(5) 2.03(5) 2.839(4) 168(5) 4_666
O14 H18 O21 0.82(5) 1.98(5) 2.799(4) 173(5) 2_655
O13 H19 O18 0.91(4) 1.91(4) 2.815(4) 171(4) 2_645
O13 H20 O9 0.91(4) 1.87(4) 2.763(3) 167(4) 4_566
O12 H21 O7 0.81(5) 2.14(5) 2.923(4) 161(5) 1_455
O12 H22 O1 0.80(5) 1.96(5) 2.747(4) 167(5) 1_455
O21 H23 O4 0.81(5) 1.97(5) 2.755(4) 161(5) 3_755
O21 H24 O6 0.77(5) 2.15(5) 2.907(4) 167(5) 3_655
O17 H25 O3 0.88(3) 2.01(4) 2.866(3) 167(4) 2_755
O17 H26 O22 0.850(2) 1.920(10) 2.759(4) 169(5) 1_655
O22 H27 O8 0.850(2) 1.868(5) 2.716(3) 176(5) .
O22 H28 O7 0.850(2) 1.888(7) 2.730(3) 170(4) 1_455
O14 H29 O8 0.83(5) 2.00(5) 2.829(4) 174(5) .
O23 H30 O2 0.85(5) 1.90(5) 2.753(4) 174(5) .
O23 H31 O9 0.80(5) 2.06(5) 2.787(4) 153(5) 4_566
O20 H33 O3 0.851(2) 1.880(9) 2.713(4) 166(3) .
