# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_mo_yyx11_0ma
_database_code_depnum_ccdc_archive 'CCDC 2246005'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/d3qi01828h 2023
loop_
_audit_author_name
_audit_author_address
'zi jie'
;Chinese academy of science
China
;
_audit_update_record             
;
2023-07-07 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_audit_creation_date             2023-07-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 Ge2 Mo12 N6 O36, 2(C2 N), 2[H2O]'
_chemical_formula_sum            'C44 H61 Ge2 Mo12 N10 O36.50'
_chemical_formula_weight         2610.48
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.6307(14)
_cell_length_b                   26.0570(16)
_cell_length_c                   16.3669(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8372.0(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9216
_cell_measurement_temperature    301.15
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.56
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.517
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5020
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30350
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.766
_diffrn_reflns_theta_min         3.127
_diffrn_ambient_temperature      301.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4256
_reflns_number_total             4719
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4719
_refine_ls_number_restraints     333
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0322
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0451P)²+33.1332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0891
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H1WB-O1W
 0.85 with sigma of 0.001
 H8-O8
 0.85 with sigma of 0.001
 O1W-H1WA
 0.85 with sigma of 0.001
 H1WB-H1WA
 1.344 with sigma of 0.001
 O8-H8
 0.87 with sigma of 0.001
 N1-C1 = N1-C5
 1.33 with sigma of 0.02
 C1-C2 = C4-C5
 1.38 with sigma of 0.02
 C2-C3 = C3-C4
 1.37 with sigma of 0.02
 N1-C2
 2.4 with sigma of 0.04
 N1-C4
 2.39 with sigma of 0.04
 C1-C3
 2.36 with sigma of 0.04
 C2-C4
 2.35 with sigma of 0.04
 C3-C5
 2.37 with sigma of 0.04
 N1-C1 \\sim N1-C5
 with sigma of 0.02
 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5
 with sigma of 0.02
 N1-C4 \\sim N1-C2
 with sigma of 0.04
 C3-C5 \\sim C3-C1 \\sim C4-C2 \\sim C5-C1
 with sigma of 0.04
 N1-C1 \\sim N6A-C12A
 with sigma of 0.02
 N1-C5 \\sim N6A-C16A
 with sigma of 0.02
 C1-C2 \\sim C12A-C13A
 with sigma of 0.02
 C2-C3 \\sim C13A-C14A
 with sigma of 0.02
 C3-C4 \\sim C14A-C15A
 with sigma of 0.02
 C4-C5 \\sim C15A-C16A
 with sigma of 0.02
 Mo1-C1 \\sim Mo1-C12A
 with sigma of 0.04
 Mo1-C5 \\sim Mo1-C16A
 with sigma of 0.04
 N1-C2 \\sim N6A-C13A
 with sigma of 0.04
 N1-C4 \\sim N6A-C15A
 with sigma of 0.04
 C1-C3 \\sim C12A-C14A
 with sigma of 0.04
 C1-C5 \\sim C12A-C16A
 with sigma of 0.04
 C2-C4 \\sim C13A-C15A
 with sigma of 0.04
 C3-C5 \\sim C14A-C16A
 with sigma of 0.04
 Mo1-N1 \\sim Mo1-N6A
 with sigma of 0.001
3. Restrained planarity
 N1, C1, C2, C3, C4, C5
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N6A) \\sim Ueq,
Uanis(C16A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C14A) \\sim Ueq,
Uanis(C13A) \\sim Ueq, Uanis(C12A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N2, C6, C7, C8, C7, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Mo1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C13, C12, C11, C10, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5, C5, C5, C5, N1, Mo1, C1, C2, C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(N6A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(H14A)=
 Sof(C13A)=Sof(H13A)=Sof(C12A)=Sof(H12A)=1-FVAR(1)
 Sof(N1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=FVAR(1)
 Fixed Sof: O1W(0.125) H1WA(0.25) H1WB(0.25) N3(0.5) H3A(0.5) C9(0.5) H9(0.5)
 C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5)
 Fixed X: H1WB(-0.8796)
 Fixed Z: H8(0.18515) H1WA(0.207709) H1WB(0.28636)
7.a Riding coordinates:
 C14(H14B,H14C,H14D)
7.b Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8A), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C16A(H16A),
 C15A(H15A), C14A(H14A), C13A(H13A), C12A(H12A), N3(H3A), C9(H9), C10(H10),
 C11(H11), C12(H12), C13(H13)
7.d Fitted hexagon refined as free rotating group:
 N3(C9,C10,C11,C12,C13)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo -0.65020(2) -0.38070(2) 0.32620(2) 0.03586(10) Uani 1 1 d D . . . .
Mo2 Mo -0.58483(2) -0.44757(2) 0.250000 0.02559(11) Uani 1 2 d S T P A .
Mo4 Mo -0.58424(2) -0.29258(2) 0.05768(2) 0.03872(11) Uani 1 1 d . . . . .
Mo3 Mo -0.500000 -0.20636(2) 0.17094(3) 0.03132(12) Uani 1 2 d S T P . .
Ge1 Ge -0.500000 -0.41030(2) 0.07945(3) 0.03148(13) Uani 1 2 d S T P A .
O1 O -0.7250(2) -0.37624(16) 0.250000 0.0517(11) Uani 1 2 d S T P A .
O11 O -0.42776(19) -0.21632(14) 0.250000 0.0348(8) Uani 1 2 d S T P . .
O2 O -0.64722(14) -0.45455(10) 0.16127(17) 0.0372(6) Uani 1 1 d . . . . .
O5 O -0.57035(17) -0.36988(12) 0.250000 0.0272(7) Uani 1 2 d S T P A .
O6 O -0.64494(14) -0.30709(10) 0.14240(19) 0.0414(6) Uani 1 1 d . . . . .
O3 O -0.57544(15) -0.37502(10) 0.07803(16) 0.0359(6) Uani 1 1 d . . . . .
O7 O -0.6360(2) -0.29308(13) -0.0252(2) 0.0679(11) Uani 1 1 d . . . . .
O9 O -0.57171(15) -0.22588(10) 0.07846(17) 0.0414(6) Uani 1 1 d . . . . .
O12 O -0.500000 -0.14342(15) 0.1479(3) 0.0465(10) Uani 1 2 d S T P . .
O10 O -0.500000 -0.30645(15) 0.0004(2) 0.0452(10) Uani 1 2 d S T P . .
O8 O -0.500000 -0.29144(12) 0.1540(2) 0.0280(7) Uani 1 2 d DS T P . .
H8 H -0.500000 -0.31803(15) 0.185150 0.042 Uiso 1 2 d DS U P . .
O13 O -0.500000 -0.44949(17) -0.0073(3) 0.0701(16) Uani 1 2 d S T P . .
O1W O -0.8578(10) -0.2801(7) 0.250000 0.074(6) Uani 0.25 2 d DS TU P . .
H1WA H -0.8828(9) -0.2820(10) 0.207709 0.112 Uiso 0.25 1 d D U P . .
H1WB H -0.879600 -0.2966(9) 0.286360 0.112 Uiso 0.25 1 d D U P . .
O4 O -0.500000 -0.45026(12) 0.16824(19) 0.0269(7) Uani 1 2 d S T P . .
N2 N -0.5867(2) -0.53316(16) 0.250000 0.0324(9) Uani 1 2 d S T P . .
C6 C -0.5897(3) -0.55940(18) 0.3197(3) 0.0555(12) Uani 1 1 d . . . . .
H6 H -0.588705 -0.541391 0.368698 0.067 Uiso 1 1 calc R U . . .
C7 C -0.5944(4) -0.61244(19) 0.3222(4) 0.0725(16) Uani 1 1 d . . . . .
H7 H -0.596435 -0.629590 0.371940 0.087 Uiso 1 1 calc R U . . .
C8 C -0.5960(4) -0.6393(3) 0.250000 0.072(2) Uani 1 2 d S T P . .
H8A H -0.598116 -0.674920 0.250001 0.086 Uiso 1 2 calc R U P . .
N4 N -0.7143(4) -0.2317(3) 0.250000 0.0738(19) Uani 1 2 d S T P . .
H4A H -0.669150 -0.234632 0.250001 0.089 Uiso 1 2 calc R U P . .
H4B H -0.731387 -0.263389 0.249999 0.089 Uiso 1 2 calc R U P . .
C14 C -0.7344(4) -0.2070(3) 0.3254(5) 0.106(3) Uani 1 1 d . . . . .
H14B H -0.780874 -0.195834 0.321177 0.159 Uiso 1 1 d R U . . .
H14C H -0.705544 -0.177984 0.335437 0.159 Uiso 1 1 d R U . . .
H14D H -0.730274 -0.230994 0.369717 0.159 Uiso 1 1 d R U . . .
