# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Aixiang Tian'
_publ_contact_author_email       tianax717ya@yahoo.com.cn
_publ_author_name                'Xiuli Wang'

data_compound-1
_database_code_depnum_ccdc_archive 'CCDC 824587'
#TrackingRef '- compounds 1-3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H14 Cu2 Mo4 N9 O14'
_chemical_formula_weight         983.1

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'
Mo Mo -1.6832 0.6857 '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'

_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                   10.7103(9)
_cell_length_b                   11.2561(10)
_cell_length_c                   11.9413(17)
_cell_angle_alpha                109.8290(10)
_cell_angle_beta                 96.5170(10)
_cell_angle_gamma                116.3170(10)
_cell_volume                     1152.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             934
_exptl_absorpt_coefficient_mu    4.008
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7137
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         28.20
_reflns_number_total             5677
_reflns_number_gt                4300
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
;

_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^)+(0.0395P)^2^+1.9755P] 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    refo
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5142
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0809
_refine_ls_wR_factor_gt          0.0756
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_restrained_S_all      0.971
_refine_ls_shift/su_max          0.000
_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 0.02936(4) 0.17796(4) 0.04755(3) 0.01278(9) Uani 1 1 d . . .
Mo2 Mo -0.31085(4) -0.09689(4) -0.06147(4) 0.01463(10) Uani 1 1 d . . .
Mo3 Mo -0.09763(5) 0.16726(5) 0.29174(4) 0.01687(10) Uani 1 1 d . . .
Mo4 Mo 0.19607(4) 0.14954(5) 0.30256(4) 0.01606(10) Uani 1 1 d . . .
Cu1 Cu -0.63460(8) -0.37807(8) 0.02098(6) 0.03008(17) Uani 1 1 d . . .
Cu2 Cu 0.38173(8) 0.52610(8) 0.62194(7) 0.03241(17) Uani 1 1 d . . .
O1 O -0.2692(4) 0.0581(4) 0.2904(4) 0.0309(9) Uani 1 1 d . . .
OW1 O -0.7085(9) -0.2549(8) 0.1656(5) 0.094(2) Uani 1 1 d . . .
O2 O 0.2289(4) 0.0232(4) 0.3251(3) 0.0275(8) Uani 1 1 d . . .
O3 O -0.0167(4) 0.2911(4) 0.0140(3) 0.0236(8) Uani 1 1 d . . .
O4 O 0.2778(4) 0.2998(4) 0.4452(3) 0.0304(9) Uani 1 1 d . . .
O5 O -0.0139(4) 0.3150(4) 0.4370(3) 0.0318(9) Uani 1 1 d . . .
O6 O 0.1945(3) 0.2187(4) 0.0143(3) 0.0187(7) Uani 1 1 d . . .
O7 O -0.4414(4) -0.2017(4) -0.0114(3) 0.0243(8) Uani 1 1 d . . .
O8 O -0.3442(3) -0.2326(4) -0.2282(3) 0.0191(7) Uani 1 1 d . . .
O9 O -0.3802(4) -0.0035(4) -0.1058(3) 0.0247(8) Uani 1 1 d . . .
O10 O 0.0963(3) 0.0120(3) 0.0972(3) 0.0154(7) Uani 1 1 d . . .
O11 O -0.1636(3) 0.0635(4) 0.0940(3) 0.0164(7) Uani 1 1 d . . .
O12 O -0.0086(4) 0.0598(4) 0.3051(3) 0.0207(7) Uani 1 1 d . . .
O13 O 0.0931(3) 0.2599(3) 0.2245(3) 0.0170(7) Uani 1 1 d . . .
C1 C -0.3554(6) -0.2946(6) 0.1788(5) 0.0257(11) Uani 1 1 d . . .
H1A H -0.3045 -0.2198 0.1558 0.031 Uiso 1 1 calc R . .
C2 C -0.5236(6) -0.4743(6) 0.1935(5) 0.0239(11) Uani 1 1 d . . .
H2A H -0.6161 -0.5497 0.1819 0.029 Uiso 1 1 calc R . .
C3 C -0.1382(5) -0.2592(6) 0.3231(5) 0.0253(11) Uani 1 1 d . . .
H3A H -0.1270 -0.2669 0.4016 0.030 Uiso 1 1 calc R . .
H3B H -0.0874 -0.1553 0.3424 0.030 Uiso 1 1 calc R . .
C4 C -0.0673(5) -0.3315(6) 0.2447(5) 0.0262(12) Uani 1 1 d . . .
H4A H -0.0844 -0.3295 0.1640 0.031 Uiso 1 1 calc R . .
H4B H 0.0378 -0.2743 0.2860 0.031 Uiso 1 1 calc R . .
C5 C -0.2538(6) -0.7166(6) 0.1357(5) 0.0236(11) Uani 1 1 d . . .
H5A H -0.3260 -0.8128 0.0800 0.028 Uiso 1 1 calc R . .
C6 C -0.0741(5) -0.5366(6) 0.2918(5) 0.0231(11) Uani 1 1 d . . .
H6A H 0.0038 -0.4791 0.3660 0.028 Uiso 1 1 calc R . .
C7 C 0.2964(6) 0.5971(6) 0.4234(5) 0.0271(12) Uani 1 1 d . . .
H7A H 0.2455 0.4994 0.3636 0.033 Uiso 1 1 calc R . .
C8 C 0.4212(5) 0.7866(6) 0.5973(5) 0.0223(11) Uani 1 1 d . . .
H8A H 0.4747 0.8502 0.6813 0.027 Uiso 1 1 calc R . .
C9 C 0.4355(6) 0.9744(6) 0.5251(5) 0.0265(12) Uani 1 1 d . . .
H9A H 0.4642 1.0408 0.6127 0.032 Uiso 1 1 calc R . .
H9B H 0.3550 0.9744 0.4788 0.032 Uiso 1 1 calc R . .
N1 N -0.5007(5) -0.3872(5) 0.1354(4) 0.0237(9) Uani 1 1 d . . .
N2 N -0.4017(4) -0.4422(4) 0.2692(4) 0.0194(9) Uani 1 1 d . . .
N3 N -0.2946(4) -0.3258(5) 0.2598(4) 0.0203(9) Uani 1 1 d . . .
N4 N -0.1222(4) -0.4836(4) 0.2245(4) 0.0193(9) Uani 1 1 d . . .
N5 N -0.2396(4) -0.6004(5) 0.1227(4) 0.0219(9) Uani 1 1 d . . .
N6 N -0.1522(4) -0.6819(5) 0.2387(4) 0.0194(9) Uani 1 1 d . . .
N7 N 0.3644(4) 0.6404(5) 0.5447(4) 0.0220(9) Uani 1 1 d . . .
N8 N 0.3090(5) 0.7065(5) 0.3980(4) 0.0309(11) Uani 1 1 d . . .
N9 N 0.3893(5) 0.8259(5) 0.5113(4) 0.0216(9) Uani 1 1 d . . .

