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

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

data_juc729
_database_code_depnum_ccdc_archive 'CCDC 2036291'
loop_
_audit_author_name
_audit_author_address
'Natalia Kuratieva'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2020-10-09 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'H10 I8 Mo6 O6, 2(N O3), 3(H2 O)'
_chemical_formula_sum            'H16 I8 Mo6 N2 O15'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         1874.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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                   10.5553(3)
_cell_length_b                   11.5145(3)
_cell_length_c                   12.9195(3)
_cell_angle_alpha                78.837(1)
_cell_angle_beta                 78.265(1)
_cell_angle_gamma                67.511(1)
_cell_volume                     1408.80(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8477
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.62
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.420
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   0.576
_exptl_transmission_factor_max   0.746
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    11.411
_shelx_estimated_absorpt_T_min   0.341
_shelx_estimated_absorpt_T_max   0.726


_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?


_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_reflns_number            12016
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.623
_diffrn_reflns_theta_max         27.619
_diffrn_reflns_theta_full        25.250
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6450
_reflns_number_gt                5978
_reflns_threshold_expression     >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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6450
_refine_ls_number_parameters     342
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0185
_refine_ls_wR_factor_ref         0.0478
_refine_ls_wR_factor_gt          0.0466
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
I1 I -0.01969(2) 0.22393(2) 0.64111(2) 0.01195(5) Uani 1 1 d . . . . .
I2 I 0.09223(2) 0.65295(2) 0.65609(2) 0.01168(5) Uani 1 1 d . . . . .
I3 I 0.24239(2) 0.44129(2) 0.27950(2) 0.01082(5) Uani 1 1 d . . . . .
I4 I 0.31586(2) 0.31422(2) 0.57532(2) 0.01153(5) Uani 1 1 d . . . . .
I5 I 0.26284(2) 0.07205(2) -0.16662(2) 0.01065(5) Uani 1 1 d . . . . .
I6 I 0.54164(2) 0.27098(2) 0.03223(2) 0.01167(5) Uani 1 1 d . . . . .
I7 I 0.38724(2) -0.13790(2) 0.24080(2) 0.01195(5) Uani 1 1 d . . . . .
I8 I 0.19176(2) 0.20459(2) 0.10666(2) 0.01021(5) Uani 1 1 d . . . . .
Mo1 Mo 0.10788(3) 0.33706(3) 0.46163(2) 0.00765(6) Uani 1 1 d . . . . .
Mo2 Mo 0.03438(3) 0.44163(3) 0.64151(2) 0.00754(6) Uani 1 1 d . . . . .
Mo3 Mo 0.15923(3) 0.54414(3) 0.46954(2) 0.00760(6) Uani 1 1 d . . . . .
Mo5 Mo 0.33298(3) -0.03121(3) 0.03505(2) 0.00734(6) Uani 1 1 d . . . . .
Mo6 Mo 0.40494(3) 0.16549(3) -0.06476(2) 0.00730(6) Uani 1 1 d . . . . .
Mo7 Mo 0.46727(3) 0.06211(3) 0.13039(2) 0.00742(6) Uani 1 1 d . . . . .
O1 O 0.2279(3) 0.1550(2) 0.4174(2) 0.0137(5) Uani 1 1 d D . . . .
H11 H 0.247(5) 0.098(4) 0.478(2) 0.040(15) Uiso 1 1 d D . . . .
O1W O 0.5429(3) 0.5162(3) 0.2815(3) 0.0297(7) Uani 1 1 d D . . . .
H11W H 0.585(5) 0.4269(14) 0.302(4) 0.058(18) Uiso 1 1 d D . . . .
H12W H 0.602(8) 0.547(8) 0.226(5) 0.16(4) Uiso 1 1 d D . . . .
O2 O 0.0749(3) 0.3813(3) 0.8011(2) 0.0144(5) Uani 1 1 d D . . . .
H21 H 0.015(5) 0.364(5) 0.863(3) 0.057(18) Uiso 1 1 d D . . . .
H22 H 0.161(3) 0.370(5) 0.822(4) 0.059(18) Uiso 1 1 d D . . . .
O2W O 0.0636(4) 0.0303(4) 0.3920(4) 0.0529(11) Uani 1 1 d D . . . .
H21W H 0.105(5) 0.091(3) 0.396(5) 0.063 Uiso 1 1 d D U . . .
H22W H 0.121(5) -0.048(2) 0.430(4) 0.063 Uiso 1 1 d D U . . .
O3 O 0.3448(3) 0.5954(3) 0.4393(2) 0.0171(6) Uani 1 1 d D . . . .
H31 H 0.420(3) 0.565(4) 0.385(3) 0.043(15) Uiso 1 1 d D . . . .
H32 H 0.345(8) 0.663(5) 0.471(6) 0.13(3) Uiso 1 1 d D . . . .
O3W O 0.9414(3) 0.0669(3) 0.2095(3) 0.0260(7) Uani 1 1 d D . . . .
H31W H 0.884(6) 0.149(3) 0.180(4) 0.09(2) Uiso 1 1 d D . . . .
H32W H 0.948(5) 0.073(8) 0.281(3) 0.40(10) Uiso 1 1 d D . . . .
O5 O 0.1378(3) -0.0661(3) 0.0741(2) 0.0163(6) Uani 1 1 d D . . . .
H51 H 0.129(5) -0.138(3) 0.055(4) 0.041(15) Uiso 1 1 d D . . . .
H52 H 0.057(5) -0.022(7) 0.120(5) 0.12(3) Uiso 1 1 d D . . . .
O6 O 0.2967(3) 0.3512(2) -0.1378(2) 0.0132(5) Uani 1 1 d D . . . .
H61 H 0.260(5) 0.413(4) -0.094(4) 0.063(19) Uiso 1 1 d D . . . .
O7 O 0.4328(3) 0.1297(3) 0.2784(2) 0.0151(6) Uani 1 1 d D . . . .
H71 H 0.507(3) 0.137(4) 0.306(4) 0.034(14) Uiso 1 1 d D . . . .
H72 H 0.356(5) 0.132(6) 0.334(4) 0.10(3) Uiso 1 1 d D . . . .
O11 O 0.6679(5) 0.0450(3) 0.4167(3) 0.0505(11) Uani 1 1 d . . . . .
O12 O 0.6966(4) 0.1803(3) 0.4951(2) 0.0310(7) Uani 1 1 d . . . . .
O13 O 0.6073(4) 0.2403(3) 0.3478(3) 0.0404(9) Uani 1 1 d . . . . .
O21 O 0.7995(3) 0.3206(3) 0.1179(2) 0.0265(7) Uani 1 1 d . . . . .
O22 O 0.8140(4) 0.4702(3) -0.0093(3) 0.0405(9) Uani 1 1 d . . . . .
O23 O 0.9104(3) 0.2759(3) -0.0400(2) 0.0234(6) Uani 1 1 d . . . . .
N1 N 0.6600(3) 0.1546(3) 0.4196(3) 0.0169(7) Uani 1 1 d . . . . .
N2 N 0.8409(3) 0.3555(3) 0.0240(3) 0.0165(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
