# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_mo_2020_1_6_jdm_tg89_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2225735'
loop_
_audit_author_name
_audit_author_address
'George T.'
;Saint Marys University
Canada
;
_audit_update_record             
;
2023-10-01 deposited with the CCDC.	2023-10-06 downloaded from the CCDC.
;
_audit_creation_date             2023-09-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Tanner.George@smu.ca
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H26 Mo2 O11'
_chemical_formula_sum            'C12 H26 Mo2 O11'
_chemical_formula_weight         538.21
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   16.7363(3)
_cell_length_b                   24.6210(5)
_cell_length_c                   8.8062(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3628.72(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    125.0
_cell_measurement_theta_max      45.19
_cell_measurement_theta_min      2.74
_shelx_estimated_absorpt_T_max   0.852
_shelx_estimated_absorpt_T_min   0.803
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.7494
_exptl_absorpt_correction_T_min  0.7016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0940 before and 0.0584 after correction. The Ratio of minimum to maximum transmission is 0.9362. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.115
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39690
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.291
_diffrn_reflns_theta_min         2.741
_diffrn_ambient_temperature      125.00
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.851
_reflns_number_gt                5824
_reflns_number_total             7050
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 
;
 Flack x determined using 2123 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         7050
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.010
_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)+(0.0160P)²+1.3443P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0487
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
;
_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 0.32751(2) 0.26441(2) 0.37675(2) 0.01110(3) Uani 1 1 d . . . . .
O1 O 0.35526(9) 0.26727(6) 0.19354(18) 0.0182(3) Uani 1 1 d . . . . .
O2 O 0.41289(8) 0.22679(6) 0.48570(19) 0.0187(3) Uani 1 1 d . . . . .
O3 O 0.37582(8) 0.32642(5) 0.47522(18) 0.0165(2) Uani 1 1 d . . . . .
O4 O 0.22735(7) 0.30899(4) 0.3751(2) 0.01265(19) Uani 1 1 d . . . . .
O5 O 0.24720(9) 0.38889(6) 0.1237(2) 0.0235(3) Uani 1 1 d . . . . .
C1 C 0.46030(13) 0.26034(8) 0.5829(3) 0.0232(4) Uani 1 1 d . . . . .
H1A H 0.516242 0.247294 0.584498 0.028 Uiso 1 1 calc R U . . .
H1B H 0.439117 0.259337 0.687843 0.028 Uiso 1 1 calc R U . . .
C2 C 0.45666(12) 0.31743(9) 0.5211(3) 0.0210(4) Uani 1 1 d . . . . .
H2A H 0.472400 0.343911 0.600248 0.025 Uiso 1 1 calc R U . . .
H2B H 0.493208 0.321418 0.433420 0.025 Uiso 1 1 calc R U . . .
C3 C 0.20400(10) 0.36512(6) 0.3794(3) 0.0149(3) Uani 1 1 d . . . . .
H3A H 0.248967 0.387431 0.417453 0.018 Uiso 1 1 calc R U . . .
H3B H 0.158371 0.369702 0.449812 0.018 Uiso 1 1 calc R U . . .
C4 C 0.18046(12) 0.38410(8) 0.2226(2) 0.0178(3) Uani 1 1 d . . . . .
H4A H 0.141801 0.358044 0.178641 0.021 Uiso 1 1 calc R U . . .
H4B H 0.153577 0.419806 0.230687 0.021 Uiso 1 1 calc R U . . .
O6 O 0.250000 0.250000 0.6224(3) 0.0168(3) Uani 1 2 d S T P . .
C5 C 0.23403(15) 0.29751(8) 0.7201(2) 0.0207(4) Uani 1 1 d . . . . .
H5A H 0.185293 0.316770 0.686051 0.025 Uiso 1 1 calc R U . . .
H5B H 0.279565 0.323157 0.717425 0.025 Uiso 1 1 calc R U . . .
C6 C 0.22274(14) 0.27492(8) 0.8785(3) 0.0249(4) Uani 1 1 d . . . . .
H6A H 0.166385 0.264569 0.896643 0.030 Uiso 1 1 calc R U . . .
H6B H 0.239481 0.301512 0.956622 0.030 Uiso 1 1 calc R U . . .
H5 H 0.2754(19) 0.4176(13) 0.154(5) 0.046(10) 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 Mo1 2.6897(3) 14 ?
Mo1 O1 1.6803(16) . ?
Mo1 O2 1.9545(14) . ?
Mo1 O3 1.9330(13) . ?
Mo1 O4 2.0038(11) . ?
Mo1 O4 2.0270(11) 14 ?
Mo1 O6 2.547(2) . ?
O2 C1 1.430(3) . ?
O3 C2 1.429(2) . ?
O4 C3 1.4368(18) . ?
O5 C4 1.421(3) . ?
O5 H5 0.89(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.508(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.510(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O6 C5 1.476(2) . ?
O6 C5 1.477(2) 14 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.514(4) . ?
C6 C6 1.529(4) 14 ?
C6 H6A 0.9900 . ?
C6 H6B 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
O1 Mo1 Mo1 106.12(5) . 14 ?
O1 Mo1 O2 106.81(7) . . ?
O1 Mo1 O3 106.38(7) . . ?
O1 Mo1 O4 101.61(7) . . ?
O1 Mo1 O4 98.96(7) . 14 ?
O1 Mo1 O6 164.15(6) . . ?
O2 Mo1 Mo1 125.47(5) . 14 ?
O2 Mo1 O4 151.02(7) . . ?
O2 Mo1 O4 84.96(6) . 14 ?
O2 Mo1 O6 83.66(5) . . ?
O3 Mo1 Mo1 127.72(4) . 14 ?
O3 Mo1 O2 81.27(6) . . ?
O3 Mo1 O4 153.74(7) . 14 ?
O3 Mo1 O4 85.44(5) . . ?
O3 Mo1 O6 86.68(5) . . ?
O4 Mo1 Mo1 47.77(3) 14 14 ?
O4 Mo1 Mo1 48.51(3) . 14 ?
O4 Mo1 O4 96.28(4) . 14 ?
O4 Mo1 O6 69.90(5) . . ?
O4 Mo1 O6 69.59(5) 14 . ?
O6 Mo1 Mo1 58.13(3) . 14 ?
C1 O2 Mo1 115.20(12) . . ?
C2 O3 Mo1 113.61(12) . . ?
Mo1 O4 Mo1 83.72(4) . 14 ?
C3 O4 Mo1 138.96(10) . . ?
C3 O4 Mo1 137.24(10) . 14 ?
C4 O5 H5 107(2) . . ?
O2 C1 H1A 110.2 . . ?
O2 C1 H1B 110.2 . . ?
O2 C1 C2 107.45(17) . . ?
H1A C1 H1B 108.5 . . ?
C2 C1 H1A 110.2 . . ?
C2 C1 H1B 110.2 . . ?
O3 C2 C1 106.52(16) . . ?
O3 C2 H2A 110.4 . . ?
O3 C2 H2B 110.4 . . ?
C1 C2 H2A 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
O4 C3 H3A 109.6 . . ?
O4 C3 H3B 109.6 . . ?
O4 C3 C4 110.14(17) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
O5 C4 C3 112.39(16) . . ?
O5 C4 H4A 109.1 . . ?
O5 C4 H4B 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
C5 O6 Mo1 118.47(10) . . ?
C5 O6 Mo1 120.87(11) 14 . ?
C5 O6 C5 108.7(2) . 14 ?
O6 C5 H5A 110.6 . . ?
O6 C5 H5B 110.6 . . ?
O6 C5 C6 105.58(16) . . ?
H5A C5 H5B 108.8 . . ?
C6 C5 H5A 110.6 . . ?
C6 C5 H5B 110.6 . . ?
C5 C6 C6 102.73(13) . 14 ?
C5 C6 H6A 111.2 . . ?
C5 C6 H6B 111.2 . . ?
C6 C6 H6A 111.2 14 . ?
C6 C6 H6B 111.2 14 . ?
H6A C6 H6B 109.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O5 H5 O2 0.89(3) 1.93(3) 2.814(2) 175(4) 12_554 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C1 C2 -26.0(2) . . . . ?
Mo1 O3 C2 C1 -40.2(2) . . . . ?
Mo1 O4 C3 C4 -82.0(2) 14 . . . ?
Mo1 O4 C3 C4 102.6(2) . . . . ?
Mo1 O6 C5 C6 -155.31(13) . . . . ?
O2 C1 C2 O3 41.0(2) . . . . ?
O4 C3 C4 O5 -71.08(19) . . . . ?
O6 C5 C6 C6 31.3(3) . . . 14 ?
C5 O6 C5 C6 -12.19(11) 14 . . . ?

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

data_mo_2020_09_16_jdm_tg187wash2_0_a
_database_code_depnum_ccdc_archive 'CCDC 2225736'
loop_
_audit_author_name
_audit_author_address
'George T.'
;Saint Marys University
Canada
;
_audit_update_record             
;
2023-10-01 deposited with the CCDC.	2023-10-06 downloaded from the CCDC.
;
_audit_creation_date             2023-09-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Tanner.George@smu.ca
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Mo6 O19, 2(C9 H20 N)'
_chemical_formula_sum            'C18 H40 Mo6 N2 O19'
_chemical_formula_weight         1164.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.4347(8)
_cell_length_b                   16.0288(12)
_cell_length_c                   10.9136(9)
_cell_angle_alpha                90
_cell_angle_beta                 101.838(3)
_cell_angle_gamma                90
_cell_volume                     1615.3(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9194
_cell_measurement_temperature    125.0
_cell_measurement_theta_max      33.18
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   0.853
_shelx_estimated_absorpt_T_min   0.665
_exptl_absorpt_coefficient_mu    2.339
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0832 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.7642. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            55716
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.259
_diffrn_reflns_theta_min         2.291
_diffrn_ambient_temperature      125.00
_diffrn_detector                 '100 \\times 140 mm^2^ CMOS sensor'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5542
_reflns_number_total             6194
_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       'SAINT V8.40B (Bruker AXS Inc., 2016)'
_computing_data_collection       'APEX4 (Bruker AXS Inc., 2021)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.772
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0332
_refine_ls_restrained_S_all      1.211
_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)+6.6219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0731
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1A-C1A \\sim N1B-C1B
 with sigma of 0.02
 N1A-C2A \\sim N1B-C2B
 with sigma of 0.02
 N1A-C5 \\sim N1B-C5
 with sigma of 0.02
 N1A-C9 \\sim N1B-C9
 with sigma of 0.02
 C2A-C3A \\sim C2B-C3B
 with sigma of 0.02
 C3A-C4A \\sim C3B-C4B
 with sigma of 0.02
 N1A-C3A \\sim N1B-C3B
 with sigma of 0.04
 C1A-C2A \\sim C1B-C2B
 with sigma of 0.04
 C1A-C5 \\sim C1B-C5
 with sigma of 0.04
 C1A-C9 \\sim C1B-C9
 with sigma of 0.04
 C2A-C4A \\sim C2B-C4B
 with sigma of 0.04
 C2A-C5 \\sim C2B-C5
 with sigma of 0.04
 C2A-C9 \\sim C2B-C9
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N1A, C1A, C2A, C3A, C4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1B, C1B, C2B, C3B, C4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H5BC)=Sof(H5BD)=Sof(H9BC)=Sof(H9BD)=Sof(C1B)=Sof(H1AA)=Sof(H1AB)=
 Sof(H1AC)=Sof(N1B)=Sof(C2B)=Sof(H2AA)=Sof(H2AB)=Sof(C3B)=Sof(H3AA)=Sof(H3AB)=
 Sof(C4B)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2A)=Sof(H2A)=Sof(H2B)=
 Sof(C3A)=Sof(H3A)=Sof(H3B)=Sof(C4A)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(H5AA)=
 Sof(H5AB)=Sof(H9AA)=Sof(H9AB)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C2A(H2A,H2B), C3A(H3A,H3B), C5(H5AA,H5AB), C5(H5BC,H5BD), C6(H6A,H6B), C7(H7A,
 H7B), C8(H8A,H8B), C9(H9AA,H9AB), C9(H9BC,H9BD), C2B(H2AA,H2AB), C3B(H3AA,H3AB)
5.b Idealised Me refined as rotating group:
 C1A(H1A,H1B,H1C), C4A(H4A,H4B,H4C), C1B(H1AA,H1AB,H1AC), C4B(H4AA,H4AB,H4AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.66220(3) 0.47445(2) 0.37248(2) 0.01945(5) Uani 1 1 d . . . . .
Mo2 Mo 0.47257(3) 0.63610(2) 0.42587(3) 0.01997(6) Uani 1 1 d . . . . .
Mo3 Mo 0.69015(3) 0.54212(2) 0.65850(2) 0.02008(5) Uani 1 1 d . . . . .
O1 O 0.500000 0.500000 0.500000 0.0175(5) Uani 1 2 d S . P . .
O2 O 0.6246(2) 0.58753(14) 0.3444(2) 0.0235(4) Uani 1 1 d . . . . .
O3 O 0.6366(2) 0.64229(13) 0.5709(2) 0.0233(4) Uani 1 1 d . . . . .
O4 O 0.7866(2) 0.50483(14) 0.5340(2) 0.0215(4) Uani 1 1 d . . . . .
O5 O 0.4850(2) 0.44379(15) 0.2702(2) 0.0232(4) Uani 1 1 d . . . . .
O6 O 0.3378(2) 0.57731(14) 0.3065(2) 0.0217(4) Uani 1 1 d . . . . .