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
Mo1 0.01454(19) 0.01142(19) 0.01133(19) 0.00522(15) 0.00285(14) 0.00598(15)
Mo2 0.01357(19) 0.0152(2) 0.0140(2) 0.00644(16) 0.00303(15) 0.00684(16)
Mo3 0.0230(2) 0.0199(2) 0.0130(2) 0.00799(16) 0.00760(16) 0.01415(18)
Mo4 0.0195(2) 0.0177(2) 0.01172(19) 0.00664(16) 0.00301(15) 0.01045(17)
Cu1 0.0333(4) 0.0358(4) 0.0246(4) 0.0144(3) 0.0010(3) 0.0215(3)
Cu2 0.0421(4) 0.0393(4) 0.0418(4) 0.0336(4) 0.0202(3) 0.0279(4)
O1 0.029(2) 0.040(2) 0.037(2) 0.0243(19) 0.0210(17) 0.0206(19)
OW1 0.177(7) 0.146(6) 0.057(4) 0.061(4) 0.065(4) 0.142(6)
O2 0.033(2) 0.034(2) 0.031(2) 0.0217(18) 0.0110(16) 0.0240(18)
O3 0.0305(19) 0.028(2) 0.0259(19) 0.0178(16) 0.0110(15) 0.0200(17)
O4 0.037(2) 0.031(2) 0.0171(18) 0.0052(16) 0.0025(16) 0.0173(18)
O5 0.049(2) 0.033(2) 0.0154(18) 0.0049(16) 0.0061(17) 0.028(2)
O6 0.0147(16) 0.0192(18) 0.0198(17) 0.0073(14) 0.0057(13) 0.0075(14)
O7 0.0160(17) 0.028(2) 0.0260(19) 0.0144(16) 0.0071(14) 0.0077(15)
O8 0.0179(16) 0.0181(17) 0.0149(16) 0.0042(14) 0.0011(13) 0.0075(14)
O9 0.032(2) 0.026(2) 0.0215(18) 0.0105(15) 0.0026(15) 0.0204(17)
O10 0.0174(16) 0.0143(16) 0.0114(15) 0.0046(13) 0.0044(12) 0.0066(13)
O11 0.0172(16) 0.0188(17) 0.0130(16) 0.0072(13) 0.0044(13) 0.0089(14)
O12 0.0259(18) 0.0188(18) 0.0244(18) 0.0126(15) 0.0110(15) 0.0139(15)
O13 0.0191(16) 0.0144(16) 0.0144(16) 0.0052(13) 0.0030(13) 0.0076(14)
C1 0.029(3) 0.026(3) 0.030(3) 0.019(2) 0.006(2) 0.015(2)
C2 0.022(3) 0.022(3) 0.021(3) 0.007(2) 0.002(2) 0.008(2)
C3 0.023(3) 0.024(3) 0.028(3) 0.014(2) 0.002(2) 0.011(2)
C4 0.019(2) 0.022(3) 0.037(3) 0.015(2) 0.005(2) 0.009(2)
C5 0.027(3) 0.025(3) 0.019(3) 0.006(2) 0.002(2) 0.018(2)
C6 0.024(3) 0.024(3) 0.018(3) 0.005(2) 0.003(2) 0.014(2)
C7 0.030(3) 0.021(3) 0.022(3) 0.009(2) 0.002(2) 0.008(2)
C8 0.024(3) 0.022(3) 0.019(3) 0.011(2) 0.002(2) 0.011(2)
C9 0.035(3) 0.023(3) 0.036(3) 0.020(2) 0.021(2) 0.019(2)
N1 0.029(2) 0.023(2) 0.022(2) 0.0123(18) 0.0046(18) 0.0153(19)
N2 0.024(2) 0.014(2) 0.019(2) 0.0099(17) 0.0028(17) 0.0078(17)
N3 0.019(2) 0.019(2) 0.023(2) 0.0115(18) 0.0063(17) 0.0085(17)
N4 0.018(2) 0.015(2) 0.022(2) 0.0060(17) 0.0021(16) 0.0083(17)
N5 0.022(2) 0.026(2) 0.015(2) 0.0058(18) 0.0008(16) 0.0139(19)
N6 0.022(2) 0.022(2) 0.019(2) 0.0099(17) 0.0059(16) 0.0143(18)
N7 0.021(2) 0.018(2) 0.025(2) 0.0123(18) 0.0048(17) 0.0082(18)
N8 0.040(3) 0.025(2) 0.022(2) 0.0091(19) 0.002(2) 0.014(2)
N9 0.026(2) 0.020(2) 0.023(2) 0.0115(18) 0.0082(17) 0.0130(19)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O3 1.698(3) . ?
Mo1 O6 1.749(3) . ?
Mo1 O13 1.891(3) . ?
Mo1 O10 1.945(3) 2 ?
Mo1 O11 2.150(3) . ?
Mo1 O10 2.490(3) . ?
Mo2 O7 1.706(3) . ?
Mo2 O9 1.708(3) . ?
Mo2 O8 1.928(3) . ?
Mo2 O11 1.931(3) . ?
Mo2 O10 2.220(3) 2 ?
Mo2 O6 2.373(3) 2 ?
Mo3 O1 1.693(4) . ?
Mo3 O5 1.716(3) . ?
Mo3 O12 1.875(3) . ?
Mo3 O11 2.111(3) . ?
Mo3 O13 2.226(3) . ?
Mo3 N6 2.269(4) 1_565 ?
Mo4 O2 1.703(4) . ?
Mo4 O4 1.709(4) . ?
Mo4 O8 1.936(3) 2 ?
Mo4 O12 1.975(3) . ?
Mo4 O10 2.217(3) . ?
Mo4 O13 2.322(3) . ?
Cu1 N1 1.927(4) . ?
Cu1 N5 1.929(4) 2_445 ?
Cu1 OW1 2.278(5) . ?
Cu1 O7 2.331(4) . ?
Cu2 N7 1.876(4) . ?
Cu2 N2 1.891(4) 2_556 ?
Cu2 O4 2.342(4) . ?
O6 Mo2 2.373(3) 2 ?
O8 Mo4 1.936(3) 2 ?
O10 Mo1 1.945(3) 2 ?
O10 Mo2 2.220(3) 2 ?
C1 N3 1.331(6) . ?
C1 N1 1.338(6) . ?
C1 H1A 0.9300 . ?
C2 N2 1.321(6) . ?
C2 N1 1.338(7) . ?
C2 H2A 0.9300 . ?
C3 N3 1.468(6) . ?
C3 C4 1.519(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.460(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N5 1.314(7) . ?
C5 N6 1.358(6) . ?
C5 H5A 0.9300 . ?
C6 N6 1.319(6) . ?
C6 N4 1.330(6) . ?
C6 H6A 0.9300 . ?
C7 N8 1.320(7) . ?
C7 N7 1.353(6) . ?
C7 H7A 0.9300 . ?
C8 N9 1.315(6) . ?
C8 N7 1.341(6) . ?
C8 H8A 0.9300 . ?
C9 N9 1.459(6) . ?
C9 C9 1.522(10) 2_676 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N2 N3 1.357(6) . ?
N2 Cu2 1.891(4) 2_556 ?
N4 N5 1.375(5) . ?
N5 Cu1 1.929(4) 2_445 ?
N6 Mo3 2.269(4) 1_545 ?
N8 N9 1.362(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
O3 Mo1 O6 104.35(17) . . ?
O3 Mo1 O13 105.03(16) . . ?
O6 Mo1 O13 101.68(14) . . ?
O3 Mo1 O10 103.55(15) . 2 ?
O6 Mo1 O10 97.71(14) . 2 ?
O13 Mo1 O10 139.97(14) . 2 ?
O3 Mo1 O11 96.84(15) . . ?
O6 Mo1 O11 158.54(14) . . ?
O13 Mo1 O11 75.60(13) . . ?
O10 Mo1 O11 73.68(12) 2 . ?
O3 Mo1 O10 179.80(14) . . ?
O6 Mo1 O10 75.84(14) . . ?
O13 Mo1 O10 74.87(12) . . ?
O10 Mo1 O10 76.47(13) 2 . ?
O11 Mo1 O10 82.98(11) . . ?
O7 Mo2 O9 104.18(18) . . ?
O7 Mo2 O8 104.10(16) . . ?
O9 Mo2 O8 96.56(15) . . ?
O7 Mo2 O11 102.57(15) . . ?
O9 Mo2 O11 98.42(15) . . ?
O8 Mo2 O11 145.03(14) . . ?
O7 Mo2 O10 153.52(15) . 2 ?
O9 Mo2 O10 102.28(15) . 2 ?
O8 Mo2 O10 73.67(12) . 2 ?
O11 Mo2 O10 72.34(12) . 2 ?
O7 Mo2 O6 82.58(14) . 2 ?
O9 Mo2 O6 172.95(15) . 2 ?
O8 Mo2 O6 79.63(13) . 2 ?
O11 Mo2 O6 81.83(12) . 2 ?
O10 Mo2 O6 71.02(12) 2 2 ?
O1 Mo3 O5 105.59(19) . . ?
O1 Mo3 O12 101.62(17) . . ?
O5 Mo3 O12 102.24(16) . . ?
O1 Mo3 O11 90.79(16) . . ?
O5 Mo3 O11 155.13(17) . . ?
O12 Mo3 O11 92.34(14) . . ?
O1 Mo3 O13 160.53(15) . . ?
O5 Mo3 O13 93.42(16) . . ?
O12 Mo3 O13 77.86(14) . . ?
O11 Mo3 O13 69.86(12) . . ?
O1 Mo3 N6 94.85(17) . 1_565 ?
O5 Mo3 N6 82.73(17) . 1_565 ?
O12 Mo3 N6 160.67(15) . 1_565 ?
O11 Mo3 N6 77.25(14) . 1_565 ?
O13 Mo3 N6 83.24(13) . 1_565 ?
O2 Mo4 O4 105.53(18) . . ?
O2 Mo4 O8 101.94(16) . 2 ?
O4 Mo4 O8 95.95(17) . 2 ?
O2 Mo4 O12 96.46(16) . . ?
O4 Mo4 O12 99.43(16) . . ?
O8 Mo4 O12 151.86(14) 2 . ?
O2 Mo4 O10 92.67(15) . . ?
O4 Mo4 O10 160.70(16) . . ?
O8 Mo4 O10 73.60(12) 2 . ?
O12 Mo4 O10 84.53(13) . . ?
O2 Mo4 O13 163.19(15) . . ?
O4 Mo4 O13 89.75(15) . . ?
O8 Mo4 O13 83.00(13) 2 . ?
O12 Mo4 O13 73.69(13) . . ?
O10 Mo4 O13 73.13(11) . . ?
N1 Cu1 N5 166.65(18) . 2_445 ?
N1 Cu1 OW1 97.6(2) . . ?
N5 Cu1 OW1 95.62(19) 2_445 . ?
N1 Cu1 O7 91.58(16) . . ?
N5 Cu1 O7 86.57(16) 2_445 . ?
OW1 Cu1 O7 107.0(2) . . ?
N7 Cu2 N2 167.76(18) . 2_556 ?
N7 Cu2 O4 99.62(16) . . ?
N2 Cu2 O4 91.80(16) 2_556 . ?
Mo4 O4 Cu2 170.3(2) . . ?
Mo1 O6 Mo2 116.39(17) . 2 ?
Mo2 O7 Cu1 169.8(2) . . ?
Mo2 O8 Mo4 113.53(16) . 2 ?
Mo1 O10 Mo4 151.25(18) 2 . ?
Mo1 O10 Mo2 103.58(13) 2 2 ?
Mo4 O10 Mo2 93.51(11) . 2 ?
Mo1 O10 Mo1 103.53(13) 2 . ?
Mo4 O10 Mo1 97.18(12) . . ?
Mo2 O10 Mo1 96.49(12) 2 . ?
Mo2 O11 Mo3 148.36(18) . . ?
Mo2 O11 Mo1 106.69(14) . . ?
Mo3 O11 Mo1 104.54(13) . . ?
Mo3 O12 Mo4 114.04(17) . . ?
Mo1 O13 Mo3 109.65(14) . . ?
Mo1 O13 Mo4 113.69(15) . . ?
Mo3 O13 Mo4 90.47(12) . . ?
N3 C1 N1 109.7(5) . . ?
N3 C1 H1A 125.1 . . ?
N1 C1 H1A 125.1 . . ?
N2 C2 N1 113.2(5) . . ?
N2 C2 H2A 123.4 . . ?
N1 C2 H2A 123.4 . . ?
N3 C3 C4 112.9(4) . . ?
N3 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
N3 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N4 C4 C3 113.5(4) . . ?
N4 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
N4 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
N5 C5 N6 113.1(4) . . ?
N5 C5 H5A 123.5 . . ?
N6 C5 H5A 123.5 . . ?
N6 C6 N4 110.6(4) . . ?
N6 C6 H6A 124.7 . . ?
N4 C6 H6A 124.7 . . ?
N8 C7 N7 113.8(5) . . ?
N8 C7 H7A 123.1 . . ?
N7 C7 H7A 123.1 . . ?
N9 C8 N7 109.1(4) . . ?
N9 C8 H8A 125.4 . . ?
N7 C8 H8A 125.4 . . ?
N9 C9 C9 108.8(5) . 2_676 ?
N9 C9 H9A 109.9 . . ?
C9 C9 H9A 109.9 2_676 . ?
N9 C9 H9B 109.9 . . ?
C9 C9 H9B 109.9 2_676 . ?
H9A C9 H9B 108.3 . . ?
C2 N1 C1 104.1(4) . . ?
C2 N1 Cu1 131.6(4) . . ?
C1 N1 Cu1 124.2(4) . . ?
C2 N2 N3 104.2(4) . . ?
C2 N2 Cu2 128.1(4) . 2_556 ?
N3 N2 Cu2 127.5(3) . 2_556 ?
C1 N3 N2 108.8(4) . . ?
C1 N3 C3 128.1(4) . . ?
N2 N3 C3 122.8(4) . . ?
C6 N4 N5 108.3(4) . . ?
C6 N4 C4 129.9(4) . . ?
N5 N4 C4 121.8(4) . . ?
C5 N5 N4 103.9(4) . . ?
C5 N5 Cu1 120.8(3) . 2_445 ?
N4 N5 Cu1 135.2(3) . 2_445 ?
C6 N6 C5 104.0(4) . . ?
C6 N6 Mo3 126.2(3) . 1_545 ?
C5 N6 Mo3 128.9(3) . 1_545 ?
C8 N7 C7 103.7(4) . . ?
C8 N7 Cu2 127.5(3) . . ?
C7 N7 Cu2 128.8(4) . . ?
C7 N8 N9 102.6(4) . . ?
C8 N9 N8 110.9(4) . . ?
C8 N9 C9 127.9(5) . . ?
N8 N9 C9 121.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.905
_diffrn_reflns_theta_full        28.20
_diffrn_measured_fraction_theta_full 0.905
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.169