I1 Mo2 2.7768(4) . ?
I1 Mo3 2.7774(4) 2_566 ?
I1 Mo1 2.7909(4) . ?
I2 Mo3 2.7706(3) . ?
I2 Mo2 2.7730(4) . ?
I2 Mo1 2.8002(4) 2_566 ?
I3 Mo3 2.7668(3) . ?
I3 Mo2 2.7749(4) 2_566 ?
I3 Mo1 2.8007(4) . ?
I4 Mo1 2.7867(4) . ?
I4 Mo3 2.7892(4) . ?
I4 Mo2 2.7980(4) . ?
I5 Mo7 2.7599(4) 2_655 ?
I5 Mo5 2.7680(4) . ?
I5 Mo6 2.7793(3) . ?
I6 Mo6 2.7917(3) . ?
I6 Mo5 2.7920(3) 2_655 ?
I6 Mo7 2.8049(4) . ?
I7 Mo5 2.7786(4) . ?
I7 Mo7 2.7890(4) . ?
I7 Mo6 2.7934(4) 2_655 ?
I8 Mo6 2.7848(4) . ?
I8 Mo7 2.7858(4) . ?
I8 Mo5 2.7867(3) . ?
Mo1 O1 2.113(2) . ?
Mo1 Mo2 2.6623(4) . ?
Mo1 Mo3 2.6638(4) . ?
Mo1 Mo2 2.6638(4) 2_566 ?
Mo1 Mo3 2.6669(4) 2_566 ?
Mo1 I2 2.8001(4) 2_566 ?
Mo2 O2 2.120(3) . ?
Mo2 Mo3 2.6552(4) . ?
Mo2 Mo1 2.6638(4) 2_566 ?
Mo2 Mo3 2.6661(4) 2_566 ?
Mo2 I3 2.7750(4) 2_566 ?
Mo3 O3 2.196(3) . ?
Mo3 Mo2 2.6660(4) 2_566 ?
Mo3 Mo1 2.6669(4) 2_566 ?
Mo3 I1 2.7774(4) 2_566 ?
Mo5 O5 2.189(3) . ?
Mo5 Mo7 2.6509(4) 2_655 ?
Mo5 Mo7 2.6588(4) . ?
Mo5 Mo6 2.6685(4) 2_655 ?
Mo5 Mo6 2.6751(4) . ?
Mo5 I6 2.7920(3) 2_655 ?
Mo6 O6 2.135(3) . ?
Mo6 Mo7 2.6641(4) 2_655 ?
Mo6 Mo7 2.6684(4) . ?
Mo6 Mo5 2.6685(4) 2_655 ?
Mo6 I7 2.7934(4) 2_655 ?
Mo7 O7 2.114(2) . ?
Mo7 Mo5 2.6510(4) 2_655 ?
Mo7 Mo6 2.6641(4) 2_655 ?
Mo7 I5 2.7599(4) 2_655 ?
O1 H11 0.921(10) . ?
O1W H11W 0.958(10) . ?
O1W H12W 0.961(10) . ?
O2 H21 0.951(10) . ?
O2 H22 0.959(10) . ?
O2W H21W 0.975(10) . ?
O2W H22W 0.977(10) . ?
O3 H31 0.948(10) . ?
O3 H32 0.955(10) . ?
O3W H31W 0.957(10) . ?
O3W H32W 0.963(10) . ?
O5 H51 0.950(10) . ?
O5 H52 0.958(10) . ?
O6 H61 0.913(10) . ?
O7 H71 0.956(10) . ?
O7 H72 0.960(10) . ?
O11 N1 1.240(4) . ?
O12 N1 1.241(4) . ?
O13 N1 1.256(4) . ?
O21 N2 1.246(4) . ?
O22 N2 1.246(4) . ?
O23 N2 1.263(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Mo2 I1 Mo3 57.372(9) . 2_566 ?
Mo2 I1 Mo1 57.132(9) . . ?
Mo3 I1 Mo1 57.233(9) 2_566 . ?
Mo3 I2 Mo2 57.235(9) . . ?
Mo3 I2 Mo1 57.201(9) . 2_566 ?
Mo2 I2 Mo1 57.104(10) . 2_566 ?
Mo3 I3 Mo2 57.511(9) . 2_566 ?
Mo3 I3 Mo1 57.165(9) . . ?
Mo2 I3 Mo1 57.077(10) 2_566 . ?
Mo1 I4 Mo3 57.073(9) . . ?
Mo1 I4 Mo2 56.942(9) . . ?
Mo3 I4 Mo2 56.747(10) . . ?
Mo7 I5 Mo5 57.313(9) 2_655 . ?
Mo7 I5 Mo6 57.494(9) 2_655 . ?
Mo5 I5 Mo6 57.662(9) . . ?
Mo6 I6 Mo5 57.097(9) . 2_655 ?
Mo6 I6 Mo7 56.951(9) . . ?
Mo5 I6 Mo7 56.543(9) 2_655 . ?
Mo5 I7 Mo7 57.050(9) . . ?
Mo5 I7 Mo6 57.228(9) . 2_655 ?
Mo7 I7 Mo6 57.009(9) . 2_655 ?
Mo6 I8 Mo7 57.242(9) . . ?
Mo6 I8 Mo5 57.389(9) . . ?
Mo7 I8 Mo5 56.996(9) . . ?
O1 Mo1 Mo2 135.58(7) . . ?
O1 Mo1 Mo3 135.17(7) . . ?
Mo2 Mo1 Mo3 59.805(10) . . ?
O1 Mo1 Mo2 134.62(7) . 2_566 ?
Mo2 Mo1 Mo2 89.796(12) . 2_566 ?
Mo3 Mo1 Mo2 60.054(11) . 2_566 ?
O1 Mo1 Mo3 134.93(7) . 2_566 ?
Mo2 Mo1 Mo3 60.036(10) . 2_566 ?
Mo3 Mo1 Mo3 89.895(12) . 2_566 ?
Mo2 Mo1 Mo3 59.748(11) 2_566 2_566 ?
O1 Mo1 I4 88.43(7) . . ?
Mo2 Mo1 I4 61.741(10) . . ?
Mo3 Mo1 I4 61.511(10) . . ?
Mo2 Mo1 I4 121.549(13) 2_566 . ?
Mo3 Mo1 I4 121.767(12) 2_566 . ?
O1 Mo1 I1 88.98(7) . . ?
Mo2 Mo1 I1 61.167(10) . . ?
Mo3 Mo1 I1 120.966(12) . . ?
Mo2 Mo1 I1 120.872(13) 2_566 . ?
Mo3 Mo1 I1 61.129(10) 2_566 . ?
I4 Mo1 I1 90.158(11) . . ?
O1 Mo1 I2 88.45(7) . 2_566 ?
Mo2 Mo1 I2 120.872(13) . 2_566 ?
Mo3 Mo1 I2 120.984(13) . 2_566 ?
Mo2 Mo1 I2 60.935(10) 2_566 2_566 ?
Mo3 Mo1 I2 60.840(9) 2_566 2_566 ?
I4 Mo1 I2 176.880(13) . 2_566 ?
I1 Mo1 I2 89.877(11) . 2_566 ?
O1 Mo1 I3 88.82(7) . . ?
Mo2 Mo1 I3 120.578(13) . . ?
Mo3 Mo1 I3 60.777(10) . . ?
Mo2 Mo1 I3 60.976(10) 2_566 . ?
Mo3 Mo1 I3 120.721(13) 2_566 . ?
I4 Mo1 I3 89.674(11) . . ?
I1 Mo1 I3 177.798(13) . . ?
I2 Mo1 I3 90.171(11) 2_566 . ?
O2 Mo2 Mo3 133.37(7) . . ?
O2 Mo2 Mo1 136.17(7) . . ?
Mo3 Mo2 Mo1 60.124(10) . . ?
O2 Mo2 Mo1 133.59(7) . 2_566 ?
Mo3 Mo2 Mo1 60.183(11) . 2_566 ?
Mo1 Mo2 Mo1 90.203(12) . 2_566 ?
O2 Mo2 Mo3 136.50(7) . 2_566 ?
Mo3 Mo2 Mo3 90.097(12) . 2_566 ?
Mo1 Mo2 Mo3 60.067(11) . 2_566 ?
Mo1 Mo2 Mo3 59.972(11) 2_566 2_566 ?
O2 Mo2 I2 85.97(7) . . ?
Mo3 Mo2 I2 61.338(10) . . ?
Mo1 Mo2 I2 121.437(13) . . ?
Mo1 Mo2 I2 61.961(10) 2_566 . ?
Mo3 Mo2 I2 121.929(13) 2_566 . ?
O2 Mo2 I3 88.25(7) . 2_566 ?
Mo3 Mo2 I3 122.129(13) . 2_566 ?
Mo1 Mo2 I3 121.119(13) . 2_566 ?
Mo1 Mo2 I3 61.948(10) 2_566 2_566 ?
Mo3 Mo2 I3 61.089(10) 2_566 2_566 ?
I2 Mo2 I3 91.273(10) . 2_566 ?
O2 Mo2 I1 90.11(7) . . ?
Mo3 Mo2 I1 121.819(12) . . ?
Mo1 Mo2 I1 61.700(10) . . ?
Mo1 Mo2 I1 121.273(13) 2_566 . ?
Mo3 Mo2 I1 61.325(10) 2_566 . ?
I2 Mo2 I1 176.081(13) . . ?
I3 Mo2 I1 88.679(11) 2_566 . ?
O2 Mo2 I4 88.08(7) . . ?
Mo3 Mo2 I4 61.461(10) . . ?
Mo1 Mo2 I4 61.317(10) . . ?
Mo1 Mo2 I4 121.636(13) 2_566 . ?
Mo3 Mo2 I4 121.373(12) 2_566 . ?
I2 Mo2 I4 89.579(11) . . ?
I3 Mo2 I4 176.172(13) 2_566 . ?
I1 Mo2 I4 90.217(10) . . ?
O3 Mo3 Mo2 133.26(7) . . ?
O3 Mo3 Mo1 135.42(7) . . ?
Mo2 Mo3 Mo1 60.071(10) . . ?
O3 Mo3 Mo2 136.83(7) . 2_566 ?
Mo2 Mo3 Mo2 89.904(12) . 2_566 ?
Mo1 Mo3 Mo2 59.975(11) . 2_566 ?
O3 Mo3 Mo1 134.42(7) . 2_566 ?
Mo2 Mo3 Mo1 60.070(11) . 2_566 ?
Mo1 Mo3 Mo1 90.107(12) . 2_566 ?
Mo2 Mo3 Mo1 59.898(10) 2_566 2_566 ?
O3 Mo3 I3 89.50(7) . . ?
Mo2 Mo3 I3 122.125(12) . . ?
Mo1 Mo3 I3 62.058(10) . . ?
Mo2 Mo3 I3 61.399(10) 2_566 . ?
Mo1 Mo3 I3 121.259(12) 2_566 . ?
O3 Mo3 I2 86.35(7) . . ?
Mo2 Mo3 I2 61.427(10) . . ?
Mo1 Mo3 I2 121.473(13) . . ?
Mo2 Mo3 I2 121.850(13) 2_566 . ?
