# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_lbl-0414-mo21_sq2
_database_code_depnum_ccdc_archive 'CCDC 1899131'
loop_
_audit_author_name
_audit_author_address
'Luo Benlong'
;Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2019-04-10 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT306_lbl-0414-mo21_sq2   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O30 Check
RESPONSE: The hydrogen atoms of the disordered O30 water molecule are not added.
;
# Added during the CSD deposition process: Wednesday 10 April 2019 04:05 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C30 H34 Mo21 N6 O58,C5H6N,3(C2H6NH2),H2O,0.5(C2H6NH),H2O'
_chemical_formula_sum            'C42 H71.50 Mo21 N10.50 O60'
_chemical_formula_weight         3698.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.212(2)
_cell_length_b                   18.987(3)
_cell_length_c                   16.985(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.746(3)
_cell_angle_gamma                90
_cell_volume                     5225.8(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13387
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.350
_exptl_crystal_F_000             3518
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    2.514
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 5.8140
_diffrn_reflns_number            55318
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.016
_diffrn_reflns_theta_max         27.516
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             11943
_reflns_number_gt                9599
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'diamond 3.0'
_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)+(0.0370P)²+32.3789P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11943
_refine_ls_number_parameters     620
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1035
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.83509(4) 0.35650(3) 0.42740(3) 0.02666(12) Uani 1 1 d . . . . .
O1 O 0.8961(3) 0.3247(2) 0.5204(2) 0.0356(11) Uani 1 1 d . . . . .
Mo2 Mo 0.80050(4) 0.26626(3) 0.53003(3) 0.02667(12) Uani 1 1 d . . . . .
O2 O 0.7818(3) 0.4319(2) 0.4801(2) 0.0332(11) Uani 1 1 d . . . . .
Mo3 Mo 0.69828(4) 0.35959(3) 0.49099(3) 0.02665(12) Uani 1 1 d . . . . .
O3 O 0.7372(3) 0.3295(2) 0.5945(2) 0.0349(11) Uani 1 1 d . . . . .
Mo4 Mo 0.750000 0.23557(3) 0.250000 0.01771(14) Uani 1 2 d S T P . .
O4 O 0.7448(2) 0.2823(2) 0.4235(2) 0.0217(8) Uani 1 1 d . . . . .
Mo5 Mo 0.83898(4) 0.41164(3) 0.21173(3) 0.02581(12) Uani 1 1 d . . . . .
O5 O 0.8681(3) 0.1843(2) 0.4743(2) 0.0285(10) Uani 1 1 d . . . . .
Mo7 Mo 0.93195(3) 0.18133(3) 0.37159(3) 0.02461(12) Uani 1 1 d . . . . .
O7 O 0.7227(3) 0.1815(2) 0.5438(2) 0.0293(10) Uani 1 1 d . . . . .
Mo10 Mo 0.55139(3) 0.09690(3) 0.33074(3) 0.02497(12) Uani 1 1 d . . . . .
O10 O 0.7453(3) 0.0791(2) 0.4343(2) 0.0282(9) Uani 1 1 d . . . . .
O17 O 0.8715(3) 0.1800(2) 0.1035(2) 0.0218(8) Uani 1 1 d . . . . .
O16 O 0.9859(3) 0.2794(2) 0.1473(2) 0.0285(9) Uani 1 1 d . . . . .
H16 H 0.835(5) 0.149(4) 0.472(4) 0.04(2) Uiso 1 1 d . . . . .
Mo9 Mo 0.78519(3) 0.05636(3) 0.32413(3) 0.02221(11) Uani 1 1 d . . . . .
O9 O 0.6583(4) 0.0490(3) 0.5699(3) 0.0436(13) Uani 1 1 d . . . . .
O13 O 1.0275(3) 0.1730(3) 0.4109(3) 0.0397(12) Uani 1 1 d . . . . .
O19 O 1.0687(3) 0.2502(3) 0.0106(3) 0.0410(12) Uani 1 1 d . . . . .
O15 O 0.9385(3) 0.3827(2) 0.2525(2) 0.0297(10) Uani 1 1 d . . . . .
Mo8 Mo 0.97546(3) 0.23653(3) 0.05061(3) 0.02579(12) Uani 1 1 d . . . . .
O8 O 0.7845(3) 0.3926(2) 0.3168(2) 0.0270(9) Uani 1 1 d . . . . .
O18 O 0.8572(3) 0.3969(2) 0.1090(2) 0.0293(10) Uani 1 1 d . . . . .
Mo11 Mo 0.66225(3) 0.11130(3) 0.49860(3) 0.02513(12) Uani 1 1 d . . . . .
O11 O 0.8953(3) 0.0846(2) 0.3660(2) 0.0268(9) Uani 1 1 d . . . . .
O14 O 1.0690(3) 0.2895(3) 0.2932(3) 0.0394(11) Uani 1 1 d . . . . .
Mo6 Mo 0.97029(3) 0.27994(3) 0.26327(3) 0.02445(12) Uani 1 1 d . . . . .
N6 N 1.003(2) -0.0082(10) 0.4438(17) 0.148(12) Uani 0.5 1 d . . P A -1
H6A H 0.972424 0.026983 0.424206 0.177 Uiso 0.5 1 calc R U P A -1
H6B H 0.992617 -0.011055 0.494904 0.177 Uiso 0.5 1 calc R U P A -1
O6 O 0.9093(3) 0.2842(2) 0.3644(2) 0.0261(9) Uani 1 1 d . . . . .
O24 O 0.7931(3) -0.0314(2) 0.3340(3) 0.0353(11) Uani 1 1 d . . . . .
C24 C 1.088(2) 0.0114(14) 0.437(3) 0.22(3) Uani 0.5 1 d . . P . .
H24A H 1.104449 0.041804 0.480124 0.337 Uiso 0.5 1 calc R U P A .
H24B H 1.095667 0.035550 0.388218 0.337 Uiso 0.5 1 calc R U P . .
H24C H 1.122191 -0.030197 0.438757 0.337 Uiso 0.5 1 calc R U P . .
O23 O 0.5885(3) 0.0495(2) 0.4173(2) 0.0289(9) Uani 1 1 d . . . . .
C23 C 0.972(3) -0.076(2) 0.405(2) 0.170(15) Uani 0.5 1 d . U P . .
H23A H 0.932715 -0.097691 0.438645 0.254 Uiso 0.5 1 calc R U P A .
H23B H 1.017530 -0.106831 0.397905 0.254 Uiso 0.5 1 calc R U P . .
H23C H 0.945911 -0.064775 0.355324 0.254 Uiso 0.5 1 calc R U P . .
O22 O 0.4742(3) 0.1470(2) 0.3768(3) 0.0316(10) Uani 1 1 d . . . . .
O21 O 0.6696(3) 0.0755(2) 0.2830(2) 0.0231(8) Uani 1 1 d . . . . .
O20 O 0.9456(3) 0.1555(2) -0.0173(2) 0.0294(10) Uani 1 1 d . . . . .
O26 O 0.4991(3) 0.0346(3) 0.2779(3) 0.0409(12) Uani 1 1 d . . . . .
O25 O 0.9089(3) 0.2991(2) 0.0023(2) 0.0294(10) Uani 1 1 d . . . . .
O29 O 0.8426(3) 0.5006(2) 0.2178(3) 0.0407(12) Uani 1 1 d . . . . .
O28 O 0.6660(3) 0.2858(2) 0.2825(2) 0.0210(8) Uani 1 1 d . . . . .
O27 O 0.9486(3) 0.1760(2) 0.2562(2) 0.0255(9) Uani 1 1 d . . . . .
N3 N 0.6298(4) 0.4451(3) 0.5483(3) 0.0359(13) Uani 1 1 d . . . . .
N1 N 0.9382(5) 0.4319(3) 0.4142(3) 0.0459(17) Uani 1 1 d . . . . .
C3 C 0.6241(6) 0.5084(4) 0.5109(5) 0.053(2) Uani 1 1 d . . . . .
H3 H 0.648135 0.513206 0.462133 0.064 Uiso 1 1 calc R U . . .
C4 C 0.5900(6) 0.4378(5) 0.6155(5) 0.053(2) Uani 1 1 d . . . . .
H4 H 0.590624 0.394446 0.640908 0.064 Uiso 1 1 calc R U . . .
C2 C 1.0156(6) 0.4113(5) 0.4255(5) 0.061(3) Uani 1 1 d . . . . .
H2 H 1.025677 0.365621 0.443070 0.073 Uiso 1 1 calc R U . . .
C1 C 0.9233(7) 0.4976(4) 0.3892(5) 0.060(3) Uani 1 1 d . . . . .
H1 H 0.869084 0.512395 0.380448 0.072 Uiso 1 1 calc R U . . .
