# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2020

####################################################################### 
# 
# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1983030'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-02-10 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        
"[2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))diphenolato]bis(methanol)tetraoxo-di-molybdenum(vi)"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H18 Mo2 N4 O9'
_chemical_formula_sum            'C17 H18 Mo2 N4 O9'
_chemical_formula_weight         614.23

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.2762(3)
_cell_length_b                   11.2625(3)
_cell_length_c                   25.8472(7)
_cell_angle_alpha                88.871(2)
_cell_angle_beta                 86.314(3)
_cell_angle_gamma                89.709(2)
_cell_volume                     2113.32(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    7174
_cell_measurement_theta_min      4.1850
_cell_measurement_theta_max      28.7940

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_F_000             1216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.245
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.87171
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            15343
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         4.090
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8699
_reflns_number_gt                7737
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0013P)²+15.8437P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8699
_refine_ls_number_parameters     593
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.1205
_refine_ls_wR_factor_gt          0.1176
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_restrained_S_all      1.195
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
# start Validation Reply Form
_vrf_PLAT342_1a                  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01046 Ang.  
RESPONSE: Relatively weak diffraction of the crystal, 
combined with presence of four heavy atoms 
in the asymmetric unit distorts the positions of lighter atoms, 
hereby lowering the precision of C-C bonds.
;
_vrf_PLAT430_1a                  
;
PROBLEM: Short Inter D...A Contact  O16      ..O16      .       2.89 Ang.  
RESPONSE: Distance between two MoO2 core oxygens (CSD lowest: 2.58 Ang.)
;
_vrf_PLAT906_1a                  
;
PROBLEM: Large K Value in the Analysis of Variance ......      6.323 Check 
RESPONSE: The K value is large only for weak reflections with Fc/Fcmax 
lower than 0.018.
;
_vrf_PLAT911_1a                  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          5 Report
RESPONSE: Data completeness is 99.87%, which is enough for a good 
refinement of the model.
;
_vrf_PLAT934_1a                  
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          1 Check 
RESPONSE: Overlap with reflection from another crystal domain.
;
_vrf_PLAT975_1a                  
;
PROBLEM: Check Calcd Resid. Dens.  1.08A   From O6              0.79 eA-3  
RESPONSE: The observed residual density has no meaningful chemical 
interpretation: peak is near MoO2 core oxygen atom.
;
_vrf_PLAT976_1a                  
;
PROBLEM: Check Calcd Resid. Dens.  1.09A   From O8             -0.50 eA-3  
RESPONSE: The observed electron density hole has no meaningful chemical 
interpretation: peak is near methanol ligand coordinated to MoO2 core.
;
_vrf_PLAT977_1a                  
;
PROBLEM: Check Negative Difference Density on H14              -0.32 eA-3  
RESPONSE: H14 is a hydrogen atom on the phenyl ring of the ligand.
;
_vrf_PLAT978_1a                  
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: A consequence of large unit cell and four heavy atoms in the
asymmetric unit.
;
_vrf_PLAT910_1a                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         38 Note 
RESPONSE: Beam-stop shadowing due to large unit cell.
;
# end Validation Reply Form
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 0.25560(8) 0.14959(5) 0.55900(2) 0.02601(13) Uani 1 1 d D . . . .
Mo2 Mo 0.71645(8) 0.35851(5) 0.04628(2) 0.02820(14) Uani 1 1 d D . . . .
Mo3 Mo 0.14209(8) 0.39495(5) 0.39052(2) 0.02935(14) Uani 1 1 d D . . . .
Mo1 Mo 0.88178(9) 0.11527(5) -0.11976(2) 0.03186(15) Uani 1 1 d D . . . .
O2 O 0.7968(7) 0.0561(4) -0.04886(17) 0.0330(10) Uani 1 1 d . . . . .
O11 O 0.2053(7) 0.4514(4) 0.46002(17) 0.0333(10) Uani 1 1 d . . . . .
O12 O 0.2511(7) 0.1313(4) 0.63331(18) 0.0383(12) Uani 1 1 d . . . . .
O10 O 0.0390(7) 0.2788(4) 0.34853(17) 0.0370(11) Uani 1 1 d . . . . .
O18 O -0.0199(6) 0.2475(4) 0.58414(19) 0.0365(11) Uani 1 1 d D . . . .
H18O H -0.028(4) 0.302(4) 0.6059(19) 0.044 Uiso 1 1 d D U . . .
O1 O 0.9953(7) 0.2385(4) -0.16198(18) 0.0397(12) Uani 1 1 d . . . . .
O13 O 0.3596(7) 0.3907(4) 0.36254(19) 0.0426(12) Uani 1 1 d . . . . .
O3 O 0.7449(8) 0.3798(4) 0.11909(18) 0.0422(12) Uani 1 1 d . . . . .
O7 O 0.8032(7) 0.4843(4) 0.0166(2) 0.0412(12) Uani 1 1 d . . . . .
O17 O -0.1411(7) 0.3653(4) 0.4337(2) 0.0388(11) Uani 1 1 d D . . . .
H17O H -0.202(4) 0.4240(19) 0.445(2) 0.047 Uiso 1 1 d D U . . .
O5 O 0.9966(8) -0.0076(4) -0.1417(2) 0.0477(13) Uani 1 1 d . . . . .
O16 O 0.1112(7) 0.0431(4) 0.54004(19) 0.0423(12) Uani 1 1 d . . . . .
O9 O 1.0333(7) 0.3239(5) 0.0490(2) 0.0439(12) Uani 1 1 d D . . . .
H9O H 1.111(2) 0.375(3) 0.039(3) 0.053 Uiso 1 1 d D U . . .
O8 O 1.1431(7) 0.1424(4) -0.0719(2) 0.0443(13) Uani 1 1 d D . . . .
H8O H 1.187(6) 0.086(3) -0.055(2) 0.053 Uiso 1 1 d D U . . .
N6 N 0.2302(7) 0.2598(4) 0.49231(19) 0.0266(11) Uani 1 1 d . . . . .
N5 N 0.1993(7) 0.2334(4) 0.44106(19) 0.0254(11) Uani 1 1 d . . . . .
N1 N 0.7999(7) 0.2740(5) -0.07008(19) 0.0284(12) Uani 1 1 d . . . . .
N4 N 0.6968(7) 0.1671(5) 0.0727(2) 0.0285(11) Uani 1 1 d . . . . .
N2 N 0.7578(7) 0.2473(4) -0.01785(19) 0.0269(11) Uani 1 1 d . . . . .
O15 O 0.4706(7) 0.1008(4) 0.5424(2) 0.0441(12) Uani 1 1 d . . . . .
O14 O 0.0536(8) 0.5285(4) 0.37151(18) 0.0423(12) Uani 1 1 d . . . . .
O6 O 0.4857(7) 0.3760(4) 0.0453(2) 0.0417(12) Uani 1 1 d . . . . .
N8 N 0.3255(7) 0.3376(4) 0.5777(2) 0.0265(11) Uani 1 1 d . . . . .
N3 N 0.7281(8) 0.0775(5) 0.0365(2) 0.0299(12) Uani 1 1 d . . . . .
N7 N 0.2943(7) 0.4267(4) 0.5409(2) 0.0275(11) Uani 1 1 d . . . . .
O4 O 0.6751(8) 0.1124(5) -0.1459(2) 0.0514(14) Uani 1 1 d . . . . .
C8 C 0.7614(9) 0.1255(5) -0.0098(2) 0.0264(13) Uani 1 1 d . . . . .
C25 C 0.2442(8) 0.3790(5) 0.4979(2) 0.0266(13) Uani 1 1 d . . . . .
C26 C 0.3821(9) 0.3741(6) 0.6211(2) 0.0283(13) Uani 1 1 d . . . . .
H26 H 0.416807 0.453227 0.622477 0.034 Uiso 1 1 calc R U . . .
C19 C 0.1005(9) 0.1686(6) 0.3357(3) 0.0316(14) Uani 1 1 d . . . . .
C27 C 0.3957(9) 0.3017(6) 0.6675(2) 0.0302(14) Uani 1 1 d . . . . .
C7 C 0.7722(10) 0.3794(6) -0.0875(3) 0.0360(16) Uani 1 1 d . . . . .
H7 H 0.719877 0.435428 -0.065043 0.043 Uiso 1 1 calc R U . . .
C28 C 0.3242(9) 0.1872(6) 0.6727(2) 0.0306(14) Uani 1 1 d . . . . .
C24 C 0.2180(9) 0.1280(6) 0.4249(2) 0.0288(13) Uani 1 1 d . . . . .
H24 H 0.253012 0.068838 0.447868 0.035 Uiso 1 1 calc R U . . .
C9 C 0.6427(9) 0.1312(6) 0.1187(3) 0.0323(14) Uani 1 1 d . . . . .
H9 H 0.612737 0.051369 0.123289 0.039 Uiso 1 1 calc R U . . .
C1 C 0.8189(10) 0.4146(6) -0.1408(3) 0.0347(15) Uani 1 1 d . . . . .
C12 C 0.6864(10) 0.3830(7) 0.2092(3) 0.0412(17) Uani 1 1 d . . . . .
H12 H 0.727081 0.461158 0.208753 0.049 Uiso 1 1 calc R U . . .
C18 C 0.1871(9) 0.0957(6) 0.3715(2) 0.0286(13) Uani 1 1 d . . . . .
C2 C 0.9256(10) 0.3456(6) -0.1765(3) 0.0345(15) Uani 1 1 d . . . . .
C32 C 0.4709(10) 0.3531(6) 0.7107(3) 0.0386(16) Uani 1 1 d . . . . .
H32 H 0.522620 0.428368 0.707248 0.046 Uiso 1 1 calc R U . . .
C10 C 0.6250(10) 0.2041(6) 0.1634(3) 0.0352(15) Uani 1 1 d . . . . .
C13 C 0.6293(11) 0.3288(7) 0.2555(3) 0.0464(19) Uani 1 1 d . . . . .
H13 H 0.634830 0.369681 0.286254 0.056 Uiso 1 1 calc R U . . .
C29 C 0.3171(10) 0.1281(7) 0.7209(3) 0.0382(16) Uani 1 1 d . . . . .
H29 H 0.264686 0.053073 0.724887 0.046 Uiso 1 1 calc R U . . .
C4 C 0.9032(11) 0.4970(8) -0.2420(3) 0.049(2) Uani 1 1 d . . . . .
H4 H 0.929533 0.524137 -0.275881 0.058 Uiso 1 1 calc R U . . .
C11 C 0.6840(9) 0.3223(6) 0.1629(3) 0.0336(15) Uani 1 1 d . . . . .
C3 C 0.9669(11) 0.3854(7) -0.2269(3) 0.0431(18) Uani 1 1 d . . . . .
H3 H 1.036009 0.338652 -0.250222 0.052 Uiso 1 1 calc R U . . .
C15 C 0.5618(11) 0.1533(7) 0.2114(3) 0.0433(18) Uani 1 1 d . . . . .
H15 H 0.517529 0.075976 0.212201 0.052 Uiso 1 1 calc R U . . .
C20 C 0.0690(10) 0.1290(7) 0.2866(3) 0.0404(17) Uani 1 1 d . . . . .
H20 H 0.008349 0.177303 0.263555 0.048 Uiso 1 1 calc R U . . .
C21 C 0.1288(11) 0.0171(7) 0.2725(3) 0.0470(19) Uani 1 1 d . . . . .
H21 H 0.110238 -0.008982 0.239296 0.056 Uiso 1 1 calc R U . . .
C30 C 0.3881(11) 0.1821(7) 0.7623(3) 0.0432(18) Uani 1 1 d . . . . .
H30 H 0.381951 0.142902 0.794391 0.052 Uiso 1 1 calc R U . . .
C6 C 0.7597(11) 0.5266(7) -0.1577(3) 0.0433(18) Uani 1 1 d . . . . .
H6 H 0.690595 0.574506 -0.134837 0.052 Uiso 1 1 calc R U . . .
C31 C 0.4692(11) 0.2939(7) 0.7577(3) 0.0430(18) Uani 1 1 d . . . . .
H31 H 0.520988 0.327836 0.785847 0.052 Uiso 1 1 calc R U . . .
C23 C 0.2438(10) -0.0187(6) 0.3557(3) 0.0400(17) Uani 1 1 d . . . . .
H23 H 0.301112 -0.068883 0.378718 0.048 Uiso 1 1 calc R U . . .
C14 C 0.5630(12) 0.2128(7) 0.2565(3) 0.048(2) Uani 1 1 d . . . . .
H14 H 0.520249 0.176785 0.287618 0.058 Uiso 1 1 calc R U . . .
C33 C -0.2715(11) 0.2735(7) 0.4266(3) 0.0485(19) Uani 1 1 d D . . . .
H33A H -0.322277 0.284158 0.393468 0.073 Uiso 1 1 calc R U . . .
H33B H -0.368546 0.276960 0.453524 0.073 Uiso 1 1 calc R U . . .
H33C H -0.211183 0.197568 0.428125 0.073 Uiso 1 1 calc R U . . .
C22 C 0.2156(12) -0.0570(7) 0.3065(3) 0.0479(19) Uani 1 1 d . . . . .
H22 H 0.254733 -0.132251 0.296318 0.057 Uiso 1 1 calc R U . . .
C5 C 0.8031(12) 0.5670(7) -0.2081(3) 0.049(2) Uani 1 1 d . . . . .
H5 H 0.763809 0.641760 -0.218718 0.059 Uiso 1 1 calc R U . . .
C16 C 1.2780(12) 0.2322(8) -0.0763(4) 0.056(2) Uani 1 1 d D . . . .
H16B H 1.355939 0.220912 -0.107232 0.084 Uiso 1 1 calc R U . . .
H16C H 1.350976 0.228356 -0.046657 0.084 Uiso 1 1 calc R U . . .
H16A H 1.218965 0.308474 -0.078046 0.084 Uiso 1 1 calc R U . . .
C34 C -0.1803(12) 0.2537(7) 0.5541(3) 0.054(2) Uani 1 1 d D . . . .
H34A H -0.170038 0.320828 0.530648 0.081 Uiso 1 1 calc R U . . .
H34B H -0.288673 0.262252 0.577003 0.081 Uiso 1 1 calc R U . . .
H34C H -0.189007 0.182321 0.534782 0.081 Uiso 1 1 calc R U . . .
C17 C 1.1267(13) 0.2265(7) 0.0712(4) 0.063(3) Uani 1 1 d D . . . .
H17A H 1.090600 0.154303 0.055609 0.095 Uiso 1 1 calc R U . . .
H17B H 1.095505 0.222357 0.107827 0.095 Uiso 1 1 calc R U . . .
H17C H 1.257230 0.237031 0.065133 0.095 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo4 O15 1.687(5) . ?
Mo4 O16 1.698(5) . ?
Mo4 O12 1.926(5) . ?
Mo4 N6 2.122(5) . ?
Mo4 N8 2.249(5) . ?
Mo4 O18 2.344(5) . ?
Mo2 O6 1.691(5) . ?
Mo2 O7 1.702(5) . ?
Mo2 O3 1.926(5) . ?
Mo2 N2 2.103(5) . ?
Mo2 N4 2.251(5) . ?
Mo2 O9 2.342(5) . ?
Mo3 O13 1.698(5) . ?
Mo3 O14 1.709(5) . ?
Mo3 O10 1.903(5) . ?
Mo3 O11 1.999(4) . ?
Mo3 N5 2.271(5) . ?
Mo3 O17 2.302(5) . ?
Mo1 O4 1.688(5) . ?
Mo1 O5 1.701(5) . ?
Mo1 O1 1.907(5) . ?
Mo1 O2 1.999(4) . ?
Mo1 N1 2.276(5) . ?
Mo1 O8 2.359(5) . ?
O2 C8 1.300(7) . ?
O11 C25 1.305(7) . ?
O12 C28 1.347(8) . ?
O10 C19 1.357(8) . ?
O18 C34 1.443(9) . ?
O18 H18O 0.839(9) . ?
O1 C2 1.362(8) . ?
O3 C11 1.345(8) . ?
O17 C33 1.430(9) . ?
O17 H17O 0.843(10) . ?
O9 C17 1.418(9) . ?
O9 H9O 0.838(9) . ?
O8 C16 1.411(9) . ?
O8 H8O 0.837(10) . ?
N6 C25 1.358(8) . ?
N6 N5 1.396(7) . ?
N5 C24 1.270(8) . ?
N1 C7 1.281(8) . ?
N1 N2 1.392(7) . ?
N4 C9 1.287(8) . ?
N4 N3 1.397(7) . ?
N2 C8 1.383(8) . ?
N8 C26 1.293(8) . ?
N8 N7 1.397(7) . ?
N3 C8 1.313(8) . ?
N7 C25 1.317(8) . ?
C26 C27 1.445(9) . ?
C26 H26 0.9300 . ?
C19 C20 1.386(9) . ?
C19 C18 1.402(9) . ?
C27 C28 1.394(9) . ?
C27 C32 1.409(9) . ?
C7 C1 1.446(9) . ?
C7 H7 0.9300 . ?
C28 C29 1.400(9) . ?
C24 C18 1.465(8) . ?
C24 H24 0.9300 . ?
C9 C10 1.429(9) . ?
C9 H9 0.9300 . ?
C1 C6 1.402(9) . ?
C1 C2 1.409(9) . ?
C12 C13 1.374(10) . ?
C12 C11 1.389(9) . ?
C12 H12 0.9300 . ?
C18 C23 1.411(9) . ?
C2 C3 1.383(9) . ?
C32 C31 1.374(10) . ?
C32 H32 0.9300 . ?
C10 C11 1.400(10) . ?
C10 C15 1.406(9) . ?
C13 C14 1.394(11) . ?
C13 H13 0.9300 . ?
C29 C30 1.371(10) . ?
C29 H29 0.9300 . ?
C4 C5 1.364(11) . ?
C4 C3 1.394(11) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C15 C14 1.357(10) . ?
C15 H15 0.9300 . ?
C20 C21 1.380(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.381(11) . ?
C21 H21 0.9300 . ?
C30 C31 1.394(11) . ?
C30 H30 0.9300 . ?
C6 C5 1.389(10) . ?
C6 H6 0.9300 . ?
C31 H31 0.9300 . ?
C23 C22 1.378(10) . ?
C23 H23 0.9300 . ?
C14 H14 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C22 H22 0.9300 . ?
C5 H5 0.9300 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 H16A 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

