# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2019

####################################################################### 
# 
# 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_koko663
_database_code_depnum_ccdc_archive 'CCDC 1882180'
loop_
_audit_author_name
_audit_author_address
'Iryna Omelchenko'
;SSI Institute for Single Crystals, Kharkiv
Ukraine
;
_audit_update_record             
;
2018-11-29 deposited with the CCDC.	2019-05-27 downloaded from the CCDC.
;
_audit_creation_date             2018-11-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
loop_
_audit_author_email
''
kokozay@univ.kiev.ua
irina@xray.isc.kharkov.com
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Mo6 O26 V2, C4 H16 Cu N4, C2 H10 N2, 2(H4 N), 4(H2 O)'
_chemical_formula_sum            'C6 H42 Cu Mo6 N8 O30 V2'
_chemical_formula_weight         1447.53
_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'
Cu Cu 0.3201 1.2651 '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'
V V 0.3005 0.5294 '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                   8.5468(5)
_cell_length_b                   10.9507(5)
_cell_length_c                   10.9914(4)
_cell_angle_alpha                102.267(4)
_cell_angle_beta                 112.333(5)
_cell_angle_gamma                99.415(5)
_cell_volume                     895.21(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2913
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.6810
_cell_measurement_theta_min      3.7250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.218
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.685
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             701
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9455
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.366
_diffrn_reflns_theta_min         3.208
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -102.00  -50.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3583  178.0000   30.0000 52

#__ type_ start__ end____ width___ exp.time_
  2 omega   10.00   40.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3583   77.0000  120.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega  -92.00    0.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3583  -77.0000    0.0000 92

#__ type_ start__ end____ width___ exp.time_
  4 omega  -53.00  -27.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3583   77.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega    7.00   65.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6083  -99.0000 -120.0000 58

#__ type_ start__ end____ width___ exp.time_
  6 omega   -5.00   29.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6083   89.0000  -17.0000 34

