# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1-2
_database_code_depnum_ccdc_archive 'CCDC 1555147'
_audit_update_record             
;
2017-11-05 deposited with the CCDC.
2017-11-07 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         ?
_chemical_formula_sum            'C8 H16 Cu4 Mo12 N16 O40 P'
_chemical_formula_weight         2412.78

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'
P P 0.1023 0.0942 '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      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                   18.8049(14)
_cell_length_b                   13.7184(10)
_cell_length_c                   17.7762(13)
_cell_angle_alpha                90
_cell_angle_beta                 95.5110(10)
_cell_angle_gamma                90
_cell_volume                     4564.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7194
_cell_measurement_theta_min      2.1761
_cell_measurement_theta_max      28.1864

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.511
_exptl_crystal_F_000             4524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    5.157
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_reflns_number            32375
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.088
_diffrn_reflns_theta_max         28.336
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11347
_reflns_number_gt                7517
_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.
;

_computing_data_collection       'Bruker SMAR'
_computing_cell_refinement       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0090P)²] 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         11347
_refine_ls_number_parameters     730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0627
_refine_ls_wR_factor_gt          0.0574
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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 0.07704(2) 0.42807(4) 0.17132(3) 0.02598(12) Uani 1 1 d . . . . .
Mo2 Mo 0.21708(2) 0.27061(3) 0.15498(3) 0.01974(11) Uani 1 1 d . . . . .
Mo3 Mo 0.29254(3) 0.50290(4) 0.45205(3) 0.02388(11) Uani 1 1 d . . . . .
Mo4 Mo 0.20566(3) 0.48201(4) 0.05215(3) 0.02326(11) Uani 1 1 d . . . . .
Mo5 Mo 0.27928(2) 0.73043(3) 0.33861(3) 0.02035(11) Uani 1 1 d . . . . .
Mo6 Mo 0.24754(2) 0.28545(4) 0.36366(3) 0.02035(11) Uani 1 1 d . . . . .
Mo7 Mo 0.11182(2) 0.67374(4) 0.25475(3) 0.01927(10) Uani 1 1 d . . . . .
Mo8 Mo 0.42883(2) 0.56109(4) 0.32275(3) 0.02429(12) Uani 1 1 d . . . . .
Mo9 Mo 0.39616(2) 0.33238(3) 0.24556(2) 0.01819(10) Uani 1 1 d . . . . .
Mo10 Mo 0.11919(2) 0.45898(4) 0.37995(3) 0.02424(12) Uani 1 1 d . . . . .
Mo11 Mo 0.39106(2) 0.53331(4) 0.12958(3) 0.02194(11) Uani 1 1 d . . . . .
Mo12 Mo 0.25079(2) 0.71636(4) 0.14523(3) 0.01989(11) Uani 1 1 d . . . . .
Cu1 Cu 0.03540(4) 0.34071(6) -0.37096(4) 0.03097(18) Uani 1 1 d . . . . .
Cu2 Cu 0.06114(4) 0.13828(6) -0.65413(4) 0.0360(2) Uani 1 1 d . . . . .
Cu3 Cu 0.54394(4) 0.34719(6) 0.13025(4) 0.02984(18) Uani 1 1 d . . . . .
Cu4 Cu 0.56999(4) 0.37436(6) 0.35105(4) 0.02999(18) Uani 1 1 d . . . . .
P1 P 0.25140(7) 0.49757(11) 0.25066(8) 0.0136(2) Uani 1 1 d . . . . .
N1 N 0.0823(2) 0.4381(3) -0.3071(2) 0.0222(10) Uani 1 1 d . . . . .
N2 N 0.1018(2) 0.4339(4) -0.2296(2) 0.0263(11) Uani 1 1 d . . . . .
N3 N 0.1581(2) 0.5561(4) -0.2760(3) 0.0311(12) Uani 1 1 d . . . . .
N4 N 0.1133(3) 0.5443(4) -0.4043(3) 0.0388(13) Uani 1 1 d . . . . .
H4A H 0.0865 0.5150 -0.4392 0.047 Uiso 1 1 calc R U . . .
H4B H 0.1380 0.5941 -0.4153 0.047 Uiso 1 1 calc R U . . .
N5 N 0.0256(2) 0.1891(4) -0.5668(2) 0.0295(12) Uani 1 1 d . . . . .
N6 N -0.0450(2) 0.1819(4) -0.5539(3) 0.0324(12) Uani 1 1 d . . . . .
N7 N 0.0064(2) 0.2705(3) -0.4608(2) 0.0229(10) Uani 1 1 d . . . . .
N8 N -0.1191(3) 0.2437(5) -0.4659(3) 0.063(2) Uani 1 1 d . . . . .
H8A H -0.1563 0.2174 -0.4894 0.075 Uiso 1 1 calc R U . . .
H8B H -0.1229 0.2772 -0.4256 0.075 Uiso 1 1 calc R U . . .
N9 N 0.5370(2) 0.1877(4) -0.0633(3) 0.0297(12) Uani 1 1 d . . . . .
N10 N 0.4645(2) 0.1895(4) -0.0526(2) 0.0275(11) Uani 1 1 d . . . . .
N11 N 0.5207(2) 0.2724(3) 0.0412(2) 0.0215(10) Uani 1 1 d . . . . .
N12 N 0.3937(2) 0.2596(4) 0.0341(3) 0.0381(14) Uani 1 1 d . . . . .
H12A H 0.3554 0.2379 0.0094 0.046 Uiso 1 1 calc R U . . .
H12B H 0.3911 0.2932 0.0745 0.046 Uiso 1 1 calc R U . . .
N13 N 0.5911(2) 0.4424(3) 0.1952(2) 0.0221(10) Uani 1 1 d . . . . .
N14 N 0.6095(2) 0.4469(3) 0.2738(2) 0.0238(11) Uani 1 1 d . . . . .