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
O15 Mo4 O16 105.9(3) . . ?
O15 Mo4 O12 100.4(2) . . ?
O16 Mo4 O12 104.7(2) . . ?
O15 Mo4 N6 96.1(2) . . ?
O16 Mo4 N6 94.8(2) . . ?
O12 Mo4 N6 149.7(2) . . ?
O15 Mo4 N8 98.3(2) . . ?
O16 Mo4 N8 153.1(2) . . ?
O12 Mo4 N8 81.84(19) . . ?
N6 Mo4 N8 70.66(19) . . ?
O15 Mo4 O18 170.6(2) . . ?
O16 Mo4 O18 83.3(2) . . ?
O12 Mo4 O18 78.8(2) . . ?
N6 Mo4 O18 80.76(19) . . ?
N8 Mo4 O18 72.26(18) . . ?
O6 Mo2 O7 104.0(2) . . ?
O6 Mo2 O3 99.6(2) . . ?
O7 Mo2 O3 105.1(2) . . ?
O6 Mo2 N2 98.5(2) . . ?
O7 Mo2 N2 96.8(2) . . ?
O3 Mo2 N2 147.0(2) . . ?
O6 Mo2 N4 93.8(2) . . ?
O7 Mo2 N4 159.5(2) . . ?
O3 Mo2 N4 81.37(19) . . ?
N2 Mo2 N4 70.17(19) . . ?
O6 Mo2 O9 177.0(2) . . ?
O7 Mo2 O9 79.0(2) . . ?
O3 Mo2 O9 80.0(2) . . ?
N2 Mo2 O9 80.4(2) . . ?
N4 Mo2 O9 83.20(18) . . ?
O13 Mo3 O14 105.3(3) . . ?
O13 Mo3 O10 97.2(2) . . ?
O14 Mo3 O10 106.1(2) . . ?
O13 Mo3 O11 97.5(2) . . ?
O14 Mo3 O11 94.4(2) . . ?
O10 Mo3 O11 150.47(19) . . ?
O13 Mo3 N5 91.1(2) . . ?
O14 Mo3 N5 160.1(2) . . ?
O10 Mo3 N5 82.45(19) . . ?
O11 Mo3 N5 71.83(17) . . ?
O13 Mo3 O17 169.3(2) . . ?
O14 Mo3 O17 85.4(2) . . ?
O10 Mo3 O17 78.8(2) . . ?
O11 Mo3 O17 82.09(19) . . ?
N5 Mo3 O17 78.59(18) . . ?
O4 Mo1 O5 105.8(3) . . ?
O4 Mo1 O1 99.1(3) . . ?
O5 Mo1 O1 102.2(2) . . ?
O4 Mo1 O2 97.2(2) . . ?
O5 Mo1 O2 99.4(2) . . ?
O1 Mo1 O2 148.2(2) . . ?
O4 Mo1 N1 92.5(2) . . ?
O5 Mo1 N1 160.6(2) . . ?
O1 Mo1 N1 80.74(19) . . ?
O2 Mo1 N1 71.37(17) . . ?
O4 Mo1 O8 169.4(2) . . ?
O5 Mo1 O8 84.1(2) . . ?
O1 Mo1 O8 82.1(2) . . ?
O2 Mo1 O8 77.12(19) . . ?
N1 Mo1 O8 77.29(19) . . ?
C8 O2 Mo1 123.4(4) . . ?
C25 O11 Mo3 122.8(4) . . ?
C28 O12 Mo4 136.8(4) . . ?
C19 O10 Mo3 130.2(4) . . ?
C34 O18 Mo4 125.0(5) . . ?
C34 O18 H18O 108.1(17) . . ?
Mo4 O18 H18O 123.9(17) . . ?
C2 O1 Mo1 129.4(4) . . ?
C11 O3 Mo2 134.9(4) . . ?
C33 O17 Mo3 128.4(4) . . ?
C33 O17 H17O 106.2(17) . . ?
Mo3 O17 H17O 119.8(17) . . ?
C17 O9 Mo2 129.3(5) . . ?
C17 O9 H9O 108.5(16) . . ?
Mo2 O9 H9O 122.0(15) . . ?
C16 O8 Mo1 129.9(5) . . ?
C16 O8 H8O 107.1(17) . . ?
Mo1 O8 H8O 120.6(17) . . ?
C25 N6 N5 110.4(5) . . ?
C25 N6 Mo4 117.8(4) . . ?
N5 N6 Mo4 131.8(4) . . ?
C24 N5 N6 120.7(5) . . ?
C24 N5 Mo3 124.9(4) . . ?
N6 N5 Mo3 114.1(4) . . ?
C7 N1 N2 119.6(5) . . ?
C7 N1 Mo1 125.0(4) . . ?
N2 N1 Mo1 115.0(4) . . ?
C9 N4 N3 115.3(5) . . ?
C9 N4 Mo2 125.0(4) . . ?
N3 N4 Mo2 119.4(4) . . ?
C8 N2 N1 109.6(5) . . ?
C8 N2 Mo2 119.2(4) . . ?
N1 N2 Mo2 130.9(4) . . ?
C26 N8 N7 115.3(5) . . ?
C26 N8 Mo4 126.4(4) . . ?
N7 N8 Mo4 118.1(4) . . ?
C8 N3 N4 109.5(5) . . ?
C25 N7 N8 109.9(5) . . ?
O2 C8 N3 118.7(5) . . ?
O2 C8 N2 119.8(5) . . ?
N3 C8 N2 121.5(5) . . ?
O11 C25 N7 117.3(5) . . ?
O11 C25 N6 120.2(5) . . ?
N7 C25 N6 122.5(6) . . ?
N8 C26 C27 125.3(6) . . ?
N8 C26 H26 117.4 . . ?
C27 C26 H26 117.4 . . ?
O10 C19 C20 117.6(6) . . ?
O10 C19 C18 121.2(6) . . ?
C20 C19 C18 121.1(6) . . ?
C28 C27 C32 118.7(6) . . ?
C28 C27 C26 122.8(6) . . ?
C32 C27 C26 118.3(6) . . ?
N1 C7 C1 122.6(6) . . ?
N1 C7 H7 118.7 . . ?
C1 C7 H7 118.7 . . ?
O12 C28 C27 122.6(6) . . ?
O12 C28 C29 117.2(6) . . ?
C27 C28 C29 120.1(6) . . ?
N5 C24 C18 122.9(6) . . ?
N5 C24 H24 118.6 . . ?
C18 C24 H24 118.6 . . ?
N4 C9 C10 125.3(6) . . ?
N4 C9 H9 117.3 . . ?
C10 C9 H9 117.3 . . ?
C6 C1 C2 117.7(6) . . ?
C6 C1 C7 117.8(6) . . ?
C2 C1 C7 124.5(6) . . ?
C13 C12 C11 120.8(7) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C19 C18 C23 117.8(6) . . ?
C19 C18 C24 124.8(6) . . ?
C23 C18 C24 117.3(6) . . ?
O1 C2 C3 117.8(6) . . ?
O1 C2 C1 120.7(6) . . ?
C3 C2 C1 121.4(6) . . ?
C31 C32 C27 121.2(7) . . ?
C31 C32 H32 119.4 . . ?
C27 C32 H32 119.4 . . ?
C11 C10 C15 117.6(7) . . ?
C11 C10 C9 122.9(6) . . ?
C15 C10 C9 119.3(6) . . ?
C12 C13 C14 120.2(7) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C30 C29 C28 119.3(7) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C5 C4 C3 121.3(7) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
O3 C11 C12 117.8(6) . . ?
O3 C11 C10 122.4(6) . . ?
C12 C11 C10 119.8(7) . . ?
C2 C3 C4 118.8(7) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C14 C15 C10 122.5(7) . . ?
C14 C15 H15 118.7 . . ?
C10 C15 H15 118.7 . . ?
C21 C20 C19 119.1(7) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C20 C21 C22 121.4(7) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C29 C30 C31 121.9(7) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
C5 C6 C1 120.8(7) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C32 C31 C30 118.6(7) . . ?
C32 C31 H31 120.7 . . ?
C30 C31 H31 120.7 . . ?
C22 C23 C18 120.9(7) . . ?
C22 C23 H23 119.5 . . ?
C18 C23 H23 119.5 . . ?
C15 C14 C13 119.0(7) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
O17 C33 H33A 109.5 . . ?
O17 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O17 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C23 C22 C21 119.5(7) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C4 C5 C6 120.0(7) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
O8 C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O8 C16 H16A 109.5 . . ?
H16B C16 H16A 109.5 . . ?
H16C C16 H16A 109.5 . . ?
O18 C34 H34A 109.5 . . ?
O18 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O18 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O9 C17 H17A 109.5 . . ?
O9 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O9 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C25 N6 N5 C24 165.9(6) . . . . ?
Mo4 N6 N5 C24 -14.5(9) . . . . ?
C25 N6 N5 Mo3 -8.6(6) . . . . ?
Mo4 N6 N5 Mo3 171.0(3) . . . . ?
C7 N1 N2 C8 167.5(6) . . . . ?
Mo1 N1 N2 C8 -5.2(6) . . . . ?
C7 N1 N2 Mo2 -18.3(9) . . . . ?
Mo1 N1 N2 Mo2 169.0(3) . . . . ?
C9 N4 N3 C8 172.7(6) . . . . ?
Mo2 N4 N3 C8 -1.6(7) . . . . ?
C26 N8 N7 C25 177.6(6) . . . . ?
Mo4 N8 N7 C25 -6.5(6) . . . . ?
Mo1 O2 C8 N3 -171.8(4) . . . . ?
Mo1 O2 C8 N2 8.8(8) . . . . ?
N4 N3 C8 O2 179.0(5) . . . . ?
N4 N3 C8 N2 -1.6(8) . . . . ?
N1 N2 C8 O2 -1.3(8) . . . . ?
Mo2 N2 C8 O2 -176.3(4) . . . . ?
N1 N2 C8 N3 179.3(6) . . . . ?
Mo2 N2 C8 N3 4.3(8) . . . . ?
Mo3 O11 C25 N7 176.1(4) . . . . ?
Mo3 O11 C25 N6 -4.7(8) . . . . ?
N8 N7 C25 O11 178.3(5) . . . . ?
N8 N7 C25 N6 -0.9(8) . . . . ?
N5 N6 C25 O11 8.8(8) . . . . ?
Mo4 N6 C25 O11 -170.8(4) . . . . ?
N5 N6 C25 N7 -172.0(6) . . . . ?
Mo4 N6 C25 N7 8.4(8) . . . . ?
N7 N8 C26 C27 169.7(6) . . . . ?
Mo4 N8 C26 C27 -5.8(9) . . . . ?
Mo3 O10 C19 C20 -145.1(5) . . . . ?
Mo3 O10 C19 C18 37.1(9) . . . . ?
N8 C26 C27 C28 -9.2(11) . . . . ?
N8 C26 C27 C32 176.1(6) . . . . ?
N2 N1 C7 C1 177.7(6) . . . . ?
Mo1 N1 C7 C1 -10.4(10) . . . . ?
Mo4 O12 C28 C27 17.0(11) . . . . ?
Mo4 O12 C28 C29 -166.5(5) . . . . ?
C32 C27 C28 O12 -179.5(6) . . . . ?
C26 C27 C28 O12 5.9(11) . . . . ?
C32 C27 C28 C29 4.1(10) . . . . ?
C26 C27 C28 C29 -170.5(6) . . . . ?
N6 N5 C24 C18 179.9(6) . . . . ?
Mo3 N5 C24 C18 -6.1(9) . . . . ?
N3 N4 C9 C10 171.5(6) . . . . ?
Mo2 N4 C9 C10 -14.6(10) . . . . ?
N1 C7 C1 C6 171.3(7) . . . . ?
N1 C7 C1 C2 -11.1(12) . . . . ?
O10 C19 C18 C23 178.7(6) . . . . ?
C20 C19 C18 C23 1.0(10) . . . . ?
O10 C19 C18 C24 0.7(10) . . . . ?
C20 C19 C18 C24 -177.0(7) . . . . ?
N5 C24 C18 C19 -13.1(10) . . . . ?
N5 C24 C18 C23 168.9(6) . . . . ?
Mo1 O1 C2 C3 -139.9(6) . . . . ?
Mo1 O1 C2 C1 41.8(10) . . . . ?
C6 C1 C2 O1 176.7(7) . . . . ?
C7 C1 C2 O1 -0.9(11) . . . . ?
C6 C1 C2 C3 -1.6(11) . . . . ?
C7 C1 C2 C3 -179.2(7) . . . . ?
C28 C27 C32 C31 -2.2(11) . . . . ?
C26 C27 C32 C31 172.7(7) . . . . ?
N4 C9 C10 C11 -7.0(11) . . . . ?
N4 C9 C10 C15 179.2(7) . . . . ?
C11 C12 C13 C14 -1.8(12) . . . . ?
O12 C28 C29 C30 -179.3(6) . . . . ?
C27 C28 C29 C30 -2.8(11) . . . . ?
Mo2 O3 C11 C12 -161.0(5) . . . . ?
Mo2 O3 C11 C10 21.1(11) . . . . ?
C13 C12 C11 O3 -178.8(7) . . . . ?
C13 C12 C11 C10 -0.8(11) . . . . ?
C15 C10 C11 O3 -179.2(7) . . . . ?
C9 C10 C11 O3 6.8(11) . . . . ?
C15 C10 C11 C12 2.9(10) . . . . ?
C9 C10 C11 C12 -171.1(7) . . . . ?
O1 C2 C3 C4 -177.4(7) . . . . ?
C1 C2 C3 C4 0.9(12) . . . . ?
C5 C4 C3 C2 0.5(13) . . . . ?
C11 C10 C15 C14 -2.5(11) . . . . ?
C9 C10 C15 C14 171.7(7) . . . . ?
O10 C19 C20 C21 -179.6(7) . . . . ?
C18 C19 C20 C21 -1.9(11) . . . . ?
C19 C20 C21 C22 1.4(12) . . . . ?
C28 C29 C30 C31 -0.6(12) . . . . ?
C2 C1 C6 C5 0.9(12) . . . . ?
C7 C1 C6 C5 178.7(8) . . . . ?
C27 C32 C31 C30 -1.1(12) . . . . ?
C29 C30 C31 C32 2.6(12) . . . . ?
C19 C18 C23 C22 0.2(11) . . . . ?
C24 C18 C23 C22 178.4(7) . . . . ?
C10 C15 C14 C13 0.0(12) . . . . ?
C12 C13 C14 C15 2.2(13) . . . . ?
C18 C23 C22 C21 -0.7(12) . . . . ?
C20 C21 C22 C23 -0.2(13) . . . . ?
C3 C4 C5 C6 -1.2(13) . . . . ?
C1 C6 C5 C4 0.5(13) . . . . ?

_refine_diff_density_max         0.902
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.129

