# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H33 Cr Cu2 Mo6 N4 O32'
_chemical_formula_weight         1548.18

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'
Cr Cr 0.3209 0.6236 '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           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.299(2)
_cell_length_b                   11.469(4)
_cell_length_c                   11.601(4)
_cell_angle_alpha                103.137(4)
_cell_angle_beta                 99.656(5)
_cell_angle_gamma                102.478(5)
_cell_volume                     899.1(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4029
_cell_measurement_theta_min      2.9874
_cell_measurement_theta_max      28.2953

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            'DARK GREEN'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             747
_exptl_absorpt_coefficient_mu    3.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_T_max  0.506
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_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            4503
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3147
_reflns_number_gt                2900
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1040P)²+17.7129P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3147
_refine_ls_number_parameters     277
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1790
_refine_ls_wR_factor_gt          0.1763
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.25817(11) 1.66823(7) 0.15864(6) 0.0113(3) Uani 1 1 d . . .
O1W O 0.5991(18) 2.0466(11) 0.2577(14) 0.085(5) Uani 1 1 d . . .
C1 C 0.0397(17) 1.1411(10) 0.3343(10) 0.028(2) Uani 1 1 d U . .
H1A H -0.0294 1.1588 0.2685 0.034 Uiso 1 1 calc R . .
Cr1 Cr 0.5000 1.5000 0.0000 0.0083(4) Uani 1 2 d S . .
Cu1 Cu 0.0955(2) 1.40730(13) 0.44107(12) 0.0314(4) Uani 1 1 d . . .
O8 O 0.6695(9) 1.5028(6) 0.1504(5) 0.0149(13) Uani 1 1 d . . .
N1 N 0.1082(14) 1.2332(9) 0.4371(8) 0.032(2) Uani 1 1 d . . .
Mo2 Mo 0.45846(11) 1.46967(7) 0.27386(6) 0.0112(3) Uani 1 1 d . . .
O9 O 0.2854(9) 1.4699(6) 0.0847(5) 0.0122(12) Uani 1 1 d . . .
C2 C 0.2047(17) 1.2030(10) 0.5264(11) 0.033(3) Uani 1 1 d . . .
H2A H 0.2549 1.2648 0.5994 0.040 Uiso 1 1 calc R . .
N2 N 0.0051(11) 0.9490(7) 0.0993(6) 0.0148(15) Uani 1 1 d . . .
O2W O -0.365(2) 1.2161(13) 0.4490(17) 0.100(5) Uani 1 1 d . . .
Mo3 Mo 0.69320(11) 1.30344(7) 0.11336(7) 0.0122(3) Uani 1 1 d . . .
O7 O 0.4987(9) 1.6740(6) 0.0547(5) 0.0132(13) Uani 1 1 d . . .
C3 C 0.2400(17) 1.0880(13) 0.5231(10) 0.036(3) Uani 1 1 d U . .
H3A H 0.3100 1.0744 0.5912 0.043 Uiso 1 1 calc R . .
O14 O 0.4726(9) 1.3135(6) 0.1828(5) 0.0139(13) Uani 1 1 d U . .
C4 C 0.1640(16) 0.9903(14) 0.4104(10) 0.036(3) Uani 1 1 d . . .
H4A H 0.1835 0.9117 0.4026 0.044 Uiso 1 1 calc R . .
O5 O 0.4453(9) 1.6341(5) 0.2744(5) 0.0136(13) Uani 1 1 d . . .
C5 C 0.0619(14) 1.0197(10) 0.3160(8) 0.022(2) Uani 1 1 d U . .
C6 C -0.0397(12) 0.9242(8) 0.1986(8) 0.0127(17) Uani 1 1 d . . .
O6 O 0.6310(11) 1.1464(6) 0.0575(7) 0.0251(16) Uani 1 1 d . . .
C7 C 0.1703(13) 1.0476(9) 0.0961(8) 0.0164(18) Uani 1 1 d . . .