N15 N 0.6617(3) 0.5681(4) 0.2214(3) 0.0356(13) Uani 1 1 d . . . . .
N16 N 0.6180(3) 0.5434(4) 0.0932(3) 0.0424(15) Uani 1 1 d . . . . .
H16A H 0.5921 0.5098 0.0601 0.051 Uiso 1 1 calc R U . . .
H16B H 0.6408 0.5937 0.0794 0.051 Uiso 1 1 calc R U . . .
C1 C 0.1163(3) 0.5123(4) -0.3330(3) 0.0253(13) Uani 1 1 d . . . . .
C2 C 0.1454(3) 0.5045(5) -0.2133(3) 0.0360(16) Uani 1 1 d . . . . .
H2B H 0.1658 0.5187 -0.1647 0.043 Uiso 1 1 calc R U . . .
C3 C 0.0540(3) 0.2412(4) -0.5093(3) 0.0246(13) Uani 1 1 d . . . . .
H3B H 0.1023 0.2566 -0.5025 0.030 Uiso 1 1 calc R U . . .
C4 C -0.0565(3) 0.2328(5) -0.4915(3) 0.0310(15) Uani 1 1 d . . . . .
C5 C 0.5675(3) 0.2370(4) -0.0058(3) 0.0267(13) Uani 1 1 d . . . . .
H5A H 0.6166 0.2468 0.0022 0.032 Uiso 1 1 calc R U . . .
C6 C 0.4560(3) 0.2414(4) 0.0100(3) 0.0233(12) Uani 1 1 d . . . . .
C7 C 0.6508(3) 0.5212(5) 0.2862(3) 0.0349(15) Uani 1 1 d . . . . .
H7A H 0.6707 0.5403 0.3339 0.042 Uiso 1 1 calc R U . . .
C8 C 0.6229(3) 0.5173(4) 0.1662(3) 0.0248(13) Uani 1 1 d . . . . .
O1 O 0.45386(18) 0.2400(3) 0.2434(2) 0.0309(10) Uani 1 1 d . . . . .
O2 O 0.1948(2) 0.4943(3) -0.0415(2) 0.0348(10) Uani 1 1 d . . . . .
O3 O 0.27222(18) 0.6337(3) 0.41180(19) 0.0260(9) Uani 1 1 d . . . . .
O4 O 0.08070(19) 0.5679(3) 0.19330(19) 0.0259(9) Uani 1 1 d . . . . .
O5 O 0.29317(18) 0.3649(3) 0.4473(2) 0.0280(9) Uani 1 1 d . . . . .
O6 O -0.00965(18) 0.4112(3) 0.1462(2) 0.0317(10) Uani 1 1 d . . . . .
O7 O 0.15963(18) 0.3247(3) 0.3910(2) 0.0276(9) Uani 1 1 d . . . . .
O8 O 0.24980(19) 0.8068(3) 0.0823(2) 0.0324(10) Uani 1 1 d . . . . .
O9 O 0.08447(19) 0.4127(3) 0.27879(19) 0.0271(9) Uani 1 1 d . . . . .
O10 O 0.31519(17) 0.2864(3) 0.17855(18) 0.0238(9) Uani 1 1 d . . . . .
O11 O 0.45203(18) 0.4212(3) 0.30724(19) 0.0238(9) Uani 1 1 d . . . . .
O12 O 0.37169(17) 0.6729(3) 0.32325(19) 0.0263(9) Uani 1 1 d . . . . .
O13 O 0.33587(18) 0.6539(3) 0.1369(2) 0.0269(9) Uani 1 1 d . . . . .
O14 O 0.25834(19) 0.1744(3) 0.4027(2) 0.0313(9) Uani 1 1 d . . . . .
O15 O 0.03490(19) 0.7335(3) 0.2617(2) 0.0335(10) Uani 1 1 d . . . . .
O16 O 0.20289(18) 0.6123(3) 0.0854(2) 0.0262(9) Uani 1 1 d . . . . .
O17 O 0.19007(18) 0.4957(3) 0.4577(2) 0.0270(9) Uani 1 1 d . . . . .
O18 O 0.11012(19) 0.5829(3) 0.33939(19) 0.0267(9) Uani 1 1 d . . . . .
O19 O 0.3224(2) 0.5218(3) 0.5423(2) 0.0343(10) Uani 1 1 d . . . . .
O20 O 0.50529(18) 0.5939(3) 0.3699(2) 0.0291(9) Uani 1 1 d . . . . .
O21 O 0.42148(18) 0.4040(3) 0.15712(19) 0.0239(8) Uani 1 1 d . . . . .
O22 O 0.30280(19) 0.8284(3) 0.3912(2) 0.0308(9) Uani 1 1 d . . . . .
O23 O 0.37602(18) 0.5111(3) 0.4024(2) 0.0281(9) Uani 1 1 d . . . . .
O24 O 0.10884(18) 0.4651(3) 0.0750(2) 0.0260(9) Uani 1 1 d . . . . .
O25 O 0.23239(17) 0.6057(3) 0.24847(18) 0.0201(8) Uani 1 1 d . . . . .
O26 O 0.04838(19) 0.4495(3) 0.4300(2) 0.0331(10) Uani 1 1 d . . . . .
O27 O 0.21367(18) 0.3398(3) 0.06438(19) 0.0272(9) Uani 1 1 d . . . . .
O28 O 0.20771(17) 0.4434(2) 0.18695(18) 0.0195(8) Uani 1 1 d . . . . .
O29 O 0.21158(19) 0.1553(3) 0.1253(2) 0.0315(9) Uani 1 1 d . . . . .
O30 O 0.44408(19) 0.5580(3) 0.06157(19) 0.0287(9) Uani 1 1 d . . . . .
