# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1950999'
loop_
_audit_author_name
_audit_author_address
'Frank Allen'
;Tonghua normal university
China
;
_audit_update_record             
;
2019-09-03 deposited with the CCDC.	2019-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H26 Cu2 Mo8 N6 O28'
_chemical_formula_sum            'C30 H26 Cu2 Mo8 N6 O28'
_chemical_formula_weight         1813.17

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.0868(6)
_cell_length_b                   15.3515(7)
_cell_length_c                   12.4671(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.5040(10)
_cell_angle_gamma                90
_cell_volume                     2258.41(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    18370
_cell_measurement_theta_min      3.138
_cell_measurement_theta_max      28.390

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.666
_exptl_crystal_F_000             1732
_exptl_transmission_factor_min   0.472
_exptl_transmission_factor_max   0.622
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    3.166
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18370
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.138
_diffrn_reflns_theta_max         28.390
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5491
_reflns_number_gt                3785
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the non-H atoms Mo, Cu, C, N and O were 
refined anisotropically.
;

_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0448P)²+22.9460P] 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         5491
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0701
_refine_ls_wR_factor_ref         0.1364
_refine_ls_wR_factor_gt          0.1209
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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 0.95603(7) 0.16104(5) 0.59933(6) 0.01724(19) Uani 1 1 d . . . . .
Mo2 Mo 1.11344(7) 0.20143(5) 0.42199(6) 0.0177(2) Uani 1 1 d . . . . .
Mo3 Mo 1.00537(7) 0.03565(5) 0.27420(6) 0.01793(19) Uani 1 1 d . . . . .
Mo4 Mo 0.85186(7) -0.00216(5) 0.44943(6) 0.01367(18) Uani 1 1 d . . . . .
Cu1 Cu 0.87816(10) 0.35161(7) 0.25001(9) 0.0193(3) Uani 1 1 d . . . . .
O1 O 1.0000(6) 0.2622(4) 0.3562(5) 0.0279(17) Uani 1 1 d . . . . .
O2 O 0.9935(5) 0.0819(4) 0.4529(4) 0.0138(13) Uani 1 1 d . . . . .
O3 O 0.8505(6) 0.2215(4) 0.5228(6) 0.0306(17) Uani 1 1 d . . . . .
O4 O 0.8718(5) 0.0487(4) 0.5963(4) 0.0158(13) Uani 1 1 d . . . . .
O5 O 0.7502(6) 0.0630(4) 0.3754(5) 0.0232(15) Uani 1 1 d . . . . .
O6 O 1.0877(6) 0.2194(4) 0.5693(5) 0.0202(14) Uani 1 1 d . . . . .
O7 O 0.8949(6) 0.1001(4) 0.2152(5) 0.0261(16) Uani 1 1 d . . . . .
O9 O 1.1236(6) 0.1187(4) 0.3103(5) 0.0211(15) Uani 1 1 d . . . . .
O10 O 0.7786(6) -0.0956(4) 0.4782(5) 0.0198(14) Uani 1 1 d . . . . .
O11 O 0.9130(5) -0.0529(4) 0.3319(4) 0.0153(13) Uani 1 1 d . . . . .
O1W O 0.7672(6) 0.2560(4) 0.2337(5) 0.0239(15) Uani 1 1 d . . . . .
O8 O 1.0421(7) -0.0192(5) 0.1685(5) 0.0313(18) Uani 1 1 d . . . . .
O12 O 0.9657(7) 0.1950(4) 0.7305(5) 0.0325(18) Uani 1 1 d . . . . .
O13 O 1.2267(7) 0.2655(5) 0.4233(6) 0.0338(18) Uani 1 1 d . . . . .
N1 N 0.9601(7) 0.3237(5) 0.1291(6) 0.0201(17) Uani 1 1 d . . . . .
N3 N 0.8176(7) 0.4210(5) 0.3621(6) 0.0222(18) Uani 1 1 d . . . . .
N2 N 0.9681(7) 0.4561(5) 0.2542(7) 0.0235(18) Uani 1 1 d . . . . .
C1 C 0.8672(9) 0.4997(6) 0.3856(8) 0.024(2) Uani 1 1 d . . . . .
C5 C 1.0353(9) 0.3855(6) 0.1159(8) 0.027(2) Uani 1 1 d . . . . .
C7 C 0.9480(9) 0.2534(7) 0.0646(8) 0.026(2) Uani 1 1 d . . . . .
H7A H 0.8980 0.2100 0.0757 0.032 Uiso 1 1 calc R U . . .
C6 C 1.0062(10) 0.2425(7) -0.0172(8) 0.033(3) Uani 1 1 d . . . . .
H6A H 0.9955 0.1927 -0.0608 0.040 Uiso 1 1 calc R U . . .
C4 C 1.0417(10) 0.4611(6) 0.1887(8) 0.027(2) Uani 1 1 d . . . . .
C3 C 0.7373(11) 0.3988(7) 0.4130(9) 0.034(3) Uani 1 1 d . . . . .
H3A H 0.7023 0.3451 0.3961 0.041 Uiso 1 1 calc R U . . .
C2 C 0.9556(9) 0.5189(6) 0.3240(8) 0.026(2) Uani 1 1 d . . . . .
C13 C 0.8367(10) 0.5545(7) 0.4625(8) 0.032(3) Uani 1 1 d . . . . .
H13A H 0.8725 0.6080 0.4786 0.038 Uiso 1 1 calc R U . . .
C14 C 0.7536(11) 0.5295(7) 0.5146(8) 0.033(3) Uani 1 1 d . . . . .
H14A H 0.7326 0.5661 0.5663 0.039 Uiso 1 1 calc R U . . .
C10 C 1.1108(10) 0.5333(7) 0.1952(10) 0.034(3) Uani 1 1 d . . . . .
H10A H 1.1635 0.5373 0.1510 0.041 Uiso 1 1 calc R U . . .
C9 C 1.0978(11) 0.3775(8) 0.0352(10) 0.041(3) Uani 1 1 d . . . . .
H9A H 1.1508 0.4197 0.0278 0.049 Uiso 1 1 calc R U . . .
C12 C 1.0224(10) 0.5932(6) 0.3317(10) 0.036(3) Uani 1 1 d . . . . .
H12A H 1.0139 0.6380 0.3794 0.043 Uiso 1 1 calc R U . . .
C15 C 0.7011(11) 0.4507(7) 0.4909(9) 0.035(3) Uani 1 1 d . . . . .
H15A H 0.6439 0.4325 0.5250 0.042 Uiso 1 1 calc R U . . .
C8 C 1.0807(11) 0.3062(8) -0.0340(10) 0.042(3) Uani 1 1 d . . . . .
H8A H 1.1188 0.3014 -0.0910 0.051 Uiso 1 1 calc R U . . .
C11 C 1.1013(11) 0.5991(7) 0.2674(10) 0.042(3) Uani 1 1 d . . . . .
H11A H 1.1482 0.6477 0.2727 0.051 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O3 1.694(7) . ?
Mo1 O12 1.696(6) . ?