#__ type_ start__ end____ width___ exp.time_
  7 omega  -36.00  100.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6083    0.0000  -30.0000 136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0782400000
_diffrn_orient_matrix_UB_12      -0.0164022000
_diffrn_orient_matrix_UB_13      0.0036244000
_diffrn_orient_matrix_UB_21      0.0307574000
_diffrn_orient_matrix_UB_22      0.0602799000
_diffrn_orient_matrix_UB_23      -0.0086954000
_diffrn_orient_matrix_UB_31      0.0402071000
_diffrn_orient_matrix_UB_32      0.0289388000
_diffrn_orient_matrix_UB_33      0.0725481000
_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_source_target            Mo
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3921
_reflns_number_total             5609
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.946
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5609
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0445
_refine_ls_restrained_S_all      0.933
_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)+(0.0057P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0710
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H,H,H,H) groups
 At 1.5 times of:
  All N(H,H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O15B) \\sim Ueq, Uanis(O15A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Others
 Fixed Sof: H3AA(0.6) H3AB(0.6) H3AC(0.6) H3BD(0.4) H3BE(0.4) H3BF(0.4)
 C3A(0.4) H3AD(0.4) H3AE(0.4) C3B(0.6) H3BA(0.6) H3BB(0.6) O15B(0.45)
 H15A(0.45) H15B(0.45) O15A(0.55) H15C(0.55) H15D(0.55)
4.a Riding coordinates:
 N4(H4A,H4B,H4C,H4D), O15B(H15A,H15B), O15A(H15C,H15D)
4.b Free rotating group:
 O14(H14A,H14B)
4.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3A(H3AD,H3AE), C3B(H3BA,
 H3BB)
4.d Me refined with riding coordinates:
 N3(H3AA,H3AB,H3AC), N3(H3BD,H3BE,H3BF)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.57723(6) 0.64155(4) 0.78381(4) 0.02213(10) Uani 1 1 d . . . . .
Mo2 Mo 0.46468(6) 0.32633(4) 0.70593(4) 0.02277(10) Uani 1 1 d . . . . .
Mo3 Mo 0.37279(6) 0.18514(4) 0.91477(4) 0.02513(10) Uani 1 1 d . . . . .
Cu1 Cu 0.500000 0.000000 0.500000 0.0315(2) Uani 1 2 d S T P . .
V1 V 0.28669(10) 0.49876(7) 0.92192(7) 0.01926(16) Uani 1 1 d . . . . .
O1 O 0.5013(4) 0.7624(3) 0.8878(3) 0.0258(7) Uani 1 1 d . . . . .
O2 O 0.4342(5) 0.6350(3) 0.6220(3) 0.0333(8) Uani 1 1 d . . . . .
O3 O 0.7723(4) 0.7387(3) 0.8099(3) 0.0343(8) Uani 1 1 d . . . . .
O4 O 0.6401(4) 0.4803(3) 0.7509(3) 0.0254(7) Uani 1 1 d . . . . .
O5 O 0.3702(4) 0.4910(3) 0.7980(3) 0.0244(7) Uani 1 1 d . . . . .
O6 O 0.3253(5) 0.3140(3) 0.5402(3) 0.0321(8) Uani 1 1 d . . . . .
O7 O 0.5820(4) 0.2159(3) 0.6857(3) 0.0316(8) Uani 1 1 d . . . . .
O8 O 0.2948(4) 0.2274(3) 0.7477(3) 0.0253(7) Uani 1 1 d . . . . .
O9 O 0.4819(5) 0.0753(3) 0.8785(3) 0.0400(9) Uani 1 1 d . . . . .
O10 O 0.1751(5) 0.0927(3) 0.8910(3) 0.0395(9) Uani 1 1 d . . . . .
O11 O 0.2997(4) 0.3675(3) 0.9893(3) 0.0240(7) Uani 1 1 d . . . . .
O12 O 0.0789(4) 0.4952(3) 0.8533(3) 0.0307(8) Uani 1 1 d . . . . .
O13 O 0.3986(4) 0.6426(3) 1.0573(3) 0.0229(7) Uani 1 1 d . . . . .
N1 N 0.7226(6) -0.0377(4) 0.6099(4) 0.0341(10) Uani 1 1 d . . . . .
H1A H 0.755984 -0.000720 0.699390 0.041 Uiso 1 1 calc R . . . .
H1B H 0.705157 -0.123037 0.594947 0.041 Uiso 1 1 calc R . . . .
N2 N 0.6457(6) 0.1039(4) 0.4297(4) 0.0380(11) Uani 1 1 d . . . . .
H2A H 0.629268 0.058458 0.346404 0.046 Uiso 1 1 calc R . . . .
H2B H 0.615628 0.177272 0.424161 0.046 Uiso 1 1 calc R . . . .
C1 C 0.8604(8) 0.0120(5) 0.5711(6) 0.0494(16) Uani 1 1 d . . . . .
H1C H 0.857993 -0.053571 0.495128 0.059 Uiso 1 1 calc R . . . .
H1D H 0.974609 0.033547 0.648474 0.059 Uiso 1 1 calc R . . . .
C2 C 0.8295(8) 0.1321(5) 0.5285(6) 0.0496(16) Uani 1 1 d . . . . .
H2C H 0.855667 0.203431 0.608972 0.060 Uiso 1 1 calc R . . . .
H2D H 0.906200 0.157154 0.486719 0.060 Uiso 1 1 calc R . . . .
N3 N 0.1088(5) 0.4458(4) 0.3861(4) 0.0330(10) Uani 1 1 d . . . . .
H3AA H 0.141349 0.481589 0.330989 0.040 Uiso 0.6 1 calc R . . A 1
H3AB H 0.202477 0.435237 0.450783 0.040 Uiso 0.6 1 calc R . . A 1
H3AC H 0.031125 0.368958 0.336829 0.040 Uiso 0.6 1 calc R . . A 1
H3BD H 0.120820 0.367909 0.353697 0.040 Uiso 0.4 1 calc R . . B 2
H3BE H 0.049430 0.473121 0.315982 0.040 Uiso 0.4 1 calc R . . B 2
H3BF H 0.214433 0.501561 0.437156 0.040 Uiso 0.4 1 calc R . . B 2
C3A C 0.0084(18) 0.4367(12) 0.4749(14) 0.036(3) Uani 0.4 1 d . . . C 2
H3AD H -0.106865 0.375825 0.420283 0.043 Uiso 0.4 1 calc R . . C 2
H3AE H 0.071822 0.406624 0.551507 0.043 Uiso 0.4 1 calc R . . C 2
C3B C 0.0281(13) 0.5314(9) 0.4522(9) 0.033(2) Uani 0.6 1 d . . . C 1
H3BA H -0.073535 0.543850 0.382202 0.039 Uiso 0.6 1 calc R . . C 1
H3BB H 0.111830 0.615548 0.505475 0.039 Uiso 0.6 1 calc R . . C 1
N4 N 0.9333(5) 0.2886(4) 0.9482(4) 0.0370(11) Uani 1 1 d . . . . .
H4A H 0.953341 0.346563 1.021548 0.056 Uiso 1 1 d R . . . .
H4B H 0.924991 0.214973 0.962198 0.056 Uiso 1 1 d R . . . .
H4C H 0.844681 0.293303 0.881368 0.056 Uiso 1 1 d R . . . .
H4D H 1.025241 0.310453 0.936208 0.056 Uiso 1 1 d R . . . .
O15B O 0.161(4) 0.805(2) 0.7620(19) 0.042(4) Uani 0.45 1 d . U . D 2
H15A H 0.138606 0.874973 0.792074 0.064 Uiso 0.45 1 d R . . D 2
H15B H 0.270836 0.814133 0.799724 0.064 Uiso 0.45 1 d R . . D 2
O14 O 0.7939(6) 0.0283(4) 0.8990(5) 0.0544(11) Uani 1 1 d . . . . .
H14A H 0.687360 0.016335 0.886155 0.082 Uiso 1 1 d G . . . .
H14B H 0.832109 -0.033326 0.924413 0.082 Uiso 1 1 d G . . . .
O15A O 0.149(3) 0.793(2) 0.7942(17) 0.051(4) Uani 0.55 1 d . U . E 1
H15C H 0.252180 0.788053 0.807974 0.076 Uiso 0.55 1 d R . . E 1
H15D H 0.150281 0.871343 0.823444 0.076 Uiso 0.55 1 d R . . E 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O1 1.918(3) . ?
Mo1 O2 1.711(3) . ?
Mo1 O3 1.709(3) . ?
Mo1 O4 1.929(3) . ?
Mo1 O5 2.289(3) . ?
Mo1 O11 2.342(3) 2_667 ?
Mo2 O4 1.895(3) . ?
Mo2 O5 2.291(3) . ?
Mo2 O6 1.717(3) . ?
Mo2 O7 1.723(3) . ?
Mo2 O8 1.922(3) . ?
Mo2 O13 2.332(3) 2_667 ?
Mo3 O1 1.921(3) 2_667 ?
Mo3 O8 1.887(3) . ?
Mo3 O9 1.710(3) . ?
Mo3 O10 1.715(3) . ?
Mo3 O11 2.269(3) . ?
Mo3 O13 2.359(3) 2_667 ?
Cu1 N1 1.993(4) 2_656 ?
Cu1 N1 1.993(4) . ?
Cu1 N2 2.020(4) 2_656 ?
Cu1 N2 2.020(4) . ?
V1 O5 1.755(3) . ?
V1 O11 1.752(3) . ?
V1 O12 1.635(3) . ?
V1 O13 1.743(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.462(6) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.464(7) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.516(7) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
N3 H3AA 0.8900 . ?
N3 H3AB 0.8900 . ?
N3 H3AC 0.8900 . ?
N3 H3BD 0.8900 . ?
N3 H3BE 0.8900 . ?
N3 H3BF 0.8900 . ?
N3 C3A 1.532(16) . ?
N3 C3B 1.478(9) . ?
C3A C3A 1.43(3) 2_566 ?
C3A H3AD 0.9700 . ?
C3A H3AE 0.9700 . ?
C3B C3B 1.545(17) 2_566 ?
C3B H3BA 0.9700 . ?
C3B H3BB 0.9700 . ?
N4 H4A 0.8509 . ?
N4 H4B 0.8492 . ?
N4 H4C 0.8499 . ?
N4 H4D 0.8499 . ?
O15B H15A 0.8499 . ?
O15B H15B 0.8496 . ?
O14 H14A 0.8497 . ?
O14 H14B 0.8500 . ?
O15A H15C 0.8496 . ?
O15A H15D 0.8502 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O4 149.64(12) . . ?
O1 Mo1 O5 83.26(12) . . ?
O1 Mo1 O11 73.45(11) . 2_667 ?
O2 Mo1 O1 98.21(15) . . ?
O2 Mo1 O4 102.42(14) . . ?
O2 Mo1 O5 91.32(13) . . ?
O2 Mo1 O11 164.07(14) . 2_667 ?
O3 Mo1 O1 100.29(14) . . ?
O3 Mo1 O2 104.36(16) . . ?
O3 Mo1 O4 95.91(15) . . ?
O3 Mo1 O5 163.13(14) . . ?
O3 Mo1 O11 90.65(13) . 2_667 ?
O4 Mo1 O5 74.30(12) . . ?
O4 Mo1 O11 80.90(11) . 2_667 ?
O5 Mo1 O11 74.44(10) . 2_667 ?
O4 Mo2 O5 74.85(12) . . ?
O4 Mo2 O8 149.83(12) . . ?
O4 Mo2 O13 83.02(11) . 2_667 ?
O5 Mo2 O13 76.11(10) . 2_667 ?
O6 Mo2 O4 101.06(14) . . ?
O6 Mo2 O5 92.39(13) . . ?
O6 Mo2 O7 104.12(15) . . ?
O6 Mo2 O8 97.08(14) . . ?
O6 Mo2 O13 166.47(14) . 2_667 ?
O7 Mo2 O4 98.49(15) . . ?
O7 Mo2 O5 163.19(13) . . ?
O7 Mo2 O8 100.21(14) . . ?
O7 Mo2 O13 87.86(12) . 2_667 ?
O8 Mo2 O5 80.52(12) . . ?
O8 Mo2 O13 74.27(11) . 2_667 ?
O1 Mo3 O11 75.13(12) 2_667 . ?
O1 Mo3 O13 81.21(12) 2_667 2_667 ?
O8 Mo3 O1 150.12(12) . 2_667 ?
O8 Mo3 O11 82.33(12) . . ?
O8 Mo3 O13 74.20(11) . 2_667 ?
O9 Mo3 O1 97.54(15) . 2_667 ?
O9 Mo3 O8 99.43(14) . . ?
O9 Mo3 O10 104.79(18) . . ?
O9 Mo3 O11 164.91(15) . . ?
O9 Mo3 O13 90.68(14) . 2_667 ?
O10 Mo3 O1 101.05(14) . 2_667 ?
O10 Mo3 O8 98.15(15) . . ?
O10 Mo3 O11 89.70(15) . . ?
O10 Mo3 O13 163.81(15) . 2_667 ?
O11 Mo3 O13 75.30(10) . 2_667 ?
N1 Cu1 N1 180.0 2_656 . ?
N1 Cu1 N2 94.59(17) . 2_656 ?
N1 Cu1 N2 85.41(17) . . ?
N1 Cu1 N2 85.41(17) 2_656 2_656 ?
N1 Cu1 N2 94.59(17) 2_656 . ?
N2 Cu1 N2 180.00(17) 2_656 . ?
O11 V1 O5 112.63(14) . . ?
O12 V1 O5 110.32(15) . . ?
O12 V1 O11 106.43(16) . . ?
O12 V1 O13 107.88(15) . . ?
O13 V1 O5 110.57(14) . . ?
O13 V1 O11 108.82(13) . . ?
Mo1 O1 Mo3 117.27(16) . 2_667 ?
Mo2 O4 Mo1 116.76(16) . . ?
Mo1 O5 Mo2 90.64(11) . . ?
V1 O5 Mo1 130.32(14) . . ?
V1 O5 Mo2 128.11(15) . . ?
Mo3 O8 Mo2 118.84(16) . . ?
Mo3 O11 Mo1 90.62(11) . 2_667 ?
V1 O11 Mo1 131.74(14) . 2_667 ?
V1 O11 Mo3 127.86(15) . . ?
Mo2 O13 Mo3 88.74(10) 2_667 2_667 ?
V1 O13 Mo2 129.52(15) . 2_667 ?
V1 O13 Mo3 128.90(15) . 2_667 ?
Cu1 N1 H1A 109.6 . . ?
Cu1 N1 H1B 109.6 . . ?
H1A N1 H1B 108.2 . . ?
C1 N1 Cu1 110.1(3) . . ?
C1 N1 H1A 109.6 . . ?
C1 N1 H1B 109.6 . . ?
Cu1 N2 H2A 110.4 . . ?
Cu1 N2 H2B 110.4 . . ?
H2A N2 H2B 108.6 . . ?
C2 N2 Cu1 106.7(3) . . ?
C2 N2 H2A 110.4 . . ?
C2 N2 H2B 110.4 . . ?
N1 C1 H1C 109.9 . . ?
N1 C1 H1D 109.9 . . ?
N1 C1 C2 108.8(5) . . ?
H1C C1 H1D 108.3 . . ?
C2 C1 H1C 109.9 . . ?
C2 C1 H1D 109.9 . . ?
N2 C2 C1 109.1(4) . . ?
N2 C2 H2C 109.9 . . ?
N2 C2 H2D 109.9 . . ?
C1 C2 H2C 109.9 . . ?
C1 C2 H2D 109.9 . . ?
H2C C2 H2D 108.3 . . ?
H3AA N3 H3AB 109.5 . . ?
H3AA N3 H3AC 109.5 . . ?
H3AB N3 H3AC 109.5 . . ?
H3BD N3 H3BE 109.5 . . ?
H3BD N3 H3BF 109.5 . . ?
H3BE N3 H3BF 109.5 . . ?
C3A N3 H3BD 109.5 . . ?
C3A N3 H3BE 109.5 . . ?
C3A N3 H3BF 109.5 . . ?
C3B N3 H3AA 109.5 . . ?
C3B N3 H3AB 109.5 . . ?
C3B N3 H3AC 109.5 . . ?
N3 C3A H3AD 110.1 . . ?
N3 C3A H3AE 110.1 . . ?
C3A C3A N3 107.9(14) 2_566 . ?
C3A C3A H3AD 110.1 2_566 . ?
C3A C3A H3AE 110.1 2_566 . ?
H3AD C3A H3AE 108.4 . . ?
N3 C3B C3B 109.2(9) . 2_566 ?
N3 C3B H3BA 109.8 . . ?
N3 C3B H3BB 109.8 . . ?
C3B C3B H3BA 109.8 2_566 . ?
C3B C3B H3BB 109.8 2_566 . ?
H3BA C3B H3BB 108.3 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4A N4 H4D 103.1 . . ?
H4B N4 H4C 114.8 . . ?
H4B N4 H4D 109.6 . . ?
H4C N4 H4D 109.6 . . ?
H15A O15B H15B 109.5 . . ?
H14A O14 H14B 109.4 . . ?
H15C O15A H15D 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 N1 C1 C2 31.4(5) . . . . ?
Cu1 N2 C2 C1 41.7(5) . . . . ?
O1 Mo3 O8 Mo2 53.8(4) 2_667 . . . ?
O5 Mo2 O4 Mo1 -16.46(14) . . . . ?
O5 V1 O11 Mo1 126.3(2) . . . 2_667 ?
O5 V1 O11 Mo3 -9.1(2) . . . . ?
O5 V1 O13 Mo2 -127.6(2) . . . 2_667 ?
O5 V1 O13 Mo3 1.4(2) . . . 2_667 ?
O6 Mo2 O4 Mo1 73.03(18) . . . . ?
O7 Mo2 O4 Mo1 179.32(16) . . . . ?
O8 Mo2 O4 Mo1 -52.8(3) . . . . ?
O9 Mo3 O8 Mo2 -70.0(2) . . . . ?
O10 Mo3 O8 Mo2 -176.59(18) . . . . ?
O11 Mo3 O8 Mo2 94.82(17) . . . . ?
O11 V1 O5 Mo1 -127.1(2) . . . . ?
O11 V1 O5 Mo2 6.1(2) . . . . ?
O11 V1 O13 Mo2 -3.4(3) . . . 2_667 ?
O11 V1 O13 Mo3 125.57(19) . . . 2_667 ?
O12 V1 O5 Mo1 114.1(2) . . . . ?
O12 V1 O5 Mo2 -112.7(2) . . . . ?
O12 V1 O11 Mo1 -112.7(2) . . . 2_667 ?
O12 V1 O11 Mo3 111.9(2) . . . . ?
O12 V1 O13 Mo2 111.7(2) . . . 2_667 ?
O12 V1 O13 Mo3 -119.3(2) . . . 2_667 ?
O13 Mo2 O4 Mo1 -93.90(16) 2_667 . . . ?
O13 Mo3 O8 Mo2 18.01(14) 2_667 . . . ?
O13 V1 O5 Mo1 -5.1(3) . . . . ?
O13 V1 O5 Mo2 128.05(18) . . . . ?
O13 V1 O11 Mo1 3.3(3) . . . 2_667 ?
O13 V1 O11 Mo3 -132.09(18) . . . . ?
N1 C1 C2 N2 -49.2(6) . . . . ?


