# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_exp_17643
_database_code_depnum_ccdc_archive 'CCDC 1814436'
_audit_update_record             
;
2018-04-13 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_audit_creation_date             2018-04-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C19 H24 Mo3 N10 O9 S'
_chemical_formula_sum            'C19 H24 Mo3 N10 O9 S'
_chemical_formula_weight         856.36
_chemical_melting_point          ?
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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6290(3)
_cell_length_b                   12.1305(4)
_cell_length_c                   17.0785(6)
_cell_angle_alpha                109.173(3)
_cell_angle_beta                 104.625(3)
_cell_angle_gamma                90.077(3)
_cell_volume                     1626.85(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6830
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.6780
_cell_measurement_theta_min      2.5020
_shelx_estimated_absorpt_T_max   0.951
_shelx_estimated_absorpt_T_min   0.704
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25698
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.916
_diffrn_reflns_theta_min         2.449
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -59.00  10.00   1.00   22.50    --  -22.85 -77.00 -90.00   69
  2  ω    -91.00  31.00   1.00   22.50    --  -22.85 -19.00 150.00  122
  3  ω    -93.00 -65.00   1.00   22.50    --  -22.85 -57.00 150.00   28
  4  ω    -47.00  -1.00   1.00   22.50    --  -22.85 -57.00 150.00   46
  5  ω    -55.00  40.00   1.00   22.50    --  -22.85  77.00-150.00   95
  6  ω    -47.00  40.00   1.00   22.50    --  -22.85  57.00 -30.00   87
  7  ω    -51.00  50.00   1.00   22.50    --  -22.85  77.00 120.00  101
  8  ω    -92.00  10.00   1.00   22.50    --  -22.85 -77.00  90.00  102
  9  ω    -77.00  -2.00   1.00   22.50    --  -22.85 -57.00 -30.00   75
 10  ω     -4.00  69.00   1.00   22.50    --   24.10 -99.00  60.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0564673000
_diffrn_orient_matrix_UB_12      0.0500537000
_diffrn_orient_matrix_UB_13      0.0164092000
_diffrn_orient_matrix_UB_21      -0.0550534000
_diffrn_orient_matrix_UB_22      0.0289608000
_diffrn_orient_matrix_UB_23      -0.0232158000
_diffrn_orient_matrix_UB_31      -0.0325448000
_diffrn_orient_matrix_UB_32      0.0228268000
_diffrn_orient_matrix_UB_33      0.0357004000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6895
_reflns_number_total             8418
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8418
_refine_ls_number_restraints     181
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0388
_refine_ls_restrained_S_all      1.043
_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)+(0.0396P)²+0.1148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0913
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N8-H8
 0.88 with sigma of 0.01
 N4-H4
 0.88 with sigma of 0.01
 N1-C5 \\sim N1-C5A
 with sigma of 0.02
 C4-C5 \\sim C4-C5A
 with sigma of 0.02
 N2-C4 \\sim N2-C4A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5
 with sigma of 0.02
 C4-C5A \\sim C4A-C5A
 with sigma of 0.02
 C4A-C5A \\sim C4-C5
 with sigma of 0.01
3. Rigid bond restraints
 O5, C2, O7, C6, N1, N3, C10, N6, C12, N9, C19, N10, C18, C4, N2, N2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O3 \\sim O2 \\sim O1 \\sim O4 \\sim O5 \\sim O8 \\sim O7 \\sim O6 \\sim O9:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.01
C4 \\sim C4A \\sim C5 \\sim C5A: within 3.8A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.01
5. Others
 Sof(H2B)=Sof(C4A)=Sof(H4AA)=1-FVAR(1)
 Sof(H2A)=Sof(C4)=Sof(H4A)=FVAR(1)
 Fixed Sof: C5(0.7) H5(0.7) C5A(0.3) H5A(0.3)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2A), N2(H2B), N6(H6), N10(H10), C14(H14), C12(H12), C8(H8A), C17(H17),
 C3(H3), C4(H4A), C11(H11), C13(H13), C16(H16), C15(H15), C9(H9), C19(H19),
 C10(H10A), C18(H18), C5(H5), C5A(H5A), C4A(H4AA)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Mo2 Mo 0.41419(3) 0.74136(3) 0.73278(2) 0.02074(8) Uani 1 1 d . . . . .
Mo1 Mo 0.64628(3) 0.68534(3) 0.84186(2) 0.02004(8) Uani 1 1 d . . . . .
Mo3 Mo 0.42288(3) 0.52614(2) 0.73199(2) 0.01988(8) Uani 1 1 d . . . . .
S1 S 0.37762(10) 0.68524(7) 0.84726(5) 0.02138(17) Uani 1 1 d . . . . .
O3 O 0.6530(3) 0.5341(2) 0.75902(14) 0.0222(5) Uani 1 1 d . U . . .
O2 O 0.3975(3) 0.5929(2) 0.64214(14) 0.0234(5) Uani 1 1 d . U . . .
O1 O 0.6462(3) 0.7635(2) 0.75917(14) 0.0227(5) Uani 1 1 d . U . . .
O4 O 0.6998(3) 0.6344(2) 0.94396(14) 0.0269(5) Uani 1 1 d . U . . .
O5 O 0.9012(3) 0.6957(2) 0.87095(15) 0.0284(5) Uani 1 1 d . U . . .
O8 O 0.4100(3) 0.8217(2) 0.63862(15) 0.0306(6) Uani 1 1 d . U . . .
O7 O 0.3807(3) 0.9062(2) 0.79384(15) 0.0329(6) Uani 1 1 d . U . . .
N7 N 0.4417(3) 0.3643(3) 0.62912(17) 0.0250(6) Uani 1 1 d . . . . .
N9 N 0.1672(4) 0.4635(3) 0.69687(19) 0.0295(7) Uani 1 1 d . U . . .
N2 N 0.7008(4) 1.0118(3) 1.05676(19) 0.0323(7) Uani 1 1 d D U . . .
H2A H 0.7030 1.0498 1.1107 0.039 Uiso 0.34(8) 1 calc R . P A 1
H2B H 0.6812 1.0526 1.1058 0.039 Uiso 0.66(8) 1 calc R . P A 2
N1 N 0.6921(4) 0.8648(3) 0.93969(18) 0.0273(6) Uani 1 1 d D U . . .
N6 N 0.4343(4) 0.3682(3) 0.92874(19) 0.0332(7) Uani 1 1 d . U . . .
H6 H 0.4016 0.3614 0.9719 0.040 Uiso 1 1 calc R . . . .
N5 N 0.4452(3) 0.4189(3) 0.81796(18) 0.0254(6) Uani 1 1 d . . . . .
N8 N 0.5061(4) 0.2562(3) 0.5125(2) 0.0331(7) Uani 1 1 d D . . . .
N3 N 0.1447(4) 0.7272(3) 0.68233(19) 0.0324(7) Uani 1 1 d . U . . .
O6 O 1.1156(3) 0.6466(3) 0.9517(2) 0.0545(8) Uani 1 1 d . U . . .
N10 N -0.0853(4) 0.4505(3) 0.6981(2) 0.0435(9) Uani 1 1 d . U . . .
H10 H -0.1743 0.4667 0.7141 0.052 Uiso 1 1 calc R . . . .
C14 C 0.4947(4) 0.3644(3) 0.5619(2) 0.0284(8) Uani 1 1 d . . . . .
H14 H 0.5208 0.4331 0.5510 0.034 Uiso 1 1 calc R . . . .
C12 C 0.5633(5) 0.3203(4) 0.9023(3) 0.0389(9) Uani 1 1 d . U . . .
H12 H 0.6353 0.2742 0.9271 0.047 Uiso 1 1 calc R . . . .
N4 N -0.1107(4) 0.7328(4) 0.6781(2) 0.0470(10) Uani 1 1 d D . . . .
C8 C 0.0376(4) 0.7617(4) 0.7268(2) 0.0339(9) Uani 1 1 d . . . . .
H8A H 0.0649 0.8027 0.7870 0.041 Uiso 1 1 calc R . . . .
O9 O 0.3769(5) 0.9866(3) 0.6117(2) 0.0746(11) Uani 1 1 d . U . . .
C17 C 0.0573(4) 0.5058(3) 0.7389(2) 0.0312(8) Uani 1 1 d . . . . .
H17 H 0.0800 0.5687 0.7922 0.037 Uiso 1 1 calc R . . . .
C2 C 0.9710(4) 0.6561(4) 0.9309(2) 0.0338(8) Uani 1 1 d . U . . .
C3 C 0.6529(5) 0.8999(3) 1.0122(2) 0.0330(8) Uani 1 1 d . U . . .
H3 H 0.5962 0.8508 1.0310 0.040 Uiso 1 1 calc R . . . .
C4 C 0.746(4) 1.0556(11) 1.0006(13) 0.039(4) Uani 0.34(8) 1 d D U P A 1
H4A H 0.7695 1.1360 1.0095 0.047 Uiso 0.34(8) 1 calc R . P A 1
C11 C 0.3672(4) 0.4268(3) 0.8775(2) 0.0303(8) Uani 1 1 d . . . . .
H11 H 0.2754 0.4690 0.8826 0.036 Uiso 1 1 calc R . . . .
C13 C 0.5684(5) 0.3511(4) 0.8348(3) 0.0382(9) Uani 1 1 d . . . . .
H13 H 0.6459 0.3293 0.8030 0.046 Uiso 1 1 calc R . . . .
C1 C 0.8609(5) 0.6139(4) 0.9741(3) 0.0450(11) Uani 1 1 d . U . . .
H1A H 0.8676 0.5289 0.9630 0.054 Uiso 1 1 calc R . . . .
H1B H 0.8980 0.6548 1.0370 0.054 Uiso 1 1 calc R . . . .
C16 C 0.4218(6) 0.2485(4) 0.6206(3) 0.0464(11) Uani 1 1 d . . . . .
H16 H 0.3854 0.2194 0.6588 0.056 Uiso 1 1 calc R . . . .
C15 C 0.4627(6) 0.1811(4) 0.5481(3) 0.0476(11) Uani 1 1 d . . . . .
H15 H 0.4609 0.0981 0.5271 0.057 Uiso 1 1 calc R . . . .
C9 C -0.1026(6) 0.6661(6) 0.5976(3) 0.0692(16) Uani 1 1 d . U . . .
H9 H -0.1905 0.6285 0.5491 0.083 Uiso 1 1 calc R . . . .
C19 C 0.0837(5) 0.3697(4) 0.6261(3) 0.0592(14) Uani 1 1 d . U . . .
H19 H 0.1287 0.3181 0.5841 0.071 Uiso 1 1 calc R . . . .
C7 C 0.3827(6) 0.9300(4) 0.6590(3) 0.0454(11) Uani 1 1 d . . . . .
C10 C 0.0566(5) 0.6642(5) 0.6007(3) 0.0655(16) Uani 1 1 d . U . . .
H10A H 0.0994 0.6255 0.5537 0.079 Uiso 1 1 calc R . . . .
C18 C -0.0719(6) 0.3640(5) 0.6270(3) 0.0660(15) Uani 1 1 d . U . . .
H18 H -0.1563 0.3094 0.5853 0.079 Uiso 1 1 calc R . . . .
C6 C 0.3611(7) 0.9840(4) 0.7489(3) 0.0539(13) Uani 1 1 d . U . . .
H6A H 0.4401 1.0532 0.7813 0.065 Uiso 1 1 calc R . . . .
H6B H 0.2521 1.0112 0.7446 0.065 Uiso 1 1 calc R . . . .
H8 H 0.540(4) 0.233(3) 0.4655(15) 0.036(11) Uiso 1 1 d D . . . .
H4 H -0.208(3) 0.730(5) 0.685(3) 0.078(18) Uiso 1 1 d D . . . .
C5 C 0.7521(9) 0.9659(6) 0.9316(4) 0.039(2) Uani 0.7 1 d D U P A 1
H5 H 0.7904 0.9699 0.8851 0.047 Uiso 0.7 1 calc R . P A 1
C5A C 0.8056(19) 0.9542(11) 0.9545(11) 0.037(4) Uani 0.3 1 d D U P A 2
H5A H 0.8884 0.9466 0.9261 0.044 Uiso 0.3 1 calc R . P A 2
C4A C 0.785(4) 1.0523(9) 1.0134(13) 0.057(3) Uani 0.66(8) 1 d D U P A 2
H4AA H 0.8212 1.1309 1.0227 0.069 Uiso 0.66(8) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Mo2 Mo1 2.6257(4) . ?
Mo2 Mo3 2.6075(4) . ?
Mo2 S1 2.3604(8) . ?
Mo2 O2 1.927(2) . ?
Mo2 O1 1.936(2) . ?
Mo2 O8 2.130(2) . ?
Mo2 O7 1.988(2) . ?
Mo2 N3 2.251(3) . ?
Mo1 Mo3 2.5980(4) . ?
Mo1 S1 2.3433(8) . ?
Mo1 O3 1.926(2) . ?
Mo1 O1 1.942(2) . ?
Mo1 O4 1.984(2) . ?
Mo1 O5 2.123(2) . ?
Mo1 N1 2.228(3) . ?
Mo3 S1 2.3764(8) . ?
Mo3 O3 1.916(2) . ?
Mo3 O2 1.925(2) . ?
Mo3 N7 2.201(3) . ?
Mo3 N9 2.198(3) . ?
Mo3 N5 2.236(3) . ?
O4 C1 1.408(4) . ?
O5 C2 1.286(4) . ?
O8 C7 1.283(5) . ?
O7 C6 1.386(5) . ?
N7 C14 1.339(4) . ?
N7 C16 1.370(5) . ?
N9 C17 1.335(4) . ?
N9 C19 1.389(5) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N2 C3 1.324(5) . ?
N2 C4 1.371(14) . ?
N2 C4A 1.354(9) . ?
N1 C3 1.302(4) . ?
N1 C5 1.391(7) . ?
N1 C5A 1.375(14) . ?
N6 H6 0.8800 . ?
N6 C12 1.365(5) . ?
N6 C11 1.327(5) . ?
N5 C11 1.334(4) . ?
N5 C13 1.376(5) . ?
N8 C14 1.326(5) . ?
N8 C15 1.348(5) . ?
N8 H8 0.881(10) . ?
N3 C8 1.324(4) . ?
N3 C10 1.368(5) . ?
O6 C2 1.225(4) . ?
N10 H10 0.8800 . ?
N10 C17 1.307(5) . ?
N10 C18 1.350(5) . ?
C14 H14 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.333(5) . ?
N4 C8 1.312(5) . ?
N4 C9 1.368(6) . ?
N4 H4 0.875(10) . ?
C8 H8A 0.9500 . ?
O9 C7 1.213(5) . ?
C17 H17 0.9500 . ?
C2 C1 1.519(5) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9500 . ?
C4 C5 1.328(9) . ?
C11 H11 0.9500 . ?
C13 H13 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C16 H16 0.9500 . ?
C16 C15 1.372(5) . ?
C15 H15 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.362(6) . ?
C19 H19 0.9500 . ?
C19 C18 1.348(6) . ?
C7 C6 1.517(5) . ?
C10 H10A 0.9500 . ?
C18 H18 0.9500 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C5 H5 0.9500 . ?
C5A H5A 0.9500 . ?
C5A C4A 1.327(9) . ?
C4A H4AA 0.9500 . ?