O7 O 0.3499(2) 0.63453(14) 0.5398(2) 0.0226(4) Uani 1 1 d . . . . .
O8 O 0.8229(3) 0.57082(16) 0.7787(2) 0.0294(5) Uani 1 1 d . . . . .
O9 O 0.7852(3) 0.45087(16) 0.2853(2) 0.0272(5) Uani 1 1 d . . . . .
O10 O 0.4618(3) 0.73414(15) 0.3695(3) 0.0307(5) Uani 1 1 d . . . . .
N1 N 0.9841(4) 0.7356(3) 0.4059(5) 0.0218(9) Uani 0.834(8) 1 d D . P A 1
C1 C 0.9849(5) 0.6711(3) 0.5044(5) 0.0273(9) Uani 0.834(8) 1 d D . P A 1
H1A H 0.907070 0.630793 0.475621 0.041 Uiso 0.834(8) 1 calc R U P A 1
H1B H 0.969932 0.697923 0.581387 0.041 Uiso 0.834(8) 1 calc R U P A 1
H1C H 1.078366 0.642080 0.520879 0.041 Uiso 0.834(8) 1 calc R U P A 1
C2 C 1.0295(4) 0.6984(2) 0.2916(4) 0.0229(8) Uani 0.834(8) 1 d D . P A 1
H2A H 1.017003 0.741331 0.224975 0.028 Uiso 0.834(8) 1 calc R U P A 1
H2B H 1.133863 0.684443 0.314029 0.028 Uiso 0.834(8) 1 calc R U P A 1
C3 C 0.9464(4) 0.6210(3) 0.2396(4) 0.0272(9) Uani 0.834(8) 1 d D . P A 1
H3A H 0.841168 0.630897 0.230217 0.033 Uiso 0.834(8) 1 calc R U P A 1
H3B H 0.973896 0.573732 0.297979 0.033 Uiso 0.834(8) 1 calc R U P A 1
C4 C 0.9814(17) 0.6000(6) 0.1119(8) 0.0330(16) Uani 0.834(8) 1 d D . P A 1
H4A H 0.953370 0.646822 0.054346 0.049 Uiso 0.834(8) 1 calc R U P A 1
H4B H 0.927678 0.549951 0.077862 0.049 Uiso 0.834(8) 1 calc R U P A 1
H4C H 1.085552 0.589662 0.121908 0.049 Uiso 0.834(8) 1 calc R U P A 1
C5 C 0.8344(3) 0.7746(2) 0.3689(4) 0.0276(6) Uani 1 1 d D . . . .
H5AA H 0.761801 0.729580 0.347463 0.033 Uiso 0.834(8) 1 calc R U P A 1
H5AB H 0.830760 0.808948 0.292911 0.033 Uiso 0.834(8) 1 calc R U P A 1
H5BC H 0.759161 0.731930 0.340115 0.033 Uiso 0.166(8) 1 calc R U P A 2
H5BD H 0.846426 0.808944 0.296308 0.033 Uiso 0.166(8) 1 calc R U P A 2
C6 C 0.7932(4) 0.8290(2) 0.4704(4) 0.0304(7) Uani 1 1 d . . . . .
H6A H 0.785284 0.793945 0.543432 0.036 Uiso 1 1 calc R U . . .
H6B H 0.697724 0.855069 0.438334 0.036 Uiso 1 1 calc R U . . .
C7 C 0.9065(4) 0.8967(2) 0.5109(3) 0.0305(7) Uani 1 1 d . . . . .
H7A H 0.907373 0.935220 0.440188 0.037 Uiso 1 1 calc R U . . .
H7B H 0.881549 0.929280 0.580613 0.037 Uiso 1 1 calc R U . . .
C8 C 1.0553(4) 0.8579(2) 0.5529(4) 0.0350(8) Uani 1 1 d . . . . .
H8A H 1.128572 0.902716 0.573369 0.042 Uiso 1 1 calc R U . . .
H8B H 1.057230 0.824697 0.629683 0.042 Uiso 1 1 calc R U . . .
C9 C 1.0939(3) 0.8024(2) 0.4528(3) 0.0258(6) Uani 1 1 d D . . . .
H9AA H 1.106061 0.837568 0.381130 0.031 Uiso 0.834(8) 1 calc R U P A 1
H9AB H 1.188260 0.775408 0.486594 0.031 Uiso 0.834(8) 1 calc R U P A 1
H9BC H 1.091555 0.834311 0.374776 0.031 Uiso 0.166(8) 1 calc R U P A 2
H9BD H 1.192072 0.778610 0.480987 0.031 Uiso 0.166(8) 1 calc R U P A 2
C1A C 0.988(3) 0.6873(14) 0.553(2) 0.036(5) Uani 0.166(8) 1 d D . P A 2
H1AA H 0.967304 0.726122 0.616021 0.054 Uiso 0.166(8) 1 calc R U P A 2
H1AB H 1.085243 0.663979 0.580241 0.054 Uiso 0.166(8) 1 calc R U P A 2
H1AC H 0.916554 0.642077 0.540523 0.054 Uiso 0.166(8) 1 calc R U P A 2
N1A N 0.9798(17) 0.7330(10) 0.4311(18) 0.031(6) Uani 0.166(8) 1 d D . P A 2
C2A C 0.9963(18) 0.6636(10) 0.3382(15) 0.022(4) Uani 0.166(8) 1 d D . P A 2
H2AA H 1.091923 0.636779 0.366577 0.027 Uiso 0.166(8) 1 calc R U P A 2
H2AB H 0.921307 0.620755 0.340303 0.027 Uiso 0.166(8) 1 calc R U P A 2
C3A C 0.984(3) 0.6918(13) 0.2048(17) 0.037(5) Uani 0.166(8) 1 d D . P A 2
H3AA H 1.069881 0.725271 0.196872 0.044 Uiso 0.166(8) 1 calc R U P A 2
H3AB H 0.896484 0.726604 0.178325 0.044 Uiso 0.166(8) 1 calc R U P A 2
C4A C 0.974(8) 0.613(3) 0.122(4) 0.035(9) Uani 0.166(8) 1 d D . P A 2
H4AA H 0.931536 0.627472 0.035521 0.052 Uiso 0.166(8) 1 calc R U P A 2
H4AB H 0.913614 0.571215 0.152533 0.052 Uiso 0.166(8) 1 calc R U P A 2
H4AC H 1.071602 0.590104 0.127036 0.052 Uiso 0.166(8) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O1 2.3065(3) . ?
Mo1 O2 1.860(2) . ?
Mo1 O4 1.968(2) . ?
Mo1 O5 1.875(2) . ?
Mo1 O7 2.006(2) 3_666 ?
Mo1 O9 1.687(2) . ?
Mo2 O1 2.3226(3) . ?
Mo2 O2 1.994(2) . ?
Mo2 O3 1.976(2) . ?
Mo2 O6 1.877(2) . ?
Mo2 O7 1.865(2) . ?
Mo2 O10 1.683(2) . ?
Mo3 O1 2.3223(3) . ?
Mo3 O3 1.884(2) . ?
Mo3 O4 1.881(2) . ?
Mo3 O5 1.979(2) 3_666 ?
Mo3 O6 1.980(2) 3_666 ?
Mo3 O8 1.681(2) . ?
N1 C1 1.490(6) . ?
N1 C2 1.522(6) . ?
N1 C5 1.521(5) . ?
N1 C9 1.505(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.514(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.534(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5AA 0.9900 . ?
C5 H5AB 0.9900 . ?
C5 H5BC 0.9900 . ?
C5 H5BD 0.9900 . ?
C5 C6 1.521(5) . ?
C5 N1A 1.551(16) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.524(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.518(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.510(5) . ?
C9 H9AA 0.9900 . ?
C9 H9AB 0.9900 . ?
C9 H9BC 0.9900 . ?
C9 H9BD 0.9900 . ?
C9 N1A 1.533(16) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C1A N1A 1.502(17) . ?
N1A C2A 1.534(16) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2A C3A 1.505(17) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C3A C4A 1.54(2) . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 O1 78.37(7) . . ?
O2 Mo1 O4 87.99(10) . . ?
O2 Mo1 O5 92.33(10) . . ?
O2 Mo1 O7 154.05(9) . 3_666 ?
O4 Mo1 O1 76.30(6) . . ?
O4 Mo1 O7 82.52(9) . 3_666 ?
O5 Mo1 O1 77.58(7) . . ?
O5 Mo1 O4 153.26(9) . . ?
O5 Mo1 O7 85.70(10) . 3_666 ?
O7 Mo1 O1 75.94(6) 3_666 . ?
O9 Mo1 O1 176.41(9) . . ?
O9 Mo1 O2 104.81(11) . . ?
O9 Mo1 O4 101.97(11) . . ?
O9 Mo1 O5 103.77(11) . . ?
O9 Mo1 O7 100.78(11) . 3_666 ?
O2 Mo2 O1 75.50(6) . . ?
O3 Mo2 O1 75.83(6) . . ?
O3 Mo2 O2 81.94(10) . . ?
O6 Mo2 O1 77.38(7) . . ?
O6 Mo2 O2 86.62(10) . . ?
O6 Mo2 O3 152.74(9) . . ?
O7 Mo2 O1 78.18(7) . . ?
O7 Mo2 O2 153.33(9) . . ?
O7 Mo2 O3 87.60(10) . . ?
O7 Mo2 O6 91.80(10) . . ?
O10 Mo2 O1 176.71(9) . . ?
O10 Mo2 O2 101.35(11) . . ?
O10 Mo2 O3 102.97(11) . . ?
O10 Mo2 O6 103.51(11) . . ?
O10 Mo2 O7 104.90(12) . . ?
O3 Mo3 O1 77.53(7) . . ?
O3 Mo3 O5 86.78(10) . 3_666 ?
O3 Mo3 O6 152.79(9) . 3_666 ?
O4 Mo3 O1 77.52(7) . . ?
O4 Mo3 O3 91.33(10) . . ?
O4 Mo3 O5 152.52(9) . 3_666 ?
O4 Mo3 O6 86.31(10) . 3_666 ?
O5 Mo3 O1 75.31(6) 3_666 . ?
O5 Mo3 O6 83.07(10) 3_666 3_666 ?
O6 Mo3 O1 75.50(6) 3_666 . ?
O8 Mo3 O1 177.03(9) . . ?
O8 Mo3 O3 104.00(11) . . ?
O8 Mo3 O4 104.90(11) . . ?
O8 Mo3 O5 102.15(11) . 3_666 ?
O8 Mo3 O6 102.79(11) . 3_666 ?
Mo1 O1 Mo1 180.0 . 3_666 ?
Mo1 O1 Mo2 89.824(10) . . ?
Mo1 O1 Mo2 90.176(10) 3_666 . ?
Mo1 O1 Mo2 90.176(10) . 3_666 ?
Mo1 O1 Mo2 89.825(10) 3_666 3_666 ?
Mo1 O1 Mo3 90.329(11) 3_666 . ?
Mo1 O1 Mo3 89.672(11) . . ?
Mo1 O1 Mo3 90.328(12) . 3_666 ?
Mo1 O1 Mo3 89.671(11) 3_666 3_666 ?
Mo2 O1 Mo2 179.999(13) . 3_666 ?
Mo3 O1 Mo2 90.012(10) 3_666 3_666 ?
Mo3 O1 Mo2 89.987(10) 3_666 . ?
Mo3 O1 Mo2 90.014(10) . . ?
Mo3 O1 Mo2 89.987(10) . 3_666 ?
Mo3 O1 Mo3 180.0 3_666 . ?
Mo1 O2 Mo2 115.95(11) . . ?
Mo3 O3 Mo2 116.62(11) . . ?
Mo3 O4 Mo1 115.95(11) . . ?
Mo1 O5 Mo3 116.76(11) . 3_666 ?
Mo2 O6 Mo3 116.71(11) . 3_666 ?
Mo2 O7 Mo1 115.71(11) . 3_666 ?
C1 N1 C2 111.0(4) . . ?
C1 N1 C5 110.2(4) . . ?
C1 N1 C9 110.3(4) . . ?
C5 N1 C2 110.2(3) . . ?
C9 N1 C2 105.5(3) . . ?
C9 N1 C5 109.5(3) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 108.6 . . ?
N1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C3 C2 N1 114.6(3) . . ?
C3 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
C2 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C2 C3 C4 109.2(6) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5AA 108.8 . . ?
N1 C5 H5AB 108.8 . . ?
N1 C5 C6 113.8(3) . . ?
H5AA C5 H5AB 107.7 . . ?
H5BC C5 H5BD 108.8 . . ?
C6 C5 H5AA 108.8 . . ?
C6 C5 H5AB 108.8 . . ?
C6 C5 H5BC 110.7 . . ?
C6 C5 H5BD 110.7 . . ?
N1A C5 H5BC 110.7 . . ?
N1A C5 H5BD 110.7 . . ?
N1A C5 C6 105.3(7) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 C7 110.5(3) . . ?
H6A C6 H6B 108.1 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C6 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 C6 110.2(3) . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
C7 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 C7 111.6(3) . . ?
C9 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
N1 C9 C8 114.4(3) . . ?
N1 C9 H9AA 108.7 . . ?
N1 C9 H9AB 108.7 . . ?
C8 C9 H9AA 108.7 . . ?
C8 C9 H9AB 108.7 . . ?
C8 C9 H9BC 110.6 . . ?
C8 C9 H9BD 110.6 . . ?
H9AA C9 H9AB 107.6 . . ?
H9BC C9 H9BD 108.7 . . ?