Mo1 Mo3 I2 61.957(10) 2_566 . ?
I3 Mo3 I2 175.842(13) . . ?
O3 Mo3 I1 89.06(7) . 2_566 ?
Mo2 Mo3 I1 121.703(13) . 2_566 ?
Mo1 Mo3 I1 121.253(13) . 2_566 ?
Mo2 Mo3 I1 61.302(10) 2_566 2_566 ?
Mo1 Mo3 I1 61.638(10) 2_566 2_566 ?
I3 Mo3 I1 88.832(10) . 2_566 ?
I2 Mo3 I1 90.768(10) . 2_566 ?
O3 Mo3 I4 87.19(7) . . ?
Mo2 Mo3 I4 61.792(10) . . ?
Mo1 Mo3 I4 61.416(10) . . ?
Mo2 Mo3 I4 121.376(13) 2_566 . ?
Mo1 Mo3 I4 121.854(13) 2_566 . ?
I3 Mo3 I4 90.320(10) . . ?
I2 Mo3 I4 89.807(10) . . ?
I1 Mo3 I4 176.157(13) 2_566 . ?
O5 Mo5 Mo7 134.67(7) . 2_655 ?
O5 Mo5 Mo7 135.56(7) . . ?
Mo7 Mo5 Mo7 89.759(12) 2_655 . ?
O5 Mo5 Mo6 135.24(8) . 2_655 ?
Mo7 Mo5 Mo6 60.214(11) 2_655 2_655 ?
Mo7 Mo5 Mo6 60.011(11) . 2_655 ?
O5 Mo5 Mo6 134.27(8) . . ?
Mo7 Mo5 Mo6 60.024(11) 2_655 . ?
Mo7 Mo5 Mo6 60.035(11) . . ?
Mo6 Mo5 Mo6 90.484(12) 2_655 . ?
O5 Mo5 I5 87.70(8) . . ?
Mo7 Mo5 I5 61.189(10) 2_655 . ?
Mo7 Mo5 I5 121.415(13) . . ?
Mo6 Mo5 I5 121.381(13) 2_655 . ?
Mo6 Mo5 I5 61.381(10) . . ?
O5 Mo5 I7 88.54(8) . . ?
Mo7 Mo5 I7 121.874(13) 2_655 . ?
Mo7 Mo5 I7 61.673(10) . . ?
Mo6 Mo5 I7 61.666(10) 2_655 . ?
Mo6 Mo5 I7 121.678(12) . . ?
I5 Mo5 I7 176.245(13) . . ?
O5 Mo5 I8 88.22(7) . . ?
Mo7 Mo5 I8 121.288(13) 2_655 . ?
Mo7 Mo5 I8 61.485(9) . . ?
Mo6 Mo5 I8 121.477(12) 2_655 . ?
Mo6 Mo5 I8 61.270(10) . . ?
I5 Mo5 I8 90.235(10) . . ?
I7 Mo5 I8 89.669(10) . . ?
O5 Mo5 I6 87.99(7) . 2_655 ?
Mo7 Mo5 I6 61.974(10) 2_655 2_655 ?
Mo7 Mo5 I6 121.446(13) . 2_655 ?
Mo6 Mo5 I6 61.446(10) 2_655 2_655 ?
Mo6 Mo5 I6 121.984(13) . 2_655 ?
I5 Mo5 I6 89.942(10) . 2_655 ?
I7 Mo5 I6 89.906(10) . 2_655 ?
I8 Mo5 I6 176.198(13) . 2_655 ?
O6 Mo6 Mo7 135.14(7) . 2_655 ?
O6 Mo6 Mo7 135.58(7) . . ?
Mo7 Mo6 Mo7 89.274(12) 2_655 . ?
O6 Mo6 Mo5 135.58(7) . 2_655 ?
Mo7 Mo6 Mo5 59.814(10) 2_655 2_655 ?
Mo7 Mo6 Mo5 59.568(11) . 2_655 ?
O6 Mo6 Mo5 134.91(7) . . ?
Mo7 Mo6 Mo5 59.538(10) 2_655 . ?
Mo7 Mo6 Mo5 59.679(11) . . ?
Mo5 Mo6 Mo5 89.516(12) 2_655 . ?
O6 Mo6 I5 88.63(7) . . ?
Mo7 Mo6 I5 60.886(10) 2_655 . ?
Mo7 Mo6 I5 120.635(13) . . ?
Mo5 Mo6 I5 120.695(12) 2_655 . ?
Mo5 Mo6 I5 60.957(10) . . ?
O6 Mo6 I8 88.48(7) . . ?
Mo7 Mo6 I8 120.873(13) 2_655 . ?
Mo7 Mo6 I8 61.398(10) . . ?
Mo5 Mo6 I8 120.957(13) 2_655 . ?
Mo5 Mo6 I8 61.341(10) . . ?
I5 Mo6 I8 90.041(11) . . ?
O6 Mo6 I6 88.59(7) . . ?
Mo7 Mo6 I6 121.261(13) 2_655 . ?
Mo7 Mo6 I6 61.773(10) . . ?
Mo5 Mo6 I6 61.457(9) 2_655 . ?
Mo5 Mo6 I6 121.442(13) . . ?
I5 Mo6 I6 177.214(13) . . ?
I8 Mo6 I6 90.112(10) . . ?
O6 Mo6 I7 88.86(7) . 2_655 ?
Mo7 Mo6 I7 61.415(10) 2_655 2_655 ?
Mo7 Mo6 I7 120.669(13) . 2_655 ?
Mo5 Mo6 I7 61.106(10) 2_655 2_655 ?
Mo5 Mo6 I7 120.949(12) . 2_655 ?
I5 Mo6 I7 90.109(10) . 2_655 ?
I8 Mo6 I7 177.334(13) . 2_655 ?
I6 Mo6 I7 89.610(10) . 2_655 ?
O7 Mo7 Mo5 134.53(7) . 2_655 ?
O7 Mo7 Mo5 135.22(7) . . ?
Mo5 Mo7 Mo5 90.240(12) 2_655 . ?
O7 Mo7 Mo6 133.76(8) . 2_655 ?
Mo5 Mo7 Mo6 60.437(10) 2_655 2_655 ?
Mo5 Mo7 Mo6 60.175(10) . 2_655 ?
O7 Mo7 Mo6 135.51(8) . . ?
Mo5 Mo7 Mo6 60.217(11) 2_655 . ?
Mo5 Mo7 Mo6 60.285(11) . . ?
Mo6 Mo7 Mo6 90.725(12) 2_655 . ?
O7 Mo7 I5 87.15(7) . 2_655 ?
Mo5 Mo7 I5 61.497(10) 2_655 2_655 ?
Mo5 Mo7 I5 121.789(13) . 2_655 ?
Mo6 Mo7 I5 61.619(10) 2_655 2_655 ?
Mo6 Mo7 I5 121.693(13) . 2_655 ?
O7 Mo7 I8 88.94(7) . . ?
Mo5 Mo7 I8 121.567(13) 2_655 . ?
Mo5 Mo7 I8 61.519(9) . . ?
Mo6 Mo7 I8 121.674(12) 2_655 . ?
Mo6 Mo7 I8 61.360(10) . . ?
I5 Mo7 I8 176.087(12) 2_655 . ?
O7 Mo7 I7 87.66(8) . . ?
Mo5 Mo7 I7 122.011(12) 2_655 . ?
Mo5 Mo7 I7 61.277(10) . . ?
Mo6 Mo7 I7 61.578(10) 2_655 . ?
Mo6 Mo7 I7 121.532(12) . . ?
I5 Mo7 I7 90.600(11) 2_655 . ?
I8 Mo7 I7 89.474(11) . . ?
O7 Mo7 I6 88.48(8) . . ?
Mo5 Mo7 I6 61.484(10) 2_655 . ?
Mo5 Mo7 I6 121.552(13) . . ?
Mo6 Mo7 I6 121.906(13) 2_655 . ?
Mo6 Mo7 I6 61.276(10) . . ?
I5 Mo7 I6 89.842(11) 2_655 . ?
I8 Mo7 I6 89.820(11) . . ?
I7 Mo7 I6 176.085(12) . . ?
Mo1 O1 H11 109(3) . . ?
H11W O1W H12W 111(6) . . ?
Mo2 O2 H21 129(3) . . ?
Mo2 O2 H22 123(3) . . ?
H21 O2 H22 108(5) . . ?
H21W O2W H22W 103.7(14) . . ?
Mo3 O3 H31 123(3) . . ?
Mo3 O3 H32 120(5) . . ?
H31 O3 H32 116(6) . . ?
H31W O3W H32W 106.9(15) . . ?
Mo5 O5 H51 122(3) . . ?
Mo5 O5 H52 127(5) . . ?
H51 O5 H52 111(5) . . ?
Mo6 O6 H61 116(4) . . ?
Mo7 O7 H71 121(3) . . ?
Mo7 O7 H72 126(4) . . ?
H71 O7 H72 111(5) . . ?
O11 N1 O12 120.5(3) . . ?
O11 N1 O13 118.8(3) . . ?
O12 N1 O13 120.7(3) . . ?
O21 N2 O22 120.8(3) . . ?
O21 N2 O23 121.0(3) . . ?
O22 N2 O23 118.2(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H11 O11 0.921(10) 1.966(17) 2.867(4) 166(5) 2_656
O2 H21 O23 0.951(10) 1.90(2) 2.811(4) 159(5) 1_456
O2 H22 O6 0.959(10) 1.542(11) 2.500(4) 177(6) 1_556
O3 H31 O1W 0.948(10) 1.678(12) 2.624(4) 175(5) .
O3 H32 O12 0.955(10) 1.80(3) 2.723(4) 162(7) 2_666
O5 H51 O23 0.950(10) 1.841(14) 2.781(4) 169(5) 2_655
O5 H52 O3W 0.958(10) 1.67(2) 2.614(4) 167(7) 1_455
O6 H61 O22 0.913(10) 1.914(12) 2.824(4) 174(5) 2_665
O7 H71 O13 0.956(10) 2.07(2) 2.955(4) 153(4) .
O7 H72 O1 0.960(10) 1.521(14) 2.475(4) 172(7) .
O1W H11W O13 0.958(10) 2.05(2) 2.969(5) 160(5) .
O1W H12W O6 0.961(10) 1.94(3) 2.871(4) 164(8) 2_665
O2W H21W O1 0.975(10) 1.80(2) 2.738(4) 160(4) .
O2W H22W O12 0.977(10) 2.21(2) 3.138(6) 157(4) 2_656
O3W H31W O21 0.957(10) 1.921(17) 2.866(4) 169(6) .
O3W H32W O2W 0.963(10) 1.937(19) 2.800(6) 148(4) 1_655

