# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CopyzW
_database_code_depnum_ccdc_archive 'CCDC 1045642'
_audit_update_record             
;
2015-01-26 deposited with the CCDC.
2015-05-11 downloaded from the CCDC.
;

_audit_creation_date             2014-03-05T18:21:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
catena-((μ2-pyrazine)-hexakis(μ2-cyano)-decakis(cyano)-decakis(dimethylformamide)-tri-cobalt(ii)-di-tungsten(v))
_chemical_formula_moiety         'C50 H74 Co3 N28 O10 W2'
_chemical_formula_sum            'C50 H74 Co3 N28 O10 W2'
_chemical_formula_weight         1771.84
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.264(1)
_cell_length_b                   10.674(1)
_cell_length_c                   17.308(1)
_cell_angle_alpha                92.084(1)
_cell_angle_beta                 103.251(1)
_cell_angle_gamma                103.060(1)
_cell_volume                     1790.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7789
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             879
_exptl_special_details           
;
A crystal was mounted with Paratone oil on a 200um Cryoloop, and cooled at 120K.
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.951
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4635
_exptl_absorpt_correction_T_max  0.5705
_exptl_absorpt_process_details   scalepack

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.896735E-1
_diffrn_orient_matrix_ub_12      0.237917E-1
_diffrn_orient_matrix_ub_13      -0.204827E-1
_diffrn_orient_matrix_ub_21      0.467011E-1
_diffrn_orient_matrix_ub_22      0.700675E-1
_diffrn_orient_matrix_ub_23      -0.282405E-1
_diffrn_orient_matrix_ub_31      -0.203036E-1
_diffrn_orient_matrix_ub_32      -0.620869E-1
_diffrn_orient_matrix_ub_33      -0.483433E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_number            14278
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_reflns_number_total             8137
_reflns_number_gt                7747
_reflns_threshold_expression     >2σ(I)
_diffrn_reflns_reduction_process 
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR97 (Altomare et al, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0269P)²+1.7801P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8137
_refine_ls_number_parameters     431
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.0581
_refine_ls_wR_factor_gt          0.0569
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.112

