# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

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

data_exp_649_auto
_database_code_depnum_ccdc_archive 'CCDC 2091110'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-06-20 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'tetrakis(((aquo)-N-(2-oxo-3-hydroxybenzylidene)isonicotinylhydrazonato)dioxomolybdenum(vi)) octamolybdate acetonitrile solvate hydrate'
_chemical_formula_moiety         
'4(C13 H12 Mo N3 O6), Mo8 O26, 4(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C56 H62 Mo12 N14 O54'
_chemical_formula_weight         2946.47
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.0881(2)
_cell_length_b                   33.6789(5)
_cell_length_c                   12.0491(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.137(2)
_cell_angle_gamma                90
_cell_volume                     4275.99(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    21463
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.2710
_cell_measurement_theta_min      3.8720
_shelx_estimated_absorpt_T_max   0.655
_shelx_estimated_absorpt_T_min   0.201
_exptl_absorpt_coefficient_mu    14.926
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.244
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
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            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2864
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -1 2 0.0172
-2 1 -2 0.0288
-1 -22 0 0.0153
0 22 -1 0.0120
-5 6 -3 0.0332
-6 3 6 0.0709
7 -5 -3 0.0564

_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.031
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37508
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.131
_diffrn_reflns_theta_min         4.078
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    102.00 159.00   0.50    0.84    --  113.25  61.00 120.00  114
  2  ω    113.00 178.00   0.50    0.84    --  113.25  45.00  90.00  130
  3  ω    102.00 174.00   0.50    0.84    --  113.25  30.00  60.00  144
  4  ω    100.00 142.00   0.50    0.84    --  113.25  15.00 -60.00   84
  5  ω    121.00 169.00   0.50    0.84    --  113.25  30.00-150.00   96
  6  ω    153.00 178.00   0.50    0.84    --  113.25  15.00-180.00   50
  7  ω    120.00 146.00   0.50    0.84    --  113.25  15.00-180.00   52
  8  ω    -12.00  13.00   0.50    0.21    --  -48.02  19.00-150.00   50
  9  ω    -82.00 -52.00   0.50    0.84    --  -91.75 107.00-167.00   60
 10  ω    -71.00 -42.00   0.50    0.21    --  -48.02 107.00-167.00   58
 11  ω    -36.00  -3.00   0.50    0.21    --  -48.02 107.00-167.00   66
 12  ω    -38.00  25.00   0.50    0.21    --  -48.02  38.00 -60.00  126
 13  ω   -148.00-122.00   0.50    0.84    --  -91.75-107.00  94.00   52
 14  ω   -116.00 -89.00   0.50    0.21    --  -48.02-125.00 150.00   54
 15  ω   -118.00 -77.00   0.50    0.21    --  -48.02-125.00 -30.00   82
 16  ω   -117.00 -74.00   0.50    0.21    --  -48.02-125.00 -60.00   86
 17  ω   -110.00 -74.00   0.50    0.21    --  -48.02-125.00-180.00   72
 18  ω     45.00  70.00   0.50    0.84    --  113.25 -61.00 -90.00   50
 19  ω     61.00  86.00   0.50    0.84    --  113.25 -77.00-180.00   50
 20  ω     65.00 105.00   0.50    0.84    --  113.25 -77.00-120.00   80
 21  ω     42.00  69.00   0.50    0.84    --  113.25 -61.00-180.00   54
 22  ω     42.00  71.00   0.50    0.84    --  113.25 -61.00   0.00   58
 23  ω     44.00  71.00   0.50    0.84    --  113.25 -61.00 120.00   54
 24  ω     46.00  72.00   0.50    0.84    --  113.25 -77.00  90.00   52
 25  ω     43.00  70.00   0.50    0.84    --  113.25 -61.00 -30.00   54
 26  ω     43.00  69.00   0.50    0.84    --  113.25 -61.00-150.00   52
 27  ω     96.00 176.00   0.50    0.84    --  113.25 125.00 -60.00  160
 28  ω    117.00 143.00   0.50    0.84    --  113.25 107.00-167.00   52
 29  ω     51.00  98.00   0.50    0.84    --  113.25 -95.00 150.00   94
 30  ω     45.00 101.00   0.50    0.84    --  113.25-107.00  94.00  112
 31  ω     49.00 111.00   0.50    0.84    --  113.25-125.00 150.00  124
 32  ω     61.00  97.00   0.50    0.84    --  113.25 -95.00 120.00   72
 33  ω     23.00  80.00   0.50    0.21    --   48.02-107.00  94.00  114
 34  ω     42.00  78.00   0.50    0.84    --  113.25-125.00   0.00   72
 35  ω     62.00 109.00   0.50    0.84    --  113.25-125.00-150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8184
_reflns_number_total             9113
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.741
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9113
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0786P)²+14.0679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1324
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O20(H20A,H20B), O21(H21A,H21B)
2.b Rotating group:
 O5(H5B,H5C), O5A(H5AA,H5AB)
2.c Aromatic/amide H refined with riding coordinates:
 N3A(H3A), N3(H3), C13A(H13A), C10(H10), C13(H13), C7(H7), C5(H5), C7A(H7A),
 C6(H6B), C12(H12), C11A(H11A), C10A(H10A), C4(H4), C12A(H12A), C6A(H6AA),
 C11(H11), C5A(H5A), C4A(H4A)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
2.e Idealised tetrahedral OH refined as rotating group:
 O6A(H6A), O6(H6)
;
_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
Mo1A Mo 0.22741(4) 0.21790(2) 0.26664(3) 0.01884(11) Uani 1 1 d . . . . .
Mo1 Mo 0.27062(4) 0.71475(2) 0.72059(3) 0.01714(11) Uani 1 1 d . . . . .
Mo2 Mo 0.62164(4) 0.49197(2) -0.06638(4) 0.01900(11) Uani 1 1 d . . . . .
Mo5 Mo 0.58301(4) 0.42531(2) 0.10961(4) 0.02061(11) Uani 1 1 d . . . . .
Mo3 Mo 0.67125(4) 0.55907(2) 0.13248(4) 0.02132(11) Uani 1 1 d . . . . .
Mo4 Mo 0.63412(4) 0.49104(2) 0.31289(4) 0.02361(12) Uani 1 1 d . . . . .
O2 O 0.3808(3) 0.67787(10) 0.6629(3) 0.0209(7) Uani 1 1 d . . . . .
O15 O 0.5483(3) 0.44007(10) -0.0582(3) 0.0205(7) Uani 1 1 d . . . . .
O11 O 0.5962(3) 0.49353(10) 0.1044(3) 0.0191(7) Uani 1 1 d . . . . .
O14 O 0.5674(4) 0.44005(11) 0.2572(3) 0.0243(7) Uani 1 1 d . . . . .
O12 O 0.6244(3) 0.54903(10) -0.0380(3) 0.0213(7) Uani 1 1 d . . . . .
O5 O 0.4716(3) 0.73349(11) 0.8484(3) 0.0218(7) Uani 1 1 d . . . . .
H5B H 0.520040 0.712536 0.868010 0.033 Uiso 1 1 d GR . . . .
H5C H 0.463363 0.741992 0.914132 0.033 Uiso 1 1 d GR . . . .
O5A O 0.0253(3) 0.23693(11) 0.1426(3) 0.0223(7) Uani 1 1 d . . . . .
H5AA H -0.024262 0.216123 0.125279 0.034 Uiso 1 1 d GR . . . .
H5AB H 0.031611 0.244785 0.075565 0.034 Uiso 1 1 d GR . . . .
O2A O 0.1184(4) 0.18030(11) 0.3220(3) 0.0214(7) Uani 1 1 d . . . . .
O13 O 0.6379(4) 0.54723(11) 0.2762(3) 0.0241(7) Uani 1 1 d . . . . .
O6A O 0.3441(4) 0.32657(11) 0.1143(3) 0.0239(7) Uani 1 1 d . . . . .
H6A H 0.393927 0.344057 0.104617 0.036 Uiso 1 1 calc GR . . . .
O1 O 0.2397(3) 0.76722(11) 0.7691(3) 0.0200(7) Uani 1 1 d . . . . .
O1A O 0.2582(4) 0.27090(11) 0.2207(3) 0.0227(7) Uani 1 1 d . . . . .
O6 O 0.1585(4) 0.82239(11) 0.8809(3) 0.0261(8) Uani 1 1 d . . . . .
H6 H 0.145220 0.842163 0.917988 0.039 Uiso 1 1 calc GR . . . .
O4 O 0.2554(4) 0.68561(12) 0.8317(3) 0.0273(8) Uani 1 1 d . . . . .
O7 O 0.7777(4) 0.48142(12) -0.0263(4) 0.0286(8) Uani 1 1 d . . . . .
O16 O 0.5759(4) 0.49443(12) -0.2193(3) 0.0265(8) Uani 1 1 d . . . . .
O19 O 0.5170(4) 0.37888(12) 0.0920(4) 0.0302(8) Uani 1 1 d . . . . .
O8 O 0.8266(4) 0.54518(12) 0.1672(4) 0.0313(9) Uani 1 1 d . . . . .
N2 N 0.4215(4) 0.72607(13) 0.5437(3) 0.0182(8) Uani 1 1 d . . . . .
O4A O 0.2380(4) 0.18969(12) 0.1524(4) 0.0303(8) Uani 1 1 d . . . . .
O10 O 0.7418(4) 0.41816(12) 0.1439(4) 0.0289(8) Uani 1 1 d . . . . .
O17 O 0.6732(4) 0.60941(12) 0.1380(4) 0.0314(9) Uani 1 1 d . . . . .
O9 O 0.7912(4) 0.48134(13) 0.3434(4) 0.0334(9) Uani 1 1 d . . . . .
O3 O 0.1359(4) 0.70735(13) 0.6071(4) 0.0292(8) Uani 1 1 d . . . . .
N1A N 0.1373(4) 0.25128(12) 0.3815(3) 0.0185(8) Uani 1 1 d . . . . .
N2A N 0.0779(4) 0.22718(13) 0.4449(4) 0.0204(8) Uani 1 1 d . . . . .
O3A O 0.3637(4) 0.20963(13) 0.3772(4) 0.0333(9) Uani 1 1 d . . . . .
O18 O 0.6105(5) 0.49480(13) 0.4459(4) 0.0362(10) Uani 1 1 d . . . . .
N1 N 0.3619(4) 0.74957(13) 0.6080(3) 0.0186(8) Uani 1 1 d . . . . .
N3A N -0.0231(4) 0.09415(14) 0.5833(4) 0.0257(9) Uani 1 1 d . . . . .
H3A H -0.041572 0.073758 0.620679 0.031 Uiso 1 1 calc R . . . .
N3 N 0.5422(4) 0.59869(14) 0.3971(4) 0.0255(9) Uani 1 1 d . . . . .
H3 H 0.565797 0.579569 0.358587 0.031 Uiso 1 1 calc R . . . .
O20 O -0.0044(5) 0.02824(16) 0.7156(6) 0.0518(14) Uani 1 1 d . . . . .
H20A H -0.064120 0.010487 0.693672 0.078 Uiso 1 1 d G . . . .
H20B H 0.065699 0.014803 0.728639 0.078 Uiso 1 1 d G . . . .
C9 C 0.4698(4) 0.65809(15) 0.5157(4) 0.0176(9) Uani 1 1 d . . . . .
C2 C 0.2501(5) 0.80483(14) 0.7364(4) 0.0186(9) Uani 1 1 d . . . . .
C13A C 0.0612(5) 0.11876(16) 0.4410(4) 0.0232(10) Uani 1 1 d . . . . .
H13A H 0.098273 0.114111 0.380944 0.028 Uiso 1 1 calc R . . . .
C8 C 0.4223(5) 0.68969(15) 0.5779(4) 0.0186(9) Uani 1 1 d . . . . .
C10 C 0.4521(5) 0.61840(16) 0.5412(4) 0.0227(10) Uani 1 1 d . . . . .
H10 H 0.414759 0.611950 0.599991 0.027 Uiso 1 1 calc R . . . .
C1 C 0.3070(5) 0.81547(15) 0.6515(4) 0.0206(9) Uani 1 1 d . . . . .
C9A C 0.0357(5) 0.15771(15) 0.4692(4) 0.0195(9) Uani 1 1 d . . . . .
C13 C 0.5251(5) 0.66689(16) 0.4294(4) 0.0224(10) Uani 1 1 d . . . . .
H13 H 0.538543 0.693651 0.411294 0.027 Uiso 1 1 calc R . . . .
C7 C 0.3601(5) 0.78705(14) 0.5906(4) 0.0188(9) Uani 1 1 d . . . . .
H7 H 0.396078 0.796739 0.533836 0.023 Uiso 1 1 calc R . . . .
C2A C 0.2472(4) 0.30792(15) 0.2555(4) 0.0189(9) Uani 1 1 d . . . . .
C5 C 0.2702(5) 0.88500(16) 0.6821(5) 0.0245(10) Uani 1 1 d . . . . .
H5 H 0.275229 0.912192 0.663044 0.029 Uiso 1 1 calc R . . . .
C8A C 0.0778(5) 0.19089(15) 0.4089(4) 0.0187(9) Uani 1 1 d . . . . .
C3 C 0.2059(5) 0.83473(16) 0.7956(4) 0.0218(10) Uani 1 1 d . . . . .
C7A C 0.1368(5) 0.28889(15) 0.3995(4) 0.0208(10) Uani 1 1 d . . . . .
H7A H 0.097880 0.298097 0.454629 0.025 Uiso 1 1 calc R . . . .
C6 C 0.3163(5) 0.85611(16) 0.6245(5) 0.0225(10) Uani 1 1 d . . . . .
H6B H 0.354159 0.863477 0.566878 0.027 Uiso 1 1 calc R . . . .
C12 C 0.5601(5) 0.63595(17) 0.3710(5) 0.0243(10) Uani 1 1 d . . . . .
H12 H 0.597257 0.641425 0.311448 0.029 Uiso 1 1 calc R . . . .
C11A C -0.0512(5) 0.13085(17) 0.6111(5) 0.0255(11) Uani 1 1 d . . . . .
H11A H -0.090816 0.134346 0.669881 0.031 Uiso 1 1 calc R . . . .
C3A C 0.2953(5) 0.33834(15) 0.1993(4) 0.0200(9) Uani 1 1 d . . . . .
C1A C 0.1915(5) 0.31820(16) 0.3412(4) 0.0218(10) Uani 1 1 d . . . . .
C10A C -0.0230(5) 0.16348(16) 0.5548(5) 0.0223(10) Uani 1 1 d . . . . .
H10A H -0.043156 0.189477 0.573940 0.027 Uiso 1 1 calc R . . . .
C4 C 0.2163(5) 0.87440(17) 0.7680(5) 0.0250(11) Uani 1 1 d . . . . .
H4 H 0.186371 0.894502 0.808183 0.030 Uiso 1 1 calc R . . . .
C12A C 0.0319(5) 0.08748(16) 0.5012(5) 0.0260(11) Uani 1 1 d . . . . .
H12A H 0.050781 0.061081 0.484230 0.031 Uiso 1 1 calc R . . . .
C6A C 0.1837(5) 0.35808(17) 0.3700(5) 0.0263(11) Uani 1 1 d . . . . .
H6AA H 0.145490 0.365025 0.427718 0.032 Uiso 1 1 calc R . . . .
O21 O 0.2213(6) -0.0106(3) 0.8190(5) 0.081(3) Uani 1 1 d . . . . .
H21A H 0.239373 -0.002474 0.890862 0.122 Uiso 1 1 d G . . . .
H21B H 0.279376 0.000016 0.793858 0.122 Uiso 1 1 d G . . . .
C11 C 0.4895(6) 0.58870(16) 0.4800(5) 0.0267(11) Uani 1 1 d . . . . .
H11 H 0.478200 0.561585 0.496058 0.032 Uiso 1 1 calc R . . . .
C5A C 0.2313(5) 0.38767(16) 0.3150(5) 0.0255(11) Uani 1 1 d . . . . .
H5A H 0.225965 0.414703 0.335482 0.031 Uiso 1 1 calc R . . . .
C4A C 0.2868(5) 0.37770(17) 0.2296(5) 0.0258(11) Uani 1 1 d . . . . .
H4A H 0.319078 0.398013 0.192005 0.031 Uiso 1 1 calc R . . . .
C14 C 0.0255(9) 0.9116(3) 0.9878(7) 0.0524(19) Uani 1 1 d . . . . .
N4 N 0.0796(15) 0.8859(3) 0.9808(13) 0.131(6) Uani 1 1 d . . . . .
C15 C -0.0538(10) 0.9456(3) 0.9884(9) 0.068(3) Uani 1 1 d . . . . .
H15A H -0.043519 0.965396 0.932400 0.103 Uiso 1 1 calc GR . . . .
H15B H -0.028937 0.957267 1.066815 0.103 Uiso 1 1 calc GR . . . .
H15C H -0.142755 0.937213 0.966453 0.103 Uiso 1 1 calc GR . . . .


_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
Mo1A O5A 2.362(4) . ?
Mo1A O2A 2.003(4) . ?
Mo1A O1A 1.930(4) . ?
Mo1A O4A 1.706(4) . ?
Mo1A N1A 2.245(4) . ?
Mo1A O3A 1.698(4) . ?
Mo1 O2 2.012(4) . ?
Mo1 O5 2.366(4) . ?
Mo1 O1 1.925(4) . ?
Mo1 O4 1.710(4) . ?
Mo1 O3 1.700(4) . ?
Mo1 N1 2.257(4) . ?
Mo2 Mo5 3.2072(5) . ?
Mo2 Mo3 3.2139(5) . ?
Mo2 O15 1.943(3) . ?
Mo2 O11 2.365(4) 3_665 ?
Mo2 O11 2.163(3) . ?
Mo2 O12 1.950(3) . ?
Mo2 O7 1.684(4) . ?
Mo2 O16 1.755(4) . ?
Mo5 Mo4 3.2183(6) . ?
Mo5 O15 2.000(4) . ?
Mo5 O11 2.304(3) . ?
Mo5 O14 1.905(4) . ?
Mo5 O12 2.355(4) 3_665 ?
Mo5 O19 1.712(4) . ?
Mo5 O10 1.696(4) . ?
Mo3 O15 2.318(4) 3_665 ?
Mo3 O11 2.346(3) . ?
Mo3 O12 1.985(4) . ?
Mo3 O13 1.922(4) . ?
Mo3 O8 1.707(4) . ?
Mo3 O17 1.697(4) . ?
Mo4 O11 2.416(4) . ?
Mo4 O14 1.907(4) . ?
Mo4 O13 1.947(4) . ?
Mo4 O16 2.302(4) 3_665 ?
Mo4 O9 1.697(4) . ?
Mo4 O18 1.708(4) . ?
O2 C8 1.308(6) . ?
O2A C8A 1.312(6) . ?
O6A C3A 1.358(6) . ?
O1 C2 1.342(6) . ?
O1A C2A 1.333(6) . ?
O6 C3 1.357(7) . ?
N2 N1 1.408(6) . ?
N2 C8 1.292(7) . ?
N1A N2A 1.410(6) . ?
N1A C7A 1.285(7) . ?
N2A C8A 1.296(7) . ?
N1 C7 1.279(7) . ?
N3A C11A 1.342(8) . ?
N3A C12A 1.333(7) . ?
N3 C12 1.324(7) . ?
N3 C11 1.347(7) . ?
C9 C8 1.490(7) . ?
C9 C10 1.399(7) . ?
C9 C13 1.393(7) . ?
C2 C1 1.405(7) . ?
C2 C3 1.408(7) . ?
C13A C9A 1.405(7) . ?
C13A C12A 1.374(8) . ?
C10 C11 1.381(8) . ?
C1 C7 1.440(7) . ?
C1 C6 1.418(7) . ?
C9A C8A 1.484(7) . ?
C9A C10A 1.394(7) . ?
C13 C12 1.379(7) . ?
C2A C3A 1.420(7) . ?
C2A C1A 1.401(7) . ?
C5 C6 1.382(8) . ?
C5 C4 1.393(8) . ?
C3 C4 1.390(8) . ?
C7A C1A 1.450(7) . ?
C11A C10A 1.378(8) . ?
C3A C4A 1.386(8) . ?
C1A C6A 1.397(8) . ?
C6A C5A 1.388(8) . ?
C5A C4A 1.394(8) . ?
C14 N4 1.073(12) . ?
C14 C15 1.445(13) . ?

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
O2A Mo1A O5A 80.22(14) . . ?
O2A Mo1A N1A 71.38(15) . . ?
O1A Mo1A O5A 77.60(15) . . ?
O1A Mo1A O2A 149.19(15) . . ?
O1A Mo1A N1A 82.29(15) . . ?
O4A Mo1A O5A 86.01(17) . . ?
O4A Mo1A O2A 96.70(18) . . ?
O4A Mo1A O1A 102.77(18) . . ?
O4A Mo1A N1A 158.71(18) . . ?
N1A Mo1A O5A 74.79(14) . . ?
O3A Mo1A O5A 168.01(19) . . ?
O3A Mo1A O2A 96.72(18) . . ?
O3A Mo1A O1A 100.54(19) . . ?
O3A Mo1A O4A 105.9(2) . . ?
O3A Mo1A N1A 93.24(19) . . ?
O2 Mo1 O5 80.76(14) . . ?
O2 Mo1 N1 71.27(15) . . ?
O1 Mo1 O2 148.89(15) . . ?
O1 Mo1 O5 77.19(14) . . ?
O1 Mo1 N1 82.01(15) . . ?
O4 Mo1 O2 97.75(17) . . ?
O4 Mo1 O5 86.91(17) . . ?
O4 Mo1 O1 102.64(17) . . ?
O4 Mo1 N1 160.16(18) . . ?
O3 Mo1 O2 96.18(18) . . ?
O3 Mo1 O5 167.42(17) . . ?
O3 Mo1 O1 100.58(18) . . ?
O3 Mo1 O4 105.6(2) . . ?
O3 Mo1 N1 92.23(18) . . ?
N1 Mo1 O5 75.22(14) . . ?
Mo5 Mo2 Mo3 91.509(14) . . ?
O15 Mo2 Mo5 36.16(11) . . ?
O15 Mo2 Mo3 124.88(11) . . ?
O15 Mo2 O11 78.06(14) . . ?
O15 Mo2 O11 77.13(14) . 3_665 ?
O15 Mo2 O12 149.48(15) . . ?
O11 Mo2 Mo5 45.90(9) . . ?
O11 Mo2 Mo5 86.22(8) 3_665 . ?
O11 Mo2 Mo3 85.81(8) 3_665 . ?
O11 Mo2 Mo3 46.87(9) . . ?
O11 Mo2 O11 75.63(15) . 3_665 ?
O12 Mo2 Mo5 124.89(11) . . ?
O12 Mo2 Mo3 35.60(11) . . ?
O12 Mo2 O11 78.99(14) . . ?
O12 Mo2 O11 77.88(14) . 3_665 ?
O7 Mo2 Mo5 89.97(14) . . ?
O7 Mo2 Mo3 90.71(13) . . ?
O7 Mo2 O15 101.80(17) . . ?
O7 Mo2 O11 174.76(16) . 3_665 ?
O7 Mo2 O11 99.14(17) . . ?
O7 Mo2 O12 101.47(17) . . ?
O7 Mo2 O16 104.28(19) . . ?
O16 Mo2 Mo5 132.30(13) . . ?
O16 Mo2 Mo3 132.56(13) . . ?
O16 Mo2 O15 96.14(17) . . ?
O16 Mo2 O11 156.56(16) . . ?
O16 Mo2 O11 80.95(15) . 3_665 ?
O16 Mo2 O12 96.97(17) . . ?
Mo2 Mo5 Mo4 89.632(14) . . ?
O15 Mo5 Mo2 34.99(10) . . ?
O15 Mo5 Mo4 122.10(10) . . ?
O15 Mo5 O11 73.66(13) . . ?
O15 Mo5 O12 71.33(14) . 3_665 ?
O11 Mo5 Mo2 42.39(9) . . ?
O11 Mo5 Mo4 48.48(9) . . ?
O11 Mo5 O12 71.78(13) . 3_665 ?
O14 Mo5 Mo2 120.29(11) . . ?
O14 Mo5 Mo4 32.44(11) . . ?
O14 Mo5 O15 146.54(15) . . ?
O14 Mo5 O11 77.91(14) . . ?
O14 Mo5 O12 83.36(15) . 3_665 ?
O12 Mo5 Mo2 79.47(9) 3_665 . ?
O12 Mo5 Mo4 86.95(9) 3_665 . ?
O19 Mo5 Mo2 134.24(14) . . ?
O19 Mo5 Mo4 133.61(14) . . ?
O19 Mo5 O15 99.30(17) . . ?
O19 Mo5 O11 159.37(17) . . ?
O19 Mo5 O14 101.18(18) . . ?
O19 Mo5 O12 87.61(17) . 3_665 ?
O10 Mo5 Mo2 85.32(14) . . ?
O10 Mo5 Mo4 89.35(14) . . ?
O10 Mo5 O15 98.06(17) . . ?
O10 Mo5 O11 94.49(16) . . ?
O10 Mo5 O14 101.44(18) . . ?
O10 Mo5 O12 164.36(16) . 3_665 ?
O10 Mo5 O19 105.8(2) . . ?
O15 Mo3 Mo2 78.78(9) 3_665 . ?
O15 Mo3 O11 70.94(13) 3_665 . ?
O11 Mo3 Mo2 42.30(8) . . ?
O12 Mo3 Mo2 34.89(10) . . ?
O12 Mo3 O15 72.39(14) . 3_665 ?
O12 Mo3 O11 73.98(13) . . ?
O13 Mo3 Mo2 119.31(11) . . ?
O13 Mo3 O15 82.91(15) . 3_665 ?
O13 Mo3 O11 77.02(14) . . ?
O13 Mo3 O12 146.66(15) . . ?
O8 Mo3 Mo2 85.15(14) . . ?
O8 Mo3 O15 163.10(16) . 3_665 ?
O8 Mo3 O11 93.62(16) . . ?
O8 Mo3 O12 97.22(18) . . ?
O8 Mo3 O13 100.69(19) . . ?
O17 Mo3 Mo2 136.81(15) . . ?
O17 Mo3 O15 90.09(17) . 3_665 ?
O17 Mo3 O11 160.99(17) . . ?
O17 Mo3 O12 101.94(18) . . ?
O17 Mo3 O13 100.10(19) . . ?
O17 Mo3 O8 105.4(2) . . ?
O11 Mo4 Mo5 45.58(8) . . ?
O14 Mo4 Mo5 32.41(11) . . ?
O14 Mo4 O11 75.09(14) . . ?
O14 Mo4 O13 145.97(16) . . ?
O14 Mo4 O16 78.28(15) . 3_665 ?
O13 Mo4 Mo5 120.45(11) . . ?
O13 Mo4 O11 74.87(13) . . ?
O13 Mo4 O16 76.81(15) . 3_665 ?
O16 Mo4 Mo5 82.06(10) 3_665 . ?
O16 Mo4 O11 70.20(13) 3_665 . ?
O9 Mo4 Mo5 87.59(15) . . ?
O9 Mo4 O11 93.81(17) . . ?
O9 Mo4 O14 99.33(19) . . ?
O9 Mo4 O13 98.25(19) . . ?
O9 Mo4 O16 163.96(18) . 3_665 ?
O9 Mo4 O18 105.0(2) . . ?
O18 Mo4 Mo5 136.32(15) . . ?
O18 Mo4 O11 161.02(19) . . ?
O18 Mo4 O14 103.93(19) . . ?
O18 Mo4 O13 99.32(19) . . ?
O18 Mo4 O16 90.94(19) . 3_665 ?
C8 O2 Mo1 118.8(3) . . ?
Mo2 O15 Mo5 108.85(17) . . ?
Mo2 O15 Mo3 112.01(16) . 3_665 ?
Mo5 O15 Mo3 103.99(15) . 3_665 ?
Mo2 O11 Mo2 104.37(15) . 3_665 ?
Mo2 O11 Mo5 91.70(12) . . ?
Mo2 O11 Mo3 90.82(12) . . ?
Mo2 O11 Mo4 92.60(12) 3_665 . ?
Mo2 O11 Mo4 163.02(18) . . ?
Mo5 O11 Mo2 98.12(13) . 3_665 ?
Mo5 O11 Mo3 163.12(18) . . ?
Mo5 O11 Mo4 85.94(11) . . ?
Mo3 O11 Mo2 97.40(12) . 3_665 ?
Mo3 O11 Mo4 86.78(12) . . ?
Mo5 O14 Mo4 115.15(18) . . ?
Mo2 O12 Mo5 109.70(16) . 3_665 ?
Mo2 O12 Mo3 109.50(17) . . ?
Mo3 O12 Mo5 103.16(15) . 3_665 ?
C8A O2A Mo1A 119.1(3) . . ?
Mo3 O13 Mo4 115.48(18) . . ?
C2 O1 Mo1 137.5(3) . . ?
C2A O1A Mo1A 137.2(3) . . ?
Mo2 O16 Mo4 116.24(19) . 3_665 ?
C8 N2 N1 108.3(4) . . ?
N2A N1A Mo1A 114.7(3) . . ?
C7A N1A Mo1A 128.6(4) . . ?
C7A N1A N2A 116.7(4) . . ?
C8A N2A N1A 108.3(4) . . ?
N2 N1 Mo1 114.5(3) . . ?
C7 N1 Mo1 128.7(3) . . ?
C7 N1 N2 116.7(4) . . ?
C12A N3A C11A 122.4(5) . . ?
C12 N3 C11 123.0(5) . . ?
C10 C9 C8 118.4(4) . . ?
C13 C9 C8 122.0(5) . . ?
C13 C9 C10 119.4(5) . . ?
O1 C2 C1 123.6(5) . . ?
O1 C2 C3 116.8(5) . . ?
C1 C2 C3 119.5(5) . . ?
C12A C13A C9A 119.3(5) . . ?
O2 C8 C9 116.2(4) . . ?
N2 C8 O2 124.8(5) . . ?
N2 C8 C9 119.0(4) . . ?
C11 C10 C9 119.2(5) . . ?
C2 C1 C7 123.3(5) . . ?
C2 C1 C6 119.6(5) . . ?
C6 C1 C7 117.0(5) . . ?
C13A C9A C8A 117.9(5) . . ?
C10A C9A C13A 118.9(5) . . ?
C10A C9A C8A 123.1(5) . . ?
C12 C13 C9 118.6(5) . . ?
N1 C7 C1 124.1(5) . . ?
O1A C2A C3A 116.2(5) . . ?
O1A C2A C1A 124.5(5) . . ?
C1A C2A C3A 119.3(5) . . ?
C6 C5 C4 120.2(5) . . ?
O2A C8A C9A 115.1(4) . . ?
N2A C8A O2A 123.9(5) . . ?
N2A C8A C9A 121.0(5) . . ?
O6 C3 C2 116.3(5) . . ?
O6 C3 C4 123.8(5) . . ?
C4 C3 C2 119.9(5) . . ?
N1A C7A C1A 124.4(5) . . ?
C5 C6 C1 120.0(5) . . ?
N3 C12 C13 120.5(5) . . ?
N3A C11A C10A 120.4(5) . . ?
O6A C3A C2A 116.5(5) . . ?
O6A C3A C4A 123.6(5) . . ?
C4A C3A C2A 119.9(5) . . ?
C2A C1A C7A 122.4(5) . . ?
C6A C1A C2A 119.8(5) . . ?
C6A C1A C7A 117.8(5) . . ?
C11A C10A C9A 118.9(5) . . ?
C3 C4 C5 120.7(5) . . ?
N3A C12A C13A 120.0(5) . . ?
C5A C6A C1A 120.6(5) . . ?
N3 C11 C10 119.1(5) . . ?
C6A C5A C4A 120.0(5) . . ?
C3A C4A C5A 120.4(5) . . ?
N4 C14 C15 175.6(14) . . ?

