#------------------------------------------------------------------------------
#$Date: 2021-07-05 20:04:06 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267099 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/27/7242713.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_7242713
loop_
_publ_author_name
'Hodorowicz, Maciej'
'Jurowska, Anna'
'Szklarzewicz, Janusz'
_publ_section_title
;
 Unusual structural changes going from Li+ to Cs+ in
 [W(CN)6(bpy)]2− ion salts: the Na+ case
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              4301
_journal_page_last               4311
_journal_paper_doi               10.1039/D1CE00328C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_sum            'C32 H28 N16 Na4 O12 W2'
_chemical_formula_weight         1288.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-04-05 deposited with the CCDC.	2021-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                92.898(2)
_cell_angle_beta                 97.773(2)
_cell_angle_gamma                100.490(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1359(3)
_cell_length_b                   13.8894(3)
_cell_length_c                   13.9395(3)
_cell_measurement_reflns_used    7071
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.5294
_cell_measurement_theta_min      2.6958
_cell_volume                     2282.32(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SIR-2014 (Burla, 2015)'
_diffrn_ambient_temperature      129.9(6)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19808
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         28.591
_diffrn_reflns_theta_min         2.701
_exptl_absorpt_coefficient_mu    5.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       red
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.228
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10320
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0179P)²+2.6915P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7659
_reflns_number_total             10320
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce00328c2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7242713--7242714.cif.'
_cod_database_code               7242713
_shelx_shelxl_version_number     2017/1
_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   0.307
_shelx_estimated_absorpt_t_max   0.627
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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.56215(2) -0.26449(2) 0.85495(2) 0.01078(6) Uani 1 1 d . . . . .
W2 W 0.94843(2) 0.26852(2) 0.64296(2) 0.01095(6) Uani 1 1 d . . . . .
Na1 Na 0.53646(16) 0.11459(16) 0.79796(14) 0.0183(5) Uani 1 1 d . . . . .
Na3 Na 0.18481(17) 0.07091(17) 0.83191(16) 0.0269(5) Uani 1 1 d . . . . .
Na2 Na 0.36706(17) 0.09370(19) 0.54480(16) 0.0308(6) Uani 1 1 d . . . . .
Na4 Na 0.97270(16) -0.12556(16) 0.71977(14) 0.0176(5) Uani 1 1 d . . . . .
O7 O 0.3584(3) 0.0223(3) 0.8785(3) 0.0306(10) Uani 1 1 d . . . . .
H7A H 0.386160 0.021718 0.945761 0.046 Uiso 1 1 d R U . . .
H7B H 0.352750 -0.045192 0.854601 0.046 Uiso 1 1 d R U . . .
O1 O 0.4557(3) -0.0048(3) 0.6537(3) 0.0245(9) Uani 1 1 d . . . . .
H1A H 0.527511 -0.023445 0.652973 0.037 Uiso 1 1 d R U . . .
H1B H 0.407161 -0.049255 0.668005 0.037 Uiso 1 1 d R U . . .
O2 O 0.4237(3) 0.2135(3) 0.7028(3) 0.0310(10) Uani 1 1 d . . . . .
O3 O 0.1708(3) 0.0494(3) 0.5441(3) 0.0254(9) Uani 1 1 d D . . . .
O4 O 0.3129(3) 0.2538(3) 0.4992(3) 0.0343(11) Uani 1 1 d . . . . .
O5 O 0.3295(3) 0.0300(3) 0.3748(3) 0.0241(9) Uani 1 1 d . . . . .
O6 O 0.5295(3) 0.1917(3) 0.5072(3) 0.0353(11) Uani 1 1 d . . . . .
O8 O 0.1647(3) -0.0560(3) 0.7062(3) 0.0212(8) Uani 1 1 d . . . . .
H8A H 0.217214 -0.098332 0.711737 0.032 Uiso 1 1 d R U . . .
H8B H 0.166982 -0.023292 0.648589 0.032 Uiso 1 1 d R U . . .
O9 O 0.0208(3) -0.0248(3) 0.8743(3) 0.0325(10) Uani 1 1 d . . . . .
O10 O 1.0575(3) -0.2510(3) 0.8008(3) 0.0319(10) Uani 1 1 d . . . . .
H10A H 1.040671 -0.248137 0.865053 0.048 Uiso 1 1 d R U . . .
