# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_akdk22011_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 2312691'
loop_
_audit_author_name
_audit_author_address
'Adrian Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2023-12-07 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_audit_creation_date             2022-11-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C19 H19 Mo N O9 S'
_chemical_formula_sum            'C19 H19 Mo N O9 S'
_chemical_formula_weight         533.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C19 H19 Mo1 N1 O9 S1'
_chemical_oxdiff_usercomment     'Lukas Geciauskas LG-1-006'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 '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                   7.97347(14)
_cell_length_b                   14.0397(3)
_cell_length_c                   18.8868(4)
_cell_angle_alpha                89.8034(16)
_cell_angle_beta                 87.7720(16)
_cell_angle_gamma                74.1423(16)
_cell_volume                     2032.23(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8402
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      76.4400
_cell_measurement_theta_min      5.7830
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.731
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0222
0 0 1 0.0528
0 0 -1 0.0285
0 0 1 0.0532
0 -1 -1 0.0494
0 1 1 0.0570
0 0 0 0.0417
0 0 0 0.0578
1 0 -1 0.0332
-1 0 1 0.0484
1 0 -1 0.0407
-1 0 1 0.0594
1 0 0 0.0408
-1 0 0 0.0604
1 1 0 0.0458
-1 -1 0 0.0701
1 0 1 0.0488
-1 0 -1 0.0608
1 1 1 0.0527
-1 -1 -1 0.0629

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol and dimethylsulfoxide'
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.075
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0010 -0.0033 -0.9997 0.0282 0.0654 0.0398
-0.0010 0.0033 0.9997 -0.0282 -0.0654 -0.0398
-0.0006 0.4960 -1.0033 -0.0104 0.0566 0.0808
0.0006 -0.4960 1.0033 0.0104 -0.0566 -0.0808
0.0026 -0.5025 -0.9961 0.0668 0.0743 -0.0012
-0.0026 0.5025 0.9961 -0.0668 -0.0743 0.0012
-0.0016 0.4993 -0.0036 -0.0386 -0.0089 0.0410
0.0016 -0.4993 0.0036 0.0386 0.0089 -0.0410
1.0030 -0.0294 -0.8078 0.1917 -0.0433 0.0883
-1.0030 0.0294 0.8078 -0.1917 0.0433 -0.0883
1.0014 0.4698 -0.8114 0.1531 -0.0521 0.1293
-1.0014 -0.4698 0.8114 -0.1531 0.0521 -0.1293
1.0004 0.4731 0.1883 0.1249 -0.1176 0.0895
-1.0004 -0.4731 -0.1883 -0.1249 0.1176 -0.0895
0.9989 0.9724 0.1847 0.0863 -0.1264 0.1305
-0.9989 -0.9724 -0.1847 -0.0863 0.1264 -0.1305
0.9995 0.4763 1.1881 0.0967 -0.1830 0.0497
-0.9995 -0.4763 -1.1881 -0.0967 0.1830 -0.0497
0.9979 0.9756 1.1845 0.0580 -0.1918 0.0907
-0.9979 -0.9756 -1.1845 -0.0580 0.1918 -0.0907

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12797
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.122
_diffrn_reflns_theta_max         67.122
_diffrn_reflns_theta_min         4.011
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00 -19.00   0.50    1.00    --  -48.95 125.00 -60.00   90
  2  ω   -103.00 -76.00   0.50    1.00    --  -48.95-125.00 120.00   54
  3  ω    -25.00  24.00   0.50    1.00    --  -48.95  37.00-120.00   98
  4  ω   -112.00 -74.00   0.50    1.00    --  -48.95-125.00  30.00   76
  5  ω    -58.00   6.00   0.50    1.00    --  -48.95  57.00 120.00  128
  6  ω   -119.00 -90.00   0.50    1.00    --  -48.95-125.00 -90.00   58
  7  ω   -119.00 -94.00   0.50    1.00    --  -48.95-125.00 -60.00   50
  8  ω      8.00  64.00   0.50    1.00    --   48.95 -57.00 -90.00  112
  9  ω    -22.00   4.00   0.50    1.00    --   48.95 -57.00 -90.00   52
 10  ω     67.00 123.00   0.50    4.00    --  107.75 -57.00-180.00  112
 11  ω    119.00 178.00   0.50    4.00    --  107.75  37.00-180.00  118
 12  ω     38.00 111.00   0.50    4.00    --  107.75 -77.00-180.00  146
 13  ω     84.00 112.00   0.50    4.00    --  107.75 -77.00 -30.00   56
 14  ω     42.00 120.00   0.50    4.00    --  107.75 -19.00   0.00  156
 15  ω     40.00  82.00   0.50    4.00    --  107.75-125.00 150.00   84
 16  ω    139.00 174.00   0.50    4.00    --  107.75  57.00 -60.00   70
 17  ω     44.00 104.00   0.50    4.00    --  107.75 -99.00-180.00  120
 18  ω     76.00 105.00   0.50    4.00    --  107.75 -99.00 -30.00   58
 19  ω    103.00 177.00   0.50    4.00    --  107.75  19.00 -30.00  148
 20  ω     37.00  72.00   0.50    4.00    --  107.75 -99.00 -30.00   70
 21  ω    101.00 177.00   0.50    4.00    --  107.75  19.00-120.00  152
 22  ω     96.00 134.00   0.50    4.00    --  107.75  57.00 -60.00   76
 23  ω     38.00 105.00   0.50    4.00    --  107.75 -99.00  60.00  134
 24  ω     69.00  94.00   0.50    4.00    --  107.75 -99.00  90.00   50
 25  ω     35.00  77.00   0.50    4.00    --  107.75 -77.00 -30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1665068000
_diffrn_orient_matrix_UB_12      -0.0770327000
_diffrn_orient_matrix_UB_13      -0.0278192000
_diffrn_orient_matrix_UB_21      -0.0964245000
_diffrn_orient_matrix_UB_22      -0.0185155000
_diffrn_orient_matrix_UB_23      -0.0654765000
_diffrn_orient_matrix_UB_31      0.0581663000
_diffrn_orient_matrix_UB_32      0.0820721000
_diffrn_orient_matrix_UB_33      -0.0400337000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11365
_reflns_number_total             12797
_reflns_special_details          
;
 _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       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         12797
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0440
_refine_ls_restrained_S_all      1.064
_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)+(0.0811P)²+0.7636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1203
_refine_special_details          
;The crystal was a non-merohedral twin modelled using two components in a 
refined ratio of 0.5773:0.4227(8).

For both of the complexes present in the asymmetric unit there was evidence 
of disorder of the ligand.  The central imine group was modelled in two 
positions in refined ratios of 0.785:0.215(7) and 0.893:0.107(8). 
The ADPs of disordered pairs of atoms were constrained to be equal 
(C8 & C8a, N1 & N1a, C27 & C27a, N2 & N2a).  Attempts to model the other 
atoms of the ligand in the minor position proved unsuccessful.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5773(8)
 0.4227(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C8A)
Uanis(N1A) = Uanis(N1)
Uanis(C27) = Uanis(C27A)
Uanis(N2) = Uanis(N2A)
4. Others
 Sof(C8A)=Sof(H8A)=Sof(N1A)=1-FVAR(1)
 Sof(C8)=Sof(H8)=Sof(N1)=FVAR(1)
 Sof(C27A)=Sof(H27A)=Sof(N2A)=1-FVAR(2)
 Sof(C27)=Sof(H27)=Sof(N2)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C8A(H8A), C11(H11), C12(H12), C14(H14),
 C22(H22), C23(H23), C26(H26), C27(H27), C27A(H27A), C30(H30), C31(H31),
 C33(H33)
5.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C)
;
_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
C1 C 1.1973(8) 0.0752(4) 0.4575(3) 0.0445(13) Uani 1 1 d . . . . .
C2 C 1.1473(7) 0.1679(4) 0.4168(3) 0.0393(11) Uani 1 1 d . . . . .
C3 C 1.0640(8) 0.1668(4) 0.3530(3) 0.0396(12) Uani 1 1 d . . . . .
H3 H 1.046890 0.106560 0.336264 0.048 Uiso 1 1 calc R U . . .
C4 C 1.0072(7) 0.2510(4) 0.3145(3) 0.0406(12) Uani 1 1 d . . . . .
H4 H 0.950142 0.249462 0.271496 0.049 Uiso 1 1 calc R U . . .
C5 C 1.0334(7) 0.3408(4) 0.3390(3) 0.0419(12) Uani 1 1 d . . . . .
C6 C 1.1207(7) 0.3417(4) 0.4022(3) 0.0392(12) Uani 1 1 d . . . . .
C7 C 1.1748(7) 0.2556(4) 0.4402(3) 0.0415(12) Uani 1 1 d . . . . .
H7 H 1.232002 0.256291 0.483321 0.050 Uiso 1 1 calc R U . . .
C8 C 1.1624(7) 0.4277(5) 0.4347(3) 0.0271(12) Uani 0.785(7) 1 d . . P A 1
H8 H 1.212058 0.420874 0.479999 0.033 Uiso 0.785(7) 1 calc R U P A 1
C8A C 1.183(3) 0.477(2) 0.4426(13) 0.0271(12) Uani 0.215(7) 1 d . . P A 2
H8A H 1.232631 0.435406 0.480205 0.033 Uiso 0.215(7) 1 calc R U P A 2
C9 C 1.1778(7) 0.5911(4) 0.4381(3) 0.0391(12) Uani 1 1 d . . . . .
C10 C 1.1260(7) 0.6757(4) 0.3970(3) 0.0372(11) Uani 1 1 d . . . . .
C11 C 1.1529(7) 0.7643(4) 0.4201(3) 0.0351(10) Uani 1 1 d . . . . .
H11 H 1.117236 0.822266 0.392277 0.042 Uiso 1 1 calc R U . . .
C12 C 1.2320(6) 0.7677(3) 0.4840(3) 0.0320(10) Uani 1 1 d . . . . .
H12 H 1.248574 0.828397 0.499999 0.038 Uiso 1 1 calc R U . . .
C13 C 1.2875(6) 0.6823(4) 0.5248(3) 0.0318(10) Uani 1 1 d . . . . .
C14 C 1.2587(7) 0.5941(4) 0.5015(3) 0.0377(11) Uani 1 1 d . . . . .
H14 H 1.294577 0.535919 0.529090 0.045 Uiso 1 1 calc R U . . .
C15 C 1.3737(6) 0.6831(4) 0.5933(3) 0.0345(10) Uani 1 1 d . . . . .
C16 C 1.3099(12) 0.0007(5) 0.5637(3) 0.065(2) Uani 1 1 d . . . . .
H16A H 1.397580 -0.052462 0.538651 0.098 Uiso 1 1 calc R U . . .
H16B H 1.204824 -0.020896 0.574292 0.098 Uiso 1 1 calc R U . . .
H16C H 1.356890 0.016533 0.607960 0.098 Uiso 1 1 calc R U . . .
C17 C 1.4523(7) 0.7820(5) 0.6793(3) 0.0455(13) Uani 1 1 d . . . . .
H17A H 1.571375 0.738110 0.679149 0.068 Uiso 1 1 calc R U . . .
H17B H 1.381531 0.762351 0.717275 0.068 Uiso 1 1 calc R U . . .
H17C H 1.455221 0.850438 0.687329 0.068 Uiso 1 1 calc R U . . .
C18 C 0.5083(6) 0.6156(4) 0.2978(3) 0.0365(11) Uani 1 1 d . . . . .
H18A H 0.581148 0.620909 0.255808 0.055 Uiso 1 1 calc R U . . .
H18B H 0.390844 0.659947 0.292980 0.055 Uiso 1 1 calc R U . . .
H18C H 0.501292 0.547208 0.302410 0.055 Uiso 1 1 calc R U . . .
C19 C 0.6151(7) 0.7692(4) 0.3481(3) 0.0381(11) Uani 1 1 d . . . . .
H19A H 0.680300 0.795032 0.382727 0.057 Uiso 1 1 calc R U . . .
H19B H 0.497167 0.813829 0.345607 0.057 Uiso 1 1 calc R U . . .
H19C H 0.675007 0.764506 0.301454 0.057 Uiso 1 1 calc R U . . .
Mo1 Mo 1.01890(4) 0.54900(3) 0.29384(2) 0.02481(12) Uani 1 1 d . . . . .
N1 N 1.1333(6) 0.5110(3) 0.4034(2) 0.0242(10) Uani 0.785(7) 1 d . . P A 1
N1A N 1.113(2) 0.4490(13) 0.3908(10) 0.0242(10) Uani 0.215(7) 1 d . . P A 2
O1 O 1.2186(4) 0.5073(3) 0.25264(17) 0.0343(7) Uani 1 1 d . . . . .
O2 O 0.8826(4) 0.6050(3) 0.22928(17) 0.0347(7) Uani 1 1 d . . . . .
O3 O 1.3774(5) 0.7747(3) 0.61223(18) 0.0383(8) Uani 1 1 d . . . . .
O4 O 1.4343(5) 0.6101(3) 0.6274(2) 0.0463(9) Uani 1 1 d . . . . .
O5 O 1.0510(5) 0.6721(3) 0.33492(19) 0.0421(8) Uani 1 1 d . . . . .
O6 O 0.9694(5) 0.4210(3) 0.3010(2) 0.0443(9) Uani 1 1 d . . . . .
O7 O 1.2665(7) 0.0877(3) 0.5195(2) 0.0532(11) Uani 1 1 d . . . . .
O8 O 1.1775(7) -0.0018(3) 0.4388(2) 0.0562(12) Uani 1 1 d . . . . .
O9 O 0.7900(4) 0.5850(2) 0.37554(16) 0.0293(7) Uani 1 1 d . . . . .
S1 S 0.60192(14) 0.64957(8) 0.37467(5) 0.0275(2) Uani 1 1 d . . . . .
C20 C -0.0457(6) 1.3683(4) 0.0214(2) 0.0322(10) Uani 1 1 d . . . . .
C21 C 0.0793(6) 1.2942(3) 0.0643(2) 0.0305(9) Uani 1 1 d . . . . .
C22 C 0.1338(6) 1.3262(4) 0.1268(2) 0.0320(10) Uani 1 1 d . . . . .
H22 H 0.088617 1.393180 0.141797 0.038 Uiso 1 1 calc R U . . .
C23 C 0.2537(6) 1.2607(4) 0.1670(2) 0.0326(10) Uani 1 1 d . . . . .
H23 H 0.293908 1.283318 0.208779 0.039 Uiso 1 1 calc R U . . .
C24 C 0.3161(6) 1.1615(4) 0.1467(3) 0.0344(10) Uani 1 1 d . . . . .
C25 C 0.2582(6) 1.1279(4) 0.0845(3) 0.0315(10) Uani 1 1 d . . . . .
C26 C 0.1421(6) 1.1962(4) 0.0435(3) 0.0321(10) Uani 1 1 d . . . . .
H26 H 0.105519 1.175066 0.000388 0.038 Uiso 1 1 calc R U . . .
C27 C 0.3114(7) 1.0269(5) 0.0574(3) 0.0271(12) Uani 0.893(8) 1 d . . P B 1
H27 H 0.275440 1.014224 0.011849 0.033 Uiso 0.893(8) 1 calc R U P B 1
C27A C 0.338(6) 0.973(4) 0.047(2) 0.0271(12) Uani 0.107(8) 1 d . . P B 2
H27A H 0.273544 0.996662 0.006770 0.033 Uiso 0.107(8) 1 calc R U P B 2
C28 C 0.4506(6) 0.8555(4) 0.0644(3) 0.0328(10) Uani 1 1 d . . . . .
C29 C 0.5625(6) 0.7891(4) 0.1074(2) 0.0318(10) Uani 1 1 d . . . . .
C30 C 0.6248(6) 0.6901(4) 0.0879(3) 0.0341(10) Uani 1 1 d . . . . .
H30 H 0.702533 0.644857 0.117200 0.041 Uiso 1 1 calc R U . . .
C31 C 0.5721(6) 0.6578(3) 0.0252(3) 0.0313(10) Uani 1 1 d . . . . .
H31 H 0.614650 0.590140 0.011548 0.038 Uiso 1 1 calc R U . . .
C32 C 0.4569(6) 0.7241(4) -0.0181(3) 0.0317(10) Uani 1 1 d . . . . .
C33 C 0.3967(6) 0.8231(4) 0.0014(3) 0.0331(10) Uani 1 1 d . . . . .
H33 H 0.319264 0.868655 -0.027795 0.040 Uiso 1 1 calc R U . . .
C34 C 0.3983(6) 0.6922(4) -0.0858(3) 0.0330(10) Uani 1 1 d . . . . .
C35 C -0.1794(7) 1.4027(4) -0.0880(3) 0.0418(12) Uani 1 1 d . . . . .
H35A H -0.134344 1.460631 -0.094264 0.063 Uiso 1 1 calc R U . . .
H35B H -0.297743 1.423472 -0.066497 0.063 Uiso 1 1 calc R U . . .
H35C H -0.182022 1.371643 -0.134145 0.063 Uiso 1 1 calc R U . . .
C36 C 0.4114(8) 0.5600(4) -0.1637(3) 0.0419(12) Uani 1 1 d . . . . .
H36A H 0.442887 0.595879 -0.204468 0.063 Uiso 1 1 calc R U . . .
H36B H 0.284610 0.570508 -0.160849 0.063 Uiso 1 1 calc R U . . .
H36C H 0.469235 0.489168 -0.169332 0.063 Uiso 1 1 calc R U . . .
C37 C 0.9368(7) 1.0533(4) 0.1973(3) 0.0355(10) Uani 1 1 d . . . . .
H37A H 0.883312 1.120819 0.181255 0.053 Uiso 1 1 calc R U . . .
H37B H 1.059564 1.045879 0.207055 0.053 Uiso 1 1 calc R U . . .
H37C H 0.875036 1.040471 0.240640 0.053 Uiso 1 1 calc R U . . .
C38 C 1.0107(7) 0.8532(4) 0.1759(3) 0.0432(12) Uani 1 1 d . . . . .
H38A H 0.946272 0.854185 0.221231 0.065 Uiso 1 1 calc R U . . .
H38B H 1.134194 0.845244 0.184421 0.065 Uiso 1 1 calc R U . . .
H38C H 0.999260 0.797795 0.146782 0.065 Uiso 1 1 calc R U . . .
Mo2 Mo 0.51422(4) 0.96005(3) 0.20159(2) 0.02659(12) Uani 1 1 d . . . . .
N2 N 0.4049(5) 0.9536(3) 0.0923(2) 0.0262(10) Uani 0.893(8) 1 d . . P B 1
N2A N 0.360(5) 1.026(3) 0.103(2) 0.0262(10) Uani 0.107(8) 1 d . . P B 2
O10 O 0.3309(5) 0.9431(3) 0.24263(18) 0.0383(8) Uani 1 1 d . . . . .
O11 O 0.6576(4) 0.9556(2) 0.26712(16) 0.0312(7) Uani 1 1 d . . . . .
O12 O -0.0677(5) 1.3326(3) -0.04229(18) 0.0369(7) Uani 1 1 d . . . . .
O13 O -0.1193(5) 1.4507(3) 0.0421(2) 0.0430(8) Uani 1 1 d . . . . .
O14 O 0.4327(5) 1.1013(3) 0.18708(19) 0.0394(8) Uani 1 1 d . . . . .
O15 O 0.6125(5) 0.8221(3) 0.16768(19) 0.0377(8) Uani 1 1 d . . . . .
O16 O 0.4663(5) 0.5962(3) -0.09963(18) 0.0371(7) Uani 1 1 d . . . . .
O17 O 0.2978(5) 0.7472(3) -0.1240(2) 0.0422(8) Uani 1 1 d . . . . .
O18 O 0.7291(4) 0.9785(3) 0.12116(16) 0.0322(7) Uani 1 1 d . . . . .
S2 S 0.92342(15) 0.96746(9) 0.13030(6) 0.0340(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.475(8) . ?
C1 O7 1.346(7) . ?
C1 O8 1.192(7) . ?
C2 C3 1.400(8) . ?
C2 C7 1.385(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.363(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.415(7) . ?
C5 C6 1.408(8) . ?
C5 O6 1.323(7) . ?
C6 C7 1.378(8) . ?
C6 C8 1.478(8) . ?
C6 N1A 1.506(18) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C8 N1 1.276(8) . ?
C8A H8A 0.9500 . ?
C8A C9 1.59(3) . ?
C8A N1A 1.26(3) . ?
C9 C10 1.391(8) . ?
C9 C14 1.388(8) . ?
C9 N1 1.436(6) . ?
C10 C11 1.392(7) . ?
C10 O5 1.344(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.389(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.399(7) . ?
C13 C14 1.395(7) . ?
C13 C15 1.490(7) . ?
C14 H14 0.9500 . ?
C15 O3 1.344(6) . ?
C15 O4 1.204(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 O7 1.446(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 O3 1.438(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 S1 1.782(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 S1 1.780(5) . ?
Mo1 N1 2.295(5) . ?
Mo1 N1A 2.324(18) . ?
Mo1 O1 1.697(3) . ?
Mo1 O2 1.708(3) . ?
Mo1 O5 1.980(4) . ?
Mo1 O6 1.946(4) . ?
Mo1 O9 2.291(3) . ?
O9 S1 1.526(3) . ?
C20 C21 1.492(7) . ?
C20 O12 1.340(6) . ?
C20 O13 1.204(6) . ?
C21 C22 1.390(7) . ?
C21 C26 1.382(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.395(7) . ?
C24 C25 1.407(7) . ?
C24 O14 1.335(6) . ?
C25 C26 1.394(7) . ?
C25 C27 1.453(8) . ?
C25 N2A 1.49(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C27 N2 1.290(7) . ?
C27A H27A 0.9500 . ?
C27A C28 1.69(5) . ?
C27A N2A 1.32(6) . ?
C28 C29 1.387(7) . ?
C28 C33 1.398(7) . ?
C28 N2 1.423(6) . ?
C29 C30 1.387(7) . ?
C29 O15 1.346(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.390(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.403(7) . ?
C32 C33 1.387(7) . ?
C32 C34 1.489(7) . ?
C33 H33 0.9500 . ?
C34 O16 1.330(6) . ?
C34 O17 1.209(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C35 O12 1.443(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C36 O16 1.443(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C37 S2 1.777(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C38 S2 1.796(6) . ?
Mo2 N2 2.283(4) . ?
Mo2 N2A 2.33(4) . ?
Mo2 O10 1.701(3) . ?
Mo2 O11 1.707(3) . ?
Mo2 O14 1.933(4) . ?
Mo2 O15 1.978(4) . ?
Mo2 O18 2.313(3) . ?
O18 S2 1.531(3) . ?