N1 N -0.7224(6) -0.3853(5) 0.4318(7) 0.053(3) Uani 0.55(3) 1 d D U P A 1
C1 C -0.7212(8) -0.4219(5) 0.4873(8) 0.070(3) Uani 0.55(3) 1 d D U P A 1
H1 H -0.686421 -0.446117 0.485277 0.083 Uiso 0.55(3) 1 calc R U P A 1
C2 C -0.7691(9) -0.4257(5) 0.5480(9) 0.085(4) Uani 0.55(3) 1 d D U P A 1
H2 H -0.765682 -0.451649 0.586780 0.102 Uiso 0.55(3) 1 calc R U P A 1
C3 C -0.8214(9) -0.3917(6) 0.5519(11) 0.088(4) Uani 0.55(3) 1 d D U P A 1
H3 H -0.854944 -0.394855 0.591690 0.105 Uiso 0.55(3) 1 calc R U P A 1
C4 C -0.8237(8) -0.3532(6) 0.4968(12) 0.081(4) Uani 0.55(3) 1 d D U P A 1
H4 H -0.858799 -0.329206 0.496693 0.097 Uiso 0.55(3) 1 calc R U P A 1
C5 C -0.7718(7) -0.3511(5) 0.4412(11) 0.069(4) Uani 0.55(3) 1 d D U P A 1
H5 H -0.771062 -0.322946 0.406340 0.083 Uiso 0.55(3) 1 calc R U P A 1
N6A N -0.7378(6) -0.3849(5) 0.4134(8) 0.039(3) Uani 0.45(3) 1 d D U P A 2
C16A C -0.7855(7) -0.3490(5) 0.4110(10) 0.049(4) Uani 0.45(3) 1 d D U P A 2
H16A H -0.783062 -0.324154 0.370280 0.059 Uiso 0.45(3) 1 calc R U P A 2
C15A C -0.8377(7) -0.3466(6) 0.4651(12) 0.064(4) Uani 0.45(3) 1 d D U P A 2
H15A H -0.869239 -0.320037 0.462450 0.077 Uiso 0.45(3) 1 calc R U P A 2
C14A C -0.8431(9) -0.3832(6) 0.5226(12) 0.075(5) Uani 0.45(3) 1 d D U P A 2
H14A H -0.877101 -0.381686 0.562024 0.090 Uiso 0.45(3) 1 calc R U P A 2
C13A C -0.7973(12) -0.4228(7) 0.5217(15) 0.104(6) Uani 0.45(3) 1 d D U P A 2
H13A H -0.801667 -0.449820 0.558382 0.125 Uiso 0.45(3) 1 calc R U P A 2
C12A C -0.7450(11) -0.4222(7) 0.4663(12) 0.078(5) Uani 0.45(3) 1 d D U P A 2
H12A H -0.713788 -0.449068 0.466306 0.093 Uiso 0.45(3) 1 calc R U P A 2
N3 N -0.8120(6) -0.5653(5) 0.2706(11) 0.166(6) Uani 0.5 1 d G U P B -1
H3A H -0.788420 -0.589079 0.293620 0.200 Uiso 0.5 1 calc R U P B -1
C9 C -0.7842(5) -0.5167(6) 0.2598(11) 0.155(5) Uani 0.5 1 d G U P B -1
H9 H -0.740087 -0.509915 0.277494 0.187 Uiso 0.5 1 calc R U P B -1
C10 C -0.8223(8) -0.4783(4) 0.2226(10) 0.158(6) Uani 0.5 1 d G U P B -1
H10 H -0.803692 -0.445820 0.215366 0.189 Uiso 0.5 1 calc R U P B -1
C11 C -0.8882(8) -0.4885(5) 0.1961(8) 0.166(6) Uani 0.5 1 d G U P B -1
H11 H -0.913711 -0.462821 0.171239 0.200 Uiso 0.5 1 calc R U P B -1
C12 C -0.9160(5) -0.5371(6) 0.2069(10) 0.157(6) Uani 0.5 1 d G U P B -1
H12 H -0.960126 -0.543918 0.189239 0.188 Uiso 0.5 1 calc R U P B -1
C13 C -0.8779(7) -0.5755(4) 0.2442(12) 0.149(5) Uani 0.5 1 d G U P B -1
H13 H -0.896521 -0.608015 0.251366 0.179 Uiso 0.5 1 calc R U P B -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Mo1 2.4943(7) 10_556 ?
Mo1 Mo2 2.4977(5) . ?
Mo1 O1 1.930(3) . ?
Mo1 O2 1.936(3) 10_556 ?
Mo1 O5 2.023(3) . ?
Mo1 O6 1.988(3) 10_556 ?
Mo1 O3 2.152(3) 10_556 ?
Mo1 N1 2.238(4) . ?
Mo1 N6A 2.238(4) . ?
Mo2 O2 1.908(3) . ?
Mo2 O2 1.908(3) 10_556 ?
Mo2 O5 2.044(3) . ?
Mo2 O4 2.137(2) 10_556 ?
Mo2 O4 2.137(2) . ?
Mo2 N2 2.231(4) . ?
Mo4 O6 1.867(3) . ?
Mo4 O3 2.181(3) . ?
Mo4 O7 1.696(3) . ?
Mo4 O9 1.788(3) . ?
Mo4 O10 1.935(2) . ?
Mo4 O8 2.285(2) . ?
Mo3 Mo3 2.5881(9) 10_556 ?
Mo3 O11 1.937(3) . ?
Mo3 O11 1.937(3) 11_455 ?
Mo3 O9 2.129(3) 11_455 ?
Mo3 O9 2.129(3) . ?
Mo3 O12 1.683(4) . ?
Mo3 O8 2.234(3) . ?
Ge1 O3 1.743(3) . ?
Ge1 O3 1.743(3) 11_455 ?
Ge1 O13 1.749(4) . ?
Ge1 O4 1.788(3) . ?
O8 H8 0.8600(7) . ?
O1W H1WA 0.8500(10) . ?
O1W H1WA 0.8500(10) 10_556 ?
O1W H1WB 0.8500(10) 10_556 ?
O1W H1WB 0.8500(10) . ?
N2 C6 1.331(5) . ?
N2 C6 1.331(5) 10_556 ?
C6 H6 0.9300 . ?
C6 C7 1.386(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.373(7) . ?
C8 H8A 0.9300 . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C14 1.447(8) . ?
N4 C14 1.447(8) 10_556 ?
C14 H14B 0.9598 . ?
C14 H14C 0.9601 . ?
C14 H14D 0.9599 . ?
N1 C1 1.318(10) . ?
N1 C5 1.324(10) . ?
C1 H1 0.9300 . ?
C1 C2 1.372(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.358(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.350(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.368(10) . ?
C5 H5 0.9300 . ?
N6A C16A 1.325(10) . ?
N6A C12A 1.310(11) . ?
C16A H16A 0.9300 . ?
C16A C15A 1.354(10) . ?
C15A H15A 0.9300 . ?
C15A C14A 1.345(12) . ?
C14A H14A 0.9300 . ?
C14A C13A 1.367(12) . ?
C13A H13A 0.9300 . ?
C13A C12A 1.369(12) . ?
C12A H12A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C9 1.3900 . ?
N3 C13 1.3900 . ?
C9 H9 0.9300 . ?
C9 C10 1.3900 . ?
C10 H10 0.9300 . ?
C10 C11 1.3900 . ?
C11 H11 0.9300 . ?
C11 C12 1.3900 . ?
C12 H12 0.9300 . ?
C12 C13 1.3900 . ?
C13 H13 0.9300 . ?

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
Mo1 Mo1 Mo2 60.045(10) 10_556 . ?
O1 Mo1 Mo1 49.74(8) . 10_556 ?
O1 Mo1 Mo2 96.33(10) . . ?
O1 Mo1 O2 98.71(15) . 10_556 ?
O1 Mo1 O5 100.53(10) . . ?
O1 Mo1 O6 98.54(15) . 10_556 ?
O1 Mo1 O3 170.14(12) . 10_556 ?
O1 Mo1 N1 91.2(4) . . ?
O1 Mo1 N6A 80.2(4) . . ?
O2 Mo1 Mo1 96.08(8) 10_556 10_556 ?
O2 Mo1 Mo2 49.00(8) 10_556 . ?
O2 Mo1 O5 100.39(12) 10_556 . ?
O2 Mo1 O6 158.40(12) 10_556 10_556 ?
O2 Mo1 O3 88.31(11) 10_556 10_556 ?
O2 Mo1 N1 83.4(3) 10_556 . ?
O2 Mo1 N6A 84.7(3) 10_556 . ?
O5 Mo1 Mo1 51.94(6) . 10_556 ?
O5 Mo1 Mo2 52.50(9) . . ?
O5 Mo1 O3 84.89(9) . 10_556 ?
O5 Mo1 N1 166.9(4) . . ?
O5 Mo1 N6A 174.7(4) . . ?
O6 Mo1 Mo1 104.98(9) 10_556 10_556 ?
O6 Mo1 Mo2 140.83(8) 10_556 . ?
O6 Mo1 O5 89.12(12) 10_556 . ?
O6 Mo1 O3 73.15(11) 10_556 10_556 ?
O6 Mo1 N1 83.4(4) 10_556 . ?
O6 Mo1 N6A 85.5(4) 10_556 . ?
O3 Mo1 Mo1 136.73(7) 10_556 10_556 ?
O3 Mo1 Mo2 93.50(7) 10_556 . ?
O3 Mo1 N1 82.7(4) 10_556 . ?
O3 Mo1 N6A 93.6(4) 10_556 . ?
N1 Mo1 Mo1 140.6(4) . 10_556 ?
N1 Mo1 Mo2 132.4(3) . . ?
N6A Mo1 Mo2 132.8(3) . . ?
Mo1 Mo2 Mo1 59.91(2) . 10_556 ?
O2 Mo2 Mo1 49.97(8) . 10_556 ?
O2 Mo2 Mo1 49.97(8) 10_556 . ?
O2 Mo2 Mo1 96.70(9) . . ?
O2 Mo2 Mo1 96.71(9) 10_556 10_556 ?
O2 Mo2 O2 99.10(17) 10_556 . ?
O2 Mo2 O5 100.58(10) 10_556 . ?
O2 Mo2 O5 100.58(10) . . ?
O2 Mo2 O4 166.72(11) 10_556 . ?
O2 Mo2 O4 91.17(11) 10_556 10_556 ?
O2 Mo2 O4 91.17(11) . . ?
O2 Mo2 O4 166.72(11) . 10_556 ?
O2 Mo2 N2 83.93(11) . . ?
O2 Mo2 N2 83.93(11) 10_556 . ?
O5 Mo2 Mo1 51.73(7) . 10_556 ?
O5 Mo2 Mo1 51.73(7) . . ?
O5 Mo2 O4 85.65(11) . 10_556 ?
O5 Mo2 O4 85.65(11) . . ?
O5 Mo2 N2 172.94(14) . . ?
O4 Mo2 Mo1 96.35(8) 10_556 . ?
O4 Mo2 Mo1 96.35(8) . 10_556 ?
O4 Mo2 Mo1 137.38(9) . . ?
O4 Mo2 Mo1 137.37(9) 10_556 10_556 ?
O4 Mo2 O4 77.52(13) 10_556 . ?
O4 Mo2 N2 88.85(12) 10_556 . ?
O4 Mo2 N2 88.84(12) . . ?
N2 Mo2 Mo1 133.57(8) . . ?
N2 Mo2 Mo1 133.57(8) . 10_556 ?
O6 Mo4 O3 74.78(11) . . ?
O6 Mo4 O10 150.15(13) . . ?
O6 Mo4 O8 87.25(11) . . ?
O3 Mo4 O8 81.38(11) . . ?
O7 Mo4 O6 102.14(18) . . ?
O7 Mo4 O3 99.33(13) . . ?
O7 Mo4 O9 104.02(14) . . ?
O7 Mo4 O10 97.08(18) . . ?
O7 Mo4 O8 170.47(17) . . ?
O9 Mo4 O6 98.24(13) . . ?
O9 Mo4 O3 156.57(11) . . ?
O9 Mo4 O10 98.99(15) . . ?
O9 Mo4 O8 75.91(12) . . ?