Mo1 O6 1.933(7) . ?
Mo1 O4 1.998(6) . ?
Mo1 O2 2.318(6) . ?
Mo1 O11 2.326(6) 3_756 ?
Mo1 Mo4 3.2150(10) . ?
Mo2 O13 1.683(8) . ?
Mo2 O1 1.714(7) . ?
Mo2 O9 1.909(6) . ?
Mo2 O6 1.948(6) . ?
Mo2 O10 2.277(6) 3_756 ?
Mo2 O2 2.421(6) . ?
Mo3 O7 1.696(7) . ?
Mo3 O8 1.701(7) . ?
Mo3 O9 1.895(7) . ?
Mo3 O11 1.990(6) . ?
Mo3 O4 2.334(6) 3_756 ?
Mo3 O2 2.372(6) . ?
Mo3 Mo4 3.2106(12) . ?
Mo4 O5 1.695(6) . ?
Mo4 O10 1.763(6) . ?
Mo4 O11 1.942(6) . ?
Mo4 O4 1.957(5) . ?
Mo4 O2 2.136(6) . ?
Mo4 O2 2.343(6) 3_756 ?
Cu1 N2 1.932(8) . ?
Cu1 O1W 1.969(7) . ?
Cu1 N3 2.015(8) . ?
Cu1 N1 2.021(8) . ?
Cu1 O1 2.227(6) . ?
O2 Mo4 2.343(6) 3_756 ?
O4 Mo3 2.334(6) 3_756 ?
O10 Mo2 2.277(6) 3_756 ?
O11 Mo1 2.326(6) 3_756 ?
N1 C7 1.335(12) . ?
N1 C5 1.348(13) . ?
N3 C3 1.315(14) . ?
N3 C1 1.353(12) . ?
N2 C2 1.329(13) . ?
N2 C4 1.333(14) . ?
C1 C13 1.385(14) . ?
C1 C2 1.474(15) . ?
C5 C9 1.389(15) . ?
C5 C4 1.464(14) . ?
C7 C6 1.368(15) . ?
C6 C8 1.376(17) . ?
C4 C10 1.379(14) . ?
C3 C15 1.397(15) . ?
C2 C12 1.388(14) . ?
C13 C14 1.363(16) . ?
C14 C15 1.369(16) . ?
C10 C11 1.375(16) . ?
C9 C8 1.381(17) . ?
C12 C11 1.376(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mo1 O12 105.1(4) . . ?
O3 Mo1 O6 100.8(3) . . ?
O12 Mo1 O6 99.0(3) . . ?
O3 Mo1 O4 98.3(3) . . ?
O12 Mo1 O4 102.2(3) . . ?
O6 Mo1 O4 146.5(3) . . ?
O3 Mo1 O2 95.5(3) . . ?
O12 Mo1 O2 159.4(3) . . ?
O6 Mo1 O2 77.4(2) . . ?
O4 Mo1 O2 73.6(2) . . ?
O3 Mo1 O11 165.4(3) . 3_756 ?
O12 Mo1 O11 88.0(3) . 3_756 ?
O6 Mo1 O11 83.0(2) . 3_756 ?
O4 Mo1 O11 72.2(2) . 3_756 ?
O2 Mo1 O11 71.51(19) . 3_756 ?
O3 Mo1 Mo4 87.0(2) . . ?
O12 Mo1 Mo4 137.4(3) . . ?
O6 Mo1 Mo4 118.96(18) . . ?
O4 Mo1 Mo4 35.20(16) . . ?
O2 Mo1 Mo4 41.60(15) . . ?
O11 Mo1 Mo4 78.93(14) 3_756 . ?
O13 Mo2 O1 104.5(4) . . ?
O13 Mo2 O9 102.5(3) . . ?
O1 Mo2 O9 100.6(3) . . ?
O13 Mo2 O6 101.7(3) . . ?
O1 Mo2 O6 95.7(3) . . ?
O9 Mo2 O6 146.2(3) . . ?
O13 Mo2 O10 92.5(3) . 3_756 ?
O1 Mo2 O10 162.6(3) . 3_756 ?
O9 Mo2 O10 78.7(2) . 3_756 ?
O6 Mo2 O10 77.0(2) . 3_756 ?
O13 Mo2 O2 162.8(3) . . ?
O1 Mo2 O2 92.6(3) . . ?
O9 Mo2 O2 75.3(2) . . ?
O6 Mo2 O2 74.6(2) . . ?
O10 Mo2 O2 70.4(2) 3_756 . ?
O7 Mo3 O8 105.4(3) . . ?
O7 Mo3 O9 101.1(3) . . ?
O8 Mo3 O9 101.9(3) . . ?
O7 Mo3 O11 96.0(3) . . ?
O8 Mo3 O11 101.7(3) . . ?
O9 Mo3 O11 145.8(2) . . ?
O7 Mo3 O4 161.2(3) . 3_756 ?
O8 Mo3 O4 91.6(3) . 3_756 ?
O9 Mo3 O4 82.8(2) . 3_756 ?
O11 Mo3 O4 72.1(2) . 3_756 ?
O7 Mo3 O2 91.8(3) . . ?
O8 Mo3 O2 162.6(3) . . ?
O9 Mo3 O2 76.8(2) . . ?
O11 Mo3 O2 73.3(2) . . ?
O4 Mo3 O2 71.04(19) 3_756 . ?
O7 Mo3 Mo4 83.3(2) . . ?
O8 Mo3 Mo4 136.3(3) . . ?
O9 Mo3 Mo4 118.52(18) . . ?
O11 Mo3 Mo4 34.77(16) . . ?
O4 Mo3 Mo4 78.67(16) 3_756 . ?
O2 Mo3 Mo4 41.71(15) . . ?
O5 Mo4 O10 104.8(3) . . ?
O5 Mo4 O11 100.1(3) . . ?
O10 Mo4 O11 96.7(3) . . ?
O5 Mo4 O4 101.7(3) . . ?
O10 Mo4 O4 95.8(3) . . ?
O11 Mo4 O4 151.2(3) . . ?
O5 Mo4 O2 97.9(3) . . ?
O10 Mo4 O2 157.3(3) . . ?
O11 Mo4 O2 79.8(2) . . ?
O4 Mo4 O2 78.7(2) . . ?
O5 Mo4 O2 173.9(3) . 3_756 ?
O10 Mo4 O2 81.3(3) . 3_756 ?
O11 Mo4 O2 78.0(2) . 3_756 ?
O4 Mo4 O2 78.4(2) . 3_756 ?
O2 Mo4 O2 76.1(2) . 3_756 ?
O5 Mo4 Mo3 88.9(2) . . ?
O10 Mo4 Mo3 132.5(2) . . ?
O11 Mo4 Mo3 35.76(18) . . ?
O4 Mo4 Mo3 126.30(19) . . ?
O2 Mo4 Mo3 47.62(15) . . ?
O2 Mo4 Mo3 86.24(15) 3_756 . ?
O5 Mo4 Mo1 90.2(2) . . ?
O10 Mo4 Mo1 131.8(2) . . ?
O11 Mo4 Mo1 125.90(18) . . ?
O4 Mo4 Mo1 36.06(18) . . ?
O2 Mo4 Mo1 46.09(16) . . ?
O2 Mo4 Mo1 86.38(14) 3_756 . ?
Mo3 Mo4 Mo1 92.48(3) . . ?
N2 Cu1 O1W 171.3(3) . . ?
N2 Cu1 N3 80.2(4) . . ?
O1W Cu1 N3 97.1(3) . . ?
N2 Cu1 N1 80.3(3) . . ?
O1W Cu1 N1 101.4(3) . . ?
N3 Cu1 N1 159.9(3) . . ?
N2 Cu1 O1 101.5(3) . . ?
O1W Cu1 O1 87.2(3) . . ?
N3 Cu1 O1 101.9(3) . . ?
N1 Cu1 O1 86.8(3) . . ?
Mo2 O1 Cu1 167.9(5) . . ?
Mo4 O2 Mo1 92.3(2) . . ?
Mo4 O2 Mo4 103.9(2) . 3_756 ?
Mo1 O2 Mo4 97.7(2) . 3_756 ?
Mo4 O2 Mo3 90.7(2) . . ?
Mo1 O2 Mo3 163.4(3) . . ?
Mo4 O2 Mo3 97.4(2) 3_756 . ?
Mo4 O2 Mo2 163.6(3) . . ?
Mo1 O2 Mo2 87.34(19) . . ?
Mo4 O2 Mo2 92.3(2) 3_756 . ?
Mo3 O2 Mo2 85.2(2) . . ?
Mo4 O4 Mo1 108.7(3) . . ?
Mo4 O4 Mo3 110.9(3) . 3_756 ?
Mo1 O4 Mo3 102.8(2) . 3_756 ?
Mo1 O6 Mo2 115.0(3) . . ?
Mo3 O9 Mo2 117.2(3) . . ?
Mo4 O10 Mo2 116.0(3) . 3_756 ?
Mo4 O11 Mo3 109.5(3) . . ?
Mo4 O11 Mo1 110.4(2) . 3_756 ?
Mo3 O11 Mo1 103.3(3) . 3_756 ?
C7 N1 C5 119.0(9) . . ?
C7 N1 Cu1 127.8(7) . . ?
C5 N1 Cu1 113.2(7) . . ?
C3 N3 C1 117.7(9) . . ?
C3 N3 Cu1 127.9(7) . . ?
C1 N3 Cu1 114.3(7) . . ?
C2 N2 C4 123.0(9) . . ?
C2 N2 Cu1 118.5(8) . . ?
C4 N2 Cu1 118.5(7) . . ?
N3 C1 C13 121.4(10) . . ?
N3 C1 C2 113.7(9) . . ?
C13 C1 C2 124.9(9) . . ?
N1 C5 C9 120.9(10) . . ?
N1 C5 C4 115.4(9) . . ?
C9 C5 C4 123.7(10) . . ?
N1 C7 C6 122.7(10) . . ?
C7 C6 C8 119.0(10) . . ?
N2 C4 C10 119.1(10) . . ?
N2 C4 C5 112.4(9) . . ?
C10 C4 C5 128.5(11) . . ?
N3 C3 C15 124.3(11) . . ?
N2 C2 C12 119.6(11) . . ?
N2 C2 C1 113.2(9) . . ?
C12 C2 C1 127.2(10) . . ?
C14 C13 C1 119.5(10) . . ?
C13 C14 C15 120.1(10) . . ?
C11 C10 C4 119.6(11) . . ?
C8 C9 C5 119.4(11) . . ?
C11 C12 C2 118.7(10) . . ?
C14 C15 C3 117.0(11) . . ?
C6 C8 C9 118.9(11) . . ?
C10 C11 C12 120.0(11) . . ?