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
O7 C1 C2 112.1(5) . . ?
O8 C1 C2 124.6(5) . . ?
O8 C1 O7 123.3(5) . . ?
C3 C2 C1 118.0(4) . . ?
C7 C2 C1 122.6(5) . . ?
C7 C2 C3 119.3(5) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 120.9(5) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.8(5) . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 119.5(5) . . ?
O6 C5 C4 117.1(6) . . ?
O6 C5 C6 123.4(5) . . ?
C5 C6 C8 126.8(5) . . ?
C5 C6 N1A 90.1(8) . . ?
C7 C6 C5 119.3(5) . . ?
C7 C6 C8 113.9(5) . . ?
C7 C6 N1A 150.6(9) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 C2 121.2(5) . . ?
C6 C7 H7 119.4 . . ?
C6 C8 H8 119.2 . . ?
N1 C8 C6 121.5(5) . . ?
N1 C8 H8 119.2 . . ?
C9 C8A H8A 123.7 . . ?
N1A C8A H8A 123.7 . . ?
N1A C8A C9 112.7(19) . . ?
C10 C9 C8A 143.8(10) . . ?
C10 C9 N1 108.9(5) . . ?
C14 C9 C8A 95.8(10) . . ?
C14 C9 C10 120.3(4) . . ?
C14 C9 N1 130.7(5) . . ?
C9 C10 C11 119.8(5) . . ?
O5 C10 C9 120.2(4) . . ?
O5 C10 C11 120.0(5) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 119.9(5) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.5(4) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C15 121.9(4) . . ?
C14 C13 C12 119.2(5) . . ?
C14 C13 C15 118.9(5) . . ?
C9 C14 C13 120.2(5) . . ?
C9 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
O3 C15 C13 112.2(4) . . ?
O4 C15 C13 123.9(5) . . ?
O4 C15 O3 124.0(5) . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O7 C16 H16A 109.5 . . ?
O7 C16 H16B 109.5 . . ?
O7 C16 H16C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 C17 H17A 109.5 . . ?
O3 C17 H17B 109.5 . . ?
O3 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
S1 C18 H18A 109.5 . . ?
S1 C18 H18B 109.5 . . ?
S1 C18 H18C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
S1 C19 H19A 109.5 . . ?
S1 C19 H19B 109.5 . . ?
S1 C19 H19C 109.5 . . ?
O1 Mo1 N1 91.84(16) . . ?
O1 Mo1 N1A 90.7(4) . . ?
O1 Mo1 O2 105.37(16) . . ?
O1 Mo1 O5 97.91(16) . . ?
O1 Mo1 O6 96.54(16) . . ?
O1 Mo1 O9 164.34(14) . . ?
O2 Mo1 N1 160.80(17) . . ?
O2 Mo1 N1A 157.9(4) . . ?
O2 Mo1 O5 96.33(17) . . ?
O2 Mo1 O6 101.82(17) . . ?
O2 Mo1 O9 90.29(14) . . ?
O5 Mo1 N1 72.48(16) . . ?
O5 Mo1 N1A 96.3(5) . . ?
O5 Mo1 O9 80.50(13) . . ?
O6 Mo1 N1 84.23(17) . . ?
O6 Mo1 N1A 60.6(5) . . ?
O6 Mo1 O5 152.86(17) . . ?
O6 Mo1 O9 79.41(14) . . ?
O9 Mo1 N1 72.76(14) . . ?
O9 Mo1 N1A 74.1(4) . . ?
C8 N1 C9 118.4(5) . . ?
C8 N1 Mo1 127.1(4) . . ?
C9 N1 Mo1 114.5(4) . . ?
C6 N1A Mo1 129.4(11) . . ?
C8A N1A C6 107.6(18) . . ?
C8A N1A Mo1 122.7(17) . . ?
C15 O3 C17 115.4(4) . . ?
C10 O5 Mo1 123.6(3) . . ?
C5 O6 Mo1 133.6(4) . . ?
C1 O7 C16 114.8(4) . . ?
S1 O9 Mo1 133.94(18) . . ?
C19 S1 C18 99.2(3) . . ?
O9 S1 C18 107.2(2) . . ?
O9 S1 C19 105.8(2) . . ?
O12 C20 C21 112.5(4) . . ?
O13 C20 C21 123.4(4) . . ?
O13 C20 O12 124.1(5) . . ?
C22 C21 C20 118.1(4) . . ?
C26 C21 C20 122.0(4) . . ?
C26 C21 C22 119.9(4) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.0(5) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.4(5) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C25 120.0(4) . . ?
O14 C24 C23 118.1(5) . . ?
O14 C24 C25 122.0(5) . . ?
C24 C25 C27 125.7(5) . . ?
C24 C25 N2A 88.3(15) . . ?
C26 C25 C24 118.5(4) . . ?
C26 C25 C27 115.7(4) . . ?
C26 C25 N2A 153.0(15) . . ?
C21 C26 C25 121.2(5) . . ?
C21 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C25 C27 H27 118.4 . . ?
N2 C27 C25 123.2(5) . . ?
N2 C27 H27 118.4 . . ?
C28 C27A H27A 127.2 . . ?
N2A C27A H27A 127.2 . . ?
N2A C27A C28 106(3) . . ?
C29 C28 C27A 148.9(17) . . ?
C29 C28 C33 120.3(5) . . ?
C29 C28 N2 112.1(4) . . ?
C33 C28 C27A 90.7(17) . . ?
C33 C28 N2 127.5(5) . . ?
C28 C29 C30 120.5(4) . . ?
O15 C29 C28 119.2(4) . . ?
O15 C29 C30 120.4(5) . . ?
C29 C30 H30 120.3 . . ?
C29 C30 C31 119.3(5) . . ?
C31 C30 H30 120.3 . . ?
C30 C31 H31 119.7 . . ?
C30 C31 C32 120.6(5) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C34 122.1(4) . . ?
C33 C32 C31 119.6(5) . . ?
C33 C32 C34 118.3(4) . . ?
C28 C33 H33 120.2 . . ?
C32 C33 C28 119.6(5) . . ?
C32 C33 H33 120.2 . . ?
O16 C34 C32 113.0(4) . . ?
O17 C34 C32 123.8(5) . . ?
O17 C34 O16 123.2(5) . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O12 C35 H35A 109.5 . . ?
O12 C35 H35B 109.5 . . ?
O12 C35 H35C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O16 C36 H36A 109.5 . . ?
O16 C36 H36B 109.5 . . ?
O16 C36 H36C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
S2 C37 H37A 109.5 . . ?
S2 C37 H37B 109.5 . . ?
S2 C37 H37C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
S2 C38 H38A 109.5 . . ?
S2 C38 H38B 109.5 . . ?
S2 C38 H38C 109.5 . . ?
N2 Mo2 O18 74.31(13) . . ?
O10 Mo2 N2 91.77(15) . . ?
O10 Mo2 N2A 91.2(8) . . ?
O10 Mo2 O11 105.64(16) . . ?
O10 Mo2 O14 98.44(17) . . ?
O10 Mo2 O15 96.89(17) . . ?
O10 Mo2 O18 166.06(14) . . ?
O11 Mo2 N2 161.35(15) . . ?
O11 Mo2 N2A 155.4(9) . . ?
O11 Mo2 O14 100.68(16) . . ?
O11 Mo2 O15 96.67(15) . . ?
O11 Mo2 O18 88.11(13) . . ?
O14 Mo2 N2 82.91(15) . . ?
O14 Mo2 N2A 58.3(10) . . ?
O14 Mo2 O15 152.76(15) . . ?
O14 Mo2 O18 80.87(14) . . ?
O15 Mo2 N2 74.22(15) . . ?
O15 Mo2 N2A 99.1(10) . . ?
O15 Mo2 O18 78.86(13) . . ?
O18 Mo2 N2A 76.5(8) . . ?
C27 N2 C28 121.2(4) . . ?
C27 N2 Mo2 126.8(4) . . ?
C28 N2 Mo2 111.9(3) . . ?
C25 N2A Mo2 133(2) . . ?
C27A N2A C25 103(3) . . ?
C27A N2A Mo2 125(3) . . ?
C20 O12 C35 115.1(4) . . ?
C24 O14 Mo2 136.1(3) . . ?
C29 O15 Mo2 122.0(3) . . ?
C34 O16 C36 115.8(4) . . ?
S2 O18 Mo2 130.72(18) . . ?
C37 S2 C38 100.0(3) . . ?
O18 S2 C37 106.7(2) . . ?
O18 S2 C38 107.4(2) . . ?

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
C1 C2 C3 C4 176.9(5) . . . . ?
C1 C2 C7 C6 -177.5(5) . . . . ?
C2 C1 O7 C16 177.0(6) . . . . ?
C2 C3 C4 C5 0.4(8) . . . . ?
C3 C2 C7 C6 0.4(8) . . . . ?
C3 C4 C5 C6 1.1(7) . . . . ?
C3 C4 C5 O6 -177.4(5) . . . . ?
C4 C5 C6 C7 -1.8(7) . . . . ?
C4 C5 C6 C8 178.7(5) . . . . ?
C4 C5 C6 N1A 175.6(8) . . . . ?
C4 C5 O6 Mo1 -160.0(4) . . . . ?
C5 C6 C7 C2 1.0(8) . . . . ?
C5 C6 C8 N1 -6.0(8) . . . . ?
C5 C6 N1A C8A 178.7(14) . . . . ?
C5 C6 N1A Mo1 -6.6(11) . . . . ?
C6 C5 O6 Mo1 21.6(7) . . . . ?
C6 C8 N1 C9 -179.8(5) . . . . ?
C6 C8 N1 Mo1 -0.9(8) . . . . ?
C7 C2 C3 C4 -1.2(8) . . . . ?
C7 C6 C8 N1 174.5(5) . . . . ?
C7 C6 N1A C8A -6(3) . . . . ?
C7 C6 N1A Mo1 168.8(8) . . . . ?
C8 C6 C7 C2 -179.4(5) . . . . ?
C8A C9 C10 C11 179.0(14) . . . . ?
C8A C9 C10 O5 -1.4(16) . . . . ?
C8A C9 C14 C13 -179.5(9) . . . . ?
C9 C8A N1A C6 -178.2(12) . . . . ?
C9 C8A N1A Mo1 7(2) . . . . ?
C9 C10 C11 C12 0.2(7) . . . . ?
C9 C10 O5 Mo1 -3.4(6) . . . . ?
C10 C9 C14 C13 0.5(7) . . . . ?
C10 C9 N1 C8 -176.5(5) . . . . ?
C10 C9 N1 Mo1 4.6(5) . . . . ?
C10 C11 C12 C13 1.0(7) . . . . ?
C11 C10 O5 Mo1 176.2(3) . . . . ?
C11 C12 C13 C14 -1.5(7) . . . . ?
C11 C12 C13 C15 179.6(4) . . . . ?
C12 C13 C14 C9 0.7(7) . . . . ?
C12 C13 C15 O3 4.9(6) . . . . ?
C12 C13 C15 O4 -174.4(5) . . . . ?
C13 C15 O3 C17 177.6(4) . . . . ?
C14 C9 C10 C11 -1.0(7) . . . . ?
C14 C9 C10 O5 178.6(4) . . . . ?
C14 C9 N1 C8 3.6(8) . . . . ?
C14 C9 N1 Mo1 -175.4(4) . . . . ?
C14 C13 C15 O3 -174.0(4) . . . . ?
C14 C13 C15 O4 6.7(7) . . . . ?
C15 C13 C14 C9 179.6(4) . . . . ?
Mo1 O9 S1 C18 51.0(3) . . . . ?
Mo1 O9 S1 C19 -54.1(3) . . . . ?
N1 C9 C10 C11 179.1(4) . . . . ?
N1 C9 C10 O5 -1.3(6) . . . . ?
N1 C9 C14 C13 -179.6(5) . . . . ?
N1A C6 C7 C2 -173.7(15) . . . . ?
N1A C8A C9 C10 -1(3) . . . . ?
N1A C8A C9 C14 178.9(16) . . . . ?
O4 C15 O3 C17 -3.1(7) . . . . ?
O5 C10 C11 C12 -179.4(4) . . . . ?
O6 C5 C6 C7 176.6(5) . . . . ?
O6 C5 C6 C8 -2.9(8) . . . . ?
O6 C5 C6 N1A -6.0(8) . . . . ?
O7 C1 C2 C3 -176.3(5) . . . . ?
O7 C1 C2 C7 1.7(8) . . . . ?
O8 C1 C2 C3 2.9(9) . . . . ?
O8 C1 C2 C7 -179.1(6) . . . . ?
O8 C1 O7 C16 -2.2(9) . . . . ?
C20 C21 C22 C23 -178.0(4) . . . . ?
C20 C21 C26 C25 -179.7(4) . . . . ?
C21 C20 O12 C35 -176.5(4) . . . . ?
C21 C22 C23 C24 -2.3(7) . . . . ?
C22 C21 C26 C25 0.8(7) . . . . ?
C22 C23 C24 C25 0.7(7) . . . . ?
C22 C23 C24 O14 179.5(4) . . . . ?
C23 C24 C25 C26 1.6(7) . . . . ?
C23 C24 C25 C27 -179.6(4) . . . . ?
C23 C24 C25 N2A -175.3(14) . . . . ?
C23 C24 O14 Mo2 159.6(4) . . . . ?
C24 C25 C26 C21 -2.4(7) . . . . ?
C24 C25 C27 N2 7.8(8) . . . . ?
C24 C25 N2A C27A -176(3) . . . . ?
C24 C25 N2A Mo2 6(2) . . . . ?
C25 C24 O14 Mo2 -21.6(7) . . . . ?
C25 C27 N2 C28 178.6(4) . . . . ?
C25 C27 N2 Mo2 -0.9(7) . . . . ?
C26 C21 C22 C23 1.5(7) . . . . ?
C26 C25 C27 N2 -173.4(4) . . . . ?
C26 C25 N2A C27A 10(5) . . . . ?
C26 C25 N2A Mo2 -167.9(10) . . . . ?
C27 C25 C26 C21 178.7(4) . . . . ?
C27A C28 C29 C30 -175(3) . . . . ?
C27A C28 C29 O15 4(3) . . . . ?
C27A C28 C33 C32 177.3(15) . . . . ?
C28 C27A N2A C25 180(2) . . . . ?
C28 C27A N2A Mo2 -2(4) . . . . ?
C28 C29 C30 C31 -0.8(7) . . . . ?
C28 C29 O15 Mo2 5.9(6) . . . . ?
C29 C28 C33 C32 -0.5(7) . . . . ?
C29 C28 N2 C27 175.3(4) . . . . ?
C29 C28 N2 Mo2 -5.2(5) . . . . ?
C29 C30 C31 C32 -0.2(7) . . . . ?
C30 C29 O15 Mo2 -175.3(3) . . . . ?
C30 C31 C32 C33 0.8(7) . . . . ?
C30 C31 C32 C34 179.8(4) . . . . ?
C31 C32 C33 C28 -0.5(7) . . . . ?
C31 C32 C34 O16 0.0(6) . . . . ?
C31 C32 C34 O17 179.3(5) . . . . ?
C32 C34 O16 C36 178.6(4) . . . . ?
C33 C28 C29 C30 1.1(7) . . . . ?
C33 C28 C29 O15 180.0(4) . . . . ?
C33 C28 N2 C27 -4.3(7) . . . . ?
C33 C28 N2 Mo2 175.3(4) . . . . ?
C33 C32 C34 O16 179.0(4) . . . . ?
C33 C32 C34 O17 -1.8(7) . . . . ?
C34 C32 C33 C28 -179.4(4) . . . . ?
Mo2 O18 S2 C37 -58.7(3) . . . . ?
Mo2 O18 S2 C38 47.8(3) . . . . ?
N2 C28 C29 C30 -178.5(4) . . . . ?
N2 C28 C29 O15 0.4(6) . . . . ?
N2 C28 C33 C32 179.0(4) . . . . ?
N2A C25 C26 C21 171(3) . . . . ?
N2A C27A C28 C29 -6(5) . . . . ?
N2A C27A C28 C33 178(3) . . . . ?
O12 C20 C21 C22 170.5(4) . . . . ?
O12 C20 C21 C26 -9.0(6) . . . . ?
O13 C20 C21 C22 -10.1(7) . . . . ?
O13 C20 C21 C26 170.4(5) . . . . ?
O13 C20 O12 C35 4.0(7) . . . . ?
O14 C24 C25 C26 -177.2(4) . . . . ?
O14 C24 C25 C27 1.6(7) . . . . ?
O14 C24 C25 N2A 5.9(14) . . . . ?
O15 C29 C30 C31 -179.6(4) . . . . ?
O17 C34 O16 C36 -0.7(7) . . . . ?

