#------------------------------------------------------------------------------
#$Date: 2022-02-20 01:47:46 +0200 (Sun, 20 Feb 2022) $
#$Revision: 273043 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/95/7709580.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_7709580
loop_
_publ_author_name
'Guan, Weiming'
'Li, Bao'
'Wu, Lixin'
_publ_section_title
;
 Chiral hexamers of organically modified polyoxometalates via ionic
 complexation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00093H
_journal_year                    2022
_chemical_formula_moiety
'Na3, 4(H2 O), 4(C3 H7 N O), 2(C H3 C N), Mn Mo6 O24 (C22 H21 N2 O2)2'
_chemical_formula_sum            'C60 H84 Mn Mo6 N10 Na3 O36'
_chemical_formula_weight         2220.92
_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
_atom_sites_solution_primary     heavy
_audit_creation_date             2022-02-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.088(4)
_cell_angle_beta                 95.059(4)
_cell_angle_gamma                99.731(4)
_cell_formula_units_Z            1
_cell_length_a                   9.3899(9)
_cell_length_b                   13.0933(13)
_cell_length_c                   16.5155(16)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.477
_cell_measurement_theta_min      2.628
_cell_volume                     1993.2(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker D8 Venture'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'Bruker APEX-II CCD'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'equatorial mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47040
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         2.628
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8969
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0369
_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)+(0.0236P)²+5.2567P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6794
_reflns_number_total             8969
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00093h2.cif
_cod_data_source_block           aa
_cod_database_code               7709580
_shelx_shelxl_version_number     2018/3
_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_max   0.757
_shelx_estimated_absorpt_t_min   0.538
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O15 \\sim N4 \\sim C25 \\sim C26 \\sim C27: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
O16 \\sim N5 \\sim C28 \\sim C29 \\sim C30: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
O16A \\sim N5A \\sim C28A \\sim C29A \\sim C30A: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004 within 2A
3. Others
 Sof(O16A)=Sof(N5A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(O16)=Sof(N5)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Fixed Sof: Na2(0.5)
4.a Free rotating group:
 O18(H18A,H18B)
4.b Rotating group:
 O17(H17A,H17B)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B)
4.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C18(H18),
 C19(H19), C20(H20), C21(H21), C25(H25), C28(H28), C28A(H28A)
4.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
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 1.16865(3) 0.29873(2) 0.00247(2) 0.01078(8) Uani 1 1 d . . . . .
Mo2 Mo 1.22615(3) 0.46144(2) 0.16374(2) 0.01086(8) Uani 1 1 d . . . . .
Mo3 Mo 1.04698(3) 0.66098(2) 0.16352(2) 0.01184(8) Uani 1 1 d . . . . .
Mn1 Mn 1.000000 0.500000 0.000000 0.00846(15) Uani 1 2 d S . P . .
Na1 Na 0.88595(18) 0.10110(13) 0.24429(11) 0.0241(4) Uani 1 1 d . . . . .
O1 O 1.1422(3) 0.33662(19) -0.10894(15) 0.0130(5) Uani 1 1 d . . . . .
O2 O 1.3508(3) 0.3001(2) 0.01080(16) 0.0176(6) Uani 1 1 d . . . . .
O3 O 1.0875(3) 0.1723(2) -0.00049(16) 0.0172(6) Uani 1 1 d . . . . .
O4 O 1.1416(3) 0.32841(19) 0.11436(15) 0.0122(5) Uani 1 1 d . . . . .
O5 O 0.9442(3) 0.35360(18) -0.01663(15) 0.0105(5) Uani 1 1 d . . . . .
O6 O 0.8009(3) 0.52319(19) -0.01719(15) 0.0110(5) Uani 1 1 d . . . . .
O7 O 0.9907(3) 0.48927(18) 0.12701(15) 0.0109(5) Uani 1 1 d . . . . .
O8 O 1.2002(3) 0.4341(2) 0.26250(16) 0.0170(6) Uani 1 1 d . . . . .
O9 O 1.4060(3) 0.4612(2) 0.15498(16) 0.0170(6) Uani 1 1 d . . . . .
O10 O 1.2252(3) 0.60725(19) 0.15830(15) 0.0135(5) Uani 1 1 d . . . . .
O11 O 1.1220(3) 0.7895(2) 0.16153(17) 0.0191(6) Uani 1 1 d . . . . .
O12 O 1.0050(3) 0.6390(2) 0.26053(16) 0.0184(6) Uani 1 1 d . . . . .