H7A H 0.2632 1.0105 0.0615 0.020 Uiso 1 1 calc R . .
H7B H 0.2332 1.0982 0.1782 0.020 Uiso 1 1 calc R . .
O4 O 0.8642(10) 1.3369(7) 0.2451(7) 0.0244(16) Uani 1 1 d . . .
O3 O 0.6489(9) 1.5083(6) 0.3962(5) 0.0159(13) Uani 1 1 d . . .
C8 C -0.1016(14) 0.8718(8) -0.0202(8) 0.0154(18) Uani 1 1 d . . .
H8A H -0.2114 0.8112 -0.0130 0.018 Uiso 1 1 calc R . .
H8B H -0.0197 0.8275 -0.0596 0.018 Uiso 1 1 calc R . .
O1 O 0.2573(9) 1.4170(6) 0.3254(6) 0.0166(13) Uani 1 1 d . . .
O10 O 0.3253(9) 1.8260(6) 0.2125(6) 0.0172(14) Uani 1 1 d . . .
O11 O 0.1426(9) 1.6457(6) -0.0090(6) 0.0144(13) Uani 1 1 d . . .
O12 O -0.1670(10) 0.8312(6) 0.1978(6) 0.0210(14) Uani 1 1 d . . .
O13 O 0.0531(9) 1.6195(6) 0.2086(6) 0.0174(13) Uani 1 1 d . . .
O2 O -0.0820(10) 1.4171(6) 0.5517(6) 0.0228(15) 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 O10 1.704(6) . ?
Mo1 O13 1.722(7) . ?
Mo1 O5 1.917(6) . ?
Mo1 O11 1.920(6) . ?
Mo1 O7 2.288(6) . ?
Mo1 O9 2.306(6) . ?
C1 N1 1.336(14) . ?
C1 C5 1.409(16) . ?
Cr1 O8 1.952(6) . ?
Cr1 O8 1.952(6) 2_685 ?
Cr1 O7 1.954(6) 2_685 ?
Cr1 O7 1.954(6) . ?
Cr1 O9 1.994(6) . ?
Cr1 O9 1.994(6) 2_685 ?
Cu1 O1 1.937(6) . ?
Cu1 O2 1.973(6) . ?
Cu1 N1 2.010(10) . ?
Cu1 O2 2.021(7) 2_586 ?
Cu1 O3 2.278(7) 2_686 ?
Cu1 Cu1 2.989(3) 2_586 ?
O8 Mo3 2.278(7) . ?
O8 Mo2 2.302(6) . ?
N1 C2 1.308(16) . ?
Mo2 O3 1.712(6) . ?
Mo2 O1 1.719(6) . ?
Mo2 O14 1.895(6) . ?
Mo2 O5 1.908(6) . ?
Mo2 O9 2.342(6) . ?
C2 C3 1.390(18) . ?
N2 C6 1.323(12) . ?
N2 C8 1.448(11) . ?
N2 C7 1.476(12) . ?
Mo3 O6 1.699(7) . ?
Mo3 O4 1.711(7) . ?
Mo3 O14 1.931(6) . ?
Mo3 O11 1.936(6) 2_685 ?
Mo3 O7 2.302(6) 2_685 ?
O7 Mo3 2.302(6) 2_685 ?
C3 C4 1.447(18) . ?
C4 C5 1.367(16) . ?
C5 C6 1.495(12) . ?
C6 O12 1.251(11) . ?
C7 C8 1.518(12) 2_575 ?
O3 Cu1 2.278(6) 2_686 ?
C8 C7 1.518(12) 2_575 ?
O11 Mo3 1.936(6) 2_685 ?
O2 Cu1 2.021(7) 2_586 ?

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
O10 Mo1 O13 105.6(3) . . ?
O10 Mo1 O5 97.8(3) . . ?
O13 Mo1 O5 100.2(3) . . ?
O10 Mo1 O11 101.5(3) . . ?
O13 Mo1 O11 99.1(3) . . ?
O5 Mo1 O11 147.8(3) . . ?