C7 C 0.5844(6) 0.5656(4) 0.5420(6) 0.061(2) Uani 1 1 d . . . . .
H7 H 0.584149 0.608815 0.516289 0.073 Uiso 1 1 calc R U . . .
C6 C 0.5454(7) 0.5573(5) 0.6118(6) 0.068(3) Uani 1 1 d . . . . .
H6 H 0.517479 0.594767 0.634124 0.081 Uiso 1 1 calc R U . . .
C5 C 0.5480(7) 0.4934(6) 0.6481(6) 0.075(3) Uani 1 1 d . . . . .
H5 H 0.521215 0.487140 0.695203 0.090 Uiso 1 1 calc R U . . .
C9 C 1.0679(11) 0.5219(8) 0.3880(6) 0.105(6) Uani 1 1 d . . . . .
H9 H 1.111544 0.552493 0.379466 0.126 Uiso 1 1 calc R U . . .
C8 C 0.9881(9) 0.5446(6) 0.3760(6) 0.081(4) Uani 1 1 d . . . . .
H8 H 0.977237 0.590433 0.359417 0.097 Uiso 1 1 calc R U . . .
C10 C 1.0831(7) 0.4552(7) 0.4123(6) 0.085(4) Uani 1 1 d . . . . .
H10 H 1.136854 0.439011 0.419910 0.102 Uiso 1 1 calc R U . . .
N4 N 0.5921(5) 0.9061(3) 0.4319(5) 0.069(2) Uani 1 1 d . . . . .
H4A H 0.548503 0.884845 0.451800 0.083 Uiso 1 1 calc R U . . .
H4B H 0.581930 0.952149 0.430567 0.083 Uiso 1 1 calc R U . . .
C16 C 0.6657(8) 0.8929(6) 0.4846(7) 0.082(3) Uani 1 1 d . . . . .
H16A H 0.672870 0.843052 0.491717 0.123 Uiso 1 1 calc R U . . .
H16B H 0.657661 0.914681 0.534827 0.123 Uiso 1 1 calc R U . . .
H16C H 0.713841 0.912322 0.461367 0.123 Uiso 1 1 calc R U . . .
C17 C 0.6033(8) 0.8806(6) 0.3510(7) 0.090(4) Uani 1 1 d . . . . .
H17A H 0.651582 0.901921 0.329974 0.135 Uiso 1 1 calc R U . . .
H17B H 0.555812 0.893008 0.318752 0.135 Uiso 1 1 calc R U . . .
H17C H 0.609654 0.830366 0.351567 0.135 Uiso 1 1 calc R U . . .
H18 H 0.830(5) 0.200(4) 0.118(4) 0.04(2) Uiso 1 1 d . . . . .
O12 O 0.7890(2) 0.17985(19) 0.3245(2) 0.0201(8) Uani 1 1 d . . . . .
N2 N 0.8584(3) 0.2315(3) 0.6448(3) 0.0470(14) Uani 1 1 d G U . . .
C11 C 0.8367(5) 0.1673(4) 0.6774(5) 0.130(4) Uani 1 1 d G U . . .
H11 H 0.804546 0.135582 0.648118 0.156 Uiso 1 1 calc R U . . .
C12 C 0.8629(7) 0.1504(5) 0.7538(5) 0.147(5) Uani 1 1 d G U . . .
H12 H 0.848308 0.107390 0.775567 0.176 Uiso 1 1 calc R U . . .
C13 C 0.9109(6) 0.1978(6) 0.7975(3) 0.134(5) Uani 1 1 d G U . . .
H13 H 0.928432 0.186460 0.848613 0.160 Uiso 1 1 calc R U . . .
C14 C 0.9327(6) 0.2620(5) 0.7649(4) 0.118(4) Uani 1 1 d G U . . .
H14 H 0.964794 0.293724 0.794211 0.142 Uiso 1 1 calc R U . . .
C15 C 0.9065(5) 0.2789(3) 0.6886(4) 0.111(4) Uani 1 1 d G U . . .
H15 H 0.921032 0.321918 0.666761 0.134 Uiso 1 1 calc R U . . .
N5 N 1.1654(12) 0.2720(11) 0.5118(11) 0.108(8) Uani 0.5 1 d G . P . .
C18 C 1.2349(11) 0.3128(12) 0.5285(13) 0.124(11) Uani 0.5 1 d G . P . .
H18A H 1.272355 0.321823 0.489373 0.148 Uiso 0.5 1 calc R U P . .
C19 C 1.2485(12) 0.3400(12) 0.6038(16) 0.121(11) Uani 0.5 1 d G . P . .
H19 H 1.294986 0.367333 0.614942 0.145 Uiso 0.5 1 calc R U P . .
C20 C 1.1925(18) 0.3265(16) 0.6623(11) 0.21(2) Uani 0.5 1 d G . P . .
H20 H 1.201550 0.344759 0.712593 0.250 Uiso 0.5 1 calc R U P . .
C21 C 1.1229(16) 0.2857(17) 0.6455(13) 0.24(3) Uani 0.5 1 d G . P . .
H21 H 1.085481 0.276675 0.684676 0.286 Uiso 0.5 1 calc R U P . .
C22 C 1.1094(11) 0.2585(11) 0.5703(16) 0.17(2) Uani 0.5 1 d G . P . .
H22 H 1.062849 0.231165 0.559108 0.204 Uiso 0.5 1 calc R U P . .
O30 O 0.750000 0.4037(10) 0.750000 0.161(7) Uani 1 2 d S T P . .


_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 1.908(4) . ?
Mo1 O1 1.936(5) . ?
Mo1 O4 2.032(4) . ?
Mo1 O6 2.135(4) . ?
Mo1 O8 2.140(4) . ?
Mo1 N1 2.217(6) . ?
Mo1 Mo3 2.4971(8) . ?
Mo1 Mo2 2.5195(8) . ?
O1 Mo2 1.917(5) . ?
Mo2 O3 1.939(4) . ?
Mo2 O4 2.021(4) . ?
Mo2 O7 2.063(4) . ?
Mo2 O5 2.141(4) . ?
Mo2 N2 2.237(4) . ?
Mo2 Mo3 2.5018(8) . ?
O2 Mo3 1.940(4) . ?
Mo3 O3 1.936(4) . ?
Mo3 O4 2.023(4) . ?
Mo3 O18 2.025(4) 2_655 ?
Mo3 O25 2.089(5) 2_655 ?
Mo3 N3 2.210(5) . ?
Mo4 O12 1.752(4) . ?
Mo4 O12 1.752(4) 2_655 ?
Mo4 O28 1.764(4) 2_655 ?
Mo4 O28 1.764(4) . ?
Mo5 O29 1.692(4) . ?
Mo5 O18 1.801(4) . ?
Mo5 O15 1.821(5) . ?
Mo5 O8 2.047(4) . ?
Mo5 O8 2.077(5) 2_655 ?
Mo5 O28 2.393(4) 2_655 ?
Mo5 Mo5 3.2005(12) 2_655 ?
O5 Mo7 2.056(4) . ?
Mo7 O13 1.676(5) . ?
Mo7 O11 1.931(4) . ?
Mo7 O27 1.989(4) . ?
Mo7 O6 1.990(4) . ?
Mo7 O12 2.429(4) . ?
Mo7 Mo6 2.7105(8) . ?
O7 Mo11 1.811(4) . ?
Mo10 O26 1.697(5) . ?
Mo10 O22 1.773(4) . ?
Mo10 O23 1.811(4) . ?
Mo10 O27 2.106(4) 2_655 ?
Mo10 O21 2.143(4) . ?
Mo10 O17 2.284(4) 2_655 ?
O10 Mo11 1.863(4) . ?
O10 Mo9 2.044(4) . ?
O17 Mo8 2.212(4) . ?
O17 Mo11 2.224(4) 2_655 ?
O16 Mo8 1.836(4) . ?
O16 Mo6 1.994(4) . ?
Mo9 O24 1.680(4) . ?
Mo9 O11 1.976(4) . ?
Mo9 O21 2.012(4) . ?
Mo9 O21 2.016(4) 2_655 ?
Mo9 O12 2.346(4) . ?
Mo9 Mo9 2.7327(11) 2_655 ?
O9 Mo11 1.695(4) . ?
O19 Mo8 1.697(5) . ?
O15 Mo6 2.025(4) . ?
Mo8 O25 1.787(4) . ?
Mo8 O20 1.975(4) . ?
Mo8 O22 2.239(5) 2_655 ?
Mo11 O20 1.973(4) 2_655 ?
Mo11 O23 2.147(4) . ?
O14 Mo6 1.674(5) . ?
Mo6 O27 2.007(4) . ?
Mo6 O6 2.009(4) . ?
Mo6 O28 2.323(4) 2_655 ?
N6 C24 1.44(4) . ?
