# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_publication_text
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
#TrackingRef '- kq136ags3-final2.cif'

# start Validation Reply Form
_vrf_CHEMW03_kq136ags3           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: A large amount of electron density (1283 electrons per unit cell) was
removed using SQUEEZE as it would not refine successfully. Based on IR
spectral evidence this is assingned as be water which has been added to the
formula in sufficient quantity to compensate for these electrons. The compound
is very difficult to isolate in the solid state and we have been unable to
acheive further characterization.
;
_vrf_PLAT043_kq136ags3           
;
PROBLEM: Check Reported Molecular Weight ................ 3058.67
RESPONSE: A large amount of electron density (1283 electrons per unit cell) was
removed using SQUEEZE as it would not refine successfully. Based on IR
spectral evidence this is assingned as be water which has been added to the
formula in sufficient quantity to compensate for these electrons. The compound
is very difficult to isolate in the solid state and we have been unable to
acheive further characterization.
;
_vrf_PLAT044_kq136ags3           
;
PROBLEM: Calculated and Reported Dx Differ .............. ?
RESPONSE: A large amount of electron density (1283 electrons per unit cell) was
removed using SQUEEZE as it would not refine successfully. Based on IR
spectral evidence this is assingned as be water which has been added to the
formula in sufficient quantity to compensate for these electrons. The compound
is very difficult to isolate in the solid state and we have been unable to
acheive further characterization.
;
# end Validation Reply Form

#Added by publCIF (Sat Jun 16 14:44:13 2012)

_audit_update_record             
;
2012-06-16 # Formatted by publCIF
;
_publ_contact_author_name        'Paul Koegerler'
_publ_contact_author_address     
;
Institut fur Anorganische Chemie, RWTH Aachen University, D-52074 Aachen,
Germany.
;
_publ_contact_author_email       paul.koegerler@ac.rwth-aachen.de
loop_
_publ_author_name
_publ_author_address
P.Koegerler
;
Institut fur Anorganische Chemie, RWTH Aachen University, D-52074 Aachen,
Germany.
;
J.Fielden
;
Ames Laboratory, Iowa State University, Ames, IA 50011, USA
;
K.Quasdorf
;
Ames Laboratory, Iowa State University, Ames, IA 50011, USA
;
L.Cronin
;
University of Glasgow, WestCHEM, Department of Chemistry, Joseph Black
Building, University Avenue, Glasgow, G12 8QQ, United Kingdom.
;

_publ_section_title              
;
ENTER SECTION TITLE
;

_publ_section_abstract           
;
ENTER ABSTRACT
;

_publ_section_exptl_refinement   
;
The structure was solved by direct methods. All non-H atoms were refined
anisotropically with restraints applied to solvent and cation atoms. H-atoms
were included in idealized positions using the riding model with thermal
parameters of 1.5 times those of the parent carbon atoms. SIMU and DELU
restraints were applied to the thermal parameters of all the cation and solvent
atoms. SAME was used on the disordered MeCN molecules. There is a large amount
of void space. Electron density in this void space was removed using the
<i>PLATON</i> squeeze routine as it comes from disordered solvent which could
not be refined successfully. Based on IR spectral evidence this is water,
which has been added to the sum formula in sufficient quantity to compensate
for the electron density removed by SQUEEZE. 3 protons per formula unit have
been added for charge balance, as no other cations were located. IR spectra
do not provide evidence for NH4+ or NBu4+ and no other typical cations were
included in the synthesis.
;

data_kq136ags3
_database_code_depnum_ccdc_archive 'CCDC 869892'
#TrackingRef '- kq136ags3-final2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
3 (H), C8 H12 Cu N4, F4 Mo12 O46 P4, 4(C2 H3 N), 32 (H2 O)
;
_chemical_formula_sum            'C16 H91 Cu F4 Mo12 N8 O78 P4'
_chemical_formula_weight         3058.67

_platon_squeeze_results          
;
Note: Data are Listed for all Voids in the P1 Unit Cell i.e. Centre of Gravity,
Solvent Accessible Volume, Recovered number of Electrons in the Void and
Details about the Squeezed Material
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 129 33 ' '
2 0.000 0.000 0.500 129 33 ' '
3 0.250 -0.014 -0.009 2294 576 ' '
4 0.750 -0.011 -0.003 2294 577 ' '
5 0.500 0.500 0.000 120 32 ' '
6 0.500 0.500 0.500 120 32 ' '
_platon_squeeze_details          
;
The void space is occupied by disordered solvent (assumed to be water on IR
spectral evidence) which does not refine successfully.