O10 Mo1 O7 91.0(3) . . ?
O13 Mo1 O7 162.9(3) . . ?
O5 Mo1 O7 81.7(2) . . ?
O11 Mo1 O7 72.6(2) . . ?
O10 Mo1 O9 158.9(3) . . ?
O13 Mo1 O9 94.0(3) . . ?
O5 Mo1 O9 70.6(2) . . ?
O11 Mo1 O9 82.6(2) . . ?
O7 Mo1 O9 70.3(2) . . ?
N1 C1 C5 126.3(11) . . ?
O8 Cr1 O8 179.999(2) . 2_685 ?
O8 Cr1 O7 85.5(3) . 2_685 ?
O8 Cr1 O7 94.5(3) 2_685 2_685 ?
O8 Cr1 O7 94.5(3) . . ?
O8 Cr1 O7 85.5(3) 2_685 . ?
O7 Cr1 O7 179.999(2) 2_685 . ?
O8 Cr1 O9 86.3(3) . . ?
O8 Cr1 O9 93.7(3) 2_685 . ?
O7 Cr1 O9 95.8(3) 2_685 . ?
O7 Cr1 O9 84.2(3) . . ?
O8 Cr1 O9 93.7(3) . 2_685 ?
O8 Cr1 O9 86.3(3) 2_685 2_685 ?
O7 Cr1 O9 84.2(3) 2_685 2_685 ?
O7 Cr1 O9 95.8(3) . 2_685 ?
O9 Cr1 O9 179.999(1) . 2_685 ?
O1 Cu1 O2 171.7(3) . . ?
O1 Cu1 N1 91.8(3) . . ?
O2 Cu1 N1 96.0(3) . . ?
O1 Cu1 O2 89.2(3) . 2_586 ?
O2 Cu1 O2 83.1(3) . 2_586 ?
N1 Cu1 O2 178.9(3) . 2_586 ?
O1 Cu1 O3 92.9(3) . 2_686 ?
O2 Cu1 O3 89.8(3) . 2_686 ?
N1 Cu1 O3 92.6(3) . 2_686 ?
O2 Cu1 O3 86.8(3) 2_586 2_686 ?
O1 Cu1 Cu1 130.1(2) . 2_586 ?
O2 Cu1 Cu1 42.2(2) . 2_586 ?
N1 Cu1 Cu1 138.1(3) . 2_586 ?
O2 Cu1 Cu1 40.95(18) 2_586 2_586 ?
O3 Cu1 Cu1 87.69(17) 2_686 2_586 ?
Cr1 O8 Mo3 102.3(3) . . ?
Cr1 O8 Mo2 102.7(3) . . ?
Mo3 O8 Mo2 92.3(2) . . ?
C2 N1 C1 114.2(11) . . ?
C2 N1 Cu1 124.1(8) . . ?
C1 N1 Cu1 121.1(8) . . ?
O3 Mo2 O1 105.6(3) . . ?
O3 Mo2 O14 102.7(3) . . ?
O1 Mo2 O14 97.6(3) . . ?
O3 Mo2 O5 97.6(3) . . ?
O1 Mo2 O5 101.5(3) . . ?
O14 Mo2 O5 147.1(3) . . ?
O3 Mo2 O8 89.9(3) . . ?
O1 Mo2 O8 162.9(3) . . ?
O14 Mo2 O8 71.5(2) . . ?
O5 Mo2 O8 83.1(3) . . ?
O3 Mo2 O9 158.0(3) . . ?
O1 Mo2 O9 94.8(3) . . ?
O14 Mo2 O9 82.0(2) . . ?
O5 Mo2 O9 69.9(2) . . ?
O8 Mo2 O9 71.0(2) . . ?
Cr1 O9 Mo1 101.8(3) . . ?
Cr1 O9 Mo2 100.0(3) . . ?
Mo1 O9 Mo2 92.5(2) . . ?
N1 C2 C3 126.6(11) . . ?
C6 N2 C8 121.0(8) . . ?
