#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:45:03 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223596 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/21/7232169.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_7232169
loop_
_publ_author_name
'Li, Wei'
'Zhu, Jian-Nan'
'Shen, Nan-Nan'
'Xiong, Wei-Wei'
'Huang, Xiao-Ying'
_publ_section_title
;
 Assembling [M(P4Mo6)2] (M = Na, Mn, Na/Cu) dimeric clusters via
 transition metal/sodium ions into 0D to 3D phosphomolybdates
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              971
_journal_paper_doi               10.1039/C8CE01866A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C24 H91 Mo12 N12 Na O66 P8'
_chemical_formula_weight         3026.11
_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-2016/6
_audit_update_record
;
2018-10-30 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                114.779(15)
_cell_angle_beta                 99.377(9)
_cell_angle_gamma                100.412(12)
_cell_formula_units_Z            1
_cell_length_a                   12.5982(13)
_cell_length_b                   13.295(3)
_cell_length_c                   13.5974(12)
_cell_measurement_reflns_used    2957
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.6810
_cell_measurement_theta_min      3.5780
_cell_volume                     1959.7(6)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  Xcalibur
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_unetI/netI     0.1587
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19769
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.439
_diffrn_reflns_theta_min         3.295
_exptl_absorpt_coefficient_mu    2.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94029
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            flake
_exptl_crystal_density_diffrn    2.564
_exptl_crystal_description       Orange
_exptl_crystal_F_000             1482
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.898
_exptl_transmission_factor_min   0.741
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8215
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0200P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4951
_reflns_number_total             8215
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce01866a2.cif
_cod_data_source_block           x
_cod_depositor_comments
'Adding full bibliography for 7232169--7232174.cif.'
_cod_original_cell_volume        1959.7(5)
_cod_database_code               7232169
_shelx_shelxl_version_number     2016/6
_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.
;
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
Mo1 Mo 0.41322(7) 0.36284(8) 0.68687(7) 0.0151(2) Uani 1 1 d . . . . .
Mo2 Mo 0.34636(8) 0.17444(8) 0.39035(8) 0.0170(2) Uani 1 1 d . . . . .
Mo3 Mo 0.49310(8) 0.19434(8) 0.28202(8) 0.0175(2) Uani 1 1 d . . . . .
Mo4 Mo 0.75763(8) 0.40460(8) 0.42394(8) 0.0185(2) Uani 1 1 d . . . . .
Mo5 Mo 0.80685(8) 0.53316(8) 0.64052(8) 0.0178(2) Uani 1 1 d . . . . .
Mo6 Mo 0.60746(7) 0.51220(8) 0.79378(7) 0.0153(2) Uani 1 1 d . . . . .
P1 P 0.6182(2) 0.2758(2) 0.5562(2) 0.0153(6) Uani 1 1 d D . . . .
P2 P 0.2723(2) 0.0828(2) 0.5674(2) 0.0206(7) Uani 1 1 d D . . . .
P3 P 0.7313(3) 0.1298(2) 0.2318(2) 0.0207(7) Uani 1 1 d . . . . .
P4 P 0.8748(2) 0.5161(3) 0.8823(2) 0.0201(7) Uani 1 1 d D . . . .
Na1 Na 0.500000 0.500000 0.500000 0.0182(13) Uani 1 2 d S . P . .
O1 O 0.4930(5) 0.2508(5) 0.5520(5) 0.0170(16) Uani 1 1 d . . . . .
O2 O 0.6814(5) 0.3945(5) 0.6536(5) 0.0153(16) Uani 1 1 d . . . . .
O3 O 0.6339(5) 0.2693(5) 0.4447(5) 0.0130(15) Uani 1 1 d . . . . .
O4 O 0.6671(7) 0.1853(6) 0.5786(6) 0.0262(19) Uani 1 1 d D . . . .
H4 H 0.672(9) 0.139(6) 0.518(3) 0.031 Uiso 1 1 d D U . . .
O5 O 0.3034(6) 0.2995(6) 0.5244(6) 0.0201(17) Uani 1 1 d D . . . .
H5 H 0.306(8) 0.353(6) 0.509(8) 0.024 Uiso 1 1 d D U . . .
O6 O 0.5405(5) 0.3665(5) 0.7902(5) 0.0161(16) Uani 1 1 d . . . . .
O7 O 0.3435(6) 0.2000(5) 0.6670(6) 0.0211(17) Uani 1 1 d . . . . .
O8 O 0.4943(5) 0.4855(5) 0.6622(5) 0.0117(15) Uani 1 1 d . . . . .
O9 O 0.3329(5) 0.4290(6) 0.7656(6) 0.0203(17) Uani 1 1 d . . . . .
O10 O 0.4410(5) 0.0781(5) 0.3260(5) 0.0171(16) Uani 1 1 d . . . . .