O13 O 0.7319(3) 0.1883(2) 0.17325(17) 0.0198(6) Uani 1 1 d . . . . .
O14 O 0.3208(3) 0.2066(2) 0.35211(18) 0.0253(7) Uani 1 1 d . . . . .
O15 O 0.8377(5) -0.0282(3) 0.1433(3) 0.0624(9) Uani 1 1 d . U . . .
O17 O 1.1214(3) 0.1576(2) 0.21634(17) 0.0199(6) Uani 1 1 d . . . . .
H17A H 1.125774 0.213702 0.187738 0.030 Uiso 1 1 d R U . . .
H17B H 1.174544 0.177029 0.261357 0.030 Uiso 1 1 d R U . . .
O18 O 0.8197(4) 0.0047(2) -0.10705(19) 0.0259(7) Uani 1 1 d G . . . .
H18A H 0.835157 0.066520 -0.127086 0.039 Uiso 1 1 d G U . B .
H18B H 0.842439 -0.035220 -0.144156 0.039 Uiso 1 1 d G U . B .
N1 N 0.6293(3) 0.3150(2) 0.10984(19) 0.0125(6) Uani 1 1 d . . . . .
H1 H 0.547481 0.339148 0.100719 0.015 Uiso 1 1 calc R U . . .
N2 N 0.5378(4) 0.1728(3) 0.31918(19) 0.0168(7) Uani 1 1 d . . . . .
H2 H 0.631318 0.180477 0.334122 0.020 Uiso 1 1 calc R U . . .
N3 N 0.8781(5) 0.2461(3) 0.3428(3) 0.0355(10) Uani 1 1 d . . . . .
N4 N 0.6297(6) -0.1487(4) 0.1369(4) 0.0581(8) Uani 1 1 d . U . . .
C1 C 0.8213(4) 0.3021(3) 0.0225(2) 0.0124(7) Uani 1 1 d . . . . .
H1A H 0.851049 0.245176 0.055824 0.015 Uiso 1 1 calc R U . . .
H1B H 0.744672 0.270926 -0.019593 0.015 Uiso 1 1 calc R U . . .
C2 C 0.8632(4) 0.4219(3) 0.1503(2) 0.0131(7) Uani 1 1 d . . . . .
H2A H 0.810863 0.461527 0.185300 0.016 Uiso 1 1 calc R U . . .
H2B H 0.893829 0.364660 0.182869 0.016 Uiso 1 1 calc R U . . .
C3 C 0.6958(4) 0.4587(3) 0.0266(2) 0.0124(7) Uani 1 1 d . . . . .
H3A H 0.616402 0.424153 -0.012702 0.015 Uiso 1 1 calc R U . . .
H3B H 0.653431 0.502975 0.063207 0.015 Uiso 1 1 calc R U . . .
C4 C 0.7582(4) 0.3753(3) 0.0773(2) 0.0110(7) Uani 1 1 d . . . . .
C5 C 0.6239(4) 0.2270(3) 0.1520(2) 0.0129(7) Uani 1 1 d . . . . .
C6 C 0.4738(4) 0.1767(3) 0.1716(2) 0.0157(8) Uani 1 1 d . . . . .
H6A H 0.425367 0.133117 0.124761 0.019 Uiso 1 1 calc R U . . .
H6B H 0.415277 0.231180 0.180726 0.019 Uiso 1 1 calc R U . . .
C7 C 0.4802(4) 0.1101(3) 0.2469(2) 0.0157(8) Uani 1 1 d . . . . .
H7A H 0.381571 0.072976 0.254768 0.019 Uiso 1 1 calc R U . . .
H7B H 0.542500 0.057626 0.238827 0.019 Uiso 1 1 calc R U . . .
C8 C 0.4540(4) 0.2190(3) 0.3637(2) 0.0170(8) Uani 1 1 d . . . . .
C9 C 0.5337(4) 0.2879(3) 0.4330(2) 0.0176(8) Uani 1 1 d . . . . .
C10 C 0.5502(4) 0.2468(3) 0.5101(2) 0.0195(8) Uani 1 1 d . . . . .
C11 C 0.5001(5) 0.1406(3) 0.5272(3) 0.0248(9) Uani 1 1 d . . . . .
H11 H 0.453951 0.094980 0.484339 0.030 Uiso 1 1 calc R U . . .
C12 C 0.5173(6) 0.1036(4) 0.6040(3) 0.0307(10) Uani 1 1 d . . . . .
H12 H 0.482564 0.032780 0.614079 0.037 Uiso 1 1 calc R U . . .