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

data_exp_5003
_database_code_depnum_ccdc_archive 'CCDC 2091109'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_exp_5003            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         26 Note
RESPONSE: Some of the low-angle reflections were fully or partially shadowed by the beam-stop. Those reflections were omitted from data reduction or refinement.
;
# Added during the CSD deposition process: Thursday 15 July 2021 10:55 AM
# end Validation Reply Form

_audit_creation_date             2021-07-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'bis((aquo)-dioxo-(N-(2-oxy-4-hydroxybenzylidene)isonicotinylhydrazonium)-molybdenum(vi)) octamolybdate acetonitrile solvate hydrate'
_chemical_formula_moiety         
'Mo8 O26, 2(C13 H13 Mo N3 O6), 2(H2 O), 4(C2 H3 N)'
_chemical_formula_sum            'C34 H42 Mo10 N10 O40'
_chemical_formula_weight         2190.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   7.9678(3)
_cell_length_b                   10.7556(6)
_cell_length_c                   18.9607(7)
_cell_angle_alpha                83.396(4)
_cell_angle_beta                 83.567(3)
_cell_angle_gamma                73.581(4)
_cell_volume                     1542.90(12)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3811
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.4370
_cell_measurement_theta_min      4.1290
_shelx_estimated_absorpt_T_max   0.922
_shelx_estimated_absorpt_T_min   0.671
_exptl_absorpt_coefficient_mu    2.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.357
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11239
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         4.039
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     27.00  52.00   1.00    5.00    --   28.34 -57.00 150.00   25
  2  ω     53.00  97.00   1.00    5.00    --   28.34  57.00 -60.00   44
  3  ω     -9.00  77.00   1.00    5.00    --   28.34-107.00  24.00   86
  4  ω    -24.00  64.00   1.00    5.00    --   28.34 -99.00 -90.00   88
  5  ω    -42.00 -12.00   1.00    5.00    --   28.34 -57.00 150.00   30
  6  ω      1.00  35.00   1.00    5.00    --  -31.31  57.00-180.00   34
  7  ω   -102.00 -53.00   1.00    5.00    --  -31.31 -57.00  30.00   49
  8  ω    -88.00 -26.00   1.00    5.00    --  -31.31 -77.00  90.00   62
  9  ω   -113.00 -44.00   1.00    5.00    --  -31.31 179.00  60.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4028
_reflns_number_total             5423
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.309
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5423
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0416
_refine_ls_restrained_S_all      1.074
_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)+(0.0329P)²+1.2941P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.1026
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H6A-O6
 0.86 with sigma of 0.02
 O6-H6B
 0.86 with sigma of 0.02
3.a Free rotating group:
 O7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C5(H5A), C7(H7), C6(H6), C3(H3A), C10(H10), C12(H12),
 C11(H11), C13(H13)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C15(H15A,H15B,H15C)
3.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo5 Mo -0.13973(7) 0.70060(5) 1.09603(3) 0.01407(15) Uani 1 1 d . . . . .
Mo4 Mo -0.21889(7) 0.53973(5) 0.97608(3) 0.01201(15) Uani 1 1 d . . . . .
Mo2 Mo 0.06784(7) 0.62602(5) 0.86432(3) 0.01379(15) Uani 1 1 d . . . . .
Mo3 Mo 0.15514(7) 0.78905(5) 0.98382(3) 0.01431(15) Uani 1 1 d . . . . .
Mo1 Mo 0.82819(9) 0.78833(6) 0.40785(3) 0.02644(18) Uani 1 1 d . . . . .
O12 O -0.0153(5) 0.6302(4) 0.9842(2) 0.0124(9) Uani 1 1 d . . . . .
O9 O -0.0696(5) 0.4980(4) 0.8870(2) 0.0129(9) Uani 1 1 d . . . . .
O17 O 0.0564(5) 0.7683(4) 1.0807(2) 0.0145(10) Uani 1 1 d . . . . .
O18 O -0.2448(5) 0.5594(4) 1.0775(2) 0.0134(9) Uani 1 1 d . . . . .
O10 O 0.2307(5) 0.7042(4) 0.8949(2) 0.0146(10) Uani 1 1 d . . . . .
O16 O -0.3155(5) 0.4118(4) 0.9785(2) 0.0141(10) Uani 1 1 d . . . . .
O20 O -0.1837(6) 0.7023(4) 1.1859(2) 0.0205(11) Uani 1 1 d . . . . .
O14 O -0.0143(5) 0.9093(4) 0.9505(2) 0.0171(10) Uani 1 1 d . . . . .
O11 O -0.0968(6) 0.7590(4) 0.8405(2) 0.0171(10) Uani 1 1 d . . . . .
O15 O -0.3685(5) 0.6743(4) 0.9439(2) 0.0164(10) Uani 1 1 d . . . . .
O19 O -0.3000(6) 0.8256(4) 1.0613(2) 0.0193(10) Uani 1 1 d . . . . .
O8 O 0.1789(6) 0.5744(4) 0.7857(2) 0.0210(11) Uani 1 1 d . . . . .
O13 O 0.3142(6) 0.8622(4) 0.9924(2) 0.0205(11) Uani 1 1 d . . . . .
O2 O 1.0028(6) 0.7048(5) 0.3309(2) 0.0249(11) Uani 1 1 d . . . . .
O1 O 0.6206(7) 0.7902(5) 0.4699(3) 0.0340(13) Uani 1 1 d . . . . .
O6 O 0.6546(7) 0.7483(5) 0.3238(3) 0.0313(13) Uani 1 1 d D . . . .
O5 O 0.2437(8) 0.7346(5) 0.6714(3) 0.0438(15) Uani 1 1 d . . . . .
H5 H 0.212284 0.676608 0.698774 0.066 Uiso 1 1 calc GR . . . .
N1 N 0.8597(7) 0.5747(5) 0.4239(3) 0.0207(13) Uani 1 1 d . . . . .
O3 O 0.9738(7) 0.7829(5) 0.4675(3) 0.0382(14) Uani 1 1 d . . . . .
O4 O 0.7796(7) 0.9426(5) 0.3680(3) 0.0366(14) Uani 1 1 d . . . . .
O7 O -0.3777(8) 0.9491(6) 0.9159(4) 0.0443(15) Uani 1 1 d . . . . .
H7A H -0.282053 0.943365 0.933532 0.067 Uiso 1 1 d G . . . .
H7B H -0.438922 1.028005 0.913028 0.067 Uiso 1 1 d G . . . .
N2 N 0.9801(7) 0.5018(6) 0.3754(3) 0.0249(14) Uani 1 1 d . . . . .
H2 H 1.006745 0.416627 0.375481 0.030 Uiso 1 1 calc R . . . .
N3 N 1.4561(8) 0.4132(8) 0.1828(4) 0.0409(19) Uani 1 1 d . . . . .
H3 H 1.545733 0.378287 0.153151 0.049 Uiso 1 1 calc R . . . .
C2 C 0.5716(9) 0.7070(7) 0.5225(3) 0.0205(16) Uani 1 1 d . . . . .
C1 C 0.6548(9) 0.5722(7) 0.5262(4) 0.0224(16) Uani 1 1 d . . . . .
C4 C 0.3791(10) 0.6779(7) 0.6249(4) 0.0264(17) Uani 1 1 d . . . . .
C5 C 0.4562(10) 0.5453(7) 0.6301(4) 0.0270(18) Uani 1 1 d . . . . .
H5A H 0.415991 0.490645 0.667148 0.032 Uiso 1 1 calc R . . . .
C8 C 1.0471(9) 0.5770(7) 0.3303(4) 0.0247(17) Uani 1 1 d . . . . .
C7 C 0.7891(9) 0.5109(7) 0.4745(4) 0.0233(17) Uani 1 1 d . . . . .
H7 H 0.827901 0.418564 0.477873 0.028 Uiso 1 1 calc R . . . .
C9 C 1.1876(9) 0.5187(8) 0.2766(4) 0.0257(17) Uani 1 1 d . . . . .
C6 C 0.5905(9) 0.4931(7) 0.5815(4) 0.0240(16) Uani 1 1 d . . . . .
H6 H 0.642007 0.401717 0.584902 0.029 Uiso 1 1 calc R . . . .
C3 C 0.4361(10) 0.7588(8) 0.5723(4) 0.035(2) Uani 1 1 d . . . . .
H3A H 0.382823 0.849965 0.569931 0.043 Uiso 1 1 calc R . . . .
C16 C -0.7524(15) 0.9890(8) 0.7976(4) 0.042(2) Uani 1 1 d . . . . .
N5 N -0.6082(13) 0.9649(8) 0.8053(4) 0.063(2) Uani 1 1 d . . . . .
C10 C 1.2685(9) 0.5996(8) 0.2309(4) 0.0315(19) Uani 1 1 d . . . . .
H10 H 1.229868 0.691388 0.232446 0.038 Uiso 1 1 calc R . . . .
C12 C 1.3788(10) 0.3341(9) 0.2242(5) 0.038(2) Uani 1 1 d . . . . .
H12 H 1.417432 0.242765 0.220886 0.046 Uiso 1 1 calc R . . . .
C11 C 1.4062(9) 0.5437(9) 0.1832(4) 0.0323(19) Uani 1 1 d . . . . .
H11 H 1.464342 0.596203 0.151448 0.039 Uiso 1 1 calc R . . . .
C13 C 1.2417(9) 0.3868(8) 0.2721(4) 0.0319(19) Uani 1 1 d . . . . .
H13 H 1.184164 0.331716 0.302110 0.038 Uiso 1 1 calc R . . . .
C17 C -0.9378(12) 1.0198(8) 0.7884(4) 0.041(2) Uani 1 1 d . . . . .
H17A H -0.967452 1.089417 0.749940 0.062 Uiso 1 1 calc GR . . . .
H17B H -1.005680 1.048658 0.832764 0.062 Uiso 1 1 calc GR . . . .
H17C H -0.965909 0.942293 0.776189 0.062 Uiso 1 1 calc GR . . . .
C14 C 0.2249(14) 0.9720(13) 0.3535(6) 0.068(3) Uani 1 1 d . . . . .
C15 C 0.1239(19) 1.0585(13) 0.4030(7) 0.099(4) Uani 1 1 d . . . . .
H15A H 0.008972 1.102286 0.385351 0.148 Uiso 1 1 calc GR . . . .
H15B H 0.184841 1.123558 0.408933 0.148 Uiso 1 1 calc GR . . . .
H15C H 0.107757 1.009685 0.448998 0.148 Uiso 1 1 calc GR . . . .
N4 N 0.3010(12) 0.8957(13) 0.3184(8) 0.122(5) Uani 1 1 d . . . A 2
H6A H 0.547(6) 0.786(12) 0.318(7) 0.147 Uiso 1 1 d DR . . . .
H6B H 0.709(16) 0.670(5) 0.315(7) 0.147 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo5 O12 2.351(4) . ?
Mo5 O9 2.323(4) 2_567 ?
Mo5 O17 1.884(4) . ?
Mo5 O18 2.009(4) . ?
Mo5 O20 1.701(4) . ?
Mo5 O19 1.699(4) . ?
Mo4 Mo2 3.1988(8) . ?
Mo4 O12 2.336(4) 2_567 ?
Mo4 O12 2.141(4) . ?
Mo4 O9 1.972(4) . ?
Mo4 O18 1.940(4) . ?
Mo4 O16 1.750(4) . ?
Mo4 O15 1.695(4) . ?
Mo2 O12 2.297(4) . ?
Mo2 O9 1.973(4) . ?
Mo2 O18 2.332(4) 2_567 ?
Mo2 O10 1.903(4) . ?
Mo2 O11 1.701(4) . ?
Mo2 O8 1.712(4) . ?
Mo3 O12 2.464(4) . ?
Mo3 O17 1.930(4) . ?
Mo3 O10 1.964(4) . ?
Mo3 O16 2.258(4) 2_567 ?
Mo3 O14 1.706(4) . ?
Mo3 O13 1.700(4) . ?
Mo1 O2 2.003(5) . ?
Mo1 O1 1.916(5) . ?
Mo1 O6 2.372(6) . ?
Mo1 N1 2.228(6) . ?
Mo1 O3 1.695(5) . ?
Mo1 O4 1.700(5) . ?
O2 C8 1.320(8) . ?
O1 C2 1.362(8) . ?
O5 C4 1.360(8) . ?
N1 N2 1.387(7) . ?
N1 C7 1.287(8) . ?
N2 C8 1.286(9) . ?
N3 C12 1.325(10) . ?
N3 C11 1.348(10) . ?
C2 C1 1.411(10) . ?
C2 C3 1.385(10) . ?
C1 C7 1.432(10) . ?
C1 C6 1.416(9) . ?
C4 C5 1.381(10) . ?
C4 C3 1.372(10) . ?
C5 C6 1.367(10) . ?
C8 C9 1.475(9) . ?
C9 C10 1.394(10) . ?
C9 C13 1.372(10) . ?
C16 N5 1.127(12) . ?
C16 C17 1.446(13) . ?
C10 C11 1.383(10) . ?
C12 C13 1.372(11) . ?
C14 C15 1.415(15) . ?
C14 N4 1.112(13) . ?

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
O9 Mo5 O12 71.11(14) 2_567 . ?
O17 Mo5 O12 77.92(16) . . ?
O17 Mo5 O9 83.99(16) . 2_567 ?
O17 Mo5 O18 146.80(18) . . ?
O18 Mo5 O12 73.01(15) . . ?
O18 Mo5 O9 71.79(15) . 2_567 ?
O20 Mo5 O12 160.63(19) . . ?
O20 Mo5 O9 89.54(18) . 2_567 ?
O20 Mo5 O17 101.5(2) . . ?
O20 Mo5 O18 100.67(19) . . ?
O19 Mo5 O12 94.01(18) . . ?
O19 Mo5 O9 162.62(18) . 2_567 ?
O19 Mo5 O17 102.06(19) . . ?
O19 Mo5 O18 95.70(19) . . ?
O19 Mo5 O20 104.9(2) . . ?
O12 Mo4 Mo2 85.74(10) 2_567 . ?
O12 Mo4 Mo2 45.85(11) . . ?
O12 Mo4 O12 75.40(16) . 2_567 ?
O9 Mo4 Mo2 35.82(12) . . ?
O9 Mo4 O12 78.09(16) . . ?
O9 Mo4 O12 77.72(15) . 2_567 ?
O18 Mo4 Mo2 125.13(12) . . ?
O18 Mo4 O12 78.64(16) . 2_567 ?
O18 Mo4 O12 79.28(16) . . ?
O18 Mo4 O9 150.62(17) . . ?
O16 Mo4 Mo2 131.21(14) . . ?
O16 Mo4 O12 156.88(18) . . ?
O16 Mo4 O12 81.55(17) . 2_567 ?
O16 Mo4 O9 95.39(18) . . ?
O16 Mo4 O18 98.12(18) . . ?
O15 Mo4 Mo2 87.42(14) . . ?
O15 Mo4 O12 97.24(18) . . ?
O15 Mo4 O12 172.28(17) . 2_567 ?
O15 Mo4 O9 98.70(19) . . ?
O15 Mo4 O18 102.53(19) . . ?
O15 Mo4 O16 105.7(2) . . ?
O12 Mo2 Mo4 41.99(10) . . ?
O12 Mo2 O18 72.19(14) . 2_567 ?
O9 Mo2 Mo4 35.81(12) . . ?
O9 Mo2 O12 74.41(16) . . ?
O9 Mo2 O18 72.20(15) . 2_567 ?
O18 Mo2 Mo4 79.68(10) 2_567 . ?
O10 Mo2 Mo4 120.58(12) . . ?
O10 Mo2 O12 78.60(16) . . ?
O10 Mo2 O9 147.12(17) . . ?
O10 Mo2 O18 81.96(16) . 2_567 ?
O11 Mo2 Mo4 86.47(14) . . ?
O11 Mo2 O12 94.50(18) . . ?
O11 Mo2 O9 98.99(19) . . ?
O11 Mo2 O18 165.45(17) . 2_567 ?
O11 Mo2 O10 101.5(2) . . ?
O11 Mo2 O8 105.1(2) . . ?
O8 Mo2 Mo4 135.75(15) . . ?
O8 Mo2 O12 160.26(19) . . ?
O8 Mo2 O9 99.96(19) . . ?
O8 Mo2 O18 88.07(18) . 2_567 ?
O8 Mo2 O10 99.1(2) . . ?
O17 Mo3 O12 74.31(15) . . ?
O17 Mo3 O10 144.37(17) . . ?
O17 Mo3 O16 77.89(16) . 2_567 ?
O10 Mo3 O12 73.45(15) . . ?
O10 Mo3 O16 77.10(16) . 2_567 ?
O16 Mo3 O12 69.76(14) 2_567 . ?
O14 Mo3 O12 90.06(17) . . ?
O14 Mo3 O17 99.13(19) . . ?
O14 Mo3 O10 95.67(19) . . ?
O14 Mo3 O16 159.71(18) . 2_567 ?
O13 Mo3 O12 164.32(18) . . ?
O13 Mo3 O17 102.66(19) . . ?
O13 Mo3 O10 104.24(19) . . ?
O13 Mo3 O16 94.57(19) . 2_567 ?
O13 Mo3 O14 105.6(2) . . ?
O2 Mo1 O6 75.55(18) . . ?
O2 Mo1 N1 72.21(19) . . ?
O1 Mo1 O2 148.7(2) . . ?
O1 Mo1 O6 81.8(2) . . ?
O1 Mo1 N1 81.4(2) . . ?
N1 Mo1 O6 75.3(2) . . ?
O3 Mo1 O2 97.1(2) . . ?
O3 Mo1 O1 101.0(2) . . ?
O3 Mo1 O6 167.9(2) . . ?
O3 Mo1 N1 93.3(2) . . ?
O3 Mo1 O4 105.6(3) . . ?
O4 Mo1 O2 97.3(2) . . ?
O4 Mo1 O1 102.1(2) . . ?
O4 Mo1 O6 85.1(2) . . ?
O4 Mo1 N1 159.5(2) . . ?
Mo5 O12 Mo3 85.21(13) . . ?
Mo4 O12 Mo5 97.81(15) 2_567 . ?
Mo4 O12 Mo5 91.68(14) . . ?
Mo4 O12 Mo4 104.60(16) . 2_567 ?
Mo4 O12 Mo2 92.16(15) . . ?
Mo4 O12 Mo3 164.1(2) . . ?
Mo4 O12 Mo3 91.32(14) 2_567 . ?
Mo2 O12 Mo5 162.7(2) . . ?
Mo2 O12 Mo4 97.55(15) . 2_567 ?
Mo2 O12 Mo3 86.47(13) . . ?
Mo4 O9 Mo5 110.39(18) . 2_567 ?
Mo4 O9 Mo2 108.37(19) . . ?
Mo2 O9 Mo5 104.53(17) . 2_567 ?
Mo5 O17 Mo3 117.4(2) . . ?
Mo5 O18 Mo2 103.03(17) . 2_567 ?
Mo4 O18 Mo5 109.54(19) . . ?
Mo4 O18 Mo2 109.01(18) . 2_567 ?
Mo2 O10 Mo3 115.1(2) . . ?
Mo4 O16 Mo3 117.4(2) . 2_567 ?
C8 O2 Mo1 119.1(4) . . ?
C2 O1 Mo1 135.5(4) . . ?
N2 N1 Mo1 115.0(4) . . ?
C7 N1 Mo1 128.2(5) . . ?
C7 N1 N2 116.6(6) . . ?
C8 N2 N1 110.0(6) . . ?
C12 N3 C11 124.2(7) . . ?
O1 C2 C1 121.3(6) . . ?
O1 C2 C3 117.8(6) . . ?
C3 C2 C1 120.9(6) . . ?
C2 C1 C7 124.0(6) . . ?
C2 C1 C6 117.0(6) . . ?
C6 C1 C7 118.8(7) . . ?
O5 C4 C5 121.9(7) . . ?
O5 C4 C3 116.9(7) . . ?
C3 C4 C5 121.2(7) . . ?
C6 C5 C4 119.6(7) . . ?
O2 C8 C9 117.2(7) . . ?
N2 C8 O2 123.6(6) . . ?
N2 C8 C9 119.0(7) . . ?
N1 C7 C1 123.3(7) . . ?
C10 C9 C8 119.0(7) . . ?
C13 C9 C8 121.2(7) . . ?
C13 C9 C10 119.8(7) . . ?
C5 C6 C1 121.6(7) . . ?
C4 C3 C2 119.7(7) . . ?
N5 C16 C17 179.5(10) . . ?
C11 C10 C9 118.7(8) . . ?
N3 C12 C13 118.6(8) . . ?
N3 C11 C10 118.5(8) . . ?
C9 C13 C12 120.2(8) . . ?
N4 C14 C15 174.1(16) . . ?

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

data_exp_947_auto
_database_code_depnum_ccdc_archive 'CCDC 2091112'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-06-20 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_audit_creation_date             2021-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'bis((aquo)-dioxo-(N-(2-oxy-4-hydroxybenzylidene)isonicotinylhydrazonium)-molybdenum(vi)) octamolybdate acetonitrile solvate hydrate'
_chemical_formula_moiety         
'Mo8 O26, 4(C13 H12 Mo N3 O6), 10(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C56 H74 Mo12 N14 O60'
_chemical_formula_weight         3054.57
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   9.4085(4)
_cell_length_b                   16.2433(5)
_cell_length_c                   17.3878(4)
_cell_angle_alpha                116.276(3)
_cell_angle_beta                 95.232(3)
_cell_angle_gamma                93.035(3)
_cell_volume                     2359.80(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    23681
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.7510
_cell_measurement_theta_min      3.0260
_shelx_estimated_absorpt_T_max   0.612
_shelx_estimated_absorpt_T_min   0.091
_exptl_absorpt_coefficient_mu    13.601
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.114
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
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            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.149
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -1 0.0817
0 -1 1 0.0523
2 -1 2 0.0807
-2 1 -2 0.1048
0 -1 0 0.0230
0 1 0 0.0145