O31 O 0.21568(17) 0.2544(3) 0.26519(19) 0.0272(9) Uani 1 1 d . . . . .
O32 O 0.28008(18) 0.7819(3) 0.23581(19) 0.0263(9) Uani 1 1 d . . . . .
O33 O 0.11542(17) 0.3020(3) 0.15889(19) 0.0256(9) Uani 1 1 d . . . . .
O34 O 0.30730(18) 0.4860(3) 0.07406(19) 0.0261(9) Uani 1 1 d . . . . .
O35 O 0.44874(18) 0.5799(3) 0.21993(19) 0.0250(9) Uani 1 1 d . . . . .
O36 O 0.33132(17) 0.4861(2) 0.24104(18) 0.0190(8) Uani 1 1 d . . . . .
O37 O 0.23542(17) 0.4545(3) 0.32692(19) 0.0210(8) Uani 1 1 d . . . . .
O38 O 0.17834(17) 0.7470(3) 0.32349(18) 0.0225(8) Uani 1 1 d . . . . .
O39 O 0.34190(18) 0.2979(3) 0.32430(19) 0.0263(9) Uani 1 1 d . . . . .
O40 O 0.15142(18) 0.7372(3) 0.17557(19) 0.0261(9) 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 O6 1.665(3) . ?
Mo1 O33 1.895(4) . ?
Mo1 O9 1.914(3) . ?
Mo1 O24 1.934(4) . ?
Mo1 O4 1.957(4) . ?
Mo1 O28 2.455(3) . ?
Mo2 O29 1.668(4) . ?
Mo2 O10 1.865(3) . ?
Mo2 O27 1.865(4) . ?
Mo2 O33 1.967(3) . ?
Mo2 O31 1.974(4) . ?
Mo2 O28 2.448(3) . ?
Mo3 O19 1.668(3) . ?
Mo3 O23 1.877(4) . ?
Mo3 O5 1.896(4) . ?
Mo3 O17 1.942(3) . ?
Mo3 O3 1.956(4) . ?
Mo3 O37 2.467(3) . ?
Mo4 O2 1.667(3) . ?
Mo4 O16 1.885(4) . ?
Mo4 O34 1.914(3) . ?
Mo4 O24 1.917(4) . ?
Mo4 O27 1.967(4) . ?
Mo4 O28 2.451(3) . ?
Mo5 O22 1.672(4) . ?
Mo5 O3 1.872(4) . ?
Mo5 O38 1.905(3) . ?
Mo5 O12 1.951(3) . ?
Mo5 O32 1.960(3) . ?
Mo5 O25 2.450(3) . ?
Mo6 O14 1.678(4) . ?
Mo6 O31 1.845(3) . ?
Mo6 O7 1.847(3) . ?
Mo6 O5 1.972(4) . ?
Mo6 O39 1.976(3) . ?
Mo6 O37 2.414(3) . ?
Mo7 O15 1.677(4) . ?
Mo7 O40 1.870(4) . ?
Mo7 O4 1.877(4) . ?
Mo7 O38 1.942(3) . ?
Mo7 O18 1.956(3) . ?
Mo7 O25 2.464(3) . ?
Mo8 O20 1.656(3) . ?
Mo8 O12 1.873(4) . ?
Mo8 O35 1.918(3) . ?
Mo8 O23 1.932(4) . ?
Mo8 O11 1.993(4) . ?
Mo8 O36 2.453(3) . ?
Mo9 O1 1.671(4) . ?
Mo9 O39 1.870(3) . ?
Mo9 O11 1.889(3) . ?
Mo9 O10 1.946(3) . ?
Mo9 O21 1.952(3) . ?
Mo9 O36 2.434(3) . ?
Mo10 O26 1.676(4) . ?
Mo10 O18 1.848(4) . ?
Mo10 O17 1.894(3) . ?
Mo10 O9 1.959(3) . ?
Mo10 O7 1.995(4) . ?
Mo10 O37 2.463(3) . ?
Mo11 O30 1.674(3) . ?
Mo11 O34 1.892(3) . ?
Mo11 O21 1.913(4) . ?
Mo11 O35 1.957(3) . ?
Mo11 O13 1.963(4) . ?
Mo11 O36 2.456(3) . ?
Mo12 O8 1.670(4) . ?
Mo12 O13 1.834(3) . ?
Mo12 O32 1.880(3) . ?
Mo12 O16 1.949(4) . ?
Mo12 O40 2.015(4) . ?
Mo12 O25 2.432(3) . ?
Cu1 N7 1.899(4) . ?
Cu1 N1 1.913(4) . ?
Cu2 N5 1.882(4) . ?
Cu2 N2 1.888(5) 4_565 ?
Cu3 N11 1.901(4) . ?
Cu3 N13 1.904(4) . ?
Cu4 N9 1.900(5) 4_566 ?
Cu4 N14 1.904(4) . ?
Cu4 O11 2.368(3) . ?
P1 O25 1.525(4) . ?
P1 O28 1.527(3) . ?
P1 O37 1.535(4) . ?
P1 O36 1.537(3) . ?
N1 C1 1.309(7) . ?
N1 N2 1.392(5) . ?
N2 C2 1.285(7) . ?
N2 Cu2 1.888(5) 4_566 ?
N3 C1 1.359(6) . ?
N3 C2 1.361(7) . ?
N4 C1 1.338(6) . ?
N5 C3 1.317(6) . ?
N5 N6 1.372(6) . ?
N6 C4 1.345(7) . ?
N7 C4 1.357(6) . ?
N7 C3 1.363(6) . ?
N8 C4 1.310(7) . ?
N9 C5 1.311(6) . ?
N9 N10 1.393(6) . ?
N9 Cu4 1.900(5) 4_565 ?
N10 C6 1.342(6) . ?
N11 C6 1.355(6) . ?
N11 C5 1.361(7) . ?