O10 Mo4 O3 79.76(14) . . ?
O10 Mo4 O8 73.63(11) . . ?
O11 Mo3 Mo3 48.09(7) 11_455 10_556 ?
O11 Mo3 Mo3 48.09(7) . 10_556 ?
O11 Mo3 O11 94.12(15) . 11_455 ?
O11 Mo3 O9 87.64(11) . 11_455 ?
O11 Mo3 O9 87.64(11) 11_455 . ?
O11 Mo3 O9 157.96(13) 11_455 11_455 ?
O11 Mo3 O9 157.97(13) . . ?
O11 Mo3 O8 87.12(12) 11_455 . ?
O11 Mo3 O8 87.12(12) . . ?
O9 Mo3 Mo3 135.32(8) . 10_556 ?
O9 Mo3 Mo3 135.32(8) 11_455 10_556 ?
O9 Mo3 O9 82.80(17) 11_455 . ?
O9 Mo3 O8 71.02(9) . . ?
O9 Mo3 O8 71.02(9) 11_455 . ?
O12 Mo3 Mo3 102.95(15) . 10_556 ?
O12 Mo3 O11 106.28(15) . 11_455 ?
O12 Mo3 O11 106.28(15) . . ?
O12 Mo3 O9 94.22(13) . 11_455 ?
O12 Mo3 O9 94.22(13) . . ?
O12 Mo3 O8 159.93(17) . . ?
O8 Mo3 Mo3 97.11(9) . 10_556 ?
O3 Ge1 O3 116.32(17) 11_455 . ?
O3 Ge1 O13 107.29(11) 11_455 . ?
O3 Ge1 O13 107.28(11) . . ?
O3 Ge1 O4 108.54(10) 11_455 . ?
O3 Ge1 O4 108.54(10) . . ?
O13 Ge1 O4 108.66(18) . . ?
Mo1 O1 Mo1 80.51(15) . 10_556 ?
Mo3 O11 Mo3 83.82(15) . 10_556 ?
Mo2 O2 Mo1 81.03(10) . 10_556 ?
Mo1 O5 Mo1 76.12(12) . 10_556 ?
Mo1 O5 Mo2 75.77(10) 10_556 . ?
Mo1 O5 Mo2 75.77(10) . . ?
Mo4 O6 Mo1 114.87(14) . 10_556 ?
Mo1 O3 Mo4 97.18(11) 10_556 . ?
Ge1 O3 Mo1 122.23(13) . 10_556 ?
Ge1 O3 Mo4 126.08(15) . . ?
Mo4 O9 Mo3 117.30(13) . . ?
Mo4 O10 Mo4 117.45(19) . 11_455 ?
Mo4 O8 Mo4 92.71(12) . 11_455 ?
Mo4 O8 H8 113.46(16) . . ?
Mo4 O8 H8 113.46(16) 11_455 . ?
Mo3 O8 Mo4 95.65(10) . . ?
Mo3 O8 Mo4 95.64(10) . 11_455 ?
Mo3 O8 H8 136.6(4) . . ?
H1WA O1W H1WA 109.0(2) . 10_556 ?
H1WA O1W H1WB 104.48(17) 10_556 10_556 ?
H1WA O1W H1WB 104.48(17) . . ?
H1WA O1W H1WB 27.1(2) . 10_556 ?
H1WB O1W H1WA 27.1(2) . 10_556 ?
H1WB O1W H1WB 88.88(14) . 10_556 ?
Mo2 O4 Mo2 102.35(13) . 11_455 ?
Ge1 O4 Mo2 119.33(10) . . ?
Ge1 O4 Mo2 119.33(10) . 11_455 ?
C6 N2 Mo2 121.0(3) 10_556 . ?
C6 N2 Mo2 121.0(3) . . ?
C6 N2 C6 117.9(5) 10_556 . ?
N2 C6 H6 118.6 . . ?
N2 C6 C7 122.7(5) . . ?
C7 C6 H6 118.6 . . ?
C6 C7 H7 120.5 . . ?
C8 C7 C6 118.9(5) . . ?
C8 C7 H7 120.5 . . ?
C7 C8 C7 118.7(7) . 10_556 ?
C7 C8 H8A 120.6 . . ?
C7 C8 H8A 120.6 10_556 . ?
H4A N4 H4B 107.3 . . ?
C14 N4 H4A 108.0 10_556 . ?
C14 N4 H4A 108.0 . . ?
C14 N4 H4B 108.0 . . ?
C14 N4 H4B 108.0 10_556 . ?
C14 N4 C14 117.1(8) 10_556 . ?
N4 C14 H14B 109.4 . . ?
N4 C14 H14C 109.6 . . ?
N4 C14 H14D 109.4 . . ?
H14B C14 H14C 109.5 . . ?
H14B C14 H14D 109.5 . . ?
H14C C14 H14D 109.5 . . ?
C1 N1 Mo1 124.0(7) . . ?
C1 N1 C5 114.8(8) . . ?
C5 N1 Mo1 121.1(7) . . ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.6(10) . . ?
C2 C1 H1 118.7 . . ?
C1 C2 H2 119.8 . . ?
C3 C2 C1 120.4(10) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.6(10) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 121.7 . . ?
C3 C4 C5 116.6(10) . . ?
C5 C4 H4 121.7 . . ?
N1 C5 C4 126.6(10) . . ?
N1 C5 H5 116.7 . . ?
C4 C5 H5 116.7 . . ?
C16A N6A Mo1 119.3(7) . . ?
C12A N6A Mo1 122.7(7) . . ?
C12A N6A C16A 117.9(8) . . ?
N6A C16A H16A 118.4 . . ?
N6A C16A C15A 123.2(10) . . ?
C15A C16A H16A 118.4 . . ?
C16A C15A H15A 120.5 . . ?
C14A C15A C16A 119.0(10) . . ?
C14A C15A H15A 120.5 . . ?
C15A C14A H14A 120.8 . . ?
C15A C14A C13A 118.4(11) . . ?
C13A C14A H14A 120.8 . . ?
C14A C13A H13A 120.3 . . ?
C14A C13A C12A 119.5(12) . . ?
C12A C13A H13A 120.3 . . ?
N6A C12A C13A 121.7(11) . . ?
N6A C12A H12A 119.1 . . ?
C13A C12A H12A 119.1 . . ?
C9 N3 H3A 120.0 . . ?
C9 N3 C13 120.0 . . ?
C13 N3 H3A 120.0 . . ?
N3 C9 H9 120.0 . . ?
C10 C9 N3 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C13 C12 H12 120.0 . . ?
N3 C13 H13 120.0 . . ?
C12 C13 N3 120.0 . . ?
C12 C13 H13 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 N1 C1 C2 -175.3(10) . . . . ?
Mo1 N1 C5 C4 171.6(13) . . . . ?
Mo1 N6A C16A C15A -175.3(13) . . . . ?
Mo1 N6A C12A C13A 176.9(16) . . . . ?
Mo2 N2 C6 C7 176.7(5) . . . . ?
O6 Mo4 O9 Mo3 81.94(17) . . . . ?
O3 Mo4 O6 Mo1 -1.35(12) . . . 10_556 ?
O3 Mo4 O9 Mo3 11.4(4) . . . . ?
O3 Ge1 O3 Mo1 -120.84(14) 11_455 . . 10_556 ?
O3 Ge1 O3 Mo4 9.1(3) 11_455 . . . ?
O3 Ge1 O4 Mo2 -126.97(14) . . . 11_455 ?
O3 Ge1 O4 Mo2 0.31(19) 11_455 . . 11_455 ?
O3 Ge1 O4 Mo2 -0.31(19) . . . . ?
O3 Ge1 O4 Mo2 126.97(14) 11_455 . . . ?
O7 Mo4 O6 Mo1 95.16(17) . . . 10_556 ?
O7 Mo4 O9 Mo3 -173.3(2) . . . . ?
O9 Mo4 O6 Mo1 -158.48(15) . . . 10_556 ?
O10 Mo4 O6 Mo1 -33.7(3) . . . 10_556 ?
O10 Mo4 O9 Mo3 -73.60(18) . . . . ?
O8 Mo4 O6 Mo1 -83.16(15) . . . 10_556 ?
O8 Mo4 O9 Mo3 -3.10(13) . . . . ?
O13 Ge1 O3 Mo1 119.08(19) . . . 10_556 ?
O13 Ge1 O3 Mo4 -111.0(2) . . . . ?
O13 Ge1 O4 Mo2 -116.67(14) . . . . ?
O13 Ge1 O4 Mo2 116.67(14) . . . 11_455 ?
O4 Ge1 O3 Mo1 1.84(19) . . . 10_556 ?
O4 Ge1 O3 Mo4 131.79(16) . . . . ?
N2 C6 C7 C8 0.0(10) . . . . ?
C6 N2 C6 C7 1.5(10) 10_556 . . . ?
C6 C7 C8 C7 -1.4(13) . . . 10_556 ?
N1 C1 C2 C3 1.5(16) . . . . ?
C1 N1 C5 C4 -6(2) . . . . ?
C1 C2 C3 C4 -2(2) . . . . ?
C2 C3 C4 C5 -1(2) . . . . ?
C3 C4 C5 N1 6(2) . . . . ?
C5 N1 C1 C2 2.7(15) . . . . ?
N6A C16A C15A C14A -2(2) . . . . ?
C16A N6A C12A C13A -4(3) . . . . ?
C16A C15A C14A C13A -3(3) . . . . ?
C15A C14A C13A C12A 4(3) . . . . ?
C14A C13A C12A N6A -1(3) . . . . ?
C12A N6A C16A C15A 6(2) . . . . ?
N3 C9 C10 C11 0.0 . . . . ?
C9 N3 C13 C12 0.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 N3 0.0 . . . . ?