O11 O 0.4261(5) 0.3055(5) 0.3766(5) 0.0165(16) Uani 1 1 d . . . . .
O12 O 0.2969(6) 0.0666(6) 0.4559(6) 0.0240(18) Uani 1 1 d . . . . .
O13 O 0.2259(6) 0.1236(6) 0.2887(6) 0.0273(19) Uani 1 1 d . . . . .
O14 O 0.6083(6) 0.3382(6) 0.2944(6) 0.0167(16) Uani 1 1 d D . . . .
H14 H 0.572(7) 0.380(7) 0.286(8) 0.020 Uiso 1 1 d D U . . .
O15 O 0.6073(6) 0.1045(6) 0.2256(6) 0.030(2) Uani 1 1 d . . . . .
O16 O 0.4093(6) 0.1469(6) 0.1519(6) 0.0277(19) Uani 1 1 d . . . . .
O17 O 0.7932(6) 0.2578(6) 0.3154(6) 0.0273(19) Uani 1 1 d . . . . .
O18 O 0.8543(5) 0.4021(6) 0.5480(6) 0.0208(17) Uani 1 1 d . . . . .
O19 O 0.6852(5) 0.5091(5) 0.5188(5) 0.0167(16) Uani 1 1 d . . . . .
O20 O 0.8369(6) 0.4883(6) 0.3842(6) 0.0273(19) Uani 1 1 d . . . . .
O21 O 0.7148(5) 0.6184(6) 0.7501(6) 0.0169(16) Uani 1 1 d D . . . .
H21 H 0.670(6) 0.644(8) 0.723(7) 0.020 Uiso 1 1 d D U . . .
O22 O 0.8969(6) 0.5267(6) 0.7783(6) 0.0248(18) Uani 1 1 d . . . . .
O23 O 0.9016(6) 0.6512(6) 0.6592(6) 0.0257(18) Uani 1 1 d . . . . .
O24 O 0.7556(6) 0.5155(6) 0.8888(6) 0.0252(18) Uani 1 1 d . . . . .
O25 O 0.5776(6) 0.6158(6) 0.9007(6) 0.0242(18) Uani 1 1 d . . . . .
O26 O 0.1498(6) 0.0692(7) 0.5604(7) 0.050(3) Uani 1 1 d . . . . .
O27 O 0.3088(7) -0.0114(7) 0.5902(7) 0.035(2) Uani 1 1 d D . . . .
H27 H 0.263(6) -0.036(8) 0.617(9) 0.041 Uiso 1 1 d D U . . .
O28 O 0.7831(6) 0.0555(6) 0.2767(6) 0.032(2) Uani 1 1 d . . . . .
O29 O 0.7502(6) 0.1016(6) 0.1179(6) 0.032(2) Uani 1 1 d . . . . .
O30 O 0.8890(6) 0.3951(6) 0.8656(6) 0.0280(19) Uani 1 1 d D . . . .
H30 H 0.947(9) 0.410(6) 0.912(12) 0.034 Uiso 0.5 1 d D U P . .
O31 O 0.9593(5) 0.6098(6) 0.9889(6) 0.0204(17) Uani 1 1 d . . . . .
N1 N 0.4618(8) -0.1434(7) 0.2219(7) 0.035(3) Uani 1 1 d . . . . .
H1E H 0.492537 -0.168235 0.268038 0.042 Uiso 1 1 calc R U . . .
H1 H 0.478030 -0.066953 0.259605 0.042 Uiso 1 1 calc R U . . .
N2 N 0.3304(7) -0.1963(8) 0.0013(7) 0.027(2) Uani 1 1 d . . . . .
H2E H 0.299676 -0.161625 -0.043678 0.033 Uiso 1 1 calc R U . . .
N3 N 0.1103(8) -0.3336(9) -0.1695(9) 0.056(3) Uani 1 1 d . . . . .
H3C H 0.038532 -0.373471 -0.192472 0.083 Uiso 1 1 calc R U . . .
H3D H 0.118204 -0.261173 -0.119630 0.083 Uiso 1 1 calc R U . . .
H3E H 0.133316 -0.334024 -0.228163 0.083 Uiso 1 1 calc R U . . .
C1 C 0.5114(10) -0.1761(10) 0.1229(10) 0.035(3) Uani 1 1 d . . . . .
H1A H 0.590559 -0.135413 0.148723 0.042 Uiso 1 1 calc R U . . .
H1B H 0.504301 -0.258148 0.088789 0.042 Uiso 1 1 calc R U . . .
C2 C 0.4542(9) -0.1471(10) 0.0372(10) 0.032(3) Uani 1 1 d . . . . .
H2A H 0.471667 -0.063855 0.068111 0.039 Uiso 1 1 calc R U . . .
H2B H 0.483255 -0.175785 -0.028101 0.039 Uiso 1 1 calc R U . . .