N12 C6 1.310(6) . ?
N13 C8 1.320(7) . ?
N13 N14 1.408(5) . ?
N14 C7 1.289(7) . ?
N15 C7 1.352(7) . ?
N15 C8 1.358(6) . ?
N16 C8 1.340(6) . ?

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
O6 Mo1 O33 102.47(17) . . ?
O6 Mo1 O9 103.20(17) . . ?
O33 Mo1 O9 91.35(15) . . ?
O6 Mo1 O24 100.19(17) . . ?
O33 Mo1 O24 89.03(15) . . ?
O9 Mo1 O24 155.94(15) . . ?
O6 Mo1 O4 101.80(17) . . ?
O33 Mo1 O4 155.66(14) . . ?
O9 Mo1 O4 84.90(15) . . ?
O24 Mo1 O4 84.91(15) . . ?
O6 Mo1 O28 170.39(16) . . ?
O33 Mo1 O28 72.74(13) . . ?
O9 Mo1 O28 85.43(13) . . ?
O24 Mo1 O28 71.73(13) . . ?
O4 Mo1 O28 82.98(13) . . ?
O29 Mo2 O10 102.18(17) . . ?
O29 Mo2 O27 102.31(18) . . ?
O10 Mo2 O27 94.95(15) . . ?
O29 Mo2 O33 100.82(17) . . ?
O10 Mo2 O33 155.58(15) . . ?
O27 Mo2 O33 88.07(15) . . ?
O29 Mo2 O31 101.59(17) . . ?
O10 Mo2 O31 84.11(14) . . ?
O27 Mo2 O31 155.72(16) . . ?
O33 Mo2 O31 83.34(14) . . ?
O29 Mo2 O28 171.25(15) . . ?
O10 Mo2 O28 85.83(14) . . ?
O27 Mo2 O28 73.17(14) . . ?
O33 Mo2 O28 71.83(13) . . ?
O31 Mo2 O28 82.58(14) . . ?
O19 Mo3 O23 102.93(18) . . ?
O19 Mo3 O5 101.24(17) . . ?
O23 Mo3 O5 91.70(16) . . ?
O19 Mo3 O17 101.66(17) . . ?
O23 Mo3 O17 155.01(15) . . ?
O5 Mo3 O17 87.83(15) . . ?
O19 Mo3 O3 104.21(17) . . ?
O23 Mo3 O3 85.17(15) . . ?
O5 Mo3 O3 154.41(15) . . ?
O17 Mo3 O3 84.57(15) . . ?
O19 Mo3 O37 170.46(17) . . ?
O23 Mo3 O37 84.46(13) . . ?
O5 Mo3 O37 72.22(13) . . ?
O17 Mo3 O37 71.60(13) . . ?
O3 Mo3 O37 82.20(13) . . ?
O2 Mo4 O16 102.26(18) . . ?
O2 Mo4 O34 102.98(17) . . ?
O16 Mo4 O34 88.08(15) . . ?
O2 Mo4 O24 101.34(17) . . ?
O16 Mo4 O24 89.59(15) . . ?
O34 Mo4 O24 155.51(15) . . ?
O2 Mo4 O27 102.22(17) . . ?
O16 Mo4 O27 155.52(15) . . ?
O34 Mo4 O27 86.63(15) . . ?
O24 Mo4 O27 85.45(15) . . ?
O2 Mo4 O28 171.01(17) . . ?
O16 Mo4 O28 84.09(13) . . ?
O34 Mo4 O28 83.43(13) . . ?
O24 Mo4 O28 72.08(13) . . ?
O27 Mo4 O28 71.56(13) . . ?
O22 Mo5 O3 102.35(17) . . ?
O22 Mo5 O38 100.94(16) . . ?
O3 Mo5 O38 92.65(15) . . ?
O22 Mo5 O12 102.24(17) . . ?
O3 Mo5 O12 86.22(15) . . ?
O38 Mo5 O12 156.49(15) . . ?
O22 Mo5 O32 101.92(17) . . ?
O3 Mo5 O32 155.57(16) . . ?
O38 Mo5 O32 85.55(14) . . ?
O12 Mo5 O32 85.90(15) . . ?
O22 Mo5 O25 170.50(15) . . ?
O3 Mo5 O25 85.08(14) . . ?
O38 Mo5 O25 72.52(13) . . ?
O12 Mo5 O25 84.00(13) . . ?
O32 Mo5 O25 71.11(13) . . ?
O14 Mo6 O31 101.42(18) . . ?
O14 Mo6 O7 103.39(17) . . ?
O31 Mo6 O7 95.72(15) . . ?
O14 Mo6 O5 99.39(17) . . ?
O31 Mo6 O5 157.11(16) . . ?
O7 Mo6 O5 88.64(15) . . ?
O14 Mo6 O39 98.50(16) . . ?
O31 Mo6 O39 84.55(14) . . ?
O7 Mo6 O39 157.58(16) . . ?
O5 Mo6 O39 83.02(15) . . ?
O14 Mo6 O37 171.26(16) . . ?
O31 Mo6 O37 87.23(14) . . ?
O7 Mo6 O37 74.20(14) . . ?
O5 Mo6 O37 72.32(13) . . ?
O39 Mo6 O37 83.43(13) . . ?
O15 Mo7 O40 103.66(18) . . ?
O15 Mo7 O4 101.40(17) . . ?
O40 Mo7 O4 92.68(16) . . ?
O15 Mo7 O38 102.08(17) . . ?
O40 Mo7 O38 87.34(15) . . ?
O4 Mo7 O38 155.82(15) . . ?
O15 Mo7 O18 100.20(18) . . ?
O40 Mo7 O18 155.90(15) . . ?
O4 Mo7 O18 85.84(15) . . ?
O38 Mo7 O18 84.41(15) . . ?