H10B H 1.134121 -0.220887 0.801243 0.048 Uiso 1 1 d R U . . .
N13 N 0.7823(4) -0.1937(3) 1.0267(3) 0.0193(10) Uani 1 1 d . . . . .
N15 N 0.6122(4) -0.0223(3) 0.8795(3) 0.0201(10) Uani 1 1 d . . . . .
N38 N 0.7279(4) 0.1777(3) 0.7494(3) 0.0211(10) Uani 1 1 d . . . . .
N32 N 0.8493(3) 0.3864(3) 0.6241(3) 0.0148(9) Uani 1 1 d . . . . .
N21 N 1.0675(3) 0.4072(3) 0.6253(3) 0.0126(9) Uani 1 1 d . . . . .
N34 N 1.0594(3) 0.2163(3) 0.4464(3) 0.0190(10) Uani 1 1 d . . . . .
N35 N 1.1925(4) 0.2140(4) 0.7354(3) 0.0214(10) Uani 1 1 d . . . . .
N36 N 0.9360(3) 0.0303(3) 0.6523(3) 0.0216(11) Uani 1 1 d . . . . .
N37 N 0.7442(4) 0.1633(4) 0.4669(3) 0.0250(11) Uani 1 1 d . . . . .
N33 N 0.9958(3) 0.3814(4) 0.8638(3) 0.0207(10) Uani 1 1 d . . . . .
N1 N 0.6468(3) -0.3929(3) 0.8628(3) 0.0123(9) Uani 1 1 d . . . . .
N12 N 0.4320(3) -0.3965(3) 0.8688(3) 0.0134(9) Uani 1 1 d . . . . .
N14 N 0.7747(3) -0.1827(4) 0.7368(3) 0.0222(11) Uani 1 1 d . . . . .
N16 N 0.3308(4) -0.1829(4) 0.7724(3) 0.0231(11) Uani 1 1 d . . . . .
N17 N 0.5017(3) -0.3503(4) 0.6236(3) 0.0213(11) Uani 1 1 d . . . . .
N18 N 0.5383(4) 0.2145(3) 0.9439(3) 0.0209(10) Uani 1 1 d . . . . .
C13 C 0.7042(4) -0.2207(4) 0.9700(4) 0.0151(11) Uani 1 1 d . . . . .
C15 C 0.5942(4) -0.1071(4) 0.8691(4) 0.0133(11) Uani 1 1 d . . . . .
C38 C 0.8070(4) 0.2093(4) 0.7154(4) 0.0179(12) Uani 1 1 d . . . . .
C27 C 0.9067(4) 0.4810(4) 0.6317(3) 0.0144(11) Uani 1 1 d . . . . .
C26 C 1.0273(4) 0.4917(4) 0.6301(3) 0.0150(11) Uani 1 1 d . . . . .
C22 C 1.1785(4) 0.4130(4) 0.6170(3) 0.0143(11) Uani 1 1 d . . . . .
H22 H 1.207231 0.354045 0.612081 0.017 Uiso 1 1 calc R U . . .
C23 C 1.2509(4) 0.5010(4) 0.6154(4) 0.0187(12) Uani 1 1 d . . . . .
H23 H 1.327939 0.502111 0.608464 0.022 Uiso 1 1 calc R U . . .
C24 C 1.2117(4) 0.5881(4) 0.6240(4) 0.0213(12) Uani 1 1 d . . . . .
H24 H 1.261430 0.649630 0.625353 0.026 Uiso 1 1 calc R U . . .
C25 C 1.0991(4) 0.5832(4) 0.6305(4) 0.0182(12) Uani 1 1 d . . . . .
H25 H 1.069614 0.641864 0.635141 0.022 Uiso 1 1 calc R U . . .
C28 C 0.8518(4) 0.5605(4) 0.6369(4) 0.0203(12) Uani 1 1 d . . . . .
H28 H 0.894208 0.625751 0.645520 0.024 Uiso 1 1 calc R U . . .
C29 C 0.7353(5) 0.5437(4) 0.6294(4) 0.0239(13) Uani 1 1 d . . . . .
H29 H 0.696726 0.597116 0.633523 0.029 Uiso 1 1 calc R U . . .
C30 C 0.6757(4) 0.4489(4) 0.6159(4) 0.0213(13) Uani 1 1 d . . . . .