C13 C 0.5868(6) 0.1702(4) 0.6688(3) 0.0313(11) Uani 1 1 d . . . . .
H13 H 0.600172 0.143276 0.721798 0.038 Uiso 1 1 calc R U . . .
C14 C 0.6340(5) 0.2716(4) 0.6558(3) 0.0266(10) Uani 1 1 d . . . . .
H14 H 0.677746 0.315473 0.700208 0.032 Uiso 1 1 calc R U . . .
C15 C 0.6195(4) 0.3141(3) 0.5766(2) 0.0206(8) Uani 1 1 d . . . . .
C16 C 0.6663(5) 0.4186(3) 0.5621(3) 0.0230(9) Uani 1 1 d . . . . .
H16 H 0.709064 0.463161 0.606323 0.028 Uiso 1 1 calc R U . . .
C17 C 0.6521(5) 0.4598(3) 0.4845(3) 0.0221(9) Uani 1 1 d . . . . .
C18 C 0.6996(5) 0.5668(3) 0.4694(3) 0.0271(10) Uani 1 1 d . . . . .
H18 H 0.740231 0.612183 0.513450 0.033 Uiso 1 1 calc R U . . .
C19 C 0.6877(5) 0.6050(3) 0.3930(3) 0.0293(10) Uani 1 1 d . . . . .
H19 H 0.723445 0.675948 0.383929 0.035 Uiso 1 1 calc R U . . .
C20 C 0.6215(5) 0.5385(4) 0.3262(3) 0.0279(10) Uani 1 1 d . . . . .
H20 H 0.613396 0.565688 0.273036 0.034 Uiso 1 1 calc R U . . .
C21 C 0.5703(5) 0.4370(3) 0.3383(3) 0.0217(9) Uani 1 1 d . . . . .
H21 H 0.524692 0.394389 0.293614 0.026 Uiso 1 1 calc R U . . .
C22 C 0.5838(4) 0.3930(3) 0.4170(2) 0.0174(8) Uani 1 1 d . . . . .
C23 C 0.9167(5) 0.3311(4) 0.3621(3) 0.0264(10) Uani 1 1 d . . . . .
C24 C 0.9635(5) 0.4393(4) 0.3858(3) 0.0287(10) Uani 1 1 d . . . . .
H24A H 1.001942 0.443980 0.443071 0.043 Uiso 1 1 calc R U . . .
H24B H 0.880752 0.476053 0.378387 0.043 Uiso 1 1 calc R U . . .
H24C H 1.039320 0.470730 0.352004 0.043 Uiso 1 1 calc R U . . .
C25 C 0.7614(7) -0.1161(5) 0.1673(5) 0.0599(8) Uani 1 1 d . U . . .
H25 H 0.804505 -0.155797 0.207576 0.072 Uiso 1 1 calc R U . . .
C26 C 0.5525(8) -0.2501(5) 0.1582(4) 0.0585(11) Uani 1 1 d . U . . .
H26A H 0.601111 -0.274134 0.207720 0.088 Uiso 1 1 calc R U . . .
H26B H 0.552175 -0.299675 0.113573 0.088 Uiso 1 1 calc R U . . .
H26C H 0.452361 -0.244693 0.167433 0.088 Uiso 1 1 calc R U . . .
C27 C 0.5561(8) -0.0927(5) 0.0746(4) 0.0609(11) Uani 1 1 d . U . . .
H27A H 0.533649 -0.135240 0.024742 0.091 Uiso 1 1 calc R U . . .
H27B H 0.619285 -0.027634 0.063296 0.091 Uiso 1 1 calc R U . . .
H27C H 0.465953 -0.077432 0.093684 0.091 Uiso 1 1 calc R U . . .
