#------------------------------------------------------------------------------
#$Date: 2019-11-14 14:17:55 +0200 (Thu, 14 Nov 2019) $
#$Revision: 227792 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/50/7235082.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_7235082
loop_
_publ_author_name
'Salcedo, Inés R.'
'Colodrero, Rosario M. P.'
'Bazaga-García, Montse'
'Vasileiou, Antonia'
'Papadaki, Maria'
'Olivera-Pastor, Pascual'
'Infantes-Molina, Antonia'
'Losilla, Enrique R.'
'Mezei, Gellert'
'Cabeza, Aurelio'
'Demadis, Konstantinos D.'
_publ_section_title
;
 From light to heavy alkali metal tetraphosphonates (M = Li, Na, K, Rb,
 Cs): cation size-induced structural diversity and water-facilitated
 proton conductivity
;
_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              7648
_journal_paper_doi               10.1039/C8CE01351A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C10 H48 N2 Na2 O23 P4'
_chemical_formula_weight         734.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-11-09 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                97.3780(10)
_cell_angle_beta                 94.7920(10)
_cell_angle_gamma                101.7050(10)
_cell_formula_units_Z            2
_cell_length_a                   7.66820(10)
_cell_length_b                   11.53350(10)
_cell_length_c                   18.0768(2)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.29
_cell_volume                     1542.61(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74089
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.028
_diffrn_reflns_theta_min         1.824
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9784
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0404P)²+1.1108P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7728
_reflns_number_total             9784
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce01351a2.cif
_cod_data_source_block           Na-HDTMP
_cod_database_code               7235082
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.854
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_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
Na1 Na 0.0000 0.0000 1.0000 0.0162(2) Uani 1 2 d S . P
Na2 Na -0.36336(8) -0.03213(6) 1.07122(4) 0.01232(13) Uani 1 1 d . . .
Na3 Na 1.0000 0.5000 1.0000 0.01305(18) Uani 1 2 d S . P
P1 P 0.56533(5) 0.43674(3) 0.20636(2) 0.00898(8) Uani 1 1 d . . .
P2 P 0.14120(5) 0.60557(3) 0.33826(2) 0.00876(8) Uani 1 1 d . . .
P3 P -0.05114(5) 0.04699(3) 0.81549(2) 0.00835(8) Uani 1 1 d . . .
P4 P 0.35806(5) -0.10337(3) 0.65714(2) 0.00837(8) Uani 1 1 d . . .
O1 O 0.67237(15) 0.35278(10) 0.17087(6) 0.0113(2) Uani 1 1 d . . .
O2 O 0.43714(15) 0.48014(11) 0.15482(7) 0.0143(2) Uani 1 1 d . . .
O3 O 0.69031(15) 0.54642(11) 0.25723(7) 0.0154(2) Uani 1 1 d D . .
H3O H 0.793(2) 0.544(2) 0.2587(13) 0.023 Uiso 1 1 d D U .
O4 O 0.01769(15) 0.55288(10) 0.26725(6) 0.0134(2) Uani 1 1 d . . .
O5 O 0.22646(16) 0.73925(10) 0.33473(7) 0.0128(2) Uani 1 1 d D . .
H5O H 0.241(3) 0.7877(18) 0.3722(10) 0.019 Uiso 1 1 d D U .
O6 O 0.06662(15) 0.58827(10) 0.41107(7) 0.0134(2) Uani 1 1 d . . .
O7 O 0.07278(15) -0.00296(10) 0.86523(6) 0.0124(2) Uani 1 1 d . . .
O8 O -0.17472(15) -0.06180(10) 0.76139(7) 0.0122(2) Uani 1 1 d D . .
H8O H -0.271(2) -0.052(2) 0.7462(12) 0.018 Uiso 1 1 d D U .
O9 O -0.15933(15) 0.12824(10) 0.85249(6) 0.0118(2) Uani 1 1 d . . .
O10 O 0.50192(14) -0.05571(10) 0.72189(6) 0.0127(2) Uani 1 1 d . . .
O11 O 0.27482(15) -0.23837(10) 0.65882(7) 0.0125(2) Uani 1 1 d D . .
