# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) 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        'Wang, Enbo'
_publ_contact_author_email       wangenbo@public.cc.jl.cn
_publ_author_name                'Enbo Wang'

data_589a
_database_code_depnum_ccdc_archive 'CCDC 776677'
#TrackingRef 'compound_1.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H50 Cu3 Mo8 N12 O44 P V6'
_chemical_formula_weight         2865.81

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'
V V 0.3005 0.5294 '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'

_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                   12.876(3)
_cell_length_b                   13.256(3)
_cell_length_c                   14.198(3)
_cell_angle_alpha                66.67(3)
_cell_angle_beta                 67.42(3)
_cell_angle_gamma                75.36(3)
_cell_volume                     2040.3(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    16087
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1386
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotation anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean 0.01
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            16087
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_sigmaI/netI    0.1038
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7152
_reflns_number_gt                4616
_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.
During the refinement, the restraint command 'DFIX' was also used to refine
the distances of C-C bonds and Cu-O bonds in the disorder of L1 ligand and
Cu2 atom. The restraint command 'ISOR' was also used to refine the non-H
atoms with NPD and ADP problems. These atoms are as follows: O18 O19 O21
O22 C16 C20 C21 C22 C26A C27A N6A C27B O2W O3W. These restraint commands
led to a relative high restraint value (114), but it cannot be totally
avoided in order to get a reasonable refinement.
;