N6 C23 1.51(5) . ?
N3 C4 1.335(9) . ?
N3 C3 1.361(9) . ?
N1 C2 1.324(12) . ?
N1 C1 1.338(11) . ?
C3 C7 1.376(10) . ?
C4 C5 1.381(12) . ?
C2 C10 1.399(13) . ?
C1 C8 1.401(13) . ?
C7 C6 1.371(12) . ?
C6 C5 1.359(14) . ?
C9 C10 1.352(19) . ?
C9 C8 1.372(19) . ?
N4 C17 1.473(13) . ?
N4 C16 1.490(14) . ?
N2 C11 1.3900 . ?
N2 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
N5 C18 1.3900 . ?
N5 C22 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?

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 O1 94.5(2) . . ?
O2 Mo1 O4 101.49(18) . . ?
O1 Mo1 O4 99.21(18) . . ?
O2 Mo1 O6 170.94(18) . . ?
O1 Mo1 O6 85.77(18) . . ?
O4 Mo1 O6 87.38(16) . . ?
O2 Mo1 O8 90.25(18) . . ?
O1 Mo1 O8 171.74(19) . . ?
O4 Mo1 O8 86.39(16) . . ?
O6 Mo1 O8 88.44(16) . . ?
O2 Mo1 N1 85.2(2) . . ?
O1 Mo1 N1 85.2(2) . . ?
O4 Mo1 N1 171.59(17) . . ?
O6 Mo1 N1 85.8(2) . . ?
O8 Mo1 N1 88.5(2) . . ?
O2 Mo1 Mo3 50.11(14) . . ?
O1 Mo1 Mo3 95.34(14) . . ?
O4 Mo1 Mo3 51.81(11) . . ?
O6 Mo1 Mo3 138.92(11) . . ?
O8 Mo1 Mo3 92.90(12) . . ?
N1 Mo1 Mo3 135.29(17) . . ?
O2 Mo1 Mo2 94.13(13) . . ?
O1 Mo1 Mo2 48.84(14) . . ?
O4 Mo1 Mo2 51.37(11) . . ?
O6 Mo1 Mo2 92.88(11) . . ?
O8 Mo1 Mo2 137.56(12) . . ?
N1 Mo1 Mo2 133.89(18) . . ?
Mo3 Mo1 Mo2 59.83(2) . . ?
Mo2 O1 Mo1 81.67(19) . . ?
O1 Mo2 O3 97.7(2) . . ?
O1 Mo2 O4 100.23(17) . . ?
O3 Mo2 O4 100.52(18) . . ?
O1 Mo2 O7 163.7(2) . . ?
O3 Mo2 O7 94.76(19) . . ?
O4 Mo2 O7 87.77(16) . . ?
O1 Mo2 O5 87.5(2) . . ?
O3 Mo2 O5 170.57(17) . . ?
O4 Mo2 O5 86.24(16) . . ?
O7 Mo2 O5 78.83(18) . . ?
O1 Mo2 N2 85.7(2) . . ?
O3 Mo2 N2 84.6(2) . . ?
O4 Mo2 N2 171.48(19) . . ?
O7 Mo2 N2 85.0(2) . . ?
O5 Mo2 N2 87.94(19) . . ?
O1 Mo2 Mo3 95.67(15) . . ?
O3 Mo2 Mo3 49.73(14) . . ?
O4 Mo2 Mo3 51.80(11) . . ?
O7 Mo2 Mo3 100.40(13) . . ?
O5 Mo2 Mo3 137.88(12) . . ?
N2 Mo2 Mo3 134.17(15) . . ?
O1 Mo2 Mo1 49.48(14) . . ?
O3 Mo2 Mo1 95.87(13) . . ?
O4 Mo2 Mo1 51.75(11) . . ?
O7 Mo2 Mo1 139.38(12) . . ?
O5 Mo2 Mo1 93.48(12) . . ?
N2 Mo2 Mo1 134.97(16) . . ?
Mo3 Mo2 Mo1 59.64(2) . . ?
Mo1 O2 Mo3 80.90(16) . . ?
O3 Mo3 O2 95.0(2) . . ?
O3 Mo3 O4 100.57(17) . . ?
O2 Mo3 O4 100.72(17) . . ?
O3 Mo3 O18 171.43(18) . 2_655 ?
O2 Mo3 O18 88.05(19) . 2_655 ?
O4 Mo3 O18 86.71(16) . 2_655 ?
O3 Mo3 O25 92.09(19) . 2_655 ?
O2 Mo3 O25 167.96(19) . 2_655 ?
O4 Mo3 O25 87.53(16) . 2_655 ?
O18 Mo3 O25 83.65(18) 2_655 2_655 ?
O3 Mo3 N3 88.4(2) . . ?
O2 Mo3 N3 83.3(2) . . ?
O4 Mo3 N3 169.7(2) . . ?
O18 Mo3 N3 84.00(19) 2_655 . ?
O25 Mo3 N3 87.1(2) 2_655 . ?
O3 Mo3 Mo1 96.68(15) . . ?
O2 Mo3 Mo1 49.00(13) . . ?
O4 Mo3 Mo1 52.15(11) . . ?
O18 Mo3 Mo1 91.35(13) 2_655 . ?
O25 Mo3 Mo1 139.64(11) 2_655 . ?
N3 Mo3 Mo1 132.28(16) . . ?
O3 Mo3 Mo2 49.84(13) . . ?
O2 Mo3 Mo2 93.89(15) . . ?
O4 Mo3 Mo2 51.75(11) . . ?
O18 Mo3 Mo2 138.07(12) 2_655 . ?
O25 Mo3 Mo2 98.12(12) 2_655 . ?
N3 Mo3 Mo2 137.86(16) . . ?
Mo1 Mo3 Mo2 60.53(2) . . ?
Mo3 O3 Mo2 80.43(16) . . ?
O12 Mo4 O12 105.7(2) . 2_655 ?
O12 Mo4 O28 106.68(18) . 2_655 ?
O12 Mo4 O28 111.42(17) 2_655 2_655 ?
O12 Mo4 O28 111.42(17) . . ?
O12 Mo4 O28 106.68(18) 2_655 . ?
O28 Mo4 O28 114.6(3) 2_655 . ?
Mo2 O4 Mo3 76.45(13) . . ?
Mo2 O4 Mo1 76.88(14) . . ?
Mo3 O4 Mo1 76.04(13) . . ?
O29 Mo5 O18 102.0(2) . . ?
O29 Mo5 O15 104.4(2) . . ?
O18 Mo5 O15 98.7(2) . . ?
O29 Mo5 O8 97.92(19) . . ?
O18 Mo5 O8 154.89(18) . . ?
O15 Mo5 O8 90.92(18) . . ?
O29 Mo5 O8 102.7(2) . 2_655 ?
O18 Mo5 O8 86.14(18) . 2_655 ?
O15 Mo5 O8 150.77(17) . 2_655 ?
O8 Mo5 O8 74.60(19) . 2_655 ?
O29 Mo5 O28 174.14(18) . 2_655 ?
O18 Mo5 O28 83.78(16) . 2_655 ?
O15 Mo5 O28 73.36(16) . 2_655 ?
O8 Mo5 O28 76.83(14) . 2_655 ?
O8 Mo5 O28 78.60(15) 2_655 2_655 ?
O29 Mo5 Mo5 90.32(18) . 2_655 ?
O18 Mo5 Mo5 124.79(15) . 2_655 ?
O15 Mo5 Mo5 130.15(13) . 2_655 ?
O8 Mo5 Mo5 39.45(13) . 2_655 ?
O8 Mo5 Mo5 38.77(11) 2_655 2_655 ?
O28 Mo5 Mo5 87.21(10) 2_655 2_655 ?
Mo7 O5 Mo2 132.3(2) . . ?
O13 Mo7 O11 102.1(2) . . ?
O13 Mo7 O27 103.7(2) . . ?
O11 Mo7 O27 87.40(17) . . ?
O13 Mo7 O6 106.4(2) . . ?
O11 Mo7 O6 150.94(18) . . ?
O27 Mo7 O6 91.09(16) . . ?
O13 Mo7 O5 98.5(2) . . ?
O11 Mo7 O5 84.57(18) . . ?
O27 Mo7 O5 157.55(18) . . ?
O6 Mo7 O5 85.92(17) . . ?
O13 Mo7 O12 172.54(19) . . ?
O11 Mo7 O12 71.57(15) . . ?
O27 Mo7 O12 80.28(15) . . ?
O6 Mo7 O12 79.57(15) . . ?
O5 Mo7 O12 77.30(16) . . ?
O13 Mo7 Mo6 96.15(17) . . ?
O11 Mo7 Mo6 134.44(12) . . ?
O27 Mo7 Mo6 47.57(12) . . ?