;

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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Cmcm

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

_cell_length_a                   30.162(5)
_cell_length_b                   17.875(3)
_cell_length_c                   20.715(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11168(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    996
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      24.92

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5984
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6380
_exptl_absorpt_correction_T_max  0.7903
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41216
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.32
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5187
_reflns_number_gt                3518
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. SIMU and DELU restraints
were applied to the thermal parameters of all the cation and solvent atoms,
and SAME was used on the disordered MeCN molecules.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5187
_refine_ls_number_parameters     265
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0671
_refine_ls_wR_factor_ref         0.2098
_refine_ls_wR_factor_gt          0.1979
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.056
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.3838(2) 0.6657(4) 0.2500 0.0568(18) Uani 1 2 d S . .
F2 F 0.5000 0.9393(3) 0.0809(3) 0.0554(18) Uani 1 2 d S . .
Mo1 Mo 0.43893(3) 1.00909(5) 0.2500 0.0425(3) Uani 1 2 d S . .
Mo4 Mo 0.5000 0.59533(5) 0.16118(5) 0.0483(3) Uani 1 2 d S . .
Mo2 Mo 0.38341(3) 0.87415(4) 0.16898(4) 0.0531(3) Uani 1 1 d . . .
Mo3 Mo 0.44425(3) 0.72952(4) 0.08069(4) 0.0522(3) Uani 1 1 d . . .
P2 P 0.5000 0.89035(14) 0.14286(14) 0.0376(6) Uani 1 2 d S . .
P1 P 0.42676(10) 0.71455(14) 0.2500 0.0394(7) Uani 1 2 d S . .
O1 O 0.4223(2) 1.0612(3) 0.3138(3) 0.0611(16) Uani 1 1 d . . .
O2 O 0.5000 1.0270(5) 0.2500 0.046(3) Uani 1 4 d S . .
O3 O 0.3893(2) 0.9366(4) 0.2500 0.0396(17) Uani 1 2 d S . .
O4 O 0.3315(2) 0.8419(4) 0.1825(4) 0.086(2) Uani 1 1 d . . .
O5 O 0.3736(3) 0.9459(4) 0.1164(3) 0.078(2) Uani 1 1 d . . .
O6 O 0.4104(2) 0.7945(4) 0.2500 0.0421(18) Uani 1 2 d S . .
O7 O 0.45108(18) 0.6938(3) 0.1888(3) 0.0430(13) Uani 1 1 d . . .
O8 O 0.40582(19) 0.8025(3) 0.1121(3) 0.0537(15) Uani 1 1 d . . .
O9 O 0.5000 0.8110(4) 0.1186(4) 0.0407(17) Uani 1 2 d S . .
O10 O 0.54173(17) 0.9116(3) 0.1785(3) 0.0389(12) Uani 1 1 d . . .
O11 O 0.4517(3) 0.7586(4) 0.0042(4) 0.082(2) Uani 1 1 d . . .
O12 O 0.4096(2) 0.6563(4) 0.0689(4) 0.075(2) Uani 1 1 d . . .
O13 O 0.5000 0.6693(4) 0.0878(4) 0.0433(18) Uani 1 2 d S . .
O14 O 0.5000 0.5792(5) 0.2500 0.051(3) Uani 1 4 d S . .
O15 O 0.5442(2) 0.5435(3) 0.1363(3) 0.0650(18) Uani 1 1 d . . .
C1 C 0.1104(6) 0.0283(11) 0.7500 0.100(5) Uani 1 2 d SU . .
H1A H 0.1388 0.0542 0.7446 0.150 Uiso 0.50 1 calc PR . .
H1B H 0.1062 -0.0070 0.7144 0.150 Uiso 0.50 1 calc PR . .
H1C H 0.1105 0.0011 0.7911 0.150 Uiso 0.50 1 calc PR . .
C2 C 0.0760(8) 0.0805(11) 0.7500 0.104(6) Uani 1 2 d SU . .