####################################################################### 
# 
# 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_5a_064_CH3OH
_database_code_depnum_ccdc_archive 'CCDC 1983032'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-02-10 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_audit_creation_date             2019-07-19
_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        
"2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))di(3-methoxyphenolato))bis(methanol)tetraoxo-di-molybdenum(vi)methanol solvate"
_chemical_formula_moiety         'C19 H22 Mo2 N4 O11, 0.64(C O)'
_chemical_formula_sum            'C19.64 H22 Mo2 N4 O11.64'
_chemical_formula_weight         692.21
_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 0.0033 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                   7.4466(4)
_cell_length_b                   13.8570(9)
_cell_length_c                   14.0640(8)
_cell_angle_alpha                112.516(5)
_cell_angle_beta                 98.637(4)
_cell_angle_gamma                97.085(5)
_cell_volume                     1299.16(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4165
_cell_measurement_theta_min      2.8320
_cell_measurement_theta_max      25.1060
_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_F_000             689.9
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.031
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.79835
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_temperature      150(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            22707
_diffrn_reflns_av_unetI/netI     0.1160
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.710
_diffrn_reflns_theta_max         29.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7246
_reflns_number_gt                4564
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7244
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0633
_refine_ls_restrained_S_all      1.054
_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)+(0.0511P)²+0.9217P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1477
_refine_special_details          ?
_vrf_PLAT077_5a_064_CH3OH        
;
PROBLEM: Unitcell Contains Non-integer Number of Atoms ..     Please Check 
RESPONSE: A consequence of solvent modelling: two methanol molecules 
with occupancy of 0.32.
;
_vrf_PLAT315_5a_064_CH3OH        
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).       C20A Check
RESPONSE: Disordered methanol molecule - no advantage is gained by modelling 
hydrogen atoms.
;
_vrf_PLAT309_5a_064_CH3OH        
;
PROBLEM: Single Bonded Oxygen (C-O > 1.3 Ang) ...........       O12A Check 
RESPONSE: Disordered methanol molecule - no advantage is gained by modelling
hydrogen atoms.
;
_vrf_PLAT342_5a_064_CH3OH        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00921 Ang.  
RESPONSE: Weak diffraction of the crystal, combined with disorder on two sites
and presence of two heavy atoms in the asymmetric unit distorts the positions of
lighter atoms, hereby lowering the precision of C-C bonds.
;
_vrf_PLAT906_5a_064_CH3OH        
;
PROBLEM: Large K Value in the Analysis of Variance ......      9.492 Check 
RESPONSE: The K value is large only for weak reflections with Fc/Fcmax 
lower than 0.012.
;
_vrf_PLAT911_5a_064_CH3OH        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: Two low angle reflections ([1 0 0] and [0 -1 2]) are omitted due 
to beam-stop shadowing.
;
_vrf_PLAT977_5a_064_CH3OH        
;
PROBLEM: Check Negative Difference Density on H6               -0.34 eA-3  
RESPONSE: H6 is a hydrogen atom on the phenyl ring of the ligand.
;
# end Validation Reply Form
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 Mo2-O7B
 1.7 with sigma of 0.005
 Mo2-O7A
 1.7 with sigma of 0.005
 Mo2-O6B
 1.7 with sigma of 0.005
 Mo2-O6A
 1.7 with sigma of 0.005
 Mo2-O11B
 2.3 with sigma of 0.01
 O11A-C19A
 1.4 with sigma of 0.02
 O11B-C19B
 1.4 with sigma of 0.02
 O10-H10
 0.84 with sigma of 0.01
 O11A-H11A
 0.84 with sigma of 0.01
 O11B-H11B
 0.84 with sigma of 0.01
 O12A-C20A
 1.4 with sigma of 0.02
 O12B-C20B
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Mo2) = Uanis(O11B) = Uanis(C19B)
Uanis(Mo2) = Uanis(O7B)
Uanis(Mo2) = Uanis(O7A)
Uanis(Mo2) = Uanis(O6B)
Uanis(Mo2) = Uanis(O6A)
4. Others
 Sof(O6B)=Sof(O11B)=Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(O7B)=Sof(H11B)=
 1-FVAR(1)
 Sof(O7A)=Sof(O11A)=Sof(O6A)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(H11A)=
 FVAR(1)
 Fixed Sof: O12A(0.32) C20B(0.32) O12B(0.32) C20A(0.32)
5.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C13(H13), C7(H7), C9(H9), C6(H6), C4(H4), C5(H5)
5.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C19A(H19A,H19B,
 H19C), C19B(H19D,H19E,H19F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.50089(7) 0.27208(4) 0.80964(4) 0.02112(14) Uani 1 1 d . . . . .
Mo2 Mo 0.75539(7) 0.61865(4) 0.76870(4) 0.02442(14) Uani 1 1 d D . . . .
O2 O 0.6307(6) 0.4153(3) 0.9233(3) 0.0273(9) Uani 1 1 d . . . . .
O1 O 0.3396(5) 0.1873(3) 0.6751(3) 0.0248(9) Uani 1 1 d . . . . .
O10 O 0.2584(6) 0.3570(3) 0.8280(3) 0.0303(10) Uani 1 1 d D . . . .
H10 H 0.243(9) 0.387(4) 0.890(2) 0.036 Uiso 1 1 d DR . . . .
O5 O 0.4265(6) 0.2231(3) 0.8948(3) 0.0316(10) Uani 1 1 d . . . . .
O9 O 1.0375(6) 0.9188(3) 0.7774(3) 0.0321(10) Uani 1 1 d . . . . .
O8 O 0.2216(6) -0.0057(3) 0.5309(3) 0.0300(10) Uani 1 1 d . . . . .
O4 O 0.6952(6) 0.2237(3) 0.7828(3) 0.0325(10) Uani 1 1 d . . . . .
O3 O 0.8617(6) 0.7663(3) 0.8147(4) 0.0334(10) Uani 1 1 d . . . . .
N3 N 0.7952(8) 0.5817(4) 0.9785(4) 0.0317(13) Uani 1 1 d . . . . .
N2 N 0.6463(7) 0.4868(4) 0.7988(4) 0.0231(10) Uani 1 1 d . . . . .
N4 N 0.8582(7) 0.6557(4) 0.9395(4) 0.0265(11) Uani 1 1 d . . . . .
N1 N 0.5611(6) 0.3843(3) 0.7299(4) 0.0203(10) Uani 1 1 d . . . . .
C8 C 0.6913(8) 0.4955(5) 0.9005(5) 0.0274(14) Uani 1 1 d . . . . .
C15 C 1.2022(8) 0.9052(4) 1.0665(5) 0.0258(13) Uani 1 1 d . . . . .
H15 H 1.239248 0.900402 1.131985 0.031 Uiso 1 1 calc R . . . .
C10 C 1.0586(8) 0.8271(4) 0.9879(5) 0.0258(13) Uani 1 1 d . . . . .
C14 C 1.2898(8) 0.9889(4) 1.0487(5) 0.0273(13) Uani 1 1 d . . . . .
H14 H 1.384027 1.042476 1.103009 0.033 Uiso 1 1 calc R . . . .
O7A O 0.5703(7) 0.5970(4) 0.6719(4) 0.02442(14) Uani 0.677(5) 1 d D . P A 1
C13 C 1.2409(8) 0.9954(5) 0.9517(5) 0.0276(13) Uani 1 1 d . . . . .
H13 H 1.305535 1.051754 0.939605 0.033 Uiso 1 1 calc R . . . .
C2 C 0.3654(8) 0.1699(4) 0.5763(4) 0.0225(12) Uani 1 1 d . . . . .
C12 C 1.0983(8) 0.9201(4) 0.8726(5) 0.0255(13) Uani 1 1 d . . . . .
C11 C 1.0048(8) 0.8354(5) 0.8917(5) 0.0263(13) Uani 1 1 d . . . . .
C17 C 1.1384(10) 0.9963(5) 0.7515(6) 0.0405(17) Uani 1 1 d . . . . .
H17A H 1.137650 1.067864 0.802972 0.061 Uiso 1 1 calc GR . . . .
H17B H 1.080462 0.988202 0.680879 0.061 Uiso 1 1 calc GR . . . .
H17C H 1.266540 0.986052 0.753006 0.061 Uiso 1 1 calc GR . . . .
C1 C 0.4485(8) 0.2511(4) 0.5520(5) 0.0247(12) Uani 1 1 d . . . . .
C7 C 0.5318(8) 0.3583(4) 0.6308(5) 0.0256(13) Uani 1 1 d . . . . .
H7 H 0.566332 0.411998 0.606935 0.031 Uiso 1 1 calc R . . . .
O11A O 0.5432(9) 0.6969(5) 0.8760(5) 0.0304(16) Uani 0.677(5) 1 d D . P A 1
C9 C 0.9751(9) 0.7403(5) 1.0095(5) 0.0280(14) Uani 1 1 d . . . . .
H9 H 1.007187 0.744814 1.079280 0.034 Uiso 1 1 calc R . . . .
C6 C 0.4564(9) 0.2279(5) 0.4463(5) 0.0355(15) Uani 1 1 d . . . . .
H6 H 0.508039 0.283098 0.428186 0.043 Uiso 1 1 calc R . . . .
C4 C 0.3139(9) 0.0466(5) 0.3955(5) 0.0347(15) Uani 1 1 d . . . . .
H4 H 0.271113 -0.023552 0.342204 0.042 Uiso 1 1 calc R . . . .
C18 C 0.1270(10) 0.3745(6) 0.7576(5) 0.0447(18) Uani 1 1 d . . . . .
H18A H 0.160070 0.350989 0.688507 0.067 Uiso 1 1 calc GR . . . .
H18B H 0.124197 0.450729 0.783942 0.067 Uiso 1 1 calc GR . . . .
H18C H 0.004577 0.334265 0.750960 0.067 Uiso 1 1 calc GR . . . .
C3 C 0.2987(8) 0.0666(5) 0.4970(5) 0.0258(13) Uani 1 1 d . . . . .
C16 C 0.1480(9) -0.1128(5) 0.4516(5) 0.0350(15) Uani 1 1 d . . . . .
H16A H 0.057424 -0.110377 0.394641 0.052 Uiso 1 1 calc GR . . . .
H16B H 0.087462 -0.155937 0.483391 0.052 Uiso 1 1 calc GR . . . .
H16C H 0.249175 -0.144501 0.422959 0.052 Uiso 1 1 calc GR . . . .
C5 C 0.3911(9) 0.1274(5) 0.3691(5) 0.0393(17) Uani 1 1 d . . . . .
H5 H 0.398198 0.112716 0.298181 0.047 Uiso 1 1 calc R . . . .
O6A O 0.9193(7) 0.5562(5) 0.7148(5) 0.02442(14) Uani 0.677(5) 1 d D . P A 1
C19A C 0.3464(13) 0.6644(12) 0.8468(10) 0.063(4) Uani 0.677(5) 1 d D . P A 1
H19A H 0.310207 0.610172 0.774194 0.094 Uiso 0.677(5) 1 calc GR . P A 1
H19B H 0.290316 0.726122 0.851952 0.094 Uiso 0.677(5) 1 calc GR . P A 1
H19C H 0.303377 0.634654 0.894275 0.094 Uiso 0.677(5) 1 calc GR . P A 1
O6B O 0.9566(11) 0.5785(10) 0.7429(11) 0.02442(14) Uani 0.323(5) 1 d D . P A 2
O11B O 0.4841(13) 0.6715(9) 0.7898(10) 0.02442(14) Uani 0.323(5) 1 d D . P A 2
C19B C 0.415(3) 0.7121(15) 0.8796(14) 0.02442(14) Uani 0.323(5) 1 d D . P A 2
H19D H 0.499310 0.710438 0.939207 0.037 Uiso 0.323(5) 1 calc GR . P A 2
H19E H 0.292834 0.668846 0.868977 0.037 Uiso 0.323(5) 1 calc GR . P A 2
H19F H 0.402339 0.785789 0.894437 0.037 Uiso 0.323(5) 1 calc GR . P A 2
O7B O 0.6417(17) 0.5774(9) 0.6399(5) 0.02442(14) Uani 0.323(5) 1 d D . P A 2
O12A O 0.844(2) 0.5835(11) 0.4840(12) 0.044(4) Uiso 0.32 1 d D . P B 2
C20B C 1.087(3) 0.6795(17) 0.5823(17) 0.035(5) Uiso 0.32 1 d D . P C 1
O12B O 1.2233(19) 0.6289(11) 0.6187(12) 0.042(4) Uiso 0.32 1 d D . P C 1
C20A C 1.016(2) 0.6476(15) 0.5362(16) 0.030(4) Uiso 0.32 1 d D . P B 2
H11A H 0.574(14) 0.725(8) 0.9421(11) 0.045 Uiso 0.677(5) 1 d DR . P A 1
H11B H 0.41(2) 0.677(15) 0.740(9) 0.045 Uiso 0.323(5) 1 d DR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O2 2.016(4) . ?
Mo1 O1 1.916(4) . ?
Mo1 O10 2.268(4) . ?
Mo1 O5 1.712(4) . ?
Mo1 O4 1.701(4) . ?
Mo1 N1 2.278(4) . ?
Mo2 O3 1.915(4) . ?
Mo2 N2 2.123(4) . ?
Mo2 N4 2.241(5) . ?
Mo2 O7A 1.693(4) . ?
Mo2 O11A 2.416(6) . ?
Mo2 O6A 1.688(4) . ?
Mo2 O6B 1.703(5) . ?
Mo2 O11B 2.255(8) . ?
Mo2 O7B 1.718(5) . ?
O2 C8 1.316(6) . ?
O1 C2 1.364(6) . ?
O10 H10 0.840(10) . ?
O10 C18 1.396(7) . ?
O9 C12 1.341(7) . ?
O9 C17 1.425(6) . ?
O8 C3 1.366(7) . ?
O8 C16 1.447(7) . ?
O3 C11 1.354(7) . ?
N3 N4 1.402(6) . ?
N3 C8 1.320(8) . ?
N2 N1 1.378(6) . ?
N2 C8 1.374(7) . ?
N4 C9 1.307(7) . ?
N1 C7 1.274(7) . ?
C15 H15 0.9500 . ?
C15 C10 1.407(8) . ?
C15 C14 1.386(7) . ?
C10 C11 1.404(8) . ?
C10 C9 1.442(7) . ?
C14 H14 0.9500 . ?
C14 C13 1.399(8) . ?
C13 H13 0.9500 . ?
C13 C12 1.391(8) . ?
C2 C1 1.397(8) . ?
C2 C3 1.405(8) . ?
C12 C11 1.425(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C1 C7 1.458(8) . ?
C1 C6 1.408(8) . ?
C7 H7 0.9500 . ?
O11A C19A 1.426(11) . ?
O11A H11A 0.840(10) . ?
C9 H9 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.368(9) . ?
C4 H4 0.9500 . ?
C4 C3 1.372(8) . ?
C4 C5 1.394(9) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C5 H5 0.9500 . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
O11B C19B 1.380(16) . ?
O11B H11B 0.840(10) . ?
C19B H19D 0.9800 . ?
C19B H19E 0.9800 . ?
C19B H19F 0.9800 . ?
O12A C20A 1.379(16) . ?
C20B O12B 1.440(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 O10 80.12(16) . . ?
O2 Mo1 N1 72.41(16) . . ?
O1 Mo1 O2 150.56(16) . . ?
O1 Mo1 O10 80.56(16) . . ?
O1 Mo1 N1 82.09(16) . . ?
O10 Mo1 N1 78.39(15) . . ?
O5 Mo1 O2 94.77(18) . . ?
O5 Mo1 O1 105.56(18) . . ?
O5 Mo1 O10 85.35(17) . . ?
O5 Mo1 N1 160.72(18) . . ?
O4 Mo1 O2 96.78(19) . . ?
O4 Mo1 O1 97.73(19) . . ?
O4 Mo1 O10 168.46(17) . . ?
O4 Mo1 O5 106.0(2) . . ?
O4 Mo1 N1 90.07(17) . . ?
O3 Mo2 N2 151.60(18) . . ?
O3 Mo2 N4 81.98(17) . . ?
O3 Mo2 O11A 80.5(2) . . ?
O3 Mo2 O11B 86.3(3) . . ?
N2 Mo2 N4 71.36(17) . . ?
N2 Mo2 O11A 80.4(2) . . ?
N2 Mo2 O11B 86.4(3) . . ?
N4 Mo2 O11A 67.5(2) . . ?
N4 Mo2 O11B 95.0(3) . . ?
O7A Mo2 O3 103.8(2) . . ?
O7A Mo2 N2 93.7(2) . . ?
O7A Mo2 N4 146.6(3) . . ?
O7A Mo2 O11A 80.8(3) . . ?
O6A Mo2 O3 103.2(3) . . ?
O6A Mo2 N2 91.6(3) . . ?
O6A Mo2 N4 101.2(3) . . ?
O6A Mo2 O7A 109.2(3) . . ?
O6A Mo2 O11A 167.7(3) . . ?
O6B Mo2 O3 93.4(5) . . ?
O6B Mo2 N2 95.9(5) . . ?
O6B Mo2 N4 89.5(5) . . ?
O6B Mo2 O11B 175.4(6) . . ?
O6B Mo2 O7B 96.9(6) . . ?
O7B Mo2 O3 105.6(4) . . ?
O7B Mo2 N2 99.8(4) . . ?
O7B Mo2 N4 169.7(4) . . ?
O7B Mo2 O11B 78.8(6) . . ?
C8 O2 Mo1 121.5(4) . . ?
C2 O1 Mo1 130.0(3) . . ?
Mo1 O10 H10 116(4) . . ?
C18 O10 Mo1 133.6(4) . . ?
C18 O10 H10 110(4) . . ?
C12 O9 C17 116.9(5) . . ?
C3 O8 C16 116.6(5) . . ?
C11 O3 Mo2 134.7(4) . . ?
C8 N3 N4 109.8(5) . . ?
N1 N2 Mo2 130.3(3) . . ?
C8 N2 Mo2 117.3(4) . . ?
C8 N2 N1 111.5(4) . . ?
N3 N4 Mo2 118.5(4) . . ?
C9 N4 Mo2 127.2(4) . . ?
C9 N4 N3 114.3(5) . . ?
N2 N1 Mo1 114.1(3) . . ?
C7 N1 Mo1 125.8(4) . . ?
C7 N1 N2 120.0(4) . . ?
O2 C8 N3 117.2(5) . . ?
O2 C8 N2 119.9(5) . . ?
N3 C8 N2 122.9(5) . . ?
C10 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C10 120.2(6) . . ?
C15 C10 C9 117.9(6) . . ?
C11 C10 C15 119.3(5) . . ?
C11 C10 C9 122.8(6) . . ?
C15 C14 H14 119.7 . . ?
C15 C14 C13 120.7(6) . . ?
C13 C14 H14 119.7 . . ?
C14 C13 H13 119.7 . . ?
C12 C13 C14 120.5(5) . . ?
C12 C13 H13 119.7 . . ?
O1 C2 C1 122.3(5) . . ?
O1 C2 C3 117.4(5) . . ?
C1 C2 C3 120.2(5) . . ?
O9 C12 C13 125.9(5) . . ?
O9 C12 C11 115.2(5) . . ?
C13 C12 C11 118.9(6) . . ?
O3 C11 C10 122.5(5) . . ?
O3 C11 C12 117.1(5) . . ?
C10 C11 C12 120.4(6) . . ?
O9 C17 H17A 109.5 . . ?
O9 C17 H17B 109.5 . . ?
O9 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C2 C1 C7 123.4(5) . . ?
C2 C1 C6 118.5(5) . . ?
C6 C1 C7 118.0(5) . . ?
N1 C7 C1 123.9(5) . . ?
N1 C7 H7 118.1 . . ?
C1 C7 H7 118.1 . . ?
Mo2 O11A H11A 122(7) . . ?
C19A O11A Mo2 125.1(7) . . ?
C19A O11A H11A 108(7) . . ?
N4 C9 C10 124.3(6) . . ?
N4 C9 H9 117.8 . . ?
C10 C9 H9 117.8 . . ?
C1 C6 H6 119.4 . . ?
C5 C6 C1 121.2(6) . . ?
C5 C6 H6 119.4 . . ?
C3 C4 H4 119.4 . . ?
C3 C4 C5 121.2(6) . . ?
C5 C4 H4 119.4 . . ?
O10 C18 H18A 109.5 . . ?
O10 C18 H18B 109.5 . . ?
O10 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O8 C3 C2 114.6(5) . . ?
O8 C3 C4 126.0(5) . . ?
C4 C3 C2 119.4(5) . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C6 C5 C4 119.4(6) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
O11A C19A H19A 109.5 . . ?
O11A C19A H19B 109.5 . . ?
O11A C19A H19C 109.5 . . ?
H19A C19A H19B 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
Mo2 O11B H11B 121(10) . . ?
C19B O11B Mo2 130.1(13) . . ?
C19B O11B H11B 109(10) . . ?
O11B C19B H19D 109.5 . . ?
O11B C19B H19E 109.5 . . ?
O11B C19B H19F 109.5 . . ?
H19D C19B H19E 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C8 N3 -171.4(4) . . . . ?
Mo1 O2 C8 N2 8.2(7) . . . . ?
Mo1 O1 C2 C1 -41.1(7) . . . . ?
Mo1 O1 C2 C3 141.2(4) . . . . ?
Mo1 N1 C7 C1 1.9(8) . . . . ?
Mo2 O3 C11 C10 -31.3(8) . . . . ?
Mo2 O3 C11 C12 150.2(4) . . . . ?
Mo2 N2 N1 Mo1 173.7(2) . . . . ?
Mo2 N2 N1 C7 -2.7(7) . . . . ?
Mo2 N2 C8 O2 -178.6(4) . . . . ?
Mo2 N2 C8 N3 1.0(8) . . . . ?
Mo2 N4 C9 C10 0.7(8) . . . . ?
O1 C2 C1 C7 6.4(9) . . . . ?
O1 C2 C1 C6 -175.1(5) . . . . ?
O1 C2 C3 O8 -2.6(7) . . . . ?
O1 C2 C3 C4 177.0(5) . . . . ?
O9 C12 C11 O3 -2.7(8) . . . . ?
O9 C12 C11 C10 178.8(5) . . . . ?
N3 N4 C9 C10 180.0(5) . . . . ?
N2 N1 C7 C1 177.8(5) . . . . ?
N4 N3 C8 O2 175.8(5) . . . . ?
N4 N3 C8 N2 -3.8(8) . . . . ?
N1 N2 C8 O2 -8.8(7) . . . . ?
N1 N2 C8 N3 170.8(5) . . . . ?
C8 N3 N4 Mo2 4.8(6) . . . . ?
C8 N3 N4 C9 -174.6(5) . . . . ?
C8 N2 N1 Mo1 5.6(5) . . . . ?
C8 N2 N1 C7 -170.8(5) . . . . ?
C15 C10 C11 O3 -176.6(5) . . . . ?
C15 C10 C11 C12 1.9(8) . . . . ?
C15 C10 C9 N4 -170.7(5) . . . . ?
C15 C14 C13 C12 2.5(9) . . . . ?
C10 C15 C14 C13 -1.9(9) . . . . ?
C14 C15 C10 C11 -0.2(8) . . . . ?
C14 C15 C10 C9 178.5(5) . . . . ?
C14 C13 C12 O9 179.0(5) . . . . ?
C14 C13 C12 C11 -0.9(8) . . . . ?
C13 C12 C11 O3 177.2(5) . . . . ?
C13 C12 C11 C10 -1.3(8) . . . . ?
C2 C1 C7 N1 10.6(9) . . . . ?
C2 C1 C6 C5 -2.5(9) . . . . ?
C11 C10 C9 N4 8.0(9) . . . . ?
C17 O9 C12 C13 5.7(8) . . . . ?
C17 O9 C12 C11 -174.4(5) . . . . ?
C1 C2 C3 O8 179.6(5) . . . . ?
C1 C2 C3 C4 -0.8(9) . . . . ?
C1 C6 C5 C4 0.5(10) . . . . ?
C7 C1 C6 C5 176.1(6) . . . . ?
C9 C10 C11 O3 4.7(9) . . . . ?
C9 C10 C11 C12 -176.9(5) . . . . ?
C6 C1 C7 N1 -167.9(6) . . . . ?
C3 C2 C1 C7 -175.9(5) . . . . ?
C3 C2 C1 C6 2.6(9) . . . . ?
C3 C4 C5 C6 1.4(10) . . . . ?
C16 O8 C3 C2 178.9(5) . . . . ?
C16 O8 C3 C4 -0.7(8) . . . . ?
C5 C4 C3 O8 178.3(6) . . . . ?
C5 C4 C3 C2 -1.3(9) . . . . ?