_olex2_date_sample_data_collection 2015-10-05
_olex2_date_sample_submission    2015-10-01
_olex2_submission_original_sample_id koko663
_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_koko786red
_database_code_depnum_ccdc_archive 'CCDC 1882182'
loop_
_audit_author_name
_audit_author_address
'Iryna Omelchenko'
;SSI Institute for Single Crystals, Kharkiv
Ukraine
;
_audit_update_record             
;
2018-11-29 deposited with the CCDC.	2019-05-27 downloaded from the CCDC.
;
_audit_creation_date             2018-11-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
loop_
_audit_author_email
''
kokozay@univ.kiev.ua
irina@xray.isc.kharkov.com
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H30 Cu2 Mo6 N6 O28 V2, 2(H4 N), 8(H2 O)'
_chemical_formula_sum            'C8 H54 Cu2 Mo6 N8 O36 V2'
_chemical_formula_weight         1643.19
_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'
Cu Cu 0.3201 1.2651 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.2569(3)
_cell_length_b                   9.1947(2)
_cell_length_c                   21.9132(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.328(2)
_cell_angle_gamma                90
_cell_volume                     2238.11(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5954
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.4350
_cell_measurement_theta_min      3.5860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.3
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19449
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         32.268
_diffrn_reflns_theta_min         2.876
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -86.00  -38.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.2300 -178.0000 -180.0000 48

#__ type_ start__ end____ width___ exp.time_
  2 omega   27.00   69.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363   57.0000  150.0000 42

#__ type_ start__ end____ width___ exp.time_
  3 omega   -3.00   44.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363   77.0000 -150.0000 47

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00   44.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363   59.0000  -79.0000 34

#__ type_ start__ end____ width___ exp.time_
  5 omega  -42.00   57.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363  -77.0000   60.0000 99