C3 C 0.0000 0.3717(9) 0.5932(11) 0.119(7) Uani 1 2 d SU . .
H3A H 0.0269 0.4020 0.5979 0.178 Uiso 0.50 1 calc PR . .
H3B H -0.0261 0.4035 0.5993 0.178 Uiso 0.50 1 calc PR . .
H3C H -0.0008 0.3495 0.5500 0.178 Uiso 1 2 calc SR . .
C4 C 0.0000 0.3142(11) 0.6401(13) 0.117(6) Uani 1 2 d SU . .
Cu1 Cu 0.0000 0.1945(2) 0.7500 0.1501(18) Uani 1 4 d SU . .
N1 N 0.0506(6) 0.1260(11) 0.7500 0.124(6) Uani 1 2 d SU . .
N2 N 0.0000 0.2666(10) 0.6723(12) 0.137(6) Uani 1 2 d SU . .
C5 C 0.3370(4) 0.7509(10) 0.9001(10) 0.105(7) Uani 0.690(14) 1 d PDU A 1
H5A H 0.3063 0.7662 0.9085 0.157 Uiso 0.690(14) 1 calc PR A 1
H5B H 0.3458 0.7676 0.8569 0.157 Uiso 0.690(14) 1 calc PR A 1
H5C H 0.3566 0.7735 0.9324 0.157 Uiso 0.690(14) 1 calc PR A 1
C6 C 0.3405(7) 0.6643(13) 0.9041(17) 0.108(7) Uani 0.690(14) 1 d PDU A 1
N3 N 0.3328(5) 0.5884(9) 0.9101(9) 0.099(6) Uani 0.690(14) 1 d PDU A 1
C5B C 0.3955(13) 0.620(2) 0.915(2) 0.135(18) Uani 0.310(14) 1 d PDU A 2
H5B1 H 0.4095 0.6654 0.9317 0.202 Uiso 0.310(14) 1 calc PR A 2
H5B2 H 0.4097 0.6060 0.8740 0.202 Uiso 0.310(14) 1 calc PR A 2
H5B3 H 0.3988 0.5793 0.9460 0.202 Uiso 0.310(14) 1 calc PR A 2
C6B C 0.3442(14) 0.636(3) 0.903(4) 0.112(14) Uani 0.310(14) 1 d PDU A 2
N3B N 0.3039(9) 0.6332(16) 0.8687(18) 0.092(10) Uani 0.310(14) 1 d PDU A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
F1 0.053(4) 0.039(4) 0.078(5) 0.000 0.000 -0.019(3)
F2 0.079(5) 0.036(3) 0.052(4) 0.022(3) 0.000 0.000
Mo1 0.0523(6) 0.0203(5) 0.0550(6) 0.000 0.000 0.0049(4)
Mo4 0.0796(8) 0.0192(5) 0.0460(6) -0.0051(4) 0.000 0.000
Mo2 0.0580(5) 0.0400(5) 0.0615(5) -0.0036(4) -0.0029(4) 0.0011(3)
Mo3 0.0672(6) 0.0347(4) 0.0547(5) -0.0021(3) -0.0028(4) -0.0009(3)
P2 0.0519(17) 0.0209(13) 0.0399(15) 0.0026(11) 0.000 0.000
P1 0.0531(17) 0.0211(13) 0.0442(16) 0.000 0.000 -0.0035(12)
O1 0.068(4) 0.033(3) 0.082(4) -0.005(3) 0.005(3) 0.006(3)
O2 0.074(8) 0.008(4) 0.054(7) 0.000 0.000 0.000
O3 0.040(4) 0.029(4) 0.050(4) 0.000 0.000 0.005(3)
O4 0.069(5) 0.090(5) 0.100(6) -0.016(5) -0.015(4) -0.007(4)
O5 0.105(6) 0.055(4) 0.074(5) -0.003(4) -0.019(4) 0.014(4)
O6 0.053(5) 0.030(4) 0.044(4) 0.000 0.000 0.000(3)
O7 0.059(3) 0.021(2) 0.048(3) -0.004(2) -0.004(3) 0.001(2)
O8 0.064(4) 0.045(3) 0.052(4) -0.007(3) -0.014(3) 0.003(3)
O9 0.057(5) 0.021(3) 0.045(4) -0.002(3) 0.000 0.000