O15 Mo7 O25 172.79(16) . . ?
O40 Mo7 O25 73.00(13) . . ?
O4 Mo7 O25 85.26(13) . . ?
O38 Mo7 O25 71.62(13) . . ?
O18 Mo7 O25 82.91(13) . . ?
O20 Mo8 O12 104.23(17) . . ?
O20 Mo8 O35 101.94(17) . . ?
O12 Mo8 O35 93.37(15) . . ?
O20 Mo8 O23 101.98(17) . . ?
O12 Mo8 O23 87.23(15) . . ?
O35 Mo8 O23 155.15(15) . . ?
O20 Mo8 O11 98.09(16) . . ?
O12 Mo8 O11 157.26(14) . . ?
O35 Mo8 O11 86.14(15) . . ?
O23 Mo8 O11 83.93(15) . . ?
O20 Mo8 O36 167.74(16) . . ?
O12 Mo8 O36 87.10(13) . . ?
O35 Mo8 O36 72.27(13) . . ?
O23 Mo8 O36 82.97(13) . . ?
O11 Mo8 O36 71.07(12) . . ?
O1 Mo9 O39 103.18(18) . . ?
O1 Mo9 O11 100.15(16) . . ?
O39 Mo9 O11 92.38(15) . . ?
O1 Mo9 O10 102.21(17) . . ?
O39 Mo9 O10 85.71(14) . . ?
O11 Mo9 O10 157.40(15) . . ?
O1 Mo9 O21 98.86(17) . . ?
O39 Mo9 O21 157.37(15) . . ?
O11 Mo9 O21 88.72(15) . . ?
O10 Mo9 O21 84.68(14) . . ?
O1 Mo9 O36 168.73(16) . . ?
O39 Mo9 O36 86.34(14) . . ?
O11 Mo9 O36 73.10(13) . . ?
O10 Mo9 O36 84.31(13) . . ?
O21 Mo9 O36 72.36(13) . . ?
O26 Mo10 O18 103.32(17) . . ?
O26 Mo10 O17 99.94(17) . . ?
O18 Mo10 O17 94.13(16) . . ?
O26 Mo10 O9 104.50(17) . . ?
O18 Mo10 O9 85.99(15) . . ?
O17 Mo10 O9 154.86(15) . . ?
O26 Mo10 O7 100.99(17) . . ?
O18 Mo10 O7 155.18(15) . . ?
O17 Mo10 O7 86.51(15) . . ?
O9 Mo10 O7 83.17(15) . . ?
O26 Mo10 O37 168.73(16) . . ?
O18 Mo10 O37 85.75(14) . . ?
O17 Mo10 O37 72.40(13) . . ?
O9 Mo10 O37 82.55(13) . . ?
O7 Mo10 O37 70.77(13) . . ?
O30 Mo11 O34 102.51(17) . . ?
O30 Mo11 O21 100.87(17) . . ?
O34 Mo11 O21 91.65(15) . . ?
O30 Mo11 O35 101.82(16) . . ?
O34 Mo11 O35 155.29(15) . . ?
O21 Mo11 O35 87.96(15) . . ?
O30 Mo11 O13 103.43(17) . . ?
O34 Mo11 O13 84.53(15) . . ?
O21 Mo11 O13 155.66(15) . . ?
O35 Mo11 O13 85.72(15) . . ?
O30 Mo11 O36 170.45(15) . . ?
O34 Mo11 O36 84.72(13) . . ?
O21 Mo11 O36 72.42(13) . . ?
O35 Mo11 O36 71.61(13) . . ?
O13 Mo11 O36 83.28(13) . . ?
O8 Mo12 O13 104.29(18) . . ?
O8 Mo12 O32 101.67(17) . . ?
O13 Mo12 O32 96.13(15) . . ?
O8 Mo12 O16 101.74(17) . . ?
O13 Mo12 O16 88.53(15) . . ?
O32 Mo12 O16 154.17(15) . . ?
O8 Mo12 O40 97.05(16) . . ?
O13 Mo12 O40 157.99(16) . . ?
O32 Mo12 O40 84.59(14) . . ?
O16 Mo12 O40 81.86(15) . . ?
O8 Mo12 O25 167.51(16) . . ?
O13 Mo12 O25 87.58(14) . . ?
O32 Mo12 O25 72.74(14) . . ?
O16 Mo12 O25 82.13(13) . . ?
O40 Mo12 O25 71.57(13) . . ?
N7 Cu1 N1 158.74(19) . . ?
N5 Cu2 N2 168.8(2) . 4_565 ?
N11 Cu3 N13 158.57(19) . . ?
N9 Cu4 N14 173.0(2) 4_566 . ?
N9 Cu4 O11 90.98(16) 4_566 . ?
N14 Cu4 O11 92.22(15) . . ?
O25 P1 O28 110.25(19) . . ?
O25 P1 O37 109.4(2) . . ?
O28 P1 O37 109.3(2) . . ?
O25 P1 O36 109.00(19) . . ?
O28 P1 O36 109.27(19) . . ?
O37 P1 O36 109.60(19) . . ?
C1 N1 N2 106.7(4) . . ?
C1 N1 Cu1 123.2(4) . . ?
N2 N1 Cu1 128.4(3) . . ?
C2 N2 N1 107.2(4) . . ?
C2 N2 Cu2 121.9(4) . 4_566 ?
N1 N2 Cu2 129.7(3) . 4_566 ?
C1 N3 C2 104.3(5) . . ?
C3 N5 N6 103.7(4) . . ?
C3 N5 Cu2 133.7(4) . . ?
N6 N5 Cu2 122.5(3) . . ?
C4 N6 N5 109.6(4) . . ?
C4 N7 C3 103.5(5) . . ?
C4 N7 Cu1 134.5(4) . . ?
C3 N7 Cu1 121.9(4) . . ?