_refine_diff_density_max         1.135
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.172



_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_symmetry_cell_setting           ?
_symmetry_int_tables_number      ?
_chemical_absolute_configuration ?

# start Validation Reply Form
_vrf_PLAT417_juc729              
;
PROBLEM: Short Inter D-H..H-D       H11      ..H21W     .       2.04 Ang.  
RESPONSE: All these problem points concern about the H atoms of Hydroxide 
anions involved in the H-bond formation with two adjacent water molecules.
;

# end Validation Reply Form
####################################################################### 
# 
# 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_VMV577-3
_database_code_depnum_ccdc_archive 'CCDC 2078011'
loop_
_audit_author_name
_audit_author_address
'Natalia Kuratieva'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2021-04-16 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'H8 I8 Mo6 O6, 12(H2 O)'
_chemical_formula_sum            'H32 I8 Mo6 O18'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         1911.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 '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                   9.4284(9)
_cell_length_b                   9.7991(10)
_cell_length_c                   10.0079(10)
_cell_angle_alpha                73.929(4)
_cell_angle_beta                 67.566(4)
_cell_angle_gamma                88.598(4)
_cell_volume                     817.81(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7707
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      36.31
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.880
_exptl_crystal_F_000             852
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    9.837
_shelx_estimated_absorpt_T_min   0.489
_shelx_estimated_absorpt_T_max   0.725

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   'Bruker SADABS-2012/1'
_exptl_absorpt_special_details   ?