#===END

data_compound-2
_database_code_depnum_ccdc_archive 'CCDC 824588'
#TrackingRef '- compounds 1-3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H28 Cu Mo4 N12 O15'
_chemical_formula_weight         1075.78

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'
Mo Mo -1.6832 0.6857 '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'

_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                   10.6009(10)
_cell_length_b                   12.2124(12)
_cell_length_c                   13.7623(14)
_cell_angle_alpha                72.1200(10)
_cell_angle_beta                 68.4780(10)
_cell_angle_gamma                87.3250(10)
_cell_volume                     1573.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1042
_exptl_absorpt_coefficient_mu    2.302
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_T_max  0.692
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            9169
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         28.21
_reflns_number_total             7734
_reflns_number_gt                5190
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
;

_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^)+(0.0477P)^2^+0.5300P] 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    refo
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6770
_refine_ls_number_parameters     431
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Mo1 Mo -0.16300(4) 0.43299(4) 1.57220(3) 0.01864(10) Uani 1 1 d . . .
Mo2 Mo 0.08008(4) 0.31640(4) 1.65388(3) 0.02027(11) Uani 1 1 d . . .
Mo3 Mo 0.18975(4) 0.49934(4) 1.20050(3) 0.02104(11) Uani 1 1 d . . .
Mo4 Mo 0.16906(4) 0.28679(4) 1.41198(3) 0.02049(11) Uani 1 1 d . . .
OW1 O -0.1427(4) 0.0081(4) 1.6787(3) 0.0415(10) Uani 1 1 d . . .
O1 O 0.0166(3) 0.3843(3) 1.5116(3) 0.0209(7) Uani 1 1 d . . .
O2 O 0.0897(3) 0.3620(3) 1.3021(3) 0.0245(8) Uani 1 1 d . . .
O3 O -0.0042(4) 0.1808(3) 1.7112(3) 0.0309(8) Uani 1 1 d . . .
O4 O -0.0772(3) 0.4011(3) 1.6991(3) 0.0221(7) Uani 1 1 d . . .
O5 O -0.2551(3) 0.5295(3) 1.6571(3) 0.0216(7) Uani 1 1 d . . .
O6 O 0.2209(3) 0.2837(3) 1.5320(3) 0.0221(7) Uani 1 1 d . . .
O7 O 0.0555(4) 0.1644(3) 1.4724(3) 0.0276(8) Uani 1 1 d . . .
O8 O -0.2648(4) 0.3086(3) 1.6278(3) 0.0291(8) Uani 1 1 d . . .
O9 O 0.1651(4) 0.3202(3) 1.7371(3) 0.0330(9) Uani 1 1 d . . .
O10 O 0.3136(4) 0.2441(3) 1.3328(3) 0.0340(9) Uani 1 1 d . . .
O11 O -0.1835(3) 0.4993(3) 1.4476(3) 0.0235(7) Uani 1 1 d . . .
O12 O 0.3325(4) 0.4470(3) 1.1264(3) 0.0315(8) Uani 1 1 d . . .
O13 O 0.0972(4) 0.5382(3) 1.1176(3) 0.0299(8) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.0000 1.5000 0.0250(2) Uani 1 2 d S . .
Cu2 Cu 0.0000 0.5000 1.0000 0.0256(2) Uani 1 2 d S . .
C1 C 0.4251(5) 0.6863(5) 1.0220(4) 0.0294(12) Uani 1 1 d . . .
H1A H 0.4682 0.6297 0.9920 0.035 Uiso 1 1 calc R . .
C2 C 0.2919(6) 0.7747(4) 1.1248(4) 0.0335(13) Uani 1 1 d . . .
H2A H 0.2213 0.7885 1.1832 0.040 Uiso 1 1 calc R . .
C3 C 0.5684(5) 0.8581(5) 0.8748(4) 0.0350(13) Uani 1 1 d . . .
H3A H 0.6158 0.8018 0.8405 0.042 Uiso 1 1 calc R . .
H3B H 0.6333 0.8976 0.8896 0.042 Uiso 1 1 calc R . .
C4 C 0.5162(6) 0.9460(5) 0.7946(4) 0.0348(13) Uani 1 1 d . . .
H4A H 0.5932 0.9836 0.7283 0.042 Uiso 1 1 calc R . .
H4B H 0.4737 1.0048 0.8275 0.042 Uiso 1 1 calc R . .
C5 C 0.4140(6) 0.8941(5) 0.7631(5) 0.0356(13) Uani 1 1 d . . .
H5A H 0.4478 0.8260 0.7426 0.043 Uiso 1 1 calc R . .
H5B H 0.3278 0.8720 0.8248 0.043 Uiso 1 1 calc R . .
C6 C 0.3954(7) 0.9848(6) 0.6671(6) 0.0527(18) Uani 1 1 d . . .
H6A H 0.3628 1.0523 0.6892 0.063 Uiso 1 1 calc R . .
H6B H 0.4833 1.0076 0.6076 0.063 Uiso 1 1 calc R . .
C7 C 0.1975(6) 1.0014(5) 0.6063(5) 0.0354(13) Uani 1 1 d . . .
H7A H 0.1651 1.0671 0.6250 0.042 Uiso 1 1 calc R . .
C8 C 0.2266(7) 0.8596(5) 0.5471(6) 0.0486(17) Uani 1 1 d . . .
H8A H 0.2153 0.8065 0.5143 0.058 Uiso 1 1 calc R . .
C9 C -0.0226(6) 0.7436(5) 0.8509(4) 0.0349(13) Uani 1 1 d . . .
H9A H 0.0153 0.7249 0.7860 0.042 Uiso 1 1 calc R . .
C10 C -0.0946(6) 0.7293(5) 1.0182(5) 0.0367(14) Uani 1 1 d . . .
H10A H -0.1192 0.7022 1.0941 0.044 Uiso 1 1 calc R . .
C11 C -0.1635(7) 0.9327(5) 1.0029(6) 0.0498(17) Uani 1 1 d . . .
H11A H -0.2155 0.9762 0.9607 0.060 Uiso 1 1 calc R . .
H11B H -0.2247 0.9034 1.0791 0.060 Uiso 1 1 calc R . .
C12 C -0.0574(9) 1.0092(9) 0.9947(12) 0.123(5) Uani 1 1 d . . .
H12A H -0.0349 1.0657 0.9224 0.148 Uiso 1 1 calc R . .
H12B H -0.1037 1.0502 1.0466 0.148 Uiso 1 1 calc R . .
C13 C -0.2117(5) 0.4437(5) 1.2355(4) 0.0290(12) Uani 1 1 d . . .
H13A H -0.1486 0.4361 1.2691 0.035 Uiso 1 1 calc R . .
C14 C -0.3022(6) 0.4723(6) 1.1169(5) 0.0471(17) Uani 1 1 d . . .
H14A H -0.3125 0.4872 1.0499 0.057 Uiso 1 1 calc R . .
C15 C -0.4241(6) 0.4061(5) 1.4066(4) 0.0335(13) Uani 1 1 d . . .
H15A H -0.3690 0.3656 1.4471 0.040 Uiso 1 1 calc R . .
H15B H -0.5041 0.3557 1.4276 0.040 Uiso 1 1 calc R . .
C16 C -0.4682(6) 0.5143(5) 1.4383(4) 0.0319(13) Uani 1 1 d . . .
H16A H -0.3900 0.5691 1.4097 0.038 Uiso 1 1 calc R . .
H16B H -0.5334 0.5497 1.4060 0.038 Uiso 1 1 calc R . .
N1 N 0.3173(4) 0.6676(4) 1.1162(3) 0.0274(10) Uani 1 1 d . . .
N2 N 0.4600(4) 0.7980(4) 0.9787(4) 0.0295(10) Uani 1 1 d . . .
N3 N 0.3761(5) 0.8572(4) 1.0431(4) 0.0387(12) Uani 1 1 d . . .
N4 N 0.3217(6) 0.8550(5) 0.5880(5) 0.0537(16) Uani 1 1 d . . .
N5 N 0.3005(5) 0.9480(4) 0.6255(4) 0.0367(12) Uani 1 1 d . . .
N6 N 0.1463(5) 0.9488(4) 0.5569(4) 0.0297(10) Uani 1 1 d . . .
N7 N -0.0390(5) 0.6675(4) 0.9518(3) 0.0287(10) Uani 1 1 d . . .
N8 N -0.1109(5) 0.8345(4) 0.9629(4) 0.0346(11) Uani 1 1 d . . .
N9 N -0.0649(6) 0.8446(4) 0.8541(4) 0.0453(13) Uani 1 1 d . . .
N10 N -0.1809(4) 0.4688(4) 1.1288(3) 0.0286(10) Uani 1 1 d . . .
N11 N -0.3459(5) 0.4308(4) 1.2881(3) 0.0303(10) Uani 1 1 d . . .
N12 N -0.4026(6) 0.4523(6) 1.2112(5) 0.0642(18) Uani 1 1 d . . .
OW2 O -0.4233(11) 0.7656(9) 1.2170(8) 0.183(4) Uiso 1 1 d . . .