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

data_5b_CH3CN
_database_code_depnum_ccdc_archive 'CCDC 1983034'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-02-10 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_audit_creation_date             2019-07-21
_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        
;
2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))
di(3-methoxyphenolato))bis(imidazol)tetraoxo-di-molybdenum(vi)
acetonitrile solvate
;
_chemical_formula_moiety         'C23 H22 Mo2 N8 O9, C2 H3 N'
_chemical_formula_sum            'C25 H25 Mo2 N9 O9'
_chemical_formula_weight         787.42
_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                   8.2715(3)
_cell_length_b                   12.1751(5)
_cell_length_c                   15.0901(5)
_cell_angle_alpha                85.958(3)
_cell_angle_beta                 87.645(3)
_cell_angle_gamma                81.166(3)
_cell_volume                     1497.20(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5500
_cell_measurement_theta_min      2.1920
_shelx_estimated_absorpt_T_max   0.915
_shelx_estimated_absorpt_T_min   0.714
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85353
_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            'dark orange'
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.855
_diffrn_reflns_theta_min         2.100
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.877
_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                7752
_reflns_number_total             9788
_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.
;
# start Validation Reply Form
_vrf_PLAT220_5b_CH3CN            
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        3.1 Ratio 
RESPONSE: Terminal methyl groups of methoxy subunits have large Ueq 
due to thermal vibration.
;
_vrf_PLAT911_5b_CH3CN            
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          4 Report
RESPONSE: Four reflections ([0 -1 1], [0 0 2], [-1 0 1] and [1 0 0]) were
omitted due to beam-stop shadowing.
;
# end Validation Reply Form
_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 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         9788
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0344
_refine_ls_restrained_S_all      1.061
_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)+(0.0277P)²+0.6461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0803
_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
 H8-N8
 0.88 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N5) = Uanis(C18B)
Uanis(C18B) = Uanis(N6B)
4. Others
 Sof(C18B)=Sof(H18B)=Sof(N6B)=Sof(H6B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=
 1-FVAR(1)
 Sof(N6A)=Sof(H6A)=Sof(C20A)=Sof(H20A)=Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=
 FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C21(H21), C23(H23), C9(H9), C6(H6), C22(H22), C13(H13), C4(H4),
 C5(H5), C15(H15), N6A(H6A), C14(H14), C20A(H20A), C19A(H19A), C18A(H18A),
 C18B(H18B), N6B(H6B), C19B(H19B), C20B(H20B)
5.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_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
Mo2 Mo 0.30988(2) 0.67114(2) 0.43768(2) 0.01519(5) Uani 1 1 d . . . . .
Mo1 Mo 0.26127(2) 0.73760(2) 0.77964(2) 0.01888(5) Uani 1 1 d . . . . .
O3 O 0.2840(2) 0.72522(13) 0.31471(10) 0.0225(3) Uani 1 1 d . . . . .
O2 O 0.3252(2) 0.83875(13) 0.67676(10) 0.0218(3) Uani 1 1 d . . . . .
O7 O 0.2079(2) 0.55873(12) 0.44889(10) 0.0221(3) Uani 1 1 d . . . . .
O1 O 0.2543(2) 0.59325(13) 0.83599(10) 0.0250(4) Uani 1 1 d . . . . .
O6 O 0.5121(2) 0.61900(14) 0.43508(11) 0.0273(4) Uani 1 1 d . . . . .
O9 O 0.3103(3) 0.68602(14) 0.14636(10) 0.0325(4) Uani 1 1 d . . . . .
N2 N 0.3041(2) 0.70695(14) 0.57575(11) 0.0162(3) Uani 1 1 d . . . . .
O8 O 0.1961(3) 0.45028(15) 0.96506(11) 0.0370(5) Uani 1 1 d . . . . .
N4 N 0.3685(2) 0.84457(14) 0.44849(11) 0.0160(3) Uani 1 1 d . . . . .
O4 O 0.0560(2) 0.77950(15) 0.76642(12) 0.0316(4) Uani 1 1 d . . . . .
N7 N 0.0449(2) 0.77134(15) 0.45759(12) 0.0183(4) Uani 1 1 d . . . . .
N3 N 0.3650(2) 0.88618(14) 0.53277(11) 0.0175(4) Uani 1 1 d . . . . .
N1 N 0.2673(2) 0.64403(14) 0.65273(11) 0.0161(3) Uani 1 1 d . . . . .
O5 O 0.3162(2) 0.81538(14) 0.85960(10) 0.0282(4) Uani 1 1 d . . . . .
N8 N -0.1737(3) 0.89907(17) 0.46449(14) 0.0271(4) Uani 1 1 d D . . . .
H8 H -0.237(3) 0.9633(17) 0.4562(18) 0.033 Uiso 1 1 d DR . . . .
N5 N 0.5336(3) 0.66479(18) 0.75988(13) 0.0249(4) Uani 1 1 d . . . . .
C8 C 0.3311(3) 0.80997(17) 0.59470(14) 0.0167(4) Uani 1 1 d . . . . .
C1 C 0.2012(3) 0.47152(17) 0.72384(14) 0.0182(4) Uani 1 1 d . . . . .
C7 C 0.2371(3) 0.54436(17) 0.64751(13) 0.0170(4) Uani 1 1 d . . . . .
H7 H 0.238266 0.516555 0.590191 0.020 Uiso 1 1 calc R . . . .
C21 C -0.0189(3) 0.87512(19) 0.43375(16) 0.0235(5) Uani 1 1 d . . . . .
H21 H 0.037871 0.926182 0.399197 0.028 Uiso 1 1 calc R . . . .
C12 C 0.3817(3) 0.77270(19) 0.16959(15) 0.0237(5) Uani 1 1 d . . . . .
C11 C 0.3684(3) 0.79109(18) 0.26126(14) 0.0193(4) Uani 1 1 d . . . . .
C23 C -0.0774(3) 0.7275(2) 0.50657(15) 0.0243(5) Uani 1 1 d . . . . .
H23 H -0.068522 0.653688 0.532971 0.029 Uiso 1 1 calc R . . . .
C9 C 0.4217(3) 0.90670(18) 0.38431(14) 0.0191(4) Uani 1 1 d . . . . .
H9 H 0.454649 0.974469 0.398820 0.023 Uiso 1 1 calc R . . . .
C10 C 0.4348(3) 0.88080(18) 0.29198(14) 0.0196(4) Uani 1 1 d . . . . .
C6 C 0.1599(3) 0.36778(19) 0.70575(15) 0.0259(5) Uani 1 1 d . . . . .
H6 H 0.155040 0.349286 0.645902 0.031 Uiso 1 1 calc R . . . .
C22 C -0.2121(3) 0.8060(2) 0.51115(16) 0.0279(5) Uani 1 1 d . . . . .
H22 H -0.313332 0.797858 0.540996 0.033 Uiso 1 1 calc R . . . .
C2 C 0.2103(3) 0.49710(18) 0.81252(14) 0.0193(4) Uani 1 1 d . . . . .
C13 C 0.4606(3) 0.8421(2) 0.11160(16) 0.0291(5) Uani 1 1 d . . . . .
H13 H 0.469542 0.829444 0.050071 0.035 Uiso 1 1 calc R . . . .
C4 C 0.1362(4) 0.3177(2) 0.86234(16) 0.0294(6) Uani 1 1 d . . . . .
H4 H 0.113509 0.265130 0.909006 0.035 Uiso 1 1 calc R . . . .
C3 C 0.1786(3) 0.4185(2) 0.88173(15) 0.0240(5) Uani 1 1 d . . . . .
C5 C 0.1267(4) 0.2932(2) 0.77366(16) 0.0322(6) Uani 1 1 d . . . . .
H5 H 0.096916 0.223977 0.760431 0.039 Uiso 1 1 calc R . . . .
C15 C 0.5139(3) 0.9498(2) 0.23118(15) 0.0266(5) Uani 1 1 d . . . . .
H15 H 0.558664 1.010352 0.251732 0.032 Uiso 1 1 calc R . . . .
N6A N 0.7964(7) 0.6642(10) 0.7391(4) 0.0365(16) Uani 0.71(2) 1 d . . P A 1
H6A H 0.891874 0.687730 0.732524 0.044 Uiso 0.71(2) 1 calc R . P A 1
C14 C 0.5268(4) 0.9302(2) 0.14243(16) 0.0304(6) Uani 1 1 d . . . . .
H14 H 0.580997 0.976849 0.102018 0.036 Uiso 1 1 calc R . . . .
C20A C 0.6060(9) 0.5603(7) 0.7490(6) 0.0337(15) Uani 0.71(2) 1 d . . P A 1
H20A H 0.550178 0.497557 0.749683 0.040 Uiso 0.71(2) 1 calc R . P A 1
C19A C 0.7711(9) 0.5564(12) 0.7370(5) 0.0383(15) Uani 0.71(2) 1 d . . P A 1
H19A H 0.850895 0.492609 0.728845 0.046 Uiso 0.71(2) 1 calc R . P A 1
C25 C -0.0229(4) 1.0231(2) 0.8461(2) 0.0448(8) Uani 1 1 d . . . . .
H25A H -0.063230 1.101379 0.856012 0.067 Uiso 1 1 calc GR . . . .
H25B H -0.058005 1.005451 0.788240 0.067 Uiso 1 1 calc GR . . . .
H25C H 0.096931 1.010134 0.847219 0.067 Uiso 1 1 calc GR . . . .
C18A C 0.6513(11) 0.7289(8) 0.7530(7) 0.0314(15) Uani 0.71(2) 1 d . . P A 1
H18A H 0.635426 0.807325 0.757202 0.038 Uiso 0.71(2) 1 calc R . P A 1
C16 C 0.1692(5) 0.3720(2) 1.03791(17) 0.0456(8) Uani 1 1 d . . . . .
H16A H 0.056349 0.356668 1.037729 0.068 Uiso 1 1 calc GR . . . .
H16B H 0.187820 0.403359 1.094017 0.068 Uiso 1 1 calc GR . . . .
H16C H 0.245142 0.302618 1.031691 0.068 Uiso 1 1 calc GR . . . .
C17 C 0.3215(5) 0.6629(3) 0.05415(17) 0.0514(9) Uani 1 1 d . . . . .
H17A H 0.274095 0.729371 0.018270 0.077 Uiso 1 1 calc GR . . . .
H17B H 0.261349 0.601395 0.045132 0.077 Uiso 1 1 calc GR . . . .
H17C H 0.436663 0.642048 0.036084 0.077 Uiso 1 1 calc GR . . . .
N9 N -0.1397(5) 0.8987(3) 0.9705(2) 0.0755(11) Uani 1 1 d . . . . .
C24 C -0.0883(5) 0.9528(2) 0.9153(2) 0.0475(8) Uani 1 1 d . . . . .
C18B C 0.590(3) 0.5472(18) 0.7698(11) 0.0249(4) Uani 0.29(2) 1 d . . P A 2
H18B H 0.524120 0.492556 0.789966 0.030 Uiso 0.29(2) 1 calc R . P A 2
N6B N 0.7452(18) 0.5262(13) 0.7472(9) 0.0249(4) Uani 0.29(2) 1 d . . P A 2
H6B H 0.802839 0.459077 0.747472 0.030 Uiso 0.29(2) 1 calc R . P A 2
C19B C 0.805(2) 0.621(2) 0.7235(13) 0.026(3) Uani 0.29(2) 1 d . . P A 2
H19B H 0.912753 0.628731 0.702809 0.032 Uiso 0.29(2) 1 calc R . P A 2
C20B C 0.678(3) 0.7026(17) 0.7355(14) 0.025(3) Uani 0.29(2) 1 d . . P A 2
H20B H 0.687156 0.779452 0.727688 0.030 Uiso 0.29(2) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo2 O3 1.9339(15) . ?
Mo2 O7 1.7100(16) . ?
Mo2 O6 1.6957(17) . ?
Mo2 N2 2.1556(17) . ?
Mo2 N4 2.2563(18) . ?
Mo2 N7 2.3574(19) . ?
Mo1 O2 2.0174(15) . ?
Mo1 O1 1.9056(15) . ?
Mo1 O4 1.7119(18) . ?
Mo1 N1 2.2914(17) . ?
Mo1 O5 1.7021(16) . ?
Mo1 N5 2.306(2) . ?
O3 C11 1.347(3) . ?
O2 C8 1.307(2) . ?
O1 C2 1.352(3) . ?
O9 C12 1.359(3) . ?
O9 C17 1.436(3) . ?
N2 N1 1.395(2) . ?
N2 C8 1.359(3) . ?
O8 C3 1.361(3) . ?
O8 C16 1.436(3) . ?
N4 N3 1.399(2) . ?
N4 C9 1.291(3) . ?
N7 C21 1.323(3) . ?
N7 C23 1.380(3) . ?
N3 C8 1.323(3) . ?
N1 C7 1.284(3) . ?
N8 H8 0.875(17) . ?
N8 C21 1.340(3) . ?
N8 C22 1.364(3) . ?
N5 C20A 1.339(7) . ?
N5 C18A 1.335(8) . ?
N5 C18B 1.44(2) . ?
N5 C20B 1.37(2) . ?
C1 C7 1.453(3) . ?
C1 C6 1.405(3) . ?
C1 C2 1.403(3) . ?
C7 H7 0.9500 . ?
C21 H21 0.9500 . ?
C12 C11 1.414(3) . ?
C12 C13 1.387(3) . ?
C11 C10 1.409(3) . ?
C23 H23 0.9500 . ?
C23 C22 1.355(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.446(3) . ?
C10 C15 1.409(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.368(3) . ?
C22 H22 0.9500 . ?
C2 C3 1.410(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.392(4) . ?
C4 H4 0.9500 . ?
C4 C3 1.381(3) . ?
C4 C5 1.399(3) . ?
C5 H5 0.9500 . ?
C15 H15 0.9500 . ?
C15 C14 1.374(3) . ?
N6A H6A 0.8800 . ?
N6A C19A 1.364(8) . ?
N6A C18A 1.348(7) . ?
C14 H14 0.9500 . ?
C20A H20A 0.9500 . ?
C20A C19A 1.365(9) . ?
C19A H19A 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 C24 1.444(4) . ?
C18A H18A 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N9 C24 1.135(4) . ?
C18B H18B 0.9500 . ?
C18B N6B 1.30(2) . ?
N6B H6B 0.8800 . ?
N6B C19B 1.344(17) . ?
C19B H19B 0.9500 . ?
C19B C20B 1.347(17) . ?
C20B H20B 0.9500 . ?

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
O3 Mo2 N2 148.73(7) . . ?
O3 Mo2 N4 81.35(6) . . ?
O3 Mo2 N7 84.06(7) . . ?
O7 Mo2 O3 104.45(7) . . ?
O7 Mo2 N2 98.09(7) . . ?
O7 Mo2 N4 160.66(7) . . ?
O7 Mo2 N7 82.98(7) . . ?
O6 Mo2 O3 99.82(8) . . ?
O6 Mo2 O7 106.21(8) . . ?
O6 Mo2 N2 94.28(8) . . ?
O6 Mo2 N4 90.63(8) . . ?
O6 Mo2 N7 168.56(8) . . ?
N2 Mo2 N4 70.66(6) . . ?
N2 Mo2 N7 77.42(7) . . ?
N4 Mo2 N7 79.25(6) . . ?
O2 Mo1 N1 72.02(6) . . ?
O2 Mo1 N5 79.62(7) . . ?
O1 Mo1 O2 151.56(7) . . ?
O1 Mo1 N1 82.86(6) . . ?
O1 Mo1 N5 81.66(8) . . ?
O4 Mo1 O2 93.47(8) . . ?
O4 Mo1 O1 99.13(8) . . ?
O4 Mo1 N1 88.57(7) . . ?
O4 Mo1 N5 164.59(8) . . ?
N1 Mo1 N5 76.22(7) . . ?
O5 Mo1 O2 95.10(7) . . ?
O5 Mo1 O1 105.66(7) . . ?
O5 Mo1 O4 105.89(9) . . ?
O5 Mo1 N1 161.44(8) . . ?
O5 Mo1 N5 88.54(8) . . ?
C11 O3 Mo2 131.64(14) . . ?
C8 O2 Mo1 122.00(14) . . ?
C2 O1 Mo1 135.82(14) . . ?
C12 O9 C17 116.9(2) . . ?
N1 N2 Mo2 131.20(13) . . ?
C8 N2 Mo2 117.43(13) . . ?
C8 N2 N1 111.25(16) . . ?
C3 O8 C16 117.0(2) . . ?
N3 N4 Mo2 118.60(12) . . ?
C9 N4 Mo2 125.69(14) . . ?
C9 N4 N3 115.33(17) . . ?
C21 N7 Mo2 132.01(16) . . ?
C21 N7 C23 105.3(2) . . ?
C23 N7 Mo2 122.56(15) . . ?
C8 N3 N4 110.34(17) . . ?
N2 N1 Mo1 113.67(12) . . ?
C7 N1 Mo1 126.37(14) . . ?
C7 N1 N2 119.95(17) . . ?
C21 N8 H8 125.6(19) . . ?
C21 N8 C22 107.4(2) . . ?
C22 N8 H8 127.0(19) . . ?
C20A N5 Mo1 130.8(4) . . ?
C18A N5 Mo1 122.2(5) . . ?
C18A N5 C20A 106.9(5) . . ?
C18B N5 Mo1 121.9(8) . . ?
C20B N5 Mo1 138.0(8) . . ?
C20B N5 C18B 100.0(11) . . ?
O2 C8 N2 120.92(19) . . ?
O2 C8 N3 116.19(18) . . ?
N3 C8 N2 122.89(18) . . ?
C6 C1 C7 116.56(19) . . ?
C2 C1 C7 124.3(2) . . ?
C2 C1 C6 119.1(2) . . ?
N1 C7 C1 124.05(19) . . ?
N1 C7 H7 118.0 . . ?
C1 C7 H7 118.0 . . ?
N7 C21 N8 111.4(2) . . ?
N7 C21 H21 124.3 . . ?
N8 C21 H21 124.3 . . ?
O9 C12 C11 114.6(2) . . ?
O9 C12 C13 125.6(2) . . ?
C13 C12 C11 119.8(2) . . ?
O3 C11 C12 118.0(2) . . ?
O3 C11 C10 122.83(19) . . ?
C10 C11 C12 119.1(2) . . ?
N7 C23 H23 125.3 . . ?
C22 C23 N7 109.4(2) . . ?
C22 C23 H23 125.3 . . ?
N4 C9 H9 117.6 . . ?
N4 C9 C10 124.9(2) . . ?
C10 C9 H9 117.6 . . ?
C11 C10 C9 122.2(2) . . ?
C15 C10 C11 119.6(2) . . ?
C15 C10 C9 118.2(2) . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.5(2) . . ?
C5 C6 H6 119.7 . . ?
N8 C22 H22 126.7 . . ?
C23 C22 N8 106.5(2) . . ?
C23 C22 H22 126.7 . . ?
O1 C2 C1 123.10(19) . . ?
O1 C2 C3 117.23(19) . . ?
C1 C2 C3 119.6(2) . . ?
C12 C13 H13 119.6 . . ?
C12 C13 C14 120.8(2) . . ?
C14 C13 H13 119.6 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.7(2) . . ?
C5 C4 H4 120.1 . . ?
O8 C3 C2 114.8(2) . . ?
O8 C3 C4 125.0(2) . . ?
C4 C3 C2 120.2(2) . . ?
C6 C5 C4 120.8(2) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C10 C15 H15 119.7 . . ?
C14 C15 C10 120.5(2) . . ?
C14 C15 H15 119.7 . . ?
C19A N6A H6A 125.6 . . ?
C18A N6A H6A 125.6 . . ?
C18A N6A C19A 108.9(6) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.1(2) . . ?
C15 C14 H14 119.9 . . ?
N5 C20A H20A 124.8 . . ?
N5 C20A C19A 110.5(6) . . ?
C19A C20A H20A 124.8 . . ?
N6A C19A C20A 104.8(6) . . ?
N6A C19A H19A 127.6 . . ?
C20A C19A H19A 127.6 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
N5 C18A N6A 108.9(6) . . ?
N5 C18A H18A 125.6 . . ?
N6A C18A H18A 125.6 . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O9 C17 H17A 109.5 . . ?
O9 C17 H17B 109.5 . . ?
O9 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N9 C24 C25 179.1(4) . . ?
N5 C18B H18B 124.9 . . ?
N6B C18B N5 110.2(15) . . ?
N6B C18B H18B 124.9 . . ?
C18B N6B H6B 124.7 . . ?
C18B N6B C19B 110.7(15) . . ?
C19B N6B H6B 124.7 . . ?
N6B C19B H19B 127.6 . . ?
N6B C19B C20B 104.8(16) . . ?
C20B C19B H19B 127.6 . . ?
N5 C20B H20B 123.0 . . ?
C19B C20B N5 114.0(15) . . ?
C19B C20B H20B 123.0 . . ?

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

data_5a_CH3OH
_database_code_depnum_ccdc_archive 'CCDC 1983033'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-02-10 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
"2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))di(3-methoxyphenolato))bis(methanol)tetraoxo-di-molybdenum(vi)methanol solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H22 Mo2 N4 O11, C H4 O'
_chemical_formula_sum            'C20 H26 Mo2 N4 O12'
_chemical_formula_weight         706.33

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6337(5)
_cell_length_b                   11.0989(6)
_cell_length_c                   13.1012(8)
_cell_angle_alpha                112.619(5)
_cell_angle_beta                 98.807(5)
_cell_angle_gamma                94.858(4)
_cell_volume                     1261.91(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    11688
_cell_measurement_theta_min      2.2720
_cell_measurement_theta_max      32.5680