_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_type              'Incoatec ImS 3.0'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 7.4
_diffrn_reflns_number            22858
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.300
_diffrn_reflns_theta_max         36.312
_diffrn_reflns_theta_full        25.250
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7293
_reflns_number_gt                5781
_reflns_threshold_expression     >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       'Bruker APEX3 V2018.7-2'
_computing_cell_refinement       'SAINT V8.38A'
_computing_data_reduction        'SAINT V8.38A'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0217P)²+0.7960P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7293
_refine_ls_number_parameters     159
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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
I1 I 0.38253(3) 0.44352(3) 0.38697(3) 0.01554(5) Uani 1 1 d . . . . .
I2 I 0.10111(3) 0.43360(3) 0.80460(3) 0.01636(5) Uani 1 1 d . . . . .
I3 I 0.21661(3) 0.79647(3) 0.22680(3) 0.01893(6) Uani 1 1 d . . . . .
I4 I 0.06304(3) 0.21316(3) 0.36052(3) 0.01803(6) Uani 1 1 d . . . . .
Mo2 Mo 0.15164(3) 0.60923(3) 0.51484(3) 0.01159(6) Uani 1 1 d . . . . .
Mo1 Mo 0.07881(3) 0.33167(3) 0.57805(3) 0.01169(6) Uani 1 1 d . . . . .
Mo3 Mo 0.13289(3) 0.50485(3) 0.30273(3) 0.01233(6) Uani 1 1 d . . . . .
O1 O 0.1705(3) 0.1475(3) 0.6632(3) 0.0208(6) Uani 1 1 d . . . . .
O2 O 0.3160(3) 0.7305(3) 0.5380(3) 0.0211(6) Uani 1 1 d . . . . .
O1W O 0.3643(4) 0.0156(3) 0.4745(4) 0.0279(7) Uani 1 1 d . . . . .
O3 O 0.2884(4) 0.5143(4) 0.0716(4) 0.0325(8) Uani 1 1 d . . . . .
O3W O 0.4986(4) 0.9005(4) -0.1719(4) 0.0323(7) Uani 1 1 d . . . . .
O4W O 0.2518(4) 0.7430(4) -0.1612(4) 0.0320(7) Uani 1 1 d . . . . .
O2W O -0.0029(5) -0.0863(4) 0.9105(4) 0.0415(9) Uani 1 1 d . . . . .
O5WA O 0.4097(5) 0.1776(5) 0.7422(5) 0.0276(9) Uani 0.724(5) 1 d . . P A 1
O6WA O 0.6823(7) 0.7677(7) -0.0110(6) 0.0404(19) Uani 0.694(10) 1 d . . P B 1
O6WB O 0.5712(14) 0.6876(13) 0.0109(12) 0.033(4) Uani 0.306(10) 1 d . . P B 2
O5WB O 0.3041(13) 0.1360(13) 0.8864(13) 0.0276(9) Uani 0.276(5) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Mo3 2.7886(4) . ?
I1 Mo2 2.8044(4) . ?
I1 Mo1 2.8057(5) . ?
I2 Mo3 2.7875(4) 2_566 ?
I2 Mo1 2.7947(4) . ?
I2 Mo2 2.7965(5) . ?
I3 Mo1 2.7947(5) 2_566 ?
I3 Mo3 2.7958(5) . ?
I3 Mo2 2.7984(5) . ?
I4 Mo1 2.7866(4) . ?
I4 Mo2 2.7901(4) 2_566 ?
I4 Mo3 2.7972(5) . ?
Mo2 O2 2.094(3) . ?
Mo2 Mo3 2.6567(5) 2_566 ?
Mo2 Mo1 2.6601(5) . ?
Mo2 Mo3 2.6610(5) . ?
Mo2 Mo1 2.6651(5) 2_566 ?
Mo2 I4 2.7900(4) 2_566 ?
Mo1 O1 2.089(3) . ?
Mo1 Mo3 2.6566(5) 2_566 ?
Mo1 Mo2 2.6651(5) 2_566 ?
Mo1 Mo3 2.6670(5) . ?
Mo1 I3 2.7947(5) 2_566 ?
Mo3 O3 2.192(3) . ?
Mo3 Mo1 2.6566(5) 2_566 ?
Mo3 Mo2 2.6567(5) 2_566 ?
Mo3 I2 2.7875(4) 2_566 ?