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
Mo3 Mo2 Mo1 59.527(11) . . ?
S1 Mo2 Mo1 55.76(2) . . ?
S1 Mo2 Mo3 56.89(2) . . ?
O2 Mo2 Mo1 93.83(7) . . ?
O2 Mo2 Mo3 47.37(7) . . ?
O2 Mo2 S1 102.68(7) . . ?
O2 Mo2 O1 94.05(9) . . ?
O2 Mo2 O8 87.04(9) . . ?
O2 Mo2 O7 160.62(10) . . ?
O2 Mo2 N3 84.23(11) . . ?
O1 Mo2 Mo1 47.49(7) . . ?
O1 Mo2 Mo3 91.86(7) . . ?
O1 Mo2 S1 102.07(7) . . ?
O1 Mo2 O8 86.16(10) . . ?
O1 Mo2 O7 96.86(10) . . ?
O1 Mo2 N3 169.64(10) . . ?
O8 Mo2 Mo1 133.62(7) . . ?
O8 Mo2 Mo3 134.16(7) . . ?
O8 Mo2 S1 166.63(7) . . ?
O8 Mo2 N3 83.56(10) . . ?
O7 Mo2 Mo1 105.35(8) . . ?
O7 Mo2 Mo3 147.53(7) . . ?
O7 Mo2 S1 90.67(7) . . ?
O7 Mo2 O8 77.79(9) . . ?
O7 Mo2 N3 82.17(12) . . ?
N3 Mo2 Mo1 142.73(8) . . ?
N3 Mo2 Mo3 94.42(9) . . ?
N3 Mo2 S1 88.26(8) . . ?
Mo3 Mo1 Mo2 59.889(11) . . ?
S1 Mo1 Mo2 56.38(2) . . ?
S1 Mo1 Mo3 57.21(2) . . ?
O3 Mo1 Mo2 92.57(7) . . ?
O3 Mo1 Mo3 47.30(7) . . ?
O3 Mo1 S1 103.36(7) . . ?
O3 Mo1 O1 92.02(9) . . ?
O3 Mo1 O4 96.04(10) . . ?
O3 Mo1 O5 85.30(9) . . ?
O3 Mo1 N1 168.24(10) . . ?
O1 Mo1 Mo2 47.29(7) . . ?
O1 Mo1 Mo3 92.01(7) . . ?
O1 Mo1 S1 102.48(7) . . ?
O1 Mo1 O4 164.48(10) . . ?
O1 Mo1 O5 88.59(9) . . ?
O1 Mo1 N1 85.56(10) . . ?
O4 Mo1 Mo2 144.93(7) . . ?
O4 Mo1 Mo3 103.20(7) . . ?
O4 Mo1 S1 88.55(7) . . ?
O4 Mo1 O5 78.92(9) . . ?
O4 Mo1 N1 83.85(11) . . ?
O5 Mo1 Mo2 135.78(7) . . ?
O5 Mo1 Mo3 132.59(7) . . ?
O5 Mo1 S1 165.54(7) . . ?
O5 Mo1 N1 83.14(10) . . ?
N1 Mo1 Mo2 94.21(8) . . ?
N1 Mo1 Mo3 144.18(8) . . ?
N1 Mo1 S1 88.40(8) . . ?
Mo1 Mo3 Mo2 60.584(11) . . ?
S1 Mo3 Mo2 56.31(2) . . ?
S1 Mo3 Mo1 55.99(2) . . ?
O3 Mo3 Mo2 93.36(7) . . ?
O3 Mo3 Mo1 47.60(7) . . ?
O3 Mo3 S1 102.46(7) . . ?
O3 Mo3 O2 95.40(9) . . ?
O3 Mo3 N7 82.61(10) . . ?
O3 Mo3 N9 163.37(11) . . ?
O3 Mo3 N5 85.58(10) . . ?
O2 Mo3 Mo2 47.44(7) . . ?
O2 Mo3 Mo1 94.75(7) . . ?
O2 Mo3 S1 102.17(7) . . ?
O2 Mo3 N7 83.04(10) . . ?
O2 Mo3 N9 94.34(10) . . ?
O2 Mo3 N5 170.12(10) . . ?
N7 Mo3 Mo2 129.87(7) . . ?
N7 Mo3 Mo1 129.89(8) . . ?
N7 Mo3 S1 172.22(8) . . ?
N7 Mo3 N5 87.35(10) . . ?
N9 Mo3 Mo2 103.16(8) . . ?
N9 Mo3 Mo1 144.55(8) . . ?
N9 Mo3 S1 88.59(8) . . ?
N9 Mo3 N7 85.23(11) . . ?
N9 Mo3 N5 82.55(11) . . ?
N5 Mo3 Mo2 142.40(7) . . ?
N5 Mo3 Mo1 93.15(8) . . ?
N5 Mo3 S1 87.17(7) . . ?
Mo2 S1 Mo3 66.80(2) . . ?
Mo1 S1 Mo2 67.87(2) . . ?
Mo1 S1 Mo3 66.79(2) . . ?
Mo3 O3 Mo1 85.10(9) . . ?
Mo3 O2 Mo2 85.19(9) . . ?
Mo2 O1 Mo1 85.22(9) . . ?
C1 O4 Mo1 117.0(2) . . ?
C2 O5 Mo1 115.3(2) . . ?
C7 O8 Mo2 116.5(2) . . ?
C6 O7 Mo2 118.3(2) . . ?
C14 N7 Mo3 122.9(2) . . ?
C14 N7 C16 105.0(3) . . ?
C16 N7 Mo3 131.8(2) . . ?
C17 N9 Mo3 128.1(2) . . ?
C17 N9 C19 104.2(3) . . ?
C19 N9 Mo3 127.7(2) . . ?
C3 N2 H2A 127.5 . . ?
C3 N2 H2B 126.1 . . ?
C3 N2 C4 105.1(7) . . ?
C3 N2 C4A 107.8(4) . . ?
C4 N2 H2A 127.5 . . ?
C4A N2 H2B 126.1 . . ?
C3 N1 Mo1 127.4(3) . . ?
C3 N1 C5 105.3(4) . . ?
C3 N1 C5A 100.2(7) . . ?
C5 N1 Mo1 126.9(3) . . ?
C5A N1 Mo1 129.6(6) . . ?
C12 N6 H6 126.2 . . ?
C11 N6 H6 126.2 . . ?
C11 N6 C12 107.5(3) . . ?
C11 N5 Mo3 127.8(2) . . ?
C11 N5 C13 104.6(3) . . ?
C13 N5 Mo3 126.1(2) . . ?
C14 N8 C15 108.2(3) . . ?
C14 N8 H8 129(3) . . ?
C15 N8 H8 123(3) . . ?
C8 N3 Mo2 127.9(3) . . ?
C8 N3 C10 105.2(3) . . ?
C10 N3 Mo2 126.2(3) . . ?
C17 N10 H10 126.0 . . ?
C17 N10 C18 107.9(3) . . ?
C18 N10 H10 126.0 . . ?
N7 C14 H14 124.4 . . ?
N8 C14 N7 111.3(3) . . ?
N8 C14 H14 124.4 . . ?
N6 C12 H12 126.8 . . ?
C13 C12 N6 106.5(3) . . ?
C13 C12 H12 126.8 . . ?
C8 N4 C9 107.0(3) . . ?
C8 N4 H4 138(3) . . ?
C9 N4 H4 113(3) . . ?
N3 C8 H8A 123.8 . . ?
N4 C8 N3 112.3(3) . . ?
N4 C8 H8A 123.8 . . ?
N9 C17 H17 124.0 . . ?
N10 C17 N9 112.0(3) . . ?
N10 C17 H17 124.0 . . ?
O5 C2 C1 115.8(3) . . ?
O6 C2 O5 124.4(3) . . ?
O6 C2 C1 119.7(4) . . ?
N2 C3 H3 123.8 . . ?
N1 C3 N2 112.4(3) . . ?
N1 C3 H3 123.8 . . ?
N2 C4 H4A 126.0 . . ?
C5 C4 N2 108.0(10) . . ?
C5 C4 H4A 126.0 . . ?
N6 C11 N5 111.2(3) . . ?
N6 C11 H11 124.4 . . ?
N5 C11 H11 124.4 . . ?
N5 C13 H13 124.9 . . ?
C12 C13 N5 110.2(3) . . ?
C12 C13 H13 124.9 . . ?
O4 C1 C2 112.0(3) . . ?
O4 C1 H1A 109.2 . . ?
O4 C1 H1B 109.2 . . ?
C2 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N7 C16 H16 125.4 . . ?
N7 C16 C15 109.2(4) . . ?
C15 C16 H16 125.4 . . ?
N8 C15 C16 106.3(4) . . ?
N8 C15 H15 126.9 . . ?
C16 C15 H15 126.9 . . ?
N4 C9 H9 126.8 . . ?
C10 C9 N4 106.4(4) . . ?
C10 C9 H9 126.8 . . ?
N9 C19 H19 125.7 . . ?
C18 C19 N9 108.6(4) . . ?
C18 C19 H19 125.7 . . ?
O8 C7 C6 114.6(3) . . ?
O9 C7 O8 123.4(4) . . ?
O9 C7 C6 121.9(4) . . ?
N3 C10 H10A 125.6 . . ?
C9 C10 N3 108.9(4) . . ?
C9 C10 H10A 125.6 . . ?
N10 C18 H18 126.4 . . ?
C19 C18 N10 107.2(4) . . ?
C19 C18 H18 126.4 . . ?
O7 C6 C7 112.6(3) . . ?
O7 C6 H6A 109.1 . . ?
O7 C6 H6B 109.1 . . ?
C7 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
N1 C5 H5 126.1 . . ?
C4 C5 N1 107.8(9) . . ?
C4 C5 H5 126.1 . . ?
N1 C5A H5A 124.1 . . ?
C4A C5A N1 111.9(10) . . ?
C4A C5A H5A 124.1 . . ?
N2 C4A H4AA 128.9 . . ?
C5A C4A N2 102.1(10) . . ?
C5A C4A H4AA 128.9 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 362.9 86.3 'H2O, C3H4N2'


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.138
_oxdiff_exptl_absorpt_empirical_full_min 0.893
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_16981
_database_code_depnum_ccdc_archive 'CCDC 1814437'
_audit_update_record             
;
2018-04-13 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_audit_creation_date             2018-04-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18.04 H36.04 Mo3 N6 Na2 O18 S, 4(H2 O)'
_chemical_formula_sum            'C18.04 H44.04 Mo3 N6 Na2 O22 S'
_chemical_formula_weight         1062.97
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.4659(7)
_cell_length_b                   12.7032(7)
_cell_length_c                   14.8254(9)
_cell_angle_alpha                105.896(5)
_cell_angle_beta                 94.713(5)
_cell_angle_gamma                119.364(6)
_cell_volume                     1901.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4322
_cell_measurement_temperature    173
_cell_measurement_theta_max      62.0368
_cell_measurement_theta_min      3.2056
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.513
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1069
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10608
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        62.127
_diffrn_reflns_theta_max         62.127
_diffrn_reflns_theta_min         3.208
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -24.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -19.0000  -90.0000 122

#__ type_ start__ end____ width___ exp.time_
  2 omega   47.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  -30.0000 48

#__ type_ start__ end____ width___ exp.time_
  3 omega   43.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega   52.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000 -180.0000 52

#__ type_ start__ end____ width___ exp.time_
  5 omega   23.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -123.0000  -19.0000 44

#__ type_ start__ end____ width___ exp.time_
  6 omega   26.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000   30.0000 37

#__ type_ start__ end____ width___ exp.time_
  7 omega   73.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
  8 omega   51.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -38.0000   90.0000 65

#__ type_ start__ end____ width___ exp.time_
  9 omega   74.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -25.0000   30.0000 54