H30 H 0.595248 0.436108 0.607573 0.026 Uiso 1 1 calc R U . . .
C31 C 0.7338(4) 0.3726(4) 0.6146(4) 0.0183(12) Uani 1 1 d . . . . .
H31 H 0.691655 0.307330 0.606747 0.022 Uiso 1 1 calc R U . . .
C34 C 1.0200(4) 0.2362(4) 0.5138(4) 0.0131(10) Uani 1 1 d . . . . .
C35 C 1.1079(4) 0.2352(4) 0.7063(4) 0.0158(11) Uani 1 1 d . . . . .
C36 C 0.9403(4) 0.1142(4) 0.6497(4) 0.0142(11) Uani 1 1 d . . . . .
C37 C 0.8166(4) 0.2030(4) 0.5266(4) 0.0169(11) Uani 1 1 d . . . . .
C33 C 0.9807(4) 0.3406(4) 0.7883(4) 0.0149(11) Uani 1 1 d . . . . .
C6 C 0.5823(4) -0.4836(4) 0.8614(3) 0.0140(11) Uani 1 1 d . . . . .
C7 C 0.4618(4) -0.4859(4) 0.8649(3) 0.0151(11) Uani 1 1 d . . . . .
C11 C 0.3229(4) -0.3934(4) 0.8799(4) 0.0170(11) Uani 1 1 d . . . . .
H11 H 0.300698 -0.331311 0.884009 0.020 Uiso 1 1 calc R U . . .
C10 C 0.2432(4) -0.4771(4) 0.8852(4) 0.0184(12) Uani 1 1 d . . . . .
H10 H 0.167519 -0.472162 0.892052 0.022 Uiso 1 1 calc R U . . .
C9 C 0.2742(4) -0.5685(4) 0.8806(4) 0.0209(13) Uani 1 1 d . . . . .
H9 H 0.220729 -0.626986 0.884052 0.025 Uiso 1 1 calc R U . . .
C8 C 0.3859(4) -0.5716(4) 0.8708(4) 0.0183(12) Uani 1 1 d . . . . .
H8 H 0.410097 -0.632914 0.868098 0.022 Uiso 1 1 calc R U . . .
C5 C 0.6280(4) -0.5687(4) 0.8610(4) 0.0175(11) Uani 1 1 d . . . . .
H5 H 0.579928 -0.631268 0.857453 0.021 Uiso 1 1 calc R U . . .
C4 C 0.7433(4) -0.5613(4) 0.8657(4) 0.0196(12) Uani 1 1 d . . . . .
H4 H 0.775774 -0.618646 0.865798 0.024 Uiso 1 1 calc R U . . .
C3 C 0.8107(4) -0.4698(4) 0.8702(4) 0.0204(12) Uani 1 1 d . . . . .
H3 H 0.890672 -0.462892 0.875350 0.025 Uiso 1 1 calc R U . . .
C2 C 0.7605(4) -0.3876(4) 0.8670(3) 0.0159(11) Uani 1 1 d . . . . .
H2 H 0.807606 -0.324838 0.867873 0.019 Uiso 1 1 calc R U . . .
C14 C 0.7009(4) -0.2103(4) 0.7780(3) 0.0138(11) Uani 1 1 d . . . . .
C16 C 0.4118(4) -0.2112(4) 0.7989(3) 0.0127(10) Uani 1 1 d . . . . .
C17 C 0.5186(4) -0.3227(4) 0.7042(4) 0.0128(11) Uani 1 1 d . . . . .
C18 C 0.5029(4) 0.2329(4) 1.0121(4) 0.0164(11) Uani 1 1 d . . . . .
O12 O 0.9971(3) 0.2442(3) 0.0081(3) 0.0307(10) Uani 1 1 d . . . . .
O11 O 0.1427(3) 0.9359(3) 0.0548(3) 0.0373(11) Uani 1 1 d . . . . .
H11B H 0.128089 0.956030 -0.010876 0.056 Uiso 1 1 d R U . . .
H11A H 0.224248 0.950980 0.063504 0.056 Uiso 1 1 d R U . . .
H3A H 0.147(6) 0.012(4) 0.485(3) 0.08(3) Uiso 1 1 d D . . . .
H3B H 0.136(5) 0.104(3) 0.545(4) 0.05(2) Uiso 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 W1 C16 69.77(18) . . ?