C6 N2 C7 125.6(8) . . ?
C8 N2 C7 113.2(7) . . ?
O6 Mo3 O4 105.8(4) . . ?
O6 Mo3 O14 96.7(3) . . ?
O4 Mo3 O14 98.7(3) . . ?
O6 Mo3 O11 101.5(3) . 2_685 ?
O4 Mo3 O11 99.3(3) . 2_685 ?
O14 Mo3 O11 149.8(3) . 2_685 ?
O6 Mo3 O8 159.8(3) . . ?
O4 Mo3 O8 92.4(3) . . ?
O14 Mo3 O8 71.5(2) . . ?
O11 Mo3 O8 83.7(2) 2_685 . ?
O6 Mo3 O7 92.2(3) . 2_685 ?
O4 Mo3 O7 161.5(3) . 2_685 ?
O14 Mo3 O7 83.5(2) . 2_685 ?
O11 Mo3 O7 72.0(2) 2_685 2_685 ?
O8 Mo3 O7 70.7(2) . 2_685 ?
Cr1 O7 Mo1 103.7(3) . . ?
Cr1 O7 Mo3 101.4(3) . 2_685 ?
Mo1 O7 Mo3 92.4(2) . 2_685 ?
C2 C3 C4 117.8(11) . . ?
Mo2 O14 Mo3 119.3(3) . . ?
C5 C4 C3 116.5(12) . . ?
Mo2 O5 Mo1 122.8(3) . . ?
C4 C5 C1 118.5(10) . . ?
C4 C5 C6 121.9(10) . . ?
C1 C5 C6 119.4(9) . . ?
O12 C6 N2 123.8(8) . . ?
O12 C6 C5 119.9(8) . . ?
N2 C6 C5 116.1(8) . . ?
N2 C7 C8 109.9(8) . 2_575 ?
Mo2 O3 Cu1 170.5(4) . 2_686 ?
N2 C8 C7 109.6(7) . 2_575 ?
Mo2 O1 Cu1 157.0(4) . . ?
Mo1 O11 Mo3 118.5(3) . 2_685 ?
Cu1 O2 Cu1 96.9(3) . 2_586 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         2.436
_refine_diff_density_min         -3.480
_refine_diff_density_rms         0.317
_database_code_depnum_ccdc_archive 'CCDC 969174'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_compound2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H38 Cr Cu2 Mo6 N4 O34'
_chemical_formula_weight         1585.22

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'
Cr Cr 0.3209 0.6236 '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           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.6170(6)
_cell_length_b                   10.4420(8)
_cell_length_c                   13.8790(11)
_cell_angle_alpha                75.7970(10)
_cell_angle_beta                 82.0180(10)
_cell_angle_gamma                71.7240(10)
_cell_volume                     1013.86(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3640
_cell_measurement_theta_min      2.8454
_cell_measurement_theta_max      28.2176

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            'DARK GREEN'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    3.189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.352
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_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            5132
_diffrn_reflns_av_R_equivalents  0.0094
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3528
_reflns_number_gt                3217
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0320P)²+2.5733P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3528
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0630
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.24762(4) 0.32527(3) 0.45438(2) 0.01341(9) Uani 1 1 d . . .
Cu1 Cu 0.84768(6) -0.46162(5) 0.23223(4) 0.01870(12) Uani 1 1 d . . .
O11 O 0.2980(4) 0.2572(3) 0.1978(2) 0.0240(6) Uani 1 1 d . . .
N1 N 1.0773(4) -0.4109(3) 0.1749(2) 0.0175(7) Uani 1 1 d . . .
Cr1 Cr 0.5000 0.0000 0.5000 0.01127(17) Uani 1 2 d S . .
C1 C 1.1644(5) -0.3677(4) 0.2319(3) 0.0184(8) Uani 1 1 d . . .
H1A H 1.1200 -0.3686 0.2979 0.022 Uiso 1 1 calc R . .
O1W O 0.9314(4) -0.6326(3) 0.1796(2) 0.0250(6) Uani 1 1 d . . .