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
Mo3 I1 Mo2 56.818(11) . . ?
Mo3 I1 Mo1 56.944(12) . . ?
Mo2 I1 Mo1 56.610(12) . . ?
Mo3 I2 Mo1 56.837(11) 2_566 . ?
Mo3 I2 Mo2 56.820(11) 2_566 . ?
Mo1 I2 Mo2 56.819(12) . . ?
Mo1 I3 Mo3 56.745(11) 2_566 . ?
Mo1 I3 Mo2 56.914(11) 2_566 . ?
Mo3 I3 Mo2 56.806(11) . . ?
Mo1 I4 Mo2 57.097(11) . 2_566 ?
Mo1 I4 Mo3 57.061(11) . . ?
Mo2 I4 Mo3 56.784(11) 2_566 . ?
O2 Mo2 Mo3 133.26(8) . 2_566 ?
O2 Mo2 Mo1 134.82(8) . . ?
Mo3 Mo2 Mo1 59.954(12) 2_566 . ?
O2 Mo2 Mo3 136.78(8) . . ?
Mo3 Mo2 Mo3 89.965(15) 2_566 . ?
Mo1 Mo2 Mo3 60.161(12) . . ?
O2 Mo2 Mo1 135.00(8) . 2_566 ?
Mo3 Mo2 Mo1 60.152(13) 2_566 2_566 ?
Mo1 Mo2 Mo1 90.128(13) . 2_566 ?
Mo3 Mo2 Mo1 59.841(12) . 2_566 ?
O2 Mo2 I4 86.97(8) . 2_566 ?
Mo3 Mo2 I4 61.745(12) 2_566 2_566 ?
Mo1 Mo2 I4 121.691(15) . 2_566 ?
Mo3 Mo2 I4 121.210(14) . 2_566 ?
Mo1 Mo2 I4 61.386(12) 2_566 2_566 ?
O2 Mo2 I2 86.81(8) . . ?
Mo3 Mo2 I2 61.419(11) 2_566 . ?
Mo1 Mo2 I2 61.556(11) . . ?
Mo3 Mo2 I2 121.709(16) . . ?
Mo1 Mo2 I2 121.555(15) 2_566 . ?
I4 Mo2 I2 90.095(13) 2_566 . ?
O2 Mo2 I3 89.34(8) . . ?
Mo3 Mo2 I3 121.613(14) 2_566 . ?
Mo1 Mo2 I3 121.693(14) . . ?
Mo3 Mo2 I3 61.548(13) . . ?
Mo1 Mo2 I3 61.474(12) 2_566 . ?
I4 Mo2 I3 89.589(14) 2_566 . ?
I2 Mo2 I3 176.148(14) . . ?
O2 Mo2 I1 89.42(8) . . ?
Mo3 Mo2 I1 121.670(15) 2_566 . ?
Mo1 Mo2 I1 61.719(12) . . ?
Mo3 Mo2 I1 61.292(11) . . ?
Mo1 Mo2 I1 121.111(15) 2_566 . ?
I4 Mo2 I1 176.291(14) 2_566 . ?
I2 Mo2 I1 90.573(13) . . ?
I3 Mo2 I1 89.500(13) . . ?
O1 Mo1 Mo3 135.38(8) . 2_566 ?
O1 Mo1 Mo2 133.89(8) . . ?
Mo3 Mo1 Mo2 59.960(13) 2_566 . ?
O1 Mo1 Mo2 136.23(8) . 2_566 ?
Mo3 Mo1 Mo2 60.003(13) 2_566 2_566 ?
Mo2 Mo1 Mo2 89.873(13) . 2_566 ?
O1 Mo1 Mo3 134.76(8) . . ?
Mo3 Mo1 Mo3 89.839(14) 2_566 . ?
Mo2 Mo1 Mo3 59.936(12) . . ?
Mo2 Mo1 Mo3 59.769(12) 2_566 . ?
O1 Mo1 I4 88.63(8) . . ?
Mo3 Mo1 I4 121.503(14) 2_566 . ?
Mo2 Mo1 I4 121.592(15) . . ?
Mo2 Mo1 I4 61.517(11) 2_566 . ?
Mo3 Mo1 I4 61.670(13) . . ?
O1 Mo1 I2 87.60(8) . . ?
Mo3 Mo1 I2 61.445(11) 2_566 . ?
Mo2 Mo1 I2 61.625(11) . . ?
Mo2 Mo1 I2 121.436(14) 2_566 . ?
Mo3 Mo1 I2 121.553(15) . . ?
I4 Mo1 I2 176.217(14) . . ?
O1 Mo1 I3 89.17(8) . 2_566 ?
Mo3 Mo1 I3 61.648(13) 2_566 2_566 ?
Mo2 Mo1 I3 121.597(14) . 2_566 ?
Mo2 Mo1 I3 61.612(13) 2_566 2_566 ?
Mo3 Mo1 I3 121.369(14) . 2_566 ?
I4 Mo1 I3 89.734(13) . 2_566 ?
I2 Mo1 I3 89.908(13) . 2_566 ?
O1 Mo1 I1 87.26(8) . . ?
Mo3 Mo1 I1 121.627(15) 2_566 . ?
Mo2 Mo1 I1 61.671(11) . . ?
Mo2 Mo1 I1 120.955(15) 2_566 . ?
Mo3 Mo1 I1 61.206(12) . . ?
I4 Mo1 I1 89.538(13) . . ?
I2 Mo1 I1 90.585(13) . . ?
I3 Mo1 I1 176.373(14) 2_566 . ?
O3 Mo3 Mo1 134.06(9) . 2_566 ?
O3 Mo3 Mo2 135.49(9) . 2_566 ?
Mo1 Mo3 Mo2 60.086(13) 2_566 2_566 ?
O3 Mo3 Mo2 134.46(9) . . ?
Mo1 Mo3 Mo2 60.157(12) 2_566 . ?
Mo2 Mo3 Mo2 90.034(14) 2_566 . ?
O3 Mo3 Mo1 135.78(9) . . ?
Mo1 Mo3 Mo1 90.162(15) 2_566 . ?
Mo2 Mo3 Mo1 60.080(12) 2_566 . ?
Mo2 Mo3 Mo1 59.904(13) . . ?
O3 Mo3 I2 87.62(9) . 2_566 ?
Mo1 Mo3 I2 61.718(12) 2_566 2_566 ?
Mo2 Mo3 I2 61.761(13) 2_566 2_566 ?
Mo2 Mo3 I2 121.863(14) . 2_566 ?
Mo1 Mo3 I2 121.825(15) . 2_566 ?
O3 Mo3 I1 87.84(9) . . ?
Mo1 Mo3 I1 122.025(15) 2_566 . ?
Mo2 Mo3 I1 121.909(16) 2_566 . ?
Mo2 Mo3 I1 61.890(11) . . ?
Mo1 Mo3 I1 61.850(11) . . ?
I2 Mo3 I1 175.453(14) 2_566 . ?
O3 Mo3 I3 87.07(10) . . ?
Mo1 Mo3 I3 61.608(12) 2_566 . ?
Mo2 Mo3 I3 121.684(14) 2_566 . ?
Mo2 Mo3 I3 61.646(12) . . ?
Mo1 Mo3 I3 121.535(14) . . ?
I2 Mo3 I3 90.034(12) 2_566 . ?
I1 Mo3 I3 89.875(12) . . ?
O3 Mo3 I4 89.28(9) . . ?
Mo1 Mo3 I4 121.551(15) 2_566 . ?
Mo2 Mo3 I4 61.472(11) 2_566 . ?
Mo2 Mo3 I4 121.160(15) . . ?
Mo1 Mo3 I4 61.269(12) . . ?
I2 Mo3 I4 90.131(12) 2_566 . ?
I1 Mo3 I4 89.670(12) . . ?
I3 Mo3 I4 176.332(14) . . ?

_refine_diff_density_max         1.462
_refine_diff_density_min         -2.278
_refine_diff_density_rms         0.285


_diffrn_radiation_monochromator  'goebel mirror'
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_details      
;
Data collection was performed by Dr. Dmitry A. Piryazev 
in XRD Facility of NIIC SB RAS.
;
_diffrn_detector                 CPAD
_diffrn_detector_type            'PHOTON III C14'
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_symmetry_cell_setting           ?
_symmetry_space_group_name_h-m   ?
_symmetry_int_tables_number      ?
_chemical_absolute_configuration ?

# start Validation Reply Form
_vrf_PLAT043_VMV577-3            
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      32.25 Check 
RESPONSE: These difference corresponds to unlocalized H atoms of the water 
molecules and hydroxid anions.
;
_vrf_PLAT306_VMV577-3            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: These isolated O atoms belong to solvate water molecules with 
unlocalized H atoms.
;

# end Validation Reply Form
####################################################################### 
# 
# 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_yv475aa
_database_code_depnum_ccdc_archive 'CCDC 2036292'
loop_
_audit_author_name
_audit_author_address
'Natalia Kuratieva'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2020-10-09 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'I8 Mo6 O6 H8, 2(C7 H7 O3 S), 2(H2 O)'
_chemical_formula_sum            'C14 H28 I8 Mo6 O14 S2'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         2075.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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                   9.4471(10)
_cell_length_b                   9.4592(10)
_cell_length_c                   11.5036(13)
_cell_angle_alpha                77.300(3)
_cell_angle_beta                 79.348(3)
_cell_angle_gamma                73.852(3)
_cell_volume                     954.84(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4305
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.609
_exptl_crystal_F_000             932
_exptl_transmission_factor_min   0.561
_exptl_transmission_factor_max   0.746
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    8.539
_shelx_estimated_absorpt_T_min   0.342
_shelx_estimated_absorpt_T_max   0.726


_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?