_refine_diff_density_max         1.377
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.253

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1951000'
loop_
_audit_author_name
_audit_author_address
'Frank Allen'
;Tonghua normal university
China
;
_audit_update_record             
;
2019-09-03 deposited with the CCDC.	2019-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H11 Cu Mo3 N5 O11'
_chemical_formula_sum            'C11 H11 Cu Mo3 N5 O11'
_chemical_formula_weight         740.61

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   7.633(5)
_cell_length_b                   10.979(5)
_cell_length_c                   11.349(5)
_cell_angle_alpha                77.076(5)
_cell_angle_beta                 85.384(5)
_cell_angle_gamma                74.767(5)
_cell_volume                     894.2(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12537
_cell_measurement_theta_min      2.963
_cell_measurement_theta_max      28.328

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.751
_exptl_crystal_F_000             710
_exptl_transmission_factor_min   0.386
_exptl_transmission_factor_max   0.609
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    3.303
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12537
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.963
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             4425
_reflns_number_gt                4239
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the non-H atoms Mo, Cu, C, N and O were 
refined anisotropically. Two H atoms were fixed to O1W, This command
led to a restraint number 2.
;

_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0252P)²+4.5487P] 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         4425
_refine_ls_number_parameters     286
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0621
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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 0.02807(3) 0.41708(2) 0.64996(2) 0.00548(6) Uani 1 1 d . . . . .
Mo2 Mo -0.53186(3) 0.59889(2) 0.35272(2) 0.00749(6) Uani 1 1 d . . . . .
Mo3 Mo -0.32118(3) 0.66069(2) 0.57118(2) 0.00949(6) Uani 1 1 d . . . . .
Cu1 Cu -0.90225(5) 0.86828(4) 0.21053(4) 0.01466(9) Uani 1 1 d . . . . .
O1 O -0.6298(3) 0.7627(2) 0.3117(2) 0.0190(5) Uani 1 1 d . . . . .
O1W O -0.5734(5) 1.0245(3) 0.3148(3) 0.0354(7) Uani 1 1 d D . . . .
H1WA H -0.524(8) 0.950(3) 0.357(5) 0.053 Uiso 1 1 d D U . . .
H1WB H -0.577(8) 1.072(5) 0.365(4) 0.053 Uiso 1 1 d D U . . .
O2 O 0.0259(3) 0.2533(2) 0.7013(2) 0.0164(5) Uani 1 1 d . . . . .
O3 O -0.2424(3) 0.4487(2) 0.6277(2) 0.0129(4) Uani 1 1 d . . . . .
O4 O -0.4531(3) 0.5556(3) 0.2192(2) 0.0197(5) Uani 1 1 d . . . . .
O5 O 0.0208(3) 0.4701(2) 0.7804(2) 0.0187(5) Uani 1 1 d . . . . .
O6 O -0.0574(3) 0.6031(2) 0.54697(19) 0.0108(4) Uani 1 1 d . . . . .
O7 O -0.2763(3) 0.6007(2) 0.3891(2) 0.0131(4) Uani 1 1 d . . . . .
O8 O -0.5307(3) 0.6044(2) 0.5449(2) 0.0116(4) Uani 1 1 d . . . . .
O9 O -0.3400(3) 0.6727(3) 0.7191(2) 0.0208(5) Uani 1 1 d . . . . .
O10 O -0.3684(3) 0.8194(2) 0.4932(2) 0.0222(5) Uani 1 1 d . . . . .
C1 C -0.7473(5) 0.6745(4) 0.0363(3) 0.0230(7) Uani 1 1 d . . . . .
H1A H -0.7773 0.5998 0.0793 0.028 Uiso 1 1 calc R U . . .
C2 C -0.6493(5) 0.6836(4) -0.0742(4) 0.0273(8) Uani 1 1 d . . . . .
H2A H -0.6039 0.6183 -0.1168 0.033 Uiso 1 1 calc R U . . .
C3 C -0.6342(5) 0.8077(4) -0.1061(3) 0.0263(8) Uani 1 1 d . . . . .
H3A H -0.5758 0.8437 -0.1750 0.032 Uiso 1 1 calc R U . . .
C4 C -0.7448(4) 0.9955(3) -0.0025(3) 0.0189(7) Uani 1 1 d . . . . .
C5 C -0.6895(5) 1.0947(4) -0.0816(3) 0.0260(8) Uani 1 1 d . . . . .
H5A H -0.6303 1.0832 -0.1547 0.031 Uiso 1 1 calc R U . . .
C6 C -0.7272(6) 1.2132(4) -0.0460(4) 0.0303(9) Uani 1 1 d . . . . .
H6A H -0.6897 1.2816 -0.0959 0.036 Uiso 1 1 calc R U . . .
C7 C -0.8185(5) 1.2311(4) 0.0612(4) 0.0264(8) Uani 1 1 d . . . . .
H7A H -0.8438 1.3102 0.0842 0.032 Uiso 1 1 calc R U . . .
C8 C -0.8709(5) 1.1265(3) 0.1329(3) 0.0177(6) Uani 1 1 d . . . . .
C9 C -1.0499(5) 1.2180(4) 0.3040(4) 0.0252(8) Uani 1 1 d . . . . .
H9A H -1.0378 1.3023 0.2865 0.030 Uiso 1 1 calc R U . . .
C10 C -1.1474(5) 1.1651(4) 0.3975(4) 0.0288(8) Uani 1 1 d . . . . .
H10A H -1.2143 1.2055 0.4565 0.035 Uiso 1 1 calc R U . . .
C11 C -1.1265(5) 1.0369(4) 0.3872(3) 0.0241(7) Uani 1 1 d . . . . .
H11A H -1.1798 0.9777 0.4393 0.029 Uiso 1 1 calc R U . . .
N1 N -0.7916(4) 0.7862(3) 0.0710(3) 0.0178(6) Uani 1 1 d . . . . .
N2 N -1.0202(4) 1.0121(3) 0.2925(3) 0.0187(6) Uani 1 1 d . . . . .
N3 N -0.8314(4) 1.0125(3) 0.1015(3) 0.0168(5) Uani 1 1 d . . . . .
N4 N -0.9731(4) 1.1250(3) 0.2405(3) 0.0193(6) Uani 1 1 d . . . . .
N5 N -0.7209(4) 0.8694(3) -0.0180(3) 0.0191(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O5 1.700(3) . ?
Mo1 O2 1.766(2) . ?
Mo1 O7 1.880(2) 2_566 ?
Mo1 O3 2.028(3) . ?
Mo1 O6 2.078(2) . ?
Mo1 O6 2.282(2) 2_566 ?
Mo2 O4 1.705(3) . ?
Mo2 O1 1.728(2) . ?
Mo2 O3 1.911(2) 2_466 ?
Mo2 O7 2.032(2) . ?
Mo2 O8 2.196(2) . ?
Mo2 O8 2.220(2) 2_466 ?
Mo3 O9 1.705(3) . ?
Mo3 O10 1.727(3) . ?
Mo3 O8 1.926(2) . ?
Mo3 O6 1.962(2) . ?
Mo3 O3 2.202(2) . ?
Mo3 O7 2.280(2) . ?
Cu1 O2 1.894(2) 2_466 ?
Cu1 N3 1.948(3) . ?
Cu1 N2 1.986(3) . ?
Cu1 N1 2.014(3) . ?
Cu1 O1 2.347(3) . ?
O2 Cu1 1.894(2) 2_466 ?
O3 Mo2 1.911(2) 2_466 ?
O6 Mo1 2.282(2) 2_566 ?
O7 Mo1 1.880(2) 2_566 ?
O8 Mo2 2.220(2) 2_466 ?
C1 N1 1.324(5) . ?
C1 C2 1.405(5) . ?
C2 C3 1.363(6) . ?
C3 N5 1.362(5) . ?
C4 N3 1.331(4) . ?
C4 C5 1.383(5) . ?
C4 N5 1.398(5) . ?
C5 C6 1.399(6) . ?
C6 C7 1.379(6) . ?
C7 C8 1.383(5) . ?
C8 N3 1.330(4) . ?
C8 N4 1.394(5) . ?
C9 C10 1.357(6) . ?
C9 N4 1.361(5) . ?
C10 C11 1.405(5) . ?
C11 N2 1.328(5) . ?
N1 N5 1.379(4) . ?
N2 N4 1.374(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Mo1 O2 103.16(12) . . ?
O5 Mo1 O7 98.58(11) . 2_566 ?
O2 Mo1 O7 100.26(10) . 2_566 ?
O5 Mo1 O3 99.04(10) . . ?
O2 Mo1 O3 85.42(10) . . ?
O7 Mo1 O3 159.72(10) 2_566 . ?
O5 Mo1 O6 92.97(11) . . ?
O2 Mo1 O6 155.40(10) . . ?
O7 Mo1 O6 95.47(9) 2_566 . ?
O3 Mo1 O6 73.66(9) . . ?
O5 Mo1 O6 164.62(10) . 2_566 ?
O2 Mo1 O6 91.84(10) . 2_566 ?
O7 Mo1 O6 75.05(9) 2_566 2_566 ?
O3 Mo1 O6 85.38(8) . 2_566 ?
O6 Mo1 O6 74.03(9) . 2_566 ?
O4 Mo2 O1 103.97(13) . . ?
O4 Mo2 O3 100.94(11) . 2_466 ?
O1 Mo2 O3 94.73(11) . 2_466 ?
O4 Mo2 O7 89.52(11) . . ?
O1 Mo2 O7 100.36(10) . . ?
O3 Mo2 O7 159.03(10) 2_466 . ?
O4 Mo2 O8 157.81(10) . . ?
O1 Mo2 O8 92.75(10) . . ?
O3 Mo2 O8 91.96(9) 2_466 . ?
O7 Mo2 O8 72.97(9) . . ?
O4 Mo2 O8 92.95(11) . 2_466 ?
O1 Mo2 O8 161.45(10) . 2_466 ?
O3 Mo2 O8 74.31(9) 2_466 2_466 ?
O7 Mo2 O8 87.15(8) . 2_466 ?
O8 Mo2 O8 73.10(9) . 2_466 ?
O9 Mo3 O10 103.62(13) . . ?
O9 Mo3 O8 104.79(11) . . ?
O10 Mo3 O8 103.59(11) . . ?
O9 Mo3 O6 102.27(11) . . ?
O10 Mo3 O6 102.27(11) . . ?
O8 Mo3 O6 136.54(10) . . ?
O9 Mo3 O3 89.83(11) . . ?
O10 Mo3 O3 166.37(11) . . ?
O8 Mo3 O3 74.48(9) . . ?
O6 Mo3 O3 72.23(8) . . ?
O9 Mo3 O7 168.32(11) . . ?
O10 Mo3 O7 88.01(11) . . ?
O8 Mo3 O7 72.99(9) . . ?
O6 Mo3 O7 73.65(8) . . ?
O3 Mo3 O7 78.50(9) . . ?
O2 Cu1 N3 166.18(11) 2_466 . ?
O2 Cu1 N2 97.18(12) 2_466 . ?
N3 Cu1 N2 79.07(13) . . ?
O2 Cu1 N1 102.00(12) 2_466 . ?
N3 Cu1 N1 78.99(12) . . ?
N2 Cu1 N1 156.27(12) . . ?
O2 Cu1 O1 92.99(10) 2_466 . ?
N3 Cu1 O1 100.83(11) . . ?
N2 Cu1 O1 105.69(11) . . ?
N1 Cu1 O1 87.25(11) . . ?
Mo2 O1 Cu1 128.56(13) . . ?
Mo1 O2 Cu1 147.75(14) . 2_466 ?
Mo2 O3 Mo1 154.23(13) 2_466 . ?
Mo2 O3 Mo3 104.09(10) 2_466 . ?
Mo1 O3 Mo3 100.75(9) . . ?
Mo3 O6 Mo1 107.56(10) . . ?
Mo3 O6 Mo1 103.07(9) . 2_566 ?
Mo1 O6 Mo1 105.97(9) . 2_566 ?
Mo1 O7 Mo2 152.64(13) 2_566 . ?
Mo1 O7 Mo3 105.92(10) 2_566 . ?
Mo2 O7 Mo3 101.41(9) . . ?
Mo3 O8 Mo2 108.12(10) . . ?
Mo3 O8 Mo2 102.92(10) . 2_466 ?
Mo2 O8 Mo2 106.90(9) . 2_466 ?
N1 C1 C2 111.1(3) . . ?
C3 C2 C1 105.8(3) . . ?
N5 C3 C2 107.1(3) . . ?
N3 C4 C5 121.7(3) . . ?
N3 C4 N5 111.5(3) . . ?
C5 C4 N5 126.8(3) . . ?
C4 C5 C6 116.5(4) . . ?
C7 C6 C5 121.8(3) . . ?
C6 C7 C8 117.2(4) . . ?
N3 C8 C7 121.5(3) . . ?
N3 C8 N4 111.6(3) . . ?
C7 C8 N4 126.8(3) . . ?
C10 C9 N4 107.5(3) . . ?
C9 C10 C11 106.1(3) . . ?
N2 C11 C10 110.4(3) . . ?
C1 N1 N5 105.2(3) . . ?
C1 N1 Cu1 142.2(3) . . ?
N5 N1 Cu1 112.2(2) . . ?
C11 N2 N4 105.8(3) . . ?
C11 N2 Cu1 141.3(3) . . ?
N4 N2 Cu1 112.9(2) . . ?
C8 N3 C4 121.2(3) . . ?
C8 N3 Cu1 119.0(2) . . ?
C4 N3 Cu1 119.8(2) . . ?
C9 N4 N2 110.3(3) . . ?
C9 N4 C8 132.7(3) . . ?
N2 N4 C8 116.8(3) . . ?
C3 N5 N1 110.7(3) . . ?
C3 N5 C4 132.0(3) . . ?
N1 N5 C4 117.4(3) . . ?