_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37525
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.466
_diffrn_reflns_theta_min         2.858
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     28.00 121.00   0.50    0.10    --   47.77  72.00-138.00  186
  2  ω    116.00 178.00   0.50    0.15    --  113.25  72.00-138.00  124
  3  ω    101.00 178.00   0.50    0.15    --  113.25  45.00-150.00  154
  4  ω    101.00 173.00   0.50    0.15    --  113.25  45.00 -90.00  144
  5  ω    143.00 178.00   0.50    0.15    --  113.25  30.00-180.00   70
  6  ω    104.00 174.00   0.50    0.15    --  113.25  45.00 -60.00  140
  7  ω    101.00 135.00   0.50    0.15    --  113.25  30.00   0.00   68
  8  ω    139.00 178.00   0.50    0.15    --  113.25  30.00  60.00   78
  9  ω    130.00 165.00   0.50    0.15    --  113.25  45.00  90.00   70
 10  ω    103.00 128.00   0.50    0.15    --  113.25  30.00  60.00   50
 11  ω    100.00 175.00   0.50    0.15    --  113.25  15.00 150.00  150
 12  ω    118.00 172.00   0.50    0.15    --  113.25  15.00  30.00  108
 13  ω    142.00 168.00   0.50    0.15    --  113.25  30.00   0.00   52
 14  ω    101.00 126.00   0.50    0.15    --  113.25  30.00-180.00   50
 15  ω    -68.00 -25.00   0.50    0.10    --  -47.77  72.00-138.00   86
 16  ω    -79.00 -54.00   0.50    0.15    --  -91.75  72.00-138.00   50
 17  ω    -16.00  11.00   0.50    0.10    --  -47.77  72.00-138.00   54
 18  ω    -50.00 -20.00   0.50    0.15    --  -91.75  45.00   0.00   60
 19  ω    -51.00 -20.00   0.50    0.15    --  -91.75  45.00  30.00   62
 20  ω     88.00 130.00   0.50    0.15    --  113.25-151.00-132.23   84
 21  ω     36.00  81.00   0.50    0.10    --   47.77-125.00 -60.00   90
 22  ω     76.00 101.00   0.50    0.15    --  113.25-125.00  30.00   50
 23  ω     42.00  68.00   0.50    0.15    --  113.25-125.00  30.00   52
 24  ω     72.00  98.00   0.50    0.15    --  113.25-125.00 -30.00   52
 25  ω     43.00  81.00   0.50    0.15    --  113.25-125.00 -60.00   76
 26  ω     52.00 110.00   0.50    0.15    --  113.25-125.00-120.00  116
 27  ω     51.00 106.00   0.50    0.15    --  113.25-108.00 -64.43  110
 28  ω     55.00 122.00   0.50    0.15    --  113.25-139.00   9.82  134
 29  ω     85.00 111.00   0.50    0.15    --  113.25-125.00  60.00   52
 30  ω     86.00 111.00   0.50    0.15    --  113.25-125.00 150.00   50
 31  ω     48.00 111.00   0.50    0.15    --  113.25-125.00 120.00  126
 32  ω     46.00  72.00   0.50    0.15    --  113.25 -95.00  60.00   52
 33  ω     76.00 102.00   0.50    0.15    --  113.25 -95.00  90.00   52
 34  ω     47.00  85.00   0.50    0.15    --  113.25 -95.00   0.00   76
 35  ω     78.00 106.00   0.50    0.15    --  113.25 -95.00  30.00   56
 36  ω     43.00 106.00   0.50    0.15    --  113.25 -95.00 150.00  126
 37  ω     43.00  75.00   0.50    0.15    --  113.25 -95.00  30.00   64
 38  ω     47.00 108.00   0.50    0.15    --  113.25-108.00-115.90  122
 39  ω     64.00 103.00   0.50    0.15    --  113.25 -95.00 -30.00   78
 40  ω     69.00 106.00   0.50    0.15    --  113.25 -95.00-150.00   74
 41  ω     81.00 106.00   0.50    0.15    --  113.25 -95.00-180.00   50
 42  ω     46.00  76.00   0.50    0.15    --  113.25 -95.00-180.00   60
 43  ω     68.00  94.00   0.50    0.15    --  113.25 -77.00-150.00   52
 44  ω     42.00  67.00   0.50    0.15    --  113.25 -61.00-150.00   50
 45  ω     45.00  71.00   0.50    0.15    --  113.25 -61.00  30.00   52
 46  ω     42.00  93.00   0.50    0.15    --  113.25 -77.00  90.00  102
 47  ω     42.00  67.00   0.50    0.15    --  113.25 -72.00  91.00   50
 48  ω     44.00  70.00   0.50    0.15    --  113.25 -61.00  90.00   52
 49  ω     11.00  65.00   0.50    0.10    --   47.77 -72.00  91.00  108
 50  ω     44.00  70.00   0.50    0.15    --  113.25 -61.00 -30.00   52
 51  ω     46.00  71.00   0.50    0.15    --  113.25 -61.00 -90.00   50
 52  ω     96.00 128.00   0.50    0.15    --  113.25 125.00-180.00   64
 53  ω    140.00 165.00   0.50    0.15    --  113.25 125.00-180.00   50
 54  ω     97.00 168.00   0.50    0.15    --  113.25 125.00 -60.00  142
 55  ω    -68.00 -14.00   0.50    0.10    --  -47.77 125.00 120.00  108
 56  ω    -77.00 -18.00   0.50    0.10    --  -47.77 125.00   0.00  118
 57  ω   -118.00 -28.00   0.50    0.10    --  -47.77 -72.00  91.00  180
 58  ω   -141.00-115.00   0.50    0.15    --  -91.75 -72.00  91.00   52
 59  ω   -102.00 -73.00   0.50    0.10    --  -47.77-125.00-120.00   58
 60  ω   -115.00 -89.00   0.50    0.10    --  -47.77-125.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9372
_reflns_number_total             10049
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.290
_refine_diff_density_min         -1.719
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.00031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         10049
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0764P)²+17.1814P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1482
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O11) = Uanis(Mo3)
3.a Free rotating group:
 O24(H24A,H24B), O20(H20A,H20B), O23(H23A,H23B), O22(H22A,H22B), O21(H21A,H21B)
3.b Rotating group:
 O5A(H5AA,H5AB), O5(H5A,H5B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N3A(H3AA), C6(H6A), C3A(H3AB), C10(H10), C13(H13), C5(H5), C12(H12),
 C11(H11), C6A(H6AB), C7(H7), C7A(H7A), C5A(H5AC), C10A(H10A), C3(H3A),
 C11A(H11A), C13A(H13A), C12A(H12A)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
3.e Idealised tetrahedral OH refined as rotating group:
 O6A(H6AA), O6(H6)
;
_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
Mo3 Mo 1.14747(4) 0.98836(3) 0.93898(3) 0.01658(12) Uani 1 1 d . . . . .
Mo4 Mo 0.85594(5) 0.86112(3) 0.84244(3) 0.02019(13) Uani 1 1 d . . . . .
Mo5 Mo 0.68576(5) 1.04356(3) 0.89228(3) 0.02165(13) Uani 1 1 d . . . . .
Mo1 Mo 0.59996(5) 0.22450(3) 0.55070(3) 0.02229(13) Uani 1 1 d . . . . .
Mo1A Mo 0.09780(5) 0.32057(3) 0.51704(3) 0.02174(13) Uani 1 1 d . . . . .
Mo2 Mo 0.98371(5) 1.17462(3) 0.99351(3) 0.01915(12) Uani 1 1 d . . . . .
O13 O 1.0523(4) 0.8630(3) 0.8965(2) 0.0185(8) Uani 1 1 d . . . . .
O2 O 0.7492(5) 0.1517(3) 0.4802(3) 0.0250(9) Uani 1 1 d . . . . .
O15 O 0.7804(4) 1.1622(3) 0.9745(3) 0.0217(8) Uani 1 1 d . . . . .
O2A O -0.0408(4) 0.2792(3) 0.4091(3) 0.0243(8) Uani 1 1 d . . . . .
O17 O 1.3089(4) 0.9664(3) 0.9813(3) 0.0218(8) Uani 1 1 d . . . . .
O1 O 0.4975(5) 0.2624(3) 0.6494(3) 0.0269(9) Uani 1 1 d . . . . .
O7 O 1.0301(5) 1.1699(3) 0.8980(3) 0.0256(9) Uani 1 1 d . . . . .
O14 O 0.6771(5) 0.9115(3) 0.8534(3) 0.0262(9) Uani 1 1 d . . . . .
O12 O 1.1602(4) 1.1204(3) 1.0187(3) 0.0206(8) Uani 1 1 d . . . . .
O11 O 0.9246(4) 1.0114(3) 0.9330(2) 0.01658(12) Uani 1 1 d . . . . .
O5A O 0.2404(5) 0.2413(3) 0.4087(3) 0.0267(9) Uani 1 1 d . . . . .
H5AA H 0.186411 0.198085 0.363636 0.040 Uiso 1 1 d GR . . . .
H5AB H 0.299091 0.211063 0.426136 0.040 Uiso 1 1 d GR . . . .
O1A O 0.2871(5) 0.3724(3) 0.5766(3) 0.0268(9) Uani 1 1 d . . . . .
O8 O 1.1825(5) 0.9891(3) 0.8458(3) 0.0235(8) Uani 1 1 d . . . . .
O6A O 0.6654(5) 0.5824(3) 0.7643(3) 0.0304(10) Uani 1 1 d . . . . .
H6AA H 0.709142 0.634346 0.777916 0.046 Uiso 1 1 calc GR . . . .
O16 O 1.0244(5) 1.2863(3) 1.0668(3) 0.0304(10) Uani 1 1 d . . . . .
O5 O 0.7928(5) 0.2753(3) 0.6623(3) 0.0320(10) Uani 1 1 d . . . . .
H5A H 0.772029 0.258207 0.701264 0.048 Uiso 1 1 d GR . . . .
H5B H 0.802390 0.335441 0.689496 0.048 Uiso 1 1 d GR . . . .
O10 O 0.7286(5) 1.0469(3) 0.8000(3) 0.0290(9) Uani 1 1 d . . . . .
O19 O 0.5097(5) 1.0619(4) 0.8942(3) 0.0311(10) Uani 1 1 d . . . . .
O9 O 0.9025(5) 0.8669(3) 0.7524(3) 0.0287(9) Uani 1 1 d . . . . .
O6 O 0.1797(5) 0.2859(3) 0.8475(3) 0.0335(10) Uani 1 1 d . . . . .
H6 H 0.129732 0.251425 0.861352 0.050 Uiso 1 1 calc GR . . . .
O4A O 0.0795(5) 0.2209(3) 0.5266(3) 0.0333(10) Uani 1 1 d . . . . .
O24 O -0.5769(5) 0.2177(4) 0.0293(3) 0.0351(11) Uani 1 1 d . . . . .
H24A H -0.653254 0.196147 0.041875 0.053 Uiso 1 1 d G . . . .
H24B H -0.555827 0.171577 -0.016905 0.053 Uiso 1 1 d G . . . .
O4 O 0.6527(6) 0.3267(3) 0.5505(3) 0.0342(11) Uani 1 1 d . . . . .
O18 O 0.7966(5) 0.7468(3) 0.8084(3) 0.0319(10) Uani 1 1 d . . . . .
N1A N 0.1407(5) 0.4156(3) 0.4578(3) 0.0219(10) Uani 1 1 d . . . . .
O20 O 0.7971(5) 0.2299(4) 0.7991(3) 0.0319(10) Uani 1 1 d . . . . .
H20A H 0.728289 0.202492 0.812344 0.048 Uiso 1 1 d G . . . .
H20B H 0.830956 0.277314 0.847684 0.048 Uiso 1 1 d G . . . .
O3A O -0.0013(6) 0.3954(4) 0.5890(3) 0.0386(11) Uani 1 1 d . . . . .
O23 O -0.1119(6) 0.4640(4) 0.7407(3) 0.0414(12) Uani 1 1 d . . . . .
H23A H -0.084562 0.460959 0.693203 0.062 Uiso 1 1 d G . . . .
H23B H -0.192288 0.488833 0.744811 0.062 Uiso 1 1 d G . . . .
N3 N 1.0292(5) -0.0973(4) 0.3010(3) 0.0236(10) Uani 1 1 d . . . . .
H3 H 1.082483 -0.133328 0.263290 0.028 Uiso 1 1 calc R . . . .
N1 N 0.6269(5) 0.1039(3) 0.5784(3) 0.0217(10) Uani 1 1 d . . . . .
N2 N 0.7164(5) 0.0412(3) 0.5275(3) 0.0204(9) Uani 1 1 d . . . . .
O3 O 0.4604(6) 0.1725(4) 0.4707(3) 0.0396(12) Uani 1 1 d . . . . .
N2A N 0.0503(5) 0.3978(3) 0.3826(3) 0.0226(10) Uani 1 1 d . . . . .
O22 O 0.9163(7) 0.4988(5) 1.1097(4) 0.0470(13) Uani 1 1 d . . . . .
H22A H 0.972071 0.507772 1.156051 0.071 Uiso 1 1 d G . . . .
H22B H 0.829855 0.494583 1.122480 0.071 Uiso 1 1 d G . . . .
N3A N -0.3660(6) 0.2464(4) 0.1558(4) 0.0338(13) Uani 1 1 d . . . . .
H3AA H -0.435819 0.229957 0.112943 0.041 Uiso 1 1 calc R . . . .
C9 C 0.8642(6) 0.0140(4) 0.4171(4) 0.0218(11) Uani 1 1 d . . . . .
C1 C 0.4706(6) 0.1373(4) 0.6879(4) 0.0217(11) Uani 1 1 d . . . . .
O21 O 0.9292(9) 0.3759(4) 0.9338(4) 0.0581(17) Uani 1 1 d . . . . .
H21A H 0.969532 0.413604 0.917054 0.087 Uiso 1 1 d G . . . .
H21B H 0.931556 0.408391 0.989421 0.087 Uiso 1 1 d G . . . .
C4A C 0.5592(6) 0.5621(4) 0.6982(4) 0.0230(11) Uani 1 1 d . . . . .
C9A C -0.1522(6) 0.2980(4) 0.2901(4) 0.0220(11) Uani 1 1 d . . . . .
C2 C 0.4359(6) 0.2239(4) 0.6944(4) 0.0231(11) Uani 1 1 d . . . . .
C8 C 0.7715(6) 0.0722(4) 0.4788(4) 0.0196(11) Uani 1 1 d . . . . .
C6 C 0.4084(7) 0.1055(4) 0.7414(4) 0.0228(11) Uani 1 1 d . . . . .
H6A H 0.432971 0.048867 0.739842 0.027 Uiso 1 1 calc R . . . .
C3A C 0.4714(6) 0.4795(4) 0.6701(4) 0.0235(12) Uani 1 1 d . . . . .
H3AB H 0.486357 0.440715 0.697262 0.028 Uiso 1 1 calc R . . . .
C10 C 0.9268(6) 0.0424(4) 0.3629(4) 0.0224(11) Uani 1 1 d . . . . .
H10 H 0.913420 0.101497 0.366414 0.027 Uiso 1 1 calc R . . . .
C13 C 0.8870(6) -0.0727(4) 0.4121(4) 0.0215(11) Uani 1 1 d . . . . .
H13 H 0.844298 -0.093254 0.448859 0.026 Uiso 1 1 calc R . . . .
C8A C -0.0409(7) 0.3280(4) 0.3653(4) 0.0228(11) Uani 1 1 d . . . . .
C5 C 0.3127(6) 0.1539(4) 0.7963(4) 0.0237(12) Uani 1 1 d . . . . .
H5 H 0.271841 0.131192 0.832100 0.028 Uiso 1 1 calc R . . . .
C4 C 0.2773(7) 0.2374(4) 0.7978(4) 0.0254(12) Uani 1 1 d . . . . .
C12 C 0.9719(7) -0.1277(4) 0.3534(4) 0.0249(12) Uani 1 1 d . . . . .
H12 H 0.989949 -0.186190 0.349781 0.030 Uiso 1 1 calc R . . . .
C11 C 1.0094(7) -0.0157(4) 0.3032(4) 0.0261(12) Uani 1 1 d . . . . .
H11 H 1.051160 0.002408 0.264615 0.031 Uiso 1 1 calc R . . . .
C1A C 0.3417(6) 0.5111(4) 0.5603(4) 0.0219(11) Uani 1 1 d . . . . .
C6A C 0.4345(7) 0.5931(4) 0.5899(4) 0.0248(12) Uani 1 1 d . . . . .
H6AB H 0.423068 0.631267 0.561761 0.030 Uiso 1 1 calc R . . . .
C7 C 0.5657(6) 0.0815(4) 0.6307(4) 0.0211(11) Uani 1 1 d . . . . .
H7 H 0.584519 0.024950 0.631540 0.025 Uiso 1 1 calc R . . . .
C7A C 0.2356(6) 0.4867(4) 0.4864(4) 0.0213(11) Uani 1 1 d . . . . .
H7A H 0.235330 0.524367 0.457361 0.026 Uiso 1 1 calc R . . . .
C5A C 0.5401(7) 0.6191(4) 0.6578(4) 0.0252(12) Uani 1 1 d . . . . .
H5AC H 0.600099 0.675294 0.677327 0.030 Uiso 1 1 calc R . . . .
C10A C -0.2551(7) 0.2238(5) 0.2704(4) 0.0306(14) Uani 1 1 d . . . . .
H10A H -0.252235 0.190690 0.303872 0.037 Uiso 1 1 calc R . . . .
C3 C 0.3402(7) 0.2730(4) 0.7483(4) 0.0257(12) Uani 1 1 d . . . . .
H3A H 0.317390 0.330676 0.751489 0.031 Uiso 1 1 calc R . . . .
C11A C -0.3598(7) 0.1997(5) 0.2023(5) 0.0333(14) Uani 1 1 d . . . . .
H11A H -0.429243 0.148854 0.187778 0.040 Uiso 1 1 calc R . . . .
C2A C 0.3629(6) 0.4546(4) 0.6026(4) 0.0220(11) Uani 1 1 d . . . . .
C13A C -0.1619(7) 0.3452(5) 0.2401(5) 0.0327(14) Uani 1 1 d . . . . .
H13A H -0.094456 0.396550 0.252607 0.039 Uiso 1 1 calc R . . . .
C12A C -0.2705(8) 0.3167(5) 0.1721(5) 0.0363(15) Uani 1 1 d . . . . .
H12A H -0.276860 0.347603 0.136835 0.044 Uiso 1 1 calc R . . . .
N4 N 0.5970(10) 0.4806(7) 1.1072(6) 0.065(2) Uani 1 1 d . . . . .
C14 C 0.4773(11) 0.4619(7) 1.0828(6) 0.055(2) Uani 1 1 d . . . . .
C15 C 0.3231(14) 0.4428(10) 1.0551(8) 0.078(3) Uani 1 1 d . . . . .
H15A H 0.304996 0.421160 0.992446 0.117 Uiso 1 1 calc GR . . . .
H15B H 0.277032 0.499348 1.084623 0.117 Uiso 1 1 calc GR . . . .
H15C H 0.283760 0.395128 1.069609 0.117 Uiso 1 1 calc GR . . . .


_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
Mo3 Mo4 3.1782(6) . ?
Mo3 O13 1.962(4) . ?
Mo3 O17 1.750(4) . ?
Mo3 O12 1.962(4) . ?
Mo3 O11 2.384(4) 2_777 ?
Mo3 O11 2.151(4) . ?
Mo3 O8 1.688(4) . ?
Mo4 O13 1.988(4) . ?
Mo4 O14 1.899(5) . ?
Mo4 O12 2.318(4) 2_777 ?
Mo4 O11 2.258(4) . ?
Mo4 O9 1.705(5) . ?
Mo4 O18 1.722(5) . ?
Mo5 O15 1.922(4) . ?
Mo5 O17 2.271(4) 2_777 ?
Mo5 O14 1.937(5) . ?
Mo5 O11 2.447(4) . ?
Mo5 O10 1.712(5) . ?
Mo5 O19 1.699(4) . ?
Mo1 O2 2.020(4) . ?
Mo1 O1 1.918(4) . ?
Mo1 O5 2.350(5) . ?
Mo1 O4 1.708(5) . ?
Mo1 N1 2.236(5) . ?
Mo1 O3 1.698(5) . ?
Mo1A O2A 2.004(4) . ?
Mo1A O5A 2.345(4) . ?
Mo1A O1A 1.920(4) . ?
Mo1A O4A 1.702(5) . ?
Mo1A N1A 2.241(5) . ?
Mo1A O3A 1.702(5) . ?
Mo2 O13 2.297(4) 2_777 ?
Mo2 O15 1.896(4) . ?
Mo2 O7 1.725(4) . ?
Mo2 O12 2.021(4) . ?
Mo2 O11 2.390(4) . ?
Mo2 O16 1.689(5) . ?
O2 C8 1.309(7) . ?
O2A C8A 1.321(7) . ?
O1 C2 1.348(7) . ?
O1A C2A 1.343(7) . ?
O6A C4A 1.360(7) . ?
O6 C4 1.352(7) . ?
N1A N2A 1.398(7) . ?
N1A C7A 1.296(8) . ?
N3 C12 1.351(8) . ?
N3 C11 1.331(8) . ?
N1 N2 1.399(7) . ?
N1 C7 1.287(8) . ?
N2 C8 1.294(8) . ?
N2A C8A 1.288(8) . ?
N3A C11A 1.329(10) . ?
N3A C12A 1.323(10) . ?
C9 C8 1.470(8) . ?
C9 C10 1.380(8) . ?
C9 C13 1.402(8) . ?
C1 C2 1.419(8) . ?
C1 C6 1.402(8) . ?
C1 C7 1.436(8) . ?
C4A C3A 1.396(8) . ?
C4A C5A 1.398(9) . ?
C9A C8A 1.474(8) . ?
C9A C10A 1.399(9) . ?
C9A C13A 1.393(9) . ?
C2 C3 1.376(9) . ?
C6 C5 1.381(9) . ?
C3A C2A 1.378(8) . ?
C10 C11 1.390(9) . ?
C13 C12 1.377(9) . ?
C5 C4 1.404(9) . ?
C4 C3 1.387(9) . ?
C1A C6A 1.410(8) . ?
C1A C7A 1.441(8) . ?
C1A C2A 1.419(8) . ?
C6A C5A 1.363(9) . ?
C10A C11A 1.365(9) . ?
C13A C12A 1.378(9) . ?
N4 C14 1.141(13) . ?
C14 C15 1.458(15) . ?

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
O13 Mo3 Mo4 36.69(12) . . ?
O13 Mo3 O11 77.32(15) . 2_777 ?
O13 Mo3 O11 78.21(16) . . ?
O17 Mo3 Mo4 132.08(14) . . ?
O17 Mo3 O13 95.38(18) . . ?
O17 Mo3 O12 96.91(18) . . ?
O17 Mo3 O11 156.37(17) . . ?
O17 Mo3 O11 80.61(16) . 2_777 ?
O12 Mo3 Mo4 124.55(12) . . ?
O12 Mo3 O13 149.40(17) . . ?
O12 Mo3 O11 79.35(16) . . ?
O12 Mo3 O11 77.21(15) . 2_777 ?
O11 Mo3 Mo4 85.95(9) 2_777 . ?
O11 Mo3 Mo4 45.24(10) . . ?
O11 Mo3 O11 75.80(15) . 2_777 ?
O8 Mo3 Mo4 90.00(15) . . ?
O8 Mo3 O13 101.39(19) . . ?
O8 Mo3 O17 104.7(2) . . ?
O8 Mo3 O12 102.40(19) . . ?
O8 Mo3 O11 174.68(17) . 2_777 ?
O8 Mo3 O11 98.90(18) . . ?
O13 Mo4 Mo3 36.14(11) . . ?
O13 Mo4 O12 72.06(15) . 2_777 ?
O13 Mo4 O11 75.15(15) . . ?
O14 Mo4 Mo3 121.04(13) . . ?
O14 Mo4 O13 148.38(18) . . ?
O14 Mo4 O12 83.90(17) . 2_777 ?
O14 Mo4 O11 78.50(17) . . ?
O12 Mo4 Mo3 80.49(10) 2_777 . ?
O11 Mo4 Mo3 42.54(10) . . ?
O11 Mo4 O12 73.27(14) . 2_777 ?
O9 Mo4 Mo3 85.83(16) . . ?
O9 Mo4 O13 97.8(2) . . ?
O9 Mo4 O14 101.7(2) . . ?
O9 Mo4 O12 166.19(19) . 2_777 ?
O9 Mo4 O11 95.31(18) . . ?
O9 Mo4 O18 105.1(2) . . ?
O18 Mo4 Mo3 135.10(17) . . ?
O18 Mo4 O13 99.0(2) . . ?
O18 Mo4 O14 99.6(2) . . ?
O18 Mo4 O12 86.11(19) . 2_777 ?
O18 Mo4 O11 159.38(19) . . ?
O15 Mo5 O17 77.82(17) . 2_777 ?
O15 Mo5 O14 145.31(17) . . ?
O15 Mo5 O11 75.49(15) . . ?
O17 Mo5 O11 70.21(14) 2_777 . ?
O14 Mo5 O17 77.89(17) . 2_777 ?
O14 Mo5 O11 73.19(16) . . ?
O10 Mo5 O15 98.1(2) . . ?
O10 Mo5 O17 164.84(19) . 2_777 ?
O10 Mo5 O14 98.9(2) . . ?
O10 Mo5 O11 94.65(18) . . ?
O19 Mo5 O15 102.4(2) . . ?
O19 Mo5 O17 90.44(19) . 2_777 ?
O19 Mo5 O14 102.2(2) . . ?
O19 Mo5 O11 160.60(18) . . ?
O19 Mo5 O10 104.7(2) . . ?
O2 Mo1 O5 81.98(18) . . ?
O2 Mo1 N1 71.97(18) . . ?
O1 Mo1 O2 150.91(18) . . ?
O1 Mo1 O5 79.73(19) . . ?
O1 Mo1 N1 81.58(18) . . ?
O4 Mo1 O2 96.7(2) . . ?
O4 Mo1 O1 102.9(2) . . ?
O4 Mo1 O5 81.8(2) . . ?
O4 Mo1 N1 155.5(2) . . ?
N1 Mo1 O5 75.25(17) . . ?
O3 Mo1 O2 95.3(2) . . ?
O3 Mo1 O1 99.5(2) . . ?
O3 Mo1 O5 171.4(2) . . ?
O3 Mo1 O4 106.6(3) . . ?
O3 Mo1 N1 96.2(2) . . ?
O2A Mo1A O5A 77.91(16) . . ?
O2A Mo1A N1A 71.71(17) . . ?
O1A Mo1A O2A 148.36(19) . . ?
O1A Mo1A O5A 78.65(18) . . ?
O1A Mo1A N1A 82.09(18) . . ?
O4A Mo1A O2A 97.1(2) . . ?
O4A Mo1A O5A 85.2(2) . . ?
O4A Mo1A O1A 101.8(2) . . ?
O4A Mo1A N1A 159.3(2) . . ?
O4A Mo1A O3A 106.6(3) . . ?
N1A Mo1A O5A 75.60(17) . . ?
O3A Mo1A O2A 98.9(2) . . ?
O3A Mo1A O5A 168.2(2) . . ?
O3A Mo1A O1A 99.7(2) . . ?
O3A Mo1A N1A 92.6(2) . . ?
O13 Mo2 O11 71.36(13) 2_777 . ?
O15 Mo2 O13 83.66(16) . 2_777 ?
O15 Mo2 O12 145.99(17) . . ?
O15 Mo2 O11 77.37(16) . . ?
O7 Mo2 O13 162.31(18) . 2_777 ?
O7 Mo2 O15 102.5(2) . . ?
O7 Mo2 O12 95.05(19) . . ?
O7 Mo2 O11 93.62(18) . . ?
O12 Mo2 O13 71.96(15) . 2_777 ?
O12 Mo2 O11 72.63(15) . . ?
O16 Mo2 O13 89.61(19) . 2_777 ?
O16 Mo2 O15 103.0(2) . . ?
O16 Mo2 O7 104.8(2) . . ?
O16 Mo2 O12 100.3(2) . . ?
O16 Mo2 O11 160.87(18) . . ?
Mo3 O13 Mo4 107.16(18) . . ?
Mo3 O13 Mo2 112.54(17) . 2_777 ?
Mo4 O13 Mo2 104.57(17) . 2_777 ?
C8 O2 Mo1 118.8(4) . . ?
Mo2 O15 Mo5 117.3(2) . . ?
C8A O2A Mo1A 119.3(4) . . ?
Mo3 O17 Mo5 117.9(2) . 2_777 ?
C2 O1 Mo1 138.1(4) . . ?
Mo4 O14 Mo5 116.0(2) . . ?
Mo3 O12 Mo4 109.30(18) . 2_777 ?
Mo3 O12 Mo2 110.00(18) . . ?
Mo2 O12 Mo4 102.73(17) . 2_777 ?
Mo3 O11 Mo3 104.20(15) . 2_777 ?
Mo3 O11 Mo4 92.22(14) . . ?
Mo3 O11 Mo5 91.30(13) 2_777 . ?
Mo3 O11 Mo5 164.40(19) . . ?
Mo3 O11 Mo2 95.97(14) 2_777 . ?
Mo3 O11 Mo2 91.72(13) . . ?
Mo4 O11 Mo3 97.71(14) . 2_777 ?
Mo4 O11 Mo5 87.36(13) . . ?
Mo4 O11 Mo2 164.37(19) . . ?
Mo2 O11 Mo5 84.80(12) . . ?
C2A O1A Mo1A 133.8(4) . . ?
N2A N1A Mo1A 115.7(4) . . ?
C7A N1A Mo1A 128.0(4) . . ?
C7A N1A N2A 116.3(5) . . ?
C11 N3 C12 123.5(5) . . ?
N2 N1 Mo1 114.9(4) . . ?
C7 N1 Mo1 129.3(4) . . ?
C7 N1 N2 115.7(5) . . ?
C8 N2 N1 109.4(5) . . ?
C8A N2A N1A 108.4(5) . . ?
C12A N3A C11A 122.0(6) . . ?
C10 C9 C8 121.3(5) . . ?
C10 C9 C13 119.4(5) . . ?
C13 C9 C8 119.3(5) . . ?
C2 C1 C7 123.9(5) . . ?
C6 C1 C2 117.4(5) . . ?
C6 C1 C7 118.7(5) . . ?
O6A C4A C3A 116.9(5) . . ?
O6A C4A C5A 122.2(5) . . ?
C3A C4A C5A 120.8(6) . . ?
C10A C9A C8A 120.2(6) . . ?
C13A C9A C8A 121.1(5) . . ?
C13A C9A C10A 118.6(6) . . ?
O1 C2 C1 121.4(5) . . ?
O1 C2 C3 117.2(5) . . ?
C3 C2 C1 121.4(6) . . ?
O2 C8 C9 117.8(5) . . ?
N2 C8 O2 124.3(5) . . ?
N2 C8 C9 117.9(5) . . ?
C5 C6 C1 122.2(6) . . ?
C2A C3A C4A 119.7(6) . . ?
C9 C10 C11 119.7(6) . . ?
C12 C13 C9 119.3(6) . . ?
O2A C8A C9A 116.7(5) . . ?
N2A C8A O2A 124.7(6) . . ?
N2A C8A C9A 118.6(5) . . ?
C6 C5 C4 118.3(6) . . ?
O6 C4 C5 121.0(6) . . ?
O6 C4 C3 117.5(6) . . ?
C3 C4 C5 121.5(6) . . ?
N3 C12 C13 119.1(6) . . ?
N3 C11 C10 119.0(6) . . ?
C6A C1A C7A 118.7(5) . . ?
C6A C1A C2A 117.8(5) . . ?
C2A C1A C7A 123.5(5) . . ?
C5A C6A C1A 121.9(6) . . ?
N1 C7 C1 123.5(5) . . ?
N1A C7A C1A 122.9(5) . . ?
C6A C5A C4A 119.2(6) . . ?
C11A C10A C9A 118.8(7) . . ?
C2 C3 C4 119.2(6) . . ?
N3A C11A C10A 121.1(7) . . ?
O1A C2A C3A 116.3(5) . . ?
O1A C2A C1A 123.0(5) . . ?
C3A C2A C1A 120.6(5) . . ?
C12A C13A C9A 119.2(6) . . ?
N3A C12A C13A 120.3(7) . . ?
N4 C14 C15 176.9(13) . . ?

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

data_exp_4506
_database_code_depnum_ccdc_archive 'CCDC 2091118'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_exp_4506            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         23 Note
RESPONSE: Some of the low-angle reflections were fully or partially shadowed by the beam-stop. Those reflections were omitted from data reduction or refinement.
;
# Added during the CSD deposition process: Thursday 15 July 2021 11:07 AM
# end Validation Reply Form

_audit_creation_date             2021-06-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'bis((acetonitrile)-dioxo-(N-(2-oxy-4-hydroxybenzylidene)isonicotinylhydrazonato)-molybdenum(vi)) hexamolybdate acetonitrile solvate'
_chemical_formula_moiety         'Mo6 O19, 2(C15 H13 Mo N4 O5), 4(C2 H3 N)'
_chemical_formula_sum            'C38 H38 Mo8 N12 O29'
_chemical_formula_weight         1894.32
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.3622(7)
_cell_length_b                   10.7026(9)
_cell_length_c                   15.8530(10)
_cell_angle_alpha                106.074(6)
_cell_angle_beta                 92.475(6)
_cell_angle_gamma                107.934(7)
_cell_volume                     1437.8(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1930
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0010
_cell_measurement_theta_min      4.3400
_shelx_estimated_absorpt_T_max   0.916
_shelx_estimated_absorpt_T_min   0.469
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.1527
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16260
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.615
_diffrn_reflns_theta_min         4.053
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     46.00  72.00   1.00    7.50    --   28.34  57.00   0.00   26
  2  ω    -87.00  -3.00   1.00    7.50    --  -31.31 -77.00 -60.00   84
  3  ω    -80.00  18.00   1.00    7.50    --  -31.31 106.00-156.00   98
  4  ω   -100.00 -65.00   1.00    7.50    --  -31.31 -77.00  90.00   35
  5  ω    -46.00  -8.00   1.00    7.50    --  -31.31 -77.00  90.00   38
  6  ω    -62.00  42.00   1.00    7.50    --  -31.31  37.00-180.00  104
  7  ω   -103.00 -11.00   1.00    7.50    --  -31.31 -77.00  30.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4268
_reflns_number_total             9435
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         9435
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1813
_refine_ls_R_factor_gt           0.0738
_refine_ls_restrained_S_all      0.985
_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)+(0.0294P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1375
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C10(H10), C3(H3A), C7(H7), C13(H13), C5(H5A), C6(H6), C12(H12),
 C11(H11)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_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
Mo4 Mo 1.05812(8) 0.16985(7) 0.63666(4) 0.04213(18) Uani 1 1 d . . . . .
Mo1 Mo 0.51450(8) 0.29419(7) 0.15340(4) 0.04172(18) Uani 1 1 d . . . . .
Mo3 Mo 0.78502(8) -0.12382(7) 0.54544(4) 0.0473(2) Uani 1 1 d . . . . .
Mo2 Mo 0.86117(8) 0.11311(7) 0.44544(5) 0.0491(2) Uani 1 1 d . . . . .
O12 O 1.000000 0.000000 0.500000 0.0327(15) Uani 1 2 d S T P . .
O14 O 0.8749(6) 0.0391(5) 0.6473(3) 0.0487(14) Uani 1 1 d . . . . .
O2 O 0.4998(5) 0.1445(5) 0.2083(3) 0.0466(13) Uani 1 1 d . . . . .
O6 O 0.8416(6) -0.0404(5) 0.3463(3) 0.0467(13) Uani 1 1 d . . . . .
O7 O 0.7723(6) -0.2326(5) 0.4256(3) 0.0501(14) Uani 1 1 d . . . . .
O9 O 0.7177(6) 0.0000(5) 0.4941(3) 0.0539(14) Uani 1 1 d . . . . .
O13 O 0.9438(6) 0.2341(5) 0.5663(3) 0.0532(14) Uani 1 1 d . . . . .
O1 O 0.6197(6) 0.4139(5) 0.0895(3) 0.0503(14) Uani 1 1 d . . . . .
O11 O 0.9340(6) -0.1939(5) 0.5795(3) 0.0554(15) Uani 1 1 d . . . . .
N1 N 0.6370(6) 0.1596(6) 0.0775(3) 0.0325(13) Uani 1 1 d . . . . .
O4 O 0.4845(6) 0.4128(5) 0.2402(3) 0.0568(15) Uani 1 1 d . . . . .
O5 O 0.8803(8) 0.6371(6) -0.1047(4) 0.0703(18) Uani 1 1 d . . . . .
H5 H 0.877938 0.705180 -0.065928 0.105 Uiso 1 1 calc GR . . . .
O15 O 1.1046(6) 0.2905(6) 0.7352(3) 0.0602(15) Uani 1 1 d . . . . .
O3 O 0.3483(6) 0.2154(6) 0.0874(4) 0.0700(17) Uani 1 1 d . . . . .
O10 O 0.6301(7) -0.2087(6) 0.5798(3) 0.077(2) Uani 1 1 d . . . . .
N2 N 0.6273(6) 0.0429(6) 0.1034(4) 0.0396(14) Uani 1 1 d . . . . .
N4 N 0.7687(8) 0.3716(7) 0.2350(4) 0.0514(17) Uani 1 1 d . . . . .
N3 N 0.4877(7) -0.2759(7) 0.2829(4) 0.0481(16) Uani 1 1 d . . . . .
H3 H 0.473850 -0.341381 0.306375 0.058 Uiso 1 1 calc R . . . .
O8 O 0.7685(7) 0.2000(6) 0.4040(4) 0.082(2) Uani 1 1 d . . . . .
C9 C 0.5331(8) -0.0666(7) 0.2103(4) 0.0372(16) Uani 1 1 d . . . . .
N6 N 0.3781(8) -0.4110(8) 0.4103(4) 0.064(2) Uani 1 1 d . . . . .
C14 C 0.8872(10) 0.4037(8) 0.2710(5) 0.0444(19) Uani 1 1 d . . . . .
C8 C 0.5574(8) 0.0469(7) 0.1709(5) 0.0398(17) Uani 1 1 d . . . . .
C10 C 0.4644(8) -0.0632(8) 0.2867(5) 0.048(2) Uani 1 1 d . . . . .
H10 H 0.432699 0.010691 0.313774 0.058 Uiso 1 1 calc R . . . .
C15 C 1.0400(9) 0.4449(9) 0.3193(5) 0.056(2) Uani 1 1 d . . . . .
H15A H 1.111829 0.443184 0.277944 0.085 Uiso 1 1 calc GR . . . .
H15B H 1.042266 0.382018 0.351944 0.085 Uiso 1 1 calc GR . . . .
H15C H 1.065829 0.536481 0.359666 0.085 Uiso 1 1 calc GR . . . .
C3 C 0.7430(8) 0.5204(8) -0.0086(4) 0.0432(18) Uani 1 1 d . . . . .
H3A H 0.711940 0.595068 0.017444 0.052 Uiso 1 1 calc R . . . .
C4 C 0.8313(9) 0.5256(9) -0.0769(5) 0.048(2) Uani 1 1 d . . . . .
C7 C 0.7134(8) 0.1750(8) 0.0135(4) 0.0422(18) Uani 1 1 d . . . . .
H7 H 0.750929 0.105460 -0.014357 0.051 Uiso 1 1 calc R . . . .
C1 C 0.7440(8) 0.2917(8) -0.0171(4) 0.0377(17) Uani 1 1 d . . . . .
C13 C 0.5758(8) -0.1804(7) 0.1721(4) 0.0384(17) Uani 1 1 d . . . . .
H13 H 0.621168 -0.185568 0.120802 0.046 Uiso 1 1 calc R . . . .
C2 C 0.7014(8) 0.4077(8) 0.0209(4) 0.0413(18) Uani 1 1 d . . . . .
C5 C 0.8749(9) 0.4121(9) -0.1173(5) 0.053(2) Uani 1 1 d . . . . .
H5A H 0.932036 0.413212 -0.163795 0.063 Uiso 1 1 calc R . . . .
C6 C 0.8325(9) 0.2985(9) -0.0874(5) 0.051(2) Uani 1 1 d . . . . .
H6 H 0.862748 0.223610 -0.114191 0.061 Uiso 1 1 calc R . . . .
C12 C 0.5521(9) -0.2853(8) 0.2092(5) 0.052(2) Uani 1 1 d . . . . .
H12 H 0.580461 -0.361720 0.183361 0.063 Uiso 1 1 calc R . . . .
C11 C 0.4441(9) -0.1697(9) 0.3215(5) 0.053(2) Uani 1 1 d . . . . .
H11 H 0.399206 -0.167743 0.372802 0.064 Uiso 1 1 calc R . . . .
C18 C 0.3526(8) -0.4321(8) 0.4730(5) 0.0465(19) Uani 1 1 d . . . . .
C19 C 0.3204(10) -0.4599(8) 0.5560(5) 0.062(2) Uani 1 1 d . . . . .
H19A H 0.213057 -0.501462 0.553449 0.093 Uiso 1 1 calc GR . . . .
H19B H 0.356283 -0.375091 0.603828 0.093 Uiso 1 1 calc GR . . . .
H19C H 0.370762 -0.521626 0.565481 0.093 Uiso 1 1 calc GR . . . .
N5 N 0.9305(10) 0.8757(10) 0.0559(6) 0.089(3) Uani 1 1 d . . . . .
C16 C 0.9675(11) 0.9715(11) 0.1135(7) 0.064(3) Uani 1 1 d . . . . .
C17 C 1.0171(12) 1.0943(10) 0.1872(6) 0.084(3) Uani 1 1 d . . . . .
H17A H 1.060673 1.172381 0.166743 0.126 Uiso 1 1 calc GR . . . .
H17B H 1.091729 1.088198 0.227916 0.126 Uiso 1 1 calc GR . . . .
H17C H 0.932139 1.105058 0.216664 0.126 Uiso 1 1 calc GR . . . .