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_F_000             708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.064
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.89554
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_temperature      150(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            28141
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.171
_diffrn_reflns_theta_max         33.040
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             8570
_reflns_number_gt                6868
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0401P)²+1.5379P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8570
_refine_ls_number_parameters     357
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0859
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
# start Validation Reply Form
_vrf_PLAT220_5a_CH3OH            
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        3.3 Ratio 
RESPONSE: Terminal methyl groups of methoxy and methanol subunits have
large Ueq due to thermal vibration.
;
_vrf_PLAT910_5a_CH3OH            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         21 Note 
RESPONSE: Beam-stop shadowing.
;
_vrf_PLAT976_5a_CH3OH            
;
PROBLEM: Check Calcd Resid. Dens.  0.61A   From O12            -0.49 eA-3  
RESPONSE: Residual density hole has no meaningful chemical interpretation.
;
# end Validation Reply Form
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.31416(2) 0.23138(2) 0.01273(2) 0.01829(6) Uani 1 1 d . . . . .
Mo2 Mo 0.59107(2) 0.22824(2) 0.38462(2) 0.01956(6) Uani 1 1 d . . . . .
O2 O 0.49938(19) 0.16590(19) 0.03902(15) 0.0205(4) Uani 1 1 d . . . . .
O1 O 0.1344(2) 0.2707(2) 0.05008(16) 0.0242(4) Uani 1 1 d . . . . .
O5 O 0.2818(2) 0.1496(2) -0.13117(15) 0.0239(4) Uani 1 1 d . . . . .
O3 O 0.73219(19) 0.1811(2) 0.47635(16) 0.0266(4) Uani 1 1 d . . . . .
O10 O 0.2265(2) 0.03373(19) 0.00678(16) 0.0232(4) Uani 1 1 d D . . . .
H10O H 0.248(4) -0.032(2) -0.038(2) 0.028 Uiso 1 1 d D U . . .
N4 N 0.7409(2) 0.1746(2) 0.26625(17) 0.0167(4) Uani 1 1 d . . . . .
O7 O 0.4340(2) 0.1944(2) 0.41983(17) 0.0303(5) Uani 1 1 d . . . . .
O9 O 0.8691(2) 0.1917(2) 0.66851(16) 0.0275(4) Uani 1 1 d . . . . .
O4 O 0.3938(2) 0.3866(2) 0.04162(18) 0.0302(4) Uani 1 1 d . . . . .
O11 O 0.5423(2) -0.0056(2) 0.27926(19) 0.0291(4) Uani 1 1 d D . . . .
H11O H 0.603(3) -0.045(3) 0.250(3) 0.035 Uiso 1 1 d D U . . .
O6 O 0.6333(2) 0.3949(2) 0.44506(17) 0.0323(5) Uani 1 1 d . . . . .
O8 O -0.1048(2) 0.3579(2) 0.02141(17) 0.0300(4) Uani 1 1 d . . . . .
N1 N 0.3668(2) 0.2655(2) 0.19796(18) 0.0180(4) Uani 1 1 d . . . . .
N2 N 0.4927(2) 0.2245(2) 0.22789(18) 0.0192(4) Uani 1 1 d . . . . .
N3 N 0.6914(2) 0.1537(2) 0.15425(17) 0.0178(4) Uani 1 1 d . . . . .
C7 C 0.2999(3) 0.3281(3) 0.2756(2) 0.0205(5) Uani 1 1 d . . . . .
H7 H 0.341089 0.346375 0.351684 0.025 Uiso 1 1 calc R U . . .
C8 C 0.5616(3) 0.1809(2) 0.1395(2) 0.0180(4) Uani 1 1 d . . . . .
C9 C 0.8710(3) 0.1572(3) 0.2903(2) 0.0194(5) Uani 1 1 d . . . . .
H9 H 0.924053 0.138690 0.232035 0.023 Uiso 1 1 calc R U . . .
C1 C 0.1652(3) 0.3723(2) 0.2534(2) 0.0199(5) Uani 1 1 d . . . . .
C11 C 0.8718(3) 0.1756(3) 0.4860(2) 0.0193(5) Uani 1 1 d . . . . .
C10 C 0.9425(3) 0.1635(3) 0.3973(2) 0.0189(5) Uani 1 1 d . . . . .
C12 C 0.9474(3) 0.1784(3) 0.5880(2) 0.0195(5) Uani 1 1 d . . . . .
C6 C 0.1086(3) 0.4438(3) 0.3475(2) 0.0229(5) Uani 1 1 d . . . . .
H6 H 0.158316 0.461780 0.421498 0.027 Uiso 1 1 calc R U . . .
C2 C 0.0897(3) 0.3442(2) 0.1446(2) 0.0202(5) Uani 1 1 d . . . . .
C15 C 1.0882(3) 0.1524(3) 0.4118(2) 0.0233(5) Uani 1 1 d . . . . .
H15 H 1.137026 0.143689 0.352150 0.028 Uiso 1 1 calc R U . . .
O12 O 0.6012(4) 0.6197(3) 0.2135(3) 0.0616(8) Uani 1 1 d D . . . .
H12O H 0.545(5) 0.575(5) 0.147(2) 0.074 Uiso 1 1 d D U . . .
C3 C -0.0413(3) 0.3900(3) 0.1302(2) 0.0220(5) Uani 1 1 d . . . . .
C14 C 1.1604(3) 0.1541(3) 0.5117(2) 0.0263(6) Uani 1 1 d . . . . .
H14 H 1.258279 0.145302 0.520145 0.032 Uiso 1 1 calc R U . . .
C13 C 1.0909(3) 0.1687(3) 0.6006(2) 0.0231(5) Uani 1 1 d . . . . .
H13 H 1.142052 0.172011 0.669887 0.028 Uiso 1 1 calc R U . . .
C5 C -0.0197(3) 0.4879(3) 0.3319(2) 0.0260(5) Uani 1 1 d . . . . .
H5 H -0.057170 0.536983 0.395801 0.031 Uiso 1 1 calc R U . . .
C18 C 0.1754(4) -0.0068(3) 0.0863(3) 0.0336(7) Uani 1 1 d . . . . .
H18A H 0.255313 0.000436 0.145530 0.050 Uiso 1 1 calc R U . . .
H18B H 0.127668 -0.098759 0.048191 0.050 Uiso 1 1 calc R U . . .
H18C H 0.107737 0.049910 0.120170 0.050 Uiso 1 1 calc R U . . .
C4 C -0.0947(3) 0.4615(3) 0.2243(2) 0.0244(5) Uani 1 1 d . . . . .
H4 H -0.182823 0.492462 0.215159 0.029 Uiso 1 1 calc R U . . .
C17 C 0.9441(3) 0.2032(3) 0.7754(2) 0.0320(6) Uani 1 1 d . . . . .
H17A H 0.986547 0.123281 0.765790 0.048 Uiso 1 1 calc R U . . .
H17B H 0.877933 0.213739 0.826972 0.048 Uiso 1 1 calc R U . . .
H17C H 1.019302 0.280327 0.806787 0.048 Uiso 1 1 calc R U . . .
C16 C -0.2317(4) 0.4110(4) 0.0035(3) 0.0460(9) Uani 1 1 d . . . . .
H16A H -0.307643 0.370317 0.027438 0.069 Uiso 1 1 calc R U . . .
H16B H -0.260258 0.392275 -0.076806 0.069 Uiso 1 1 calc R U . . .
H16C H -0.214222 0.506779 0.047703 0.069 Uiso 1 1 calc R U . . .
C20 C 0.5536(6) 0.5852(5) 0.2957(4) 0.0690(14) Uani 1 1 d . . . . .
H20A H 0.615401 0.637771 0.369466 0.104 Uiso 1 1 calc R U . . .
H20B H 0.556216 0.491055 0.276776 0.104 Uiso 1 1 calc R U . . .
H20C H 0.455887 0.602495 0.298409 0.104 Uiso 1 1 calc R U . . .
C19 C 0.4644(5) -0.0904(4) 0.3170(4) 0.0597(12) Uani 1 1 d . . . . .
H19A H 0.518716 -0.086396 0.388143 0.089 Uiso 1 1 calc R U . . .
H19B H 0.448327 -0.181358 0.259914 0.089 Uiso 1 1 calc R U . . .
H19C H 0.372600 -0.061376 0.328748 0.089 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O4 1.698(2) . ?
Mo1 O5 1.7121(18) . ?
Mo1 O1 1.9115(19) . ?
Mo1 O2 2.0136(18) . ?
Mo1 O10 2.2508(19) . ?
Mo1 N1 2.274(2) . ?
Mo2 O6 1.691(2) . ?
Mo2 O7 1.7013(19) . ?
Mo2 O3 1.9160(18) . ?
Mo2 N2 2.109(2) . ?
Mo2 N4 2.228(2) . ?
Mo2 O11 2.388(2) . ?
O2 C8 1.301(3) . ?
O1 C2 1.352(3) . ?
O3 C11 1.340(3) . ?
O10 C18 1.418(3) . ?
O10 H10O 0.808(18) . ?
N4 C9 1.294(3) . ?
N4 N3 1.392(3) . ?
O9 C12 1.359(3) . ?
O9 C17 1.427(3) . ?
O11 C19 1.430(4) . ?
O11 H11O 0.810(18) . ?
O8 C3 1.355(3) . ?
O8 C16 1.427(3) . ?
N1 C7 1.291(3) . ?
N1 N2 1.385(3) . ?
N2 C8 1.369(3) . ?
N3 C8 1.315(3) . ?
C7 C1 1.452(3) . ?
C7 H7 0.9500 . ?
C9 C10 1.437(3) . ?
C9 H9 0.9500 . ?
C1 C2 1.400(4) . ?
C1 C6 1.404(4) . ?
C11 C10 1.404(3) . ?
C11 C12 1.408(3) . ?
C10 C15 1.410(3) . ?
C12 C13 1.385(3) . ?
C6 C5 1.383(4) . ?
C6 H6 0.9500 . ?
C2 C3 1.413(3) . ?
C15 C14 1.378(4) . ?
C15 H15 0.9500 . ?
O12 C20 1.399(5) . ?
O12 H12O 0.881(19) . ?
C3 C4 1.388(4) . ?
C14 C13 1.393(4) . ?
C14 H14 0.9500 . ?
C13 H13 0.9500 . ?
C5 C4 1.389(4) . ?
C5 H5 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C4 H4 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Mo1 O5 105.77(10) . . ?
O4 Mo1 O1 99.08(10) . . ?
O5 Mo1 O1 105.78(9) . . ?
O4 Mo1 O2 93.88(9) . . ?
O5 Mo1 O2 95.05(8) . . ?
O1 Mo1 O2 151.28(8) . . ?
O4 Mo1 O10 169.71(9) . . ?
O5 Mo1 O10 83.86(8) . . ?
O1 Mo1 O10 81.37(8) . . ?
O2 Mo1 O10 81.45(7) . . ?
O4 Mo1 N1 91.71(9) . . ?
O5 Mo1 N1 159.38(9) . . ?
O1 Mo1 N1 81.55(8) . . ?
O2 Mo1 N1 72.50(7) . . ?
O10 Mo1 N1 78.16(7) . . ?
O6 Mo2 O7 105.21(11) . . ?
O6 Mo2 O3 100.54(10) . . ?
O7 Mo2 O3 105.68(9) . . ?
O6 Mo2 N2 93.59(9) . . ?
O7 Mo2 N2 93.71(9) . . ?
O3 Mo2 N2 151.87(8) . . ?
O6 Mo2 N4 101.34(9) . . ?
O7 Mo2 N4 150.10(9) . . ?
O3 Mo2 N4 82.42(8) . . ?
N2 Mo2 N4 70.95(8) . . ?
O6 Mo2 O11 172.74(9) . . ?
O7 Mo2 O11 80.42(9) . . ?
O3 Mo2 O11 82.02(9) . . ?
N2 Mo2 O11 81.35(8) . . ?
N4 Mo2 O11 72.15(7) . . ?
C8 O2 Mo1 121.47(16) . . ?
C2 O1 Mo1 135.42(16) . . ?
C11 O3 Mo2 136.39(17) . . ?
C18 O10 Mo1 133.39(17) . . ?
C18 O10 H10O 105(3) . . ?
Mo1 O10 H10O 118(2) . . ?
C9 N4 N3 115.4(2) . . ?
C9 N4 Mo2 126.31(17) . . ?
N3 N4 Mo2 118.23(14) . . ?
C12 O9 C17 116.4(2) . . ?
C19 O11 Mo2 121.4(2) . . ?
C19 O11 H11O 107(3) . . ?
Mo2 O11 H11O 120(3) . . ?
C3 O8 C16 116.6(2) . . ?
C7 N1 N2 119.2(2) . . ?
C7 N1 Mo1 126.82(17) . . ?
N2 N1 Mo1 113.60(15) . . ?
C8 N2 N1 111.4(2) . . ?
C8 N2 Mo2 118.44(16) . . ?
N1 N2 Mo2 130.13(15) . . ?
C8 N3 N4 111.0(2) . . ?
N1 C7 C1 123.9(2) . . ?
N1 C7 H7 118.1 . . ?
C1 C7 H7 118.1 . . ?
O2 C8 N3 118.7(2) . . ?
O2 C8 N2 120.4(2) . . ?
N3 C8 N2 120.8(2) . . ?
N4 C9 C10 125.8(2) . . ?
N4 C9 H9 117.1 . . ?
C10 C9 H9 117.1 . . ?
C2 C1 C6 119.7(2) . . ?
C2 C1 C7 123.3(2) . . ?
C6 C1 C7 117.0(2) . . ?
O3 C11 C10 122.1(2) . . ?
O3 C11 C12 118.1(2) . . ?
C10 C11 C12 119.7(2) . . ?
C11 C10 C15 119.0(2) . . ?
C11 C10 C9 122.6(2) . . ?
C15 C10 C9 118.4(2) . . ?
O9 C12 C13 125.0(2) . . ?
O9 C12 C11 114.9(2) . . ?
C13 C12 C11 120.1(2) . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
O1 C2 C1 122.9(2) . . ?
O1 C2 C3 117.2(2) . . ?
C1 C2 C3 119.9(2) . . ?
C14 C15 C10 120.5(2) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
C20 O12 H12O 111(3) . . ?
O8 C3 C4 125.5(2) . . ?
O8 C3 C2 115.0(2) . . ?
C4 C3 C2 119.5(2) . . ?
C15 C14 C13 120.5(2) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C12 C13 C14 120.1(2) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
O10 C18 H18A 109.5 . . ?
O10 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O10 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C3 C4 C5 120.2(2) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
O9 C17 H17A 109.5 . . ?
O9 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O9 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O12 C20 H20A 109.5 . . ?
O12 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O12 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O11 C19 H19A 109.5 . . ?
O11 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O11 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N1 N2 C8 -169.4(2) . . . . ?
Mo1 N1 N2 C8 4.3(3) . . . . ?
C7 N1 N2 Mo2 7.6(3) . . . . ?
Mo1 N1 N2 Mo2 -178.71(12) . . . . ?
C9 N4 N3 C8 -176.4(2) . . . . ?
Mo2 N4 N3 C8 5.3(3) . . . . ?
N2 N1 C7 C1 -178.2(2) . . . . ?
Mo1 N1 C7 C1 9.0(4) . . . . ?
Mo1 O2 C8 N3 -170.38(17) . . . . ?
Mo1 O2 C8 N2 9.6(3) . . . . ?
N4 N3 C8 O2 -179.7(2) . . . . ?
N4 N3 C8 N2 0.4(3) . . . . ?
N1 N2 C8 O2 -8.7(3) . . . . ?
Mo2 N2 C8 O2 173.88(18) . . . . ?
N1 N2 C8 N3 171.2(2) . . . . ?
Mo2 N2 C8 N3 -6.2(3) . . . . ?
N3 N4 C9 C10 -175.2(2) . . . . ?
Mo2 N4 C9 C10 3.0(4) . . . . ?
N1 C7 C1 C2 4.1(4) . . . . ?
N1 C7 C1 C6 -177.5(3) . . . . ?
Mo2 O3 C11 C10 -23.0(4) . . . . ?
Mo2 O3 C11 C12 158.9(2) . . . . ?
O3 C11 C10 C15 -177.2(3) . . . . ?
C12 C11 C10 C15 0.9(4) . . . . ?
O3 C11 C10 C9 0.6(4) . . . . ?
C12 C11 C10 C9 178.7(2) . . . . ?
N4 C9 C10 C11 7.2(4) . . . . ?
N4 C9 C10 C15 -175.0(3) . . . . ?
C17 O9 C12 C13 3.4(4) . . . . ?
C17 O9 C12 C11 -176.3(2) . . . . ?
O3 C11 C12 O9 -2.4(4) . . . . ?
C10 C11 C12 O9 179.4(2) . . . . ?
O3 C11 C12 C13 177.9(2) . . . . ?
C10 C11 C12 C13 -0.3(4) . . . . ?
C2 C1 C6 C5 -1.2(4) . . . . ?
C7 C1 C6 C5 -179.6(2) . . . . ?
Mo1 O1 C2 C1 -26.0(4) . . . . ?
Mo1 O1 C2 C3 155.8(2) . . . . ?
C6 C1 C2 O1 -176.9(2) . . . . ?
C7 C1 C2 O1 1.4(4) . . . . ?
C6 C1 C2 C3 1.2(4) . . . . ?
C7 C1 C2 C3 179.5(2) . . . . ?
C11 C10 C15 C14 -0.3(4) . . . . ?
C9 C10 C15 C14 -178.2(3) . . . . ?
C16 O8 C3 C4 4.9(4) . . . . ?
C16 O8 C3 C2 -175.3(3) . . . . ?
O1 C2 C3 O8 -2.3(4) . . . . ?
C1 C2 C3 O8 179.6(2) . . . . ?
O1 C2 C3 C4 177.5(2) . . . . ?
C1 C2 C3 C4 -0.6(4) . . . . ?
C10 C15 C14 C13 -0.9(4) . . . . ?
O9 C12 C13 C14 179.4(3) . . . . ?
C11 C12 C13 C14 -1.0(4) . . . . ?
C15 C14 C13 C12 1.6(4) . . . . ?
C1 C6 C5 C4 0.6(4) . . . . ?
O8 C3 C4 C5 179.8(3) . . . . ?
C2 C3 C4 C5 0.1(4) . . . . ?
C6 C5 C4 C3 -0.1(4) . . . . ?

_refine_diff_density_max         1.559
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.119

####################################################################### 
# 
# 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_1b_CH3CN
_database_code_depnum_ccdc_archive 'CCDC 1983031'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-02-10 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        
"2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))diphenolato)bis(imidazol)tetraoxo-di-molybdenum(vi)) acetonitrile solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H18 Mo2 N8 O7, C2 H3 N'
_chemical_formula_sum            'C23 H21 Mo2 N9 O7'
_chemical_formula_weight         727.37

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.6920(4)
_cell_length_b                   26.7430(8)
_cell_length_c                   11.6059(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.219(4)
_cell_angle_gamma                90
_cell_volume                     2681.92(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4532
_cell_measurement_theta_min      4.5140
_cell_measurement_theta_max      27.9140