_refine_diff_density_max         1.178
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.135

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1951002'
loop_
_audit_author_name
_audit_author_address
'Frank Allen'
;Tonghua normal university
China
;
_audit_update_record             
;
2019-09-03 deposited with the CCDC.	2019-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H9 Cu Mo4 N5 O14'
_chemical_formula_sum            'C11 H9 Cu Mo4 N5 O14'
_chemical_formula_weight         882.53

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   9.638(5)
_cell_length_b                   14.761(5)
_cell_length_c                   15.417(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.889(5)
_cell_angle_gamma                90
_cell_volume                     2119.7(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    21593
_cell_measurement_theta_min      3.031
_cell_measurement_theta_max      24.999

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.765
_exptl_crystal_F_000             1676
_exptl_transmission_factor_min   0.450
_exptl_transmission_factor_max   0.714
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.371
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21593
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.031
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             3696
_reflns_number_gt                2873
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the non-H atoms Mo, Cu, C, N and O were 
refined anisotropically. Since most O atoms on the polyanion and lattice water 
molecules as well as some C atoms exhibit obvious ADP and NPD problems with 
the anisotropic parameters, they are just refined isotropically.
But this treatment didn't influence the precise of the 
polyanion structure and the final R values.
The 'omit -3 50' command was used to omit the weak reflections above 50
degree.
The restraint command 'isor' was employed to restrain several C and O 
N atoms so as to avoid the ADP and NPD problems on them. This command
led to a restraint number 24.
;