C3 C 0.2851(9) -0.1597(10) 0.1031(9) 0.028(3) Uani 1 1 d . . . . .
H3A H 0.297704 -0.076708 0.138337 0.033 Uiso 1 1 calc R U . . .
H3B H 0.204980 -0.195202 0.079593 0.033 Uiso 1 1 calc R U . . .
C4 C 0.3392(9) -0.1929(10) 0.1869(9) 0.027(3) Uani 1 1 d . . . . .
H4A H 0.309908 -0.165378 0.252178 0.032 Uiso 1 1 calc R U . . .
H4B H 0.321421 -0.276244 0.154063 0.032 Uiso 1 1 calc R U . . .
C5 C 0.3030(10) -0.3227(10) -0.0749(10) 0.039(3) Uani 1 1 d . . . . .
H5A H 0.341870 -0.357373 -0.035591 0.047 Uiso 1 1 calc R U . . .
H5B H 0.331638 -0.333626 -0.139654 0.047 Uiso 1 1 calc R U . . .
C6 C 0.1783(9) -0.3869(11) -0.1166(10) 0.037(3) Uani 1 1 d . . . . .
H6A H 0.168129 -0.466205 -0.170846 0.044 Uiso 1 1 calc R U . . .
H6B H 0.151826 -0.387611 -0.053756 0.044 Uiso 1 1 calc R U . . .
N4 N 1.1007(9) 0.1900(10) 0.8930(10) 0.059(4) Uani 1 1 d . . . . .
H4C H 1.137307 0.165904 0.936668 0.070 Uiso 1 1 calc R U . . .
H4D H 1.068594 0.240831 0.934419 0.070 Uiso 1 1 calc R U . . .
N5 N 1.0298(9) 0.1840(9) 0.6777(9) 0.047(3) Uani 1 1 d . . . . .
H5C H 1.064818 0.127572 0.632177 0.057 Uiso 1 1 calc R U . . .
N6 N 1.0248(17) 0.1669(19) 0.4252(17) 0.048(6) Uani 0.5 1 d . . P A 1
H6C H 1.055160 0.201482 0.388798 0.071 Uiso 0.5 1 calc R U P A 1
H6D H 0.952523 0.131964 0.389898 0.071 Uiso 0.5 1 calc R U P A 1
H6E H 1.059662 0.114878 0.426934 0.071 Uiso 0.5 1 calc R U P A 1
N6B N 0.9790(19) 0.2582(19) 0.457(2) 0.051(7) Uani 0.5 1 d . . P A 2
H6BA H 1.023606 0.277640 0.419472 0.077 Uiso 0.5 1 calc R U P A 2
H6BB H 0.944813 0.312681 0.485367 0.077 Uiso 0.5 1 calc R U P A 2
H6BC H 0.928040 0.191418 0.410357 0.077 Uiso 0.5 1 calc R U P A 2
C7 C 1.1838(11) 0.2489(12) 0.8507(12) 0.057(4) Uani 1 1 d . . . . .
H7A H 1.237901 0.315960 0.913454 0.069 Uiso 1 1 calc R U . . .
H7B H 1.223662 0.196253 0.810146 0.069 Uiso 1 1 calc R U . . .
C8 C 1.1192(10) 0.2839(11) 0.7754(11) 0.054(4) Uani 1 1 d . . . . .
H8A H 1.170391 0.320537 0.746244 0.065 Uiso 1 1 calc R U . . .
H8B H 1.084078 0.340453 0.818628 0.065 Uiso 1 1 calc R U . . .
C9 C 0.9520(11) 0.1289(12) 0.7256(11) 0.047(4) Uani 1 1 d . . . . .
H9A H 0.915190 0.183940 0.768236 0.056 Uiso 1 1 calc R U . . .
H9B H 0.894658 0.063284 0.664600 0.056 Uiso 1 1 calc R U . . .
C10 C 1.0127(11) 0.0903(12) 0.7993(12) 0.063(5) Uani 1 1 d . . . . .
H10A H 1.046699 0.032423 0.756250 0.076 Uiso 1 1 calc R U . . .
H10B H 0.960720 0.055754 0.829283 0.076 Uiso 1 1 calc R U . . .
C11 C 0.9627(12) 0.2231(14) 0.6045(14) 0.066(5) Uani 1 1 d . . . . .
H11A H 0.943292 0.291909 0.650787 0.079 Uiso 1 1 calc R U . . .
H11B H 0.894109 0.163171 0.556144 0.079 Uiso 1 1 calc R U . . .
C12 C 1.0355(16) 0.2484(19) 0.5341(16) 0.096(7) Uani 1 1 d . . . . .
