# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2023

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

data_mof199-pmo10v2_chiral
_database_code_depnum_ccdc_archive 'CCDC 2256821'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2023-04-15 deposited with the CCDC.	2023-07-18 downloaded from the CCDC.
;
_audit_creation_date             2023-04-15
_audit_creation_method           
;
Olex2 1.5-alpha
(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         
'Mo10 O40 P V2, C72 H48 Cu12 O60, 5(C4 H12 N), 16(O)'
_chemical_formula_sum            'C92 H108 Cu12 Mo10 N5 O116 P V2'
_chemical_formula_weight         4994.56
_chemical_absolute_configuration unk
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C288  H192  Cu48  Mo48  O416  P4  '
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'
Cu Cu -1.9646 0.5888 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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      cubic
_space_group_IT_number           196
_space_group_name_H-M_alt        'F 2 3'
_space_group_name_Hall           'F 2 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'

_cell_length_a                   26.2487(4)
_cell_length_b                   26.2487(4)
_cell_length_c                   26.2487(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18085.2(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2078
_cell_measurement_temperature    106(9)
_cell_measurement_theta_max      74.4830
_cell_measurement_theta_min      3.3820
_shelx_estimated_absorpt_T_max   0.578
_shelx_estimated_absorpt_T_min   0.373
_exptl_absorpt_coefficient_mu    8.780
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.74a (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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             9808
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -4 -16 0.0555
-2 -10 14 0.0222
-14 6 7 0.0665
-1 2 1 0.0683
2 -1 2 0.0539
1 1 -1 0.0320
0 0 1 0.0550
1 1 2 0.0595
-2 -1 0 0.0370
-2 2 -5 0.0465
1 0 1 0.0470
0 0 -1 0.0579
-2 0 -1 0.0444
-4 3 5 0.0671
-7 -14 -7 0.0539
0 -1 0 0.0626
-1 -1 -1 0.0494
8 0 -15 0.0607
-2 -2 1 0.0307
17 -4 -1 0.0661
-12 0 -12 0.0444
11 -13 1 0.0686
-10 14 0 0.0667
0 -1 1 0.0350
0 1 0 0.0602
1 1 1 0.0537
1 17 3 0.0588
16 2 -5 0.0517
7 -13 -8 0.0699
-2 -1 -1 0.0337
9 -8 -12 0.0666
-2 17 4 0.0605
-1 -8 -15 0.0615
-1 -3 5 0.0248
-1 -2 1 0.0324
1 2 -1 0.0419

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
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
-4.5090 -4.4121 -15.8414 0.0244 0.0907 0.9956
-1.7210 -9.7945 13.8157 -0.5233 -0.6853 -0.5065
-14.0849 6.4917 7.0418 0.7086 -0.6703 -0.2203
-1.0059 1.9981 1.0102 0.1233 -0.0223 -0.0708
1.9956 -1.0071 1.9986 -0.1244 0.0151 -0.1237
1.0001 1.0048 -0.9901 0.0255 0.0973 0.0140
-0.0026 -0.0034 0.9997 -0.0067 -0.0261 -0.0521
0.9923 0.9945 2.0090 0.0055 0.0189 -0.1424
-1.9969 -1.0017 -0.0125 0.0119 -0.1174 0.0574
-1.9897 2.0183 -4.9910 0.1941 0.0883 0.2610
0.9968 -0.0031 1.0026 -0.0374 0.0200 -0.0713
0.0026 0.0034 -0.9997 0.0067 0.0261 0.0521
-1.9963 0.0027 -1.0055 0.0682 -0.0662 0.0905
-4.0165 2.9842 5.0070 0.2385 -0.2403 -0.2406
-6.5033 -14.1914 -6.8833 -0.4577 -0.4810 0.7478
0.0019 -1.0010 -0.0067 -0.0496 -0.0250 0.0190