C13 N3 C9 C10 0.0 . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.507 504.1 164.2 '4 H2O'
2 0.500 0.000 -0.433 504.1 164.2 '4 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_sbmo2_0m
_database_code_depnum_ccdc_archive 'CCDC 2245819'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/d3qi01828h 2023
loop_
_audit_author_name
_audit_author_address
'zi jie'
;Chinese academy of science
China
;
_audit_update_record             
;
2023-07-07 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_audit_creation_date             2023-06-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H37 Mo12 N7 O34 Sb2 Zn'
_chemical_formula_sum            'C35 H37 Mo12 N7 O34 Sb2 Zn'
_chemical_formula_weight         2559.86
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

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

_cell_length_a                   17.2850(8)
_cell_length_b                   14.7526(7)
_cell_length_c                   25.0511(12)
_cell_angle_alpha                90
_cell_angle_beta                 95.010(2)
_cell_angle_gamma                90
_cell_volume                     6363.6(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9003
_cell_measurement_temperature    210.98
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.37
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.568
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.672
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4816
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28917
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.714
_diffrn_reflns_theta_min         2.373
_diffrn_ambient_temperature      210.98
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5346
_reflns_number_total             6023
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6023
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0373
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0427P)²+64.8386P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1019
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 N4-C16 = C16-C17 = C17-C18 = C18-C19 = C19-C20 = C20-N4
 1.36 with sigma of 0.01
 N4-C17 = C17-C19 = C19-N4
 2.37 with sigma of 0.01
 N1-C15 = C14-C15
 1.36 with sigma of 0.01
 C15-C13 = C15-C11
 2.37 with sigma of 0.01
 O8-H8A
 0.9 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: Zn1(0.5) N4(0.5) C17(0.5) H17(0.5) C16(0.5) H16(0.5) C19(0.5)
 H19(0.5) C20(0.5) H20(0.5) C18(0.5) H18(0.5)
5.a Riding coordinates:
 O8(H8A)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C16(H16),
  C19(H19), C20(H20), C18(H18)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.32765(2) 0.58842(3) 0.78119(2) 0.02441(11) Uani 1 1 d . . . . .
C1 C 0.2045(4) 0.5966(5) 0.6127(3) 0.0434(18) Uani 1 1 d . . . . .
H1 H 0.218755 0.548374 0.636016 0.052 Uiso 1 1 calc R U . . .
O3 O 0.3753(2) 0.6684(3) 0.83792(17) 0.0281(9) Uani 1 1 d . . . . .
N3 N 0.2572(3) 0.6589(4) 0.6038(2) 0.0313(12) Uani 1 1 d . . . . .
Zn1 Zn 0.55519(11) 0.86984(13) 0.86432(9) 0.0524(5) Uani 0.5 1 d . . P . .
Mo2 Mo 0.46668(3) 0.54082(3) 0.68618(2) 0.01996(12) Uani 1 1 d . . . . .
Mo6 Mo 0.37544(3) 0.65959(3) 0.64748(2) 0.02269(13) Uani 1 1 d . . . . .
C2 C 0.1296(5) 0.6001(7) 0.5890(4) 0.061(3) Uani 1 1 d . . . . .
H2 H 0.092983 0.556235 0.597129 0.074 Uiso 1 1 calc R U . . .
O17 O 0.3192(2) 0.6723(3) 0.71951(17) 0.0243(9) Uani 1 1 d . . . . .
N2 N 0.4628(3) 0.3905(4) 0.6859(2) 0.0272(11) Uani 1 1 d . . . . .
Mo1 Mo 0.51162(3) 0.65475(4) 0.62169(2) 0.02571(13) Uani 1 1 d . . . . .
C3 C 0.1090(5) 0.6685(7) 0.5531(4) 0.061(2) Uani 1 1 d . . . . .
H3 H 0.059318 0.669850 0.534548 0.073 Uiso 1 1 calc R U . . .
O4 O 0.4285(2) 0.5357(3) 0.76339(15) 0.0214(8) Uani 1 1 d . . . . .
N1 N 0.5656(4) 0.6364(4) 0.5437(2) 0.0431(15) Uani 1 1 d D . . . .
Mo4 Mo 0.63978(3) 0.81150(4) 0.65269(2) 0.03237(15) Uani 1 1 d . . . . .
N4 N 0.5999(9) 0.9667(9) 0.9149(6) 0.084(7) Uani 0.5 1 d D U P . .
C4 C 0.1621(5) 0.7343(6) 0.5452(4) 0.057(2) Uani 1 1 d . . . . .
H4 H 0.148441 0.783529 0.522534 0.069 Uiso 1 1 calc R U . . .
O5 O 0.4745(2) 0.6782(3) 0.69529(16) 0.0221(8) Uani 1 1 d . . . . .
Mo5 Mo 0.70300(3) 0.81219(4) 0.78135(2) 0.02969(14) Uani 1 1 d . . . . .
C5 C 0.2359(4) 0.7285(5) 0.5706(3) 0.0463(19) Uani 1 1 d . . . . .
H5 H 0.272306 0.773890 0.564651 0.056 Uiso 1 1 calc R U . . .
O1 O 0.4140(3) 0.6636(3) 0.57772(18) 0.0335(10) Uani 1 1 d . . . . .
Mo3 Mo 0.57103(3) 0.96441(4) 0.73595(3) 0.03756(17) Uani 1 1 d . . . . .
C6 C 0.5283(4) 0.3430(4) 0.6787(3) 0.0320(14) Uani 1 1 d . . . . .
H6 H 0.575055 0.374844 0.676592 0.038 Uiso 1 1 calc R U . . .
O13 O 0.5226(2) 0.5248(3) 0.62426(17) 0.0289(9) Uani 1 1 d . . . . .
O2 O 0.3626(2) 0.5297(3) 0.65304(16) 0.0254(9) Uani 1 1 d . . . . .
O6 O 0.5393(3) 0.7883(3) 0.61833(19) 0.0372(11) Uani 1 1 d . . . . .
C7 C 0.5292(4) 0.2508(5) 0.6745(3) 0.0382(16) Uani 1 1 d . . . . .
H7 H 0.575868 0.220278 0.669907 0.046 Uiso 1 1 calc R U . . .
O7 O 0.6949(3) 0.8110(4) 0.5998(2) 0.0500(14) Uani 1 1 d . . . . .
C8 C 0.4614(4) 0.2027(5) 0.6771(3) 0.0417(17) Uani 1 1 d . . . . .
H8 H 0.460661 0.139232 0.673929 0.050 Uiso 1 1 calc R U . . .
O10 O 0.7239(2) 0.7898(3) 0.70800(19) 0.0331(10) Uani 1 1 d . . . . .
C9 C 0.3944(4) 0.2505(5) 0.6844(3) 0.0406(17) Uani 1 1 d . . . . .
H9 H 0.346891 0.219927 0.685810 0.049 Uiso 1 1 calc R U . . .
O9 O 0.6250(3) 0.9289(3) 0.6661(2) 0.0404(12) Uani 1 1 d . . . . .
C10 C 0.3977(4) 0.3435(4) 0.6895(3) 0.0321(14) Uani 1 1 d . . . . .
H10 H 0.352101 0.375079 0.695732 0.039 Uiso 1 1 calc R U . . .
O8 O 0.5849(2) 0.8139(3) 0.73199(18) 0.0281(9) Uani 1 1 d D . . . .
H8A H 0.553759 0.768860 0.741481 0.034 Uiso 1 1 d DR U . . .
C11 C 0.5859(7) 0.5512(6) 0.5261(4) 0.082(3) Uani 1 1 d D . . . .
H11 H 0.578661 0.499909 0.547433 0.099 Uiso 1 1 calc R U . . .
O12 O 0.5926(3) 1.0743(3) 0.7317(3) 0.0537(15) Uani 1 1 d . . . . .
C12 C 0.6165(8) 0.5416(9) 0.4776(5) 0.094(4) Uani 1 1 d . . . . .
H12 H 0.627001 0.483224 0.465020 0.113 Uiso 1 1 calc R U . . .
C13 C 0.6314(6) 0.6135(8) 0.4481(4) 0.072(3) Uani 1 1 d D . . . .
H13 H 0.659824 0.607928 0.417936 0.086 Uiso 1 1 calc R U . . .
C14 C 0.6048(9) 0.6941(10) 0.4628(4) 0.111(5) Uani 1 1 d D . . . .
H14 H 0.608417 0.743831 0.439709 0.133 Uiso 1 1 calc R U . . .
O16 O 0.7949(3) 0.8133(3) 0.8102(2) 0.0407(12) Uani 1 1 d . . . . .
C15 C 0.5724(8) 0.7069(6) 0.5104(4) 0.101(5) Uani 1 1 d D U . . .
H15 H 0.554893 0.764696 0.519580 0.121 Uiso 1 1 calc R U . . .
O11 O 0.5287(3) 0.9472(3) 0.8054(2) 0.0416(12) Uani 1 1 d . . . . .
C17 C 0.7038(9) 1.0731(12) 0.9276(7) 0.068(5) Uani 0.5 1 d D . P . .
H17 H 0.747610 1.100956 0.914899 0.082 Uiso 0.5 1 calc R U P . .
O15 O 0.6460(2) 0.7929(3) 0.84297(19) 0.0315(10) Uani 1 1 d . . . . .
C16 C 0.6646(10) 1.0075(12) 0.8993(6) 0.071(6) Uani 0.5 1 d D . P . .
H16 H 0.683208 0.988819 0.866946 0.085 Uiso 0.5 1 calc R U P . .
C19 C 0.6107(14) 1.0618(15) 0.9911(7) 0.097(9) Uani 0.5 1 d D . P . .
H19 H 0.591778 1.080095 1.023466 0.116 Uiso 0.5 1 calc R U P . .
C20 C 0.5717(9) 0.9989(14) 0.9593(7) 0.092(9) Uani 0.5 1 d D U P . .
H20 H 0.523660 0.977328 0.968849 0.111 Uiso 0.5 1 calc R U P . .
O14 O 0.6796(3) 0.9304(3) 0.7744(2) 0.0387(11) Uani 1 1 d . . . . .
C18 C 0.6775(12) 1.0976(15) 0.9752(7) 0.093(8) Uani 0.5 1 d D . P . .
H18 H 0.705761 1.139744 0.997264 0.112 Uiso 0.5 1 calc R U 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
Sb1 O3 1.971(4) . ?
Sb1 O17 1.976(4) . ?
Sb1 O4 1.994(4) . ?
C1 H1 0.9400 . ?
C1 N3 1.326(9) . ?
C1 C2 1.377(10) . ?
O3 Mo1 2.130(4) 2_656 ?
O3 Mo4 2.142(4) 2_656 ?
N3 Mo6 2.233(5) . ?
N3 C5 1.352(9) . ?
Zn1 N4 2.018(12) . ?
Zn1 O6 2.104(5) 2_656 ?
Zn1 O11 1.890(6) . ?
Zn1 O15 2.045(5) . ?
Mo2 Mo6 2.4960(7) . ?
Mo2 N2 2.218(5) . ?
Mo2 Mo1 2.5015(7) . ?
Mo2 O4 2.099(4) . ?
Mo2 O4 2.118(4) 2_656 ?