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_F_000             1448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.997
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.93856
_exptl_absorpt_correction_T_max  1.00000
_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.
;
# start Validation Reply Form
_vrf_PLAT906_1b_CH3CN            
;
PROBLEM: Large K Value in the Analysis of Variance ......      4.498 Check 
RESPONSE: The K value is large only for weak reflections with Fc/Fcmax 
lower than 0.013.
;
_vrf_PLAT910_1b_CH3CN            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         22 Note 
RESPONSE: Beam-stop shadowing due to large unit cell.
;
_diffrn_ambient_temperature      150(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            22137
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.132
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6465
_reflns_number_gt                4455
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0343P)²+0.3084P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6465
_refine_ls_number_parameters     377
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.0977
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.71123(4) 0.66050(2) 0.73766(3) 0.01742(10) Uani 1 1 d . . . . .
Mo2 Mo 0.70778(4) 0.46739(2) 0.65561(3) 0.01751(10) Uani 1 1 d . . . . .
O2 O 0.6749(3) 0.60370(9) 0.8429(2) 0.0200(6) Uani 1 1 d . . . . .
O3 O 0.7439(3) 0.39933(9) 0.7102(2) 0.0214(7) Uani 1 1 d . . . . .
O5 O 0.6572(3) 0.70625(9) 0.8270(2) 0.0251(7) Uani 1 1 d . . . . .
O1 O 0.6943(3) 0.68985(9) 0.5862(2) 0.0211(6) Uani 1 1 d . . . . .
O6 O 0.5215(3) 0.45964(10) 0.5980(2) 0.0270(7) Uani 1 1 d . . . . .
O7 O 0.8143(4) 0.47384(9) 0.5413(2) 0.0253(7) Uani 1 1 d . . . . .
O4 O 0.9090(3) 0.65957(9) 0.7576(2) 0.0239(7) Uani 1 1 d . . . . .
N4 N 0.6362(4) 0.47550(11) 0.8347(3) 0.0188(8) Uani 1 1 d . . . . .
N2 N 0.6913(4) 0.54512(11) 0.6971(3) 0.0176(7) Uani 1 1 d . . . . .
N1 N 0.7198(4) 0.58823(11) 0.6348(3) 0.0155(7) Uani 1 1 d . . . . .
N3 N 0.6401(4) 0.52294(11) 0.8860(3) 0.0169(7) Uani 1 1 d . . . . .
N7 N 0.9499(4) 0.48197(12) 0.7655(3) 0.0207(8) Uani 1 1 d . . . . .
N5 N 0.4529(4) 0.64721(12) 0.6823(3) 0.0224(8) Uani 1 1 d . . . . .
N8 N 1.1556(4) 0.48046(13) 0.8945(3) 0.0272(9) Uani 1 1 d D . . . .
H8N H 1.218(5) 0.4749(14) 0.957(3) 0.033 Uiso 1 1 d D U . . .
C8 C 0.6684(5) 0.55679(14) 0.8089(3) 0.0185(9) Uani 1 1 d . . . . .
C11 C 0.6506(5) 0.36993(14) 0.7659(3) 0.0195(9) Uani 1 1 d . . . . .
N6 N 0.2036(4) 0.64296(16) 0.6926(4) 0.0354(10) Uani 1 1 d D . . . .
H6N H 0.119(3) 0.6425(18) 0.726(4) 0.042 Uiso 1 1 d D U . . .
C19 C 1.0102(5) 0.46497(15) 0.8676(3) 0.0228(10) Uani 1 1 d . . . . .
H19 H 0.956366 0.444166 0.916100 0.027 Uiso 1 1 calc R U . . .
C9 C 0.5769(5) 0.44021(14) 0.8917(3) 0.0204(9) Uani 1 1 d . . . . .
H9 H 0.537326 0.448502 0.962400 0.025 Uiso 1 1 calc R U . . .
C2 C 0.7690(5) 0.67798(14) 0.4930(3) 0.0195(9) Uani 1 1 d . . . . .
C1 C 0.7930(5) 0.62749(14) 0.4626(3) 0.0194(9) Uani 1 1 d . . . . .
C12 C 0.6436(5) 0.31920(15) 0.7396(3) 0.0241(10) Uani 1 1 d . . . . .
H12 H 0.701539 0.306207 0.681464 0.029 Uiso 1 1 calc R U . . .
C10 C 0.5676(5) 0.38875(14) 0.8535(3) 0.0193(9) Uani 1 1 d . . . . .
C6 C 0.8629(5) 0.61857(16) 0.3612(4) 0.0255(10) Uani 1 1 d . . . . .
H6 H 0.876936 0.585008 0.337600 0.031 Uiso 1 1 calc R U . . .
C7 C 0.7546(5) 0.58474(14) 0.5305(3) 0.0195(9) Uani 1 1 d . . . . .
H7 H 0.755297 0.552514 0.496065 0.023 Uiso 1 1 calc R U . . .
C3 C 0.8176(5) 0.71658(15) 0.4248(4) 0.0244(10) Uani 1 1 d . . . . .
H3 H 0.800577 0.750371 0.445280 0.029 Uiso 1 1 calc R U . . .
C13 C 0.5523(5) 0.28762(15) 0.7978(4) 0.0254(10) Uani 1 1 d . . . . .
H13 H 0.546696 0.253148 0.778022 0.030 Uiso 1 1 calc R U . . .
C4 C 0.8898(5) 0.70606(16) 0.3282(4) 0.0281(11) Uani 1 1 d . . . . .
H4 H 0.924995 0.732765 0.283833 0.034 Uiso 1 1 calc R U . . .
C16 C 0.3430(5) 0.64624(15) 0.7517(4) 0.0270(10) Uani 1 1 d . . . . .
H16 H 0.360997 0.647695 0.833860 0.032 Uiso 1 1 calc R U . . .
C21 C 1.0678(5) 0.51025(15) 0.7254(4) 0.0269(10) Uani 1 1 d . . . . .
H21 H 1.060935 0.527381 0.653351 0.032 Uiso 1 1 calc R U . . .
N9 N 1.1268(6) 0.63278(18) 0.9783(4) 0.0529(14) Uani 1 1 d . . . . .
C20 C 1.1941(5) 0.50956(15) 0.8053(4) 0.0279(11) Uani 1 1 d . . . . .
H20 H 1.290022 0.526012 0.800136 0.034 Uiso 1 1 calc R U . . .
C14 C 0.4687(5) 0.30548(15) 0.8848(4) 0.0272(10) Uani 1 1 d . . . . .
H14 H 0.406814 0.283497 0.924694 0.033 Uiso 1 1 calc R U . . .
C17 C 0.2230(6) 0.64159(18) 0.5781(4) 0.0377(13) Uani 1 1 d . . . . .
H17 H 0.144149 0.639381 0.514859 0.045 Uiso 1 1 calc R U . . .
C5 C 0.9123(5) 0.65713(15) 0.2942(4) 0.0292(11) Uani 1 1 d . . . . .
H5 H 0.960630 0.650146 0.226325 0.035 Uiso 1 1 calc R U . . .
C15 C 0.4772(5) 0.35588(15) 0.9124(4) 0.0259(10) Uani 1 1 d . . . . .
H15 H 0.421002 0.368416 0.971953 0.031 Uiso 1 1 calc R U . . .
C18 C 0.3766(6) 0.64398(17) 0.5722(4) 0.0341(12) Uani 1 1 d . . . . .
H18 H 0.425008 0.643520 0.502687 0.041 Uiso 1 1 calc R U . . .
C22 C 1.0602(6) 0.6679(2) 0.9947(4) 0.0381(13) Uani 1 1 d . . . . .
C23 C 0.9749(6) 0.71348(18) 1.0140(4) 0.0459(15) Uani 1 1 d . . . . .
H23A H 0.968866 0.734408 0.944385 0.069 Uiso 1 1 calc R U . . .
H23B H 1.028318 0.731851 1.079668 0.069 Uiso 1 1 calc R U . . .
H23C H 0.870152 0.704852 1.031108 0.069 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O5 1.702(3) . ?
Mo1 O4 1.710(3) . ?
Mo1 O1 1.916(3) . ?
Mo1 O2 1.996(3) . ?
Mo1 N1 2.277(3) . ?
Mo1 N5 2.295(3) . ?
Mo2 O6 1.696(3) . ?
Mo2 O7 1.707(3) . ?
Mo2 O3 1.941(2) . ?
Mo2 N2 2.142(3) . ?
Mo2 N4 2.244(3) . ?
Mo2 N7 2.372(3) . ?
O2 C8 1.315(4) . ?
O3 C11 1.345(5) . ?
O1 C2 1.358(5) . ?
N4 C9 1.291(5) . ?
N4 N3 1.401(4) . ?
N2 C8 1.371(5) . ?
N2 N1 1.397(4) . ?
N1 C7 1.283(5) . ?
N3 C8 1.314(5) . ?
N7 C19 1.323(5) . ?
N7 C21 1.394(5) . ?
N5 C16 1.315(5) . ?
N5 C18 1.377(5) . ?
N8 C19 1.334(5) . ?
N8 C20 1.365(6) . ?
N8 H8N 0.873(19) . ?
C11 C12 1.391(5) . ?
C11 C10 1.402(6) . ?
N6 C16 1.329(5) . ?
N6 C17 1.358(6) . ?
N6 H6N 0.865(19) . ?
C19 H19 0.9500 . ?
C9 C10 1.445(5) . ?
C9 H9 0.9500 . ?
C2 C3 1.394(6) . ?
C2 C1 1.417(5) . ?
C1 C6 1.402(6) . ?
C1 C7 1.448(5) . ?
C12 C13 1.384(6) . ?
C12 H12 0.9500 . ?
C10 C15 1.405(6) . ?
C6 C5 1.388(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C3 C4 1.372(6) . ?
C3 H3 0.9500 . ?
C13 C14 1.391(6) . ?
C13 H13 0.9500 . ?
C4 C5 1.387(6) . ?
C4 H4 0.9500 . ?
C16 H16 0.9500 . ?
C21 C20 1.358(6) . ?
C21 H21 0.9500 . ?
N9 C22 1.130(6) . ?
C20 H20 0.9500 . ?
C14 C15 1.385(5) . ?
C14 H14 0.9500 . ?
C17 C18 1.345(6) . ?
C17 H17 0.9500 . ?
C5 H5 0.9500 . ?
C15 H15 0.9500 . ?
C18 H18 0.9500 . ?
C22 C23 1.457(7) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Mo1 O4 105.53(13) . . ?
O5 Mo1 O1 105.38(12) . . ?
O4 Mo1 O1 96.10(13) . . ?
O5 Mo1 O2 95.84(12) . . ?
O4 Mo1 O2 97.44(12) . . ?
O1 Mo1 O2 150.68(11) . . ?
O5 Mo1 N1 162.97(13) . . ?
O4 Mo1 N1 88.23(12) . . ?
O1 Mo1 N1 82.55(11) . . ?
O2 Mo1 N1 72.03(11) . . ?
O5 Mo1 N5 87.46(13) . . ?
O4 Mo1 N5 167.01(12) . . ?
O1 Mo1 N5 80.28(12) . . ?
O2 Mo1 N5 80.72(12) . . ?
N1 Mo1 N5 78.96(12) . . ?
O6 Mo2 O7 106.31(14) . . ?
O6 Mo2 O3 97.33(12) . . ?
O7 Mo2 O3 105.43(13) . . ?
O6 Mo2 N2 97.06(13) . . ?
O7 Mo2 N2 97.57(13) . . ?
O3 Mo2 N2 148.10(12) . . ?
O6 Mo2 N4 91.61(13) . . ?
O7 Mo2 N4 159.82(13) . . ?
O3 Mo2 N4 80.78(11) . . ?
N2 Mo2 N4 70.49(12) . . ?
O6 Mo2 N7 170.23(14) . . ?
O7 Mo2 N7 82.94(13) . . ?
O3 Mo2 N7 82.88(11) . . ?
N2 Mo2 N7 78.27(11) . . ?
N4 Mo2 N7 78.76(13) . . ?
C8 O2 Mo1 123.2(3) . . ?
C11 O3 Mo2 128.3(3) . . ?
C2 O1 Mo1 129.7(2) . . ?
C9 N4 N3 115.9(3) . . ?
C9 N4 Mo2 124.7(3) . . ?
N3 N4 Mo2 119.0(2) . . ?
C8 N2 N1 110.7(3) . . ?
C8 N2 Mo2 117.0(3) . . ?
N1 N2 Mo2 131.7(2) . . ?
C7 N1 N2 120.1(3) . . ?
C7 N1 Mo1 125.5(3) . . ?
N2 N1 Mo1 114.3(2) . . ?
C8 N3 N4 109.4(3) . . ?
C19 N7 C21 104.5(4) . . ?
C19 N7 Mo2 131.9(3) . . ?
C21 N7 Mo2 123.5(3) . . ?
C16 N5 C18 105.0(4) . . ?
C16 N5 Mo1 125.8(3) . . ?
C18 N5 Mo1 128.9(3) . . ?
C19 N8 C20 107.7(3) . . ?
C19 N8 H8N 129(3) . . ?
C20 N8 H8N 123(3) . . ?
N3 C8 O2 117.3(3) . . ?
N3 C8 N2 123.0(3) . . ?
O2 C8 N2 119.7(4) . . ?
O3 C11 C12 118.6(4) . . ?
O3 C11 C10 121.6(3) . . ?
C12 C11 C10 119.7(4) . . ?
C16 N6 C17 107.7(4) . . ?
C16 N6 H6N 123(3) . . ?
C17 N6 H6N 130(3) . . ?
N7 C19 N8 112.1(4) . . ?
N7 C19 H19 124.0 . . ?
N8 C19 H19 124.0 . . ?
N4 C9 C10 123.4(4) . . ?
N4 C9 H9 118.3 . . ?
C10 C9 H9 118.3 . . ?
O1 C2 C3 118.7(4) . . ?
O1 C2 C1 121.1(4) . . ?
C3 C2 C1 120.2(4) . . ?
C6 C1 C2 117.4(4) . . ?
C6 C1 C7 117.9(4) . . ?
C2 C1 C7 124.7(4) . . ?
C13 C12 C11 120.1(4) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C11 C10 C15 119.1(4) . . ?
C11 C10 C9 123.2(4) . . ?
C15 C10 C9 117.5(4) . . ?
C5 C6 C1 122.2(4) . . ?
C5 C6 H6 118.9 . . ?
C1 C6 H6 118.9 . . ?
N1 C7 C1 123.2(4) . . ?
N1 C7 H7 118.4 . . ?
C1 C7 H7 118.4 . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C12 C13 C14 121.1(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C3 C4 C5 121.2(4) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
N5 C16 N6 111.5(4) . . ?
N5 C16 H16 124.2 . . ?
N6 C16 H16 124.2 . . ?
C20 C21 N7 109.5(4) . . ?
C20 C21 H21 125.2 . . ?
N7 C21 H21 125.2 . . ?
C21 C20 N8 106.2(4) . . ?
C21 C20 H20 126.9 . . ?
N8 C20 H20 126.9 . . ?
C15 C14 C13 118.8(4) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C18 C17 N6 106.1(4) . . ?
C18 C17 H17 127.0 . . ?
N6 C17 H17 127.0 . . ?
C4 C5 C6 118.7(4) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C14 C15 C10 121.0(4) . . ?
C14 C15 H15 119.5 . . ?
C10 C15 H15 119.5 . . ?
C17 C18 N5 109.7(4) . . ?
C17 C18 H18 125.1 . . ?
N5 C18 H18 125.1 . . ?
N9 C22 C23 179.1(6) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 N2 N1 C7 175.2(4) . . . . ?
Mo2 N2 N1 C7 4.6(5) . . . . ?
C8 N2 N1 Mo1 -1.6(4) . . . . ?
Mo2 N2 N1 Mo1 -172.26(17) . . . . ?
C9 N4 N3 C8 -165.4(3) . . . . ?
Mo2 N4 N3 C8 8.4(4) . . . . ?
N4 N3 C8 O2 179.6(3) . . . . ?
N4 N3 C8 N2 -0.7(5) . . . . ?
Mo1 O2 C8 N3 -178.4(3) . . . . ?
Mo1 O2 C8 N2 1.8(5) . . . . ?
N1 N2 C8 N3 -179.6(3) . . . . ?
Mo2 N2 C8 N3 -7.5(5) . . . . ?
N1 N2 C8 O2 0.1(5) . . . . ?
Mo2 N2 C8 O2 172.3(3) . . . . ?
Mo2 O3 C11 C12 142.2(3) . . . . ?
Mo2 O3 C11 C10 -41.2(5) . . . . ?
C21 N7 C19 N8 0.2(5) . . . . ?
Mo2 N7 C19 N8 176.1(3) . . . . ?
C20 N8 C19 N7 0.2(5) . . . . ?
N3 N4 C9 C10 -178.1(3) . . . . ?
Mo2 N4 C9 C10 8.5(6) . . . . ?
Mo1 O1 C2 C3 -140.4(3) . . . . ?
Mo1 O1 C2 C1 41.7(5) . . . . ?
O1 C2 C1 C6 176.3(4) . . . . ?
C3 C2 C1 C6 -1.6(6) . . . . ?
O1 C2 C1 C7 -5.6(6) . . . . ?
C3 C2 C1 C7 176.6(4) . . . . ?
O3 C11 C12 C13 178.1(3) . . . . ?
C10 C11 C12 C13 1.4(6) . . . . ?
O3 C11 C10 C15 -177.2(3) . . . . ?
C12 C11 C10 C15 -0.7(6) . . . . ?
O3 C11 C10 C9 -0.9(6) . . . . ?
C12 C11 C10 C9 175.6(4) . . . . ?
N4 C9 C10 C11 14.4(6) . . . . ?
N4 C9 C10 C15 -169.2(4) . . . . ?
C2 C1 C6 C5 2.2(6) . . . . ?
C7 C1 C6 C5 -176.1(4) . . . . ?
N2 N1 C7 C1 -176.9(3) . . . . ?
Mo1 N1 C7 C1 -0.4(6) . . . . ?
C6 C1 C7 N1 165.6(4) . . . . ?
C2 C1 C7 N1 -12.5(6) . . . . ?
O1 C2 C3 C4 -178.3(4) . . . . ?
C1 C2 C3 C4 -0.4(6) . . . . ?
C11 C12 C13 C14 -1.3(6) . . . . ?
C2 C3 C4 C5 1.8(6) . . . . ?
C18 N5 C16 N6 -0.4(5) . . . . ?
Mo1 N5 C16 N6 173.4(3) . . . . ?
C17 N6 C16 N5 0.2(5) . . . . ?
C19 N7 C21 C20 -0.5(5) . . . . ?
Mo2 N7 C21 C20 -176.8(3) . . . . ?
N7 C21 C20 N8 0.6(5) . . . . ?
C19 N8 C20 C21 -0.5(5) . . . . ?
C12 C13 C14 C15 0.4(6) . . . . ?
C16 N6 C17 C18 0.2(6) . . . . ?
C3 C4 C5 C6 -1.2(6) . . . . ?
C1 C6 C5 C4 -0.8(6) . . . . ?
C13 C14 C15 C10 0.4(6) . . . . ?
C11 C10 C15 C14 -0.2(6) . . . . ?
C9 C10 C15 C14 -176.7(4) . . . . ?
N6 C17 C18 N5 -0.4(5) . . . . ?
C16 N5 C18 C17 0.5(5) . . . . ?
Mo1 N5 C18 C17 -173.1(3) . . . . ?

_refine_diff_density_max         0.759
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.140

####################################################################### 
# 
# 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_H4L6
_database_code_depnum_ccdc_archive 'CCDC 1983037'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;

_audit_update_record             
;
2020-02-10 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;

_audit_creation_date             2019-07-16
_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        
1,3-bis[(E)-[(2-hydroxy-4-methoxyphenyl)methylidene]amino]urea
_chemical_formula_moiety         'C17 H18 N4 O5'
_chemical_formula_sum            'C17 H18 N4 O5'
_chemical_formula_weight         358.35
_chemical_melting_point          ?
# start Validation Reply Form
_vrf_PLAT906_H4L6                
;
PROBLEM: Large K Value in the Analysis of Variance ......     43.960 Check 
RESPONSE: The K value is large (>1.5) only for weak reflections with Fc/Fcmax 
lower than 0.01.
;
_vrf_PLAT910_H4L6                
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).          6 Note  
RESPONSE: Reflections shadowed by beam-stop.
;
_vrf_PLAT911_H4L6                
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
RESPONSE: Two low angle reflections ([-1 1 3] and [1 1 4]) are omitted due 
to beam-stop shadowing.
;
_vrf_PLAT978_H4L6                
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: Low quality of high resolution data (I/sig(I)<3 for d<1.17 angstroms).
;
# end Validation Reply Form
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'
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           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                   9.3305(8)
_cell_length_b                   10.2881(7)
_cell_length_c                   18.0461(16)
_cell_angle_alpha                90
_cell_angle_beta                 104.692(8)
_cell_angle_gamma                90
_cell_volume                     1675.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    922
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.7390
_cell_measurement_theta_min      4.5700
_shelx_estimated_absorpt_T_max   0.995
_shelx_estimated_absorpt_T_min   0.979
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_preparation       
'Reaction between carbohydrazide and 4-methoxysalicylaldehide in methanol.'
_exptl_crystal_recrystallization_method 'crystallized from methanol'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7739
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.987
_diffrn_reflns_theta_min         4.130
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    5.00   88.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   37.0000   30.0000 83

#__ type_ start__ end____ width___ exp.time_
  2 omega  -38.00   10.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -57.0000 -150.0000 48

#__ type_ start__ end____ width___ exp.time_
  3 omega   33.00   92.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432 -179.0000 -120.0000 59

#__ type_ start__ end____ width___ exp.time_
  4 omega    7.00   43.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   57.0000   90.0000 36

#__ type_ start__ end____ width___ exp.time_
  5 omega    7.00   87.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   57.0000  -90.0000 80

#__ type_ start__ end____ width___ exp.time_
  6 omega   35.00   89.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  179.0000    0.0000 54

#__ type_ start__ end____ width___ exp.time_
  7 omega  -10.00   92.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       22.3432    0.0000  -30.0000 102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0627765000
_diffrn_orient_matrix_UB_12      -0.0352947000
_diffrn_orient_matrix_UB_13      -0.0206153000
_diffrn_orient_matrix_UB_21      0.0471391000
_diffrn_orient_matrix_UB_22      -0.0493886000
_diffrn_orient_matrix_UB_23      -0.0078486000
_diffrn_orient_matrix_UB_31      -0.0033814000
_diffrn_orient_matrix_UB_32      -0.0326777000
_diffrn_orient_matrix_UB_33      0.0341320000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                995
_reflns_number_total             1821
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXD (Sheldrick, 2008)'
_refine_diff_density_max         0.142
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1821
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.0664
_refine_ls_restrained_S_all      1.052
_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)+(0.0317P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1242
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-H2
 0.86 with sigma of 0.02
 O1-H1
 0.82 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C6(H6), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 1.4255(2) 0.11747(17) 0.44052(10) 0.0661(6) Uani 1 1 d . . . . .
O1 O 0.9157(2) 0.07695(15) 0.33566(11) 0.0584(6) Uani 1 1 d D . . . .
H1 H 0.840(2) 0.124(2) 0.3219(15) 0.070 Uiso 1 1 d DR . . . .
O2 O 0.500000 0.1492(2) 0.250000 0.0541(7) Uani 1 2 d S T P . .
N1 N 0.7580(2) 0.28374(18) 0.30178(11) 0.0436(5) Uani 1 1 d . . . . .
N2 N 0.6244(2) 0.34307(19) 0.27240(12) 0.0488(6) Uani 1 1 d D . . . .
H2 H 0.617(3) 0.4195(17) 0.2533(12) 0.059 Uiso 1 1 d DR . . . .
C5 C 1.2843(3) 0.3164(2) 0.40119(13) 0.0482(7) Uani 1 1 d . . . . .
H5 H 1.367450 0.369429 0.415418 0.058 Uiso 1 1 calc R . . . .
C7 C 0.8760(3) 0.3533(2) 0.31582(13) 0.0447(6) Uani 1 1 d . U . . .
H7 H 0.869608 0.441909 0.305250 0.054 Uiso 1 1 calc R . . . .
C6 C 1.1460(3) 0.3691(2) 0.36996(13) 0.0478(7) Uani 1 1 d . . . . .
H6 H 1.138000 0.458712 0.363340 0.057 Uiso 1 1 calc R . . . .
C8 C 0.500000 0.2672(3) 0.250000 0.0431(9) Uani 1 2 d S T P . .
C1 C 1.0185(3) 0.2942(2) 0.34800(13) 0.0384(6) Uani 1 1 d . U . . .
C3 C 1.1713(3) 0.1054(2) 0.38887(13) 0.0492(7) Uani 1 1 d . . . . .
H3 H 1.179938 0.015808 0.395550 0.059 Uiso 1 1 calc R . . . .
C2 C 1.0350(3) 0.1588(2) 0.35739(13) 0.0414(6) Uani 1 1 d . . . . .
C9 C 1.5587(3) 0.1900(3) 0.46450(16) 0.0681(9) Uani 1 1 d . . . . .
H9A H 1.640008 0.131919 0.483954 0.102 Uiso 1 1 calc R . . . .
H9B H 1.575788 0.237465 0.421735 0.102 Uiso 1 1 calc R . . . .
H9C H 1.550261 0.249821 0.504026 0.102 Uiso 1 1 calc R . . . .
C4 C 1.2965(3) 0.1827(2) 0.41092(13) 0.0458(7) 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
O3 C9 1.420(3) . ?
O3 C4 1.363(3) . ?
O1 H1 0.840(17) . ?
O1 C2 1.372(3) . ?
O2 C8 1.214(4) . ?
N1 N2 1.369(3) . ?
N1 C7 1.283(3) . ?
N2 H2 0.854(15) . ?
N2 C8 1.372(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.381(3) . ?
C5 C4 1.388(3) . ?
C7 H7 0.9300 . ?
C7 C1 1.444(3) . ?
C6 H6 0.9300 . ?
C6 C1 1.388(3) . ?
C1 C2 1.407(3) . ?
C3 H3 0.9300 . ?
C3 C2 1.369(3) . ?
C3 C4 1.386(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?