Mo2 Mo 0.48467(4) 0.18483(3) 0.26950(2) 0.01349(9) Uani 1 1 d . . .
O8 O 0.6767(3) 0.0409(3) 0.38740(18) 0.0146(5) Uani 1 1 d . . .
C2 C 1.1447(6) -0.4126(4) 0.0797(3) 0.0241(9) Uani 1 1 d . . .
H2A H 1.0864 -0.4446 0.0399 0.029 Uiso 1 1 calc R . .
N2 N 1.5225(4) -0.1416(3) 0.0101(3) 0.0217(7) Uani 1 1 d . . .
O2W O 0.6629(4) -0.5255(4) 0.3271(2) 0.0348(8) Uani 1 1 d . . .
Mo3 Mo 0.74123(4) -0.13789(3) 0.31305(2) 0.01347(9) Uani 1 1 d . . .
O15 O 0.4690(3) 0.1652(2) 0.55316(18) 0.0138(5) Uani 1 1 d . . .
O3W O 0.9855(10) 0.0920(10) 0.4039(6) 0.177(4) Uani 1 1 d . . .
C3 C 1.2968(6) -0.3684(4) 0.0396(3) 0.0240(9) Uani 1 1 d . . .
H3A H 1.3402 -0.3698 -0.0262 0.029 Uiso 1 1 calc R . .
O4W O 1.2501(5) -0.2631(4) 0.4336(3) 0.0533(10) Uani 1 1 d . . .
O4 O 0.3146(3) 0.1263(2) 0.40723(18) 0.0140(5) Uani 1 1 d . . .
C4 C 1.3169(5) -0.3219(4) 0.1976(3) 0.0197(8) Uani 1 1 d . . .
H4A H 1.3736 -0.2918 0.2393 0.024 Uiso 1 1 calc R . .
O5 O 0.5302(3) -0.0039(3) 0.25403(19) 0.0166(5) Uani 1 1 d . . .
C5 C 1.3845(5) -0.3215(4) 0.0997(3) 0.0178(8) Uani 1 1 d . . .
O6 O 0.6679(4) 0.2284(3) 0.1980(2) 0.0229(6) Uani 1 1 d . . .
C6 C 1.5522(5) -0.2722(4) 0.0608(3) 0.0176(8) Uani 1 1 d . . .
O7 O 0.2906(4) 0.4527(3) 0.4978(2) 0.0248(6) Uani 1 1 d . . .
C7 C 1.3397(5) -0.0418(4) -0.0092(3) 0.0214(8) Uani 1 1 d . . .
H7A H 1.2435 -0.0836 0.0228 0.026 Uiso 1 1 calc R . .
H7B H 1.3245 -0.0150 -0.0802 0.026 Uiso 1 1 calc R . .
O2 O 0.0609(4) 0.4034(3) 0.3839(2) 0.0227(6) Uani 1 1 d . . .
C8 C 1.3219(6) 0.0851(4) 0.0311(3) 0.0228(9) Uani 1 1 d . . .
H8A H 1.2058 0.1545 0.0131 0.027 Uiso 1 1 calc R . .
H8B H 1.3215 0.0603 0.1032 0.027 Uiso 1 1 calc R . .
O9 O 0.4491(4) 0.3202(3) 0.34981(19) 0.0162(5) Uani 1 1 d . . .
O10 O 0.1229(3) 0.2351(3) 0.56894(19) 0.0176(6) Uani 1 1 d . . .
O1 O 0.7375(4) -0.2830(3) 0.2730(2) 0.0211(6) Uani 1 1 d . . .
O12 O 0.9163(4) -0.0864(3) 0.2423(2) 0.0241(6) Uani 1 1 d . . .
O3 O 1.7081(4) -0.3534(3) 0.0779(2) 0.0247(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 O2 1.707(3) . ?
Mo1 O7 1.721(3) . ?
Mo1 O10 1.930(3) . ?
Mo1 O9 1.957(3) . ?
