# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_329_auto
_database_code_depnum_ccdc_archive 'CCDC 2181232'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;Xiamen University
China
;
_audit_update_record             
;
2022-06-22 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_audit_creation_date             2022-03-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H14 Mo2 N4 O9 S, 0.5(H4 O2)'
_chemical_formula_sum            'C10 H16 Mo2 N4 O10 S'
_chemical_formula_weight         576.21
_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'
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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   13.1969(3)
_cell_length_b                   23.5561(7)
_cell_length_c                   5.9279(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1842.79(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3635
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9650
_cell_measurement_theta_min      6.9450
_shelx_estimated_absorpt_T_max   0.568
_shelx_estimated_absorpt_T_min   0.362
_exptl_absorpt_coefficient_mu    12.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6129
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.432
_diffrn_reflns_theta_min         3.753
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     33.00  58.00   0.50    0.60    --  105.19-125.00 150.00   50
  2  ω     78.00 108.00   0.50    0.60    --  105.19-125.00 150.00   60
  3  ω     77.00 119.00   0.50    0.18    --   47.87 169.00  54.00   84
  4  ω     74.00 151.00   0.50    0.60    --  105.19 169.00  54.00  154
  5  ω     41.00  66.00   0.50    0.60    --  105.19 -61.00-150.00   50
  6  ω     49.00  90.00   0.50    0.60    --  105.19-125.00-150.00   82
  7  ω    -24.00   1.00   0.50    0.18    --  -47.87  19.00 120.00   50
  8  ω   -165.00 -95.00   0.50    0.60    --  -99.00-103.00  81.00  140
  9  ω   -166.00 -89.00   0.50    0.60    --  -99.00 -25.00 -97.00  154
 10  ω   -117.00 -92.00   0.50    0.18    --  -47.87 -77.00-120.00   50
 11  ω    -68.00 -26.00   0.50    0.18    --  -47.87 -77.00-120.00   84
 12  ω    -21.00  27.00   0.50    0.18    --  -47.87  19.00-180.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0366929000
_diffrn_orient_matrix_UB_12      0.0450571000
_diffrn_orient_matrix_UB_13      -0.1698069000
_diffrn_orient_matrix_UB_21      0.0101899000
_diffrn_orient_matrix_UB_22      0.0461783000
_diffrn_orient_matrix_UB_23      0.1825961000
_diffrn_orient_matrix_UB_31      0.1103043000
_diffrn_orient_matrix_UB_32      0.0107124000
_diffrn_orient_matrix_UB_33      -0.0735552000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1720
_reflns_number_total             1873
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1873
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0348
_refine_ls_restrained_S_all      1.178
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)²+6.3158P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0973
_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 O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H1WB(0.5)
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3A), C4(H4), C5(H5)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_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 0.25021(2) 0.69324(2) 0.53022(6) 0.01947(15) Uani 1 1 d . . . . .
S1 S 0.20068(9) 0.750000 0.2275(2) 0.0195(3) Uani 1 2 d S T P . .
O3 O 0.39092(19) 0.67565(12) 0.3243(5) 0.0225(6) Uani 1 1 d . . . . .
H3 H 0.416405 0.697387 0.227383 0.034 Uiso 1 1 calc R U . . .
O1 O 0.3278(3) 0.750000 0.6914(7) 0.0221(8) Uani 1 2 d S T P . .
O1W O 0.4562(3) 0.750000 0.0233(7) 0.0256(9) Uani 1 2 d GS T P . .
H1WA H 0.419245 0.749875 -0.097722 0.038 Uiso 1 2 d G U P . .
H1WB H 0.516383 0.761280 -0.016799 0.038 Uiso 0.5 1 d G U P . .
O2 O 0.1450(2) 0.68387(12) 0.6866(5) 0.0246(6) Uani 1 1 d . . . . .
O4 O 0.3415(2) 0.63640(13) 0.7073(5) 0.0294(7) Uani 1 1 d . . . . .
O5 O 0.4822(2) 0.58642(13) 0.7572(6) 0.0360(8) Uani 1 1 d . . . . .
N1 N 0.2053(2) 0.61558(14) 0.3422(6) 0.0233(7) Uani 1 1 d . . . . .
N2 N 0.1399(3) 0.57795(15) 0.4387(6) 0.0271(8) Uani 1 1 d . . . . .
H2 H 0.110769 0.582682 0.570878 0.032 Uiso 1 1 calc R U . . .
C2 C 0.4302(3) 0.61974(17) 0.6476(7) 0.0253(9) Uani 1 1 d . . . . .
C3 C 0.1259(3) 0.53279(18) 0.3049(8) 0.0322(10) Uani 1 1 d . . . . .
H3A H 0.082888 0.501309 0.334372 0.039 Uiso 1 1 calc R U . . .
C4 C 0.1848(3) 0.5404(2) 0.1188(9) 0.0352(11) Uani 1 1 d . . . . .
H4 H 0.191759 0.515142 -0.005136 0.042 Uiso 1 1 calc R U . . .
C5 C 0.2327(3) 0.5925(2) 0.1461(8) 0.0290(9) Uani 1 1 d . . . . .
H5 H 0.278136 0.609104 0.040892 0.035 Uiso 1 1 calc R U . . .
C1 C 0.4690(3) 0.6430(2) 0.4276(8) 0.0310(10) Uani 1 1 d . . . . .
H1A H 0.529149 0.667195 0.454916 0.037 Uiso 1 1 calc R U . . .
H1B H 0.489201 0.611491 0.326837 0.037 Uiso 1 1 calc R U . . .


_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 2.6741(6) 7_575 ?
Mo1 S1 2.3312(11) . ?
Mo1 O3 2.260(3) . ?
Mo1 O1 1.936(3) . ?
Mo1 O2 1.684(3) . ?
Mo1 O4 2.085(3) . ?
Mo1 N1 2.222(3) . ?
O3 H3 0.8400 . ?
O3 C1 1.424(5) . ?
O1W H1WA 0.8676 . ?
O1W H1WB 0.8702 . ?
O1W H1WB 0.87(6) 7_575 ?
O4 C2 1.285(5) . ?
O5 C2 1.228(5) . ?
N1 N2 1.364(5) . ?
N1 C5 1.333(5) . ?
N2 H2 0.8800 . ?
N2 C3 1.340(6) . ?
C2 C1 1.505(6) . ?
C3 H3A 0.9500 . ?
C3 C4 1.361(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(7) . ?
C5 H5 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?

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
S1 Mo1 Mo1 55.00(2) . 7_575 ?
O3 Mo1 Mo1 100.56(7) . 7_575 ?
O3 Mo1 S1 85.41(8) . . ?
O1 Mo1 Mo1 46.32(8) . 7_575 ?
O1 Mo1 S1 97.58(9) . . ?
O1 Mo1 O3 87.63(13) . . ?
O1 Mo1 O4 83.66(12) . . ?
O1 Mo1 N1 163.10(13) . . ?
O2 Mo1 Mo1 97.53(10) . 7_575 ?
O2 Mo1 S1 105.53(10) . . ?
O2 Mo1 O3 161.90(12) . . ?
O2 Mo1 O1 104.76(15) . . ?
O2 Mo1 O4 96.60(13) . . ?
O2 Mo1 N1 87.06(13) . . ?
O4 Mo1 Mo1 129.96(9) . 7_575 ?
O4 Mo1 S1 156.63(9) . . ?
O4 Mo1 O3 71.30(11) . . ?
O4 Mo1 N1 82.98(12) . . ?
N1 Mo1 Mo1 145.40(9) . 7_575 ?
N1 Mo1 S1 90.65(9) . . ?
N1 Mo1 O3 78.30(11) . . ?
Mo1 S1 Mo1 69.99(4) . 7_575 ?
Mo1 O3 H3 125.9 . . ?
C1 O3 Mo1 117.5(2) . . ?
C1 O3 H3 109.5 . . ?
Mo1 O1 Mo1 87.36(16) . 7_575 ?
H1WA O1W H1WB 106.6 . 7_575 ?
H1WA O1W H1WB 106.8 . . ?
H1WB O1W H1WB 35.5 . 7_575 ?
C2 O4 Mo1 125.8(3) . . ?
N2 N1 Mo1 119.6(3) . . ?
C5 N1 Mo1 134.5(3) . . ?
C5 N1 N2 105.8(3) . . ?
N1 N2 H2 124.6 . . ?
C3 N2 N1 110.8(4) . . ?
C3 N2 H2 124.6 . . ?
O4 C2 C1 115.9(4) . . ?
O5 C2 O4 123.9(4) . . ?
O5 C2 C1 120.1(4) . . ?
N2 C3 H3A 126.4 . . ?
N2 C3 C4 107.2(4) . . ?
C4 C3 H3A 126.4 . . ?
C3 C4 H4 126.8 . . ?
C3 C4 C5 106.4(4) . . ?
C5 C4 H4 126.8 . . ?
N1 C5 C4 109.8(4) . . ?
N1 C5 H5 125.1 . . ?
C4 C5 H5 125.1 . . ?
O3 C1 C2 108.9(3) . . ?
O3 C1 H1A 109.9 . . ?
O3 C1 H1B 109.9 . . ?
C2 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O3 C1 C2 8.8(4) . . . . ?
Mo1 O4 C2 O5 179.5(3) . . . . ?
Mo1 O4 C2 C1 -1.3(5) . . . . ?
Mo1 N1 N2 C3 -177.0(3) . . . . ?
Mo1 N1 C5 C4 175.5(3) . . . . ?
O4 C2 C1 O3 -5.2(5) . . . . ?
O5 C2 C1 O3 174.1(4) . . . . ?
N1 N2 C3 C4 1.1(5) . . . . ?
N2 N1 C5 C4 0.0(5) . . . . ?
N2 C3 C4 C5 -1.1(5) . . . . ?
C3 C4 C5 N1 0.7(5) . . . . ?
C5 N1 N2 C3 -0.7(4) . . . . ?