O6 Mo7 Mo6 47.62(11) . . ?
O5 Mo7 Mo6 133.53(13) . . ?
O12 Mo7 Mo6 91.18(9) . . ?
Mo11 O7 Mo2 148.3(2) . . ?
O26 Mo10 O22 105.1(2) . . ?
O26 Mo10 O23 103.4(2) . . ?
O22 Mo10 O23 97.5(2) . . ?
O26 Mo10 O27 97.9(2) . 2_655 ?
O22 Mo10 O27 86.65(18) . 2_655 ?
O23 Mo10 O27 156.36(18) . 2_655 ?
O26 Mo10 O21 96.1(2) . . ?
O22 Mo10 O21 156.95(18) . . ?
O23 Mo10 O21 86.21(18) . . ?
O27 Mo10 O21 81.41(15) 2_655 . ?
O26 Mo10 O17 176.4(2) . 2_655 ?
O22 Mo10 O17 78.26(18) . 2_655 ?
O23 Mo10 O17 77.42(17) . 2_655 ?
O27 Mo10 O17 80.70(15) 2_655 2_655 ?
O21 Mo10 O17 80.39(15) . 2_655 ?
Mo11 O10 Mo9 149.4(2) . . ?
Mo8 O17 Mo11 98.09(16) . 2_655 ?
Mo8 O17 Mo10 96.97(17) . 2_655 ?
Mo11 O17 Mo10 95.43(15) 2_655 2_655 ?
Mo8 O16 Mo6 151.0(2) . . ?
O24 Mo9 O11 99.7(2) . . ?
O24 Mo9 O21 106.4(2) . . ?
O11 Mo9 O21 153.79(16) . . ?
O24 Mo9 O21 103.91(19) . 2_655 ?
O11 Mo9 O21 85.82(17) . 2_655 ?
O21 Mo9 O21 90.82(16) . 2_655 ?
O24 Mo9 O10 98.28(19) . . ?
O11 Mo9 O10 85.44(17) . . ?
O21 Mo9 O10 87.82(17) . . ?
O21 Mo9 O10 157.22(16) 2_655 . ?
O24 Mo9 O12 171.8(2) . . ?
O11 Mo9 O12 72.79(15) . . ?
O21 Mo9 O12 81.04(15) . . ?
O21 Mo9 O12 79.13(14) 2_655 . ?
O10 Mo9 O12 78.19(15) . . ?
O24 Mo9 Mo9 96.92(17) . 2_655 ?
O11 Mo9 Mo9 132.78(12) . 2_655 ?
O21 Mo9 Mo9 47.33(11) . 2_655 ?
O21 Mo9 Mo9 47.23(12) 2_655 2_655 ?
O10 Mo9 Mo9 135.11(13) . 2_655 ?
O12 Mo9 Mo9 90.71(9) . 2_655 ?
Mo5 O15 Mo6 123.1(2) . . ?
O19 Mo8 O25 104.3(2) . . ?
O19 Mo8 O16 103.4(2) . . ?
O25 Mo8 O16 98.84(19) . . ?
O19 Mo8 O20 95.2(2) . . ?
O25 Mo8 O20 96.64(19) . . ?
O16 Mo8 O20 151.92(18) . . ?
O19 Mo8 O17 159.4(2) . . ?
O25 Mo8 O17 92.99(18) . . ?
O16 Mo8 O17 84.43(16) . . ?
O20 Mo8 O17 71.46(16) . . ?
O19 Mo8 O22 91.3(2) . 2_655 ?
O25 Mo8 O22 164.17(18) . 2_655 ?
O16 Mo8 O22 79.77(18) . 2_655 ?
O20 Mo8 O22 78.98(18) . 2_655 ?
O17 Mo8 O22 71.18(16) . 2_655 ?
Mo5 O8 Mo5 101.78(18) . 2_655 ?
Mo5 O8 Mo1 131.2(2) . . ?
Mo5 O8 Mo1 126.97(19) 2_655 . ?
Mo5 O18 Mo3 141.7(3) . 2_655 ?
O9 Mo11 O7 104.0(2) . . ?
O9 Mo11 O10 103.5(2) . . ?
O7 Mo11 O10 95.7(2) . . ?
O9 Mo11 O20 97.4(2) . 2_655 ?
O7 Mo11 O20 95.13(19) . 2_655 ?
O10 Mo11 O20 153.30(18) . 2_655 ?
O9 Mo11 O23 92.6(2) . . ?
O7 Mo11 O23 163.36(17) . . ?
O10 Mo11 O23 80.90(18) . . ?
O20 Mo11 O23 81.79(18) 2_655 . ?
O9 Mo11 O17 162.2(2) . 2_655 ?
O7 Mo11 O17 90.94(17) . 2_655 ?
O10 Mo11 O17 84.26(17) . 2_655 ?
O20 Mo11 O17 71.22(16) 2_655 2_655 ?
O23 Mo11 O17 72.55(16) . 2_655 ?
Mo7 O11 Mo9 123.3(2) . . ?
O14 Mo6 O16 98.7(2) . . ?
O14 Mo6 O27 106.8(2) . . ?
O16 Mo6 O27 87.89(16) . . ?
O14 Mo6 O6 103.1(2) . . ?
O16 Mo6 O6 157.71(18) . . ?
O27 Mo6 O6 90.05(16) . . ?
O14 Mo6 O15 99.3(2) . . ?
O16 Mo6 O15 87.40(17) . . ?
O27 Mo6 O15 153.87(18) . . ?
O6 Mo6 O15 84.73(17) . . ?
O14 Mo6 O28 170.9(2) . 2_655 ?
O16 Mo6 O28 79.47(16) . 2_655 ?
O27 Mo6 O28 82.13(15) . 2_655 ?
O6 Mo6 O28 78.26(15) . 2_655 ?
O15 Mo6 O28 71.74(16) . 2_655 ?
O14 Mo6 Mo7 96.08(17) . . ?
O16 Mo6 Mo7 134.90(12) . . ?
O27 Mo6 Mo7 47.02(11) . . ?
O6 Mo6 Mo7 47.04(12) . . ?
O15 Mo6 Mo7 131.61(12) . . ?
O28 Mo6 Mo7 91.41(9) 2_655 . ?
C24 N6 C23 119(3) . . ?
Mo7 O6 Mo6 85.33(16) . . ?
Mo7 O6 Mo1 134.9(2) . . ?
Mo6 O6 Mo1 138.9(2) . . ?
Mo10 O23 Mo11 114.5(2) . . ?
Mo10 O22 Mo8 113.6(2) . 2_655 ?
Mo9 O21 Mo9 85.44(15) . 2_655 ?
Mo9 O21 Mo10 137.5(2) . . ?
Mo9 O21 Mo10 136.9(2) 2_655 . ?
Mo11 O20 Mo8 116.13(19) 2_655 . ?
Mo8 O25 Mo3 146.3(2) . 2_655 ?
Mo4 O28 Mo6 127.2(2) . 2_655 ?
Mo4 O28 Mo5 125.4(2) . 2_655 ?
Mo6 O28 Mo5 91.61(14) 2_655 2_655 ?
Mo7 O27 Mo6 85.41(16) . . ?
Mo7 O27 Mo10 136.8(2) . 2_655 ?
Mo6 O27 Mo10 137.7(2) . 2_655 ?
C4 N3 C3 117.6(6) . . ?
C4 N3 Mo3 124.3(5) . . ?
C3 N3 Mo3 118.1(4) . . ?
C2 N1 C1 118.9(8) . . ?
C2 N1 Mo1 120.6(6) . . ?
C1 N1 Mo1 120.3(7) . . ?
N3 C3 C7 122.9(7) . . ?
N3 C4 C5 121.4(8) . . ?
N1 C2 C10 122.9(11) . . ?
N1 C1 C8 121.0(11) . . ?
C6 C7 C3 118.4(8) . . ?
C5 C6 C7 119.0(8) . . ?
C6 C5 C4 120.6(8) . . ?
C10 C9 C8 120.1(11) . . ?
C9 C8 C1 119.0(11) . . ?
C9 C10 C2 118.1(13) . . ?
C17 N4 C16 112.8(9) . . ?
Mo4 O12 Mo9 126.37(19) . . ?
Mo4 O12 Mo7 123.41(19) . . ?
Mo9 O12 Mo7 92.12(13) . . ?
C11 N2 C15 120.0 . . ?
C11 N2 Mo2 120.0(4) . . ?
C15 N2 Mo2 119.3(4) . . ?
C12 C11 N2 120.0 . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C14 C15 N2 120.0 . . ?
C18 N5 C22 120.0 . . ?
N5 C18 C19 120.0 . . ?
C18 C19 C20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C20 C21 C22 120.0 . . ?
C21 C22 N5 120.0 . . ?