H12A H 1.023767 0.316979 0.530491 0.115 Uiso 0.5 1 calc R U P A 1
H12B H 1.112862 0.268523 0.575876 0.115 Uiso 0.5 1 calc R U P A 1
H12C H 1.094993 0.319122 0.581486 0.115 Uiso 0.5 1 calc R U P A 2
H12D H 1.069682 0.186267 0.502971 0.115 Uiso 0.5 1 calc R U P A 2
O1W O 0.1980(15) 0.1005(15) 0.0130(11) 0.164(8) Uani 1 1 d D . . . .
H1C H 0.191(16) 0.129(14) 0.077(6) 0.247 Uiso 1 1 d D U . . .
H1D H 0.251(12) 0.073(19) 0.005(9) 0.247 Uiso 1 1 d D U . . .
O2W O 0.9721(11) 0.1314(10) 0.0486(9) 0.096(4) Uani 1 1 d D . . . .
H2C H 0.958(2) 0.1496(18) -0.0016(17) 0.144 Uiso 1 1 d D U . . .
H2D H 1.009(14) 0.183(4) 0.110(4) 0.144 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 0.0000 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'
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'
Mo Mo -1.6832 0.6857 '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'
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
O9 Mo1 O6 106.3(3) . .
O9 Mo1 O8 101.7(3) . .
O6 Mo1 O8 95.1(3) . .
O9 Mo1 O7 96.3(3) . .
O6 Mo1 O7 85.8(3) . .
O8 Mo1 O7 160.9(3) . .
O9 Mo1 O5 99.2(3) . .
O6 Mo1 O5 153.4(3) . .
O8 Mo1 O5 87.2(3) . .
O7 Mo1 O5 83.7(3) . .
O9 Mo1 O1 169.3(3) . .
O6 Mo1 O1 83.0(2) . .
O8 Mo1 O1 82.5(2) . .
O7 Mo1 O1 78.7(2) . .
O5 Mo1 O1 71.0(2) . .
O9 Mo1 Mo6 100.8(2) . .
O6 Mo1 Mo6 48.30(19) . .
O8 Mo1 Mo6 48.50(18) . .
O7 Mo1 Mo6 133.8(2) . .
O5 Mo1 Mo6 134.2(2) . .
O1 Mo1 Mo6 89.43(16) . .
O13 Mo2 O11 102.5(3) . .
O13 Mo2 O10 105.5(3) . .
O11 Mo2 O10 94.5(3) . .
O13 Mo2 O12 94.7(3) . .
O11 Mo2 O12 161.4(3) . .
O10 Mo2 O12 87.5(3) . .
O13 Mo2 O5 100.0(3) . .
O11 Mo2 O5 84.9(3) . .
O10 Mo2 O5 153.9(3) . .
O12 Mo2 O5 85.2(3) . .
O13 Mo2 O1 170.0(3) . .
O11 Mo2 O1 82.2(3) . .
O10 Mo2 O1 82.7(2) . .
O12 Mo2 O1 79.8(3) . .
O5 Mo2 O1 71.3(2) . .
O13 Mo2 Mo3 101.4(2) . .
O11 Mo2 Mo3 48.13(18) . .
O10 Mo2 Mo3 47.78(19) . .
O12 Mo2 Mo3 135.02(19) . .
O5 Mo2 Mo3 131.5(2) . .
O1 Mo2 Mo3 88.27(16) . .
O16 Mo3 O10 104.8(3) . .
O16 Mo3 O11 102.6(3) . .
O10 Mo3 O11 95.2(3) . .
O16 Mo3 O15 94.6(3) . .
O10 Mo3 O15 85.9(3) . .
O11 Mo3 O15 161.8(3) . .
O16 Mo3 O14 99.6(3) . .
O10 Mo3 O14 154.7(3) . .
O11 Mo3 O14 85.7(3) . .
O15 Mo3 O14 85.6(3) . .
O16 Mo3 O3 168.9(3) . .
O10 Mo3 O3 83.8(3) . .
O11 Mo3 O3 83.2(2) . .
O15 Mo3 O3 78.9(3) . .
O14 Mo3 O3 71.1(2) . .
O16 Mo3 Mo2 101.0(2) . .
O10 Mo3 Mo2 48.35(18) . .
O11 Mo3 Mo2 48.30(19) . .
O15 Mo3 Mo2 134.0(2) . .
O14 Mo3 Mo2 132.63(18) . .
O3 Mo3 Mo2 89.96(16) . .
O20 Mo4 O18 106.8(3) . .
O20 Mo4 O19 102.5(3) . .
O18 Mo4 O19 94.0(3) . .
O20 Mo4 O17 92.3(3) . .
O18 Mo4 O17 88.8(3) . .
O19 Mo4 O17 163.3(3) . .
O20 Mo4 O14 100.3(3) . .
O18 Mo4 O14 151.9(3) . .
O19 Mo4 O14 87.5(3) . .
O17 Mo4 O14 82.4(3) . .
O20 Mo4 O3 169.7(3) . .
O18 Mo4 O3 81.3(3) . .
O19 Mo4 O3 82.8(2) . .