_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 1.385
_oxdiff_exptl_absorpt_empirical_full_min 0.811
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2181233'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;Xiamen University
China
;
_audit_update_record             
;
2022-06-22 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_audit_creation_date             2022-06-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H7 Mo2 O9 S2, C10 H10 N3'
_chemical_formula_sum            'C14 H17 Mo2 N3 O9 S2'
_chemical_formula_weight         627.30
_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'
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                   6.8529(3)
_cell_length_b                   10.7593(4)
_cell_length_c                   14.1435(6)
_cell_angle_alpha                74.526(3)
_cell_angle_beta                 85.918(3)
_cell_angle_gamma                89.947(3)
_cell_volume                     1002.31(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4419
_cell_measurement_temperature    230
_cell_measurement_theta_max      71.6790
_cell_measurement_theta_min      3.2400
_shelx_estimated_absorpt_T_max   0.785
_shelx_estimated_absorpt_T_min   0.095
_exptl_absorpt_coefficient_mu    12.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7558
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.588
_diffrn_reflns_theta_min         3.251
_diffrn_ambient_temperature      230
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00  64.00   1.00    2.50    --    0.00-178.00 -60.00   29
  2  ω    -64.00 -37.00   1.00    2.50    --    0.00 -57.00-120.00   27
  3  ω     37.00  76.00   1.00    2.50    --    0.00-178.00 150.00   39
  4  ω     -6.00  24.00   1.00    2.50    --    0.00 -57.00-120.00   30
  5  ω   -125.00 -81.00   1.00   10.00    --  -57.00 -61.00 120.00   44
  6  ω   -131.00-106.00   1.00   10.00    --  -57.00 -95.00 -60.00   25
  7  ω    -57.00 -32.00   1.00   10.00    --  -57.00 -61.00 150.00   25
  8  ω    -66.00 -34.00   1.00   10.00    --  -57.00 -61.00 120.00   32
  9  ω    -76.00   8.00   1.00   10.00    --  -57.00  61.00 -90.00   84
 10  ω   -117.00  -4.00   1.00   10.00    --  -57.00 126.00 -90.00  113
 11  ω   -119.00 -87.00   1.00   10.00    --  -57.00 -95.00  60.00   32
 12  ω   -114.00 -81.00   1.00   10.00    --  -57.00 -95.00 -90.00   33
 13  ω     32.00 119.00   1.00   10.00    --   57.00  61.00 150.00   87
 14  ω    -10.00  82.00   1.00   10.00    --   57.00 -61.00   0.00   92
 15  ω     90.00 151.00   1.00   17.50    --  114.00  50.00  30.00   61
 16  ω     85.00 116.00   1.00   17.50    --  114.00-112.00 -30.00   31
 17  ω     93.00 130.00   1.00   17.50    --  114.00 -50.00 -90.00   37
 18  ω     60.00  86.00   1.00   17.50    --  114.00 -50.00 -90.00   26
 19  ω     81.00 140.00   1.00   17.50    --  114.00 -38.00   0.00   59
 20  ω     43.00 144.00   1.00   17.50    --  114.00 -38.00-150.00  101
 21  ω    124.00 176.00   1.00   17.50    --  114.00 -12.00-150.00   52
 22  ω     40.00  98.00   1.00   17.50    --  114.00 -12.00-150.00   58
 23  ω    152.00 177.00   1.00   17.50    --  114.00  77.00  90.00   25
 24  ω    109.00 139.00   1.00   17.50    --  114.00 -64.00  60.00   30
 25  ω     89.00 172.00   1.00   17.50    --  114.00  50.00-120.00   83
 26  ω     47.00  81.00   1.00   17.50    --  114.00-112.00 -30.00   34
 27  ω    130.00 156.00   1.00   17.50    --  114.00  50.00-180.00   26
 28  ω     44.00  93.00   1.00   17.50    --  114.00 -64.00  60.00   49
 29  ω     41.00  75.00   1.00   17.50    --  114.00 -38.00   0.00   34
 30  ω     87.00 115.00   1.00   17.50    --  114.00-112.00-120.00   28
 31  ω     44.00  81.00   1.00   17.50    --  114.00-112.00-120.00   37
 32  ω     68.00 106.00   1.00   17.50    --  114.00-112.00  90.00   38
 33  ω    121.00 172.00   1.00   17.50    --  114.00  25.00 120.00   51
 34  ω     73.00  98.00   1.00   17.50    --  114.00  25.00 120.00   25
 35  ω     44.00  85.00   1.00   17.50    --  114.00 -77.00 120.00   41
 36  ω    100.00 146.00   1.00   17.50    --  114.00 -77.00 120.00   46
 37  ω     43.00  69.00   1.00   17.50    --  114.00 -92.00  60.00   26
 38  ω     90.00 115.00   1.00   17.50    --  114.00 -92.00  60.00   25
 39  ω     81.00 116.00   1.00   17.50    --  114.00-112.00-180.00   35
 40  ω    106.00 177.00   1.00   17.50    --  114.00 112.00 120.00   71
 41  ω     53.00  92.00   1.00   17.50    --  114.00 -92.00-180.00   39
 42  ω     45.00 133.00   1.00   17.50    --  114.00 -25.00  90.00   88
 43  ω     68.00  94.00   1.00   17.50    --  114.00-112.00  60.00   26
 44  ω     73.00 105.00   1.00   17.50    --  114.00 -77.00-150.00   32
 45  ω    124.00 149.00   1.00   17.50    --  114.00 178.00-180.00   25
 46  ω    106.00 132.00   1.00   17.50    --  114.00 -92.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0024246000
_diffrn_orient_matrix_UB_12      0.0237834000
_diffrn_orient_matrix_UB_13      0.1027655000
_diffrn_orient_matrix_UB_21      0.1774786000
_diffrn_orient_matrix_UB_22      0.0928021000
_diffrn_orient_matrix_UB_23      -0.0348098000
_diffrn_orient_matrix_UB_31      -0.1389507000
_diffrn_orient_matrix_UB_32      0.1135903000
_diffrn_orient_matrix_UB_33      -0.0327229000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3214
_reflns_number_total             3887
_reflns_odcompleteness_completeness 94.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.016
_refine_diff_density_min         -1.952
_refine_diff_density_rms         0.250
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3887
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0598
_refine_ls_restrained_S_all      1.141
_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)+(0.1276P)²+4.3590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.2167
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 Mo2-H4
 2.923871 with sigma of 0.02
 C3-H4
 1.882004 with sigma of 0.02
 Mo2-H9A \\sim Mo2-H9B
 with sigma of 0.02
3.a Free rotating group:
 O9(H9A,H9B)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C6(H6), C9(H9), C8(H8), C11(H11), C7(H7), C12(H12), C14(H14),
 C13(H13)
;
_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 0.77620(10) 0.29703(6) 0.19592(4) 0.0291(3) Uani 1 1 d D . . . .
Mo1 Mo 0.87993(10) 0.54821(6) 0.19843(5) 0.0297(3) Uani 1 1 d . . . . .
S1 S 1.0682(3) 0.4057(2) 0.13695(18) 0.0374(5) Uani 1 1 d . . . . .
S2 S 0.5683(4) 0.4607(2) 0.2091(2) 0.0456(6) Uani 1 1 d . . . . .
O4 O 0.7009(10) 0.3363(7) 0.0374(4) 0.0400(15) Uani 1 1 d D . . . .
H4 H 0.772(5) 0.355(9) -0.0168(14) 0.060 Uiso 1 1 d D U . . .
O9 O 0.9167(9) 0.1391(7) 0.1496(6) 0.0452(17) Uani 1 1 d G . . . .
H9A H 0.868074 0.064996 0.153865 0.068 Uiso 1 1 d DG U . . .
H9B H 1.036703 0.133717 0.131525 0.068 Uiso 1 1 d DG U . . .
O5 O 0.5198(10) 0.1855(6) 0.1908(5) 0.0397(15) Uani 1 1 d . . . . .
O2 O 0.7225(10) 0.7161(6) 0.1742(6) 0.0428(16) Uani 1 1 d . . . . .
O7 O 0.9423(12) 0.5279(7) 0.3140(5) 0.0486(18) Uani 1 1 d . . . . .
O1 O 1.0625(10) 0.6832(6) 0.1074(5) 0.0397(15) Uani 1 1 d . . . . .
O8 O 0.8039(12) 0.2224(7) 0.3139(5) 0.0481(18) Uani 1 1 d . . . . .
O6 O 0.2906(11) 0.1246(8) 0.1105(7) 0.060(2) Uani 1 1 d . . . . .
O3 O 0.7395(12) 0.9311(7) 0.1397(7) 0.056(2) Uani 1 1 d . . . . .
N2 N 0.2429(13) 0.0337(8) 0.5295(6) 0.0399(18) Uani 1 1 d . . . . .
H2 H 0.265631 -0.048579 0.546976 0.048 Uiso 1 1 calc R U . . .
N3 N 0.3057(12) -0.1779(8) 0.4749(6) 0.0391(18) Uani 1 1 d . . . . .
N1 N 0.3083(13) 0.0290(8) 0.3672(6) 0.0440(19) Uani 1 1 d . . . . .
H1 H 0.335297 0.074524 0.306890 0.053 Uiso 1 1 calc R U . . .
C10 C 0.3229(14) -0.0992(10) 0.3829(7) 0.041(2) Uani 1 1 d . . . . .
C4 C 0.4368(13) 0.1897(9) 0.1115(8) 0.039(2) Uani 1 1 d . . . . .
C5 C 0.2553(14) 0.0989(9) 0.4351(7) 0.037(2) Uani 1 1 d . . . . .
C6 C 0.2187(15) 0.2299(10) 0.4035(8) 0.046(2) Uani 1 1 d . . . . .
H6 H 0.227197 0.273439 0.336175 0.055 Uiso 1 1 calc R U . . .
C2 C 0.8133(15) 0.8272(8) 0.1406(7) 0.037(2) Uani 1 1 d . . . . .
C9 C 0.1949(17) 0.0969(11) 0.5974(7) 0.048(2) Uani 1 1 d . . . . .
H9 H 0.183675 0.050988 0.664170 0.058 Uiso 1 1 calc R U . . .
C1 C 1.0212(15) 0.8123(9) 0.1019(7) 0.040(2) Uani 1 1 d . . . . .
H1A H 1.040745 0.863758 0.033304 0.048 Uiso 1 1 calc R U . . .
H1B H 1.112156 0.845237 0.140292 0.048 Uiso 1 1 calc R U . . .
C8 C 0.1614(16) 0.2273(12) 0.5719(9) 0.052(3) Uani 1 1 d . . . . .
H8 H 0.133151 0.270884 0.620525 0.062 Uiso 1 1 calc R U . . .
C11 C 0.3615(17) -0.1547(12) 0.3028(8) 0.051(3) Uani 1 1 d . . . . .
H11 H 0.379602 -0.102379 0.237847 0.061 Uiso 1 1 calc R U . . .
C7 C 0.1703(18) 0.2933(10) 0.4728(9) 0.052(3) Uani 1 1 d . . . . .
H7 H 0.142924 0.381774 0.453645 0.062 Uiso 1 1 calc R U . . .
C3 C 0.5212(15) 0.2828(11) 0.0205(8) 0.047(2) Uani 1 1 d D . . . .
H3A H 0.543606 0.238812 -0.031646 0.056 Uiso 1 1 calc R U . . .
H3B H 0.428435 0.352067 -0.001519 0.056 Uiso 1 1 calc R U . . .
C12 C 0.3714(18) -0.2858(13) 0.3225(10) 0.060(3) Uani 1 1 d . . . . .
H12 H 0.390519 -0.323897 0.270026 0.072 Uiso 1 1 calc R U . . .
C14 C 0.3196(16) -0.3074(11) 0.4924(8) 0.049(2) Uani 1 1 d . . . . .
H14 H 0.305028 -0.359069 0.557656 0.059 Uiso 1 1 calc R U . . .
C13 C 0.3537(16) -0.3645(12) 0.4188(10) 0.054(3) Uani 1 1 d . . . . .
H13 H 0.365187 -0.454504 0.432006 0.065 Uiso 1 1 calc R U . . .


_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 2.8050(9) . ?
Mo2 S1 2.305(2) . ?
Mo2 S2 2.301(3) . ?
Mo2 O4 2.265(6) . ?
Mo2 O9 2.178(6) . ?
Mo2 O5 2.145(6) . ?
Mo2 O8 1.672(6) . ?
Mo1 S1 2.307(2) . ?
Mo1 S2 2.314(3) . ?
Mo1 O2 2.064(7) . ?
Mo1 O7 1.676(7) . ?
Mo1 O1 2.027(6) . ?
O4 H4 0.854(10) . ?
O4 C3 1.422(11) . ?
O9 H9A 0.8502 . ?
O9 H9B 0.8499 . ?
O5 C4 1.283(12) . ?
O2 C2 1.304(10) . ?
O1 C1 1.400(11) . ?
O6 C4 1.226(11) . ?
O3 C2 1.224(12) . ?
N2 H2 0.8700 . ?
N2 C5 1.329(12) . ?
N2 C9 1.340(13) . ?
N3 C10 1.347(12) . ?
N3 C14 1.353(14) . ?
N1 H1 0.8700 . ?
N1 C10 1.341(13) . ?
N1 C5 1.399(13) . ?
C10 C11 1.425(14) . ?
C4 C3 1.484(14) . ?
C5 C6 1.389(14) . ?
C6 H6 0.9400 . ?
C6 C7 1.358(17) . ?
C2 C1 1.513(14) . ?
C9 H9 0.9400 . ?
C9 C8 1.375(16) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C8 H8 0.9400 . ?
C8 C7 1.389(16) . ?
C11 H11 0.9400 . ?
C11 C12 1.365(18) . ?
C7 H7 0.9400 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C12 H12 0.9400 . ?
C12 C13 1.396(18) . ?
C14 H14 0.9400 . ?
C14 C13 1.350(16) . ?
C13 H13 0.9400 . ?