_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
Mo4 O12 2.3243(7) . ?
Mo4 O14 1.899(5) . ?
Mo4 O6 1.965(5) 2_756 ?
Mo4 O7 1.948(5) 2_756 ?
Mo4 O13 1.907(5) . ?
Mo4 O15 1.666(5) . ?
Mo1 O2 1.997(5) . ?
Mo1 O1 1.914(5) . ?
Mo1 N1 2.239(5) . ?
Mo1 O4 1.694(5) . ?
Mo1 O3 1.670(5) . ?
Mo1 N4 2.439(7) . ?
Mo3 O12 2.3103(6) . ?
Mo3 O14 1.943(5) . ?
Mo3 O7 1.910(5) . ?
Mo3 O9 1.970(5) . ?
Mo3 O11 1.898(6) . ?
Mo3 O10 1.661(5) . ?
Mo2 O12 2.3140(7) . ?
Mo2 O6 1.888(5) . ?
Mo2 O9 1.863(5) . ?
Mo2 O13 1.956(5) . ?
Mo2 O11 1.954(5) 2_756 ?
Mo2 O8 1.684(5) . ?
O2 C8 1.328(8) . ?
O1 C2 1.356(7) . ?
N1 N2 1.399(7) . ?
N1 C7 1.285(7) . ?
O5 C4 1.342(8) . ?
N2 C8 1.276(8) . ?
N4 C14 1.130(9) . ?
N3 C12 1.330(8) . ?
N3 C11 1.325(10) . ?
C9 C8 1.476(9) . ?
C9 C10 1.394(9) . ?
C9 C13 1.387(9) . ?
N6 C18 1.099(8) . ?
C14 C15 1.469(11) . ?
C10 C11 1.364(10) . ?
C3 C4 1.394(9) . ?
C3 C2 1.364(9) . ?
C4 C5 1.396(10) . ?
C7 C1 1.416(9) . ?
C1 C2 1.405(10) . ?
C1 C6 1.422(9) . ?
C13 C12 1.371(9) . ?
C5 C6 1.378(10) . ?
C18 C19 1.451(10) . ?
N5 C16 1.113(11) . ?
C16 C17 1.427(12) . ?

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
O14 Mo4 O12 76.83(13) . . ?
O14 Mo4 O6 86.5(2) . 2_756 ?
O14 Mo4 O7 152.8(2) . 2_756 ?
O14 Mo4 O13 89.2(2) . . ?
O6 Mo4 O12 75.87(13) 2_756 . ?
O7 Mo4 O12 76.10(14) 2_756 . ?
O7 Mo4 O6 84.5(2) 2_756 2_756 ?
O13 Mo4 O12 77.09(15) . . ?
O13 Mo4 O6 152.9(2) . 2_756 ?
O13 Mo4 O7 87.3(2) . 2_756 ?
O15 Mo4 O12 178.2(2) . . ?
O15 Mo4 O14 104.0(2) . . ?
O15 Mo4 O6 102.6(2) . 2_756 ?
O15 Mo4 O7 103.0(2) . 2_756 ?
O15 Mo4 O13 104.4(3) . . ?
O2 Mo1 N1 72.16(19) . . ?
O2 Mo1 N4 78.5(2) . . ?
O1 Mo1 O2 150.6(2) . . ?
O1 Mo1 N1 81.8(2) . . ?
O1 Mo1 N4 81.0(2) . . ?
N1 Mo1 N4 73.0(2) . . ?
O4 Mo1 O2 99.5(2) . . ?
O4 Mo1 O1 99.2(2) . . ?
O4 Mo1 N1 156.9(2) . . ?
O4 Mo1 N4 84.3(2) . . ?
O3 Mo1 O2 96.1(3) . . ?
O3 Mo1 O1 100.3(3) . . ?
O3 Mo1 N1 96.6(2) . . ?
O3 Mo1 O4 105.8(3) . . ?
O3 Mo1 N4 169.3(3) . . ?
O14 Mo3 O12 76.36(13) . . ?
O14 Mo3 O9 85.0(2) . . ?
O7 Mo3 O12 77.15(14) . . ?
O7 Mo3 O14 153.34(19) . . ?
O7 Mo3 O9 85.8(2) . . ?
O9 Mo3 O12 75.71(15) . . ?
O11 Mo3 O12 77.25(14) . . ?
O11 Mo3 O14 87.8(2) . . ?
O11 Mo3 O7 89.2(2) . . ?
O11 Mo3 O9 152.9(2) . . ?
O10 Mo3 O12 178.4(2) . . ?
O10 Mo3 O14 102.3(2) . . ?
O10 Mo3 O7 104.2(2) . . ?
O10 Mo3 O9 103.4(3) . . ?
O10 Mo3 O11 103.6(3) . . ?
O6 Mo2 O12 77.54(15) . . ?
O6 Mo2 O13 153.8(2) . . ?
O6 Mo2 O11 87.0(2) . 2_756 ?
O9 Mo2 O12 77.58(16) . . ?
O9 Mo2 O6 89.8(2) . . ?
O9 Mo2 O13 87.7(2) . . ?
O9 Mo2 O11 153.6(2) . 2_756 ?
O13 Mo2 O12 76.43(15) . . ?
O11 Mo2 O12 76.13(16) 2_756 . ?
O11 Mo2 O13 83.8(2) 2_756 . ?
O8 Mo2 O12 177.0(2) . . ?
O8 Mo2 O6 102.4(3) . . ?
O8 Mo2 O9 105.4(3) . . ?
O8 Mo2 O13 103.5(3) . . ?
O8 Mo2 O11 100.8(3) . 2_756 ?
Mo4 O12 Mo4 180.0 2_756 . ?
Mo3 O12 Mo4 90.10(2) 2_756 . ?
Mo3 O12 Mo4 89.91(2) 2_756 2_756 ?
Mo3 O12 Mo4 89.91(2) . . ?
Mo3 O12 Mo4 90.09(2) . 2_756 ?
Mo3 O12 Mo3 180.0 . 2_756 ?
Mo3 O12 Mo2 89.84(3) 2_756 2_756 ?
Mo3 O12 Mo2 90.16(3) 2_756 . ?
Mo3 O12 Mo2 89.84(3) . . ?
Mo3 O12 Mo2 90.16(3) . 2_756 ?
Mo2 O12 Mo4 89.95(3) . 2_756 ?
Mo2 O12 Mo4 89.95(3) 2_756 . ?
Mo2 O12 Mo4 90.05(3) . . ?
Mo2 O12 Mo4 90.05(3) 2_756 2_756 ?
Mo2 O12 Mo2 180.00(2) . 2_756 ?
Mo4 O14 Mo3 116.9(2) . . ?
C8 O2 Mo1 118.6(4) . . ?
Mo2 O6 Mo4 116.6(2) . 2_756 ?
Mo3 O7 Mo4 116.5(2) . 2_756 ?
Mo2 O9 Mo3 116.8(3) . . ?
Mo4 O13 Mo2 116.3(3) . . ?
C2 O1 Mo1 138.3(5) . . ?
Mo3 O11 Mo2 116.5(2) . 2_756 ?
N2 N1 Mo1 115.0(4) . . ?
C7 N1 Mo1 128.8(5) . . ?
C7 N1 N2 116.2(6) . . ?
C8 N2 N1 108.8(6) . . ?
C14 N4 Mo1 177.7(7) . . ?
C11 N3 C12 122.7(7) . . ?
C10 C9 C8 120.8(7) . . ?
C13 C9 C8 121.4(6) . . ?
C13 C9 C10 117.8(7) . . ?
N4 C14 C15 178.9(8) . . ?
O2 C8 C9 116.2(6) . . ?
N2 C8 O2 125.1(7) . . ?
N2 C8 C9 118.6(7) . . ?
C11 C10 C9 119.2(7) . . ?
C2 C3 C4 121.2(7) . . ?
O5 C4 C3 122.8(7) . . ?
O5 C4 C5 117.9(7) . . ?
C3 C4 C5 119.3(7) . . ?
N1 C7 C1 123.8(7) . . ?
C7 C1 C6 118.8(6) . . ?
C2 C1 C7 124.7(6) . . ?
C2 C1 C6 116.4(7) . . ?
C12 C13 C9 120.8(6) . . ?
O1 C2 C3 117.0(7) . . ?
O1 C2 C1 121.5(7) . . ?
C3 C2 C1 121.5(6) . . ?
C6 C5 C4 119.3(7) . . ?
C5 C6 C1 122.3(7) . . ?
N3 C12 C13 118.8(7) . . ?
N3 C11 C10 120.7(7) . . ?
N6 C18 C19 179.4(9) . . ?
N5 C16 C17 179.2(11) . . ?

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

data_exp_5005
_database_code_depnum_ccdc_archive 'CCDC 2091114'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_exp_5005            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         24 Note
RESPONSE: Some of the low-angle reflections were fully or partially shadowed by the beam-stop. Those reflections were omitted from data reduction or refinement.
;
# Added during the CSD deposition process: Thursday 15 July 2021 10:39 AM
# end Validation Reply Form

_audit_creation_date             2021-07-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'bis((aquo)-dioxo-(N-(2-oxy-4-methoxybenzylidene)isonicotinylhydrazonato)-molybdenum(vi)) hexamolybdate acetonitrile solvate'
_chemical_formula_moiety         'Mo6 O19, 2(C14 H14 Mo N3 O6), 4(C2 H3 N)'
_chemical_formula_sum            'C36 H40 Mo8 N10 O31'
_chemical_formula_weight         1876.30
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.8617(4)
_cell_length_b                   10.9074(4)
_cell_length_c                   13.8765(6)
_cell_angle_alpha                97.652(3)
_cell_angle_beta                 107.915(3)
_cell_angle_gamma                114.577(4)
_cell_volume                     1356.26(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7355
_cell_measurement_temperature    150
_cell_measurement_theta_max      32.0980
_cell_measurement_theta_min      4.2240
_shelx_estimated_absorpt_T_max   0.819
_shelx_estimated_absorpt_T_min   0.692
_exptl_absorpt_coefficient_mu    1.891
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.297
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22244
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         4.259
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     69.00 101.00   1.00    1.00    --   28.65 179.00 -90.00   32
  2  ω     49.00  88.00   1.00    1.00    --   28.65 179.00  90.00   39
  3  ω    -96.00  43.00   1.00    1.00    --  -31.62  19.00 -60.00  139
  4  ω   -111.00 -44.00   1.00    1.00    --  -31.62-179.00 -30.00   67
  5  ω    -70.00  -8.00   1.00    1.00    --  -31.62 -57.00  30.00   62
  6  ω    -64.00 -36.00   1.00    1.00    --  -31.62 -57.00 -30.00   28
  7  ω   -107.00 -80.00   1.00    1.00    --  -31.62 179.00  60.00   27
  8  ω    -58.00 -32.00   1.00    1.00    --  -31.62 179.00  60.00   26
  9  ω   -107.00   3.00   1.00    1.00    --  -31.62 -19.00-180.00  110
 10  ω    -76.00 -32.00   1.00    1.00    --  -31.62 179.00  30.00   44
 11  ω     43.00  71.00   1.00    1.00    --   28.65 -99.00 150.00   28
 12  ω     16.00  73.00   1.00    1.00    --   28.65 -99.00 -90.00   57
 13  ω    -46.00  -7.00   1.00    1.00    --  -31.62 -77.00   0.00   39
 14  ω     12.00  39.00   1.00    1.00    --  -31.62  77.00 150.00   27
 15  ω   -102.00 -44.00   1.00    1.00    --  -31.62 -57.00 -60.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6501
_reflns_number_total             7891
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.443
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7891
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.136
_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)+(0.0338P)²+0.3977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0847
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H6A-O6
 0.86 with sigma of 0.02
 O6-H6B
 0.86 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C7(H7), C5(H5), C3(H3A), C6(H6), C13(H13), C12(H12), C11(H11), C10(H10)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo3 Mo -0.05093(3) 0.65943(3) 0.08447(2) 0.01883(7) Uani 1 1 d . . . . .
Mo2 Mo 0.17128(3) 0.52653(3) 0.16301(2) 0.01917(7) Uani 1 1 d . . . . .
Mo4 Mo 0.18374(3) 0.68365(3) -0.02174(2) 0.01763(7) Uani 1 1 d . . . . .
Mo1 Mo 0.73160(3) 0.77860(3) 0.54234(2) 0.01834(7) Uani 1 1 d . . . . .
O12 O 0.000000 0.500000 0.000000 0.0156(6) Uani 1 2 d S T P . .
O13 O 0.1915(2) 0.5233(2) -0.08622(17) 0.0200(4) Uani 1 1 d . . . . .
O8 O 0.1932(2) 0.4096(2) 0.06794(17) 0.0212(5) Uani 1 1 d . . . . .
O9 O 0.2855(2) 0.6841(2) 0.11197(17) 0.0210(5) Uani 1 1 d . . . . .
O15 O 0.0907(2) 0.7736(2) 0.03729(17) 0.0206(5) Uani 1 1 d . . . . .
O11 O -0.0016(3) 0.3842(2) 0.15643(17) 0.0224(5) Uani 1 1 d . . . . .
O10 O 0.0973(2) 0.6592(2) 0.19661(16) 0.0210(5) Uani 1 1 d . . . . .
O2 O 0.6037(3) 0.8419(2) 0.44641(17) 0.0219(5) Uani 1 1 d . . . . .
O1 O 0.8562(3) 0.6923(2) 0.56419(17) 0.0229(5) Uani 1 1 d . . . . .
O6 O 0.5773(3) 0.5743(3) 0.39236(19) 0.0249(5) Uani 1 1 d D . . . .
O14 O 0.3070(3) 0.8198(2) -0.04475(18) 0.0245(5) Uani 1 1 d . . . . .
O3 O 0.8509(3) 0.9406(2) 0.63237(17) 0.0252(5) Uani 1 1 d . . . . .
O16 O -0.0946(3) 0.7702(2) 0.14413(18) 0.0251(5) Uani 1 1 d . . . . .
O4 O 0.6068(3) 0.6951(2) 0.59314(18) 0.0255(5) Uani 1 1 d . . . . .
O5 O 1.2771(3) 0.6238(3) 0.63470(18) 0.0286(5) Uani 1 1 d . . . . .
O7 O 0.3026(3) 0.5603(3) 0.28246(18) 0.0305(6) Uani 1 1 d . . . . .
N1 N 0.8158(3) 0.8308(3) 0.41778(19) 0.0184(5) Uani 1 1 d . . . . .
N2 N 0.7468(3) 0.8877(3) 0.3491(2) 0.0208(5) Uani 1 1 d . . . . .
N3 N 0.3930(3) 1.0518(3) 0.1921(2) 0.0230(6) Uani 1 1 d . . . . .
H3 H 0.341564 1.086772 0.155079 0.028 Uiso 1 1 calc R . . . .
C8 C 0.6408(3) 0.8897(3) 0.3719(2) 0.0184(6) Uani 1 1 d . . . . .
C1 C 1.0018(3) 0.7589(3) 0.4604(2) 0.0179(6) Uani 1 1 d . . . . .
C2 C 0.9741(3) 0.7066(3) 0.5434(2) 0.0186(6) Uani 1 1 d . . . . .
C7 C 0.9167(3) 0.8123(3) 0.3983(2) 0.0190(6) Uani 1 1 d . . . . .
H7 H 0.935326 0.835752 0.338877 0.023 Uiso 1 1 calc R . . . .
N5 N 0.5827(4) 0.7769(4) -0.0176(3) 0.0448(9) Uani 1 1 d . . . . .
C5 C 1.2087(4) 0.7124(3) 0.4965(2) 0.0223(7) Uani 1 1 d . . . . .
H5 H 1.287032 0.712324 0.479673 0.027 Uiso 1 1 calc R . . . .
C3 C 1.0653(4) 0.6614(3) 0.6044(2) 0.0202(6) Uani 1 1 d . . . . .
H3A H 1.047645 0.628248 0.661330 0.024 Uiso 1 1 calc R . . . .
C6 C 1.1196(4) 0.7584(3) 0.4387(2) 0.0226(7) Uani 1 1 d . . . . .
H6 H 1.137926 0.791196 0.381806 0.027 Uiso 1 1 calc R . . . .
N4 N 0.1603(4) 1.1124(4) 0.1273(3) 0.0419(8) Uani 1 1 d . . . . .
C9 C 0.5544(3) 0.9481(3) 0.3095(2) 0.0186(6) Uani 1 1 d . . . . .
C13 C 0.5864(4) 0.9978(3) 0.2277(2) 0.0221(6) Uani 1 1 d . . . . .
H13 H 0.665309 0.995906 0.212635 0.027 Uiso 1 1 calc R . . . .
C12 C 0.5032(4) 1.0493(3) 0.1694(3) 0.0230(7) Uani 1 1 d . . . . .
H12 H 0.523609 1.082824 0.113395 0.028 Uiso 1 1 calc R . . . .
C4 C 1.1828(4) 0.6654(3) 0.5810(2) 0.0218(6) Uani 1 1 d . . . . .
C15 C 0.0562(4) 1.0925(4) 0.1391(3) 0.0284(7) Uani 1 1 d . . . . .
C11 C 0.3583(4) 1.0038(4) 0.2682(3) 0.0247(7) Uani 1 1 d . . . . .
H11 H 0.277917 1.005910 0.280710 0.030 Uiso 1 1 calc R . . . .
C17 C 0.5759(4) 0.7121(4) 0.0398(3) 0.0314(8) Uani 1 1 d . . . . .
C10 C 0.4377(4) 0.9513(3) 0.3287(3) 0.0229(7) Uani 1 1 d . . . . .
H10 H 0.413040 0.917346 0.383428 0.028 Uiso 1 1 calc R . . . .
C14 C 1.2632(4) 0.5824(4) 0.7264(3) 0.0291(8) Uani 1 1 d . . . . .
H14A H 1.164482 0.502254 0.705499 0.044 Uiso 1 1 calc GR . . . .
H14B H 1.277610 0.661962 0.779097 0.044 Uiso 1 1 calc GR . . . .
H14C H 1.338180 0.554766 0.757137 0.044 Uiso 1 1 calc GR . . . .
C16 C -0.0765(4) 1.0658(4) 0.1564(3) 0.0299(8) Uani 1 1 d . . . . .
H16A H -0.161341 1.025039 0.087718 0.045 Uiso 1 1 calc GR . . . .
H16B H -0.064588 1.154877 0.194882 0.045 Uiso 1 1 calc GR . . . .
H16C H -0.093359 0.999495 0.198183 0.045 Uiso 1 1 calc GR . . . .
C18 C 0.5656(4) 0.6274(4) 0.1125(3) 0.0355(9) Uani 1 1 d . . . . .
H18A H 0.461568 0.559949 0.093274 0.053 Uiso 1 1 calc GR . . . .
H18B H 0.608394 0.689401 0.185272 0.053 Uiso 1 1 calc GR . . . .
H18C H 0.620032 0.575738 0.108054 0.053 Uiso 1 1 calc GR . . . .
H6A H 0.494(3) 0.570(5) 0.365(3) 0.043 Uiso 1 1 d DR . . . .
H6B H 0.569(5) 0.505(3) 0.415(3) 0.052(15) Uiso 1 1 d 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
Mo3 O12 2.3152(3) . ?
Mo3 O13 1.951(2) 2_565 ?
Mo3 O8 2.006(2) 2_565 ?
Mo3 O15 1.894(2) . ?
Mo3 O10 1.865(2) . ?
Mo3 O16 1.680(2) . ?
Mo2 O12 2.3346(3) . ?
Mo2 O8 1.850(2) . ?
Mo2 O9 2.021(2) . ?
Mo2 O11 1.838(2) . ?
Mo2 O10 1.993(2) . ?
Mo2 O7 1.693(2) . ?
Mo4 O12 2.3005(3) . ?
Mo4 O13 1.902(2) . ?
Mo4 O9 1.843(2) . ?
Mo4 O15 1.943(2) . ?
Mo4 O11 2.023(2) 2_565 ?
Mo4 O14 1.684(2) . ?
Mo1 O2 2.021(2) . ?
Mo1 O1 1.922(2) . ?
Mo1 O6 2.370(2) . ?
Mo1 O3 1.695(2) . ?
Mo1 O4 1.702(2) . ?
Mo1 N1 2.225(3) . ?
O2 C8 1.314(4) . ?
O1 C2 1.349(4) . ?
O5 C4 1.348(4) . ?
O5 C14 1.435(4) . ?
N1 N2 1.400(4) . ?
N1 C7 1.291(4) . ?
N2 C8 1.293(4) . ?
N3 C12 1.337(4) . ?
N3 C11 1.326(4) . ?
C8 C9 1.476(4) . ?
C1 C2 1.409(4) . ?
C1 C7 1.424(4) . ?
C1 C6 1.403(5) . ?
C2 C3 1.394(4) . ?
N5 C17 1.132(5) . ?
C5 C6 1.366(5) . ?
C5 C4 1.400(4) . ?
C3 C4 1.396(5) . ?
N4 C15 1.128(5) . ?
C9 C13 1.396(4) . ?
C9 C10 1.387(5) . ?
C13 C12 1.371(5) . ?
C15 C16 1.450(5) . ?
C11 C10 1.367(5) . ?
C17 C18 1.455(6) . ?

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
O13 Mo3 O12 76.07(6) 2_565 . ?
O13 Mo3 O8 82.54(9) 2_565 2_565 ?
O8 Mo3 O12 75.24(6) 2_565 . ?
O15 Mo3 O12 76.99(7) . . ?
O15 Mo3 O13 152.43(9) . 2_565 ?
O15 Mo3 O8 85.07(9) . 2_565 ?
O10 Mo3 O12 77.80(7) . . ?
O10 Mo3 O13 89.21(10) . 2_565 ?
O10 Mo3 O8 152.98(9) . 2_565 ?
O10 Mo3 O15 90.78(10) . . ?
O16 Mo3 O12 177.82(8) . . ?
O16 Mo3 O13 102.02(11) . 2_565 ?
O16 Mo3 O8 103.56(10) . 2_565 ?
O16 Mo3 O15 104.80(11) . . ?
O16 Mo3 O10 103.32(11) . . ?
O8 Mo2 O12 77.61(7) . . ?
O8 Mo2 O9 85.99(10) . . ?
O8 Mo2 O10 151.76(9) . . ?
O9 Mo2 O12 74.96(6) . . ?
O11 Mo2 O12 78.00(7) . . ?
O11 Mo2 O8 93.92(10) . . ?
O11 Mo2 O9 152.33(9) . . ?
O11 Mo2 O10 87.00(10) . . ?
O10 Mo2 O12 74.99(6) . . ?
O10 Mo2 O9 80.50(9) . . ?
O7 Mo2 O12 175.26(9) . . ?
O7 Mo2 O8 104.64(11) . . ?
O7 Mo2 O9 100.91(11) . . ?
O7 Mo2 O11 105.83(11) . . ?
O7 Mo2 O10 102.21(11) . . ?
O13 Mo4 O12 77.35(7) . . ?
O13 Mo4 O15 153.06(9) . . ?
O13 Mo4 O11 84.52(9) . 2_565 ?
O9 Mo4 O12 79.11(7) . . ?
O9 Mo4 O13 91.37(10) . . ?
O9 Mo4 O15 89.77(10) . . ?
O9 Mo4 O11 154.50(9) . 2_565 ?
O15 Mo4 O12 76.45(6) . . ?
O15 Mo4 O11 82.97(9) . 2_565 ?
O11 Mo4 O12 75.43(6) 2_565 . ?
O14 Mo4 O12 175.20(8) . . ?
O14 Mo4 O13 104.41(10) . . ?
O14 Mo4 O9 105.20(11) . . ?
O14 Mo4 O15 101.23(10) . . ?
O14 Mo4 O11 100.20(10) . 2_565 ?
O2 Mo1 O6 78.28(9) . . ?
O2 Mo1 N1 72.03(9) . . ?
O1 Mo1 O2 150.42(9) . . ?
O1 Mo1 O6 81.81(9) . . ?
O1 Mo1 N1 81.81(10) . . ?
O3 Mo1 O2 95.55(10) . . ?
O3 Mo1 O1 100.13(11) . . ?
O3 Mo1 O6 168.87(10) . . ?
O3 Mo1 O4 105.54(11) . . ?
O3 Mo1 N1 94.51(10) . . ?
O4 Mo1 O2 95.04(10) . . ?
O4 Mo1 O1 104.58(11) . . ?
O4 Mo1 O6 84.38(10) . . ?
O4 Mo1 N1 157.25(10) . . ?
N1 Mo1 O6 74.84(9) . . ?
Mo3 O12 Mo3 180.0 . 2_565 ?
Mo3 O12 Mo2 90.089(11) 2_565 2_565 ?
Mo3 O12 Mo2 89.912(10) 2_565 . ?
Mo3 O12 Mo2 90.088(10) . . ?
Mo3 O12 Mo2 89.911(11) . 2_565 ?
Mo2 O12 Mo2 180.0 . 2_565 ?
Mo4 O12 Mo3 90.316(11) . 2_565 ?
Mo4 O12 Mo3 89.683(10) . . ?
Mo4 O12 Mo3 89.684(10) 2_565 2_565 ?
Mo4 O12 Mo3 90.317(11) 2_565 . ?
Mo4 O12 Mo2 89.868(10) 2_565 2_565 ?
Mo4 O12 Mo2 89.866(11) . . ?
Mo4 O12 Mo2 90.133(11) 2_565 . ?
Mo4 O12 Mo2 90.133(11) . 2_565 ?
Mo4 O12 Mo4 180.0 . 2_565 ?
Mo4 O13 Mo3 116.26(11) . 2_565 ?
Mo2 O8 Mo3 116.78(11) . 2_565 ?
Mo4 O9 Mo2 115.77(11) . . ?
Mo3 O15 Mo4 116.02(11) . . ?
Mo2 O11 Mo4 116.31(11) . 2_565 ?
Mo3 O10 Mo2 117.00(10) . . ?
C8 O2 Mo1 118.7(2) . . ?
C2 O1 Mo1 136.1(2) . . ?
C4 O5 C14 118.3(3) . . ?
N2 N1 Mo1 115.5(2) . . ?
C7 N1 Mo1 128.9(2) . . ?
C7 N1 N2 115.5(3) . . ?
C8 N2 N1 109.0(3) . . ?
C11 N3 C12 122.6(3) . . ?
O2 C8 C9 117.8(3) . . ?
N2 C8 O2 124.3(3) . . ?
N2 C8 C9 117.9(3) . . ?
C2 C1 C7 123.2(3) . . ?
C6 C1 C2 118.1(3) . . ?
C6 C1 C7 118.7(3) . . ?
O1 C2 C1 122.1(3) . . ?
O1 C2 C3 117.3(3) . . ?
C3 C2 C1 120.6(3) . . ?
N1 C7 C1 124.1(3) . . ?
C6 C5 C4 119.0(3) . . ?
C2 C3 C4 119.3(3) . . ?
C5 C6 C1 122.2(3) . . ?
C13 C9 C8 120.5(3) . . ?
C10 C9 C8 120.9(3) . . ?
C10 C9 C13 118.7(3) . . ?
C12 C13 C9 119.6(3) . . ?
N3 C12 C13 119.5(3) . . ?
O5 C4 C5 115.1(3) . . ?
O5 C4 C3 124.1(3) . . ?
C3 C4 C5 120.8(3) . . ?
N4 C15 C16 178.7(4) . . ?
N3 C11 C10 120.4(3) . . ?
N5 C17 C18 179.3(5) . . ?
C11 C10 C9 119.4(3) . . ?