C5 N9 N10 104.2(4) . . ?
C5 N9 Cu4 134.7(4) . 4_565 ?
N10 N9 Cu4 121.1(3) . 4_565 ?
C6 N10 N9 108.6(4) . . ?
C6 N11 C5 104.1(4) . . ?
C6 N11 Cu3 129.5(4) . . ?
C5 N11 Cu3 126.3(4) . . ?
C8 N13 N14 106.0(4) . . ?
C8 N13 Cu3 120.0(4) . . ?
N14 N13 Cu3 133.4(3) . . ?
C7 N14 N13 107.0(4) . . ?
C7 N14 Cu4 124.1(4) . . ?
N13 N14 Cu4 128.1(3) . . ?
C7 N15 C8 104.9(5) . . ?
N1 C1 N4 127.5(5) . . ?
N1 C1 N3 110.4(5) . . ?
N4 C1 N3 122.0(5) . . ?
N2 C2 N3 111.3(5) . . ?
N5 C3 N7 114.1(5) . . ?
N8 C4 N6 124.5(5) . . ?
N8 C4 N7 126.4(5) . . ?
N6 C4 N7 109.1(5) . . ?
N9 C5 N11 113.6(5) . . ?
N12 C6 N10 123.6(5) . . ?
N12 C6 N11 126.9(5) . . ?
N10 C6 N11 109.4(5) . . ?
N14 C7 N15 111.6(5) . . ?
N13 C8 N16 126.4(5) . . ?
N13 C8 N15 110.5(5) . . ?
N16 C8 N15 123.1(5) . . ?
Mo5 O3 Mo3 151.7(2) . . ?
Mo7 O4 Mo1 151.3(2) . . ?
Mo3 O5 Mo6 125.55(18) . . ?
Mo6 O7 Mo10 125.82(19) . . ?
Mo1 O9 Mo10 150.0(2) . . ?
Mo2 O10 Mo9 150.9(2) . . ?
Mo9 O11 Mo8 125.76(17) . . ?
Mo9 O11 Cu4 117.85(17) . . ?
Mo8 O11 Cu4 115.22(15) . . ?
Mo8 O12 Mo5 148.3(2) . . ?
Mo12 O13 Mo11 150.5(2) . . ?
Mo4 O16 Mo12 147.19(19) . . ?
Mo10 O17 Mo3 127.47(19) . . ?
Mo10 O18 Mo7 151.4(2) . . ?
Mo11 O21 Mo9 125.68(18) . . ?
Mo3 O23 Mo8 151.4(2) . . ?
Mo4 O24 Mo1 126.88(18) . . ?
P1 O25 Mo12 125.19(19) . . ?
P1 O25 Mo5 126.42(18) . . ?
Mo12 O25 Mo5 89.38(12) . . ?
P1 O25 Mo7 125.56(19) . . ?
Mo12 O25 Mo7 89.77(11) . . ?
Mo5 O25 Mo7 88.90(11) . . ?
Mo2 O27 Mo4 126.58(19) . . ?
P1 O28 Mo2 126.72(18) . . ?
P1 O28 Mo4 125.2(2) . . ?
Mo2 O28 Mo4 88.68(11) . . ?
P1 O28 Mo1 125.95(19) . . ?
Mo2 O28 Mo1 89.10(11) . . ?
Mo4 O28 Mo1 89.22(10) . . ?
Mo6 O31 Mo2 151.8(2) . . ?
Mo12 O32 Mo5 126.8(2) . . ?
Mo1 O33 Mo2 125.87(19) . . ?
Mo11 O34 Mo4 151.8(2) . . ?
Mo8 O35 Mo11 126.47(18) . . ?
P1 O36 Mo9 125.23(19) . . ?
P1 O36 Mo8 125.08(19) . . ?
Mo9 O36 Mo8 90.00(11) . . ?
P1 O36 Mo11 126.22(18) . . ?
Mo9 O36 Mo11 89.34(11) . . ?
Mo8 O36 Mo11 89.63(11) . . ?
P1 O37 Mo6 125.99(19) . . ?
P1 O37 Mo10 125.77(18) . . ?
Mo6 O37 Mo10 89.13(11) . . ?
P1 O37 Mo3 125.98(19) . . ?
Mo6 O37 Mo3 89.61(11) . . ?
Mo10 O37 Mo3 88.49(11) . . ?
Mo5 O38 Mo7 126.87(19) . . ?
Mo9 O39 Mo6 149.28(19) . . ?
Mo7 O40 Mo12 125.60(18) . . ?

_refine_diff_density_max         1.070
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.165

####################################################################### 
# 
# 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_2-1
_database_code_depnum_ccdc_archive 'CCDC 1555148'
_audit_update_record             
;
2017-11-05 deposited with the CCDC.
2017-11-07 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         ?
_chemical_formula_sum            'C6 H12 Cu3 Mo12 N12 O40 P'
_chemical_formula_weight         2265.15

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'
P P 0.1023 0.0942 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.6135(3)
_cell_length_b                   17.6135(3)
_cell_length_c                   23.0663(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6197.3(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8969
_cell_measurement_theta_min      2.2138
_cell_measurement_theta_max      28.2864

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.642
_exptl_crystal_F_000             6348
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    5.186
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_T_max  0.595
_exptl_absorpt_process_details   SADABS
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_reflns_number            15253
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.600
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3410
_reflns_number_gt                3193
_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.
;

_computing_data_collection       'Bruker SMAR'
_computing_cell_refinement       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0340P)²+30.9039P] 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         3410
_refine_ls_number_parameters     223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0714
_refine_ls_wR_factor_gt          0.0704
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_restrained_S_all      1.185
_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 0.56588(2) 0.36796(2) -0.01073(2) 0.01843(9) Uani 1 1 d . . . . .