-0.9949 -0.9979 -1.0093 -0.0122 -0.0451 0.0903
7.6408 -0.1120 -15.2223 -0.1404 0.7454 0.6516
-1.9976 -2.0061 0.9805 -0.0444 -0.1685 0.0242
16.5050 -4.1405 -0.5171 -0.7095 0.6725 -0.2104
-11.7833 0.2693 -12.2999 0.4568 -0.2195 0.8621
10.7720 -13.1184 1.4486 -0.9909 0.1295 -0.0367
-10.2951 13.5762 -0.1619 0.9904 -0.1292 -0.0481
-0.0007 -1.0044 0.9930 -0.0563 -0.0512 -0.0332
-0.0019 1.0010 0.0067 0.0496 0.0250 -0.0190
0.9949 0.9979 1.0093 0.0122 0.0451 -0.0903
1.4147 16.7907 2.6452 0.7710 0.4211 -0.4778
16.2799 1.7838 -4.6377 -0.3820 0.9186 -0.1012
7.4742 -13.3682 -7.5032 -0.8429 0.2027 0.4984
-1.9943 -0.9983 -1.0122 0.0186 -0.0913 0.1095
9.3528 -7.6140 -12.0463 -0.5857 0.5528 0.5928
-1.5971 16.6073 3.5516 0.8486 0.2536 -0.4643
-1.3480 -8.0820 -14.9633 -0.2605 0.1214 0.9578
-1.0066 -3.0204 4.9756 -0.1514 -0.2519 -0.1845
-0.9982 -2.0057 0.9834 -0.0751 -0.1224 0.0050
0.9982 2.0057 -0.9834 0.0751 0.1224 -0.0050

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10093
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.486
_diffrn_reflns_theta_min         2.916
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      106(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -160.00 -76.00   0.50   27.29    --  -88.50 -91.00-127.00  168
  2  ω   -119.00 -70.00   0.50    6.82    --  -47.12-125.00-180.00   98
  3  ω   -119.00 -72.00   0.50    6.82    --  -47.12-125.00-120.00   94
  4  ω     35.00  81.00   0.50   27.29    --  105.44 -61.00-150.00   92
  5  ω    114.00 160.00   0.50   27.29    --  107.31  99.00 176.00   92
  6  ω    -98.00 -71.00   0.50    6.82    --  -47.12-125.00-120.00   54
  7  ω    -82.00 -54.00   0.50   27.29    --  -88.50  45.00-180.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0307655000
_diffrn_orient_matrix_UB_12      0.0495461000
_diffrn_orient_matrix_UB_13      -0.0065819000
_diffrn_orient_matrix_UB_21      0.0462720000
_diffrn_orient_matrix_UB_22      0.0252635000
_diffrn_orient_matrix_UB_23      -0.0259297000
_diffrn_orient_matrix_UB_31      -0.0190582000
_diffrn_orient_matrix_UB_32      -0.0186215000
_diffrn_orient_matrix_UB_33      -0.0522360000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                2461
_reflns_number_total             2902
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     182
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0552
_refine_ls_restrained_S_all      1.050
_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)+(0.1151P)²+40.7463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1682
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.51(4)
 0.49(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.955 with sigma of 0.001
 N1_1-C1_1 = N1_1-C3_1 = N1_1-C2_1 = N1_1-C4_1
 1.5 with sigma of 0.01
 C5-C4 \\sim C2-C1
 with sigma of 0.002
 O1-C5 \\sim O10-C2
 with sigma of 0.002
 C3-C2 \\sim C6-C5
 with sigma of 0.002
 O4-C1 \\sim O2-C4
 with sigma of 0.002
 O10-C1 \\sim O1-C4
 with sigma of 0.002
 N1_1-C1_1 \\sim N1_1-C2_1 \\sim N1_1-C3_1 \\sim N1_1-C4_1
 with sigma of 0.02
 N1_1-C1_1 \\sim N1_1-C4_1 \\sim N1_1-C3_1 \\sim N1_1-C2_1
 with sigma of 0.002
 C3_1-C2_1 \\sim C4_1-C2_1 \\sim C2_1-C1_1 \\sim C4_1-C3_1 \\sim C3_1-C1_1
\\sim C4_1-C1_1
 with sigma of 0.002
 C1_1-C3_1 \\sim C1_1-C2_1 \\sim C1_1-C4_1 \\sim C2_1-C3_1 \\sim C2_1-C4_1