_olex2_date_sample_data_collection 2022-11-01
_olex2_date_sample_submission    2022-10-31
_olex2_exptl_crystal_mounting_method 'oil on 75 micrometre micromount'
_olex2_submission_original_sample_id LG-1-006
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.350
_oxdiff_exptl_absorpt_empirical_full_min 0.812
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5773(8) 9635 6258 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4227(8) 9528 6258 nmt 0.9989 0.0031 0.0010 0.9731 -0.9986 -0.0032 0.1852
0.0068 -0.9998

_twin_special_details            
;
Component 2 rotated by 179.7333° 
around [0.90 0.44 0.08] (reciprocal) or [1.00 0.00 0.00] (direct)
;
####################################################################### 
# 
# 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_akdk22013
_database_code_depnum_ccdc_archive 'CCDC 2312692'
loop_
_audit_author_name
_audit_author_address
'Adrian Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2023-12-07 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_audit_creation_date             2022-11-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H15 Mo N O5 S, C2 H6 O S'
_chemical_formula_sum            'C17 H21 Mo N O6 S2'
_chemical_formula_weight         495.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C17 H21 Mo1 N1 O6 S2'
_chemical_oxdiff_usercomment     'Lukas Geciauskas LG-1-016'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.51400(14)
_cell_length_b                   6.72111(8)
_cell_length_c                   23.5861(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.9945(11)
_cell_angle_gamma                90
_cell_volume                     1978.96(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7746
_cell_measurement_temperature    109.95(10)
_cell_measurement_theta_max      76.4600
_cell_measurement_theta_min      3.5510
_shelx_estimated_absorpt_T_max   0.780
_shelx_estimated_absorpt_T_min   0.471
_exptl_absorpt_coefficient_mu    7.697
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 1 0.0535
1 -1 1 0.0458
-1 1 -1 0.0458
1 0 -1 0.0281
-1 0 1 0.0281
1 0 1 0.0258
1 0 0 0.0240
-1 0 0 0.0300
1 1 1 0.0503
-1 -1 -1 0.0540
1 -1 -1 0.0497
0 1 1 0.0517
0 0 -1 0.0171
0 0 1 0.0171

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethylether and dimethylsulfoxide'
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.034
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 -1.0000 1.0001 0.0591 0.2210 0.0669
1.0000 -1.0000 1.0001 0.0731 0.1845 0.1840
-1.0000 1.0000 -1.0001 -0.0731 -0.1845 -0.1840
1.0000 -0.0000 -1.0000 -0.0514 -0.0391 0.1193
-1.0000 0.0000 1.0000 0.0514 0.0391 -0.1193
1.0000 0.0000 1.0000 0.0793 -0.0340 0.1149
1.0000 0.0000 -0.0000 0.0140 -0.0365 0.1171
-1.0000 -0.0000 0.0000 -0.0140 0.0365 -0.1171
1.0000 1.0000 0.9998 0.0856 -0.2525 0.0458
-1.0000 -1.0000 -0.9998 -0.0856 0.2525 -0.0458
1.0000 -1.0000 -0.9998 -0.0576 0.1794 0.1884
0.0000 1.0000 0.9998 0.0716 -0.2159 -0.0713
0.0000 -0.0000 -1.0000 -0.0654 -0.0025 0.0022
-0.0000 0.0000 1.0000 0.0654 0.0025 -0.0022

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            12118
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         3.541
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109.95(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -81.00  18.00   0.50    2.50    --  -48.70 101.00 -36.00  198
  2  ω     10.00  36.00   0.50    2.50    --   48.70-101.00-140.00   52
  3  ω     71.00  96.00   0.50   10.00    --  107.75-101.00-140.00   50
  4  ω    116.00 177.00   0.50   10.00    --  107.75 101.00 -36.00  122
  5  ω   -120.00 -37.00   0.50    2.50    --  -48.70 -57.00-150.00  166
  6  ω   -117.00 -74.00   0.50    2.50    --  -48.70-125.00   0.00   86
  7  ω   -117.00 -82.00   0.50    2.50    --  -48.70-125.00  90.00   70
  8  ω   -118.00 -93.00   0.50    2.50    --  -48.70-125.00  30.00   50
  9  ω     45.00  80.00   0.50   10.00    --  107.75 -99.00  30.00   70
 10  ω     85.00 162.00   0.50   10.00    --  107.75  77.00 120.00  154
 11  ω     57.00 113.00   0.50   10.00    --  107.75 -37.00-180.00  112
 12  ω     65.00  91.00   0.50   10.00    --  107.75 -99.00 120.00   52
 13  ω     57.00  82.00   0.50   10.00    --  107.75 -99.00 -30.00   50
 14  ω    104.00 177.00   0.50   10.00    --  107.75  37.00-120.00  146
 15  ω     41.00 102.00   0.50   10.00    --  107.75 -99.00 -60.00  122
 16  ω     33.00  96.00   0.50   10.00    --  107.75 -19.00 -60.00  126
 17  ω     41.00 100.00   0.50   10.00    --  107.75 -99.00-180.00  118
 18  ω     52.00 121.00   0.50   10.00    --  107.75 -57.00   0.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0139554000
_diffrn_orient_matrix_UB_12      0.0062449000
_diffrn_orient_matrix_UB_13      0.0653639000
_diffrn_orient_matrix_UB_21      -0.0365375000
_diffrn_orient_matrix_UB_22      -0.2184885000
_diffrn_orient_matrix_UB_23      0.0025471000
_diffrn_orient_matrix_UB_31      0.1170791000
_diffrn_orient_matrix_UB_32      -0.0691128000
_diffrn_orient_matrix_UB_33      -0.0021839000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3216
_reflns_number_total             3512
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         3512
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0258
_refine_ls_restrained_S_all      1.032
_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)+(0.0309P)²+1.4631P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0658
_refine_special_details          
;
The structure exhibited considerable disorder.  
Within the complex all atoms except for the oxo oxygens were disordered
and modelled in two positions with refined occupancies of 0.5697:0.4303(19).
Pairs of overlapping C-C bond lengths within the aromatic rings were restrained
to be equal (e.g.C1-C6 and C8A-C13A).  The ADP of disordered pairs of atoms
were constrained to be equal (e.g. O3 & O4a, C1 & C13a etc).  The ADPs of 
C1, C6, C8, C13, C1a, C8a & C13a were constrained to be approximately isotropic.

The DMSO of crystallisation was also disordered and modelled in two sites with 
refined occupancies of 0.9220:0.0780(18).  Within this the bond lengths of 
like bonds were restrained to be equal (e.g. S2-C16, S2-C17, S2a-C16a & S2a-C17a)
as were the 1-3 distances (e.g. C16-O6, C17-O6, C16a-O6a, C17a-O6a).
The ADPS of pairs of atoms were restrained to be equal (e.g. C16 & C16a).
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C16-C17 \\sim C16A-C17A
 with sigma of 0.02
 C1-C6 \\sim C13A-C8A
 with sigma of 0.02
 C1-C2 \\sim C13A-C12A
 with sigma of 0.02
 C16A-O6A \\sim O6A-C17A \\sim C17-O6 \\sim O6-C16
 with sigma of 0.02
 C1-C3 \\sim C13A-C11A
 with sigma of 0.04
 S2A-O6A \\sim S2-O6
 with sigma of 0.02
 S2-C16 \\sim S2A-C16A \\sim S2-C17 \\sim S2A-C17A
 with sigma of 0.02
 C1-C5 \\sim C13A-C9A
 with sigma of 0.04
 C1-C7 \\sim C13A-C7
 with sigma of 0.04
 C1-N1A \\sim C13A-N1A
 with sigma of 0.04
 O4A-C13A \\sim O3-C1
 with sigma of 0.02
 C6-C2 \\sim C8A-C12A
 with sigma of 0.04
 C6-C7 \\sim C8A-C7
 with sigma of 0.02
 C6-N1A \\sim C8A-N1A
 with sigma of 0.02
 C6A-C5A \\sim C9-C8
 with sigma of 0.02
 C6-C5 \\sim C8A-C9A
 with sigma of 0.02
 C6-C4 \\sim C8A-C10A
 with sigma of 0.04
 C8-C13 \\sim C1A-C6A
 with sigma of 0.02
 C2A-C1A \\sim C12-C13
 with sigma of 0.02
 C4A-C3A \\sim C10-C11
 with sigma of 0.02
 C11-C12 \\sim C2A-C3A
 with sigma of 0.02
 C4A-C5A \\sim C10-C9
 with sigma of 0.02
 C5-C7 \\sim C9A-C7
 with sigma of 0.04
 C2-C3 \\sim C12A-C11A
 with sigma of 0.02
 C4-C5 \\sim C10A-C9A
 with sigma of 0.02
 C2-C4 \\sim C12A-C10A
 with sigma of 0.04
 C3-C5 \\sim C11A-C9A
 with sigma of 0.04
 C5-N1A \\sim C9A-N1A
 with sigma of 0.04
 C3-C4 \\sim C11A-C10A
 with sigma of 0.02
 Mo4-O4A \\sim Mo1-O3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C8)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C6) \\sim Ueq, Uanis(C8A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C13A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C16A) = Uanis(C16)
Uanis(O3) = Uanis(O4A)
Uanis(O6) = Uanis(O6A)
Uanis(S2A) = Uanis(S2)
Uanis(C13A) = Uanis(C1)
Uanis(C1) = Uanis(C13A)
Uanis(N1) = Uanis(N1A)
Uanis(C6A) = Uanis(C8)
Uanis(C8A) = Uanis(C6)
Uanis(C7A) = Uanis(C7)
Uanis(C12) = Uanis(C2A)
Uanis(C13) = Uanis(C1A)
Uanis(C4A) = Uanis(C10)
Uanis(C3A) = Uanis(C11)
Uanis(C5A) = Uanis(C9)
Uanis(C9A) = Uanis(C5)
Uanis(C12A) = Uanis(C2)
Uanis(C10A) = Uanis(C4)
Uanis(C11A) = Uanis(C3)
4. Others
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=
 Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(N1A)=Sof(O3A)=Sof(O4A)=
 Sof(O5A)=Sof(S1A)=Sof(Mo4)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=
 Sof(C6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=
 Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=Sof(Mo1)=Sof(N1)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(S1)=FVAR(1)
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(O6A)=Sof(S2A)=1-FVAR(2)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(O6)=Sof(S2)=FVAR(2)
5.a Riding coordinates:
 C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C2A(H2A), C3(H3), C3A(H3A), C4(H4), C4A(H4A), C5(H5), C5A(H5A),
 C7(H7), C7A(H7A), C9(H9), C9A(H9A), C10(H10), C10A(H10A), C11(H11), C11A(H11A),
  C12(H12), C12A(H12A)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14(H14D,H14E,H14F), C15(H15A,H15B,H15C), C15(H15D,H15E,
 H15F), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_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
C1 C 0.2338(15) 0.3673(15) 0.1787(4) 0.0264(17) Uani 0.5697(19) 1 d D U P A 1
C1A C 0.1465(15) 0.362(3) 0.3745(7) 0.0263(18) Uani 0.4303(19) 1 d D U P A 2
C2 C 0.263(2) 0.389(3) 0.1224(5) 0.0274(17) Uani 0.5697(19) 1 d D . P A 1
H2 H 0.300248 0.505692 0.112047 0.033 Uiso 0.5697(19) 1 calc R U P A 1
C2A C 0.1197(10) 0.380(3) 0.4300(7) 0.0298(16) Uani 0.4303(19) 1 d D . P A 2
H2A H 0.155758 0.478681 0.452898 0.036 Uiso 0.4303(19) 1 calc R U P A 2
C3 C 0.2388(18) 0.2431(18) 0.0815(6) 0.0317(19) Uani 0.5697(19) 1 d D . P A 1
H3 H 0.259455 0.262578 0.043878 0.038 Uiso 0.5697(19) 1 calc R U P A 1
C3A C 0.043(3) 0.263(4) 0.4553(12) 0.038(2) Uani 0.4303(19) 1 d D . P A 2
H3A H 0.021845 0.293646 0.492104 0.046 Uiso 0.4303(19) 1 calc R U P A 2
C4 C 0.1846(11) 0.0682(17) 0.0945(3) 0.0339(16) Uani 0.5697(19) 1 d D . P A 1
H4 H 0.170471 -0.032324 0.066681 0.041 Uiso 0.5697(19) 1 calc R U P A 1
C4A C 0.0003(12) 0.103(2) 0.4251(6) 0.0319(16) Uani 0.4303(19) 1 d D . P A 2
H4A H -0.049701 0.017854 0.441674 0.038 Uiso 0.4303(19) 1 calc R U P A 2
C5 C 0.1526(9) 0.0462(15) 0.1484(3) 0.0292(17) Uani 0.5697(19) 1 d D . P A 1
H5 H 0.112461 -0.067900 0.157548 0.035 Uiso 0.5697(19) 1 calc R U P A 1
C5A C 0.0300(10) 0.066(2) 0.3710(6) 0.0273(14) Uani 0.4303(19) 1 d D . P A 2
H5A H 0.003530 -0.047969 0.350832 0.033 Uiso 0.4303(19) 1 calc R U P A 2
C6 C 0.1781(12) 0.1901(12) 0.1904(5) 0.0255(17) Uani 0.5697(19) 1 d D U P A 1
C6A C 0.0986(18) 0.196(2) 0.3461(9) 0.0232(17) Uani 0.4303(19) 1 d D U P A 2
C7 C 0.1402(3) 0.1569(6) 0.24692(19) 0.0245(7) Uani 0.5697(19) 1 d . . P A 1
H7 H 0.105365 0.034709 0.253891 0.029 Uiso 0.5697(19) 1 calc R U P A 1
C7A C 0.1212(4) 0.1601(9) 0.2868(3) 0.0245(7) Uani 0.4303(19) 1 d . . P A 2
H7A H 0.099363 0.035534 0.270845 0.029 Uiso 0.4303(19) 1 calc R U P A 2
C8 C 0.1100(13) 0.2427(16) 0.3399(6) 0.0232(17) Uani 0.5697(19) 1 d D U P A 1
C8A C 0.1821(17) 0.2438(19) 0.1970(7) 0.0255(17) Uani 0.4303(19) 1 d D U P A 2
C9 C 0.0523(7) 0.0767(17) 0.3560(4) 0.0273(14) Uani 0.5697(19) 1 d D . P A 1
H9 H 0.037430 -0.028122 0.329647 0.033 Uiso 0.5697(19) 1 calc R U P A 1
C9A C 0.1572(13) 0.067(2) 0.1674(4) 0.0292(17) Uani 0.4303(19) 1 d D . P A 2
H9A H 0.124740 -0.040100 0.186323 0.035 Uiso 0.4303(19) 1 calc R U P A 2
C10 C 0.0165(8) 0.0634(16) 0.4100(4) 0.0319(16) Uani 0.5697(19) 1 d D . P A 1
H10 H -0.022312 -0.050756 0.420551 0.038 Uiso 0.5697(19) 1 calc R U P A 1
C10A C 0.1793(16) 0.045(2) 0.1111(5) 0.0339(16) Uani 0.4303(19) 1 d D . P A 2
H10A H 0.158006 -0.073416 0.091549 0.041 Uiso 0.4303(19) 1 calc R U P A 2
C11 C 0.037(2) 0.217(3) 0.4493(9) 0.038(2) Uani 0.5697(19) 1 d D . P A 1
H11 H 0.014411 0.201480 0.486651 0.046 Uiso 0.5697(19) 1 calc R U P A 1
C11A C 0.231(2) 0.191(3) 0.0824(8) 0.0317(19) Uani 0.4303(19) 1 d D . P A 2
H11A H 0.247481 0.171340 0.044033 0.038 Uiso 0.4303(19) 1 calc R U P A 2
C12 C 0.0895(6) 0.392(2) 0.4356(5) 0.0298(16) Uani 0.5697(19) 1 d D . P A 1
H12 H 0.099614 0.500219 0.461403 0.036 Uiso 0.5697(19) 1 calc R U P A 1
C12A C 0.260(3) 0.368(3) 0.1102(8) 0.0274(17) Uani 0.4303(19) 1 d D . P A 2
H12A H 0.295529 0.471029 0.091449 0.033 Uiso 0.4303(19) 1 calc R U P A 2
C13 C 0.1258(10) 0.395(2) 0.3811(5) 0.0263(18) Uani 0.5697(19) 1 d D U P A 1
C13A C 0.235(2) 0.389(2) 0.1660(6) 0.0264(17) Uani 0.4303(19) 1 d D U P A 2
C14 C 0.4803(3) 0.1136(5) 0.33255(17) 0.0601(9) Uani 1 1 d . . . . .
H14A H 0.426688 0.012356 0.321137 0.090 Uiso 0.5697(19) 1 calc R U P A 1
H14B H 0.477806 0.141333 0.373235 0.090 Uiso 0.5697(19) 1 calc R U P A 1
H14C H 0.551711 0.064928 0.324980 0.090 Uiso 0.5697(19) 1 calc R U P A 1
H14D H 0.524888 0.096857 0.300350 0.090 Uiso 0.4303(19) 1 calc R U P A 2
H14E H 0.415138 0.033365 0.326328 0.090 Uiso 0.4303(19) 1 calc R U P A 2
H14F H 0.520315 0.070186 0.367561 0.090 Uiso 0.4303(19) 1 calc R U P A 2
C15 C 0.5720(2) 0.4615(6) 0.32121(18) 0.0599(9) Uani 1 1 d . . . . .
H15A H 0.576205 0.596112 0.305528 0.090 Uiso 0.5697(19) 1 calc R U P A 1
H15B H 0.634515 0.384444 0.311302 0.090 Uiso 0.5697(19) 1 calc R U P A 1
H15C H 0.570812 0.469135 0.362655 0.090 Uiso 0.5697(19) 1 calc R U P A 1
H15D H 0.624298 0.443505 0.353706 0.090 Uiso 0.4303(19) 1 calc R U P A 2
H15E H 0.565892 0.603349 0.311881 0.090 Uiso 0.4303(19) 1 calc R U P A 2
H15F H 0.595717 0.388456 0.288393 0.090 Uiso 0.4303(19) 1 calc R U P A 2
Mo1 Mo 0.2136(2) 0.6047(4) 0.28628(9) 0.0194(3) Uani 0.5697(19) 1 d D . P A 1
N1 N 0.1513(3) 0.2820(6) 0.28712(16) 0.0229(6) Uani 0.5697(19) 1 d . . P A 1
N1A N 0.1684(4) 0.2830(8) 0.2537(2) 0.0229(6) Uani 0.4303(19) 1 d . . P A 2
O1 O 0.09322(13) 0.6788(2) 0.26239(8) 0.0305(4) Uani 1 1 d . . . . .
O2 O 0.29209(17) 0.8089(3) 0.29434(9) 0.0507(5) Uani 1 1 d . . . . .
O3 O 0.2675(4) 0.5156(9) 0.21513(16) 0.0318(9) Uani 0.5697(19) 1 d D . P A 1
O3A O 0.2158(4) 0.4969(9) 0.3532(2) 0.0329(12) Uani 0.4303(19) 1 d . . P A 2
O4 O 0.1798(3) 0.5537(7) 0.36498(17) 0.0312(9) Uani 0.5697(19) 1 d . . P A 1
O4A O 0.2541(6) 0.5517(13) 0.1965(2) 0.0318(9) Uani 0.4303(19) 1 d D . P A 2
O5 O 0.3606(2) 0.4331(5) 0.32269(14) 0.0351(8) Uani 0.5697(19) 1 d . . P A 1
O5A O 0.3777(3) 0.4049(7) 0.28274(19) 0.0344(10) Uani 0.4303(19) 1 d . . P A 2
S1 S 0.45158(8) 0.34189(16) 0.29207(4) 0.0271(3) Uani 0.5697(19) 1 d . . P A 1
S1A S 0.44478(11) 0.3692(3) 0.33878(6) 0.0373(5) Uani 0.4303(19) 1 d . . P A 2
C16 C 0.2892(5) 0.9308(9) 0.4553(2) 0.0866(17) Uani 0.9220(18) 1 d D . P B 1
H16A H 0.267574 0.906851 0.415140 0.130 Uiso 0.9220(18) 1 calc R U P B 1
H16B H 0.337931 1.045039 0.458562 0.130 Uiso 0.9220(18) 1 calc R U P B 1
H16C H 0.225645 0.958636 0.475988 0.130 Uiso 0.9220(18) 1 calc R U P B 1
C16A C 0.304(4) 0.921(7) 0.450(3) 0.0866(17) Uani 0.0780(18) 1 d D . P B 2
H16D H 0.280992 0.985283 0.484081 0.130 Uiso 0.0780(18) 1 d R U P B 2
H16E H 0.247132 0.834983 0.433351 0.130 Uiso 0.0780(18) 1 d R U P B 2
H16F H 0.320552 1.023763 0.421961 0.130 Uiso 0.0780(18) 1 d R U P B 2
C17 C 0.4613(4) 0.7176(8) 0.43850(15) 0.0794(16) Uani 0.9220(18) 1 d D . P B 1
H17A H 0.509315 0.604979 0.447425 0.119 Uiso 0.9220(18) 1 calc R U P B 1
H17B H 0.501549 0.842282 0.443384 0.119 Uiso 0.9220(18) 1 calc R U P B 1
H17C H 0.431530 0.706798 0.399086 0.119 Uiso 0.9220(18) 1 calc R U P B 1
C17A C 0.355(3) 0.544(4) 0.4657(16) 0.053(10) Uani 0.0780(18) 1 d D U P B 2
H17D H 0.408957 0.440751 0.460918 0.079 Uiso 0.0780(18) 1 d R U P B 2
H17E H 0.300607 0.538841 0.433788 0.079 Uiso 0.0780(18) 1 d R U P B 2
H17F H 0.321097 0.521661 0.501358 0.079 Uiso 0.0780(18) 1 d R U P B 2
O6 O 0.40327(19) 0.7740(4) 0.54230(9) 0.0472(6) Uani 0.9220(18) 1 d D . P B 1
O6A O 0.450(2) 0.819(4) 0.5301(8) 0.0472(6) Uani 0.0780(18) 1 d D . P B 2
S2 S 0.35580(7) 0.71549(15) 0.48480(3) 0.0503(2) Uani 0.9220(18) 1 d D . P B 1
S2A S 0.4225(9) 0.7790(17) 0.4676(4) 0.0503(2) Uani 0.0780(18) 1 d D . P B 2
Mo4 Mo 0.2251(3) 0.5878(6) 0.27575(13) 0.0228(4) Uani 0.4303(19) 1 d D . 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
C1 C2 1.412(9) . ?
C1 C6 1.417(8) . ?
C1 O3 1.363(8) . ?
C1A C2A 1.380(12) . ?
C1A C6A 1.415(13) . ?
C1A O3A 1.37(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.395(9) . ?
C2A H2A 0.9500 . ?
C2A C3A 1.399(15) . ?
C3 H3 0.9500 . ?
C3 C4 1.403(9) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.381(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.366(8) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.377(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.405(8) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.383(12) . ?
C6 C7 1.463(11) . ?
C6A C7A 1.47(2) . ?
C7 H7 0.9500 . ?
C7 N1 1.268(6) . ?
C7A H7A 0.9500 . ?
C7A N1A 1.306(8) . ?
C8 C9 1.396(8) . ?
C8 C13 1.418(10) . ?
C8 N1 1.406(14) . ?
C8A C9A 1.405(11) . ?
C8A C13A 1.409(12) . ?
C8A N1A 1.384(16) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(8) . ?
C9A H9A 0.9500 . ?
C9A C10A 1.383(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.398(10) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.381(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.397(11) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.391(12) . ?
C12 H12 0.9500 . ?
C12 C13 1.394(9) . ?
C12A H12A 0.9500 . ?
C12A C13A 1.381(12) . ?
C13 O4 1.329(15) . ?
C13A O4A 1.322(11) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 H14D 0.9800 . ?
C14 H14E 0.9800 . ?
C14 H14F 0.9800 . ?
C14 S1 1.829(4) . ?
C14 S1A 1.783(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 H15D 0.9800 . ?
C15 H15E 0.9800 . ?
C15 H15F 0.9800 . ?
C15 S1 1.802(3) . ?
C15 S1A 1.784(3) . ?
Mo1 N1 2.305(5) . ?
Mo1 O1 1.648(3) . ?
Mo1 O2 1.691(3) . ?
Mo1 O3 1.946(5) . ?
Mo1 O4 1.963(5) . ?
Mo1 O5 2.287(4) . ?
N1A Mo4 2.218(6) . ?
O1 Mo4 1.768(4) . ?
O2 Mo4 1.747(4) . ?
O3A Mo4 1.937(7) . ?
O4A Mo4 1.944(7) . ?
O5 S1 1.519(3) . ?
O5A S1A 1.534(4) . ?
O5A Mo4 2.267(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 S2 1.787(5) . ?
C16A H16D 0.9801 . ?
C16A H16E 0.9800 . ?
C16A H16F 0.9796 . ?
C16A S2A 1.788(18) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 S2 1.771(4) . ?
C17A H17D 0.9799 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9803 . ?
C17A S2A 1.790(17) . ?
O6 S2 1.495(2) . ?
O6A S2A 1.515(16) . ?