O17 Mo4 O3 81.4(2) . .
O14 Mo4 O3 71.0(2) . .
O20 Mo4 Mo5 102.1(2) . .
O18 Mo4 Mo5 47.82(19) . .
O19 Mo4 Mo5 47.68(19) . .
O17 Mo4 Mo5 136.6(2) . .
O14 Mo4 Mo5 133.14(18) . .
O3 Mo4 Mo5 87.99(16) . .
O23 Mo5 O19 103.1(3) . .
O23 Mo5 O18 106.0(3) . .
O19 Mo5 O18 93.9(3) . .
O23 Mo5 O22 94.0(3) . .
O19 Mo5 O22 161.9(3) . .
O18 Mo5 O22 87.0(3) . .
O23 Mo5 O21 97.8(3) . .
O19 Mo5 O21 86.6(3) . .
O18 Mo5 O21 155.3(3) . .
O22 Mo5 O21 85.1(3) . .
O23 Mo5 O2 168.2(3) . .
O19 Mo5 O2 83.8(3) . .
O18 Mo5 O2 82.7(2) . .
O22 Mo5 O2 78.4(3) . .
O21 Mo5 O2 72.8(2) . .
O23 Mo5 Mo4 101.9(2) . .
O19 Mo5 Mo4 47.88(18) . .
O18 Mo5 Mo4 47.5(2) . .
O22 Mo5 Mo4 134.3(2) . .
O21 Mo5 Mo4 133.30(19) . .
O2 Mo5 Mo4 89.77(16) . .
O25 Mo6 O6 106.6(3) . .
O25 Mo6 O8 103.1(3) . .
O6 Mo6 O8 94.4(3) . .
O25 Mo6 O24 95.9(3) . .
O6 Mo6 O24 87.4(3) . .
O8 Mo6 O24 159.4(3) . .
O25 Mo6 O21 98.8(3) . .
O6 Mo6 O21 153.8(3) . .
O8 Mo6 O21 85.7(3) . .
O24 Mo6 O21 83.8(3) . .
O25 Mo6 O2 169.0(3) . .
O6 Mo6 O2 82.6(2) . .
O8 Mo6 O2 81.7(2) . .
O24 Mo6 O2 78.3(2) . .
O21 Mo6 O2 71.5(2) . .
O25 Mo6 Mo1 102.1(2) . .
O6 Mo6 Mo1 47.84(19) . .
O8 Mo6 Mo1 48.22(18) . .
O24 Mo6 Mo1 134.8(2) . .
O21 Mo6 Mo1 132.5(2) . .
O2 Mo6 Mo1 88.48(16) . .
O2 P1 O3 110.7(4) . .
O2 P1 O1 109.6(4) . .
O3 P1 O1 110.1(4) . .
O2 P1 O4 107.4(4) . .
O3 P1 O4 109.4(4) . .
O1 P1 O4 109.4(4) . .
O26 P2 O12 111.5(5) . .
O26 P2 O27 110.0(5) . .
O12 P2 O27 105.7(4) . .
O26 P2 O7 110.5(4) . .
O12 P2 O7 112.2(4) . .
O27 P2 O7 106.7(4) . .
O29 P3 O15 111.3(4) . .
O29 P3 O28 108.6(4) . .
O15 P3 O28 109.0(4) . .
O29 P3 O17 110.0(4) . .
O15 P3 O17 110.8(4) . .
O28 P3 O17 107.1(4) . .
O31 P4 O24 111.6(4) . .
O31 P4 O22 110.9(4) . .
O24 P4 O22 111.7(4) . .
O31 P4 O30 109.1(4) . .
O24 P4 O30 107.3(4) . .
O22 P4 O30 106.0(4) . .
O19 Na1 O19 180.0 2_666 .
O19 Na1 O8 95.2(2) 2_666 2_666
O19 Na1 O8 84.8(2) . 2_666
O19 Na1 O8 84.8(2) 2_666 .
O19 Na1 O8 95.2(2) . .
O8 Na1 O8 180.0 2_666 .
O19 Na1 O11 98.3(2) 2_666 2_666
O19 Na1 O11 81.7(2) . 2_666
O8 Na1 O11 96.8(2) 2_666 2_666
O8 Na1 O11 83.2(2) . 2_666
O19 Na1 O11 81.7(2) 2_666 .
O19 Na1 O11 98.3(2) . .
O8 Na1 O11 83.2(2) 2_666 .
O8 Na1 O11 96.8(2) . .
O11 Na1 O11 180.0(2) 2_666 .
P1 O1 Mo2 125.2(4) . .
P1 O1 Mo1 125.8(4) . .
Mo2 O1 Mo1 100.9(2) . .
P1 O2 Mo5 124.8(4) . .
P1 O2 Mo6 126.1(4) . .
Mo5 O2 Mo6 100.0(2) . .