_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^)+(0.0592P)^2^+21.2970P] 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         7152
_refine_ls_number_parameters     651
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.1778
_refine_ls_wR_factor_gt          0.1549
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.151
_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 0.55863(9) 0.20523(8) 0.56654(9) 0.0231(3) Uani 1 1 d . A .
Mo2 Mo 0.71841(9) -0.07890(10) 0.62031(9) 0.0291(3) Uani 1 1 d . A .
Mo3 Mo 0.28459(10) 0.08435(9) 0.71340(10) 0.0281(3) Uani 1 1 d . A .
Mo4 Mo 0.44611(12) -0.20205(9) 0.76346(10) 0.0345(3) Uani 1 1 d . . .
V1 V 0.50140(18) 0.00511(16) 0.77681(17) 0.0222(5) Uani 1 1 d . A .
V2 V 0.34381(16) 0.27487(14) 0.45090(14) 0.0137(4) Uani 1 1 d . . .
V3 V 0.76326(17) 0.11855(15) 0.36071(18) 0.0246(5) Uani 1 1 d . . .
P1 P 0.5000 0.0000 0.5000 0.0191(9) Uani 1 2 d S . .
O1 O 0.4269(7) 0.1361(6) 0.6981(6) 0.0257(19) Uani 1 1 d . . .
O2 O 0.5749(8) -0.1281(7) 0.7485(8) 0.036(2) Uani 1 1 d . . .
O3 O 0.2663(8) 0.2010(8) 0.6007(7) 0.043(3) Uani 1 1 d . . .
O4 O 0.8795(7) 0.1709(7) 0.2986(8) 0.037(2) Uani 1 1 d . . .
O5 O 0.5071(7) 0.0154(7) 0.8894(7) 0.035(2) Uani 1 1 d D . .
O6 O 0.4578(8) 0.2890(8) 0.4990(7) 0.040(3) Uani 1 1 d . . .
O7 O 0.4234(9) -0.2881(7) 0.8906(7) 0.039(2) Uani 1 1 d . . .
O8 O 0.8097(8) -0.1101(7) 0.6868(8) 0.038(2) Uani 1 1 d . . .
O9 O 0.5860(10) 0.2911(7) 0.6100(8) 0.046(3) Uani 1 1 d . . .
O10 O 0.1944(8) 0.1197(9) 0.8196(8) 0.046(3) Uani 1 1 d . . .
O11 O 0.7341(10) -0.1995(11) 0.5867(9) 0.067(4) Uani 1 1 d . . .
O12 O 0.6295(7) 0.0611(7) 0.6572(8) 0.043(3) Uani 1 1 d . . .
O13 O 0.4578(10) 0.2865(11) 0.3118(9) 0.074(4) Uani 1 1 d . . .
O14 O 0.2763(8) 0.3957(7) 0.4305(10) 0.057(3) Uani 1 1 d . . .
O15 O 0.3754(10) -0.0533(8) 0.7902(11) 0.060(4) Uani 1 1 d . . .
O16 O 0.7905(9) 0.0085(9) 0.4879(9) 0.066(4) Uani 1 1 d . . .
O17 O 0.6800(9) 0.2067(9) 0.4510(9) 0.070(4) Uani 1 1 d . . .
O18 O 0.3211(12) -0.2029(9) 0.7367(12) 0.076(4) Uani 1 1 d U . .
O19 O 0.2083(12) -0.0023(9) 0.6996(12) 0.074(4) Uani 1 1 d U . .
O20 O 0.5844(12) 0.0450(11) 0.5188(12) 0.015(3) Uani 0.50 1 d P . .
O21 O 0.5585(12) -0.0960(11) 0.5735(11) 0.014(3) Uani 0.50 1 d PU . .
O22 O 0.4025(12) -0.0347(11) 0.6148(11) 0.012(3) Uani 0.50 1 d PU . .
O23 O 0.4534(12) 0.0946(11) 0.5386(13) 0.018(3) Uani 0.50 1 d P . .
Cu1 Cu 0.5000 -0.5000 1.5000 0.0351(6) Uani 1 2 d S . .
N1 N 0.7233(13) -0.0888(12) 0.9418(12) 0.059(4) Uani 1 1 d . . .
N2 N 0.6127(8) -0.4863(8) 1.3639(8) 0.027(2) Uani 1 1 d . A .
N3 N 0.9738(15) 0.8677(12) 0.3766(14) 0.066(4) Uani 1 1 d . . .
N4 N 1.0834(10) 0.7403(10) 0.4600(11) 0.048(3) Uani 1 1 d . . .
C1 C 0.8302(16) -0.0927(11) 0.9274(13) 0.049(4) Uani 1 1 d . A .
H1 H 0.8591 -0.0249 0.9057 0.059 Uiso 1 1 calc R . .
C2 C 0.9057(13) -0.1904(10) 0.9419(11) 0.036(3) Uani 1 1 d . . .
H2 H 0.9832 -0.1900 0.9311 0.043 Uiso 1 1 calc R A .
C3 C 0.8608(12) -0.2868(11) 0.9729(10) 0.034(3) Uani 1 1 d . A .
C4 C 0.7486(11) -0.2815(11) 0.9841(10) 0.034(3) Uani 1 1 d . . .
H4 H 0.7164 -0.3472 1.0045 0.041 Uiso 1 1 calc R A .
C5 C 0.6840(14) -0.1811(12) 0.9657(12) 0.047(4) Uani 1 1 d . A .
H5 H 0.6077 -0.1780 0.9704 0.056 Uiso 1 1 calc R . .
C6 C 0.9348(10) -0.3951(9) 0.9905(9) 0.023(3) Uani 1 1 d . . .
C7 C 0.8970(10) -0.4873(10) 1.0808(10) 0.025(3) Uani 1 1 d . A .
C8 C 0.9631(11) -0.5910(10) 1.0879(10) 0.028(3) Uani 1 1 d . . .
H8 H 0.9365 -0.6537 1.1487 0.034 Uiso 1 1 calc R A .
C9 C 0.7955(10) -0.4805(10) 1.1738(9) 0.026(3) Uani 1 1 d . . .
C10 C 0.7147(12) -0.5536(10) 1.2166(10) 0.031(3) Uani 1 1 d . A .
H10 H 0.7203 -0.6030 1.1808 0.037 Uiso 1 1 calc R . .
C11 C 0.6279(11) -0.5541(9) 1.3096(10) 0.029(3) Uani 1 1 d . . .
H11 H 0.5751 -0.6058 1.3375 0.035 Uiso 1 1 calc R A .
C12 C 0.6882(12) -0.4129(10) 1.3208(11) 0.037(3) Uani 1 1 d . . .
H12 H 0.6790 -0.3622 1.3563 0.044 Uiso 1 1 calc R A .
C13 C 0.7777(12) -0.4084(9) 1.2277(10) 0.032(3) Uani 1 1 d . A .
H13 H 0.8283 -0.3546 1.2002 0.038 Uiso 1 1 calc R . .
C14 C 0.9894(16) 0.7627(13) 0.4376(16) 0.060(5) Uani 1 1 d . . .
H14 H 0.9381 0.7103 0.4620 0.072 Uiso 1 1 calc R . .
C15 C 1.0651(18) 0.9123(15) 0.3642(19) 0.086(8) Uani 1 1 d . . .
H15 H 1.0782 0.9872 0.3242 0.103 Uiso 1 1 calc R . .
C16 C 1.1317(18) 0.8382(17) 0.4147(19) 0.082(6) Uani 1 1 d U . .
H16 H 1.1994 0.8491 0.4194 0.098 Uiso 1 1 calc R . .
C17 C 1.1280(14) 0.6347(13) 0.5270(16) 0.070(6) Uani 1 1 d . . .
H17A H 1.1825 0.6481 0.5534 0.084 Uiso 1 1 calc R . .
H17B H 1.1688 0.5861 0.4829 0.084 Uiso 1 1 calc R . .
C18 C 1.0352(15) 0.5798(13) 0.6198(15) 0.051(4) Uani 1 1 d . . .
C19 C 0.9574(17) 0.6303(16) 0.6857(15) 0.063(5) Uani 1 1 d . . .
H19 H 0.9595 0.7055 0.6742 0.076 Uiso 1 1 calc R . .
C20 C 0.9530(18) 0.407(2) 0.7273(16) 0.107(8) Uani 1 1 d DU . .
H20 H 0.9547 0.3302 0.7426 0.129 Uiso 1 1 calc R . .
C21 C 0.869(2) 0.5691(16) 0.7758(18) 0.098(8) Uani 1 1 d DU . .
H21 H 0.8123 0.6050 0.8227 0.118 Uiso 1 1 calc R . .
C22 C 0.866(2) 0.461(2) 0.7934(16) 0.108(8) Uani 1 1 d DU . .
C23 C 1.036(2) 0.4654(18) 0.6395(16) 0.082(7) Uani 1 1 d . . .
H23 H 1.0931 0.4294 0.5930 0.098 Uiso 1 1 calc R A .
Cu2A Cu 0.6593(5) 0.0668(4) 0.8991(4) 0.0427(12) Uani 0.40 1 d PD A 1
C24A C 0.7664(18) 0.405(2) 0.872(2) 0.064 Uiso 0.40 1 d PD A 1
H24A H 0.7990 0.3324 0.9127 0.051 Uiso 0.40 1 calc PR A 1
H24B H 0.7320 0.4466 0.9236 0.051 Uiso 0.40 1 calc PR A 1
N6A N 0.641(3) 0.221(3) 0.871(3) 0.054(9) Uani 0.40 1 d PGU A 1
C25A C 0.701(3) 0.271(3) 0.895(3) 0.052(10) Uani 0.40 1 d PGU A 1
H25A H 0.7563 0.2355 0.9301 0.062 Uiso 0.40 1 calc PR A 1
N5A N 0.669(2) 0.380(2) 0.860(2) 0.049(7) Uani 0.40 1 d PGDU A 1
C26A C 0.589(3) 0.397(2) 0.814(3) 0.068(9) Uani 0.40 1 d PGU A 1
H26A H 0.5517 0.4667 0.7827 0.081 Uiso 0.40 1 calc PR A 1
C27A C 0.572(3) 0.299(3) 0.821(3) 0.057(9) Uani 0.40 1 d PGU A 1
H27A H 0.5198 0.2861 0.7956 0.068 Uiso 0.40 1 calc PR A 1
Cu2B Cu 0.5966(3) 0.0377(2) 0.9538(3) 0.0330(7) Uani 0.60 1 d PD . 2
C24B C 0.7993(17) 0.3865(15) 0.8993(13) 0.049 Uiso 0.60 1 d PD A 2
H24C H 0.8504 0.3369 0.9406 0.040 Uiso 0.60 1 calc PR A 2
H24D H 0.7433 0.4307 0.9431 0.040 Uiso 0.60 1 calc PR A 2
N6B N 0.6498(19) 0.1860(16) 0.8940(17) 0.046(6) Uani 0.60 1 d PGU A 2
C25B C 0.7240(17) 0.2095(17) 0.9298(15) 0.047(6) Uani 0.60 1 d PGU A 2
H25B H 0.7578 0.1588 0.9823 0.056 Uiso 0.60 1 calc PR A 2
N5B N 0.7401(18) 0.3199(17) 0.8757(15) 0.058(7) Uani 0.60 1 d PGDU A 2
C26B C 0.676(2) 0.3647(16) 0.8065(17) 0.068(9) Uani 0.60 1 d PGU A 2
H26B H 0.6709 0.4391 0.7595 0.081 Uiso 0.60 1 calc PR A 2
C27B C 0.620(2) 0.2819(17) 0.8178(18) 0.056(7) Uani 0.60 1 d PGU A 2
H27B H 0.5701 0.2896 0.7799 0.068 Uiso 0.60 1 calc PR A 2
O1W O -0.0387(17) 0.102(2) 0.933(2) 0.070(8) Uani 0.50 1 d P . .
O2W O 0.591(3) 0.541(3) 0.989(3) 0.039(9) Uani 0.25 1 d PU . .
O3W O -0.155(5) 0.176(5) 1.081(5) 0.089(18) Uani 0.25 1 d PU . .