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
W1 W 0.195683(9) 0.146141(8) 0.236877(5) 0.01126(4) Uani 1 1 d . . .
Co2 Co 0.5 0 0.5 0.02008(11) Uani 1 2 d S . .
Co3 Co 0.21954(3) 0.22408(3) -0.064856(18) 0.01209(7) Uani 1 1 d . . .
C2 C 0.2224(2) 0.1654(2) 0.11689(14) 0.0141(4) Uani 1 1 d . . .
O4 O 0.18482(19) 0.29463(17) -0.17952(10) 0.0183(4) Uani 1 1 d . . .
C6 C 0.2156(3) 0.2933(2) 0.33208(14) 0.0173(5) Uani 1 1 d . . .
O5 O 0.06927(19) 0.31700(18) -0.04982(11) 0.0197(4) Uani 1 1 d . . .
N6 N 0.2268(3) 0.3693(2) 0.38314(14) 0.0266(5) Uani 1 1 d . . .
O3 O 0.35992(19) 0.13185(18) -0.09460(11) 0.0210(4) Uani 1 1 d . . .
C1 C 0.3228(3) 0.0994(2) 0.34471(14) 0.0167(5) Uani 1 1 d . . .
N41 N 0.0296(3) 0.3716(2) -0.26908(14) 0.0235(5) Uani 1 1 d . . .
N4 N -0.0111(3) 0.3343(3) 0.16731(15) 0.0324(6) Uani 1 1 d . . .
N9 N 0.3870(2) 0.3940(2) -0.02450(12) 0.0149(4) Uani 1 1 d . . .
N2 N 0.2364(2) 0.1760(2) 0.05310(12) 0.0162(4) Uani 1 1 d . . .
N31 N 0.3771(2) -0.0243(2) -0.18146(15) 0.0252(5) Uani 1 1 d . . .
O1 O 0.3233(2) -0.1273(2) 0.51820(13) 0.0333(5) Uani 1 1 d . . .
N51 N -0.1463(2) 0.3091(3) -0.03729(15) 0.0259(5) Uani 1 1 d . . .
C23 C 0.5871(3) -0.4597(3) 0.41445(18) 0.0305(6) Uani 1 1 d . . .
H23C H 0.6228 -0.4509 0.4725 0.046 Uiso 1 1 calc R . .
H23A H 0.6581 -0.4762 0.3887 0.046 Uiso 1 1 calc R . .
H23B H 0.5053 -0.532 0.3991 0.046 Uiso 1 1 calc R . .
C41 C 0.0634(3) 0.2913(2) -0.21615(15) 0.0192(5) Uani 1 1 d . . .
H41 H -0.0088 0.227 -0.2051 0.023 Uiso 1 1 calc R . .
N5 N -0.0301(3) 0.0044(3) 0.33485(15) 0.0308(6) Uani 1 1 d . . .
O2 O 0.5248(3) -0.1421(2) 0.42331(13) 0.0355(5) Uani 1 1 d . . .
N7 N 0.4957(2) 0.3477(2) 0.24245(14) 0.0246(5) Uani 1 1 d . . .
N3 N -0.0655(2) -0.0548(2) 0.11130(13) 0.0171(4) Uani 1 1 d . . .
N21 N 0.5500(3) -0.3405(3) 0.38909(15) 0.0288(5) Uani 1 1 d . . .
N1 N 0.3861(2) 0.0692(2) 0.40166(13) 0.0216(5) Uani 1 1 d . . .
C3 C 0.0223(2) 0.0187(2) 0.15371(14) 0.0134(4) Uani 1 1 d . . .
N8 N 0.2965(3) -0.1183(2) 0.19829(14) 0.0248(5) Uani 1 1 d . . .
N11 N 0.0957(3) -0.2039(3) 0.51118(15) 0.0309(6) Uani 1 1 d . . .
C32 C 0.4588(4) -0.0829(3) -0.1196(2) 0.0342(7) Uani 1 1 d . . .
H32C H 0.5567 -0.0523 -0.1186 0.051 Uiso 1 1 calc R . .
H32B H 0.431 -0.1771 -0.1307 0.051 Uiso 1 1 calc R . .
H32A H 0.4437 -0.0587 -0.0677 0.051 Uiso 1 1 calc R . .
C51 C -0.0341(3) 0.2669(3) -0.02505(16) 0.0217(5) Uani 1 1 d . . .
H51 H -0.0308 0.1938 0.0044 0.026 Uiso 1 1 calc R . .
C7 C 0.3928(3) 0.2774(2) 0.24199(14) 0.0176(5) Uani 1 1 d . . .
C33 C 0.3490(4) -0.0788(4) -0.2641(2) 0.0414(9) Uani 1 1 d . . .
H33C H 0.2854 -0.0364 -0.2986 0.062 Uiso 1 1 calc R . .
H33A H 0.3074 -0.1717 -0.2681 0.062 Uiso 1 1 calc R . .
H33B H 0.4355 -0.0648 -0.2812 0.062 Uiso 1 1 calc R . .
C21 C 0.5538(3) -0.2449(3) 0.44114(18) 0.0274(6) Uani 1 1 d . . .
H21 H 0.5808 -0.2564 0.4962 0.033 Uiso 1 1 calc R . .
C10 C 0.4462(3) 0.4313(3) 0.05234(16) 0.0236(6) Uani 1 1 d . . .
H10 H 0.4104 0.3846 0.0916 0.028 Uiso 1 1 calc R . .
C9 C 0.4413(3) 0.4636(3) -0.07664(16) 0.0245(6) Uani 1 1 d . . .
H9 H 0.4021 0.4407 -0.132 0.029 Uiso 1 1 calc R . .
C13 C -0.0469(4) -0.1960(4) 0.4807(2) 0.0370(7) Uani 1 1 d . . .
H13A H -0.0869 -0.1809 0.5254 0.055 Uiso 1 1 calc R . .
H13C H -0.1004 -0.2772 0.4494 0.055 Uiso 1 1 calc R . .
H13B H -0.0492 -0.1246 0.4468 0.055 Uiso 1 1 calc R . .
C43 C -0.1137(3) 0.3634(3) -0.3085(2) 0.0344(7) Uani 1 1 d . . .
H43C H -0.1734 0.2923 -0.2894 0.052 Uiso 1 1 calc R . .
H43A H -0.1272 0.3476 -0.3662 0.052 Uiso 1 1 calc R . .
H43B H -0.1372 0.4447 -0.2964 0.052 Uiso 1 1 calc R . .
C5 C 0.0487(3) 0.0540(3) 0.30118(15) 0.0196(5) Uani 1 1 d . . .
C52 C -0.1630(3) 0.4176(3) -0.0845(2) 0.0344(7) Uani 1 1 d . . .
H52A H -0.0815 0.4469 -0.1056 0.052 Uiso 1 1 calc R . .
H52C H -0.1736 0.4886 -0.0507 0.052 Uiso 1 1 calc R . .
H52B H -0.2451 0.3902 -0.1288 0.052 Uiso 1 1 calc R . .
C31 C 0.3333(3) 0.0766(3) -0.16356(16) 0.0232(5) Uani 1 1 d . . .
H31 H 0.2777 0.1101 -0.2055 0.028 Uiso 1 1 calc R . .
C8 C 0.2638(3) -0.0251(2) 0.21160(14) 0.0164(5) Uani 1 1 d . . .
C11 C 0.2008(3) -0.1221(3) 0.49419(17) 0.0272(6) Uani 1 1 d . . .
H11 H 0.1817 -0.0554 0.4617 0.033 Uiso 1 1 calc R . .
C4 C 0.0628(3) 0.2707(2) 0.19153(15) 0.0191(5) Uani 1 1 d . . .
C53 C -0.2616(3) 0.2487(4) -0.0046(2) 0.0432(9) Uani 1 1 d . . .
H53C H -0.2418 0.1729 0.0217 0.065 Uiso 1 1 calc R . .
H53A H -0.3455 0.2218 -0.0477 0.065 Uiso 1 1 calc R . .
H53B H -0.275 0.3107 0.0343 0.065 Uiso 1 1 calc R . .
C22 C 0.5053(5) -0.3316(4) 0.3041(2) 0.0538(11) Uani 1 1 d . . .
H22A H 0.4689 -0.2545 0.2952 0.081 Uiso 1 1 calc R . .
H22B H 0.4329 -0.4086 0.2799 0.081 Uiso 1 1 calc R . .
H22C H 0.5837 -0.3255 0.2799 0.081 Uiso 1 1 calc R . .
C42 C 0.1333(4) 0.4780(3) -0.2861(2) 0.0365(7) Uani 1 1 d . . .
H42A H 0.2254 0.4712 -0.2578 0.055 Uiso 1 1 calc R . .
H42C H 0.1175 0.5604 -0.2684 0.055 Uiso 1 1 calc R . .
H42B H 0.1265 0.474 -0.3436 0.055 Uiso 1 1 calc R . .
C12 C 0.1182(5) -0.3048(4) 0.5627(3) 0.0522(10) Uani 1 1 d . . .
H12A H 0.2175 -0.2967 0.5824 0.078 Uiso 1 1 calc R . .
H12B H 0.0753 -0.3894 0.5327 0.078 Uiso 1 1 calc R . .
H12C H 0.0772 -0.2967 0.608 0.078 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
W1 C4 2.156(3) . ?
W1 C5 2.159(3) . ?
W1 C1 2.163(3) . ?
W1 C3 2.163(2) . ?
W1 C8 2.164(3) . ?
W1 C7 2.166(3) . ?
W1 C2 2.167(2) . ?
W1 C6 2.177(3) . ?
Co2 O2 2.076(2) 2_656 ?
Co2 O2 2.076(2) . ?
Co2 N1 2.093(2) . ?
Co2 N1 2.093(2) 2_656 ?
Co2 O1 2.101(2) . ?
Co2 O1 2.101(2) 2_656 ?
Co3 O3 2.063(2) . ?
Co3 O5 2.070(2) . ?
Co3 N2 2.101(2) . ?
Co3 N3 2.105(2) 2 ?
Co3 O4 2.1304(18) . ?
Co3 N9 2.164(2) . ?
C2 N2 1.152(3) . ?
O4 C41 1.254(3) . ?
C6 N6 1.145(3) . ?
O5 C51 1.251(3) . ?
O3 C31 1.254(3) . ?
C1 N1 1.149(4) . ?
N41 C41 1.318(3) . ?
N41 C43 1.454(4) . ?
N41 C42 1.460(4) . ?
N4 C4 1.148(4) . ?
N9 C9 1.330(3) . ?
N9 C10 1.334(3) . ?
N31 C31 1.310(4) . ?
N31 C32 1.454(4) . ?
N31 C33 1.464(4) . ?
O1 C11 1.245(4) . ?
N51 C51 1.305(4) . ?
N51 C53 1.458(4) . ?
N51 C52 1.460(4) . ?
C23 N21 1.463(4) . ?
N5 C5 1.148(4) . ?
O2 C21 1.232(4) . ?
N7 C7 1.147(4) . ?
N3 C3 1.140(3) . ?
N3 Co3 2.105(2) 2 ?
N21 C21 1.325(4) . ?
N21 C22 1.450(4) . ?
N8 C8 1.150(4) . ?
N11 C11 1.324(4) . ?
N11 C12 1.449(4) . ?
N11 C13 1.460(4) . ?
C10 C9 1.387(4) 2_665 ?
C9 C10 1.387(4) 2_665 ?