O16 O 0.8268(8) -0.0070(5) 0.3492(5) 0.0509(15) Uani 0.682(9) 1 d . U P A 1
N5 N 0.9810(11) -0.1121(7) 0.4021(7) 0.0533(16) Uani 0.682(9) 1 d . U P A 1
C28 C 0.8624(10) -0.0678(7) 0.3991(6) 0.0513(15) Uani 0.682(9) 1 d . U P A 1
H28 H 0.799307 -0.085902 0.440621 0.062 Uiso 0.682(9) 1 calc R U P A 1
C29 C 1.0824(11) -0.0895(8) 0.3392(6) 0.056(2) Uani 0.682(9) 1 d . U P A 1
H29A H 1.034821 -0.058733 0.292395 0.084 Uiso 0.682(9) 1 calc R U P A 1
H29B H 1.112128 -0.153806 0.322053 0.084 Uiso 0.682(9) 1 calc R U P A 1
H29C H 1.168096 -0.040699 0.361183 0.084 Uiso 0.682(9) 1 calc R U P A 1
C30 C 1.0174(12) -0.1832(9) 0.4635(8) 0.063(2) Uani 0.682(9) 1 d . U P A 1
H30A H 0.944877 -0.191111 0.503191 0.095 Uiso 0.682(9) 1 calc R U P A 1
H30B H 1.113276 -0.156356 0.491008 0.095 Uiso 0.682(9) 1 calc R U P A 1
H30C H 1.019079 -0.250675 0.438140 0.095 Uiso 0.682(9) 1 calc R U P A 1
O16A O 0.8892(19) -0.0254(12) 0.3355(9) 0.050(3) Uani 0.318(9) 1 d . U P A 2
N5A N 0.964(2) -0.1404(15) 0.4229(11) 0.046(3) Uani 0.318(9) 1 d . U P A 2
C28A C 0.962(2) -0.0967(16) 0.3574(13) 0.048(3) Uani 0.318(9) 1 d . U P A 2
H28A H 1.020714 -0.117935 0.318675 0.058 Uiso 0.318(9) 1 calc R U P A 2
C29A C 0.892(2) -0.1195(15) 0.4931(11) 0.046(3) Uani 0.318(9) 1 d . U P A 2
H29D H 0.961875 -0.110913 0.541287 0.069 Uiso 0.318(9) 1 calc R U P A 2
H29E H 0.813945 -0.177621 0.500947 0.069 Uiso 0.318(9) 1 calc R U P A 2
H29F H 0.850904 -0.055956 0.484688 0.069 Uiso 0.318(9) 1 calc R U P A 2
C30A C 1.055(2) -0.2239(16) 0.4351(11) 0.044(3) Uani 0.318(9) 1 d . U P A 2
H30D H 1.094303 -0.237639 0.383783 0.065 Uiso 0.318(9) 1 calc R U P A 2
H30E H 0.995386 -0.287321 0.452582 0.065 Uiso 0.318(9) 1 calc R U P A 2
H30F H 1.135433 -0.201342 0.476699 0.065 Uiso 0.318(9) 1 calc R U P A 2
Na2 Na 0.9739(5) 0.0012(4) 0.0161(3) 0.0275(11) Uani 0.5 1 d . . P B -1
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'
Mn Mn 0.3368 0.7283 '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'
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'
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
O1 Mo1 O4 147.12(11) . . ?
O1 Mo1 O5 72.81(10) . . ?
O1 Mo1 O6 79.96(10) . 2_765 ?
O2 Mo1 O1 99.38(12) . . ?
O2 Mo1 O4 99.82(12) . . ?
O2 Mo1 O5 161.36(11) . . ?
O2 Mo1 O6 92.18(11) . 2_765 ?
O3 Mo1 O1 102.02(12) . . ?
O3 Mo1 O2 106.94(13) . . ?
O3 Mo1 O4 97.57(12) . . ?
O3 Mo1 O5 91.39(11) . . ?
O3 Mo1 O6 160.02(12) . 2_765 ?
O4 Mo1 O5 80.63(10) . . ?
O4 Mo1 O6 72.89(9) . 2_765 ?
O6 Mo1 O5 70.01(9) 2_765 . ?
O4 Mo2 O6 70.27(9) . 2_765 ?
O4 Mo2 O7 79.63(10) . . ?
O7 Mo2 O6 72.38(9) . 2_765 ?
O8 Mo2 O4 99.31(12) . . ?
O8 Mo2 O6 165.14(11) . 2_765 ?
O8 Mo2 O7 95.73(11) . . ?
O8 Mo2 O9 105.80(13) . . ?
O8 Mo2 O10 103.42(12) . . ?
O9 Mo2 O4 100.63(12) . . ?
O9 Mo2 O6 86.94(11) . 2_765 ?
O9 Mo2 O7 158.04(11) . . ?
O9 Mo2 O10 99.50(12) . . ?
O10 Mo2 O4 144.05(10) . . ?
O10 Mo2 O6 81.45(10) . 2_765 ?
O10 Mo2 O7 70.77(10) . . ?
O1 Mo3 O5 70.08(10) 2_765 2_765 ?
O1 Mo3 O7 82.18(10) 2_765 . ?
O1 Mo3 O10 144.33(11) 2_765 . ?
O7 Mo3 O5 71.80(8) . 2_765 ?
O10 Mo3 O5 78.97(10) . 2_765 ?