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
Mo1 0.0190(2) 0.0197(2) 0.0220(2) -0.00963(17) -0.01064(16) 0.00353(16)
Mo2 0.0230(2) 0.0203(2) 0.0218(2) -0.00856(17) -0.01199(17) 0.00609(17)
Mo3 0.0249(2) 0.0219(2) 0.0201(2) -0.00910(17) -0.01070(17) 0.00416(18)
Mo4 0.0250(2) 0.0178(2) 0.0225(2) -0.00923(17) -0.01108(17) 0.00515(17)
OW1 0.044(3) 0.043(2) 0.038(2) -0.0100(19) -0.0166(19) 0.000(2)
O1 0.0247(18) 0.0199(17) 0.0224(17) -0.0096(14) -0.0116(14) 0.0061(14)
O2 0.030(2) 0.0243(19) 0.0237(18) -0.0079(15) -0.0149(15) 0.0015(15)
O3 0.033(2) 0.0208(19) 0.038(2) -0.0117(16) -0.0099(17) 0.0047(16)
O4 0.0222(18) 0.0258(19) 0.0245(18) -0.0126(15) -0.0123(14) 0.0068(15)
O5 0.0196(17) 0.0240(18) 0.0275(18) -0.0128(15) -0.0124(14) 0.0059(14)
O6 0.0213(18) 0.0228(18) 0.0274(18) -0.0107(15) -0.0133(14) 0.0086(14)
O7 0.034(2) 0.0190(18) 0.035(2) -0.0089(15) -0.0188(17) 0.0035(15)
O8 0.029(2) 0.027(2) 0.035(2) -0.0121(16) -0.0145(16) 0.0020(16)
O9 0.041(2) 0.037(2) 0.032(2) -0.0134(17) -0.0240(18) 0.0080(18)
O10 0.036(2) 0.037(2) 0.034(2) -0.0194(18) -0.0133(17) 0.0134(18)
O11 0.0229(18) 0.0254(19) 0.0282(18) -0.0110(15) -0.0145(15) 0.0048(15)
O12 0.031(2) 0.033(2) 0.0281(19) -0.0119(16) -0.0062(16) 0.0070(17)
O13 0.036(2) 0.032(2) 0.030(2) -0.0121(16) -0.0204(17) 0.0055(17)
Cu1 0.0289(5) 0.0177(4) 0.0353(5) -0.0088(4) -0.0194(4) 0.0041(4)
Cu2 0.0334(5) 0.0212(5) 0.0228(4) -0.0083(4) -0.0104(4) 0.0067(4)
C1 0.029(3) 0.030(3) 0.031(3) -0.014(2) -0.011(2) 0.007(2)
C2 0.038(3) 0.021(3) 0.033(3) -0.009(2) -0.003(2) 0.002(2)
C3 0.024(3) 0.050(4) 0.026(3) -0.006(3) -0.009(2) 0.002(3)
C4 0.034(3) 0.039(3) 0.032(3) -0.004(3) -0.018(3) -0.005(3)
C5 0.037(3) 0.038(3) 0.037(3) -0.010(3) -0.020(3) 0.004(3)
C6 0.059(5) 0.051(4) 0.056(4) -0.005(3) -0.038(4) -0.010(3)
C7 0.049(4) 0.024(3) 0.049(4) -0.016(3) -0.033(3) 0.014(3)
C8 0.064(5) 0.039(4) 0.071(5) -0.029(3) -0.049(4) 0.021(3)
C9 0.059(4) 0.023(3) 0.028(3) -0.010(2) -0.021(3) 0.004(3)
C10 0.054(4) 0.033(3) 0.029(3) -0.013(2) -0.021(3) 0.017(3)
C11 0.058(4) 0.034(4) 0.071(5) -0.031(3) -0.031(4) 0.028(3)
C12 0.078(7) 0.106(8) 0.269(14) -0.148(9) -0.090(9) 0.053(6)
C13 0.030(3) 0.031(3) 0.030(3) -0.013(2) -0.013(2) 0.000(2)
C14 0.032(3) 0.090(5) 0.022(3) -0.021(3) -0.011(2) 0.012(3)
C15 0.032(3) 0.043(3) 0.028(3) -0.013(3) -0.013(2) 0.002(3)
C16 0.026(3) 0.043(3) 0.031(3) -0.017(3) -0.012(2) 0.009(2)
N1 0.028(2) 0.025(2) 0.028(2) -0.0089(18) -0.0077(19) 0.0039(19)
N2 0.028(2) 0.032(3) 0.028(2) -0.009(2) -0.0115(19) 0.004(2)
N3 0.039(3) 0.029(3) 0.040(3) -0.012(2) -0.004(2) 0.005(2)
N4 0.059(4) 0.055(4) 0.087(4) -0.049(3) -0.054(3) 0.038(3)
N5 0.044(3) 0.034(3) 0.043(3) -0.008(2) -0.031(2) 0.006(2)
N6 0.033(3) 0.023(2) 0.040(3) -0.012(2) -0.020(2) 0.007(2)
N7 0.041(3) 0.020(2) 0.027(2) -0.0094(18) -0.013(2) 0.007(2)
N8 0.050(3) 0.023(2) 0.041(3) -0.017(2) -0.023(2) 0.012(2)
N9 0.072(4) 0.033(3) 0.040(3) -0.012(2) -0.032(3) 0.007(3)
N10 0.032(3) 0.030(2) 0.026(2) -0.0134(19) -0.0101(19) 0.004(2)
N11 0.031(3) 0.039(3) 0.026(2) -0.016(2) -0.012(2) 0.005(2)
N12 0.039(3) 0.112(6) 0.052(4) -0.036(4) -0.021(3) 0.010(3)