H11O H 0.258(3) -0.2842(18) 0.6205(10) 0.019 Uiso 1 1 d D U .
O12 O 0.40766(15) -0.08058(10) 0.58137(6) 0.0132(2) Uani 1 1 d . . .
O13 O 0.26233(16) 0.14485(11) 1.02851(7) 0.0144(2) Uani 1 1 d D . .
H13A H 0.321(3) 0.136(2) 1.0655(10) 0.022 Uiso 1 1 d D U .
H13B H 0.246(3) 0.2140(15) 1.0339(13) 0.022 Uiso 1 1 d D U .
O14 O -0.27810(19) 0.10979(11) 0.98941(7) 0.0197(3) Uani 1 1 d D . .
H14A H -0.249(3) 0.111(2) 0.9468(10) 0.030 Uiso 1 1 d D U .
H14B H -0.272(3) 0.1808(15) 1.0045(13) 0.030 Uiso 1 1 d D U .
O15 O -0.48060(15) -0.15581(11) 1.15855(7) 0.0129(2) Uani 1 1 d D . .
H15A H -0.475(3) -0.2191(15) 1.1373(12) 0.019 Uiso 1 1 d D U .
H15B H -0.583(2) -0.157(2) 1.1646(12) 0.019 Uiso 1 1 d D U .
O16 O 0.72902(17) 0.35786(11) 1.02285(7) 0.0164(2) Uani 1 1 d D . .
H16A H 0.712(3) 0.357(2) 1.0661(9) 0.025 Uiso 1 1 d D U .
H16B H 0.635(2) 0.363(2) 0.9990(12) 0.025 Uiso 1 1 d D U .
O17 O 1.00987(19) 0.37995(12) 0.88274(7) 0.0208(3) Uani 1 1 d D . .
H17A H 0.950(3) 0.3118(16) 0.8761(14) 0.031 Uiso 1 1 d D U .
H17B H 0.984(3) 0.396(2) 0.8403(10) 0.031 Uiso 1 1 d D U .
O18 O 0.84162(17) 0.63592(11) 0.94538(7) 0.0157(2) Uani 1 1 d D . .
H18A H 0.758(3) 0.5978(19) 0.9167(12) 0.024 Uiso 1 1 d D U .
H18B H 0.909(3) 0.661(2) 0.9146(11) 0.024 Uiso 1 1 d D U .
O19 O 0.00404(16) 0.72312(11) 0.82346(7) 0.0157(2) Uani 1 1 d D . .
H19A H 0.094(2) 0.701(2) 0.8160(13) 0.024 Uiso 1 1 d D U .
H19B H 0.028(3) 0.7944(14) 0.8328(13) 0.024 Uiso 1 1 d D U .
O20 O 0.20539(17) 0.58694(11) 0.55368(7) 0.0162(2) Uani 1 1 d D . .
H20A H 0.136(3) 0.5322(18) 0.5655(13) 0.024 Uiso 1 1 d D U .
H20B H 0.173(3) 0.595(2) 0.5108(10) 0.024 Uiso 1 1 d D U .
O21 O 0.28898(16) 0.91717(11) 0.43714(7) 0.0159(2) Uani 1 1 d D . .
H21A H 0.312(3) 0.907(2) 0.4809(10) 0.024 Uiso 1 1 d D U .
H21B H 0.372(3) 0.9678(18) 0.4290(13) 0.024 Uiso 1 1 d D U .
O22 O 0.58032(17) 0.64441(11) 0.07457(8) 0.0177(2) Uani 1 1 d D . .
H22A H 0.684(2) 0.641(2) 0.0667(13) 0.027 Uiso 1 1 d D U .
H22B H 0.548(3) 0.5897(18) 0.0990(12) 0.027 Uiso 1 1 d D U .
O23 O -0.47485(16) 0.11764(11) 1.13699(7) 0.0136(2) Uani 1 1 d D . .
H23A H -0.480(3) 0.100(2) 1.1798(9) 0.020 Uiso 1 1 d D U .
H23B H -0.423(3) 0.1873(15) 1.1457(12) 0.020 Uiso 1 1 d D U .