N1A C9 C8 105.9(8) . . ?
N1A C9 H9BC 110.6 . . ?
N1A C9 H9BD 110.6 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
N1A C1A H1AA 109.5 . . ?
N1A C1A H1AB 109.5 . . ?
N1A C1A H1AC 109.5 . . ?
C5 N1A C2A 102.9(11) . . ?
C9 N1A C5 106.6(10) . . ?
C9 N1A C2A 117.7(13) . . ?
C1A N1A C5 118.4(16) . . ?
C1A N1A C9 108.1(14) . . ?
C1A N1A C2A 103.7(14) . . ?
N1A C2A H2AA 108.5 . . ?
N1A C2A H2AB 108.5 . . ?
H2AA C2A H2AB 107.5 . . ?
C3A C2A N1A 115.1(14) . . ?
C3A C2A H2AA 108.5 . . ?
C3A C2A H2AB 108.5 . . ?
C2A C3A H3AA 110.2 . . ?
C2A C3A H3AB 110.2 . . ?
C2A C3A C4A 108(2) . . ?
H3AA C3A H3AB 108.5 . . ?
C4A C3A H3AA 110.2 . . ?
C4A C3A H3AB 110.2 . . ?
C3A C4A H4AA 109.5 . . ?
C3A C4A H4AB 109.5 . . ?
C3A C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?

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
O1 Mo1 O2 Mo2 -5.31(10) . . . . ?
O1 Mo1 O5 Mo3 1.26(10) . . . 3_666 ?
O1 Mo2 O6 Mo3 5.84(9) . . . 3_666 ?
O1 Mo2 O7 Mo1 -0.58(9) . . . 3_666 ?
O1 Mo3 O3 Mo2 0.86(10) . . . . ?
O1 Mo3 O4 Mo1 6.57(9) . . . . ?
O2 Mo1 O5 Mo3 -76.29(14) . . . 3_666 ?
O2 Mo2 O6 Mo3 81.72(13) . . . 3_666 ?
O2 Mo2 O7 Mo1 -9.9(3) . . . 3_666 ?
O3 Mo2 O6 Mo3 16.6(3) . . . 3_666 ?
O3 Mo2 O7 Mo1 -76.61(12) . . . 3_666 ?
O3 Mo3 O4 Mo1 -70.34(13) . . . . ?
O4 Mo1 O2 Mo2 -81.74(13) . . . . ?
O4 Mo1 O5 Mo3 13.9(3) . . . 3_666 ?
O4 Mo3 O3 Mo2 77.77(13) . . . . ?
O5 Mo1 O2 Mo2 71.51(13) . . . . ?
O5 Mo3 O3 Mo2 -74.80(13) 3_666 . . . ?
O5 Mo3 O4 Mo1 15.2(3) 3_666 . . . ?
O6 Mo2 O7 Mo1 76.12(13) . . . 3_666 ?
O6 Mo3 O3 Mo2 -6.8(3) 3_666 . . . ?
O6 Mo3 O4 Mo1 82.52(12) 3_666 . . . ?
O7 Mo1 O2 Mo2 -13.5(3) 3_666 . . . ?
O7 Mo1 O5 Mo3 77.79(13) 3_666 . . 3_666 ?
O7 Mo2 O6 Mo3 -71.62(13) . . . 3_666 ?
O8 Mo3 O3 Mo2 -176.52(13) . . . . ?
O8 Mo3 O4 Mo1 -175.21(13) . . . . ?
O9 Mo1 O2 Mo2 176.41(13) . . . . ?
O9 Mo1 O5 Mo3 177.85(13) . . . 3_666 ?
O10 Mo2 O6 Mo3 -177.41(13) . . . 3_666 ?
O10 Mo2 O7 Mo1 -179.39(13) . . . 3_666 ?
N1 C2 C3 C4 169.2(6) . . . . ?
N1 C5 C6 C7 55.7(4) . . . . ?
C1 N1 C2 C3 52.0(5) . . . . ?
C1 N1 C5 C6 69.3(4) . . . . ?
C1 N1 C9 C8 -70.2(4) . . . . ?
C2 N1 C5 C6 -167.8(3) . . . . ?
C2 N1 C9 C8 169.8(3) . . . . ?
C5 N1 C2 C3 -70.3(4) . . . . ?
C5 N1 C9 C8 51.2(5) . . . . ?
C5 C6 C7 C8 -55.7(4) . . . . ?
C5 N1A C2A C3A 52.9(19) . . . . ?
C6 C5 N1A C9 -69.3(11) . . . . ?
C6 C5 N1A C1A 52.6(15) . . . . ?
C6 C5 N1A C2A 166.2(9) . . . . ?
C6 C7 C8 C9 55.1(4) . . . . ?
C7 C8 C9 N1 -54.3(4) . . . . ?
C7 C8 C9 N1A -61.5(8) . . . . ?
C8 C9 N1A C5 68.5(11) . . . . ?
C8 C9 N1A C1A -59.8(14) . . . . ?
C8 C9 N1A C2A -176.7(11) . . . . ?
C9 N1 C2 C3 171.5(3) . . . . ?
C9 N1 C5 C6 -52.1(5) . . . . ?
C9 N1A C2A C3A -64(2) . . . . ?
C1A N1A C2A C3A 176.9(19) . . . . ?
N1A C5 C6 C7 62.5(8) . . . . ?
N1A C2A C3A C4A -169(3) . . . . ?

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

data_mo_2021_03_03_jdm_tg216a_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2225737'
loop_
_audit_author_name
_audit_author_address
'George T.'
;Saint Marys University
Canada
;
_audit_update_record             
;
2023-10-01 deposited with the CCDC.	2023-10-06 downloaded from the CCDC.
;
_audit_creation_date             2023-09-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Tanner.George@smu.ca
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H54 Mo8 O32, 2(C2 H6 O2)'
_chemical_formula_sum            'C28 H66 Mo8 O36'
_chemical_formula_weight         1746.32
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5318(4)
_cell_length_b                   11.0284(5)
_cell_length_c                   14.5245(7)
_cell_angle_alpha                81.706(2)
_cell_angle_beta                 77.862(2)
_cell_angle_gamma                69.992(2)
_cell_volume                     1251.55(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9042
_cell_measurement_temperature    125.0
_cell_measurement_theta_max      33.82
_cell_measurement_theta_min      2.53
_shelx_estimated_absorpt_T_max   0.923
_shelx_estimated_absorpt_T_min   0.792
_exptl_absorpt_coefficient_mu    2.040
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1101 before and 0.0533 after correction.
The Ratio of minimum to maximum transmission is 0.9192.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.317
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Blade
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            126602
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.901
_diffrn_reflns_theta_min         2.347
_diffrn_ambient_temperature      125.00
_diffrn_detector                 '100 \\times 140 mm^2^ CMOS sensor'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'κ--geometry diffractometer'
# end Validation Reply Form
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9085
_reflns_number_total             10104
_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       'SAINT V8.40B (Bruker AXS Inc., 2016)'
_computing_data_collection       'APEX4 (Bruker AXS Inc., 2021)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.303
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         10104
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0219
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0198P)²+1.9118P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0554
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O18-H18
 0.84 with sigma of 0.02
 O14-C10A \\sim O14-C10B
 with sigma of 0.02
 C9-C10A \\sim C9-C10B
 with sigma of 0.02
3. Others
 Sof(H9BC)=Sof(H9BD)=Sof(C10B)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9AA,H9AB), C9(H9BC,H9BD), C11(H11A,H11B),
 C12(H12A,H12B), C10A(H10A,H10B), C10B(H10C,H10D), C13(H13A,H13B), C14(H14A,
 H14B)
;
_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 0.64979(2) 0.09591(2) 0.72451(2) 0.01592(3) Uani 1 1 d . . . . .
Mo2 Mo 0.73598(2) 0.29312(2) 0.74767(2) 0.01495(3) Uani 1 1 d . . . . .
Mo3 Mo 0.48794(2) 0.39712(2) 0.55096(2) 0.01163(3) Uani 1 1 d . . . . .
Mo4 Mo 0.46284(2) 0.60001(2) 0.63030(2) 0.01253(3) Uani 1 1 d . . . . .
O1 O 0.8015(2) 0.01461(14) 0.63996(11) 0.0255(3) Uani 1 1 d . . . . .
O2 O 0.92106(18) 0.27863(16) 0.67404(11) 0.0251(3) Uani 1 1 d . . . . .
O3 O 0.42880(19) 0.10330(13) 0.69879(10) 0.0205(3) Uani 1 1 d . . . . .
O4 O 0.5999(2) -0.04015(14) 0.81960(11) 0.0227(3) Uani 1 1 d . . . . .
O5 O 0.58675(17) 0.48349(12) 0.74074(9) 0.0161(2) Uani 1 1 d . . . . .
O6 O 0.76293(19) 0.34509(14) 0.86483(10) 0.0215(3) Uani 1 1 d . . . . .
O7 O 0.82249(18) 0.10189(14) 0.80626(10) 0.0202(3) Uani 1 1 d . . . . .
O8 O 0.52908(17) 0.22899(13) 0.84208(9) 0.0163(2) Uani 1 1 d . . . . .
O9 O 0.59223(16) 0.27542(12) 0.66277(9) 0.0149(2) Uani 1 1 d . . . . .
O10 O 0.66118(16) 0.48808(12) 0.54198(9) 0.0137(2) Uani 1 1 d . . . . .
O11 O 0.30709(16) 0.49259(12) 0.65453(9) 0.0146(2) Uani 1 1 d . . . . .
O12 O 0.22269(19) 0.41113(15) 0.85436(10) 0.0218(3) Uani 1 1 d . . . . .
H12 H 0.310(4) 0.364(3) 0.848(2) 0.038(9) Uiso 1 1 d . . . . .
O13 O 0.26656(17) 0.73946(13) 0.71937(10) 0.0178(2) Uani 1 1 d . . . . .
H13 H 0.226(4) 0.714(3) 0.782(2) 0.037(8) Uiso 1 1 d . . . . .
O14 O 0.32527(18) 0.72331(12) 0.54118(9) 0.0177(2) Uani 1 1 d D . . . .
O15 O 0.59460(17) 0.70779(13) 0.63249(9) 0.0166(2) Uani 1 1 d . . . . .
O16 O 0.66165(18) 0.73161(14) 0.43237(10) 0.0184(2) Uani 1 1 d . . . . .
H16 H 0.641(4) 0.781(3) 0.390(2) 0.040(9) Uiso 1 1 d . . . . .
C1 C 0.3744(3) -0.0050(2) 0.73804(16) 0.0272(4) Uani 1 1 d . . . . .
H1A H 0.425041 -0.076478 0.695773 0.033 Uiso 1 1 calc R U . . .
H1B H 0.249576 0.019727 0.746583 0.033 Uiso 1 1 calc R U . . .
C2 C 0.4323(3) -0.0460(2) 0.83120(16) 0.0285(4) Uani 1 1 d . . . . .
H2A H 0.355663 0.012248 0.879382 0.034 Uiso 1 1 calc R U . . .
H2B H 0.431634 -0.135358 0.852260 0.034 Uiso 1 1 calc R U . . .
C3 C 0.6135(3) 0.55541(19) 0.80877(14) 0.0212(3) Uani 1 1 d . . . . .
H3A H 0.512435 0.631831 0.824215 0.025 Uiso 1 1 calc R U . . .
H3B H 0.712282 0.585290 0.783180 0.025 Uiso 1 1 calc R U . . .
C4 C 0.6445(3) 0.4645(2) 0.89433(15) 0.0242(4) Uani 1 1 d . . . . .
H4A H 0.689850 0.500369 0.937605 0.029 Uiso 1 1 calc R U . . .
H4B H 0.537248 0.451515 0.928243 0.029 Uiso 1 1 calc R U . . .
C5 C 0.7692(3) 0.0860(2) 0.90652(14) 0.0231(4) Uani 1 1 d . . . . .
H5A H 0.836922 0.116082 0.940163 0.028 Uiso 1 1 calc R U . . .
H5B H 0.784616 -0.006358 0.926939 0.028 Uiso 1 1 calc R U . . .
C6 C 0.5792(3) 0.16779(19) 0.92899(13) 0.0208(3) Uani 1 1 d . . . . .
H6A H 0.510567 0.111454 0.958727 0.025 Uiso 1 1 calc R U . . .
H6B H 0.562868 0.233473 0.973013 0.025 Uiso 1 1 calc R U . . .
C7 C 0.1413(2) 0.49216(18) 0.69981(13) 0.0166(3) Uani 1 1 d . . . . .
H7A H 0.082572 0.476078 0.653171 0.020 Uiso 1 1 calc R U . . .
H7B H 0.075394 0.578257 0.723144 0.020 Uiso 1 1 calc R U . . .
C8 C 0.1475(2) 0.38998(19) 0.78149(14) 0.0198(3) Uani 1 1 d . . . . .
H8A H 0.030916 0.389610 0.808282 0.024 Uiso 1 1 calc R U . . .
H8B H 0.213222 0.303941 0.757989 0.024 Uiso 1 1 calc R U . . .
C9 C 0.1375(2) 0.82964(18) 0.66912(14) 0.0206(3) Uani 1 1 d D . . . .
H9AA H 0.088956 0.913139 0.698531 0.025 Uiso 0.719(7) 1 calc R U P A 1
H9AB H 0.045009 0.793977 0.670691 0.025 Uiso 0.719(7) 1 calc R U P A 1
H9BC H 0.146631 0.917542 0.664133 0.025 Uiso 0.281(7) 1 calc R U P A 2
H9BD H 0.023719 0.832769 0.704507 0.025 Uiso 0.281(7) 1 calc R U P A 2
C11 C 0.7576(2) 0.70183(19) 0.58164(13) 0.0194(3) Uani 1 1 d . . . . .