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
C4 W1 C5 89.74(11) . . ?
C4 W1 C1 143.30(9) . . ?
C5 W1 C1 76.14(10) . . ?
C4 W1 C3 76.06(10) . . ?
C5 W1 C3 70.98(9) . . ?
C1 W1 C3 127.84(9) . . ?
C4 W1 C8 145.76(9) . . ?
C5 W1 C8 95.93(10) . . ?
C1 W1 C8 70.35(9) . . ?
C3 W1 C8 74.04(10) . . ?
C4 W1 C7 98.80(11) . . ?
C5 W1 C7 147.49(9) . . ?
C1 W1 C7 78.48(10) . . ?
C3 W1 C7 141.51(9) . . ?
C8 W1 C7 94.33(10) . . ?
C4 W1 C2 77.43(9) . . ?
C5 W1 C2 141.60(9) . . ?
C1 W1 C2 133.01(9) . . ?
C3 W1 C2 70.83(9) . . ?
C8 W1 C2 77.31(9) . . ?
C7 W1 C2 70.83(9) . . ?
C4 W1 C6 71.92(10) . . ?
C5 W1 C6 76.79(10) . . ?
C1 W1 C6 71.92(9) . . ?
C3 W1 C6 134.09(10) . . ?
C8 W1 C6 142.22(9) . . ?
C7 W1 C6 76.25(10) . . ?
C2 W1 C6 130.27(9) . . ?
O2 Co2 O2 180 2_656 . ?
O2 Co2 N1 91.10(9) 2_656 . ?
O2 Co2 N1 88.90(9) . . ?
O2 Co2 N1 88.90(9) 2_656 2_656 ?
O2 Co2 N1 91.10(9) . 2_656 ?
N1 Co2 N1 180.00(9) . 2_656 ?
O2 Co2 O1 90.26(10) 2_656 . ?
O2 Co2 O1 89.74(10) . . ?
N1 Co2 O1 92.48(9) . . ?
N1 Co2 O1 87.52(9) 2_656 . ?
O2 Co2 O1 89.74(10) 2_656 2_656 ?
O2 Co2 O1 90.26(10) . 2_656 ?
N1 Co2 O1 87.52(9) . 2_656 ?
N1 Co2 O1 92.48(9) 2_656 2_656 ?
O1 Co2 O1 180 . 2_656 ?
O3 Co3 O5 172.99(8) . . ?
O3 Co3 N2 99.03(8) . . ?
O5 Co3 N2 87.63(8) . . ?
O3 Co3 N3 87.80(9) . 2 ?
O5 Co3 N3 89.75(9) . 2 ?
N2 Co3 N3 92.70(8) . 2 ?
O3 Co3 O4 90.01(8) . . ?
O5 Co3 O4 83.41(7) . . ?
N2 Co3 O4 170.73(8) . . ?
N3 Co3 O4 89.64(8) 2 . ?
O3 Co3 N9 88.03(8) . . ?
O5 Co3 N9 94.10(8) . . ?
N2 Co3 N9 90.42(8) . . ?
N3 Co3 N9 175.13(8) 2 . ?
O4 Co3 N9 87.86(8) . . ?
N2 C2 W1 179.8(2) . . ?
C41 O4 Co3 118.65(16) . . ?
N6 C6 W1 178.8(2) . . ?
C51 O5 Co3 124.69(18) . . ?
C31 O3 Co3 118.64(17) . . ?
N1 C1 W1 176.9(2) . . ?
C41 N41 C43 121.2(3) . . ?
C41 N41 C42 121.4(3) . . ?
C43 N41 C42 117.2(3) . . ?
C9 N9 C10 116.3(2) . . ?
C9 N9 Co3 120.60(17) . . ?
C10 N9 Co3 123.05(17) . . ?
C2 N2 Co3 164.0(2) . . ?
C31 N31 C32 120.6(2) . . ?
C31 N31 C33 121.2(3) . . ?
C32 N31 C33 118.1(3) . . ?
C11 O1 Co2 127.9(2) . . ?
C51 N51 C53 121.1(3) . . ?
C51 N51 C52 122.0(3) . . ?
C53 N51 C52 116.9(3) . . ?
O4 C41 N41 124.1(2) . . ?
C21 O2 Co2 126.8(2) . . ?
C3 N3 Co3 161.7(2) . 2 ?
C21 N21 C22 120.7(3) . . ?
C21 N21 C23 121.9(3) . . ?
C22 N21 C23 117.4(2) . . ?
C1 N1 Co2 175.3(2) . . ?
N3 C3 W1 175.7(2) . . ?
C11 N11 C12 120.8(3) . . ?
C11 N11 C13 122.3(3) . . ?
C12 N11 C13 116.9(3) . . ?
O5 C51 N51 123.9(3) . . ?
N7 C7 W1 178.0(2) . . ?
O2 C21 N21 124.7(3) . . ?
N9 C10 C9 122.0(2) . 2_665 ?
N9 C9 C10 121.8(2) . 2_665 ?
N5 C5 W1 179.5(3) . . ?
O3 C31 N31 124.3(3) . . ?
N8 C8 W1 178.1(2) . . ?
O1 C11 N11 123.9(3) . . ?
N4 C4 W1 178.1(3) . . ?


# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_chemical_properties_physical    
'Moisture-sensitive, Heat-sensitive, Light-sensitive'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CupyzW
_database_code_depnum_ccdc_archive 'CCDC 1045643'
_audit_update_record             
;
2015-02-23 deposited with the CCDC.
2015-05-11 downloaded from the CCDC.
;

_audit_creation_date             2015-02-21T11:49:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
catena-((μ2-pyrazine)-hexakis(μ2-cyano)-decakis(cyano)-decakis(dimethylformamide)-tri-copper(ii)-di-tungsten(v))
_chemical_formula_moiety         'C50 H74 Cu3 N28 O10 W2'
_chemical_formula_sum            'C50 H74 Cu3 N28 O10 W2'
_chemical_formula_weight         1785.70
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0670(10)
_cell_length_b                   10.7140(10)
_cell_length_c                   17.4490(3)
_cell_angle_alpha                93.2860(10)
_cell_angle_beta                 104.1910(10)
_cell_angle_gamma                102.9860(10)
_cell_volume                     1765.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7409
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.68
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             885
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.205
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3463
_exptl_absorpt_correction_T_max  0.5711
_exptl_absorpt_process_details   scalepack

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.650387E-1
_diffrn_orient_matrix_ub_12      0.493866E-1
_diffrn_orient_matrix_ub_13      -0.298511E-1
_diffrn_orient_matrix_ub_21      0.579272E-1
_diffrn_orient_matrix_ub_22      0.810647E-1
_diffrn_orient_matrix_ub_23      0.347056E-1
_diffrn_orient_matrix_ub_31      0.599493E-1
_diffrn_orient_matrix_ub_32      0.172242E-1
_diffrn_orient_matrix_ub_33      -0.380673E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_number            14386
_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       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.16
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_reflns_number_total             7998
_reflns_number_gt                7227
_reflns_threshold_expression     >2σ(I)
_diffrn_reflns_reduction_process 
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR97 (Altomare et al, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0309P)²+3.1607P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7998
_refine_ls_number_parameters     431
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0656
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.584
_refine_diff_density_min         -2.448
_refine_diff_density_rms         0.13