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
S1 Mo2 Mo1 52.57(6) . . ?
S2 Mo2 Mo1 52.77(6) . . ?
S2 Mo2 S1 102.74(8) . . ?
O4 Mo2 Mo1 99.36(17) . . ?
O4 Mo2 S1 87.26(17) . . ?
O4 Mo2 S2 87.3(2) . . ?
O9 Mo2 Mo1 136.72(18) . . ?
O9 Mo2 S1 84.18(18) . . ?
O9 Mo2 S2 163.0(2) . . ?
O9 Mo2 O4 77.5(3) . . ?
O5 Mo2 Mo1 139.43(19) . . ?
O5 Mo2 S1 156.21(19) . . ?
O5 Mo2 S2 86.89(19) . . ?
O5 Mo2 O4 71.3(2) . . ?
O5 Mo2 O9 81.2(2) . . ?
O8 Mo2 Mo1 98.5(2) . . ?
O8 Mo2 S1 105.4(3) . . ?
O8 Mo2 S2 101.9(3) . . ?
O8 Mo2 O4 162.0(3) . . ?
O8 Mo2 O9 90.9(4) . . ?
O8 Mo2 O5 93.5(3) . . ?
S1 Mo1 Mo2 52.51(6) . . ?
S1 Mo1 S2 102.30(8) . . ?
S2 Mo1 Mo2 52.37(7) . . ?
O2 Mo1 Mo2 131.68(18) . . ?
O2 Mo1 S1 149.5(2) . . ?
O2 Mo1 S2 81.00(19) . . ?
O7 Mo1 Mo2 102.7(2) . . ?
O7 Mo1 S1 105.4(3) . . ?
O7 Mo1 S2 106.9(3) . . ?
O7 Mo1 O2 102.4(3) . . ?
O7 Mo1 O1 108.4(3) . . ?
O1 Mo1 Mo2 131.88(18) . . ?
O1 Mo1 S1 83.85(19) . . ?
O1 Mo1 S2 141.0(2) . . ?
O1 Mo1 O2 75.7(3) . . ?
Mo2 S1 Mo1 74.93(8) . . ?
Mo2 S2 Mo1 74.86(9) . . ?
Mo2 O4 H4 132(2) . . ?
C3 O4 Mo2 116.8(6) . . ?
C3 O4 H4 107.9(19) . . ?
Mo2 O9 H9A 127.4 . . ?
Mo2 O9 H9B 127.5 . . ?
H9A O9 H9B 104.5 . . ?
C4 O5 Mo2 123.8(6) . . ?
C2 O2 Mo1 119.7(6) . . ?
C1 O1 Mo1 116.7(5) . . ?
C5 N2 H2 120.6 . . ?
C5 N2 C9 118.8(9) . . ?
C9 N2 H2 120.6 . . ?
C10 N3 C14 121.8(9) . . ?
C10 N1 H1 115.8 . . ?
C10 N1 C5 128.5(8) . . ?
C5 N1 H1 115.8 . . ?
N3 C10 C11 118.5(10) . . ?
N1 C10 N3 120.8(9) . . ?
N1 C10 C11 120.7(9) . . ?
O5 C4 C3 116.5(8) . . ?
O6 C4 O5 122.5(10) . . ?
O6 C4 C3 120.9(10) . . ?
N2 C5 N1 116.6(9) . . ?
N2 C5 C6 122.8(9) . . ?
C6 C5 N1 120.6(9) . . ?
C5 C6 H6 121.0 . . ?
C7 C6 C5 118.0(10) . . ?
C7 C6 H6 121.0 . . ?
O2 C2 C1 111.7(8) . . ?
O3 C2 O2 124.3(10) . . ?
O3 C2 C1 124.0(8) . . ?
N2 C9 H9 119.1 . . ?
N2 C9 C8 121.8(10) . . ?
C8 C9 H9 119.1 . . ?
O1 C1 C2 111.5(7) . . ?
O1 C1 H1A 109.3 . . ?
O1 C1 H1B 109.3 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C9 C8 H8 120.7 . . ?
C9 C8 C7 118.6(10) . . ?
C7 C8 H8 120.7 . . ?
C10 C11 H11 120.8 . . ?
C12 C11 C10 118.4(10) . . ?
C12 C11 H11 120.8 . . ?
C6 C7 C8 119.9(10) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
O4 C3 C4 110.7(8) . . ?
O4 C3 H3A 109.5 . . ?
O4 C3 H3B 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C11 C12 H12 119.3 . . ?
C11 C12 C13 121.5(11) . . ?
C13 C12 H12 119.3 . . ?
N3 C14 H14 119.1 . . ?
C13 C14 N3 121.8(11) . . ?
C13 C14 H14 119.1 . . ?
C12 C13 H13 121.0 . . ?
C14 C13 C12 117.9(11) . . ?
C14 C13 H13 121.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo2 O4 C3 C4 -10.9(11) . . . . ?
Mo2 O5 C4 O6 179.7(7) . . . . ?
Mo2 O5 C4 C3 -3.1(12) . . . . ?
Mo1 O2 C2 O3 -166.9(8) . . . . ?
Mo1 O2 C2 C1 13.4(11) . . . . ?
Mo1 O1 C1 C2 -17.9(10) . . . . ?
O5 C4 C3 O4 9.1(13) . . . . ?
O2 C2 C1 O1 2.9(12) . . . . ?
O6 C4 C3 O4 -173.7(9) . . . . ?
O3 C2 C1 O1 -176.8(10) . . . . ?
N2 C5 C6 C7 0.7(15) . . . . ?
N2 C9 C8 C7 2.6(17) . . . . ?
N3 C10 C11 C12 2.6(15) . . . . ?
N3 C14 C13 C12 -1.1(17) . . . . ?
N1 C10 C11 C12 -178.8(10) . . . . ?
N1 C5 C6 C7 -179.1(10) . . . . ?
C10 N3 C14 C13 0.8(16) . . . . ?
C10 N1 C5 N2 10.1(15) . . . . ?
C10 N1 C5 C6 -170.1(10) . . . . ?
C10 C11 C12 C13 -3.0(18) . . . . ?
C5 N2 C9 C8 -1.1(16) . . . . ?
C5 N1 C10 N3 -7.4(16) . . . . ?
C5 N1 C10 C11 174.0(10) . . . . ?
C5 C6 C7 C8 0.9(16) . . . . ?
C9 N2 C5 N1 179.2(9) . . . . ?
C9 N2 C5 C6 -0.6(14) . . . . ?
C9 C8 C7 C6 -2.5(17) . . . . ?
C11 C12 C13 C14 2.2(18) . . . . ?
C14 N3 C10 N1 179.9(9) . . . . ?
C14 N3 C10 C11 -1.5(14) . . . . ?

_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 3.179
_oxdiff_exptl_absorpt_empirical_full_min 0.485
####################################################################### 
# 
# 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_1830
_database_code_depnum_ccdc_archive 'CCDC 2181234'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;Xiamen University
China
;
_audit_update_record             
;
2022-06-22 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_audit_creation_date             2022-06-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H4 Mo4 O18 S6, 4(C10 H10 N3)'
_chemical_formula_sum            'C44 H44 Mo4 N12 O18 S6'
_chemical_formula_weight         1605.03
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Fe Dy C O N'
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'
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                   11.1684(2)
_cell_length_b                   11.2139(2)
_cell_length_c                   11.8751(2)
_cell_angle_alpha                104.9280(10)
_cell_angle_beta                 103.8410(10)
_cell_angle_gamma                98.2450(10)
_cell_volume                     1361.60(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8788
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      74.2540
_cell_measurement_theta_min      4.0180
_shelx_estimated_absorpt_T_max   0.628
_shelx_estimated_absorpt_T_min   0.149
_exptl_absorpt_coefficient_mu    10.264
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13703
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.830
_diffrn_reflns_theta_min         4.024
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     84.00 178.00   0.50    0.28    --  107.68  30.00  30.00  188
  2  ω    138.00 174.00   0.50    0.28    --  107.68  45.00 -60.00   72
  3  ω     98.00 178.00   0.50    0.28    --  107.68  45.00 -90.00  160
  4  ω     93.00 124.00   0.50    0.28    --  107.68  45.00 -60.00   62
  5  ω    -28.00  43.00   0.50    0.07    --   43.80 -38.00   0.00  142
  6  ω     38.00  66.00   0.50    0.28    --  107.68 -61.00 150.00   56
  7  ω     34.00  59.00   0.50    0.28    --  107.68 -61.00 120.00   50
  8  ω     49.00  91.00   0.50    0.28    --  107.68 -77.00   0.00   84
  9  ω     34.00  70.00   0.50    0.28    --  107.68 -61.00 -60.00   72
 10  ω     37.00 102.00   0.50    0.28    --  107.68 -77.00-120.00  130
 11  ω     81.00 108.00   0.50    0.28    --  107.68 -94.00 -60.00   54
 12  ω     89.00 115.00   0.50    0.28    --  107.68-125.00 -90.00   52
 13  ω     81.00 111.00   0.50    0.28    --  107.68-125.00 -30.00   60
 14  ω     39.00  70.00   0.50    0.28    --  107.68-125.00 -90.00   62
 15  ω     84.00 116.00   0.50    0.28    --  107.68-125.00  60.00   64
 16  ω     48.00  99.00   0.50    0.28    --  107.68 -94.00 120.00  102
 17  ω     52.00  80.00   0.50    0.28    --  107.68-125.00 120.00   56
 18  ω     91.00 116.00   0.50    0.28    --  107.68-125.00 120.00   50
 19  ω     34.00 102.00   0.50    0.28    --  107.68 -94.00-150.00  136
 20  ω     31.00  91.00   0.50    0.07    --   43.80-125.00 -90.00  120
 21  ω      2.00  40.00   0.50    0.07    --   43.80 -99.00 -30.00   76
 22  ω     53.00  79.00   0.50    0.07    --   43.80 -99.00 -30.00   52
 23  ω    101.00 127.00   0.50    0.28    --  107.68 125.00 -60.00   52
 24  ω     93.00 118.00   0.50    0.28    --  107.68 125.00-150.00   50
 25  ω    144.00 178.00   0.50    0.28    --  107.68 125.00-150.00   68
 26  ω    146.00 178.00   0.50    0.28    --  107.68 125.00 -60.00   64
 27  ω    -24.00  36.00   0.50    0.07    --  -43.80  19.00-180.00  120
 28  ω    -50.00 -16.00   0.50    0.28    --  -90.25  45.00 -30.00   68
 29  ω    -46.00 -15.00   0.50    0.28    --  -90.25  45.00  30.00   62
 30  ω      8.00  36.00   0.50    0.07    --  -43.80  19.00  90.00   56
 31  ω    -37.00  -5.00   0.50    0.07    --  -43.80  38.00  60.00   64
 32  ω    -49.00 -14.00   0.50    0.28    --  -90.25  45.00-180.00   70
 33  ω   -101.00 -21.00   0.50    0.28    --  -90.25  77.00  60.00  160
 34  ω    -51.00 -14.00   0.50    0.28    --  -90.25  45.00   0.00   74
 35  ω    -51.00 -26.00   0.50    0.28    --  -90.25  45.00  60.00   50
 36  ω    -51.00 -16.00   0.50    0.28    --  -90.25  45.00 120.00   70
 37  ω   -143.00 -69.00   0.50    0.28    --  -90.25 -45.00  90.00  148
 38  ω   -161.00-109.00   0.50    0.28    --  -90.25 -61.00  60.00  104
 39  ω   -114.00 -71.00   0.50    0.07    --  -43.80-125.00  90.00   86
 40  ω   -115.00 -74.00   0.50    0.07    --  -43.80-125.00   0.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1082090000
_diffrn_orient_matrix_UB_12      0.0441318000
_diffrn_orient_matrix_UB_13      0.1198380000
_diffrn_orient_matrix_UB_21      0.0174532000
_diffrn_orient_matrix_UB_22      -0.1368580000
_diffrn_orient_matrix_UB_23      -0.0187828000
_diffrn_orient_matrix_UB_31      0.0958157000
_diffrn_orient_matrix_UB_32      0.0234729000
_diffrn_orient_matrix_UB_33      -0.0703768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5163
_reflns_number_total             5299
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.250
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      1.045
_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)+(0.0329P)²+9.5031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1103
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), N4(H4A), N1(H1), C10(H10), C14(H14), C9(H9), C8(H8), C13(H13),
  C4(H4), C11(H11), C16(H16), C15(H15), C21(H21), C20(H20), C19(H19), C6(H6),
 C7(H7), C22(H22), C23(H23)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.23191(3) 0.07138(3) 0.00401(3) 0.02077(11) Uani 1 1 d . . . . .
Mo2 Mo 0.02437(4) -0.11963(3) -0.11106(3) 0.02273(12) Uani 1 1 d . . . . .
S3 S 0.30062(11) 0.25884(11) 0.30289(10) 0.0250(2) Uani 1 1 d . . . . .
S1 S 0.13043(11) 0.00172(12) -0.20393(11) 0.0265(3) Uani 1 1 d . . . . .
S2 S 0.13349(13) 0.16996(14) 0.31346(12) 0.0341(3) Uani 1 1 d . . . . .
O5 O 0.1045(3) -0.0153(3) 0.0609(3) 0.0228(7) Uani 1 1 d . . . . .
O1 O 0.1166(3) 0.2009(3) 0.0452(3) 0.0265(7) Uani 1 1 d . . . . .
O2 O 0.3129(3) 0.2349(3) -0.0228(3) 0.0235(7) Uani 1 1 d . . . . .
O3 O 0.3016(4) 0.4263(3) -0.0380(3) 0.0315(8) Uani 1 1 d . . . . .
O7 O 0.3334(4) 0.1786(3) 0.2000(3) 0.0294(8) Uani 1 1 d . . . . .
O4 O 0.3510(3) -0.0052(3) 0.0178(3) 0.0289(8) Uani 1 1 d . . . . .
O8 O 0.3943(4) 0.2698(4) 0.4178(4) 0.0381(9) Uani 1 1 d . . . . .
O6 O 0.0864(4) -0.2484(3) -0.1228(3) 0.0315(8) Uani 1 1 d . . . . .
O9 O 0.2889(4) 0.3829(4) 0.2901(4) 0.0354(9) Uani 1 1 d . . . . .
N2 N 0.7271(4) 0.1404(4) 0.6648(4) 0.0295(9) Uani 1 1 d . . . . .
H2 H 0.738768 0.070738 0.622224 0.035 Uiso 1 1 calc R U . . .
N3 N 0.6742(4) -0.0292(4) 0.4567(4) 0.0300(9) Uani 1 1 d . . . . .
N5 N 0.2659(4) 0.6887(4) 0.6858(4) 0.0272(9) Uani 1 1 d . . . . .
H5 H 0.216898 0.732800 0.656543 0.033 Uiso 1 1 calc R U . . .
N6 N 0.1019(4) 0.7095(4) 0.4961(4) 0.0306(9) Uani 1 1 d . . . . .
N4 N 0.2082(5) 0.5441(5) 0.4912(4) 0.0364(11) Uani 1 1 d . . . . .
H4A H 0.225631 0.480711 0.444434 0.044 Uiso 1 1 calc R U . . .
N1 N 0.5951(5) 0.1519(5) 0.4855(4) 0.0376(11) Uani 1 1 d . . . . .
H1 H 0.547610 0.195056 0.452687 0.045 Uiso 1 1 calc R U . . .
C12 C 0.6019(5) 0.0417(5) 0.4069(5) 0.0281(10) Uani 1 1 d . . . . .
C1 C 0.1362(5) 0.3141(5) 0.0171(5) 0.0232(10) Uani 1 1 d . . . . .
C3 C 0.6517(5) 0.2047(5) 0.6080(5) 0.0275(10) Uani 1 1 d . . . . .
C2 C 0.2591(5) 0.3302(5) -0.0169(4) 0.0235(10) Uani 1 1 d . . . . .
C10 C 0.5474(5) -0.1076(5) 0.2102(5) 0.0303(11) Uani 1 1 d . . . . .
H10 H 0.506633 -0.133528 0.127098 0.036 Uiso 1 1 calc R U . . .
C14 C 0.4057(5) 0.6609(6) 0.8546(5) 0.0324(12) Uani 1 1 d . . . . .
H14 H 0.448376 0.687852 0.937275 0.039 Uiso 1 1 calc R U . . .
C17 C 0.2774(5) 0.5815(5) 0.6106(5) 0.0279(10) Uani 1 1 d . . . . .
C9 C 0.6192(5) -0.1830(5) 0.2606(5) 0.0318(11) Uani 1 1 d . . . . .
H9 H 0.625284 -0.260551 0.212662 0.038 Uiso 1 1 calc R U . . .
C18 C 0.1126(5) 0.5955(5) 0.4352(5) 0.0296(11) Uani 1 1 d . . . . .
C8 C 0.6810(5) -0.1395(5) 0.3837(5) 0.0293(11) Uani 1 1 d . . . . .
H8 H 0.729667 -0.189080 0.417523 0.035 Uiso 1 1 calc R U . . .
C13 C 0.3291(5) 0.7298(5) 0.8066(5) 0.0286(11) Uani 1 1 d . . . . .
H13 H 0.319828 0.804910 0.856140 0.034 Uiso 1 1 calc R U . . .
C4 C 0.6341(5) 0.3181(5) 0.6755(5) 0.0331(12) Uani 1 1 d . . . . .
H4 H 0.583691 0.364121 0.637839 0.040 Uiso 1 1 calc R U . . .
C11 C 0.5367(5) 0.0049(5) 0.2831(5) 0.0296(11) Uani 1 1 d . . . . .
H11 H 0.487519 0.055186 0.250985 0.036 Uiso 1 1 calc R U . . .
C16 C 0.3582(5) 0.5101(5) 0.6569(5) 0.0351(12) Uani 1 1 d . . . . .
H16 H 0.369894 0.437268 0.605852 0.042 Uiso 1 1 calc R U . . .
C15 C 0.4199(5) 0.5498(6) 0.7792(5) 0.0360(12) Uani 1 1 d . . . . .
H15 H 0.471661 0.501780 0.811949 0.043 Uiso 1 1 calc R U . . .
C21 C -0.0661(5) 0.6996(6) 0.3240(5) 0.0361(12) Uani 1 1 d . . . . .
H21 H -0.124844 0.738986 0.286917 0.043 Uiso 1 1 calc R U . . .
C20 C -0.0570(5) 0.5792(6) 0.2632(5) 0.0348(12) Uani 1 1 d . . . . .
H20 H -0.111775 0.535283 0.186356 0.042 Uiso 1 1 calc R U . . .
C19 C 0.0349(5) 0.5261(5) 0.3193(5) 0.0328(11) Uani 1 1 d . . . . .
H19 H 0.044586 0.446164 0.280759 0.039 Uiso 1 1 calc R U . . .
C6 C 0.7678(6) 0.2933(6) 0.8557(5) 0.0380(13) Uani 1 1 d . . . . .
H6 H 0.806008 0.322555 0.939350 0.046 Uiso 1 1 calc R U . . .
C7 C 0.7849(5) 0.1819(6) 0.7862(5) 0.0347(12) Uani 1 1 d . . . . .
H7 H 0.835781 0.135286 0.822299 0.042 Uiso 1 1 calc R U . . .
C22 C 0.0125(5) 0.7601(6) 0.4393(5) 0.0333(12) Uani 1 1 d . . . . .
H22 H 0.003637 0.839534 0.480100 0.040 Uiso 1 1 calc R U . . .
C23 C 0.6920(5) 0.3616(5) 0.7983(6) 0.0379(13) Uani 1 1 d . . . . .
H23 H 0.680570 0.437747 0.844024 0.045 Uiso 1 1 calc R U . . .
H1A H 0.143(5) 0.377(5) 0.085(5) 0.021(13) Uiso 1 1 d . . . . .
H1B H 0.077(6) 0.313(5) -0.044(6) 0.024(14) Uiso 1 1 d . . . . .