Mo2 Mo 0.44804(2) 0.29275(2) 0.11388(2) 0.01899(9) Uani 1 1 d . . . . .
Mo3 Mo 0.54220(2) 0.24143(2) 0.24055(2) 0.01957(9) Uani 1 1 d . . . . .
Mo4 Mo 0.49556(2) 0.11061(2) 0.10554(2) 0.01840(9) Uani 1 1 d . . . . .
Cu1 Cu 0.60662(4) 0.50078(5) -0.15755(3) 0.04497(17) Uani 1 1 d . . . . .
P1 P 0.6667 0.3333 0.11218(6) 0.0116(3) Uani 1 3 d S T P . .
O1 O 0.53818(19) 0.3841(2) -0.07769(12) 0.0268(6) Uani 1 1 d . . . . .
O2 O 0.57133(18) 0.26678(17) -0.01866(11) 0.0201(5) Uani 1 1 d . . . . .
O3 O 0.45971(16) 0.31541(18) 0.02927(11) 0.0205(5) Uani 1 1 d . . . . .
O4 O 0.34051(18) 0.25511(19) 0.12236(13) 0.0274(6) Uani 1 1 d . . . . .
O5 O 0.45166(17) 0.18763(17) 0.09471(11) 0.0200(5) Uani 1 1 d . . . . .
O6 O 0.49364(17) 0.41585(17) 0.12182(11) 0.0197(5) Uani 1 1 d . . . . .
O7 O 0.48362(17) 0.28297(17) 0.18787(11) 0.0207(5) Uani 1 1 d . . . . .
O8 O 0.46444(19) 0.1907(2) 0.29155(12) 0.0290(6) Uani 1 1 d . . . . .
O9 O 0.63742(17) 0.23553(17) 0.27053(11) 0.0203(5) Uani 1 1 d . . . . .
O10 O 0.6667 0.3333 0.17896(17) 0.0150(8) Uani 1 3 d S T P . .
O11 O 0.51731(17) 0.15543(17) 0.18568(11) 0.0192(5) Uani 1 1 d . . . . .
O12 O 0.40281(18) 0.01347(18) 0.11295(13) 0.0260(6) Uani 1 1 d . . . . .
O13 O 0.52127(17) 0.11149(17) 0.02690(11) 0.0206(5) Uani 1 1 d . . . . .
O14 O 0.63803(15) 0.24075(15) 0.09002(10) 0.0146(5) Uani 1 1 d . . . . .
N1 N 0.5222(2) 0.4530(3) -0.21713(16) 0.0298(8) Uani 1 1 d . . . . .
N2 N 0.4612(3) 0.3655(3) -0.22746(17) 0.0341(8) Uani 1 1 d . . . . .
N3 N 0.4439(3) 0.4428(3) -0.29352(17) 0.0396(9) Uani 1 1 d . . . . .
N4 N 0.5533(3) 0.5859(3) -0.26466(17) 0.0388(9) Uani 1 1 d . . . . .
H4B H 0.5946 0.6184 -0.2409 0.047 Uiso 1 1 calc R U . . .
H4C H 0.5401 0.6095 -0.2927 0.047 Uiso 1 1 calc R U . . .
C1 C 0.4157(3) 0.3619(4) -0.2728(2) 0.0393(11) Uani 1 1 d . . . . .
H1B H 0.3703 0.3107 -0.2886 0.047 Uiso 1 1 calc R U . . .
C2 C 0.5093(3) 0.4985(3) -0.25799(19) 0.0316(9) 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 O1 1.686(3) . ?
Mo1 O2 1.841(3) . ?
Mo1 O3 1.864(3) . ?
Mo1 O13 1.977(3) 3_665 ?
Mo1 O2 1.986(3) 3_665 ?
Mo1 O14 2.429(2) 3_665 ?
Mo2 O4 1.676(3) . ?
Mo2 O7 1.856(3) . ?
Mo2 O6 1.908(3) . ?
Mo2 O5 1.935(3) . ?
Mo2 O3 1.982(3) . ?
Mo2 O14 2.427(2) 3_665 ?
Mo3 O8 1.683(3) . ?
Mo3 O11 1.851(3) . ?
Mo3 O9 1.865(3) . ?
Mo3 O7 1.957(3) . ?
Mo3 O9 1.975(3) 3_665 ?
Mo3 O10 2.428(2) . ?
Mo4 O12 1.682(3) . ?
Mo4 O13 1.868(3) . ?
Mo4 O5 1.884(3) . ?
Mo4 O6 1.952(3) 2_655 ?
Mo4 O11 1.971(3) . ?
Mo4 O14 2.435(2) . ?
Cu1 N1 1.886(4) . ?
Cu1 N2 1.892(4) 17_554 ?
P1 O14 1.534(2) 2_655 ?
P1 O14 1.534(2) 3_665 ?
P1 O14 1.534(2) . ?
P1 O10 1.541(4) . ?
O2 Mo1 1.986(3) 2_655 ?
O6 Mo4 1.952(3) 3_665 ?
O9 Mo3 1.975(3) 2_655 ?
O10 Mo3 2.428(2) 2_655 ?
O10 Mo3 2.428(2) 3_665 ?
O13 Mo1 1.977(3) 2_655 ?
O14 Mo2 2.427(2) 2_655 ?
O14 Mo1 2.429(2) 2_655 ?
N1 C2 1.328(6) . ?
N1 N2 1.389(5) . ?
N2 C1 1.299(6) . ?
N2 Cu1 1.892(4) 18_544 ?
N3 C1 1.341(7) . ?
N3 C2 1.353(6) . ?
N4 C2 1.342(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O2 103.41(13) . . ?
O1 Mo1 O3 103.54(13) . . ?
O2 Mo1 O3 95.36(12) . . ?
O1 Mo1 O13 100.01(13) . 3_665 ?