Mo1 O4 2.217(2) . ?
Mo1 O15 2.295(2) . ?
Cu1 O2W 1.950(3) . ?
Cu1 O1 1.976(3) . ?
Cu1 O1W 1.981(3) . ?
Cu1 N1 1.989(3) . ?
Cu1 O3 2.384(3) 1_455 ?
O11 Mo2 1.713(3) . ?
N1 C1 1.334(5) . ?
N1 C2 1.353(5) . ?
Cr1 O8 1.971(2) . ?
Cr1 O8 1.971(2) 2_656 ?
Cr1 O4 1.973(2) . ?
Cr1 O4 1.973(2) 2_656 ?
Cr1 O15 1.974(2) 2_656 ?
Cr1 O15 1.974(2) . ?
C1 C4 1.374(5) . ?
Mo2 O6 1.712(3) . ?
Mo2 O9 1.939(2) . ?
Mo2 O5 1.951(3) . ?
Mo2 O4 2.223(2) . ?
Mo2 O8 2.270(2) . ?
O8 Mo3 2.241(2) . ?
C2 C3 1.377(6) . ?
N2 C6 1.337(5) . ?
N2 C7 1.467(5) . ?
N2 C8 1.471(5) 2_855 ?
Mo3 O12 1.690(3) . ?
Mo3 O1 1.747(3) . ?
Mo3 O5 1.899(3) . ?
Mo3 O10 1.944(3) 2_656 ?
Mo3 O15 2.301(2) 2_656 ?
O15 Mo3 2.301(2) 2_656 ?
C3 C5 1.394(6) . ?
C4 C5 1.384(6) . ?
C5 C6 1.507(5) . ?
C6 O3 1.238(5) . ?
C7 C8 1.521(6) . ?
C8 N2 1.471(5) 2_855 ?
O10 Mo3 1.944(3) 2_656 ?
O3 Cu1 2.384(3) 1_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 O7 106.66(14) . . ?
O2 Mo1 O10 97.61(12) . . ?
O7 Mo1 O10 102.62(12) . . ?
O2 Mo1 O9 100.16(12) . . ?
O7 Mo1 O9 93.88(12) . . ?
O10 Mo1 O9 151.11(11) . . ?
O2 Mo1 O4 94.47(12) . . ?
O7 Mo1 O4 156.54(12) . . ?
O10 Mo1 O4 84.11(10) . . ?
O9 Mo1 O4 72.00(9) . . ?
O2 Mo1 O15 163.23(11) . . ?
O7 Mo1 O15 88.71(11) . . ?
O10 Mo1 O15 71.91(10) . . ?
O9 Mo1 O15 85.10(10) . . ?
O4 Mo1 O15 71.86(9) . . ?
O2W Cu1 O1 85.84(13) . . ?
O2W Cu1 O1W 93.11(13) . . ?
O1 Cu1 O1W 172.52(12) . . ?
O2W Cu1 N1 161.76(14) . . ?
O1 Cu1 N1 91.56(12) . . ?
O1W Cu1 N1 91.71(12) . . ?
O2W Cu1 O3 107.67(12) . 1_455 ?
O1 Cu1 O3 87.43(11) . 1_455 ?
O1W Cu1 O3 85.83(11) . 1_455 ?
N1 Cu1 O3 90.21(12) . 1_455 ?
C1 N1 C2 118.4(3) . . ?
C1 N1 Cu1 118.4(3) . . ?
C2 N1 Cu1 123.1(3) . . ?
O8 Cr1 O8 180.0 . 2_656 ?
O8 Cr1 O4 83.09(10) . . ?
O8 Cr1 O4 96.91(10) 2_656 . ?
O8 Cr1 O4 96.91(10) . 2_656 ?
O8 Cr1 O4 83.09(10) 2_656 2_656 ?
O4 Cr1 O4 180.0 . 2_656 ?
O8 Cr1 O15 83.61(10) . 2_656 ?
O8 Cr1 O15 96.39(10) 2_656 2_656 ?