P1 O3 Mo3 125.1(4) . .
P1 O3 Mo4 125.9(4) . .
Mo3 O3 Mo4 101.4(2) . .
P1 O4 H4 106(5) . .
Mo2 O5 Mo1 115.6(3) . .
Mo2 O5 H5 104(7) . .
Mo1 O5 H5 108(7) . .
Mo1 O6 Mo6 83.9(2) . .
P2 O7 Mo1 135.7(4) . .
Mo1 O8 Mo6 83.3(2) . .
Mo1 O8 Na1 131.6(3) . .
Mo6 O8 Na1 134.5(3) . .
Mo3 O10 Mo2 83.9(2) . .
Mo3 O11 Mo2 83.6(2) . .
Mo3 O11 Na1 130.9(3) . .
Mo2 O11 Na1 133.5(3) . .
P2 O12 Mo2 134.9(4) . .
Mo4 O14 Mo3 115.2(3) . .
Mo4 O14 H14 121(7) . .
Mo3 O14 H14 106(7) . .
P3 O15 Mo3 138.5(4) . .
P3 O17 Mo4 138.9(4) . .
Mo4 O18 Mo5 84.7(3) . .
Mo5 O19 Mo4 84.4(3) . .
Mo5 O19 Na1 133.9(3) . .
Mo4 O19 Na1 130.3(3) . .
Mo6 O21 Mo5 114.9(3) . .
Mo6 O21 H21 101(7) . .
Mo5 O21 H21 114(7) . .
P4 O22 Mo5 137.5(4) . .
P4 O24 Mo6 139.3(4) . .
P2 O27 H27 108(5) . .
P4 O30 H30 105(5) . .
C4 N1 C1 112.0(9) . .
C4 N1 H1E 109.2 . .
C1 N1 H1E 109.2 . .
C4 N1 H1 109.2 . .
C1 N1 H1 109.2 . .
H1E N1 H1 107.9 . .
C2 N2 C5 108.7(9) . .
C2 N2 C3 109.5(8) . .
C5 N2 C3 117.2(9) . .
C2 N2 H2E 107.0 . .
C5 N2 H2E 107.0 . .
C3 N2 H2E 107.0 . .
C6 N3 H3C 109.5 . .
C6 N3 H3D 109.5 . .
H3C N3 H3D 109.5 . .
C6 N3 H3E 109.5 . .
H3C N3 H3E 109.5 . .
H3D N3 H3E 109.5 . .
C2 C1 N1 111.3(9) . .
C2 C1 H1A 109.4 . .
N1 C1 H1A 109.4 . .
C2 C1 H1B 109.4 . .
N1 C1 H1B 109.4 . .
H1A C1 H1B 108.0 . .
N2 C2 C1 113.1(9) . .
N2 C2 H2A 109.0 . .
C1 C2 H2A 109.0 . .
N2 C2 H2B 109.0 . .
C1 C2 H2B 109.0 . .
H2A C2 H2B 107.8 . .
C4 C3 N2 112.0(9) . .
C4 C3 H3A 109.2 . .
N2 C3 H3A 109.2 . .
C4 C3 H3B 109.2 . .
N2 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
N1 C4 C3 110.8(9) . .
N1 C4 H4A 109.5 . .
C3 C4 H4A 109.5 . .
N1 C4 H4B 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 108.1 . .
N2 C5 C6 115.0(10) . .
N2 C5 H5A 108.5 . .
C6 C5 H5A 108.5 . .
N2 C5 H5B 108.5 . .
C6 C5 H5B 108.5 . .
H5A C5 H5B 107.5 . .
N3 C6 C5 112.5(10) . .
N3 C6 H6A 109.1 . .
C5 C6 H6A 109.1 . .
N3 C6 H6B 109.1 . .
C5 C6 H6B 109.1 . .
H6A C6 H6B 107.8 . .
C10 N4 C7 112.0(11) . .
C10 N4 H4C 109.2 . .
C7 N4 H4C 109.2 . .
C10 N4 H4D 109.2 . .
C7 N4 H4D 109.2 . .
H4C N4 H4D 107.9 . .
C9 N5 C8 107.6(10) . .
C9 N5 C11 108.9(10) . .
C8 N5 C11 111.9(11) . .
C9 N5 H5C 109.5 . .
C8 N5 H5C 109.5 . .
C11 N5 H5C 109.5 . .
C12 N6 H6C 109.5 . .
C12 N6 H6D 109.5 . .
H6C N6 H6D 109.5 . .
C12 N6 H6E 109.5 . .
H6C N6 H6E 109.5 . .
H6D N6 H6E 109.5 . .
C12 N6B H6BA 109.5 . .
C12 N6B H6BB 109.5 . .
H6BA N6B H6BB 109.5 . .
C12 N6B H6BC 109.5 . .
H6BA N6B H6BC 109.5 . .