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
C2 C1 C6 115.7(8) . . ?
O3 C1 C2 115.3(8) . . ?
O3 C1 C6 128.9(7) . . ?
C2A C1A C6A 113(2) . . ?
O3A C1A C2A 119.4(16) . . ?
O3A C1A C6A 127.2(13) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.3(10) . . ?
C3 C2 H2 119.4 . . ?
C1A C2A H2A 117.5 . . ?
C1A C2A C3A 125(2) . . ?
C3A C2A H2A 117.5 . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.6(10) . . ?
C4 C3 H3 119.2 . . ?
C2A C3A H3A 120.9 . . ?
C4A C3A C2A 118(2) . . ?
C4A C3A H3A 120.9 . . ?
C3 C4 H4 120.9 . . ?
C5 C4 C3 118.2(9) . . ?
C5 C4 H4 120.9 . . ?
C3A C4A H4A 120.1 . . ?
C5A C4A C3A 119.7(19) . . ?
C5A C4A H4A 120.1 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.0(9) . . ?
C6 C5 H5 119.5 . . ?
C4A C5A H5A 120.1 . . ?
C4A C5A C6A 119.9(18) . . ?
C6A C5A H5A 120.1 . . ?
C1 C6 C7 120.0(7) . . ?
C5 C6 C1 122.2(8) . . ?
C5 C6 C7 117.8(7) . . ?
C1A C6A C7A 118.6(13) . . ?
C5A C6A C1A 123(2) . . ?
C5A C6A C7A 118.0(14) . . ?
C6 C7 H7 118.1 . . ?
N1 C7 C6 123.7(5) . . ?
N1 C7 H7 118.1 . . ?
C6A C7A H7A 116.8 . . ?
N1A C7A C6A 126.3(7) . . ?
N1A C7A H7A 116.8 . . ?
C9 C8 C13 116.2(13) . . ?
C9 C8 N1 128.4(12) . . ?
N1 C8 C13 115.3(7) . . ?
C9A C8A C13A 115.1(12) . . ?
N1A C8A C9A 127.1(11) . . ?
N1A C8A C13A 117.6(10) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.7(12) . . ?
C10 C9 H9 119.7 . . ?
C8A C9A H9A 119.6 . . ?
C10A C9A C8A 120.8(13) . . ?
C10A C9A H9A 119.6 . . ?
C9 C10 H10 119.8 . . ?
C9 C10 C11 120.4(13) . . ?
C11 C10 H10 119.8 . . ?
C9A C10A H10A 119.0 . . ?
C11A C10A C9A 122.0(13) . . ?
C11A C10A H10A 119.0 . . ?
C10 C11 H11 118.7 . . ?
C12 C11 C10 122.5(16) . . ?
C12 C11 H11 118.7 . . ?
C10A C11A H11A 120.3 . . ?
C10A C11A C12A 119.3(14) . . ?
C12A C11A H11A 120.3 . . ?
C11 C12 H12 122.8 . . ?
C13 C12 C11 114.5(15) . . ?
C13 C12 H12 122.8 . . ?
C11A C12A H12A 121.0 . . ?
C13A C12A C11A 117.9(13) . . ?
C13A C12A H12A 121.0 . . ?
C12 C13 C8 125.6(14) . . ?
O4 C13 C8 115.7(9) . . ?
O4 C13 C12 118.7(11) . . ?
C12A C13A C8A 124.7(11) . . ?
O4A C13A C8A 111.4(12) . . ?
O4A C13A C12A 123.8(12) . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
H14D C14 H14E 109.5 . . ?
H14D C14 H14F 109.5 . . ?
H14E C14 H14F 109.5 . . ?
S1 C14 H14A 109.5 . . ?
S1 C14 H14B 109.5 . . ?
S1 C14 H14C 109.5 . . ?
S1A C14 H14D 109.5 . . ?
S1A C14 H14E 109.5 . . ?
S1A C14 H14F 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
H15D C15 H15E 109.5 . . ?
H15D C15 H15F 109.5 . . ?
H15E C15 H15F 109.5 . . ?
S1 C15 H15A 109.5 . . ?
S1 C15 H15B 109.5 . . ?
S1 C15 H15C 109.5 . . ?
S1A C15 H15D 109.5 . . ?
S1A C15 H15E 109.5 . . ?
S1A C15 H15F 109.5 . . ?
O1 Mo1 N1 89.19(15) . . ?
O1 Mo1 O2 107.62(18) . . ?
O1 Mo1 O3 99.29(18) . . ?
O1 Mo1 O4 97.12(17) . . ?
O1 Mo1 O5 166.6(2) . . ?
O2 Mo1 N1 163.13(19) . . ?
O2 Mo1 O3 96.5(2) . . ?
O2 Mo1 O4 101.38(19) . . ?
O2 Mo1 O5 85.50(16) . . ?
O3 Mo1 N1 81.7(2) . . ?
O3 Mo1 O4 150.7(2) . . ?
O3 Mo1 O5 81.41(17) . . ?
O4 Mo1 N1 74.46(18) . . ?
O4 Mo1 O5 77.15(18) . . ?
O5 Mo1 N1 77.64(15) . . ?
C7 N1 C8 120.7(6) . . ?
C7 N1 Mo1 129.6(3) . . ?
C8 N1 Mo1 109.3(5) . . ?
C7A N1A C8A 123.2(7) . . ?
C7A N1A Mo4 126.5(4) . . ?
C8A N1A Mo4 110.1(6) . . ?
C1 O3 Mo1 131.1(7) . . ?
C1A O3A Mo4 129.3(9) . . ?
C13 O4 Mo1 123.8(6) . . ?
C13A O4A Mo4 125.9(8) . . ?
S1 O5 Mo1 129.4(2) . . ?
S1A O5A Mo4 123.7(3) . . ?
C15 S1 C14 92.67(18) . . ?
O5 S1 C14 102.50(19) . . ?
O5 S1 C15 105.85(18) . . ?
C14 S1A C15 94.84(19) . . ?
O5A S1A C14 101.8(2) . . ?
O5A S1A C15 100.9(2) . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
S2 C16 H16A 109.5 . . ?
S2 C16 H16B 109.5 . . ?
S2 C16 H16C 109.5 . . ?
H16D C16A H16E 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
S2A C16A H16D 109.2 . . ?
S2A C16A H16E 110.2 . . ?
S2A C16A H16F 109.1 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
S2 C17 H17A 109.5 . . ?
S2 C17 H17B 109.5 . . ?
S2 C17 H17C 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.4 . . ?
H17E C17A H17F 109.5 . . ?
S2A C17A H17D 107.5 . . ?
S2A C17A H17E 110.6 . . ?
S2A C17A H17F 110.3 . . ?
C17 S2 C16 95.8(3) . . ?
O6 S2 C16 106.6(2) . . ?
O6 S2 C17 106.91(19) . . ?
C16A S2A C17A 94.9(15) . . ?
O6A S2A C16A 105.3(14) . . ?
O6A S2A C17A 104.9(12) . . ?
N1A Mo4 O5A 76.73(19) . . ?
O1 Mo4 N1A 89.9(2) . . ?
O1 Mo4 O3A 99.2(2) . . ?
O1 Mo4 O4A 96.1(3) . . ?
O1 Mo4 O5A 166.3(2) . . ?
O2 Mo4 N1A 169.9(2) . . ?
O2 Mo4 O1 100.1(2) . . ?
O2 Mo4 O3A 95.2(2) . . ?
O2 Mo4 O4A 103.3(3) . . ?
O2 Mo4 O5A 93.2(2) . . ?
O3A Mo4 N1A 83.7(3) . . ?
O3A Mo4 O4A 153.5(4) . . ?
O3A Mo4 O5A 82.3(3) . . ?
O4A Mo4 N1A 74.7(3) . . ?
O4A Mo4 O5A 77.9(2) . . ?

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
C1 C2 C3 C4 0(4) . . . . ?
C1 C6 C7 N1 2.2(17) . . . . ?
C1A C2A C3A C4A 8(5) . . . . ?
C1A C6A C7A N1A -11(3) . . . . ?
C2 C1 C6 C5 -1(3) . . . . ?
C2 C1 C6 C7 -177.5(17) . . . . ?
C2 C1 O3 Mo1 157.1(15) . . . . ?
C2 C3 C4 C5 2(3) . . . . ?
C2A C1A C6A C5A 1(3) . . . . ?
C2A C1A C6A C7A -179.8(15) . . . . ?
C2A C1A O3A Mo4 -151.3(11) . . . . ?
C2A C3A C4A C5A -2(5) . . . . ?
C3 C4 C5 C6 -3(2) . . . . ?
C3A C4A C5A C6A -3(3) . . . . ?
C4 C5 C6 C1 3(2) . . . . ?
C4 C5 C6 C7 179.5(11) . . . . ?
C4A C5A C6A C1A 4(3) . . . . ?
C4A C5A C6A C7A -175.1(15) . . . . ?
C5 C6 C7 N1 -174.7(9) . . . . ?
C5A C6A C7A N1A 167.7(12) . . . . ?
C6 C1 C2 C3 0(3) . . . . ?
C6 C1 O3 Mo1 -26(2) . . . . ?
C6 C7 N1 C8 178.1(11) . . . . ?
C6 C7 N1 Mo1 7.2(9) . . . . ?
C6A C1A C2A C3A -7(3) . . . . ?
C6A C1A O3A Mo4 31(2) . . . . ?
C6A C7A N1A C8A -176.4(16) . . . . ?
C6A C7A N1A Mo4 -2.0(14) . . . . ?
C8 C9 C10 C11 0(2) . . . . ?
C8 C13 O4 Mo1 11.4(14) . . . . ?
C8A C9A C10A C11A 3(3) . . . . ?
C8A C13A O4A Mo4 4(3) . . . . ?
C9 C8 C13 C12 1(2) . . . . ?
C9 C8 C13 O4 -179.3(11) . . . . ?
C9 C8 N1 C7 -2(2) . . . . ?
C9 C8 N1 Mo1 171.0(13) . . . . ?
C9 C10 C11 C12 3(3) . . . . ?
C9A C8A C13A C12A 1(4) . . . . ?
C9A C8A C13A O4A 179.2(18) . . . . ?
C9A C8A N1A C7A -6(3) . . . . ?
C9A C8A N1A Mo4 179.1(17) . . . . ?
C9A C10A C11A C12A -2(4) . . . . ?
C10 C11 C12 C13 -4(3) . . . . ?
C10A C11A C12A C13A 0(5) . . . . ?
C11 C12 C13 C8 2(2) . . . . ?
C11 C12 C13 O4 -177.8(17) . . . . ?
C11A C12A C13A C8A 0(5) . . . . ?
C11A C12A C13A O4A -178(3) . . . . ?
C12 C13 O4 Mo1 -168.4(6) . . . . ?
C12A C13A O4A Mo4 -178(2) . . . . ?
C13 C8 C9 C10 -2(2) . . . . ?
C13 C8 N1 C7 -178.9(9) . . . . ?
C13 C8 N1 Mo1 -6.4(14) . . . . ?
C13A C8A C9A C10A -3(3) . . . . ?
C13A C8A N1A C7A -179.8(15) . . . . ?
C13A C8A N1A Mo4 5(2) . . . . ?
Mo1 O5 S1 C14 -143.3(2) . . . . ?
Mo1 O5 S1 C15 120.2(3) . . . . ?
N1 C8 C9 C10 -179.3(12) . . . . ?
N1 C8 C13 C12 178.2(10) . . . . ?
N1 C8 C13 O4 -1.6(18) . . . . ?
N1A C8A C9A C10A -177.3(18) . . . . ?
N1A C8A C13A C12A 176(3) . . . . ?
N1A C8A C13A O4A -6(3) . . . . ?
O3 C1 C2 C3 177(2) . . . . ?
O3 C1 C6 C5 -177.3(15) . . . . ?
O3 C1 C6 C7 6(3) . . . . ?
O3A C1A C2A C3A 174(3) . . . . ?
O3A C1A C6A C5A 179.5(17) . . . . ?
O3A C1A C6A C7A -2(3) . . . . ?
Mo4 O5A S1A C14 139.2(3) . . . . ?
Mo4 O5A S1A C15 -123.5(3) . . . . ?