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 0.0267(6) 0.0196(5) 0.0246(6) -0.0117(4) -0.0051(5) -0.0031(4)
Mo2 0.0209(6) 0.0429(7) 0.0221(6) -0.0071(5) -0.0097(5) -0.0032(5)
Mo3 0.0313(7) 0.0287(6) 0.0339(7) -0.0214(5) -0.0160(5) 0.0076(5)
Mo4 0.0583(9) 0.0250(6) 0.0262(6) 0.0031(5) -0.0243(6) -0.0167(5)
V1 0.0270(12) 0.0243(10) 0.0206(11) -0.0096(8) -0.0118(9) -0.0017(8)
V2 0.0191(10) 0.0099(8) 0.0124(9) -0.0064(7) -0.0045(8) 0.0012(7)
V3 0.0156(11) 0.0154(10) 0.0397(13) -0.0016(9) -0.0112(10) -0.0053(8)
P1 0.022(2) 0.017(2) 0.022(2) -0.0069(17) -0.0094(19) -0.0019(16)
O1 0.024(5) 0.026(4) 0.019(4) -0.006(4) -0.002(4) -0.001(3)
O2 0.037(6) 0.034(5) 0.042(6) -0.027(4) 0.000(5) -0.013(4)
O3 0.027(5) 0.067(7) 0.023(5) 0.008(5) -0.009(4) -0.018(5)
O4 0.024(5) 0.039(5) 0.035(5) -0.015(4) 0.009(4) -0.004(4)
O5 0.034(6) 0.053(6) 0.031(5) -0.027(4) -0.018(4) 0.004(4)
O6 0.029(5) 0.063(6) 0.016(5) 0.002(4) -0.003(4) -0.016(5)
O7 0.062(7) 0.026(5) 0.020(5) -0.002(4) -0.004(5) -0.016(4)
O8 0.031(5) 0.045(5) 0.060(7) -0.035(5) -0.033(5) 0.017(4)
O9 0.076(8) 0.034(5) 0.046(6) -0.008(5) -0.039(6) -0.014(5)
O10 0.025(5) 0.082(8) 0.027(5) -0.023(5) -0.001(4) -0.002(5)
O11 0.060(8) 0.114(10) 0.043(7) -0.057(7) 0.032(6) -0.066(7)
O12 0.017(5) 0.028(5) 0.054(7) 0.002(5) 0.002(4) 0.003(4)
O13 0.065(8) 0.123(10) 0.056(8) -0.069(8) 0.035(6) -0.071(8)
O14 0.032(6) 0.019(5) 0.101(10) 0.000(5) -0.028(6) 0.009(4)
O15 0.057(7) 0.025(5) 0.124(11) -0.019(6) -0.067(8) 0.006(5)
O16 0.041(7) 0.049(7) 0.040(6) 0.004(5) 0.017(5) 0.028(5)
O17 0.049(7) 0.043(6) 0.040(6) 0.012(5) 0.019(5) 0.026(5)
O18 0.097(8) 0.046(6) 0.130(9) -0.038(6) -0.081(7) 0.002(5)
O19 0.096(8) 0.052(6) 0.121(8) -0.039(6) -0.085(7) 0.013(5)
O20 0.012(8) 0.011(7) 0.027(9) -0.012(6) -0.004(7) -0.002(6)
O21 0.018(5) 0.010(5) 0.012(5) -0.007(4) -0.003(4) 0.004(4)
O22 0.010(6) 0.017(6) 0.015(6) -0.014(5) -0.003(5) 0.001(5)
O23 0.017(8) 0.004(7) 0.027(9) 0.002(6) -0.010(7) 0.001(6)
Cu1 0.0297(13) 0.0332(12) 0.0218(12) -0.0102(10) 0.0121(10) -0.0001(10)
N1 0.071(11) 0.066(10) 0.063(10) -0.048(8) -0.046(9) 0.038(8)
N2 0.020(6) 0.020(5) 0.024(5) -0.011(4) 0.011(4) 0.003(4)
N3 0.085(12) 0.047(9) 0.079(11) -0.025(8) -0.038(10) -0.005(8)
N4 0.032(7) 0.037(7) 0.063(9) -0.004(6) -0.012(7) -0.010(5)
C1 0.088(14) 0.019(7) 0.045(9) -0.009(6) -0.032(10) -0.002(7)
C2 0.049(9) 0.023(7) 0.033(8) -0.016(6) -0.010(7) 0.006(6)
C3 0.035(8) 0.032(7) 0.019(7) -0.006(6) -0.002(6) 0.006(6)
C4 0.030(8) 0.039(8) 0.023(7) -0.008(6) 0.000(6) -0.004(6)
C5 0.055(10) 0.041(9) 0.040(9) -0.022(7) -0.022(8) 0.024(7)
C6 0.027(7) 0.015(5) 0.016(6) -0.006(5) 0.001(5) 0.006(5)
C7 0.020(7) 0.027(6) 0.020(6) -0.011(5) 0.003(5) -0.003(5)
C8 0.031(7) 0.027(6) 0.014(6) -0.011(5) 0.008(5) -0.001(5)
C9 0.019(6) 0.026(6) 0.015(6) 0.000(5) 0.005(5) -0.003(5)
C10 0.045(9) 0.022(6) 0.018(6) -0.008(5) -0.003(6) 0.000(6)
C11 0.026(7) 0.018(6) 0.029(7) -0.002(5) 0.006(6) -0.011(5)
C12 0.041(9) 0.026(7) 0.029(7) -0.007(6) 0.003(6) -0.008(6)
C13 0.045(9) 0.017(6) 0.021(7) -0.006(5) 0.002(6) -0.004(5)
C14 0.071(13) 0.050(10) 0.095(15) -0.030(10) -0.050(12) -0.018(9)
C15 0.066(14) 0.042(10) 0.098(17) 0.000(11) 0.002(12) -0.002(10)
C16 0.059(9) 0.073(9) 0.104(11) -0.019(8) -0.021(8) -0.017(8)
C17 0.038(10) 0.038(9) 0.090(15) 0.008(9) -0.011(10) 0.004(7)
C18 0.061(12) 0.043(9) 0.060(11) -0.012(8) -0.031(10) -0.013(8)
C19 0.072(14) 0.065(11) 0.060(12) -0.017(10) -0.020(11) -0.030(10)
C20 0.115(12) 0.101(11) 0.110(12) -0.036(9) -0.021(9) -0.044(9)
C21 0.107(12) 0.118(12) 0.081(11) -0.041(9) -0.031(9) -0.018(9)
C22 0.114(12) 0.107(11) 0.111(12) -0.033(9) -0.018(9) -0.063(9)
C23 0.104(18) 0.093(15) 0.058(13) -0.018(11) -0.018(12) -0.054(14)
Cu2A 0.056(3) 0.023(2) 0.033(3) -0.007(2) -0.005(3) 0.005(2)
N6A 0.048(13) 0.059(10) 0.061(14) -0.022(9) -0.019(10) -0.007(8)
C25A 0.06(3) 0.071(19) 0.03(2) -0.01(2) -0.02(2) -0.02(2)
N5A 0.05(2) 0.063(15) 0.021(18) -0.018(16) 0.012(15) -0.023(15)
C26A 0.072(13) 0.064(10) 0.065(14) -0.021(9) -0.023(10) -0.003(9)
C27A 0.048(13) 0.064(12) 0.058(14) -0.019(9) -0.021(10) -0.003(9)
Cu2B 0.044(2) 0.0292(16) 0.0310(17) -0.0152(13) -0.0177(15) 0.0051(14)
N6B 0.048(15) 0.071(13) 0.024(12) -0.012(10) -0.004(10) -0.032(13)
C25B 0.034(15) 0.079(15) 0.037(17) -0.037(12) -0.005(11) -0.004(13)
N5B 0.066(18) 0.095(17) 0.036(14) -0.037(13) 0.002(12) -0.049(15)
C26B 0.09(2) 0.085(16) 0.025(15) 0.000(13) 0.001(14) -0.059(18)
C27B 0.070(12) 0.070(11) 0.051(11) -0.026(8) -0.030(9) -0.019(8)
O1W 0.022(12) 0.094(18) 0.14(2) -0.091(18) -0.024(14) 0.007(11)
O2W 0.038(13) 0.034(12) 0.037(13) -0.003(9) -0.014(9) -0.002(9)
O3W 0.08(2) 0.09(2) 0.09(2) -0.028(11) -0.028(12) -0.009(11)