H11A H 0.825103 0.611078 0.569198 0.023 Uiso 1 1 calc R U . . .
H11B H 0.817194 0.734243 0.619126 0.023 Uiso 1 1 calc R U . . .
C12 C 0.7388(3) 0.7835(2) 0.48993(13) 0.0199(3) Uani 1 1 d . . . . .
H12A H 0.667652 0.873382 0.502663 0.024 Uiso 1 1 calc R U . . .
H12B H 0.851488 0.785066 0.455672 0.024 Uiso 1 1 calc R U . . .
C10A C 0.2217(3) 0.8483(2) 0.57053(18) 0.0173(6) Uani 0.719(7) 1 d D . P A 1
H10A H 0.136189 0.889730 0.529128 0.021 Uiso 0.719(7) 1 calc R U P A 1
H10B H 0.292111 0.904543 0.567081 0.021 Uiso 0.719(7) 1 calc R U P A 1
C10B C 0.1607(8) 0.7855(7) 0.5673(5) 0.0217(16) Uani 0.281(7) 1 d D . P A 2
H10C H 0.093711 0.727518 0.568302 0.026 Uiso 0.281(7) 1 calc R U P A 2
H10D H 0.122089 0.861699 0.522500 0.026 Uiso 0.281(7) 1 calc R U P A 2
O17 O 0.18813(19) 0.65012(16) 0.88843(11) 0.0230(3) Uani 1 1 d . . . . .
H17 H 0.189(4) 0.581(3) 0.883(2) 0.038(9) Uiso 1 1 d . . . . .
O18 O -0.1349(2) 0.73702(17) 0.82824(12) 0.0279(3) Uani 1 1 d D . . . .
H18 H -0.202(3) 0.8051(19) 0.830(2) 0.023(7) Uiso 1 1 d D . . . .
C13 C 0.0337(3) 0.7128(2) 0.94862(15) 0.0252(4) Uani 1 1 d . . . . .
H13A H 0.017137 0.806670 0.944379 0.030 Uiso 1 1 calc R U . . .
H13B H 0.042502 0.678412 1.014827 0.030 Uiso 1 1 calc R U . . .
C14 C -0.1170(3) 0.6937(2) 0.92326(15) 0.0255(4) Uani 1 1 d . . . . .
H14A H -0.105756 0.600652 0.933544 0.031 Uiso 1 1 calc R U . . .
H14B H -0.220380 0.741446 0.965535 0.031 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 Mo2 2.6064(2) . ?
Mo1 O1 1.6861(15) . ?
Mo1 O3 1.9707(14) . ?
Mo1 O4 1.9830(14) . ?
Mo1 O7 2.0999(14) . ?
Mo1 O8 2.2538(13) . ?
Mo1 O9 1.9930(12) . ?
Mo2 O2 1.6820(15) . ?
Mo2 O5 2.0500(13) . ?
Mo2 O6 1.9528(14) . ?
Mo2 O7 2.0972(14) . ?
Mo2 O8 2.2479(13) . ?
Mo2 O9 1.9830(13) . ?
Mo3 Mo3 2.5700(3) 2_666 ?
Mo3 Mo4 2.5870(2) . ?
Mo3 Mo4 2.5746(2) 2_666 ?
Mo3 O9 2.0958(12) . ?
Mo3 O10 2.0258(12) . ?
Mo3 O10 2.0421(12) 2_666 ?
Mo3 O11 2.0301(13) . ?
Mo3 O14 2.0645(13) 2_666 ?
Mo3 O16 2.1712(13) 2_666 ?
Mo4 O5 2.1286(13) . ?
Mo4 O10 2.0365(13) . ?
Mo4 O11 2.0133(12) . ?
Mo4 O13 2.1780(14) . ?
Mo4 O14 1.9852(13) . ?
Mo4 O15 1.9020(13) . ?
O3 C1 1.427(2) . ?
O4 C2 1.427(3) . ?
O5 C3 1.450(2) . ?
O6 C4 1.417(3) . ?
O7 C5 1.436(2) . ?
O8 C6 1.420(2) . ?
O11 C7 1.430(2) . ?
O12 H12 0.74(3) . ?
O12 C8 1.430(2) . ?
O13 H13 0.94(3) . ?
O13 C9 1.454(2) . ?
O14 C10A 1.429(3) . ?
O14 C10B 1.334(7) . ?
O15 C11 1.415(2) . ?
O16 H16 0.77(3) . ?
O16 C12 1.444(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.494(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.489(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.552(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.510(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9AA 0.9900 . ?
C9 H9AB 0.9900 . ?
C9 H9BC 0.9900 . ?
C9 H9BD 0.9900 . ?
C9 C10A 1.481(3) . ?
C9 C10B 1.575(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.502(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
O17 H17 0.77(3) . ?
O17 C13 1.430(3) . ?
O18 H18 0.773(17) . ?
O18 C14 1.416(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.496(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 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
O1 Mo1 Mo2 105.85(6) . . ?
O1 Mo1 O3 107.91(7) . . ?
O1 Mo1 O4 104.95(7) . . ?
O1 Mo1 O7 94.13(7) . . ?
O1 Mo1 O8 158.28(7) . . ?
O1 Mo1 O9 100.88(6) . . ?
O3 Mo1 Mo2 126.04(4) . . ?
O3 Mo1 O4 79.64(6) . . ?
O3 Mo1 O7 156.46(6) . . ?
O3 Mo1 O8 92.67(6) . . ?
O3 Mo1 O9 84.03(5) . . ?
O4 Mo1 Mo2 129.13(4) . . ?
O4 Mo1 O7 86.89(6) . . ?
O4 Mo1 O8 85.12(6) . . ?
O4 Mo1 O9 152.65(6) . . ?
O7 Mo1 Mo2 51.56(4) . . ?
O7 Mo1 O8 66.82(5) . . ?
O8 Mo1 Mo2 54.52(3) . . ?
O9 Mo1 Mo2 48.87(4) . . ?
O9 Mo1 O7 100.20(5) . . ?
O9 Mo1 O8 73.82(5) . . ?
O2 Mo2 Mo1 105.77(6) . . ?
O2 Mo2 O5 108.66(7) . . ?
O2 Mo2 O6 105.28(7) . . ?
O2 Mo2 O7 92.68(7) . . ?
O2 Mo2 O8 157.64(7) . . ?
O2 Mo2 O9 102.12(7) . . ?
O5 Mo2 Mo1 126.01(4) . . ?
O5 Mo2 O7 157.07(6) . . ?
O5 Mo2 O8 92.98(5) . . ?
O6 Mo2 Mo1 128.15(4) . . ?
O6 Mo2 O5 79.91(6) . . ?
O6 Mo2 O7 86.56(6) . . ?
O6 Mo2 O8 83.53(6) . . ?
O6 Mo2 O9 151.30(6) . . ?
O7 Mo2 Mo1 51.66(4) . . ?
O7 Mo2 O8 66.98(5) . . ?
O8 Mo2 Mo1 54.73(3) . . ?
O9 Mo2 Mo1 49.21(4) . . ?
O9 Mo2 O5 83.43(5) . . ?
O9 Mo2 O7 100.62(5) . . ?
O9 Mo2 O8 74.14(5) . . ?
Mo3 Mo3 Mo4 60.380(7) 2_666 2_666 ?
Mo3 Mo3 Mo4 59.896(7) 2_666 . ?
Mo4 Mo3 Mo4 120.276(7) 2_666 . ?
O9 Mo3 Mo3 138.90(4) . 2_666 ?
O9 Mo3 Mo4 91.05(4) . . ?
O9 Mo3 Mo4 137.21(4) . 2_666 ?
O9 Mo3 O16 83.10(5) . 2_666 ?
O10 Mo3 Mo3 51.10(3) . 2_666 ?
O10 Mo3 Mo3 50.54(3) 2_666 2_666 ?
O10 Mo3 Mo4 90.61(4) . 2_666 ?
O10 Mo3 Mo4 50.63(4) . . ?
O10 Mo3 Mo4 89.89(4) 2_666 . ?
O10 Mo3 Mo4 50.76(4) 2_666 2_666 ?
O10 Mo3 O9 88.33(5) . . ?
O10 Mo3 O9 167.77(5) 2_666 . ?
O10 Mo3 O10 101.64(4) . 2_666 ?
O10 Mo3 O11 99.94(5) . . ?
O10 Mo3 O14 99.75(5) 2_666 2_666 ?
O10 Mo3 O14 83.90(5) . 2_666 ?
O10 Mo3 O16 87.63(5) 2_666 2_666 ?
O10 Mo3 O16 169.61(5) . 2_666 ?
O11 Mo3 Mo3 95.13(4) . 2_666 ?
O11 Mo3 Mo4 137.39(4) . 2_666 ?
O11 Mo3 Mo4 49.94(4) . . ?
O11 Mo3 O9 84.66(5) . . ?
O11 Mo3 O10 86.63(5) . 2_666 ?
O11 Mo3 O14 171.80(5) . 2_666 ?
O11 Mo3 O16 85.12(5) . 2_666 ?
O14 Mo3 Mo3 92.91(4) 2_666 2_666 ?
O14 Mo3 Mo4 49.18(4) 2_666 2_666 ?
O14 Mo3 Mo4 134.51(4) 2_666 . ?
O14 Mo3 O9 88.24(5) 2_666 . ?
O14 Mo3 O16 89.98(6) 2_666 2_666 ?
O16 Mo3 Mo3 137.95(4) 2_666 2_666 ?
O16 Mo3 Mo4 91.72(4) 2_666 2_666 ?
O16 Mo3 Mo4 135.06(4) 2_666 . ?
Mo3 Mo4 Mo3 59.724(6) 2_666 . ?
O5 Mo4 Mo3 135.99(4) . 2_666 ?
O5 Mo4 Mo3 91.44(4) . . ?
O5 Mo4 O13 96.69(5) . . ?
O10 Mo4 Mo3 50.96(3) . 2_666 ?
O10 Mo4 Mo3 50.26(3) . . ?
O10 Mo4 O5 85.17(5) . . ?
O10 Mo4 O13 172.44(5) . . ?
O11 Mo4 Mo3 95.41(4) . 2_666 ?
O11 Mo4 Mo3 50.51(4) . . ?
O11 Mo4 O5 88.28(5) . . ?
O11 Mo4 O10 100.15(5) . . ?
O11 Mo4 O13 87.26(5) . . ?
O13 Mo4 Mo3 127.25(4) . 2_666 ?
O13 Mo4 Mo3 136.76(4) . . ?
O14 Mo4 Mo3 51.90(4) . 2_666 ?
O14 Mo4 Mo3 94.31(4) . . ?
O14 Mo4 O5 172.11(5) . . ?
O14 Mo4 O10 102.67(5) . . ?
O14 Mo4 O11 91.21(6) . . ?
O14 Mo4 O13 75.42(5) . . ?
O15 Mo4 Mo3 95.41(4) . 2_666 ?
O15 Mo4 Mo3 138.90(4) . . ?
O15 Mo4 O5 85.71(5) . . ?
O15 Mo4 O10 88.67(5) . . ?
O15 Mo4 O11 168.88(5) . . ?
O15 Mo4 O13 84.17(6) . . ?
O15 Mo4 O14 93.46(6) . . ?
C1 O3 Mo1 115.32(12) . . ?
C2 O4 Mo1 115.14(12) . . ?
Mo2 O5 Mo4 130.49(6) . . ?
C3 O5 Mo2 111.97(11) . . ?
C3 O5 Mo4 114.72(11) . . ?
C4 O6 Mo2 115.11(11) . . ?
Mo2 O7 Mo1 76.78(4) . . ?
C5 O7 Mo1 114.91(12) . . ?
C5 O7 Mo2 114.26(12) . . ?
Mo2 O8 Mo1 70.76(4) . . ?
C6 O8 Mo1 111.23(11) . . ?
C6 O8 Mo2 111.14(11) . . ?
Mo1 O9 Mo3 144.97(7) . . ?
Mo2 O9 Mo1 81.92(5) . . ?
Mo2 O9 Mo3 132.07(6) . . ?
Mo3 O10 Mo3 78.36(4) . 2_666 ?
Mo3 O10 Mo4 79.11(5) . . ?
Mo4 O10 Mo3 78.28(4) . 2_666 ?
Mo4 O11 Mo3 79.55(5) . . ?
C7 O11 Mo3 136.26(11) . . ?
C7 O11 Mo4 142.71(11) . . ?
C8 O12 H12 105(3) . . ?
Mo4 O13 H13 120.2(19) . . ?
C9 O13 Mo4 113.47(11) . . ?
C9 O13 H13 114(2) . . ?
Mo4 O14 Mo3 78.92(5) . 2_666 ?
C10A O14 Mo3 152.36(14) . 2_666 ?
C10A O14 Mo4 118.58(13) . . ?
C10B O14 Mo4 121.8(3) . . ?
C11 O15 Mo4 129.43(12) . . ?
Mo3 O16 H16 109(3) 2_666 . ?
C12 O16 Mo3 138.84(11) . 2_666 ?
C12 O16 H16 108(3) . . ?
O3 C1 H1A 110.4 . . ?
O3 C1 H1B 110.4 . . ?
O3 C1 C2 106.63(17) . . ?