Mo2 O5 2.042(4) . ?
Mo2 O13 1.913(4) . ?
Mo2 O2 1.922(4) . ?
Mo6 O17 2.131(4) . ?
Mo6 Mo1 2.4958(7) . ?
Mo6 O5 2.020(4) . ?
Mo6 O1 1.925(5) . ?
Mo6 O2 1.935(4) . ?
Mo6 O15 2.020(4) 2_656 ?
C2 H2 0.9400 . ?
C2 C3 1.377(12) . ?
O17 Mo5 2.098(4) 2_656 ?
N2 C6 1.358(8) . ?
N2 C10 1.332(8) . ?
Mo1 N1 2.253(6) . ?
Mo1 O5 2.034(4) . ?
Mo1 O1 1.938(4) . ?
Mo1 O13 1.927(4) . ?
Mo1 O6 2.031(5) . ?
C3 H3 0.9400 . ?
C3 C4 1.362(12) . ?
N1 C11 1.387(10) . ?
N1 C15 1.346(8) . ?
Mo4 O6 1.901(5) . ?
Mo4 O7 1.698(5) . ?
Mo4 O10 1.945(5) . ?
Mo4 O9 1.787(5) . ?
Mo4 O8 2.275(4) . ?
N4 C16 1.356(10) . ?
N4 C20 1.340(10) . ?
C4 H4 0.9400 . ?
C4 C5 1.377(10) . ?
Mo5 O10 1.932(5) . ?
Mo5 O8 2.292(4) . ?
Mo5 O16 1.686(5) . ?
Mo5 O15 1.924(5) . ?
Mo5 O14 1.796(5) . ?
C5 H5 0.9400 . ?
Mo3 Mo3 2.6130(11) 2_656 ?
Mo3 O9 2.119(5) . ?
Mo3 O8 2.236(4) . ?
Mo3 O12 1.668(5) . ?
Mo3 O11 1.948(5) 2_656 ?
Mo3 O11 1.963(5) . ?
Mo3 O14 2.095(5) . ?
C6 H6 0.9400 . ?
C6 C7 1.364(9) . ?
C7 H7 0.9400 . ?
C7 C8 1.376(10) . ?
C8 H8 0.9400 . ?
C8 C9 1.382(10) . ?
C9 H9 0.9400 . ?
C9 C10 1.379(10) . ?
C10 H10 0.9400 . ?
O8 H8A 0.9003 . ?
C11 H11 0.9400 . ?
C11 C12 1.375(14) . ?
C12 H12 0.9400 . ?
C12 C13 1.332(16) . ?
C13 H13 0.9400 . ?
C13 C14 1.338(15) . ?
C14 H14 0.9400 . ?
C14 C15 1.373(8) . ?
C15 H15 0.9400 . ?
C17 H17 0.9400 . ?
C17 C16 1.346(9) . ?
C17 C18 1.362(9) . ?
C16 H16 0.9400 . ?
C19 H19 0.9400 . ?
C19 C20 1.362(10) . ?
C19 C18 1.361(10) . ?
C20 H20 0.9400 . ?
C18 H18 0.9400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Sb1 O17 100.74(18) . . ?
O3 Sb1 O4 94.38(16) . . ?
O17 Sb1 O4 94.36(16) . . ?
N3 C1 H1 118.8 . . ?
N3 C1 C2 122.3(7) . . ?
C2 C1 H1 118.8 . . ?
Sb1 O3 Mo1 126.4(2) . 2_656 ?
Sb1 O3 Mo4 128.5(2) . 2_656 ?
Mo1 O3 Mo4 99.01(17) 2_656 2_656 ?
C1 N3 Mo6 122.2(5) . . ?
C1 N3 C5 118.4(6) . . ?
C5 N3 Mo6 119.1(5) . . ?
N4 Zn1 O6 122.5(6) . 2_656 ?
N4 Zn1 O15 107.3(5) . . ?
O11 Zn1 N4 96.6(5) . . ?
O11 Zn1 O6 111.5(2) . 2_656 ?
O11 Zn1 O15 105.7(2) . . ?
O15 Zn1 O6 111.3(2) . 2_656 ?
Mo6 Mo2 Mo1 59.92(2) . . ?
N2 Mo2 Mo6 133.05(13) . . ?
N2 Mo2 Mo1 132.90(13) . . ?
O4 Mo2 Mo6 98.30(11) . . ?
O4 Mo2 Mo6 137.35(11) 2_656 . ?
O4 Mo2 N2 87.40(17) . . ?
O4 Mo2 N2 89.42(17) 2_656 . ?
O4 Mo2 Mo1 96.41(11) 2_656 . ?
O4 Mo2 Mo1 139.45(11) . . ?
O4 Mo2 O4 76.74(16) . 2_656 ?
O5 Mo2 Mo6 51.70(11) . . ?
O5 Mo2 N2 173.59(17) . . ?
O5 Mo2 Mo1 52.00(11) . . ?
O5 Mo2 O4 85.65(15) . 2_656 ?
O5 Mo2 O4 87.48(15) . . ?
O13 Mo2 Mo6 96.83(13) . . ?
O13 Mo2 N2 83.76(19) . . ?
O13 Mo2 Mo1 49.60(13) . . ?
O13 Mo2 O4 90.71(16) . 2_656 ?
O13 Mo2 O4 164.73(17) . . ?
O13 Mo2 O5 100.38(17) . . ?
O13 Mo2 O2 99.19(18) . . ?
O2 Mo2 Mo6 49.91(13) . . ?
O2 Mo2 N2 83.49(18) . . ?
O2 Mo2 Mo1 96.32(13) . . ?
O2 Mo2 O4 92.12(16) . . ?
O2 Mo2 O4 167.09(16) . 2_656 ?
O2 Mo2 O5 100.55(17) . . ?
N3 Mo6 Mo2 135.02(14) . . ?
N3 Mo6 Mo1 135.77(15) . . ?
O17 Mo6 N3 87.12(18) . . ?
O17 Mo6 Mo2 93.02(11) . . ?
O17 Mo6 Mo1 137.05(11) . . ?
Mo1 Mo6 Mo2 60.15(2) . . ?
O5 Mo6 N3 169.50(19) . . ?
O5 Mo6 Mo2 52.49(11) . . ?
O5 Mo6 O17 84.95(15) . . ?
O5 Mo6 Mo1 52.25(11) . . ?
O1 Mo6 N3 86.0(2) . . ?
O1 Mo6 Mo2 96.72(13) . . ?
O1 Mo6 O17 170.26(17) . . ?
O1 Mo6 Mo1 49.97(13) . . ?
O1 Mo6 O5 101.04(17) . . ?
O1 Mo6 O2 98.42(19) . . ?
O1 Mo6 O15 99.16(19) . 2_656 ?
O2 Mo6 N3 85.68(19) . . ?
O2 Mo6 Mo2 49.44(12) . . ?
O2 Mo6 O17 87.87(17) . . ?
O2 Mo6 Mo1 96.15(12) . . ?
O2 Mo6 O5 100.86(16) . . ?
O2 Mo6 O15 158.82(18) . 2_656 ?
O15 Mo6 N3 83.88(19) 2_656 . ?
O15 Mo6 Mo2 138.92(13) 2_656 . ?
O15 Mo6 O17 73.27(17) 2_656 . ?
O15 Mo6 Mo1 104.19(13) 2_656 . ?
O15 Mo6 O5 87.26(17) 2_656 . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.3(8) . . ?
C3 C2 H2 120.4 . . ?
Sb1 O17 Mo6 126.8(2) . . ?
Sb1 O17 Mo5 128.7(2) . 2_656 ?
Mo5 O17 Mo6 100.05(17) 2_656 . ?
C6 N2 Mo2 119.5(4) . . ?
C10 N2 Mo2 123.1(4) . . ?
C10 N2 C6 117.4(6) . . ?
O3 Mo1 Mo2 94.62(12) 2_656 . ?
O3 Mo1 Mo6 136.15(12) 2_656 . ?
O3 Mo1 N1 89.5(2) 2_656 . ?
Mo6 Mo1 Mo2 59.930(19) . . ?
N1 Mo1 Mo2 130.87(17) . . ?
N1 Mo1 Mo6 134.38(16) . . ?
O5 Mo1 O3 84.40(16) . 2_656 ?
O5 Mo1 Mo2 52.29(11) . . ?
O5 Mo1 Mo6 51.76(11) . . ?
O5 Mo1 N1 173.4(2) . . ?
O1 Mo1 O3 168.83(18) . 2_656 ?
O1 Mo1 Mo2 96.21(14) . . ?
O1 Mo1 Mo6 49.52(13) . . ?
O1 Mo1 N1 85.5(2) . . ?
O1 Mo1 O5 100.12(17) . . ?
O1 Mo1 O6 96.19(19) . . ?
O13 Mo1 O3 89.68(18) . 2_656 ?
O13 Mo1 Mo2 49.11(13) . . ?
O13 Mo1 Mo6 96.46(13) . . ?
O13 Mo1 N1 82.1(2) . . ?
O13 Mo1 O5 100.18(17) . . ?
O13 Mo1 O1 99.47(19) . . ?
O13 Mo1 O6 160.65(18) . . ?
O6 Mo1 O3 73.63(17) . 2_656 ?
O6 Mo1 Mo2 140.01(14) . . ?
O6 Mo1 Mo6 102.35(14) . . ?
O6 Mo1 N1 87.9(2) . . ?
O6 Mo1 O5 88.10(18) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 C2 118.5(7) . . ?
C4 C3 H3 120.8 . . ?
Sb1 O4 Mo2 124.86(19) . 2_656 ?
Sb1 O4 Mo2 122.91(19) . . ?
Mo2 O4 Mo2 103.10(16) . 2_656 ?
C11 N1 Mo1 121.3(5) . . ?
C15 N1 Mo1 120.6(5) . . ?
C15 N1 C11 117.7(7) . . ?
O3 Mo4 O8 81.69(16) 2_656 . ?
O6 Mo4 O3 75.94(18) . 2_656 ?
O6 Mo4 O10 152.78(19) . . ?
O6 Mo4 O8 87.95(18) . . ?
O7 Mo4 O3 99.4(2) . 2_656 ?
O7 Mo4 O6 101.5(3) . . ?
O7 Mo4 O10 96.9(2) . . ?
O7 Mo4 O9 104.5(3) . . ?
O7 Mo4 O8 170.5(2) . . ?
O10 Mo4 O3 81.38(18) . 2_656 ?