#__ type_ start__ end____ width___ exp.time_
  6 omega    5.00   95.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363   57.0000   30.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0105267000
_diffrn_orient_matrix_UB_12      0.0459844000
_diffrn_orient_matrix_UB_13      0.0262718000
_diffrn_orient_matrix_UB_21      0.0525512000
_diffrn_orient_matrix_UB_22      0.0276253000
_diffrn_orient_matrix_UB_23      -0.0099743000
_diffrn_orient_matrix_UB_31      -0.0348151000
_diffrn_orient_matrix_UB_32      0.0553952000
_diffrn_orient_matrix_UB_33      -0.0168946000
_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_source_target            Mo
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5746
_reflns_number_total             7174
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.971
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         7174
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.042
_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)+(0.0446P)²+3.3013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1048
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All N(H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N1S-H1SC = N1S-H1SD
 0.85 with sigma of 0.01
 N1S-H1SF = N1S-H1SE
 0.85 with sigma of 0.01
 H1SF-H1SE \\sim H1SF-H1SC \\sim H1SE-H1SC \\sim H1SE-H1SD \\sim H1SF-H1SD
 with sigma of 0.01
 H1SC-H1SD \\sim H1SD-H1SF
 with sigma of 0.01
 H1SD-H1SC \\sim H1SC-H1SE
 with sigma of 0.01
3.a Riding coordinates:
 O1S(H1SA,H1SB), N1S(H1SC,H1SD,H1SE,H1SF), O4S(H4SA,H4SB), O2S(H2SA,H2SB),
 O3S(H3SA,H3SB), O5S(H5SA,H5SB)
3.b Ternary CH refined with riding coordinates:
 N2(H2)
3.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B), C1(H1C,H1D), C3(H3C,H3D), C4(H4A,H4B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.26630(3) 0.30343(3) 0.44459(2) 0.02340(8) Uani 1 1 d . . . . .
Mo2 Mo 0.45551(3) 0.40761(3) 0.35440(2) 0.02205(8) Uani 1 1 d . . . . .
Mo3 Mo 0.68628(3) 0.60605(4) 0.40953(2) 0.02336(8) Uani 1 1 d . . . . .
Cu1 Cu 0.53242(5) -0.00610(6) 0.33796(2) 0.02903(12) Uani 1 1 d . . . . .
V1 V 0.58369(5) 0.34870(6) 0.51861(3) 0.01781(12) Uani 1 1 d . . . . .
O1 O 0.5125(2) 0.3947(3) 0.58210(12) 0.0235(5) Uani 1 1 d . . . . .
O1S O 0.5366(4) 0.0040(4) 0.42790(17) 0.0562(10) Uani 1 1 d . . . . .
H1SA H 0.581270 -0.064044 0.445554 0.084 Uiso 1 1 d R . . . .
H1SB H 0.465480 -0.006004 0.436174 0.084 Uiso 1 1 d R . . . .
O2 O 0.6821(2) 0.4862(3) 0.50114(12) 0.0230(5) Uani 1 1 d . . . . .
O3 O 0.6619(3) 0.2018(3) 0.53616(14) 0.0319(6) Uani 1 1 d . . . . .
O4 O 0.4752(2) 0.3120(3) 0.45365(12) 0.0244(5) Uani 1 1 d . . . . .
O5 O 0.3081(3) 0.2446(3) 0.52871(12) 0.0256(5) Uani 1 1 d . . . . .
O6 O 0.1177(3) 0.3463(3) 0.44196(14) 0.0340(7) Uani 1 1 d . . . . .
O7 O 0.2644(3) 0.1343(3) 0.41142(14) 0.0357(7) Uani 1 1 d . . . . .
O8 O 0.2985(2) 0.4229(3) 0.37781(12) 0.0244(5) Uani 1 1 d . . . . .
O9 O 0.4473(3) 0.2353(3) 0.32462(13) 0.0314(6) Uani 1 1 d . . . . .
O10 O 0.4294(3) 0.5182(3) 0.29072(13) 0.0308(6) Uani 1 1 d . . . . .
O11 O 0.6269(2) 0.4226(3) 0.37507(12) 0.0261(6) Uani 1 1 d . . . . .
O12 O 0.8375(3) 0.5690(4) 0.41664(14) 0.0343(7) Uani 1 1 d . . . . .
O13 O 0.6573(3) 0.7183(3) 0.34681(13) 0.0347(7) Uani 1 1 d . . . . .
N1 N 0.6925(4) 0.0942(5) 0.3376(2) 0.0442(10) Uani 1 1 d . . . . .
H1A H 0.692273 0.181369 0.355300 0.053 Uiso 1 1 calc R . . . .
H1B H 0.751732 0.041782 0.358840 0.053 Uiso 1 1 calc R . . . .
N2 N 0.5290(3) -0.0256(4) 0.24742(16) 0.0322(8) Uani 1 1 d . . . . .
H2 H 0.485091 0.057770 0.227023 0.039 Uiso 1 1 calc R . . . .
N3 N 0.3927(3) -0.1457(4) 0.32408(18) 0.0360(8) Uani 1 1 d . . . . .
H3A H 0.415385 -0.231995 0.340327 0.043 Uiso 1 1 calc R . . . .
H3B H 0.333001 -0.112472 0.342326 0.043 Uiso 1 1 calc R . . . .
C1 C 0.7110(5) 0.1095(6) 0.2730(3) 0.0587(16) Uani 1 1 d . . . . .
H1C H 0.796496 0.112350 0.271078 0.070 Uiso 1 1 calc R . . . .
H1D H 0.675106 0.199507 0.255790 0.070 Uiso 1 1 calc R . . . .
C2 C 0.6538(5) -0.0174(6) 0.2365(3) 0.0488(13) Uani 1 1 d . . . . .
H2A H 0.654(5) -0.011(6) 0.192(3) 0.059 Uiso 1 1 d R . . . .
H2B H 0.690(5) -0.106(6) 0.257(3) 0.059 Uiso 1 1 d R . . . .
C3 C 0.4617(5) -0.1585(5) 0.2265(2) 0.0393(11) Uani 1 1 d . . . . .
H3C H 0.510578 -0.243928 0.238358 0.047 Uiso 1 1 calc R . . . .
H3D H 0.439128 -0.158014 0.181858 0.047 Uiso 1 1 calc R . . . .
C4 C 0.3515(5) -0.1602(5) 0.2568(2) 0.0424(11) Uani 1 1 d . . . . .
H4A H 0.298666 -0.080228 0.241735 0.051 Uiso 1 1 calc R . . . .
H4B H 0.307878 -0.250693 0.247812 0.051 Uiso 1 1 calc R . . . .
N1S N 0.9163(4) 0.3322(5) 0.5141(2) 0.0441(10) Uani 1 1 d D . . . .
H1SC H 0.935975 0.348956 0.552481 0.066 Uiso 1 1 d DR . . . .
H1SD H 0.976755 0.344596 0.496061 0.066 Uiso 1 1 d DR . . . .
H1SE H 0.891255 0.245156 0.508751 0.066 Uiso 1 1 d DR . . . .
H1SF H 0.860325 0.390216 0.498821 0.066 Uiso 1 1 d DR . . . .
O4S O 0.9039(4) -0.1125(5) 0.3824(3) 0.0789(15) Uani 1 1 d . . . . .
H4SA H 0.883503 -0.205969 0.372086 0.118 Uiso 1 1 d R . . . .
H4SB H 0.964753 -0.097559 0.363166 0.118 Uiso 1 1 d R . . . .
O2S O 0.1165(3) -0.0524(4) 0.33535(16) 0.0484(9) Uani 1 1 d . . . . .
H2SA H 0.145981 0.018232 0.357826 0.073 Uiso 1 1 d R . . . .
H2SB H 0.101711 -0.025328 0.297826 0.073 Uiso 1 1 d R . . . .
O3S O 0.3827(3) 0.1441(4) 0.14683(17) 0.0475(9) Uani 1 1 d . . . . .
H3SA H 0.320957 0.090115 0.138255 0.071 Uiso 1 1 d R . . . .
H3SB H 0.360787 0.230415 0.153355 0.071 Uiso 1 1 d R . . . .
O5S O 0.8578(5) 0.0430(5) 0.4871(3) 0.104(2) Uani 1 1 d . . . . .
H5SA H 0.819003 -0.006162 0.510190 0.156 Uiso 1 1 d R . . . .
H5SB H 0.864353 -0.005922 0.454970 0.156 Uiso 1 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O2 2.295(3) 3_666 ?
Mo1 O4 2.329(3) . ?
Mo1 O5 1.905(3) . ?
Mo1 O6 1.711(3) . ?
Mo1 O7 1.715(3) . ?
Mo1 O8 1.911(3) . ?
Mo2 O1 2.282(3) 3_666 ?
Mo2 O4 2.323(3) . ?
Mo2 O8 1.924(3) . ?
Mo2 O9 1.710(3) . ?
Mo2 O10 1.713(3) . ?
Mo2 O11 1.914(3) . ?
Mo3 O1 2.275(3) 3_666 ?
Mo3 O2 2.297(3) . ?
Mo3 O5 1.922(3) 3_666 ?
Mo3 O11 1.923(3) . ?
Mo3 O12 1.718(3) . ?
Mo3 O13 1.708(3) . ?
Cu1 O1S 1.966(4) . ?
Cu1 O9 2.417(3) . ?
Cu1 N1 2.026(4) . ?
Cu1 N2 1.986(4) . ?
Cu1 N3 2.014(4) . ?
V1 O1 1.766(3) . ?
V1 O2 1.763(3) . ?
V1 O3 1.624(3) . ?
V1 O4 1.752(3) . ?
O1S H1SA 0.8545 . ?
O1S H1SB 0.8543 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.472(7) . ?
N2 H2 0.9800 . ?
N2 C2 1.465(7) . ?
N2 C3 1.471(6) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C4 1.478(6) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.500(8) . ?
C2 H2A 0.98(6) . ?
C2 H2B 0.99(6) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C3 C4 1.498(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N1S H1SC 0.8474 . ?
N1S H1SD 0.8484 . ?
N1S H1SE 0.8508 . ?
N1S H1SF 0.8519 . ?
O4S H4SA 0.9083 . ?
O4S H4SB 0.8718 . ?
O2S H2SA 0.8499 . ?
O2S H2SB 0.8494 . ?
O3S H3SA 0.8501 . ?
O3S H3SB 0.8500 . ?
O5S H5SA 0.8499 . ?
O5S H5SB 0.8497 . ?