H1A C1 H1B 108.6 . . ?
C2 C1 H1A 110.4 . . ?
C2 C1 H1B 110.4 . . ?
O4 C2 C1 107.78(18) . . ?
O4 C2 H2A 110.1 . . ?
O4 C2 H2B 110.1 . . ?
C1 C2 H2A 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.5 . . ?
O5 C3 H3A 110.5 . . ?
O5 C3 H3B 110.5 . . ?
O5 C3 C4 106.15(16) . . ?
H3A C3 H3B 108.7 . . ?
C4 C3 H3A 110.5 . . ?
C4 C3 H3B 110.5 . . ?
O6 C4 C3 108.09(17) . . ?
O6 C4 H4A 110.1 . . ?
O6 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
O7 C5 H5A 110.2 . . ?
O7 C5 H5B 110.2 . . ?
O7 C5 C6 107.37(14) . . ?
H5A C5 H5B 108.5 . . ?
C6 C5 H5A 110.2 . . ?
C6 C5 H5B 110.2 . . ?
O8 C6 C5 107.20(15) . . ?
O8 C6 H6A 110.3 . . ?
O8 C6 H6B 110.3 . . ?
C5 C6 H6A 110.3 . . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.5 . . ?
O11 C7 H7A 109.2 . . ?
O11 C7 H7B 109.2 . . ?
O11 C7 C8 111.84(14) . . ?
H7A C7 H7B 107.9 . . ?
C8 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
O12 C8 C7 112.39(16) . . ?
O12 C8 H8A 109.1 . . ?
O12 C8 H8B 109.1 . . ?
C7 C8 H8A 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
O13 C9 H9AA 110.4 . . ?
O13 C9 H9AB 110.4 . . ?
O13 C9 H9BC 109.7 . . ?
O13 C9 H9BD 109.7 . . ?
O13 C9 C10A 106.73(16) . . ?
O13 C9 C10B 109.9(3) . . ?
H9AA C9 H9AB 108.6 . . ?
H9BC C9 H9BD 108.2 . . ?
C10A C9 H9AA 110.4 . . ?
C10A C9 H9AB 110.4 . . ?
C10B C9 H9BC 109.7 . . ?
C10B C9 H9BD 109.7 . . ?
O15 C11 H11A 109.9 . . ?
O15 C11 H11B 109.9 . . ?
O15 C11 C12 108.83(15) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
O16 C12 C11 110.13(15) . . ?
O16 C12 H12A 109.6 . . ?
O16 C12 H12B 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
O14 C10A C9 107.21(18) . . ?
O14 C10A H10A 110.3 . . ?
O14 C10A H10B 110.3 . . ?
C9 C10A H10A 110.3 . . ?
C9 C10A H10B 110.3 . . ?
H10A C10A H10B 108.5 . . ?
O14 C10B C9 107.0(4) . . ?
O14 C10B H10C 110.3 . . ?
O14 C10B H10D 110.3 . . ?
C9 C10B H10C 110.3 . . ?
C9 C10B H10D 110.3 . . ?
H10C C10B H10D 108.6 . . ?
C13 O17 H17 108(3) . . ?
C14 O18 H18 105(2) . . ?
O17 C13 H13A 109.1 . . ?
O17 C13 H13B 109.1 . . ?
O17 C13 C14 112.52(18) . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
O18 C14 C13 112.38(18) . . ?
O18 C14 H14A 109.1 . . ?
O18 C14 H14B 109.1 . . ?
C13 C14 H14A 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O12 H12 O8 0.74(3) 1.95(3) 2.686(2) 174(4) . yes
O13 H13 O17 0.94(3) 1.62(3) 2.552(2) 170(3) . yes
O16 H16 O3 0.77(3) 1.73(3) 2.4891(19) 174(4) 2_666 yes
O17 H17 O12 0.77(3) 1.89(3) 2.657(2) 171(4) . yes
O18 H18 O4 0.773(17) 1.963(18) 2.720(2) 166(3) 1_465 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O3 C1 C2 36.0(2) . . . . ?
Mo1 O4 C2 C1 31.6(2) . . . . ?
Mo1 O7 C5 C6 -42.54(18) . . . . ?
Mo1 O8 C6 C5 38.68(17) . . . . ?
Mo2 O5 C3 C4 -35.81(18) . . . . ?
Mo2 O6 C4 C3 -38.1(2) . . . . ?
Mo2 O7 C5 C6 43.60(18) . . . . ?
Mo2 O8 C6 C5 -38.09(17) . . . . ?
Mo3 O11 C7 C8 86.34(19) . . . . ?
Mo3 O14 C10A C9 -167.9(2) 2_666 . . . ?
Mo3 O14 C10B C9 165.6(2) 2_666 . . . ?
Mo3 O16 C12 C11 19.2(3) 2_666 . . . ?
Mo4 O5 C3 C4 161.15(13) . . . . ?
Mo4 O11 C7 C8 -113.68(18) . . . . ?
Mo4 O13 C9 C10A -31.01(19) . . . . ?
Mo4 O13 C9 C10B 9.4(3) . . . . ?
Mo4 O14 C10A C9 -43.2(2) . . . . ?
Mo4 O14 C10B C9 41.6(6) . . . . ?
Mo4 O15 C11 C12 90.08(18) . . . . ?
O3 C1 C2 O4 -41.7(2) . . . . ?
O5 C3 C4 O6 46.5(2) . . . . ?
O7 C5 C6 O8 -0.6(2) . . . . ?
O11 C7 C8 O12 62.1(2) . . . . ?
O13 C9 C10A O14 45.0(2) . . . . ?
O13 C9 C10B O14 -29.5(5) . . . . ?
O15 C11 C12 O16 -63.2(2) . . . . ?
O17 C13 C14 O18 -56.9(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT417_mo_2021_03_03_jdm_tg216a_0m_a 
;
PROBLEM: Short Inter D-H..H-D       H13      ..H17      .       1.98 Ang.  
RESPONSE: This is due to a hydrogen bonding network between multiple 
ethylene glycol molecules and is not an issue.
;
####################################################################### 
# 
# 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_mo_2019_09_24_jdm_tg_moglyc_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2225739'
loop_
_audit_author_name
_audit_author_address
'George T.'
;Saint Marys University
Canada
;
_audit_update_record             
;
2023-10-01 deposited with the CCDC.	2023-10-06 downloaded from the CCDC.
;
_audit_creation_date             2023-09-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Tanner.George@smu.ca
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H10 Mo O6'
_chemical_formula_sum            'C4 H10 Mo O6'
_chemical_formula_weight         250.06
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_H-M_alt        'P 41'
_space_group_name_Hall           'P 4w'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'

_cell_length_a                   9.46450(10)
_cell_length_b                   9.46450(10)
_cell_length_c                   17.3160(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1551.11(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9030
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      52.15
_cell_measurement_theta_min      2.45
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.675
_exptl_absorpt_correction_T_max  0.7503
_exptl_absorpt_correction_T_min  0.6410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0996 before and 0.0613 after correction.
The Ratio of minimum to maximum transmission is 0.8543.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.225
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            110585
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         44.998
_diffrn_reflns_theta_min         2.152
_diffrn_ambient_temperature      100.00
_diffrn_detector                 '100 \\times 140 mm^2^ CMOS sensor'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12338
_reflns_number_total             12760
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS Inc., 2016)'
_computing_data_collection       'APEX4 (Bruker AXS Inc., 2021)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.0023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         12760
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0208
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0163P)²+1.0349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0518
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.97(2)
 0.03(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 O6-H6
 0.87 with sigma of 0.01
 O10-H10
 0.87 with sigma of 0.01
 O4-H4
 0.87 with sigma of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B)
;
_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 1.25321(2) 0.31262(2) 0.24855(2) 0.00887(2) Uani 1 1 d . . . . .
O1 O 1.35008(16) 0.27292(15) 0.16850(8) 0.0160(2) Uani 1 1 d . . . . .
O2 O 1.23314(15) 0.15663(14) 0.29636(8) 0.01443(19) Uani 1 1 d . . . . .
O3 O 1.39523(14) 0.38720(14) 0.32073(8) 0.01355(18) Uani 1 1 d . . . . .
O4 O 1.28304(14) 0.54738(13) 0.21246(7) 0.01301(18) Uani 1 1 d D . . . .
H4 H 1.316(4) 0.559(4) 0.1672(11) 0.020 Uiso 1 1 d D U . . .
O5 O 1.07192(13) 0.32833(13) 0.19416(7) 0.01148(16) Uani 1 1 d . . . . .
O6 O 1.10618(13) 0.42797(14) 0.33020(7) 0.01270(18) Uani 1 1 d D . . . .
H6 H 1.133(4) 0.482(3) 0.3668(16) 0.019 Uiso 1 1 d D U . . .
C1 C 1.4750(2) 0.5095(2) 0.29929(12) 0.0188(3) Uani 1 1 d . . . . .
H1A H 1.546598 0.484033 0.259988 0.023 Uiso 1 1 calc R U . . .
H1B H 1.524535 0.548308 0.344964 0.023 Uiso 1 1 calc R U . . .
C2 C 1.3740(2) 0.61830(19) 0.26687(11) 0.0173(3) Uani 1 1 d . . . . .
H2A H 1.317191 0.660581 0.308950 0.021 Uiso 1 1 calc R U . . .
H2B H 1.427157 0.694669 0.240760 0.021 Uiso 1 1 calc R U . . .
C3 C 0.94496(17) 0.35727(18) 0.23720(9) 0.0134(2) Uani 1 1 d . . . . .
H3A H 0.914092 0.271597 0.265335 0.016 Uiso 1 1 calc R U . . .
H3B H 0.868193 0.386505 0.201807 0.016 Uiso 1 1 calc R U . . .
C4 C 0.97750(17) 0.47372(18) 0.29311(10) 0.0134(2) Uani 1 1 d . . . . .
H4A H 0.991731 0.564528 0.265817 0.016 Uiso 1 1 calc R U . . .
H4B H 0.900340 0.484967 0.331219 0.016 Uiso 1 1 calc R U . . .
Mo02 Mo 1.19245(2) 0.76395(2) 0.49709(2) 0.00850(2) Uani 1 1 d . . . . .
O7 O 1.33850(14) 0.76412(15) 0.43988(8) 0.0153(2) Uani 1 1 d . . . . .
O8 O 1.24892(14) 0.71144(15) 0.58594(8) 0.01441(19) Uani 1 1 d . . . . .
O9 O 1.11328(13) 0.58866(13) 0.45481(7) 0.01216(17) Uani 1 1 d . . . . .
O10 O 0.96108(13) 0.74932(13) 0.54814(7) 0.01134(16) Uani 1 1 d D . . . .
H10 H 0.952(4) 0.736(4) 0.5967(9) 0.022(9) Uiso 1 1 d D . . . .
O11 O 1.18119(13) 0.96507(13) 0.52812(7) 0.01087(16) Uani 1 1 d . . . . .
O12 O 1.05704(15) 0.86985(14) 0.41085(7) 0.01382(19) Uani 1 1 d . . . . .
H12 H 1.026(4) 0.848(4) 0.373(2) 0.021 Uiso 1 1 d . U . . .
C5 C 1.00131(18) 0.52114(15) 0.49663(12) 0.0143(2) Uani 1 1 d . . . . .
H5A H 1.037349 0.482291 0.545925 0.017 Uiso 1 1 calc R U . . .
H5B H 0.961130 0.442665 0.465861 0.017 Uiso 1 1 calc R U . . .
C6 C 0.88974(17) 0.63177(19) 0.51200(9) 0.0139(2) Uani 1 1 d . . . . .
H6A H 0.844859 0.661963 0.463068 0.017 Uiso 1 1 calc R U . . .
H6B H 0.815696 0.593696 0.546614 0.017 Uiso 1 1 calc R U . . .
C7 C 1.14789(18) 1.06989(18) 0.47135(10) 0.0134(2) Uani 1 1 d . . . . .
H7A H 1.229661 1.085621 0.436743 0.016 Uiso 1 1 calc R U . . .
H7B H 1.123620 1.160513 0.496625 0.016 Uiso 1 1 calc R U . . .
C8 C 1.02366(18) 1.01499(18) 0.42613(10) 0.0133(2) Uani 1 1 d . . . . .
H8A H 0.935527 1.022758 0.456632 0.016 Uiso 1 1 calc R U . . .
H8B H 1.011994 1.068279 0.377351 0.016 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 O1 1.7038(14) . ?
Mo1 O2 1.7033(13) . ?
Mo1 O3 1.9666(13) . ?
Mo1 O4 2.3252(13) . ?
Mo1 O5 1.9628(12) . ?
Mo1 O6 2.2644(12) . ?
O3 C1 1.431(2) . ?
O4 H4 0.851(13) . ?
O4 C2 1.442(2) . ?
O5 C3 1.440(2) . ?
O6 H6 0.854(13) . ?
O6 C4 1.443(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.513(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.499(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
Mo02 O7 1.7006(13) . ?
Mo02 O8 1.7028(13) . ?
Mo02 O9 1.9622(12) . ?
Mo02 O10 2.3655(12) . ?
Mo02 O11 1.9807(12) . ?
Mo02 O12 2.2084(13) . ?
O9 C5 1.434(2) . ?
O10 H10 0.855(13) . ?
O10 C6 1.444(2) . ?
O11 C7 1.432(2) . ?
O12 H12 0.76(4) . ?
O12 C8 1.434(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.511(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.505(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 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
O1 Mo1 O3 103.20(7) . . ?
O1 Mo1 O4 85.80(6) . . ?