_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 O8 1.701(3) . ?
Mo1 O11 1.745(3) . ?
Mo1 O5 1.900(3) . ?
Mo1 O1 1.926(3) . ?
Mo1 O4 2.179(3) . ?
Mo1 O1 2.479(3) 2_568 ?
Mo2 O9 1.709(3) . ?
Mo2 O3 1.727(3) . ?
Mo2 O4 1.926(3) . ?
Mo2 O6 1.929(3) . ?
Mo2 O1 2.212(3) . ?
Mo2 O11 2.323(3) 2_568 ?
Mo3 O12 1.708(4) . ?
Mo3 O13 1.713(3) . ?
Mo3 O2 1.879(3) . ?
Mo3 O4 2.121(3) 2_568 ?
Mo3 O5 2.234(3) 2_568 ?
Mo3 N1 2.245(4) . ?
Mo3 Mo4 3.1941(6) . ?
Mo4 O10 1.690(4) . ?
Mo4 O7 1.745(3) . ?
Mo4 O6 1.913(3) . ?
Mo4 O2 1.961(3) . ?
Mo4 O5 2.239(3) 2_568 ?
Mo4 O1 2.259(3) . ?
OW1 Cu1 2.398(4) . ?
O1 Mo1 2.479(3) 2_568 ?
O4 Mo3 2.121(3) 2_568 ?
O5 Mo3 2.234(3) 2_568 ?
O5 Mo4 2.239(3) 2_568 ?
O7 Cu1 2.000(3) . ?
O11 Mo2 2.323(3) 2_568 ?
O13 Cu2 2.373(3) . ?
Cu1 N6 1.977(4) 2_567 ?
Cu1 N6 1.977(4) 1_546 ?
Cu1 O7 2.000(3) 2_558 ?
Cu1 OW1 2.398(4) 2_558 ?
Cu2 N7 2.021(4) 2_567 ?
Cu2 N7 2.021(4) . ?
Cu2 N10 2.031(4) 2_567 ?
Cu2 N10 2.031(4) . ?
Cu2 O13 2.373(3) 2_567 ?
C1 N2 1.319(7) . ?
C1 N1 1.339(6) . ?
C1 H1A 0.9300 . ?
C2 N3 1.316(7) . ?
C2 N1 1.354(7) . ?
C2 H2A 0.9300 . ?
C3 N2 1.460(6) . ?
C3 C4 1.530(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.531(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.511(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N5 1.472(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N5 1.314(7) . ?
C7 N6 1.320(6) . ?
C7 H7A 0.9300 . ?
C8 N4 1.315(7) . ?
C8 N6 1.360(7) . ?
C8 H8A 0.9300 . ?
C9 N9 1.301(7) . ?
C9 N7 1.366(6) . ?
C9 H9A 0.9300 . ?
C10 N8 1.317(7) . ?
C10 N7 1.320(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.445(10) . ?
C11 N8 1.472(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C12 1.281(16) 2_577 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N10 1.317(6) . ?
C13 N11 1.330(7) . ?
C13 H13A 0.9300 . ?
C14 N12 1.301(7) . ?
C14 N10 1.352(7) . ?
C14 H14A 0.9300 . ?
C15 N11 1.472(6) . ?
C15 C16 1.516(8) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C16 1.510(10) 2_468 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
N2 N3 1.362(6) . ?
N4 N5 1.363(7) . ?
N6 Cu1 1.977(4) 1_564 ?
N8 N9 1.361(6) . ?
N11 N12 1.353(7) . ?