\\sim C3_1-C4_1
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
Uanis(Mo1) \\sim Ueq, Uanis(V1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1_1) \\sim Ueq, Uanis(N1_1) \\sim Ueq, Uanis(C4_1) \\sim Ueq, Uanis(O2W)
\\sim Ueq, Uanis(O3W) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(Mo1) = Uanis(V1)
Uanis(C2) = Uanis(C5)
Uanis(C4) = Uanis(C1)
Uanis(C6) = Uanis(C3)
Uanis(O2W) = Uanis(C4_1)
Uanis(C3_1) = Uanis(C2_1) = Uanis(C1_1) = Uanis(C4_1)
5. Rigid body (RIGU) restrains
 O10, C1, O4, C2, C3
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C4, O2, C5, C6
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 N1T, C1T
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 N1_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4_1, N1_1, C1_1, C2_1, C3_1
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
6. Others
 Fixed Sof: Mo1(0.833333) V1(0.166667) H1TA(0.333333) H1TB(0.333333)
 H1TC(0.333333) O3W(0.666667) O2W(0.666667) N1(0.333333) C1(0.333333)
 H1A(0.333333) H1B(0.333333) H1C(0.333333) C2(0.333333) H2A(0.333333)
 H2B(0.333333) H2C(0.333333) C3(0.333333) H3A(0.333333) H3B(0.333333)
 H3C(0.333333) C4(0.333333) H4A(0.333333) H4B(0.333333) H4C(0.333333)
 Fixed X: H1WA(0.385921) H1WB(0.387409)
 Fixed Y: H1WA(0.61461) H1WB(0.613111)
 Fixed Z: H1WA(0.274639) H1WB(0.21715)
7.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6)
7.c Idealised Me refined as rotating group:
 C1T(H1TA,H1TB,H1TC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.34573(12) 0.34554(14) 0.25044(16) 0.0679(5) Uani 0.8333 1 d . U P A 1
V1 V 0.3395(16) 0.3423(18) 0.2443(16) 0.0679(5) Uani 0.1667 1 d . U P A 2
Cu1 Cu 0.46437(3) 0.53563(3) 0.24997(10) 0.0473(3) Uani 1 1 d . . . . .
P1 P 0.250000 0.250000 0.250000 0.0441(11) Uani 1 12 d S T P . .
C2 C 0.4275(5) 0.4270(5) 0.3611(4) 0.0550(7) Uani 1 1 d D . . . .
O4 O 0.4922(3) 0.4312(3) 0.3022(4) 0.059(2) Uani 1 1 d D . . . .
O1 O 0.4335(3) 0.4928(4) 0.1966(4) 0.069(3) Uani 1 1 d D . . . .
O10 O 0.4320(3) 0.4941(3) 0.3023(3) 0.0529(16) Uani 1 1 d D . . . .
O2 O 0.4946(3) 0.4344(3) 0.1968(4) 0.061(2) Uani 1 1 d D . . . .
C4 C 0.4534(4) 0.4524(4) 0.1798(5) 0.0546(7) Uani 1 1 d D . . . .
C3 C 0.3853(5) 0.4476(5) 0.3832(6) 0.0550(9) Uani 1 1 d D . . . .
H3 H 0.369418 0.481096 0.366368 0.066 Uiso 1 1 calc R U . . .
O6 O 0.3730(7) 0.3007(5) 0.3000(6) 0.102(6) Uani 1 1 d . . . . .
O9 O 0.3897(3) 0.3900(3) 0.2500(7) 0.095(3) Uani 1 1 d . . . . .
O1W O 0.4025(3) 0.5982(3) 0.24671(5) 0.109(3) Uani 1 1 d D . . . .
H1WA H 0.385921 0.614610 0.274639 0.163 Uiso 1 1 d D U . . .
H1WB H 0.387409 0.613111 0.217150 0.163 Uiso 1 1 d D U . . .
O8 O 0.2834(2) 0.2834(2) 0.2166(2) 0.050(2) Uani 1 3 d S T P . .
O7 O 0.2999(6) 0.3689(6) 0.2010(6) 0.107(6) Uani 1 1 d . . . . .
C6 C 0.4499(4) 0.3842(6) 0.1184(6) 0.0550(9) Uani 1 1 d D . . . .
H6 H 0.483580 0.368590 0.135095 0.066 Uiso 1 1 calc R U . . .
C1T C 0.4656(6) 0.5344(6) 0.4656(6) 0.091(6) Uani 1 3 d S T P . .
H1TA H 0.486292 0.568405 0.455238 0.136 Uiso 0.3333 1 calc R U P B -1
H1TB H 0.431595 0.544762 0.486292 0.136 Uiso 0.3333 1 calc R U P B -1
H1TC H 0.455238 0.513708 0.431595 0.136 Uiso 0.3333 1 calc R U P B -1
C1 C 0.4521(4) 0.4531(4) 0.3172(5) 0.0546(7) Uani 1 1 d D . . . .