_refine_diff_density_max         1.444
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.162



####################################################################### 
# 
# 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_20170619-l16-a_sq_sq
_database_code_depnum_ccdc_archive 'CCDC 1899132'
loop_
_audit_author_name
_audit_author_address
'Luo Benlong'
;Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2019-04-11 deposited with the CCDC.	2019-04-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT342_20170619-l16-a_sq_sq 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.027 Ang.
RESPONSE: This is caused by the disordered solvent molecule .
;
_vrf_PLAT430_20170619-l16-a_sq_sq 
;
PROBLEM: Short Inter D...A Contact  O10      ..O20      .       2.70 Ang.
RESPONSE: This is caused by the O10 ...O20 hydrogen bond.
;
# Added during the CSD deposition process: Thursday 11 April 2019 04:51 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H62 Ge5 Mo32 N12 O96 Zn,2(C5H5N),3(C5H5N)'
_chemical_formula_sum            'C85 H87 Ge5 Mo32 N17 O96 Zn'
_chemical_formula_weight         6381.11

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'
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'
Ge Ge 0.1547 1.8001 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.763(4)
_cell_length_b                   13.703(2)
_cell_length_c                   27.665(5)
_cell_angle_alpha                90
_cell_angle_beta                 112.075(3)
_cell_angle_gamma                90
_cell_volume                     7997(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9795
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.650
_exptl_crystal_F_000             6036
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    3.583
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 5.814
_diffrn_reflns_number            39566
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.036
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             9454
_reflns_number_gt                8410
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     0.988
_reflns_Friedel_fraction_full    0.988

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'diamond 3.0'
_refine_special_details          
'According to the elemental analysis (Ge:Zn = 5:1), cluster 2 results from the alternative arrangement of [??Ge3??] and [??Ge2Zn??]2-, which gives the formal presence of Zn1 and Ge2 at the same position.'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+278.6125P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9454
_refine_ls_number_parameters     532
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0643
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1198
_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_restrained_S_all      1.290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.34936(5) 0.500000 0.29328(4) 0.0316(3) Uani 1 2 d S T P A .
N1 N 0.4408(5) 0.500000 0.2810(4) 0.034(3) Uani 1 2 d S T P . .
O1 O 0.3868(3) 0.3934(7) 0.3397(2) 0.050(2) Uani 1 1 d . . . . .
Ge1 Ge 0.11096(6) 0.500000 0.26110(5) 0.0316(3) Uani 1 2 d S T P . .
Mo2 Mo 0.30975(4) 0.40996(9) 0.35354(3) 0.0424(3) Uani 1 1 d . . . . .
Ge2 Ge 0.26574(4) 0.29992(8) 0.23535(4) 0.0321(2) Uani 0.75 1 d . . P A 1
O10 O 0.3039(6) 0.1970(8) 0.2259(6) 0.057(4) Uani 0.75 1 d . . P A 1
Zn1 Zn 0.26574(4) 0.29992(8) 0.23535(4) 0.0321(2) Uani 0.25 1 d . . P A 2
O10A O 0.299(2) 0.157(4) 0.2484(19) 0.087(14) Uani 0.25 1 d . . P A 2
O2 O 0.3435(5) 0.500000 0.4111(4) 0.060(4) Uani 1 2 d S T P . .
Mo3 Mo 0.26626(4) 0.500000 0.16484(4) 0.0219(2) Uani 1 2 d S T P A .
N3 N 0.3567(4) 0.500000 0.1511(4) 0.023(2) Uani 1 2 d S T P . .
O3 O 0.2614(4) 0.500000 0.2949(3) 0.031(2) Uani 1 2 d S T P . .
Mo4 Mo 0.16348(3) 0.41028(6) 0.12706(3) 0.02207(15) Uani 1 1 d . . . . .
O4 O 0.3106(3) 0.4046(5) 0.2288(2) 0.0278(13) Uani 1 1 d . . . . .
Mo5 Mo 0.10157(3) 0.27661(6) 0.19199(3) 0.02691(17) Uani 1 1 d . . . . .
O5 O 0.2432(3) 0.3930(5) 0.1169(2) 0.0271(13) Uani 1 1 d . . . . .
N5 N 0.4598(15) 0.500000 0.5819(13) 0.153(8) Uani 1 2 d S TU P . .
Mo6 Mo 0.00795(5) 0.500000 0.12424(4) 0.0249(2) Uani 1 2 d S T P . .
O6 O 0.1250(4) 0.500000 0.0707(3) 0.0248(18) Uani 1 2 d S T P . .
Mo7 Mo -0.03843(3) 0.37748(6) 0.20694(3) 0.02909(18) Uani 1 1 d . . . . .
O7 O 0.1930(4) 0.500000 0.1891(3) 0.0213(17) Uani 1 2 d S T P . .
C17 C 0.4275(13) 0.420(2) 0.5814(9) 0.139(6) Uani 1 1 d . U . . .
H17 H 0.447539 0.360656 0.581223 0.167 Uiso 1 1 calc R U . . .
O17 O 0.0225(4) 0.2989(8) 0.3807(3) 0.064(3) Uani 1 1 d . . . . .
O13 O 0.1080(3) 0.2942(7) 0.3290(3) 0.048(2) Uani 1 1 d . . . . .
C18 C 0.3709(14) 0.416(2) 0.5811(10) 0.158(8) Uani 1 1 d . U . . .
H18 H 0.351760 0.355596 0.580236 0.190 Uiso 1 1 calc R U . . .
O18 O 0.0249(4) 0.500000 0.3669(4) 0.049(3) Uani 1 2 d S T P . .
O14 O 0.1380(3) 0.4038(8) 0.4103(3) 0.065(3) Uani 1 1 d . . . . .
O12 O 0.2154(4) 0.1819(8) 0.3593(4) 0.074(3) Uani 1 1 d . . . . .
O11 O 0.2239(3) 0.3949(7) 0.3636(2) 0.048(2) Uani 1 1 d . . . . .
O8 O 0.2641(3) 0.2993(6) 0.3002(3) 0.0437(19) Uani 1 1 d . . . . .
Mo8 Mo 0.18355(4) 0.27689(8) 0.31900(4) 0.0434(3) Uani 1 1 d . . . . .
O9 O 0.1883(3) 0.2991(5) 0.1833(2) 0.0296(14) Uani 1 1 d . . . . .
Mo9 Mo 0.18751(6) 0.500000 0.40176(5) 0.0537(5) Uani 1 2 d S T P . .
Mo10 Mo 0.05285(4) 0.37725(9) 0.34916(3) 0.0461(3) Uani 1 1 d . . . . .
O19 O -0.0083(3) 0.3773(6) 0.2804(3) 0.0387(16) Uani 1 1 d . . . . .
C19 C 0.3386(16) 0.500000 0.5821(9) 0.124(7) Uani 1 2 d S TU P . .
H19 H 0.298347 0.499999 0.583268 0.149 Uiso 1 2 calc R U P . .
O26 O -0.0825(4) 0.500000 0.2010(3) 0.030(2) Uani 1 2 d S T P . .
O25 O 0.0336(4) 0.500000 0.2135(3) 0.0260(19) Uani 1 2 d S T P . .
O24 O -0.0422(3) 0.5972(5) 0.1321(2) 0.0289(13) Uani 1 1 d . . . . .
O23 O -0.0084(4) 0.500000 0.0597(3) 0.037(2) Uani 1 2 d S T P . .
O22 O 0.0822(2) 0.3944(4) 0.1443(2) 0.0230(12) Uani 1 1 d . . . . .
N4 N 0.1262(4) 0.2973(6) 0.0646(3) 0.0362(18) Uani 1 1 d . . . . .
N2 N 0.3499(4) 0.2912(10) 0.4133(3) 0.067(4) Uani 1 1 d . . . . .
O20 O -0.1004(3) 0.2990(5) 0.1905(3) 0.0420(17) Uani 1 1 d . . . . .
O21 O 0.0289(3) 0.2948(5) 0.2065(3) 0.0341(15) Uani 1 1 d . . . . .
C1 C 0.4697(4) 0.4178(8) 0.2797(4) 0.043(3) Uani 1 1 d . . . . .
H1 H 0.449316 0.359301 0.280392 0.051 Uiso 1 1 calc R U . . .
O29 O 0.1456(3) 0.3899(5) 0.2549(2) 0.0330(15) Uani 1 1 d . . . . .
O28 O 0.1465(3) 0.2080(5) 0.2554(3) 0.0413(18) Uani 1 1 d . . . . .
O27 O 0.0799(3) 0.1811(6) 0.1510(3) 0.0479(19) Uani 1 1 d . . . . .
C10 C 0.4714(6) 0.500000 0.1398(5) 0.037(3) Uani 1 2 d S T P . .