_olex2_date_sample_data_collection 2022-11-01
_olex2_date_sample_submission    2022-10-31
_olex2_exptl_crystal_mounting_method 'oil on 75 micrometre micromount'
_olex2_submission_original_sample_id LG-1-016
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.182
_oxdiff_exptl_absorpt_empirical_full_min 0.821
####################################################################### 
# 
# 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_akdk23003
_database_code_depnum_ccdc_archive 'CCDC 2312693'
loop_
_audit_author_name
_audit_author_address
'Adrian Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2023-12-07 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_audit_creation_date             2023-02-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H17 Mo N O7'
_chemical_formula_sum            'C16 H17 Mo N O7'
_chemical_formula_weight         431.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16 H17 Mo1 N1 O7'
_chemical_oxdiff_usercomment     'Samuel Steinfeld'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.93153(10)
_cell_length_b                   11.74560(18)
_cell_length_c                   20.3314(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.9309(13)
_cell_angle_gamma                90
_cell_volume                     1649.15(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5818
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      76.1820
_cell_measurement_theta_min      4.3140
_shelx_estimated_absorpt_T_max   0.541
_shelx_estimated_absorpt_T_min   0.326
_exptl_absorpt_coefficient_mu    6.876
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.342
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             872
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -2 0.0434
0 -1 2 0.0587
0 1 2 0.0528
0 -1 -2 0.0745
-2 0 1 0.1030
2 0 -1 0.0934
0 -1 0 0.0835
0 1 0 0.0678

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol and tetrahydrofuran'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.102
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 1.0001 -1.9998 -0.1181 -0.1293 -0.0985
0.0000 -1.0001 1.9998 0.1181 0.1293 0.0985
-0.0000 0.9999 2.0001 0.0968 0.0777 -0.1578
0.0000 -0.9999 -2.0001 -0.0968 -0.0777 0.1578
-2.0000 -0.0000 1.0001 -0.2861 0.3394 -0.0447
2.0000 0.0000 -1.0001 0.2861 -0.3394 0.0447
0.0000 -1.0000 -0.0001 0.0107 0.0258 0.1281
-0.0000 1.0000 0.0001 -0.0107 -0.0258 -0.1281

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.039
_diffrn_reflns_theta_max         67.039
_diffrn_reflns_theta_min         4.351
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -123.00 -51.00   0.50    0.20    --  -48.70 -16.00 162.00  144
  2  ω    -61.00  -2.00   0.50    0.20    --  -48.70  16.00 -28.00  118
  3  ω     -6.00  19.00   0.50    0.20    --   48.70 -16.00 162.00   50
  4  ω     73.00 111.00   0.50    0.20    --   48.70  16.00 -28.00   76
  5  ω     47.00 106.00   0.50    0.80    --  107.75 -16.00 162.00  118
  6  ω     94.00 178.00   0.50    0.80    --  107.75  16.00 -28.00  168
  7  ω    -26.00  60.00   0.50    0.20    --   48.70 -19.00  30.00  172
  8  ω     42.00  75.00   0.50    0.20    --   48.70-125.00  90.00   66
  9  ω     45.00 116.00   0.50    0.80    --  107.75 -57.00  90.00  142
 10  ω     36.00 119.00   0.50    0.80    --  107.75 -19.00 -30.00  166
 11  ω     36.00 126.00   0.50    0.80    --  107.75 -77.00  90.00  180
 12  ω    110.00 153.00   0.50    0.80    --  107.75  37.00  30.00   86
 13  ω     39.00  65.00   0.50    0.80    --  107.75-125.00 150.00   52
 14  ω     42.00  94.00   0.50    0.80    --  107.75 -99.00 -90.00  104
 15  ω     86.00 111.00   0.50    0.80    --  107.75-125.00 150.00   50
 16  ω     81.00 106.00   0.50    0.80    --  107.75 -99.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1698990000
_diffrn_orient_matrix_UB_12      -0.0106853000
_diffrn_orient_matrix_UB_13      0.0537262000
_diffrn_orient_matrix_UB_21      -0.1438020000
_diffrn_orient_matrix_UB_22      -0.0258024000
_diffrn_orient_matrix_UB_23      0.0517541000
_diffrn_orient_matrix_UB_31      0.0149235000
_diffrn_orient_matrix_UB_32      -0.1281444000
_diffrn_orient_matrix_UB_33      -0.0148336000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2779
_reflns_number_total             2945
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         2945
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0283
_refine_ls_restrained_S_all      1.066
_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)+(0.0210P)²+1.8646P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0676
_refine_special_details          
;
The ligand was disordered and modelled in two positions with one methoxyphenyl 
in a common site but the other and the imine bridge modelled in two sites with 
refined occupancies of 0.638:0.362(3).  The ADP of pairs of proximal atoms 
were constrained to be equal as follows:
C1 & C1A, C2 & C2A C3 & C3A, C4 & C4A, C5 & C5A, C6 & C6A, C7 & C7A, C14 & C14A
O3 & O3A, O4 & O4A, N1 & N1A
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5A) = Uanis(C5)
Uanis(O4A) = Uanis(O4)
Uanis(C3) = Uanis(C3A)
Uanis(C2) = Uanis(C2A)
Uanis(C6) = Uanis(C6A)
Uanis(C4) = Uanis(C4A)
Uanis(C1) = Uanis(C1A)
Uanis(C14A) = Uanis(C14)
Uanis(C7A) = Uanis(C7)
Uanis(N1A) = Uanis(N1)
Uanis(O3) = Uanis(O3A)
3. Others
 Sof(C6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(C3A)=Sof(H3A)=Sof(C2A)=Sof(H2A)=
 Sof(C1A)=Sof(C7A)=Sof(H7A)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(N1A)=
 Sof(O3A)=Sof(O4A)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(C7)=Sof(H7)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(N1)=Sof(O3)=Sof(O4)=
 FVAR(1)
4.a Riding coordinates:
 O7(H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C5A(H5A), C3A(H3A), C2A(H2A), C7(H7), C7A(H7A),
 C9(H9), C11(H11), C12(H12)
4.c Fitted hexagon refined as free rotating group:
 C6A(C5A,C4A,C3A,C2A,C1A)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_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
C1 C 0.7174(8) 0.5584(6) 0.5722(3) 0.0279(15) Uani 0.637(3) 1 d . . P A 1
C2 C 0.7302(11) 0.4457(8) 0.5497(5) 0.0282(12) Uani 0.637(3) 1 d . . P A 1
H2 H 0.832402 0.423967 0.524039 0.034 Uiso 0.637(3) 1 calc R U P A 1
C3 C 0.5948(17) 0.3674(7) 0.5649(7) 0.0274(14) Uani 0.637(3) 1 d . . P A 1
H3 H 0.604772 0.290913 0.550412 0.033 Uiso 0.637(3) 1 calc R U P A 1
C4 C 0.4415(13) 0.3993(8) 0.6017(6) 0.0273(12) Uani 0.637(3) 1 d . . P A 1
C5 C 0.4252(8) 0.5091(6) 0.6225(3) 0.0259(11) Uani 0.637(3) 1 d . . P A 1
H5 H 0.319774 0.530453 0.646823 0.031 Uiso 0.637(3) 1 calc R U P A 1
C6 C 0.5643(8) 0.5907(5) 0.6081(3) 0.0274(13) Uani 0.637(3) 1 d . . P A 1
C6A C 0.6326(15) 0.5933(9) 0.5961(5) 0.0274(13) Uani 0.363(3) 1 d G . P A 2
C5A C 0.4821(14) 0.5232(13) 0.6122(6) 0.0259(11) Uani 0.363(3) 1 d G . P A 2
H5A H 0.382177 0.552894 0.636437 0.031 Uiso 0.363(3) 1 calc R U P A 2
C4A C 0.478(2) 0.4096(13) 0.5930(11) 0.0273(12) Uani 0.363(3) 1 d G . P A 2
C3A C 0.624(3) 0.3662(11) 0.5576(13) 0.0274(14) Uani 0.363(3) 1 d G . P A 2
H3A H 0.621357 0.288524 0.544387 0.033 Uiso 0.363(3) 1 calc R U P A 2
C2A C 0.775(2) 0.4363(13) 0.5414(10) 0.0282(12) Uani 0.363(3) 1 d G . P A 2
H2A H 0.874603 0.406564 0.517214 0.034 Uiso 0.363(3) 1 calc R U P A 2
C1A C 0.7788(13) 0.5498(12) 0.5607(6) 0.0279(15) Uani 0.363(3) 1 d G . P A 2
C7 C 0.5354(6) 0.7039(4) 0.6325(2) 0.0257(8) Uani 0.637(3) 1 d . . P A 1
H7 H 0.419111 0.718924 0.652538 0.031 Uiso 0.637(3) 1 calc R U P A 1
C7A C 0.5508(14) 0.7670(8) 0.6415(4) 0.0257(8) Uani 0.363(3) 1 d . . P A 2
H7A H 0.433094 0.735382 0.653934 0.031 Uiso 0.363(3) 1 calc R U P A 2
C8 C 0.6047(5) 0.8934(2) 0.65525(14) 0.0379(7) Uani 1 1 d . . . . .
C9 C 0.4479(5) 0.9310(2) 0.68895(14) 0.0360(7) Uani 1 1 d . . . . .
H9 H 0.348416 0.879570 0.698733 0.043 Uiso 1 1 calc R U . . .
C10 C 0.4406(4) 1.0439(2) 0.70765(13) 0.0336(6) Uani 1 1 d . . . . .
C11 C 0.5870(4) 1.1185(2) 0.69301(14) 0.0359(6) Uani 1 1 d . . . . .
H11 H 0.581006 1.196141 0.705837 0.043 Uiso 1 1 calc R U . . .
C12 C 0.7408(4) 1.0808(3) 0.66005(15) 0.0386(7) Uani 1 1 d . . . . .
H12 H 0.839737 1.132470 0.650119 0.046 Uiso 1 1 calc R U . . .
C13 C 0.7509(4) 0.9678(3) 0.64145(14) 0.0367(7) Uani 1 1 d . . . . .
C14 C 0.1749(12) 0.3353(6) 0.6583(4) 0.0387(15) Uani 0.637(3) 1 d . . P A 1
H14A H 0.075638 0.385882 0.637217 0.058 Uiso 0.637(3) 1 calc R U P A 1
H14B H 0.238389 0.372652 0.697495 0.058 Uiso 0.637(3) 1 calc R U P A 1
H14C H 0.114210 0.264358 0.671440 0.058 Uiso 0.637(3) 1 calc R U P A 1
C14A C 0.183(2) 0.3775(12) 0.6483(8) 0.0387(15) Uani 0.363(3) 1 d . . P A 2
H14D H 0.235(17) 0.385(12) 0.690(6) 0.058 Uiso 0.363(3) 1 d . U P A 2
H14E H 0.100(19) 0.305(12) 0.649(6) 0.058 Uiso 0.363(3) 1 d . U P A 2
H14F H 0.116(17) 0.437(10) 0.633(5) 0.058 Uiso 0.363(3) 1 d . U P A 2
C15 C 0.1512(5) 1.0131(3) 0.76019(16) 0.0495(8) Uani 1 1 d . . . . .
H15A H 0.086994 0.974540 0.721525 0.074 Uiso 1 1 calc R U . . .
H15B H 0.054890 1.055255 0.783054 0.074 Uiso 1 1 calc R U . . .
H15C H 0.214193 0.956398 0.790207 0.074 Uiso 1 1 calc R U . . .
C16 C 0.7391(5) 0.9336(3) 0.46580(16) 0.0489(8) Uani 1 1 d . . . . .
H16A H 0.841374 0.944329 0.435983 0.073 Uiso 1 1 calc R U . . .
H16B H 0.749766 0.992526 0.500023 0.073 Uiso 1 1 calc R U . . .
H16C H 0.612260 0.939062 0.440675 0.073 Uiso 1 1 calc R U . . .
Mo01 Mo 0.96303(3) 0.77332(2) 0.58848(2) 0.03058(9) Uani 1 1 d . . . . .
N1 N 0.6569(5) 0.7863(3) 0.62894(17) 0.0243(6) Uani 0.637(3) 1 d . . P A 1
N1A N 0.6722(9) 0.7078(5) 0.6128(3) 0.0243(6) Uani 0.363(3) 1 d . . P A 2
O1 O 1.0668(3) 0.73076(18) 0.66372(10) 0.0391(5) Uani 1 1 d . . . . .
O2 O 1.1519(3) 0.79792(17) 0.54237(11) 0.0395(5) Uani 1 1 d . . . . .
O3 O 0.8545(6) 0.6340(3) 0.5551(2) 0.0316(8) Uani 0.637(3) 1 d . . P A 1
O3A O 0.9277(10) 0.6141(7) 0.5454(4) 0.0316(8) Uani 0.363(3) 1 d . . P A 2
O4 O 0.3147(14) 0.3104(5) 0.6132(5) 0.0311(12) Uani 0.637(3) 1 d . . P A 1
O4A O 0.333(3) 0.3399(12) 0.6072(10) 0.0311(12) Uani 0.363(3) 1 d . . P A 2
O5 O 0.2929(3) 1.09016(19) 0.73950(10) 0.0417(5) Uani 1 1 d . . . . .
O6 O 0.9029(3) 0.9305(2) 0.60915(10) 0.0447(5) Uani 1 1 d . . . . .
O7 O 0.7590(3) 0.82481(18) 0.49576(10) 0.0428(5) Uani 1 1 d . . . . .
H7B H 0.744212 0.776207 0.462305 0.063(12) Uiso 1 1 d R . . . .


_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
C1 C2 1.407(7) . ?
C1 C6 1.392(7) . ?
C1 O3 1.366(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.367(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.402(7) . ?
C4 C5 1.365(7) . ?
C4 O4 1.398(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.408(7) . ?
C6 C7 1.440(8) . ?
C6A C5A 1.3900 . ?
C6A C1A 1.3900 . ?
C6A N1A 1.408(12) . ?
C5A H5A 0.9500 . ?
C5A C4A 1.3900 . ?
C4A C3A 1.3900 . ?
C4A O4A 1.349(15) . ?
C3A H3A 0.9500 . ?
C3A C2A 1.3900 . ?
C2A H2A 0.9500 . ?
C2A C1A 1.3900 . ?
C1A O3A 1.337(11) . ?
C7 H7 0.9500 . ?
C7 N1 1.289(6) . ?
C7A H7A 0.9500 . ?
C7A C8 1.550(9) . ?
C7A N1A 1.272(12) . ?
C8 C9 1.405(5) . ?
C8 C13 1.386(5) . ?
C8 N1 1.425(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(4) . ?
C10 C11 1.392(4) . ?
C10 O5 1.370(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.380(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(4) . ?
C13 O6 1.361(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 O4 1.422(13) . ?
C14A H14D 0.89(12) . ?
C14A H14E 1.02(14) . ?
C14A H14F 0.88(12) . ?
C14A O4A 1.46(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 O5 1.426(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 O7 1.417(4) . ?
Mo01 N1 2.346(4) . ?
Mo01 N1A 2.253(6) . ?
Mo01 O1 1.708(2) . ?
Mo01 O2 1.699(2) . ?
Mo01 O3 1.901(4) . ?
Mo01 O3A 2.070(8) . ?
Mo01 O6 1.946(2) . ?
Mo01 O7 2.337(2) . ?
O7 H7B 0.8871 . ?