O3W O 0.4846(8) 0.2516(11) 0.3291(5) 0.143(7) Uani 0.6667 1 d . U P C -2
C5 C 0.4261(5) 0.4262(5) 0.1376(4) 0.0550(7) Uani 1 1 d D . . . .
N1T N 0.500000 0.500000 0.500000 0.098(9) Uani 1 12 d S T P . .
O2W O 0.4844(6) 0.3298(6) 0.2476(10) 0.126(4) Uani 0.6667 1 d . U P D -2
N1_1 N 0.5160(7) 0.2487(8) 0.2507(9) 0.126(4) Uani 0.3333 1 d D U P E -1
C1_1 C 0.5722(7) 0.2453(15) 0.2418(14) 0.126(4) Uani 0.3333 1 d D U P E -1
H1A_1 H 0.579164 0.219790 0.215431 0.189 Uiso 0.3333 1 calc R U P E -1
H1B_1 H 0.585101 0.278524 0.230669 0.189 Uiso 0.3333 1 calc R U P E -1
H1C_1 H 0.589270 0.235344 0.273509 0.189 Uiso 0.3333 1 calc R U P E -1
C2_1 C 0.4900(13) 0.2639(13) 0.2023(11) 0.126(4) Uani 0.3333 1 d D . P E -1
H2A_1 H 0.497650 0.235754 0.173202 0.189 Uiso 0.3333 1 calc R U P E -1
H2B_1 H 0.449449 0.266306 0.208667 0.189 Uiso 0.3333 1 calc R U P E -1
H2C_1 H 0.504201 0.300482 0.189991 0.189 Uiso 0.3333 1 calc R U P E -1
C3_1 C 0.4964(13) 0.1979(10) 0.2677(13) 0.126(4) Uani 0.3333 1 d D . P E -1
H3A_1 H 0.504022 0.169812 0.238625 0.189 Uiso 0.3333 1 calc R U P E -1
H3B_1 H 0.515171 0.186951 0.302628 0.189 Uiso 0.3333 1 calc R U P E -1
H3C_1 H 0.455823 0.200340 0.274113 0.189 Uiso 0.3333 1 calc R U P E -1
C4_1 C 0.5054(13) 0.2876(11) 0.2910(12) 0.126(4) Uani 0.3333 1 d D U P E -1
H4A_1 H 0.464878 0.290057 0.297378 0.189 Uiso 0.3333 1 calc R U P E -1
H4B_1 H 0.524217 0.276653 0.325904 0.189 Uiso 0.3333 1 calc R U P E -1
H4C_1 H 0.519622 0.324240 0.278693 0.189 Uiso 0.3333 1 calc R U P E -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
Mo1 O6 1.924(14) 5 ?
Mo1 O6 1.896(14) . ?
Mo1 O9 1.641(6) . ?
Mo1 O8 2.474(6) . ?
Mo1 O7 1.872(14) . ?
Mo1 O7 1.901(14) 23 ?
V1 O6 1.98(5) 5 ?
V1 O6 2.03(5) . ?
V1 O9 1.82(4) . ?
V1 O8 2.26(4) . ?
V1 O7 1.69(5) . ?
V1 O7 1.80(5) 23 ?
Cu1 Cu1 2.6451(16) 2_665 ?
Cu1 O4 1.984(10) 2_665 ?
Cu1 O1 1.971(9) . ?
Cu1 O10 1.949(9) . ?
Cu1 O2 1.931(9) 2_665 ?
Cu1 O1W 2.3112(18) . ?
P1 O8 1.520(11) 38 ?
P1 O8 1.520(11) 16 ?
P1 O8 1.520(11) . ?
P1 O8 1.520(11) 27 ?
C2 C3 1.361(17) . ?
C2 C3 1.41(2) 9 ?
C2 C1 1.488(7) . ?
O4 C1 1.263(6) . ?
O1 C4 1.260(6) . ?
O10 C1 1.261(6) . ?
O2 C4 1.262(6) . ?
C4 C5 1.489(7) . ?
C3 H3 1.0700 . ?
O1W H1WA 0.9552(14) . ?
O1W H1WB 0.9552(14) . ?
C6 H6 1.0700 . ?
C6 C5 1.441(19) 23 ?
C6 C5 1.362(17) . ?
C1T H1TA 1.0801 . ?