_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 O9 1.652(9) . ?
Mo1 O17 1.777(10) . ?
Mo1 O6 1.795(9) . ?
Mo1 O1 2.050(8) . ?
Mo1 O12 2.052(8) . ?
Mo1 O20 2.386(14) . ?
Mo1 O23 2.454(15) . ?
Mo1 V1 3.086(3) . ?
Mo2 O8 1.656(8) . ?
Mo2 O11 1.786(11) . ?
Mo2 O16 1.794(10) . ?
Mo2 O2 2.059(9) . ?
Mo2 O12 2.066(10) . ?
Mo2 O21 2.477(14) . ?
Mo2 V1 3.099(3) . ?
Mo3 O10 1.669(10) . ?
Mo3 O3 1.775(8) . ?
Mo3 O19 1.794(11) . ?
Mo3 O1 2.021(8) . ?
Mo3 O15 2.052(9) . ?
Mo3 O22 2.379(14) . ?
Mo3 V1 3.067(2) . ?
Mo4 O7 1.666(8) . ?
Mo4 O13 1.778(12) 2_656 ?
Mo4 O18 1.793(11) . ?
Mo4 O2 2.035(9) . ?
Mo4 O15 2.070(11) . ?
Mo4 O22 2.503(13) . ?
Mo4 V1 3.096(2) . ?
V1 O5 1.688(8) . ?
V1 O15 1.883(10) . ?
V1 O2 1.897(9) . ?
V1 O12 1.904(9) . ?
V1 O1 1.905(8) . ?
V2 O14 1.590(9) . ?
V2 O11 1.906(10) 2_656 ?
V2 O6 1.914(9) . ?
V2 O3 1.922(9) . ?
V2 O13 1.930(11) . ?
V3 O4 1.589(9) . ?
V3 O16 1.911(10) . ?
V3 O17 1.912(12) . ?
V3 O18 1.913(11) 2_656 ?
V3 O19 1.940(12) 2_656 ?
P1 O23 1.465(15) 2_656 ?
P1 O23 1.465(15) . ?
P1 O20 1.512(14) . ?
P1 O20 1.512(14) 2_656 ?
P1 O21 1.531(13) 2_656 ?
P1 O21 1.531(13) . ?
P1 O22 1.604(14) 2_656 ?
P1 O22 1.604(14) . ?
O5 Cu2B 1.857(6) . ?
O5 Cu2B 2.046(10) 2_657 ?
O5 Cu2A 2.297(7) . ?
O11 V2 1.906(10) 2_656 ?
O13 Mo4 1.778(12) 2_656 ?
O18 V3 1.913(11) 2_656 ?
O19 V3 1.940(12) 2_656 ?
O20 O23 1.61(2) . ?
O20 O21 1.782(19) . ?
O21 O23 1.65(2) 2_656 ?
O22 O23 1.759(19) . ?
O23 O21 1.65(2) 2_656 ?
Cu1 N2 1.890(10) . ?
Cu1 N2 1.890(10) 2_648 ?
N1 C1 1.30(2) . ?
N1 C5 1.31(2) . ?
N1 Cu2A 1.958(14) . ?
N1 Cu2B 2.033(13) . ?
N2 C11 1.337(17) . ?
N2 C12 1.347(16) . ?
N3 C14 1.33(2) . ?
N3 C15 1.37(3) . ?
N4 C14 1.302(19) . ?
N4 C16 1.39(2) . ?
N4 C17 1.467(18) . ?
C1 C2 1.404(19) . ?
C1 H1 0.9500 . ?
C2 C3 1.376(19) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(19) . ?
C3 C6 1.497(16) . ?
C4 C5 1.365(18) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C8 1.385(17) 2_747 ?
C6 C7 1.398(15) . ?
C7 C8 1.410(16) . ?
C7 C9 1.474(16) . ?
C8 C6 1.385(17) 2_747 ?
C8 H8 0.9500 . ?
C9 C13 1.374(18) . ?
C9 C10 1.395(17) . ?
C10 C11 1.363(17) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.372(18) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.30(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.47(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.33(3) . ?
C18 C23 1.43(3) . ?
C19 C21 1.46(2) . ?
C19 H19 0.9500 . ?
C20 C23 1.39(2) . ?
C20 C22 1.40(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.35(3) . ?
C21 H21 0.9500 . ?
C22 C24A 1.477(10) . ?
C22 C24B 1.498(10) . ?
C23 H23 0.9500 . ?
Cu2A N6A 1.89(3) . ?
C24A N5A 1.464(11) . ?
C24A C25A 2.02(4) . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
N6A C27A 1.34(2) . ?
N6A C25A 1.34(2) . ?
C25A N5A 1.34(2) . ?
C25A H25A 0.9500 . ?
N5A C26A 1.34(2) . ?
C26A C27A 1.34(2) . ?
C26A H26A 0.9500 . ?
C27A H27A 0.9500 . ?
Cu2B N6B 1.992(17) . ?
Cu2B O5 2.046(10) 2_657 ?
Cu2B Cu2B 2.574(7) 2_657 ?
C24B N5B 1.498(10) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
N6B C25B 1.384(13) . ?
N6B C27B 1.384(13) . ?
C25B N5B 1.384(13) . ?
C25B H25B 0.9500 . ?
N5B C26B 1.384(13) . ?
C26B C27B 1.384(13) . ?
C26B H26B 0.9500 . ?
C27B H27B 0.9500 . ?