O10 Mo3 O7 71.43(10) . . ?
O11 Mo3 O1 100.73(12) . 2_765 ?
O11 Mo3 O5 90.37(11) . 2_765 ?
O11 Mo3 O7 159.93(12) . . ?
O11 Mo3 O10 96.68(12) . . ?
O12 Mo3 O1 100.91(12) . 2_765 ?
O12 Mo3 O5 163.28(11) . 2_765 ?
O12 Mo3 O7 93.38(11) . . ?
O12 Mo3 O10 104.11(12) . . ?
O12 Mo3 O11 105.40(13) . . ?
O5 Mn1 O5 180.0 . 2_765 ?
O5 Mn1 O6 87.49(10) . 2_765 ?
O5 Mn1 O6 92.51(10) 2_765 2_765 ?
O5 Mn1 O6 92.51(10) . . ?
O5 Mn1 O6 87.49(10) 2_765 . ?
O5 Mn1 O7 87.15(10) . 2_765 ?
O5 Mn1 O7 92.85(10) . . ?
O5 Mn1 O7 87.15(10) 2_765 . ?
O5 Mn1 O7 92.85(10) 2_765 2_765 ?
O6 Mn1 O6 180.0 . 2_765 ?
O6 Mn1 O7 92.41(10) 2_765 2_765 ?
O6 Mn1 O7 87.59(10) . 2_765 ?
O6 Mn1 O7 92.41(10) . . ?
O6 Mn1 O7 87.59(10) 2_765 . ?
O7 Mn1 O7 180.0 2_765 . ?
O13 Na1 O15 88.97(16) . . ?
O13 Na1 O17 111.46(12) . . ?
O13 Na1 N3 79.35(13) . . ?
O13 Na1 O16 124.8(2) . . ?
O15 Na1 N3 166.53(17) . . ?
O17 Na1 O15 95.20(15) . . ?
O17 Na1 N3 95.29(14) . . ?
O16 Na1 O15 95.6(2) . . ?
O16 Na1 O17 122.7(2) . . ?
O16 Na1 N3 85.8(2) . . ?
O16A Na1 O13 141.2(5) . . ?
O16A Na1 O15 87.5(4) . . ?
O16A Na1 O17 107.3(5) . . ?
O16A Na1 N3 97.3(4) . . ?
Mo1 O1 Mo3 122.13(14) . 2_765 ?
Mo1 O3 Na2 171.51(19) . . ?
Mo2 O4 Mo1 120.28(13) . . ?
Mo1 O5 Mo3 89.29(9) . 2_765 ?
Mn1 O5 Mo1 101.25(10) . . ?
Mn1 O5 Mo3 100.87(10) . 2_765 ?
C1 O5 Mo1 121.0(2) . . ?
C1 O5 Mo3 121.1(2) . 2_765 ?
C1 O5 Mn1 117.9(2) . . ?
Mo1 O6 Mo2 90.27(8) 2_765 2_765 ?
Mn1 O6 Mo1 101.24(10) . 2_765 ?
Mn1 O6 Mo2 100.96(10) . 2_765 ?
C3 O6 Mo1 119.8(2) . 2_765 ?
C3 O6 Mo2 122.5(2) . 2_765 ?
C3 O6 Mn1 116.9(2) . . ?
Mo3 O7 Mo2 92.59(8) . . ?
Mn1 O7 Mo2 99.08(10) . . ?
Mn1 O7 Mo3 100.11(10) . . ?
C2 O7 Mo2 123.3(2) . . ?
C2 O7 Mo3 123.1(2) . . ?
C2 O7 Mn1 113.61(19) . . ?
Mo2 O10 Mo3 120.56(13) . . ?
C5 O13 Na1 161.8(3) . . ?
Na1 O15 Na2 117.7(2) . . ?
C25 O15 Na1 113.3(4) . . ?
C25 O15 Na2 127.8(4) . . ?
Na1 O17 H17A 109.5 . . ?
Na1 O17 H17B 109.4 . . ?
H17A O17 H17B 104.5 . . ?
H18A O18 H18B 104.7 . . ?
Na2 O18 H18A 109.1 . . ?
Na2 O18 H18B 110.9 . . ?
C4 N1 H1 116.7 . . ?
C5 N1 H1 116.7 . . ?
C5 N1 C4 126.6(3) . . ?
C7 N2 H2 118.7 . . ?
C8 N2 H2 118.7 . . ?
C8 N2 C7 122.6(3) . . ?
C23 N3 Na1 148.2(4) . . ?