N1 N 0.27878(17) 0.40608(11) 0.29525(7) 0.0088(2) Uani 1 1 d D . .
H1 H 0.206(2) 0.3992(19) 0.2560(10) 0.013 Uiso 1 1 d D U .
N2 N 0.22400(17) 0.08946(11) 0.71926(7) 0.0083(2) Uani 1 1 d D . .
H2 H 0.303(2) 0.0936(18) 0.7557(10) 0.012 Uiso 1 1 d D U .
C1 C 0.4325(2) 0.35490(14) 0.26959(9) 0.0121(3) Uani 1 1 d . . .
H1A H 0.3854 0.2735 0.2447 0.015 Uiso 1 1 calc R U .
H1B H 0.5115 0.3509 0.3136 0.015 Uiso 1 1 calc R U .
C2 C 0.33294(19) 0.53642(13) 0.32708(9) 0.0100(3) Uani 1 1 d . . .
H2A H 0.4088 0.5781 0.2942 0.012 Uiso 1 1 calc R U .
H2B H 0.4027 0.5453 0.3756 0.012 Uiso 1 1 calc R U .
C3 C 0.0756(2) 0.13693(14) 0.75345(9) 0.0101(3) Uani 1 1 d . . .
H3A H -0.0082 0.1475 0.7129 0.012 Uiso 1 1 calc R U .
H3B H 0.1269 0.2156 0.7817 0.012 Uiso 1 1 calc R U .
C4 C 0.17010(19) -0.03893(13) 0.68389(9) 0.0095(3) Uani 1 1 d . . .
H4A H 0.0862 -0.0454 0.6396 0.011 Uiso 1 1 calc R U .
H4B H 0.1086 -0.0852 0.7188 0.011 Uiso 1 1 calc R U .
C5 C 0.1816(2) 0.32945(13) 0.34776(8) 0.0097(3) Uani 1 1 d . . .
H5A H 0.1551 0.2464 0.3243 0.012 Uiso 1 1 calc R U .
H5B H 0.0683 0.3523 0.3545 0.012 Uiso 1 1 calc R U .
C6 C 0.2857(2) 0.33953(14) 0.42452(9) 0.0118(3) Uani 1 1 d . . .
H6A H 0.2937 0.4185 0.4524 0.014 Uiso 1 1 calc R U .
H6B H 0.4065 0.3294 0.4185 0.014 Uiso 1 1 calc R U .
C7 C 0.1932(2) 0.24421(14) 0.46839(9) 0.0125(3) Uani 1 1 d . . .
H7A H 0.0707 0.2523 0.4722 0.015 Uiso 1 1 calc R U .
H7B H 0.1896 0.1654 0.4412 0.015 Uiso 1 1 calc R U .
C8 C 0.2895(2) 0.25501(14) 0.54673(9) 0.0120(3) Uani 1 1 d . . .
H8A H 0.2927 0.3338 0.5738 0.014 Uiso 1 1 calc R U .
H8B H 0.4122 0.2475 0.5427 0.014 Uiso 1 1 calc R U .
C9 C 0.1999(2) 0.16032(14) 0.59137(9) 0.0113(3) Uani 1 1 d . . .
H9A H 0.0802 0.1711 0.5991 0.014 Uiso 1 1 calc R U .
H9B H 0.1897 0.0812 0.5634 0.014 Uiso 1 1 calc R U .
C10 C 0.30998(19) 0.17092(13) 0.66676(8) 0.0093(3) Uani 1 1 d . . .
H10A H 0.4255 0.1530 0.6581 0.011 Uiso 1 1 calc R U .
H10B H 0.3314 0.2532 0.6913 0.011 Uiso 1 1 calc R 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 0.0000 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'
Na Na 0.0362 0.0249 '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'
P P 0.1023 0.0942 '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
O13 Na1 O13 180.0 . 2_557
O13 Na1 O7 95.32(4) . 2_557
O13 Na1 O7 84.68(4) 2_557 2_557
O13 Na1 O7 84.68(4) . .
O13 Na1 O7 95.32(4) 2_557 .
O7 Na1 O7 180.0 2_557 .