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
O8 Mo1 O11 104.15(16) . . ?
O8 Mo1 O5 105.02(16) . . ?
O11 Mo1 O5 102.10(15) . . ?
O8 Mo1 O1 103.81(16) . . ?
O11 Mo1 O1 97.04(15) . . ?
O5 Mo1 O1 140.00(14) . . ?
O8 Mo1 O4 96.84(15) . . ?
O11 Mo1 O4 158.65(14) . . ?
O5 Mo1 O4 75.75(13) . . ?
O1 Mo1 O4 73.81(13) . . ?
O8 Mo1 O1 178.88(14) . 2_568 ?
O11 Mo1 O1 74.76(13) . 2_568 ?
O5 Mo1 O1 75.07(12) . 2_568 ?
O1 Mo1 O1 76.64(14) . 2_568 ?
O4 Mo1 O1 84.28(11) . 2_568 ?
O9 Mo2 O3 104.46(18) . . ?
O9 Mo2 O4 104.46(16) . . ?
O3 Mo2 O4 96.90(16) . . ?
O9 Mo2 O6 102.26(16) . . ?
O3 Mo2 O6 96.13(16) . . ?
O4 Mo2 O6 146.17(14) . . ?
O9 Mo2 O1 155.65(15) . . ?
O3 Mo2 O1 99.87(15) . . ?
O4 Mo2 O1 73.05(13) . . ?
O6 Mo2 O1 74.02(13) . . ?
O9 Mo2 O11 84.80(15) . 2_568 ?
O3 Mo2 O11 170.56(15) . 2_568 ?
O4 Mo2 O11 82.28(13) . 2_568 ?
O6 Mo2 O11 79.86(13) . 2_568 ?
O1 Mo2 O11 70.85(11) . 2_568 ?
O12 Mo3 O13 104.91(18) . . ?
O12 Mo3 O2 101.16(16) . . ?
O13 Mo3 O2 100.11(16) . . ?
O12 Mo3 O4 156.03(15) . 2_568 ?
O13 Mo3 O4 92.08(15) . 2_568 ?
O2 Mo3 O4 92.15(14) . 2_568 ?
O12 Mo3 O5 93.25(15) . 2_568 ?
O13 Mo3 O5 161.84(15) . 2_568 ?
O2 Mo3 O5 76.34(13) . 2_568 ?
O4 Mo3 O5 70.46(12) 2_568 2_568 ?
O12 Mo3 N1 83.19(17) . . ?
O13 Mo3 N1 91.93(16) . . ?
O2 Mo3 N1 165.57(15) . . ?
O4 Mo3 N1 79.39(14) 2_568 . ?
O5 Mo3 N1 89.75(14) 2_568 . ?
O12 Mo3 Mo4 88.73(12) . . ?
O13 Mo3 Mo4 134.65(12) . . ?
O2 Mo3 Mo4 34.55(10) . . ?
O4 Mo3 Mo4 91.20(9) 2_568 . ?
O5 Mo3 Mo4 44.49(8) 2_568 . ?
N1 Mo3 Mo4 133.04(11) . . ?
O10 Mo4 O7 104.40(18) . . ?
O10 Mo4 O6 98.82(16) . . ?
O7 Mo4 O6 100.29(15) . . ?
O10 Mo4 O2 100.66(16) . . ?
O7 Mo4 O2 94.55(15) . . ?
O6 Mo4 O2 151.68(14) . . ?
O10 Mo4 O5 91.45(15) . 2_568 ?
O7 Mo4 O5 162.40(15) . 2_568 ?
O6 Mo4 O5 84.49(13) . 2_568 ?
O2 Mo4 O5 74.69(12) . 2_568 ?
O10 Mo4 O1 163.81(15) . . ?
O7 Mo4 O1 91.04(15) . . ?
O6 Mo4 O1 73.19(13) . . ?
O2 Mo4 O1 82.62(13) . . ?
O5 Mo4 O1 74.01(12) 2_568 . ?
O10 Mo4 Mo3 87.80(13) . . ?
O7 Mo4 Mo3 127.28(11) . . ?
O6 Mo4 Mo3 128.74(10) . . ?
O2 Mo4 Mo3 32.92(10) . . ?
O5 Mo4 Mo3 44.38(8) 2_568 . ?
O1 Mo4 Mo3 86.61(8) . . ?
Mo1 O1 Mo2 104.48(14) . . ?
Mo1 O1 Mo4 153.10(17) . . ?
Mo2 O1 Mo4 92.93(12) . . ?
Mo1 O1 Mo1 103.36(13) . 2_568 ?
Mo2 O1 Mo1 96.17(11) . 2_568 ?
Mo4 O1 Mo1 94.80(12) . 2_568 ?
Mo3 O2 Mo4 112.53(16) . . ?
Mo2 O4 Mo3 149.23(17) . 2_568 ?
Mo2 O4 Mo1 105.72(14) . . ?
Mo3 O4 Mo1 103.89(14) 2_568 . ?
Mo1 O5 Mo3 109.68(15) . 2_568 ?
Mo1 O5 Mo4 114.78(15) . 2_568 ?
Mo3 O5 Mo4 91.13(11) 2_568 2_568 ?
Mo4 O6 Mo2 115.08(16) . . ?
Mo4 O7 Cu1 154.3(2) . . ?
Mo1 O11 Mo2 117.76(16) . 2_568 ?
Mo3 O13 Cu2 151.6(2) . . ?
N6 Cu1 N6 180.000(2) 2_567 1_546 ?
N6 Cu1 O7 89.96(16) 2_567 . ?
N6 Cu1 O7 90.04(16) 1_546 . ?
N6 Cu1 O7 90.04(16) 2_567 2_558 ?
N6 Cu1 O7 89.96(16) 1_546 2_558 ?
O7 Cu1 O7 180.000(1) . 2_558 ?
N6 Cu1 OW1 88.98(16) 2_567 2_558 ?
N6 Cu1 OW1 91.02(16) 1_546 2_558 ?
O7 Cu1 OW1 95.78(14) . 2_558 ?
O7 Cu1 OW1 84.22(14) 2_558 2_558 ?
N6 Cu1 OW1 91.02(16) 2_567 . ?
N6 Cu1 OW1 88.98(16) 1_546 . ?
O7 Cu1 OW1 84.22(14) . . ?
O7 Cu1 OW1 95.78(14) 2_558 . ?
OW1 Cu1 OW1 180.000(1) 2_558 . ?
N7 Cu2 N7 180.000(1) 2_567 . ?
N7 Cu2 N10 89.30(18) 2_567 2_567 ?
N7 Cu2 N10 90.70(18) . 2_567 ?
N7 Cu2 N10 90.70(18) 2_567 . ?
N7 Cu2 N10 89.30(18) . . ?
N10 Cu2 N10 180.000(1) 2_567 . ?
N7 Cu2 O13 90.37(15) 2_567 2_567 ?
N7 Cu2 O13 89.63(15) . 2_567 ?
N10 Cu2 O13 86.98(15) 2_567 2_567 ?
N10 Cu2 O13 93.02(15) . 2_567 ?
N7 Cu2 O13 89.63(15) 2_567 . ?
N7 Cu2 O13 90.37(15) . . ?
N10 Cu2 O13 93.02(15) 2_567 . ?
N10 Cu2 O13 86.98(15) . . ?
O13 Cu2 O13 180.000(1) 2_567 . ?
N2 C1 N1 109.0(5) . . ?
N2 C1 H1A 125.5 . . ?
N1 C1 H1A 125.5 . . ?
N3 C2 N1 113.9(5) . . ?
N3 C2 H2A 123.1 . . ?
N1 C2 H2A 123.1 . . ?
N2 C3 C4 113.0(4) . . ?
N2 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
N2 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C5 114.1(5) . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C6 C5 C4 107.6(5) . . ?
C6 C5 H5A 110.2 . . ?
C4 C5 H5A 110.2 . . ?
C6 C5 H5B 110.2 . . ?
C4 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
N5 C6 C5 114.6(5) . . ?
N5 C6 H6A 108.6 . . ?
C5 C6 H6A 108.6 . . ?
N5 C6 H6B 108.6 . . ?
C5 C6 H6B 108.6 . . ?
H6A C6 H6B 107.6 . . ?
N5 C7 N6 110.6(5) . . ?
N5 C7 H7A 124.7 . . ?
N6 C7 H7A 124.7 . . ?
N4 C8 N6 114.1(5) . . ?
N4 C8 H8A 123.0 . . ?
N6 C8 H8A 123.0 . . ?
N9 C9 N7 113.8(5) . . ?
N9 C9 H9A 123.1 . . ?
N7 C9 H9A 123.1 . . ?
N8 C10 N7 111.1(5) . . ?
N8 C10 H10A 124.4 . . ?
N7 C10 H10A 124.4 . . ?
C12 C11 N8 113.1(6) . . ?
C12 C11 H11A 109.0 . . ?
N8 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
N8 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C12 C12 C11 132.3(12) 2_577 . ?
C12 C12 H12A 104.2 2_577 . ?
C11 C12 H12A 104.2 . . ?
C12 C12 H12B 104.2 2_577 . ?
C11 C12 H12B 104.2 . . ?
H12A C12 H12B 105.5 . . ?
N10 C13 N11 110.3(5) . . ?
N10 C13 H13A 124.9 . . ?
N11 C13 H13A 124.9 . . ?
N12 C14 N10 111.3(5) . . ?
N12 C14 H14A 124.3 . . ?
N10 C14 H14A 124.3 . . ?
N11 C15 C16 112.8(4) . . ?
N11 C15 H15A 109.0 . . ?
C16 C15 H15A 109.0 . . ?
N11 C15 H15B 109.0 . . ?
C16 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C16 C16 C15 110.5(6) 2_468 . ?
C16 C16 H16A 109.5 2_468 . ?
C15 C16 H16A 109.5 . . ?
C16 C16 H16B 109.5 2_468 . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C1 N1 C2 103.7(4) . . ?
C1 N1 Mo3 122.4(4) . . ?
C2 N1 Mo3 131.7(4) . . ?
C1 N2 N3 110.8(4) . . ?
C1 N2 C3 128.0(5) . . ?
N3 N2 C3 121.1(4) . . ?
C2 N3 N2 102.6(4) . . ?
C8 N4 N5 102.4(5) . . ?
C7 N5 N4 110.0(5) . . ?
C7 N5 C6 128.2(5) . . ?
N4 N5 C6 121.3(5) . . ?
C7 N6 C8 102.9(5) . . ?
C7 N6 Cu1 127.0(4) . 1_564 ?
C8 N6 Cu1 129.9(4) . 1_564 ?
C10 N7 C9 102.5(4) . . ?
C10 N7 Cu2 125.2(4) . . ?
C9 N7 Cu2 132.3(4) . . ?
C10 N8 N9 108.9(4) . . ?
C10 N8 C11 129.5(5) . . ?
N9 N8 C11 121.6(5) . . ?
C9 N9 N8 103.6(5) . . ?
C13 N10 C14 104.8(5) . . ?
C13 N10 Cu2 132.1(4) . . ?
C14 N10 Cu2 123.1(4) . . ?
C13 N11 N12 107.3(4) . . ?
C13 N11 C15 128.4(4) . . ?
N12 N11 C15 124.1(5) . . ?
C14 N12 N11 106.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.875
_diffrn_reflns_theta_full        28.21
_diffrn_measured_fraction_theta_full 0.875
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.143

#===END

data_compound-3
_database_code_depnum_ccdc_archive 'CCDC 824589'
#TrackingRef '- compounds 1-3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H16 Cu Mo4 N6 O15'
_chemical_formula_weight         931.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   14.5811(9)
_cell_length_b                   11.2874(7)
_cell_length_c                   15.8490(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.0460(10)
_cell_angle_gamma                90.00
_cell_volume                     2506.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1772
_exptl_absorpt_coefficient_mu    2.861
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            14921
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         28.22
_reflns_number_total             6183
_reflns_number_gt                5018
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
;