O1 Mo1 O5 95.56(7) . . ?
O1 Mo1 O6 160.91(6) . . ?
O2 Mo1 O1 105.32(7) . . ?
O2 Mo1 O3 94.49(6) . . ?
O2 Mo1 O4 166.50(6) . . ?
O2 Mo1 O5 101.62(6) . . ?
O2 Mo1 O6 92.63(6) . . ?
O3 Mo1 O4 75.22(5) . . ?
O3 Mo1 O6 81.38(5) . . ?
O5 Mo1 O3 151.07(5) . . ?
O5 Mo1 O4 84.54(5) . . ?
O5 Mo1 O6 74.09(5) . . ?
O6 Mo1 O4 77.39(5) . . ?
C1 O3 Mo1 119.08(11) . . ?
Mo1 O4 H4 115(2) . . ?
C2 O4 Mo1 109.99(10) . . ?
C2 O4 H4 109(2) . . ?
C3 O5 Mo1 119.70(10) . . ?
Mo1 O6 H6 125(2) . . ?
C4 O6 Mo1 112.66(9) . . ?
C4 O6 H6 113(2) . . ?
O3 C1 H1A 110.0 . . ?
O3 C1 H1B 110.0 . . ?
O3 C1 C2 108.25(15) . . ?
H1A C1 H1B 108.4 . . ?
C2 C1 H1A 110.0 . . ?
C2 C1 H1B 110.0 . . ?
O4 C2 C1 107.63(15) . . ?
O4 C2 H2A 110.2 . . ?
O4 C2 H2B 110.2 . . ?
C1 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
O5 C3 H3A 110.2 . . ?
O5 C3 H3B 110.2 . . ?
O5 C3 C4 107.61(13) . . ?
H3A C3 H3B 108.5 . . ?
C4 C3 H3A 110.2 . . ?
C4 C3 H3B 110.2 . . ?
O6 C4 C3 103.90(13) . . ?
O6 C4 H4A 111.0 . . ?
O6 C4 H4B 111.0 . . ?
C3 C4 H4A 111.0 . . ?
C3 C4 H4B 111.0 . . ?
H4A C4 H4B 109.0 . . ?
O7 Mo02 O8 105.75(7) . . ?
O7 Mo02 O9 95.38(6) . . ?
O7 Mo02 O10 165.97(6) . . ?
O7 Mo02 O11 101.59(6) . . ?
O7 Mo02 O12 94.44(6) . . ?
O8 Mo02 O9 102.14(6) . . ?
O8 Mo02 O10 86.32(6) . . ?
O8 Mo02 O11 93.00(6) . . ?
O8 Mo02 O12 157.75(6) . . ?
O9 Mo02 O10 74.72(5) . . ?
O9 Mo02 O11 153.28(5) . . ?
O9 Mo02 O12 84.82(5) . . ?
O11 Mo02 O10 84.55(5) . . ?
O11 Mo02 O12 73.51(5) . . ?
O12 Mo02 O10 75.05(5) . . ?
C5 O9 Mo02 118.07(10) . . ?
Mo02 O10 H10 118(3) . . ?
C6 O10 Mo02 108.43(9) . . ?
C6 O10 H10 105(3) . . ?
C7 O11 Mo02 119.43(10) . . ?
Mo02 O12 H12 134(3) . . ?
C8 O12 Mo02 115.96(9) . . ?
C8 O12 H12 110(3) . . ?
O9 C5 H5A 110.3 . . ?
O9 C5 H5B 110.3 . . ?
O9 C5 C6 107.26(13) . . ?
H5A C5 H5B 108.5 . . ?
C6 C5 H5A 110.3 . . ?
C6 C5 H5B 110.3 . . ?
O10 C6 C5 106.47(13) . . ?
O10 C6 H6A 110.4 . . ?
O10 C6 H6B 110.4 . . ?
C5 C6 H6A 110.4 . . ?
C5 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
O11 C7 H7A 110.4 . . ?
O11 C7 H7B 110.4 . . ?
O11 C7 C8 106.86(13) . . ?
H7A C7 H7B 108.6 . . ?
C8 C7 H7A 110.4 . . ?
C8 C7 H7B 110.4 . . ?
O12 C8 C7 104.75(13) . . ?
O12 C8 H8A 110.8 . . ?
O12 C8 H8B 110.8 . . ?
C7 C8 H8A 110.8 . . ?
C7 C8 H8B 110.8 . . ?
H8A C8 H8B 108.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O4 H4 O3 0.851(13) 1.852(14) 2.7000(18) 174(4) 4_674 yes
O6 H6 O9 0.854(13) 1.836(19) 2.6406(17) 156(4) . yes
O10 H10 O5 0.855(13) 1.808(15) 2.6517(16) 169(4) 2_765 yes
O12 H12 O11 0.76(4) 1.75(4) 2.5047(17) 171(4) 4_574 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O3 C1 C2 46.1(2) . . . . ?
Mo1 O4 C2 C1 29.87(17) . . . . ?
Mo1 O5 C3 C4 45.17(16) . . . . ?
Mo1 O6 C4 C3 36.07(15) . . . . ?
O3 C1 C2 O4 -47.0(2) . . . . ?
O5 C3 C4 O6 -49.29(16) . . . . ?
Mo02 O9 C5 C6 51.51(17) . . . . ?
Mo02 O10 C6 C5 33.13(14) . . . . ?
Mo02 O11 C7 C8 46.54(16) . . . . ?
Mo02 O12 C8 C7 29.08(16) . . . . ?
O9 C5 C6 O10 -52.76(17) . . . . ?
O11 C7 C8 O12 -44.58(17) . . . . ?

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

####################################################################### 
# 
# 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_mo_jasontemp2021_0m_a_pl
_database_code_depnum_ccdc_archive 'CCDC 2225738'
loop_
_audit_author_name
_audit_author_address
'George T.'
;Saint Marys University
Canada
;
_audit_update_record             
;
2023-10-01 deposited with the CCDC.	2023-10-06 downloaded from the CCDC.
;
_audit_creation_date             2023-09-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Tanner.George@smu.ca
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H36 Mo4 O20'
_chemical_formula_sum            'C16 H36 Mo4 O20'
_chemical_formula_weight         932.21
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   34.2851(19)
_cell_length_b                   9.7131(5)
_cell_length_c                   8.4881(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2826.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    125
_cell_measurement_theta_max      35.67
_cell_measurement_theta_min      2.68
_shelx_estimated_absorpt_T_max   0.811
_shelx_estimated_absorpt_T_min   0.669
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  0.1100
_exptl_absorpt_correction_T_min  0.0655
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1031 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.5955.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            281755
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.335
_diffrn_reflns_theta_min         2.179
_diffrn_ambient_temperature      125.00
_diffrn_detector                 '100 \\times 140 mm^2^ CMOS sensor'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                13061
_reflns_number_total             13707
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS Inc., 2016)'
_computing_data_collection       'APEX4 (Bruker AXS Inc., 2021)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.508
_refine_diff_density_min         -2.102
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(7)
_refine_ls_extinction_coef       0.00076(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         13707
_refine_ls_number_restraints     219
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0655
_refine_ls_restrained_S_all      1.081
_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)+(0.0002P)²+20.8382P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1339
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.95(8)
 0.05(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 O5-H5
 0.87 with sigma of 0.01
 C5-H5
 1.922041 with sigma of 0.02
 Mo2-H5
 2.676213 with sigma of 0.02
 O1A-C1 \\sim O1B-C1B
 with sigma of 0.02
 C1B-C1A \\sim C1-C2A
 with sigma of 0.02
 C1A-O2 \\sim O2-C2A
 with sigma of 0.02
 O14A-C12A \\sim O14B-C12B
 with sigma of 0.02
 C12B-C11B \\sim C12A-C11A
 with sigma of 0.02
 C11A-O13 \\sim O13-C11B
 with sigma of 0.02
 O17-C15A \\sim O17-C15B
 with sigma of 0.02
 O18-C16A \\sim O18-C16B
 with sigma of 0.02
 C15A-C16A \\sim C15B-C16B
 with sigma of 0.02
 O17-C16A \\sim O17-C16B
 with sigma of 0.04
 O18-C15A \\sim O18-C15B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O1A \\sim C1 \\sim C2A \\sim O1B \\sim C1A \\sim C1B: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
O13 \\sim O13 \\sim O14A \\sim C11A \\sim C12A \\sim O14B \\sim C11B \\sim
C12B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
C15A \\sim C16A \\sim C15B \\sim C16B: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Uanis(O1B) = Uanis(O1A)
5. Rigid body (RIGU) restrains
 O2, O1A, C1, C2A, O1B, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15A, C16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15B, C16B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O1A)=Sof(H1A)=Sof(C1)=Sof(H1B)=Sof(H1C)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-
 FVAR(1)
 Sof(O1B)=Sof(H1BA)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BB)=Sof(H1BC)=
 FVAR(1)
 Sof(O14B)=Sof(H14D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12C)=
 Sof(H12D)=1-FVAR(2)
 Sof(O14A)=Sof(H14C)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=
 Sof(H12B)=FVAR(2)
 Sof(H17A)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(H16C)=Sof(H16D)=1-FVAR(3)
 Sof(H17)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(H16A)=Sof(H16B)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B), C1(H1B,H1C),
 C2A(H2AA,H2AB), C11A(H11A,H11B), C12A(H12A,H12B), C15A(H15A,H15B), C16A(H16A,
 H16B), C1A(H1AA,H1AB), C1B(H1BB,H1BC), C11B(H11C,H11D), C12B(H12C,H12D),
 C15B(H15C,H15D), C16B(H16C,H16D)
7.b Tetrahedral OH refined with riding coordinates:
 O17(H17), O17(H17A)
7.c Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O14A(H14C), O1B(H1BA), O14B(H14D)
;
_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 0.29733(2) 0.91332(8) -0.05656(14) 0.0482(2) Uani 1 1 d . . . . .
Mo2 Mo 0.35563(2) 1.06408(7) 0.06330(11) 0.03999(16) Uani 1 1 d D . . . .
Mo3 Mo 0.44055(2) 0.79314(8) -0.43726(12) 0.04268(17) Uani 1 1 d . . . . .
Mo4 Mo 0.40153(2) 0.57270(7) -0.55101(11) 0.04021(17) Uani 1 1 d . . . . .
O2 O 0.3231(2) 1.0940(7) -0.1286(10) 0.0529(19) Uani 1 1 d D . . . .
O3 O 0.33069(17) 0.8836(6) 0.1416(8) 0.0372(12) Uani 1 1 d . . . . .
O4 O 0.38667(16) 0.8144(6) 0.3763(7) 0.0343(11) Uani 1 1 d . . . . .
O5 O 0.40337(18) 0.9927(7) 0.1609(7) 0.0383(13) Uani 1 1 d D . . . .
H5 H 0.4090(9) 0.929(9) 0.230(11) 0.057 Uiso 1 1 d D U . . .
O6 O 0.3936(2) 1.1779(7) -0.0398(10) 0.0497(16) Uani 1 1 d . . . . .
O7 O 0.2845(2) 0.8815(8) -0.2739(9) 0.0512(18) Uani 1 1 d . . . . .
O8 O 0.2899(2) 0.7157(7) -0.0498(13) 0.063(2) Uani 1 1 d . . . . .
O9 O 0.2578(2) 0.9819(8) 0.0264(10) 0.054(2) Uani 1 1 d . . . . .
O10 O 0.3323(2) 1.1654(8) 0.1923(11) 0.056(2) Uani 1 1 d . . . . .
O11 O 0.36712(19) 0.8807(6) -0.1238(7) 0.0381(13) Uani 1 1 d . . . . .
O12 O 0.3933(2) 0.6868(6) -0.3556(8) 0.0423(15) Uani 1 1 d . . . . .
O13 O 0.45060(18) 0.6737(7) -0.6253(10) 0.0491(18) Uani 1 1 d D U . . .
O15 O 0.39102(19) 0.5290(7) -0.7695(8) 0.0408(14) Uani 1 1 d . . . . .
O16 O 0.34626(17) 0.5424(7) -0.5364(8) 0.0435(15) Uani 1 1 d . . . . .
O17 O 0.4160(2) 0.9524(7) -0.3366(9) 0.0506(18) Uani 1 1 d D . . . .
H17 H 0.399162 0.957780 -0.265058 0.076 Uiso 0.544(17) 1 calc R U P A 1
H17A H 0.403522 0.958224 -0.251760 0.076 Uiso 0.456(17) 1 calc R U P A 2
O18 O 0.46555(17) 0.9386(7) -0.5532(10) 0.0463(14) Uani 1 1 d D . . . .
O19 O 0.4736(3) 0.7318(9) -0.3085(11) 0.063(2) Uani 1 1 d . . . . .
O20 O 0.4226(2) 0.4359(8) -0.4661(11) 0.057(2) Uani 1 1 d . . . . .
C3 C 0.3189(2) 0.8449(9) 0.2963(10) 0.0369(17) Uani 1 1 d . . . . .
H3A H 0.313453 0.744861 0.298662 0.044 Uiso 1 1 calc R U . . .
H3B H 0.294549 0.894031 0.324019 0.044 Uiso 1 1 calc R U . . .
C4 C 0.3498(2) 0.8783(9) 0.4153(9) 0.0361(16) Uani 1 1 d . . . . .
H4A H 0.353319 0.979374 0.420601 0.043 Uiso 1 1 calc R U . . .
H4B H 0.341278 0.846147 0.520500 0.043 Uiso 1 1 calc R U . . .