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
W1 W 0.199208(13) 0.639025(12) 0.738532(8) 0.01164(5) Uani 1 1 d . . .
Cu2 Cu 0.5 0.5 1 0.01869(13) Uani 1 2 d S . .
Cu3 Cu 0.22411(4) 0.73069(4) 0.43182(2) 0.01327(9) Uani 1 1 d . . .
C4 C 0.0536(4) 0.7544(3) 0.6924(2) 0.0197(7) Uani 1 1 d . . .
C2 C 0.2197(3) 0.6606(3) 0.6188(2) 0.0156(7) Uani 1 1 d . . .
O4 O 0.1825(3) 0.8015(2) 0.29927(16) 0.0218(5) Uani 1 1 d . . .
C10 C 0.4581(4) 0.9211(3) 0.5503(2) 0.0195(7) Uani 1 1 d . . .
H10 H 0.4306 0.8666 0.5877 0.023 Uiso 1 1 calc R . .
O5 O 0.0848(3) 0.8315(2) 0.44325(15) 0.0207(5) Uani 1 1 d . . .
C13 C 1.0721(5) 0.6924(5) 1.0245(3) 0.0361(10) Uani 1 1 d . . .
H13A H 1.0703 0.6187 1.0553 0.054 Uiso 1 1 calc R . .
H13B H 1.1316 0.7709 1.0587 0.054 Uiso 1 1 calc R . .
H13C H 1.1109 0.6775 0.9795 0.054 Uiso 1 1 calc R . .
C52 C -0.1551(5) 0.9276(4) 0.4010(3) 0.0363(10) Uani 1 1 d . . .
H52A H -0.0672 0.9613 0.3862 0.054 Uiso 1 1 calc R . .
H52B H -0.1793 0.9978 0.4289 0.054 Uiso 1 1 calc R . .
H52C H -0.2315 0.8909 0.3529 0.054 Uiso 1 1 calc R . .
C33 C 0.3355(4) 0.4172(5) 0.2368(3) 0.0355(10) Uani 1 1 d . . .
H33A H 0.2823 0.4667 0.201 0.053 Uiso 1 1 calc R . .
H33B H 0.2796 0.3279 0.2308 0.053 Uiso 1 1 calc R . .
H33C H 0.4247 0.4183 0.2234 0.053 Uiso 1 1 calc R . .
C7 C 0.3990(4) 0.7723(3) 0.7440(2) 0.0173(7) Uani 1 1 d . . .
C22 C 0.4675(6) 0.8174(5) 1.1931(3) 0.0447(12) Uani 1 1 d . . .
H22A H 0.3789 0.8099 1.2084 0.067 Uiso 1 1 calc R . .
H22B H 0.5387 0.8926 1.2246 0.067 Uiso 1 1 calc R . .
H22C H 0.5012 0.7393 1.2032 0.067 Uiso 1 1 calc R . .
N6 N 0.2345(4) 0.8675(3) 0.8838(2) 0.0273(7) Uani 1 1 d . . .
C12 C 0.9115(6) 0.8088(5) 0.9447(3) 0.0478(13) Uani 1 1 d . . .
H12A H 0.8123 0.8128 0.9308 0.072 Uiso 1 1 calc R . .
H12B H 0.9392 0.7904 0.896 0.072 Uiso 1 1 calc R . .
H12C H 0.9711 0.8917 0.9732 0.072 Uiso 1 1 calc R . .
C23 C 0.4129(5) 0.9544(4) 1.0857(3) 0.0366(11) Uani 1 1 d . . .
H23A H 0.4985 1.0247 1.1052 0.055 Uiso 1 1 calc R . .
H23B H 0.3383 0.9721 1.1085 0.055 Uiso 1 1 calc R . .
H23C H 0.3813 0.9476 1.0275 0.055 Uiso 1 1 calc R . .
C5 C 0.0508(4) 0.5527(3) 0.8023(2) 0.0175(7) Uani 1 1 d . . .
N41 N 0.0081(4) 0.8732(3) 0.2176(2) 0.0252(7) Uani 1 1 d . . .
C1 C 0.3291(3) 0.5926(3) 0.8472(2) 0.0144(7) Uani 1 1 d . . .
C51 C -0.0209(4) 0.7855(4) 0.4680(2) 0.0238(8) Uani 1 1 d . . .
H51 H -0.017 0.716 0.4992 0.029 Uiso 1 1 calc R . .
N51 N -0.1362(3) 0.8272(3) 0.4535(2) 0.0270(7) Uani 1 1 d . . .
O1 O 0.6949(3) 0.6417(3) 0.98713(18) 0.0349(7) Uani 1 1 d . . .
O2 O 0.4690(3) 0.6353(3) 1.07395(17) 0.0336(7) Uani 1 1 d . . .
C21 C 0.4491(4) 0.7410(4) 1.0574(2) 0.0279(9) Uani 1 1 d . . .
H21 H 0.4369 0.7576 1.0035 0.034 Uiso 1 1 calc R . .
N8 N 0.3159(3) 0.3847(3) 0.6964(2) 0.0256(7) Uani 1 1 d . . .
C43 C -0.1430(5) 0.8580(5) 0.1838(3) 0.0385(11) Uani 1 1 d . . .
H43A H -0.1958 0.7803 0.2002 0.058 Uiso 1 1 calc R . .
H43B H -0.1641 0.8499 0.1256 0.058 Uiso 1 1 calc R . .
H43C H -0.1707 0.9336 0.2029 0.058 Uiso 1 1 calc R . .
C6 C 0.2219(4) 0.7900(3) 0.8326(2) 0.0175(7) Uani 1 1 d . . .
O3 O 0.3597(3) 0.6381(2) 0.40559(15) 0.0196(5) Uani 1 1 d . . .
N2 N 0.2338(3) 0.6730(3) 0.55640(18) 0.0192(6) Uani 1 1 d . . .
N9 N 0.3869(3) 0.8921(3) 0.47315(17) 0.0149(6) Uani 1 1 d . . .
C42 C 0.1032(5) 0.9819(4) 0.1974(3) 0.0374(11) Uani 1 1 d . . .
H42A H 0.201 0.9837 0.2251 0.056 Uiso 1 1 calc R . .
H42B H 0.0812 1.0622 0.2138 0.056 Uiso 1 1 calc R . .
H42C H 0.0916 0.9731 0.1398 0.056 Uiso 1 1 calc R . .
N1 N 0.3911(3) 0.5626(3) 0.90372(18) 0.0202(6) Uani 1 1 d . . .
N3 N -0.0678(3) 0.4244(3) 0.61592(17) 0.0164(6) Uani 1 1 d . . .
N11 N 0.9291(4) 0.7078(3) 0.9950(2) 0.0282(7) Uani 1 1 d . . .
N4 N -0.0266(4) 0.8122(3) 0.6669(2) 0.0338(8) Uani 1 1 d . . .
N7 N 0.5013(4) 0.8451(3) 0.7431(2) 0.0292(8) Uani 1 1 d . . .
N21 N 0.4438(4) 0.8327(3) 1.1095(2) 0.0286(7) Uani 1 1 d . . .
C41 C 0.0555(4) 0.7949(3) 0.2670(2) 0.0220(8) Uani 1 1 d . . .
H41 H -0.0128 0.7277 0.2791 0.026 Uiso 1 1 calc R . .
N5 N -0.0283(3) 0.5056(3) 0.8358(2) 0.0293(8) Uani 1 1 d . . .
N31 N 0.3652(3) 0.4749(3) 0.3192(2) 0.0237(7) Uani 1 1 d . . .
C9 C 0.4295(4) 0.9715(3) 0.4234(2) 0.0211(7) Uani 1 1 d . . .
H9 H 0.3816 0.9541 0.3683 0.025 Uiso 1 1 calc R . .
C3 C 0.0229(4) 0.5024(3) 0.6566(2) 0.0151(7) Uani 1 1 d . . .
C8 C 0.2782(4) 0.4742(3) 0.7113(2) 0.0160(7) Uani 1 1 d . . .
C32 C 0.4372(5) 0.4109(4) 0.3817(3) 0.0359(10) Uani 1 1 d . . .
H32A H 0.425 0.4417 0.4329 0.054 Uiso 1 1 calc R . .
H32B H 0.5382 0.4302 0.3842 0.054 Uiso 1 1 calc R . .
H32C H 0.3971 0.3175 0.3702 0.054 Uiso 1 1 calc R . .
C53 C -0.2539(5) 0.7713(6) 0.4851(3) 0.0451(13) Uani 1 1 d . . .
H53A H -0.232 0.7006 0.5152 0.068 Uiso 1 1 calc R . .
H53B H -0.3391 0.7379 0.4411 0.068 Uiso 1 1 calc R . .
H53C H -0.2701 0.8375 0.5204 0.068 Uiso 1 1 calc R . .
C31 C 0.3303(4) 0.5811(4) 0.3360(2) 0.0217(8) Uani 1 1 d . . .
H31 H 0.2799 0.6177 0.2934 0.026 Uiso 1 1 calc R . .
C11 C 0.8177(4) 0.6307(4) 1.0102(2) 0.0289(9) Uani 1 1 d . . .
H11 H 0.8334 0.5625 1.0409 0.035 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
W1 C5 2.154(3) . ?
W1 C4 2.162(4) . ?
W1 C3 2.165(3) . ?
W1 C7 2.166(3) . ?
W1 C8 2.167(3) . ?
W1 C2 2.169(3) . ?
W1 C6 2.169(4) . ?
W1 C1 2.176(3) . ?
Cu2 N1 2.008(3) 2_667 ?
Cu2 N1 2.008(3) . ?
Cu2 O2 2.012(3) . ?
Cu2 O2 2.012(3) 2_667 ?
Cu2 O1 2.263(3) 2_667 ?
Cu2 O1 2.263(3) . ?
Cu3 O3 1.980(2) . ?
Cu3 N3 1.989(3) 2_566 ?
Cu3 O5 1.991(2) . ?
Cu3 N9 2.050(3) . ?
Cu3 N2 2.279(3) . ?
C4 N4 1.146(5) . ?
C2 N2 1.144(5) . ?
O4 C41 1.248(4) . ?
C10 N9 1.342(4) . ?
C10 C9 1.384(5) 2_676 ?
O5 C51 1.256(4) . ?
C13 N11 1.455(5) . ?
C52 N51 1.467(6) . ?
C33 N31 1.465(5) . ?
C7 N7 1.148(5) . ?
C22 N21 1.444(5) . ?
N6 C6 1.148(5) . ?
C12 N11 1.447(5) . ?
C23 N21 1.467(6) . ?
C5 N5 1.146(5) . ?
N41 C41 1.317(5) . ?
N41 C42 1.451(5) . ?
N41 C43 1.458(5) . ?
C1 N1 1.136(5) . ?
C51 N51 1.308(5) . ?
N51 C53 1.452(5) . ?
O1 C11 1.237(5) . ?
O2 C21 1.232(5) . ?
C21 N21 1.320(5) . ?
N8 C8 1.146(5) . ?
O3 C31 1.262(4) . ?
N9 C9 1.328(4) . ?
N3 C3 1.143(4) . ?
N3 Cu3 1.989(3) 2_566 ?
N11 C11 1.328(5) . ?
N31 C31 1.302(5) . ?
N31 C32 1.452(5) . ?
C9 C10 1.384(5) 2_676 ?