#__ type_ start__ end____ width___ exp.time_
 10 omega   91.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   77.0000   90.0000 76

#__ type_ start__ end____ width___ exp.time_
 11 omega   79.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  112.0000 -120.0000 38

#__ type_ start__ end____ width___ exp.time_
 12 omega   71.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  151.0000 -137.0000 26

#__ type_ start__ end____ width___ exp.time_
 13 omega   47.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  178.0000  -90.0000 31

#__ type_ start__ end____ width___ exp.time_
 14 omega   37.00  171.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   12.0000   60.0000 134

#__ type_ start__ end____ width___ exp.time_
 15 omega   40.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -99.0000  120.0000 35

#__ type_ start__ end____ width___ exp.time_
 16 omega   23.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000   30.0000 82

#__ type_ start__ end____ width___ exp.time_
 17 omega   32.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -25.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 18 omega   21.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -93.0000   53.4868 106

#__ type_ start__ end____ width___ exp.time_
 19 omega   22.00  132.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  -90.0000 110

#__ type_ start__ end____ width___ exp.time_
 20 omega   21.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000  -90.0000 39

#__ type_ start__ end____ width___ exp.time_
 21 omega  -35.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -57.0000 -120.0000 72

#__ type_ start__ end____ width___ exp.time_
 22 omega  -22.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -99.0000  120.0000 36

#__ type_ start__ end____ width___ exp.time_
 23 omega -101.00  -74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 24 omega -110.00  -70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
 25 omega -112.00  -75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000   90.0000 37

#__ type_ start__ end____ width___ exp.time_
 26 omega -113.00  -85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066  178.0000 -150.0000 28
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5410
_reflns_number_total             5910
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         5910
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0686
_refine_ls_restrained_S_all      1.138
_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)+(0.0821P)²+17.9074P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.1832
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H7A,H7B} of C7, {H1A,H1B} of C1, All C(H,H,H,H,H,H,H,H,H,
  H,H,H,H,H,H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
 At 2 times of:
  {H8WA,H8WB} of C15A
2. Restrained distances
 O2W-H2WB = O2W-H2WA
 0.85 with sigma of 0.01
 H2WA-H2WB
 1.39 with sigma of 0.01
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.01
 H1WA-H1WB
 1.39 with sigma of 0.01
 O3W-H3WA = O3W-H3WB
 0.9 with sigma of 0.01
 O7W-H7WA
 0.85 with sigma of 0.01
 O5W-H5WA = O5W-H5WB
 0.9 with sigma of 0.01
 H5WA-H5WB
 1.39 with sigma of 0.01
 O4W-H4WA = O4W-H4WB
 0.85 with sigma of 0.01
 H4WA-H4WB
 1.39 with sigma of 0.01
 O8W-H8WA
 0.85 with sigma of 0.01
 O10W-H10B = O10W-H10A
 0.85 with sigma of 0.01
 H10B-H10A
 1.39 with sigma of 0.01
 O9W-H9WA = O9W-H9WB
 0.85 with sigma of 0.01
 H9WA-H9WB
 1.39 with sigma of 0.01
 C15A-C13A \\sim C15-C13
 with sigma of 0.01
3. Rigid bond restraints
 C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C15A \\sim C15 \\sim C13A \\sim C13: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C3A) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C3A) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C13A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(H1B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(H1A)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
 Sof(H7B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
 Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
 Sof(C13A)=Sof(H13A)=FVAR(3)
 Fixed Sof: C13(0.46) H13(0.46) C15(0.6) H15A(0.6) H15B(0.6) H15C(0.6)
 C15A(0.4) H15D(0.4) H15E(0.4) H15F(0.4)
6.a Riding coordinates:
 C15A(H9WA,H9WB,H10A,H10B,H8WA,H4WA,H4WB,H7WA,H5WA,H5WB,H7WB,H8WB,H6WA,H6WB,
 H3WA,H3WB,H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
 C7(H7A), C7(H7B), C1(H1A), C1(H1B), C13(H13), C13A(H13A)
6.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N6(H6), N4(H4), C6(H6A), C4(H4A), C16(H16), C18(H18), C11(H11),
 C17(H17), C12(H12), C10(H10), C5(H5)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C),
 C9A(H9AA,H9AB,H9AC), C15A(H15D,H15E,H15F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.82418(6) 0.57013(6) 0.22015(5) 0.0170(2) Uani 1 1 d . . . . .
Mo2 Mo 0.79113(7) 0.34903(6) 0.21662(5) 0.0179(2) Uani 1 1 d . . . . .
Mo3 Mo 0.60297(6) 0.38598(6) 0.22225(5) 0.0177(2) Uani 1 1 d . . . . .
S1 S 0.69174(19) 0.37261(19) 0.08710(15) 0.0175(4) Uani 1 1 d . . . . .
Na1 Na 1.1198(3) 1.1753(3) 0.4042(3) 0.0268(8) Uani 1 1 d . . . . .
Na2 Na 0.8875(5) 0.2299(5) 0.4416(4) 0.0511(12) Uani 1 1 d . . . . .
O10 O 0.4445(6) 0.2114(6) 0.1515(5) 0.0265(14) Uani 1 1 d . . . . .
O11 O 0.4864(6) 0.3754(6) 0.3210(5) 0.0251(14) Uani 1 1 d . . . . .
O2 O 0.6789(6) 0.3274(6) 0.3008(4) 0.0221(13) Uani 1 1 d . . . . .
O1 O 0.9163(6) 0.5273(6) 0.3002(5) 0.0236(14) Uani 1 1 d . . . . .
O5 O 0.9543(6) 0.7659(6) 0.3157(5) 0.0242(14) Uani 1 1 d . . . . .
O3 O 0.7134(6) 0.5667(6) 0.3044(5) 0.0216(13) Uani 1 1 d . . . . .
O4 O 0.7894(7) 0.6664(6) 0.1483(5) 0.0269(14) Uani 1 1 d . . . . .
O7 O 0.9079(6) 0.3259(6) 0.1401(5) 0.0276(15) Uani 1 1 d . . . . .
O8 O 0.8825(7) 0.2943(6) 0.3055(5) 0.0285(15) Uani 1 1 d . . . . .
N1 N 0.9830(7) 0.6169(7) 0.1465(6) 0.0247(17) Uani 1 1 d . . . . .
N5 N 0.4918(8) 0.4487(8) 0.1482(6) 0.0267(18) Uani 1 1 d . . . . .
O3W O 0.9400(8) 0.0871(7) 0.4829(5) 0.053(2) Uani 1 1 d D . . . .
O9 O 0.9981(9) 0.2085(9) 0.3052(6) 0.053(2) Uani 1 1 d . . . . .
N2 N 1.0895(8) 0.6691(8) 0.0392(6) 0.0319(19) Uani 1 1 d . . . . .
H2 H 1.1063 0.6794 -0.0153 0.038 Uiso 1 1 calc R . . . .
O12 O 0.3051(8) 0.2512(8) 0.3486(6) 0.055(2) Uani 1 1 d . . . . .
N3 N 0.6673(8) 0.1342(7) 0.1399(6) 0.0248(17) Uani 1 1 d . . . . .
O6 O 1.0541(8) 0.9657(7) 0.3184(6) 0.046(2) Uani 1 1 d . . . . .
O1W O 1.2356(8) 1.1985(7) 0.5550(6) 0.053(2) Uani 1 1 d D . . . .
N6 N 0.3606(8) 0.4428(8) 0.0363(6) 0.0305(19) Uani 1 1 d . . . . .
H6 H 0.3085 0.4173 -0.0198 0.037 Uiso 1 1 calc R . . . .
N4 N 0.5915(8) -0.0584(7) 0.0291(6) 0.0271(18) Uani 1 1 d . . . . .
H4 H 0.5736 -0.1189 -0.0265 0.033 Uiso 1 1 calc R . . . .
O7W O 0.6999(8) 0.0263(10) 0.6116(8) 0.069(3) Uani 1 1 d D . . . .
O9W O 0.4570(8) 0.8180(9) 0.5911(7) 0.056(2) Uani 1 1 d D . . . .
C6 C 1.1088(9) 0.6710(10) 0.1870(8) 0.032(2) Uani 1 1 d . . . . .
H6A H 1.1436 0.6837 0.2513 0.038 Uiso 1 1 calc R . . . .
C4 C 0.9755(9) 0.6169(9) 0.0571(7) 0.029(2) Uani 1 1 d . . . . .
H4A H 0.8983 0.5838 0.0113 0.035 Uiso 1 1 calc R . . . .
C16 C 0.4221(9) 0.3875(10) 0.0589(7) 0.028(2) Uani 1 1 d . . . . .
H16 H 0.4154 0.3130 0.0152 0.034 Uiso 1 1 calc R . . . .
O6W O 0.4381(11) -0.1662(12) 0.3077(9) 0.083(3) Uani 1 1 d . . . . .
C18 C 0.4760(10) 0.5493(10) 0.1853(8) 0.031(2) Uani 1 1 d . . . . .
H18 H 0.5162 0.6117 0.2494 0.038 Uiso 1 1 calc R . . . .
C11 C 0.5561(10) -0.0779(10) 0.1126(7) 0.030(2) Uani 1 1 d . . . . .
H11 H 0.5082 -0.1586 0.1208 0.036 Uiso 1 1 calc R . . . .
C17 C 0.3957(11) 0.5476(10) 0.1184(8) 0.035(2) Uani 1 1 d . . . . .
H17 H 0.3683 0.6067 0.1260 0.042 Uiso 1 1 calc R . . . .
C2 C 0.9641(10) 0.8515(10) 0.2816(8) 0.036(2) Uani 1 1 d . . . . .
C12 C 0.6027(10) 0.0394(9) 0.1789(7) 0.031(2) Uani 1 1 d . . . . .
H12 H 0.5932 0.0559 0.2433 0.037 Uiso 1 1 calc R . . . .
C10 C 0.6574(9) 0.0687(9) 0.0493(7) 0.025(2) Uani 1 1 d . . . . .
H10 H 0.6930 0.1080 0.0045 0.030 Uiso 1 1 calc R . . . .
C8 C 0.9554(11) 0.2613(11) 0.2684(8) 0.037(3) Uani 1 1 d . . . . .
O10W O 0.3576(11) 0.4826(9) 0.4815(7) 0.094(4) Uani 1 1 d D . . . .
C5 C 1.1767(11) 0.7039(10) 0.1222(8) 0.036(2) Uani 1 1 d . . . . .
H5 H 1.2662 0.7430 0.1317 0.043 Uiso 1 1 calc R . . . .
C14 C 0.3778(10) 0.2718(11) 0.2967(8) 0.040(3) Uani 1 1 d . . . . .
O2W O 1.1205(11) 0.4051(13) 0.5061(8) 0.088(4) Uani 1 1 d D . . . .
C7 C 0.9884(12) 0.2925(13) 0.1792(9) 0.048(3) Uani 1 1 d . U . . .
H7A H 1.0727 0.3765 0.2062 0.058 Uiso 0.55(3) 1 calc R . P A 1
H7B H 0.9614 0.2067 0.1298 0.058 Uiso 0.45(3) 1 calc R . P A 2
C1 C 0.8642(14) 0.8037(11) 0.1907(9) 0.055(3) Uani 1 1 d . U . . .
H1A H 0.9153 0.8293 0.1433 0.067 Uiso 0.51(3) 1 calc R . P B 1
H1B H 0.8017 0.8181 0.2213 0.067 Uiso 0.49(3) 1 calc R . P B 2
C13 C 0.3615(19) 0.153(2) 0.2087(17) 0.026(5) Uani 0.46 1 d D U P C 1
H13 H 0.4117 0.1274 0.2431 0.031 Uiso 0.46 1 calc R . P C 1
O8W O 0.4888(14) 0.6964(13) 0.4249(8) 0.119(5) Uani 1 1 d D . . . .
O4W O 1.1266(9) 0.6095(9) 0.4420(6) 0.071(3) Uani 1 1 d D . . . .
O5W O 0.6731(8) 0.0681(8) 0.4324(6) 0.065(3) Uani 1 1 d D . . . .
C3 C 0.806(3) 0.869(2) 0.198(2) 0.060(9) Uani 0.51(3) 1 d . U P B 1
H3A H 0.7960 0.8859 0.1379 0.090 Uiso 0.51(3) 1 calc GR . P B 1
H3B H 0.8569 0.9520 0.2528 0.090 Uiso 0.51(3) 1 calc GR . P B 1
H3C H 0.7216 0.8182 0.2084 0.090 Uiso 0.51(3) 1 calc GR . P B 1
C3A C 0.881(2) 0.877(2) 0.1270(18) 0.045(8) Uani 0.49(3) 1 d . U P B 2
H3AA H 0.9397 0.8704 0.0891 0.067 Uiso 0.49(3) 1 calc GR . P B 2
H3AB H 0.9158 0.9676 0.1661 0.067 Uiso 0.49(3) 1 calc GR . P B 2
H3AC H 0.7983 0.8407 0.0830 0.067 Uiso 0.49(3) 1 calc GR . P B 2
C15 C 0.255(2) 0.0490(19) 0.1758(16) 0.056(5) Uani 0.6 1 d D U P C 1
H15A H 0.2440 0.0037 0.1074 0.084 Uiso 0.6 1 calc GR . P C 1
H15B H 0.1874 0.0677 0.1814 0.084 Uiso 0.6 1 calc GR . P C 1
H15C H 0.2490 -0.0058 0.2129 0.084 Uiso 0.6 1 calc GR . P C 1
C9 C 1.012(3) 0.212(3) 0.1063(19) 0.055(7) Uani 0.55(3) 1 d . U P A 1
H9A H 0.9498 0.1205 0.0944 0.083 Uiso 0.55(3) 1 calc GR . P A 1
H9B H 1.0983 0.2309 0.1287 0.083 Uiso 0.55(3) 1 calc GR . P A 1
H9C H 1.0052 0.2286 0.0461 0.083 Uiso 0.55(3) 1 calc GR . P A 1
C9A C 1.115(3) 0.362(3) 0.194(2) 0.056(9) Uani 0.45(3) 1 d . U P A 2
H9AA H 1.1362 0.3558 0.1308 0.084 Uiso 0.45(3) 1 calc GR . P A 2
H9AB H 1.1535 0.3278 0.2281 0.084 Uiso 0.45(3) 1 calc GR . P A 2
H9AC H 1.1489 0.4527 0.2323 0.084 Uiso 0.45(3) 1 calc GR . P A 2
C15A C 0.2287(7) 0.0891(6) 0.1410(5) 0.041(6) Uani 0.4 1 d D U P C 2
H15D H 0.2037 0.1014 0.0821 0.061 Uiso 0.4 1 calc GR . P C 2
H15E H 0.1652 0.0783 0.1785 0.061 Uiso 0.4 1 calc GR . P C 2
H15F H 0.2336 0.0116 0.1230 0.061 Uiso 0.4 1 calc GR . P C 2
H9WA H 0.4408 0.7721 0.6236 0.049 Uiso 1 1 d DR . . . .
H9WB H 0.3986 0.8296 0.5752 0.049 Uiso 1 1 d DR . . . .
H10A H 0.3117 0.4034 0.4455 0.049 Uiso 1 1 d DR . . . .
H10B H 0.4050 0.4933 0.5311 0.049 Uiso 1 1 d DR . . . .
H8WA H 0.5217 0.7519 0.4820 0.081 Uiso 1 1 d DR . . . .
H4WA H 1.0714 0.5834 0.3891 0.049 Uiso 1 1 d DR . . . .
H4WB H 1.1412 0.5507 0.4407 0.049 Uiso 1 1 d DR . . . .
H7WA H 0.7713 0.0368 0.6341 0.049 Uiso 1 1 d DR . . . .
H5WA H 0.6907 0.0523 0.4818 0.049 Uiso 1 1 d DR . . . .
H5WB H 0.6112 -0.0037 0.3891 0.049 Uiso 1 1 d DR . . . .
H7WB H 0.6217 -0.0395 0.5944 0.049 Uiso 1 1 d R . . . .
H8WB H 0.4913 0.6172 0.4248 0.081 Uiso 1 1 d R . . . .
H6WA H 0.3626 -0.1661 0.2825 0.049 Uiso 1 1 d R . . . .
H6WB H 0.4208 -0.2203 0.3441 0.049 Uiso 1 1 d R . . . .
H3WA H 0.9628 0.1235 0.5539 0.049 Uiso 1 1 d DR . . . .
H3WB H 0.8965 -0.0072 0.4726 0.049 Uiso 1 1 d DR . . . .
H1WA H 1.2826 1.1675 0.5511 0.049 Uiso 1 1 d DR . . . .
H1WB H 1.2790 1.2776 0.5926 0.049 Uiso 1 1 d DR . . . .
H2WA H 1.195(5) 0.419(11) 0.505(7) 0.049 Uiso 1 1 d DR . . . .
H2WB H 1.124(9) 0.453(10) 0.561(4) 0.049 Uiso 1 1 d DR . . . .
C13A C 0.3354(16) 0.1862(17) 0.1915(14) 0.028(6) Uani 0.58(4) 1 d D U P C 2
H13A H 0.3217 0.2466 0.1683 0.034 Uiso 0.58(4) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Mo2 2.6158(9) . ?
Mo1 Mo3 2.6086(10) . ?
Mo1 S1 2.367(2) . ?
Mo1 O1 1.941(6) . ?
Mo1 O5 2.135(6) . ?
Mo1 O3 1.929(6) . ?
Mo1 O4 1.994(6) . ?
Mo1 N1 2.241(8) . ?
Mo2 Mo3 2.6114(9) . ?
Mo2 S1 2.366(2) . ?
Mo2 O2 1.921(6) . ?
Mo2 O1 1.944(6) . ?
Mo2 O7 1.999(7) . ?
Mo2 O8 2.133(6) . ?
Mo2 N3 2.237(8) . ?
Mo3 S1 2.373(2) . ?
Mo3 O10 2.003(6) . ?
Mo3 O11 2.131(6) . ?
Mo3 O2 1.946(6) . ?
Mo3 O3 1.934(6) . ?
Mo3 N5 2.252(8) . ?
Na1 Na2 3.346(6) 1_565 ?
Na1 O3W 2.514(9) 1_565 ?
Na1 O9 2.287(8) 1_565 ?
Na1 O12 2.348(8) 1_665 ?
Na1 O6 2.284(8) . ?
Na1 O1W 2.420(9) . ?
Na1 O2W 2.890(15) 1_565 ?
Na2 Na1 3.346(6) 1_545 ?
Na2 O8 2.383(8) . ?
Na2 O3W 2.409(9) . ?
Na2 O9 2.566(10) . ?
Na2 C8 2.837(13) . ?
Na2 O2W 2.519(13) . ?
Na2 O4W 2.376(10) 2_766 ?
Na2 O5W 2.406(10) . ?
Na2 H5WA 2.6486 . ?
O10 C13 1.44(2) . ?
O10 C13A 1.454(18) . ?
O11 C14 1.268(13) . ?
O5 C2 1.278(12) . ?
O4 C1 1.419(13) . ?
O7 C7 1.406(12) . ?
O8 C8 1.277(13) . ?
N1 C6 1.363(13) . ?
N1 C4 1.321(13) . ?
N5 C16 1.302(13) . ?
N5 C18 1.362(13) . ?
O3W Na1 2.514(9) 1_545 ?
O3W H3WA 0.9785 . ?
O3W H3WB 1.0012 . ?
O9 Na1 2.287(8) 1_545 ?
O9 C8 1.239(13) . ?
N2 H2 0.8800 . ?
N2 C4 1.328(13) . ?
N2 C5 1.378(14) . ?
O12 Na1 2.348(8) 1_445 ?
O12 C14 1.214(14) . ?
N3 C12 1.392(13) . ?
N3 C10 1.331(12) . ?
O6 C2 1.237(13) . ?
O1W H1WA 0.8495 . ?
O1W H1WB 0.8502 . ?
N6 H6 0.8800 . ?
N6 C16 1.344(13) . ?
N6 C17 1.379(14) . ?
N4 H4 0.8800 . ?
N4 C11 1.393(13) . ?
N4 C10 1.328(12) . ?
O7W H7WA 0.8550 . ?
O7W H7WB 0.8707 . ?
O9W H9WA 0.8171 . ?
O9W H9WB 0.8396 . ?
C6 H6A 0.9500 . ?
C6 C5 1.350(15) . ?
C4 H4A 0.9500 . ?
C16 H16 0.9500 . ?
O6W H6WA 0.9843 . ?
O6W H6WB 0.9424 . ?
C18 H18 0.9500 . ?
C18 C17 1.339(14) . ?
C11 H11 0.9500 . ?
C11 C12 1.333(14) . ?
C17 H17 0.9500 . ?
C2 C1 1.507(17) . ?
C12 H12 0.9500 . ?
C10 H10 0.9500 . ?
C8 C7 1.515(18) . ?
O10W H10A 0.8463 . ?
O10W H10B 0.8395 . ?
C5 H5 0.9500 . ?
C14 C13 1.61(3) . ?
C14 C13A 1.51(2) . ?
O2W Na1 2.890(15) 1_545 ?
O2W H2WA 0.856(10) . ?
O2W H2WB 0.850(10) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C7 C9 1.43(3) . ?
C7 C9A 1.34(3) . ?
C1 H1A 1.0000 . ?
C1 H1B 1.0000 . ?
C1 C3 1.34(3) . ?
C1 C3A 1.45(2) . ?
C13 H13 1.0000 . ?
C13 C15 1.255(17) . ?
O8W H8WA 0.8450 . ?
O8W H8WB 1.0216 . ?
O4W Na2 2.376(10) 2_766 ?
O4W H4WA 0.8627 . ?
O4W H4WB 0.8461 . ?
O5W H5WA 0.8495 . ?
O5W H5WB 0.8644 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 0.9800 . ?
C15A C13A 1.254(15) . ?
C13A H13A 1.0000 . ?