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
C4 O3 C9 118.6(2) . . ?
C2 O1 H1 107(2) . . ?
C7 N1 N2 118.6(2) . . ?
N1 N2 H2 122.9(17) . . ?
N1 N2 C8 118.7(2) . . ?
C8 N2 H2 115.2(17) . . ?
C6 C5 H5 120.7 . . ?
C6 C5 C4 118.6(2) . . ?
C4 C5 H5 120.7 . . ?
N1 C7 H7 120.0 . . ?
N1 C7 C1 120.1(2) . . ?
C1 C7 H7 120.0 . . ?
C5 C6 H6 118.6 . . ?
C5 C6 C1 122.9(2) . . ?
C1 C6 H6 118.6 . . ?
O2 C8 N2 124.68(15) . 2_655 ?
O2 C8 N2 124.68(15) . . ?
N2 C8 N2 110.6(3) . 2_655 ?
C6 C1 C7 121.1(2) . . ?
C6 C1 C2 117.1(2) . . ?
C2 C1 C7 121.8(2) . . ?
C2 C3 H3 119.5 . . ?
C2 C3 C4 121.0(2) . . ?
C4 C3 H3 119.5 . . ?
O1 C2 C1 121.1(2) . . ?
C3 C2 O1 118.2(2) . . ?
C3 C2 C1 120.6(2) . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C4 C5 125.0(2) . . ?
O3 C4 C3 115.3(2) . . ?
C3 C4 C5 119.7(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 N2 C8 O2 -4.6(2) . . . . ?
N1 N2 C8 N2 175.4(2) . . . 2_655 ?
N1 C7 C1 C6 -174.3(2) . . . . ?
N1 C7 C1 C2 6.8(3) . . . . ?
N2 N1 C7 C1 178.98(19) . . . . ?
C5 C6 C1 C7 179.8(2) . . . . ?
C5 C6 C1 C2 -1.2(3) . . . . ?
C7 N1 N2 C8 173.37(18) . . . . ?
C7 C1 C2 O1 0.5(3) . . . . ?
C7 C1 C2 C3 -179.3(2) . . . . ?
C6 C5 C4 O3 179.6(2) . . . . ?
C6 C5 C4 C3 0.4(3) . . . . ?
C6 C1 C2 O1 -178.5(2) . . . . ?
C6 C1 C2 C3 1.7(3) . . . . ?
C2 C3 C4 O3 -179.2(2) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C9 O3 C4 C5 0.8(3) . . . . ?
C9 O3 C4 C3 -179.9(2) . . . . ?
C4 C5 C6 C1 0.2(4) . . . . ?
C4 C3 C2 O1 179.0(2) . . . . ?
C4 C3 C2 C1 -1.2(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'mounted on glass fiber with shellac glue'
_olex2_submission_special_instructions 'No special instructions were received'



_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_6b_2CH3CN
_database_code_depnum_ccdc_archive 'CCDC 1983036'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-02-10 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_audit_creation_date             2019-07-21
_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        
"2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))di(4-methoxyphenolato))bis(imidazol)tetraoxo-di-molybdenum(vi)acetonitrile solvate"
_chemical_formula_moiety         'C23 H22 Mo2 N8 O9, 2(C2 H3 N)'
_chemical_formula_sum            'C27 H28 Mo2 N10 O9'
_chemical_formula_weight         828.47
_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 0.0033 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                   8.6152(4)
_cell_length_b                   13.1856(7)
_cell_length_c                   15.5721(8)
_cell_angle_alpha                75.325(4)
_cell_angle_beta                 74.393(4)
_cell_angle_gamma                85.158(4)
_cell_volume                     1647.89(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6967
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.6180
_cell_measurement_theta_min      2.3640
_shelx_estimated_absorpt_T_max   0.922
_shelx_estimated_absorpt_T_min   0.789
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82403
_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            'dark red'
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18887
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.499
_diffrn_reflns_theta_min         2.362
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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                6740
_reflns_number_total             9170
_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.
;
# start Validation Reply Form
_vrf_PLAT244_6b_2CH3CN           
;
PROBLEM: Low    'Solvent' Ueq as Compared to Neighbors of        C26 Check 
RESPONSE: C26 is the central carbon atom of acetonitrile solvent molecule.
;
_vrf_PLAT906_6b_2CH3CN           
;
PROBLEM: Large K Value in the Analysis of Variance ......      5.644 Check 
RESPONSE: The K value is large only for weak reflections with Fc/Fcmax 
lower than 0.013
;
_vrf_PLAT911_6b_2CH3CN           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          5 Report
RESPONSE: Five low angle reflections ([1 0 0], [1 0 1], [1 1 1], [1 2 2] 
and [-1 2 2]) were omitted due to beam-stop shadowing.
;
_vrf_PLAT934_6b_2CH3CN           
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          1 Check 
RESPONSE: Overlap with reflection from another crystal domain.
;
_vrf_PLAT975_6b_2CH3CN           
;
PROBLEM: Check Calcd Resid. Dens.  0.72A   From O5              0.46 eA-3  
RESPONSE: Residual density peak has no meaningful chemical interpretation.
;
# end Validation Reply Form
_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-2018 (Sheldrick, 2018)'
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         9170
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.021
_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)+(0.0391P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1001
_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
 H8-N8
 0.88 with sigma of 0.02
 H6-N6
 0.88 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C26, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C18(H18), C21(H21), C12(H12), C23(H23), C20(H20), C7(H7), C19(H19),
 C22(H22), C15(H15), C3(H3), C6(H6A), C14(H14), C5(H5)
4.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.71482(3) 0.27043(2) 0.18823(2) 0.02034(8) Uani 1 1 d . . . . .
Mo2 Mo 0.48303(3) 0.63382(2) 0.24284(2) 0.01718(7) Uani 1 1 d . . . . .
O2 O 0.6759(3) 0.40064(17) 0.09623(14) 0.0216(5) Uani 1 1 d . . . . .
O3 O 0.4713(3) 0.78661(17) 0.20692(15) 0.0223(5) Uani 1 1 d . . . . .
O1 O 0.7596(3) 0.20168(18) 0.30338(15) 0.0260(5) Uani 1 1 d . . . . .
O5 O 0.8459(3) 0.21259(18) 0.11062(15) 0.0268(5) Uani 1 1 d . . . . .
O7 O 0.5266(3) 0.60126(18) 0.34719(15) 0.0233(5) Uani 1 1 d . . . . .
O6 O 0.2795(3) 0.61443(19) 0.26612(15) 0.0271(5) Uani 1 1 d . . . . .
N2 N 0.5649(3) 0.4885(2) 0.21154(17) 0.0177(5) Uani 1 1 d . . . . .
O9 O 0.1919(3) 1.1060(2) 0.11210(17) 0.0359(6) Uani 1 1 d . . . . .
N7 N 0.7562(3) 0.6709(2) 0.18897(18) 0.0199(6) Uani 1 1 d . . . . .
O4 O 0.5328(3) 0.2156(2) 0.20632(17) 0.0338(6) Uani 1 1 d . . . . .
N5 N 0.9364(3) 0.3690(2) 0.17926(18) 0.0216(6) Uani 1 1 d . . . . .
N4 N 0.5196(3) 0.6508(2) 0.09176(17) 0.0188(6) Uani 1 1 d . . . . .
O8 O 0.6268(4) 0.0056(2) 0.61535(16) 0.0382(7) Uani 1 1 d . . . . .
N3 N 0.5898(3) 0.5669(2) 0.05472(18) 0.0209(6) Uani 1 1 d . . . . .
N1 N 0.5951(3) 0.3921(2) 0.26748(17) 0.0184(5) Uani 1 1 d . . . . .
N6 N 1.1837(4) 0.4259(3) 0.1196(2) 0.0310(7) Uani 1 1 d D . . . .
H6 H 1.269(3) 0.446(3) 0.083(2) 0.037 Uiso 1 1 d DR . . . .
C8 C 0.6106(4) 0.4866(3) 0.1197(2) 0.0194(7) Uani 1 1 d . . . . .
N8 N 1.0067(4) 0.6740(3) 0.1937(2) 0.0363(8) Uani 1 1 d D . . . .
H8 H 1.091(3) 0.668(3) 0.215(3) 0.044 Uiso 1 1 d DR . . . .
C9 C 0.4795(4) 0.7317(3) 0.0353(2) 0.0214(7) Uani 1 1 d . . . . .
H9 H 0.498269 0.728566 -0.026991 0.026 Uiso 1 1 calc R . . . .
C18 C 1.0528(4) 0.3961(3) 0.1034(2) 0.0273(8) Uani 1 1 d . . . . .
H18 H 1.044132 0.394559 0.044184 0.033 Uiso 1 1 calc R . . . .
C21 C 0.8579(4) 0.6443(3) 0.2417(2) 0.0284(8) Uani 1 1 d . . . . .
H21 H 0.828790 0.609006 0.304870 0.034 Uiso 1 1 calc R . . . .
C12 C 0.3304(4) 0.9429(3) 0.1642(2) 0.0223(7) Uani 1 1 d . . . . .
H12 H 0.326121 0.957984 0.221337 0.027 Uiso 1 1 calc R . . . .
C23 C 0.8474(4) 0.7202(3) 0.1027(2) 0.0259(7) Uani 1 1 d . . . . .
H23 H 0.807696 0.748299 0.050056 0.031 Uiso 1 1 calc R . . . .
C20 C 0.9999(4) 0.3832(3) 0.2474(2) 0.0320(9) Uani 1 1 d . . . . .
H20 H 0.944692 0.370319 0.310650 0.038 Uiso 1 1 calc R . . . .
C7 C 0.5436(4) 0.3738(3) 0.3555(2) 0.0226(7) Uani 1 1 d . . . . .
H7 H 0.482755 0.427486 0.381040 0.027 Uiso 1 1 calc R . . . .
C10 C 0.4080(4) 0.8267(3) 0.0597(2) 0.0200(7) Uani 1 1 d . . . . .
C19 C 1.1518(5) 0.4181(3) 0.2113(3) 0.0382(10) Uani 1 1 d . . . . .
H19 H 1.222239 0.434113 0.243483 0.046 Uiso 1 1 calc R . . . .
C11 C 0.4023(4) 0.8499(2) 0.1447(2) 0.0199(6) Uani 1 1 d . . . . .
C1 C 0.5723(4) 0.2767(3) 0.4179(2) 0.0229(7) Uani 1 1 d . . . . .
C2 C 0.6747(4) 0.1950(3) 0.3913(2) 0.0235(7) Uani 1 1 d . . . . .
C22 C 1.0027(4) 0.7216(3) 0.1060(3) 0.0352(9) Uani 1 1 d . . . . .
H22 H 1.091446 0.750220 0.056681 0.042 Uiso 1 1 calc R . . . .
C17 C 0.1809(5) 1.1316(3) 0.1979(3) 0.0354(9) Uani 1 1 d . . . . .
H17A H 0.121406 1.077015 0.248560 0.053 Uiso 1 1 calc GR . . . .
H17B H 0.124315 1.199196 0.198733 0.053 Uiso 1 1 calc GR . . . .
H17C H 0.289561 1.136171 0.205034 0.053 Uiso 1 1 calc GR . . . .
C15 C 0.3444(4) 0.9021(3) -0.0042(2) 0.0249(7) Uani 1 1 d . . . . .
H15 H 0.352467 0.889580 -0.062694 0.030 Uiso 1 1 calc R . . . .
C13 C 0.2649(4) 1.0136(3) 0.0997(2) 0.0256(7) Uani 1 1 d . . . . .
C3 C 0.6968(4) 0.1032(3) 0.4561(2) 0.0262(7) Uani 1 1 d . . . . .
H3 H 0.766728 0.048743 0.437304 0.031 Uiso 1 1 calc R . . . .
C6 C 0.4967(5) 0.2633(3) 0.5121(2) 0.0289(8) Uani 1 1 d . . . . .
H6A H 0.428439 0.317881 0.531888 0.035 Uiso 1 1 calc R . . . .
C14 C 0.2712(4) 0.9930(3) 0.0152(2) 0.0285(8) Uani 1 1 d . . . . .
H14 H 0.225371 1.041255 -0.028282 0.034 Uiso 1 1 calc R . . . .
C4 C 0.6158(5) 0.0925(3) 0.5479(2) 0.0317(8) Uani 1 1 d . . . . .
N10 N 0.0617(6) 0.1047(4) 0.6433(3) 0.0716(13) Uani 1 1 d . U . . .
C16 C 0.7202(5) -0.0825(3) 0.5871(3) 0.0419(10) Uani 1 1 d . . . . .
H16A H 0.684233 -0.098616 0.537540 0.063 Uiso 1 1 calc GR . . . .
H16B H 0.705013 -0.143679 0.639459 0.063 Uiso 1 1 calc GR . . . .
H16C H 0.834606 -0.064626 0.565212 0.063 Uiso 1 1 calc GR . . . .
C5 C 0.5181(5) 0.1748(3) 0.5760(2) 0.0338(9) Uani 1 1 d . . . . .
H5 H 0.466948 0.168882 0.639179 0.041 Uiso 1 1 calc R . . . .
C26 C 0.1167(6) 0.0821(4) 0.7041(3) 0.0517(12) Uani 1 1 d . U . . .
C25 C 0.0990(6) 0.6793(4) 0.4649(3) 0.0584(13) Uani 1 1 d . . . . .
H25A H 0.145366 0.699248 0.398292 0.088 Uiso 1 1 calc GR . . . .
H25B H 0.132889 0.728961 0.493428 0.088 Uiso 1 1 calc GR . . . .
H25C H -0.018855 0.680623 0.477966 0.088 Uiso 1 1 calc GR . . . .
N9 N 0.1979(6) 0.4916(4) 0.5311(4) 0.0883(16) Uani 1 1 d . . . . .
C24 C 0.1533(6) 0.5772(5) 0.5009(4) 0.0624(14) Uani 1 1 d . . . . .
C27 C 0.1886(7) 0.0489(4) 0.7814(3) 0.0671(15) Uani 1 1 d . . . . .
H27A H 0.299374 0.024058 0.760146 0.101 Uiso 1 1 calc GR . . . .
H27B H 0.125500 -0.007944 0.827618 0.101 Uiso 1 1 calc GR . . . .
H27C H 0.189252 0.108264 0.808494 0.101 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
Mo1 O2 2.007(2) . ?
Mo1 O1 1.917(2) . ?
Mo1 O5 1.704(2) . ?
Mo1 O4 1.706(2) . ?
Mo1 N5 2.353(3) . ?
Mo1 N1 2.280(2) . ?
Mo2 O3 1.951(2) . ?
Mo2 O7 1.707(2) . ?
Mo2 O6 1.720(2) . ?
Mo2 N2 2.113(2) . ?
Mo2 N7 2.325(3) . ?
Mo2 N4 2.243(3) . ?
O2 C8 1.314(4) . ?
O3 C11 1.343(4) . ?
O1 C2 1.352(4) . ?
N2 N1 1.396(4) . ?
N2 C8 1.383(4) . ?
O9 C17 1.437(4) . ?
O9 C13 1.357(4) . ?
N7 C21 1.324(4) . ?
N7 C23 1.386(4) . ?
N5 C18 1.318(4) . ?
N5 C20 1.375(4) . ?
N4 N3 1.395(3) . ?
N4 C9 1.288(4) . ?
O8 C4 1.360(4) . ?
O8 C16 1.449(4) . ?
N3 C8 1.304(4) . ?
N1 C7 1.287(4) . ?
N6 H6 0.816(18) . ?
N6 C18 1.330(5) . ?
N6 C19 1.358(4) . ?
N8 H8 0.866(18) . ?
N8 C21 1.334(4) . ?
N8 C22 1.359(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.442(4) . ?
C18 H18 0.9500 . ?
C21 H21 0.9500 . ?
C12 H12 0.9500 . ?
C12 C11 1.392(4) . ?
C12 C13 1.393(5) . ?
C23 H23 0.9500 . ?
C23 C22 1.354(5) . ?
C20 H20 0.9500 . ?
C20 C19 1.347(5) . ?
C7 H7 0.9500 . ?
C7 C1 1.446(5) . ?
C10 C11 1.420(4) . ?
C10 C15 1.407(4) . ?
C19 H19 0.9500 . ?
C1 C2 1.407(5) . ?
C1 C6 1.407(4) . ?
C2 C3 1.402(5) . ?
C22 H22 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C15 H15 0.9500 . ?
C15 C14 1.370(5) . ?
C13 C14 1.397(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.390(5) . ?
C6 H6A 0.9500 . ?
C6 C5 1.364(5) . ?
C14 H14 0.9500 . ?
C4 C5 1.401(5) . ?
N10 C26 1.133(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C5 H5 0.9500 . ?
C26 C27 1.454(7) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 C24 1.414(7) . ?
N9 C24 1.182(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 N5 80.54(9) . . ?
O2 Mo1 N1 72.48(9) . . ?
O1 Mo1 O2 151.29(9) . . ?
O1 Mo1 N5 80.64(10) . . ?
O1 Mo1 N1 82.54(9) . . ?
O5 Mo1 O2 95.81(10) . . ?
O5 Mo1 O1 104.18(10) . . ?
O5 Mo1 O4 105.26(11) . . ?
O5 Mo1 N5 85.69(10) . . ?
O5 Mo1 N1 161.24(11) . . ?
O4 Mo1 O2 96.08(11) . . ?
O4 Mo1 O1 98.23(12) . . ?
O4 Mo1 N5 168.86(10) . . ?
O4 Mo1 N1 90.80(10) . . ?
N1 Mo1 N5 78.07(9) . . ?
O3 Mo2 N2 150.60(10) . . ?
O3 Mo2 N7 80.05(9) . . ?
O3 Mo2 N4 82.51(9) . . ?
O7 Mo2 O3 106.66(10) . . ?
O7 Mo2 O6 105.37(11) . . ?
O7 Mo2 N2 94.26(10) . . ?
O7 Mo2 N7 83.10(10) . . ?
O7 Mo2 N4 158.31(10) . . ?
O6 Mo2 O3 96.19(11) . . ?
O6 Mo2 N2 97.92(10) . . ?
O6 Mo2 N7 171.46(10) . . ?
O6 Mo2 N4 92.81(10) . . ?
N2 Mo2 N7 82.27(9) . . ?
N2 Mo2 N4 71.17(9) . . ?
N4 Mo2 N7 79.14(9) . . ?
C8 O2 Mo1 122.79(19) . . ?
C11 O3 Mo2 129.79(19) . . ?
C2 O1 Mo1 132.2(2) . . ?
N1 N2 Mo2 131.20(18) . . ?
C8 N2 Mo2 117.1(2) . . ?
C8 N2 N1 111.4(2) . . ?
C13 O9 C17 117.4(3) . . ?
C21 N7 Mo2 122.8(2) . . ?
C21 N7 C23 106.0(3) . . ?
C23 N7 Mo2 131.2(2) . . ?
C18 N5 Mo1 122.5(2) . . ?
C18 N5 C20 104.5(3) . . ?
C20 N5 Mo1 130.4(2) . . ?
N3 N4 Mo2 118.18(19) . . ?
C9 N4 Mo2 125.6(2) . . ?
C9 N4 N3 116.3(3) . . ?
C4 O8 C16 116.9(3) . . ?
C8 N3 N4 110.4(2) . . ?
N2 N1 Mo1 113.84(17) . . ?
C7 N1 Mo1 124.9(2) . . ?
C7 N1 N2 121.0(3) . . ?
C18 N6 H6 128(3) . . ?
C18 N6 C19 107.5(3) . . ?
C19 N6 H6 124(3) . . ?
O2 C8 N2 119.4(3) . . ?
N3 C8 O2 118.0(3) . . ?
N3 C8 N2 122.5(3) . . ?
C21 N8 H8 126(3) . . ?
C21 N8 C22 108.3(3) . . ?
C22 N8 H8 125(3) . . ?
N4 C9 H9 117.7 . . ?
N4 C9 C10 124.7(3) . . ?
C10 C9 H9 117.7 . . ?
N5 C18 N6 111.9(3) . . ?
N5 C18 H18 124.0 . . ?
N6 C18 H18 124.0 . . ?
N7 C21 N8 110.5(3) . . ?
N7 C21 H21 124.7 . . ?
N8 C21 H21 124.7 . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.8(3) . . ?
C13 C12 H12 120.1 . . ?
N7 C23 H23 125.7 . . ?
C22 C23 N7 108.6(3) . . ?
C22 C23 H23 125.7 . . ?
N5 C20 H20 125.0 . . ?
C19 C20 N5 110.1(3) . . ?
C19 C20 H20 125.0 . . ?
N1 C7 H7 117.9 . . ?
N1 C7 C1 124.2(3) . . ?
C1 C7 H7 117.9 . . ?
C11 C10 C9 123.2(3) . . ?
C15 C10 C9 119.0(3) . . ?
C15 C10 C11 117.8(3) . . ?
N6 C19 H19 127.0 . . ?
C20 C19 N6 106.0(3) . . ?
C20 C19 H19 127.0 . . ?
O3 C11 C12 117.7(3) . . ?
O3 C11 C10 122.0(3) . . ?
C12 C11 C10 120.3(3) . . ?
C2 C1 C7 124.4(3) . . ?
C2 C1 C6 117.3(3) . . ?
C6 C1 C7 118.3(3) . . ?
O1 C2 C1 122.3(3) . . ?
O1 C2 C3 116.7(3) . . ?
C3 C2 C1 121.0(3) . . ?
N8 C22 H22 126.7 . . ?
C23 C22 N8 106.5(3) . . ?
C23 C22 H22 126.7 . . ?
O9 C17 H17A 109.5 . . ?
O9 C17 H17B 109.5 . . ?
O9 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C10 C15 H15 118.9 . . ?
C14 C15 C10 122.2(3) . . ?
C14 C15 H15 118.9 . . ?
O9 C13 C12 124.4(3) . . ?
O9 C13 C14 114.7(3) . . ?
C12 C13 C14 120.9(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.5(3) . . ?
C4 C3 H3 120.3 . . ?
C1 C6 H6A 118.8 . . ?
C5 C6 C1 122.3(3) . . ?
C5 C6 H6A 118.8 . . ?
C15 C14 C13 119.1(3) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
O8 C4 C3 123.7(3) . . ?
O8 C4 C5 116.1(3) . . ?
C3 C4 C5 120.1(3) . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
N10 C26 C27 177.7(5) . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
N9 C24 C25 179.6(8) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C8 N2 -0.5(4) . . . . ?
Mo1 O2 C8 N3 -179.7(2) . . . . ?
Mo1 O1 C2 C1 -32.4(5) . . . . ?
Mo1 O1 C2 C3 149.4(3) . . . . ?
Mo1 N5 C18 N6 -163.2(2) . . . . ?
Mo1 N5 C20 C19 161.4(3) . . . . ?
Mo1 N1 C7 C1 8.3(5) . . . . ?
Mo2 O3 C11 C12 144.6(2) . . . . ?
Mo2 O3 C11 C10 -38.5(4) . . . . ?
Mo2 N2 N1 Mo1 -172.13(14) . . . . ?
Mo2 N2 N1 C7 14.3(4) . . . . ?
Mo2 N2 C8 O2 173.9(2) . . . . ?
Mo2 N2 C8 N3 -7.0(4) . . . . ?
Mo2 N7 C21 N8 179.5(2) . . . . ?
Mo2 N7 C23 C22 -179.3(2) . . . . ?
Mo2 N4 N3 C8 5.3(3) . . . . ?
Mo2 N4 C9 C10 1.9(5) . . . . ?
O1 C2 C3 C4 178.6(3) . . . . ?
N2 N1 C7 C1 -178.9(3) . . . . ?
O9 C13 C14 C15 179.2(3) . . . . ?
N7 C23 C22 N8 -0.3(4) . . . . ?
N5 C20 C19 N6 0.0(5) . . . . ?
N4 N3 C8 O2 -180.0(2) . . . . ?
N4 N3 C8 N2 0.9(4) . . . . ?
N4 C9 C10 C11 12.7(5) . . . . ?
N4 C9 C10 C15 -169.1(3) . . . . ?
O8 C4 C5 C6 -177.9(4) . . . . ?
N3 N4 C9 C10 -178.9(3) . . . . ?
N1 N2 C8 O2 -1.1(4) . . . . ?
N1 N2 C8 N3 178.0(3) . . . . ?
N1 C7 C1 C2 7.5(6) . . . . ?
N1 C7 C1 C6 -174.3(3) . . . . ?
C8 N2 N1 Mo1 2.0(3) . . . . ?
C8 N2 N1 C7 -171.6(3) . . . . ?
C9 N4 N3 C8 -173.9(3) . . . . ?
C9 C10 C11 O3 3.6(5) . . . . ?
C9 C10 C11 C12 -179.6(3) . . . . ?
C9 C10 C15 C14 178.4(3) . . . . ?
C18 N5 C20 C19 -0.1(4) . . . . ?
C18 N6 C19 C20 0.1(5) . . . . ?
C21 N7 C23 C22 0.2(4) . . . . ?
C21 N8 C22 C23 0.3(4) . . . . ?
C12 C13 C14 C15 -0.6(5) . . . . ?
C23 N7 C21 N8 0.0(4) . . . . ?
C20 N5 C18 N6 0.1(4) . . . . ?
C7 C1 C2 O1 1.6(5) . . . . ?
C7 C1 C2 C3 179.8(3) . . . . ?
C7 C1 C6 C5 -179.4(4) . . . . ?
C10 C15 C14 C13 2.6(5) . . . . ?
C19 N6 C18 N5 -0.1(5) . . . . ?
C11 C12 C13 O9 179.8(3) . . . . ?
C11 C12 C13 C14 -0.4(5) . . . . ?
C11 C10 C15 C14 -3.4(5) . . . . ?
C1 C2 C3 C4 0.3(5) . . . . ?
C1 C6 C5 C4 -1.3(6) . . . . ?
C2 C1 C6 C5 -1.0(5) . . . . ?
C2 C3 C4 O8 178.5(3) . . . . ?
C2 C3 C4 C5 -2.7(6) . . . . ?
C22 N8 C21 N7 -0.2(4) . . . . ?
C17 O9 C13 C12 -0.5(5) . . . . ?
C17 O9 C13 C14 179.7(3) . . . . ?
C15 C10 C11 O3 -174.6(3) . . . . ?
C15 C10 C11 C12 2.2(5) . . . . ?
C13 C12 C11 O3 176.6(3) . . . . ?
C13 C12 C11 C10 -0.4(5) . . . . ?
C3 C4 C5 C6 3.1(6) . . . . ?
C6 C1 C2 O1 -176.6(3) . . . . ?
C6 C1 C2 C3 1.5(5) . . . . ?
C16 O8 C4 C3 -4.3(6) . . . . ?
C16 O8 C4 C5 176.8(3) . . . . ?