O10 Mo4 O8 73.93(16) . . ?
O9 Mo4 O3 156.02(19) . 2_656 ?
O9 Mo4 O6 96.9(2) . . ?
O9 Mo4 O10 97.8(2) . . ?
O9 Mo4 O8 75.13(19) . . ?
C16 N4 Zn1 114.5(11) . . ?
C20 N4 Zn1 128.7(13) . . ?
C20 N4 C16 116.7(10) . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(8) . . ?
C5 C4 H4 120.1 . . ?
Mo6 O5 Mo2 75.81(14) . . ?
Mo6 O5 Mo1 75.99(14) . . ?
Mo1 O5 Mo2 75.71(14) . . ?
O17 Mo5 O8 81.49(15) 2_656 . ?
O10 Mo5 O17 82.60(18) . 2_656 ?
O10 Mo5 O8 73.75(16) . . ?
O16 Mo5 O17 100.3(2) . 2_656 ?
O16 Mo5 O10 99.4(2) . . ?
O16 Mo5 O8 172.7(2) . . ?
O16 Mo5 O15 100.8(2) . . ?
O16 Mo5 O14 103.1(2) . . ?
O15 Mo5 O17 75.94(17) . 2_656 ?
O15 Mo5 O10 152.78(18) . . ?
O15 Mo5 O8 86.55(17) . . ?
O14 Mo5 O17 156.19(18) . 2_656 ?
O14 Mo5 O10 97.7(2) . . ?
O14 Mo5 O8 75.81(18) . . ?
O14 Mo5 O15 95.4(2) . . ?
N3 C5 C4 121.5(7) . . ?
N3 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
Mo6 O1 Mo1 80.51(17) . . ?
O9 Mo3 Mo3 135.60(14) . 2_656 ?
O9 Mo3 O8 70.21(16) . . ?
O8 Mo3 Mo3 96.83(10) . 2_656 ?
O12 Mo3 Mo3 103.75(19) . 2_656 ?
O12 Mo3 O9 94.0(3) . . ?
O12 Mo3 O8 159.4(2) . . ?
O12 Mo3 O11 106.6(3) . . ?
O12 Mo3 O11 106.5(2) . 2_656 ?
O12 Mo3 O14 93.8(2) . . ?
O11 Mo3 Mo3 48.33(16) 2_656 2_656 ?
O11 Mo3 Mo3 47.85(14) . 2_656 ?
O11 Mo3 O9 157.73(19) . . ?
O11 Mo3 O9 87.8(2) 2_656 . ?
O11 Mo3 O8 87.75(19) . . ?
O11 Mo3 O8 86.58(19) 2_656 . ?
O11 Mo3 O11 94.2(2) 2_656 . ?
O11 Mo3 O14 158.3(2) 2_656 . ?
O11 Mo3 O14 87.1(2) . . ?
O14 Mo3 Mo3 134.54(15) . 2_656 ?
O14 Mo3 O9 83.1(2) . . ?
O14 Mo3 O8 71.79(16) . . ?
N2 C6 H6 118.7 . . ?
N2 C6 C7 122.7(6) . . ?
C7 C6 H6 118.7 . . ?
Mo2 O13 Mo1 81.29(16) . . ?
Mo2 O2 Mo6 80.65(16) . . ?
Mo1 O6 Zn1 110.9(2) . 2_656 ?
Mo4 O6 Zn1 119.9(3) . 2_656 ?
Mo4 O6 Mo1 111.4(2) . . ?
C6 C7 H7 120.2 . . ?
C6 C7 C8 119.7(6) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 121.0 . . ?
C7 C8 C9 118.0(7) . . ?
C9 C8 H8 121.0 . . ?
Mo5 O10 Mo4 117.4(2) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.4(7) . . ?
C10 C9 H9 120.3 . . ?
Mo4 O9 Mo3 118.4(2) . . ?
N2 C10 C9 122.7(6) . . ?
N2 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
Mo4 O8 Mo5 92.95(14) . . ?
Mo4 O8 H8A 121.6 . . ?
Mo5 O8 H8A 112.0 . . ?
Mo3 O8 Mo4 96.24(16) . . ?
Mo3 O8 Mo5 94.64(16) . . ?
Mo3 O8 H8A 130.7 . . ?
N1 C11 H11 119.9 . . ?
C12 C11 N1 120.1(9) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.1(11) . . ?
C13 C12 H12 119.4 . . ?
C12 C13 H13 121.1 . . ?
C12 C13 C14 117.9(9) . . ?
C14 C13 H13 121.1 . . ?
C13 C14 H14 118.7 . . ?
C13 C14 C15 122.5(11) . . ?
C15 C14 H14 118.7 . . ?
N1 C15 C14 119.8(9) . . ?
N1 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
Zn1 O11 Mo3 133.3(3) . . ?
Zn1 O11 Mo3 129.6(3) . 2_656 ?
Mo3 O11 Mo3 83.8(2) 2_656 . ?
C16 C17 H17 121.3 . . ?
C16 C17 C18 117.3(10) . . ?
C18 C17 H17 121.3 . . ?
Mo6 O15 Zn1 110.9(2) 2_656 . ?
Mo5 O15 Zn1 125.9(2) . . ?
Mo5 O15 Mo6 110.5(2) . 2_656 ?
N4 C16 H16 118.0 . . ?
C17 C16 N4 123.9(11) . . ?
C17 C16 H16 118.0 . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C18 C19 C20 118.8(10) . . ?
N4 C20 C19 122.0(11) . . ?
N4 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
Mo5 O14 Mo3 117.5(2) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.7(11) . . ?
C19 C18 H18 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N3 C5 C4 -1.6(12) . . . . ?
C1 C2 C3 C4 -4.5(16) . . . . ?
O3 Mo4 O9 Mo3 13.4(7) 2_656 . . . ?
N3 C1 C2 C3 2.5(15) . . . . ?
Zn1 N4 C16 C17 -179.3(17) . . . . ?
Zn1 N4 C20 C19 176.6(17) . . . . ?
Mo2 N2 C6 C7 -175.5(6) . . . . ?
Mo2 N2 C10 C9 173.9(6) . . . . ?
Mo6 N3 C5 C4 -175.9(7) . . . . ?
C2 C1 N3 Mo6 174.7(7) . . . . ?
C2 C1 N3 C5 0.6(12) . . . . ?
C2 C3 C4 C5 3.6(16) . . . . ?
O17 Mo5 O14 Mo3 -13.8(7) 2_656 . . . ?
N2 C6 C7 C8 0.6(12) . . . . ?
Mo1 N1 C11 C12 177.9(9) . . . . ?
Mo1 N1 C15 C14 -179.4(11) . . . . ?
C3 C4 C5 N3 -0.5(15) . . . . ?
N1 C11 C12 C13 4(2) . . . . ?
N4 Zn1 O11 Mo3 -125.1(6) . . . 2_656 ?
N4 Zn1 O11 Mo3 108.9(6) . . . . ?
C6 N2 C10 C9 -2.2(10) . . . . ?
C6 C7 C8 C9 -0.6(12) . . . . ?
O6 Zn1 O11 Mo3 -122.3(3) 2_656 . . . ?
O6 Zn1 O11 Mo3 3.7(4) 2_656 . . 2_656 ?
O6 Mo4 O9 Mo3 84.1(3) . . . . ?
C7 C8 C9 C10 -0.8(12) . . . . ?
O7 Mo4 O9 Mo3 -172.1(3) . . . . ?
C8 C9 C10 N2 2.3(12) . . . . ?
O10 Mo4 O9 Mo3 -72.9(3) . . . . ?
O10 Mo5 O14 Mo3 75.2(3) . . . . ?
C10 N2 C6 C7 0.8(10) . . . . ?
O8 Mo4 O9 Mo3 -1.9(2) . . . . ?
O8 Mo5 O14 Mo3 4.2(2) . . . . ?
C11 N1 C15 C14 -5.6(18) . . . . ?
C11 C12 C13 C14 -10(2) . . . . ?
C12 C13 C14 C15 9(2) . . . . ?
C13 C14 C15 N1 -1(2) . . . . ?
O16 Mo5 O14 Mo3 176.8(3) . . . . ?
C15 N1 C11 C12 4.2(17) . . . . ?
O15 Zn1 O11 Mo3 -1.2(4) . . . . ?
O15 Zn1 O11 Mo3 124.8(3) . . . 2_656 ?
O15 Mo5 O14 Mo3 -80.8(3) . . . . ?
C16 N4 C20 C19 -8(3) . . . . ?
C16 C17 C18 C19 -5(4) . . . . ?
C20 N4 C16 C17 4(3) . . . . ?
C20 C19 C18 C17 2(4) . . . . ?
C18 C17 C16 N4 2(3) . . . . ?
C18 C19 C20 N4 5(4) . . . . ?

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

data_mo_202106068_0m
_database_code_depnum_ccdc_archive 'CCDC 2246017'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/d3qi01828h 2023
loop_
_audit_author_name
_audit_author_address
'zi jie'
;Chinese academy of science
China
;
_audit_update_record             
;
2023-07-07 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_audit_creation_date             2023-06-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C30 H32 Mo12 N6 O34 Sb2, C10 H2 N2, 2(C2 H8 N), 2(H O0.25), 4[H2O]'
_chemical_formula_sum            'C44 H61 Mo12 N10 O35.50 Sb2'
_chemical_formula_weight         2692.80
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, -z'
'-x, y, -z+1/2'
'-x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, z'
'x, -y, z-1/2'
'x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z-1/2'
'x+1/2, y+1/2, -z-1/2'

_cell_length_a                   19.5638(9)
_cell_length_b                   26.0006(13)
_cell_length_c                   16.2089(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8245.0(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      30.84
_cell_measurement_theta_min      2.57
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.481
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.169
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5140
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32381
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.047
_diffrn_reflns_theta_min         2.831
_diffrn_ambient_temperature      299.03
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5182
_reflns_number_total             6932
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.190
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         6932
_refine_ls_number_restraints     128
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0413
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0467P)²+45.3115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1108
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N3-C9 = C9-C10 = C10-C11 = C11-C12 = C12-C13 = C13-N3
 1.36 with sigma of 0.02
 O1W-H1WB
 0.87 with sigma of 0.001
 O1W-H1WA
 0.87 with sigma of 0.001
 N3-C10 = C10-C12 = C12-N3
 2.37 with sigma of 0.02
 H1WA-H1WB
 1.35 with sigma of 0.01
 O8-H8
 0.77 with sigma of 0.001
3. Rigid bond restraints
 C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 N3, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C3, C2, C1, N1, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: N3(0.5) C9(0.5) H9(0.5) C10(0.5) H10(0.5) C11(0.5) H11(0.5)
 C12(0.5) H12(0.5) C13(0.5) H13(0.5) O1W(0.375) H1WA(0.375) H1WB(0.375)
 Fixed X: H1WA(0.14553)
 Fixed Z: H1WA(0.76855)
7.a Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B)
7.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C1(H1), C2(H2), C3(H3),
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8A)
7.c Fitted hexagon refined as free rotating group:
 N3(C9,C10,C11,C12,C13)
7.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.500000 0.42458(2) 0.94379(2) 0.03147(10) Uani 1 2 d S T P . .