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 O4 76.12(9) 3_666 . ?
O5 Mo1 O2 74.69(10) . 3_666 ?
O5 Mo1 O4 80.77(11) . . ?
O5 Mo1 O8 148.90(11) . . ?
O6 Mo1 O2 89.28(13) . 3_666 ?
O6 Mo1 O4 164.49(13) . . ?
O6 Mo1 O5 100.65(13) . . ?
O6 Mo1 O7 104.44(15) . . ?
O6 Mo1 O8 98.49(13) . . ?
O7 Mo1 O2 165.53(13) . 3_666 ?
O7 Mo1 O4 90.57(13) . . ?
O7 Mo1 O5 97.87(13) . . ?
O7 Mo1 O8 100.82(13) . . ?
O8 Mo1 O2 81.30(10) . 3_666 ?
O8 Mo1 O4 74.43(10) . . ?
O1 Mo2 O4 75.45(9) 3_666 . ?
O8 Mo2 O1 80.80(10) . 3_666 ?
O8 Mo2 O4 74.36(10) . . ?
O9 Mo2 O1 164.57(12) . 3_666 ?
O9 Mo2 O4 89.86(12) . . ?
O9 Mo2 O8 100.05(13) . . ?
O9 Mo2 O10 104.34(14) . . ?
O9 Mo2 O11 98.47(13) . . ?
O10 Mo2 O1 90.75(12) . 3_666 ?
O10 Mo2 O4 164.80(12) . . ?
O10 Mo2 O8 97.46(13) . . ?
O10 Mo2 O11 100.57(13) . . ?
O11 Mo2 O1 75.21(10) . 3_666 ?
O11 Mo2 O4 82.31(11) . . ?
O11 Mo2 O8 150.00(11) . . ?
O1 Mo3 O2 76.59(9) 3_666 . ?
O5 Mo3 O1 82.30(11) 3_666 3_666 ?
O5 Mo3 O2 74.35(10) 3_666 . ?
O5 Mo3 O11 150.79(12) 3_666 . ?
O11 Mo3 O1 75.22(10) . 3_666 ?
O11 Mo3 O2 82.38(10) . . ?
O12 Mo3 O1 164.85(13) . 3_666 ?
O12 Mo3 O2 89.21(13) . . ?
O12 Mo3 O5 99.13(13) . 3_666 ?
O12 Mo3 O11 97.94(13) . . ?
O13 Mo3 O1 90.29(13) . 3_666 ?
O13 Mo3 O2 164.82(13) . . ?
O13 Mo3 O5 96.61(13) . 3_666 ?
O13 Mo3 O11 101.85(13) . . ?
O13 Mo3 O12 104.46(15) . . ?
O1S Cu1 O9 91.30(13) . . ?
O1S Cu1 N1 96.03(18) . . ?
O1S Cu1 N2 177.49(15) . . ?
O1S Cu1 N3 94.17(17) . . ?
N1 Cu1 O9 85.23(15) . . ?
N2 Cu1 O9 91.09(12) . . ?
N2 Cu1 N1 84.90(17) . . ?
N2 Cu1 N3 84.45(16) . . ?
N3 Cu1 O9 106.41(13) . . ?
N3 Cu1 N1 164.34(17) . . ?
O2 V1 O1 112.36(12) . . ?
O3 V1 O1 108.10(14) . . ?
O3 V1 O2 108.19(14) . . ?
O3 V1 O4 108.18(14) . . ?
O4 V1 O1 109.92(13) . . ?
O4 V1 O2 109.97(12) . . ?
Mo3 O1 Mo2 90.77(9) 3_666 3_666 ?
V1 O1 Mo2 128.64(14) . 3_666 ?
V1 O1 Mo3 129.85(14) . 3_666 ?
Cu1 O1S H1SA 109.6 . . ?
Cu1 O1S H1SB 109.7 . . ?
H1SA O1S H1SB 109.2 . . ?
Mo1 O2 Mo3 90.53(9) 3_666 . ?
V1 O2 Mo1 127.37(14) . 3_666 ?
V1 O2 Mo3 129.51(13) . . ?
Mo2 O4 Mo1 89.50(9) . . ?
V1 O4 Mo1 129.58(14) . . ?
V1 O4 Mo2 129.50(14) . . ?
Mo1 O5 Mo3 116.95(13) . 3_666 ?
Mo1 O8 Mo2 117.29(13) . . ?
Mo2 O9 Cu1 143.99(16) . . ?
Mo2 O11 Mo3 115.42(13) . . ?
Cu1 N1 H1A 110.1 . . ?
Cu1 N1 H1B 110.1 . . ?
H1A N1 H1B 108.4 . . ?
C1 N1 Cu1 108.2(3) . . ?
C1 N1 H1A 110.1 . . ?
C1 N1 H1B 110.1 . . ?
Cu1 N2 H2 108.2 . . ?
C2 N2 Cu1 107.1(3) . . ?
C2 N2 H2 108.2 . . ?
C2 N2 C3 116.8(4) . . ?
C3 N2 Cu1 108.2(3) . . ?
C3 N2 H2 108.2 . . ?
Cu1 N3 H3A 110.0 . . ?
Cu1 N3 H3B 110.0 . . ?
H3A N3 H3B 108.3 . . ?
C4 N3 Cu1 108.6(3) . . ?
C4 N3 H3A 110.0 . . ?
C4 N3 H3B 110.0 . . ?
N1 C1 H1C 109.9 . . ?
N1 C1 H1D 109.9 . . ?
N1 C1 C2 108.8(4) . . ?
H1C C1 H1D 108.3 . . ?
C2 C1 H1C 109.9 . . ?
C2 C1 H1D 109.9 . . ?
N2 C2 C1 107.1(4) . . ?
N2 C2 H2A 109(4) . . ?
N2 C2 H2B 102(4) . . ?
C1 C2 H2A 115(3) . . ?
C1 C2 H2B 107(3) . . ?
H2A C2 H2B 116(5) . . ?
N2 C3 H3C 110.3 . . ?
N2 C3 H3D 110.3 . . ?
N2 C3 C4 107.0(4) . . ?
H3C C3 H3D 108.6 . . ?
C4 C3 H3C 110.3 . . ?
C4 C3 H3D 110.3 . . ?
N3 C4 C3 107.0(4) . . ?
N3 C4 H4A 110.3 . . ?
N3 C4 H4B 110.3 . . ?
C3 C4 H4A 110.3 . . ?
C3 C4 H4B 110.3 . . ?
H4A C4 H4B 108.6 . . ?
H1SC N1S H1SD 109.8 . . ?
H1SC N1S H1SE 109.6 . . ?
H1SC N1S H1SF 109.6 . . ?
H1SD N1S H1SE 109.5 . . ?
H1SD N1S H1SF 109.3 . . ?
H1SE N1S H1SF 109.1 . . ?
H4SA O4S H4SB 102.5 . . ?
H2SA O2S H2SB 109.5 . . ?
H3SA O3S H3SB 109.4 . . ?
H5SA O5S H5SB 109.4 . . ?