_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 2.7167(5) . ?
Mo1 S1 2.3250(12) . ?
Mo1 O5 1.956(3) . ?
Mo1 O1 2.117(3) . ?
Mo1 O2 2.060(3) . ?
Mo1 O7 2.247(4) . ?
Mo1 O4 1.682(4) . ?
Mo2 S1 2.3254(12) . ?
Mo2 S2 2.4883(14) 2 ?
Mo2 O5 1.984(3) . ?
Mo2 O5 2.299(3) 2 ?
Mo2 O1 2.113(3) 2 ?
Mo2 O6 1.678(4) . ?
S3 S2 2.0338(18) . ?
S3 O7 1.476(4) . ?
S3 O8 1.471(4) . ?
S3 O9 1.459(4) . ?
O1 C1 1.394(6) . ?
O2 C2 1.294(6) . ?
O3 C2 1.224(6) . ?
N2 H2 0.8600 . ?
N2 C3 1.355(7) . ?
N2 C7 1.354(7) . ?
N3 C12 1.353(7) . ?
N3 C8 1.338(7) . ?
N5 H5 0.8600 . ?
N5 C17 1.343(6) . ?
N5 C13 1.361(7) . ?
N6 C18 1.335(7) . ?
N6 C22 1.345(7) . ?
N4 H4A 0.8600 . ?
N4 C17 1.364(7) . ?
N4 C18 1.396(7) . ?
N1 H1 0.8600 . ?
N1 C12 1.368(7) . ?
N1 C3 1.369(7) . ?
C12 C11 1.397(7) . ?
C1 C2 1.521(7) . ?
C1 H1A 0.90(6) . ?
C1 H1B 0.85(6) . ?
C3 C4 1.386(8) . ?
C10 H10 0.9300 . ?
C10 C9 1.394(8) . ?
C10 C11 1.373(8) . ?
C14 H14 0.9300 . ?
C14 C13 1.354(8) . ?
C14 C15 1.389(8) . ?
C17 C16 1.398(7) . ?
C9 H9 0.9300 . ?
C9 C8 1.379(8) . ?
C18 C19 1.391(7) . ?
C8 H8 0.9300 . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C4 C23 1.369(9) . ?
C11 H11 0.9300 . ?
C16 H16 0.9300 . ?
C16 C15 1.372(8) . ?
C15 H15 0.9300 . ?
C21 H21 0.9300 . ?
C21 C20 1.388(8) . ?
C21 C22 1.371(8) . ?
C20 H20 0.9300 . ?
C20 C19 1.380(8) . ?
C19 H19 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.376(9) . ?
C6 C23 1.396(9) . ?
C7 H7 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?