H10 H 0.510291 0.499998 0.136106 0.044 Uiso 1 2 calc R U P . .
C6 C 0.5294(5) 0.4149(10) 0.2773(5) 0.053(3) Uani 1 1 d . . . . .
H6 H 0.548911 0.355611 0.276560 0.064 Uiso 1 1 calc R U . . .
C9 C 0.4428(4) 0.4138(8) 0.1426(4) 0.041(2) Uani 1 1 d . . . . .
H9 H 0.461904 0.354545 0.140957 0.049 Uiso 1 1 calc R U . . .
C8 C 0.3849(4) 0.4163(7) 0.1478(4) 0.037(2) Uani 1 1 d . . . . .
H8 H 0.364813 0.357779 0.149070 0.045 Uiso 1 1 calc R U . . .
C7 C 0.5584(6) 0.500000 0.2761(6) 0.052(5) Uani 1 2 d S T P . .
H7 H 0.598467 0.499999 0.274416 0.063 Uiso 1 2 calc R U P . .
C11 C 0.0854(6) 0.3178(10) 0.0177(5) 0.063(4) Uani 1 1 d . . . . .
H11 H 0.069507 0.380890 0.010416 0.075 Uiso 1 1 calc R U . . .
C4 C 0.3922(6) 0.2284(13) 0.4104(5) 0.078(5) Uani 1 1 d . . . . .
H4 H 0.407168 0.234153 0.383562 0.093 Uiso 1 1 calc R U . . .
C2 C 0.3287(7) 0.2801(16) 0.4526(5) 0.094(7) Uani 1 1 d . . . . .
H2 H 0.298520 0.323639 0.454948 0.113 Uiso 1 1 calc R U . . .
C3 C 0.3494(8) 0.2083(18) 0.4887(6) 0.114(8) Uani 1 1 d . . . . .
H3 H 0.333623 0.203430 0.515102 0.137 Uiso 1 1 calc R U . . .
C5 C 0.4144(9) 0.1558(15) 0.4457(7) 0.110(7) Uani 1 1 d . . . . .
H5 H 0.444596 0.112763 0.442915 0.132 Uiso 1 1 calc R U . . .
C12 C 0.1478(9) 0.2078(11) 0.0735(5) 0.092(6) Uani 1 1 d . . . . .
H12 H 0.175961 0.191849 0.106819 0.110 Uiso 1 1 calc R U . . .
C13 C 0.3925(9) 0.1446(16) 0.4864(6) 0.106(7) Uani 1 1 d . . . . .
H13 H 0.407392 0.094787 0.510830 0.128 Uiso 1 1 calc R U . . .
C14 C 0.0653(10) 0.2473(15) -0.0218(6) 0.107(7) Uani 1 1 d . . . . .
H14 H 0.036835 0.263792 -0.054961 0.129 Uiso 1 1 calc R U . . .
C15 C 0.0868(14) 0.1585(15) -0.0116(8) 0.147(11) Uani 1 1 d . . . . .
H15 H 0.071898 0.110390 -0.037081 0.177 Uiso 1 1 calc R U . . .
O15 O 0.2491(5) 0.500000 0.4599(4) 0.087(6) Uani 1 2 d S T P . .
C16 C 0.1305(11) 0.1360(18) 0.0356(9) 0.128(8) Uani 1 1 d . U . . .
H16 H 0.148448 0.074086 0.042552 0.154 Uiso 1 1 calc R U . . .
O16 O 0.1037(4) 0.500000 0.3222(3) 0.036(2) Uani 1 2 d S T P . .


_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 1.921(8) . ?
Mo1 O1 1.921(8) 6_565 ?
Mo1 O3 2.019(8) . ?
Mo1 O4 2.119(6) . ?
Mo1 O4 2.119(6) 6_565 ?
Mo1 N1 2.232(10) . ?
Mo1 Mo2 2.4988(12) . ?
Mo1 Mo2 2.4989(12) 6_565 ?
N1 C1 1.311(12) 6_565 ?
N1 C1 1.311(12) . ?
O1 Mo2 1.943(6) . ?
Ge1 O29 1.741(7) 6_565 ?
Ge1 O29 1.741(7) . ?
Ge1 O25 1.759(8) . ?
Ge1 O16 1.759(8) . ?
Mo2 O2 1.931(7) . ?
Mo2 O3 2.006(6) . ?
Mo2 O11 2.085(6) . ?
Mo2 O8 2.098(8) . ?
Mo2 N2 2.254(10) . ?
Mo2 Mo2 2.468(2) 6_565 ?
Ge2 O10 1.727(10) . ?
Ge2 O8 1.809(7) . ?
Ge2 O4 1.809(6) . ?
Ge2 O9 1.810(6) . ?
Zn1 O8 1.809(7) . ?
Zn1 O4 1.809(6) . ?
Zn1 O9 1.810(6) . ?
Zn1 O10A 2.08(5) . ?
Mo3 O5 1.913(6) . ?
Mo3 O5 1.913(6) 6_565 ?
Mo3 O7 2.019(7) . ?
Mo3 O4 2.125(6) 6_565 ?
Mo3 O4 2.125(6) . ?
Mo3 N3 2.231(9) . ?
Mo3 Mo4 2.4978(11) 6_565 ?
Mo3 Mo4 2.4978(11) . ?
N3 C8 1.333(11) 6_565 ?
N3 C8 1.333(11) . ?
Mo4 O6 1.918(6) . ?
Mo4 O5 1.952(5) . ?
Mo4 O7 2.011(6) . ?
Mo4 O22 2.090(5) . ?
Mo4 O9 2.097(6) . ?
Mo4 N4 2.236(8) . ?
Mo4 Mo4 2.4587(16) 6_565 ?
Mo5 O27 1.680(8) . ?
Mo5 O21 1.858(6) . ?
Mo5 O28 1.912(7) . ?
Mo5 O22 2.025(6) . ?
Mo5 O9 2.100(6) . ?
Mo5 O29 2.266(7) . ?
N5 C17 1.32(3) 6_565 ?
N5 C17 1.32(3) . ?
Mo6 O23 1.682(9) . ?
Mo6 O24 1.820(6) . ?
Mo6 O24 1.820(6) 6_565 ?
Mo6 O22 2.133(6) 6_565 ?
Mo6 O22 2.133(5) . ?
Mo6 O25 2.313(8) . ?
Mo7 O20 1.694(6) . ?
Mo7 O19 1.885(7) . ?
Mo7 O21 1.911(6) . ?
Mo7 O26 1.930(4) . ?
Mo7 O24 2.068(6) 6_565 ?
Mo7 O25 2.306(5) . ?
C17 C18 1.29(3) . ?
O17 Mo10 1.688(8) . ?
O13 Mo8 1.858(6) . ?
O13 Mo10 1.925(8) . ?
C18 C19 1.37(3) . ?
O18 Mo10 1.926(4) . ?
O18 Mo10 1.926(4) 6_565 ?
O14 Mo9 1.808(9) . ?
O14 Mo10 2.070(7) . ?
O12 Mo8 1.690(8) . ?
O11 Mo8 2.032(9) . ?
O11 Mo9 2.129(8) . ?
O8 Mo8 2.108(6) . ?
Mo8 O28 1.893(8) . ?
Mo8 O29 2.265(6) . ?
Mo9 O15 1.690(11) . ?
Mo9 O16 2.308(8) . ?
Mo10 O19 1.888(7) . ?
Mo10 O16 2.318(6) . ?
N4 C12 1.308(16) . ?
N4 C11 1.312(14) . ?
N2 C4 1.315(17) . ?
N2 C2 1.355(15) . ?
C1 C6 1.386(13) . ?
C10 C9 1.365(12) . ?
C10 C9 1.365(12) 6_565 ?
C6 C7 1.347(14) . ?
C9 C8 1.379(12) . ?
C11 C14 1.399(19) . ?
C4 C5 1.35(2) . ?
C2 C3 1.35(2) . ?
C3 C13 1.33(2) . ?
C5 C13 1.40(2) . ?
C12 C16 1.38(2) . ?
C14 C15 1.30(3) . ?
C15 C16 1.35(3) . ?

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 O1 99.1(5) . 6_565 ?
O1 Mo1 O3 100.3(2) . . ?
O1 Mo1 O3 100.3(2) 6_565 . ?
O1 Mo1 O4 91.9(3) . . ?
O1 Mo1 O4 166.5(3) 6_565 . ?
O3 Mo1 O4 85.2(2) . . ?
O1 Mo1 O4 166.5(3) . 6_565 ?
O1 Mo1 O4 91.9(3) 6_565 6_565 ?
O3 Mo1 O4 85.2(2) . 6_565 ?
O4 Mo1 O4 76.2(3) . 6_565 ?
O1 Mo1 N1 84.1(3) . . ?