_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0341P)²+110.0000P] 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         3696
_refine_ls_number_parameters     316
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0710
_refine_ls_wR_factor_ref         0.1652
_refine_ls_wR_factor_gt          0.1537
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.076
_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 0.34759(12) 0.48356(8) 1.04233(7) 0.0155(3) Uani 1 1 d . . . . .
Mo2 Mo 0.44290(13) 0.68563(8) 0.95253(7) 0.0181(3) Uani 1 1 d . . . . .
Mo3 Mo 0.17550(12) 0.56513(8) 0.83187(7) 0.0186(3) Uani 1 1 d . . . . .
Mo4 Mo 0.39303(13) 0.39451(8) 0.84050(7) 0.0186(3) Uani 1 1 d . . . . .
Cu1 Cu 0.29841(19) 0.64080(12) 0.61024(11) 0.0242(4) Uani 1 1 d . . . . .
O1 O 0.2168(11) 0.5908(7) 0.7328(7) 0.030(2) Uani 1 1 d . . . . .
O1W O 0.4917(10) 0.6174(7) 0.6845(6) 0.027(2) Uani 1 1 d . . . . .
O2 O 0.4381(11) 0.7828(7) 1.0123(7) 0.030(2) Uani 1 1 d . . . . .
O3 O 0.3684(11) 0.2821(7) 0.8161(7) 0.031(3) Uani 1 1 d . . . . .
O4 O 0.5041(11) 0.7179(7) 0.8640(7) 0.029(2) Uani 1 1 d . . . . .
O5 O 0.3136(10) 0.4422(7) 1.1364(6) 0.024(2) Uani 1 1 d . . . . .
O6 O 0.3703(9) 0.3696(6) 0.9826(6) 0.017(2) Uani 1 1 d . . . . .
O7 O 0.5739(10) 0.4650(6) 1.0815(6) 0.021(2) Uani 1 1 d . . . . .
O8 O -0.0071(10) 0.5737(7) 0.8077(7) 0.029(2) Uani 1 1 d . . . . .
O9 O 0.1794(10) 0.5126(7) 0.9715(6) 0.023(2) Uani 1 1 d . . . . .
O10 O 0.4095(9) 0.6063(6) 1.0764(6) 0.018(2) Uani 1 1 d . U . . .
O11 O 0.4404(11) 0.4417(7) 0.7509(6) 0.029(2) Uani 1 1 d . . . . .
O12 O 0.2033(9) 0.4363(6) 0.8221(6) 0.0169(19) Uani 1 1 d . U . . .
O13 O 0.2418(10) 0.6709(6) 0.9019(6) 0.022(2) Uani 1 1 d . . . . .
C1 C 0.2779(17) 0.8200(10) 0.7196(9) 0.028(3) Uani 1 1 d . . . . .
H1A H 0.3560 0.8139 0.7692 0.033 Uiso 1 1 calc R U . . .
C2 C 0.1818(16) 0.8918(11) 0.7066(10) 0.030(4) Uani 1 1 d . . . . .
H2A H 0.1833 0.9409 0.7446 0.035 Uiso 1 1 calc R U . . .
C3 C 0.0853(18) 0.8758(11) 0.6272(10) 0.033(4) Uani 1 1 d . . . . .
H3A H 0.0079 0.9123 0.5996 0.039 Uiso 1 1 calc R U . . .
C4 C 0.0599(15) 0.7463(10) 0.5191(9) 0.022(3) Uani 1 1 d . U . . .
C5 C -0.0587(17) 0.7714(12) 0.4510(11) 0.036(4) Uani 1 1 d . U . . .
H5A H -0.1031 0.8272 0.4514 0.043 Uiso 1 1 calc R U . . .
C6 C -0.1075(18) 0.7104(14) 0.3834(12) 0.046(5) Uani 1 1 d . . . . .
H6A H -0.1888 0.7245 0.3381 0.056 Uiso 1 1 calc R U . . .
C7 C -0.0402(19) 0.6287(12) 0.3800(12) 0.042(4) Uani 1 1 d . . . . .
H7A H -0.0722 0.5885 0.3326 0.050 Uiso 1 1 calc R U . . .
C8 C 0.0770(17) 0.6092(11) 0.4503(9) 0.030(4) Uani 1 1 d . . . . .
C9 C 0.1523(17) 0.4551(11) 0.4108(10) 0.034(4) Uani 1 1 d . . . . .
H9A H 0.0827 0.4428 0.3580 0.041 Uiso 1 1 calc R U . . .
C10 C 0.2619(19) 0.4010(12) 0.4506(11) 0.040(4) Uani 1 1 d . . . . .
H10A H 0.2824 0.3441 0.4312 0.048 Uiso 1 1 calc R U . . .
C11 C 0.3398(17) 0.4474(11) 0.5275(11) 0.034(4) Uani 1 1 d . . . . .
H11A H 0.4224 0.4255 0.5674 0.041 Uiso 1 1 calc R U . . .
N1 N 0.1226(12) 0.6673(8) 0.5182(8) 0.023(3) Uani 1 1 d . . . . .
N2 N 0.2789(12) 0.5268(9) 0.5351(8) 0.025(3) Uani 1 1 d . . . . .
N3 N 0.2444(13) 0.7608(8) 0.6521(8) 0.024(3) Uani 1 1 d . . . . .
N4 N 0.1614(13) 0.5312(9) 0.4615(8) 0.029(3) Uani 1 1 d . . . . .
N5 N 0.1231(13) 0.7969(9) 0.5959(8) 0.027(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O5 1.681(9) . ?
Mo1 O9 1.759(9) . ?
Mo1 O10 1.937(9) . ?
Mo1 O6 1.957(9) . ?
Mo1 O7 2.127(9) . ?
Mo1 O7 2.353(9) 3_667 ?
Mo1 Mo2 3.200(2) 3_667 ?
Mo2 O4 1.689(10) . ?
Mo2 O2 1.712(10) . ?
Mo2 O13 1.907(9) . ?
Mo2 O6 1.995(9) 3_667 ?
Mo2 O7 2.280(10) 3_667 ?
Mo2 O10 2.332(9) . ?
Mo2 Mo1 3.200(2) 3_667 ?
Mo3 O8 1.707(10) . ?
Mo3 O1 1.717(10) . ?
Mo3 O13 1.912(9) . ?
Mo3 O12 1.932(9) . ?
Mo3 O9 2.279(9) . ?
Mo3 O7 2.481(9) 3_667 ?
Mo4 O3 1.705(11) . ?
Mo4 O11 1.711(10) . ?
Mo4 O12 1.881(9) . ?
Mo4 O10 2.003(9) 3_667 ?
Mo4 O6 2.287(9) . ?
Mo4 O7 2.377(10) 3_667 ?
Cu1 O1W 1.950(10) . ?
Cu1 N1 1.950(11) . ?
Cu1 N3 2.000(12) . ?
Cu1 N2 2.024(13) . ?
Cu1 O1 2.345(10) . ?
O6 Mo2 1.995(9) 3_667 ?
O7 Mo2 2.280(10) 3_667 ?
O7 Mo1 2.353(9) 3_667 ?
O7 Mo4 2.377(10) 3_667 ?
O7 Mo3 2.481(9) 3_667 ?
O10 Mo4 2.003(9) 3_667 ?
C1 N3 1.332(19) . ?
C1 C2 1.39(2) . ?
C2 C3 1.35(2) . ?
C3 N5 1.35(2) . ?
C4 N1 1.315(19) . ?
C4 C5 1.39(2) . ?
C4 N5 1.399(19) . ?
C5 C6 1.37(2) . ?
C6 C7 1.38(3) . ?
C7 C8 1.38(2) . ?
C8 N1 1.337(19) . ?
C8 N4 1.39(2) . ?
C9 C10 1.34(2) . ?
C9 N4 1.36(2) . ?
C10 C11 1.41(2) . ?
C11 N2 1.33(2) . ?
N2 N4 1.383(15) . ?
N3 N5 1.372(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Mo1 O9 105.7(5) . . ?
O5 Mo1 O10 102.7(4) . . ?
O9 Mo1 O10 96.3(4) . . ?
O5 Mo1 O6 99.4(4) . . ?
O9 Mo1 O6 96.6(4) . . ?
O10 Mo1 O6 150.2(4) . . ?
O5 Mo1 O7 97.0(4) . . ?
O9 Mo1 O7 157.3(4) . . ?
O10 Mo1 O7 79.7(4) . . ?
O6 Mo1 O7 78.0(4) . . ?
O5 Mo1 O7 172.5(4) . 3_667 ?
O9 Mo1 O7 81.6(4) . 3_667 ?
O10 Mo1 O7 77.1(4) . 3_667 ?
O6 Mo1 O7 78.3(3) . 3_667 ?
O7 Mo1 O7 75.6(4) . 3_667 ?
O5 Mo1 Mo2 87.5(3) . 3_667 ?
O9 Mo1 Mo2 132.9(3) . 3_667 ?
O10 Mo1 Mo2 125.1(3) . 3_667 ?
O6 Mo1 Mo2 36.3(3) . 3_667 ?
O7 Mo1 Mo2 45.4(3) . 3_667 ?
O7 Mo1 Mo2 86.5(2) 3_667 3_667 ?
O4 Mo2 O2 105.2(5) . . ?
O4 Mo2 O13 103.4(5) . . ?
O2 Mo2 O13 98.7(5) . . ?
O4 Mo2 O6 93.6(4) . 3_667 ?
O2 Mo2 O6 102.6(4) . 3_667 ?
O13 Mo2 O6 148.2(4) . 3_667 ?
O4 Mo2 O7 96.2(4) . 3_667 ?
O2 Mo2 O7 158.5(4) . 3_667 ?
O13 Mo2 O7 77.9(4) . 3_667 ?
O6 Mo2 O7 73.7(3) 3_667 3_667 ?
O4 Mo2 O10 162.6(4) . . ?
O2 Mo2 O10 87.2(4) . . ?
O13 Mo2 O10 86.4(4) . . ?
O6 Mo2 O10 71.4(3) 3_667 . ?
O7 Mo2 O10 71.5(3) 3_667 . ?
O4 Mo2 Mo1 83.7(4) . 3_667 ?
O2 Mo2 Mo1 138.1(3) . 3_667 ?
O13 Mo2 Mo1 119.3(3) . 3_667 ?
O6 Mo2 Mo1 35.5(3) 3_667 3_667 ?
O7 Mo2 Mo1 41.6(2) 3_667 3_667 ?
O10 Mo2 Mo1 78.9(2) . 3_667 ?
O8 Mo3 O1 104.6(5) . . ?
O8 Mo3 O13 103.8(5) . . ?
O1 Mo3 O13 101.7(5) . . ?
O8 Mo3 O12 102.2(5) . . ?
O1 Mo3 O12 94.5(4) . . ?
O13 Mo3 O12 144.6(4) . . ?
O8 Mo3 O9 89.8(4) . . ?
O1 Mo3 O9 164.6(4) . . ?
O13 Mo3 O9 79.8(4) . . ?
O12 Mo3 O9 76.7(4) . . ?
O8 Mo3 O7 159.5(4) . 3_667 ?
O1 Mo3 O7 95.9(4) . 3_667 ?
O13 Mo3 O7 72.8(4) . 3_667 ?
O12 Mo3 O7 74.4(3) . 3_667 ?
O9 Mo3 O7 69.7(3) . 3_667 ?
O3 Mo4 O11 105.6(5) . . ?
O3 Mo4 O12 102.2(4) . . ?
O11 Mo4 O12 101.3(4) . . ?
O3 Mo4 O10 101.0(4) . 3_667 ?
O11 Mo4 O10 96.5(4) . 3_667 ?
O12 Mo4 O10 145.7(4) . 3_667 ?
O3 Mo4 O6 90.7(4) . . ?
O11 Mo4 O6 161.9(4) . . ?
O12 Mo4 O6 82.4(3) . . ?
O10 Mo4 O6 72.3(3) 3_667 . ?
O3 Mo4 O7 162.5(4) . 3_667 ?
O11 Mo4 O7 91.4(4) . 3_667 ?
O12 Mo4 O7 77.8(4) . 3_667 ?
O10 Mo4 O7 72.5(3) 3_667 3_667 ?
O6 Mo4 O7 71.9(3) . 3_667 ?
O1W Cu1 N1 169.4(5) . . ?
O1W Cu1 N3 104.8(5) . . ?
N1 Cu1 N3 78.9(5) . . ?
O1W Cu1 N2 97.1(4) . . ?
N1 Cu1 N2 79.3(5) . . ?
N3 Cu1 N2 158.1(5) . . ?
O1W Cu1 O1 86.5(4) . . ?
N1 Cu1 O1 103.9(4) . . ?
N3 Cu1 O1 81.4(4) . . ?
N2 Cu1 O1 101.4(4) . . ?
Mo3 O1 Cu1 171.5(6) . . ?
Mo1 O6 Mo2 108.1(4) . 3_667 ?
Mo1 O6 Mo4 111.2(4) . . ?
Mo2 O6 Mo4 104.4(4) 3_667 . ?
Mo1 O7 Mo2 93.1(4) . 3_667 ?
Mo1 O7 Mo1 104.4(4) . 3_667 ?
Mo2 O7 Mo1 98.4(3) 3_667 3_667 ?
Mo1 O7 Mo4 91.5(3) . 3_667 ?
Mo2 O7 Mo4 163.6(4) 3_667 3_667 ?
Mo1 O7 Mo4 95.7(3) 3_667 3_667 ?
Mo1 O7 Mo3 164.1(4) . 3_667 ?
Mo2 O7 Mo3 87.2(3) 3_667 3_667 ?
Mo1 O7 Mo3 91.3(3) 3_667 3_667 ?
Mo4 O7 Mo3 84.2(3) 3_667 3_667 ?
Mo1 O9 Mo3 117.3(5) . . ?
Mo1 O10 Mo4 110.1(4) . 3_667 ?
Mo1 O10 Mo2 110.2(4) . . ?
Mo4 O10 Mo2 102.6(4) 3_667 . ?
Mo4 O12 Mo3 117.4(5) . . ?
Mo2 O13 Mo3 118.8(5) . . ?
N3 C1 C2 111.7(13) . . ?
C3 C2 C1 106.0(14) . . ?
N5 C3 C2 106.8(14) . . ?
N1 C4 C5 121.2(14) . . ?
N1 C4 N5 112.4(12) . . ?
C5 C4 N5 126.3(14) . . ?
C6 C5 C4 117.2(16) . . ?
C5 C6 C7 122.2(15) . . ?
C6 C7 C8 116.8(16) . . ?
N1 C8 C7 121.3(15) . . ?
N1 C8 N4 111.7(12) . . ?
C7 C8 N4 127.0(15) . . ?
C10 C9 N4 107.6(14) . . ?
C9 C10 C11 106.5(15) . . ?
N2 C11 C10 110.5(14) . . ?
C4 N1 C8 121.2(13) . . ?
C4 N1 Cu1 119.0(10) . . ?
C8 N1 Cu1 119.3(10) . . ?
C11 N2 N4 104.8(12) . . ?
C11 N2 Cu1 143.6(10) . . ?
N4 N2 Cu1 111.6(9) . . ?
C1 N3 N5 103.6(12) . . ?
C1 N3 Cu1 143.3(10) . . ?
N5 N3 Cu1 112.9(9) . . ?
C9 N4 N2 110.6(12) . . ?
C9 N4 C8 131.5(12) . . ?
N2 N4 C8 117.9(12) . . ?
C3 N5 N3 112.0(12) . . ?
C3 N5 C4 131.8(13) . . ?
N3 N5 C4 116.3(12) . . ?