C15 W1 C14 71.23(18) . . ?
C16 W1 C14 111.02(18) . . ?
C15 W1 C13 74.06(19) . . ?
C16 W1 C13 137.37(19) . . ?
C14 W1 C13 76.71(18) . . ?
C15 W1 C18 77.38(18) . 2_657 ?
C16 W1 C18 78.99(18) . 2_657 ?
C14 W1 C18 140.28(19) . 2_657 ?
C13 W1 C18 71.66(18) . 2_657 ?
C15 W1 C17 112.13(19) . . ?
C16 W1 C17 74.13(18) . . ?
C14 W1 C17 71.18(17) . . ?
C13 W1 C17 142.40(17) . . ?
C18 W1 C17 145.45(18) 2_657 . ?
C15 W1 N1 142.92(16) . . ?
C16 W1 N1 145.81(17) . . ?
C14 W1 N1 81.59(16) . . ?
C13 W1 N1 75.51(17) . . ?
C18 W1 N1 112.18(17) 2_657 . ?
C17 W1 N1 80.87(17) . . ?
C15 W1 N12 142.71(16) . . ?
C16 W1 N12 80.68(16) . . ?
C14 W1 N12 143.19(17) . . ?
C13 W1 N12 119.02(17) . . ?
C18 W1 N12 75.01(17) 2_657 . ?
C17 W1 N12 79.52(16) . . ?
N1 W1 N12 72.02(14) . . ?
C36 W2 C37 75.6(2) . . ?
C36 W2 C35 68.12(19) . . ?
C37 W2 C35 135.4(2) . . ?
C36 W2 C34 79.90(18) . . ?
C37 W2 C34 69.49(17) . . ?
C35 W2 C34 79.17(18) . . ?
C36 W2 C38 71.17(18) . . ?
C37 W2 C38 75.65(19) . . ?
C35 W2 C38 114.10(19) . . ?
C34 W2 C38 139.1(2) . . ?
C36 W2 C33 110.05(19) . . ?
C37 W2 C33 143.83(17) . . ?
C35 W2 C33 75.23(18) . . ?
C34 W2 C33 146.01(17) . . ?
C38 W2 C33 73.00(19) . . ?
C36 W2 N32 145.42(16) . . ?
C37 W2 N32 78.60(18) . . ?
C35 W2 N32 144.28(18) . . ?
C34 W2 N32 111.93(16) . . ?
C38 W2 N32 80.44(17) . . ?
C33 W2 N32 78.83(17) . . ?
C36 W2 N21 141.89(16) . . ?
C37 W2 N21 120.68(17) . . ?
C35 W2 N21 78.84(17) . . ?
C34 W2 N21 75.63(16) . . ?
C38 W2 N21 142.98(18) . . ?
C33 W2 N21 77.77(16) . . ?
N32 W2 N21 71.94(15) . . ?
N18 Na1 O2 91.50(16) . . ?
N18 Na1 O1 157.81(15) . . ?
O2 Na1 O1 80.12(15) . . ?
N18 Na1 N15 96.36(16) . . ?
O2 Na1 N15 165.48(18) . . ?
O1 Na1 N15 88.13(15) . . ?
N18 Na1 N38 103.17(16) . . ?
O2 Na1 N38 99.81(15) . . ?
O1 Na1 N38 98.52(14) . . ?
N15 Na1 N38 90.29(15) . . ?
N18 Na1 O7 75.30(14) . . ?
O2 Na1 O7 93.60(14) . . ?
O1 Na1 O7 84.70(13) . . ?
N15 Na1 O7 76.72(13) . . ?
N38 Na1 O7 166.55(16) . . ?
N18 Na1 Na2 133.25(14) . . ?
O2 Na1 Na2 43.14(11) . . ?
O1 Na1 Na2 37.54(10) . . ?
N15 Na1 Na2 125.67(13) . . ?
N38 Na1 Na2 96.72(12) . . ?
O7 Na1 Na2 93.74(10) . . ?
O7 Na3 O9 117.89(18) . . ?
O7 Na3 O8 82.77(15) . . ?
O9 Na3 O8 84.06(14) . . ?
O7 Na3 N35 115.80(16) . 1_455 ?
O9 Na3 N35 126.23(17) . 1_455 ?