H6BB N6B H6BC 109.5 . .
C8 C7 N4 107.5(10) . .
C8 C7 H7A 110.2 . .
N4 C7 H7A 110.2 . .
C8 C7 H7B 110.2 . .
N4 C7 H7B 110.2 . .
H7A C7 H7B 108.5 . .
C7 C8 N5 113.2(12) . .
C7 C8 H8A 108.9 . .
N5 C8 H8A 108.9 . .
C7 C8 H8B 108.9 . .
N5 C8 H8B 108.9 . .
H8A C8 H8B 107.8 . .
C10 C9 N5 111.5(11) . .
C10 C9 H9A 109.3 . .
N5 C9 H9A 109.3 . .
C10 C9 H9B 109.3 . .
N5 C9 H9B 109.3 . .
H9A C9 H9B 108.0 . .
C9 C10 N4 109.8(12) . .
C9 C10 H10A 109.7 . .
N4 C10 H10A 109.7 . .
C9 C10 H10B 109.7 . .
N4 C10 H10B 109.7 . .
H10A C10 H10B 108.2 . .
N5 C11 C12 107.2(13) . .
N5 C11 H11A 110.3 . .
C12 C11 H11A 110.3 . .
N5 C11 H11B 110.3 . .
C12 C11 H11B 110.3 . .
H11A C11 H11B 108.5 . .
N6B C12 C11 110.6(19) . .
N6 C12 C11 121.2(19) . .
N6 C12 H12A 107.0 . .
C11 C12 H12A 107.0 . .
N6 C12 H12B 107.0 . .
C11 C12 H12B 107.0 . .
H12A C12 H12B 106.8 . .
N6B C12 H12C 109.5 . .
C11 C12 H12C 109.5 . .
N6B C12 H12D 109.5 . .
C11 C12 H12D 109.5 . .
H12C C12 H12D 108.1 . .
H1C O1W H1D 116(2) . .
H2C O2W H2D 116(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O9 1.682(6) .
Mo1 O6 1.931(6) .
Mo1 O8 1.945(6) .
Mo1 O7 2.068(7) .
Mo1 O5 2.128(7) .
Mo1 O1 2.333(6) .
Mo1 Mo6 2.5902(14) .
Mo2 O13 1.683(7) .
Mo2 O11 1.944(6) .
Mo2 O10 1.944(6) .
Mo2 O12 2.041(7) .
Mo2 O5 2.118(7) .
Mo2 O1 2.325(6) .
Mo2 Mo3 2.5875(13) .
Mo3 O16 1.691(7) .
Mo3 O10 1.927(6) .
Mo3 O11 1.939(6) .
Mo3 O15 2.073(7) .
Mo3 O14 2.107(7) .
Mo3 O3 2.294(6) .
Mo4 O20 1.675(7) .
Mo4 O18 1.929(7) .
Mo4 O19 1.941(6) .
Mo4 O17 2.075(7) .
Mo4 O14 2.107(7) .
Mo4 O3 2.302(6) .
Mo4 Mo5 2.6041(14) .
Mo5 O23 1.686(7) .
Mo5 O19 1.935(6) .
Mo5 O18 1.938(6) .
Mo5 O22 2.069(7) .
Mo5 O21 2.115(6) .
Mo5 O2 2.289(6) .
Mo6 O25 1.684(6) .
Mo6 O6 1.945(6) .
Mo6 O8 1.953(6) .
Mo6 O24 2.072(7) .
Mo6 O21 2.109(7) .
Mo6 O2 2.357(6) .
P1 O2 1.526(7) .
P1 O3 1.530(6) .
P1 O1 1.538(7) .
P1 O4 1.561(7) .
P2 O26 1.503(7) .
P2 O12 1.532(7) .
P2 O27 1.538(8) .
P2 O7 1.547(7) .
P3 O29 1.503(7) .
P3 O15 1.518(7) .
P3 O28 1.543(8) .
P3 O17 1.551(7) .
P4 O31 1.514(7) .
P4 O24 1.517(7) .
P4 O22 1.544(7) .
P4 O30 1.575(7) .
Na1 O19 2.281(6) 2_666
Na1 O19 2.281(6) .
Na1 O8 2.304(6) 2_666
Na1 O8 2.304(6) .
Na1 O11 2.314(6) 2_666
Na1 O11 2.314(6) .
O4 H4 0.818(10) .
O5 H5 0.817(10) .
O14 H14 0.819(10) .
O21 H21 0.818(10) .
O27 H27 0.819(10) .
O30 H30 0.820(10) .
N1 C4 1.474(12) .
N1 C1 1.509(13) .
N1 H1E 0.8900 .
N1 H1 0.8900 .
N2 C2 1.488(13) .
N2 C5 1.493(13) .
N2 C3 1.508(12) .
N2 H2E 0.9800 .
N3 C6 1.483(14) .