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
C6 C1 C2 119.9(4) . . ?
O3 C1 C2 117.7(5) . . ?
O3 C1 C6 122.3(5) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.7(5) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.5(4) . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 120.4(4) . . ?
C5 C4 O4 125.7(8) . . ?
O4 C4 C3 113.9(8) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.1(4) . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 119.4(4) . . ?
C1 C6 C7 124.6(5) . . ?
C5 C6 C7 116.0(4) . . ?
C5A C6A C1A 120.0 . . ?
C5A C6A N1A 130.0(9) . . ?
C1A C6A N1A 109.9(9) . . ?
C6A C5A H5A 120.0 . . ?
C4A C5A C6A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C5A C4A C3A 120.0 . . ?
O4A C4A C5A 121.3(15) . . ?
O4A C4A C3A 118.7(15) . . ?
C4A C3A H3A 120.0 . . ?
C4A C3A C2A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C3A C2A H2A 120.0 . . ?
C3A C2A C1A 120.0 . . ?
C1A C2A H2A 120.0 . . ?
C2A C1A C6A 120.0 . . ?
O3A C1A C6A 121.7(10) . . ?
O3A C1A C2A 118.3(10) . . ?
C6 C7 H7 117.9 . . ?
N1 C7 C6 124.3(4) . . ?
N1 C7 H7 117.9 . . ?
C8 C7A H7A 121.7 . . ?
N1A C7A H7A 121.7 . . ?
N1A C7A C8 116.6(8) . . ?
C9 C8 C7A 101.8(5) . . ?
C9 C8 N1 133.8(3) . . ?
C13 C8 C7A 137.5(5) . . ?
C13 C8 C9 120.7(3) . . ?
C13 C8 N1 105.5(3) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 C8 118.9(3) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 C11 120.1(3) . . ?
O5 C10 C9 123.8(3) . . ?
O5 C10 C11 116.1(3) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0(3) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C8 119.7(3) . . ?
O6 C13 C8 120.3(3) . . ?
O6 C13 C12 120.0(3) . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O4 C14 H14A 109.5 . . ?
O4 C14 H14B 109.5 . . ?
O4 C14 H14C 109.5 . . ?
H14D C14A H14E 104(10) . . ?
H14D C14A H14F 115(10) . . ?
H14E C14A H14F 113(10) . . ?
O4A C14A H14D 109(7) . . ?
O4A C14A H14E 101(8) . . ?
O4A C14A H14F 115(7) . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O5 C15 H15A 109.5 . . ?
O5 C15 H15B 109.5 . . ?
O5 C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O7 C16 H16A 109.5 . . ?
O7 C16 H16B 109.5 . . ?
O7 C16 H16C 109.5 . . ?
N1A Mo01 O7 76.97(16) . . ?
O1 Mo01 N1 91.66(11) . . ?
O1 Mo01 N1A 91.10(16) . . ?
O1 Mo01 O3 100.98(15) . . ?
O1 Mo01 O3A 98.0(2) . . ?
O1 Mo01 O6 99.55(10) . . ?
O1 Mo01 O7 167.72(9) . . ?
O2 Mo01 N1 160.99(11) . . ?
O2 Mo01 N1A 157.80(17) . . ?
O2 Mo01 O1 105.00(10) . . ?
O2 Mo01 O3 104.45(14) . . ?
O2 Mo01 O3A 89.4(2) . . ?
O2 Mo01 O6 98.48(10) . . ?
O2 Mo01 O7 87.28(10) . . ?
O3 Mo01 N1 80.73(14) . . ?
O3 Mo01 O6 143.87(13) . . ?
O3 Mo01 O7 75.03(14) . . ?
O3A Mo01 N1A 73.1(2) . . ?
O3A Mo01 O7 81.4(2) . . ?
O6 Mo01 N1 69.24(11) . . ?
O6 Mo01 N1A 93.69(17) . . ?
O6 Mo01 O3A 158.1(2) . . ?
O6 Mo01 O7 78.62(8) . . ?
O7 Mo01 N1 76.29(10) . . ?
C7 N1 C8 116.9(4) . . ?
C7 N1 Mo01 125.9(3) . . ?
C8 N1 Mo01 117.1(3) . . ?
C6A N1A Mo01 115.7(6) . . ?
C7A N1A C6A 120.7(8) . . ?
C7A N1A Mo01 123.6(6) . . ?
C1 O3 Mo01 137.0(4) . . ?
C1A O3A Mo01 118.5(7) . . ?
C4 O4 C14 115.3(7) . . ?
C4A O4A C14A 121.5(15) . . ?
C10 O5 C15 116.7(3) . . ?
C13 O6 Mo01 126.8(2) . . ?
C16 O7 Mo01 127.58(18) . . ?
C16 O7 H7B 104.5 . . ?
Mo01 O7 H7B 118.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 1.2(6) . . . . ?
C1 C6 C7 N1 -6.4(8) . . . . ?
C2 C1 C6 C5 1.1(6) . . . . ?
C2 C1 C6 C7 -178.9(7) . . . . ?
C2 C1 O3 Mo01 -156.2(5) . . . . ?
C2 C3 C4 C5 0.2(6) . . . . ?
C2 C3 C4 O4 179.9(11) . . . . ?
C3 C4 C5 C6 -1.0(6) . . . . ?
C3 C4 O4 C14 171.0(7) . . . . ?
C4 C5 C6 C1 0.4(6) . . . . ?
C4 C5 C6 C7 -179.7(7) . . . . ?
C5 C4 O4 C14 -9.4(16) . . . . ?
C5 C6 C7 N1 173.7(5) . . . . ?
C6 C1 C2 C3 -1.8(6) . . . . ?
C6 C1 O3 Mo01 26.5(9) . . . . ?
C6 C7 N1 C8 179.7(4) . . . . ?
C6 C7 N1 Mo01 -4.0(6) . . . . ?
C6A C5A C4A C3A 0.0 . . . . ?
C6A C5A C4A O4A -179(2) . . . . ?
C6A C1A O3A Mo01 10.1(13) . . . . ?
C5A C6A C1A C2A 0.0 . . . . ?
C5A C6A C1A O3A -178.7(12) . . . . ?
C5A C6A N1A C7A -8.0(14) . . . . ?
C5A C6A N1A Mo01 170.0(8) . . . . ?
C5A C4A C3A C2A 0.0 . . . . ?
C5A C4A O4A C14A -6(3) . . . . ?
C4A C3A C2A C1A 0.0 . . . . ?
C3A C4A O4A C14A 175.3(14) . . . . ?
C3A C2A C1A C6A 0.0 . . . . ?
C3A C2A C1A O3A 178.7(12) . . . . ?
C2A C1A O3A Mo01 -168.6(9) . . . . ?
C1A C6A C5A C4A 0.0 . . . . ?
C1A C6A N1A C7A 175.2(7) . . . . ?
C1A C6A N1A Mo01 -6.7(9) . . . . ?
C7A C8 C9 C10 -177.6(4) . . . . ?
C7A C8 C13 C12 176.2(5) . . . . ?
C7A C8 C13 O6 -3.0(6) . . . . ?
C8 C7A N1A C6A -177.6(6) . . . . ?
C8 C7A N1A Mo01 4.5(9) . . . . ?
C8 C9 C10 C11 0.1(4) . . . . ?
C8 C9 C10 O5 178.7(2) . . . . ?
C8 C13 O6 Mo01 -9.1(4) . . . . ?
C9 C8 C13 C12 -1.1(4) . . . . ?
C9 C8 C13 O6 179.6(2) . . . . ?
C9 C8 N1 C7 4.0(5) . . . . ?
C9 C8 N1 Mo01 -172.7(3) . . . . ?
C9 C10 C11 C12 -0.3(4) . . . . ?
C9 C10 O5 C15 6.9(4) . . . . ?
C10 C11 C12 C13 -0.3(4) . . . . ?
C11 C10 O5 C15 -174.5(2) . . . . ?
C11 C12 C13 C8 1.0(4) . . . . ?
C11 C12 C13 O6 -179.8(3) . . . . ?
C12 C13 O6 Mo01 171.7(2) . . . . ?
C13 C8 C9 C10 0.6(4) . . . . ?
C13 C8 N1 C7 -176.1(3) . . . . ?
C13 C8 N1 Mo01 7.2(3) . . . . ?
N1 C8 C9 C10 -179.5(3) . . . . ?
N1 C8 C13 C12 179.0(3) . . . . ?
N1 C8 C13 O6 -0.3(3) . . . . ?
N1A C6A C5A C4A -176.5(14) . . . . ?
N1A C6A C1A C2A 177.1(11) . . . . ?
N1A C6A C1A O3A -1.6(13) . . . . ?
N1A C7A C8 C9 -177.6(6) . . . . ?
N1A C7A C8 C13 4.7(9) . . . . ?
O3 C1 C2 C3 -179.2(6) . . . . ?
O3 C1 C6 C5 178.3(6) . . . . ?
O3 C1 C6 C7 -1.6(9) . . . . ?
O4 C4 C5 C6 179.4(11) . . . . ?
O4A C4A C3A C2A 179(2) . . . . ?
O5 C10 C11 C12 -178.9(2) . . . . ?

_olex2_date_sample_data_collection 2023-02-20
_olex2_date_sample_submission    2023-02-16
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id SS-025-1
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.191
_oxdiff_exptl_absorpt_empirical_full_min 0.882
####################################################################### 
# 
# 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_akdk23005
_database_code_depnum_ccdc_archive 'CCDC 2312695'
loop_
_audit_author_name
_audit_author_address
'Adrian Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2023-12-07 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_audit_creation_date             2023-03-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H15 F2 Mo N O5, 0.5(C4 H8 O)'
_chemical_formula_sum            'C19 H19 F2 Mo N O5.50'
_chemical_formula_weight         483.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C19 H18.5 F2 Mo1 N1 O5.5'
_chemical_oxdiff_usercomment     'Samuel Steinfeld  SS-034-1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.7559(4)
_cell_length_b                   12.1951(7)
_cell_length_c                   12.2098(7)
_cell_angle_alpha                71.970(5)
_cell_angle_beta                 80.752(5)
_cell_angle_gamma                77.252(5)
_cell_volume                     928.32(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1838
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      75.7910
_cell_measurement_theta_min      6.1730
_shelx_estimated_absorpt_T_max   0.744
_shelx_estimated_absorpt_T_min   0.366
_exptl_absorpt_coefficient_mu    6.283
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             488
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0162
0 -1 0 0.0325
-1 -1 0 0.0601
0 -1 -2 0.0937
0 1 2 0.0788
1 2 2 0.0419
1 1 0 0.0953

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Heptane and tetrahydrofuran'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0001 0.9999 -0.0003 0.1259 0.0064 -0.0486
0.0001 -0.9999 0.0003 -0.1259 -0.0064 0.0486
-0.9999 -1.0000 0.0006 -0.0045 -0.0850 0.2338
-0.0001 -1.0003 -1.9997 -0.0483 0.2477 0.0718
0.0001 1.0003 1.9997 0.0483 -0.2477 -0.0718
0.9999 2.0002 1.9991 0.0528 -0.1627 -0.3056
0.9999 1.0000 -0.0006 0.0045 0.0850 -0.2338

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9376
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.072
_diffrn_reflns_theta_max         67.072
_diffrn_reflns_theta_min         3.826
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -101.00 -39.00   0.50    0.20    --  -48.70 148.00  96.00  124
  2  ω    -87.00 -61.00   0.50    0.20    --  -48.70-148.00  49.00   52
  3  ω    -80.00 -47.00   0.50    0.20    --  -48.70 123.00 -67.00   66
  4  ω     48.00  92.00   0.50    0.20    --   48.70-123.00-147.00   88
  5  ω     48.00  92.00   0.50    0.20    --   48.70-148.00  49.00   88
  6  ω     99.00 124.00   0.50    0.80    --  107.75 148.00  96.00   50
  7  ω     73.00 105.00   0.50    0.80    --  107.75-123.00-147.00   64
  8  ω     64.00  90.00   0.50    0.80    --  107.75-148.00  49.00   52
  9  ω    122.00 153.00   0.50    0.80    --  107.75 123.00 -67.00   62
 10  ω   -111.00 -74.00   0.50    0.20    --  -48.70-125.00 -60.00   74
 11  ω   -111.00 -81.00   0.50    0.20    --  -48.70-125.00 -90.00   60
 12  ω   -120.00 -29.00   0.50    0.20    --  -48.70 -77.00-120.00  182
 13  ω   -115.00 -74.00   0.50    0.20    --  -48.70-125.00  60.00   82
 14  ω   -113.00 -75.00   0.50    0.20    --  -48.70-125.00-150.00   76
 15  ω   -109.00 -76.00   0.50    0.20    --  -48.70-125.00-120.00   66
 16  ω     19.00  58.00   0.50    0.20    --   48.70 -99.00  30.00   78
 17  ω     38.00  97.00   0.50    0.80    --  107.75 -99.00  90.00  118
 18  ω    100.00 176.00   0.50    0.80    --  107.75  37.00-180.00  152
 19  ω     85.00 117.00   0.50    0.80    --  107.75 -37.00   0.00   64
 20  ω     39.00 119.00   0.50    0.80    --  107.75 -77.00 -60.00  160
 21  ω     80.00 106.00   0.50    0.80    --  107.75 -99.00-150.00   52
 22  ω    136.00 162.00   0.50    0.80    --  107.75 125.00-120.00   52
 23  ω     37.00  76.00   0.50    0.80    --  107.75 -99.00-150.00   78
 24  ω     39.00 102.00   0.50    0.80    --  107.75 -57.00-180.00  126
 25  ω    137.00 177.00   0.50    0.80    --  107.75  57.00 150.00   80
 26  ω     93.00 132.00   0.50    0.80    --  107.75  57.00 150.00   78
 27  ω     97.00 174.00   0.50    0.80    --  107.75  19.00 -60.00  154
 28  ω     54.00  99.00   0.50    0.80    --  107.75 -99.00 -90.00   90
 29  ω    101.00 132.00   0.50    0.80    --  107.75 125.00-180.00   62
 30  ω     39.00  64.00   0.50    0.80    --  107.75 -99.00 -60.00   50
 31  ω     67.00  95.00   0.50    0.80    --  107.75 -99.00 -60.00   56
 32  ω     40.00 106.00   0.50    0.80    --  107.75 -99.00 120.00  132
 33  ω     39.00  84.00   0.50    0.80    --  107.75 -99.00   0.00   90
 34  ω     35.00  77.00   0.50    0.80    --  107.75 -37.00   0.00   84
 35  ω    118.00 178.00   0.50    0.80    --  107.75  19.00-120.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1213981000
_diffrn_orient_matrix_UB_12      0.1258976000
_diffrn_orient_matrix_UB_13      -0.0388359000
_diffrn_orient_matrix_UB_21      0.0785918000
_diffrn_orient_matrix_UB_22      0.0063263000
_diffrn_orient_matrix_UB_23      -0.1270450000
_diffrn_orient_matrix_UB_31      -0.1851890000
_diffrn_orient_matrix_UB_32      -0.0486256000
_diffrn_orient_matrix_UB_33      -0.0115982000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3175
_reflns_number_total             3307
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3307
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0279
_refine_ls_restrained_S_all      1.059
_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)+(0.0257P)²+1.0117P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0668
_refine_special_details          
;
The ligand was disordered with the imine group being modelled in two positions 
with refined occupancies of 0.532:0.468(17).  The ADPs of disordered pairs of 
atoms were constrained to be equal (C7 & C7A, N1 & N1A).  The bound 
tetrahydrofuran (THF) was also disordered with the carbons modelled in two positions
with refined occupancies of 0.520:0.480(6).The asymmetric unit contained half a THF of crystallisation which was disordered 
about the centre of inversion. C-C bond lengths were restrained to be 1.51 
angstroms and the C-O bond-lengths to 1.42 angstroms.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C18-C19 = C20-C19 = C20-C21
 1.5 with sigma of 0.01
 O6-C18 = O6-C21
 1.42 with sigma of 0.01
3. Others
 Sof(C7A)=Sof(H7A)=Sof(N1A)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(N1)=FVAR(1)
 Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=
 Sof(H16C)=Sof(H16D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=1-FVAR(2)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=FVAR(2)
 Fixed Sof: C18(0.5) H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5) H19B(0.5) C20(0.5)
 H20A(0.5) H20B(0.5) C21(0.5) H21A(0.5) H21B(0.5) O6(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C14A(H14C,H14D), C15(H15A,H15B), C15A(H15C,H15D), C16(H16A,
 H16B), C16A(H16C,H16D), C17(H17A,H17B), C17A(H17C,H17D), C18(H18A,H18B),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C7A(H7A), C9(H9), C11(H11), C12(H12)
;
_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
C1 C 0.5544(6) 0.8044(3) 0.7757(3) 0.0534(9) Uani 1 1 d . . . . .
C2 C 0.5169(6) 0.9227(3) 0.7712(4) 0.0562(9) Uani 1 1 d . . . . .
H2 H 0.621982 0.967669 0.741277 0.067 Uiso 1 1 calc R U . . .
C3 C 0.3298(6) 0.9738(3) 0.8095(4) 0.0644(10) Uani 1 1 d . . . . .
H3 H 0.303274 1.054572 0.806039 0.077 Uiso 1 1 calc R U . . .
C4 C 0.1791(6) 0.9078(4) 0.8533(5) 0.0737(12) Uani 1 1 d . . . . .
C5 C 0.2102(7) 0.7908(4) 0.8623(4) 0.0737(14) Uani 1 1 d . . . . .
H5 H 0.103510 0.747266 0.893644 0.088 Uiso 1 1 calc R U . . .
C6 C 0.3999(7) 0.7374(3) 0.8249(3) 0.0601(11) Uani 1 1 d . . . . .
C7 C 0.3865(10) 0.6150(8) 0.8516(4) 0.026(2) Uani 0.534(17) 1 d . . P A 2
H7 H 0.266041 0.585797 0.888412 0.032 Uiso 0.534(17) 1 calc R U P A 2
C7A C 0.4169(11) 0.5351(9) 0.8556(5) 0.027(3) Uani 0.466(17) 1 d . . P A 1
H7A H 0.279419 0.548161 0.888371 0.033 Uiso 0.466(17) 1 calc R U P A 1
C8 C 0.5287(6) 0.4207(3) 0.8505(3) 0.0515(9) Uani 1 1 d . . . . .
C9 C 0.3835(5) 0.3508(4) 0.9039(3) 0.0573(10) Uani 1 1 d . . . . .
H9 H 0.251044 0.384368 0.930771 0.069 Uiso 1 1 calc R U . . .
C10 C 0.4346(5) 0.2329(4) 0.9172(3) 0.0530(9) Uani 1 1 d . . . . .
C11 C 0.6245(5) 0.1798(3) 0.8796(3) 0.0445(7) Uani 1 1 d . . . . .
H11 H 0.656246 0.097430 0.891202 0.053 Uiso 1 1 calc R U . . .
C12 C 0.7670(5) 0.2498(3) 0.8247(3) 0.0426(7) Uani 1 1 d . . . . .
H12 H 0.898471 0.215368 0.797503 0.051 Uiso 1 1 calc R U . . .
C13 C 0.7201(6) 0.3697(3) 0.8088(3) 0.0443(7) Uani 1 1 d . . . . .
C14 C 0.5331(9) 0.7216(6) 0.5435(5) 0.0465(17) Uani 0.525(6) 1 d . . P B 1
H14A H 0.414649 0.700081 0.599300 0.056 Uiso 0.525(6) 1 calc R U P B 1
H14B H 0.547507 0.801692 0.539975 0.056 Uiso 0.525(6) 1 calc R U P B 1
C14A C 0.5609(12) 0.6007(8) 0.5541(6) 0.055(2) Uani 0.475(6) 1 d . . P B 2
H14C H 0.432504 0.642923 0.585278 0.066 Uiso 0.475(6) 1 calc R U P B 2
H14D H 0.567089 0.515501 0.590837 0.066 Uiso 0.475(6) 1 calc R U P B 2
C15 C 0.5066(12) 0.7153(8) 0.4262(6) 0.056(2) Uani 0.525(6) 1 d . . P B 1
H15A H 0.446198 0.792872 0.376838 0.068 Uiso 0.525(6) 1 calc R U P B 1
H15B H 0.419912 0.657703 0.431875 0.068 Uiso 0.525(6) 1 calc R U P B 1
C15A C 0.5656(16) 0.6271(9) 0.4281(7) 0.064(2) Uani 0.475(6) 1 d . . P B 2
H15C H 0.634999 0.557726 0.402056 0.076 Uiso 0.475(6) 1 calc R U P B 2
H15D H 0.425560 0.650916 0.404162 0.076 Uiso 0.475(6) 1 calc R U P B 2
C16 C 0.726(3) 0.6756(13) 0.3798(13) 0.064(3) Uani 0.525(6) 1 d . . P B 1
H16A H 0.728788 0.633659 0.321694 0.077 Uiso 0.525(6) 1 calc R U P B 1
H16B H 0.795055 0.743591 0.343494 0.077 Uiso 0.525(6) 1 calc R U P B 1
C16A C 0.678(3) 0.7230(15) 0.3795(16) 0.074(5) Uani 0.475(6) 1 d . . P B 2
H16C H 0.583747 0.799119 0.358684 0.088 Uiso 0.475(6) 1 calc R U P B 2
H16D H 0.767721 0.712773 0.309348 0.088 Uiso 0.475(6) 1 calc R U P B 2
C17 C 0.8249(11) 0.5968(6) 0.4816(5) 0.0512(18) Uani 0.525(6) 1 d . . P B 1
H17A H 0.811695 0.514769 0.492267 0.061 Uiso 0.525(6) 1 calc R U P B 1
H17B H 0.971627 0.600881 0.472073 0.061 Uiso 0.525(6) 1 calc R U P B 1
C17A C 0.8063(17) 0.7177(9) 0.4752(7) 0.078(3) Uani 0.475(6) 1 d . . P B 2
H17C H 0.952596 0.689195 0.455366 0.093 Uiso 0.475(6) 1 calc R U P B 2
H17D H 0.790249 0.795927 0.487334 0.093 Uiso 0.475(6) 1 calc R U P B 2
F1 F -0.0077(4) 0.9614(3) 0.8878(4) 0.1218(13) Uani 1 1 d . . . . .
F2 F 0.2918(3) 0.1650(3) 0.9682(2) 0.0819(8) Uani 1 1 d . . . . .
Mo01 Mo 0.86451(3) 0.59468(2) 0.75281(2) 0.03026(9) Uani 1 1 d . . . . .
N1 N 0.5490(9) 0.5483(9) 0.8220(4) 0.0244(19) Uani 0.534(17) 1 d . . P A 2
N1A N 0.5210(10) 0.6169(10) 0.8118(5) 0.026(2) Uani 0.466(17) 1 d . . P A 1
O1 O 0.7348(5) 0.7574(2) 0.7314(2) 0.0648(7) Uani 1 1 d . . . . .
O2 O 0.8587(5) 0.4374(2) 0.7512(2) 0.0607(7) Uani 1 1 d . . . . .
O3 O 0.9201(3) 0.5651(2) 0.89042(18) 0.0483(6) Uani 1 1 d . . . . .
O4 O 1.0879(3) 0.6130(2) 0.6685(2) 0.0490(6) Uani 1 1 d . . . . .
O5 O 0.7244(3) 0.6351(2) 0.57825(17) 0.0425(5) Uani 1 1 d . . . . .
C18 C 0.194(2) 0.9722(12) 0.5169(10) 0.103(5) Uani 0.5 1 d D . P C -1
H18A H 0.318642 1.007654 0.496386 0.124 Uiso 0.5 1 calc R U P C -1
H18B H 0.208243 0.912306 0.592768 0.124 Uiso 0.5 1 calc R U P C -1
C19 C 0.015(2) 1.0656(11) 0.5301(10) 0.125(6) Uani 0.5 1 d D . P C -1
H19A H 0.050234 1.144969 0.504071 0.150 Uiso 0.5 1 calc R U P C -1
H19B H -0.053200 1.050211 0.609981 0.150 Uiso 0.5 1 calc R U P C -1
C20 C -0.105(3) 1.0448(14) 0.4469(11) 0.108(6) Uani 0.5 1 d D . P C -1
H20A H -0.216423 1.003727 0.491552 0.129 Uiso 0.5 1 calc R U P C -1
H20B H -0.168347 1.121589 0.397385 0.129 Uiso 0.5 1 calc R U P C -1
C21 C 0.0188(16) 0.9752(14) 0.3721(13) 0.130(5) Uani 0.5 1 d D . P C -1
H21A H -0.058809 0.920557 0.360175 0.156 Uiso 0.5 1 calc R U P C -1
H21B H 0.061723 1.026972 0.295774 0.156 Uiso 0.5 1 calc R U P C -1
O6 O 0.1868(11) 0.9141(6) 0.4317(6) 0.092(2) Uani 0.5 1 d D . P C -1