O8 Na3 N35 100.04(16) . 1_455 ?
O7 Na3 N13 92.17(16) . 2_657 ?
O9 Na3 N13 95.91(15) . 2_657 ?
O8 Na3 N13 174.22(17) . 2_657 ?
N35 Na3 N13 84.66(16) 1_455 2_657 ?
O7 Na3 Na4 112.44(13) . 1_455 ?
O9 Na3 Na4 43.81(10) . 1_455 ?
O8 Na3 Na4 42.44(9) . 1_455 ?
N35 Na3 Na4 110.73(13) 1_455 1_455 ?
N13 Na3 Na4 138.85(12) 2_657 1_455 ?
O6 Na2 O3 154.00(18) . . ?
O6 Na2 O1 98.17(15) . . ?
O3 Na2 O1 107.45(15) . . ?
O6 Na2 O5 86.87(15) . . ?
O3 Na2 O5 86.19(15) . . ?
O1 Na2 O5 115.30(17) . . ?
O6 Na2 O4 73.55(15) . . ?
O3 Na2 O4 81.53(15) . . ?
O1 Na2 O4 152.41(18) . . ?
O5 Na2 O4 90.90(15) . . ?
O6 Na2 O2 80.08(15) . . ?
O3 Na2 O2 100.30(15) . . ?
O1 Na2 O2 78.76(14) . . ?
O5 Na2 O2 162.23(16) . . ?
O4 Na2 O2 73.93(15) . . ?
O6 Na2 Na1 83.81(12) . . ?
O3 Na2 Na1 113.09(12) . . ?
O1 Na2 Na1 40.07(11) . . ?
O5 Na2 Na1 151.13(12) . . ?
O4 Na2 Na1 112.34(13) . . ?
O2 Na2 Na1 39.24(10) . . ?
O8 Na4 O10 83.50(14) 1_655 . ?
O8 Na4 N14 175.27(18) 1_655 . ?
O10 Na4 N14 100.05(16) . . ?
O8 Na4 O9 81.62(14) 1_655 1_655 ?
O10 Na4 O9 87.70(16) . 1_655 ?
N14 Na4 O9 95.33(15) . 1_655 ?
O8 Na4 N36 82.85(14) 1_655 . ?
O10 Na4 N36 164.82(17) . . ?
N14 Na4 N36 93.24(16) . . ?
O9 Na4 N36 83.76(16) 1_655 . ?
O8 Na4 N34 92.49(14) 1_655 2_756 ?
O10 Na4 N34 94.27(16) . 2_756 ?
N14 Na4 N34 90.37(16) . 2_756 ?
O9 Na4 N34 173.55(15) 1_655 2_756 ?
N36 Na4 N34 92.94(16) . 2_756 ?
O8 Na4 Na3 42.16(10) 1_655 1_655 ?
O10 Na4 Na3 94.45(12) . 1_655 ?
N14 Na4 Na3 133.89(14) . 1_655 ?
O9 Na4 Na3 41.56(10) 1_655 1_655 ?
N36 Na4 Na3 70.89(12) . 1_655 ?
N34 Na4 Na3 132.06(11) 2_756 1_655 ?
Na3 O7 Na1 115.91(17) . . ?
Na3 O7 H7A 119.6 . . ?
Na1 O7 H7A 105.6 . . ?
Na3 O7 H7B 109.1 . . ?
Na1 O7 H7B 101.8 . . ?
H7A O7 H7B 102.6 . . ?
Na2 O1 Na1 102.39(16) . . ?
Na2 O1 H1A 127.7 . . ?
Na1 O1 H1A 90.5 . . ?
Na2 O1 H1B 109.1 . . ?
Na1 O1 H1B 110.8 . . ?
H1A O1 H1B 112.9 . . ?
Na1 O2 Na2 97.61(16) . . ?
Na2 O3 H3A 102(4) . . ?
Na2 O3 H3B 113(4) . . ?
H3A O3 H3B 110(4) . . ?
Na3 O8 Na4 95.39(13) . 1_455 ?
Na3 O8 H8A 117.5 . . ?
Na4 O8 H8A 117.1 1_455 . ?
Na3 O8 H8B 104.9 . . ?
Na4 O8 H8B 109.6 1_455 . ?
H8A O8 H8B 111.0 . . ?