O10 0.047(3) 0.021(2) 0.049(3) -0.004(2) 0.001(2) -0.005(2)
O11 0.114(6) 0.077(5) 0.054(4) 0.007(4) 0.006(4) 0.031(4)
O12 0.097(5) 0.053(4) 0.076(5) -0.013(4) -0.010(4) -0.012(4)
O13 0.065(5) 0.023(4) 0.042(4) -0.005(3) 0.000 0.000
O14 0.094(9) 0.007(5) 0.051(7) 0.000 0.000 0.000
O15 0.102(5) 0.028(3) 0.065(4) -0.009(3) 0.002(4) 0.016(3)
C1 0.100(12) 0.089(12) 0.111(14) 0.000 0.000 -0.019(7)
C2 0.104(13) 0.061(11) 0.146(16) 0.000 0.000 -0.032(6)
C3 0.146(17) 0.039(8) 0.171(18) -0.030(7) 0.000 0.000
C4 0.153(16) 0.045(9) 0.155(15) -0.042(6) 0.000 0.000
Cu1 0.168(4) 0.059(2) 0.223(5) 0.000 0.000 0.000
N1 0.099(11) 0.097(12) 0.176(16) 0.000 0.000 -0.017(6)
N2 0.147(14) 0.072(11) 0.191(16) -0.007(8) 0.000 0.000
C5 0.036(8) 0.126(10) 0.153(17) 0.077(13) -0.026(9) -0.040(8)
C6 0.087(12) 0.109(10) 0.128(15) -0.061(13) -0.066(11) 0.046(10)
N3 0.068(9) 0.109(9) 0.122(13) -0.062(11) -0.018(9) 0.013(9)
C5B 0.20(3) 0.10(3) 0.11(3) -0.09(2) -0.10(3) 0.10(3)
C6B 0.15(2) 0.09(3) 0.10(2) -0.01(3) -0.009(19) 0.03(3)
N3B 0.073(15) 0.063(17) 0.14(3) 0.009(18) 0.050(14) 0.006(15)

_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
F1 P1 1.562(7) . ?
F2 P2 1.554(6) . ?
Mo1 O1 1.693(6) 10_556 ?
Mo1 O1 1.693(6) . ?
Mo1 O2 1.8697(18) . ?
Mo1 O3 1.981(7) . ?
Mo1 O10 2.360(5) 3_655 ?
Mo1 O10 2.360(5) 12_655 ?
Mo4 O15 1.703(6) . ?
Mo4 O15 1.703(6) 12_655 ?
Mo4 O14 1.8623(17) . ?
Mo4 O13 2.014(7) . ?
Mo4 O7 2.367(5) 12_655 ?
Mo4 O7 2.367(5) . ?
Mo2 O4 1.693(7) . ?
Mo2 O5 1.710(7) . ?
Mo2 O8 1.867(6) . ?
Mo2 O3 2.023(4) . ?
Mo2 O6 2.347(5) . ?
Mo2 O10 2.363(5) 12_655 ?
Mo3 O11 1.683(7) . ?
Mo3 O12 1.692(6) . ?
Mo3 O8 1.862(6) . ?
Mo3 O13 2.002(4) . ?
Mo3 O7 2.339(5) . ?
Mo3 O9 2.359(5) . ?
P2 O9 1.506(7) . ?
P2 O10 1.508(5) . ?
P2 O10 1.508(5) 12_655 ?
P1 O7 1.510(6) . ?
P1 O7 1.510(6) 10_556 ?
P1 O6 1.511(7) . ?
O2 Mo1 1.8697(18) 3_655 ?
O3 Mo2 2.023(4) 10_556 ?
O6 Mo2 2.347(5) 10_556 ?
O9 Mo3 2.359(5) 12_655 ?
O10 Mo1 2.360(5) 3_655 ?
O10 Mo2 2.363(5) 12_655 ?
O13 Mo3 2.002(4) 12_655 ?
O14 Mo4 1.8623(17) 10_556 ?
C1 C2 1.40(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.12(2) . ?
C3 C4 1.41(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N2 1.08(3) . ?
Cu1 N1 1.96(2) . ?
Cu1 N1 1.96(2) 3_556 ?
Cu1 N2 2.06(2) . ?
Cu1 N2 2.06(2) 10_557 ?
C5 C6 1.55(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N3 1.38(3) . ?