_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_koko786green
_database_code_depnum_ccdc_archive 'CCDC 1882181'
loop_
_audit_author_name
_audit_author_address
'Iryna Omelchenko'
;SSI Institute for Single Crystals, Kharkiv
Ukraine
;
_audit_update_record             
;
2018-11-29 deposited with the CCDC.	2019-05-27 downloaded from the CCDC.
;
_audit_creation_date             2018-11-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
loop_
_audit_author_email
''
kokozay@univ.kiev.ua
irina@xray.isc.kharkov.com
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H30 Cu2 Mo6 N6 O28 V2, 2(H4 N), 5(H2 O)'
_chemical_formula_sum            'C8 H48 Cu2 Mo6 N8 O33 V2'
_chemical_formula_weight         1589.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         'V2 C10 N4 O20 H10 Mo6 Cu2'
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'
Cu Cu 0.3201 1.2651 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   11.8618(8)
_cell_length_b                   23.2484(12)
_cell_length_c                   15.7977(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4356.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1102
_cell_measurement_temperature    298
_cell_measurement_theta_max      19.1880
_cell_measurement_theta_min      3.1170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.132
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34175
_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            'dull light green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.423
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1797
_diffrn_reflns_av_unetI/netI     0.1658
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30081
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         30.303
_diffrn_reflns_theta_min         3.098
_diffrn_ambient_temperature      298.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -93.00   25.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3633    0.0000 -150.0000 118

#__ type_ start__ end____ width___ exp.time_
  2 omega  -23.00   22.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3633  -99.0000  -30.0000 45

#__ type_ start__ end____ width___ exp.time_
  3 omega   35.00   79.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6133  178.0000   90.0000 44

#__ type_ start__ end____ width___ exp.time_
  4 omega    6.00   47.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6133   57.0000  -90.0000 41

#__ type_ start__ end____ width___ exp.time_
  5 omega  -42.00  -13.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6133  -57.0000 -150.0000 29