O13 Na1 O14 108.56(4) . .
O13 Na1 O14 71.44(4) 2_557 .
O7 Na1 O14 81.99(4) 2_557 .
O7 Na1 O14 98.01(4) . .
O13 Na1 O14 71.44(4) . 2_557
O13 Na1 O14 108.56(4) 2_557 2_557
O7 Na1 O14 98.01(4) 2_557 2_557
O7 Na1 O14 81.99(4) . 2_557
O14 Na1 O14 180.00(3) . 2_557
O13 Na1 Na2 48.47(3) . 2_557
O13 Na1 Na2 131.53(3) 2_557 2_557
O7 Na1 Na2 132.51(3) 2_557 2_557
O7 Na1 Na2 47.49(3) . 2_557
O14 Na1 Na2 132.73(3) . 2_557
O14 Na1 Na2 47.27(3) 2_557 2_557
O13 Na1 Na2 131.52(3) . .
O13 Na1 Na2 48.48(3) 2_557 .
O7 Na1 Na2 47.49(3) 2_557 .
O7 Na1 Na2 132.51(3) . .
O14 Na1 Na2 47.27(3) . .
O14 Na1 Na2 132.73(3) 2_557 .
Na2 Na1 Na2 180.0 2_557 .
O13 Na1 P3 93.12(3) . .
O13 Na1 P3 86.88(3) 2_557 .
O7 Na1 P3 156.70(3) 2_557 .
O7 Na1 P3 23.30(3) . .
O14 Na1 P3 74.73(3) . .
O14 Na1 P3 105.27(3) 2_557 .
Na2 Na1 P3 67.722(13) 2_557 .
Na2 Na1 P3 112.279(13) . .
O13 Na1 P3 86.88(3) . 2_557
O13 Na1 P3 93.12(3) 2_557 2_557
O7 Na1 P3 23.30(3) 2_557 2_557
O7 Na1 P3 156.70(3) . 2_557
O14 Na1 P3 105.27(3) . 2_557
O14 Na1 P3 74.73(3) 2_557 2_557
Na2 Na1 P3 112.278(13) 2_557 2_557
Na2 Na1 P3 67.721(13) . 2_557
P3 Na1 P3 180.000(13) . 2_557
O23 Na2 O7 100.64(5) . 2_557
O23 Na2 O13 160.36(5) . 2_557
O7 Na2 O13 87.94(5) 2_557 2_557
O23 Na2 O15 86.67(5) . .
O7 Na2 O15 91.31(4) 2_557 .
O13 Na2 O15 110.96(5) 2_557 .
O23 Na2 O14 85.07(5) . .
O7 Na2 O14 93.33(5) 2_557 .
O13 Na2 O14 76.75(5) 2_557 .
O15 Na2 O14 171.16(5) . .
O23 Na2 O14 82.16(4) . 2_457
O7 Na2 O14 169.31(5) 2_557 2_457
O13 Na2 O14 92.67(5) 2_557 2_457
O15 Na2 O14 78.50(4) . 2_457
O14 Na2 O14 97.19(5) . 2_457
O23 Na2 Na1 126.46(4) . .
O7 Na2 Na1 52.79(3) 2_557 .
O13 Na2 Na1 47.12(3) 2_557 .
O15 Na2 Na1 131.81(4) . .
O14 Na2 Na1 56.54(4) . .
O14 Na2 Na1 133.19(4) 2_457 .
O23 Na2 Na2 80.19(4) . 2_457
O7 Na2 Na2 147.13(5) 2_557 2_457
O13 Na2 Na2 83.07(4) 2_557 2_457
O15 Na2 Na2 121.43(4) . 2_457
O14 Na2 Na2 53.84(4) . 2_457
O14 Na2 Na2 43.35(3) 2_457 2_457
Na1 Na2 Na2 100.11(3) . 2_457
O23 Na2 H15A 103.4(4) . .
O7 Na2 H15A 92.2(5) 2_557 .
O13 Na2 H15A 93.7(4) 2_557 .
O15 Na2 H15A 17.3(4) . .
O14 Na2 H15A 168.8(4) . .
O14 Na2 H15A 77.1(5) 2_457 .