O1 Mo1 N1 84.1(3) 6_565 . ?
O3 Mo1 N1 173.1(4) . . ?
O4 Mo1 N1 89.4(3) . . ?
O4 Mo1 N1 89.4(3) 6_565 . ?
O1 Mo1 Mo2 50.10(18) . . ?
O1 Mo1 Mo2 96.3(2) 6_565 . ?
O3 Mo1 Mo2 51.40(17) . . ?
O4 Mo1 Mo2 96.71(16) . . ?
O4 Mo1 Mo2 136.57(15) 6_565 . ?
N1 Mo1 Mo2 133.8(2) . . ?
O1 Mo1 Mo2 96.3(2) . 6_565 ?
O1 Mo1 Mo2 50.10(18) 6_565 6_565 ?
O3 Mo1 Mo2 51.40(17) . 6_565 ?
O4 Mo1 Mo2 136.57(15) . 6_565 ?
O4 Mo1 Mo2 96.72(16) 6_565 6_565 ?
N1 Mo1 Mo2 133.8(2) . 6_565 ?
Mo2 Mo1 Mo2 59.18(6) . 6_565 ?
C1 N1 C1 118.4(11) 6_565 . ?
C1 N1 Mo1 120.7(6) 6_565 . ?
C1 N1 Mo1 120.7(6) . . ?
Mo1 O1 Mo2 80.6(3) . . ?
O29 Ge1 O29 120.2(4) 6_565 . ?
O29 Ge1 O25 106.8(2) 6_565 . ?
O29 Ge1 O25 106.8(2) . . ?
O29 Ge1 O16 107.7(2) 6_565 . ?
O29 Ge1 O16 107.7(2) . . ?
O25 Ge1 O16 106.9(4) . . ?
O2 Mo2 O1 97.4(4) . . ?
O2 Mo2 O3 101.6(2) . . ?
O1 Mo2 O3 100.0(3) . . ?
O2 Mo2 O11 93.2(4) . . ?
O1 Mo2 O11 167.1(4) . . ?
O3 Mo2 O11 85.0(3) . . ?
O2 Mo2 O8 168.5(3) . . ?
O1 Mo2 O8 91.2(3) . . ?
O3 Mo2 O8 84.2(2) . . ?
O11 Mo2 O8 77.4(3) . . ?
O2 Mo2 N2 86.0(4) . . ?
O1 Mo2 N2 85.0(3) . . ?
O3 Mo2 N2 170.2(3) . . ?
O11 Mo2 N2 88.4(3) . . ?
O8 Mo2 N2 87.2(4) . . ?
O2 Mo2 Mo2 50.27(18) . 6_565 ?
O1 Mo2 Mo2 96.7(3) . 6_565 ?
O3 Mo2 Mo2 52.05(14) . 6_565 ?
O11 Mo2 Mo2 95.7(3) . 6_565 ?
O8 Mo2 Mo2 136.28(18) . 6_565 ?
N2 Mo2 Mo2 136.2(3) . 6_565 ?
O2 Mo2 Mo1 95.9(2) . . ?
O1 Mo2 Mo1 49.3(2) . . ?
O3 Mo2 Mo1 51.9(2) . . ?
O11 Mo2 Mo1 136.84(19) . . ?
O8 Mo2 Mo1 95.46(18) . . ?
N2 Mo2 Mo1 134.2(2) . . ?
Mo2 Mo2 Mo1 60.41(3) 6_565 . ?
O10 Ge2 O8 110.2(5) . . ?
O10 Ge2 O4 107.3(4) . . ?
O8 Ge2 O4 109.0(3) . . ?
O10 Ge2 O9 105.6(5) . . ?
O8 Ge2 O9 114.4(3) . . ?
O4 Ge2 O9 110.0(3) . . ?
O8 Zn1 O4 109.0(3) . . ?
O8 Zn1 O9 114.4(3) . . ?
O4 Zn1 O9 110.0(3) . . ?
O8 Zn1 O10A 88.1(13) . . ?
O4 Zn1 O10A 125.3(13) . . ?
O9 Zn1 O10A 108.5(14) . . ?
Mo2 O2 Mo2 79.5(4) 6_565 . ?
O5 Mo3 O5 100.1(4) . 6_565 ?
O5 Mo3 O7 100.6(2) . . ?
O5 Mo3 O7 100.6(2) 6_565 . ?
O5 Mo3 O4 165.7(3) . 6_565 ?
O5 Mo3 O4 91.5(3) 6_565 6_565 ?
O7 Mo3 O4 85.2(2) . 6_565 ?
O5 Mo3 O4 91.5(3) . . ?
O5 Mo3 O4 165.7(3) 6_565 . ?
O7 Mo3 O4 85.2(2) . . ?
O4 Mo3 O4 75.9(3) 6_565 . ?
O5 Mo3 N3 85.0(2) . . ?
O5 Mo3 N3 85.0(2) 6_565 . ?
O7 Mo3 N3 171.1(3) . . ?
O4 Mo3 N3 87.8(2) 6_565 . ?
O4 Mo3 N3 87.8(2) . . ?
O5 Mo3 Mo4 96.75(18) . 6_565 ?
O5 Mo3 Mo4 50.42(17) 6_565 6_565 ?
O7 Mo3 Mo4 51.56(17) . 6_565 ?
O4 Mo3 Mo4 97.05(16) 6_565 6_565 ?
O4 Mo3 Mo4 136.75(15) . 6_565 ?
N3 Mo3 Mo4 135.08(18) . 6_565 ?
O5 Mo3 Mo4 50.42(17) . . ?
O5 Mo3 Mo4 96.75(18) 6_565 . ?
O7 Mo3 Mo4 51.56(17) . . ?
O4 Mo3 Mo4 136.76(15) 6_565 . ?
O4 Mo3 Mo4 97.06(16) . . ?
N3 Mo3 Mo4 135.08(18) . . ?
Mo4 Mo3 Mo4 58.97(4) 6_565 . ?
C8 N3 C8 118.7(10) 6_565 . ?
C8 N3 Mo3 120.6(5) 6_565 . ?
C8 N3 Mo3 120.6(5) . . ?
Mo2 O3 Mo2 75.9(3) . 6_565 ?
Mo2 O3 Mo1 76.7(3) . . ?
Mo2 O3 Mo1 76.7(3) 6_565 . ?
O6 Mo4 O5 97.3(3) . . ?
O6 Mo4 O7 101.9(2) . . ?
O5 Mo4 O7 99.6(3) . . ?
O6 Mo4 O22 94.5(3) . . ?
O5 Mo4 O22 166.2(2) . . ?
O7 Mo4 O22 84.7(3) . . ?
O6 Mo4 O9 168.9(3) . . ?
O5 Mo4 O9 90.7(2) . . ?
O7 Mo4 O9 84.3(2) . . ?
O22 Mo4 O9 76.7(2) . . ?
O6 Mo4 N4 83.8(3) . . ?
O5 Mo4 N4 84.7(3) . . ?
O7 Mo4 N4 172.3(3) . . ?
O22 Mo4 N4 89.6(3) . . ?
O9 Mo4 N4 89.3(3) . . ?
O6 Mo4 Mo4 50.15(15) . 6_565 ?
O5 Mo4 Mo4 96.99(19) . 6_565 ?
O7 Mo4 Mo4 52.32(13) . 6_565 ?
O22 Mo4 Mo4 95.97(16) . 6_565 ?
O9 Mo4 Mo4 136.58(18) . 6_565 ?
N4 Mo4 Mo4 133.8(2) . 6_565 ?
O6 Mo4 Mo3 95.4(2) . . ?
O5 Mo4 Mo3 49.06(18) . . ?
O7 Mo4 Mo3 51.8(2) . . ?
O22 Mo4 Mo3 136.57(16) . . ?
O9 Mo4 Mo3 95.63(17) . . ?
N4 Mo4 Mo3 133.5(2) . . ?
Mo4 Mo4 Mo3 60.52(2) 6_565 . ?
Zn1 O4 Mo1 118.5(3) . . ?
Ge2 O4 Mo1 118.5(3) . . ?
Zn1 O4 Mo3 117.5(3) . . ?
Ge2 O4 Mo3 117.5(3) . . ?
Mo1 O4 Mo3 103.8(3) . . ?
O27 Mo5 O21 101.0(3) . . ?
O27 Mo5 O28 99.0(4) . . ?
O21 Mo5 O28 94.7(3) . . ?
O27 Mo5 O22 104.2(3) . . ?
O21 Mo5 O22 92.3(2) . . ?
O28 Mo5 O22 154.1(3) . . ?
O27 Mo5 O9 95.0(3) . . ?
O21 Mo5 O9 163.0(3) . . ?
O28 Mo5 O9 88.6(2) . . ?