#__ type_ start__ end____ width___ exp.time_
  6 omega   -4.00   54.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6133   37.0000  150.0000 58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0390692000
_diffrn_orient_matrix_UB_12      -0.0195381000
_diffrn_orient_matrix_UB_13      -0.0181018000
_diffrn_orient_matrix_UB_21      -0.0402054000
_diffrn_orient_matrix_UB_22      -0.0224528000
_diffrn_orient_matrix_UB_23      0.0035902000
_diffrn_orient_matrix_UB_31      -0.0207815000
_diffrn_orient_matrix_UB_32      0.0066708000
_diffrn_orient_matrix_UB_33      -0.0409496000
_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_source_target            Mo
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2707
_reflns_number_total             5929
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5929
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1731
_refine_ls_R_factor_gt           0.0626
_refine_ls_restrained_S_all      0.953
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0210P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1247
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All N(H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H3SC-N3S
 0.85 with sigma of 0.01
 N3S-H3SD
 0.85 with sigma of 0.01
 N3S-H3SB = N3S-H3SA
 0.85 with sigma of 0.01
 O1S-H1SB = O1S-H1SA
 0.9 with sigma of 0.01
 H3SA-H3SB \\sim H3SB-H3SC
 with sigma of 0.01
 H3SA-H3SB \\sim H3SB-H3SD
 with sigma of 0.01
 H3SB-H3SD \\sim H3SD-H3SC
 with sigma of 0.01
 H3SD-H3SC \\sim H3SC-H3SB
 with sigma of 0.01
 H3SD-H3SC \\sim H3SC-H3SA
 with sigma of 0.01
 H3SA-H3SD \\sim H3SD-H3SB
 with sigma of 0.01
 H3SA-H3SD \\sim H3SD-H3SC
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6S) \\sim Ueq, Uanis(O7S) \\sim Ueq, Uanis(O4S) \\sim Ueq, Uanis(O5S)
\\sim Ueq, Uanis(O8S) \\sim Ueq, Uanis(O9S) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.03
4. Others
 Fixed Sof: O4S(0.75) H4SA(0.75) H4SB(0.75) O5S(0.25) H5SA(0.25) H5SB(0.25)
 O6S(0.3) H6SA(0.3) H6SB(0.3) O7S(0.7) H7SA(0.7) H7SB(0.7) O8S(0.07) H8SA(0.07)
 H8SB(0.07) O9S(0.35) H9SA(0.35) H9SB(0.35) O0AA(0.08) H0AA(0.08) H0AB(0.08)
5.a Riding coordinates:
 O1S(H1SA,H1SB), N3S(H3SA,H3SB,H3SC,H3SD), O4S(H4SA,H4SB), O5S(H5SA,H5SB),
 O6S(H6SA,H6SB), O7S(H7SA,H7SB), O8S(H8SA,H8SB), O9S(H9SA,H9SB), O0AA(H0AA,H0AB)
5.b Ternary CH refined with riding coordinates:
 N2(H2)
5.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B), C1(H1C,H1D), C2(H2A,H2B), C3(H3C,H3D), C4(H4A,H4B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 1.12782(7) 0.88245(3) 0.56037(5) 0.0375(2) Uani 1 1 d . . . . .
Mo2 Mo 0.85512(7) 0.89388(3) 0.58523(5) 0.0344(2) Uani 1 1 d . . . . .
Mo3 Mo 0.72715(7) 1.01288(3) 0.52524(5) 0.0326(2) Uani 1 1 d . . . . .
Cu1 Cu 0.97811(11) 0.86539(5) 0.25448(7) 0.0467(4) Uani 1 1 d . . . . .
V1 V 0.97879(13) 0.97068(6) 0.40131(9) 0.0300(4) Uani 1 1 d . . . . .
O1 O 0.9548(5) 0.9421(2) 0.3067(4) 0.0404(16) Uani 1 1 d . . . . .
O1S O 1.1692(6) 0.8721(3) 0.2998(4) 0.080(3) Uani 1 1 d D . . . .
H1SA H 1.203760 0.866566 0.250991 0.119 Uiso 1 1 d DR . . . .
H1SB H 1.191460 0.844806 0.330871 0.119 Uiso 1 1 d DR . . . .
O2 O 0.8679(5) 1.0185(2) 0.4226(3) 0.0337(14) Uani 1 1 d . . . . .
O3 O 0.9828(5) 0.9172(2) 0.4770(3) 0.0322(14) Uani 1 1 d . . . . .
O4 O 1.1076(5) 1.0066(2) 0.3996(3) 0.0308(14) Uani 1 1 d . . . . .
O5 O 1.2304(5) 0.8760(3) 0.6352(4) 0.0522(19) Uani 1 1 d . . . . .
O6 O 1.1087(6) 0.8144(2) 0.5239(4) 0.0493(18) Uani 1 1 d . . . . .
O7 O 1.0014(5) 0.8894(2) 0.6351(3) 0.0364(15) Uani 1 1 d . . . . .
O8 O 0.8408(5) 0.8275(2) 0.5455(3) 0.0443(17) Uani 1 1 d . . . . .
O9 O 0.7772(5) 0.8941(3) 0.6751(4) 0.0442(17) Uani 1 1 d . . . . .
O10 O 0.7524(5) 0.9326(2) 0.5099(3) 0.0342(15) Uani 1 1 d . . . . .
O11 O 0.6541(5) 1.0126(2) 0.6185(3) 0.0391(15) Uani 1 1 d . . . . .
O12 O 0.7866(5) 1.0895(2) 0.5337(3) 0.0321(14) Uani 1 1 d . . . . .
O13 O 0.6292(5) 1.0219(2) 0.4483(3) 0.0434(16) Uani 1 1 d . . . . .
N1 N 0.9288(9) 0.8209(3) 0.3562(5) 0.070(3) Uani 1 1 d . . . . .
H1A H 0.963758 0.834039 0.402082 0.084 Uiso 1 1 calc R . . . .
H1B H 0.854878 0.824887 0.363644 0.084 Uiso 1 1 calc R . . . .
N2 N 0.9911(8) 0.7892(3) 0.1971(5) 0.060(3) Uani 1 1 d . . . . .
H2 H 1.071264 0.779097 0.194575 0.072 Uiso 1 1 calc R . . . .
N3 N 0.9803(6) 0.8961(3) 0.1381(4) 0.045(2) Uani 1 1 d . . . . .
H3A H 0.915781 0.914270 0.127621 0.053 Uiso 1 1 calc R . . . .
H3B H 1.036214 0.921419 0.133009 0.053 Uiso 1 1 calc R . . . .
C1 C 0.9567(13) 0.7596(4) 0.3432(7) 0.096(5) Uani 1 1 d . . . . .
H1C H 0.910397 0.735543 0.379475 0.115 Uiso 1 1 calc R . . . .
H1D H 1.035295 0.752544 0.356684 0.115 Uiso 1 1 calc R . . . .
C2 C 0.9340(13) 0.7461(5) 0.2513(8) 0.096(5) Uani 1 1 d . . . . .
H2A H 0.961692 0.707903 0.237969 0.115 Uiso 1 1 calc R . . . .
H2B H 0.853450 0.746858 0.240694 0.115 Uiso 1 1 calc R . . . .
C3 C 0.9505(10) 0.7953(4) 0.1107(6) 0.059(3) Uani 1 1 d . . . . .
H3C H 0.868709 0.796362 0.110109 0.071 Uiso 1 1 calc R . . . .
H3D H 0.975150 0.762950 0.076725 0.071 Uiso 1 1 calc R . . . .
C4 C 0.9960(8) 0.8492(4) 0.0759(6) 0.050(3) Uani 1 1 d . . . . .
H4A H 0.957311 0.858644 0.023604 0.060 Uiso 1 1 calc R . . . .
H4B H 1.075541 0.844514 0.063441 0.060 Uiso 1 1 calc R . . . .
N3S N 0.7161(7) 1.0008(3) 0.2760(4) 0.059(3) Uani 1 1 d D . . . .
H3SA H 0.748974 1.004824 0.323397 0.089 Uiso 1 1 d DR . . . .
H3SB H 0.759504 0.983174 0.241877 0.089 Uiso 1 1 d DR . . . .
H3SC H 0.655834 0.981494 0.282597 0.089 Uiso 1 1 d DR . . . .
H3SD H 0.700034 1.033754 0.255867 0.089 Uiso 1 1 d DR . . . .
O4S O 0.5255(9) 0.9311(4) 0.3012(7) 0.063(3) Uani 0.75 1 d . U . A 1
H4SA H 0.493432 0.918435 0.256866 0.095 Uiso 0.75 1 d R . . A 1
H4SB H 0.476132 0.944455 0.334856 0.095 Uiso 0.75 1 d R . . A 1
O5S O 0.480(4) 0.8965(15) 0.302(3) 0.102(15) Uani 0.25 1 d . U . B 2
H5SA H 0.434828 0.907162 0.341102 0.153 Uiso 0.25 1 d R . . B 2
H5SB H 0.451518 0.867932 0.276052 0.153 Uiso 0.25 1 d R . . B 2
O6S O 0.673(5) 0.8783(19) 0.363(3) 0.104(19) Uani 0.3 1 d . U . C 2
H6SA H 0.678476 0.877874 0.418752 0.156 Uiso 0.3 1 d R . . C 2
H6SB H 0.605846 0.883314 0.346392 0.156 Uiso 0.3 1 d R . . C 2
O7S O 0.6957(17) 0.8571(7) 0.3770(12) 0.083(6) Uani 0.7 1 d . U . D 1
H7SA H 0.626216 0.859586 0.362624 0.125 Uiso 0.7 1 d R . . D 1
H7SB H 0.714356 0.888506 0.403494 0.125 Uiso 0.7 1 d R . . D 1
O8S O 1.250000 0.750000 0.734(4) 0.05(2) Uani 0.14 2 d S TU P E 2
H8SA H 1.217660 0.778650 0.711409 0.079 Uiso 0.07 1 d R . . E 2
H8SB H 1.268310 0.726780 0.694359 0.079 Uiso 0.07 1 d R . . E 2
O9S O 1.250000 0.750000 0.6709(10) 0.067(5) Uani 0.7 2 d S TU P F 1
H9SA H 1.266540 0.721360 0.639878 0.101 Uiso 0.35 1 d R . . F 1
H9SB H 1.233460 0.778640 0.639878 0.101 Uiso 0.35 1 d R . . F 1
O0AA O 1.250000 0.750000 0.392(3) 0.048(15) Uani 0.16 2 d S TU P G 3
H0AA H 1.191480 0.750000 0.422818 0.072 Uiso 0.08 1 d R . . G 3
H0AB H 1.308520 0.750000 0.422818 0.072 Uiso 0.08 1 d R . . G 3


_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 2.320(5) 5_776 ?
Mo1 O3 2.312(6) . ?
Mo1 O5 1.704(6) . ?
Mo1 O6 1.700(6) . ?
Mo1 O7 1.915(6) . ?
Mo1 O12 1.915(5) 5_776 ?
Mo2 O3 2.348(5) . ?
Mo2 O4 2.368(5) 5_776 ?
Mo2 O7 1.909(6) . ?
Mo2 O8 1.675(6) . ?
Mo2 O9 1.694(6) . ?
Mo2 O10 1.926(6) . ?
Mo3 O2 2.331(5) . ?
Mo3 O4 2.336(5) 5_776 ?
Mo3 O10 1.906(5) . ?
Mo3 O11 1.709(6) . ?
Mo3 O12 1.920(5) . ?
Mo3 O13 1.694(6) . ?
Cu1 O1 1.983(6) . ?
Cu1 O1S 2.382(8) . ?
Cu1 N1 1.998(7) . ?
Cu1 N2 1.996(8) . ?
Cu1 N3 1.972(7) . ?
V1 O1 1.661(6) . ?
V1 O2 1.754(6) . ?
V1 O3 1.726(5) . ?
V1 O4 1.741(6) . ?
O1S H1SA 0.8831 . ?
O1S H1SB 0.8442 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.477(12) . ?
N2 H2 0.9800 . ?
N2 C2 1.481(12) . ?
N2 C3 1.455(11) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C4 1.481(10) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.510(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C3 C4 1.470(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N3S H3SA 0.8498 . ?
N3S H3SB 0.8502 . ?
N3S H3SC 0.8505 . ?
N3S H3SD 0.8511 . ?
O4S H4SA 0.8502 . ?
O4S H4SB 0.8498 . ?
O5S H5SA 0.8498 . ?
O5S H5SB 0.8505 . ?
O6S H6SA 0.8857 . ?
O6S H6SB 0.8500 . ?
O7S H7SA 0.8570 . ?
O7S H7SB 0.8698 . ?
O8S H8SA 0.8489 . ?
O8S H8SA 0.8489 2_765 ?
O8S H8SB 0.8574 . ?
O8S H8SB 0.8575 2_765 ?
O9S H9SA 0.8501 . ?
O9S H9SB 0.8501 . ?
O0AA H0AA 0.8503 . ?
O0AA H0AB 0.8502 . ?