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
O9 Mo1 O17 101.3(6) . . ?
O9 Mo1 O6 102.8(5) . . ?
O17 Mo1 O6 98.8(5) . . ?
O9 Mo1 O1 100.0(5) . . ?
O17 Mo1 O1 155.2(5) . . ?
O6 Mo1 O1 88.7(4) . . ?
O9 Mo1 O12 97.8(4) . . ?
O17 Mo1 O12 90.4(4) . . ?
O6 Mo1 O12 155.1(4) . . ?
O1 Mo1 O12 74.1(3) . . ?
O9 Mo1 O20 157.9(5) . . ?
O17 Mo1 O20 69.1(6) . . ?
O6 Mo1 O20 98.4(5) . . ?
O1 Mo1 O20 86.4(4) . . ?
O12 Mo1 O20 63.4(5) . . ?
O9 Mo1 O23 160.7(6) . . ?
O17 Mo1 O23 96.8(6) . . ?
O6 Mo1 O23 67.4(4) . . ?
O1 Mo1 O23 64.2(4) . . ?
O12 Mo1 O23 88.7(4) . . ?
O20 Mo1 O23 38.7(5) . . ?
O9 Mo1 V1 100.8(3) . . ?
O17 Mo1 V1 125.1(3) . . ?
O6 Mo1 V1 123.8(3) . . ?
O1 Mo1 V1 37.1(2) . . ?
O12 Mo1 V1 37.1(3) . . ?
O20 Mo1 V1 71.7(4) . . ?
O23 Mo1 V1 73.7(3) . . ?
O8 Mo2 O11 103.9(5) . . ?
O8 Mo2 O16 103.4(6) . . ?
O11 Mo2 O16 97.6(5) . . ?
O8 Mo2 O2 99.7(5) . . ?
O11 Mo2 O2 90.6(4) . . ?
O16 Mo2 O2 152.8(4) . . ?
O8 Mo2 O12 98.7(4) . . ?
O11 Mo2 O12 154.2(5) . . ?
O16 Mo2 O12 88.9(4) . . ?
O2 Mo2 O12 73.4(3) . . ?
O8 Mo2 O21 158.9(5) . . ?
O11 Mo2 O21 65.0(5) . . ?
O16 Mo2 O21 96.0(5) . . ?
O2 Mo2 O21 64.1(4) . . ?
O12 Mo2 O21 89.6(4) . . ?
O8 Mo2 V1 101.0(3) . . ?
O11 Mo2 V1 124.7(3) . . ?
O16 Mo2 V1 123.1(3) . . ?
O2 Mo2 V1 36.6(2) . . ?
O12 Mo2 V1 36.8(2) . . ?
O21 Mo2 V1 74.4(3) . . ?
O10 Mo3 O3 103.5(5) . . ?
O10 Mo3 O19 103.1(6) . . ?
O3 Mo3 O19 95.8(5) . . ?
O10 Mo3 O1 100.1(4) . . ?
O3 Mo3 O1 90.3(4) . . ?
O19 Mo3 O1 153.9(5) . . ?
O10 Mo3 O15 100.0(5) . . ?
O3 Mo3 O15 153.8(5) . . ?
O19 Mo3 O15 90.1(4) . . ?
O1 Mo3 O15 74.1(4) . . ?
O10 Mo3 O22 157.6(5) . . ?
O3 Mo3 O22 97.3(5) . . ?
O19 Mo3 O22 66.2(6) . . ?
O1 Mo3 O22 87.9(4) . . ?
O15 Mo3 O22 61.9(5) . . ?
O10 Mo3 V1 101.1(3) . . ?
O3 Mo3 V1 125.3(3) . . ?
O19 Mo3 V1 124.8(4) . . ?
O1 Mo3 V1 37.3(2) . . ?
O15 Mo3 V1 36.9(3) . . ?
O22 Mo3 V1 72.8(3) . . ?
O7 Mo4 O13 102.3(6) . 2_656 ?
O7 Mo4 O18 102.5(6) . . ?
O13 Mo4 O18 98.4(6) 2_656 . ?
O7 Mo4 O2 99.6(4) . . ?
O13 Mo4 O2 91.3(4) 2_656 . ?
O18 Mo4 O2 153.3(5) . . ?
O7 Mo4 O15 100.3(5) . . ?
O13 Mo4 O15 154.3(5) 2_656 . ?
O18 Mo4 O15 88.5(5) . . ?
O2 Mo4 O15 72.8(4) . . ?
O7 Mo4 O22 155.3(5) . . ?
O13 Mo4 O22 101.0(6) 2_656 . ?
O18 Mo4 O22 65.8(5) . . ?
O2 Mo4 O22 88.0(4) . . ?
O15 Mo4 O22 59.4(5) . . ?
O7 Mo4 V1 101.8(3) . . ?
O13 Mo4 V1 125.4(3) 2_656 . ?
O18 Mo4 V1 122.7(4) . . ?
O2 Mo4 V1 36.5(3) . . ?
O15 Mo4 V1 36.3(3) . . ?
O22 Mo4 V1 70.7(3) . . ?
O5 V1 O15 117.4(5) . . ?
O5 V1 O2 115.6(4) . . ?
O15 V1 O2 80.3(4) . . ?
O5 V1 O12 109.6(5) . . ?
O15 V1 O12 133.0(6) . . ?
O2 V1 O12 80.9(4) . . ?
O5 V1 O1 112.0(4) . . ?
O15 V1 O1 80.8(4) . . ?
O2 V1 O1 132.3(4) . . ?
O12 V1 O1 80.9(4) . . ?
O5 V1 Mo3 121.4(3) . . ?
O15 V1 Mo3 40.8(3) . . ?
O2 V1 Mo3 110.9(3) . . ?
O12 V1 Mo3 111.1(3) . . ?
O1 V1 Mo3 40.0(3) . . ?
O5 V1 Mo1 117.4(3) . . ?
O15 V1 Mo1 110.3(4) . . ?
O2 V1 Mo1 110.1(3) . . ?
O12 V1 Mo1 40.5(3) . . ?
O1 V1 Mo1 40.5(2) . . ?
Mo3 V1 Mo1 74.68(6) . . ?
O5 V1 Mo4 125.0(3) . . ?
O15 V1 Mo4 40.6(3) . . ?
O2 V1 Mo4 39.7(3) . . ?
O12 V1 Mo4 110.2(3) . . ?
O1 V1 Mo4 110.4(3) . . ?
Mo3 V1 Mo4 75.54(6) . . ?
Mo1 V1 Mo4 117.57(7) . . ?
O5 V1 Mo2 119.8(3) . . ?
O15 V1 Mo2 110.0(4) . . ?
O2 V1 Mo2 40.3(3) . . ?
O12 V1 Mo2 40.6(3) . . ?
O1 V1 Mo2 110.3(3) . . ?
Mo3 V1 Mo2 118.63(7) . . ?
Mo1 V1 Mo2 74.50(6) . . ?
Mo4 V1 Mo2 73.93(6) . . ?
O14 V2 O11 103.3(6) . 2_656 ?
O14 V2 O6 101.4(5) . . ?
O11 V2 O6 155.4(5) 2_656 . ?
O14 V2 O3 102.2(6) . . ?
O11 V2 O3 88.5(4) 2_656 . ?
O6 V2 O3 86.5(4) . . ?
O14 V2 O13 102.6(6) . . ?
O11 V2 O13 86.5(4) 2_656 . ?
O6 V2 O13 88.0(5) . . ?
O3 V2 O13 155.2(6) . . ?
O4 V3 O16 102.3(5) . . ?
O4 V3 O17 101.9(5) . . ?
O16 V3 O17 86.0(5) . . ?
O4 V3 O18 101.3(6) . 2_656 ?
O16 V3 O18 156.4(6) . 2_656 ?
O17 V3 O18 89.4(5) . 2_656 ?
O4 V3 O19 101.2(6) . 2_656 ?
O16 V3 O19 88.6(5) . 2_656 ?
O17 V3 O19 156.9(6) . 2_656 ?
O18 V3 O19 86.6(5) 2_656 2_656 ?
O23 P1 O23 180.0(12) 2_656 . ?
O23 P1 O20 114.7(8) 2_656 . ?
O23 P1 O20 65.3(8) . . ?
O23 P1 O20 65.3(8) 2_656 2_656 ?
O23 P1 O20 114.7(8) . 2_656 ?
O20 P1 O20 180.0(9) . 2_656 ?
O23 P1 O21 113.2(8) 2_656 2_656 ?
O23 P1 O21 66.8(8) . 2_656 ?
O20 P1 O21 108.3(7) . 2_656 ?
O20 P1 O21 71.7(7) 2_656 2_656 ?
O23 P1 O21 66.8(8) 2_656 . ?
O23 P1 O21 113.2(8) . . ?
O20 P1 O21 71.7(7) . . ?
O20 P1 O21 108.3(7) 2_656 . ?
O21 P1 O21 180.0(10) 2_656 . ?
O23 P1 O22 69.8(7) 2_656 2_656 ?
O23 P1 O22 110.2(7) . 2_656 ?
O20 P1 O22 74.9(7) . 2_656 ?
O20 P1 O22 105.1(7) 2_656 2_656 ?
O21 P1 O22 75.5(7) 2_656 2_656 ?
O21 P1 O22 104.5(7) . 2_656 ?
O23 P1 O22 110.2(7) 2_656 . ?
O23 P1 O22 69.8(7) . . ?
O20 P1 O22 105.1(7) . . ?
O20 P1 O22 74.9(7) 2_656 . ?
O21 P1 O22 104.5(7) 2_656 . ?
O21 P1 O22 75.5(7) . . ?
O22 P1 O22 180.0(9) 2_656 . ?
V1 O1 Mo3 102.7(4) . . ?
V1 O1 Mo1 102.5(4) . . ?
Mo3 O1 Mo1 132.9(4) . . ?
V1 O2 Mo4 103.8(4) . . ?
V1 O2 Mo2 103.1(4) . . ?
Mo4 O2 Mo2 131.0(5) . . ?
Mo3 O3 V2 141.5(6) . . ?
V1 O5 Cu2B 146.1(6) . . ?
V1 O5 Cu2B 130.1(4) . 2_657 ?
Cu2B O5 Cu2B 82.4(4) . 2_657 ?
V1 O5 Cu2A 124.2(5) . . ?
Cu2B O5 Cu2A 22.48(16) . . ?
Cu2B O5 Cu2A 104.8(4) 2_657 . ?
Mo1 O6 V2 140.6(6) . . ?
Mo2 O11 V2 141.7(8) . 2_656 ?
V1 O12 Mo1 102.5(4) . . ?