O22 Mo5 O9 78.0(2) . . ?
O27 Mo5 O29 170.1(3) . . ?
O21 Mo5 O29 85.2(3) . . ?
O28 Mo5 O29 72.7(3) . . ?
O22 Mo5 O29 83.1(2) . . ?
O9 Mo5 O29 79.8(2) . . ?
Mo3 O5 Mo4 80.5(2) . . ?
C17 N5 C17 113(4) 6_565 . ?
O23 Mo6 O24 103.2(3) . . ?
O23 Mo6 O24 103.2(3) . 6_565 ?
O24 Mo6 O24 94.0(4) . 6_565 ?
O23 Mo6 O22 96.6(3) . 6_565 ?
O24 Mo6 O22 86.8(2) . 6_565 ?
O24 Mo6 O22 159.4(2) 6_565 6_565 ?
O23 Mo6 O22 96.6(3) . . ?
O24 Mo6 O22 159.4(2) . . ?
O24 Mo6 O22 86.8(2) 6_565 . ?
O22 Mo6 O22 85.4(3) 6_565 . ?
O23 Mo6 O25 178.3(4) . . ?
O24 Mo6 O25 77.9(2) . . ?
O24 Mo6 O25 77.9(2) 6_565 . ?
O22 Mo6 O25 82.2(2) 6_565 . ?
O22 Mo6 O25 82.2(2) . . ?
Mo4 O6 Mo4 79.7(3) . 6_565 ?
O20 Mo7 O19 102.6(3) . . ?
O20 Mo7 O21 102.2(3) . . ?
O19 Mo7 O21 92.2(3) . . ?
O20 Mo7 O26 100.1(3) . . ?
O19 Mo7 O26 93.4(3) . . ?
O21 Mo7 O26 155.2(3) . . ?
O20 Mo7 O24 96.9(3) . 6_565 ?
O19 Mo7 O24 160.1(3) . 6_565 ?
O21 Mo7 O24 79.9(3) . 6_565 ?
O26 Mo7 O24 86.8(3) . 6_565 ?
O20 Mo7 O25 168.2(3) . . ?
O19 Mo7 O25 87.5(3) . . ?
O21 Mo7 O25 83.3(2) . . ?
O26 Mo7 O25 72.8(2) . . ?
O24 Mo7 O25 73.6(3) 6_565 . ?
Mo4 O7 Mo4 75.4(3) 6_565 . ?
Mo4 O7 Mo3 76.6(2) 6_565 . ?
Mo4 O7 Mo3 76.6(2) . . ?
C18 C17 N5 126(3) . . ?
Mo8 O13 Mo10 149.3(5) . . ?
C17 C18 C19 120(3) . . ?
Mo10 O18 Mo10 121.7(4) . 6_565 ?
Mo9 O14 Mo10 117.3(4) . . ?
Mo8 O11 Mo2 103.3(3) . . ?
Mo8 O11 Mo9 131.9(3) . . ?
Mo2 O11 Mo9 123.9(4) . . ?
Zn1 O8 Mo2 120.3(4) . . ?
Ge2 O8 Mo2 120.3(4) . . ?
Zn1 O8 Mo8 126.1(4) . . ?
Ge2 O8 Mo8 126.1(4) . . ?
Mo2 O8 Mo8 100.3(3) . . ?
O12 Mo8 O13 101.0(4) . . ?
O12 Mo8 O28 99.2(4) . . ?
O13 Mo8 O28 95.1(3) . . ?
O12 Mo8 O11 103.2(4) . . ?
O13 Mo8 O11 92.3(3) . . ?
O28 Mo8 O11 154.6(3) . . ?
O12 Mo8 O8 94.5(3) . . ?
O13 Mo8 O8 163.4(3) . . ?
O28 Mo8 O8 88.2(3) . . ?
O11 Mo8 O8 78.3(3) . . ?
O12 Mo8 O29 170.2(4) . . ?
O13 Mo8 O29 85.8(3) . . ?
O28 Mo8 O29 73.0(3) . . ?
O11 Mo8 O29 83.3(3) . . ?
O8 Mo8 O29 79.5(2) . . ?
Zn1 O9 Mo4 119.8(3) . . ?
Ge2 O9 Mo4 119.8(3) . . ?
Zn1 O9 Mo5 125.9(3) . . ?
Ge2 O9 Mo5 125.9(3) . . ?
Mo4 O9 Mo5 100.9(2) . . ?
O15 Mo9 O14 102.2(3) . . ?
O15 Mo9 O14 102.2(3) . 6_565 ?
O14 Mo9 O14 93.7(6) . 6_565 ?
O15 Mo9 O11 97.6(3) . 6_565 ?
O14 Mo9 O11 159.5(3) . 6_565 ?
O14 Mo9 O11 87.1(4) 6_565 6_565 ?
O15 Mo9 O11 97.6(3) . . ?
O14 Mo9 O11 87.1(4) . . ?
O14 Mo9 O11 159.5(3) 6_565 . ?
O11 Mo9 O11 85.2(4) 6_565 . ?
O15 Mo9 O16 179.7(4) . . ?
O14 Mo9 O16 78.0(3) . . ?
O14 Mo9 O16 78.0(3) 6_565 . ?
O11 Mo9 O16 82.2(2) 6_565 . ?
O11 Mo9 O16 82.2(2) . . ?
O17 Mo10 O19 103.4(4) . . ?
O17 Mo10 O13 102.3(4) . . ?
O19 Mo10 O13 91.3(3) . . ?
O17 Mo10 O18 100.6(4) . . ?
O19 Mo10 O18 93.9(4) . . ?
O13 Mo10 O18 154.6(3) . . ?
O17 Mo10 O14 97.4(4) . . ?
O19 Mo10 O14 158.8(3) . . ?
O13 Mo10 O14 80.2(3) . . ?
O18 Mo10 O14 86.3(4) . . ?
O17 Mo10 O16 168.3(4) . . ?
O19 Mo10 O16 86.8(3) . . ?
O13 Mo10 O16 83.0(3) . . ?
O18 Mo10 O16 72.6(3) . . ?
O14 Mo10 O16 73.1(3) . . ?
Mo7 O19 Mo10 156.6(3) . . ?
C18 C19 C18 114(4) 6_565 . ?
Mo7 O26 Mo7 120.8(4) 6_565 . ?
Ge1 O25 Mo7 122.7(2) . 6_565 ?
Ge1 O25 Mo7 122.7(2) . . ?
Mo7 O25 Mo7 93.4(3) 6_565 . ?
Ge1 O25 Mo6 125.4(4) . . ?
Mo7 O25 Mo6 91.7(2) 6_565 . ?
Mo7 O25 Mo6 91.7(2) . . ?
Mo6 O24 Mo7 116.8(3) . 6_565 ?
Mo5 O22 Mo4 103.7(2) . . ?
Mo5 O22 Mo6 131.9(3) . . ?
Mo4 O22 Mo6 123.5(3) . . ?
C12 N4 C11 117.5(11) . . ?
C12 N4 Mo4 119.8(8) . . ?
C11 N4 Mo4 122.6(8) . . ?
C4 N2 C2 117.7(13) . . ?
C4 N2 Mo2 122.2(8) . . ?
C2 N2 Mo2 120.1(10) . . ?
Mo5 O21 Mo7 149.6(4) . . ?
N1 C1 C6 122.5(11) . . ?
Ge1 O29 Mo8 124.7(3) . . ?
Ge1 O29 Mo5 125.7(3) . . ?
Mo8 O29 Mo5 93.5(3) . . ?
Mo8 O28 Mo5 120.4(4) . . ?
C9 C10 C9 119.9(12) . 6_565 ?
C7 C6 C1 118.4(12) . . ?
C10 C9 C8 118.6(10) . . ?
N3 C8 C9 122.1(9) . . ?
C6 C7 C6 119.9(13) 6_565 . ?
N4 C11 C14 121.8(14) . . ?
N2 C4 C5 121.5(14) . . ?
C3 C2 N2 122.9(16) . . ?
C13 C3 C2 120.0(14) . . ?
C4 C5 C13 120.7(17) . . ?
N4 C12 C16 123.0(16) . . ?
C3 C13 C5 117.2(14) . . ?
C15 C14 C11 119.3(17) . . ?
C14 C15 C16 120.2(18) . . ?
C15 C16 C12 118(2) . . ?
Ge1 O16 Mo9 125.0(4) . . ?
Ge1 O16 Mo10 123.2(3) . . ?
Mo9 O16 Mo10 91.5(2) . . ?
Ge1 O16 Mo10 123.2(3) . 6_565 ?
Mo9 O16 Mo10 91.5(2) . 6_565 ?
Mo10 O16 Mo10 93.0(3) . 6_565 ?

_refine_diff_density_max         2.007
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.195