C1T H1TB 1.0801 . ?
C1T H1TC 1.0801 . ?
C1T N1T 1.56(3) . ?
N1_1 C1_1 1.497(7) . ?
N1_1 C2_1 1.497(7) . ?
N1_1 C3_1 1.497(7) . ?
N1_1 C4_1 1.497(7) . ?
C1_1 H1A_1 0.9800 . ?
C1_1 H1B_1 0.9800 . ?
C1_1 H1C_1 0.9800 . ?
C2_1 H2A_1 1.0800 . ?
C2_1 H2B_1 1.0800 . ?
C2_1 H2C_1 1.0800 . ?
C3_1 H3A_1 1.0800 . ?
C3_1 H3B_1 1.0800 . ?
C3_1 H3C_1 1.0800 . ?
C4_1 H4A_1 1.0800 . ?
C4_1 H4B_1 1.0800 . ?
C4_1 H4C_1 1.0800 . ?

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
O6 Mo1 O6 90.0(7) . 5 ?
O6 Mo1 O8 95.0(6) . . ?
O6 Mo1 O8 94.6(6) 5 . ?
O6 Mo1 O7 87.5(4) . 23 ?
O9 Mo1 O6 100.5(8) . . ?
O9 Mo1 O6 100.2(9) . 5 ?
O9 Mo1 O8 158.5(7) . . ?
O9 Mo1 O7 103.1(8) . 23 ?
O9 Mo1 O7 102.3(8) . . ?
O7 Mo1 O6 157.2(5) . . ?
O7 Mo1 O6 87.2(4) . 5 ?
O7 Mo1 O6 156.6(5) 23 5 ?
O7 Mo1 O8 62.8(5) . . ?
O7 Mo1 O8 62.5(5) 23 . ?
O7 Mo1 O7 86.3(9) . 23 ?
O6 V1 O6 84.7(18) 5 . ?
O6 V1 O8 100.2(18) 5 . ?
O6 V1 O8 98(2) . . ?
O9 V1 O6 92(2) . 5 ?
O9 V1 O6 89.9(17) . . ?
O9 V1 O8 166(3) . . ?
O7 V1 O6 91(2) . 5 ?
O7 V1 O6 165(3) 23 5 ?
O7 V1 O6 167(2) . . ?
O7 V1 O6 86(2) 23 . ?
O7 V1 O9 100(2) 23 . ?
O7 V1 O9 102(3) . . ?
O7 V1 O8 68.8(15) 23 . ?
O7 V1 O8 70.4(14) . . ?
O7 V1 O7 95(2) . 23 ?
O4 Cu1 Cu1 84.5(2) 2_665 2_665 ?
O4 Cu1 O1W 96.7(3) 2_665 . ?
O1 Cu1 Cu1 83.5(3) . 2_665 ?
O1 Cu1 O4 167.9(4) . 2_665 ?
O1 Cu1 O1W 95.2(3) . . ?
O10 Cu1 Cu1 85.0(2) . 2_665 ?
O10 Cu1 O4 90.5(4) . 2_665 ?
O10 Cu1 O1 90.1(3) . . ?
O10 Cu1 O1W 96.8(3) . . ?
O2 Cu1 Cu1 83.9(2) 2_665 2_665 ?
O2 Cu1 O4 90.0(3) 2_665 2_665 ?
O2 Cu1 O1 87.0(5) 2_665 . ?
O2 Cu1 O10 168.7(4) 2_665 . ?
O2 Cu1 O1W 94.4(3) 2_665 . ?
O1W Cu1 Cu1 177.85(9) . 2_665 ?
O8 P1 O8 109.5 16 27 ?
O8 P1 O8 109.471(1) . 27 ?
O8 P1 O8 109.471(1) 38 27 ?
O8 P1 O8 109.471(2) . 16 ?
O8 P1 O8 109.471(1) 38 16 ?
O8 P1 O8 109.5 . 38 ?
C3 C2 C3 115.7(13) . 9 ?
C3 C2 C1 120.1(9) . . ?
C3 C2 C1 124.0(11) 9 . ?
C1 O4 Cu1 119.6(7) . 2_665 ?
C4 O1 Cu1 124.0(6) . . ?
C1 O10 Cu1 120.9(6) . . ?
C4 O2 Cu1 125.6(7) . 2_665 ?
O1 C4 O2 123.0(8) . . ?