V1 O12 Mo2 102.6(4) . . ?
Mo1 O12 Mo2 130.8(6) . . ?
Mo4 O13 V2 140.8(8) 2_656 . ?
V1 O15 Mo3 102.3(4) . . ?
V1 O15 Mo4 103.0(5) . . ?
Mo3 O15 Mo4 132.7(6) . . ?
Mo2 O16 V3 141.8(7) . . ?
Mo1 O17 V3 140.0(7) . . ?
Mo4 O18 V3 140.8(8) . 2_656 ?
Mo3 O19 V3 139.8(8) . 2_656 ?
P1 O20 O23 55.9(7) . . ?
P1 O20 O21 54.7(6) . . ?
O23 O20 O21 95.1(10) . . ?
P1 O20 Mo1 128.7(8) . . ?
O23 O20 Mo1 72.9(7) . . ?
O21 O20 Mo1 142.9(9) . . ?
P1 O21 O23 54.7(7) . 2_656 ?
P1 O21 O20 53.7(6) . . ?
O23 O21 O20 93.8(9) 2_656 . ?
P1 O21 Mo2 123.9(7) . . ?
O23 O21 Mo2 133.3(9) 2_656 . ?
O20 O21 Mo2 70.4(7) . . ?
P1 O22 O23 51.4(7) . . ?
P1 O22 Mo3 126.6(7) . . ?
O23 O22 Mo3 75.4(7) . . ?
P1 O22 Mo4 118.4(7) . . ?
O23 O22 Mo4 135.9(8) . . ?
Mo3 O22 Mo4 101.3(5) . . ?
P1 O23 O20 58.7(7) . . ?
P1 O23 O21 58.5(7) . 2_656 ?
O20 O23 O21 98.5(12) . 2_656 ?
P1 O23 O22 58.8(7) . . ?
O20 O23 O22 94.5(9) . . ?
O21 O23 O22 93.3(10) 2_656 . ?
P1 O23 Mo1 126.9(8) . . ?
O20 O23 Mo1 68.3(7) . . ?
O21 O23 Mo1 130.6(9) 2_656 . ?
O22 O23 Mo1 133.7(9) . . ?
N2 Cu1 N2 180.0(6) . 2_648 ?
C1 N1 C5 118.3(13) . . ?
C1 N1 Cu2A 108.3(12) . . ?
C5 N1 Cu2A 132.6(12) . . ?
C1 N1 Cu2B 129.5(12) . . ?
C5 N1 Cu2B 111.6(12) . . ?
Cu2A N1 Cu2B 26.5(2) . . ?
C11 N2 C12 116.3(11) . . ?
C11 N2 Cu1 122.2(8) . . ?
C12 N2 Cu1 121.2(9) . . ?
C14 N3 C15 104.2(15) . . ?
C14 N4 C16 107.0(14) . . ?
C14 N4 C17 127.6(14) . . ?
C16 N4 C17 125.2(15) . . ?
N1 C1 C2 124.4(14) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
C3 C2 C1 116.0(14) . . ?
C3 C2 H2 122.0 . . ?
C1 C2 H2 122.0 . . ?
C2 C3 C4 119.2(12) . . ?
C2 C3 C6 119.8(13) . . ?
C4 C3 C6 120.9(12) . . ?
C5 C4 C3 119.4(14) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 122.5(16) . . ?
N1 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C8 C6 C7 118.5(10) 2_747 . ?
C8 C6 C3 120.5(10) 2_747 . ?
C7 C6 C3 120.7(11) . . ?
C6 C7 C8 119.0(11) . . ?
C6 C7 C9 123.2(10) . . ?
C8 C7 C9 117.6(10) . . ?
C6 C8 C7 122.5(11) 2_747 . ?
C6 C8 H8 118.8 2_747 . ?
C7 C8 H8 118.8 . . ?
C13 C9 C10 116.1(12) . . ?
C13 C9 C7 123.0(12) . . ?
C10 C9 C7 120.8(12) . . ?
C11 C10 C9 119.9(12) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
N2 C11 C10 123.9(12) . . ?
N2 C11 H11 118.0 . . ?
C10 C11 H11 118.0 . . ?
N2 C12 C13 122.7(13) . . ?
N2 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
C12 C13 C9 121.0(12) . . ?
C12 C13 H13 119.5 . . ?
C9 C13 H13 119.5 . . ?
N4 C14 N3 111.7(14) . . ?
N4 C14 H14 124.1 . . ?
N3 C14 H14 124.1 . . ?
C16 C15 N3 111.0(17) . . ?
C16 C15 H15 124.5 . . ?
N3 C15 H15 124.5 . . ?
C15 C16 N4 106.0(19) . . ?
C15 C16 H16 127.0 . . ?
N4 C16 H16 127.0 . . ?
N4 C17 C18 110.4(13) . . ?
N4 C17 H17A 109.6 . . ?
C18 C17 H17A 109.6 . . ?
N4 C17 H17B 109.6 . . ?
C18 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
C19 C18 C23 120.7(18) . . ?
C19 C18 C17 123.2(16) . . ?
C23 C18 C17 116.0(18) . . ?
C18 C19 C21 119.3(19) . . ?
C18 C19 H19 120.3 . . ?
C21 C19 H19 120.3 . . ?
C23 C20 C22 120(2) . . ?
C23 C20 H20 119.9 . . ?
C22 C20 H20 119.9 . . ?
C22 C21 C19 121(2) . . ?
C22 C21 H21 119.7 . . ?
C19 C21 H21 119.7 . . ?
C21 C22 C20 119.6(17) . . ?
C21 C22 C24A 120(2) . . ?
C20 C22 C24A 120(2) . . ?
C21 C22 C24B 123(2) . . ?
C20 C22 C24B 114.9(19) . . ?
C24A C22 C24B 24.1(14) . . ?
C20 C23 C18 119(2) . . ?
C20 C23 H23 120.3 . . ?
C18 C23 H23 120.3 . . ?
N6A Cu2A N1 159.5(11) . . ?
N6A Cu2A O5 110.6(11) . . ?
N1 Cu2A O5 89.6(6) . . ?
N5A C24A C22 133(3) . . ?
N5A C24A C25A 41.5(12) . . ?
C22 C24A C25A 135(2) . . ?
N5A C24A H24A 104.1 . . ?
C22 C24A H24A 104.1 . . ?
C25A C24A H24A 63.3 . . ?
N5A C24A H24B 104.1 . . ?
C22 C24A H24B 104.1 . . ?
C25A C24A H24B 120.9 . . ?
H24A C24A H24B 105.5 . . ?
C27A N6A C25A 108.0 . . ?
C27A N6A Cu2A 128(2) . . ?
C25A N6A Cu2A 124(2) . . ?
N6A C25A N5A 108.0 . . ?
N6A C25A C24A 152.0(14) . . ?
N5A C25A C24A 46.4(12) . . ?
N6A C25A H25A 126.0 . . ?
N5A C25A H25A 126.0 . . ?
C24A C25A H25A 80.5 . . ?
C26A N5A C25A 108.0 . . ?
C26A N5A C24A 156(2) . . ?
C25A N5A C24A 92(2) . . ?
C27A C26A N5A 108.0 . . ?
C27A C26A H26A 126.0 . . ?
N5A C26A H26A 126.0 . . ?
C26A C27A N6A 108.0 . . ?
C26A C27A H27A 126.0 . . ?
N6A C27A H27A 126.0 . . ?
O5 Cu2B N6B 117.2(6) . . ?
O5 Cu2B N1 101.2(5) . . ?
N6B Cu2B N1 114.2(9) . . ?
O5 Cu2B O5 97.6(4) . 2_657 ?
N6B Cu2B O5 119.2(7) . 2_657 ?
N1 Cu2B O5 104.6(5) . 2_657 ?
O5 Cu2B Cu2B 52.0(3) . 2_657 ?
N6B Cu2B Cu2B 135.8(7) . 2_657 ?
N1 Cu2B Cu2B 109.9(5) . 2_657 ?
O5 Cu2B Cu2B 45.7(2) 2_657 2_657 ?
N5B C24B C22 107.9(15) . . ?
N5B C24B H24C 110.1 . . ?
C22 C24B H24C 110.1 . . ?
N5B C24B H24D 110.1 . . ?
C22 C24B H24D 110.1 . . ?
H24C C24B H24D 108.4 . . ?
C25B N6B C27B 108.0 . . ?
C25B N6B Cu2B 122.4(11) . . ?
C27B N6B Cu2B 129.6(11) . . ?
N6B C25B N5B 108.0 . . ?
N6B C25B H25B 126.0 . . ?
N5B C25B H25B 126.0 . . ?
C25B N5B C26B 108.0 . . ?
C25B N5B C24B 127.0(16) . . ?
C26B N5B C24B 124.2(16) . . ?
C27B C26B N5B 108.0 . . ?
C27B C26B H26B 126.0 . . ?
N5B C26B H26B 126.0 . . ?
C26B C27B N6B 108.0 . . ?
C26B C27B H27B 126.0 . . ?
N6B C27B H27B 126.0 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.859
_refine_diff_density_min         -1.855
_refine_diff_density_rms         0.204