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
Mo3 Mo1 Mo2 59.98(3) . . ?
S1 Mo1 Mo2 56.44(5) . . ?
S1 Mo1 Mo3 56.71(6) . . ?
O1 Mo1 Mo2 47.72(19) . . ?
O1 Mo1 Mo3 92.76(18) . . ?
O1 Mo1 S1 103.0(2) . . ?
O1 Mo1 O5 85.4(3) . . ?
O1 Mo1 O4 160.4(3) . . ?
O1 Mo1 N1 84.7(3) . . ?
O5 Mo1 Mo2 133.02(17) . . ?
O5 Mo1 Mo3 133.31(18) . . ?
O5 Mo1 S1 167.31(18) . . ?
O5 Mo1 N1 81.8(3) . . ?
O3 Mo1 Mo2 93.26(17) . . ?
O3 Mo1 Mo3 47.61(18) . . ?
O3 Mo1 S1 103.00(19) . . ?
O3 Mo1 O1 93.1(3) . . ?
O3 Mo1 O5 85.8(3) . . ?
O3 Mo1 O4 97.1(3) . . ?
O3 Mo1 N1 167.6(3) . . ?
O4 Mo1 Mo2 147.33(18) . . ?
O4 Mo1 Mo3 106.5(2) . . ?
O4 Mo1 S1 90.99(19) . . ?
O4 Mo1 O5 78.8(2) . . ?
O4 Mo1 N1 81.7(3) . . ?
N1 Mo1 Mo2 94.3(2) . . ?
N1 Mo1 Mo3 144.6(2) . . ?
N1 Mo1 S1 89.4(2) . . ?
Mo3 Mo2 Mo1 59.87(3) . . ?
S1 Mo2 Mo1 56.47(5) . . ?
S1 Mo2 Mo3 56.68(5) . . ?
O2 Mo2 Mo1 93.32(17) . . ?
O2 Mo2 Mo3 47.93(17) . . ?
O2 Mo2 S1 103.30(19) . . ?
O2 Mo2 O1 93.0(3) . . ?
O2 Mo2 O7 161.5(3) . . ?
O2 Mo2 O8 86.0(3) . . ?
O2 Mo2 N3 86.2(3) . . ?
O1 Mo2 Mo1 47.63(18) . . ?
O1 Mo2 Mo3 92.61(18) . . ?
O1 Mo2 S1 102.90(18) . . ?
O1 Mo2 O7 95.8(3) . . ?
O1 Mo2 O8 86.7(3) . . ?
O1 Mo2 N3 168.5(3) . . ?
O7 Mo2 Mo1 104.64(19) . . ?
O7 Mo2 Mo3 147.33(19) . . ?
O7 Mo2 S1 90.65(19) . . ?
O7 Mo2 O8 78.3(3) . . ?
O7 Mo2 N3 82.0(3) . . ?
O8 Mo2 Mo1 134.28(18) . . ?
O8 Mo2 Mo3 133.84(19) . . ?
O8 Mo2 S1 166.10(18) . . ?
O8 Mo2 N3 81.8(3) . . ?
N3 Mo2 Mo1 143.8(2) . . ?
N3 Mo2 Mo3 95.3(2) . . ?
N3 Mo2 S1 88.4(2) . . ?
Mo1 Mo3 Mo2 60.15(3) . . ?
S1 Mo3 Mo1 56.50(5) . . ?
S1 Mo3 Mo2 56.44(5) . . ?
O10 Mo3 Mo1 148.45(18) . . ?
O10 Mo3 Mo2 105.59(18) . . ?
O10 Mo3 S1 91.97(19) . . ?
O10 Mo3 O11 78.0(2) . . ?
O10 Mo3 N5 81.7(3) . . ?
O11 Mo3 Mo1 133.03(17) . . ?
O11 Mo3 Mo2 132.44(18) . . ?
O11 Mo3 S1 168.01(18) . . ?
O11 Mo3 N5 84.6(3) . . ?
O2 Mo3 Mo1 92.94(19) . . ?
O2 Mo3 Mo2 47.11(18) . . ?
O2 Mo3 S1 102.27(19) . . ?
O2 Mo3 O10 95.4(3) . . ?
O2 Mo3 O11 85.5(3) . . ?
O2 Mo3 N5 170.0(3) . . ?
O3 Mo3 Mo1 47.45(19) . . ?
O3 Mo3 Mo2 93.28(18) . . ?
O3 Mo3 S1 102.65(19) . . ?
O3 Mo3 O10 160.5(3) . . ?
O3 Mo3 O11 85.8(2) . . ?
O3 Mo3 O2 94.0(3) . . ?
O3 Mo3 N5 86.2(3) . . ?
N5 Mo3 Mo1 94.4(2) . . ?
N5 Mo3 Mo2 142.9(2) . . ?
N5 Mo3 S1 87.4(2) . . ?
Mo1 S1 Mo3 66.78(6) . . ?
Mo2 S1 Mo1 67.10(6) . . ?
Mo2 S1 Mo3 66.87(6) . . ?
O3W Na1 Na2 45.9(2) 1_565 1_565 ?
O3W Na1 O2W 78.2(3) 1_565 1_565 ?
O9 Na1 Na2 50.0(2) 1_565 1_565 ?
O9 Na1 O3W 88.6(3) 1_565 1_565 ?
O9 Na1 O12 100.6(4) 1_565 1_665 ?
O9 Na1 O1W 157.4(3) 1_565 . ?
O9 Na1 O2W 69.1(3) 1_565 1_565 ?
O12 Na1 Na2 142.0(3) 1_665 1_565 ?
O12 Na1 O3W 170.7(4) 1_665 1_565 ?
O12 Na1 O1W 90.9(3) 1_665 . ?
O12 Na1 O2W 104.9(4) 1_665 1_565 ?
O6 Na1 Na2 115.6(3) . 1_565 ?
O6 Na1 O3W 87.4(3) . 1_565 ?
O6 Na1 O9 101.1(3) . 1_565 ?
O6 Na1 O12 90.9(3) . 1_665 ?
O6 Na1 O1W 98.1(3) . . ?
O6 Na1 O2W 162.5(4) . 1_565 ?
O1W Na1 Na2 110.3(2) . 1_565 ?
O1W Na1 O3W 80.3(3) . 1_565 ?
O1W Na1 O2W 89.2(3) . 1_565 ?
O2W Na1 Na2 46.9(3) 1_565 1_565 ?
Na1 Na2 H5WA 116.7 1_545 . ?
O8 Na2 Na1 94.3(2) . 1_545 ?
O8 Na2 O3W 135.7(3) . . ?
O8 Na2 O9 52.4(2) . . ?
O8 Na2 C8 26.5(3) . . ?
O8 Na2 O2W 88.9(4) . . ?
O8 Na2 O5W 108.1(3) . . ?
O8 Na2 H5WA 126.6 . . ?
O3W Na2 Na1 48.5(2) . 1_545 ?
O3W Na2 O9 84.9(3) . . ?
O3W Na2 C8 110.2(3) . . ?
O3W Na2 O2W 87.9(4) . . ?
O3W Na2 H5WA 70.2 . . ?
O9 Na2 Na1 43.05(19) . 1_545 ?
O9 Na2 C8 25.9(3) . . ?
O9 Na2 H5WA 131.0 . . ?
C8 Na2 Na1 68.1(2) . 1_545 ?
C8 Na2 H5WA 134.9 . . ?
O2W Na2 Na1 57.0(4) . 1_545 ?
O2W Na2 O9 71.7(4) . . ?
O2W Na2 C8 78.7(4) . . ?
O2W Na2 H5WA 144.2 . . ?
O4W Na2 Na1 135.0(3) 2_766 1_545 ?
O4W Na2 O8 99.6(3) 2_766 . ?
O4W Na2 O3W 123.3(3) 2_766 . ?
O4W Na2 O9 139.8(4) 2_766 . ?
O4W Na2 C8 121.2(4) 2_766 . ?
O4W Na2 O2W 80.6(4) 2_766 . ?
O4W Na2 O5W 90.4(4) 2_766 . ?
O4W Na2 H5WA 88.1 2_766 . ?
O5W Na2 Na1 125.3(3) . 1_545 ?
O5W Na2 O3W 84.1(3) . . ?
O5W Na2 O9 123.4(4) . . ?
O5W Na2 C8 119.3(4) . . ?
O5W Na2 O2W 161.9(4) . . ?
O5W Na2 H5WA 18.6 . . ?
C13 O10 Mo3 116.8(9) . . ?
C13A O10 Mo3 115.0(7) . . ?
C14 O11 Mo3 116.9(6) . . ?
Mo2 O2 Mo3 85.0(2) . . ?
Mo1 O1 Mo2 84.6(2) . . ?
C2 O5 Mo1 114.9(6) . . ?
Mo1 O3 Mo3 84.9(3) . . ?
C1 O4 Mo1 116.7(6) . . ?
C7 O7 Mo2 117.9(7) . . ?
Mo2 O8 Na2 147.0(4) . . ?
C8 O8 Mo2 114.9(7) . . ?
C8 O8 Na2 97.0(6) . . ?
C6 N1 Mo1 128.1(7) . . ?
C4 N1 Mo1 125.4(7) . . ?
C4 N1 C6 105.6(8) . . ?
C16 N5 Mo3 124.9(6) . . ?
C16 N5 C18 105.8(8) . . ?
C18 N5 Mo3 129.2(7) . . ?
Na1 O3W H3WA 116.0 1_545 . ?
Na1 O3W H3WB 116.6 1_545 . ?
Na2 O3W Na1 85.6(3) . 1_545 ?
Na2 O3W H3WA 101.5 . . ?
Na2 O3W H3WB 137.9 . . ?
H3WA O3W H3WB 99.6 . . ?
Na1 O9 Na2 87.0(3) 1_545 . ?
C8 O9 Na1 162.4(8) . 1_545 ?
C8 O9 Na2 89.4(7) . . ?
C4 N2 H2 126.4 . . ?
C4 N2 C5 107.2(9) . . ?
C5 N2 H2 126.4 . . ?
C14 O12 Na1 163.0(8) . 1_445 ?
C12 N3 Mo2 128.5(6) . . ?
C10 N3 Mo2 126.0(7) . . ?
C10 N3 C12 104.7(8) . . ?
C2 O6 Na1 147.1(8) . . ?
Na1 O1W H1WA 117.2 . . ?
Na1 O1W H1WB 110.1 . . ?
H1WA O1W H1WB 109.6 . . ?
C16 N6 H6 126.9 . . ?
C16 N6 C17 106.2(8) . . ?
C17 N6 H6 126.9 . . ?
C11 N4 H4 126.5 . . ?
C10 N4 H4 126.5 . . ?
C10 N4 C11 107.0(8) . . ?
H7WA O7W H7WB 132.7 . . ?
H9WA O9W H9WB 114.0 . . ?
N1 C6 H6A 125.1 . . ?
C5 C6 N1 109.9(9) . . ?
C5 C6 H6A 125.1 . . ?
N1 C4 N2 111.5(9) . . ?
N1 C4 H4A 124.3 . . ?
N2 C4 H4A 124.3 . . ?
N5 C16 N6 111.7(9) . . ?
N5 C16 H16 124.1 . . ?
N6 C16 H16 124.1 . . ?
H6WA O6W H6WB 112.3 . . ?
N5 C18 H18 124.9 . . ?
C17 C18 N5 110.2(9) . . ?
C17 C18 H18 124.9 . . ?
N4 C11 H11 126.8 . . ?
C12 C11 N4 106.3(9) . . ?
C12 C11 H11 126.8 . . ?
N6 C17 H17 127.0 . . ?
C18 C17 N6 106.0(8) . . ?
C18 C17 H17 127.0 . . ?
O5 C2 C1 116.1(9) . . ?
O6 C2 O5 121.8(10) . . ?
O6 C2 C1 121.9(10) . . ?
N3 C12 H12 125.0 . . ?
C11 C12 N3 110.1(9) . . ?
C11 C12 H12 125.0 . . ?
N3 C10 H10 124.1 . . ?
N4 C10 N3 111.9(9) . . ?
N4 C10 H10 124.1 . . ?
O8 C8 Na2 56.5(5) . . ?
O8 C8 C7 116.6(9) . . ?
O9 C8 Na2 64.8(7) . . ?
O9 C8 O8 121.2(11) . . ?
O9 C8 C7 122.2(10) . . ?
C7 C8 Na2 172.4(7) . . ?
H10A O10W H10B 110.9 . . ?
N2 C5 H5 127.1 . . ?
C6 C5 N2 105.8(9) . . ?
C6 C5 H5 127.1 . . ?
O11 C14 C13 113.9(11) . . ?
O11 C14 C13A 114.4(10) . . ?
O12 C14 O11 123.3(10) . . ?
O12 C14 C13 120.1(11) . . ?
O12 C14 C13A 121.4(11) . . ?
Na1 O2W H2WA 66(8) 1_545 . ?
Na1 O2W H2WB 145(9) 1_545 . ?
Na2 O2W Na1 76.1(4) . 1_545 ?
Na2 O2W H2WA 142(7) . . ?
Na2 O2W H2WB 103(7) . . ?
H2WA O2W H2WB 109.2(18) . . ?
O7 C7 C8 110.8(9) . . ?
O7 C7 H7A 103.3 . . ?
O7 C7 H7B 103.6 . . ?
O7 C7 C9 113.1(13) . . ?
C8 C7 H7A 103.3 . . ?
C8 C7 H7B 103.6 . . ?
C9 C7 C8 120.7(14) . . ?
C9 C7 H7A 103.3 . . ?
C9A C7 O7 122.9(17) . . ?
C9A C7 C8 109.9(15) . . ?
C9A C7 H7B 103.6 . . ?
O4 C1 C2 112.2(9) . . ?
O4 C1 H1A 103.3 . . ?
O4 C1 H1B 98.8 . . ?
O4 C1 C3A 118.0(13) . . ?
C2 C1 H1A 103.3 . . ?
C2 C1 H1B 98.8 . . ?
C3 C1 O4 118.9(17) . . ?
C3 C1 C2 113.5(15) . . ?
C3 C1 H1A 103.3 . . ?
C3A C1 C2 122.9(14) . . ?
C3A C1 H1B 98.8 . . ?
O10 C13 C14 105.8(13) . . ?
O10 C13 H13 100.8 . . ?
C14 C13 H13 100.8 . . ?
C15 C13 O10 125(2) . . ?
C15 C13 C14 118(2) . . ?
C15 C13 H13 100.8 . . ?
H8WA O8W H8WB 108.6 . . ?
Na2 O4W H4WA 106.1 2_766 . ?
Na2 O4W H4WB 138.2 2_766 . ?
H4WA O4W H4WB 108.9 . . ?
Na2 O5W H5WA 97.1 . . ?
Na2 O5W H5WB 136.4 . . ?
H5WA O5W H5WB 108.3 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C3A H3AA 109.5 . . ?
C1 C3A H3AB 109.5 . . ?
C1 C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C9A H9AA 109.5 . . ?
C7 C9A H9AB 109.5 . . ?
C7 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
H15D C15A H15E 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C13A C15A H15D 109.5 . . ?
C13A C15A H15E 109.5 . . ?
C13A C15A H15F 109.5 . . ?
O10 C13A C14 110.7(11) . . ?
O10 C13A H13A 93.3 . . ?
C14 C13A H13A 93.3 . . ?
C15A C13A O10 117.6(14) . . ?
C15A C13A C14 130.6(14) . . ?
C15A C13A H13A 93.3 . . ?