Mo1 Mo 0.34905(2) 0.38476(2) 0.67288(2) 0.03191(9) Uani 1 1 d . . . . .
Mo2 Mo 0.41512(2) 0.45196(2) 0.750000 0.02761(11) Uani 1 2 d S T P . .
Mo3 Mo 0.500000 0.21014(2) 0.66995(3) 0.03287(12) Uani 1 2 d S T P . .
Mo4 Mo 0.41545(2) 0.29680(2) 0.55576(2) 0.03399(10) Uani 1 1 d . . . . .
O1 O 0.2742(2) 0.38034(18) 0.750000 0.0417(11) Uani 1 2 d S T P . .
O2 O 0.35240(15) 0.45942(12) 0.6594(2) 0.0357(7) Uani 1 1 d . . . . .
O3 O 0.42246(15) 0.37901(12) 0.92455(19) 0.0339(6) Uani 1 1 d . . . . .
O5 O 0.4293(2) 0.37403(15) 0.750000 0.0300(8) Uani 1 2 d S T P . .
O4 O 0.500000 0.45546(15) 0.8319(2) 0.0283(8) Uani 1 2 d S T P . .
O6 O 0.35438(15) 0.31076(12) 0.6423(2) 0.0372(7) Uani 1 1 d . . . . .
O8 O 0.500000 0.29567(16) 0.6523(3) 0.0307(8) Uani 1 2 d DS T P . .
H8 H 0.500000 0.3183(11) 0.683(2) 0.04(2) Uiso 1 2 d DS . P . .
O7 O 0.3628(2) 0.29645(14) 0.4725(2) 0.0508(9) Uani 1 1 d . . . . .
O9 O 0.42864(17) 0.22956(12) 0.5764(2) 0.0380(7) Uani 1 1 d . . . . .
O10 O 0.500000 0.31091(17) 0.4970(3) 0.0384(10) Uani 1 2 d S T P . .
O11 O 0.5730(2) 0.21971(17) 0.750000 0.0374(10) Uani 1 2 d S T P . .
O12 O 0.500000 0.14681(19) 0.6464(4) 0.0495(12) Uani 1 2 d S T P . .
N1 N 0.2674(2) 0.38803(17) 0.5771(3) 0.0518(10) Uani 1 1 d . . . . .
N2 N 0.4127(3) 0.5379(2) 0.750000 0.0345(11) Uani 1 2 d S T P . .
N3 N 0.2162(6) 0.5177(8) 0.7518(18) 0.189(7) Uani 0.5 1 d DG . P A -1
C9 C 0.1913(9) 0.5672(6) 0.7643(19) 0.172(5) Uani 0.5 1 d DG U P A -1
H9 H 0.219635 0.592380 0.786333 0.206 Uiso 0.5 1 calc R U P A -1
C10 C 0.1241(10) 0.5789(6) 0.7438(17) 0.170(5) Uani 0.5 1 d DG U P A -1
H10 H 0.107472 0.612047 0.752219 0.204 Uiso 0.5 1 calc R U P A -1
C11 C 0.0817(7) 0.5413(8) 0.7109(12) 0.172(5) Uani 0.5 1 d DG U P A -1
H11 H 0.036788 0.549145 0.697202 0.206 Uiso 0.5 1 calc R U P A -1
C12 C 0.1066(10) 0.4918(7) 0.6984(10) 0.173(5) Uani 0.5 1 d DG U P A -1
H12 H 0.078266 0.466575 0.676300 0.208 Uiso 0.5 1 calc R U P A -1
C13 C 0.1738(10) 0.4800(6) 0.7188(14) 0.173(5) Uani 0.5 1 d DG U P A -1
H13 H 0.190430 0.446906 0.710413 0.208 Uiso 0.5 1 calc R U P A -1
N4 N 0.2861(4) 0.2346(3) 0.750000 0.0625(19) Uani 1 2 d S T P . .
H4A H 0.331526 0.236691 0.749999 0.075 Uiso 1 2 calc R U P . .
H4B H 0.269899 0.266530 0.749999 0.075 Uiso 1 2 calc R U P . .
C1 C 0.2223(4) 0.3509(3) 0.5727(6) 0.082(2) Uani 1 1 d . . . . .
H1 H 0.226187 0.323527 0.609268 0.098 Uiso 1 1 calc R U . . .
C2 C 0.1683(4) 0.3504(3) 0.5156(6) 0.093(2) Uani 1 1 d . . . . .
H2 H 0.137035 0.323468 0.515413 0.111 Uiso 1 1 calc R U . . .
C3 C 0.1626(5) 0.3875(4) 0.4636(6) 0.101(3) Uani 1 1 d . . . . .
H3 H 0.125866 0.388536 0.427280 0.121 Uiso 1 1 calc R U . . .
C4 C 0.2111(5) 0.4254(4) 0.4623(6) 0.0918(18) Uani 1 1 d . U . . .
H4 H 0.209947 0.451216 0.422633 0.110 Uiso 1 1 calc R U . . .
C5 C 0.2630(5) 0.4240(3) 0.5228(6) 0.105(3) Uani 1 1 d . U . . .
H5 H 0.295308 0.450262 0.523400 0.126 Uiso 1 1 calc R U . . .
C6 C 0.4098(4) 0.5650(2) 0.8202(4) 0.0580(15) Uani 1 1 d . . . . .
H6 H 0.410149 0.547381 0.870140 0.070 Uiso 1 1 calc R U . . .
C7 C 0.4062(4) 0.6179(3) 0.8211(5) 0.076(2) Uani 1 1 d . . . . .
H7 H 0.404973 0.635305 0.871255 0.091 Uiso 1 1 calc R U . . .
C8 C 0.4045(5) 0.6448(3) 0.750000 0.067(3) Uani 1 2 d S T P . .
H8A H 0.402176 0.680517 0.750000 0.081 Uiso 1 2 calc R U P . .
C14 C 0.2653(5) 0.2102(3) 0.6748(5) 0.090(3) Uani 1 1 d . . . . .
H14A H 0.286695 0.177109 0.670566 0.134 Uiso 1 1 calc R U . . .
H14B H 0.278812 0.231163 0.628786 0.134 Uiso 1 1 calc R U . . .
H14C H 0.216566 0.206170 0.674637 0.134 Uiso 1 1 calc R U . . .
O1W O 0.1384(8) 0.2867(6) 0.750000 0.175(7) Uani 0.75 2 d DS TU P . .
H1WA H 0.145530 0.3176(6) 0.768550 0.262 Uiso 0.375 1 d D U P . .
H1WB H 0.1795(11) 0.2739(9) 0.750000 0.262 Uiso 0.75 2 d DS U 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
Sb1 O3 1.950(3) 10_655 ?
Sb1 O3 1.950(3) . ?
Sb1 O4 1.983(4) . ?
Mo1 Mo1 2.5001(8) 12_557 ?
Mo1 Mo2 2.5073(6) . ?
Mo1 O1 1.928(3) . ?
Mo1 O2 1.955(3) . ?
Mo1 O3 2.140(3) 12_557 ?
Mo1 O5 2.026(3) . ?
Mo1 O6 1.990(3) . ?
Mo1 N1 2.229(5) . ?
Mo2 O2 1.923(3) . ?
Mo2 O2 1.923(3) 12_557 ?
Mo2 O5 2.045(4) . ?
Mo2 O4 2.128(2) 3_656 ?
Mo2 O4 2.128(2) . ?
Mo2 N2 2.236(5) . ?
Mo3 Mo3 2.5951(11) 3_656 ?
Mo3 O8 2.242(4) . ?
Mo3 O9 2.122(3) . ?
Mo3 O9 2.122(3) 10_655 ?
Mo3 O11 1.946(3) . ?
Mo3 O11 1.946(3) 10_655 ?
Mo3 O12 1.690(5) . ?
Mo4 O3 2.166(3) 12_557 ?
Mo4 O6 1.877(3) . ?
Mo4 O8 2.277(3) . ?
Mo4 O7 1.698(4) . ?
Mo4 O9 1.798(3) . ?
Mo4 O10 1.944(2) . ?
O8 H8 0.7700(10) . ?
N1 C1 1.309(7) . ?
N1 C5 1.289(10) . ?
N2 C6 1.338(6) 12_557 ?
N2 C6 1.338(6) . ?
N3 C9 1.3900 . ?
N3 C13 1.3900 . ?
C9 H9 0.9300 . ?
C9 C10 1.3900 . ?
C10 H10 0.9300 . ?
C10 C11 1.3900 . ?
C11 H11 0.9300 . ?
C11 C12 1.3900 . ?
C12 H12 0.9300 . ?
C12 C13 1.3900 . ?
C13 H13 0.9300 . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C14 1.432(8) . ?
N4 C14 1.432(8) 12_557 ?
C1 H1 0.9300 . ?
C1 C2 1.404(10) . ?
C2 H2 0.9300 . ?
C2 C3 1.286(12) . ?
C3 H3 0.9300 . ?
C3 C4 1.368(12) . ?
C4 H4 0.9300 . ?
C4 C5 1.411(12) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.380(8) . ?
C7 H7 0.9300 . ?
C7 C8 1.348(9) . ?
C8 H8A 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
O1W H1WA 0.8700(10) . ?
O1W H1WA 0.8700(10) 12_557 ?
O1W H1WB 0.8700(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Sb1 O3 102.15(18) 10_655 . ?
O3 Sb1 O4 95.73(12) 10_655 . ?
O3 Sb1 O4 95.73(12) . . ?
Mo1 Mo1 Mo2 60.095(11) 12_557 . ?
O1 Mo1 Mo1 49.59(8) . 12_557 ?
O1 Mo1 Mo2 96.29(11) . . ?
O1 Mo1 O2 99.03(17) . . ?
O1 Mo1 O3 169.66(14) . 12_557 ?