Na1 Na2 H15A 120.8(4) . .
Na2 Na2 H15A 119.8(5) 2_457 .
O23 Na2 H23A 17.5(4) . .
O7 Na2 H23A 93.1(5) 2_557 .
O13 Na2 H23A 177.8(4) 2_557 .
O15 Na2 H23A 70.9(4) . .
O14 Na2 H23A 101.3(4) . .
O14 Na2 H23A 86.6(5) 2_457 .
Na1 Na2 H23A 132.5(5) . .
Na2 Na2 H23A 95.0(4) 2_457 .
H15A Na2 H23A 88.1(6) . .
O17 Na3 O17 180.00(6) . 2_767
O17 Na3 O18 94.87(5) . .
O17 Na3 O18 85.13(5) 2_767 .
O17 Na3 O18 85.13(5) . 2_767
O17 Na3 O18 94.87(5) 2_767 2_767
O18 Na3 O18 180.00(3) . 2_767
O17 Na3 O16 90.63(4) . .
O17 Na3 O16 89.37(4) 2_767 .
O18 Na3 O16 95.91(4) . .
O18 Na3 O16 84.09(4) 2_767 .
O17 Na3 O16 89.37(4) . 2_767
O17 Na3 O16 90.63(4) 2_767 2_767
O18 Na3 O16 84.09(4) . 2_767
O18 Na3 O16 95.91(4) 2_767 2_767
O16 Na3 O16 180.0 . 2_767
O2 P1 O1 117.18(7) . .
O2 P1 O3 109.19(7) . .
O1 P1 O3 111.05(6) . .
O2 P1 C1 106.88(7) . .
O1 P1 C1 106.21(7) . .
O3 P1 C1 105.57(7) . .
O6 P2 O4 116.89(7) . .
O6 P2 O5 112.58(7) . .
O4 P2 O5 109.43(7) . .
O6 P2 C2 111.98(7) . .
O4 P2 C2 103.15(7) . .
O5 P2 C2 101.30(7) . .
O7 P3 O9 117.83(7) . .
O7 P3 O8 107.34(7) . .
O9 P3 O8 111.42(6) . .
O7 P3 C3 110.34(7) . .
O9 P3 C3 104.31(7) . .
O8 P3 C3 104.86(7) . .
O7 P3 Na1 42.03(5) . .
O9 P3 Na1 77.92(5) . .
O8 P3 Na1 113.82(5) . .
C3 P3 Na1 137.47(5) . .
O12 P4 O10 116.28(7) . .
O12 P4 O11 112.37(7) . .
O10 P4 O11 110.24(7) . .
O12 P4 C4 112.95(7) . .
O10 P4 C4 104.16(7) . .
O11 P4 C4 99.26(7) . .
P1 O3 H3O 112.8(17) . .
P2 O5 H5O 119.4(17) . .
P3 O7 Na2 144.57(7) . 2_557
P3 O7 Na1 114.67(6) . .
Na2 O7 Na1 79.71(4) 2_557 .
P3 O8 H8O 116.0(16) . .
P4 O11 H11O 118.8(17) . .
Na1 O13 Na2 84.41(4) . 2_557
Na1 O13 H13A 112.1(17) . .
Na2 O13 H13A 104.4(17) 2_557 .
Na1 O13 H13B 113.5(16) . .
Na2 O13 H13B 131.4(16) 2_557 .
H13A O13 H13B 109(2) . .
Na2 O14 Na1 76.19(4) . .
Na2 O14 Na2 82.81(5) . 2_457
Na1 O14 Na2 133.35(5) . 2_457
Na2 O14 H14A 138.9(18) . .
Na1 O14 H14A 80.5(18) . .
Na2 O14 H14A 89.4(17) 2_457 .
Na2 O14 H14B 118.7(18) . .
Na1 O14 H14B 124.3(18) . .
Na2 O14 H14B 102.4(17) 2_457 .
H14A O14 H14B 102(2) . .
Na2 O15 H15A 99.8(17) . .
Na2 O15 H15B 114.8(16) . .
H15A O15 H15B 109(2) . .
Na3 O16 H16A 116.2(17) . .