_refine_diff_density_max         1.433
_refine_diff_density_min         -2.220
_refine_diff_density_rms         0.272

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1951001'
loop_
_audit_author_name
_audit_author_address
'Frank Allen'
;Tong hua normal university
China
;
_audit_update_record             
;
2019-09-22 deposited with the CCDC.	2019-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H22.50 Cu2 Mo8 N6 O26.25'
_chemical_formula_sum            'C30 H22.50 Cu2 Mo8 N6 O26.25'
_chemical_formula_weight         1781.64

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.531(5)
_cell_length_b                   13.190(5)
_cell_length_c                   13.589(5)
_cell_angle_alpha                77.378(5)
_cell_angle_beta                 89.683(5)
_cell_angle_gamma                89.474(5)
_cell_volume                     2191.7(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17905
_cell_measurement_theta_min      2.923
_cell_measurement_theta_max      28.250

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.700
_exptl_crystal_F_000             1697
_exptl_transmission_factor_min   0.391
_exptl_transmission_factor_max   0.594
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    3.257
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14155
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.923
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             7632
_reflns_number_gt                6198
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
During the refinement, the non-H atoms Mo, Cu, C, N and O were 
refined anisotropically.O1W has been assigned 0.25 occupancies 
to improve the data.
The 'omit -3 50' command was used to omit the weak reflections above 50
degree.
The restraint command 'isor' was employed to restrain O1W atom so as to avoid the ADP and NPD problems on them. This command
led to a restraint number 6.
;

_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0483P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00077(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7632
_refine_ls_number_parameters     659
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.004
_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 -0.43564(4) 0.13409(4) 0.81614(4) 0.01691(13) Uani 1 1 d . . . . .
Mo2 Mo -0.46958(4) 0.10709(4) 1.05423(4) 0.01473(13) Uani 1 1 d . . . . .
Mo3 Mo -0.73023(4) 0.06552(4) 1.13844(4) 0.02068(13) Uani 1 1 d . . . . .
Mo4 Mo -0.69128(4) 0.08964(4) 0.89743(4) 0.02028(13) Uani 1 1 d . . . . .
Mo5 Mo -0.26251(4) 0.42013(4) 0.59308(4) 0.01915(13) Uani 1 1 d . . . . .
Mo6 Mo -0.09260(4) 0.35619(4) 0.38705(4) 0.01885(13) Uani 1 1 d . . . . .
Mo7 Mo -0.09860(4) 0.58460(4) 0.44920(4) 0.01928(13) Uani 1 1 d . . . . .
Mo8 Mo -0.13918(4) 0.56564(4) 0.71581(4) 0.01943(13) Uani 1 1 d . . . . .
Cu1 Cu -0.26485(6) 0.15860(6) 0.56316(6) 0.02321(18) Uani 1 1 d . . . . .
Cu2 Cu -0.30715(5) 0.34750(6) 0.88336(6) 0.02208(18) Uani 1 1 d . . . . .
O1 O -0.2706(3) 0.2856(3) 0.6105(3) 0.0264(10) Uani 1 1 d . . . . .
O2 O -0.1510(4) 0.2385(3) 0.4287(3) 0.0317(10) Uani 1 1 d . . . . .
O3 O -0.3416(3) 0.2259(3) 0.8324(3) 0.0219(9) Uani 1 1 d . . . . .
O4 O -0.2233(3) 0.4323(3) 0.7197(3) 0.0255(9) Uani 1 1 d . . . . .
O5 O -0.7777(4) 0.1434(4) 1.2123(3) 0.0328(11) Uani 1 1 d . . . . .
O6 O -0.8332(3) -0.0132(4) 1.1287(3) 0.0330(11) Uani 1 1 d . . . . .
O7 O -0.7376(3) 0.1497(3) 1.0051(3) 0.0225(9) Uani 1 1 d . . . . .
O8 O -0.7854(3) -0.0011(3) 0.8959(3) 0.0322(11) Uani 1 1 d . . . . .
O9 O -0.7180(4) 0.1866(4) 0.7970(3) 0.0342(11) Uani 1 1 d . . . . .
O10 O -0.5695(3) 0.0159(3) 0.8436(3) 0.0183(8) Uani 1 1 d . . . . .
O11 O -0.5314(3) 0.1684(3) 0.9233(3) 0.0158(8) Uani 1 1 d . . . . .
O12 O -0.3966(3) 0.0160(3) 0.9624(3) 0.0175(8) Uani 1 1 d . . . . .
O13 O -0.5012(3) 0.1929(3) 0.7111(3) 0.0278(10) Uani 1 1 d . . . . .
O14 O -0.5713(3) 0.1472(3) 1.1262(3) 0.0197(8) Uani 1 1 d . . . . .
O15 O -0.3701(3) 0.1922(3) 1.0580(3) 0.0249(9) Uani 1 1 d . . . . .
O16 O -0.1543(3) 0.4066(4) 0.2778(3) 0.0322(11) Uani 1 1 d . . . . .
O17 O -0.1782(3) 0.4335(3) 0.4728(3) 0.0243(9) Uani 1 1 d . . . . .
O18 O -0.0042(3) 0.4984(3) 0.3966(3) 0.0221(9) Uani 1 1 d . . . . .
O19 O -0.1769(4) 0.6409(4) 0.3528(3) 0.0354(11) Uani 1 1 d . . . . .
O20 O -0.0113(3) 0.6815(3) 0.4667(3) 0.0247(9) Uani 1 1 d . . . . .
O21 O -0.1920(3) 0.5732(3) 0.5666(3) 0.0207(9) Uani 1 1 d . . . . .
O22 O -0.3881(3) 0.4641(4) 0.5684(4) 0.0353(11) Uani 1 1 d . . . . .
O23 O -0.0426(3) 0.6753(3) 0.6624(3) 0.0225(9) Uani 1 1 d . . . . .
O24 O -0.6439(3) -0.0368(3) 1.2340(3) 0.0232(9) Uani 1 1 d . . . . .
O25 O -0.0668(3) 0.5034(4) 0.8162(3) 0.0306(10) Uani 1 1 d . . . . .
O26 O -0.2358(4) 0.6320(4) 0.7621(4) 0.0380(12) Uani 1 1 d . . . . .
C1 C -0.0661(5) 0.1339(6) 0.6893(5) 0.0351(16) Uani 1 1 d . . . . .
H1A H -0.0832 0.1981 0.7032 0.042 Uiso 1 1 calc R U . . .
C2 C 0.0264(6) 0.0837(6) 0.7292(5) 0.0406(18) Uani 1 1 d . . . . .
H2A H 0.0726 0.1147 0.7670 0.049 Uiso 1 1 calc R U . . .
C3 C 0.0482(6) -0.0126(7) 0.7117(6) 0.0446(19) Uani 1 1 d . . . . .
H3A H 0.1088 -0.0488 0.7396 0.054 Uiso 1 1 calc R U . . .
C4 C -0.0192(6) -0.0566(6) 0.6526(6) 0.0403(18) Uani 1 1 d . . . . .
H4A H -0.0050 -0.1223 0.6410 0.048 Uiso 1 1 calc R U . . .
C5 C -0.1084(5) -0.0004(5) 0.6112(5) 0.0270(14) Uani 1 1 d . . . . .
C6 C -0.1847(5) -0.0345(5) 0.5432(5) 0.0242(13) Uani 1 1 d . . . . .
C7 C -0.1765(6) -0.1223(5) 0.5045(5) 0.0353(16) Uani 1 1 d . . . . .