_olex2_exptl_crystal_mounting_method set
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_15827
_database_code_depnum_ccdc_archive 'CCDC 1814439'
_audit_update_record             
;
2018-04-13 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_audit_creation_date             2018-04-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C32 H24 Mo12 Na12 O64)'
_chemical_formula_sum            'C16 H12 Mo6 Na6 O32'
_chemical_formula_weight         1429.84
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           44
_space_group_name_H-M_alt        'I m m 2'
_space_group_name_Hall           'I 2 -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, z'
'-x, y, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   15.0786(10)
_cell_length_b                   18.8242(10)
_cell_length_c                   7.2176(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2048.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2274
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.0955
_cell_measurement_theta_min      3.7528
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.318
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5531
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        62.185
_diffrn_reflns_theta_max         62.185
_diffrn_reflns_theta_min         3.756
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -105.00  -74.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000   90.0000 31

#__ type_ start__ end____ width___ exp.time_
  2 omega -104.00  -58.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000  -90.0000 46

#__ type_ start__ end____ width___ exp.time_
  3 omega  -75.00  -39.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066   97.0000  115.0000 36

#__ type_ start__ end____ width___ exp.time_
  4 omega -113.00  -69.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066  178.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
  5 omega  -42.00   72.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -19.0000  150.0000 114

#__ type_ start__ end____ width___ exp.time_
  6 omega  -38.00   26.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -57.0000  -60.0000 64

#__ type_ start__ end____ width___ exp.time_
  7 omega  -39.00   64.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -38.0000   60.0000 103

#__ type_ start__ end____ width___ exp.time_
  8 omega   23.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   23.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000  150.0000 68

#__ type_ start__ end____ width___ exp.time_
 10 omega   74.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 11 omega   68.00  162.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   64.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
 12 omega  115.00  165.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   50.0000 -150.0000 50

#__ type_ start__ end____ width___ exp.time_
 13 omega   71.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000 -120.0000 28

#__ type_ start__ end____ width___ exp.time_
 14 omega  117.00  153.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   64.0000 -120.0000 36

#__ type_ start__ end____ width___ exp.time_
 15 omega   99.00  169.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   25.0000  -30.0000 70

#__ type_ start__ end____ width___ exp.time_
 16 omega   32.00   67.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000 -150.0000 35

#__ type_ start__ end____ width___ exp.time_
 17 omega   27.00  136.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  -30.0000 109

#__ type_ start__ end____ width___ exp.time_
 18 omega   53.00  120.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000 -150.0000 67

#__ type_ start__ end____ width___ exp.time_
 19 omega   64.00  168.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   38.0000   30.0000 104

#__ type_ start__ end____ width___ exp.time_
 20 omega   83.00  132.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  120.0000 49

#__ type_ start__ end____ width___ exp.time_
 21 omega   34.00  120.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000  -30.0000 86

#__ type_ start__ end____ width___ exp.time_
 22 omega   24.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000  120.0000 29

#__ type_ start__ end____ width___ exp.time_
 23 omega  102.00  134.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  112.0000  -30.0000 32