# Attachment 'compound_2.CIF'

data_meng
_database_code_depnum_ccdc_archive 'CCDC 776678'
#TrackingRef 'compound_2.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H21 Cl2 Cu2 N4 O'
_chemical_formula_weight         603.45

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'

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

_cell_length_a                   11.366(2)
_cell_length_b                   11.188(2)
_cell_length_c                   19.927(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2533.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    18015
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1220
_exptl_absorpt_coefficient_mu    1.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotation anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean 0.01
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            18015
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2211
_reflns_number_gt                1383
_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.
During the refinement, the restraint command 'isor' was used to refine the
non-H atom (C13) with NPD and ADP problems. This restraint command led to
a restraint value (6), but it cannot be totally avoided in order to get
a reasonable refinement.
;

_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^)+(0.1076P)^2^+5.0010P] 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         2211
_refine_ls_number_parameters     172
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0671
_refine_ls_wR_factor_ref         0.2062
_refine_ls_wR_factor_gt          0.1763
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.019
_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
Cu1 Cu 0.12712(9) 0.08788(8) 0.68407(5) 0.0639(4) Uani 1 1 d . . .
Cl1 Cl 0.0964(2) 0.2567(2) 0.63190(14) 0.0877(8) Uani 1 1 d . . .
C1 C 0.1942(7) 0.1404(7) 0.8216(4) 0.066(2) Uani 1 1 d . . .
H1A H 0.1353 0.1977 0.8176 0.079 Uiso 1 1 calc R . .
C2 C 0.2537(8) 0.1338(8) 0.8814(4) 0.073(2) Uani 1 1 d . . .
H2A H 0.2336 0.1846 0.9165 0.088 Uiso 1 1 calc R . .
C3 C 0.3412(8) 0.0539(6) 0.8892(4) 0.067(2) Uani 1 1 d . . .
C4 C 0.3662(7) -0.0201(6) 0.8349(4) 0.066(2) Uani 1 1 d . . .
H4A H 0.4258 -0.0767 0.8379 0.079 Uiso 1 1 calc R . .
C5 C 0.3014(7) -0.0087(6) 0.7765(4) 0.0564(18) Uani 1 1 d . . .
H5A H 0.3192 -0.0586 0.7406 0.068 Uiso 1 1 calc R . .
C6 C 0.4121(10) 0.0456(8) 0.9542(5) 0.093(3) Uani 1 1 d . . .
C7 C 0.4015(8) -0.0773(7) 0.9860(4) 0.068(2) Uani 1 1 d . . .
H7A H 0.4316 -0.1368 0.9550 0.082 Uiso 1 1 calc R . .
H7B H 0.3190 -0.0948 0.9939 0.082 Uiso 1 1 calc R . .
C8 C 0.5307(10) 0.0867(8) 0.9470(5) 0.092(3) Uani 1 1 d . . .
C9 C 0.5931(9) 0.3300(7) 0.8235(4) 0.078(3) Uani 1 1 d . . .
H9A H 0.6162 0.3336 0.7788 0.094 Uiso 1 1 calc R . .
C10 C 0.5769(8) 0.2199(7) 0.8510(4) 0.070(2) Uani 1 1 d . . .
H10A H 0.5878 0.1517 0.8251 0.084 Uiso 1 1 calc R . .
C11 C 0.5452(8) 0.2098(6) 0.9155(4) 0.067(2) Uani 1 1 d . . .
C12 C 0.5279(11) 0.3117(9) 0.9487(4) 0.105(4) Uani 1 1 d . . .
H12A H 0.5047 0.3091 0.9934 0.126 Uiso 1 1 calc R . .
C13 C 0.5441(10) 0.4225(8) 0.9176(4) 0.088(3) Uani 1 1 d U . .
H13A H 0.5297 0.4916 0.9422 0.105 Uiso 1 1 calc R . .
N1 N 0.2148(5) 0.0704(4) 0.7691(3) 0.0512(14) Uani 1 1 d . . .
N2 N 0.5784(6) 0.4326(5) 0.8559(3) 0.0586(16) Uani 1 1 d . . .
O1 O 0.3453(15) 0.1510(12) 1.0020(7) 0.055(4) Uani 0.30 1 d P . .
H1B H 0.3474 0.1306 1.0415 0.082 Uiso 0.30 1 calc PR . .
O2 O 0.595(2) 0.0037(19) 0.8943(10) 0.056(6) Uani 0.20 1 d P . .
H2B H 0.6234 -0.0542 0.9137 0.083 Uiso 0.20 1 calc PR . .