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

data_exp_5022_twin1_hklf5
_database_code_depnum_ccdc_archive 'CCDC 2091111'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_exp_5022_twin1_hklf5 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         22 Note
RESPONSE: Some of the low-angle reflections were fully or partially shadowed by the beam-stop. Those reflections were omitted from data reduction or refinement.
;
# Added during the CSD deposition process: Thursday 15 July 2021 08:36 AM
# end Validation Reply Form

_audit_creation_date             2021-07-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[bis-(N'-(2-oxo-3-methoxybenzylidene)isonicotinoylhydrazonato)tetraoxodimolybdenum(vi) hexamolybdate"
_chemical_formula_moiety         'Mo6 O19, C28 H24 Mo2 N6 O10'
_chemical_formula_sum            'C28 H24 Mo8 N6 O29'
_chemical_formula_weight         1676.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo8 O27 C24 N6 H20'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   7.5406(6)
_cell_length_b                   8.6650(15)
_cell_length_c                   17.325(3)
_cell_angle_alpha                103.429(14)
_cell_angle_beta                 90.359(9)
_cell_angle_gamma                89.999(10)
_cell_volume                     1101.0(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1869
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.1530
_cell_measurement_theta_min      4.5300
_shelx_estimated_absorpt_T_max   0.982
_shelx_estimated_absorpt_T_min   0.392
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             802
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.008
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.2860
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9183
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.723
_diffrn_reflns_theta_min         4.511
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     44.00  70.00   1.00   10.00    --   28.19  57.00 150.00   26
  2  ω    -57.00 -18.00   1.00   10.00    --  -31.31 -57.00   0.00   39
  3  ω    -51.00  29.00   1.00   10.00    --  -31.31  77.00   0.00   80
  4  ω    -57.00  26.00   1.00   10.00    --  -31.31  77.00  90.00   83
  5  ω    -98.00  -6.00   1.00   10.00    --  -31.31 -37.00-180.00   92
  6  ω    -52.00  33.00   1.00   10.00    --  -31.31  57.00-120.00   85
  7  ω   -101.00 -10.00   1.00   10.00    --  -31.31 -57.00 -60.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0889549000
_diffrn_orient_matrix_UB_12      0.0235829000
_diffrn_orient_matrix_UB_13      -0.0039120000
_diffrn_orient_matrix_UB_21      0.0202574000
_diffrn_orient_matrix_UB_22      -0.0775962000
_diffrn_orient_matrix_UB_23      -0.0220395000
_diffrn_orient_matrix_UB_31      -0.0229766000
_diffrn_orient_matrix_UB_32      0.0223859000
_diffrn_orient_matrix_UB_33      -0.0356627000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3706
_reflns_number_total             9183
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         3.613
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.274
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.780
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         9183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1783
_refine_ls_R_factor_gt           0.0765
_refine_ls_restrained_S_all      0.780
_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)+(0.0756P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1486
_refine_ls_wR_factor_ref         0.1747
_refine_special_details          'Refined as a 2-component perfect twin.,Twin'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), N3(H3), C5(H5), C11(H11), C12(H12), C10(H10), C6(H6), C4(H4), C13(H13)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo2 Mo 0.12342(15) 0.04691(14) 0.12609(7) 0.0286(3) Uani 1 1 d . . . . .
Mo3 Mo -0.22015(16) 0.18626(14) 0.04569(8) 0.0293(3) Uani 1 1 d . . . . .
Mo4 Mo -0.18061(15) -0.19421(13) 0.02894(8) 0.0269(3) Uani 1 1 d . . . . .
Mo1 Mo 0.43082(16) 0.31624(14) 0.46194(8) 0.0279(3) Uani 1 1 d . . . . .
O12 O -0.3251(10) -0.0140(10) 0.0564(5) 0.028(2) Uani 1 1 d . . . . .
O9 O -0.0882(12) 0.1922(10) 0.1361(6) 0.034(2) Uani 1 1 d . . . . .
O8 O -0.0501(11) -0.1105(10) 0.1279(6) 0.030(2) Uani 1 1 d . . . . .
O6 O 0.2027(12) 0.0919(11) 0.2186(6) 0.038(2) Uani 1 1 d . . . . .
O11 O -0.3001(13) -0.3385(10) 0.0524(6) 0.038(3) Uani 1 1 d . . . . .
O10 O 0.000000 0.000000 0.000000 0.024(3) Uani 1 2 d S T P . .
O13 O -0.3791(12) 0.3187(11) 0.0757(7) 0.045(3) Uani 1 1 d . . . . .
O4 O 0.6350(11) 0.4082(10) 0.4846(5) 0.030(2) Uani 1 1 d . . . . .
O2 O 0.3937(12) 0.3957(11) 0.3627(6) 0.034(2) Uani 1 1 d . . . . .
O1 O 0.3489(11) 0.2977(11) 0.5621(5) 0.037(2) Uani 1 1 d . . . . .
N2 N 0.0923(14) 0.3872(13) 0.3754(7) 0.031(3) Uani 1 1 d . . . . .
N1 N 0.1452(14) 0.3265(12) 0.4407(6) 0.029(3) Uani 1 1 d . . . . .
O3 O 0.4704(14) 0.1264(11) 0.4207(6) 0.046(3) Uani 1 1 d . . . . .
C1 C 0.0415(17) 0.2213(15) 0.5473(9) 0.032(3) Uani 1 1 d . . . . .
C7 C 0.0192(17) 0.2793(15) 0.4792(8) 0.032(3) Uani 1 1 d . . . . .
H7 H -0.095796 0.284038 0.460144 0.039 Uiso 1 1 calc R . . . .
C8 C 0.2313(19) 0.4153(15) 0.3387(9) 0.032(3) Uani 1 1 d . . . . .
C9 C 0.2092(18) 0.4785(14) 0.2666(8) 0.027(3) Uani 1 1 d . . . . .
N3 N 0.1619(16) 0.5799(13) 0.1326(7) 0.035(3) Uani 1 1 d . . . . .
H3 H 0.145612 0.610736 0.089360 0.042 Uiso 1 1 calc R . . . .
O5 O 0.3900(13) 0.1798(12) 0.6881(6) 0.043(3) Uani 1 1 d . . . . .
C5 C -0.079(2) 0.0840(18) 0.6414(10) 0.044(4) Uani 1 1 d . . . . .
H5 H -0.174261 0.034319 0.659779 0.053 Uiso 1 1 calc R . . . .
C3 C 0.2255(19) 0.1597(16) 0.6541(8) 0.033(3) Uani 1 1 d . . . . .
C11 C 0.326(2) 0.5555(17) 0.1543(9) 0.042(4) Uani 1 1 d . . . . .
H11 H 0.421783 0.572462 0.123670 0.050 Uiso 1 1 calc R . . . .
C12 C 0.024(2) 0.5594(16) 0.1738(8) 0.035(3) Uani 1 1 d . . . . .
H12 H -0.088095 0.582117 0.156938 0.042 Uiso 1 1 calc R . . . .
C10 C 0.353(2) 0.5046(17) 0.2229(9) 0.040(4) Uani 1 1 d . . . . .
H10 H 0.467737 0.487966 0.239565 0.048 Uiso 1 1 calc R . . . .
C6 C -0.104(2) 0.1503(17) 0.5779(8) 0.037(4) Uani 1 1 d . . . . .
H6 H -0.215602 0.148962 0.554650 0.045 Uiso 1 1 calc R . . . .
C4 C 0.085(2) 0.0896(17) 0.6789(10) 0.049(4) Uani 1 1 d . . . . .
H4 H 0.097171 0.043747 0.722125 0.058 Uiso 1 1 calc R . . . .
C2 C 0.2071(17) 0.2238(15) 0.5860(8) 0.029(3) Uani 1 1 d . . . . .
C13 C 0.0414(19) 0.5054(16) 0.2411(8) 0.034(3) Uani 1 1 d . . . . .
H13 H -0.057908 0.487116 0.269269 0.041 Uiso 1 1 calc R . . . .
C14 C 0.428(2) 0.092(2) 0.7490(10) 0.056(5) Uani 1 1 d . . . . .
H14A H 0.403969 -0.018330 0.728292 0.084 Uiso 1 1 calc GR . . . .
H14B H 0.355180 0.131997 0.794450 0.084 Uiso 1 1 calc GR . . . .
H14C H 0.550951 0.106002 0.764315 0.084 Uiso 1 1 calc GR . . . .
O7 O 0.2767(11) -0.1039(10) 0.0707(5) 0.029(2) Uani 1 1 d . . . . .
O15 O -0.2295(12) -0.2069(10) -0.0798(6) 0.032(2) Uani 1 1 d . . . . .
O14 O -0.0433(11) 0.3077(9) 0.0066(5) 0.027(2) 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
Mo2 O9 2.015(9) . ?
Mo2 O8 1.896(8) . ?
Mo2 O6 1.666(9) . ?
Mo2 O10 2.3164(12) . ?
Mo2 O7 1.843(9) . ?
Mo2 O15 1.931(9) 2 ?
Mo3 O12 1.956(8) . ?
Mo3 O9 1.840(9) . ?
Mo3 O10 2.3260(12) . ?
Mo3 O13 1.659(9) . ?
Mo3 O7 2.019(9) 2 ?
Mo3 O14 1.920(8) . ?
Mo4 O12 1.874(8) . ?
Mo4 O8 1.959(10) . ?
Mo4 O11 1.668(8) . ?
Mo4 O10 2.3106(11) . ?
Mo4 O15 1.895(10) . ?
Mo4 O14 1.982(8) 2 ?
Mo1 O4 1.734(9) . ?
Mo1 O4 2.405(9) 2_666 ?
Mo1 O2 2.012(9) . ?
Mo1 O1 1.887(9) . ?
Mo1 N1 2.188(11) . ?
Mo1 O3 1.662(9) . ?
O2 C8 1.315(16) . ?
O1 C2 1.362(14) . ?
N2 N1 1.409(14) . ?
N2 C8 1.281(17) . ?
N1 C7 1.284(16) . ?
C1 C7 1.396(18) . ?
C1 C6 1.421(17) . ?
C1 C2 1.411(18) . ?
C8 C9 1.486(18) . ?
C9 C10 1.377(18) . ?
C9 C13 1.375(17) . ?
N3 C11 1.324(17) . ?
N3 C12 1.298(17) . ?
O5 C3 1.364(16) . ?
O5 C14 1.463(16) . ?
C5 C6 1.365(19) . ?
C5 C4 1.39(2) . ?
C3 C4 1.346(19) . ?
C3 C2 1.421(17) . ?
C11 C10 1.373(19) . ?
C12 C13 1.359(17) . ?

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
O9 Mo2 O10 74.7(3) . . ?
O8 Mo2 O9 83.6(3) . . ?
O8 Mo2 O10 76.9(3) . . ?
O8 Mo2 O15 152.0(4) . 2 ?
O6 Mo2 O9 101.3(4) . . ?
O6 Mo2 O8 103.7(4) . . ?
O6 Mo2 O10 175.9(3) . . ?
O6 Mo2 O7 104.9(4) . . ?
O6 Mo2 O15 102.8(4) . 2 ?
O7 Mo2 O9 153.8(4) . . ?
O7 Mo2 O8 91.0(4) . . ?
O7 Mo2 O10 79.1(3) . . ?
O7 Mo2 O15 90.7(4) . 2 ?
O15 Mo2 O9 82.6(4) 2 . ?
O15 Mo2 O10 76.0(3) 2 . ?
O12 Mo3 O10 76.2(2) . . ?
O12 Mo3 O7 84.0(3) . 2 ?
O9 Mo3 O12 89.2(4) . . ?
O9 Mo3 O10 77.7(3) . . ?
O9 Mo3 O7 153.2(4) . 2 ?
O9 Mo3 O14 91.0(4) . . ?
O13 Mo3 O12 103.9(4) . . ?
O13 Mo3 O9 103.9(5) . . ?
O13 Mo3 O10 178.4(4) . . ?
O13 Mo3 O7 102.9(5) . 2 ?
O13 Mo3 O14 102.7(4) . . ?
O7 Mo3 O10 75.5(2) 2 . ?
O14 Mo3 O12 152.5(4) . . ?
O14 Mo3 O10 77.0(2) . . ?
O14 Mo3 O7 83.4(4) . 2 ?
O12 Mo4 O8 87.2(4) . . ?
O12 Mo4 O10 78.1(2) . . ?
O12 Mo4 O15 89.7(4) . . ?
O12 Mo4 O14 154.2(3) . 2 ?
O8 Mo4 O10 75.9(2) . . ?
O8 Mo4 O14 84.5(4) . 2 ?
O11 Mo4 O12 104.5(4) . . ?
O11 Mo4 O8 101.6(4) . . ?
O11 Mo4 O10 176.4(3) . . ?
O11 Mo4 O15 105.5(4) . . ?
O11 Mo4 O14 101.1(4) . 2 ?
O15 Mo4 O8 152.6(4) . . ?
O15 Mo4 O10 76.9(3) . . ?
O15 Mo4 O14 86.7(4) . 2 ?
O14 Mo4 O10 76.2(2) 2 . ?
O4 Mo1 O4 74.6(4) . 2_666 ?
O4 Mo1 O2 94.7(4) . . ?
O4 Mo1 O1 102.7(4) . . ?
O4 Mo1 N1 151.1(4) . . ?
O2 Mo1 O4 78.2(3) . 2_666 ?
O2 Mo1 N1 71.9(4) . . ?
O1 Mo1 O4 82.3(4) . 2_666 ?
O1 Mo1 O2 149.3(4) . . ?
O1 Mo1 N1 81.0(4) . . ?
N1 Mo1 O4 77.5(3) . 2_666 ?
O3 Mo1 O4 107.0(5) . . ?
O3 Mo1 O4 177.0(4) . 2_666 ?
O3 Mo1 O2 99.1(5) . . ?
O3 Mo1 O1 99.7(5) . . ?
O3 Mo1 N1 100.5(5) . . ?
Mo4 O12 Mo3 116.4(4) . . ?
Mo3 O9 Mo2 117.2(5) . . ?
Mo2 O8 Mo4 116.7(4) . . ?
Mo2 O10 Mo2 180.0 . 2 ?
Mo2 O10 Mo3 89.63(5) 2 . ?
Mo2 O10 Mo3 90.37(5) 2 2 ?
Mo2 O10 Mo3 89.63(5) . 2 ?
Mo2 O10 Mo3 90.37(5) . . ?
Mo3 O10 Mo3 180.0 . 2 ?
Mo4 O10 Mo2 90.36(4) . . ?
Mo4 O10 Mo2 90.37(4) 2 2 ?
Mo4 O10 Mo2 89.63(4) 2 . ?
Mo4 O10 Mo2 89.63(4) . 2 ?
Mo4 O10 Mo3 89.20(4) 2 2 ?
Mo4 O10 Mo3 89.20(4) . . ?
Mo4 O10 Mo3 90.80(4) . 2 ?
Mo4 O10 Mo3 90.80(4) 2 . ?
Mo4 O10 Mo4 180.0 . 2 ?
Mo1 O4 Mo1 105.4(4) . 2_666 ?
C8 O2 Mo1 119.3(8) . . ?
C2 O1 Mo1 133.5(8) . . ?
C8 N2 N1 108.6(11) . . ?
N2 N1 Mo1 116.5(8) . . ?
C7 N1 Mo1 127.8(9) . . ?
C7 N1 N2 115.7(11) . . ?
C7 C1 C6 119.8(13) . . ?
C7 C1 C2 122.3(11) . . ?
C2 C1 C6 117.8(12) . . ?
N1 C7 C1 125.1(13) . . ?
O2 C8 C9 117.8(12) . . ?
N2 C8 O2 123.6(13) . . ?
N2 C8 C9 118.6(13) . . ?
C10 C9 C8 121.2(13) . . ?
C13 C9 C8 119.4(12) . . ?
C13 C9 C10 119.3(13) . . ?
C12 N3 C11 122.8(12) . . ?
C3 O5 C14 116.8(11) . . ?
C6 C5 C4 121.1(13) . . ?
O5 C3 C2 114.0(12) . . ?
C4 C3 O5 127.0(13) . . ?
C4 C3 C2 119.0(14) . . ?
N3 C11 C10 119.0(14) . . ?
N3 C12 C13 121.2(13) . . ?
C11 C10 C9 119.2(14) . . ?
C5 C6 C1 119.9(14) . . ?
C3 C4 C5 121.5(14) . . ?
O1 C2 C1 120.4(11) . . ?
O1 C2 C3 118.8(11) . . ?
C1 C2 C3 120.6(12) . . ?
C12 C13 C9 118.4(13) . . ?
Mo2 O7 Mo3 115.8(4) . 2 ?
Mo4 O15 Mo2 116.9(5) . 2 ?
Mo3 O14 Mo4 115.5(4) . 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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.864
_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 0.5543 2255 10582 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.4457 2252 10582 nmt -0.9987 -0.0006 0.0006 -0.0005 0.9984 -0.0004 -0.0012
-0.9150 -0.9988

_twin_special_details            
;
Component 2 rotated by 179.9636° 
around [0.00 0.91 -0.42] (reciprocal) or [-0.00 1.00 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_exp_653
_database_code_depnum_ccdc_archive 'CCDC 2091115'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_exp_653             
;
PROBLEM: D-H Bond Without Acceptor  O21      --H21B     .     Please Check
RESPONSE: Due to presence of high-Z atoms, no hydrogen atoms could be unambiguously located in the difference Fourier map. Thus, hydrogen atoms on water molecules were placed and refined using riding model according to their environment. In case of disordered water molecule O21/O21A one of the hydrogen atoms was placed a bit further away from nearest acceptor.
;
# Added during the CSD deposition process: Thursday 15 July 2021 10:16 AM
# end Validation Reply Form

_audit_creation_date             2021-07-15
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'[N-(2-oxo-4-methoxybenzylidene)isonicotinoylhydrazonato](aqua)dioxomolybdenum(vi) octamolybdate acetonitrile solvate hydrate'
_chemical_formula_moiety         
'Mo8 O26, 2(C14 H15 Mo N3 O6), 4(H2 O), 1.5(C4 H6 N2)'
_chemical_formula_sum            'C34 H47 Mo10 N9 O42'
_chemical_formula_weight         2213.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.2611(2)
_cell_length_b                   10.5249(2)
_cell_length_c                   15.9967(2)
_cell_angle_alpha                100.3730(10)
_cell_angle_beta                 104.041(2)
_cell_angle_gamma                106.410(2)
_cell_volume                     1549.28(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    28564
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.6620
_cell_measurement_theta_min      4.5340
_shelx_estimated_absorpt_T_max   0.343
_shelx_estimated_absorpt_T_min   0.256
_exptl_absorpt_coefficient_mu    17.002
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44714
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.744
_diffrn_reflns_theta_min         4.545
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     91.00 130.00   0.50    0.25    --  113.25  77.00 120.00   78
  2  ω    133.00 178.00   0.50    0.25    --  113.25  77.00 120.00   90
  3  ω     93.00 172.00   0.50    0.25    --  113.25  77.00 150.00  158
  4  ω    100.00 175.00   0.50    0.25    --  113.25  77.00  60.00  150
  5  ω     94.00 155.00   0.50    0.25    --  113.25  77.00  30.00  122
  6  ω    148.00 178.00   0.50    0.25    --  113.25  77.00 -90.00   60
  7  ω    136.00 177.00   0.50    0.25    --  113.25  77.00-120.00   82
  8  ω     91.00 136.00   0.50    0.25    --  113.25  77.00-180.00   90
  9  ω     91.00 130.00   0.50    0.25    --  113.25  77.00-120.00   78
 10  ω     94.00 139.00   0.50    0.25    --  113.25  77.00 -90.00   90
 11  ω    104.00 175.00   0.50    0.25    --  113.25  77.00-150.00  142
 12  ω    100.00 135.00   0.50    0.25    --  113.25  61.00 -30.00   70
 13  ω     91.00 173.00   0.50    0.25    --  113.25  77.00  90.00  164
 14  ω     94.00 169.00   0.50    0.25    --  113.25  77.00 -30.00  150
 15  ω    102.00 149.00   0.50    0.25    --  113.25  61.00  90.00   94
 16  ω     91.00 156.00   0.50    0.25    --  113.25  77.00 -60.00  130
 17  ω    115.00 177.00   0.50    0.25    --  113.25  61.00 -60.00  124
 18  ω    100.00 162.00   0.50    0.25    --  113.25  61.00 -90.00  124
 19  ω     98.00 171.00   0.50    0.25    --  113.25  61.00-120.00  146
 20  ω     99.00 176.00   0.50    0.25    --  113.25  61.00-180.00  154
 21  ω     97.00 150.00   0.50    0.25    --  113.25  61.00-150.00  106
 22  ω    108.00 155.00   0.50    0.25    --  113.25  61.00   0.00   94
 23  ω    127.00 167.00   0.50    0.25    --  113.25  30.00  30.00   80
 24  ω    100.00 156.00   0.50    0.25    --  113.25  61.00  60.00  112
 25  ω    107.00 176.00   0.50    0.25    --  113.25  51.00 131.00  138
 26  ω     99.00 125.00   0.50    0.25    --  113.25  61.00 150.00   52
 27  ω     34.00  67.00   0.50    0.06    --   48.02  51.00 131.00   66
 28  ω   -120.00 -79.00   0.50    0.06    --  -48.02 -77.00  30.00   82
 29  ω    -57.00 -25.00   0.50    0.06    --  -48.02 -77.00 -90.00   64
 30  ω    -54.00 -25.00   0.50    0.06    --  -48.02 -77.00 -30.00   58
 31  ω    -56.00 -25.00   0.50    0.06    --  -48.02 -77.00-150.00   62
 32  ω    -95.00 -25.00   0.50    0.06    --  -48.02 -77.00-180.00  140
 33  ω   -113.00 -87.00   0.50    0.06    --  -48.02 -77.00-150.00   52
 34  ω   -108.00 -82.00   0.50    0.06    --  -48.02 -77.00 -90.00   52
 35  ω    -61.00 -33.00   0.50    0.06    --  -48.02 -57.00 -60.00   56
 36  ω    -64.00 -26.00   0.50    0.06    --  -48.02 -77.00  30.00   76
 37  ω    -53.00 -25.00   0.50    0.06    --  -48.02 -77.00  90.00   56
 38  ω    -56.00 -25.00   0.50    0.06    --  -48.02 -77.00 120.00   62
 39  ω    -89.00 -63.00   0.50    0.06    --  -48.02 -77.00 120.00   52
 40  ω    -80.00 -34.00   0.50    0.06    --  -48.02 -51.00 -14.00   92
 41  ω    -92.00 -36.00   0.50    0.06    --  -48.02 -38.00  30.00  112
 42  ω   -119.00 -37.00   0.50    0.06    --  -48.02 -38.00  90.00  164
 43  ω   -119.00 -93.00   0.50    0.06    --  -48.02 -51.00 -14.00   52
 44  ω   -118.00 -68.00   0.50    0.06    --  -48.02 -57.00 -60.00  100
 45  ω    -64.00 -37.00   0.50    0.06    --  -48.02 -38.00-120.00   54
 46  ω    -60.00 -35.00   0.50    0.06    --  -48.02 -57.00-150.00   50
 47  ω   -121.00 -75.00   0.50    0.06    --  -48.02 -19.00-180.00   92
 48  ω    -71.00 -44.00   0.50    0.06    --  -48.02 -19.00-180.00   54
 49  ω    -57.00 -19.00   0.50    0.25    --  -91.75  61.00 -60.00   76
 50  ω    -44.00  23.00   0.50    0.06    --  -48.02  51.00 131.00  134
 51  ω    -52.00 -27.00   0.50    0.25    --  -91.75  51.00 131.00   50
 52  ω    -95.00 -69.00   0.50    0.25    --  -91.75 -77.00  60.00   52
 53  ω   -139.00-113.00   0.50    0.25    --  -91.75 -77.00 -60.00   52
 54  ω   -105.00 -70.00   0.50    0.25    --  -91.75 -77.00 -30.00   70
 55  ω    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00 -60.00   50
 56  ω    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00 -90.00   50
 57  ω    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00-120.00   50
 58  ω   -122.00 -69.00   0.50    0.25    --  -91.75 -77.00-180.00  106
 59  ω   -163.00-129.00   0.50    0.25    --  -91.75 -77.00-180.00   68
 60  ω   -154.00-128.00   0.50    0.25    --  -91.75 -77.00   0.00   52
 61  ω    -97.00 -71.00   0.50    0.25    --  -91.75 -77.00  30.00   52
 62  ω    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00   0.00   50
 63  ω    -95.00 -69.00   0.50    0.25    --  -91.75 -77.00  94.40   52
 64  ω    -95.00 -69.00   0.50    0.25    --  -91.75 -77.00 150.00   52
 65  ω   -103.00 -69.00   0.50    0.25    --  -91.75 -76.00 123.13   68
 66  ω   -147.00-121.00   0.50    0.25    --  -91.75 -76.00 123.13   52
 67  ω   -107.00 -69.00   0.50    0.25    --  -91.75 -76.00  50.46   76
 68  ω   -100.00 -70.00   0.50    0.25    --  -91.75 -75.00 132.77   60
 69  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -75.00  33.55   50
 70  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00  10.45   50
 71  ω   -103.00 -70.00   0.50    0.25    --  -91.75 -75.00 -17.78   66
 72  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00-108.94   50
 73  ω    -96.00 -70.00   0.50    0.25    --  -91.75 -75.00-142.63   52
 74  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00-174.72   50
 75  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00-160.09   50
 76  ω    -96.00 -70.00   0.50    0.25    --  -91.75 -74.00 -73.47   52
 77  ω   -107.00 -71.00   0.50    0.25    --  -91.75 -71.00 -52.45   72
 78  ω    -99.00 -74.00   0.50    0.25    --  -91.75 -63.00-148.79   50
 79  ω   -154.00-128.00   0.50    0.25    --  -91.75 -74.00-108.94   52
 80  ω   -145.00-120.00   0.50    0.25    --  -91.75 -51.00 -14.00   50
 81  ω    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00  73.92   50
 82  ω    -98.00 -71.00   0.50    0.25    --  -91.75 -71.00 101.08   54
 83  ω    -99.00 -74.00   0.50    0.25    --  -91.75 -68.00 158.24   50
 84  ω    104.00 165.00   0.50    0.25    --  113.25 125.00   0.00  122
 85  ω    123.00 148.00   0.50    0.25    --  113.25 125.00 -30.00   50
 86  ω     43.00  68.00   0.50    0.25    --  113.25 -61.00  90.00   50
 87  ω     42.00  69.00   0.50    0.25    --  113.25 -61.00  30.00   54
 88  ω     47.00  89.00   0.50    0.25    --  113.25 -77.00 -60.00   84
 89  ω     43.00  96.00   0.50    0.25    --  113.25 -77.00 -90.00  106
 90  ω    -23.00  53.00   0.50    0.06    --   48.02 -51.00 -14.00  152
 91  ω     43.00  97.00   0.50    0.25    --  113.25 -95.00  90.00  108
 92  ω     71.00 117.00   0.50    0.25    --  113.25-132.00 172.24   92
 93  ω     85.00 111.00   0.50    0.25    --  113.25-125.00  90.00   52
 94  ω     42.00  81.00   0.50    0.25    --  113.25-125.00  90.00   78
 95  ω     76.00 111.00   0.50    0.25    --  113.25-125.00   0.00   70
 96  ω     45.00  71.00   0.50    0.25    --  113.25-125.00   0.00   52
 97  ω     43.00 111.00   0.50    0.25    --  113.25-125.00 -90.00  136
 98  ω     43.00 111.00   0.50    0.25    --  113.25-125.00-120.00  136
 99  ω     44.00 107.00   0.50    0.25    --  113.25-125.00-150.00  126
100  ω     36.00  78.00   0.50    0.06    --   48.02-125.00-150.00   84
101  ω     46.00 111.00   0.50    0.25    --  113.25-125.00 -60.00  130
102  ω     78.00 108.00   0.50    0.25    --  113.25-112.00  43.18   60
103  ω     47.00 102.00   0.50    0.25    --  113.25-125.00  30.00  110
104  ω     45.00  75.00   0.50    0.25    --  113.25-112.00  43.18   60
105  ω     81.00 106.00   0.50    0.25    --  113.25-102.00  36.80   50
106  ω     86.00 111.00   0.50    0.25    --  113.25-125.00 120.00   50
107  ω     44.00  69.00   0.50    0.25    --  113.25-125.00 120.00   50
108  ω     64.00  90.00   0.50    0.25    --  113.25 -95.00 150.00   52
109  ω     51.00  76.00   0.50    0.25    --  113.25-102.00  36.80   50
110  ω      6.00  82.00   0.50    0.06    --   48.02 -99.00-180.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6244
_reflns_number_total             6624
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_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         1.398
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.00072(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6624
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      1.086
_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)+(0.0473P)²+5.7164P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0944
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H3-N3
 0.86 with sigma of 0.02
 N4-C15
 1.14 with sigma of 0.02
 C16-N4
 2.593 with sigma of 0.02
 C15-N4
 1.137 with sigma of 0.01
 C15-C16
 1.456 with sigma of 0.01
 N4-C16
 2.59 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N4 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C17) = Uanis(C18A)
Uanis(C15) = Uanis(C16)
Uanis(C17) = Uanis(C18)
Uanis(N5) = Uanis(C17)
4. Rigid body (RIGU) restrains
 N4, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C15(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C18A(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) C18(0.5) H18D(0.5) H18E(0.5) H18F(0.5) O21(0.5)
 H21A(0.5) H21B(0.5) O21A(0.5) H21C(0.5) H21D(0.5)
6.a Free rotating group:
 O20(H20A,H20B), O21(H21A,H21B), O21A(H21C,H21D)
6.b Rotating group:
 O5(H5A,H5B)
6.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C13(H13), C10(H10), C7(H7), C11(H11), C6(H6), C12(H12), C3(H3A), C5(H5)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18A(H18A,H18B,H18C), C18(H18D,H18E,
 H18F)
;
_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
Mo3 Mo 0.49559(3) 0.89956(3) 0.39677(2) 0.01448(9) Uani 1 1 d . . . . .
Mo2 Mo 0.80419(3) 1.07158(3) 0.54314(2) 0.01556(9) Uani 1 1 d . . . . .
Mo4 Mo 0.39513(3) 0.74213(3) 0.53544(2) 0.01817(10) Uani 1 1 d . . . . .
Mo5 Mo 0.70569(3) 0.91165(3) 0.68670(2) 0.01876(10) Uani 1 1 d . . . . .
Mo1 Mo 0.66523(4) 0.44000(4) 0.17980(3) 0.02862(11) Uani 1 1 d . . . . .
O12 O 0.6651(3) 1.0633(3) 0.42886(18) 0.0159(5) Uani 1 1 d . . . . .
O14 O 0.5061(3) 0.7980(3) 0.6589(2) 0.0218(6) Uani 1 1 d . . . . .
O11 O 0.5780(3) 0.9260(3) 0.53804(18) 0.0146(5) Uani 1 1 d . . . . .
O15 O 0.8339(3) 1.0641(3) 0.66369(19) 0.0205(6) Uani 1 1 d . . . . .
O13 O 0.3269(3) 0.7941(3) 0.42285(18) 0.0157(5) Uani 1 1 d . . . . .
O17 O 0.4020(3) 0.9285(3) 0.29893(19) 0.0188(6) Uani 1 1 d . . . . .
O7 O 0.8501(3) 0.9353(3) 0.5008(2) 0.0225(6) Uani 1 1 d . . . . .
O8 O 0.5595(3) 0.7751(3) 0.3621(2) 0.0233(6) Uani 1 1 d . . . . .
O16 O 0.9444(3) 1.2138(3) 0.5542(2) 0.0247(6) Uani 1 1 d . . . . .
O9 O 0.4628(4) 0.6249(3) 0.4933(2) 0.0286(7) Uani 1 1 d . . . . .
O5 O 0.5331(4) 0.4395(4) 0.2826(2) 0.0334(8) Uani 1 1 d . . . . .
H5A H 0.509512 0.357390 0.296320 0.050 Uiso 1 1 d R U . . .
H5B H 0.587282 0.499479 0.336748 0.050 Uiso 1 1 d R U . . .
O2 O 0.7230(3) 0.6429(3) 0.2352(2) 0.0301(7) Uani 1 1 d . . . . .
O10 O 0.7636(3) 0.7856(3) 0.6425(2) 0.0281(7) Uani 1 1 d . . . . .
O18 O 0.2344(3) 0.6467(3) 0.5424(2) 0.0289(7) Uani 1 1 d . . . . .
O1 O 0.5199(4) 0.2613(4) 0.1224(2) 0.0365(8) Uani 1 1 d . . . . .
O19 O 0.7699(4) 0.9407(4) 0.7987(2) 0.0309(7) Uani 1 1 d . . . . .
O4 O 0.7756(4) 0.4031(4) 0.2634(3) 0.0430(10) Uani 1 1 d . . . . .
O20 O 0.7410(5) 0.6384(4) 0.4562(3) 0.0457(10) Uani 1 1 d G . . . .
H20A H 0.685935 0.642378 0.489498 0.069 Uiso 1 1 d G U . . .
H20B H 0.793116 0.723639 0.465009 0.069 Uiso 1 1 d G U . . .
O3 O 0.7485(4) 0.4539(4) 0.1012(3) 0.0432(9) Uani 1 1 d . . . . .
N1 N 0.4898(4) 0.5099(4) 0.1159(2) 0.0254(8) Uani 1 1 d . . . . .
N3 N 0.8156(4) 1.1410(4) 0.2923(3) 0.0296(8) Uani 1 1 d D . . . .
N2 N 0.5214(4) 0.6524(4) 0.1383(2) 0.0240(7) Uani 1 1 d . . . . .
H2 H 0.466207 0.695508 0.114472 0.029 Uiso 1 1 calc R U . . .
C13 C 0.6273(5) 0.9423(5) 0.1992(3) 0.0256(9) Uani 1 1 d . . . . .
H13 H 0.535803 0.900492 0.155403 0.031 Uiso 1 1 calc R U . . .
O6 O 0.1556(5) -0.1345(4) -0.0708(3) 0.0618(13) Uani 1 1 d . . . . .
C8 C 0.6438(5) 0.7107(5) 0.1991(3) 0.0238(9) Uani 1 1 d . . . . .
C10 C 0.8377(5) 0.9262(5) 0.2955(3) 0.0288(9) Uani 1 1 d . . . . .
H10 H 0.891043 0.872998 0.318950 0.035 Uiso 1 1 calc R U . . .
C9 C 0.7035(5) 0.8618(5) 0.2314(3) 0.0240(9) Uani 1 1 d . . . . .
C1 C 0.3128(5) 0.2918(5) 0.0299(3) 0.0265(9) Uani 1 1 d . . . . .
C7 C 0.3638(5) 0.4376(5) 0.0606(3) 0.0258(9) Uani 1 1 d . . . . .
H7 H 0.301798 0.484828 0.039331 0.031 Uiso 1 1 calc R U . . .
C11 C 0.8920(5) 1.0670(5) 0.3245(3) 0.0329(10) Uani 1 1 d . . . . .
H11 H 0.983944 1.111766 0.367506 0.040 Uiso 1 1 calc R U . . .
C6 C 0.1764(5) 0.2253(6) -0.0340(3) 0.0339(11) Uani 1 1 d . . . . .
H6 H 0.121589 0.279305 -0.054099 0.041 Uiso 1 1 calc R U . . .
C12 C 0.6855(5) 1.0831(5) 0.2314(3) 0.0309(10) Uani 1 1 d . . . . .
H12 H 0.633771 1.139077 0.210454 0.037 Uiso 1 1 calc R U . . .
C2 C 0.3915(5) 0.2093(5) 0.0591(3) 0.0293(10) Uani 1 1 d . . . . .
C3 C 0.3365(6) 0.0672(5) 0.0237(4) 0.0383(12) Uani 1 1 d . . . . .
H3A H 0.391498 0.012459 0.042268 0.046 Uiso 1 1 calc R U . . .
C5 C 0.1199(6) 0.0841(6) -0.0682(4) 0.0394(12) Uani 1 1 d . . . . .
H5 H 0.027401 0.041760 -0.110913 0.047 Uiso 1 1 calc R U . . .
C4 C 0.2006(6) 0.0050(5) -0.0392(4) 0.0370(11) Uani 1 1 d . . . . .
C14 C 0.0185(9) -0.2131(8) -0.1310(6) 0.070(2) Uani 1 1 d . . . . .
H14A H 0.002598 -0.178230 -0.184042 0.106 Uiso 1 1 calc R U . . .
H14B H -0.053928 -0.206151 -0.101917 0.106 Uiso 1 1 calc R U . . .
H14C H 0.011693 -0.309406 -0.148765 0.106 Uiso 1 1 calc R U . . .
H3 H 0.846(5) 1.229(2) 0.306(3) 0.022(13) Uiso 1 1 d D . . . .
N4 N 0.000000 0.500000 0.000000 0.074(3) Uani 1 2 d DS U P A 1
C15 C 0.0877(11) 0.6020(9) 0.0470(9) 0.056(2) Uani 0.5 1 d D U P A 1
C16 C 0.2079(12) 0.7305(10) 0.0930(10) 0.056(2) Uani 0.5 1 d D U P A 1
H16A H 0.220230 0.787492 0.051379 0.083 Uiso 0.5 1 calc R U P A 1
H16B H 0.295407 0.709609 0.114408 0.083 Uiso 0.5 1 calc R U P A 1
H16C H 0.188537 0.780170 0.143869 0.083 Uiso 0.5 1 calc R U P A 1
N5 N 0.2844(7) 0.5030(8) 0.2497(5) 0.0748(15) Uani 1 1 d . . . . .
C17 C 0.1985(9) 0.5517(10) 0.2423(6) 0.0748(15) Uani 1 1 d . . . . .
C18A C 0.0977(17) 0.6437(19) 0.2110(12) 0.0748(15) Uani 0.5 1 d . . P B 2
H18A H 0.136875 0.697196 0.173036 0.112 Uiso 0.5 1 calc R U P B 2
H18B H 0.096689 0.706260 0.264023 0.112 Uiso 0.5 1 calc R U P B 2
H18C H 0.000014 0.582090 0.177379 0.112 Uiso 0.5 1 calc R U P B 2
C18 C 0.0819(17) 0.5742(19) 0.2633(12) 0.0748(15) Uani 0.5 1 d . . P B 1
H18D H -0.005345 0.497150 0.227635 0.112 Uiso 0.5 1 calc R U P B 1
H18E H 0.073590 0.659524 0.250144 0.112 Uiso 0.5 1 calc R U P B 1
H18F H 0.095147 0.581901 0.327031 0.112 Uiso 0.5 1 calc R U P B 1
O21 O 1.0159(8) 1.3955(10) 0.4240(7) 0.0320(18) Uani 0.5 1 d G . P C 1
H21A H 0.948594 1.408334 0.444973 0.048 Uiso 0.5 1 d G U P C 1
H21B H 1.031646 1.456143 0.393834 0.048 Uiso 0.5 1 d G U P C 1
O21A O 1.0502(12) 1.3807(9) 0.3840(8) 0.048(2) Uani 0.5 1 d G . P D 2
H21C H 1.132955 1.387163 0.376810 0.072 Uiso 0.5 1 d G U P D 2
H21D H 1.068077 1.405244 0.441717 0.072 Uiso 0.5 1 d G U P D 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
Mo3 Mo4 3.1933(4) . ?
Mo3 O12 1.953(3) . ?
Mo3 O11 2.346(3) 2_676 ?
Mo3 O11 2.148(3) . ?
Mo3 O13 1.958(3) . ?
Mo3 O17 1.753(3) . ?
Mo3 O8 1.689(3) . ?
Mo2 O12 1.998(3) . ?
Mo2 O11 2.365(3) . ?
Mo2 O15 1.898(3) . ?
Mo2 O13 2.293(3) 2_676 ?
Mo2 O7 1.710(3) . ?
Mo2 O16 1.705(3) . ?
Mo4 O12 2.317(3) 2_676 ?
Mo4 O14 1.911(3) . ?
Mo4 O11 2.269(3) . ?
Mo4 O13 1.998(3) . ?
Mo4 O9 1.695(3) . ?
Mo4 O18 1.713(3) . ?
Mo5 O14 1.951(3) . ?
Mo5 O11 2.475(3) . ?
Mo5 O15 1.922(3) . ?
Mo5 O17 2.267(3) 2_676 ?
Mo5 O10 1.710(3) . ?
Mo5 O19 1.690(3) . ?
Mo1 O5 2.371(4) . ?
Mo1 O2 2.011(3) . ?
Mo1 O1 1.932(3) . ?
Mo1 O4 1.710(3) . ?
Mo1 O3 1.688(4) . ?
Mo1 N1 2.225(4) . ?
O5 H5A 0.9107 . ?
O5 H5B 0.9108 . ?
O2 C8 1.323(5) . ?
O1 C2 1.344(6) . ?
O20 H20A 0.8700 . ?
O20 H20B 0.8699 . ?
N1 N2 1.400(5) . ?
N1 C7 1.296(6) . ?
N3 C11 1.335(7) . ?
N3 C12 1.341(6) . ?
N3 H3 0.861(19) . ?
N2 H2 0.8800 . ?
N2 C8 1.287(6) . ?
C13 H13 0.9500 . ?
C13 C9 1.389(6) . ?
C13 C12 1.376(7) . ?
O6 C4 1.364(7) . ?
O6 C14 1.410(9) . ?
C8 C9 1.474(6) . ?
C10 H10 0.9500 . ?
C10 C9 1.395(6) . ?
C10 C11 1.372(7) . ?
C1 C7 1.421(7) . ?
C1 C6 1.410(7) . ?
C1 C2 1.409(7) . ?
C7 H7 0.9500 . ?
C11 H11 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.382(8) . ?
C12 H12 0.9500 . ?
C2 C3 1.392(7) . ?
C3 H3A 0.9500 . ?
C3 C4 1.397(8) . ?
C5 H5 0.9500 . ?
C5 C4 1.392(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N4 C15 1.167(7) 2_565 ?
N4 C15 1.167(7) . ?
C15 C16 1.466(8) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N5 C17 1.131(11) . ?
C17 C18A 1.66(2) . ?
C17 C18 1.388(18) . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C18 H18D 0.9800 . ?
C18 H18E 0.9800 . ?
C18 H18F 0.9800 . ?
O21 H21A 0.8698 . ?
O21 H21B 0.8701 . ?
O21A H21C 0.8701 . ?
O21A H21D 0.8700 . ?