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 Mo1 O2 74.67(18) . 5_776 ?
O5 Mo1 O2 89.5(3) . 5_776 ?
O5 Mo1 O3 163.3(3) . . ?
O5 Mo1 O7 98.0(3) . . ?
O5 Mo1 O12 101.0(3) . 5_776 ?
O6 Mo1 O2 165.2(3) . 5_776 ?
O6 Mo1 O3 91.9(3) . . ?
O6 Mo1 O5 104.4(3) . . ?
O6 Mo1 O7 100.5(3) . . ?
O6 Mo1 O12 97.2(3) . 5_776 ?
O7 Mo1 O2 82.1(2) . 5_776 ?
O7 Mo1 O3 74.9(2) . . ?
O7 Mo1 O12 149.9(2) . 5_776 ?
O12 Mo1 O2 74.9(2) 5_776 5_776 ?
O12 Mo1 O3 80.4(2) 5_776 . ?
O3 Mo2 O4 74.19(18) . 5_776 ?
O7 Mo2 O3 74.2(2) . . ?
O7 Mo2 O4 80.9(2) . 5_776 ?
O7 Mo2 O10 148.8(2) . . ?
O8 Mo2 O3 90.3(2) . . ?
O8 Mo2 O4 163.2(2) . 5_776 ?
O8 Mo2 O7 101.3(3) . . ?
O8 Mo2 O9 105.2(3) . . ?
O8 Mo2 O10 97.8(3) . . ?
O9 Mo2 O3 164.1(2) . . ?
O9 Mo2 O4 90.8(2) . 5_776 ?
O9 Mo2 O7 98.6(3) . . ?
O9 Mo2 O10 99.9(3) . . ?
O10 Mo2 O3 81.4(2) . . ?
O10 Mo2 O4 74.0(2) . 5_776 ?
O2 Mo3 O4 76.33(18) . 5_776 ?
O10 Mo3 O2 81.6(2) . . ?
O10 Mo3 O4 75.1(2) . 5_776 ?
O10 Mo3 O12 149.3(2) . . ?
O11 Mo3 O2 164.4(2) . . ?
O11 Mo3 O4 89.2(2) . 5_776 ?
O11 Mo3 O10 100.7(3) . . ?
O11 Mo3 O12 97.4(3) . . ?
O12 Mo3 O2 74.6(2) . . ?
O12 Mo3 O4 80.6(2) . 5_776 ?
O13 Mo3 O2 89.2(2) . . ?
O13 Mo3 O4 164.6(2) . 5_776 ?
O13 Mo3 O10 97.9(3) . . ?
O13 Mo3 O11 105.7(3) . . ?
O13 Mo3 O12 100.8(3) . . ?
O1 Cu1 O1S 87.1(3) . . ?
O1 Cu1 N1 95.2(3) . . ?
O1 Cu1 N2 175.8(3) . . ?
N1 Cu1 O1S 94.0(3) . . ?
N2 Cu1 O1S 96.9(3) . . ?
N2 Cu1 N1 85.8(3) . . ?
N3 Cu1 O1 93.7(3) . . ?
N3 Cu1 O1S 104.1(3) . . ?
N3 Cu1 N1 160.2(4) . . ?
N3 Cu1 N2 84.1(3) . . ?
O1 V1 O2 107.3(3) . . ?
O1 V1 O3 109.9(3) . . ?
O1 V1 O4 109.2(3) . . ?
O3 V1 O2 110.1(3) . . ?
O3 V1 O4 109.4(3) . . ?
O4 V1 O2 110.9(3) . . ?
V1 O1 Cu1 135.3(3) . . ?
Cu1 O1S H1SA 99.8 . . ?
Cu1 O1S H1SB 115.1 . . ?
H1SA O1S H1SB 104.7 . . ?
Mo1 O2 Mo3 89.44(19) 5_776 . ?
V1 O2 Mo1 129.4(3) . 5_776 ?
V1 O2 Mo3 129.4(3) . . ?
Mo1 O3 Mo2 89.11(18) . . ?
V1 O3 Mo1 131.8(3) . . ?
V1 O3 Mo2 130.8(3) . . ?
Mo3 O4 Mo2 88.91(19) 5_776 5_776 ?
V1 O4 Mo2 129.1(3) . 5_776 ?
V1 O4 Mo3 129.4(3) . 5_776 ?
Mo2 O7 Mo1 117.5(3) . . ?
Mo3 O10 Mo2 118.6(3) . . ?
Mo1 O12 Mo3 117.2(3) 5_776 . ?
Cu1 N1 H1A 109.9 . . ?
Cu1 N1 H1B 109.9 . . ?
H1A N1 H1B 108.3 . . ?
C1 N1 Cu1 108.9(6) . . ?
C1 N1 H1A 109.9 . . ?
C1 N1 H1B 109.9 . . ?
Cu1 N2 H2 107.8 . . ?
C2 N2 Cu1 107.6(6) . . ?
C2 N2 H2 107.8 . . ?
C3 N2 Cu1 108.2(6) . . ?
C3 N2 H2 107.8 . . ?
C3 N2 C2 117.2(9) . . ?
Cu1 N3 H3A 109.5 . . ?
Cu1 N3 H3B 109.5 . . ?
H3A N3 H3B 108.1 . . ?
C4 N3 Cu1 110.7(6) . . ?
C4 N3 H3A 109.5 . . ?
C4 N3 H3B 109.5 . . ?
N1 C1 H1C 110.3 . . ?
N1 C1 H1D 110.3 . . ?
N1 C1 C2 107.0(10) . . ?
H1C C1 H1D 108.6 . . ?
C2 C1 H1C 110.3 . . ?
C2 C1 H1D 110.3 . . ?
N2 C2 C1 109.5(10) . . ?
N2 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 H3C 110.0 . . ?
N2 C3 H3D 110.0 . . ?
N2 C3 C4 108.3(8) . . ?
H3C C3 H3D 108.4 . . ?
C4 C3 H3C 110.0 . . ?
C4 C3 H3D 110.0 . . ?
N3 C4 H4A 109.8 . . ?
N3 C4 H4B 109.8 . . ?
C3 C4 N3 109.4(8) . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
H3SA N3S H3SB 109.5 . . ?
H3SA N3S H3SC 109.6 . . ?
H3SA N3S H3SD 109.4 . . ?
H3SB N3S H3SC 109.4 . . ?
H3SB N3S H3SD 109.5 . . ?
H3SC N3S H3SD 109.4 . . ?
H4SA O4S H4SB 109.4 . . ?
H5SA O5S H5SB 109.5 . . ?
H6SA O6S H6SB 111.8 . . ?
H7SA O7S H7SB 108.4 . . ?
H8SA O8S H8SB 107.3 . . ?
H9SA O9S H8SA 76.0 . 2_765 ?
H9SA O9S H8SB 174.6 . 2_765 ?
H9SA O9S H9SB 109.5 . . ?
H9SB O9S H8SA 168.4 . 2_765 ?
H9SB O9S H8SB 67.9 . 2_765 ?
H0AA O0AA H0AB 109.5 . . ?


_olex2_submission_original_sample_id koko786green
_olex2_submission_special_instructions 'No special instructions were received'