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
Cu1 0.0689(7) 0.0628(6) 0.0600(6) -0.0057(4) -0.0211(5) 0.0062(5)
Cl1 0.0705(16) 0.0721(13) 0.1206(19) 0.0269(12) -0.0123(13) 0.0066(10)
C1 0.052(5) 0.073(5) 0.072(5) -0.012(4) -0.010(4) 0.010(4)
C2 0.084(6) 0.082(5) 0.054(4) -0.010(4) -0.007(4) -0.003(5)
C3 0.096(7) 0.047(4) 0.058(4) 0.011(3) -0.033(4) -0.025(4)
C4 0.065(5) 0.041(4) 0.092(6) 0.013(4) -0.035(4) -0.002(3)
C5 0.064(5) 0.042(3) 0.063(4) -0.008(3) -0.010(4) 0.003(3)
C6 0.133(9) 0.069(5) 0.077(6) 0.032(4) -0.061(6) -0.043(5)
C7 0.082(6) 0.066(5) 0.058(4) 0.011(3) -0.027(4) -0.032(4)
C8 0.113(8) 0.080(6) 0.082(6) 0.035(5) -0.055(6) -0.039(5)
C9 0.097(7) 0.060(5) 0.078(5) -0.006(4) 0.039(5) -0.011(4)
C10 0.073(6) 0.055(4) 0.082(6) 0.005(4) 0.019(5) -0.007(4)
C11 0.087(6) 0.049(4) 0.065(5) 0.003(4) -0.037(4) -0.012(4)
C12 0.178(12) 0.087(6) 0.050(5) 0.009(5) 0.032(6) -0.016(7)
C13 0.133(7) 0.070(5) 0.061(4) -0.002(4) 0.032(5) -0.008(5)
N1 0.060(4) 0.044(3) 0.049(3) -0.004(2) -0.012(3) 0.005(3)
N2 0.076(4) 0.049(3) 0.051(3) 0.008(3) 0.018(3) 0.005(3)
O1 0.069(11) 0.041(8) 0.053(9) -0.006(7) 0.010(8) 0.008(7)
O2 0.10(2) 0.040(11) 0.031(11) -0.011(9) -0.012(11) 0.021(12)

_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
Cu1 N1 1.976(5) . ?
Cu1 N2 1.990(5) 6_557 ?
Cu1 Cl1 2.184(2) . ?
C1 N1 1.327(9) . ?
C1 C2 1.372(11) . ?
C1 H1A 0.9300 . ?
C2 C3 1.347(12) . ?
C2 H2A 0.9300 . ?
C3 C4 1.392(11) . ?
C3 C6 1.527(10) . ?
C4 C5 1.384(10) . ?
C4 H4A 0.9300 . ?
C5 N1 1.332(9) . ?
C5 H5A 0.9300 . ?
C6 C8 1.432(14) . ?
C6 C7 1.519(10) . ?
C6 O1 1.696(18) . ?
C7 C8 1.546(10) 5_657 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C11 1.524(10) . ?
C8 C7 1.546(10) 5_657 ?
C8 O2 1.58(2) . ?
C9 N2 1.328(10) . ?
C9 C10 1.361(11) . ?
C9 H9A 0.9300 . ?
C10 C11 1.339(11) . ?
C10 H10A 0.9300 . ?
C11 C12 1.333(12) . ?
C12 C13 1.397(12) . ?
C12 H12A 0.9300 . ?
C13 N2 1.294(10) . ?
C13 H13A 0.9300 . ?
N2 Cu1 1.990(5) 6_667 ?
O1 H1B 0.8200 . ?
O2 H2B 0.8200 . ?

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
N1 Cu1 N2 113.4(2) . 6_557 ?
N1 Cu1 Cl1 125.07(17) . . ?
N2 Cu1 Cl1 121.31(18) 6_557 . ?
N1 C1 C2 124.5(8) . . ?
N1 C1 H1A 117.8 . . ?
C2 C1 H1A 117.8 . . ?
C3 C2 C1 120.0(8) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 117.1(7) . . ?
C2 C3 C6 121.9(8) . . ?
C4 C3 C6 121.1(8) . . ?
C5 C4 C3 119.4(7) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
N1 C5 C4 123.2(7) . . ?
N1 C5 H5A 118.4 . . ?
C4 C5 H5A 118.4 . . ?
C8 C6 C7 114.0(8) . . ?
C8 C6 C3 113.1(8) . . ?
C7 C6 C3 111.5(6) . . ?
C8 C6 O1 104.7(9) . . ?
C7 C6 O1 111.1(9) . . ?
C3 C6 O1 101.5(9) . . ?
C6 C7 C8 112.5(6) . 5_657 ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 5_657 . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 5_657 . ?
H7A C7 H7B 107.8 . . ?
C6 C8 C11 115.6(8) . . ?
C6 C8 C7 111.2(8) . 5_657 ?
C11 C8 C7 111.3(6) . 5_657 ?
C6 C8 O2 108.3(12) . . ?
C11 C8 O2 102.0(11) . . ?
C7 C8 O2 107.7(11) 5_657 . ?
N2 C9 C10 124.8(7) . . ?
N2 C9 H9A 117.6 . . ?
C10 C9 H9A 117.6 . . ?
C11 C10 C9 119.9(8) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C12 C11 C10 116.4(7) . . ?
C12 C11 C8 123.6(8) . . ?
C10 C11 C8 120.1(8) . . ?
C11 C12 C13 121.3(8) . . ?
C11 C12 H12A 119.4 . . ?
C13 C12 H12A 119.4 . . ?
N2 C13 C12 122.6(8) . . ?
N2 C13 H13A 118.7 . . ?
C12 C13 H13A 118.7 . . ?
C1 N1 C5 115.8(6) . . ?
C1 N1 Cu1 121.9(5) . . ?
C5 N1 Cu1 122.2(5) . . ?
C13 N2 C9 115.1(7) . . ?
C13 N2 Cu1 122.7(5) . 6_667 ?
C9 N2 Cu1 121.7(5) . 6_667 ?
C6 O1 H1B 109.5 . . ?
C8 O2 H2B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.086