Na3 O16 H16B 114.9(17) . .
H16A O16 H16B 108(2) . .
Na3 O17 H17A 116.7(18) . .
Na3 O17 H17B 126.7(18) . .
H17A O17 H17B 97(2) . .
Na3 O18 H18A 109.3(17) . .
Na3 O18 H18B 101.9(17) . .
H18A O18 H18B 99(2) . .
H19A O19 H19B 108(2) . .
H20A O20 H20B 108(2) . .
H21A O21 H21B 106(2) . .
H22A O22 H22B 105(2) . .
Na2 O23 H23A 105.2(16) . .
Na2 O23 H23B 124.2(16) . .
H23A O23 H23B 102(2) . .
C2 N1 C1 113.05(11) . .
C2 N1 C5 113.43(12) . .
C1 N1 C5 109.96(12) . .
C2 N1 H1 107.7(14) . .
C1 N1 H1 105.4(14) . .
C5 N1 H1 106.7(14) . .
C4 N2 C3 113.83(11) . .
C4 N2 C10 112.85(12) . .
C3 N2 C10 110.83(12) . .
C4 N2 H2 107.1(14) . .
C3 N2 H2 105.0(14) . .
C10 N2 H2 106.5(14) . .
N1 C1 P1 115.81(10) . .
N1 C1 H1A 108.3 . .
P1 C1 H1A 108.3 . .
N1 C1 H1B 108.3 . .
P1 C1 H1B 108.3 . .
H1A C1 H1B 107.4 . .
N1 C2 P2 112.62(10) . .
N1 C2 H2A 109.1 . .
P2 C2 H2A 109.1 . .
N1 C2 H2B 109.1 . .
P2 C2 H2B 109.1 . .
H2A C2 H2B 107.8 . .
N2 C3 P3 117.25(10) . .
N2 C3 H3A 108.0 . .
P3 C3 H3A 108.0 . .
N2 C3 H3B 108.0 . .
P3 C3 H3B 108.0 . .
H3A C3 H3B 107.2 . .
N2 C4 P4 113.61(10) . .
N2 C4 H4A 108.8 . .
P4 C4 H4A 108.8 . .
N2 C4 H4B 108.8 . .
P4 C4 H4B 108.8 . .
H4A C4 H4B 107.7 . .
N1 C5 C6 114.20(12) . .
N1 C5 H5A 108.7 . .
C6 C5 H5A 108.7 . .
N1 C5 H5B 108.7 . .
C6 C5 H5B 108.7 . .
H5A C5 H5B 107.6 . .
C5 C6 C7 110.49(12) . .
C5 C6 H6A 109.6 . .
C7 C6 H6A 109.6 . .
C5 C6 H6B 109.6 . .
C7 C6 H6B 109.6 . .
H6A C6 H6B 108.1 . .
C8 C7 C6 111.91(13) . .
C8 C7 H7A 109.2 . .
C6 C7 H7A 109.2 . .
C8 C7 H7B 109.2 . .
C6 C7 H7B 109.2 . .
H7A C7 H7B 107.9 . .
C7 C8 C9 112.78(13) . .
C7 C8 H8A 109.0 . .
C9 C8 H8A 109.0 . .
C7 C8 H8B 109.0 . .
C9 C8 H8B 109.0 . .
H8A C8 H8B 107.8 . .
C10 C9 C8 109.93(12) . .
C10 C9 H9A 109.7 . .
C8 C9 H9A 109.7 . .
C10 C9 H9B 109.7 . .
C8 C9 H9B 109.7 . .
H9A C9 H9B 108.2 . .
N2 C10 C9 114.54(12) . .
N2 C10 H10A 108.6 . .
C9 C10 H10A 108.6 . .
N2 C10 H10B 108.6 . .
C9 C10 H10B 108.6 . .
H10A C10 H10B 107.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na1 O13 2.3120(12) .
Na1 O13 2.3120(12) 2_557
Na1 O7 2.5418(11) 2_557
Na1 O7 2.5419(11) .
Na1 O14 2.6977(14) .