O1 C4 C5 116.8(5) . . ?
O2 C4 C5 120.1(8) . . ?
C2 C3 C2 124.3(13) . 5 ?
C2 C3 H3 117.9 5 . ?
C2 C3 H3 117.9 . . ?
Mo1 O6 Mo1 135.4(10) . 9 ?
Mo1 O6 V1 7.0(11) 9 9 ?
Mo1 O6 V1 132.1(16) . 9 ?
V1 O6 V1 127(2) 9 . ?
Cu1 O1W H1WA 127.76(13) . . ?
Cu1 O1W H1WB 127.79(13) . . ?
H1WA O1W H1WB 104.45(15) . . ?
Mo1 O8 Mo1 92.2(3) . 23 ?
Mo1 O8 Mo1 92.2(3) . 32 ?
Mo1 O8 Mo1 92.2(3) 23 32 ?
V1 O8 Mo1 91.7(13) . 23 ?
V1 O8 Mo1 2.6(13) 32 32 ?
V1 O8 Mo1 91.7(13) 23 32 ?
V1 O8 Mo1 2.6(13) 23 23 ?
V1 O8 Mo1 89.7(13) . 32 ?
V1 O8 Mo1 89.7(13) 32 23 ?
V1 O8 V1 89.1(16) 23 32 ?
V1 O8 V1 89.1(16) . 32 ?
P1 O8 Mo1 123.7(2) . 32 ?
P1 O8 Mo1 123.7(2) . . ?
P1 O8 Mo1 123.7(2) . 23 ?
P1 O8 V1 125.9(11) . 23 ?
P1 O8 V1 125.9(12) . 32 ?
P1 O8 V1 125.9(11) . . ?
Mo1 O7 Mo1 141.9(10) . 32 ?
V1 O7 Mo1 136.7(18) . 32 ?
V1 O7 Mo1 6.9(12) 32 32 ?
V1 O7 V1 130(2) . 32 ?
C5 C6 H6 122.5 23 . ?
C5 C6 H6 122.5 . . ?
C5 C6 C5 115.0(11) . 23 ?
H1TA C1T H1TB 109.5 . . ?
H1TA C1T H1TC 109.5 . . ?
H1TB C1T H1TC 109.5 . . ?
N1T C1T H1TA 109.5 . . ?
N1T C1T H1TB 109.5 . . ?
N1T C1T H1TC 109.5 . . ?
O4 C1 C2 113.3(8) . . ?
O10 C1 C2 116.8(5) . . ?
O10 C1 O4 129.8(9) . . ?
C6 C5 C4 119.0(9) 32 . ?
C6 C5 C4 115.5(11) . . ?
C6 C5 C6 124.9(12) . 32 ?
C1T N1T C1T 109.471(2) . 2_665 ?
C1T N1T C1T 109.471(1) 4_566 2_665 ?
C1T N1T C1T 109.471(9) . 3_656 ?
C1T N1T C1T 109.471(10) 3_656 2_665 ?
C1T N1T C1T 109.5 . 4_566 ?
C1T N1T C1T 109.471(1) 3_656 4_566 ?
C1_1 N1_1 C2_1 109.46(16) . . ?
C1_1 N1_1 C3_1 109.46(16) . . ?
C2_1 N1_1 C3_1 109.49(16) . . ?
C4_1 N1_1 C1_1 109.47(16) . . ?
C4_1 N1_1 C2_1 109.48(16) . . ?
C4_1 N1_1 C3_1 109.48(16) . . ?
N1_1 C1_1 H1A_1 109.5 . . ?
N1_1 C1_1 H1B_1 109.5 . . ?
N1_1 C1_1 H1C_1 109.5 . . ?
H1A_1 C1_1 H1B_1 109.5 . . ?
H1A_1 C1_1 H1C_1 109.5 . . ?
H1B_1 C1_1 H1C_1 109.5 . . ?
N1_1 C2_1 H2A_1 109.5 . . ?
N1_1 C2_1 H2B_1 109.5 . . ?
N1_1 C2_1 H2C_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
N1_1 C3_1 H3A_1 109.5 . . ?
N1_1 C3_1 H3B_1 109.5 . . ?
N1_1 C3_1 H3C_1 109.5 . . ?
H3A_1 C3_1 H3B_1 109.5 . . ?
H3A_1 C3_1 H3C_1 109.5 . . ?
H3B_1 C3_1 H3C_1 109.5 . . ?