H7A H -0.1222 -0.1707 0.5247 0.042 Uiso 1 1 calc R U . . .
C8 C -0.2529(6) -0.1365(5) 0.4336(5) 0.0383(17) Uani 1 1 d . . . . .
H8A H -0.2496 -0.1952 0.4062 0.046 Uiso 1 1 calc R U . . .
C9 C -0.3326(6) -0.0636(5) 0.4044(5) 0.0322(15) Uani 1 1 d . . . . .
H9A H -0.3820 -0.0716 0.3559 0.039 Uiso 1 1 calc R U . . .
C10 C -0.3377(5) 0.0201(5) 0.4476(5) 0.0267(14) Uani 1 1 d . . . . .
C11 C -0.4174(5) 0.1061(5) 0.4282(4) 0.0215(12) Uani 1 1 d . . . . .
C12 C -0.5023(5) 0.1141(5) 0.3629(5) 0.0327(15) Uani 1 1 d . . . . .
H12A H -0.5128 0.0633 0.3261 0.039 Uiso 1 1 calc R U . . .
C13 C -0.5718(5) 0.1979(5) 0.3522(5) 0.0345(16) Uani 1 1 d . . . . .
H13A H -0.6282 0.2049 0.3069 0.041 Uiso 1 1 calc R U . . .
C14 C -0.5567(5) 0.2698(5) 0.4086(5) 0.0333(16) Uani 1 1 d . . . . .
H14A H -0.6042 0.3252 0.4042 0.040 Uiso 1 1 calc R U . . .
C15 C -0.4692(5) 0.2597(5) 0.4734(5) 0.0295(15) Uani 1 1 d . . . . .
H15A H -0.4581 0.3100 0.5107 0.035 Uiso 1 1 calc R U . . .
C16 C -0.1188(5) 0.2073(5) 0.9510(6) 0.0346(17) Uani 1 1 d . . . . .
H16A H -0.1454 0.1653 0.9102 0.042 Uiso 1 1 calc R U . . .
C17 C -0.0279(6) 0.1762(6) 1.0063(6) 0.044(2) Uani 1 1 d . . . . .
H17A H 0.0083 0.1158 1.0011 0.053 Uiso 1 1 calc R U . . .
C18 C 0.0076(6) 0.2366(6) 1.0692(6) 0.045(2) Uani 1 1 d . . . . .
H18A H 0.0671 0.2159 1.1095 0.054 Uiso 1 1 calc R U . . .
C19 C -0.0446(5) 0.3279(6) 1.0728(5) 0.0342(16) Uani 1 1 d . . . . .
H19A H -0.0200 0.3702 1.1142 0.041 Uiso 1 1 calc R U . . .
C20 C -0.1343(5) 0.3559(5) 1.0138(4) 0.0211(12) Uani 1 1 d . . . . .
C21 C -0.1970(5) 0.4509(5) 1.0130(4) 0.0232(13) Uani 1 1 d . . . . .
C22 C -0.1746(5) 0.5289(5) 1.0612(5) 0.0273(14) Uani 1 1 d . . . . .
H22A H -0.1133 0.5266 1.0998 0.033 Uiso 1 1 calc R U . . .
C23 C -0.2461(5) 0.6122(5) 1.0509(5) 0.0328(16) Uani 1 1 d . . . . .
H23A H -0.2335 0.6653 1.0843 0.039 Uiso 1 1 calc R U . . .
C24 C -0.3350(5) 0.6158(5) 0.9916(5) 0.0306(15) Uani 1 1 d . . . . .
H24A H -0.3828 0.6713 0.9843 0.037 Uiso 1 1 calc R U . . .
C25 C -0.3524(5) 0.5361(5) 0.9432(4) 0.0229(13) Uani 1 1 d . . . . .
C26 C -0.4416(5) 0.5266(5) 0.8742(5) 0.0234(13) Uani 1 1 d . . . . .
C27 C -0.5207(5) 0.6005(5) 0.8465(5) 0.0320(15) Uani 1 1 d . . . . .
H27A H -0.5210 0.6611 0.8709 0.038 Uiso 1 1 calc R U . . .
C28 C -0.5989(6) 0.5829(6) 0.7821(6) 0.0395(17) Uani 1 1 d . . . . .
H28A H -0.6531 0.6318 0.7629 0.047 Uiso 1 1 calc R U . . .
C29 C -0.5979(5) 0.4946(6) 0.7463(5) 0.0365(17) Uani 1 1 d . . . . .
H29A H -0.6510 0.4823 0.7029 0.044 Uiso 1 1 calc R U . . .
C30 C -0.5157(5) 0.4228(5) 0.7761(5) 0.0309(15) Uani 1 1 d . . . . .
H30A H -0.5141 0.3626 0.7510 0.037 Uiso 1 1 calc R U . . .
N1 N -0.2635(4) 0.0326(4) 0.5151(4) 0.0228(11) Uani 1 1 d . . . . .
N2 N -0.4014(4) 0.1800(4) 0.4831(4) 0.0230(11) Uani 1 1 d . . . . .
N3 N -0.1319(4) 0.0932(4) 0.6314(4) 0.0245(11) Uani 1 1 d . . . . .
N4 N -0.1703(4) 0.2962(4) 0.9539(4) 0.0231(11) Uani 1 1 d . . . . .
N5 N -0.2851(4) 0.4554(4) 0.9557(4) 0.0202(10) Uani 1 1 d . . . . .
N6 N -0.4390(4) 0.4375(4) 0.8394(4) 0.0247(11) Uani 1 1 d . . . . .
O1W O 0.2560(18) -0.1864(17) 0.7523(17) 0.054(6) Uani 0.25 1 d . 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
Mo1 O13 1.683(4) . ?
Mo1 O3 1.747(4) . ?
Mo1 O24 1.859(4) 2_457 ?
Mo1 O11 2.006(4) . ?
Mo1 O10 2.274(4) . ?
Mo1 O12 2.293(4) . ?
Mo1 Mo2 3.2030(14) . ?
Mo2 O15 1.694(4) . ?
Mo2 O14 1.750(4) . ?
Mo2 O11 1.947(4) . ?
Mo2 O10 1.951(4) 2_457 ?
Mo2 O12 2.112(4) . ?
Mo2 O12 2.390(4) 2_457 ?
Mo3 O5 1.688(4) . ?
Mo3 O6 1.688(4) . ?
Mo3 O7 1.909(4) . ?
Mo3 O24 1.975(4) . ?
Mo3 O14 2.261(4) . ?
Mo3 O12 2.479(4) 2_457 ?
Mo4 O9 1.686(4) . ?
Mo4 O8 1.691(4) . ?
Mo4 O7 1.896(4) . ?
Mo4 O10 2.020(4) . ?
Mo4 O11 2.329(4) . ?
Mo4 O12 2.370(4) 2_457 ?
Mo5 O22 1.682(4) . ?
Mo5 O1 1.742(4) . ?
Mo5 O4 1.833(4) . ?
Mo5 O17 1.918(4) . ?
Mo5 O21 2.168(4) . ?
Mo5 Mo8 3.2149(10) . ?
Mo6 O16 1.678(4) . ?
Mo6 O2 1.702(4) . ?
Mo6 O23 1.895(4) 2_566 ?
Mo6 O17 2.008(4) . ?
Mo6 O18 2.216(4) . ?
Mo6 O20 2.340(4) 2_566 ?
Mo7 O19 1.675(4) . ?
Mo7 O20 1.746(4) . ?
Mo7 O18 1.877(4) . ?
Mo7 O21 1.954(4) . ?
Mo7 O17 2.196(4) . ?
Mo7 O18 2.501(4) 2_566 ?
Mo8 O26 1.686(5) . ?
Mo8 O25 1.694(4) . ?
Mo8 O23 1.910(4) . ?
Mo8 O4 2.049(4) . ?
Mo8 O21 2.117(4) . ?
Cu1 N1 1.914(5) . ?
Cu1 O1 1.922(4) . ?
Cu1 N3 2.006(5) . ?
Cu1 N2 2.017(5) . ?
Cu1 O2 2.375(4) . ?
Cu2 N5 1.920(5) . ?
Cu2 O3 1.934(4) . ?
Cu2 N4 2.008(5) . ?
Cu2 N6 2.039(5) . ?
O10 Mo2 1.951(4) 2_457 ?
O12 Mo4 2.370(4) 2_457 ?
O12 Mo2 2.390(4) 2_457 ?
O12 Mo3 2.479(4) 2_457 ?
O18 Mo7 2.501(4) 2_566 ?
O20 Mo6 2.340(4) 2_566 ?
O23 Mo6 1.895(4) 2_566 ?
O24 Mo1 1.859(4) 2_457 ?
C1 N3 1.337(8) . ?
C1 C2 1.383(10) . ?
C2 C3 1.368(11) . ?
C3 C4 1.383(10) . ?
C4 C5 1.388(9) . ?
C5 N3 1.351(8) . ?
C5 C6 1.472(8) . ?
C6 N1 1.321(8) . ?
C6 C7 1.376(9) . ?
C7 C8 1.404(10) . ?
C8 C9 1.377(10) . ?
C9 C10 1.360(9) . ?
C10 N1 1.346(7) . ?
C10 C11 1.485(9) . ?
C11 N2 1.368(7) . ?
C11 C12 1.377(8) . ?
C12 C13 1.384(9) . ?
C13 C14 1.359(9) . ?
C14 C15 1.397(9) . ?
C15 N2 1.330(8) . ?
C16 N4 1.341(8) . ?
C16 C17 1.378(9) . ?
C17 C18 1.367(10) . ?
C18 C19 1.376(10) . ?
C19 C20 1.384(8) . ?
C20 N4 1.332(7) . ?
C20 C21 1.470(8) . ?
C21 N5 1.349(7) . ?
C21 C22 1.367(8) . ?
C22 C23 1.393(9) . ?
C23 C24 1.373(9) . ?
C24 C25 1.376(9) . ?
C25 N5 1.334(7) . ?
C25 C26 1.486(8) . ?
C26 N6 1.360(8) . ?
C26 C27 1.378(9) . ?
C27 C28 1.372(9) . ?
C28 C29 1.356(10) . ?
C29 C30 1.394(9) . ?
C30 N6 1.336(8) . ?