Na1 O14 2.6977(14) 2_557
Na1 Na2 3.1402(6) 2_557
Na1 Na2 3.1402(6) .
Na1 P3 3.4501(4) .
Na1 P3 3.4502(4) 2_557
Na2 O23 2.3174(14) .
Na2 O7 2.3528(13) 2_557
Na2 O13 2.3623(14) 2_557
Na2 O15 2.3729(14) .
Na2 O14 2.3754(14) .
Na2 O14 2.7942(16) 2_457
Na2 Na2 3.4334(13) 2_457
Na2 H15A 2.63(2) .
Na2 H23A 2.66(2) .
Na3 O17 2.3941(13) .
Na3 O17 2.3941(13) 2_767
Na3 O18 2.4243(12) .
Na3 O18 2.4243(12) 2_767
Na3 O16 2.4720(13) .
Na3 O16 2.4720(13) 2_767
P1 O2 1.5005(12) .
P1 O1 1.5080(12) .
P1 O3 1.5577(12) .
P1 C1 1.8210(16) .
P2 O6 1.4986(12) .
P2 O4 1.5089(12) .
P2 O5 1.5595(12) .
P2 C2 1.8229(16) .
P3 O7 1.5019(12) .
P3 O9 1.5036(12) .
P3 O8 1.5737(12) .
P3 C3 1.8304(16) .
P4 O12 1.4929(12) .
P4 O10 1.5039(11) .
P4 O11 1.5635(12) .
P4 C4 1.8228(15) .
O3 H3O 0.793(16) .
O5 H5O 0.805(15) .
O7 Na2 2.3528(13) 2_557
O8 H8O 0.797(15) .
O11 H11O 0.800(15) .
O13 Na2 2.3622(14) 2_557
O13 H13A 0.804(16) .
O13 H13B 0.827(16) .
O14 Na2 2.7942(16) 2_457
O14 H14A 0.822(16) .
O14 H14B 0.820(16) .
O15 H15A 0.791(16) .
O15 H15B 0.802(16) .
O16 H16A 0.805(16) .
O16 H16B 0.824(16) .
O17 H17A 0.815(16) .
O17 H17B 0.829(16) .
O18 H18A 0.805(16) .
O18 H18B 0.828(16) .
O19 H19A 0.801(16) .
O19 H19B 0.798(16) .
O20 H20A 0.802(16) .
O20 H20B 0.816(16) .
O21 H21A 0.824(16) .
O21 H21B 0.807(16) .
O22 H22A 0.828(16) .
O22 H22B 0.825(16) .
O23 H23A 0.826(16) .
O23 H23B 0.809(16) .
N1 C2 1.4994(19) .
N1 C1 1.502(2) .
N1 C5 1.5180(19) .
N1 H1 0.849(15) .
N2 C4 1.4956(19) .
N2 C3 1.5033(19) .
N2 C10 1.5167(19) .
N2 H2 0.845(15) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.521(2) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.530(2) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.519(2) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.527(2) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.519(2) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
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
C10 H10B O3 0.97 2.42 3.3718(19) 166.3 2_666
C5 H5A O8 0.97 2.51 3.4318(19) 159.7 2_556
C4 H4B O8 0.97 2.42 3.0748(19) 124.6 .
C3 H3A O5 0.97 2.49 3.3549(19) 148.9 2_566
C2 H2A O3 0.97 2.40 3.0991(19) 129.0 .
C1 H1B O11 0.97 2.35 3.115(2) 135.5 2_656
C1 H1A O8 0.97 2.62 3.5024(19) 150.7 2_556
N2 H2 O15 0.845(15) 1.935(15) 2.7504(17) 162(2) 2_557
N1 H1 O19 0.849(15) 2.196(17) 2.9357(18) 145.5(19) 2_566
N1 H1 O4 0.849(15) 2.50(2) 2.9253(17) 111.7(16) .
O23 H23B O1 0.809(16) 1.882(16) 2.6870(16) 173(2) 1_456
O22 H22B O2 0.825(16) 1.837(17) 2.6509(17) 169(2) .