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
S1 Mo1 Mo2 54.26(3) . . ?
O5 Mo1 Mo2 46.82(10) . . ?
O5 Mo1 S1 99.53(10) . . ?
O5 Mo1 O1 74.40(13) . . ?
O5 Mo1 O2 148.53(13) . . ?
O5 Mo1 O7 87.69(13) . . ?
O1 Mo1 Mo2 90.75(9) . . ?
O1 Mo1 S1 94.62(11) . . ?
O1 Mo1 O7 78.20(14) . . ?
O2 Mo1 Mo2 137.28(9) . . ?
O2 Mo1 S1 86.66(10) . . ?
O2 Mo1 O1 74.36(13) . . ?
O2 Mo1 O7 82.36(13) . . ?
O7 Mo1 Mo2 134.32(9) . . ?
O7 Mo1 S1 168.16(10) . . ?
O4 Mo1 Mo2 103.02(12) . . ?
O4 Mo1 S1 103.53(13) . . ?
O4 Mo1 O5 105.96(16) . . ?
O4 Mo1 O1 161.41(16) . . ?
O4 Mo1 O2 102.41(15) . . ?
O4 Mo1 O7 83.23(16) . . ?
S1 Mo2 Mo1 54.25(3) . . ?
S1 Mo2 S2 78.72(4) . 2 ?
S2 Mo2 Mo1 130.79(4) 2 . ?
O5 Mo2 Mo1 90.58(8) 2 . ?
O5 Mo2 Mo1 45.99(9) . . ?
O5 Mo2 S1 96.52(8) 2 . ?
O5 Mo2 S1 98.72(10) . . ?
O5 Mo2 S2 152.57(10) . 2 ?
O5 Mo2 S2 80.29(9) 2 2 ?
O5 Mo2 O5 72.83(15) . 2 ?
O5 Mo2 O1 85.23(13) . 2 ?
O1 Mo2 Mo1 131.12(10) 2 . ?
O1 Mo2 S1 162.10(10) 2 . ?
O1 Mo2 S2 89.72(11) 2 2 ?
O1 Mo2 O5 67.82(12) 2 2 ?
O6 Mo2 Mo1 102.33(13) . . ?
O6 Mo2 S1 105.15(13) . . ?
O6 Mo2 S2 103.24(14) . 2 ?
O6 Mo2 O5 158.33(15) . 2 ?
O6 Mo2 O5 103.76(16) . . ?
O6 Mo2 O1 90.69(15) . 2 ?
O7 S3 S2 108.84(16) . . ?
O8 S3 S2 105.48(18) . . ?
O8 S3 O7 109.5(2) . . ?
O9 S3 S2 108.79(18) . . ?
O9 S3 O7 112.6(2) . . ?
O9 S3 O8 111.4(2) . . ?
Mo1 S1 Mo2 71.49(4) . . ?
S3 S2 Mo2 107.59(6) . 2 ?
Mo1 O5 Mo2 87.18(13) . . ?
Mo1 O5 Mo2 108.27(14) . 2 ?
Mo2 O5 Mo2 107.17(15) . 2 ?
Mo2 O1 Mo1 109.50(15) 2 . ?
C1 O1 Mo1 118.8(3) . . ?
C1 O1 Mo2 131.4(3) . 2 ?
C2 O2 Mo1 121.8(3) . . ?
S3 O7 Mo1 135.9(2) . . ?
C3 N2 H2 118.8 . . ?
C3 N2 C7 122.4(5) . . ?
C7 N2 H2 118.8 . . ?
C8 N3 C12 118.0(5) . . ?
C17 N5 H5 118.9 . . ?
C17 N5 C13 122.2(5) . . ?
C13 N5 H5 118.9 . . ?
C18 N6 C22 117.1(5) . . ?
C17 N4 H4A 115.9 . . ?
C17 N4 C18 128.3(4) . . ?
C18 N4 H4A 115.9 . . ?
C12 N1 H1 114.8 . . ?
C12 N1 C3 130.4(5) . . ?
C3 N1 H1 114.8 . . ?
N3 C12 N1 116.0(5) . . ?
N3 C12 C11 122.5(5) . . ?
N1 C12 C11 121.5(5) . . ?
O1 C1 C2 108.9(4) . . ?
O1 C1 H1A 107(4) . . ?
O1 C1 H1B 111(4) . . ?
C2 C1 H1A 110(4) . . ?
C2 C1 H1B 108(4) . . ?
H1A C1 H1B 113(5) . . ?
N2 C3 N1 117.4(5) . . ?
N2 C3 C4 119.3(5) . . ?
N1 C3 C4 123.4(5) . . ?
O2 C2 C1 114.9(4) . . ?
O3 C2 O2 123.5(5) . . ?
O3 C2 C1 121.6(5) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C11 C10 C9 120.1(5) . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.5(5) . . ?
C15 C14 H14 120.3 . . ?
N5 C17 N4 119.0(5) . . ?
N5 C17 C16 119.3(5) . . ?
N4 C17 C16 121.7(5) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 C10 118.1(5) . . ?
C8 C9 H9 120.9 . . ?
N6 C18 N4 117.7(5) . . ?
N6 C18 C19 123.8(5) . . ?
C19 C18 N4 118.5(5) . . ?
N3 C8 C9 123.2(5) . . ?
N3 C8 H8 118.4 . . ?
C9 C8 H8 118.4 . . ?
N5 C13 H13 120.1 . . ?
C14 C13 N5 119.8(5) . . ?
C14 C13 H13 120.1 . . ?
C3 C4 H4 120.4 . . ?
C23 C4 C3 119.2(5) . . ?
C23 C4 H4 120.4 . . ?
C12 C11 H11 121.0 . . ?
C10 C11 C12 118.1(5) . . ?
C10 C11 H11 121.0 . . ?
C17 C16 H16 120.7 . . ?
C15 C16 C17 118.6(5) . . ?
C15 C16 H16 120.7 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.6(5) . . ?
C16 C15 H15 119.7 . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C22 C21 C20 119.4(5) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 C21 118.6(5) . . ?
C19 C20 H20 120.7 . . ?
C18 C19 H19 121.0 . . ?
C20 C19 C18 118.1(5) . . ?
C20 C19 H19 121.0 . . ?
C7 C6 H6 120.7 . . ?
C7 C6 C23 118.6(5) . . ?
C23 C6 H6 120.7 . . ?
N2 C7 C6 119.7(5) . . ?
N2 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
N6 C22 C21 123.0(5) . . ?
N6 C22 H22 118.5 . . ?
C21 C22 H22 118.5 . . ?
C4 C23 C6 120.9(5) . . ?
C4 C23 H23 119.6 . . ?
C6 C23 H23 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O1 C1 C2 -11.1(5) . . . . ?
Mo1 O2 C2 O3 -176.4(4) . . . . ?
Mo1 O2 C2 C1 2.8(5) . . . . ?
Mo2 O1 C1 C2 175.3(3) 2 . . . ?
S2 S3 O7 Mo1 47.5(3) . . . . ?
O1 C1 C2 O2 5.4(6) . . . . ?
O1 C1 C2 O3 -175.3(4) . . . . ?
O8 S3 O7 Mo1 162.3(3) . . . . ?
O9 S3 O7 Mo1 -73.2(4) . . . . ?
N2 C3 C4 C23 -1.0(8) . . . . ?
N3 C12 C11 C10 -0.1(7) . . . . ?
N5 C17 C16 C15 2.3(8) . . . . ?
N6 C18 C19 C20 1.3(9) . . . . ?
N4 C17 C16 C15 -176.5(5) . . . . ?
N4 C18 C19 C20 -178.2(5) . . . . ?
N1 C12 C11 C10 -179.4(5) . . . . ?
N1 C3 C4 C23 178.2(5) . . . . ?
C12 N3 C8 C9 0.8(8) . . . . ?
C12 N1 C3 N2 -0.4(8) . . . . ?
C12 N1 C3 C4 -179.5(5) . . . . ?
C3 N2 C7 C6 -0.2(8) . . . . ?
C3 N1 C12 N3 1.2(8) . . . . ?
C3 N1 C12 C11 -179.4(5) . . . . ?
C3 C4 C23 C6 0.0(8) . . . . ?
C10 C9 C8 N3 0.6(8) . . . . ?
C17 N5 C13 C14 -0.7(8) . . . . ?
C17 N4 C18 N6 15.0(9) . . . . ?
C17 N4 C18 C19 -165.5(6) . . . . ?
C17 C16 C15 C14 -2.2(9) . . . . ?
C9 C10 C11 C12 1.5(7) . . . . ?
C18 N6 C22 C21 0.2(8) . . . . ?
C18 N4 C17 N5 -7.8(9) . . . . ?
C18 N4 C17 C16 171.1(6) . . . . ?
C8 N3 C12 N1 178.3(5) . . . . ?
C8 N3 C12 C11 -1.1(7) . . . . ?
C13 N5 C17 N4 178.0(5) . . . . ?
C13 N5 C17 C16 -0.9(8) . . . . ?
C13 C14 C15 C16 0.7(9) . . . . ?
C11 C10 C9 C8 -1.8(7) . . . . ?
C15 C14 C13 N5 0.8(8) . . . . ?
C21 C20 C19 C18 1.1(8) . . . . ?
C20 C21 C22 N6 2.1(9) . . . . ?
C7 N2 C3 N1 -178.1(5) . . . . ?
C7 N2 C3 C4 1.1(7) . . . . ?
C7 C6 C23 C4 0.9(9) . . . . ?
C22 N6 C18 N4 177.6(5) . . . . ?
C22 N6 C18 C19 -1.9(8) . . . . ?
C22 C21 C20 C19 -2.7(8) . . . . ?
C23 C6 C7 N2 -0.8(8) . . . . ?

_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 2.022
_oxdiff_exptl_absorpt_empirical_full_min 0.695

# start Validation Reply Form
_vrf_PLAT971_exp_1830            
;
PROBLEM: Check Calcd Resid. Dens.  0.91Ang From S3              3.30 eA-3  
RESPONSE: The large residual hole is around the center of sulfur.

This alert, probably due to difficulties in absorption correction.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_1_sq
_database_code_depnum_ccdc_archive 'CCDC 2181235'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;Xiamen University
China
;
_audit_update_record             
;
2022-06-22 deposited with the CCDC.	2022-11-08 downloaded from the CCDC.
;
_audit_creation_date             2022-06-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H50 Mo16 N24 Na2 O46'
_chemical_formula_sum            'C44 H50 Mo16 N24 Na2 O46'
_chemical_formula_weight         3232.10
_chemical_melting_point          ?
_chemical_oxdiff_formula         C44H50Mo16N24O44
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'