C25 N4 C26 120.7(7) . . ?
C25 N4 C27 122.7(6) . . ?
C27 N4 C26 116.4(5) . . ?
O5 C1 H1A 109.0 . . ?
O5 C1 H1B 109.0 . . ?
O5 C1 C4 113.0(3) . . ?
H1A C1 H1B 107.8 . . ?
C4 C1 H1A 109.0 . . ?
C4 C1 H1B 109.0 . . ?
O7 C2 H2A 108.9 . . ?
O7 C2 H2B 108.9 . . ?
O7 C2 C4 113.5(3) . . ?
H2A C2 H2B 107.7 . . ?
C4 C2 H2A 108.9 . . ?
C4 C2 H2B 108.9 . . ?
O6 C3 H3A 108.8 . . ?
O6 C3 H3B 108.8 . . ?
O6 C3 C4 113.8(3) . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
N1 C4 C1 107.7(3) . . ?
N1 C4 C2 107.6(3) . . ?
N1 C4 C3 103.3(3) . . ?
C1 C4 C2 114.2(3) . . ?
C3 C4 C1 110.8(3) . . ?
C3 C4 C2 112.5(3) . . ?
O13 C5 N1 123.4(3) . . ?
O13 C5 C6 121.4(3) . . ?
N1 C5 C6 115.2(3) . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
C5 C6 C7 111.5(3) . . ?
H6A C6 H6B 108.0 . . ?
C7 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
N2 C7 C6 111.3(3) . . ?
N2 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
O14 C8 N2 124.0(4) . . ?
O14 C8 C9 120.6(4) . . ?
N2 C8 C9 115.4(3) . . ?
C10 C9 C8 119.4(4) . . ?
C10 C9 C22 122.3(4) . . ?
C22 C9 C8 118.3(3) . . ?
C9 C10 C11 123.0(4) . . ?
C9 C10 C15 119.1(4) . . ?
C11 C10 C15 118.0(4) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 C10 121.1(4) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.5(4) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.5(4) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.2(4) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 C10 118.7(4) . . ?
C16 C15 C10 119.2(4) . . ?
C16 C15 C14 122.1(4) . . ?
C15 C16 H16 119.1 . . ?
C15 C16 C17 121.9(4) . . ?
C17 C16 H16 119.1 . . ?
C16 C17 C18 122.1(4) . . ?
C16 C17 C22 119.4(4) . . ?
C18 C17 C22 118.4(4) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 C17 121.2(4) . . ?
C19 C18 H18 119.4 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.2(4) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.5(4) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 119.4 . . ?
C20 C21 C22 121.2(4) . . ?
C22 C21 H21 119.4 . . ?
C9 C22 C17 118.0(4) . . ?
C9 C22 C21 123.6(4) . . ?
C21 C22 C17 118.4(4) . . ?
N3 C23 C24 179.1(5) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O15 C25 H25 119.3 . . ?
N4 C25 O15 121.5(7) . . ?
N4 C25 H25 119.3 . . ?
N4 C26 H26A 109.5 . . ?
N4 C26 H26B 109.5 . . ?
N4 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N4 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
N4 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C28 O16 Na1 148.7(7) . . ?
C28 N5 C29 119.6(9) . . ?
C28 N5 C30 124.3(10) . . ?
C30 N5 C29 116.1(9) . . ?
O16 C28 N5 127.1(10) . . ?
O16 C28 H28 116.5 . . ?
N5 C28 H28 116.5 . . ?
N5 C29 H29A 109.5 . . ?
N5 C29 H29B 109.5 . . ?
N5 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N5 C30 H30A 109.5 . . ?
N5 C30 H30B 109.5 . . ?
N5 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28A O16A Na1 140.6(15) . . ?
C28A N5A C29A 128(2) . . ?
C28A N5A C30A 118(2) . . ?
C29A N5A C30A 114.1(17) . . ?
O16A C28A H28A 116.5 . . ?
N5A C28A O16A 127(2) . . ?
N5A C28A H28A 116.5 . . ?
N5A C29A H29D 109.5 . . ?
N5A C29A H29E 109.5 . . ?
N5A C29A H29F 109.5 . . ?
H29D C29A H29E 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
N5A C30A H30D 109.5 . . ?
N5A C30A H30E 109.5 . . ?
N5A C30A H30F 109.5 . . ?
H30D C30A H30E 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
O3 Na2 O15 114.6(2) . . ?
O3 Na2 O18 91.9(2) . . ?
O3 Na2 H18B 77(7) . 2_755 ?
O15 Na2 H18B 71(8) . 2_755 ?