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
C5 W1 C4 86.98(13) . . ?
C5 W1 C3 70.81(13) . . ?
C4 W1 C3 76.13(13) . . ?
C5 W1 C7 147.19(13) . . ?
C4 W1 C7 100.54(14) . . ?
C3 W1 C7 141.99(12) . . ?
C5 W1 C8 100.07(13) . . ?
C4 W1 C8 144.82(13) . . ?
C3 W1 C8 73.92(13) . . ?
C7 W1 C8 91.97(13) . . ?
C5 W1 C2 141.84(13) . . ?
C4 W1 C2 76.03(13) . . ?
C3 W1 C2 72.03(12) . . ?
C7 W1 C2 70.49(13) . . ?
C8 W1 C2 77.52(13) . . ?
C5 W1 C6 76.35(13) . . ?
C4 W1 C6 72.55(13) . . ?
C3 W1 C6 135.25(13) . . ?
C7 W1 C6 75.65(13) . . ?
C8 W1 C6 142.62(13) . . ?
C2 W1 C6 127.85(13) . . ?
C5 W1 C1 75.29(13) . . ?
C4 W1 C1 143.90(13) . . ?
C3 W1 C1 124.52(12) . . ?
C7 W1 C1 80.37(13) . . ?
C8 W1 C1 70.37(12) . . ?
C2 W1 C1 135.41(12) . . ?
C6 W1 C1 72.81(13) . . ?
N1 Cu2 N1 180.0000(10) 2_667 . ?
N1 Cu2 O2 87.99(12) 2_667 . ?
N1 Cu2 O2 92.01(12) . . ?
N1 Cu2 O2 92.01(12) 2_667 2_667 ?
N1 Cu2 O2 87.99(12) . 2_667 ?
O2 Cu2 O2 180.000(2) . 2_667 ?
N1 Cu2 O1 87.16(12) 2_667 2_667 ?
N1 Cu2 O1 92.84(12) . 2_667 ?
O2 Cu2 O1 90.43(12) . 2_667 ?
O2 Cu2 O1 89.57(12) 2_667 2_667 ?
N1 Cu2 O1 92.84(12) 2_667 . ?
N1 Cu2 O1 87.16(12) . . ?
O2 Cu2 O1 89.57(12) . . ?
O2 Cu2 O1 90.43(12) 2_667 . ?
O1 Cu2 O1 180.0000(10) 2_667 . ?
O3 Cu3 N3 89.23(11) . 2_566 ?
O3 Cu3 O5 172.09(11) . . ?
N3 Cu3 O5 90.50(11) 2_566 . ?
O3 Cu3 N9 89.23(11) . . ?
N3 Cu3 N9 175.97(12) 2_566 . ?
O5 Cu3 N9 90.52(11) . . ?
O3 Cu3 N2 98.23(11) . . ?
N3 Cu3 N2 91.05(11) 2_566 . ?
O5 Cu3 N2 89.68(11) . . ?
N9 Cu3 N2 92.85(11) . . ?
N4 C4 W1 177.9(4) . . ?
N2 C2 W1 178.4(3) . . ?
N9 C10 C9 121.5(3) . 2_676 ?
C51 O5 Cu3 122.1(2) . . ?
N7 C7 W1 176.2(3) . . ?
N5 C5 W1 179.3(3) . . ?
C41 N41 C42 121.6(4) . . ?
C41 N41 C43 121.2(3) . . ?
C42 N41 C43 117.1(3) . . ?
N1 C1 W1 176.3(3) . . ?
O5 C51 N51 124.1(4) . . ?
C51 N51 C53 121.4(4) . . ?
C51 N51 C52 121.4(3) . . ?
C53 N51 C52 117.0(4) . . ?
C11 O1 Cu2 125.5(3) . . ?
C21 O2 Cu2 126.0(3) . . ?
O2 C21 N21 124.3(4) . . ?
N6 C6 W1 178.2(3) . . ?
C31 O3 Cu3 117.9(2) . . ?
C2 N2 Cu3 165.5(3) . . ?
C9 N9 C10 116.8(3) . . ?
C9 N9 Cu3 120.7(2) . . ?
C10 N9 Cu3 122.4(2) . . ?
C1 N1 Cu2 176.7(3) . . ?
C3 N3 Cu3 166.7(3) . 2_566 ?
C11 N11 C12 120.5(4) . . ?
C11 N11 C13 122.7(3) . . ?
C12 N11 C13 116.8(4) . . ?
C21 N21 C22 121.4(4) . . ?
C21 N21 C23 121.9(4) . . ?
C22 N21 C23 116.7(3) . . ?
O4 C41 N41 125.6(3) . . ?
C31 N31 C32 121.0(3) . . ?
C31 N31 C33 121.3(4) . . ?
C32 N31 C33 117.7(3) . . ?
N9 C9 C10 121.7(3) . 2_676 ?
N3 C3 W1 175.8(3) . . ?
N8 C8 W1 177.9(3) . . ?
O3 C31 N31 123.8(4) . . ?
O1 C11 N11 124.6(4) . . ?


# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_chemical_properties_physical    'Moisture-sensitive, Photo-sensitive'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CupyzMo
_database_code_depnum_ccdc_archive 'CCDC 1045644'
_audit_update_record             
;
2015-01-26 deposited with the CCDC.
2015-05-11 downloaded from the CCDC.
;

_audit_creation_date             2014-03-05T19:03:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
catena-((μ2-pyrazine)-hexakis(μ2-cyano)-decakis(cyano)-decakis(dimethylformamide)-tri-copper(ii)-di-molybdenum(v))
_chemical_formula_sum            'C50 H74 Cu3 Mo2 N28 O10'
_chemical_formula_moiety         'C50 H74 Cu3 Mo2 N28 O10'
_chemical_formula_weight         1609.87
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0560(3)
_cell_length_b                   10.6970(3)
_cell_length_c                   17.4100(5)
_cell_angle_alpha                93.364(2)
_cell_angle_beta                 104.168(2)
_cell_angle_gamma                102.945(2)
_cell_volume                     1756.85(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7262
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             821
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.05
0 0 -1 0.03
-1 1 0 0.11
1 1 0 0.165
1 -1 0 0.09
-1 -1 0 0.15
1 0 0 0.12
-1 0 0 0.13
0 -1 0 0.13

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_process_details   scalepack

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      0.0841837
_diffrn_orient_matrix_ub_12      -0.0046723
_diffrn_orient_matrix_ub_13      0.0433853
_diffrn_orient_matrix_ub_21      0.0223653
_diffrn_orient_matrix_ub_22      -0.0639768
_diffrn_orient_matrix_ub_23      -0.0360271
_diffrn_orient_matrix_ub_31      0.0600994
_diffrn_orient_matrix_ub_32      0.0722518
_diffrn_orient_matrix_ub_33      -0.0195092
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_number            13838
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_reflns_number_total             7939
_reflns_number_gt                6646
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR97 (Altomare et al, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0383P)²+1.2405P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7939
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.032
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_gt    27.107
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.089