O2 Mo1 O13 155.30(11) . 3_665 ?
O3 Mo1 O13 86.63(11) . 3_665 ?
O1 Mo1 O2 100.16(13) . 3_665 ?
O2 Mo1 O2 84.83(16) . 3_665 ?
O3 Mo1 O2 155.55(11) . 3_665 ?
O13 Mo1 O2 83.42(11) 3_665 3_665 ?
O1 Mo1 O14 171.76(12) . 3_665 ?
O2 Mo1 O14 84.76(10) . 3_665 ?
O3 Mo1 O14 74.23(10) . 3_665 ?
O13 Mo1 O14 72.06(9) 3_665 3_665 ?
O2 Mo1 O14 81.46(9) 3_665 3_665 ?
O4 Mo2 O7 102.90(13) . . ?
O4 Mo2 O6 100.88(13) . . ?
O7 Mo2 O6 92.72(11) . . ?
O4 Mo2 O5 102.68(13) . . ?
O7 Mo2 O5 86.97(11) . . ?
O6 Mo2 O5 155.90(11) . . ?
O4 Mo2 O3 100.22(13) . . ?
O7 Mo2 O3 156.71(11) . . ?
O6 Mo2 O3 85.60(11) . . ?
O5 Mo2 O3 85.30(11) . . ?
O4 Mo2 O14 171.05(12) . 3_665 ?
O7 Mo2 O14 84.77(10) . 3_665 ?
O6 Mo2 O14 73.85(9) . 3_665 ?
O5 Mo2 O14 82.14(10) . 3_665 ?
O3 Mo2 O14 72.44(9) . 3_665 ?
O8 Mo3 O11 104.28(13) . . ?
O8 Mo3 O9 103.14(13) . . ?
O11 Mo3 O9 93.41(12) . . ?
O8 Mo3 O7 101.00(13) . . ?
O11 Mo3 O7 85.87(11) . . ?
O9 Mo3 O7 155.24(11) . . ?
O8 Mo3 O9 99.35(13) . 3_665 ?
O11 Mo3 O9 155.51(11) . 3_665 ?
O9 Mo3 O9 87.36(16) . 3_665 ?
O7 Mo3 O9 83.38(11) . 3_665 ?
O8 Mo3 O10 170.53(12) . . ?
O11 Mo3 O10 84.89(10) . . ?
O9 Mo3 O10 73.54(10) . . ?
O7 Mo3 O10 81.75(9) . . ?
O9 Mo3 O10 71.84(9) 3_665 . ?
O12 Mo4 O13 102.42(13) . . ?
O12 Mo4 O5 101.91(13) . . ?
O13 Mo4 O5 92.89(11) . . ?
O12 Mo4 O6 101.11(13) . 2_655 ?
O13 Mo4 O6 87.87(11) . 2_655 ?
O5 Mo4 O6 156.23(11) . 2_655 ?
O12 Mo4 O11 101.98(13) . . ?
O13 Mo4 O11 155.47(11) . . ?
O5 Mo4 O11 84.47(11) . . ?
O6 Mo4 O11 85.08(11) 2_655 . ?
O12 Mo4 O14 172.78(11) . . ?
O13 Mo4 O14 73.62(10) . . ?
O5 Mo4 O14 84.46(10) . . ?
O6 Mo4 O14 72.96(9) 2_655 . ?
O11 Mo4 O14 81.86(9) . . ?
N1 Cu1 N2 168.07(16) . 17_554 ?
O14 P1 O14 109.48(10) 2_655 3_665 ?
O14 P1 O14 109.48(10) 2_655 . ?
O14 P1 O14 109.48(10) 3_665 . ?
O14 P1 O10 109.46(10) 2_655 . ?
O14 P1 O10 109.46(10) 3_665 . ?
O14 P1 O10 109.46(10) . . ?
Mo1 O2 Mo1 152.44(15) . 2_655 ?
Mo1 O3 Mo2 124.39(13) . . ?
Mo4 O5 Mo2 151.67(15) . . ?
Mo2 O6 Mo4 124.08(13) . 3_665 ?
Mo2 O7 Mo3 150.61(15) . . ?
Mo3 O9 Mo3 125.32(13) . 2_655 ?
P1 O10 Mo3 125.81(8) . . ?
P1 O10 Mo3 125.81(8) . 2_655 ?
Mo3 O10 Mo3 89.23(11) . 2_655 ?
P1 O10 Mo3 125.81(8) . 3_665 ?
Mo3 O10 Mo3 89.23(11) . 3_665 ?
Mo3 O10 Mo3 89.23(11) 2_655 3_665 ?
Mo3 O11 Mo4 152.66(15) . . ?
Mo4 O13 Mo1 125.08(13) . 2_655 ?
P1 O14 Mo2 125.72(13) . 2_655 ?
P1 O14 Mo1 126.09(14) . 2_655 ?
Mo2 O14 Mo1 88.94(8) 2_655 2_655 ?
P1 O14 Mo4 126.03(13) . . ?
Mo2 O14 Mo4 89.07(8) 2_655 . ?
Mo1 O14 Mo4 89.08(8) 2_655 . ?
C2 N1 N2 106.1(4) . . ?
C2 N1 Cu1 125.6(3) . . ?
N2 N1 Cu1 128.3(3) . . ?
C1 N2 N1 107.9(4) . . ?
C1 N2 Cu1 127.5(4) . 18_544 ?
N1 N2 Cu1 123.9(3) . 18_544 ?
C1 N3 C2 106.5(4) . . ?
N2 C1 N3 110.1(5) . . ?
N1 C2 N4 126.8(4) . . ?
N1 C2 N3 109.4(4) . . ?
N4 C2 N3 123.8(4) . . ?

_refine_diff_density_max         1.629
_refine_diff_density_min         -2.315
_refine_diff_density_rms         0.259