O18 Na2 O15 114.0(2) . . ?
O18 Na2 H18B 169(6) . 2_755 ?
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
Mo1 O1 1.912(3) . ?
Mo1 O2 1.701(3) . ?
Mo1 O3 1.700(3) . ?
Mo1 O4 1.935(3) . ?
Mo1 O5 2.335(3) . ?
Mo1 O6 2.310(2) 2_765 ?
Mo2 O4 1.935(2) . ?
Mo2 O6 2.424(2) 2_765 ?
Mo2 O7 2.329(2) . ?
Mo2 O8 1.700(3) . ?
Mo2 O9 1.708(3) . ?
Mo2 O10 1.913(3) . ?
Mo3 O1 1.925(3) 2_765 ?
Mo3 O5 2.443(2) 2_765 ?
Mo3 O7 2.288(2) . ?
Mo3 O10 1.930(3) . ?
Mo3 O11 1.712(3) . ?
Mo3 O12 1.697(3) . ?
Mn1 O5 1.913(2) . ?
Mn1 O5 1.913(2) 2_765 ?
Mn1 O6 1.941(3) . ?
Mn1 O6 1.941(3) 2_765 ?
Mn1 O7 2.111(3) 2_765 ?
Mn1 O7 2.111(3) . ?
Na1 O13 2.244(3) . ?
Na1 O15 2.336(4) . ?
Na1 O17 2.297(3) . ?
Na1 N3 2.513(5) . ?
Na1 O16 2.286(7) . ?
Na1 O16A 2.242(15) . ?
O3 Na2 2.340(6) . ?
O5 C1 1.440(4) . ?
O6 C3 1.434(4) . ?
O7 C2 1.445(4) . ?
O13 C5 1.234(5) . ?
O14 C8 1.232(5) . ?
O15 C25 1.329(8) . ?
O15 Na2 2.550(6) . ?
O17 H17A 0.8715 . ?
O17 H17B 0.8705 . ?
O18 H18A 0.8691 . ?
O18 H18B 0.8685 . ?
O18 Na2 2.396(6) . ?
N1 H1 0.8800 . ?
N1 C4 1.473(5) . ?
N1 C5 1.343(5) . ?
N2 H2 0.8800 . ?
N2 C7 1.458(5) . ?
N2 C8 1.336(5) . ?
N3 C23 1.147(6) . ?
N4 C25 1.294(8) . ?
N4 C26 1.461(8) . ?
N4 C27 1.458(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C4 1.540(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C4 1.543(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.540(5) . ?
C5 C6 1.514(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.523(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.517(5) . ?
C9 C10 1.389(6) . ?
C9 C22 1.411(6) . ?
C10 C11 1.427(6) . ?
C10 C15 1.443(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.364(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.420(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.350(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.427(6) . ?
C15 C16 1.393(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.396(6) . ?
C17 C18 1.425(6) . ?
C17 C22 1.448(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.359(7) . ?
C19 H19 0.9500 . ?
C19 C20 1.434(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.356(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.427(6) . ?
C23 C24 1.452(7) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O16 C28 1.212(10) . ?
N5 C28 1.337(13) . ?
N5 C29 1.468(14) . ?
N5 C30 1.435(13) . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O16A C28A 1.28(3) . ?
N5A C28A 1.23(3) . ?
N5A C29A 1.44(3) . ?
N5A C30A 1.50(3) . ?
C28A H28A 0.9500 . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 0.9800 . ?
C30A H30D 0.9800 . ?
C30A H30E 0.9800 . ?
C30A H30F 0.9800 . ?
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
O17 H17A O4 0.87 1.93 2.793(4) 173.3 . yes
O17 H17B O14 0.87 1.93 2.792(4) 168.5 1_655 yes
O18 H18A O11 0.87 1.96 2.823(4) 174.4 2_765 yes
O18 H18B O17 0.87 2.09 2.939(4) 167.2 2_755 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
Mo1 O5 C1 C4 121.7(3) . . . . ?
Mo1 O6 C3 C4 -126.4(3) 2_765 . . . ?
Mo2 O6 C3 C4 121.8(3) 2_765 . . . ?
Mo2 O7 C2 C4 -121.7(3) . . . . ?
Mo3 O5 C1 C4 -128.1(2) 2_765 . . . ?
Mo3 O7 C2 C4 118.8(3) . . . . ?
Mn1 O5 C1 C4 -3.4(4) . . . . ?
Mn1 O6 C3 C4 -3.5(4) . . . . ?