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
O12 Mo3 Mo4 124.55(8) . . ?
O12 Mo3 O11 79.33(11) . . ?
O12 Mo3 O11 77.26(10) . 2_676 ?
O12 Mo3 O13 149.93(12) . . ?
O11 Mo3 Mo4 45.23(7) . . ?
O11 Mo3 Mo4 86.36(6) 2_676 . ?
O11 Mo3 O11 75.63(11) . 2_676 ?
O13 Mo3 Mo4 36.61(8) . . ?
O13 Mo3 O11 78.12(11) . . ?
O13 Mo3 O11 78.06(10) . 2_676 ?
O17 Mo3 Mo4 132.89(10) . . ?
O17 Mo3 O12 96.63(13) . . ?
O17 Mo3 O11 156.77(12) . . ?
O17 Mo3 O11 81.16(11) . 2_676 ?
O17 Mo3 O13 96.28(13) . . ?
O8 Mo3 Mo4 89.39(11) . . ?
O8 Mo3 O12 101.02(13) . . ?
O8 Mo3 O11 97.70(13) . . ?
O8 Mo3 O11 173.29(12) . 2_676 ?
O8 Mo3 O13 101.49(13) . . ?
O8 Mo3 O17 105.52(14) . . ?
O12 Mo2 O11 73.32(10) . . ?
O12 Mo2 O13 72.17(10) . 2_676 ?
O15 Mo2 O12 146.74(12) . . ?
O15 Mo2 O11 77.66(11) . . ?
O15 Mo2 O13 83.63(11) . 2_676 ?
O13 Mo2 O11 71.66(10) 2_676 . ?
O7 Mo2 O12 96.44(13) . . ?
O7 Mo2 O11 92.22(12) . . ?
O7 Mo2 O15 100.61(14) . . ?
O7 Mo2 O13 162.21(12) . 2_676 ?
O16 Mo2 O12 101.42(13) . . ?
O16 Mo2 O11 162.43(13) . . ?
O16 Mo2 O15 101.37(14) . . ?
O16 Mo2 O13 90.78(13) . 2_676 ?
O16 Mo2 O7 105.12(15) . . ?
O12 Mo4 Mo3 79.45(7) 2_676 . ?
O14 Mo4 Mo3 121.30(9) . . ?
O14 Mo4 O12 84.54(11) . 2_676 ?
O14 Mo4 O11 79.10(11) . . ?
O14 Mo4 O13 148.67(12) . . ?
O11 Mo4 Mo3 42.22(7) . . ?
O11 Mo4 O12 72.16(10) . 2_676 ?
O13 Mo4 Mo3 35.76(8) . . ?
O13 Mo4 O12 71.61(10) . 2_676 ?
O13 Mo4 O11 74.49(10) . . ?
O9 Mo4 Mo3 85.20(11) . . ?
O9 Mo4 O12 164.36(13) . 2_676 ?
O9 Mo4 O14 101.06(15) . . ?
O9 Mo4 O11 94.40(13) . . ?
O9 Mo4 O13 97.51(14) . . ?
O9 Mo4 O18 104.85(17) . . ?
O18 Mo4 Mo3 135.44(11) . . ?
O18 Mo4 O12 88.38(13) . 2_676 ?
O18 Mo4 O14 99.61(15) . . ?
O18 Mo4 O11 160.54(14) . . ?
O18 Mo4 O13 99.73(14) . . ?
O14 Mo5 O11 73.35(11) . . ?
O14 Mo5 O17 77.90(12) . 2_676 ?
O15 Mo5 O14 144.89(12) . . ?
O15 Mo5 O11 74.50(10) . . ?
O15 Mo5 O17 77.93(12) . 2_676 ?
O17 Mo5 O11 69.39(10) 2_676 . ?
O10 Mo5 O14 97.37(15) . . ?
O10 Mo5 O11 93.33(13) . . ?
O10 Mo5 O15 98.19(15) . . ?
O10 Mo5 O17 162.71(13) . 2_676 ?
O19 Mo5 O14 103.01(15) . . ?
O19 Mo5 O11 161.36(14) . . ?
O19 Mo5 O15 102.90(15) . . ?
O19 Mo5 O17 91.98(14) . 2_676 ?
O19 Mo5 O10 105.30(17) . . ?
O2 Mo1 O5 79.31(13) . . ?
O2 Mo1 N1 72.18(13) . . ?
O1 Mo1 O5 81.86(15) . . ?
O1 Mo1 O2 150.84(15) . . ?
O1 Mo1 N1 82.01(14) . . ?
O4 Mo1 O5 81.17(18) . . ?
O4 Mo1 O2 98.01(16) . . ?
O4 Mo1 O1 100.88(16) . . ?
O4 Mo1 N1 157.24(19) . . ?
O3 Mo1 O5 172.51(15) . . ?
O3 Mo1 O2 96.42(18) . . ?
O3 Mo1 O1 99.6(2) . . ?
O3 Mo1 O4 105.6(2) . . ?
O3 Mo1 N1 95.99(16) . . ?
N1 Mo1 O5 76.89(13) . . ?
Mo3 O12 Mo2 109.61(12) . . ?
Mo3 O12 Mo4 109.49(12) . 2_676 ?
Mo2 O12 Mo4 103.44(12) . 2_676 ?
Mo4 O14 Mo5 115.64(15) . . ?
Mo3 O11 Mo3 104.38(11) . 2_676 ?
Mo3 O11 Mo2 91.22(10) . . ?
Mo3 O11 Mo2 96.40(9) 2_676 . ?
Mo3 O11 Mo4 92.56(10) . . ?
Mo3 O11 Mo5 164.00(13) . . ?
Mo3 O11 Mo5 91.50(9) 2_676 . ?
Mo2 O11 Mo5 84.94(9) . . ?
Mo4 O11 Mo3 98.37(10) . 2_676 ?
Mo4 O11 Mo2 163.33(13) . . ?
Mo4 O11 Mo5 86.99(9) . . ?
Mo2 O15 Mo5 117.69(14) . . ?
Mo3 O13 Mo2 111.19(12) . 2_676 ?
Mo3 O13 Mo4 107.62(12) . . ?
Mo4 O13 Mo2 104.31(12) . 2_676 ?
Mo3 O17 Mo5 117.93(14) . 2_676 ?
Mo1 O5 H5A 111.4 . . ?
Mo1 O5 H5B 111.4 . . ?
H5A O5 H5B 102.5 . . ?
C8 O2 Mo1 118.4(3) . . ?
C2 O1 Mo1 137.1(3) . . ?
H20A O20 H20B 104.5 . . ?
N2 N1 Mo1 115.0(3) . . ?
C7 N1 Mo1 129.2(3) . . ?
C7 N1 N2 115.8(4) . . ?
C11 N3 C12 122.5(4) . . ?
C11 N3 H3 124(4) . . ?
C12 N3 H3 113(4) . . ?
N1 N2 H2 125.3 . . ?
C8 N2 N1 109.4(4) . . ?
C8 N2 H2 125.3 . . ?
C9 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C9 119.4(4) . . ?
C4 O6 C14 123.1(6) . . ?
O2 C8 C9 116.4(4) . . ?
N2 C8 O2 123.9(4) . . ?
N2 C8 C9 119.6(4) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C11 C10 C9 119.4(4) . . ?
C13 C9 C8 120.9(4) . . ?
C13 C9 C10 119.0(4) . . ?
C10 C9 C8 120.1(4) . . ?
C6 C1 C7 118.5(4) . . ?
C2 C1 C7 123.7(4) . . ?
C2 C1 C6 117.8(5) . . ?
N1 C7 C1 123.9(4) . . ?
N1 C7 H7 118.0 . . ?
C1 C7 H7 118.0 . . ?
N3 C11 C10 120.0(4) . . ?
N3 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C1 C6 H6 118.9 . . ?
C5 C6 C1 122.2(5) . . ?
C5 C6 H6 118.9 . . ?
N3 C12 C13 119.7(4) . . ?
N3 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
O1 C2 C1 122.7(4) . . ?
O1 C2 C3 116.8(5) . . ?
C3 C2 C1 120.4(5) . . ?
C2 C3 H3A 119.9 . . ?
C2 C3 C4 120.1(5) . . ?
C4 C3 H3A 119.9 . . ?
C6 C5 H5 120.5 . . ?
C6 C5 C4 118.9(5) . . ?
C4 C5 H5 120.5 . . ?
O6 C4 C3 116.2(5) . . ?
O6 C4 C5 123.3(5) . . ?
C5 C4 C3 120.6(5) . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 N4 C15 180.0 . 2_565 ?
N4 C15 C16 170.1(16) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C17 C18A 162.5(12) . . ?
N5 C17 C18 151.5(15) . . ?
C17 C18A H18A 109.5 . . ?
C17 C18A H18B 109.5 . . ?
C17 C18A H18C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C17 C18 H18D 109.5 . . ?
C17 C18 H18E 109.5 . . ?
C17 C18 H18F 109.5 . . ?
H18D C18 H18E 109.5 . . ?
H18D C18 H18F 109.5 . . ?
H18E C18 H18F 109.5 . . ?
H21A O21 H21B 104.5 . . ?
H21C O21A H21D 104.5 . . ?

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
Mo4 Mo3 O17 Mo5 75.30(18) . . . 2_676 ?
Mo1 O2 C8 N2 9.8(6) . . . . ?
Mo1 O2 C8 C9 -169.5(3) . . . . ?
Mo1 O1 C2 C1 -15.2(8) . . . . ?
Mo1 O1 C2 C3 165.8(4) . . . . ?
Mo1 N1 N2 C8 -6.2(4) . . . . ?
Mo1 N1 C7 C1 0.4(7) . . . . ?
O12 Mo3 O17 Mo5 -77.23(16) . . . 2_676 ?
O12 Mo2 O15 Mo5 50.8(3) . . . . ?
O11 Mo3 O17 Mo5 1.1(4) . . . 2_676 ?
O11 Mo3 O17 Mo5 -1.27(13) 2_676 . . 2_676 ?
O11 Mo2 O15 Mo5 21.19(15) . . . . ?
O13 Mo3 O17 Mo5 75.56(16) . . . 2_676 ?
O13 Mo2 O15 Mo5 93.75(16) 2_676 . . . ?
O7 Mo2 O15 Mo5 -68.77(19) . . . . ?
O8 Mo3 O17 Mo5 179.36(15) . . . 2_676 ?
O16 Mo2 O15 Mo5 -176.74(17) . . . . ?
O2 C8 C9 C13 -178.5(4) . . . . ?
O2 C8 C9 C10 1.0(6) . . . . ?
O1 C2 C3 C4 176.9(5) . . . . ?
N1 N2 C8 O2 -1.7(6) . . . . ?
N1 N2 C8 C9 177.6(4) . . . . ?
N2 N1 C7 C1 179.7(4) . . . . ?
N2 C8 C9 C13 2.2(7) . . . . ?
N2 C8 C9 C10 -178.3(4) . . . . ?
C9 C13 C12 N3 0.9(7) . . . . ?
C9 C10 C11 N3 1.0(7) . . . . ?
C1 C6 C5 C4 -0.5(8) . . . . ?
C1 C2 C3 C4 -2.0(8) . . . . ?
C7 N1 N2 C8 174.4(4) . . . . ?
C7 C1 C6 C5 179.0(5) . . . . ?
C7 C1 C2 O1 3.3(7) . . . . ?
C7 C1 C2 C3 -177.8(5) . . . . ?
C11 N3 C12 C13 -0.7(7) . . . . ?
C11 C10 C9 C13 -0.8(7) . . . . ?
C11 C10 C9 C8 179.7(4) . . . . ?
C6 C1 C7 N1 -176.7(5) . . . . ?
C6 C1 C2 O1 -177.2(5) . . . . ?
C6 C1 C2 C3 1.7(7) . . . . ?
C6 C5 C4 O6 -178.3(5) . . . . ?
C6 C5 C4 C3 0.2(8) . . . . ?
C12 N3 C11 C10 -0.2(8) . . . . ?
C12 C13 C9 C8 179.4(4) . . . . ?
C12 C13 C9 C10 -0.2(7) . . . . ?
C2 C1 C7 N1 2.8(7) . . . . ?
C2 C1 C6 C5 -0.5(8) . . . . ?
C2 C3 C4 O6 179.6(5) . . . . ?
C2 C3 C4 C5 1.1(8) . . . . ?
C14 O6 C4 C3 176.6(6) . . . . ?
C14 O6 C4 C5 -4.9(10) . . . . ?

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

data_exp_5000_autored
_database_code_depnum_ccdc_archive 'CCDC 2091113'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_exp_5000_autored    
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         17 Note
RESPONSE: Some of the low-angle reflections were fully or partially shadowed by the beam-stop. Those reflections were omitted from data reduction or refinement.
;
# Added during the CSD deposition process: Thursday 15 July 2021 10:23 AM
# end Validation Reply Form

_audit_creation_date             2021-06-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'bis((aquo)-dioxo-(N-(2-oxy-3-hydroxybenzylidene)isonicotinylhydrazonato)-molybdenum(vi)) hexamolybdate'
_chemical_formula_moiety         'Mo6 O19, 2(C13 H12 Mo N3 O6)'
_chemical_formula_sum            'C26 H24 Mo8 N6 O31'
_chemical_formula_weight         1684.03
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/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                   7.6794(2)
_cell_length_b                   9.3605(3)
_cell_length_c                   29.2326(9)
_cell_angle_alpha                90
_cell_angle_beta                 89.706(3)
_cell_angle_gamma                90
_cell_volume                     2101.30(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7205
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.7240
_cell_measurement_theta_min      4.4030
_shelx_estimated_absorpt_T_max   0.889
_shelx_estimated_absorpt_T_min   0.713
_exptl_absorpt_coefficient_mu    2.421
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.662
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            31071
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.737
_diffrn_reflns_theta_min         4.026
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     46.00 108.00   1.00   30.00    --   28.19 179.00  90.00   62
  2  ω    -20.00  12.00   1.00   30.00    --   28.19  19.00 -60.00   32
  3  ω   -101.00 -24.00   1.00   30.00    --  -31.15 -37.00-120.00   77
  4  ω     19.00  45.00   1.00   30.00    --   28.19 -57.00  30.00   26
  5  ω    -53.00 -26.00   1.00   30.00    --  -31.15 -57.00   0.00   27
  6  ω   -102.00 -56.00   1.00   30.00    --  -31.15 -57.00   0.00   46
  7  ω     80.00 106.00   1.00   30.00    --   28.19-179.00  30.00   26
  8  ω      0.00  35.00   1.00   30.00    --  -31.15 -19.00 -90.00   35
  9  ω    -81.00 -28.00   1.00   30.00    --  -31.15 -19.00 -90.00   53
 10  ω     38.00  69.00   1.00   30.00    --   28.19 179.00-120.00   31
 11  ω     42.00  77.00   1.00   30.00    --   28.19 179.00 -30.00   35
 12  ω    -85.00 -39.00   1.00   30.00    --  -31.15-179.00   0.00   46
 13  ω    -56.00  -2.00   1.00   30.00    --  -31.15 -77.00   0.00   54
 14  ω   -109.00 -81.00   1.00   30.00    --  -31.15-179.00  30.00   28
 15  ω    -87.00 -38.00   1.00   30.00    --  -31.15-179.00 -60.00   49
 16  ω    -35.00  -8.00   1.00   30.00    --  -31.15 -57.00  30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5238
_reflns_number_total             7112
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.887
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.213
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7112
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0525
_refine_ls_restrained_S_all      1.089
_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)+(0.0287P)²+6.0964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1056
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H) groups
2. Restrained distances
 N3-H3
 0.82 with sigma of 0.02
 O6-H6A
 0.82 with sigma of 0.02
 O6-H6B
 0.82 with sigma of 0.02
 O5-H5
 0.82 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C7(H7), C11(H11), C5(H5A), C10(H10), C6(H6), C4(H4)
;
_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
Mo3 Mo -0.13728(6) 1.02307(4) 0.42960(2) 0.01572(10) Uani 1 1 d . . . . .
Mo2 Mo 0.09984(6) 0.77664(5) 0.47838(2) 0.01992(11) Uani 1 1 d . . . . .
Mo1 Mo 0.68902(6) 0.00292(4) 0.69855(2) 0.01825(10) Uani 1 1 d . . . . .
Mo4 Mo 0.24973(6) 1.10272(5) 0.46938(2) 0.02108(11) Uani 1 1 d . . . . .
O10 O 0.000000 1.000000 0.500000 0.0125(9) Uani 1 2 d S T P . .
O7 O 0.1833(5) 0.7945(3) 0.53970(12) 0.0173(7) Uani 1 1 d . . . . .
O15 O -0.3065(5) 0.9371(4) 0.46477(12) 0.0202(8) Uani 1 1 d . . . . .
O9 O 0.2885(5) 0.9046(4) 0.46060(12) 0.0199(7) Uani 1 1 d . . . . .
O14 O 0.0985(5) 1.1117(4) 0.42044(12) 0.0196(7) Uani 1 1 d . . . . .
O13 O -0.0159(5) 0.8467(3) 0.42381(11) 0.0180(7) Uani 1 1 d . . . . .
O11 O -0.1231(5) 0.7359(4) 0.50275(13) 0.0209(8) Uani 1 1 d . . . . .
O2 O 0.5950(5) 0.1563(4) 0.65797(12) 0.0208(8) Uani 1 1 d . . . . .
O1 O 0.7258(5) -0.0632(4) 0.75979(12) 0.0210(8) Uani 1 1 d . . . . .
O16 O -0.2303(5) 1.0459(4) 0.37798(13) 0.0235(8) Uani 1 1 d . . . . .
O6 O 0.4204(5) 0.0617(4) 0.73239(15) 0.0269(9) Uani 1 1 d D . . . .
O5 O 0.8472(5) -0.2601(4) 0.81526(14) 0.0257(9) Uani 1 1 d D . . . .
O3 O 0.8979(5) 0.0028(4) 0.67918(14) 0.0276(9) Uani 1 1 d . . . . .
O4 O 0.5901(6) -0.1401(4) 0.67451(15) 0.0328(10) Uani 1 1 d . . . . .
O8 O 0.1773(6) 0.6159(4) 0.46232(14) 0.0302(10) Uani 1 1 d . . . . .
N2 N 0.6692(6) 0.3339(4) 0.70889(14) 0.0164(8) Uani 1 1 d . . . . .
N1 N 0.7326(5) 0.2162(4) 0.73299(14) 0.0159(8) Uani 1 1 d . . . . .
N3 N 0.3621(6) 0.5747(4) 0.57968(15) 0.0192(9) Uani 1 1 d D . . . .
O12 O 0.4322(5) 1.1835(5) 0.45096(15) 0.0329(10) Uani 1 1 d . . . . .
C9 C 0.5237(6) 0.3932(5) 0.63815(16) 0.0140(9) Uani 1 1 d . . . . .
C8 C 0.6021(6) 0.2910(5) 0.67066(17) 0.0158(9) Uani 1 1 d . . . . .
C3 C 0.8994(7) -0.1216(5) 0.82263(18) 0.0184(10) Uani 1 1 d . . . . .
C2 C 0.8368(6) -0.0187(5) 0.79240(17) 0.0157(9) Uani 1 1 d . . . . .
C13 C 0.5127(7) 0.5382(5) 0.64826(17) 0.0170(10) Uani 1 1 d . . . . .
H13 H 0.562340 0.574566 0.675593 0.020 Uiso 1 1 calc R . . . .
C1 C 0.8820(7) 0.1266(5) 0.79902(16) 0.0163(9) Uani 1 1 d . . . . .
C12 C 0.4296(7) 0.6286(5) 0.61835(17) 0.0181(10) Uani 1 1 d . . . . .
H12 H 0.420027 0.727656 0.624947 0.022 Uiso 1 1 calc R . . . .
C7 C 0.8165(7) 0.2396(5) 0.77005(17) 0.0175(10) Uani 1 1 d . . . . .
H7 H 0.836583 0.335822 0.778913 0.021 Uiso 1 1 calc R . . . .
C11 C 0.3725(7) 0.4370(5) 0.56841(18) 0.0201(10) Uani 1 1 d . . . . .
H11 H 0.322958 0.404130 0.540626 0.024 Uiso 1 1 calc R . . . .
C5 C 1.0476(7) 0.0622(6) 0.86581(18) 0.0205(10) Uani 1 1 d . . . . .
H5A H 1.118592 0.088536 0.890956 0.025 Uiso 1 1 calc R . . . .
C10 C 0.4551(7) 0.3427(5) 0.59703(18) 0.0204(11) Uani 1 1 d . . . . .
H10 H 0.465485 0.244709 0.588998 0.024 Uiso 1 1 calc R . . . .
C6 C 0.9873(7) 0.1649(6) 0.83605(17) 0.0198(10) Uani 1 1 d . . . . .
H6 H 1.017341 0.262261 0.840678 0.024 Uiso 1 1 calc R . . . .
C4 C 1.0037(7) -0.0806(6) 0.85876(18) 0.0210(11) Uani 1 1 d . . . . .
H4 H 1.046245 -0.151146 0.879204 0.025 Uiso 1 1 calc R . . . .
H3 H 0.309(7) 0.630(5) 0.5630(17) 0.025 Uiso 1 1 d DR . . . .
H6A H 0.340(6) 0.116(5) 0.727(2) 0.025 Uiso 1 1 d DR . . . .
H6B H 0.384(8) -0.003(5) 0.7487(17) 0.025 Uiso 1 1 d DR . . . .
H5 H 0.884(8) -0.320(5) 0.8329(16) 0.025 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo3 O10 2.3271(4) . ?
Mo3 O7 1.961(3) 3_576 ?
Mo3 O15 1.838(4) . ?
Mo3 O14 2.008(4) . ?
Mo3 O13 1.903(3) . ?
Mo3 O16 1.687(4) . ?
Mo2 O10 2.3138(4) . ?
Mo2 O7 1.914(3) . ?
Mo2 O9 1.948(4) . ?
Mo2 O13 1.944(3) . ?
Mo2 O11 1.890(4) . ?
Mo2 O8 1.684(4) . ?
Mo1 O2 2.000(3) . ?
Mo1 O1 1.916(4) . ?
Mo1 O6 2.348(4) . ?
Mo1 O3 1.699(4) . ?
Mo1 O4 1.693(4) . ?
Mo1 N1 2.261(4) . ?
Mo4 O10 2.3207(5) . ?
Mo4 O15 2.011(4) 3_576 ?
Mo4 O9 1.895(3) . ?
Mo4 O14 1.849(3) . ?
Mo4 O11 1.971(4) 3_576 ?
Mo4 O12 1.678(4) . ?
O2 C8 1.316(5) . ?
O1 C2 1.348(6) . ?
O5 C3 1.374(6) . ?
N2 N1 1.397(5) . ?
N2 C8 1.297(6) . ?
N1 C7 1.282(6) . ?
N3 C12 1.344(6) . ?
N3 C11 1.333(6) . ?
C9 C8 1.479(6) . ?
C9 C13 1.392(6) . ?
C9 C10 1.397(7) . ?
C3 C2 1.395(6) . ?
C3 C4 1.383(7) . ?
C2 C1 1.417(7) . ?
C13 C12 1.376(6) . ?
C1 C7 1.447(6) . ?
C1 C6 1.401(7) . ?
C11 C10 1.374(7) . ?
C5 C6 1.378(7) . ?
C5 C4 1.394(7) . ?