#__ type_ start__ end____ width___ exp.time_
 24 omega   74.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -93.0000 -151.7662 27
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0399832000
_diffrn_orient_matrix_UB_12      0.0884728000
_diffrn_orient_matrix_UB_13      -0.0378755000
_diffrn_orient_matrix_UB_21      -0.0623435000
_diffrn_orient_matrix_UB_22      -0.0510719000
_diffrn_orient_matrix_UB_23      -0.0667095000
_diffrn_orient_matrix_UB_31      -0.2001062000
_diffrn_orient_matrix_UB_32      -0.0020187000
_diffrn_orient_matrix_UB_33      0.0285808000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                1405
_reflns_number_total             1451
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.745
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.215
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1451
_refine_ls_number_restraints     153
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0546
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1163P)²+15.2479P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1541
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.97(6)
 0.03(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Rigid bond restraints
 O2, C2, Mo2, O1
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O5, C4, O4, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C1 \\sim C3 \\sim C4 \\sim C2: within 3.8A with sigma of 0.005 and sigma for
terminal atoms of 0.01
O1 \\sim O10 \\sim O9 \\sim O7 \\sim O2 \\sim O5 \\sim O8 \\sim O3 \\sim O4
\\sim O6: within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.41521(8) 0.5000 0.4413(3) 0.0277(5) Uani 1 2 d S T P . .
Mo2 Mo 0.27671(8) 0.43103(6) 0.7776(2) 0.0379(5) Uani 1 1 d . U . . .
O1 O 0.3099(8) 0.4266(5) 0.4804(19) 0.0398(16) Uani 1 1 d . U . . .
O10 O 0.5000 0.5742(7) 0.493(3) 0.036(3) Uani 1 2 d S TU P . .
O9 O 0.4022(10) 0.5000 0.206(3) 0.037(3) Uani 1 2 d S TU P . .
O7 O 0.3762(10) 0.5000 0.751(3) 0.0386(19) Uani 1 2 d S TU P . .
O2 O 0.3669(7) 0.3462(5) 0.7414(19) 0.0421(17) Uani 1 1 d . U . . .
O5 O 0.0996(8) 0.2875(7) 0.529(2) 0.050(2) Uani 1 1 d . U . . .
O8 O 0.1890(11) 0.5000 0.713(3) 0.043(2) Uani 1 2 d S TU P . .
O3 O 0.4059(8) 0.2590(6) 0.549(2) 0.045(2) Uani 1 1 d . U . . .
O4 O 0.1838(8) 0.3575(6) 0.691(2) 0.0457(17) Uani 1 1 d . U . . .
O6 O 0.2688(8) 0.4122(7) 1.003(2) 0.049(3) Uani 1 1 d . U . . .
C1 C 0.3232(8) 0.3534(7) 0.418(3) 0.036(2) Uani 1 1 d . U . . .
H1 H 0.3607 0.3512 0.3041 0.043 Uiso 1 1 calc R . . . .
C3 C 0.2337(9) 0.3190(8) 0.388(3) 0.037(2) Uani 1 1 d . U . . .
H3A H 0.2058 0.3422 0.2794 0.044 Uiso 1 1 calc R . . . .
H3B H 0.2439 0.2687 0.3547 0.044 Uiso 1 1 calc R . . . .
C4 C 0.1685(10) 0.3208(8) 0.543(3) 0.038(2) Uani 1 1 d . U . . .
C2 C 0.3690(10) 0.3151(8) 0.586(3) 0.037(2) Uani 1 1 d . U . . .
Na1 Na 0.5000 0.2187(7) 0.781(2) 0.073(4) Uani 1 2 d S T P . .
Na2 Na 0.0000 0.2718(12) 0.788(2) 0.105(6) Uani 1 2 d S T P . .
Na3 Na 0.5000 0.362(2) 0.063(7) 0.24(3) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Mo1 2.557(3) 2_665 ?
Mo1 O1 2.123(11) 3_565 ?
Mo1 O1 2.123(11) . ?
Mo1 O10 1.930(10) . ?
Mo1 O10 1.930(10) 2_665 ?
Mo1 O9 1.71(2) . ?
Mo1 O7 2.31(2) . ?
Mo2 Mo2 2.597(2) 3_565 ?
Mo2 O1 2.204(14) . ?
Mo2 O7 1.993(11) . ?
Mo2 O2 2.113(11) . ?
Mo2 O8 1.911(13) . ?
Mo2 O4 2.067(12) . ?
Mo2 O6 1.669(15) . ?
O1 C1 1.465(17) . ?
O10 Mo1 1.930(10) 2_665 ?
O7 Mo2 1.993(11) 3_565 ?
O2 C2 1.27(2) . ?
O5 C4 1.22(2) . ?
O5 Na1 2.335(19) 6_554 ?
O5 Na2 2.418(19) . ?
O8 Mo2 1.911(13) 3_565 ?
O3 C2 1.22(2) . ?
O3 Na1 2.324(17) . ?
O3 Na2 2.430(19) 6_554 ?
O4 C4 1.29(2) . ?
C1 H1 1.0000 . ?
C1 C3 1.512(18) . ?
C1 C2 1.57(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.49(2) . ?
Na1 O5 2.335(19) 6 ?
Na1 O5 2.335(19) 7 ?
Na1 O3 2.324(17) 4_655 ?
Na1 C2 3.032(19) 4_655 ?
Na1 Na2 3.57(2) 6_554 ?
Na1 Na2 3.66(2) 6 ?
Na1 Na3 3.37(3) 1_556 ?
Na2 O5 2.418(19) 4 ?
Na2 O3 2.430(19) 6 ?
Na2 O3 2.430(19) 7_455 ?
Na2 Na1 3.57(2) 6 ?
Na2 Na1 3.66(2) 6_554 ?
Na2 Na3 2.99(6) 6 ?
Na3 Na1 3.37(3) 1_554 ?
Na3 Na2 2.99(6) 6_554 ?

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 Mo1 138.4(3) . 2_665 ?
O1 Mo1 Mo1 138.4(3) 3_565 2_665 ?
O1 Mo1 O1 81.1(6) 3_565 . ?
O1 Mo1 O7 71.4(4) 3_565 . ?
O1 Mo1 O7 71.4(4) . . ?
O10 Mo1 Mo1 48.5(3) 2_665 2_665 ?
O10 Mo1 Mo1 48.5(3) . 2_665 ?
O10 Mo1 O1 90.0(4) 2_665 . ?
O10 Mo1 O1 160.2(7) 2_665 3_565 ?
O10 Mo1 O1 160.2(7) . . ?
O10 Mo1 O1 90.0(4) . 3_565 ?
O10 Mo1 O10 92.8(6) 2_665 . ?
O10 Mo1 O7 89.0(6) . . ?
O10 Mo1 O7 89.0(6) 2_665 . ?
O9 Mo1 Mo1 96.6(5) . 2_665 ?
O9 Mo1 O1 92.7(5) . 3_565 ?
O9 Mo1 O1 92.7(5) . . ?
O9 Mo1 O10 105.4(7) . 2_665 ?
O9 Mo1 O10 105.4(7) . . ?
O9 Mo1 O7 158.7(6) . . ?
O7 Mo1 Mo1 104.7(4) . 2_665 ?
O1 Mo2 Mo2 92.1(2) . 3_565 ?
O7 Mo2 Mo2 49.4(3) . 3_565 ?
O7 Mo2 O1 76.2(6) . . ?
O7 Mo2 O2 89.8(4) . . ?
O7 Mo2 O4 156.6(7) . . ?
O2 Mo2 Mo2 139.1(3) . 3_565 ?
O2 Mo2 O1 72.9(5) . . ?
O8 Mo2 Mo2 47.2(4) . 3_565 ?
O8 Mo2 O1 86.8(6) . . ?
O8 Mo2 O7 93.2(5) . . ?
O8 Mo2 O2 158.2(6) . . ?
O8 Mo2 O4 84.9(5) . . ?
O4 Mo2 Mo2 132.1(3) . 3_565 ?
O4 Mo2 O1 80.4(5) . . ?
O4 Mo2 O2 83.8(5) . . ?
O6 Mo2 Mo2 102.3(5) . 3_565 ?
O6 Mo2 O1 163.0(5) . . ?
O6 Mo2 O7 106.5(7) . . ?
O6 Mo2 O2 90.3(6) . . ?
O6 Mo2 O8 109.5(7) . . ?
O6 Mo2 O4 96.0(6) . . ?
Mo1 O1 Mo2 106.0(5) . . ?
C1 O1 Mo1 118.0(9) . . ?
C1 O1 Mo2 111.4(10) . . ?
Mo1 O10 Mo1 83.0(5) . 2_665 ?
Mo2 O7 Mo1 106.5(7) 3_565 . ?
Mo2 O7 Mo1 106.5(7) . . ?
Mo2 O7 Mo2 81.3(6) 3_565 . ?
C2 O2 Mo2 118.4(11) . . ?
C4 O5 Na1 129.8(14) . 6_554 ?
C4 O5 Na2 121.7(13) . . ?
Na1 O5 Na2 100.7(6) 6_554 . ?
Mo2 O8 Mo2 85.6(7) 3_565 . ?
C2 O3 Na1 113.9(13) . . ?
C2 O3 Na2 129.7(13) . 6_554 ?
Na1 O3 Na2 97.2(6) . 6_554 ?
C4 O4 Mo2 136.9(11) . . ?
O1 C1 H1 111.6 . . ?
O1 C1 C3 108.9(11) . . ?
O1 C1 C2 104.9(14) . . ?
C3 C1 H1 111.6 . . ?
C3 C1 C2 108.0(13) . . ?
C2 C1 H1 111.6 . . ?
C1 C3 H3A 107.8 . . ?
C1 C3 H3B 107.8 . . ?
H3A C3 H3B 107.1 . . ?
C4 C3 C1 118.0(16) . . ?
C4 C3 H3A 107.8 . . ?
C4 C3 H3B 107.8 . . ?
O5 C4 O4 120.0(16) . . ?
O5 C4 C3 119.0(17) . . ?
O4 C4 C3 120.9(13) . . ?
O2 C2 C1 117.3(13) . . ?
O3 C2 O2 127.0(17) . . ?
O3 C2 C1 115.6(16) . . ?
O5 Na1 O5 80.0(8) 7 6 ?
O5 Na1 C2 88.1(5) 7 4_655 ?
O5 Na1 C2 143.6(8) 6 4_655 ?
O5 Na1 Na2 140.0(4) 6 6_554 ?
O5 Na1 Na2 40.5(4) 6 6 ?
O5 Na1 Na2 40.5(4) 7 6 ?
O5 Na1 Na2 140.0(4) 7 6_554 ?
O5 Na1 Na3 65.1(9) 7 1_556 ?
O5 Na1 Na3 65.1(9) 6 1_556 ?
O3 Na1 O5 100.1(5) . 6 ?
O3 Na1 O5 100.1(5) 4_655 7 ?
O3 Na1 O5 163.8(8) 4_655 6 ?
O3 Na1 O5 163.8(8) . 7 ?
O3 Na1 O3 75.3(8) 4_655 . ?
O3 Na1 C2 82.3(6) . 4_655 ?
O3 Na1 C2 21.6(5) 4_655 4_655 ?
O3 Na1 Na2 42.5(5) 4_655 6_554 ?
O3 Na1 Na2 134.8(6) 4_655 6 ?
O3 Na1 Na2 42.5(5) . 6_554 ?
O3 Na1 Na2 134.8(6) . 6 ?
O3 Na1 Na3 100.0(9) 4_655 1_556 ?
O3 Na1 Na3 100.0(9) . 1_556 ?
C2 Na1 Na2 60.3(5) 4_655 6_554 ?
C2 Na1 Na2 115.8(6) 4_655 6 ?
C2 Na1 Na3 78.6(8) 4_655 1_556 ?
Na2 Na1 Na2 174.3(8) 6_554 6 ?
Na3 Na1 Na2 50.1(11) 1_556 6 ?
Na3 Na1 Na2 124.1(11) 1_556 6_554 ?
O5 Na2 O5 76.8(8) 4 . ?
O5 Na2 O3 173.0(11) 4 6 ?
O5 Na2 O3 105.5(5) 4 7_455 ?
O5 Na2 O3 105.5(5) . 6 ?
O5 Na2 O3 173.0(11) . 7_455 ?
O5 Na2 Na1 140.1(5) 4 6 ?
O5 Na2 Na1 38.8(4) . 6_554 ?
O5 Na2 Na1 38.8(4) 4 6_554 ?
O5 Na2 Na1 140.1(5) . 6 ?
O5 Na2 Na3 71.5(8) . 6 ?
O5 Na2 Na3 71.5(8) 4 6 ?
O3 Na2 O3 71.5(7) 6 7_455 ?
O3 Na2 Na1 141.9(5) 6 6_554 ?
O3 Na2 Na1 40.3(4) 6 6 ?
O3 Na2 Na1 40.3(4) 7_455 6 ?
O3 Na2 Na1 141.9(5) 7_455 6_554 ?
O3 Na2 Na3 102.8(9) 6 6 ?
O3 Na2 Na3 102.8(9) 7_455 6 ?
Na1 Na2 Na1 174.3(8) 6 6_554 ?
Na3 Na2 Na1 125.8(9) 6 6 ?
Na3 Na2 Na1 59.9(8) 6 6_554 ?
Na2 Na3 Na1 69.9(9) 6_554 1_554 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 -0.257 149.9 50.8 5H2O
2 0.500 0.000 -0.026 149.9 50.8 5H2O