_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_reflns_number            7699
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.831
_diffrn_reflns_theta_max         27.157
_diffrn_reflns_theta_full        25.250
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             4143
_reflns_number_gt                3684
_reflns_threshold_expression     >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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.1332P)²+19.2287P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4143
_refine_ls_number_parameters     210
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.2010
_refine_ls_wR_factor_gt          0.1967
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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
I1 I 0.52699(8) 0.20194(8) 0.36912(7) 0.0155(2) Uani 1 1 d . . . . .
I2 I 0.44696(8) 0.82072(7) 0.28929(6) 0.0152(2) Uani 1 1 d . . . . .
I3 I 0.20625(8) 0.52974(8) 0.72369(6) 0.0154(2) Uani 1 1 d . . . . .
I4 I 0.18011(8) 0.54910(8) 0.38130(7) 0.0146(2) Uani 1 1 d . . . . .
Mo1 Mo 0.37234(9) 0.37086(9) 0.54480(7) 0.0089(2) Uani 1 1 d . . . . .
Mo2 Mo 0.48737(9) 0.51048(9) 0.33708(7) 0.0101(2) Uani 1 1 d . . . . .
Mo3 Mo 0.33573(9) 0.66525(9) 0.50555(8) 0.0101(2) Uani 1 1 d . . . . .
S1 S 0.7161(4) 0.7258(3) -0.0960(3) 0.0217(6) Uani 1 1 d . . . . .
O1 O 0.2317(8) 0.2307(8) 0.5890(7) 0.0129(14) Uani 1 1 d . . . . .
O1W O 0.1319(9) 0.1395(8) 0.4320(8) 0.0194(17) Uani 1 1 d . . . . .
O2 O 0.4700(10) 0.5306(10) 0.1479(7) 0.0205(17) Uani 1 1 d . U . . .
O3 O 0.1476(9) 0.8559(9) 0.5131(10) 0.028(2) Uani 1 1 d . . . . .
O11A O 0.6879(14) 0.5802(13) -0.0314(10) 0.019(2) Uani 0.795(13) 1 d . . P A 1
O11B O 0.744(6) 0.569(6) -0.068(4) 0.019(2) Uani 0.205(13) 1 d . . P A 2
O12A O 0.8235(14) 0.7065(13) -0.2041(11) 0.028(3) Uani 0.795(13) 1 d . . P A 1
O12B O 0.719(5) 0.813(5) -0.204(4) 0.028(3) Uani 0.205(13) 1 d . . P A 2
O13A O 0.5800(14) 0.8362(14) -0.1201(11) 0.032(3) Uani 0.795(13) 1 d . . P A 1
O13B O 0.554(6) 0.733(5) -0.032(4) 0.032(3) Uani 0.205(13) 1 d . . P A 2
C1 C 0.8024(14) 0.7890(14) -0.0017(11) 0.021(2) Uani 1 1 d . . . . .
C2 C 0.9451(15) 0.7189(13) 0.0219(12) 0.024(3) Uani 1 1 d . . . . .
H2 H 0.9968 0.6313 -0.0100 0.029 Uiso 1 1 calc R U . . .
C3 C 1.0140(15) 0.7743(14) 0.0912(12) 0.024(3) Uani 1 1 d . . . . .
H3 H 1.1132 0.7254 0.1054 0.029 Uiso 1 1 calc R U . . .
C4 C 0.9383(14) 0.9036(14) 0.1417(10) 0.021(2) Uani 1 1 d . . . . .
C5 C 0.7951(15) 0.9724(14) 0.1160(11) 0.023(2) Uani 1 1 d . . . . .
H5 H 0.7422 1.0600 0.1476 0.028 Uiso 1 1 calc R U . . .
C6 C 0.7271(13) 0.9170(14) 0.0457(11) 0.022(2) Uani 1 1 d . . . . .
H6 H 0.6285 0.9664 0.0297 0.026 Uiso 1 1 calc R U . . .
C7 C 1.0099(17) 0.9660(15) 0.2167(12) 0.029(3) Uani 1 1 d . . . . .
H7A H 0.9697 1.0746 0.2067 0.044 Uiso 1 1 calc R U . . .
H7B H 1.1175 0.9435 0.1915 0.044 Uiso 1 1 calc R U . . .
H7C H 0.9897 0.9210 0.3014 0.044 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
I1 Mo3 2.7808(11) 2_666 ?
I1 Mo2 2.7864(11) . ?
I1 Mo1 2.7932(11) . ?
I2 Mo3 2.7822(11) . ?
I2 Mo1 2.7936(10) 2_666 ?
I2 Mo2 2.7938(11) . ?
I3 Mo3 2.7855(11) . ?
I3 Mo2 2.7870(11) 2_666 ?
I3 Mo1 2.7946(11) . ?
I4 Mo2 2.7864(11) . ?
I4 Mo3 2.7887(11) . ?
I4 Mo1 2.8005(10) . ?
Mo1 O1 2.053(7) . ?
Mo1 Mo2 2.6507(12) 2_666 ?
Mo1 Mo3 2.6515(12) 2_666 ?
Mo1 Mo3 2.6546(12) . ?
Mo1 Mo2 2.6620(12) . ?
Mo1 I2 2.7935(10) 2_666 ?
Mo2 O2 2.175(8) . ?
Mo2 Mo3 2.6469(12) . ?
Mo2 Mo1 2.6508(12) 2_666 ?
Mo2 Mo3 2.6615(12) 2_666 ?
Mo2 I3 2.7870(11) 2_666 ?
Mo3 O3 2.156(8) . ?
Mo3 Mo1 2.6516(12) 2_666 ?
Mo3 Mo2 2.6615(12) 2_666 ?
Mo3 I1 2.7808(11) 2_666 ?
S1 O12B 1.33(5) . ?
S1 O11B 1.41(5) . ?
S1 O13A 1.442(12) . ?
S1 O12A 1.463(12) . ?
S1 O11A 1.484(11) . ?
S1 O13B 1.56(5) . ?
S1 C1 1.756(13) . ?
C1 C2 1.375(18) . ?
C1 C6 1.392(18) . ?
C2 C3 1.378(18) . ?
C2 H2 0.9500 . ?
C3 C4 1.420(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(18) . ?
C4 C7 1.487(16) . ?
C5 C6 1.381(17) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 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
Mo3 I1 Mo2 57.12(3) 2_666 . ?
Mo3 I1 Mo1 56.81(3) 2_666 . ?
Mo2 I1 Mo1 56.99(3) . . ?
Mo3 I2 Mo1 56.79(3) . 2_666 ?
Mo3 I2 Mo2 56.68(3) . . ?
Mo1 I2 Mo2 56.64(3) 2_666 . ?
Mo3 I3 Mo2 57.06(3) . 2_666 ?
Mo3 I3 Mo1 56.81(3) . . ?
Mo2 I3 Mo1 56.71(3) 2_666 . ?
Mo2 I4 Mo3 56.69(3) . . ?
Mo2 I4 Mo1 56.91(3) . . ?
Mo3 I4 Mo1 56.71(3) . . ?
O1 Mo1 Mo2 136.4(2) . 2_666 ?
O1 Mo1 Mo3 135.2(2) . 2_666 ?
Mo2 Mo1 Mo3 59.90(3) 2_666 2_666 ?
O1 Mo1 Mo3 134.8(2) . . ?
Mo2 Mo1 Mo3 60.22(3) 2_666 . ?
Mo3 Mo1 Mo3 89.91(3) 2_666 . ?
O1 Mo1 Mo2 133.6(2) . . ?
Mo2 Mo1 Mo2 90.05(4) 2_666 . ?
Mo3 Mo1 Mo2 60.12(3) 2_666 . ?
Mo3 Mo1 Mo2 59.72(3) . . ?
O1 Mo1 I1 87.5(2) . . ?
Mo2 Mo1 I1 121.25(4) 2_666 . ?
Mo3 Mo1 I1 61.36(3) 2_666 . ?
Mo3 Mo1 I1 121.09(4) . . ?
Mo2 Mo1 I1 61.38(3) . . ?
O1 Mo1 I2 89.2(2) . 2_666 ?
Mo2 Mo1 I2 61.68(3) 2_666 2_666 ?
Mo3 Mo1 I2 61.39(3) 2_666 2_666 ?
Mo3 Mo1 I2 121.90(4) . 2_666 ?
Mo2 Mo1 I2 121.49(4) . 2_666 ?
I1 Mo1 I2 89.63(3) . 2_666 ?
O1 Mo1 I3 89.2(2) . . ?
Mo2 Mo1 I3 61.50(3) 2_666 . ?
Mo3 Mo1 I3 121.39(4) 2_666 . ?
Mo3 Mo1 I3 61.42(3) . . ?
Mo2 Mo1 I3 121.13(4) . . ?
I1 Mo1 I3 176.77(4) . . ?
I2 Mo1 I3 90.47(3) 2_666 . ?
O1 Mo1 I4 87.1(2) . . ?
Mo2 Mo1 I4 121.63(4) 2_666 . ?
Mo3 Mo1 I4 121.38(4) 2_666 . ?
Mo3 Mo1 I4 61.42(3) . . ?
Mo2 Mo1 I4 61.28(3) . . ?
I1 Mo1 I4 89.79(3) . . ?
I2 Mo1 I4 176.25(4) 2_666 . ?
I3 Mo1 I4 89.90(3) . . ?
O2 Mo2 Mo3 133.3(3) . . ?
O2 Mo2 Mo1 133.9(2) . 2_666 ?
Mo3 Mo2 Mo1 60.07(3) . 2_666 ?
O2 Mo2 Mo3 136.8(3) . 2_666 ?
Mo3 Mo2 Mo3 89.86(4) . 2_666 ?
Mo1 Mo2 Mo3 59.96(3) 2_666 2_666 ?
O2 Mo2 Mo1 136.1(2) . . ?
Mo3 Mo2 Mo1 60.00(3) . . ?
Mo1 Mo2 Mo1 89.95(4) 2_666 . ?
Mo3 Mo2 Mo1 59.75(3) 2_666 . ?
O2 Mo2 I4 87.5(2) . . ?
Mo3 Mo2 I4 61.70(3) . . ?
Mo1 Mo2 I4 121.75(4) 2_666 . ?
Mo3 Mo2 I4 121.55(4) 2_666 . ?
Mo1 Mo2 I4 61.81(3) . . ?
O2 Mo2 I1 90.2(2) . . ?
Mo3 Mo2 I1 121.63(4) . . ?
Mo1 Mo2 I1 121.27(4) 2_666 . ?
Mo3 Mo2 I1 61.34(3) 2_666 . ?
Mo1 Mo2 I1 61.63(3) . . ?
I4 Mo2 I1 90.22(3) . . ?
O2 Mo2 I3 88.5(2) . 2_666 ?
Mo3 Mo2 I3 121.85(4) . 2_666 ?
Mo1 Mo2 I3 61.79(3) 2_666 2_666 ?
Mo3 Mo2 I3 61.45(3) 2_666 2_666 ?
Mo1 Mo2 I3 121.17(4) . 2_666 ?
I4 Mo2 I3 175.97(4) . 2_666 ?
I1 Mo2 I3 89.16(3) . 2_666 ?
O2 Mo2 I2 86.2(2) . . ?
Mo3 Mo2 I2 61.44(3) . . ?
Mo1 Mo2 I2 61.67(3) 2_666 . ?
Mo3 Mo2 I2 121.63(4) 2_666 . ?
Mo1 Mo2 I2 121.43(4) . . ?
I4 Mo2 I2 89.74(3) . . ?
I1 Mo2 I2 176.31(4) . . ?
I3 Mo2 I2 90.62(3) 2_666 . ?
O3 Mo3 Mo2 135.2(3) . . ?
O3 Mo3 Mo1 134.7(2) . 2_666 ?
Mo2 Mo3 Mo1 60.04(3) . 2_666 ?
O3 Mo3 Mo1 135.2(2) . . ?
Mo2 Mo3 Mo1 60.28(3) . . ?
Mo1 Mo3 Mo1 90.09(3) 2_666 . ?
O3 Mo3 Mo2 134.7(3) . 2_666 ?
Mo2 Mo3 Mo2 90.14(4) . 2_666 ?
Mo1 Mo3 Mo2 60.14(3) 2_666 2_666 ?
Mo1 Mo3 Mo2 59.82(3) . 2_666 ?
O3 Mo3 I1 87.5(3) . 2_666 ?
Mo2 Mo3 I1 121.86(4) . 2_666 ?
Mo1 Mo3 I1 61.83(3) 2_666 2_666 ?
Mo1 Mo3 I1 121.34(4) . 2_666 ?
Mo2 Mo3 I1 61.55(3) 2_666 2_666 ?
O3 Mo3 I2 87.7(3) . . ?
Mo2 Mo3 I2 61.88(3) . . ?
Mo1 Mo3 I2 61.82(3) 2_666 . ?
Mo1 Mo3 I2 122.15(4) . . ?
Mo2 Mo3 I2 121.94(4) 2_666 . ?
I1 Mo3 I2 90.12(3) 2_666 . ?
O3 Mo3 I3 87.8(3) . . ?
Mo2 Mo3 I3 122.03(4) . . ?
Mo1 Mo3 I3 121.61(4) 2_666 . ?
Mo1 Mo3 I3 61.77(3) . . ?
Mo2 Mo3 I3 61.50(3) 2_666 . ?
I1 Mo3 I3 89.31(3) 2_666 . ?
I2 Mo3 I3 175.48(4) . . ?
O3 Mo3 I4 88.4(3) . . ?
Mo2 Mo3 I4 61.61(3) . . ?
Mo1 Mo3 I4 121.63(4) 2_666 . ?
Mo1 Mo3 I4 61.87(3) . . ?
Mo2 Mo3 I4 121.68(4) 2_666 . ?
I1 Mo3 I4 175.89(4) 2_666 . ?
I2 Mo3 I4 89.93(3) . . ?
I3 Mo3 I4 90.33(3) . . ?
O12B S1 O11B 129(3) . . ?
O13A S1 O12A 112.9(7) . . ?
O13A S1 O11A 111.9(8) . . ?
O12A S1 O11A 110.8(7) . . ?
O12B S1 O13B 112(3) . . ?
O11B S1 O13B 88(3) . . ?
O12B S1 C1 109.6(19) . . ?
O11B S1 C1 109(2) . . ?
O13A S1 C1 108.2(6) . . ?
O12A S1 C1 105.7(6) . . ?
O11A S1 C1 107.1(6) . . ?
O13B S1 C1 105.6(17) . . ?
C2 C1 C6 119.3(11) . . ?
C2 C1 S1 121.4(10) . . ?
C6 C1 S1 119.2(9) . . ?
C1 C2 C3 120.7(12) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C2 C3 C4 120.8(12) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 117.2(11) . . ?
C5 C4 C7 120.8(12) . . ?
C3 C4 C7 122.0(12) . . ?
C6 C5 C4 121.7(11) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C1 120.2(11) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_refine_diff_density_max         2.813
_refine_diff_density_min         -7.017
_refine_diff_density_rms         0.595