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 Mo3 O10 75.97(10) 3_576 . ?
O7 Mo3 O14 82.05(15) 3_576 . ?
O15 Mo3 O10 77.70(11) . . ?
O15 Mo3 O7 90.00(15) . 3_576 ?
O15 Mo3 O14 152.82(15) . . ?
O15 Mo3 O13 90.83(16) . . ?
O14 Mo3 O10 75.17(10) . . ?
O13 Mo3 O10 76.96(10) . . ?
O13 Mo3 O7 152.08(14) . 3_576 ?
O13 Mo3 O14 84.58(15) . . ?
O16 Mo3 O10 177.35(14) . . ?
O16 Mo3 O7 102.87(16) . 3_576 ?
O16 Mo3 O15 104.74(18) . . ?
O16 Mo3 O14 102.36(17) . . ?
O16 Mo3 O13 103.89(16) . . ?
O7 Mo2 O10 77.15(10) . . ?
O7 Mo2 O9 86.79(15) . . ?
O7 Mo2 O13 153.60(14) . . ?
O9 Mo2 O10 76.24(10) . . ?
O13 Mo2 O10 76.52(10) . . ?
O13 Mo2 O9 85.19(15) . . ?
O11 Mo2 O10 77.37(10) . . ?
O11 Mo2 O7 88.38(16) . . ?
O11 Mo2 O9 153.58(15) . . ?
O11 Mo2 O13 87.72(16) . . ?
O8 Mo2 O10 178.58(16) . . ?
O8 Mo2 O7 102.67(17) . . ?
O8 Mo2 O9 102.36(19) . . ?
O8 Mo2 O13 103.61(16) . . ?
O8 Mo2 O11 104.04(19) . . ?
O2 Mo1 O6 76.26(15) . . ?
O2 Mo1 N1 71.65(14) . . ?
O1 Mo1 O2 147.29(15) . . ?
O1 Mo1 O6 79.38(15) . . ?
O1 Mo1 N1 81.16(14) . . ?
O3 Mo1 O2 98.40(18) . . ?
O3 Mo1 O1 99.64(18) . . ?
O3 Mo1 O6 165.15(17) . . ?
O3 Mo1 N1 90.42(17) . . ?
O4 Mo1 O2 99.03(16) . . ?
O4 Mo1 O1 101.61(17) . . ?
O4 Mo1 O6 88.01(19) . . ?
O4 Mo1 O3 106.6(2) . . ?
O4 Mo1 N1 161.84(19) . . ?
N1 Mo1 O6 74.77(15) . . ?
O15 Mo4 O10 74.73(11) 3_576 . ?
O9 Mo4 O10 77.04(11) . . ?
O9 Mo4 O15 85.04(15) . 3_576 ?
O9 Mo4 O11 151.99(16) . 3_576 ?
O14 Mo4 O10 78.24(11) . . ?
O14 Mo4 O15 152.76(16) . 3_576 ?
O14 Mo4 O9 92.20(15) . . ?
O14 Mo4 O11 88.55(15) . 3_576 ?
O11 Mo4 O10 75.71(11) 3_576 . ?
O11 Mo4 O15 81.68(15) 3_576 3_576 ?
O12 Mo4 O10 175.71(16) . . ?
O12 Mo4 O15 101.89(18) . 3_576 ?
O12 Mo4 O9 105.50(19) . . ?
O12 Mo4 O14 104.95(18) . . ?
O12 Mo4 O11 101.32(19) . 3_576 ?
Mo3 O10 Mo3 180.0 3_576 . ?
Mo2 O10 Mo3 90.386(15) 3_576 . ?
Mo2 O10 Mo3 89.615(15) . . ?
Mo2 O10 Mo3 90.384(15) . 3_576 ?
Mo2 O10 Mo3 89.615(15) 3_576 3_576 ?
Mo2 O10 Mo2 180.0 . 3_576 ?
Mo2 O10 Mo4 90.172(18) . 3_576 ?
Mo2 O10 Mo4 89.828(18) 3_576 3_576 ?
Mo2 O10 Mo4 89.828(18) . . ?
Mo2 O10 Mo4 90.172(18) 3_576 . ?
Mo4 O10 Mo3 90.130(16) 3_576 . ?
Mo4 O10 Mo3 90.131(16) . 3_576 ?
Mo4 O10 Mo3 89.871(16) 3_576 3_576 ?
Mo4 O10 Mo3 89.867(16) . . ?
Mo4 O10 Mo4 180.0 3_576 . ?
Mo2 O7 Mo3 116.37(16) . 3_576 ?
Mo3 O15 Mo4 117.43(18) . 3_576 ?
Mo4 O9 Mo2 116.71(18) . . ?
Mo4 O14 Mo3 116.59(17) . . ?
Mo3 O13 Mo2 116.46(17) . . ?
Mo2 O11 Mo4 116.42(17) . 3_576 ?
C8 O2 Mo1 120.3(3) . . ?
C2 O1 Mo1 131.1(3) . . ?
C8 N2 N1 109.4(4) . . ?
N2 N1 Mo1 114.8(3) . . ?
C7 N1 Mo1 127.1(3) . . ?
C7 N1 N2 118.0(4) . . ?
C11 N3 C12 123.2(4) . . ?
C13 C9 C8 121.3(4) . . ?
C13 C9 C10 119.3(4) . . ?
C10 C9 C8 119.4(4) . . ?
O2 C8 C9 114.9(4) . . ?
N2 C8 O2 123.9(4) . . ?
N2 C8 C9 121.2(4) . . ?
O5 C3 C2 116.8(5) . . ?
O5 C3 C4 123.5(4) . . ?
C4 C3 C2 119.6(5) . . ?
O1 C2 C3 117.1(4) . . ?
O1 C2 C1 123.3(4) . . ?
C3 C2 C1 119.4(5) . . ?
C12 C13 C9 119.5(4) . . ?
C2 C1 C7 122.4(4) . . ?
C6 C1 C2 119.6(4) . . ?
C6 C1 C7 118.0(4) . . ?
N3 C12 C13 119.1(4) . . ?
N1 C7 C1 123.2(4) . . ?
N3 C11 C10 119.9(5) . . ?
C6 C5 C4 119.5(5) . . ?
C11 C10 C9 118.9(5) . . ?
C5 C6 C1 120.4(5) . . ?
C3 C4 C5 121.4(5) . . ?

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

data_exp_449_auto
_database_code_depnum_ccdc_archive 'CCDC 2091116'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_audit_creation_date             2021-07-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'[N-(2-oxo-4-methoxybenzylidene)isonicotinoylhydrazonato](aqua)dioxomolybdenum(vi) octamolybdate acetonitrile solvate hydrate'
_chemical_formula_moiety         
'Mo8 O26, 2(C14 H15 Mo N3 O6), 2(C2 H3 N), 3(H2 O)'
_chemical_formula_sum            'C32 H42 Mo10 N8 O41'
_chemical_formula_weight         2154.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.5703(2)
_cell_length_b                   11.3121(2)
_cell_length_c                   14.2003(2)
_cell_angle_alpha                107.1590(10)
_cell_angle_beta                 102.4120(10)
_cell_angle_gamma                105.877(2)
_cell_volume                     1477.54(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    27176
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      79.3330
_cell_measurement_theta_min      3.4250
_shelx_estimated_absorpt_T_max   0.330
_shelx_estimated_absorpt_T_min   0.176
_exptl_absorpt_coefficient_mu    17.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40227
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.134
_diffrn_reflns_theta_min         3.440
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -119.00 -70.00   0.50    0.16    --  -48.02-164.00 104.00   98
  2  ω    -80.00  -8.00   0.50    0.16    --  -48.02 117.00 -19.00  144
  3  ω     29.00  92.00   0.50    0.16    --   48.02-117.00-106.00  126
  4  ω     87.00 116.00   0.50    0.16    --   48.02 164.00 129.00   58
  5  ω     88.00 119.00   0.50    0.16    --   48.02-164.00 104.00   62
  6  ω    -93.00 -68.00   0.50    0.65    --  -91.75-164.00 104.00   50
  7  ω    -75.00 -50.00   0.50    0.65    --  -91.75 117.00 -19.00   50
  8  ω   -145.00-120.00   0.50    0.65    --  -91.75-117.00-106.00   50
  9  ω    100.00 137.00   0.50    0.65    --  113.25-164.00 104.00   74
 10  ω     52.00  78.00   0.50    0.65    --  113.25-117.00-106.00   52
 11  ω     90.00 116.00   0.50    0.65    --  113.25 164.00 129.00   52
 12  ω    125.00 150.00   0.50    0.65    --  113.25 117.00 -19.00   50
 13  ω     81.00 109.00   0.50    0.65    --  113.25-117.00-106.00   56
 14  ω    -87.00 -33.00   0.50    0.16    --  -48.02 -57.00   0.00  108
 15  ω   -118.00 -91.00   0.50    0.16    --  -48.02 -57.00 -60.00   54
 16  ω   -117.00 -37.00   0.50    0.16    --  -48.02 -19.00-180.00  160
 17  ω    -82.00 -33.00   0.50    0.16    --  -48.02 -57.00 -60.00   98
 18  ω    -51.00 -25.00   0.50    0.16    --  -48.02 -77.00-120.00   52
 19  ω   -103.00 -35.00   0.50    0.16    --  -48.02 -38.00 150.00  136
 20  ω   -107.00 -82.00   0.50    0.16    --  -48.02 -77.00-120.00   50
 21  ω    -54.00 -26.00   0.50    0.16    --  -48.02 -77.00  90.00   56
 22  ω    -69.00 -36.00   0.50    0.16    --  -48.02 -38.00  60.00   66
 23  ω    -85.00 -60.00   0.50    0.16    --  -48.02 -77.00 120.00   50
 24  ω    -97.00 -72.00   0.50    0.16    --  -48.02 164.00 129.00   50
 25  ω    -51.00 -25.00   0.50    0.16    --  -48.02 -77.00 120.00   52
 26  ω    -63.00 -25.00   0.50    0.16    --  -48.02 -77.00  30.00   76
 27  ω   -118.00 -37.00   0.50    0.16    --  -48.02 -43.00  47.35  162
 28  ω   -118.00 -93.00   0.50    0.16    --  -48.02 -57.00   0.00   50
 29  ω   -112.00 -86.00   0.50    0.16    --  -48.02 -77.00  90.00   52
 30  ω    -75.00 -26.00   0.50    0.16    --  -48.02 -77.00-180.00   98
 31  ω    -60.00 -25.00   0.50    0.16    --  -48.02 -77.00 -30.00   70
 32  ω   -112.00 -79.00   0.50    0.16    --  -48.02 -77.00 -30.00   66
 33  ω     27.00  54.00   0.50    0.16    --   48.02  77.00 -60.00   54
 34  ω     25.00  72.00   0.50    0.16    --   48.02  77.00-120.00   94
 35  ω    -96.00 -71.00   0.50    0.65    --  -91.75 -72.00  40.76   50
 36  ω    -95.00 -69.00   0.50    0.65    --  -91.75 -76.00-143.60   52
 37  ω   -113.00 -76.00   0.50    0.65    --  -91.75 -61.00 114.47   74
 38  ω    -97.00 -71.00   0.50    0.65    --  -91.75 -72.00  68.10   52
 39  ω    -99.00 -71.00   0.50    0.65    --  -91.75 -74.00 -18.69   56
 40  ω    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00  60.00   52
 41  ω   -161.00-135.00   0.50    0.65    --  -91.75 -72.00  40.76   52
 42  ω   -136.00-110.00   0.50    0.65    --  -91.75 -72.00  68.10   52
 43  ω    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00  90.00   52
 44  ω    -99.00 -69.00   0.50    0.65    --  -91.75 -77.00  30.00   60
 45  ω   -149.00-123.00   0.50    0.65    --  -91.75 -76.00-143.60   52
 46  ω    -99.00 -73.00   0.50    0.65    --  -91.75 -68.00-176.64   52
 47  ω   -110.00 -73.00   0.50    0.65    --  -91.75 -68.00 146.56   74
 48  ω    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00 -49.38   52
 49  ω   -158.00-117.00   0.50    0.65    --  -91.75 -71.00 160.68   82
 50  ω    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00   0.00   52
 51  ω   -101.00 -69.00   0.50    0.65    --  -91.75 -76.00 104.29   64
 52  ω   -100.00 -72.00   0.50    0.65    --  -91.75 -69.00 -84.60   56
 53  ω    -97.00 -71.00   0.50    0.65    --  -91.75 -72.00  73.72   52
 54  ω   -100.00 -74.00   0.50    0.65    --  -91.75 -67.00-122.90   52
 55  ω    -96.00 -71.00   0.50    0.65    --  -91.75 -71.00 160.68   50
 56  ω   -152.00-125.00   0.50    0.65    --  -91.75 -64.00 -44.04   54
 57  ω    -94.00 -69.00   0.50    0.65    --  -91.75 -76.00-128.85   50
 58  ω    -96.00 -70.00   0.50    0.65    --  -91.75 -77.00-150.00   52
 59  ω    -94.00 -69.00   0.50    0.65    --  -91.75 -77.00 120.00   50
 60  ω    -95.00 -70.00   0.50    0.65    --  -91.75 -74.00-175.37   50
 61  ω    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00 -60.00   52
 62  ω   -113.00 -69.00   0.50    0.65    --  -91.75 -77.00 -90.00   88
 63  ω    -94.00 -69.00   0.50    0.65    --  -91.75 -77.00 150.00   50
 64  ω   -100.00 -74.00   0.50    0.65    --  -91.75 -69.00-112.01   52
 65  ω    -94.00 -69.00   0.50    0.65    --  -91.75 -76.00  10.80   50
 66  ω   -100.00 -74.00   0.50    0.65    --  -91.75 -64.00 -44.04   52
 67  ω    -99.00 -73.00   0.50    0.65    --  -91.75 -66.00 -53.02   52
 68  ω     43.00  70.00   0.50    0.65    --  113.25 -95.00 -30.00   54
 69  ω     91.00 176.00   0.50    0.65    --  113.25  77.00 -60.00  170
 70  ω     82.00 107.00   0.50    0.65    --  113.25-109.00 -49.41   50
 71  ω     99.00 177.00   0.50    0.65    --  113.25  61.00-150.00  156
 72  ω     42.00  77.00   0.50    0.65    --  113.25-109.00 -49.41   70
 73  ω    135.00 178.00   0.50    0.65    --  113.25  15.00-180.00   86
 74  ω     93.00 127.00   0.50    0.65    --  113.25  77.00  30.00   68
 75  ω    131.00 156.00   0.50    0.65    --  113.25  77.00  30.00   50
 76  ω    100.00 128.00   0.50    0.65    --  113.25  15.00-180.00   56
 77  ω     43.00 106.00   0.50    0.65    --  113.25 -95.00 150.00  126
 78  ω     42.00  77.00   0.50    0.65    --  113.25 -95.00   0.00   70
 79  ω    136.00 175.00   0.50    0.65    --  113.25  77.00 -90.00   78
 80  ω     92.00 128.00   0.50    0.65    --  113.25  77.00 -90.00   72
 81  ω     98.00 161.00   0.50    0.65    --  113.25 125.00-150.00  126
 82  ω     93.00 151.00   0.50    0.65    --  113.25  77.00 150.00  116
 83  ω     43.00  68.00   0.50    0.65    --  113.25 -77.00 120.00   50
 84  ω     97.00 138.00   0.50    0.65    --  113.25  61.00 -90.00   82
 85  ω     42.00  67.00   0.50    0.65    --  113.25 -61.00  90.00   50
 86  ω     95.00 172.00   0.50    0.65    --  113.25  67.00 -31.14  154
 87  ω     76.00 111.00   0.50    0.65    --  113.25-125.00-180.00   70
 88  ω     91.00 178.00   0.50    0.65    --  113.25  77.00-180.00  174
 89  ω    140.00 178.00   0.50    0.65    --  113.25  77.00 120.00   76
 90  ω     78.00 106.00   0.50    0.65    --  113.25 -95.00  30.00   56
 91  ω     42.00  71.00   0.50    0.65    --  113.25 -95.00  30.00   58
 92  ω     86.00 111.00   0.50    0.65    --  113.25-125.00 -30.00   50
 93  ω     42.00 106.00   0.50    0.65    --  113.25-125.00-120.00  128
 94  ω     43.00  77.00   0.50    0.65    --  113.25-125.00 -30.00   68
 95  ω    146.00 172.00   0.50    0.65    --  113.25  77.00  90.00   52
 96  ω     91.00 117.00   0.50    0.65    --  113.25  77.00 120.00   52
 97  ω     74.00 100.00   0.50    0.65    --  113.25 -95.00  60.00   52
 98  ω    106.00 138.00   0.50    0.65    --  113.25  45.00 -90.00   64
 99  ω    147.00 173.00   0.50    0.65    --  113.25  45.00 -90.00   52
100  ω     91.00 142.00   0.50    0.65    --  113.25  77.00  90.00  102
101  ω     91.00 152.00   0.50    0.65    --  113.25  77.00  60.00  122
102  ω     48.00  93.00   0.50    0.65    --  113.25 -95.00 -90.00   90
103  ω     93.00 150.00   0.50    0.65    --  113.25  77.00 -30.00  114
104  ω    152.00 177.00   0.50    0.65    --  113.25  61.00 150.00   50
105  ω     99.00 125.00   0.50    0.65    --  113.25  61.00 150.00   52
106  ω    104.00 162.00   0.50    0.65    --  113.25 125.00  90.00  116
107  ω     99.00 178.00   0.50    0.65    --  113.25  61.00   0.00  158
108  ω    100.00 158.00   0.50    0.65    --  113.25  61.00  30.00  116
109  ω     46.00  71.00   0.50    0.65    --  113.25 -61.00-150.00   50
110  ω     43.00  89.00   0.50    0.65    --  113.25-125.00 -60.00   92
111  ω     42.00  71.00   0.50    0.65    --  113.25 -61.00-180.00   58
112  ω     92.00 115.00   0.50    0.65    --  113.25  77.00   0.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5812
_reflns_number_total             6253
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.00039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6253
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0315
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0434P)²+4.0660P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0850
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H3-N3
 0.86 with sigma of 0.02
 H20B-O20
 0.82 with sigma of 0.02
3. Others
 Fixed Sof: O21(0.5) H21A(0.5) H21B(0.5)
4.a Free rotating group:
 O20(H20A), O21(H21A,H21B)
4.b Rotating group:
 O5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3A), C5(H5), C6(H6), C7(H7), C13(H13), C10(H10), C11(H11), C12(H12)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), 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
Mo3 Mo 1.01295(3) 0.35171(3) 0.42091(2) 0.01399(9) Uani 1 1 d . . . . .
Mo4 Mo 1.28247(3) 0.55800(3) 0.61676(2) 0.01546(9) Uani 1 1 d . . . . .
Mo2 Mo 1.00696(3) 0.57636(3) 0.32731(2) 0.01633(9) Uani 1 1 d . . . . .
Mo5 Mo 1.27835(3) 0.78765(3) 0.52185(2) 0.01725(9) Uani 1 1 d . . . . .
Mo1 Mo 0.68961(3) 0.67673(3) -0.02488(2) 0.01861(9) Uani 1 1 d . . . . .
O12 O 0.8948(3) 0.4012(3) 0.3254(2) 0.0162(5) Uani 1 1 d . . . . .
O13 O 1.1222(3) 0.3855(3) 0.5620(2) 0.0158(5) Uani 1 1 d . . . . .
O1 O 0.5180(3) 0.7002(3) -0.0206(2) 0.0217(6) Uani 1 1 d . . . . .
O14 O 1.3398(3) 0.7410(3) 0.6381(2) 0.0199(6) Uani 1 1 d . . . . .
O11 O 1.1158(3) 0.5640(3) 0.47920(19) 0.0142(5) Uani 1 1 d . . . . .
O15 O 1.1215(3) 0.7564(3) 0.4074(2) 0.0201(6) Uani 1 1 d . . . . .
O19 O 0.8873(3) 0.2009(3) 0.4007(2) 0.0197(6) Uani 1 1 d . . . . .
O2 O 0.8847(3) 0.7024(3) 0.0516(2) 0.0228(6) Uani 1 1 d . . . . .
O9 O 1.1181(3) 0.3097(3) 0.3534(2) 0.0215(6) Uani 1 1 d . . . . .
O16 O 1.3682(3) 0.5626(3) 0.7345(2) 0.0237(6) Uani 1 1 d . . . . .
O5 O 0.6589(3) 0.6120(3) 0.1123(2) 0.0278(7) Uani 1 1 d . . . . .
H5A H 0.702707 0.557952 0.118302 0.042 Uiso 1 1 d GR . . . .
H5B H 0.571503 0.564197 0.097000 0.042 Uiso 1 1 d GR . . . .
O18 O 0.8868(3) 0.5914(3) 0.2347(2) 0.0262(6) Uani 1 1 d . . . . .
O10 O 1.3727(3) 0.5055(3) 0.5368(2) 0.0217(6) Uani 1 1 d . . . . .
O6 O 0.1572(3) 0.8779(3) -0.0152(2) 0.0285(7) Uani 1 1 d . . . . .
O7 O 1.3759(3) 0.7303(3) 0.4511(2) 0.0259(6) Uani 1 1 d . . . . .
O17 O 1.3594(3) 0.9565(3) 0.5730(3) 0.0287(7) Uani 1 1 d . . . . .
O4 O 0.6340(3) 0.5101(3) -0.0967(2) 0.0282(7) Uani 1 1 d . . . . .
O3 O 0.7279(3) 0.7492(3) -0.1090(2) 0.0270(6) Uani 1 1 d . . . . .
O8 O 1.1143(3) 0.5223(3) 0.2654(2) 0.0226(6) Uani 1 1 d . . . . .
N1 N 0.7731(3) 0.8650(4) 0.1155(3) 0.0211(7) Uani 1 1 d . . . . .
N2 N 0.9106(3) 0.9015(4) 0.1740(3) 0.0261(8) Uani 1 1 d . . . . .
H2 H 0.957960 0.974699 0.229374 0.031 Uiso 1 1 calc R . . . .
N3 N 1.3655(4) 0.8601(5) 0.2902(3) 0.0320(9) Uani 1 1 d D . . . .
C2 C 0.4757(4) 0.7995(4) 0.0207(3) 0.0180(7) Uani 1 1 d . . . . .
C8 C 0.9582(4) 0.8124(5) 0.1352(3) 0.0244(9) Uani 1 1 d . . . . .
C3 C 0.3362(4) 0.7823(4) -0.0229(3) 0.0218(8) Uani 1 1 d . . . . .
H3A H 0.275294 0.703646 -0.080211 0.026 Uiso 1 1 calc R . . . .
N4 N 1.4135(4) 1.2738(5) 0.6778(4) 0.0406(10) Uani 1 1 d . . . . .
C5 C 0.3764(4) 0.9993(4) 0.1044(3) 0.0240(8) Uani 1 1 d . . . . .
H5 H 0.341837 1.066225 0.132646 0.029 Uiso 1 1 calc R . . . .
C4 C 0.2890(4) 0.8828(4) 0.0197(3) 0.0219(8) Uani 1 1 d . . . . .
C1 C 0.5653(4) 0.9165(4) 0.1053(3) 0.0199(8) Uani 1 1 d . . . . .
C6 C 0.5126(4) 1.0154(4) 0.1462(3) 0.0234(8) Uani 1 1 d . . . . .
H6 H 0.572485 1.094448 0.203643 0.028 Uiso 1 1 calc R . . . .
C7 C 0.7090(4) 0.9415(4) 0.1521(3) 0.0224(8) Uani 1 1 d . . . . .
H7 H 0.760410 1.018479 0.213370 0.027 Uiso 1 1 calc R . . . .
C9 C 1.1029(4) 0.8290(5) 0.1882(3) 0.0264(9) Uani 1 1 d . . . . .
C13 C 1.1868(4) 0.9459(5) 0.2728(4) 0.0311(10) Uani 1 1 d . . . . .
H13 H 1.153469 1.015924 0.294876 0.037 Uiso 1 1 calc R . . . .
C10 C 1.1550(5) 0.7298(5) 0.1554(4) 0.0294(9) Uani 1 1 d . . . . .
H10 H 1.099133 0.650319 0.097049 0.035 Uiso 1 1 calc R . . . .
C11 C 1.2892(5) 0.7476(5) 0.2083(4) 0.0322(10) Uani 1 1 d . . . . .
H11 H 1.326561 0.680710 0.186688 0.039 Uiso 1 1 calc R . . . .
C15 C 1.2995(5) 1.2066(5) 0.6400(4) 0.0318(10) Uani 1 1 d . . . . .
C14 C 0.0621(5) 0.7668(6) -0.1053(4) 0.0375(12) Uani 1 1 d . . . . .
H14A H 0.100172 0.758902 -0.163006 0.056 Uiso 1 1 calc GR . . . .
H14B H -0.026683 0.779383 -0.124501 0.056 Uiso 1 1 calc GR . . . .
H14C H 0.047301 0.685805 -0.090297 0.056 Uiso 1 1 calc GR . . . .
C12 C 1.3195(5) 0.9582(6) 0.3241(4) 0.0351(11) Uani 1 1 d . . . . .
H12 H 1.377620 1.036019 0.383096 0.042 Uiso 1 1 calc R . . . .
C16 C 1.1539(5) 1.1194(5) 0.5934(5) 0.0407(12) Uani 1 1 d . . . . .
H16A H 1.108614 1.142058 0.536960 0.061 Uiso 1 1 calc GR . . . .
H16B H 1.107489 1.130406 0.646410 0.061 Uiso 1 1 calc GR . . . .
H16C H 1.147734 1.027000 0.565407 0.061 Uiso 1 1 calc GR . . . .
O20 O 1.3702(4) 0.4767(4) 0.3182(3) 0.0378(8) Uani 1 1 d D . . . .
H20A H 1.396320 0.482192 0.382213 0.057 Uiso 1 1 d G . . . .
O21 O 1.3594(10) 0.2415(10) 0.3984(11) 0.085(4) Uani 0.5 1 d . . P A 1
H21A H 1.414877 0.288645 0.461723 0.127 Uiso 0.5 1 d G . P A 1
H21B H 1.292269 0.272114 0.392450 0.127 Uiso 0.5 1 d G . P A 1
H3 H 1.450(3) 0.877(7) 0.326(5) 0.06(2) Uiso 1 1 d D . . . .
H20B H 1.288(4) 0.475(8) 0.300(6) 0.07(2) Uiso 1 1 d 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
Mo3 Mo2 3.2052(4) . ?
Mo3 O12 1.953(3) . ?
Mo3 O13 1.950(3) . ?
Mo3 O11 2.155(3) . ?
Mo3 O11 2.348(3) 2_766 ?
Mo3 O19 1.751(3) . ?
Mo3 O9 1.691(3) . ?
Mo4 O12 2.305(3) 2_766 ?
Mo4 O13 2.003(3) . ?
Mo4 O14 1.900(3) . ?
Mo4 O11 2.364(2) . ?
Mo4 O16 1.700(3) . ?
Mo4 O10 1.711(3) . ?
Mo2 O12 2.000(3) . ?
Mo2 O13 2.317(3) 2_766 ?
Mo2 O11 2.279(2) . ?
Mo2 O15 1.898(3) . ?
Mo2 O18 1.704(3) . ?
Mo2 O8 1.710(3) . ?
Mo5 O14 1.914(3) . ?
Mo5 O11 2.447(3) . ?
Mo5 O15 1.923(3) . ?
Mo5 O19 2.272(3) 2_766 ?
Mo5 O7 1.709(3) . ?
Mo5 O17 1.711(3) . ?
Mo1 O1 1.914(3) . ?
Mo1 O2 2.010(3) . ?
Mo1 O5 2.327(3) . ?
Mo1 O4 1.715(3) . ?
Mo1 O3 1.694(3) . ?
Mo1 N1 2.236(3) . ?
O1 C2 1.344(5) . ?
O2 C8 1.328(5) . ?
O6 C4 1.354(5) . ?
O6 C14 1.426(6) . ?
N1 N2 1.386(4) . ?
N1 C7 1.298(6) . ?
N2 C8 1.281(6) . ?
N3 C11 1.336(7) . ?
N3 C12 1.334(7) . ?
C2 C3 1.405(5) . ?
C2 C1 1.407(6) . ?
C8 C9 1.485(6) . ?
C3 C4 1.394(6) . ?
N4 C15 1.139(7) . ?
C5 C4 1.399(6) . ?
C5 C6 1.373(6) . ?
C1 C6 1.413(6) . ?
C1 C7 1.432(5) . ?
C9 C13 1.393(7) . ?
C9 C10 1.387(7) . ?
C13 C12 1.383(6) . ?
C10 C11 1.383(6) . ?
C15 C16 1.459(7) . ?