_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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   43.6195(7)
_cell_length_b                   13.79520(10)
_cell_length_c                   20.6277(3)
_cell_angle_alpha                90
_cell_angle_beta                 121.411(2)
_cell_angle_gamma                90
_cell_volume                     10593.5(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14923
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.4490
_cell_measurement_theta_min      2.3750
_shelx_estimated_absorpt_T_max   0.649
_shelx_estimated_absorpt_T_min   0.301
_exptl_absorpt_coefficient_mu    15.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
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    2.027
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30981
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.073
_diffrn_reflns_theta_min         2.374
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  22.00   0.50    1.30    --    0.00  50.00 -39.00   52
  2  ω     29.00  71.00   0.50    1.30    --    0.00  50.00 -39.00   84
  3  ω   -169.00-122.00   0.50    6.00    --  -96.86 -50.00 174.00   94
  4  ω    -53.00 -25.00   0.50    6.00    --  -96.86  50.00 -39.00   56
  5  ω     85.00 152.00   0.50    6.00    --   96.86  50.00 -39.00  134
  6  ω     27.00  59.00   0.50    6.00    --   96.86 -50.00 174.00   64
  7  ω    -16.00  29.00   0.50    1.30    --    0.00 -99.00  60.00   90
  8  ω    -54.00  12.00   0.50    1.30    --    0.00 -50.00 174.00  132
  9  ω   -168.00 -85.00   0.50    6.00    --  -96.86 -57.00 120.00  166
 10  ω    -63.00 -28.00   0.50    6.00    --  -96.86  57.00 -90.00   70
 11  ω    -64.00 -26.00   0.50    6.00    --  -96.86  57.00  90.00   76
 12  ω    -62.00 -26.00   0.50    6.00    --  -96.86  57.00 150.00   72
 13  ω    -64.00 -39.00   0.50    6.00    --  -96.86  57.00   0.00   50
 14  ω    -64.00 -36.00   0.50    6.00    --  -96.86  57.00 120.00   56
 15  ω    -63.00 -26.00   0.50    6.00    --  -96.86  57.00  60.00   74
 16  ω     25.00  62.00   0.50    6.00    --   96.86 -99.00 150.00   74
 17  ω     30.00  60.00   0.50    6.00    --   96.86 -57.00 150.00   60
 18  ω    133.00 158.00   0.50    6.00    --   96.86  57.00-120.00   50
 19  ω     88.00 115.00   0.50    6.00    --   96.86 125.00-180.00   54
 20  ω    139.00 164.00   0.50    6.00    --   96.86 125.00-180.00   50
 21  ω     42.00  67.00   0.50    6.00    --   96.86 -57.00 120.00   50
 22  ω     37.00  64.00   0.50    6.00    --   96.86 -57.00-120.00   54
 23  ω     75.00 104.00   0.50    6.00    --   96.86 -99.00 150.00   58
 24  ω     25.00  70.00   0.50    6.00    --   96.86 -99.00  60.00   90
 25  ω     83.00 121.00   0.50    6.00    --   96.86  57.00-120.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0373286000
_diffrn_orient_matrix_UB_12      0.0258446000
_diffrn_orient_matrix_UB_13      -0.0139645000
_diffrn_orient_matrix_UB_21      0.0177524000
_diffrn_orient_matrix_UB_22      0.0628161000
_diffrn_orient_matrix_UB_23      0.0723499000
_diffrn_orient_matrix_UB_31      -0.0017137000
_diffrn_orient_matrix_UB_32      0.0886525000
_diffrn_orient_matrix_UB_33      -0.0472264000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8156
_reflns_number_total             10101
_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.587
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         10101
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0469
_refine_ls_restrained_S_all      1.044
_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)+(0.0893P)²+15.5338P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1322
_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 O(H) groups
2. Restrained distances
 O16-H16
 0.87 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N12(H12), C7(H7), C15(H15), C6(H6A), C14(H14), C16(H16A), C8(H8),
 C13(H13), C5(H5), C11(H11), C9(H9), C10(H10), C12(H12A), C17(H17), C22(H22),
 C18(H18), C19(H19), C21(H21), C20(H20)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 0.25789(2) 0.32139(3) 0.54862(3) 0.02736(12) Uani 1 1 d . . . . .
Mo2 Mo 0.28412(2) 0.31622(3) 0.46292(3) 0.02830(12) Uani 1 1 d . . . . .
Mo3 Mo 0.32421(2) 0.06003(4) 0.48073(3) 0.03144(13) Uani 1 1 d . . . . .
Mo6 Mo 0.35732(2) 0.33054(4) 0.67764(3) 0.03190(13) Uani 1 1 d . . . . .
Mo7 Mo 0.38621(2) 0.28683(4) 0.53150(3) 0.03515(14) Uani 1 1 d . . . . .
Mo5 Mo 0.37777(2) 0.15243(4) 0.69200(3) 0.03288(13) Uani 1 1 d . . . . .
Mo8 Mo 0.36289(2) 0.46180(4) 0.51685(3) 0.03577(14) Uani 1 1 d . . . . .
Mo4 Mo 0.39231(2) 0.02495(4) 0.54304(3) 0.03713(14) Uani 1 1 d . . . . .
O3 O 0.29042(11) 0.1754(3) 0.4585(2) 0.0306(9) Uani 1 1 d . . . . .
O2 O 0.30875(11) 0.3308(3) 0.5724(2) 0.0312(9) Uani 1 1 d . . . . .
O1 O 0.26906(11) 0.1751(3) 0.5685(2) 0.0296(9) Uani 1 1 d . . . . .
O5 O 0.36590(12) 0.1478(3) 0.5133(3) 0.0360(10) Uani 1 1 d . . . . .
O13 O 0.33659(12) 0.3390(3) 0.4846(2) 0.0327(9) Uani 1 1 d . . . . .
O16 O 0.33361(12) 0.0988(3) 0.5926(2) 0.0332(9) Uani 1 1 d D . . . .
H16 H 0.3131(10) 0.110(5) 0.589(4) 0.040 Uiso 1 1 d D U . . .
O20 O 0.36090(13) 0.4614(3) 0.6215(2) 0.0371(10) Uani 1 1 d . . . . .
O9 O 0.38086(12) 0.2593(3) 0.6318(2) 0.0371(10) Uani 1 1 d . . . . .
O8 O 0.34299(12) 0.2154(3) 0.7093(2) 0.0345(10) Uani 1 1 d . . . . .
O12 O 0.41084(13) 0.4048(4) 0.5849(3) 0.0420(11) Uani 1 1 d . . . . .
O6 O 0.31183(13) 0.0395(3) 0.3905(3) 0.0397(10) Uani 1 1 d . . . . .
O17 O 0.40390(12) 0.0525(3) 0.6578(3) 0.0381(10) Uani 1 1 d . . . . .
O4 O 0.35314(13) -0.0535(3) 0.5347(3) 0.0393(10) Uani 1 1 d . . . . .
O21 O 0.38280(14) 0.5978(4) 0.5688(3) 0.0478(12) Uani 1 1 d . . . . .
O10 O 0.41619(13) 0.1584(4) 0.7787(3) 0.0425(11) Uani 1 1 d . . . . .
N7 N 0.24917(14) 0.0208(4) 0.4542(3) 0.0312(11) Uani 1 1 d . . . . .
O18 O 0.42652(14) -0.0883(4) 0.6101(3) 0.0477(12) Uani 1 1 d . . . . .
O7 O 0.39636(14) -0.0101(4) 0.4702(3) 0.0464(12) Uani 1 1 d . . . . .
N3 N 0.27987(15) 0.4678(4) 0.4398(3) 0.0335(11) Uani 1 1 d . . . . .
O14 O 0.39022(13) 0.2837(4) 0.4540(3) 0.0429(11) Uani 1 1 d . . . . .
O11 O 0.39098(13) 0.3757(3) 0.7600(3) 0.0418(11) Uani 1 1 d . . . . .
O15 O 0.36706(13) 0.4969(4) 0.4435(3) 0.0440(11) Uani 1 1 d . . . . .
N2 N 0.31956(14) 0.3941(4) 0.7035(3) 0.0348(12) Uani 1 1 d . . . . .
N1 N 0.28483(15) 0.3604(4) 0.6687(3) 0.0316(11) Uani 1 1 d . . . . .
N8 N 0.28118(14) -0.0212(4) 0.4749(3) 0.0324(11) Uani 1 1 d . . . . .
N4 N 0.30972(15) 0.5243(4) 0.4646(3) 0.0347(12) Uani 1 1 d . . . . .
N10 N 0.43669(15) 0.2159(4) 0.5996(3) 0.0415(13) Uani 1 1 d . . . . .
N6 N 0.22603(16) 0.3339(4) 0.2873(3) 0.0350(12) Uani 1 1 d . . . . .
H6 H 0.208860 0.335281 0.297727 0.042 Uiso 1 1 calc R U . . .
N11 N 0.36297(16) 0.0178(4) 0.7295(3) 0.0386(12) Uani 1 1 d . . . . .
N9 N 0.43935(15) 0.1181(4) 0.5892(3) 0.0417(13) Uani 1 1 d . . . . .
N5 N 0.26129(16) 0.3173(4) 0.3396(3) 0.0345(12) Uani 1 1 d . . . . .
O19 O 0.46121(19) -0.1515(5) 0.7237(4) 0.0750(19) Uani 1 1 d . . . . .
O22 O 0.3915(3) 0.7031(5) 0.6566(4) 0.100(3) Uani 1 1 d . . . . .
N12 N 0.35404(19) -0.0643(4) 0.6886(4) 0.0527(16) Uani 1 1 d . . . . .
H12 H 0.353294 -0.071188 0.645413 0.063 Uiso 1 1 calc R U . . .
C7 C 0.27083(19) 0.3921(5) 0.7089(3) 0.0348(14) Uani 1 1 d . . . . .
H7 H 0.246818 0.381402 0.696264 0.042 Uiso 1 1 calc R U . . .
C15 C 0.24082(18) -0.1384(4) 0.4437(4) 0.0343(14) Uani 1 1 d . . . . .
H15 H 0.229794 -0.200377 0.434392 0.041 Uiso 1 1 calc R U . . .
C6 C 0.2967(2) 0.4432(5) 0.7719(4) 0.0413(16) Uani 1 1 d . . . . .
H6A H 0.294262 0.472005 0.810873 0.050 Uiso 1 1 calc R U . . .
C14 C 0.2249(2) -0.0488(4) 0.4343(4) 0.0349(14) Uani 1 1 d . . . . .
H14 H 0.200154 -0.038570 0.416224 0.042 Uiso 1 1 calc R U . . .
C16 C 0.27650(19) -0.1177(4) 0.4698(4) 0.0361(14) Uani 1 1 d . . . . .
H16A H 0.294761 -0.164412 0.482139 0.043 Uiso 1 1 calc R U . . .
C8 C 0.2505(2) 0.5238(5) 0.3972(4) 0.0367(14) Uani 1 1 d . . . . .
H8 H 0.226342 0.502369 0.373774 0.044 Uiso 1 1 calc R U . . .
C13 C 0.2209(2) 0.3474(5) 0.2194(4) 0.0446(17) Uani 1 1 d . . . . .
H13 H 0.198529 0.359365 0.174151 0.053 Uiso 1 1 calc R U . . .
C5 C 0.3264(2) 0.4426(5) 0.7654(4) 0.0403(15) Uani 1 1 d . . . . .
H5 H 0.348720 0.472615 0.800138 0.048 Uiso 1 1 calc R U . . .
C11 C 0.2783(2) 0.3222(5) 0.3023(4) 0.0378(15) Uani 1 1 d . . . . .
H11 H 0.303419 0.314081 0.324388 0.045 Uiso 1 1 calc R U . . .
C9 C 0.2611(2) 0.6169(5) 0.3930(4) 0.0417(16) Uani 1 1 d . . . . .
H9 H 0.246184 0.670800 0.366570 0.050 Uiso 1 1 calc R U . . .
C10 C 0.2981(2) 0.6139(5) 0.4358(4) 0.0377(14) Uani 1 1 d . . . . .
H10 H 0.313337 0.667522 0.443945 0.045 Uiso 1 1 calc R U . . .
C3 C 0.3730(2) 0.5461(5) 0.6665(4) 0.0426(16) Uani 1 1 d . . . . .
H3A H 0.394301 0.530330 0.716739 0.051 Uiso 1 1 calc R U . . .
H3B H 0.353948 0.570577 0.674540 0.051 Uiso 1 1 calc R U . . .
C2 C 0.4413(2) -0.0867(5) 0.6824(5) 0.0483(18) Uani 1 1 d . . . . .
C12 C 0.2538(2) 0.3412(5) 0.2253(4) 0.0470(18) Uani 1 1 d . . . . .
H12A H 0.258749 0.348195 0.185819 0.056 Uiso 1 1 calc R U . . .
C1 C 0.4328(2) -0.0024(6) 0.7154(4) 0.0514(19) Uani 1 1 d . . . . .
H1A H 0.426385 -0.025840 0.752176 0.062 Uiso 1 1 calc R U . . .
H1B H 0.454287 0.039513 0.743091 0.062 Uiso 1 1 calc R U . . .
C17 C 0.4742(2) 0.0972(6) 0.6228(5) 0.0508(19) Uani 1 1 d . . . . .
H17 H 0.483469 0.034635 0.623677 0.061 Uiso 1 1 calc R U . . .
C22 C 0.3622(2) 0.0000(6) 0.7915(4) 0.0504(19) Uani 1 1 d . . . . .
H22 H 0.368363 0.044439 0.831720 0.061 Uiso 1 1 calc R U . . .
C18 C 0.4950(2) 0.1788(6) 0.6563(6) 0.062(2) Uani 1 1 d . . . . .
H18 H 0.520464 0.183687 0.684661 0.074 Uiso 1 1 calc R U . . .
C19 C 0.4701(2) 0.2513(6) 0.6388(5) 0.0525(19) Uani 1 1 d . . . . .
H19 H 0.475830 0.317450 0.652679 0.063 Uiso 1 1 calc R U . . .
C4 C 0.3826(3) 0.6220(6) 0.6296(5) 0.060(2) Uani 1 1 d . . . . .
C21 C 0.3507(4) -0.0957(8) 0.7878(7) 0.089(4) Uani 1 1 d . . . . .
H21 H 0.346717 -0.127198 0.823772 0.107 Uiso 1 1 calc R U . . .
C20 C 0.3463(3) -0.1351(7) 0.7234(7) 0.076(3) Uani 1 1 d . . . . .
H20 H 0.339277 -0.199666 0.706052 0.092 Uiso 1 1 calc R U . . .
Na1 Na 0.3625(2) 0.7736(5) 0.4786(5) 0.147(3) Uani 1 1 d . . . . .
O1W O 0.3809(4) 0.7789(11) 0.3742(6) 0.161(5) Uani 1 1 d . . . . .


_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 2.6340(9) 7_556 ?
Mo1 Mo2 2.5588(7) . ?
Mo1 Mo2 2.5620(7) 7_556 ?
Mo1 O3 2.035(4) 7_556 ?
Mo1 O2 2.011(4) . ?
Mo1 O1 2.065(4) 7_556 ?
Mo1 O1 2.067(4) . ?
Mo1 N7 2.195(5) 7_556 ?
Mo1 N1 2.184(5) . ?
Mo2 O3 1.971(4) . ?
Mo2 O2 1.940(4) . ?
Mo2 O1 2.061(4) 7_556 ?
Mo2 O13 2.114(5) . ?
Mo2 N3 2.132(5) . ?
Mo2 N5 2.196(5) . ?
Mo3 Mo4 2.5944(7) . ?
Mo3 O3 2.052(4) . ?
Mo3 O5 1.988(5) . ?
Mo3 O16 2.190(4) . ?
Mo3 O6 1.670(5) . ?
Mo3 O4 1.955(4) . ?
Mo3 N8 2.135(6) . ?
Mo6 Mo5 2.5778(7) . ?
Mo6 O2 2.100(4) . ?
Mo6 O20 2.195(4) . ?
Mo6 O9 1.981(5) . ?
Mo6 O8 1.940(4) . ?
Mo6 O11 1.682(5) . ?
Mo6 N2 2.164(6) . ?
Mo7 Mo8 2.5753(8) . ?
Mo7 O5 2.063(4) . ?
Mo7 O13 1.989(5) . ?
Mo7 O9 2.232(5) . ?
Mo7 O12 1.944(5) . ?
Mo7 O14 1.697(5) . ?
Mo7 N10 2.134(6) . ?
Mo5 O16 2.084(4) . ?
Mo5 O9 1.976(5) . ?
Mo5 O8 1.935(5) . ?
Mo5 O17 2.129(5) . ?
Mo5 O10 1.700(5) . ?
Mo5 N11 2.232(6) . ?
Mo8 O13 1.958(4) . ?
Mo8 O20 2.205(5) . ?
Mo8 O12 1.976(5) . ?
Mo8 O21 2.110(5) . ?
Mo8 O15 1.686(5) . ?
Mo8 N4 2.163(6) . ?
Mo4 O5 1.960(4) . ?
Mo4 O17 2.182(5) . ?
Mo4 O4 1.953(5) . ?
Mo4 O18 2.105(5) . ?
Mo4 O7 1.674(5) . ?
Mo4 N9 2.175(6) . ?
Mo4 Na1 3.699(7) 1_545 ?
O16 H16 0.867(10) . ?
O20 C3 1.412(8) . ?
O17 C1 1.418(8) . ?
O4 Na1 2.774(8) 1_545 ?
O21 C4 1.302(10) . ?
O21 Na1 2.900(9) . ?
N7 N8 1.358(7) . ?
N7 C14 1.327(8) . ?
O18 C2 1.278(9) . ?
N3 N4 1.367(8) . ?
N3 C8 1.355(8) . ?
N2 N1 1.376(7) . ?
N2 C5 1.330(8) . ?
N1 C7 1.334(8) . ?
N8 C16 1.343(8) . ?
N4 C10 1.350(8) . ?
N10 N9 1.381(9) . ?
N10 C19 1.336(9) . ?
N6 H6 0.8800 . ?
N6 N5 1.361(8) . ?
N6 C13 1.313(9) . ?
N11 N12 1.343(8) . ?
N11 C22 1.321(9) . ?
N9 C17 1.331(9) . ?
N5 C11 1.319(9) . ?
O19 C2 1.227(9) . ?
O22 C4 1.219(10) . ?
N12 H12 0.8800 . ?
N12 C20 1.353(12) . ?
C7 H7 0.9500 . ?
C7 C6 1.389(9) . ?
C15 H15 0.9500 . ?
C15 C14 1.381(9) . ?
C15 C16 1.386(10) . ?
C6 H6A 0.9500 . ?
C6 C5 1.373(11) . ?
C14 H14 0.9500 . ?
C16 H16A 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.382(10) . ?
C13 H13 0.9500 . ?
C13 C12 1.376(12) . ?
C5 H5 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.402(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.379(10) . ?
C10 H10 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.477(11) . ?
C2 C1 1.490(12) . ?
C12 H12A 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C17 H17 0.9500 . ?
C17 C18 1.384(12) . ?
C22 H22 0.9500 . ?
C22 C21 1.401(14) . ?
C18 H18 0.9500 . ?
C18 C19 1.381(12) . ?
C19 H19 0.9500 . ?
C21 H21 0.9500 . ?
C21 C20 1.354(16) . ?
C20 H20 0.9500 . ?
Na1 O1W 2.661(11) . ?