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
O13 Mo1 O3 103.7(2) . . ?
O13 Mo1 O24 100.06(19) . 2_457 ?
O3 Mo1 O24 103.88(18) . 2_457 ?
O13 Mo1 O11 101.00(19) . . ?
O3 Mo1 O11 92.24(17) . . ?
O24 Mo1 O11 149.51(17) 2_457 . ?
O13 Mo1 O10 87.03(17) . . ?
O3 Mo1 O10 162.81(16) . . ?
O24 Mo1 O10 87.06(16) 2_457 . ?
O11 Mo1 O10 72.32(14) . . ?
O13 Mo1 O12 159.80(17) . . ?
O3 Mo1 O12 95.98(16) . . ?
O24 Mo1 O12 79.22(16) 2_457 . ?
O11 Mo1 O12 73.41(14) . . ?
O10 Mo1 O12 72.77(13) . . ?
O13 Mo1 Mo2 136.28(15) . . ?
O3 Mo1 Mo2 83.49(13) . . ?
O24 Mo1 Mo2 120.30(12) 2_457 . ?
O11 Mo1 Mo2 35.28(10) . . ?
O10 Mo1 Mo2 79.52(9) . . ?
O12 Mo1 Mo2 41.18(9) . . ?
O15 Mo2 O14 103.65(19) . . ?
O15 Mo2 O11 100.26(18) . . ?
O14 Mo2 O11 96.13(17) . . ?
O15 Mo2 O10 104.37(18) . 2_457 ?
O14 Mo2 O10 94.97(17) . 2_457 ?
O11 Mo2 O10 149.69(15) . 2_457 ?
O15 Mo2 O12 99.75(18) . . ?
O14 Mo2 O12 156.59(16) . . ?
O11 Mo2 O12 78.80(15) . . ?
O10 Mo2 O12 79.85(15) 2_457 . ?
O15 Mo2 O12 175.57(17) . 2_457 ?
O14 Mo2 O12 80.53(15) . 2_457 ?
O11 Mo2 O12 77.66(14) . 2_457 ?
O10 Mo2 O12 76.49(14) 2_457 2_457 ?
O12 Mo2 O12 76.06(16) . 2_457 ?
O15 Mo2 Mo1 90.42(14) . . ?
O14 Mo2 Mo1 132.61(12) . . ?
O11 Mo2 Mo1 36.51(11) . . ?
O10 Mo2 Mo1 125.36(11) 2_457 . ?
O12 Mo2 Mo1 45.63(10) . . ?
O12 Mo2 Mo1 85.61(9) 2_457 . ?
O5 Mo3 O6 104.3(2) . . ?
O5 Mo3 O7 104.2(2) . . ?
O6 Mo3 O7 97.4(2) . . ?
O5 Mo3 O24 102.3(2) . . ?
O6 Mo3 O24 97.4(2) . . ?
O7 Mo3 O24 145.32(17) . . ?
O5 Mo3 O14 90.32(18) . . ?
O6 Mo3 O14 165.42(19) . . ?
O7 Mo3 O14 78.69(15) . . ?
O24 Mo3 O14 79.15(15) . . ?
O5 Mo3 O12 160.05(18) . 2_457 ?
O6 Mo3 O12 95.58(18) . 2_457 ?
O7 Mo3 O12 74.86(14) . 2_457 ?
O24 Mo3 O12 72.62(15) . 2_457 ?
O14 Mo3 O12 69.85(13) . 2_457 ?
O9 Mo4 O8 105.4(2) . . ?
O9 Mo4 O7 101.3(2) . . ?
O8 Mo4 O7 102.5(2) . . ?
O9 Mo4 O10 101.2(2) . . ?
O8 Mo4 O10 97.14(19) . . ?
O7 Mo4 O10 144.89(16) . . ?
O9 Mo4 O11 90.43(19) . . ?
O8 Mo4 O11 161.99(17) . . ?
O7 Mo4 O11 82.28(15) . . ?
O10 Mo4 O11 70.90(14) . . ?
O9 Mo4 O12 161.77(19) . 2_457 ?
O8 Mo4 O12 92.47(18) . 2_457 ?
O7 Mo4 O12 77.82(15) . 2_457 ?
O10 Mo4 O12 72.48(14) . 2_457 ?
O11 Mo4 O12 71.37(13) . 2_457 ?
O22 Mo5 O1 105.1(2) . . ?
O22 Mo5 O4 110.2(2) . . ?
O1 Mo5 O4 100.72(19) . . ?
O22 Mo5 O17 112.2(2) . . ?
O1 Mo5 O17 93.08(18) . . ?
O4 Mo5 O17 129.75(18) . . ?
O22 Mo5 O21 94.95(19) . . ?
O1 Mo5 O21 159.16(18) . . ?
O4 Mo5 O21 76.85(16) . . ?
O17 Mo5 O21 73.91(16) . . ?
O22 Mo5 Mo8 109.93(16) . . ?
O1 Mo5 Mo8 131.91(14) . . ?
O4 Mo5 Mo8 36.33(13) . . ?
O17 Mo5 Mo8 102.74(12) . . ?
O21 Mo5 Mo8 40.79(10) . . ?
O16 Mo6 O2 104.4(2) . . ?
O16 Mo6 O23 100.0(2) . 2_566 ?
O2 Mo6 O23 104.6(2) . 2_566 ?
O16 Mo6 O17 96.7(2) . . ?
O2 Mo6 O17 96.82(19) . . ?
O23 Mo6 O17 148.47(16) 2_566 . ?
O16 Mo6 O18 96.30(19) . . ?
O2 Mo6 O18 157.57(18) . . ?
O23 Mo6 O18 79.78(16) 2_566 . ?
O17 Mo6 O18 71.92(16) . . ?
O16 Mo6 O20 168.33(19) . 2_566 ?
O2 Mo6 O20 87.25(18) . 2_566 ?
O23 Mo6 O20 77.35(16) 2_566 2_566 ?
O17 Mo6 O20 80.91(16) . 2_566 ?
O18 Mo6 O20 72.08(14) . 2_566 ?
O19 Mo7 O20 105.4(2) . . ?
O19 Mo7 O18 105.6(2) . . ?
O20 Mo7 O18 100.34(19) . . ?
O19 Mo7 O21 103.4(2) . . ?
O20 Mo7 O21 101.21(18) . . ?
O18 Mo7 O21 137.46(17) . . ?
O19 Mo7 O17 94.4(2) . . ?
O20 Mo7 O17 160.19(17) . . ?
O18 Mo7 O17 74.76(16) . . ?
O21 Mo7 O17 72.58(15) . . ?
O19 Mo7 O18 174.78(19) . 2_566 ?
O20 Mo7 O18 76.03(16) . 2_566 ?
O18 Mo7 O18 78.90(16) . 2_566 ?
O21 Mo7 O18 71.41(15) . 2_566 ?
O17 Mo7 O18 84.17(14) . 2_566 ?
O26 Mo8 O25 106.2(2) . . ?
O26 Mo8 O23 100.7(2) . . ?
O25 Mo8 O23 99.08(19) . . ?
O26 Mo8 O4 97.6(2) . . ?
O25 Mo8 O4 89.81(19) . . ?
O23 Mo8 O4 156.55(16) . . ?
O26 Mo8 O21 102.2(2) . . ?
O25 Mo8 O21 148.73(19) . . ?
O23 Mo8 O21 88.01(16) . . ?
O4 Mo8 O21 73.71(16) . . ?
O26 Mo8 Mo5 105.25(16) . . ?
O25 Mo8 Mo5 116.16(15) . . ?
O23 Mo8 Mo5 127.11(12) . . ?
O4 Mo8 Mo5 31.99(11) . . ?
O21 Mo8 Mo5 41.98(11) . . ?
N1 Cu1 O1 178.3(2) . . ?
N1 Cu1 N3 80.8(2) . . ?
O1 Cu1 N3 100.76(19) . . ?
N1 Cu1 N2 81.1(2) . . ?
O1 Cu1 N2 97.31(19) . . ?
N3 Cu1 N2 161.8(2) . . ?
N1 Cu1 O2 90.64(19) . . ?
O1 Cu1 O2 90.07(17) . . ?
N3 Cu1 O2 86.06(19) . . ?
N2 Cu1 O2 96.27(19) . . ?
N5 Cu2 O3 169.8(2) . . ?
N5 Cu2 N4 80.48(19) . . ?
O3 Cu2 N4 98.64(18) . . ?
N5 Cu2 N6 79.9(2) . . ?
O3 Cu2 N6 100.53(19) . . ?
N4 Cu2 N6 160.4(2) . . ?
Mo5 O1 Cu1 152.7(3) . . ?
Mo6 O2 Cu1 137.5(2) . . ?
Mo1 O3 Cu2 148.9(2) . . ?
Mo5 O4 Mo8 111.7(2) . . ?
Mo4 O7 Mo3 117.6(2) . . ?
Mo2 O10 Mo4 108.59(19) 2_457 . ?
Mo2 O10 Mo1 111.48(16) 2_457 . ?
Mo4 O10 Mo1 104.40(16) . . ?
Mo2 O11 Mo1 108.22(17) . . ?
Mo2 O11 Mo4 111.93(17) . . ?
Mo1 O11 Mo4 102.93(15) . . ?
Mo2 O12 Mo1 93.19(14) . . ?
Mo2 O12 Mo4 91.84(14) . 2_457 ?
Mo1 O12 Mo4 164.45(18) . 2_457 ?
Mo2 O12 Mo2 103.94(15) . 2_457 ?
Mo1 O12 Mo2 96.61(13) . 2_457 ?
Mo4 O12 Mo2 96.45(14) 2_457 2_457 ?
Mo2 O12 Mo3 165.23(18) . 2_457 ?
Mo1 O12 Mo3 87.14(13) . 2_457 ?
Mo4 O12 Mo3 84.29(12) 2_457 2_457 ?
Mo2 O12 Mo3 90.67(12) 2_457 2_457 ?
Mo2 O14 Mo3 118.88(18) . . ?
Mo5 O17 Mo6 145.0(2) . . ?
Mo5 O17 Mo7 106.76(18) . . ?
Mo6 O17 Mo7 103.41(18) . . ?
Mo7 O18 Mo6 107.28(19) . . ?
Mo7 O18 Mo7 101.10(16) . 2_566 ?
Mo6 O18 Mo7 95.14(14) . 2_566 ?
Mo7 O20 Mo6 116.3(2) . 2_566 ?
Mo7 O21 Mo8 124.89(19) . . ?
Mo7 O21 Mo5 106.57(17) . . ?
Mo8 O21 Mo5 97.23(16) . . ?
Mo6 O23 Mo8 119.8(2) 2_566 . ?
Mo1 O24 Mo3 118.3(2) 2_457 . ?
N3 C1 C2 122.1(7) . . ?
C3 C2 C1 118.3(6) . . ?
C2 C3 C4 120.5(7) . . ?
C3 C4 C5 118.5(7) . . ?
N3 C5 C4 121.0(6) . . ?
N3 C5 C6 114.1(5) . . ?
C4 C5 C6 124.9(6) . . ?
N1 C6 C7 120.3(6) . . ?
N1 C6 C5 113.1(5) . . ?
C7 C6 C5 126.6(6) . . ?
C6 C7 C8 117.9(6) . . ?
C9 C8 C7 120.2(6) . . ?
C10 C9 C8 118.9(6) . . ?
N1 C10 C9 120.0(6) . . ?
N1 C10 C11 112.5(5) . . ?
C9 C10 C11 127.5(6) . . ?
N2 C11 C12 120.6(6) . . ?
N2 C11 C10 114.0(5) . . ?
C12 C11 C10 125.4(6) . . ?
C11 C12 C13 119.8(6) . . ?
C14 C13 C12 119.2(6) . . ?
C13 C14 C15 119.4(6) . . ?
N2 C15 C14 121.7(6) . . ?
N4 C16 C17 122.2(6) . . ?
C18 C17 C16 118.2(6) . . ?
C17 C18 C19 120.0(6) . . ?
C18 C19 C20 119.0(6) . . ?
N4 C20 C19 121.2(6) . . ?
N4 C20 C21 115.4(5) . . ?
C19 C20 C21 123.4(5) . . ?
N5 C21 C22 120.7(5) . . ?
N5 C21 C20 111.5(5) . . ?
C22 C21 C20 127.8(5) . . ?
C21 C22 C23 118.4(6) . . ?
C24 C23 C22 120.1(6) . . ?
C23 C24 C25 119.0(6) . . ?
N5 C25 C24 120.4(5) . . ?
N5 C25 C26 112.2(5) . . ?
C24 C25 C26 127.4(6) . . ?
N6 C26 C27 121.8(6) . . ?
N6 C26 C25 114.0(5) . . ?
C27 C26 C25 124.1(6) . . ?
C28 C27 C26 118.7(6) . . ?
C29 C28 C27 120.5(6) . . ?
C28 C29 C30 118.5(6) . . ?
N6 C30 C29 122.3(6) . . ?
C6 N1 C10 122.7(5) . . ?
C6 N1 Cu1 118.5(4) . . ?
C10 N1 Cu1 118.6(4) . . ?
C15 N2 C11 119.3(5) . . ?
C15 N2 Cu1 127.3(4) . . ?
C11 N2 Cu1 113.3(4) . . ?
C1 N3 C5 119.5(6) . . ?
C1 N3 Cu1 126.9(5) . . ?
C5 N3 Cu1 113.5(4) . . ?
C20 N4 C16 119.4(5) . . ?
C20 N4 Cu2 113.9(4) . . ?
C16 N4 Cu2 126.5(4) . . ?
C25 N5 C21 121.4(5) . . ?
C25 N5 Cu2 119.9(4) . . ?
C21 N5 Cu2 118.5(4) . . ?
C30 N6 C26 118.1(5) . . ?
C30 N6 Cu2 128.0(4) . . ?
C26 N6 Cu2 113.7(4) . . ?

_refine_diff_density_max         1.139
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.167