O4 Cr1 O15 95.71(10) . 2_656 ?
O4 Cr1 O15 84.29(10) 2_656 2_656 ?
O8 Cr1 O15 96.39(10) . . ?
O8 Cr1 O15 83.61(10) 2_656 . ?
O4 Cr1 O15 84.29(10) . . ?
O4 Cr1 O15 95.71(10) 2_656 . ?
O15 Cr1 O15 179.999(1) 2_656 . ?
N1 C1 C4 123.0(4) . . ?
O6 Mo2 O11 106.19(14) . . ?
O6 Mo2 O9 93.93(12) . . ?
O11 Mo2 O9 101.68(12) . . ?
O6 Mo2 O5 101.15(12) . . ?
O11 Mo2 O5 96.37(12) . . ?
O9 Mo2 O5 152.22(11) . . ?
O6 Mo2 O4 157.80(11) . . ?
O11 Mo2 O4 93.79(12) . . ?
O9 Mo2 O4 72.19(10) . . ?
O5 Mo2 O4 85.80(10) . . ?
O6 Mo2 O8 90.76(11) . . ?
O11 Mo2 O8 161.22(12) . . ?
O9 Mo2 O8 84.78(10) . . ?
O5 Mo2 O8 71.93(10) . . ?
O4 Mo2 O8 71.20(9) . . ?
Cr1 O8 Mo3 103.93(11) . . ?
Cr1 O8 Mo2 102.04(11) . . ?
Mo3 O8 Mo2 93.17(9) . . ?
N1 C2 C3 122.1(4) . . ?
C6 N2 C7 125.2(3) . . ?
C6 N2 C8 121.0(3) . 2_855 ?
C7 N2 C8 113.8(3) . 2_855 ?
O12 Mo3 O1 104.75(13) . . ?
O12 Mo3 O5 101.69(12) . . ?
O1 Mo3 O5 100.91(12) . . ?
O12 Mo3 O10 97.01(12) . 2_656 ?
O1 Mo3 O10 97.45(12) . 2_656 ?
O5 Mo3 O10 149.37(11) . 2_656 ?
O12 Mo3 O8 90.35(12) . . ?
O1 Mo3 O8 164.76(11) . . ?
O5 Mo3 O8 73.53(10) . . ?
O10 Mo3 O8 82.38(10) 2_656 . ?
O12 Mo3 O15 158.73(12) . 2_656 ?
O1 Mo3 O15 94.67(11) . 2_656 ?
O5 Mo3 O15 82.68(10) . 2_656 ?
O10 Mo3 O15 71.53(10) 2_656 2_656 ?
O8 Mo3 O15 70.74(9) . 2_656 ?
Cr1 O15 Mo1 100.55(10) . . ?
Cr1 O15 Mo3 101.71(10) . 2_656 ?
Mo1 O15 Mo3 93.08(9) . 2_656 ?
C2 C3 C5 118.7(4) . . ?
Cr1 O4 Mo1 103.28(11) . . ?
Cr1 O4 Mo2 103.65(11) . . ?
Mo1 O4 Mo2 96.03(9) . . ?
C1 C4 C5 118.7(4) . . ?
Mo3 O5 Mo2 116.68(13) . . ?
C4 C5 C3 119.0(4) . . ?
C4 C5 C6 119.5(3) . . ?
C3 C5 C6 121.5(3) . . ?
O3 C6 N2 123.9(3) . . ?
O3 C6 C5 118.8(3) . . ?
N2 C6 C5 117.3(3) . . ?
N2 C7 C8 109.7(3) . . ?
N2 C8 C7 110.0(3) 2_855 . ?
Mo2 O9 Mo1 115.77(12) . . ?
Mo1 O10 Mo3 118.89(13) . 2_656 ?
Mo3 O1 Cu1 155.32(17) . . ?
C6 O3 Cu1 130.1(3) . 1_655 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.327
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.105




_database_code_depnum_ccdc_archive 'CCDC 969175'