C5B C6B 1.59(3) . ?
C5B H5B1 0.9800 . ?
C5B H5B2 0.9800 . ?
C5B H5B3 0.9800 . ?
C6B N3B 1.40(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O1 102.7(4) 10_556 . ?
O1 Mo1 O2 101.4(3) 10_556 . ?
O1 Mo1 O2 101.4(3) . . ?
O1 Mo1 O3 97.8(2) 10_556 . ?
O1 Mo1 O3 97.8(2) . . ?
O2 Mo1 O3 149.0(3) . . ?
O1 Mo1 O10 165.7(2) 10_556 3_655 ?
O1 Mo1 O10 89.4(2) . 3_655 ?
O2 Mo1 O10 83.3(2) . 3_655 ?
O3 Mo1 O10 72.77(19) . 3_655 ?
O1 Mo1 O10 89.4(2) 10_556 12_655 ?
O1 Mo1 O10 165.7(2) . 12_655 ?
O2 Mo1 O10 83.3(2) . 12_655 ?
O3 Mo1 O10 72.77(19) . 12_655 ?
O10 Mo1 O10 77.7(2) 3_655 12_655 ?
O15 Mo4 O15 102.9(4) . 12_655 ?
O15 Mo4 O14 102.4(3) . . ?
O15 Mo4 O14 102.4(3) 12_655 . ?
O15 Mo4 O13 97.4(3) . . ?
O15 Mo4 O13 97.4(3) 12_655 . ?
O14 Mo4 O13 147.9(3) . . ?
O15 Mo4 O7 89.5(3) . 12_655 ?
O15 Mo4 O7 165.0(2) 12_655 12_655 ?
O14 Mo4 O7 82.9(3) . 12_655 ?
O13 Mo4 O7 72.2(2) . 12_655 ?
O15 Mo4 O7 165.0(3) . . ?
O15 Mo4 O7 89.5(3) 12_655 . ?
O14 Mo4 O7 82.9(3) . . ?
O13 Mo4 O7 72.2(2) . . ?
O7 Mo4 O7 77.1(3) 12_655 . ?
O4 Mo2 O5 101.6(4) . . ?
O4 Mo2 O8 101.9(3) . . ?
O5 Mo2 O8 100.1(3) . . ?
O4 Mo2 O3 97.5(3) . . ?
O5 Mo2 O3 97.5(3) . . ?
O8 Mo2 O3 150.5(3) . . ?
O4 Mo2 O6 89.8(3) . . ?
O5 Mo2 O6 166.3(3) . . ?
O8 Mo2 O6 84.8(2) . . ?
O3 Mo2 O6 73.2(2) . . ?
O4 Mo2 O10 165.2(3) . 12_655 ?
O5 Mo2 O10 90.3(3) . 12_655 ?
O8 Mo2 O10 84.3(2) . 12_655 ?
O3 Mo2 O10 72.0(2) . 12_655 ?
O6 Mo2 O10 77.3(2) . 12_655 ?
O11 Mo3 O12 100.7(4) . . ?
O11 Mo3 O8 101.3(3) . . ?
O12 Mo3 O8 102.0(3) . . ?
O11 Mo3 O13 97.1(3) . . ?
O12 Mo3 O13 96.5(3) . . ?
O8 Mo3 O13 150.9(3) . . ?
O11 Mo3 O7 167.1(3) . . ?
O12 Mo3 O7 88.9(3) . . ?
O8 Mo3 O7 84.9(2) . . ?
O13 Mo3 O7 73.0(2) . . ?
O11 Mo3 O9 91.6(3) . . ?
O12 Mo3 O9 164.9(3) . . ?
O8 Mo3 O9 84.0(2) . . ?
O13 Mo3 O9 73.1(2) . . ?
O7 Mo3 O9 77.7(2) . . ?
O9 P2 O10 113.6(2) . . ?
O9 P2 O10 113.6(2) . 12_655 ?
O10 P2 O10 113.2(4) . 12_655 ?
O9 P2 F2 104.7(4) . . ?
O10 P2 F2 105.3(3) . . ?
O10 P2 F2 105.3(3) 12_655 . ?
O7 P1 O7 114.0(4) . 10_556 ?
O7 P1 O6 113.0(2) . . ?
O7 P1 O6 113.0(2) 10_556 . ?