N1_1 C4_1 H4A_1 109.5 . . ?
N1_1 C4_1 H4B_1 109.5 . . ?
N1_1 C4_1 H4C_1 109.5 . . ?
H4A_1 C4_1 H4B_1 109.5 . . ?
H4A_1 C4_1 H4C_1 109.5 . . ?
H4B_1 C4_1 H4C_1 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O4 C1 C2 -172.3(9) 2_665 . . . ?
Cu1 O4 C1 O10 4(2) 2_665 . . . ?
Cu1 O1 C4 O2 2(2) . . . . ?
Cu1 O1 C4 C5 -176.9(10) . . . . ?
Cu1 O10 C1 C2 173.6(9) . . . . ?
Cu1 O10 C1 O4 -3(2) . . . . ?
Cu1 O2 C4 O1 -1(2) 2_665 . . . ?
Cu1 O2 C4 C5 178.3(11) 2_665 . . . ?
O1 C4 C5 C6 176.7(15) . . . . ?
O1 C4 C5 C6 5(2) . . . 32 ?
O2 C4 C5 C6 -174.5(15) . . . 32 ?
O2 C4 C5 C6 -3(2) . . . . ?
C3 C2 C3 C2 -1(3) 9 . . 5 ?
C3 C2 C1 O4 176.7(14) . . . . ?
C3 C2 C1 O4 2(2) 9 . . . ?
C3 C2 C1 O10 -174.3(14) 9 . . . ?
C3 C2 C1 O10 0(2) . . . . ?
O6 Mo1 O6 Mo1 54.8(16) 5 . . 9 ?
O6 Mo1 O7 Mo1 -22(3) . . . 32 ?
O6 Mo1 O7 Mo1 -105.6(17) 5 . . 32 ?
O6 V1 O7 V1 -113(3) 5 . . 32 ?
O6 V1 O7 V1 -44(15) . . . 32 ?
O9 Mo1 O6 Mo1 155.2(12) . . . 9 ?
O9 Mo1 O7 Mo1 154.6(15) . . . 32 ?
O9 V1 O7 V1 154(3) . . . 32 ?
O8 Mo1 O6 Mo1 -39.8(12) . . . 9 ?
O8 Mo1 O7 Mo1 -8.9(12) . . . 32 ?
O8 V1 O7 V1 -13(3) . . . 32 ?
O8 P1 O8 Mo1 60.11(12) 16 . . 23 ?
O8 P1 O8 Mo1 -179.89(12) 16 . . 32 ?
O8 P1 O8 Mo1 -59.89(12) 27 . . 32 ?
O8 P1 O8 Mo1 -59.89(12) 38 . . 23 ?
O8 P1 O8 Mo1 -179.90(12) 38 . . . ?
O8 P1 O8 Mo1 -179.89(12) 27 . . 23 ?
O8 P1 O8 Mo1 -59.90(12) 16 . . . ?
O8 P1 O8 Mo1 60.10(12) 27 . . . ?
O8 P1 O8 Mo1 60.11(12) 38 . . 32 ?
O8 P1 O8 V1 178.4(16) 38 . . . ?
O8 P1 O8 V1 58.4(16) 16 . . 23 ?
O8 P1 O8 V1 178.4(16) 16 . . 32 ?
O8 P1 O8 V1 -61.6(16) 16 . . . ?
O8 P1 O8 V1 178.4(16) 27 . . 23 ?
O8 P1 O8 V1 58.4(16) 27 . . . ?
O8 P1 O8 V1 -61.6(16) 27 . . 32 ?
O8 P1 O8 V1 -61.6(16) 38 . . 23 ?
O8 P1 O8 V1 58.4(16) 38 . . 32 ?
O7 Mo1 O6 Mo1 -28(3) . . . 9 ?
O7 Mo1 O6 Mo1 -101.9(14) 23 . . 9 ?
O7 Mo1 O7 Mo1 52.0(18) 23 . . 32 ?
O7 V1 O7 V1 53(4) 23 . . 32 ?
C1 C2 C3 C2 -175.8(10) . . . 5 ?
C5 C6 C5 C4 -173.3(9) 23 . . . ?
C5 C6 C5 C6 -2(3) 23 . . 32 ?

_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone'
_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 1.467
_oxdiff_exptl_absorpt_empirical_full_min 0.770
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.51(4)
2 0.49(4)