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.97(6)
2 0.03(6)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_17169
_database_code_depnum_ccdc_archive 'CCDC 1814438'
_audit_update_record             
;
2018-04-13 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_exp_17169           
;
PROBLEM: D-H Without Acceptor       O6       --H6A            Please Check
RESPONSE: The unit cell of compound 3 includes a large region of disordered solvent water molecules which are of no interest. We employed a solvent mask to calculate the disraction contribution of the solvent molecules, and to produce a set of solvent-free disraction intensities. The Mask calculations showed a total solvent accessible area volume of 542.5 \%A3 and the residual electron density amounted to 168.7 electrons per unit cell, corresponding to 16 water molecules.
;
_vrf_PLAT420_exp_17169_2         
;
PROBLEM: D-H Without Acceptor       N2       --H2             Please Check
RESPONSE: The unit cell of compound 3 includes a large region of disordered solvent water molecules which are of no interest. We employed a solvent mask to calculate the disraction contribution of the solvent molecules, and to produce a set of solvent-free disraction intensities. The Mask calculations showed a total solvent accessible area volume of 542.5 \%A3 and the residual electron density amounted to 168.7 electrons per unit cell, corresponding to 16 water molecules.
;
# Added during the CSD deposition process: Friday 13 April 2018 02:14 PM
# end Validation Reply Form

_audit_creation_date             2018-04-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H50 Mo6 N20 O16'
_chemical_formula_sum            'C36 H50 Mo6 N20 O16'
_chemical_formula_weight         1594.60
_chemical_melting_point          ?
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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6194(5)
_cell_length_b                   11.9177(5)
_cell_length_c                   14.7094(10)
_cell_angle_alpha                90.197(4)
_cell_angle_beta                 106.313(5)
_cell_angle_gamma                110.829(4)
_cell_volume                     1658.78(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2311
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.5550
_cell_measurement_theta_min      2.9070
_shelx_estimated_absorpt_T_max   0.955
_shelx_estimated_absorpt_T_min   0.800
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.152
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      7.00  73.00   1.00   26.00    --   24.10  57.00 -60.00   66
  2  ω     51.00  81.00   1.00   26.00    --   24.10-129.00 119.00   30
  3  ω     68.00  95.00   1.00   26.00    --   24.10-143.00 -51.00   27
  4  ω    -73.00 -44.00   1.00   26.00    --  -22.85-178.00  60.00   29
  5  ω    -95.00 -35.00   1.00   26.00    --  -22.85-178.00  90.00   60
  6  ω    -96.00   7.00   1.00   26.00    --  -22.85 -38.00 -60.00  103
  7  ω    -96.00   8.00   1.00   26.00    --  -22.85 -38.00  30.00  104
  8  ω   -104.00 -78.00   1.00   26.00    --  -22.85 178.00-180.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0088040000
_diffrn_orient_matrix_UB_12      0.0032397000
_diffrn_orient_matrix_UB_13      -0.0460913000
_diffrn_orient_matrix_UB_21      0.0740253000
_diffrn_orient_matrix_UB_22      0.0171863000
_diffrn_orient_matrix_UB_23      0.0206530000
_diffrn_orient_matrix_UB_31      -0.0078557000
_diffrn_orient_matrix_UB_32      -0.0616733000
_diffrn_orient_matrix_UB_33      -0.0027214000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4536
_reflns_number_total             5853
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.153
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5853
_refine_ls_number_restraints     419
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0520
_refine_ls_restrained_S_all      1.067
_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)+(0.0493P)²+0.3511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1199
_refine_special_details          ?
_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
2. Restrained distances
 N10-H10A
 0.88 with sigma of 0.01
 O6-H6A
 0.85 with sigma of 0.01
 C2-C1
 1.5 with sigma of 0.01
3. Rigid bond restraints
 C1, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 O6, C1, Mo3, N7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.0025
 Mo3, O3
 with sigma for 1-2 distances of 0.00125 and sigma for 1-3 distances of 0.000625
 C18, C17, C17, N10, N10, C16, C15, C14, C14, N8, N8, C13, C2, O7, C2, O8, C1,
 C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C18 \\sim C17 \\sim C17 \\sim N10 \\sim N10 \\sim C16 \\sim C15 \\sim C14 \\sim
C14 \\sim N8 \\sim N8 \\sim C13 \\sim C2 \\sim O7 \\sim C2 \\sim O8 \\sim C1
\\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C7 \\sim C10 \\sim C4 \\sim C9 \\sim C12 \\sim C11 \\sim C2 \\sim C8 \\sim C6
\\sim C16 \\sim C15 \\sim C18 \\sim C5 \\sim C13 \\sim C17 \\sim C1 \\sim C14
\\sim C3 \\sim C3A: within 3.8A with sigma of 0.01 and sigma for terminal atoms
of 0.02
N3 \\sim N5 \\sim N1 \\sim N4 \\sim N9 \\sim N6 \\sim N7 \\sim N2 \\sim N8
\\sim N10: within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01
O2 \\sim O5 \\sim O1 \\sim O3 \\sim O4 \\sim O7 \\sim O8 \\sim O6: within 3.8A
with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(C3) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.01
Uanis(N8) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Sof(H1B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(H1A)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
6.a Riding coordinates:
 C3A(H6A)
6.b Ternary CH refined with riding coordinates:
 C1(H1A), C1(H1B)
6.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6), C7(H7), N2(H2), C10(H10), C4(H4A), C9(H9), C12(H12), C11(H11),
  C8(H8), C6(H6B), C16(H16), C15(H15), C18(H18), C5(H5), C13(H13), C17(H17),
 N8(H8A), N10(H10A), C14(H14)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.37482(6) 0.58778(4) 0.55856(4) 0.02377(16) Uani 1 1 d . . . . .
Mo2 Mo 0.62358(6) 0.61897(4) 0.41397(4) 0.02320(15) Uani 1 1 d . . . . .
Mo3 Mo 0.36465(6) 0.50881(5) 0.71864(4) 0.02708(16) Uani 1 1 d . U . . .
O2 O 0.7524(4) 0.5707(3) 0.5088(3) 0.0268(8) Uani 1 1 d . U . . .
O5 O 0.4929(4) 0.6263(3) 0.4772(3) 0.0274(8) Uani 1 1 d . U . . .
O1 O 0.5234(4) 0.5432(3) 0.6568(3) 0.0301(7) Uani 1 1 d . U . . .
O3 O 0.2438(4) 0.3465(3) 0.6650(3) 0.0311(7) Uani 1 1 d . U . . .
O4 O 0.2596(4) 0.5935(3) 0.6439(3) 0.0310(8) Uani 1 1 d . U . . .
O7 O 0.4836(5) 0.2991(4) 0.7014(3) 0.0338(8) Uani 1 1 d . U . . .
O8 O 0.4839(5) 0.4233(4) 0.8187(3) 0.0367(8) Uani 1 1 d . U . . .
N3 N 0.2311(5) 0.6559(4) 0.4570(4) 0.0254(11) Uani 1 1 d . U . . .
N5 N 0.7528(6) 0.8050(4) 0.4831(4) 0.0305(11) Uani 1 1 d . U . . .
N1 N 0.5011(6) 0.7794(4) 0.6230(4) 0.0311(10) Uani 1 1 d . U . . .
N4 N 0.0375(5) 0.6830(4) 0.3815(4) 0.0333(12) Uani 1 1 d . U . . .
H4 H -0.0480 0.6843 0.3687 0.040 Uiso 1 1 calc R . . . .
N9 N 0.2306(6) 0.4851(5) 0.8115(4) 0.0417(13) Uani 1 1 d . U . . .
N6 N 0.9164(6) 0.9611(4) 0.5767(4) 0.0389(13) Uani 1 1 d . U . . .
H6 H 0.9950 1.0066 0.6201 0.047 Uiso 1 1 calc R . . . .
N7 N 0.5112(6) 0.6641(5) 0.8246(4) 0.0386(12) Uani 1 1 d . U . . .
C7 C 0.1022(7) 0.6446(5) 0.4571(5) 0.0297(14) Uani 1 1 d . U . . .
H7 H 0.0619 0.6126 0.5059 0.036 Uiso 1 1 calc R . . . .
N2 N 0.6788(7) 0.9363(5) 0.7037(4) 0.0426(13) Uani 1 1 d . U . . .
H2 H 0.7649 0.9819 0.7383 0.051 Uiso 1 1 calc R . . . .
C10 C 0.8787(7) 0.8452(5) 0.5501(5) 0.0328(15) Uani 1 1 d . U . . .
H10 H 0.9328 0.7974 0.5748 0.039 Uiso 1 1 calc R . . . .
C4 C 0.6358(7) 0.8201(5) 0.6729(5) 0.0345(14) Uani 1 1 d . U . . .
H4A H 0.6935 0.7733 0.6850 0.041 Uiso 1 1 calc R . . . .
C9 C 0.2456(7) 0.7036(5) 0.3744(5) 0.0333(15) Uani 1 1 d . U . . .
H9 H 0.3274 0.7218 0.3541 0.040 Uiso 1 1 calc R . . . .
C12 C 0.7127(7) 0.9031(6) 0.4684(5) 0.0395(16) Uani 1 1 d . U . . .
H12 H 0.6277 0.9032 0.4247 0.047 Uiso 1 1 calc R . . . .
O6 O 0.6092(7) 0.1837(5) 0.8265(4) 0.0706(14) Uani 1 1 d D U . . .
C11 C 0.8144(7) 0.9977(6) 0.5263(5) 0.0389(16) Uani 1 1 d . U . . .
H11 H 0.8147 1.0773 0.5311 0.047 Uiso 1 1 calc R . . . .
C2 C 0.5277(8) 0.3420(5) 0.7926(5) 0.0388(16) Uani 1 1 d D U . . .
C8 C 0.1261(7) 0.7213(6) 0.3255(5) 0.0373(16) Uani 1 1 d . U . . .
H8 H 0.1077 0.7529 0.2661 0.045 Uiso 1 1 calc R . . . .
C6 C 0.4604(8) 0.8758(6) 0.6236(6) 0.0440(17) Uani 1 1 d . U . . .
H6B H 0.3681 0.8742 0.5932 0.053 Uiso 1 1 calc R . . . .
C16 C 0.1411(9) 0.5386(7) 0.8122(6) 0.0572(19) Uani 1 1 d . U . . .
H16 H 0.1238 0.5955 0.7703 0.069 Uiso 1 1 calc R . . . .
C15 C 0.6493(8) 0.6880(6) 0.8734(6) 0.0501(18) Uani 1 1 d . U . . .
H15 H 0.7000 0.6377 0.8692 0.060 Uiso 1 1 calc R . . . .
C18 C 0.2191(10) 0.4114(8) 0.8793(6) 0.061(2) Uani 1 1 d . U . . .
H18 H 0.2702 0.3595 0.8955 0.074 Uiso 1 1 calc R . . . .
C5 C 0.5704(8) 0.9728(6) 0.6735(6) 0.0472(17) Uani 1 1 d . U . . .
H5 H 0.5711 1.0516 0.6851 0.057 Uiso 1 1 calc R . . . .
C13 C 0.4826(9) 0.7582(6) 0.8507(6) 0.0543(18) Uani 1 1 d . U . . .
H13 H 0.3935 0.7663 0.8290 0.065 Uiso 1 1 calc R . . . .
C17 C 0.1270(10) 0.4202(8) 0.9212(6) 0.067(2) Uani 1 1 d . U . . .
H17 H 0.1007 0.3766 0.9711 0.080 Uiso 1 1 calc R . . . .
N8 N 0.6011(7) 0.8402(6) 0.9132(5) 0.0598(15) Uani 1 1 d . U . . .
H8A H 0.6093 0.9103 0.9388 0.072 Uiso 1 1 calc R . . . .
N10 N 0.0783(8) 0.5024(6) 0.8792(5) 0.0673(17) Uani 1 1 d D U . . .
H10A H 0.0167 0.5276 0.8932 0.081 Uiso 1 1 calc DR . . . .
C1 C 0.6053(10) 0.2900(7) 0.8642(6) 0.061(2) Uani 1 1 d D U . . .
H1A H 0.7051 0.3484 0.8793 0.073 Uiso 0.496(14) 1 calc R . P A 1
H1B H 0.5662 0.2755 0.9194 0.073 Uiso 0.504(14) 1 calc R . P A 2
C14 C 0.7024(9) 0.7947(7) 0.9285(6) 0.061(2) Uani 1 1 d . U . . .
H14 H 0.7956 0.8312 0.9708 0.073 Uiso 1 1 calc R . . . .
C3 C 0.581(2) 0.2836(15) 0.9472(13) 0.065(4) Uani 0.496(14) 1 d . U P A 1
H3A H 0.4921 0.2168 0.9418 0.098 Uiso 0.496(14) 1 calc GR . P A 1
H3B H 0.5759 0.3596 0.9675 0.098 Uiso 0.496(14) 1 calc GR . P A 1
H3C H 0.6587 0.2695 0.9944 0.098 Uiso 0.496(14) 1 calc GR . P A 1
C3A C 0.742(2) 0.3780(12) 0.8913(13) 0.082(5) Uani 0.504(14) 1 d . U P A 2
H3AA H 0.8042 0.3507 0.9409 0.123 Uiso 0.504(14) 1 calc GR . P A 2
H3AB H 0.7401 0.4537 0.9161 0.123 Uiso 0.504(14) 1 calc GR . P A 2
H3AC H 0.7771 0.3915 0.8358 0.123 Uiso 0.504(14) 1 calc GR . P A 2
H6A H 0.6039 0.1140 0.8518 0.098 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Mo2 2.5034(7) 2_666 ?
Mo1 Mo3 2.5550(8) . ?
Mo1 O2 1.948(4) 2_666 ?
Mo1 O5 1.911(4) . ?
Mo1 O1 2.044(4) . ?
Mo1 O4 2.000(4) . ?
Mo1 N3 2.198(5) . ?
Mo1 N1 2.237(5) . ?
Mo2 Mo1 2.5035(7) 2_666 ?
Mo2 Mo3 2.5282(8) 2_666 ?
Mo2 O2 1.908(4) . ?
Mo2 O5 1.900(4) . ?
Mo2 O1 2.045(4) 2_666 ?
Mo2 O3 2.003(4) 2_666 ?
Mo2 O7 2.201(4) 2_666 ?
Mo2 N5 2.207(5) . ?
Mo3 Mo2 2.5282(8) 2_666 ?
Mo3 O1 2.052(4) . ?
Mo3 O3 1.915(4) . ?
Mo3 O4 1.895(4) . ?
Mo3 O8 2.165(4) . ?
Mo3 N9 2.186(6) . ?
Mo3 N7 2.202(6) . ?
O2 Mo1 1.948(4) 2_666 ?
O1 Mo2 2.045(4) 2_666 ?
O3 Mo2 2.003(4) 2_666 ?
O7 Mo2 2.201(4) 2_666 ?
O7 C2 1.324(7) . ?
O8 C2 1.312(7) . ?
N3 C7 1.327(8) . ?
N3 C9 1.368(8) . ?
N5 C10 1.338(8) . ?
N5 C12 1.377(8) . ?
N1 C4 1.317(8) . ?
N1 C6 1.364(8) . ?
N4 H4 0.8800 . ?
N4 C7 1.309(8) . ?
N4 C8 1.381(8) . ?
N9 C16 1.322(9) . ?
N9 C18 1.334(9) . ?
N6 H6 0.8800 . ?
N6 C10 1.318(8) . ?
N6 C11 1.342(8) . ?
N7 C15 1.362(9) . ?
N7 C13 1.342(9) . ?
C7 H7 0.9500 . ?
N2 H2 0.8800 . ?
N2 C4 1.327(8) . ?
N2 C5 1.335(9) . ?
C10 H10 0.9500 . ?
C4 H4A 0.9500 . ?
C9 H9 0.9500 . ?
C9 C8 1.361(9) . ?
C12 H12 0.9500 . ?
C12 C11 1.332(9) . ?
O6 C1 1.399(9) . ?
O6 H6A 0.9008 . ?
C11 H11 0.9500 . ?
C2 C1 1.432(7) . ?
C8 H8 0.9500 . ?
C6 H6B 0.9500 . ?
C6 C5 1.339(9) . ?
C16 H16 0.9500 . ?
C16 N10 1.330(10) . ?
C15 H15 0.9500 . ?
C15 C14 1.348(10) . ?
C18 H18 0.9500 . ?
C18 C17 1.325(11) . ?
C5 H5 0.9500 . ?
C13 H13 0.9500 . ?
C13 N8 1.360(9) . ?
C17 H17 0.9500 . ?
C17 N10 1.340(10) . ?
N8 H8A 0.8800 . ?
N8 C14 1.334(10) . ?
N10 H10A 0.8800 . ?
C1 H1A 1.0000 . ?
C1 H1B 1.0000 . ?
C1 C3 1.312(18) . ?
C1 C3A 1.398(18) . ?
C14 H14 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?