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
O12 Mo3 Mo2 36.33(8) . . ?
O12 Mo3 O11 77.92(11) . . ?
O12 Mo3 O11 77.74(10) . 2_766 ?
O13 Mo3 Mo2 124.66(8) . . ?
O13 Mo3 O12 149.88(11) . . ?
O13 Mo3 O11 77.57(10) . 2_766 ?
O13 Mo3 O11 79.41(11) . . ?
O11 Mo3 Mo2 45.27(7) . . ?
O11 Mo3 Mo2 85.98(6) 2_766 . ?
O11 Mo3 O11 75.50(10) . 2_766 ?
O19 Mo3 Mo2 132.82(9) . . ?
O19 Mo3 O12 96.49(12) . . ?
O19 Mo3 O13 96.71(12) . . ?
O19 Mo3 O11 157.08(12) . . ?
O19 Mo3 O11 81.60(11) . 2_766 ?
O9 Mo3 Mo2 89.45(10) . . ?
O9 Mo3 O12 101.36(12) . . ?
O9 Mo3 O13 101.14(12) . . ?
O9 Mo3 O11 173.29(12) . 2_766 ?
O9 Mo3 O11 97.80(12) . . ?
O9 Mo3 O19 105.10(14) . . ?
O12 Mo4 O11 71.17(9) 2_766 . ?
O13 Mo4 O12 72.18(10) . 2_766 ?
O13 Mo4 O11 73.45(10) . . ?
O14 Mo4 O12 83.09(11) . 2_766 ?
O14 Mo4 O13 146.06(11) . . ?
O14 Mo4 O11 76.81(10) . . ?
O16 Mo4 O12 91.71(12) . 2_766 ?
O16 Mo4 O13 101.78(13) . . ?
O16 Mo4 O14 101.83(14) . . ?
O16 Mo4 O11 162.88(12) . . ?
O16 Mo4 O10 104.77(14) . . ?
O10 Mo4 O12 161.77(11) . 2_766 ?
O10 Mo4 O13 96.43(13) . . ?
O10 Mo4 O14 100.72(13) . . ?
O10 Mo4 O11 92.19(11) . . ?
O12 Mo2 Mo3 35.35(7) . . ?
O12 Mo2 O13 71.96(10) . 2_766 ?
O12 Mo2 O11 74.12(10) . . ?
O13 Mo2 Mo3 79.69(7) 2_766 . ?
O11 Mo2 Mo3 42.21(6) . . ?
O11 Mo2 O13 72.28(9) . 2_766 ?
O15 Mo2 Mo3 120.53(8) . . ?
O15 Mo2 O12 147.68(11) . . ?
O15 Mo2 O13 83.88(11) . 2_766 ?
O15 Mo2 O11 78.33(11) . . ?
O18 Mo2 Mo3 134.35(11) . . ?
O18 Mo2 O12 99.08(13) . . ?
O18 Mo2 O13 88.77(12) . 2_766 ?
O18 Mo2 O11 160.99(12) . . ?
O18 Mo2 O15 101.59(14) . . ?
O18 Mo2 O8 105.25(14) . . ?
O8 Mo2 Mo3 84.51(10) . . ?
O8 Mo2 O12 97.20(13) . . ?
O8 Mo2 O13 163.71(12) . 2_766 ?
O8 Mo2 O11 93.32(12) . . ?
O8 Mo2 O15 100.97(13) . . ?
O14 Mo5 O11 74.49(10) . . ?
O14 Mo5 O15 144.98(12) . . ?
O14 Mo5 O19 77.92(11) . 2_766 ?
O15 Mo5 O11 73.70(10) . . ?
O15 Mo5 O19 77.87(11) . 2_766 ?
O19 Mo5 O11 70.18(10) 2_766 . ?
O7 Mo5 O14 97.90(13) . . ?
O7 Mo5 O11 92.96(12) . . ?
O7 Mo5 O15 97.97(13) . . ?
O7 Mo5 O19 163.14(13) . 2_766 ?
O7 Mo5 O17 104.71(15) . . ?
O17 Mo5 O14 102.19(14) . . ?
O17 Mo5 O11 162.33(13) . . ?
O17 Mo5 O15 103.64(14) . . ?
O17 Mo5 O19 92.15(13) . 2_766 ?
O1 Mo1 O2 148.96(12) . . ?
O1 Mo1 O5 79.70(12) . . ?
O1 Mo1 N1 81.29(12) . . ?
O2 Mo1 O5 78.24(11) . . ?
O2 Mo1 N1 71.99(12) . . ?
O4 Mo1 O1 101.68(13) . . ?
O4 Mo1 O2 97.93(14) . . ?
O4 Mo1 O5 85.15(14) . . ?
O4 Mo1 N1 158.75(14) . . ?
O3 Mo1 O1 100.74(14) . . ?
O3 Mo1 O2 97.52(13) . . ?
O3 Mo1 O5 170.42(13) . . ?
O3 Mo1 O4 104.04(15) . . ?
O3 Mo1 N1 95.94(14) . . ?
N1 Mo1 O5 74.61(12) . . ?
Mo3 O12 Mo4 111.52(11) . 2_766 ?
Mo3 O12 Mo2 108.32(12) . . ?
Mo2 O12 Mo4 103.81(12) . 2_766 ?
Mo3 O13 Mo4 109.50(12) . . ?
Mo3 O13 Mo2 109.53(11) . 2_766 ?
Mo4 O13 Mo2 103.29(11) . 2_766 ?
C2 O1 Mo1 137.7(2) . . ?
Mo4 O14 Mo5 117.83(14) . . ?
Mo3 O11 Mo3 104.50(10) . 2_766 ?
Mo3 O11 Mo4 96.86(9) 2_766 . ?
Mo3 O11 Mo4 91.06(9) . . ?
Mo3 O11 Mo2 92.52(9) . . ?
Mo3 O11 Mo5 163.94(13) . . ?
Mo3 O11 Mo5 91.49(9) 2_766 . ?
Mo4 O11 Mo5 85.50(8) . . ?
Mo2 O11 Mo3 97.95(10) . 2_766 ?
Mo2 O11 Mo4 163.36(13) . . ?
Mo2 O11 Mo5 86.59(8) . . ?
Mo2 O15 Mo5 116.18(14) . . ?
Mo3 O19 Mo5 116.73(14) . 2_766 ?
C8 O2 Mo1 118.6(3) . . ?
C4 O6 C14 118.3(4) . . ?
N2 N1 Mo1 115.3(3) . . ?
C7 N1 Mo1 128.9(3) . . ?
C7 N1 N2 115.7(3) . . ?
C8 N2 N1 109.7(3) . . ?
C12 N3 C11 123.3(4) . . ?
O1 C2 C3 117.5(4) . . ?
O1 C2 C1 122.3(3) . . ?
C3 C2 C1 120.2(4) . . ?
O2 C8 C9 117.0(4) . . ?
N2 C8 O2 124.2(4) . . ?
N2 C8 C9 118.7(4) . . ?
C4 C3 C2 118.7(4) . . ?
C6 C5 C4 119.1(4) . . ?
O6 C4 C3 124.2(4) . . ?
O6 C4 C5 113.9(4) . . ?
C3 C4 C5 121.8(4) . . ?
C2 C1 C6 119.1(4) . . ?
C2 C1 C7 123.1(4) . . ?
C6 C1 C7 117.8(4) . . ?
C5 C6 C1 121.1(4) . . ?
N1 C7 C1 123.8(4) . . ?
C13 C9 C8 119.3(4) . . ?
C10 C9 C8 121.0(4) . . ?
C10 C9 C13 119.7(4) . . ?
C12 C13 C9 118.7(5) . . ?
C11 C10 C9 119.3(5) . . ?
N3 C11 C10 119.2(5) . . ?
N4 C15 C16 178.7(6) . . ?
N3 C12 C13 119.7(5) . . ?

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

data_exp_1373_auto
_database_code_depnum_ccdc_archive 'CCDC 2091117'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2021-06-20 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_audit_creation_date             2021-06-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[N'-(2-oxo-4-hydroxybenzylidene)isonicotinoylhydrazonato](acetonitrile)dioxomolybdenum(vi) hexamolybdate acetonitrile solvate"
_chemical_formula_moiety         'Mo6 O19, 2(C15 H13 Mo N4 O5), 2(C2 H3 N)'
_chemical_formula_sum            'C34 H32 Mo8 N10 O29'
_chemical_formula_weight         1812.21
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.0479(4)
_cell_length_b                   8.6686(2)
_cell_length_c                   29.2039(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.920(2)
_cell_angle_gamma                90
_cell_volume                     5300.01(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21240
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      78.9310
_cell_measurement_theta_min      3.0440
_shelx_estimated_absorpt_T_max   0.386
_shelx_estimated_absorpt_T_min   0.138
_exptl_absorpt_coefficient_mu    15.881
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.173
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
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            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3496
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 2 2 0.0592
1 -2 2 0.0573
-6 -1 -15 0.0590
-11 0 12 0.0247
11 0 -12 0.0494
7 0 15 0.0929

_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.074
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            49371
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.359
_diffrn_reflns_theta_min         3.043
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     26.00  53.00   0.50    0.05    --   47.77  77.00  90.00   54
  2  ω     96.00 174.00   0.50    0.10    --  113.25  77.00 150.00  156
  3  ω     92.00 149.00   0.50    0.10    --  113.25  77.00  30.00  114
  4  ω     95.00 120.00   0.50    0.10    --  113.25  77.00 -60.00   50
  5  ω    123.00 172.00   0.50    0.10    --  113.25  77.00-150.00   98
  6  ω     91.00 118.00   0.50    0.10    --  113.25  77.00-150.00   54
  7  ω     92.00 162.00   0.50    0.10    --  113.25  77.00 -90.00  140
  8  ω    136.00 178.00   0.50    0.10    --  113.25  77.00 -60.00   84
  9  ω    120.00 175.00   0.50    0.10    --  113.25  77.00-180.00  110
 10  ω    136.00 178.00   0.50    0.10    --  113.25  77.00   0.00   84
 11  ω     91.00 131.00   0.50    0.10    --  113.25  77.00   0.00   80
 12  ω     99.00 176.00   0.50    0.10    --  113.25  77.00 120.00  154
 13  ω     92.00 175.00   0.50    0.10    --  113.25  77.00  90.00  166
 14  ω     96.00 142.00   0.50    0.10    --  113.25  77.00  60.00   92
 15  ω     91.00 125.00   0.50    0.10    --  113.25  77.00 -30.00   68
 16  ω    129.00 170.00   0.50    0.10    --  113.25  77.00 -30.00   82
 17  ω     99.00 151.00   0.50    0.10    --  113.25  61.00 120.00  104
 18  ω     96.00 170.00   0.50    0.10    --  113.25  77.00-120.00  148
 19  ω     98.00 162.00   0.50    0.10    --  113.25  61.00-150.00  128
 20  ω     91.00 117.00   0.50    0.10    --  113.25  77.00-180.00   52
 21  ω    103.00 129.00   0.50    0.10    --  113.25  61.00-180.00   52
 22  ω     99.00 159.00   0.50    0.10    --  113.25  61.00 -90.00  120
 23  ω     99.00 154.00   0.50    0.10    --  113.25  61.00-120.00  110
 24  ω     98.00 152.00   0.50    0.10    --  113.25  61.00   0.00  108
 25  ω     98.00 170.00   0.50    0.10    --  113.25  61.00  30.00  144
 26  ω    152.00 178.00   0.50    0.10    --  113.25  61.00  60.00   52
 27  ω     97.00 140.00   0.50    0.10    --  113.25  61.00  90.00   86
 28  ω     98.00 135.00   0.50    0.10    --  113.25  61.00  60.00   74
 29  ω     97.00 158.00   0.50    0.10    --  113.25  61.00 -30.00  122
 30  ω    140.00 178.00   0.50    0.10    --  113.25  15.00-180.00   76
 31  ω    -83.00 -14.00   0.50    0.05    --  -47.77 125.00-120.00  138
 32  ω    -74.00 -49.00   0.50    0.10    --  -91.75  93.00 -75.00   50
 33  ω    -76.00 -28.00   0.50    0.05    --  -47.77  93.00 -75.00   96
 34  ω     42.00 111.00   0.50    0.10    --  113.25-125.00 150.00  138
 35  ω     51.00  91.00   0.50    0.10    --  113.25-145.00  45.02   80
 36  ω     47.00  88.00   0.50    0.05    --   47.77-125.00 -90.00   82
 37  ω     69.00 111.00   0.50    0.10    --  113.25-125.00 -90.00   84
 38  ω     52.00 111.00   0.50    0.10    --  113.25-125.00-120.00  118
 39  ω     59.00 111.00   0.50    0.10    --  113.25-125.00-180.00  104
 40  ω     43.00  69.00   0.50    0.10    --  113.25-112.00-115.17   52
 41  ω     74.00 108.00   0.50    0.10    --  113.25-112.00-115.17   68
 42  ω     82.00 107.00   0.50    0.10    --  113.25-107.00 -39.75   50
 43  ω     75.00 106.00   0.50    0.10    --  113.25-106.00  27.75   62
 44  ω     43.00  72.00   0.50    0.10    --  113.25-106.00  27.75   58
 45  ω     65.00 108.00   0.50    0.10    --  113.25-112.00  80.53   86
 46  ω     44.00 106.00   0.50    0.10    --  113.25-110.00 103.09  124
 47  ω     61.00  88.00   0.50    0.10    --  113.25 -93.00 172.00   54
 48  ω      7.00  77.00   0.50    0.05    --   47.77 -93.00 172.00  140
 49  ω     55.00 103.00   0.50    0.10    --  113.25 -95.00 -30.00   96
 50  ω     42.00 103.00   0.50    0.10    --  113.25 -95.00 -90.00  122
 51  ω     44.00  71.00   0.50    0.10    --  113.25 -61.00-120.00   54
 52  ω     56.00  99.00   0.50    0.10    --  113.25 -77.00   0.00   86
 53  ω     43.00  76.00   0.50    0.10    --  113.25 -77.00  30.00   66
 54  ω     45.00  70.00   0.50    0.10    --  113.25 -61.00  60.00   50
 55  ω     42.00  90.00   0.50    0.10    --  113.25 -77.00 120.00   96
 56  ω    113.00 173.00   0.50    0.10    --  113.25  93.00 -75.00  120
 57  ω    153.00 178.00   0.50    0.10    --  113.25 125.00  30.00   50
 58  ω    113.00 178.00   0.50    0.10    --  113.25 125.00  60.00  130
 59  ω    106.00 134.00   0.50    0.10    --  113.25 125.00  30.00   56
 60  ω   -120.00 -36.00   0.50    0.05    --  -47.77 -19.00 -90.00  168
 61  ω   -119.00 -94.00   0.50    0.05    --  -47.77 -77.00-120.00   50
 62  ω   -116.00 -90.00   0.50    0.05    --  -47.77 -77.00   0.00   52
 63  ω    -92.00 -60.00   0.50    0.05    --  -47.77 -77.00 120.00   64
 64  ω    -64.00 -25.00   0.50    0.05    --  -47.77 -77.00 150.00   78
 65  ω    -57.00 -26.00   0.50    0.05    --  -47.77 -77.00 120.00   62
 66  ω    -83.00 -28.00   0.50    0.05    --  -47.77 -77.00  60.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5378
_reflns_number_total             5738
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.885
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.000026(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5738
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0607P)²+48.4649P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1208
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H3
 0.86 with sigma of 0.02
 O5-H5
 0.82 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C3(H3A), C11(H11), C5(H5A), C7(H7), C13(H13), C12(H12), C6(H6)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), 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
Mo4 Mo 0.51600(2) 0.13675(5) 0.69615(2) 0.02866(12) Uani 1 1 d . . . . .
Mo3 Mo 0.39158(2) 0.32352(4) 0.72580(2) 0.02772(12) Uani 1 1 d . . . . .
Mo1 Mo 0.59867(2) 0.25696(5) 0.48009(2) 0.03226(13) Uani 1 1 d . . . . .
Mo2 Mo 0.51441(2) 0.51549(5) 0.69585(2) 0.03165(13) Uani 1 1 d . . . . .
O16 O 0.60006(17) 0.1718(4) 0.72288(13) 0.0317(8) Uani 1 1 d . . . . .
O15 O 0.59952(17) 0.4763(4) 0.72309(13) 0.0316(7) Uani 1 1 d . . . . .
O7 O 0.42251(17) 0.4792(4) 0.68844(14) 0.0337(8) Uani 1 1 d . . . . .
O8 O 0.42223(18) 0.1701(4) 0.68851(14) 0.0334(8) Uani 1 1 d . . . . .
O10 O 0.500000 0.6323(5) 0.750000 0.0328(11) Uani 1 2 d S T P . .
O2 O 0.61024(18) 0.2444(4) 0.41274(13) 0.0338(8) Uani 1 1 d . . . . .
O1 O 0.61293(18) 0.3594(5) 0.53936(13) 0.0385(9) Uani 1 1 d . . . . .
O9 O 0.500000 0.3244(5) 0.750000 0.0245(9) Uani 1 2 d S T P . .
O5 O 0.70922(18) 0.5244(5) 0.68515(13) 0.0346(8) Uani 1 1 d D . . . .
O12 O 0.52033(18) 0.3252(4) 0.66151(14) 0.0340(8) Uani 1 1 d . . . . .
O14 O 0.500000 0.0191(6) 0.750000 0.0319(11) Uani 1 2 d S T P . .
O6 O 0.31178(18) 0.3234(4) 0.71181(14) 0.0354(8) Uani 1 1 d . . . . .
O13 O 0.52290(19) 0.0013(5) 0.65590(15) 0.0397(9) Uani 1 1 d . . . . .
O11 O 0.5250(2) 0.6502(5) 0.65616(17) 0.0448(10) Uani 1 1 d . . . . .
N3 N 0.6913(2) 0.2311(5) 0.25996(16) 0.0320(9) Uani 1 1 d D . . . .
O4 O 0.5187(2) 0.2229(6) 0.47493(15) 0.0466(10) Uani 1 1 d . . . . .
O3 O 0.6328(2) 0.0841(5) 0.49475(15) 0.0457(10) Uani 1 1 d . . . . .
N1 N 0.6878(2) 0.3862(5) 0.46835(15) 0.0312(9) Uani 1 1 d . . . . .
N2 N 0.7045(2) 0.3834(5) 0.42339(15) 0.0340(9) Uani 1 1 d . . . . .
N5 N 0.6658(2) 0.1277(6) 0.16781(17) 0.0386(10) Uani 1 1 d . . . . .
C10 C 0.6293(3) 0.1897(6) 0.32086(19) 0.0319(10) Uani 1 1 d . . . . .
H10 H 0.593059 0.144837 0.332480 0.038 Uiso 1 1 calc R . . . .
N4 N 0.5651(3) 0.5173(7) 0.45573(19) 0.0457(12) Uani 1 1 d . . . . .
C8 C 0.6617(2) 0.3042(6) 0.39783(19) 0.0304(10) Uani 1 1 d . . . . .
C9 C 0.6721(3) 0.2788(6) 0.34934(18) 0.0304(10) Uani 1 1 d . . . . .
C3 C 0.6595(2) 0.4387(6) 0.61178(18) 0.0326(10) Uani 1 1 d . . . . .
H3A H 0.623982 0.397523 0.625277 0.039 Uiso 1 1 calc R . . . .
C4 C 0.7087(2) 0.5115(6) 0.63931(18) 0.0299(10) Uani 1 1 d . . . . .
C2 C 0.6625(2) 0.4263(6) 0.56468(18) 0.0326(10) Uani 1 1 d . . . . .
C11 C 0.6403(3) 0.1678(6) 0.2760(2) 0.0344(11) Uani 1 1 d . . . . .
H11 H 0.611558 0.107314 0.256183 0.041 Uiso 1 1 calc R . . . .
C5 C 0.7612(3) 0.5751(6) 0.61972(19) 0.0338(11) Uani 1 1 d . . . . .
H5A H 0.794070 0.627243 0.638409 0.041 Uiso 1 1 calc R . . . .
C7 C 0.7241(3) 0.4691(7) 0.49678(18) 0.0342(11) Uani 1 1 d . . . . .
H7 H 0.758693 0.522206 0.485437 0.041 Uiso 1 1 calc R . . . .
C13 C 0.7246(3) 0.3454(6) 0.33123(19) 0.0321(10) Uani 1 1 d . . . . .
H13 H 0.753737 0.408133 0.349942 0.038 Uiso 1 1 calc R . . . .
C1 C 0.7153(3) 0.4860(6) 0.54433(19) 0.0333(11) Uani 1 1 d . . . . .
C12 C 0.7332(3) 0.3187(6) 0.28604(19) 0.0332(11) Uani 1 1 d . . . . .
H12 H 0.768903 0.362069 0.273230 0.040 Uiso 1 1 calc R . . . .
C16 C 0.6432(3) 0.1376(6) 0.1310(2) 0.0360(12) Uani 1 1 d . . . . .
C6 C 0.7642(3) 0.5604(7) 0.57322(19) 0.0357(11) Uani 1 1 d . . . . .
H6 H 0.800018 0.601259 0.560026 0.043 Uiso 1 1 calc R . . . .
C14 C 0.5550(3) 0.6422(8) 0.4464(2) 0.0421(13) Uani 1 1 d . . . . .
C15 C 0.5433(4) 0.8020(8) 0.4342(2) 0.0525(16) Uani 1 1 d . . . . .
H15A H 0.568181 0.830176 0.408872 0.079 Uiso 1 1 calc GR . . . .
H15B H 0.556093 0.867500 0.460936 0.079 Uiso 1 1 calc GR . . . .
H15C H 0.497743 0.816840 0.424551 0.079 Uiso 1 1 calc GR . . . .
C17 C 0.6130(4) 0.1519(9) 0.0841(2) 0.0539(17) Uani 1 1 d . . . . .
H17A H 0.623104 0.060988 0.066300 0.081 Uiso 1 1 calc GR . . . .
H17B H 0.628861 0.244765 0.069906 0.081 Uiso 1 1 calc GR . . . .
H17C H 0.566579 0.159637 0.084535 0.081 Uiso 1 1 calc GR . . . .
H5 H 0.675(2) 0.498(10) 0.692(3) 0.065 Uiso 1 1 d DR . . . .
H3 H 0.692(4) 0.206(10) 0.2317(11) 0.065 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo4 O16 1.883(4) . ?
Mo4 O8 1.985(4) . ?
Mo4 O9 2.311(3) . ?
Mo4 O12 1.929(4) . ?
Mo4 O14 1.933(3) . ?
Mo4 O13 1.678(4) . ?
Mo3 O16 1.988(4) 2_656 ?
Mo3 O15 1.990(4) 2_656 ?
Mo3 O7 1.893(4) . ?
Mo3 O8 1.875(4) . ?
Mo3 O9 2.3183(4) . ?
Mo3 O6 1.687(4) . ?
Mo1 O2 2.009(4) . ?
Mo1 O1 1.941(4) . ?
Mo1 O4 1.700(4) . ?
Mo1 O3 1.697(5) . ?
Mo1 N1 2.242(4) . ?
Mo1 N4 2.448(6) . ?
Mo2 O15 1.914(4) . ?
Mo2 O7 1.950(4) . ?
Mo2 O10 1.928(3) . ?
Mo2 O9 2.331(3) . ?
Mo2 O12 1.941(4) . ?
Mo2 O11 1.677(4) . ?
O2 C8 1.315(6) . ?
O1 C2 1.346(6) . ?
O5 C4 1.342(6) . ?
N3 C11 1.332(8) . ?
N3 C12 1.341(7) . ?
N1 N2 1.394(6) . ?
N1 C7 1.288(7) . ?
N2 C8 1.304(7) . ?
N5 C16 1.133(8) . ?
C10 C9 1.394(7) . ?
C10 C11 1.368(8) . ?
N4 C14 1.132(9) . ?
C8 C9 1.472(8) . ?
C9 C13 1.397(7) . ?
C3 C4 1.394(7) . ?
C3 C2 1.387(7) . ?
C4 C5 1.409(7) . ?
C2 C1 1.412(7) . ?
C5 C6 1.372(8) . ?
C7 C1 1.427(7) . ?
C13 C12 1.371(8) . ?
C1 C6 1.417(7) . ?
C16 C17 1.455(9) . ?
C14 C15 1.445(10) . ?

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
O16 Mo4 O8 154.68(16) . . ?
O16 Mo4 O9 78.52(11) . . ?
O16 Mo4 O12 89.28(17) . . ?
O16 Mo4 O14 89.03(12) . . ?
O8 Mo4 O9 76.16(11) . . ?
O12 Mo4 O8 85.27(16) . . ?
O12 Mo4 O9 77.21(14) . . ?
O12 Mo4 O14 153.56(17) . . ?
O14 Mo4 O8 85.06(12) . . ?
O14 Mo4 O9 76.59(15) . . ?
O13 Mo4 O16 104.94(18) . . ?
O13 Mo4 O8 100.38(18) . . ?
O13 Mo4 O9 176.52(14) . . ?
O13 Mo4 O12 102.3(2) . . ?
O13 Mo4 O14 103.6(2) . . ?
O16 Mo3 O15 83.15(16) 2_656 2_656 ?
O16 Mo3 O9 76.38(13) 2_656 . ?
O15 Mo3 O9 75.85(13) 2_656 . ?
O7 Mo3 O16 153.81(15) . 2_656 ?
O7 Mo3 O15 86.92(17) . 2_656 ?
O7 Mo3 O9 77.71(14) . . ?
O8 Mo3 O16 87.70(17) . 2_656 ?
O8 Mo3 O15 153.68(16) . 2_656 ?
O8 Mo3 O7 90.65(18) . . ?
O8 Mo3 O9 78.03(14) . . ?
O6 Mo3 O16 100.98(17) . 2_656 ?
O6 Mo3 O15 101.33(17) . 2_656 ?
O6 Mo3 O7 104.72(17) . . ?
O6 Mo3 O8 104.62(18) . . ?
O6 Mo3 O9 176.28(14) . . ?
O2 Mo1 N1 71.92(15) . . ?
O2 Mo1 N4 79.99(17) . . ?
O1 Mo1 O2 150.98(16) . . ?
O1 Mo1 N1 81.54(16) . . ?
O1 Mo1 N4 81.42(19) . . ?
O4 Mo1 O2 97.05(18) . . ?
O4 Mo1 O1 102.65(19) . . ?
O4 Mo1 N1 155.5(2) . . ?
O4 Mo1 N4 83.2(2) . . ?
O3 Mo1 O2 96.21(19) . . ?
O3 Mo1 O1 99.0(2) . . ?
O3 Mo1 O4 105.0(2) . . ?
O3 Mo1 N1 98.09(19) . . ?
O3 Mo1 N4 171.5(2) . . ?
N1 Mo1 N4 73.50(18) . . ?
O15 Mo2 O7 153.23(16) . . ?
O15 Mo2 O10 88.39(12) . . ?
O15 Mo2 O9 76.92(11) . . ?
O15 Mo2 O12 87.52(17) . . ?
O7 Mo2 O9 76.33(11) . . ?
O10 Mo2 O7 86.42(12) . . ?
O10 Mo2 O9 76.96(15) . . ?
O10 Mo2 O12 153.38(17) . . ?
O12 Mo2 O7 85.49(17) . . ?
O12 Mo2 O9 76.49(14) . . ?
O11 Mo2 O15 103.00(18) . . ?
O11 Mo2 O7 103.74(18) . . ?
O11 Mo2 O10 104.2(2) . . ?
O11 Mo2 O9 178.88(19) . . ?
O11 Mo2 O12 102.4(2) . . ?
Mo4 O16 Mo3 115.19(18) . 2_656 ?
Mo2 O15 Mo3 116.21(17) . 2_656 ?
Mo3 O7 Mo2 116.58(18) . . ?
Mo3 O8 Mo4 115.84(18) . . ?
Mo2 O10 Mo2 116.6(2) . 2_656 ?
C8 O2 Mo1 119.3(3) . . ?
C2 O1 Mo1 136.6(3) . . ?
Mo4 O9 Mo4 90.53(15) 2_656 . ?
Mo4 O9 Mo3 89.90(8) . . ?
Mo4 O9 Mo3 89.90(8) 2_656 2_656 ?
Mo4 O9 Mo3 89.84(8) . 2_656 ?
Mo4 O9 Mo3 89.84(8) 2_656 . ?
Mo4 O9 Mo2 179.01(9) 2_656 . ?
Mo4 O9 Mo2 90.019(15) . . ?
Mo4 O9 Mo2 90.018(15) 2_656 2_656 ?
Mo4 O9 Mo2 179.01(9) . 2_656 ?
Mo3 O9 Mo3 179.6(2) . 2_656 ?
Mo3 O9 Mo2 90.93(8) . 2_656 ?
Mo3 O9 Mo2 89.33(8) 2_656 2_656 ?
Mo3 O9 Mo2 90.93(8) 2_656 . ?
Mo3 O9 Mo2 89.33(8) . . ?
Mo2 O9 Mo2 89.44(15) . 2_656 ?
Mo4 O12 Mo2 116.1(2) . . ?
Mo4 O14 Mo4 116.3(2) 2_656 . ?
C11 N3 C12 122.8(5) . . ?
N2 N1 Mo1 115.6(3) . . ?
C7 N1 Mo1 129.1(4) . . ?
C7 N1 N2 115.3(4) . . ?
C8 N2 N1 108.8(4) . . ?
C11 C10 C9 119.1(5) . . ?
C14 N4 Mo1 173.5(5) . . ?
O2 C8 C9 118.0(5) . . ?
N2 C8 O2 124.2(5) . . ?
N2 C8 C9 117.8(5) . . ?
C10 C9 C8 120.4(5) . . ?
C10 C9 C13 119.3(5) . . ?
C13 C9 C8 120.3(5) . . ?
C2 C3 C4 120.0(5) . . ?
O5 C4 C3 122.8(5) . . ?
O5 C4 C5 116.5(5) . . ?
C3 C4 C5 120.7(5) . . ?
O1 C2 C3 117.8(5) . . ?
O1 C2 C1 121.7(5) . . ?
C3 C2 C1 120.5(5) . . ?
N3 C11 C10 120.1(5) . . ?
C6 C5 C4 118.9(5) . . ?
N1 C7 C1 123.9(5) . . ?
C12 C13 C9 118.9(5) . . ?
C2 C1 C7 124.0(5) . . ?
C2 C1 C6 118.1(5) . . ?
C6 C1 C7 117.9(5) . . ?
N3 C12 C13 119.8(5) . . ?
N5 C16 C17 178.8(7) . . ?
C5 C6 C1 121.8(5) . . ?
N4 C14 C15 179.0(8) . . ?

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