_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^)+(0.0478P)^2^+13.6823P] 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    refo
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5856
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1103
_refine_ls_wR_factor_gt          0.1057
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
Mo1 Mo 0.92973(3) -0.20726(4) 0.07446(3) 0.03191(12) Uani 1 1 d . . .
Mo2 Mo 0.80158(3) 0.21342(4) -0.11039(3) 0.03401(12) Uani 1 1 d . . .
Mo3 Mo 0.77630(3) 0.00288(5) 0.02265(3) 0.03699(13) Uani 1 1 d . . .
Mo4 Mo 0.93396(3) -0.03318(4) -0.10739(3) 0.02900(11) Uani 1 1 d . . .
Cu1 Cu 0.60218(5) 0.14732(7) -0.28146(5) 0.03722(17) Uani 1 1 d . . .
O1 O 0.9357(3) 0.1617(3) -0.1011(2) 0.0333(8) Uani 1 1 d . . .
OW1 O 0.6229(4) -0.0399(5) -0.2260(4) 0.0690(15) Uani 1 1 d . . .
O2 O 0.7856(4) 0.0200(5) 0.1307(3) 0.0541(12) Uani 1 1 d . . .
OW2 O 0.5274(3) 0.0757(4) -0.3948(3) 0.0441(10) Uani 1 1 d . . .
O3 O 1.0639(3) 0.0163(3) -0.0484(2) 0.0317(8) Uani 1 1 d . . .
O4 O 0.8277(3) 0.3591(4) -0.1045(3) 0.0542(12) Uani 1 1 d . . .
O5 O 0.6567(3) 0.0022(5) -0.0277(3) 0.0560(12) Uani 1 1 d . . .
O6 O 0.9324(3) -0.0418(4) -0.2141(3) 0.0425(9) Uani 1 1 d . . .
O7 O 0.6806(3) 0.2063(4) -0.1668(3) 0.0397(9) Uani 1 1 d . . .
O8 O 0.8036(3) 0.1741(4) 0.0025(2) 0.0383(9) Uani 1 1 d . . .
O9 O 0.8020(3) -0.1655(4) 0.0174(3) 0.0395(9) Uani 1 1 d . . .
O10 O 0.9383(3) -0.3553(4) 0.0489(3) 0.0409(9) Uani 1 1 d . . .
O11 O 0.8082(3) 0.0085(3) -0.1090(2) 0.0342(8) Uani 1 1 d . . .
O12 O 0.9403(3) -0.1808(4) -0.0727(3) 0.0371(8) Uani 1 1 d . . .
O13 O 0.9224(3) -0.2090(4) 0.1794(3) 0.0457(10) Uani 1 1 d . . .
C1 C 0.7482(4) 0.1267(6) -0.3855(4) 0.0429(14) Uani 1 1 d . . .
H1A H 0.7076 0.0976 -0.4373 0.051 Uiso 1 1 calc R . .
C2 C 0.8720(4) 0.1880(6) -0.2900(4) 0.0410(13) Uani 1 1 d . . .
H2A H 0.9342 0.2116 -0.2627 0.049 Uiso 1 1 calc R . .
C3 C 0.8996(5) 0.1444(8) -0.4349(5) 0.065(2) Uani 1 1 d . . .
H3A H 0.9652 0.1277 -0.4028 0.077 Uiso 1 1 calc R . .
H3B H 0.8983 0.2206 -0.4635 0.077 Uiso 1 1 calc R . .
C4 C 0.8648(5) 0.0501(7) -0.5037(4) 0.0496(16) Uani 1 1 d . . .
C5 C 0.8136(6) 0.0799(7) -0.5868(5) 0.064(2) Uani 1 1 d . . .
H5A H 0.7976 0.1586 -0.6007 0.077 Uiso 1 1 calc R . .
C6 C 0.7856(7) -0.0067(7) -0.6503(5) 0.064(2) Uani 1 1 d . . .
H6A H 0.7525 0.0152 -0.7071 0.077 Uiso 1 1 calc R . .
C7 C 0.8052(4) -0.1232(6) -0.6318(4) 0.0443(14) Uani 1 1 d . . .
C8 C 0.8547(5) -0.1549(7) -0.5482(5) 0.0558(17) Uani 1 1 d . . .
H8A H 0.8676 -0.2344 -0.5346 0.067 Uiso 1 1 calc R . .
C9 C 0.8859(5) -0.0692(8) -0.4835(5) 0.0582(19) Uani 1 1 d . . .
H9A H 0.9205 -0.0912 -0.4271 0.070 Uiso 1 1 calc R . .
C10 C 0.7691(4) -0.2151(7) -0.7029(5) 0.0544(18) Uani 1 1 d . . .
H10A H 0.7999 -0.2041 -0.7493 0.065 Uiso 1 1 calc R . .
H10B H 0.7845 -0.2938 -0.6787 0.065 Uiso 1 1 calc R . .
C11 C 0.6001(4) -0.2073(6) -0.6950(4) 0.0478(15) Uani 1 1 d . . .
H11A H 0.6122 -0.2246 -0.6356 0.057 Uiso 1 1 calc R . .
C12 C 0.6236(5) -0.1757(8) -0.8230(4) 0.0564(18) Uani 1 1 d . . .
H12A H 0.6524 -0.1667 -0.8682 0.068 Uiso 1 1 calc R . .
N1 N 0.7231(3) 0.1500(4) -0.3149(3) 0.0372(10) Uani 1 1 d . . .
N2 N 0.8413(3) 0.1508(5) -0.3731(3) 0.0385(11) Uani 1 1 d . . .
N3 N 0.8031(3) 0.1867(5) -0.2521(3) 0.0391(11) Uani 1 1 d . . .
N4 N 0.6656(4) -0.2034(5) -0.7388(4) 0.0463(12) Uani 1 1 d . . .
N5 N 0.5340(6) -0.1644(9) -0.8271(5) 0.094(3) Uani 1 1 d . . .
N6 N 0.5157(4) -0.1830(5) -0.7481(3) 0.0412(11) Uani 1 1 d . . .