O7 P1 F1 105.4(3) . . ?
O7 P1 F1 105.4(3) 10_556 . ?
O6 P1 F1 105.0(4) . . ?
Mo1 O2 Mo1 160.3(5) . 3_655 ?
Mo1 O3 Mo2 115.3(2) . 10_556 ?
Mo1 O3 Mo2 115.3(2) . . ?
Mo2 O3 Mo2 112.1(3) 10_556 . ?
P1 O6 Mo2 133.38(14) . 10_556 ?
P1 O6 Mo2 133.38(14) . . ?
Mo2 O6 Mo2 91.3(2) 10_556 . ?
P1 O7 Mo3 133.9(3) . . ?
P1 O7 Mo4 133.5(3) . . ?
Mo3 O7 Mo4 91.49(19) . . ?
Mo3 O8 Mo2 157.9(3) . . ?
P2 O9 Mo3 133.86(13) . . ?
P2 O9 Mo3 133.86(13) . 12_655 ?
Mo3 O9 Mo3 91.0(2) . 12_655 ?
P2 O10 Mo1 134.4(3) . 3_655 ?
P2 O10 Mo2 133.3(3) . 12_655 ?
Mo1 O10 Mo2 91.45(18) 3_655 12_655 ?
Mo3 O13 Mo3 114.2(3) . 12_655 ?
Mo3 O13 Mo4 114.1(2) . . ?
Mo3 O13 Mo4 114.1(2) 12_655 . ?
Mo4 O14 Mo4 162.2(5) 10_556 . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 175(2) . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 C3 175(2) . . ?
N1 Cu1 N1 102.4(10) . 3_556 ?
N1 Cu1 N2 113.0(4) . . ?
N1 Cu1 N2 113.0(4) 3_556 . ?
N1 Cu1 N2 113.0(4) . 10_557 ?
N1 Cu1 N2 113.0(4) 3_556 10_557 ?
N2 Cu1 N2 102.7(11) . 10_557 ?
C2 N1 Cu1 172.2(18) . . ?
C4 N2 Cu1 167(2) . . ?
N3 C6 C5 166(2) . . ?
C6B C5B H5B1 109.5 . . ?
C6B C5B H5B2 109.5 . . ?
H5B1 C5B H5B2 109.5 . . ?
C6B C5B H5B3 109.5 . . ?
H5B1 C5B H5B3 109.5 . . ?
H5B2 C5B H5B3 109.5 . . ?
N3B C6B C5B 156(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Mo1 O2 Mo1 -127.2(2) 10_556 . . 3_655 ?
O1 Mo1 O2 Mo1 127.2(2) . . . 3_655 ?
O3 Mo1 O2 Mo1 0.0 . . . 3_655 ?
O10 Mo1 O2 Mo1 39.18(12) 3_655 . . 3_655 ?
O10 Mo1 O2 Mo1 -39.18(12) 12_655 . . 3_655 ?
O1 Mo1 O3 Mo2 -165.5(3) 10_556 . . 10_556 ?
O1 Mo1 O3 Mo2 -61.5(4) . . . 10_556 ?
O2 Mo1 O3 Mo2 66.5(3) . . . 10_556 ?
O10 Mo1 O3 Mo2 25.5(3) 3_655 . . 10_556 ?
O10 Mo1 O3 Mo2 107.6(3) 12_655 . . 10_556 ?
O1 Mo1 O3 Mo2 61.5(4) 10_556 . . . ?
O1 Mo1 O3 Mo2 165.5(3) . . . . ?
O2 Mo1 O3 Mo2 -66.5(3) . . . . ?
O10 Mo1 O3 Mo2 -107.6(3) 3_655 . . . ?
O10 Mo1 O3 Mo2 -25.5(3) 12_655 . . . ?
O4 Mo2 O3 Mo1 -165.2(4) . . . . ?
O5 Mo2 O3 Mo1 -62.4(4) . . . . ?
O8 Mo2 O3 Mo1 63.8(6) . . . . ?
O6 Mo2 O3 Mo1 107.3(4) . . . . ?
O10 Mo2 O3 Mo1 25.6(3) 12_655 . . . ?
O4 Mo2 O3 Mo2 60.3(4) . . . 10_556 ?
O5 Mo2 O3 Mo2 163.1(4) . . . 10_556 ?