_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
C1 C2 1.394(5) . ?
C1 C6 1.410(6) . ?
C1 O1 1.333(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.359(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.375(6) . ?
C4 C5 1.367(6) . ?
C4 F1 1.355(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(7) . ?
C6 C7 1.447(9) . ?
C6 N1A 1.558(12) . ?
C7 H7 0.9500 . ?
C7 N1 1.287(15) . ?
C7A H7A 0.9500 . ?
C7A C8 1.447(10) . ?
C7A N1A 1.279(18) . ?
C8 C9 1.391(6) . ?
C8 C13 1.395(5) . ?
C8 N1 1.519(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.366(5) . ?
C10 C11 1.379(5) . ?
C10 F2 1.358(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.381(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(4) . ?
C13 O2 1.351(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.498(8) . ?
C14 O5 1.504(6) . ?
C14A H14C 0.9900 . ?
C14A H14D 0.9900 . ?
C14A C15A 1.468(10) . ?
C14A O5 1.367(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.528(17) . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C15A C16A 1.46(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.470(15) . ?
C16A H16C 0.9900 . ?
C16A H16D 0.9900 . ?
C16A C17A 1.54(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 O5 1.420(6) . ?
C17A H17C 0.9900 . ?
C17A H17D 0.9900 . ?
C17A O5 1.463(8) . ?
Mo01 N1 2.288(6) . ?
Mo01 N1A 2.298(7) . ?
Mo01 O1 1.939(3) . ?
Mo01 O2 1.933(2) . ?
Mo01 O3 1.692(2) . ?
Mo01 O4 1.702(2) . ?
Mo01 O5 2.3396(19) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.493(10) . ?
C18 O6 1.441(9) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.508(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.475(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 O6 1.389(9) . ?

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
C2 C1 C6 119.5(4) . . ?
O1 C1 C2 119.2(4) . . ?
O1 C1 C6 121.3(3) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(4) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.5(4) . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 122.6(4) . . ?
F1 C4 C3 118.4(4) . . ?
F1 C4 C5 119.0(4) . . ?
C4 C5 H5 120.7 . . ?
C4 C5 C6 118.5(4) . . ?
C6 C5 H5 120.7 . . ?
C1 C6 C7 135.2(5) . . ?
C1 C6 N1A 98.2(5) . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 C7 105.0(5) . . ?
C5 C6 N1A 141.9(5) . . ?
C6 C7 H7 122.3 . . ?
N1 C7 C6 115.4(7) . . ?
N1 C7 H7 122.3 . . ?
C8 C7A H7A 123.3 . . ?
N1A C7A H7A 123.3 . . ?
N1A C7A C8 113.5(8) . . ?
C9 C8 C7A 101.2(5) . . ?
C9 C8 C13 119.4(3) . . ?
C9 C8 N1 138.3(4) . . ?
C13 C8 C7A 139.3(5) . . ?
C13 C8 N1 102.3(4) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 C8 118.8(3) . . ?
C10 C9 H9 120.6 . . ?
C9 C10 C11 122.9(4) . . ?
F2 C10 C9 118.7(3) . . ?
F2 C10 C11 118.4(3) . . ?
C10 C11 H11 120.9 . . ?
C10 C11 C12 118.1(3) . . ?
C12 C11 H11 120.9 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.6(3) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C8 120.1(3) . . ?
O2 C13 C8 120.1(3) . . ?
O2 C13 C12 119.8(3) . . ?
H14A C14 H14B 108.8 . . ?
C15 C14 H14A 110.7 . . ?
C15 C14 H14B 110.7 . . ?
C15 C14 O5 105.2(5) . . ?
O5 C14 H14A 110.7 . . ?
O5 C14 H14B 110.7 . . ?
H14C C14A H14D 108.3 . . ?
C15A C14A H14C 110.0 . . ?
C15A C14A H14D 110.0 . . ?
O5 C14A H14C 110.0 . . ?
O5 C14A H14D 110.0 . . ?
O5 C14A C15A 108.7(6) . . ?
C14 C15 H15A 111.3 . . ?
C14 C15 H15B 111.3 . . ?
C14 C15 C16 102.2(8) . . ?
H15A C15 H15B 109.2 . . ?
C16 C15 H15A 111.3 . . ?
C16 C15 H15B 111.3 . . ?
C14A C15A H15C 110.7 . . ?
C14A C15A H15D 110.7 . . ?
H15C C15A H15D 108.8 . . ?
C16A C15A C14A 105.4(10) . . ?
C16A C15A H15C 110.7 . . ?
C16A C15A H15D 110.7 . . ?
C15 C16 H16A 110.7 . . ?
C15 C16 H16B 110.7 . . ?
H16A C16 H16B 108.8 . . ?
C17 C16 C15 105.1(10) . . ?
C17 C16 H16A 110.7 . . ?
C17 C16 H16B 110.7 . . ?
C15A C16A H16C 110.6 . . ?
C15A C16A H16D 110.6 . . ?
C15A C16A C17A 105.5(11) . . ?
H16C C16A H16D 108.8 . . ?
C17A C16A H16C 110.6 . . ?
C17A C16A H16D 110.6 . . ?
C16 C17 H17A 110.4 . . ?
C16 C17 H17B 110.4 . . ?
H17A C17 H17B 108.6 . . ?
O5 C17 C16 106.6(7) . . ?
O5 C17 H17A 110.4 . . ?
O5 C17 H17B 110.4 . . ?
C16A C17A H17C 110.9 . . ?
C16A C17A H17D 110.9 . . ?
H17C C17A H17D 108.9 . . ?
O5 C17A C16A 104.2(9) . . ?
O5 C17A H17C 110.9 . . ?
O5 C17A H17D 110.9 . . ?
N1 Mo01 O5 80.03(12) . . ?
N1A Mo01 O5 78.18(13) . . ?
O1 Mo01 N1 86.9(3) . . ?
O1 Mo01 N1A 67.1(3) . . ?
O1 Mo01 O5 79.26(10) . . ?
O2 Mo01 N1 69.3(3) . . ?
O2 Mo01 N1A 88.6(3) . . ?
O2 Mo01 O1 150.61(13) . . ?
O2 Mo01 O5 79.70(10) . . ?
O3 Mo01 N1 89.50(13) . . ?
O3 Mo01 N1A 91.10(14) . . ?
O3 Mo01 O1 97.73(12) . . ?
O3 Mo01 O2 99.12(12) . . ?
O3 Mo01 O4 105.49(10) . . ?
O3 Mo01 O5 169.22(9) . . ?
O4 Mo01 N1 162.41(17) . . ?
O4 Mo01 N1A 160.5(2) . . ?
O4 Mo01 O1 99.79(13) . . ?
O4 Mo01 O2 98.67(12) . . ?
O4 Mo01 O5 85.26(9) . . ?
C7 N1 C8 113.9(6) . . ?
C7 N1 Mo01 128.1(8) . . ?
C8 N1 Mo01 117.6(5) . . ?
C6 N1A Mo01 120.1(6) . . ?
C7A N1A C6 112.0(7) . . ?
C7A N1A Mo01 126.7(10) . . ?
C1 O1 Mo01 130.5(3) . . ?
C13 O2 Mo01 127.7(2) . . ?
C14 O5 Mo01 125.3(3) . . ?
C14A O5 C17A 110.2(5) . . ?
C14A O5 Mo01 130.8(3) . . ?
C17 O5 C14 109.2(4) . . ?
C17 O5 Mo01 124.7(3) . . ?
C17A O5 Mo01 118.8(4) . . ?
H18A C18 H18B 107.4 . . ?
C19 C18 H18A 108.3 . . ?
C19 C18 H18B 108.3 . . ?
O6 C18 H18A 108.3 . . ?
O6 C18 H18B 108.3 . . ?
O6 C18 C19 115.9(10) . . ?
C18 C19 H19A 112.7 . . ?
C18 C19 H19B 112.7 . . ?
C18 C19 C20 95.1(10) . . ?
H19A C19 H19B 110.2 . . ?
C20 C19 H19A 112.7 . . ?
C20 C19 H19B 112.7 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 C19 113.5(13) . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C20 C21 H21A 110.8 . . ?
C20 C21 H21B 110.8 . . ?
H21A C21 H21B 108.9 . . ?
O6 C21 C20 104.7(12) . . ?
O6 C21 H21A 110.8 . . ?
O6 C21 H21B 110.8 . . ?
C21 O6 C18 106.6(11) . . ?

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
C1 C2 C3 C4 0.4(7) . . . . ?
C1 C6 C7 N1 -2.4(7) . . . . ?
C1 C6 N1A C7A 177.1(4) . . . . ?
C1 C6 N1A Mo01 8.3(4) . . . . ?
C2 C1 C6 C5 3.4(5) . . . . ?
C2 C1 C6 C7 -174.8(4) . . . . ?
C2 C1 C6 N1A -178.2(3) . . . . ?
C2 C1 O1 Mo01 163.7(3) . . . . ?
C2 C3 C4 C5 1.3(8) . . . . ?
C2 C3 C4 F1 -178.1(4) . . . . ?
C3 C4 C5 C6 -0.6(7) . . . . ?
C4 C5 C6 C1 -1.8(6) . . . . ?
C4 C5 C6 C7 177.0(4) . . . . ?
C4 C5 C6 N1A -179.1(5) . . . . ?
C5 C6 C7 N1 179.1(4) . . . . ?
C5 C6 N1A C7A -5.2(8) . . . . ?
C5 C6 N1A Mo01 -174.0(4) . . . . ?
C6 C1 C2 C3 -2.8(6) . . . . ?
C6 C1 O1 Mo01 -17.5(5) . . . . ?
C6 C7 N1 C8 -179.5(3) . . . . ?
C6 C7 N1 Mo01 7.9(6) . . . . ?
C7A C8 C9 C10 -179.2(3) . . . . ?
C7A C8 C13 C12 179.1(4) . . . . ?
C7A C8 C13 O2 -2.1(6) . . . . ?
C8 C7A N1A C6 -176.9(3) . . . . ?
C8 C7A N1A Mo01 -9.0(7) . . . . ?
C8 C9 C10 C11 -0.1(5) . . . . ?
C8 C9 C10 F2 -179.2(3) . . . . ?
C8 C13 O2 Mo01 19.4(4) . . . . ?
C9 C8 C13 C12 -2.5(4) . . . . ?
C9 C8 C13 O2 176.4(3) . . . . ?
C9 C8 N1 C7 -2.4(6) . . . . ?
C9 C8 N1 Mo01 171.0(3) . . . . ?
C9 C10 C11 C12 -1.1(5) . . . . ?
C10 C11 C12 C13 0.5(5) . . . . ?
C11 C12 C13 C8 1.3(5) . . . . ?
C11 C12 C13 O2 -177.6(3) . . . . ?
C12 C13 O2 Mo01 -161.8(2) . . . . ?
C13 C8 C9 C10 1.9(5) . . . . ?
C13 C8 N1 C7 179.1(3) . . . . ?
C13 C8 N1 Mo01 -7.5(3) . . . . ?
C14 C15 C16 C17 34.5(12) . . . . ?
C14A C15A C16A C17A 21.6(14) . . . . ?
C15 C14 O5 C17 10.2(7) . . . . ?
C15 C14 O5 Mo01 -179.7(4) . . . . ?
C15 C16 C17 O5 -29.1(13) . . . . ?
C15A C14A O5 C17A 18.2(10) . . . . ?
C15A C14A O5 Mo01 -167.1(5) . . . . ?
C15A C16A C17A O5 -11.4(14) . . . . ?
C16 C17 O5 C14 12.0(10) . . . . ?
C16 C17 O5 Mo01 -158.3(9) . . . . ?
C16A C17A O5 C14A -4.1(11) . . . . ?
C16A C17A O5 Mo01 -179.5(7) . . . . ?
F1 C4 C5 C6 178.8(4) . . . . ?
F2 C10 C11 C12 178.1(3) . . . . ?
N1 C8 C9 C10 -176.4(4) . . . . ?
N1 C8 C13 C12 176.4(3) . . . . ?
N1 C8 C13 O2 -4.8(4) . . . . ?
N1A C7A C8 C9 179.3(4) . . . . ?
N1A C7A C8 C13 -2.1(7) . . . . ?
O1 C1 C2 C3 176.0(4) . . . . ?
O1 C1 C6 C5 -175.3(3) . . . . ?
O1 C1 C6 C7 6.4(6) . . . . ?
O1 C1 C6 N1A 3.0(4) . . . . ?
O5 C14 C15 C16 -26.8(10) . . . . ?
O5 C14A C15A C16A -25.2(12) . . . . ?
C18 C19 C20 C21 -16.0(14) . . . . ?
C19 C18 O6 C21 8.2(16) . . . . ?
C19 C20 C21 O6 22.3(17) . . . . ?
C20 C21 O6 C18 -17.3(16) . . . . ?
O6 C18 C19 C20 4.7(13) . . . . ?

_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.124
_oxdiff_exptl_absorpt_empirical_full_min 0.906
###end
####################################################################### 
# 
# 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_akdk23004_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 2312694'
loop_
_audit_author_name
_audit_author_address
'Adrian Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2023-12-07 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_audit_creation_date             2023-03-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H9 F6 Mo N O5, C4 H8 O'
_chemical_formula_sum            'C19 H17 F6 Mo N O6'
_chemical_formula_weight         565.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16 H11 F6 Mo1 N1 O5 C4 H8 O'
_chemical_oxdiff_usercomment     'Samuel Steinfeld  SS-038-2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.3516(3)
_cell_length_b                   14.8110(3)
_cell_length_c                   11.4468(3)
_cell_angle_alpha                90
_cell_angle_beta                 112.217(3)
_cell_angle_gamma                90
_cell_volume                     2095.56(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10337
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      76.7250
_cell_measurement_theta_min      3.5740
_shelx_estimated_absorpt_T_max   0.604
_shelx_estimated_absorpt_T_min   0.392
_exptl_absorpt_coefficient_mu    5.975
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 1 0.0391
-1 1 -1 0.0554
-1 2 0 0.0895
0 1 1 0.1012
0 -1 -1 0.0848
-1 2 1 0.0974
1 -2 -1 0.0812
0 -1 -2 0.0769
-1 -1 1 0.0325
1 1 -1 0.0614
-1 0 0 0.0324
1 1 0 0.0769
2 1 -1 0.0611

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Heptane and tetrahydrofuran'
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.094
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.1173 -1.0007 0.9997 0.1083 -0.0662 0.2251
-1.1173 1.0007 -0.9997 -0.1083 0.0662 -0.2251
-1.0003 2.0008 0.0004 -0.1905 0.1310 -0.0740
0.1170 1.0002 1.0001 -0.0822 0.0647 0.1511
-0.1170 -1.0002 -1.0001 0.0822 -0.0647 -0.1511
-0.8831 2.0004 1.0003 -0.2183 0.1071 0.0731
0.8831 -2.0004 -1.0003 0.2183 -0.1071 -0.0731
-0.2341 -0.9997 -2.0001 0.1099 -0.0409 -0.2982
-0.8827 -1.0013 0.9997 -0.0551 -0.1587 0.0610
0.8827 1.0013 -0.9997 0.0551 0.1587 -0.0610
-1.0000 -0.0003 -0.0000 -0.0817 -0.0463 -0.0820
0.9999 1.0009 0.0002 0.0273 0.1349 0.0860
1.8827 1.0016 -0.9997 0.1368 0.2050 0.0210