Na3 O9 Na4 94.63(14) . 1_455 ?
Na4 O10 H10A 106.3 . . ?
Na4 O10 H10B 97.1 . . ?
H10A O10 H10B 108.9 . . ?
C13 N13 Na3 130.9(4) . 2_657 ?
C15 N15 Na1 136.3(4) . . ?
C38 N38 Na1 170.5(4) . . ?
C27 N32 C31 116.8(5) . . ?
C27 N32 W2 118.1(3) . . ?
C31 N32 W2 124.8(4) . . ?
C26 N21 C22 118.0(4) . . ?
C26 N21 W2 117.2(3) . . ?
C22 N21 W2 124.6(4) . . ?
C34 N34 Na4 146.7(4) . 2_756 ?
C35 N35 Na3 117.1(4) . 1_655 ?
C36 N36 Na4 157.6(4) . . ?
C6 N1 C2 116.9(5) . . ?
C6 N1 W1 118.7(3) . . ?
C2 N1 W1 124.4(3) . . ?
C7 N12 C11 117.4(4) . . ?
C7 N12 W1 118.6(3) . . ?
C11 N12 W1 123.9(4) . . ?
C14 N14 Na4 155.3(4) . . ?
C18 N18 Na1 152.6(4) . . ?
N13 C13 W1 175.6(4) . . ?
N15 C15 W1 178.0(5) . . ?
N38 C38 W2 176.3(5) . . ?
N32 C27 C28 122.0(4) . . ?
N32 C27 C26 114.8(5) . . ?
C28 C27 C26 123.2(5) . . ?
N21 C26 C25 121.2(4) . . ?
N21 C26 C27 115.9(5) . . ?
C25 C26 C27 122.9(5) . . ?
N21 C22 C23 122.5(5) . . ?
N21 C22 H22 118.8 . . ?
C23 C22 H22 118.8 . . ?
C22 C23 C24 119.9(5) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 118.2(5) . . ?
C25 C24 H24 120.9 . . ?
C23 C24 H24 120.9 . . ?
C24 C25 C26 120.1(5) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C29 C28 C27 119.4(5) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C30 C29 C28 119.3(5) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C29 C30 C31 119.2(5) . . ?
C29 C30 H30 120.4 . . ?
C31 C30 H30 120.4 . . ?
N32 C31 C30 123.1(5) . . ?
N32 C31 H31 118.5 . . ?
C30 C31 H31 118.5 . . ?
N34 C34 W2 177.7(4) . . ?
N35 C35 W2 176.1(5) . . ?
N36 C36 W2 179.3(4) . . ?
N37 C37 W2 176.3(5) . . ?
N33 C33 W2 177.4(5) . . ?
N1 C6 C5 122.4(4) . . ?
N1 C6 C7 115.4(5) . . ?
C5 C6 C7 122.2(5) . . ?
N12 C7 C8 122.4(5) . . ?
N12 C7 C6 114.7(4) . . ?
C8 C7 C6 122.7(5) . . ?
N12 C11 C10 122.5(5) . . ?
N12 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
C11 C10 C9 119.7(5) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C9 C8 117.8(5) . . ?
C10 C9 H9 121.1 . . ?
C8 C9 H9 121.1 . . ?
C7 C8 C9 120.1(5) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C4 C5 C6 119.6(5) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C4 C3 C2 119.2(5) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
N1 C2 C3 123.0(5) . . ?
N1 C2 H2 118.5 . . ?
C3 C2 H2 118.5 . . ?
N14 C14 W1 179.1(5) . . ?
N16 C16 W1 177.6(4) . . ?
N17 C17 W1 175.9(4) . . ?
N18 C18 W1 178.0(5) . 2_657 ?
H11B O11 H11A 98.5 . . ?
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
W1 C15 2.143(5) . ?
W1 C16 2.157(5) . ?
W1 C14 2.159(5) . ?
W1 C13 2.164(5) . ?
W1 C18 2.166(5) 2_657 ?
W1 C17 2.172(5) . ?
W1 N1 2.215(4) . ?
W1 N12 2.227(4) . ?
W2 C36 2.135(5) . ?
W2 C37 2.153(6) . ?
W2 C35 2.155(5) . ?
W2 C34 2.163(5) . ?
W2 C38 2.164(5) . ?
W2 C33 2.167(5) . ?