C5 C 0.4393(3) 1.0497(12) 0.0993(14) 0.052(3) Uani 1 1 d D . . . .
H5A H 0.449275 0.992238 0.011858 0.063 Uiso 1 1 calc R U . . .
H5B H 0.459365 1.054298 0.182801 0.063 Uiso 1 1 calc R U . . .
C6 C 0.4295(3) 1.1893(11) 0.0423(17) 0.056(3) Uani 1 1 d . . . . .
H6A H 0.426847 1.253683 0.132098 0.068 Uiso 1 1 calc R U . . .
H6B H 0.450178 1.223931 -0.028688 0.068 Uiso 1 1 calc R U . . .
C7 C 0.2692(4) 0.7501(12) -0.3105(15) 0.057(3) Uani 1 1 d . . . . .
H7A H 0.287267 0.701672 -0.382808 0.068 Uiso 1 1 calc R U . . .
H7B H 0.243840 0.760668 -0.364618 0.068 Uiso 1 1 calc R U . . .
C8 C 0.2639(5) 0.6671(15) -0.164(2) 0.090(6) Uani 1 1 d . . . . .
H8A H 0.236770 0.675711 -0.126159 0.107 Uiso 1 1 calc R U . . .
H8B H 0.269183 0.568740 -0.186596 0.107 Uiso 1 1 calc R U . . .
C9 C 0.3874(3) 0.7563(9) -0.0819(10) 0.043(2) Uani 1 1 d . . . . .
H9A H 0.378555 0.725849 0.023565 0.052 Uiso 1 1 calc R U . . .
H9B H 0.415666 0.775527 -0.075684 0.052 Uiso 1 1 calc R U . . .
C10 C 0.3806(3) 0.6442(10) -0.1967(12) 0.048(2) Uani 1 1 d . . . . .
H10A H 0.395225 0.561152 -0.163953 0.058 Uiso 1 1 calc R U . . .
H10B H 0.352486 0.620680 -0.198949 0.058 Uiso 1 1 calc R U . . .
C13 C 0.3520(3) 0.4878(10) -0.8056(10) 0.0406(19) Uani 1 1 d . . . . .
H13A H 0.352234 0.407533 -0.877381 0.049 Uiso 1 1 calc R U . . .
H13B H 0.337880 0.564050 -0.858039 0.049 Uiso 1 1 calc R U . . .
C14 C 0.3320(3) 0.4506(11) -0.6528(13) 0.049(2) Uani 1 1 d . . . . .
H14A H 0.303386 0.460097 -0.663591 0.058 Uiso 1 1 calc R U . . .
H14B H 0.338045 0.354279 -0.623456 0.058 Uiso 1 1 calc R U . . .
O1A O 0.2987(10) 1.108(3) -0.442(4) 0.142(8) Uani 0.500(15) 1 d D U P B 1
H1A H 0.314361 1.053541 -0.399570 0.213 Uiso 0.500(15) 1 calc R U P B 1
O14A O 0.4527(3) 0.5372(16) -0.9642(16) 0.061(4) Uani 0.630(16) 1 d D U P C 1
H14C H 0.431794 0.529179 -0.913280 0.091 Uiso 0.630(16) 1 calc R U P C 1
C1 C 0.2856(10) 1.206(4) -0.329(3) 0.090(8) Uani 0.500(15) 1 d D U P B 1
H1B H 0.261373 1.172605 -0.278773 0.108 Uiso 0.500(15) 1 calc R U P B 1
H1C H 0.279634 1.294558 -0.382561 0.108 Uiso 0.500(15) 1 calc R U P B 1
C2A C 0.3158(10) 1.228(3) -0.209(4) 0.090(8) Uani 0.500(15) 1 d D U P B 1
H2AA H 0.306969 1.297716 -0.131474 0.108 Uiso 0.500(15) 1 calc R U P B 1
H2AB H 0.340126 1.261853 -0.258711 0.108 Uiso 0.500(15) 1 calc R U P B 1
C11A C 0.4818(7) 0.661(3) -0.736(3) 0.081(7) Uani 0.630(16) 1 d D U P C 1
H11A H 0.486501 0.755296 -0.777253 0.097 Uiso 0.630(16) 1 calc R U P C 1
H11B H 0.505178 0.636256 -0.674258 0.097 Uiso 0.630(16) 1 calc R U P C 1
C12A C 0.4816(7) 0.575(3) -0.866(3) 0.109(9) Uani 0.630(16) 1 d D U P C 1
H12A H 0.501913 0.613845 -0.936000 0.130 Uiso 0.630(16) 1 calc R U P C 1
H12B H 0.492346 0.487433 -0.825979 0.130 Uiso 0.630(16) 1 calc R U P C 1
C15A C 0.4232(5) 1.0896(15) -0.402(2) 0.041(2) Uani 0.544(17) 1 d D U P A 1
H15A H 0.422508 1.161962 -0.320125 0.049 Uiso 0.544(17) 1 calc R U P A 1
H15B H 0.404545 1.112700 -0.487225 0.049 Uiso 0.544(17) 1 calc R U P A 1
C16A C 0.4642(5) 1.0664(16) -0.465(2) 0.041(2) Uani 0.544(17) 1 d D U P A 1
H16A H 0.471761 1.143950 -0.534410 0.049 Uiso 0.544(17) 1 calc R U P A 1
H16B H 0.482918 1.062324 -0.376453 0.049 Uiso 0.544(17) 1 calc R U P A 1
O1B O 0.2671(10) 1.270(4) -0.215(4) 0.142(8) Uani 0.500(15) 1 d D U P B 2
H1BA H 0.261841 1.194280 -0.258265 0.213 Uiso 0.500(15) 1 calc R U P B 2
O14B O 0.5299(7) 0.604(4) -0.700(4) 0.091(11) Uani 0.370(16) 1 d D U P C 2
H14D H 0.527297 0.665073 -0.630448 0.137 Uiso 0.370(16) 1 calc R U P C 2
C1A C 0.3273(8) 1.174(2) -0.277(2) 0.052(5) Uani 0.500(15) 1 d D U P B 2
H1AA H 0.355174 1.191104 -0.301246 0.062 Uiso 0.500(15) 1 calc R U P B 2
H1AB H 0.315381 1.124454 -0.366931 0.062 Uiso 0.500(15) 1 calc R U P B 2
C1B C 0.3066(10) 1.306(3) -0.248(4) 0.085(7) Uani 0.500(15) 1 d D U P B 2
H1BB H 0.318418 1.355859 -0.158275 0.103 Uiso 0.500(15) 1 calc R U P B 2
H1BC H 0.307932 1.366275 -0.342707 0.103 Uiso 0.500(15) 1 calc R U P B 2
C11B C 0.4692(7) 0.700(3) -0.770(3) 0.045(6) Uani 0.370(16) 1 d D U P C 2
H11C H 0.450204 0.698998 -0.858116 0.054 Uiso 0.370(16) 1 calc R U P C 2
H11D H 0.482719 0.789924 -0.768575 0.054 Uiso 0.370(16) 1 calc R U P C 2
C12B C 0.4956(8) 0.592(3) -0.783(4) 0.059(8) Uani 0.370(16) 1 d D U P C 2
H12C H 0.482439 0.506503 -0.749211 0.071 Uiso 0.370(16) 1 calc R U P C 2
H12D H 0.502253 0.580960 -0.896299 0.071 Uiso 0.370(16) 1 calc R U P C 2
C15B C 0.4429(6) 1.0731(19) -0.352(2) 0.041(2) Uani 0.456(17) 1 d D U P A 2
H15C H 0.428884 1.159455 -0.326291 0.049 Uiso 0.456(17) 1 calc R U P A 2
H15D H 0.465137 1.063437 -0.277954 0.049 Uiso 0.456(17) 1 calc R U P A 2
C16B C 0.4569(7) 1.0762(18) -0.515(2) 0.041(2) Uani 0.456(17) 1 d D U P A 2
H16C H 0.436509 1.113225 -0.585511 0.049 Uiso 0.456(17) 1 calc R U P A 2
H16D H 0.480461 1.134445 -0.523524 0.049 Uiso 0.456(17) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Mo2 2.6786(10) . ?
Mo1 O2 2.057(7) . ?
Mo1 O3 2.054(6) . ?
Mo1 O7 1.921(8) . ?
Mo1 O8 1.937(7) . ?
Mo1 O9 1.667(8) . ?
Mo1 O11 2.480(7) . ?
Mo2 O2 1.996(8) . ?
Mo2 O3 2.060(6) . ?
Mo2 O5 1.961(6) . ?
Mo2 O6 1.920(7) . ?
Mo2 O10 1.675(8) . ?
Mo2 O11 2.418(6) . ?
Mo3 Mo4 2.7030(10) . ?
Mo3 O4 2.441(6) 1_554 ?
Mo3 O12 2.042(7) . ?
Mo3 O13 2.003(8) . ?
Mo3 O17 1.957(8) . ?
Mo3 O18 1.923(7) . ?
Mo3 O19 1.683(8) . ?
Mo4 O4 2.481(6) 1_554 ?
Mo4 O12 2.015(7) . ?
Mo4 O13 2.047(6) . ?
Mo4 O15 1.936(7) . ?
Mo4 O16 1.922(6) . ?
Mo4 O20 1.675(8) . ?
O2 C2A 1.49(2) . ?
O2 C1A 1.49(2) . ?
O3 C3 1.424(11) . ?
O4 C4 1.446(9) . ?
O5 H5 0.873(13) . ?
O5 C5 1.447(11) . ?
O6 C6 1.417(13) . ?
O7 C7 1.414(12) . ?
O8 C8 1.401(15) . ?
O11 C9 1.438(11) . ?
O12 C10 1.477(12) . ?
O13 C11A 1.43(2) . ?
O13 C11B 1.41(2) . ?
O15 C13 1.430(11) . ?
O16 C14 1.418(11) . ?
O17 H17 0.8400 . ?
O17 H17A 0.8400 . ?
O17 C15A 1.465(16) . ?
O17 C15B 1.497(17) . ?
O18 C16A 1.449(15) . ?
O18 C16B 1.408(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.500(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.478(16) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.49(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.480(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.510(14) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
O1A H1A 0.8400 . ?
O1A C1 1.42(3) . ?
O14A H14C 0.8400 . ?
O14A C12A 1.35(2) . ?
C1 H1B 0.9900 . ?
C1 H1C 0.9900 . ?
C1 C2A 1.47(3) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11A C12A 1.38(2) . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C15A C16A 1.521(19) . ?
C16A H16A 0.9900 . ?
C16A H16B 0.9900 . ?
O1B H1BA 0.8400 . ?
O1B C1B 1.43(4) . ?
O14B H14D 0.8400 . ?
O14B C12B 1.38(3) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1A C1B 1.49(3) . ?
C1B H1BB 0.9900 . ?
C1B H1BC 0.9900 . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C11B C12B 1.39(3) . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
C15B H15C 0.9900 . ?
C15B H15D 0.9900 . ?
C15B C16B 1.46(2) . ?
C16B H16C 0.9900 . ?
C16B H16D 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
O2 Mo1 Mo2 47.7(2) . . ?
O2 Mo1 O11 68.1(3) . . ?
O3 Mo1 Mo2 49.48(17) . . ?
O3 Mo1 O2 97.1(3) . . ?
O3 Mo1 O11 68.5(2) . . ?
O7 Mo1 Mo2 128.6(2) . . ?
O7 Mo1 O2 87.1(3) . . ?
O7 Mo1 O3 153.0(3) . . ?
O7 Mo1 O8 80.7(4) . . ?
O7 Mo1 O11 88.8(3) . . ?
O8 Mo1 Mo2 128.9(2) . . ?
O8 Mo1 O2 155.6(4) . . ?
O8 Mo1 O3 84.8(3) . . ?
O8 Mo1 O11 90.4(3) . . ?
O9 Mo1 Mo2 103.2(3) . . ?
O9 Mo1 O2 97.7(4) . . ?
O9 Mo1 O3 99.4(3) . . ?
O9 Mo1 O7 106.5(4) . . ?
O9 Mo1 O8 106.1(4) . . ?
O9 Mo1 O11 158.9(3) . . ?
O11 Mo1 Mo2 55.75(13) . . ?
O2 Mo2 Mo1 49.6(2) . . ?
O2 Mo2 O3 98.9(3) . . ?
O2 Mo2 O11 70.3(3) . . ?
O3 Mo2 Mo1 49.28(18) . . ?
O3 Mo2 O11 69.7(2) . . ?
O5 Mo2 Mo1 126.16(19) . . ?
O5 Mo2 O2 149.7(3) . . ?
O5 Mo2 O3 84.8(3) . . ?
O5 Mo2 O11 83.2(2) . . ?
O6 Mo2 Mo1 130.4(3) . . ?
O6 Mo2 O2 85.6(3) . . ?
O6 Mo2 O3 156.7(3) . . ?
O6 Mo2 O5 80.2(3) . . ?
O6 Mo2 O11 90.8(3) . . ?
O10 Mo2 Mo1 102.4(3) . . ?
O10 Mo2 O2 100.4(4) . . ?
O10 Mo2 O3 95.2(3) . . ?
O10 Mo2 O5 109.2(4) . . ?
O10 Mo2 O6 106.4(4) . . ?
O10 Mo2 O11 160.0(3) . . ?
O11 Mo2 Mo1 57.97(16) . . ?
O4 Mo3 Mo4 57.39(15) 1_554 . ?
O12 Mo3 Mo4 47.79(18) . . ?