_symmetry_space_group_name_Hall  ?
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         0
_diffrn_standards_decay_%        0


# start Validation Reply Form
_vrf_DIFMN02_yv475aa             
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: The crystal was twinned. So, some refinement parameters are out 
from expected range of values.
;
_vrf_PLAT972_yv475aa             
;
PROBLEM: Check Calcd Resid. Dens.  0.99A   From Mo3            -6.48 eA-3  
RESPONSE: Some peaks and holes in the differnece map are occured because of 
the lack of the crystal quality. Investigated crystal was twinned. The 
diffraction peaks were integrated using two cell orientations.
;
_vrf_PLAT976_yv475aa             
;
PROBLEM: Check Calcd Resid. Dens.  0.57A   From O3             -2.56 eA-3  
RESPONSE: Some peaks and holes in the differnece map are occured because of 
the lack of the crystal quality. Investigated crystal was twinned. The 
diffraction peaks were integrated using two cell orientations.
;
_vrf_PLAT098_yv475aa             
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -7.02 eA-3  
RESPONSE: Some peaks and holes in the differnece map are occured because of 
the lack of the crystal quality. Investigated crystal was twinned. The 
diffraction peaks were integrated using two cell orientations.
;
_vrf_PLAT306_yv475aa             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: The Hydrogen atoms for co-crystallized water molecules were not 
localized.
;
_vrf_PLAT430_yv475aa             
;
PROBLEM: Short Inter D...A Contact  O1       ..O1W      .       2.58 Ang.  
RESPONSE: This distance correspons to the hydrogen bond between the 
co-crystallized water molecule and water/hydroxyl ligand of the cluster 
complex.
;
_vrf_PLAT971_yv475aa             
;
PROBLEM: Check Calcd Resid. Dens.  0.88A   From I4              2.78 eA-3  
RESPONSE: Some peaks and holes in the differnece map are occured because of 
the lack of the crystal quality. Investigated crystal was twinned. The 
diffraction peaks were integrated using two cell orientations.
;

# end Validation Reply Form