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

data_6a
_database_code_depnum_ccdc_archive 'CCDC 1983035'
loop_
_audit_author_name
_audit_author_address
'Edi Topic'
;Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-02-10 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        
2,2'-(carbonylbis(hydrazin-2-yl-1-ylidenemethylylidene))di(4-methoxyphenolato))bis(methanol)tetraoxo-di-molybdenum(vi)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H22 Mo2 N4 O11'
_chemical_formula_sum            'C19 H22 Mo2 N4 O11'
_chemical_formula_weight         674.28

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'
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4676(3)
_cell_length_b                   11.7394(4)
_cell_length_c                   14.8772(6)
_cell_angle_alpha                105.949(3)
_cell_angle_beta                 103.394(3)
_cell_angle_gamma                96.009(3)
_cell_volume                     1199.98(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3865
_cell_measurement_theta_min      4.5070
_cell_measurement_theta_max      30.3470

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.111
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.91105
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_diffrn_ambient_temperature      295(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            12820
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.224
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6347
_reflns_number_gt                4394
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0343P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6347
_refine_ls_number_parameters     335
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.0929
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.56132(4) 0.43080(3) 0.20283(2) 0.03131(10) Uani 1 1 d . . . . .
Mo1 Mo 0.83668(5) 0.20897(3) 0.44760(2) 0.03490(10) Uani 1 1 d . . . . .
O2 O 0.7969(3) 0.3796(2) 0.47397(17) 0.0369(6) Uani 1 1 d . . . . .
O3 O 0.4955(3) 0.5657(2) 0.16107(18) 0.0394(6) Uani 1 1 d . . . . .
O1 O 0.8988(3) 0.0697(2) 0.36802(18) 0.0399(6) Uani 1 1 d . . . . .
O7 O 0.6544(4) 0.3547(2) 0.11497(19) 0.0475(7) Uani 1 1 d . . . . .
O4 O 0.6192(4) 0.1496(2) 0.4466(2) 0.0531(8) Uani 1 1 d . . . . .
N4 N 0.5897(4) 0.5607(2) 0.3486(2) 0.0304(7) Uani 1 1 d . . . . .
N2 N 0.6844(4) 0.3555(2) 0.3100(2) 0.0314(7) Uani 1 1 d . . . . .
O11 O 0.8656(4) 0.5480(2) 0.2598(2) 0.0481(7) Uani 1 1 d D . . . .
H11O H 0.883(6) 0.6173(19) 0.290(3) 0.058 Uiso 1 1 d D U . . .
O8 O 0.8883(4) -0.2950(2) 0.1412(2) 0.0458(7) Uani 1 1 d . . . . .
O9 O 0.2573(4) 0.8961(2) 0.09831(19) 0.0450(7) Uani 1 1 d . . . . .
N3 N 0.6745(4) 0.5287(3) 0.4303(2) 0.0324(7) Uani 1 1 d . . . . .
O6 O 0.3467(4) 0.3475(2) 0.1780(2) 0.0503(8) Uani 1 1 d . . . . .
N1 N 0.7284(4) 0.2410(2) 0.3013(2) 0.0294(6) Uani 1 1 d . . . . .
O10 O 1.0979(4) 0.3001(2) 0.4180(2) 0.0441(7) Uani 1 1 d D . . . .
H10O H 1.159(5) 0.350(3) 0.466(2) 0.053 Uiso 1 1 d D U . . .
O5 O 0.9749(4) 0.2298(2) 0.5615(2) 0.0521(8) Uani 1 1 d . . . . .
C8 C 0.7176(5) 0.4220(3) 0.4053(3) 0.0313(8) Uani 1 1 d . . . . .
C1 C 0.7523(4) 0.0463(3) 0.1999(2) 0.0287(8) Uani 1 1 d . . . . .
C9 C 0.5497(5) 0.6675(3) 0.3679(3) 0.0333(8) Uani 1 1 d . . . . .
H9 H 0.571902 0.711248 0.433025 0.040 Uiso 1 1 calc R U . . .
C7 C 0.7065(5) 0.1651(3) 0.2167(3) 0.0306(8) Uani 1 1 d . . . . .
H7 H 0.657580 0.188765 0.162726 0.037 Uiso 1 1 calc R U . . .
C2 C 0.8441(5) 0.0023(3) 0.2743(3) 0.0293(8) Uani 1 1 d . . . . .
C6 C 0.7100(5) -0.0282(3) 0.1042(3) 0.0329(8) Uani 1 1 d . . . . .
H6 H 0.652354 0.000698 0.054680 0.039 Uiso 1 1 calc R U . . .
C11 C 0.4462(5) 0.6728(3) 0.1969(3) 0.0306(8) Uani 1 1 d . . . . .
C12 C 0.3712(5) 0.7321(3) 0.1321(3) 0.0342(8) Uani 1 1 d . . . . .
H12 H 0.349813 0.696124 0.065659 0.041 Uiso 1 1 calc R U . . .
C10 C 0.4737(5) 0.7247(3) 0.2975(3) 0.0316(8) Uani 1 1 d . . . . .
C13 C 0.3284(5) 0.8456(3) 0.1673(3) 0.0335(8) Uani 1 1 d . . . . .
C3 C 0.8849(5) -0.1123(3) 0.2508(3) 0.0334(8) Uani 1 1 d . . . . .
H3 H 0.944527 -0.141263 0.299866 0.040 Uiso 1 1 calc R U . . .
C4 C 0.8382(5) -0.1851(3) 0.1547(3) 0.0320(8) Uani 1 1 d . . . . .
C5 C 0.7501(5) -0.1431(3) 0.0799(3) 0.0349(8) Uani 1 1 d . . . . .
H5 H 0.719277 -0.191178 0.015378 0.042 Uiso 1 1 calc R U . . .
C17 C 0.2155(5) 1.0149(3) 0.1295(3) 0.0450(10) Uani 1 1 d . . . . .
H17A H 0.124615 1.014476 0.165675 0.068 Uiso 1 1 calc R U . . .
H17B H 0.166332 1.039682 0.073701 0.068 Uiso 1 1 calc R U . . .
H17C H 0.327767 1.070038 0.169856 0.068 Uiso 1 1 calc R U . . .
C15 C 0.4303(5) 0.8389(3) 0.3295(3) 0.0391(9) Uani 1 1 d . . . . .
H15 H 0.450420 0.875537 0.395815 0.047 Uiso 1 1 calc R U . . .
C14 C 0.3584(5) 0.8993(3) 0.2659(3) 0.0402(9) Uani 1 1 d . . . . .
H14 H 0.330332 0.975388 0.289124 0.048 Uiso 1 1 calc R U . . .
C18 C 1.2045(6) 0.2543(4) 0.3537(3) 0.0578(12) Uani 1 1 d . . . . .
H18A H 1.252045 0.186599 0.368269 0.087 Uiso 1 1 calc R U . . .
H18B H 1.307007 0.315815 0.361214 0.087 Uiso 1 1 calc R U . . .
H18C H 1.126702 0.229178 0.288078 0.087 Uiso 1 1 calc R U . . .
C16 C 0.8367(7) -0.3774(4) 0.0458(3) 0.0644(14) Uani 1 1 d . . . . .
H16A H 0.703193 -0.391968 0.020127 0.097 Uiso 1 1 calc R U . . .
H16B H 0.877546 -0.451783 0.047563 0.097 Uiso 1 1 calc R U . . .
H16C H 0.894564 -0.344043 0.005100 0.097 Uiso 1 1 calc R U . . .
C19 C 1.0379(6) 0.5083(4) 0.2585(4) 0.0672(14) Uani 1 1 d . . . . .
H19A H 1.091327 0.495511 0.319381 0.101 Uiso 1 1 calc R U . . .
H19C H 1.122288 0.568292 0.248615 0.101 Uiso 1 1 calc R U . . .
H19B H 1.016850 0.434289 0.206718 0.101 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
# start Validation Reply Form
_vrf_PLAT906_6a                  
;
PROBLEM: Large K Value in the Analysis of Variance ......     10.310 Check 
RESPONSE: The K value is large only for weak reflections with Fc/Fcmax 
lower than 0.009.
;
_vrf_PLAT975_6a                  
;
PROBLEM: Check Calcd Resid. Dens.  0.47A   From O4              0.40 eA-3  
RESPONSE: Residual density peak has no meaningful chemical interpretation.
;
_vrf_PLAT977_6a                  
;
PROBLEM: Check Negative Difference Density on H11O             -0.33 eA-3  
RESPONSE: H11O is a methanol O hydrogen atom, modelled in the most probable 
conformation.
;
_vrf_PLAT910_6a                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         21 Note 
RESPONSE: Beam-stop shadowing.
;
# end Validation Reply Form
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 O6 1.691(3) . ?
Mo2 O7 1.703(3) . ?
Mo2 O3 1.923(2) . ?
Mo2 N2 2.105(3) . ?
Mo2 N4 2.230(3) . ?
Mo2 O11 2.364(3) . ?
Mo1 O4 1.694(3) . ?
Mo1 O5 1.704(3) . ?
Mo1 O1 1.908(3) . ?
Mo1 O2 2.000(2) . ?
Mo1 N1 2.287(3) . ?
Mo1 O10 2.316(3) . ?
O2 C8 1.305(4) . ?
O3 C11 1.349(4) . ?
O1 C2 1.341(4) . ?
N4 C9 1.290(4) . ?
N4 N3 1.402(4) . ?
N2 C8 1.367(4) . ?
N2 N1 1.396(4) . ?
O11 C19 1.416(5) . ?
O11 H11O 0.794(18) . ?
O8 C4 1.357(4) . ?
O8 C16 1.418(5) . ?
O9 C13 1.354(4) . ?
O9 C17 1.435(4) . ?
N3 C8 1.303(4) . ?
N1 C7 1.289(4) . ?
O10 C18 1.413(5) . ?
O10 H10O 0.791(18) . ?
C1 C6 1.393(5) . ?
C1 C2 1.414(4) . ?
C1 C7 1.439(5) . ?
C9 C10 1.435(5) . ?
C9 H9 0.9300 . ?
C7 H7 0.9300 . ?
C2 C3 1.379(5) . ?
C6 C5 1.381(5) . ?
C6 H6 0.9300 . ?
C11 C12 1.388(5) . ?
C11 C10 1.407(5) . ?
C12 C13 1.392(5) . ?
C12 H12 0.9300 . ?
C10 C15 1.394(5) . ?
C13 C14 1.382(5) . ?
C3 C4 1.390(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(5) . ?
C5 H5 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C15 C14 1.377(5) . ?
C15 H15 0.9300 . ?
C14 H14 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19C 0.9600 . ?
C19 H19B 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Mo2 O7 104.17(14) . . ?
O6 Mo2 O3 100.53(12) . . ?
O7 Mo2 O3 103.04(12) . . ?
O6 Mo2 N2 93.92(12) . . ?
O7 Mo2 N2 96.54(12) . . ?
O3 Mo2 N2 151.88(11) . . ?
O6 Mo2 N4 102.14(13) . . ?
O7 Mo2 N4 151.75(12) . . ?
O3 Mo2 N4 81.94(10) . . ?
N2 Mo2 N4 71.44(11) . . ?
O6 Mo2 O11 172.15(13) . . ?
O7 Mo2 O11 81.31(12) . . ?
O3 Mo2 O11 83.45(10) . . ?
N2 Mo2 O11 79.75(10) . . ?
N4 Mo2 O11 71.56(11) . . ?
O4 Mo1 O5 105.83(14) . . ?
O4 Mo1 O1 99.22(13) . . ?
O5 Mo1 O1 104.61(12) . . ?
O4 Mo1 O2 96.29(12) . . ?
O5 Mo1 O2 95.00(11) . . ?
O1 Mo1 O2 150.49(11) . . ?
O4 Mo1 N1 92.20(12) . . ?
O5 Mo1 N1 159.10(12) . . ?
O1 Mo1 N1 82.26(10) . . ?
O2 Mo1 N1 72.16(10) . . ?
O4 Mo1 O10 166.96(12) . . ?
O5 Mo1 O10 86.59(12) . . ?
O1 Mo1 O10 81.01(10) . . ?
O2 Mo1 O10 78.35(10) . . ?
N1 Mo1 O10 74.87(10) . . ?
C8 O2 Mo1 122.5(2) . . ?
C11 O3 Mo2 138.9(2) . . ?
C2 O1 Mo1 137.2(2) . . ?
C9 N4 N3 114.6(3) . . ?
C9 N4 Mo2 127.7(2) . . ?
N3 N4 Mo2 117.5(2) . . ?
C8 N2 N1 111.2(3) . . ?
C8 N2 Mo2 118.1(2) . . ?
N1 N2 Mo2 130.5(2) . . ?
C19 O11 Mo2 128.1(3) . . ?
C19 O11 H11O 111(3) . . ?
Mo2 O11 H11O 121(3) . . ?
C4 O8 C16 118.6(3) . . ?
C13 O9 C17 118.0(3) . . ?
C8 N3 N4 111.2(3) . . ?
C7 N1 N2 120.3(3) . . ?
C7 N1 Mo1 126.3(2) . . ?
N2 N1 Mo1 113.4(2) . . ?
C18 O10 Mo1 131.0(2) . . ?
C18 O10 H10O 113(3) . . ?
Mo1 O10 H10O 110(3) . . ?
N3 C8 O2 118.2(3) . . ?
N3 C8 N2 121.7(3) . . ?
O2 C8 N2 120.1(3) . . ?
C6 C1 C2 118.0(3) . . ?
C6 C1 C7 118.0(3) . . ?
C2 C1 C7 124.0(3) . . ?
N4 C9 C10 125.6(3) . . ?
N4 C9 H9 117.2 . . ?
C10 C9 H9 117.2 . . ?
N1 C7 C1 124.7(3) . . ?
N1 C7 H7 117.6 . . ?
C1 C7 H7 117.6 . . ?
O1 C2 C3 118.1(3) . . ?
O1 C2 C1 122.2(3) . . ?
C3 C2 C1 119.7(3) . . ?
C5 C6 C1 122.8(3) . . ?
C5 C6 H6 118.6 . . ?
C1 C6 H6 118.6 . . ?
O3 C11 C12 118.2(3) . . ?
O3 C11 C10 121.1(3) . . ?
C12 C11 C10 120.7(3) . . ?
C11 C12 C13 119.6(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C15 C10 C11 117.8(3) . . ?
C15 C10 C9 119.0(3) . . ?
C11 C10 C9 123.2(3) . . ?
O9 C13 C14 124.4(3) . . ?
O9 C13 C12 115.0(3) . . ?
C14 C13 C12 120.6(3) . . ?
C2 C3 C4 120.9(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
O8 C4 C3 115.1(3) . . ?
O8 C4 C5 124.4(3) . . ?
C3 C4 C5 120.5(3) . . ?
C6 C5 C4 118.1(3) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
O9 C17 H17A 109.5 . . ?
O9 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O9 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C15 C10 122.0(4) . . ?
C14 C15 H15 119.0 . . ?
C10 C15 H15 119.0 . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
O10 C18 H18A 109.5 . . ?
O10 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O10 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O8 C16 H16A 109.5 . . ?
O8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O11 C19 H19A 109.5 . . ?
O11 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
O11 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19C C19 H19B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N4 N3 C8 -177.5(3) . . . . ?
Mo2 N4 N3 C8 -2.3(4) . . . . ?
C8 N2 N1 C7 -179.9(3) . . . . ?
Mo2 N2 N1 C7 5.3(5) . . . . ?
C8 N2 N1 Mo1 0.1(3) . . . . ?
Mo2 N2 N1 Mo1 -174.65(16) . . . . ?
N4 N3 C8 O2 -179.6(3) . . . . ?
N4 N3 C8 N2 1.4(5) . . . . ?
Mo1 O2 C8 N3 170.8(2) . . . . ?
Mo1 O2 C8 N2 -10.2(5) . . . . ?
N1 N2 C8 N3 -175.2(3) . . . . ?
Mo2 N2 C8 N3 0.3(5) . . . . ?
N1 N2 C8 O2 5.8(5) . . . . ?
Mo2 N2 C8 O2 -178.7(2) . . . . ?
N3 N4 C9 C10 175.8(3) . . . . ?
Mo2 N4 C9 C10 1.2(5) . . . . ?
N2 N1 C7 C1 178.2(3) . . . . ?
Mo1 N1 C7 C1 -1.8(5) . . . . ?
C6 C1 C7 N1 176.1(3) . . . . ?
C2 C1 C7 N1 -6.4(6) . . . . ?
Mo1 O1 C2 C3 -161.0(3) . . . . ?
Mo1 O1 C2 C1 21.0(5) . . . . ?
C6 C1 C2 O1 176.6(3) . . . . ?
C7 C1 C2 O1 -0.9(5) . . . . ?
C6 C1 C2 C3 -1.4(5) . . . . ?
C7 C1 C2 C3 -178.9(3) . . . . ?
C2 C1 C6 C5 1.5(5) . . . . ?
C7 C1 C6 C5 179.2(3) . . . . ?
Mo2 O3 C11 C12 -166.4(3) . . . . ?
Mo2 O3 C11 C10 15.1(5) . . . . ?
O3 C11 C12 C13 -176.5(3) . . . . ?
C10 C11 C12 C13 2.0(5) . . . . ?
O3 C11 C10 C15 176.0(3) . . . . ?
C12 C11 C10 C15 -2.5(5) . . . . ?
O3 C11 C10 C9 -1.8(5) . . . . ?
C12 C11 C10 C9 179.7(3) . . . . ?
N4 C9 C10 C15 177.3(4) . . . . ?
N4 C9 C10 C11 -4.8(6) . . . . ?
C17 O9 C13 C14 2.1(5) . . . . ?
C17 O9 C13 C12 -178.0(3) . . . . ?
C11 C12 C13 O9 179.5(3) . . . . ?
C11 C12 C13 C14 -0.5(6) . . . . ?
O1 C2 C3 C4 -177.7(3) . . . . ?
C1 C2 C3 C4 0.4(5) . . . . ?
C16 O8 C4 C3 176.6(4) . . . . ?
C16 O8 C4 C5 -4.9(6) . . . . ?
C2 C3 C4 O8 179.1(3) . . . . ?
C2 C3 C4 C5 0.5(6) . . . . ?
C1 C6 C5 C4 -0.6(5) . . . . ?
O8 C4 C5 C6 -178.9(3) . . . . ?
C3 C4 C5 C6 -0.4(5) . . . . ?
C11 C10 C15 C14 1.5(6) . . . . ?
C9 C10 C15 C14 179.5(3) . . . . ?
C10 C15 C14 C13 -0.1(6) . . . . ?
O9 C13 C14 C15 179.5(3) . . . . ?
C12 C13 C14 C15 -0.4(6) . . . . ?

_refine_diff_density_max         0.733
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.099