O22 H22A O18 0.828(16) 2.59(2) 3.2063(18) 132(2) 1_554
O22 H22A O17 0.828(16) 2.516(19) 3.249(2) 148(2) 2_766
O21 H21B O12 0.807(16) 1.953(16) 2.7548(16) 172(2) 2_666
O21 H21A O12 0.824(16) 1.878(17) 2.6839(17) 166(2) 1_565
O20 H20B O6 0.816(16) 1.902(16) 2.7088(17) 170(2) .
O20 H20A O6 0.802(16) 1.978(16) 2.7717(17) 170(2) 2_566
O19 H19B O7 0.798(16) 2.283(16) 3.0780(17) 175(2) 1_565
O19 H19A O1 0.801(16) 2.015(17) 2.7921(17) 164(2) 2_666
O18 H18B O19 0.828(16) 2.015(17) 2.8179(18) 163(2) 1_655
O18 H18A O2 0.805(16) 1.882(16) 2.6854(17) 175(2) 2_666
O17 H17B O4 0.829(16) 2.104(17) 2.9166(18) 167(2) 2_666
O17 H17A O9 0.815(16) 2.087(17) 2.8906(17) 169(3) 1_655
O16 H16B O22 0.824(16) 2.014(16) 2.8273(19) 169(2) 2_666
O16 H16A O1 0.805(16) 1.948(16) 2.7524(17) 179(3) 1_556
O15 H15B O9 0.802(16) 2.070(17) 2.8363(16) 160(2) 2_457
O14 H14B O16 0.820(16) 2.025(17) 2.8357(19) 170(2) 1_455
O14 H14A O9 0.822(16) 1.908(17) 2.7267(17) 174(2) .
O13 H13B O18 0.827(16) 1.984(16) 2.7974(18) 168(2) 2_667
O13 H13A O23 0.804(16) 2.007(17) 2.7857(17) 163(2) 1_655
O11 H11O O20 0.800(15) 1.745(16) 2.5233(17) 164(2) 1_545
O8 H8O O10 0.797(15) 1.754(16) 2.5399(16) 169(2) 1_455
O5 H5O O21 0.805(15) 1.732(16) 2.5189(17) 165(2) .
O3 H3O O4 0.793(16) 1.697(16) 2.4870(16) 174(3) 1_655
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_4
O9 P3 O7 Na2 -87.75(13) 2_557
O8 P3 O7 Na2 145.56(11) 2_557
C3 P3 O7 Na2 31.84(14) 2_557
Na1 P3 O7 Na2 -107.85(14) 2_557
O9 P3 O7 Na1 20.10(9) .
O8 P3 O7 Na1 -106.59(7) .
C3 P3 O7 Na1 139.69(6) .
C2 N1 C1 P1 -51.72(16) .
C5 N1 C1 P1 -179.62(10) .
O2 P1 C1 N1 -37.92(13) .
O1 P1 C1 N1 -163.75(11) .
O3 P1 C1 N1 78.26(12) .
C1 N1 C2 P2 167.01(10) .
C5 N1 C2 P2 -66.93(14) .
O6 P2 C2 N1 84.93(12) .
O4 P2 C2 N1 -41.60(12) .
O5 P2 C2 N1 -154.87(10) .
C4 N2 C3 P3 48.91(15) .
C10 N2 C3 P3 177.39(10) .
O7 P3 C3 N2 41.03(13) .
O9 P3 C3 N2 168.50(11) .
O8 P3 C3 N2 -74.27(12) .
Na1 P3 C3 N2 80.87(13) .
C3 N2 C4 P4 -169.95(10) .
C10 N2 C4 P4 62.61(14) .
O12 P4 C4 N2 -85.46(12) .
O10 P4 C4 N2 41.60(12) .
O11 P4 C4 N2 155.34(11) .
C2 N1 C5 C6 -56.23(17) .
C1 N1 C5 C6 71.45(16) .
N1 C5 C6 C7 -170.21(13) .
C5 C6 C7 C8 -177.60(14) .
C6 C7 C8 C9 -179.72(13) .
C7 C8 C9 C10 176.08(14) .
C4 N2 C10 C9 53.13(17) .
C3 N2 C10 C9 -75.89(16) .
C8 C9 C10 N2 174.07(13) .