O12 Mo3 O4 70.3(2) . 1_554 ?
O13 Mo3 Mo4 48.83(18) . . ?
O13 Mo3 O4 70.3(2) . 1_554 ?
O13 Mo3 O12 96.5(3) . . ?
O17 Mo3 Mo4 124.7(2) . . ?
O17 Mo3 O4 83.7(3) . 1_554 ?
O17 Mo3 O12 84.9(3) . . ?
O17 Mo3 O13 151.6(3) . . ?
O18 Mo3 Mo4 128.3(2) . . ?
O18 Mo3 O4 86.7(2) . 1_554 ?
O18 Mo3 O12 154.0(3) . . ?
O18 Mo3 O13 86.6(3) . . ?
O18 Mo3 O17 80.5(3) . . ?
O19 Mo3 Mo4 106.5(3) . . ?
O19 Mo3 O4 163.8(3) . 1_554 ?
O19 Mo3 O12 97.7(4) . . ?
O19 Mo3 O13 101.3(4) . . ?
O19 Mo3 O17 106.6(4) . . ?
O19 Mo3 O18 107.0(3) . . ?
O4 Mo4 Mo3 55.99(13) 1_554 . ?
O12 Mo4 Mo3 48.64(19) . . ?
O12 Mo4 O4 69.8(2) . 1_554 ?
O12 Mo4 O13 96.0(3) . . ?
O13 Mo4 Mo3 47.4(2) . . ?
O13 Mo4 O4 68.8(2) . 1_554 ?
O15 Mo4 Mo3 127.4(2) . . ?
O15 Mo4 O4 86.0(2) . 1_554 ?
O15 Mo4 O12 152.0(3) . . ?
O15 Mo4 O13 87.9(3) . . ?
O16 Mo4 Mo3 125.89(17) . . ?
O16 Mo4 O4 87.6(3) . 1_554 ?
O16 Mo4 O12 83.9(3) . . ?
O16 Mo4 O13 154.6(3) . . ?
O16 Mo4 O15 81.1(3) . . ?
O20 Mo4 Mo3 105.1(3) . . ?
O20 Mo4 O4 161.1(3) . 1_554 ?
O20 Mo4 O12 98.2(4) . . ?
O20 Mo4 O13 99.1(3) . . ?
O20 Mo4 O15 108.6(4) . . ?
O20 Mo4 O16 106.0(3) . . ?
Mo2 O2 Mo1 82.7(3) . . ?
C2A O2 Mo1 144.1(15) . . ?
C2A O2 Mo2 126.4(15) . . ?
C1A O2 Mo1 137.7(10) . . ?
C1A O2 Mo2 135.4(11) . . ?
Mo1 O3 Mo2 81.2(2) . . ?
C3 O3 Mo1 129.3(5) . . ?
C3 O3 Mo2 129.8(5) . . ?
Mo3 O4 Mo4 66.62(16) 1_556 1_556 ?
C4 O4 Mo3 123.3(4) . 1_556 ?
C4 O4 Mo4 121.9(5) . 1_556 ?
Mo2 O5 H5 136(2) . . ?
C5 O5 Mo2 114.9(6) . . ?
C5 O5 H5 109(2) . . ?
C6 O6 Mo2 114.2(7) . . ?
C7 O7 Mo1 116.2(7) . . ?
C8 O8 Mo1 113.4(7) . . ?
Mo2 O11 Mo1 66.29(17) . . ?
C9 O11 Mo1 121.0(6) . . ?
C9 O11 Mo2 122.4(5) . . ?
Mo4 O12 Mo3 83.6(3) . . ?
C10 O12 Mo3 133.3(6) . . ?
C10 O12 Mo4 129.7(5) . . ?
Mo3 O13 Mo4 83.7(3) . . ?
C11A O13 Mo3 134.6(11) . . ?
C11A O13 Mo4 141.0(11) . . ?
C11B O13 Mo3 132.0(13) . . ?
C11B O13 Mo4 136.7(14) . . ?
C13 O15 Mo4 116.1(5) . . ?
C14 O16 Mo4 113.0(5) . . ?
Mo3 O17 H17 131.4 . . ?
Mo3 O17 H17A 130.3 . . ?
C15A O17 Mo3 118.7(8) . . ?
C15A O17 H17 109.5 . . ?
C15B O17 Mo3 108.5(9) . . ?
C15B O17 H17A 109.5 . . ?
C16A O18 Mo3 110.6(9) . . ?
C16B O18 Mo3 118.9(9) . . ?
O3 C3 H3A 109.4 . . ?
O3 C3 H3B 109.4 . . ?
O3 C3 C4 111.3(7) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
O4 C4 C3 111.7(6) . . ?
O4 C4 H4A 109.3 . . ?
O4 C4 H4B 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
O5 C5 H5A 110.5 . . ?
O5 C5 H5B 110.5 . . ?
O5 C5 C6 106.0(9) . . ?
H5A C5 H5B 108.7 . . ?
C6 C5 H5A 110.5 . . ?
C6 C5 H5B 110.5 . . ?
O6 C6 C5 106.6(8) . . ?
O6 C6 H6A 110.4 . . ?
O6 C6 H6B 110.4 . . ?
C5 C6 H6A 110.4 . . ?
C5 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
O7 C7 H7A 109.5 . . ?
O7 C7 H7B 109.5 . . ?
O7 C7 C8 110.5(10) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
O8 C8 C7 108.5(10) . . ?
O8 C8 H8A 110.0 . . ?
O8 C8 H8B 110.0 . . ?
C7 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
O11 C9 H9A 109.1 . . ?
O11 C9 H9B 109.1 . . ?
O11 C9 C10 112.3(8) . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
O12 C10 C9 110.4(7) . . ?
O12 C10 H10A 109.6 . . ?
O12 C10 H10B 109.6 . . ?
C9 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
O15 C13 H13A 110.1 . . ?
O15 C13 H13B 110.1 . . ?
O15 C13 C14 107.9(7) . . ?
H13A C13 H13B 108.4 . . ?
C14 C13 H13A 110.1 . . ?
C14 C13 H13B 110.1 . . ?
O16 C14 C13 106.9(7) . . ?
O16 C14 H14A 110.3 . . ?
O16 C14 H14B 110.3 . . ?
C13 C14 H14A 110.3 . . ?
C13 C14 H14B 110.3 . . ?
H14A C14 H14B 108.6 . . ?
C1 O1A H1A 109.5 . . ?
C12A O14A H14C 109.5 . . ?
O1A C1 H1B 109.7 . . ?
O1A C1 H1C 109.7 . . ?
O1A C1 C2A 110(3) . . ?
H1B C1 H1C 108.2 . . ?
C2A C1 H1B 109.7 . . ?
C2A C1 H1C 109.7 . . ?
O2 C2A H2AA 110.1 . . ?
O2 C2A H2AB 110.1 . . ?
C1 C2A O2 108(2) . . ?
C1 C2A H2AA 110.1 . . ?
C1 C2A H2AB 110.1 . . ?
H2AA C2A H2AB 108.4 . . ?
O13 C11A H11A 106.1 . . ?
O13 C11A H11B 106.1 . . ?
H11A C11A H11B 106.3 . . ?
C12A C11A O13 125(2) . . ?
C12A C11A H11A 106.1 . . ?
C12A C11A H11B 106.1 . . ?
O14A C12A C11A 132(2) . . ?
O14A C12A H12A 104.4 . . ?
O14A C12A H12B 104.4 . . ?
C11A C12A H12A 104.4 . . ?
C11A C12A H12B 104.4 . . ?
H12A C12A H12B 105.6 . . ?
O17 C15A H15A 112.0 . . ?
O17 C15A H15B 112.0 . . ?
O17 C15A C16A 98.9(12) . . ?
H15A C15A H15B 109.7 . . ?
C16A C15A H15A 112.0 . . ?
C16A C15A H15B 112.0 . . ?
O18 C16A C15A 109.7(11) . . ?
O18 C16A H16A 109.7 . . ?
O18 C16A H16B 109.7 . . ?
C15A C16A H16A 109.7 . . ?
C15A C16A H16B 109.7 . . ?
H16A C16A H16B 108.2 . . ?
C1B O1B H1BA 109.5 . . ?
C12B O14B H14D 109.5 . . ?
O2 C1A H1AA 110.7 . . ?
O2 C1A H1AB 110.7 . . ?
H1AA C1A H1AB 108.8 . . ?
C1B C1A O2 105.4(18) . . ?
C1B C1A H1AA 110.7 . . ?
C1B C1A H1AB 110.7 . . ?
O1B C1B C1A 106(3) . . ?
O1B C1B H1BB 110.6 . . ?
O1B C1B H1BC 110.6 . . ?
C1A C1B H1BB 110.6 . . ?
C1A C1B H1BC 110.6 . . ?
H1BB C1B H1BC 108.7 . . ?
O13 C11B H11C 111.1 . . ?
O13 C11B H11D 111.1 . . ?
H11C C11B H11D 109.1 . . ?
C12B C11B O13 103(2) . . ?
C12B C11B H11C 111.1 . . ?
C12B C11B H11D 111.1 . . ?
O14B C12B C11B 117(3) . . ?
O14B C12B H12C 108.1 . . ?
O14B C12B H12D 108.1 . . ?
C11B C12B H12C 108.1 . . ?
C11B C12B H12D 108.1 . . ?
H12C C12B H12D 107.3 . . ?
O17 C15B H15C 110.3 . . ?
O17 C15B H15D 110.3 . . ?
H15C C15B H15D 108.5 . . ?
C16B C15B O17 107.3(14) . . ?
C16B C15B H15C 110.3 . . ?
C16B C15B H15D 110.3 . . ?
O18 C16B C15B 105.7(15) . . ?
O18 C16B H16C 110.6 . . ?
O18 C16B H16D 110.6 . . ?
C15B C16B H16C 110.6 . . ?
C15B C16B H16D 110.6 . . ?
H16C C16B H16D 108.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O5 H5 O4 0.873(13) 1.83(3) 2.582(9) 142(3) . yes
O5 H5 O18 0.873(13) 2.67(6) 3.273(9) 127(6) 1_556 yes
O17 H17 O11 0.84 1.79 2.561(10) 151.7 . yes
C5 H5B O18 0.99 2.52 3.268(15) 132.6 1_556 yes
C6 H6B O14B 0.99 2.32 3.19(4) 147.0 2_675 yes
C8 H8A O1A 0.99 2.08 2.91(4) 140.2 3_545 yes
C13 H13A O10 0.99 2.52 3.203(12) 126.1 1_544 yes
C14 H14B O10 0.99 2.42 3.066(12) 122.5 1_544 yes
O1A H1A O7 0.84 2.23 2.67(4) 112.9 . yes
O14A H14C O15 0.84 1.86 2.685(13) 168.7 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C2A C1 -33(4) . . . . ?
Mo1 O2 C1A C1B 116(2) . . . . ?
Mo1 O3 C3 C4 -161.7(5) . . . . ?
Mo1 O7 C7 C8 4.0(15) . . . . ?
Mo1 O8 C8 C7 36.1(17) . . . . ?
Mo1 O11 C9 C10 82.6(9) . . . . ?
Mo2 O2 C2A C1 -171.3(16) . . . . ?
Mo2 O2 C1A C1B -96(2) . . . . ?
Mo2 O3 C3 C4 -46.6(10) . . . . ?
Mo2 O5 C5 C6 28.2(10) . . . . ?
Mo2 O6 C6 C5 42.9(11) . . . . ?
Mo2 O11 C9 C10 162.6(6) . . . . ?
Mo3 O4 C4 C3 -165.0(6) 1_556 . . . ?
Mo3 O12 C10 C9 41.3(13) . . . . ?
Mo3 O13 C11A C12A -176(3) . . . . ?
Mo3 O13 C11B C12B 129.5(17) . . . . ?
Mo3 O17 C15A C16A -31.1(14) . . . . ?
Mo3 O17 C15B C16B 45.8(18) . . . . ?
Mo3 O18 C16A C15A -47.0(16) . . . . ?
Mo3 O18 C16B C15B 23(2) . . . . ?
Mo4 O4 C4 C3 -83.6(8) 1_556 . . . ?
Mo4 O12 C10 C9 167.0(7) . . . . ?
Mo4 O13 C11A C12A 17(5) . . . . ?
Mo4 O13 C11B C12B -93(2) . . . . ?
Mo4 O15 C13 C14 -16.0(10) . . . . ?
Mo4 O16 C14 C13 -42.1(10) . . . . ?
O2 C1A C1B O1B -60(3) . . . . ?
O3 C3 C4 O4 -56.3(10) . . . . ?
O5 C5 C6 O6 -43.5(12) . . . . ?
O7 C7 C8 O8 -25.2(18) . . . . ?
O11 C9 C10 O12 58.6(12) . . . . ?
O13 C11A C12A O14A 36(6) . . . . ?
O13 C11B C12B O14B -80(3) . . . . ?
O15 C13 C14 O16 35.9(11) . . . . ?
O17 C15A C16A O18 47.4(17) . . . . ?
O17 C15B C16B O18 -43(2) . . . . ?
O1A C1 C2A O2 -61(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.95(8)
2 0.05(8)

# start Validation Reply Form
_vrf_PLAT975_mo_jasontemp2021_0m_a_pl 
;
PROBLEM: Check Calcd Resid. Dens.  0.99Ang From O20     .       1.56 eA-3  
RESPONSE: This occurs between two  M=O oxygen atoms and is thought to be due 
to high localized electron density between the O=Mo-Mo=O unit.
;