O1 Mo1 O5 100.36(11) . . ?
O1 Mo1 O6 98.28(17) . . ?
O1 Mo1 N1 84.81(16) . . ?
O2 Mo1 Mo1 96.41(10) . 12_557 ?
O2 Mo1 Mo2 49.18(9) . . ?
O2 Mo1 O3 87.96(13) . 12_557 ?
O2 Mo1 O5 100.35(14) . . ?
O2 Mo1 O6 158.55(14) . . ?
O2 Mo1 N1 84.74(15) . . ?
O3 Mo1 Mo1 137.56(8) 12_557 12_557 ?
O3 Mo1 Mo2 94.05(8) 12_557 . ?
O3 Mo1 N1 88.28(15) 12_557 . ?
O5 Mo1 Mo1 51.90(7) . 12_557 ?
O5 Mo1 Mo2 52.33(11) . . ?
O5 Mo1 O3 85.75(11) . 12_557 ?
O5 Mo1 N1 171.99(15) . . ?
O6 Mo1 Mo1 104.45(10) . 12_557 ?
O6 Mo1 Mo2 140.47(9) . . ?
O6 Mo1 O3 73.34(13) . 12_557 ?
O6 Mo1 O5 88.87(14) . . ?
O6 Mo1 N1 84.31(15) . . ?
N1 Mo1 Mo1 134.12(13) . 12_557 ?
N1 Mo1 Mo2 133.63(12) . . ?
Mo1 Mo2 Mo1 59.81(2) . 12_557 ?
O2 Mo2 Mo1 50.27(9) 12_557 12_557 ?
O2 Mo2 Mo1 50.27(9) . . ?
O2 Mo2 Mo1 97.01(10) 12_557 . ?
O2 Mo2 Mo1 97.01(10) . 12_557 ?
O2 Mo2 O2 99.54(19) 12_557 . ?
O2 Mo2 O5 100.74(12) 12_557 . ?
O2 Mo2 O5 100.74(12) . . ?
O2 Mo2 O4 165.89(14) 12_557 3_656 ?
O2 Mo2 O4 165.89(13) . . ?
O2 Mo2 O4 90.98(13) 12_557 . ?
O2 Mo2 O4 90.98(12) . 3_656 ?
O2 Mo2 N2 83.42(13) 12_557 . ?
O2 Mo2 N2 83.42(13) . . ?
O5 Mo2 Mo1 51.63(8) . 12_557 ?
O5 Mo2 Mo1 51.63(8) . . ?
O5 Mo2 O4 86.37(14) . . ?
O5 Mo2 O4 86.37(14) . 3_656 ?
O5 Mo2 N2 173.45(17) . . ?
O4 Mo2 Mo1 138.00(11) . . ?
O4 Mo2 Mo1 138.00(11) 3_656 12_557 ?
O4 Mo2 Mo1 96.94(10) 3_656 . ?
O4 Mo2 Mo1 96.95(10) . 12_557 ?
O4 Mo2 O4 77.21(16) . 3_656 ?
O4 Mo2 N2 88.51(15) . . ?
O4 Mo2 N2 88.51(15) 3_656 . ?
N2 Mo2 Mo1 133.29(10) . 12_557 ?
N2 Mo2 Mo1 133.29(10) . . ?
O8 Mo3 Mo3 97.35(11) . 3_656 ?
O9 Mo3 Mo3 135.62(9) 10_655 3_656 ?
O9 Mo3 Mo3 135.62(9) . 3_656 ?
O9 Mo3 O8 70.89(11) 10_655 . ?
O9 Mo3 O8 70.89(11) . . ?
O9 Mo3 O9 82.25(18) 10_655 . ?
O11 Mo3 Mo3 48.17(9) 10_655 3_656 ?
O11 Mo3 Mo3 48.17(9) . 3_656 ?
O11 Mo3 O8 87.62(15) . . ?
O11 Mo3 O8 87.62(15) 10_655 . ?
O11 Mo3 O9 87.90(13) 10_655 . ?
O11 Mo3 O9 87.90(13) . 10_655 ?
O11 Mo3 O9 158.28(16) 10_655 10_655 ?
O11 Mo3 O9 158.28(16) . . ?
O11 Mo3 O11 94.46(18) 10_655 . ?
O12 Mo3 Mo3 103.0(2) . 3_656 ?
O12 Mo3 O8 159.6(2) . . ?
O12 Mo3 O9 94.05(17) . . ?
O12 Mo3 O9 94.05(17) . 10_655 ?
O12 Mo3 O11 105.96(18) . . ?
O12 Mo3 O11 105.96(19) . 10_655 ?
O3 Mo4 O8 82.27(13) 12_557 . ?
O6 Mo4 O3 74.90(12) . 12_557 ?
O6 Mo4 O8 87.24(13) . . ?
O6 Mo4 O10 150.59(16) . . ?
O7 Mo4 O3 99.26(15) . 12_557 ?
O7 Mo4 O6 102.05(17) . . ?
O7 Mo4 O8 170.68(16) . . ?
O7 Mo4 O9 103.27(16) . . ?
O7 Mo4 O10 97.31(18) . . ?
O9 Mo4 O3 157.37(13) . 12_557 ?
O9 Mo4 O6 98.09(14) . . ?
O9 Mo4 O8 75.85(14) . . ?
O9 Mo4 O10 98.76(17) . . ?
O10 Mo4 O3 80.33(15) . 12_557 ?
O10 Mo4 O8 73.80(14) . . ?
Mo1 O1 Mo1 80.83(17) 12_557 . ?
Mo2 O2 Mo1 80.56(12) . . ?
Sb1 O3 Mo1 126.71(15) . 12_557 ?
Sb1 O3 Mo4 128.72(15) . 12_557 ?
Mo1 O3 Mo4 97.76(12) 12_557 12_557 ?
Mo1 O5 Mo1 76.21(14) 12_557 . ?
Mo1 O5 Mo2 76.04(13) 12_557 . ?
Mo1 O5 Mo2 76.03(13) . . ?
Sb1 O4 Mo2 123.59(11) . . ?
Sb1 O4 Mo2 123.59(11) . 10_655 ?
Mo2 O4 Mo2 102.57(16) 10_655 . ?
Mo4 O6 Mo1 113.99(16) . . ?
Mo3 O8 Mo4 95.78(13) . . ?
Mo3 O8 Mo4 95.78(13) . 10_655 ?
Mo3 O8 H8 132(3) . . ?
Mo4 O8 Mo4 93.20(16) 10_655 . ?
Mo4 O8 H8 116(2) . . ?
Mo4 O8 H8 116(2) 10_655 . ?
Mo4 O9 Mo3 117.29(15) . . ?
Mo4 O10 Mo4 116.6(2) . 10_655 ?
Mo3 O11 Mo3 83.66(18) 3_656 . ?
C1 N1 Mo1 119.6(5) . . ?
C5 N1 Mo1 123.5(5) . . ?
C5 N1 C1 116.9(7) . . ?
C6 N2 Mo2 121.7(3) 12_557 . ?
C6 N2 Mo2 121.7(3) . . ?
C6 N2 C6 116.4(7) 12_557 . ?
C9 N3 C13 120.0 . . ?
N3 C9 H9 120.0 . . ?
C10 C9 N3 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C13 C12 H12 120.0 . . ?
N3 C13 H13 120.0 . . ?
C12 C13 N3 120.0 . . ?
C12 C13 H13 120.0 . . ?
H4A N4 H4B 107.3 . . ?
C14 N4 H4A 108.1 12_557 . ?
C14 N4 H4A 108.1 . . ?
C14 N4 H4B 108.1 12_557 . ?
C14 N4 H4B 108.1 . . ?
C14 N4 C14 116.7(8) 12_557 . ?
N1 C1 H1 118.3 . . ?
N1 C1 C2 123.4(7) . . ?
C2 C1 H1 118.3 . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.3(8) . . ?
C3 C2 H2 120.3 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.4(8) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 121.0 . . ?
C3 C4 C5 118.0(9) . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 122.7(8) . . ?
N1 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
N2 C6 H6 118.8 . . ?
N2 C6 C7 122.4(6) . . ?
C7 C6 H6 118.8 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.6(7) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C7 117.5(8) 12_557 . ?
C7 C8 H8A 121.2 12_557 . ?
C7 C8 H8A 121.2 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
H1WA O1W H1WA 40.43(5) . 12_557 ?
H1WA O1W H1WB 101.7(11) . . ?
H1WB O1W H1WA 101.7(11) . 12_557 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 N1 C1 C2 178.6(7) . . . . ?
Mo1 N1 C5 C4 179.6(7) . . . . ?
Mo2 N2 C6 C7 -178.1(6) . . . . ?
O3 Mo4 O6 Mo1 0.89(15) 12_557 . . . ?
O3 Mo4 O9 Mo3 -11.3(5) 12_557 . . . ?
O6 Mo4 O9 Mo3 -81.27(19) . . . . ?
O8 Mo4 O6 Mo1 83.63(18) . . . . ?
O8 Mo4 O9 Mo3 3.80(15) . . . . ?
O7 Mo4 O6 Mo1 -95.58(19) . . . . ?
O7 Mo4 O9 Mo3 174.2(2) . . . . ?
O9 Mo4 O6 Mo1 158.91(17) . . . . ?
O10 Mo4 O6 Mo1 34.5(4) . . . . ?
O10 Mo4 O9 Mo3 74.5(2) . . . . ?
N1 C1 C2 C3 1.1(15) . . . . ?
N2 C6 C7 C8 1.0(13) . . . . ?
N3 C9 C10 C11 0.0 . . . . ?
C9 N3 C13 C12 0.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 N3 0.0 . . . . ?
C13 N3 C9 C10 0.0 . . . . ?
C1 N1 C5 C4 2.1(14) . . . . ?
C1 C2 C3 C4 3.2(16) . . . . ?
C2 C3 C4 C5 -4.7(15) . . . . ?
C3 C4 C5 N1 2.0(15) . . . . ?
C5 N1 C1 C2 -3.8(13) . . . . ?
C6 N2 C6 C7 -2.1(12) 12_557 . . . ?
C6 C7 C8 C7 0.1(16) . . . 12_557 ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 154 electrons were 
found in a volume of 1086Å³ in 1 void per unit cell. 
This is consistent with the presence of 
4[H2O] per Asymmetric Unit 
which account for 160 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.025 543.0 76.6 '8 H2O'
2 0.500 0.000 0.570 543.0 76.6 '8 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