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.69930(2) 0.139394(17) 0.738481(11) 0.01267(6) Uani 1 1 d . . .
Cu2 Cu 1 0 1 0.01929(10) Uani 1 2 d S . .
Cu3 Cu 0.72409(3) 0.23042(2) 0.431452(16) 0.01417(7) Uani 1 1 d . . .
C1 C 0.8286(2) 0.0928(2) 0.84655(14) 0.0164(5) Uani 1 1 d . . .
N1 N 0.8909(2) 0.0628(2) 0.90392(12) 0.0202(4) Uani 1 1 d . . .
C8 C 0.7784(2) -0.0257(2) 0.71123(13) 0.0173(5) Uani 1 1 d . . .
N8 N 0.8160(2) -0.1156(2) 0.69675(13) 0.0235(5) Uani 1 1 d . . .
C3 C 0.5234(2) 0.0029(2) 0.65689(13) 0.0155(4) Uani 1 1 d . . .
N3 N 0.4328(2) -0.07453(19) 0.61608(11) 0.0174(4) Uani 1 1 d . . .
C5 C 0.5506(3) 0.0524(2) 0.80216(14) 0.0189(5) Uani 1 1 d . . .
N5 N 0.4710(2) 0.0058(2) 0.83573(13) 0.0276(5) Uani 1 1 d . . .
C7 C 0.8989(3) 0.2735(2) 0.74363(13) 0.0178(5) Uani 1 1 d . . .
N7 N 1.0012(2) 0.3462(2) 0.74259(13) 0.0264(5) Uani 1 1 d . . .
C2 C 0.7200(2) 0.1601(2) 0.61905(13) 0.0152(4) Uani 1 1 d . . .
N2 N 0.7335(2) 0.17246(19) 0.55600(12) 0.0199(4) Uani 1 1 d . . .
C4 C 0.5548(3) 0.2559(2) 0.69309(14) 0.0210(5) Uani 1 1 d . . .
N4 N 0.4743(3) 0.3145(2) 0.66740(14) 0.0333(6) Uani 1 1 d . . .
C6 C 0.7217(3) 0.2898(2) 0.83311(14) 0.0187(5) Uani 1 1 d . . .
N6 N 0.7346(3) 0.3675(2) 0.88411(13) 0.0272(5) Uani 1 1 d . . .
O1 O 1.1963(2) 0.14241(19) 0.98723(12) 0.0329(4) Uani 1 1 d . . .
C11 C 1.3183(3) 0.1309(3) 1.01056(16) 0.0258(5) Uani 1 1 d . . .
N11 N 1.4305(2) 0.2080(2) 0.99501(13) 0.0272(5) Uani 1 1 d . . .
C13 C 1.5733(3) 0.1918(3) 1.02495(18) 0.0329(6) Uani 1 1 d . . .
H13C H 1.5706 0.1176 1.0555 0.049 Uiso 1 1 calc R . .
H13B H 1.6328 0.27 1.0595 0.049 Uiso 1 1 calc R . .
H13A H 1.6127 0.177 0.98 0.049 Uiso 1 1 calc R . .
C12 C 1.4134(4) 0.3079(3) 0.9436(2) 0.0439(8) Uani 1 1 d . . .
H12B H 1.4459 0.2903 0.8963 0.066 Uiso 1 1 calc R . .
H12C H 1.4695 0.3919 0.9725 0.066 Uiso 1 1 calc R . .
H12A H 1.3134 0.3092 0.9271 0.066 Uiso 1 1 calc R . .
O2 O 1.0302(2) -0.13499(19) 0.92576(11) 0.0318(4) Uani 1 1 d . . .
C21 C 1.0504(3) -0.2408(3) 0.94278(16) 0.0276(6) Uani 1 1 d . . .
N21 N 1.0555(2) -0.3328(2) 0.89033(13) 0.0272(5) Uani 1 1 d . . .
C23 C 1.0860(3) -0.4542(3) 0.91432(17) 0.0343(7) Uani 1 1 d . . .
H23C H 1.1118 -0.449 0.9727 0.051 Uiso 1 1 calc R . .
H23B H 1.1646 -0.4697 0.8944 0.051 Uiso 1 1 calc R . .
H23A H 1.0019 -0.5253 0.892 0.051 Uiso 1 1 calc R . .
C22 C 1.0324(4) -0.3174(3) 0.80626(18) 0.0413(8) Uani 1 1 d . . .
H22A H 0.9966 -0.2403 0.7959 0.062 Uiso 1 1 calc R . .
H22B H 0.963 -0.3936 0.7745 0.062 Uiso 1 1 calc R . .
H22C H 1.1218 -0.3078 0.7915 0.062 Uiso 1 1 calc R . .
O3 O 0.85958(17) 0.13807(16) 0.40541(10) 0.0202(4) Uani 1 1 d . . .
C31 C 0.8300(3) 0.0809(2) 0.33522(15) 0.0202(5) Uani 1 1 d . . .
N31 N 0.8654(2) -0.0259(2) 0.31883(13) 0.0225(4) Uani 1 1 d . . .
C32 C 0.9381(3) -0.0900(3) 0.38174(18) 0.0332(6) Uani 1 1 d . . .
H32A H 1.039 -0.0708 0.384 0.05 Uiso 1 1 calc R . .
H32B H 0.8978 -0.1835 0.3704 0.05 Uiso 1 1 calc R . .
H32C H 0.9263 -0.0587 0.4331 0.05 Uiso 1 1 calc R . .
C33 C 0.8361(3) -0.0841(3) 0.23616(17) 0.0338(7) Uani 1 1 d . . .
H33A H 0.7802 -0.0365 0.2003 0.051 Uiso 1 1 calc R . .
H33C H 0.783 -0.1744 0.2306 0.051 Uiso 1 1 calc R . .
H33B H 0.9256 -0.0804 0.2223 0.051 Uiso 1 1 calc R . .
O4 O 0.68226(18) 0.30101(16) 0.29878(10) 0.0222(4) Uani 1 1 d . . .
C41 C 0.5553(3) 0.2943(2) 0.26691(15) 0.0218(5) Uani 1 1 d . . .
N41 N 0.5073(2) 0.3729(2) 0.21719(13) 0.0240(5) Uani 1 1 d . . .
C42 C 0.6025(3) 0.4817(3) 0.19653(18) 0.0337(6) Uani 1 1 d . . .
H42A H 0.7006 0.4828 0.2235 0.051 Uiso 1 1 calc R . .
H42C H 0.5815 0.5624 0.2135 0.051 Uiso 1 1 calc R . .
H42B H 0.5897 0.4729 0.1387 0.051 Uiso 1 1 calc R . .