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 Mo1 58.99(2) 7_556 7_556 ?
Mo2 Mo1 Mo1 59.10(2) . 7_556 ?
Mo2 Mo1 Mo2 118.09(2) . 7_556 ?
O3 Mo1 Mo1 96.41(12) 7_556 7_556 ?
O3 Mo1 Mo2 49.14(12) 7_556 7_556 ?
O3 Mo1 Mo2 140.35(12) 7_556 . ?
O3 Mo1 O1 88.79(17) 7_556 7_556 ?
O3 Mo1 O1 99.41(17) 7_556 . ?
O3 Mo1 N7 81.42(18) 7_556 7_556 ?
O3 Mo1 N1 90.07(19) 7_556 . ?
O2 Mo1 Mo1 92.94(12) . 7_556 ?
O2 Mo1 Mo2 48.44(12) . . ?
O2 Mo1 Mo2 135.66(12) . 7_556 ?
O2 Mo1 O3 170.15(17) . 7_556 ?
O2 Mo1 O1 99.58(17) . 7_556 ?
O2 Mo1 O1 84.20(17) . . ?
O2 Mo1 N7 93.67(18) . 7_556 ?
O2 Mo1 N1 80.46(19) . . ?
O1 Mo1 Mo1 50.36(11) . 7_556 ?
O1 Mo1 Mo1 50.43(11) 7_556 7_556 ?
O1 Mo1 Mo2 88.06(12) . . ?
O1 Mo1 Mo2 88.02(11) 7_556 7_556 ?
O1 Mo1 Mo2 51.60(13) 7_556 . ?
O1 Mo1 Mo2 51.53(12) . 7_556 ?
O1 Mo1 O1 100.79(14) 7_556 . ?
O1 Mo1 N7 87.68(17) 7_556 7_556 ?
O1 Mo1 N7 171.49(17) . 7_556 ?
O1 Mo1 N1 164.37(17) 7_556 . ?
O1 Mo1 N1 94.77(17) . . ?
N7 Mo1 Mo1 138.10(13) 7_556 7_556 ?
N7 Mo1 Mo2 130.44(14) 7_556 7_556 ?
N7 Mo1 Mo2 96.70(14) 7_556 . ?
N1 Mo1 Mo1 145.11(14) . 7_556 ?
N1 Mo1 Mo2 128.32(15) . . ?
N1 Mo1 Mo2 102.95(14) . 7_556 ?
N1 Mo1 N7 76.74(19) . 7_556 ?
Mo1 Mo2 Mo1 61.91(2) . 7_556 ?
O3 Mo2 Mo1 100.56(13) . . ?
O3 Mo2 Mo1 51.37(13) . 7_556 ?
O3 Mo2 O1 101.78(17) . 7_556 ?
O3 Mo2 O13 89.67(17) . . ?
O3 Mo2 N3 162.67(19) . . ?
O3 Mo2 N5 86.73(18) . . ?
O2 Mo2 Mo1 96.92(13) . 7_556 ?
O2 Mo2 Mo1 50.87(13) . . ?
O2 Mo2 O3 98.66(17) . . ?
O2 Mo2 O1 102.13(17) . 7_556 ?
O2 Mo2 O13 81.75(17) . . ?
O2 Mo2 N3 95.14(18) . . ?
O2 Mo2 N5 171.5(2) . . ?
O1 Mo2 Mo1 51.74(11) 7_556 7_556 ?
O1 Mo2 Mo1 51.74(11) 7_556 . ?
O1 Mo2 O13 167.09(16) 7_556 . ?
O1 Mo2 N3 85.41(19) 7_556 . ?
O1 Mo2 N5 83.01(19) 7_556 . ?
O13 Mo2 Mo1 140.59(11) . 7_556 ?
O13 Mo2 Mo1 132.39(12) . . ?
O13 Mo2 N3 82.0(2) . . ?
O13 Mo2 N5 91.81(19) . . ?
N3 Mo2 Mo1 96.28(15) . . ?
N3 Mo2 Mo1 137.02(16) . 7_556 ?
N3 Mo2 N5 78.45(19) . . ?
N5 Mo2 Mo1 134.74(16) . . ?
N5 Mo2 Mo1 91.54(15) . 7_556 ?
O3 Mo3 Mo4 139.37(12) . . ?
O3 Mo3 O16 76.37(16) . . ?
O3 Mo3 N8 83.49(18) . . ?
O5 Mo3 Mo4 48.45(13) . . ?
O5 Mo3 O3 91.53(18) . . ?
O5 Mo3 O16 81.90(18) . . ?
O5 Mo3 N8 164.03(19) . . ?
O16 Mo3 Mo4 89.22(12) . . ?
O6 Mo3 Mo4 98.17(17) . . ?
O6 Mo3 O3 96.0(2) . . ?
O6 Mo3 O5 100.8(2) . . ?
O6 Mo3 O16 172.1(2) . . ?
O6 Mo3 O4 103.7(2) . . ?
O6 Mo3 N8 94.8(2) . . ?
O4 Mo3 Mo4 48.38(14) . . ?
O4 Mo3 O3 157.54(19) . . ?
O4 Mo3 O5 95.20(19) . . ?
O4 Mo3 O16 83.39(18) . . ?
O4 Mo3 N8 84.2(2) . . ?
N8 Mo3 Mo4 132.55(14) . . ?
N8 Mo3 O16 82.18(18) . . ?
O2 Mo6 Mo5 102.88(11) . . ?
O2 Mo6 O20 76.33(16) . . ?
O2 Mo6 N2 76.52(18) . . ?
O20 Mo6 Mo5 136.84(13) . . ?
O9 Mo6 Mo5 49.28(13) . . ?
O9 Mo6 O2 90.12(17) . . ?
O9 Mo6 O20 87.67(18) . . ?
O9 Mo6 N2 165.69(19) . . ?
O8 Mo6 Mo5 48.23(14) . . ?
O8 Mo6 O2 91.20(17) . . ?
O8 Mo6 O20 167.21(18) . . ?
O8 Mo6 O9 95.28(19) . . ?
O8 Mo6 N2 80.1(2) . . ?
O11 Mo6 Mo5 99.75(17) . . ?
O11 Mo6 O2 157.3(2) . . ?
O11 Mo6 O20 87.9(2) . . ?
O11 Mo6 O9 105.6(2) . . ?
O11 Mo6 O8 103.2(2) . . ?
O11 Mo6 N2 88.7(2) . . ?
N2 Mo6 Mo5 128.32(15) . . ?
N2 Mo6 O20 94.00(19) . . ?
O5 Mo7 Mo8 138.06(13) . . ?
O5 Mo7 O9 76.58(17) . . ?
O5 Mo7 N10 83.8(2) . . ?
O13 Mo7 Mo8 48.76(12) . . ?
O13 Mo7 O5 89.55(18) . . ?
O13 Mo7 O9 84.21(17) . . ?
O13 Mo7 N10 166.8(2) . . ?
O9 Mo7 Mo8 92.45(12) . . ?
O12 Mo7 Mo8 49.47(15) . . ?
O12 Mo7 O5 159.87(18) . . ?
O12 Mo7 O13 96.48(19) . . ?
O12 Mo7 O9 84.92(18) . . ?
O12 Mo7 N10 86.3(2) . . ?
O14 Mo7 Mo8 98.13(17) . . ?
O14 Mo7 O5 92.9(2) . . ?
O14 Mo7 O13 99.9(2) . . ?
O14 Mo7 O9 168.8(2) . . ?
O14 Mo7 O12 104.9(2) . . ?
O14 Mo7 N10 91.8(2) . . ?
N10 Mo7 Mo8 135.71(16) . . ?
N10 Mo7 O9 83.2(2) . . ?
O16 Mo5 Mo6 97.94(12) . . ?
O16 Mo5 O17 79.90(18) . . ?
O16 Mo5 N11 76.08(19) . . ?
O9 Mo5 Mo6 49.44(14) . . ?
O9 Mo5 O16 88.71(17) . . ?
O9 Mo5 O17 92.96(19) . . ?
O9 Mo5 N11 164.7(2) . . ?
O8 Mo5 Mo6 48.39(13) . . ?
O8 Mo5 O16 85.92(18) . . ?
O8 Mo5 O9 95.60(19) . . ?
O8 Mo5 O17 163.25(19) . . ?
O8 Mo5 N11 85.0(2) . . ?
O17 Mo5 Mo6 142.38(13) . . ?
O17 Mo5 N11 82.9(2) . . ?
O10 Mo5 Mo6 99.62(17) . . ?
O10 Mo5 O16 162.0(2) . . ?
O10 Mo5 O9 105.8(2) . . ?
O10 Mo5 O8 102.8(2) . . ?
O10 Mo5 O17 88.6(2) . . ?
O10 Mo5 N11 88.9(2) . . ?
N11 Mo5 Mo6 133.42(15) . . ?
O13 Mo8 Mo7 49.79(13) . . ?
O13 Mo8 O20 90.88(17) . . ?
O13 Mo8 O12 96.45(19) . . ?
O13 Mo8 O21 162.7(2) . . ?
O13 Mo8 N4 83.65(19) . . ?
O20 Mo8 Mo7 95.60(12) . . ?
O12 Mo8 Mo7 48.41(14) . . ?
O12 Mo8 O20 82.59(19) . . ?
O12 Mo8 O21 89.4(2) . . ?
O12 Mo8 N4 167.4(2) . . ?
O21 Mo8 Mo7 137.80(15) . . ?
O21 Mo8 O20 73.75(18) . . ?
O21 Mo8 N4 87.1(2) . . ?
O15 Mo8 Mo7 98.82(18) . . ?
O15 Mo8 O13 105.2(2) . . ?
O15 Mo8 O20 163.1(2) . . ?
O15 Mo8 O12 100.5(2) . . ?
O15 Mo8 O21 89.6(2) . . ?
O15 Mo8 N4 91.6(2) . . ?
N4 Mo8 Mo7 133.42(14) . . ?
N4 Mo8 O20 84.80(19) . . ?
Mo3 Mo4 Na1 84.25(14) . 1_545 ?
O5 Mo4 Mo3 49.39(13) . . ?
O5 Mo4 O17 87.42(18) . . ?
O5 Mo4 O18 161.34(19) . . ?
O5 Mo4 N9 83.8(2) . . ?
O5 Mo4 Na1 131.26(19) . 1_545 ?
O17 Mo4 Mo3 93.62(12) . . ?
O17 Mo4 Na1 113.12(17) . 1_545 ?
O4 Mo4 Mo3 48.44(13) . . ?
O4 Mo4 O5 96.16(19) . . ?
O4 Mo4 O17 83.64(19) . . ?
O4 Mo4 O18 86.2(2) . . ?
O4 Mo4 N9 161.5(2) . . ?
O4 Mo4 Na1 47.27(18) . 1_545 ?
O18 Mo4 Mo3 134.47(15) . . ?
O18 Mo4 O17 74.42(18) . . ?
O18 Mo4 N9 88.1(2) . . ?
O18 Mo4 Na1 62.4(2) . 1_545 ?
O7 Mo4 Mo3 103.79(17) . . ?
O7 Mo4 O5 106.8(2) . . ?
O7 Mo4 O17 162.2(2) . . ?
O7 Mo4 O4 104.9(2) . . ?
O7 Mo4 O18 90.3(2) . . ?
O7 Mo4 N9 92.7(2) . . ?
O7 Mo4 Na1 65.7(2) . 1_545 ?
N9 Mo4 Mo3 133.01(16) . . ?
N9 Mo4 O17 77.9(2) . . ?
N9 Mo4 Na1 141.8(2) . 1_545 ?
Mo1 O3 Mo3 129.0(2) 7_556 . ?
Mo2 O3 Mo1 79.49(15) . 7_556 ?
Mo2 O3 Mo3 148.8(2) . . ?
Mo1 O2 Mo6 130.0(2) . . ?
Mo2 O2 Mo1 80.69(16) . . ?
Mo2 O2 Mo6 148.4(2) . . ?
Mo1 O1 Mo1 79.21(14) 7_556 . ?
Mo2 O1 Mo1 76.73(15) 7_556 . ?
Mo2 O1 Mo1 76.66(14) 7_556 7_556 ?
Mo3 O5 Mo7 149.1(2) . . ?
Mo4 O5 Mo3 82.16(17) . . ?
Mo4 O5 Mo7 128.3(2) . . ?
Mo7 O13 Mo2 146.4(2) . . ?
Mo8 O13 Mo2 125.3(2) . . ?
Mo8 O13 Mo7 81.45(17) . . ?