Mn1 O7 C2 C4 -2.1(4) . . . . ?
Na1 O13 C5 N1 149.4(7) . . . . ?
Na1 O13 C5 C6 -31.1(11) . . . . ?
Na1 O15 C25 N4 112.5(6) . . . . ?
Na1 O16 C28 N5 -12(2) . . . . ?
Na1 O16A C28A N5A 159.8(17) . . . . ?
O5 C1 C4 N1 176.9(3) . . . . ?
O5 C1 C4 C2 -63.7(4) . . . . ?
O5 C1 C4 C3 64.6(4) . . . . ?
O6 C3 C4 N1 -175.3(3) . . . . ?
O6 C3 C4 C1 -60.3(4) . . . . ?
O6 C3 C4 C2 68.9(4) . . . . ?
O7 C2 C4 N1 -175.9(3) . . . . ?
O7 C2 C4 C1 64.6(4) . . . . ?
O7 C2 C4 C3 -62.8(4) . . . . ?
O13 C5 C6 C7 25.7(5) . . . . ?
O14 C8 C9 C10 85.1(5) . . . . ?
O14 C8 C9 C22 -92.6(5) . . . . ?
N1 C5 C6 C7 -154.8(3) . . . . ?
N2 C8 C9 C10 -93.4(5) . . . . ?
N2 C8 C9 C22 88.9(5) . . . . ?
C4 N1 C5 O13 4.6(6) . . . . ?
C4 N1 C5 C6 -174.9(3) . . . . ?
C5 N1 C4 C1 55.9(4) . . . . ?
C5 N1 C4 C2 -67.6(4) . . . . ?
C5 N1 C4 C3 173.2(3) . . . . ?
C5 C6 C7 N2 64.6(4) . . . . ?
C7 N2 C8 O14 6.1(6) . . . . ?
C7 N2 C8 C9 -175.5(3) . . . . ?
C8 N2 C7 C6 86.4(4) . . . . ?
C8 C9 C10 C11 2.4(6) . . . . ?
C8 C9 C10 C15 -176.8(4) . . . . ?
C8 C9 C22 C17 176.4(4) . . . . ?
C8 C9 C22 C21 -3.3(6) . . . . ?
C9 C10 C11 C12 -179.4(4) . . . . ?
C9 C10 C15 C14 179.0(4) . . . . ?
C9 C10 C15 C16 0.8(6) . . . . ?
C10 C9 C22 C17 -1.2(6) . . . . ?
C10 C9 C22 C21 179.0(4) . . . . ?
C10 C11 C12 C13 -0.4(7) . . . . ?
C10 C15 C16 C17 -2.0(6) . . . . ?
C11 C10 C15 C14 -0.2(6) . . . . ?
C11 C10 C15 C16 -178.4(4) . . . . ?
C11 C12 C13 C14 1.4(8) . . . . ?
C12 C13 C14 C15 -1.8(7) . . . . ?
C13 C14 C15 C10 1.2(6) . . . . ?
C13 C14 C15 C16 179.4(4) . . . . ?
C14 C15 C16 C17 179.9(4) . . . . ?
C15 C10 C11 C12 -0.2(6) . . . . ?
C15 C16 C17 C18 179.9(4) . . . . ?
C15 C16 C17 C22 1.5(6) . . . . ?
C16 C17 C18 C19 178.5(4) . . . . ?
C16 C17 C22 C9 0.1(6) . . . . ?
C16 C17 C22 C21 179.9(4) . . . . ?
C17 C18 C19 C20 2.4(7) . . . . ?
C18 C17 C22 C9 -178.3(4) . . . . ?
C18 C17 C22 C21 1.4(6) . . . . ?
C18 C19 C20 C21 -0.1(7) . . . . ?
C19 C20 C21 C22 -1.5(7) . . . . ?
C20 C21 C22 C9 -179.5(4) . . . . ?
C20 C21 C22 C17 0.8(6) . . . . ?
C22 C9 C10 C11 180.0(4) . . . . ?
C22 C9 C10 C15 0.8(6) . . . . ?
C22 C17 C18 C19 -3.1(7) . . . . ?
C26 N4 C25 O15 174.0(5) . . . . ?
C27 N4 C25 O15 0.4(10) . . . . ?
C29 N5 C28 O16 -1.1(17) . . . . ?
C30 N5 C28 O16 179.6(11) . . . . ?
C29A N5A C28A O16A -3(4) . . . . ?
C30A N5A C28A O16A 179(2) . . . . ?
Na2 O15 C25 N4 -80.7(8) . . . . ?