N3 H3C 0.8900 .
N3 H3D 0.8900 .
N3 H3E 0.8900 .
C1 C2 1.493(15) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.495(14) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.529(15) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
N4 C10 1.485(15) .
N4 C7 1.521(16) .
N4 H4C 0.8900 .
N4 H4D 0.8900 .
N5 C9 1.507(15) .
N5 C8 1.513(15) .
N5 C11 1.515(16) .
N5 H5C 0.9800 .
N6 C12 1.39(2) .
N6 H6C 0.8900 .
N6 H6D 0.8900 .
N6 H6E 0.8900 .
N6B C12 1.24(2) .
N6B H6BA 0.8900 .
N6B H6BB 0.8900 .
N6B H6BC 0.8900 .
C7 C8 1.481(18) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.475(18) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.52(2) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C12 H12C 0.9700 .
C12 H12D 0.9700 .
O1W H1C 0.821(10) .
O1W H1D 0.821(10) .
O2W H2C 0.817(10) .
O2W H2D 0.818(10) .
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
O4 H4 O27 0.818(10) 1.81(3) 2.596(10) 161(8) 2_656
O5 H5 O19 0.817(10) 2.010(15) 2.826(9) 176(10) 2_666
O14 H14 O8 0.819(10) 2.01(4) 2.774(8) 156(9) 2_666
O21 H21 O11 0.818(10) 2.07(3) 2.874(9) 167(10) 2_666
O27 H27 O28 0.819(10) 1.74(5) 2.507(10) 155(11) 2_656
O30 H30 O31 0.820(10) 1.78(5) 2.548(10) 156(14) 2_767
N1 H1E O6 0.89 2.34 2.895(11) 120.1 2_656
N1 H1E O7 0.89 2.29 3.046(11) 142.2 2_656
N1 H1 O10 0.89 1.94 2.766(10) 154.1 .
N2 H2E O29 0.98 1.64 2.623(12) 179.1 2_655
N3 H3C O22 0.89 1.89 2.766(12) 167.4 1_444
N3 H3C O23 0.89 2.60 3.130(13) 118.7 1_444
N3 H3D O29 0.89 2.43 2.986(13) 120.5 2_655
N3 H3D O2W 0.89 2.21 2.978(17) 144.4 2_655
N3 H3E O17 0.89 2.08 2.907(13) 154.4 2_655
N3 H3E O20 0.89 2.40 3.048(12) 130.3 2_655
C2 H2A O15 0.97 2.43 3.217(14) 137.5 .
C2 H2B O16 0.97 2.43 3.319(13) 152.0 2_655
C3 H3A O10 0.97 2.60 3.289(13) 128.2 .
C4 H4A O4 0.97 2.40 3.162(13) 134.9 2_656
C4 H4B O6 0.97 2.48 3.071(12) 119.5 2_656
C5 H5B O14 0.97 2.33 3.294(14) 172.1 2_655
C6 H6B O31 0.97 2.58 3.312(13) 132.2 1_444
N4 H4C O1W 0.89 1.78 2.663(18) 172.8 1_656
N4 H4D O31 0.89 1.95 2.788(12) 157.1 2_767
N5 H5C O26 0.98 1.65 2.596(12) 162.3 1_655
N6 H6C O23 0.89 2.31 3.14(2) 155.1 2_766
N6 H6D O28 0.89 2.19 3.07(2) 168.3 .
N6 H6E O26 0.89 2.33 3.06(3) 138.2 1_655
N6B H6BA O23 0.89 1.94 2.81(2) 165.0 2_766
N6B H6BB O18 0.89 1.84 2.72(2) 167.9 .
N6B H6BC O28 0.89 2.21 3.07(3) 164.2 .
C7 H7A O24 0.97 2.66 3.449(15) 138.8 2_767
C8 H8A O9 0.97 2.19 3.072(13) 151.3 1_655
C8 H8B O31 0.97 2.59 3.316(14) 131.2 2_767
C9 H9B O12 0.97 2.52 3.440(15) 159.4 2_656
C10 H10A O28 0.97 2.64 3.526(16) 152.8 2_756
C10 H10A N6 0.97 2.62 3.38(3) 135.7 2_756
C12 H12A O18 0.97 2.59 3.31(2) 130.8 .
C12 H12C O20 0.97 2.36 3.19(2) 143.3 2_766
C12 H12B O5 0.97 2.62 3.36(2) 133.0 1_655
C12 H12C O20 0.97 2.36 3.19(2) 143.3 2_766
C12 H12D O26 0.97 2.32 3.11(2) 137.9 1_655
O1W H1D O16 0.821(10) 2.29(13) 2.797(15) 120(12) .
O1W H1D O29 0.821(10) 2.22(16) 2.796(14) 128(18) 2_655
O2W H2C N4 0.817(10) 2.589(11) 3.123(16) 124(2) 1_554