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
Mo2 Mo1 Mo3 59.96(2) 2_666 . ?
O2 Mo1 Mo2 48.81(12) 2_666 2_666 ?
O2 Mo1 Mo3 90.66(12) 2_666 . ?
O2 Mo1 O1 100.99(16) 2_666 . ?
O2 Mo1 O4 95.37(17) 2_666 . ?
O2 Mo1 N3 84.98(17) 2_666 . ?
O2 Mo1 N1 172.39(18) 2_666 . ?
O5 Mo1 Mo2 97.75(11) . 2_666 ?
O5 Mo1 Mo3 141.51(13) . . ?
O5 Mo1 O2 96.55(17) . 2_666 ?
O5 Mo1 O1 89.97(17) . . ?
O5 Mo1 O4 164.95(16) . . ?
O5 Mo1 N3 87.90(18) . . ?
O5 Mo1 N1 83.51(18) . . ?
O1 Mo1 Mo2 52.27(11) . 2_666 ?
O1 Mo1 Mo3 51.56(12) . . ?
O1 Mo1 N3 173.86(17) . . ?
O1 Mo1 N1 86.62(18) . . ?
O4 Mo1 Mo2 97.01(11) . 2_666 ?
O4 Mo1 Mo3 47.25(12) . . ?
O4 Mo1 O1 96.75(17) . . ?
O4 Mo1 N3 84.01(18) . . ?
O4 Mo1 N1 83.46(18) . . ?
N3 Mo1 Mo2 133.76(13) . 2_666 ?
N3 Mo1 Mo3 130.47(13) . . ?
N3 Mo1 N1 87.42(19) . . ?
N1 Mo1 Mo2 138.77(14) . 2_666 ?
N1 Mo1 Mo3 94.00(14) . . ?
Mo1 Mo2 Mo3 61.03(2) 2_666 2_666 ?
O2 Mo2 Mo1 50.22(12) . 2_666 ?
O2 Mo2 Mo3 92.42(12) . 2_666 ?
O2 Mo2 O1 102.36(16) . 2_666 ?
O2 Mo2 O3 89.27(17) . 2_666 ?
O2 Mo2 O7 167.67(16) . 2_666 ?
O2 Mo2 N5 86.12(18) . . ?
O5 Mo2 Mo1 101.15(11) . 2_666 ?
O5 Mo2 Mo3 139.71(12) . 2_666 ?
O5 Mo2 O2 102.60(17) . . ?
O5 Mo2 O1 88.04(17) . 2_666 ?
O5 Mo2 O3 164.16(16) . 2_666 ?
O5 Mo2 O7 86.75(17) . 2_666 ?
O5 Mo2 N5 85.65(18) . . ?
O1 Mo2 Mo1 52.24(11) 2_666 2_666 ?
O1 Mo2 Mo3 52.03(12) 2_666 2_666 ?
O1 Mo2 O7 85.79(16) 2_666 2_666 ?
O1 Mo2 N5 170.38(18) 2_666 . ?
O3 Mo2 Mo1 94.50(11) 2_666 2_666 ?
O3 Mo2 Mo3 48.31(11) 2_666 2_666 ?
O3 Mo2 O1 99.74(17) 2_666 2_666 ?
O3 Mo2 O7 80.15(17) 2_666 2_666 ?
O3 Mo2 N5 84.73(18) 2_666 . ?
O7 Mo2 Mo1 136.42(11) 2_666 2_666 ?
O7 Mo2 Mo3 85.31(12) 2_666 2_666 ?
O7 Mo2 N5 86.60(18) 2_666 . ?
N5 Mo2 Mo1 136.33(14) . 2_666 ?
N5 Mo2 Mo3 133.04(14) . 2_666 ?
Mo2 Mo3 Mo1 59.01(2) 2_666 . ?
O1 Mo3 Mo1 51.27(12) . . ?
O1 Mo3 Mo2 51.77(11) . 2_666 ?
O1 Mo3 O8 84.52(17) . . ?
O1 Mo3 N9 168.4(2) . . ?
O1 Mo3 N7 86.3(2) . . ?
O3 Mo3 Mo1 95.10(13) . . ?
O3 Mo3 Mo2 51.35(13) . 2_666 ?
O3 Mo3 O1 102.50(17) . . ?
O3 Mo3 O8 84.34(17) . . ?
O3 Mo3 N9 84.9(2) . . ?
O3 Mo3 N7 160.37(19) . . ?
O4 Mo3 Mo1 50.81(13) . . ?
O4 Mo3 Mo2 99.04(13) . 2_666 ?
O4 Mo3 O1 99.90(17) . . ?
O4 Mo3 O3 99.66(18) . . ?
O4 Mo3 O8 173.18(18) . . ?
O4 Mo3 N9 87.5(2) . . ?
O4 Mo3 N7 95.98(19) . . ?
O8 Mo3 Mo1 134.72(13) . . ?
O8 Mo3 Mo2 87.77(12) . 2_666 ?
O8 Mo3 N9 87.4(2) . . ?
O8 Mo3 N7 79.03(18) . . ?
N9 Mo3 Mo1 137.80(16) . . ?
N9 Mo3 Mo2 136.23(15) . 2_666 ?
N9 Mo3 N7 84.0(2) . . ?
N7 Mo3 Mo1 104.00(15) . . ?
N7 Mo3 Mo2 137.23(16) . 2_666 ?
Mo2 O2 Mo1 80.97(16) . 2_666 ?
Mo2 O5 Mo1 160.4(2) . . ?
Mo1 O1 Mo2 75.49(15) . 2_666 ?
Mo1 O1 Mo3 77.17(15) . . ?
Mo2 O1 Mo3 76.20(14) 2_666 . ?
Mo3 O3 Mo2 80.34(15) . 2_666 ?
Mo3 O4 Mo1 81.94(16) . . ?
C2 O7 Mo2 123.7(4) . 2_666 ?
C2 O8 Mo3 123.4(4) . . ?
C7 N3 Mo1 126.3(4) . . ?
C7 N3 C9 105.1(5) . . ?
C9 N3 Mo1 128.1(4) . . ?
C10 N5 Mo2 128.5(4) . . ?
C10 N5 C12 106.1(5) . . ?
C12 N5 Mo2 125.3(5) . . ?
C4 N1 Mo1 124.4(4) . . ?
C4 N1 C6 105.5(6) . . ?
C6 N1 Mo1 130.0(5) . . ?
C7 N4 H4 125.7 . . ?
C7 N4 C8 108.5(6) . . ?
C8 N4 H4 125.7 . . ?
C16 N9 Mo3 128.0(5) . . ?
C16 N9 C18 104.3(7) . . ?
C18 N9 Mo3 127.6(5) . . ?
C10 N6 H6 125.9 . . ?
C10 N6 C11 108.2(6) . . ?
C11 N6 H6 125.9 . . ?
C15 N7 Mo3 127.9(5) . . ?
C13 N7 Mo3 126.0(5) . . ?
C13 N7 C15 106.0(6) . . ?
N3 C7 H7 124.2 . . ?
N4 C7 N3 111.6(6) . . ?
N4 C7 H7 124.2 . . ?
C4 N2 H2 125.5 . . ?
C4 N2 C5 109.0(6) . . ?
C5 N2 H2 125.5 . . ?
N5 C10 H10 125.2 . . ?
N6 C10 N5 109.7(6) . . ?
N6 C10 H10 125.2 . . ?
N1 C4 N2 109.9(6) . . ?
N1 C4 H4A 125.1 . . ?
N2 C4 H4A 125.1 . . ?
N3 C9 H9 124.9 . . ?
C8 C9 N3 110.2(6) . . ?
C8 C9 H9 124.9 . . ?
N5 C12 H12 126.1 . . ?
C11 C12 N5 107.8(6) . . ?
C11 C12 H12 126.1 . . ?
C1 O6 H6A 130.5 . . ?
N6 C11 H11 125.9 . . ?
C12 C11 N6 108.2(6) . . ?
C12 C11 H11 125.9 . . ?
O7 C2 C1 121.4(6) . . ?
O8 C2 O7 118.7(6) . . ?
O8 C2 C1 119.3(6) . . ?
N4 C8 H8 127.7 . . ?
C9 C8 N4 104.5(6) . . ?
C9 C8 H8 127.7 . . ?
N1 C6 H6B 125.2 . . ?
C5 C6 N1 109.7(6) . . ?
C5 C6 H6B 125.2 . . ?
N9 C16 H16 124.3 . . ?
N9 C16 N10 111.3(7) . . ?
N10 C16 H16 124.3 . . ?
N7 C15 H15 125.5 . . ?
C14 C15 N7 109.0(8) . . ?
C14 C15 H15 125.5 . . ?
N9 C18 H18 124.4 . . ?
C17 C18 N9 111.2(8) . . ?
C17 C18 H18 124.4 . . ?
N2 C5 C6 105.9(6) . . ?
N2 C5 H5 127.0 . . ?
C6 C5 H5 127.0 . . ?
N7 C13 H13 125.3 . . ?
N7 C13 N8 109.5(7) . . ?
N8 C13 H13 125.3 . . ?
C18 C17 H17 126.7 . . ?
C18 C17 N10 106.6(8) . . ?
N10 C17 H17 126.7 . . ?
C13 N8 H8A 126.3 . . ?
C14 N8 C13 107.4(6) . . ?
C14 N8 H8A 126.3 . . ?
C16 N10 C17 106.6(7) . . ?
C16 N10 H10A 126.7 . . ?
C17 N10 H10A 126.7 . . ?
O6 C1 C2 111.5(7) . . ?
O6 C1 H1A 103.6 . . ?
O6 C1 H1B 111.1 . . ?
O6 C1 C3A 108.7(10) . . ?
C2 C1 H1A 103.6 . . ?
C2 C1 H1B 111.1 . . ?
C3 C1 O6 114.2(10) . . ?
C3 C1 C2 118.1(11) . . ?
C3 C1 H1A 103.6 . . ?
C3A C1 C2 103.1(8) . . ?
C3A C1 H1B 111.1 . . ?
C15 C14 H14 126.0 . . ?
N8 C14 C15 108.0(7) . . ?
N8 C14 H14 126.0 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C3A H3AA 109.5 . . ?
C1 C3A H3AB 109.5 . . ?
C1 C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.449 0.000 0.000 542.5 168.7 16H2O
2 0.500 0.500 0.000 11.9 0.0 ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.930