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6751
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.034
_diffrn_reflns_theta_max         67.034
_diffrn_reflns_theta_min         3.576
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -103.00 -63.00   0.50    1.00    --  -48.70-140.00  92.00   80
  2  ω    -86.00 -46.00   0.50    1.00    --  -48.70 129.00 -21.00   80
  3  ω    -83.00 -58.00   0.50    1.00    --  -48.70 140.00 150.00   50
  4  ω   -118.00 -71.00   0.50    1.00    --  -48.70-129.00 -94.00   94
  5  ω     43.00  68.00   0.50    1.00    --   48.70-129.00 -94.00   50
  6  ω     50.00  75.00   0.50    1.00    --   48.70-140.00  92.00   50
  7  ω     89.00 137.00   0.50    4.00    --  107.75 140.00 150.00   96
  8  ω     82.00 112.00   0.50    4.00    --  107.75-129.00 -94.00   60
  9  ω     78.00 121.00   0.50    4.00    --  107.75-140.00  92.00   86
 10  ω    101.00 154.00   0.50    4.00    --  107.75 129.00 -21.00  106
 11  ω   -117.00 -83.00   0.50    1.00    --  -48.70-125.00  30.00   68
 12  ω   -117.00 -73.00   0.50    1.00    --  -48.70-125.00 -30.00   88
 13  ω     69.00 120.00   0.50    1.00    --   48.70  77.00 150.00  102
 14  ω     15.00  80.00   0.50    1.00    --   48.70 -99.00-150.00  130
 15  ω     26.00  65.00   0.50    1.00    --   48.70  77.00 150.00   78
 16  ω     36.00  83.00   0.50    4.00    --  107.75 -57.00  30.00   94
 17  ω     98.00 158.00   0.50    4.00    --  107.75  37.00-180.00  120
 18  ω    153.00 178.00   0.50    4.00    --  107.75  57.00-120.00   50
 19  ω    143.00 170.00   0.50    4.00    --  107.75 125.00  30.00   54
 20  ω     95.00 125.00   0.50    4.00    --  107.75 125.00  30.00   60
 21  ω     37.00 105.00   0.50    4.00    --  107.75 -99.00 -60.00  136
 22  ω    100.00 143.00   0.50    4.00    --  107.75 125.00  60.00   86
 23  ω    152.00 178.00   0.50    4.00    --  107.75 125.00  60.00   52
 24  ω    102.00 129.00   0.50    4.00    --  107.75  57.00-120.00   54
 25  ω     38.00 115.00   0.50    4.00    --  107.75 -37.00  30.00  154
 26  ω    130.00 156.00   0.50    4.00    --  107.75 129.00 -21.00   52
 27  ω   -103.00 -76.00   0.50    1.00    --  -48.70-125.00   0.00   54
 28  ω     44.00  80.00   0.50    1.00    --   48.70-125.00-180.00   72
 29  ω     80.00 106.00   0.50    4.00    --  107.75 -99.00 -90.00   52
 30  ω     37.00  62.00   0.50    4.00    --  107.75 -99.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0817125000
_diffrn_orient_matrix_UB_12      -0.0543492000
_diffrn_orient_matrix_UB_13      -0.0373684000
_diffrn_orient_matrix_UB_21      0.0462275000
_diffrn_orient_matrix_UB_22      0.0885655000
_diffrn_orient_matrix_UB_23      -0.0292448000
_diffrn_orient_matrix_UB_31      0.0820077000
_diffrn_orient_matrix_UB_32      0.0040068000
_diffrn_orient_matrix_UB_33      0.1374819000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6164
_reflns_number_total             6751
_reflns_special_details          
;
 _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       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6751
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0297
_refine_ls_restrained_S_all      1.058
_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)+(0.0426P)²+1.2447P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0793
_refine_special_details          
;The ligand is disordered and modelled over two sites which required the imine to be 
modelled in two sites with refined occupancies of 0.547:0.453(4).  The ADPs of pairs
of disordered atoms were constrained to be equal (N1 & N1a, C7 & C7a).The crystal was also non-merohedrally twinned and modelled in two components with
refined occupancies of 0.5076:0.4924(8).,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5076(8)
 0.4924(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C7A) = Uanis(C7)
Uanis(N1A) = Uanis(N1)
4. Others
 Sof(C7A)=Sof(H7A)=Sof(N1A)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(N1)=FVAR(1)
5.a Rotating group:
 O3(H3A,H3B)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C7A(H7A), C9(H9), C11(H11), C12(H12)
;
_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
C1 C 0.7018(3) 0.3984(3) 0.7691(3) 0.0462(9) Uani 1 1 d . . . . .
C2 C 0.8135(3) 0.3980(2) 0.8267(3) 0.0434(8) Uani 1 1 d . . . . .
H2 H 0.851463 0.342406 0.850011 0.052 Uiso 1 1 calc R U . . .
C3 C 0.8694(3) 0.4782(2) 0.8501(3) 0.0386(8) Uani 1 1 d . . . . .
H3 H 0.946183 0.477823 0.887938 0.046 Uiso 1 1 calc R U . . .
C4 C 0.8144(3) 0.5602(2) 0.8189(3) 0.0373(7) Uani 1 1 d . . . . .
C5 C 0.7031(3) 0.5615(3) 0.7622(3) 0.0436(9) Uani 1 1 d . . . . .
H5 H 0.665877 0.617492 0.740819 0.052 Uiso 1 1 calc R U . . .
C6 C 0.6457(3) 0.4815(3) 0.7364(3) 0.0476(10) Uani 1 1 d . . . . .
C7 C 0.4659(5) 0.5153(4) 0.6398(5) 0.0246(10) Uani 0.547(4) 1 d . . P A 1
H7 H 0.487405 0.576906 0.649545 0.030 Uiso 0.547(4) 1 calc R U P A 1
C7A C 0.5285(6) 0.5131(5) 0.6739(7) 0.0246(10) Uani 0.453(4) 1 d . . P A 2
H7A H 0.509466 0.575238 0.663788 0.030 Uiso 0.453(4) 1 calc R U P A 2
C8 C 0.3478(3) 0.4874(3) 0.5784(3) 0.0513(11) Uani 1 1 d . . . . .
C9 C 0.2899(3) 0.5670(3) 0.5424(3) 0.0469(9) Uani 1 1 d . . . . .
H9 H 0.327067 0.623192 0.558075 0.056 Uiso 1 1 calc R U . . .
C10 C 0.1788(3) 0.5654(2) 0.4839(3) 0.0398(8) Uani 1 1 d . . . . .
C11 C 0.1233(3) 0.4831(2) 0.4598(3) 0.0380(7) Uani 1 1 d . . . . .
H11 H 0.046867 0.482094 0.417917 0.046 Uiso 1 1 calc R U . . .
C12 C 0.1797(3) 0.4037(3) 0.4967(4) 0.0455(8) Uani 1 1 d . . . . .
H12 H 0.142248 0.347747 0.481747 0.055 Uiso 1 1 calc R U . . .
C13 C 0.2919(3) 0.4056(3) 0.5561(4) 0.0520(11) Uani 1 1 d . . . . .
C14 C 0.8775(3) 0.6459(2) 0.8498(4) 0.0495(10) Uani 1 1 d . . . . .
C15 C 0.1157(3) 0.6511(3) 0.4502(4) 0.0531(10) Uani 1 1 d . . . . .
F1 F 0.9110(2) 0.66609(17) 0.9736(3) 0.0743(7) Uani 1 1 d . . . . .
F2 F 0.9676(2) 0.64112(17) 0.8268(3) 0.0749(8) Uani 1 1 d . . . . .
F3 F 0.8225(3) 0.71630(17) 0.7875(3) 0.0889(10) Uani 1 1 d . . . . .
F4 F 0.1733(2) 0.71999(17) 0.4355(3) 0.0869(10) Uani 1 1 d . . . . .
F5 F 0.0284(2) 0.64443(17) 0.3438(3) 0.0694(7) Uani 1 1 d . . . . .
F6 F 0.0788(2) 0.67579(17) 0.5398(3) 0.0749(8) Uani 1 1 d . . . . .
Mo1 Mo 0.49603(2) 0.29880(2) 0.64686(2) 0.02502(9) Uani 1 1 d . . . . .
N1 N 0.5345(4) 0.4509(3) 0.6775(4) 0.0215(7) Uani 0.547(4) 1 d . . P A 1
N1A N 0.4571(4) 0.4499(4) 0.6359(5) 0.0215(7) Uani 0.453(4) 1 d . . P A 2
O1 O 0.49195(19) 0.18802(13) 0.6821(2) 0.0349(5) Uani 1 1 d . . . . .
O2 O 0.5043(2) 0.30338(13) 0.5018(2) 0.0355(5) Uani 1 1 d . . . . .
O3 O 0.4905(2) 0.33045(16) 0.8378(2) 0.0440(6) Uani 1 1 d . . . . .
H3A H 0.489888 0.279048 0.882309 0.066 Uiso 1 1 d R U . . .
H3B H 0.426853 0.357741 0.830060 0.066 Uiso 1 1 d R U . . .
O4 O 0.6479(2) 0.3200(2) 0.7460(3) 0.0588(8) Uani 1 1 d . . . . .
O5 O 0.3446(2) 0.3269(2) 0.5935(3) 0.0656(9) Uani 1 1 d . . . . .
C16 C 0.2450(4) 0.4202(3) 0.8550(5) 0.0738(15) Uani 1 1 d . . . . .
H16A H 0.249373 0.390032 0.933965 0.089 Uiso 1 1 calc R U . . .
H16B H 0.210801 0.378392 0.783380 0.089 Uiso 1 1 calc R U . . .
C17 C 0.1823(4) 0.5067(5) 0.8358(5) 0.0887(19) Uani 1 1 d . . . . .
H17A H 0.133467 0.513293 0.746250 0.106 Uiso 1 1 calc R U . . .
H17B H 0.138063 0.507385 0.888458 0.106 Uiso 1 1 calc R U . . .
C18 C 0.2634(4) 0.5814(3) 0.8738(5) 0.0694(13) Uani 1 1 d . . . . .
H18A H 0.256642 0.620403 0.800927 0.083 Uiso 1 1 calc R U . . .
H18B H 0.255342 0.618941 0.941266 0.083 Uiso 1 1 calc R U . . .
C19 C 0.3685(3) 0.5321(3) 0.9204(4) 0.0513(10) Uani 1 1 d . . . . .
H19A H 0.423018 0.565528 0.898197 0.062 Uiso 1 1 calc R U . . .
H19B H 0.395689 0.525413 1.013266 0.062 Uiso 1 1 calc R U . . .
O6 O 0.3491(2) 0.44685(16) 0.8620(3) 0.0447(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.385(5) . ?
C1 C6 1.415(6) . ?
C1 O4 1.340(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.375(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.394(5) . ?
C4 C5 1.379(5) . ?
C4 C14 1.490(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.381(6) . ?
C6 C7A 1.528(8) . ?
C6 N1 1.452(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.520(7) . ?
C7 N1 1.280(8) . ?
C7A H7A 0.9500 . ?
C7A N1A 1.289(10) . ?
C8 C9 1.384(6) . ?
C8 C13 1.396(6) . ?
C8 N1A 1.464(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.378(5) . ?
C10 C11 1.398(5) . ?
C10 C15 1.491(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.374(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.391(5) . ?
C13 O5 1.345(5) . ?
C14 F1 1.348(5) . ?
C14 F2 1.327(4) . ?
C14 F3 1.319(4) . ?
C15 F4 1.326(4) . ?
C15 F5 1.333(5) . ?
C15 F6 1.346(5) . ?
Mo1 N1 2.307(4) . ?
Mo1 N1A 2.290(5) . ?
Mo1 O1 1.695(2) . ?
Mo1 O2 1.707(2) . ?
Mo1 O3 2.264(2) . ?
Mo1 O4 1.939(3) . ?
Mo1 O5 1.924(3) . ?
O3 H3A 0.9177 . ?
O3 H3B 0.9150 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.500(8) . ?
C16 O6 1.418(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.495(8) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.489(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 O6 1.407(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 119.8(3) . . ?
O4 C1 C2 119.4(4) . . ?
O4 C1 C6 120.7(3) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3 119.7 . . ?
C2 C3 C4 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C14 119.0(3) . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 C14 120.8(3) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.1(3) . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C7A 137.4(4) . . ?
C1 C6 N1 101.4(4) . . ?
C5 C6 C1 119.6(3) . . ?
C5 C6 C7A 103.0(4) . . ?
C5 C6 N1 139.0(4) . . ?
C8 C7 H7 122.0 . . ?
N1 C7 H7 122.0 . . ?
N1 C7 C8 116.0(5) . . ?
C6 C7A H7A 122.2 . . ?
N1A C7A C6 115.6(6) . . ?
N1A C7A H7A 122.2 . . ?
C9 C8 C7 105.7(4) . . ?
C9 C8 C13 119.0(3) . . ?
C9 C8 N1A 143.7(4) . . ?
C13 C8 C7 135.2(4) . . ?
C13 C8 N1A 97.2(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.5(4) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 C15 120.6(3) . . ?
C11 C10 C15 119.1(3) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11 120.1 . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.8(4) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C8 120.6(4) . . ?
O5 C13 C8 121.0(4) . . ?
O5 C13 C12 118.4(4) . . ?
F1 C14 C4 111.8(3) . . ?
F2 C14 C4 112.4(3) . . ?
F2 C14 F1 104.8(3) . . ?
F3 C14 C4 113.3(3) . . ?
F3 C14 F1 106.8(3) . . ?
F3 C14 F2 107.2(4) . . ?
F4 C15 C10 113.0(3) . . ?
F4 C15 F5 106.9(4) . . ?
F4 C15 F6 106.6(3) . . ?
F5 C15 C10 112.7(3) . . ?
F5 C15 F6 105.7(3) . . ?
F6 C15 C10 111.6(4) . . ?
O1 Mo1 N1 159.05(13) . . ?
O1 Mo1 N1A 158.68(15) . . ?
O1 Mo1 O2 106.84(10) . . ?
O1 Mo1 O3 87.42(10) . . ?
O1 Mo1 O4 97.92(12) . . ?
O1 Mo1 O5 99.24(13) . . ?
O2 Mo1 N1 90.95(12) . . ?
O2 Mo1 N1A 90.27(14) . . ?
O2 Mo1 O3 165.68(9) . . ?
O2 Mo1 O4 97.20(12) . . ?
O2 Mo1 O5 97.41(12) . . ?
O3 Mo1 N1 74.80(12) . . ?
O3 Mo1 N1A 76.17(14) . . ?
O4 Mo1 N1 68.27(15) . . ?
O4 Mo1 N1A 92.28(17) . . ?
O4 Mo1 O3 79.03(11) . . ?
O5 Mo1 N1 89.07(15) . . ?
O5 Mo1 N1A 65.25(17) . . ?
O5 Mo1 O3 81.26(12) . . ?
O5 Mo1 O4 153.14(15) . . ?
C6 N1 Mo1 120.4(3) . . ?
C7 N1 C6 113.5(5) . . ?
C7 N1 Mo1 126.0(4) . . ?
C7A N1A C8 111.1(5) . . ?
C7A N1A Mo1 124.6(5) . . ?
C8 N1A Mo1 124.2(4) . . ?
Mo1 O3 H3A 112.0 . . ?
Mo1 O3 H3B 111.5 . . ?
H3A O3 H3B 102.5 . . ?
C1 O4 Mo1 128.4(3) . . ?
C13 O5 Mo1 130.5(3) . . ?
H16A C16 H16B 108.9 . . ?
C17 C16 H16A 110.8 . . ?
C17 C16 H16B 110.8 . . ?
O6 C16 H16A 110.8 . . ?
O6 C16 H16B 110.8 . . ?
O6 C16 C17 104.6(4) . . ?
C16 C17 H17A 110.4 . . ?
C16 C17 H17B 110.4 . . ?
H17A C17 H17B 108.6 . . ?
C18 C17 C16 106.7(4) . . ?
C18 C17 H17A 110.4 . . ?
C18 C17 H17B 110.4 . . ?
C17 C18 H18A 111.2 . . ?
C17 C18 H18B 111.2 . . ?
H18A C18 H18B 109.1 . . ?
C19 C18 C17 102.8(4) . . ?
C19 C18 H18A 111.2 . . ?
C19 C18 H18B 111.2 . . ?
C18 C19 H19A 110.3 . . ?
C18 C19 H19B 110.3 . . ?
H19A C19 H19B 108.6 . . ?
O6 C19 C18 106.9(4) . . ?
O6 C19 H19A 110.3 . . ?
O6 C19 H19B 110.3 . . ?
C19 O6 C16 106.1(3) . . ?

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
O3 H3A O2 0.92 1.79 2.688(3) 165.8 4_566 yes
O3 H3B O6 0.91 1.80 2.648(3) 152.9 . 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
C1 C2 C3 C4 1.4(6) . . . . ?
C1 C6 C7A N1A -1.9(9) . . . . ?
C1 C6 N1 C7 179.4(4) . . . . ?
C1 C6 N1 Mo1 -4.7(4) . . . . ?
C2 C1 C6 C5 0.1(5) . . . . ?
C2 C1 C6 C7A 179.6(5) . . . . ?
C2 C1 C6 N1 178.6(3) . . . . ?
C2 C1 O4 Mo1 -170.4(3) . . . . ?
C2 C3 C4 C5 -1.0(6) . . . . ?
C2 C3 C4 C14 177.9(4) . . . . ?
C3 C4 C5 C6 0.1(5) . . . . ?
C3 C4 C14 F1 -76.5(4) . . . . ?
C3 C4 C14 F2 41.1(5) . . . . ?
C3 C4 C14 F3 162.8(4) . . . . ?
C4 C5 C6 C1 0.3(5) . . . . ?
C4 C5 C6 C7A -179.4(4) . . . . ?
C4 C5 C6 N1 -177.5(4) . . . . ?
C5 C4 C14 F1 102.4(4) . . . . ?
C5 C4 C14 F2 -140.1(4) . . . . ?
C5 C4 C14 F3 -18.3(5) . . . . ?
C5 C6 C7A N1A 177.7(5) . . . . ?
C5 C6 N1 C7 -2.6(7) . . . . ?
C5 C6 N1 Mo1 173.3(4) . . . . ?
C6 C1 C2 C3 -1.0(5) . . . . ?
C6 C1 O4 Mo1 10.2(5) . . . . ?
C6 C7A N1A C8 179.7(4) . . . . ?
C6 C7A N1A Mo1 -3.4(8) . . . . ?
C7 C8 C9 C10 -179.5(4) . . . . ?
C7 C8 C13 C12 179.2(4) . . . . ?
C7 C8 C13 O5 0.6(7) . . . . ?
C8 C7 N1 C6 -179.4(4) . . . . ?
C8 C7 N1 Mo1 5.0(6) . . . . ?
C8 C9 C10 C11 -0.3(6) . . . . ?
C8 C9 C10 C15 177.2(4) . . . . ?
C8 C13 O5 Mo1 -14.9(5) . . . . ?
C9 C8 C13 C12 1.0(5) . . . . ?
C9 C8 C13 O5 -177.7(3) . . . . ?
C9 C8 N1A C7A 4.6(9) . . . . ?
C9 C8 N1A Mo1 -172.3(4) . . . . ?
C9 C10 C11 C12 1.3(6) . . . . ?
C9 C10 C15 F4 24.6(6) . . . . ?
C9 C10 C15 F5 145.9(4) . . . . ?
C9 C10 C15 F6 -95.4(4) . . . . ?
C10 C11 C12 C13 -1.1(6) . . . . ?
C11 C10 C15 F4 -157.8(4) . . . . ?
C11 C10 C15 F5 -36.6(5) . . . . ?
C11 C10 C15 F6 82.2(4) . . . . ?
C11 C12 C13 C8 -0.1(6) . . . . ?
C11 C12 C13 O5 178.6(3) . . . . ?
C12 C13 O5 Mo1 166.3(3) . . . . ?
C13 C8 C9 C10 -0.8(5) . . . . ?
C13 C8 N1A C7A -176.4(5) . . . . ?
C13 C8 N1A Mo1 6.7(4) . . . . ?
C14 C4 C5 C6 -178.7(3) . . . . ?
C15 C10 C11 C12 -176.3(4) . . . . ?
N1 C7 C8 C9 -178.3(4) . . . . ?
N1 C7 C8 C13 3.4(8) . . . . ?
N1A C8 C9 C10 178.0(5) . . . . ?
N1A C8 C13 C12 -178.3(4) . . . . ?
N1A C8 C13 O5 3.0(5) . . . . ?
O4 C1 C2 C3 179.7(3) . . . . ?
O4 C1 C6 C5 179.4(3) . . . . ?
O4 C1 C6 C7A -1.1(7) . . . . ?
O4 C1 C6 N1 -2.1(4) . . . . ?
C16 C17 C18 C19 -3.5(5) . . . . ?
C17 C16 O6 C19 33.6(5) . . . . ?
C17 C18 C19 O6 24.2(5) . . . . ?
C18 C19 O6 C16 -37.0(5) . . . . ?
O6 C16 C17 C18 -17.9(6) . . . . ?

_olex2_date_sample_data_collection 2023-02-28
_olex2_date_sample_submission    2023-02-24
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id SS-038-2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.157
_oxdiff_exptl_absorpt_empirical_full_min 0.887
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5076(8) 9975 5772 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4924(8) 9970 5772 nmt -0.9999 0.0002 -0.8831 -0.0002 -1.0000 -0.0006
-0.0001 -0.0002 0.9999

_twin_special_details            
;
Component 2 rotated by -179.9899° 
around [-0.40 0.00 0.91] (reciprocal) or [-0.00 -0.00 1.00] (direct)
;