W2 N32 2.208(4) . ?
W2 N21 2.233(4) . ?
Na1 N18 2.398(5) . ?
Na1 O2 2.429(4) . ?
Na1 O1 2.508(4) . ?
Na1 N15 2.515(5) . ?
Na1 N38 2.523(4) . ?
Na1 O7 2.714(4) . ?
Na1 Na2 3.805(3) . ?
Na3 O7 2.347(4) . ?
Na3 O9 2.347(4) . ?
Na3 O8 2.378(4) . ?
Na3 N35 2.451(5) 1_455 ?
Na3 N13 2.481(5) 2_657 ?
Na3 Na4 3.527(3) 1_455 ?
Na2 O6 2.321(4) . ?
Na2 O3 2.347(4) . ?
Na2 O1 2.374(4) . ?
Na2 O5 2.440(4) . ?
Na2 O4 2.519(5) . ?
Na2 O2 2.625(5) . ?
Na4 O8 2.391(4) 1_655 ?
Na4 O10 2.430(5) . ?
Na4 N14 2.437(4) . ?
Na4 O9 2.450(4) 1_655 ?
Na4 N36 2.493(5) . ?
Na4 N34 2.528(5) 2_756 ?
O7 H7A 0.9535 . ?
O7 H7B 0.9667 . ?
O1 H1A 0.9550 . ?
O1 H1B 0.8245 . ?
O3 H3A 0.931(19) . ?
O3 H3B 0.931(19) . ?
O8 H8A 0.9408 . ?
O8 H8B 0.9438 . ?
O10 H10A 0.9459 . ?
O10 H10B 0.9470 . ?
N13 C13 1.141(6) . ?
N15 C15 1.156(7) . ?
N38 C38 1.152(6) . ?
N32 C27 1.363(6) . ?
N32 C31 1.367(6) . ?
N21 C26 1.353(6) . ?
N21 C22 1.356(6) . ?
N34 C34 1.153(6) . ?
N35 C35 1.147(6) . ?
N36 C36 1.159(7) . ?
N37 C37 1.160(7) . ?
N33 C33 1.146(6) . ?
N1 C6 1.355(6) . ?
N1 C2 1.361(6) . ?
N12 C7 1.356(7) . ?
N12 C11 1.362(6) . ?
N14 C14 1.146(6) . ?
N16 C16 1.146(6) . ?
N17 C17 1.148(6) . ?
N18 C18 1.131(6) . ?
C27 C28 1.394(7) . ?
C27 C26 1.447(7) . ?
C26 C25 1.403(7) . ?
C22 C23 1.372(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.371(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C28 C29 1.379(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.372(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.376(7) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C6 C5 1.394(7) . ?
C6 C7 1.464(7) . ?
C7 C8 1.379(7) . ?
C11 C10 1.384(7) . ?
C11 H11 0.9500 . ?
C10 C9 1.389(8) . ?
C10 H10 0.9500 . ?
C9 C8 1.389(7) . ?
C9 H9 0.9500 . ?
C8 H8 0.9500 . ?
C5 C4 1.377(7) . ?
C5 H5 0.9500 . ?
C4 C3 1.374(7) . ?
C4 H4 0.9500 . ?
C3 C2 1.389(7) . ?
C3 H3 0.9500 . ?
C2 H2 0.9500 . ?
O11 H11B 0.9727 . ?
O11 H11A 0.9634 . ?