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
Mo1 0.0301(2) 0.0338(2) 0.0329(2) 0.00054(18) 0.01066(18) -0.00300(18)
Mo2 0.0303(2) 0.0338(3) 0.0383(3) -0.00021(19) 0.01023(19) 0.00323(18)
Mo3 0.0309(2) 0.0450(3) 0.0372(3) 0.0009(2) 0.0131(2) 0.0040(2)
Mo4 0.0295(2) 0.0301(2) 0.0273(2) -0.00257(17) 0.00767(16) 0.00091(17)
Cu1 0.0322(3) 0.0429(4) 0.0358(4) -0.0033(3) 0.0082(3) 0.0036(3)
O1 0.0343(19) 0.032(2) 0.0330(19) -0.0010(15) 0.0087(15) -0.0015(15)
OW1 0.087(4) 0.045(3) 0.062(3) 0.002(2) 0.000(3) -0.004(3)
O2 0.063(3) 0.065(3) 0.041(2) 0.003(2) 0.026(2) 0.007(2)
OW2 0.050(2) 0.046(2) 0.035(2) -0.0029(18) 0.0090(18) -0.009(2)
O3 0.0309(18) 0.0322(19) 0.0324(19) -0.0016(15) 0.0096(15) -0.0004(15)
O4 0.055(3) 0.039(2) 0.071(3) -0.002(2) 0.021(2) 0.000(2)
O5 0.033(2) 0.068(3) 0.066(3) 0.003(2) 0.012(2) 0.000(2)
O6 0.056(3) 0.043(2) 0.0298(19) -0.0021(17) 0.0150(18) 0.002(2)
O7 0.0335(19) 0.051(2) 0.033(2) -0.0041(17) 0.0070(16) 0.0105(18)
O8 0.040(2) 0.042(2) 0.0320(19) -0.0053(17) 0.0092(16) 0.0073(18)
O9 0.0313(19) 0.041(2) 0.047(2) 0.0009(18) 0.0105(17) -0.0029(17)
O10 0.043(2) 0.034(2) 0.045(2) 0.0029(17) 0.0097(18) -0.0013(17)
O11 0.0272(17) 0.039(2) 0.0341(19) -0.0037(16) 0.0054(15) -0.0004(15)
O12 0.041(2) 0.034(2) 0.038(2) -0.0014(17) 0.0144(17) -0.0008(17)
O13 0.039(2) 0.064(3) 0.037(2) 0.003(2) 0.0157(18) -0.004(2)
C1 0.041(3) 0.056(4) 0.033(3) -0.006(3) 0.012(2) -0.008(3)
C2 0.036(3) 0.047(3) 0.040(3) -0.003(3) 0.009(2) -0.006(3)
C3 0.057(4) 0.096(6) 0.052(4) -0.028(4) 0.033(3) -0.033(4)
C4 0.043(3) 0.070(5) 0.043(3) -0.006(3) 0.024(3) -0.016(3)
C5 0.092(6) 0.050(4) 0.052(4) -0.004(3) 0.022(4) -0.006(4)
C6 0.102(6) 0.051(4) 0.038(4) 0.003(3) 0.016(4) -0.010(4)
C7 0.038(3) 0.054(4) 0.045(3) -0.003(3) 0.020(3) 0.000(3)
C8 0.043(3) 0.056(4) 0.068(5) 0.010(4) 0.015(3) 0.003(3)
C9 0.043(4) 0.084(6) 0.043(4) 0.004(4) 0.006(3) -0.002(4)
C10 0.037(3) 0.064(5) 0.067(4) -0.018(4) 0.022(3) -0.004(3)
C11 0.037(3) 0.069(5) 0.041(3) 0.006(3) 0.015(3) 0.001(3)
C12 0.044(3) 0.093(6) 0.039(3) -0.004(3) 0.023(3) 0.002(4)
N1 0.030(2) 0.045(3) 0.034(2) -0.004(2) 0.0031(18) 0.004(2)
N2 0.039(2) 0.045(3) 0.032(2) -0.001(2) 0.012(2) -0.005(2)
N3 0.033(2) 0.045(3) 0.039(3) 0.001(2) 0.0082(19) 0.000(2)
N4 0.041(3) 0.054(3) 0.050(3) -0.009(2) 0.022(2) -0.001(2)
N5 0.091(6) 0.140(8) 0.053(4) -0.011(5) 0.024(4) 0.010(5)
N6 0.039(3) 0.047(3) 0.038(3) -0.002(2) 0.012(2) 0.003(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O13 1.696(4) . ?
Mo1 O10 1.732(4) . ?
Mo1 O9 1.892(4) . ?
Mo1 O1 1.958(4) 3_755 ?
Mo1 O3 2.201(4) 3_755 ?
Mo1 O12 2.399(4) . ?
Mo1 Mo3 3.2078(7) . ?
Mo2 O4 1.684(5) . ?
Mo2 O7 1.744(4) . ?
Mo2 O8 1.836(4) . ?
Mo2 O1 2.007(4) . ?
Mo2 N3 2.272(5) . ?
Mo2 O11 2.315(4) . ?
Mo3 O2 1.691(4) . ?
Mo3 O5 1.706(4) . ?
Mo3 O9 1.943(4) . ?
Mo3 O8 2.016(4) . ?
Mo3 O11 2.261(4) . ?
Mo3 O3 2.262(4) 3_755 ?
Mo4 O6 1.688(4) . ?
Mo4 O12 1.749(4) . ?
Mo4 O11 1.886(4) . ?
Mo4 O3 1.949(4) . ?
Mo4 O1 2.201(4) . ?
Mo4 O3 2.468(4) 3_755 ?
Cu1 N6 1.945(5) 3_654 ?
Cu1 N1 1.976(5) . ?
Cu1 O7 1.977(4) . ?
Cu1 OW2 1.996(4) . ?
Cu1 OW1 2.277(5) . ?
O1 Mo1 1.958(4) 3_755 ?
O3 Mo1 2.201(4) 3_755 ?
O3 Mo3 2.262(4) 3_755 ?
O3 Mo4 2.468(4) 3_755 ?
C1 N1 1.297(7) . ?
C1 N2 1.345(7) . ?
C2 N3 1.304(7) . ?
C2 N2 1.336(7) . ?
C3 N2 1.466(8) . ?
C3 C4 1.508(10) . ?
C4 C5 1.364(10) . ?
C4 C9 1.399(11) . ?
C5 C6 1.382(10) . ?
C6 C7 1.360(10) . ?
C7 C8 1.370(9) . ?
C7 C10 1.515(9) . ?
C8 C9 1.392(11) . ?
C10 N4 1.464(8) . ?
C11 N6 1.313(8) . ?
C11 N4 1.327(8) . ?
C12 N5 1.297(10) . ?
C12 N4 1.342(9) . ?
N1 N3 1.372(6) . ?
N5 N6 1.366(9) . ?
N6 Cu1 1.945(5) 3_654 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 Mo1 O10 104.3(2) . . ?
O13 Mo1 O9 98.71(19) . . ?
O10 Mo1 O9 104.70(19) . . ?
O13 Mo1 O1 97.03(18) . 3_755 ?
O10 Mo1 O1 99.86(18) . 3_755 ?
O9 Mo1 O1 146.41(17) . 3_755 ?
O13 Mo1 O3 102.29(19) . 3_755 ?
O10 Mo1 O3 153.02(17) . 3_755 ?
O9 Mo1 O3 75.71(16) . 3_755 ?
O1 Mo1 O3 72.03(15) 3_755 3_755 ?
O13 Mo1 O12 173.52(19) . . ?
O10 Mo1 O12 82.20(17) . . ?
O9 Mo1 O12 79.84(16) . . ?
O1 Mo1 O12 81.19(14) 3_755 . ?
O3 Mo1 O12 71.23(14) 3_755 . ?
O13 Mo1 Mo3 91.79(16) . . ?
O10 Mo1 Mo3 138.05(14) . . ?
O9 Mo1 Mo3 33.74(12) . . ?
O1 Mo1 Mo3 116.57(11) 3_755 . ?
O3 Mo1 Mo3 44.82(10) 3_755 . ?
O12 Mo1 Mo3 83.51(10) . . ?
O4 Mo2 O7 104.8(2) . . ?
O4 Mo2 O8 103.9(2) . . ?
O7 Mo2 O8 103.29(18) . . ?
O4 Mo2 O1 94.5(2) . . ?
O7 Mo2 O1 148.29(17) . . ?
O8 Mo2 O1 96.02(16) . . ?
O4 Mo2 N3 96.9(2) . . ?
O7 Mo2 N3 76.85(18) . . ?
O8 Mo2 N3 158.32(18) . . ?
O1 Mo2 N3 76.01(16) . . ?
O4 Mo2 O11 165.12(19) . . ?
O7 Mo2 O11 89.56(17) . . ?
O8 Mo2 O11 76.10(16) . . ?
O1 Mo2 O11 70.80(14) . . ?
N3 Mo2 O11 82.23(16) . . ?
O2 Mo3 O5 105.0(2) . . ?
O2 Mo3 O9 101.1(2) . . ?
O5 Mo3 O9 99.2(2) . . ?
O2 Mo3 O8 95.0(2) . . ?
O5 Mo3 O8 98.7(2) . . ?
O9 Mo3 O8 151.84(16) . . ?
O2 Mo3 O11 162.2(2) . . ?
O5 Mo3 O11 90.8(2) . . ?
O9 Mo3 O11 84.05(16) . . ?
O8 Mo3 O11 74.15(15) . . ?
O2 Mo3 O3 92.18(19) . 3_755 ?
O5 Mo3 O3 162.4(2) . 3_755 ?
O9 Mo3 O3 73.33(15) . 3_755 ?
O8 Mo3 O3 83.19(15) . 3_755 ?
O11 Mo3 O3 72.81(13) . 3_755 ?
O2 Mo3 Mo1 88.28(17) . . ?
O5 Mo3 Mo1 131.83(18) . . ?
O9 Mo3 Mo1 32.75(11) . . ?
O8 Mo3 Mo1 126.49(11) . . ?
O11 Mo3 Mo1 87.13(10) . . ?
O3 Mo3 Mo1 43.30(9) 3_755 . ?
O6 Mo4 O12 104.17(19) . . ?
O6 Mo4 O11 104.86(19) . . ?
O12 Mo4 O11 102.06(18) . . ?
O6 Mo4 O3 103.87(19) . . ?
O12 Mo4 O3 99.34(17) . . ?
O11 Mo4 O3 138.39(16) . . ?
O6 Mo4 O1 95.71(17) . . ?
O12 Mo4 O1 159.83(16) . . ?
O11 Mo4 O1 75.56(15) . . ?
O3 Mo4 O1 72.19(14) . . ?
O6 Mo4 O3 178.86(17) . 3_755 ?
O12 Mo4 O3 76.96(15) . 3_755 ?
O11 Mo4 O3 74.81(14) . 3_755 ?
O3 Mo4 O3 75.87(15) . 3_755 ?
O1 Mo4 O3 83.15(13) . 3_755 ?
N6 Cu1 N1 167.1(2) 3_654 . ?
N6 Cu1 O7 91.97(19) 3_654 . ?
N1 Cu1 O7 84.77(18) . . ?
N6 Cu1 OW2 90.0(2) 3_654 . ?
N1 Cu1 OW2 94.08(19) . . ?
O7 Cu1 OW2 175.65(18) . . ?
N6 Cu1 OW1 97.5(2) 3_654 . ?
N1 Cu1 OW1 94.8(2) . . ?
O7 Cu1 OW1 88.63(19) . . ?
OW2 Cu1 OW1 87.28(19) . . ?
Mo1 O1 Mo2 146.9(2) 3_755 . ?
Mo1 O1 Mo4 105.71(17) 3_755 . ?
Mo2 O1 Mo4 106.76(16) . . ?
Mo4 O3 Mo1 106.05(16) . 3_755 ?
Mo4 O3 Mo3 151.10(19) . 3_755 ?
Mo1 O3 Mo3 91.88(14) 3_755 3_755 ?
Mo4 O3 Mo4 104.13(15) . 3_755 ?
Mo1 O3 Mo4 97.06(13) 3_755 3_755 ?
Mo3 O3 Mo4 95.72(13) 3_755 3_755 ?
Mo2 O7 Cu1 137.1(2) . . ?
Mo2 O8 Mo3 115.82(19) . . ?
Mo1 O9 Mo3 113.5(2) . . ?
Mo4 O11 Mo3 115.32(17) . . ?
Mo4 O11 Mo2 106.69(17) . . ?
Mo3 O11 Mo2 91.02(14) . . ?
Mo4 O12 Mo1 114.31(19) . . ?
N1 C1 N2 110.3(5) . . ?
N3 C2 N2 111.1(5) . . ?
N2 C3 C4 112.1(5) . . ?
C5 C4 C9 119.1(7) . . ?
C5 C4 C3 120.6(7) . . ?
C9 C4 C3 120.3(7) . . ?
C4 C5 C6 120.1(8) . . ?
C7 C6 C5 121.7(7) . . ?
C6 C7 C8 118.9(7) . . ?
C6 C7 C10 119.5(6) . . ?
C8 C7 C10 121.5(7) . . ?
C7 C8 C9 120.6(7) . . ?
C8 C9 C4 119.6(6) . . ?
N4 C10 C7 109.7(5) . . ?
N6 C11 N4 109.9(6) . . ?
N5 C12 N4 104.3(6) . . ?
C1 N1 N3 107.5(5) . . ?
C1 N1 Cu1 135.5(4) . . ?
N3 N1 Cu1 117.0(4) . . ?
C2 N2 C1 104.9(5) . . ?
C2 N2 C3 125.2(5) . . ?
C1 N2 C3 129.9(5) . . ?
C2 N3 N1 106.2(5) . . ?
C2 N3 Mo2 132.3(4) . . ?
N1 N3 Mo2 121.2(4) . . ?
C11 N4 C12 109.4(5) . . ?
C11 N4 C10 127.4(6) . . ?
C12 N4 C10 123.0(6) . . ?
C12 N5 N6 112.9(7) . . ?
C11 N6 N5 103.5(6) . . ?
C11 N6 Cu1 128.6(4) . 3_654 ?
N5 N6 Cu1 126.7(5) . 3_654 ?

_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        28.22
_diffrn_measured_fraction_theta_full 0.947
_refine_diff_density_max         2.566
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.134

#===END