O8 Mo2 O3 Mo2 -70.7(6) . . . 10_556 ?
O6 Mo2 O3 Mo2 -27.2(3) . . . 10_556 ?
O10 Mo2 O3 Mo2 -109.0(3) 12_655 . . 10_556 ?
O7 P1 O6 Mo2 -166.0(4) . . . 10_556 ?
O7 P1 O6 Mo2 -34.7(7) 10_556 . . 10_556 ?
F1 P1 O6 Mo2 79.6(5) . . . 10_556 ?
O7 P1 O6 Mo2 34.7(7) . . . . ?
O7 P1 O6 Mo2 166.0(4) 10_556 . . . ?
F1 P1 O6 Mo2 -79.6(5) . . . . ?
O4 Mo2 O6 P1 88.6(6) . . . . ?
O5 Mo2 O6 P1 -124.9(12) . . . . ?
O8 Mo2 O6 P1 -13.4(6) . . . . ?
O3 Mo2 O6 P1 -173.5(6) . . . . ?
O10 Mo2 O6 P1 -98.7(6) 12_655 . . . ?
O4 Mo2 O6 Mo2 -76.5(3) . . . 10_556 ?
O5 Mo2 O6 Mo2 70.0(13) . . . 10_556 ?
O8 Mo2 O6 Mo2 -178.5(3) . . . 10_556 ?
O3 Mo2 O6 Mo2 21.4(2) . . . 10_556 ?
O10 Mo2 O6 Mo2 96.2(2) 12_655 . . 10_556 ?
O7 P1 O7 Mo3 -163.56(14) 10_556 . . . ?
O6 P1 O7 Mo3 -32.8(6) . . . . ?
F1 P1 O7 Mo3 81.4(5) . . . . ?
O7 P1 O7 Mo4 31.8(7) 10_556 . . . ?
O6 P1 O7 Mo4 162.6(4) . . . . ?
F1 P1 O7 Mo4 -83.3(5) . . . . ?
O11 Mo3 O7 P1 129.5(12) . . . . ?
O12 Mo3 O7 P1 -91.9(5) . . . . ?
O8 Mo3 O7 P1 10.2(4) . . . . ?
O13 Mo3 O7 P1 171.0(5) . . . . ?
O9 Mo3 O7 P1 95.2(4) . . . . ?
O11 Mo3 O7 Mo4 -61.6(13) . . . . ?
O12 Mo3 O7 Mo4 77.0(3) . . . . ?
O8 Mo3 O7 Mo4 179.1(2) . . . . ?
O13 Mo3 O7 Mo4 -20.1(2) . . . . ?
O9 Mo3 O7 Mo4 -95.91(18) . . . . ?
O15 Mo4 O7 P1 -123.1(10) . . . . ?
O15 Mo4 O7 P1 91.1(5) 12_655 . . . ?
O14 Mo4 O7 P1 -11.5(4) . . . . ?
O13 Mo4 O7 P1 -170.9(5) . . . . ?
O7 Mo4 O7 P1 -95.7(4) 12_655 . . . ?
O15 Mo4 O7 Mo3 68.0(10) . . . . ?
O15 Mo4 O7 Mo3 -77.9(3) 12_655 . . . ?
O14 Mo4 O7 Mo3 179.6(2) . . . . ?
O13 Mo4 O7 Mo3 20.09(17) . . . . ?
O7 Mo4 O7 Mo3 95.28(16) 12_655 . . . ?
O11 Mo3 O8 Mo2 -132.4(9) . . . . ?
O12 Mo3 O8 Mo2 123.9(10) . . . . ?
O13 Mo3 O8 Mo2 -4.3(13) . . . . ?
O7 Mo3 O8 Mo2 36.1(9) . . . . ?
O9 Mo3 O8 Mo2 -42.0(9) . . . . ?
O4 Mo2 O8 Mo3 -123.7(10) . . . . ?
O5 Mo2 O8 Mo3 132.0(10) . . . . ?
O3 Mo2 O8 Mo3 6.4(13) . . . . ?
O6 Mo2 O8 Mo3 -35.0(9) . . . . ?
O10 Mo2 O8 Mo3 42.7(9) 12_655 . . . ?
O10 P2 O9 Mo3 164.2(4) . . . . ?