Mo3 O16 H16 109(5) . . ?
Mo5 O16 Mo3 133.8(2) . . ?
Mo5 O16 H16 114(5) . . ?
Mo6 O20 Mo8 124.6(2) . . ?
C3 O20 Mo6 116.0(4) . . ?
C3 O20 Mo8 116.7(4) . . ?
Mo6 O9 Mo7 133.5(2) . . ?
Mo5 O9 Mo6 81.28(18) . . ?
Mo5 O9 Mo7 141.6(2) . . ?
Mo5 O8 Mo6 83.38(18) . . ?
Mo7 O12 Mo8 82.13(18) . . ?
Mo5 O17 Mo4 127.6(2) . . ?
C1 O17 Mo5 117.6(4) . . ?
C1 O17 Mo4 114.7(4) . . ?
Mo3 O4 Na1 130.0(3) . 1_545 ?
Mo4 O4 Mo3 83.19(18) . . ?
Mo4 O4 Na1 101.6(3) . 1_545 ?
Mo8 O21 Na1 120.7(3) . . ?
C4 O21 Mo8 120.7(5) . . ?
C4 O21 Na1 104.5(5) . . ?
N8 N7 Mo1 122.6(4) . 7_556 ?
C14 N7 Mo1 129.1(4) . 7_556 ?
C14 N7 N8 108.2(5) . . ?
C2 O18 Mo4 120.6(5) . . ?
N4 N3 Mo2 121.3(4) . . ?
C8 N3 Mo2 130.3(5) . . ?
C8 N3 N4 108.2(5) . . ?
N1 N2 Mo6 120.4(4) . . ?
C5 N2 Mo6 128.4(5) . . ?
C5 N2 N1 107.9(6) . . ?
N2 N1 Mo1 118.1(4) . . ?
C7 N1 Mo1 129.4(4) . . ?
C7 N1 N2 107.5(5) . . ?
N7 N8 Mo3 121.6(4) . . ?
C16 N8 Mo3 128.2(5) . . ?
C16 N8 N7 108.0(5) . . ?
N3 N4 Mo8 121.6(4) . . ?
C10 N4 Mo8 130.0(5) . . ?
C10 N4 N3 106.9(5) . . ?
N9 N10 Mo7 119.2(4) . . ?
C19 N10 Mo7 131.0(5) . . ?
C19 N10 N9 107.3(6) . . ?
N5 N6 H6 124.4 . . ?
C13 N6 H6 124.4 . . ?
C13 N6 N5 111.2(6) . . ?
N12 N11 Mo5 121.8(5) . . ?
C22 N11 Mo5 130.4(5) . . ?
C22 N11 N12 107.8(6) . . ?
N10 N9 Mo4 120.6(4) . . ?
C17 N9 Mo4 131.3(5) . . ?
C17 N9 N10 107.2(6) . . ?
N6 N5 Mo2 124.2(4) . . ?
C11 N5 Mo2 128.5(5) . . ?
C11 N5 N6 106.0(5) . . ?
N11 N12 H12 124.9 . . ?
N11 N12 C20 110.3(8) . . ?
C20 N12 H12 124.9 . . ?
N1 C7 H7 125.1 . . ?
N1 C7 C6 109.7(6) . . ?
C6 C7 H7 125.1 . . ?
C14 C15 H15 127.7 . . ?
C14 C15 C16 104.6(6) . . ?
C16 C15 H15 127.7 . . ?
C7 C6 H6A 127.7 . . ?
C5 C6 C7 104.7(6) . . ?
C5 C6 H6A 127.7 . . ?
N7 C14 C15 110.0(6) . . ?
N7 C14 H14 125.0 . . ?
C15 C14 H14 125.0 . . ?
N8 C16 C15 109.2(6) . . ?
N8 C16 H16A 125.4 . . ?
C15 C16 H16A 125.4 . . ?
N3 C8 H8 125.1 . . ?
N3 C8 C9 109.7(6) . . ?
C9 C8 H8 125.1 . . ?
N6 C13 H13 126.0 . . ?
N6 C13 C12 107.9(7) . . ?
C12 C13 H13 126.0 . . ?
N2 C5 C6 110.1(6) . . ?
N2 C5 H5 124.9 . . ?
C6 C5 H5 124.9 . . ?
N5 C11 H11 125.0 . . ?
N5 C11 C12 110.1(7) . . ?
C12 C11 H11 125.0 . . ?
C8 C9 H9 127.8 . . ?
C10 C9 C8 104.4(6) . . ?
C10 C9 H9 127.8 . . ?
N4 C10 C9 110.8(6) . . ?
N4 C10 H10 124.6 . . ?
C9 C10 H10 124.6 . . ?
O20 C3 H3A 109.4 . . ?
O20 C3 H3B 109.4 . . ?
O20 C3 C4 111.0(6) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
O18 C2 C1 116.8(6) . . ?
O19 C2 O18 122.8(8) . . ?
O19 C2 C1 120.4(8) . . ?
C13 C12 C11 104.8(6) . . ?
C13 C12 H12A 127.6 . . ?
C11 C12 H12A 127.6 . . ?
O17 C1 C2 111.0(6) . . ?
O17 C1 H1A 109.4 . . ?
O17 C1 H1B 109.4 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N9 C17 H17 124.5 . . ?
N9 C17 C18 111.0(7) . . ?
C18 C17 H17 124.5 . . ?
N11 C22 H22 125.9 . . ?
N11 C22 C21 108.2(8) . . ?
C21 C22 H22 125.9 . . ?
C17 C18 H18 128.2 . . ?
C19 C18 C17 103.6(7) . . ?
C19 C18 H18 128.2 . . ?
N10 C19 C18 110.8(7) . . ?
N10 C19 H19 124.6 . . ?
C18 C19 H19 124.6 . . ?
O21 C4 C3 117.3(7) . . ?
O22 C4 O21 121.0(8) . . ?
O22 C4 C3 121.6(8) . . ?
C22 C21 H21 126.4 . . ?
C20 C21 C22 107.1(9) . . ?
C20 C21 H21 126.4 . . ?
N12 C20 C21 106.6(9) . . ?
N12 C20 H20 126.7 . . ?
C21 C20 H20 126.7 . . ?
O4 Na1 Mo4 31.15(13) 1_565 1_565 ?
O4 Na1 O21 120.9(3) 1_565 . ?
O21 Na1 Mo4 128.4(3) . 1_565 ?
O1W Na1 Mo4 93.9(3) . 1_565 ?
O1W Na1 O4 119.1(4) . 1_565 ?
O1W Na1 O21 115.0(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 N7 N8 Mo3 -15.1(6) 7_556 . . . ?
Mo1 N7 N8 C16 -179.3(4) 7_556 . . . ?
Mo1 N7 C14 C15 178.8(4) 7_556 . . . ?
Mo1 N1 C7 C6 -156.5(5) . . . . ?
Mo2 N3 N4 Mo8 7.6(6) . . . . ?
Mo2 N3 N4 C10 175.1(4) . . . . ?
Mo2 N3 C8 C9 -174.5(5) . . . . ?
Mo2 N5 C11 C12 -167.8(4) . . . . ?
Mo3 N8 C16 C15 -161.4(4) . . . . ?
Mo6 O20 C3 C4 166.4(6) . . . . ?
Mo6 N2 N1 Mo1 -39.2(6) . . . . ?
Mo6 N2 N1 C7 163.4(4) . . . . ?
Mo6 N2 C5 C6 -160.2(5) . . . . ?
Mo7 N10 N9 Mo4 -25.4(7) . . . . ?
Mo7 N10 N9 C17 164.3(5) . . . . ?
Mo7 N10 C19 C18 -162.6(6) . . . . ?
Mo5 O17 C1 C2 164.0(5) . . . . ?
Mo5 N11 N12 C20 179.8(6) . . . . ?
Mo5 N11 C22 C21 179.5(7) . . . . ?
Mo8 O20 C3 C4 3.8(8) . . . . ?
Mo8 O21 C4 O22 -174.3(8) . . . . ?
Mo8 O21 C4 C3 8.7(11) . . . . ?
Mo8 N4 C10 C9 166.5(5) . . . . ?
Mo4 O17 C1 C2 -17.2(8) . . . . ?
Mo4 O18 C2 O19 179.4(7) . . . . ?
Mo4 O18 C2 C1 0.7(10) . . . . ?
Mo4 N9 C17 C18 -168.3(6) . . . . ?
O20 C3 C4 O21 -7.9(11) . . . . ?
O20 C3 C4 O22 175.1(9) . . . . ?
N7 N8 C16 C15 1.5(7) . . . . ?
O18 C2 C1 O17 11.2(10) . . . . ?
N3 N4 C10 C9 0.5(8) . . . . ?
N3 C8 C9 C10 -0.7(8) . . . . ?
N2 N1 C7 C6 -2.5(7) . . . . ?
N1 N2 C5 C6 -0.9(8) . . . . ?
N1 C7 C6 C5 1.9(8) . . . . ?
N8 N7 C14 C15 1.7(7) . . . . ?
N4 N3 C8 C9 1.0(7) . . . . ?
N10 N9 C17 C18 0.6(9) . . . . ?
N6 N5 C11 C12 -0.5(7) . . . . ?
N6 C13 C12 C11 0.4(8) . . . . ?
N11 N12 C20 C21 -0.1(12) . . . . ?
N11 C22 C21 C20 2.8(13) . . . . ?
N9 N10 C19 C18 -1.4(9) . . . . ?
N9 C17 C18 C19 -1.4(10) . . . . ?
N5 N6 C13 C12 -0.8(8) . . . . ?
N5 C11 C12 C13 0.1(8) . . . . ?
O19 C2 C1 O17 -167.6(8) . . . . ?
N12 N11 C22 C21 -2.8(10) . . . . ?
C7 C6 C5 N2 -0.6(8) . . . . ?
C14 N7 N8 Mo3 162.2(4) . . . . ?
C14 N7 N8 C16 -2.0(7) . . . . ?
C14 C15 C16 N8 -0.4(8) . . . . ?
C16 C15 C14 N7 -0.8(7) . . . . ?
C8 N3 N4 Mo8 -168.3(4) . . . . ?
C8 N3 N4 C10 -0.9(7) . . . . ?
C8 C9 C10 N4 0.1(8) . . . . ?
C13 N6 N5 Mo2 168.8(4) . . . . ?
C13 N6 N5 C11 0.8(7) . . . . ?
C5 N2 N1 Mo1 159.5(4) . . . . ?
C5 N2 N1 C7 2.1(7) . . . . ?
C17 C18 C19 N10 1.7(10) . . . . ?
C22 N11 N12 C20 1.9(9) . . . . ?
C22 C21 C20 N12 -1.6(13) . . . . ?
C19 N10 N9 Mo4 170.8(5) . . . . ?
C19 N10 N9 C17 0.5(8) . . . . ?
Na1 O21 C4 O22 -34.3(12) . . . . ?
Na1 O21 C4 C3 148.7(7) . . . . ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_details          ?
_platon_squeeze_special_details  ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.006 0.008 1342 521 '52 H2O'
2 0.500 0.003 0.485 1342 521 '52 H2O'

_platon_squeeze_void_probe_radius 1.20
_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 1.663
_oxdiff_exptl_absorpt_empirical_full_min 0.704