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
_geom_hbond_publ_flag
O7 H7A N15 0.95 2.43 3.344(6) 159.8 2_657 yes
O7 H7B N16 0.97 2.13 3.086(6) 167.8 . yes
O1 H1A O5 0.96 1.85 2.771(5) 162.4 2_656 yes
O1 H1B N37 0.82 2.67 3.185(6) 122.0 2_656 yes
O1 H1B N16 0.82 2.54 3.298(6) 154.3 . yes
O8 H8A N16 0.94 2.09 2.996(6) 161.1 . yes
O8 H8B O3 0.94 1.81 2.756(5) 175.0 . yes
O10 H10A O12 0.95 1.89 2.832(5) 178.4 2_756 yes
O10 H10B N16 0.95 2.44 3.363(6) 164.2 1_655 yes
C22 H22 O4 0.95 2.65 3.452(6) 142.2 1_655 yes
C22 H22 N35 0.95 2.66 3.310(7) 126.3 . yes
C23 H23 N17 0.95 2.64 3.337(6) 130.8 1_665 yes
C28 H28 N34 0.95 2.61 3.406(7) 141.9 2_766 yes
C31 H31 O6 0.95 2.50 3.325(7) 144.8 . yes
C11 H11 N16 0.95 2.65 3.343(7) 130.5 . yes
C10 H10 N33 0.95 2.61 3.243(7) 124.7 1_445 yes
C5 H5 N18 0.95 2.52 3.331(7) 143.9 1_545 yes
O11 H11B O9 0.97 1.98 2.870(6) 150.5 1_564 yes
O11 H11A N15 0.96 2.08 2.997(6) 158.2 2_666 yes
O3 H3A N36 0.931(19) 2.05(3) 2.935(6) 159(6) 2_656 yes
O3 H3B N34 0.931(19) 2.37(4) 3.165(6) 144(5) 1_455 yes
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
C31 N32 C27 C28 4.6(7) . . . . ?
W2 N32 C27 C28 -169.2(4) . . . . ?
C31 N32 C27 C26 -173.1(4) . . . . ?
W2 N32 C27 C26 13.1(5) . . . . ?
C22 N21 C26 C25 -2.4(7) . . . . ?
W2 N21 C26 C25 173.0(4) . . . . ?
C22 N21 C26 C27 175.6(4) . . . . ?
W2 N21 C26 C27 -8.9(5) . . . . ?
N32 C27 C26 N21 -2.5(6) . . . . ?
C28 C27 C26 N21 179.8(4) . . . . ?
N32 C27 C26 C25 175.5(4) . . . . ?
C28 C27 C26 C25 -2.2(8) . . . . ?
C26 N21 C22 C23 1.3(7) . . . . ?
W2 N21 C22 C23 -173.7(4) . . . . ?
N21 C22 C23 C24 1.0(8) . . . . ?
C22 C23 C24 C25 -2.3(7) . . . . ?
C23 C24 C25 C26 1.2(7) . . . . ?
N21 C26 C25 C24 1.2(7) . . . . ?
C27 C26 C25 C24 -176.7(5) . . . . ?
N32 C27 C28 C29 -3.2(7) . . . . ?
C26 C27 C28 C29 174.3(5) . . . . ?
C27 C28 C29 C30 -0.7(8) . . . . ?
C28 C29 C30 C31 2.9(8) . . . . ?
C27 N32 C31 C30 -2.3(7) . . . . ?
W2 N32 C31 C30 171.1(4) . . . . ?
C29 C30 C31 N32 -1.4(8) . . . . ?
C2 N1 C6 C5 -2.1(7) . . . . ?
W1 N1 C6 C5 176.6(4) . . . . ?
C2 N1 C6 C7 175.2(4) . . . . ?
W1 N1 C6 C7 -6.1(5) . . . . ?
C11 N12 C7 C8 0.6(7) . . . . ?
W1 N12 C7 C8 -178.6(4) . . . . ?
C11 N12 C7 C6 -175.0(4) . . . . ?
W1 N12 C7 C6 5.8(6) . . . . ?
N1 C6 C7 N12 0.1(6) . . . . ?
C5 C6 C7 N12 177.5(4) . . . . ?
N1 C6 C7 C8 -175.4(4) . . . . ?
C5 C6 C7 C8 1.9(8) . . . . ?
C7 N12 C11 C10 -1.2(7) . . . . ?
W1 N12 C11 C10 177.9(4) . . . . ?
N12 C11 C10 C9 0.9(8) . . . . ?
C11 C10 C9 C8 0.1(7) . . . . ?
N12 C7 C8 C9 0.3(8) . . . . ?
C6 C7 C8 C9 175.6(5) . . . . ?
C10 C9 C8 C7 -0.7(8) . . . . ?
N1 C6 C5 C4 2.4(8) . . . . ?
C7 C6 C5 C4 -174.7(5) . . . . ?
C6 C5 C4 C3 -0.3(8) . . . . ?
C5 C4 C3 C2 -1.8(8) . . . . ?
C6 N1 C2 C3 -0.2(7) . . . . ?
W1 N1 C2 C3 -178.8(4) . . . . ?
C4 C3 C2 N1 2.2(8) . . . . ?