O10 P2 O9 Mo3 32.9(7) 12_655 . . . ?
F2 P2 O9 Mo3 -81.4(5) . . . . ?
O10 P2 O9 Mo3 -32.9(7) . . . 12_655 ?
O10 P2 O9 Mo3 -164.2(4) 12_655 . . 12_655 ?
F2 P2 O9 Mo3 81.4(5) . . . 12_655 ?
O11 Mo3 O9 P2 90.3(6) . . . . ?
O12 Mo3 O9 P2 -125.0(11) . . . . ?
O8 Mo3 O9 P2 -10.9(6) . . . . ?
O13 Mo3 O9 P2 -172.7(7) . . . . ?
O7 Mo3 O9 P2 -96.9(6) . . . . ?
O11 Mo3 O9 Mo3 -77.4(3) . . . 12_655 ?
O12 Mo3 O9 Mo3 67.3(11) . . . 12_655 ?
O8 Mo3 O9 Mo3 -178.6(3) . . . 12_655 ?
O13 Mo3 O9 Mo3 19.6(3) . . . 12_655 ?
O7 Mo3 O9 Mo3 95.3(2) . . . 12_655 ?
O9 P2 O10 Mo1 -162.7(4) . . . 3_655 ?
O10 P2 O10 Mo1 -31.2(7) 12_655 . . 3_655 ?
F2 P2 O10 Mo1 83.3(5) . . . 3_655 ?
O9 P2 O10 Mo2 31.4(6) . . . 12_655 ?
O10 P2 O10 Mo2 162.94(13) 12_655 . . 12_655 ?
F2 P2 O10 Mo2 -82.6(4) . . . 12_655 ?
O11 Mo3 O13 Mo3 63.8(4) . . . 12_655 ?
O12 Mo3 O13 Mo3 165.6(4) . . . 12_655 ?
O8 Mo3 O13 Mo3 -65.1(7) . . . 12_655 ?
O7 Mo3 O13 Mo3 -107.6(4) . . . 12_655 ?
O9 Mo3 O13 Mo3 -25.6(3) . . . 12_655 ?
O11 Mo3 O13 Mo4 -162.3(4) . . . . ?
O12 Mo3 O13 Mo4 -60.6(4) . . . . ?
O8 Mo3 O13 Mo4 68.7(6) . . . . ?
O7 Mo3 O13 Mo4 26.3(3) . . . . ?
O9 Mo3 O13 Mo4 108.2(4) . . . . ?
O15 Mo4 O13 Mo3 165.1(3) . . . . ?
O15 Mo4 O13 Mo3 61.0(4) 12_655 . . . ?
O14 Mo4 O13 Mo3 -67.0(3) . . . . ?
O7 Mo4 O13 Mo3 -107.8(3) 12_655 . . . ?
O7 Mo4 O13 Mo3 -26.1(3) . . . . ?
O15 Mo4 O13 Mo3 -61.0(4) . . . 12_655 ?
O15 Mo4 O13 Mo3 -165.1(3) 12_655 . . 12_655 ?
O14 Mo4 O13 Mo3 67.0(3) . . . 12_655 ?
O7 Mo4 O13 Mo3 26.1(3) 12_655 . . 12_655 ?
O7 Mo4 O13 Mo3 107.8(3) . . . 12_655 ?
O15 Mo4 O14 Mo4 126.8(2) . . . 10_556 ?
O15 Mo4 O14 Mo4 -126.8(2) 12_655 . . 10_556 ?
O13 Mo4 O14 Mo4 0.000(4) . . . 10_556 ?
O7 Mo4 O14 Mo4 38.92(13) 12_655 . . 10_556 ?
O7 Mo4 O14 Mo4 -38.91(13) . . . 10_556 ?
C1 C2 N1 Cu1 180.0 . . . . ?
N1 Cu1 N1 C2 0.0 3_556 . . . ?
N2 Cu1 N1 C2 -122.0(5) . . . . ?
N2 Cu1 N1 C2 122.0(5) 10_557 . . . ?
C3 C4 N2 Cu1 180.00(5) . . . . ?
N1 Cu1 N2 C4 -122.1(5) . . . . ?
N1 Cu1 N2 C4 122.1(5) 3_556 . . . ?
N2 Cu1 N2 C4 0.00(2) 10_557 . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.149
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.181