C43 C 0.3561(3) 0.3582(3) 0.18365(19) 0.0360(7) Uani 1 1 d . . .
H43C H 0.3031 0.2819 0.2014 0.054 Uiso 1 1 calc R . .
H43A H 0.3342 0.3475 0.1253 0.054 Uiso 1 1 calc R . .
H43B H 0.3293 0.4352 0.2017 0.054 Uiso 1 1 calc R . .
O5 O 0.58467(18) 0.33097(16) 0.44316(10) 0.0205(4) Uani 1 1 d . . .
C51 C 0.4790(3) 0.2847(3) 0.46806(15) 0.0232(5) Uani 1 1 d . . .
C52 C 0.3442(3) 0.4272(3) 0.40153(19) 0.0339(7) Uani 1 1 d . . .
H52A H 0.4312 0.4597 0.3854 0.051 Uiso 1 1 calc R . .
H52C H 0.3221 0.4983 0.4301 0.051 Uiso 1 1 calc R . .
H52B H 0.266 0.3908 0.354 0.051 Uiso 1 1 calc R . .
C53 C 0.2455(3) 0.2701(4) 0.48574(19) 0.0417(8) Uani 1 1 d . . .
H53C H 0.2654 0.196 0.5129 0.063 Uiso 1 1 calc R . .
H53A H 0.1589 0.2414 0.442 0.063 Uiso 1 1 calc R . .
H53B H 0.2329 0.3348 0.5238 0.063 Uiso 1 1 calc R . .
N51 N 0.3638(2) 0.3271(2) 0.45366(13) 0.0277(5) Uani 1 1 d . . .
C9 C 0.9307(3) 0.4712(2) 0.42276(14) 0.0208(5) Uani 1 1 d . . .
H9 H 0.8838 0.4532 0.3674 0.025 Uiso 1 1 calc R . .
C10 C 0.9569(3) 0.4211(2) 0.55020(14) 0.0199(5) Uani 1 1 d . . .
H10 H 0.9288 0.3666 0.5875 0.024 Uiso 1 1 calc R . .
N9 N 0.8868(2) 0.39200(18) 0.47315(11) 0.0151(4) Uani 1 1 d . . .
H31 H 0.773(3) 0.111(3) 0.2898(18) 0.026(8) Uiso 1 1 d . . .
H11 H 1.345(3) 0.062(3) 1.0448(18) 0.025(7) Uiso 1 1 d . . .
H41 H 0.477(3) 0.232(3) 0.2775(18) 0.027(8) Uiso 1 1 d . . .
H51 H 0.472(3) 0.215(3) 0.4987(19) 0.032(8) Uiso 1 1 d . . .
H21 H 1.071(4) -0.264(3) 1.002(2) 0.040(9) Uiso 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C5 2.155(2) . ?
Mo1 C3 2.156(2) . ?
Mo1 C4 2.157(3) . ?
Mo1 C2 2.159(2) . ?
Mo1 C1 2.164(2) . ?
Mo1 C8 2.165(2) . ?
Mo1 C6 2.167(2) . ?
Mo1 C7 2.168(2) . ?
Cu2 N1 2.004(2) . ?
Cu2 N1 2.004(2) 2_757 ?
Cu2 O2 2.0045(19) . ?
Cu2 O2 2.0045(19) 2_757 ?
Cu2 O1 2.274(2) . ?
Cu2 O1 2.274(2) 2_757 ?
Cu3 O3 1.9725(17) . ?
Cu3 O5 1.9884(17) . ?
Cu3 N3 1.9936(19) 2_656 ?
Cu3 N9 2.0482(19) . ?
Cu3 N2 2.276(2) . ?
Cu3 O4 2.4401(17) . ?
C1 N1 1.146(3) . ?
C8 N8 1.147(3) . ?
C3 N3 1.139(3) . ?
N3 Cu3 1.9936(19) 2_656 ?
C5 N5 1.147(3) . ?
C7 N7 1.147(3) . ?
C2 N2 1.150(3) . ?
C4 N4 1.154(3) . ?
C6 N6 1.143(3) . ?
O1 C11 1.231(3) . ?
C11 N11 1.336(4) . ?
C11 H11 1.02(3) . ?
N11 C12 1.447(4) . ?
N11 C13 1.455(4) . ?
C13 H13C 0.98 . ?
C13 H13B 0.98 . ?
C13 H13A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C12 H12A 0.98 . ?
O2 C21 1.234(3) . ?
C21 N21 1.322(4) . ?
C21 H21 1.06(3) . ?
N21 C22 1.450(4) . ?
N21 C23 1.460(4) . ?
C23 H23C 0.98 . ?
C23 H23B 0.98 . ?
C23 H23A 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
O3 C31 1.268(3) . ?
C31 N31 1.306(3) . ?
C31 H31 0.97(3) . ?
N31 C32 1.458(4) . ?
N31 C33 1.467(3) . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
C33 H33A 0.98 . ?
C33 H33C 0.98 . ?
C33 H33B 0.98 . ?
O4 C41 1.245(3) . ?
C41 N41 1.325(3) . ?
C41 H41 0.97(3) . ?
N41 C42 1.456(3) . ?
N41 C43 1.457(4) . ?
C42 H42A 0.98 . ?
C42 H42C 0.98 . ?
C42 H42B 0.98 . ?
C43 H43C 0.98 . ?
C43 H43A 0.98 . ?
C43 H43B 0.98 . ?
O5 C51 1.256(3) . ?
C51 N51 1.311(4) . ?
C51 H51 0.94(3) . ?
C52 N51 1.460(4) . ?
C52 H52A 0.98 . ?
C52 H52C 0.98 . ?
C52 H52B 0.98 . ?
C53 N51 1.462(4) . ?
C53 H53C 0.98 . ?
C53 H53A 0.98 . ?
C53 H53B 0.98 . ?
C9 N9 1.338(3) . ?
C9 C10 1.385(3) 2_766 ?
C9 H9 0.95 . ?
C10 N9 1.335(3) . ?
C10 C9 1.385(3) 2_766 ?
C10 H10 0.95 . ?

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
C5 Mo1 C3 70.51(9) . . ?
C5 Mo1 C4 87.14(9) . . ?
C3 Mo1 C4 76.56(9) . . ?
C5 Mo1 C2 141.72(8) . . ?
C3 Mo1 C2 72.11(8) . . ?
C4 Mo1 C2 76.42(9) . . ?
C5 Mo1 C1 75.33(9) . . ?
C3 Mo1 C1 124.34(8) . . ?
C4 Mo1 C1 143.71(9) . . ?
C2 Mo1 C1 135.15(9) . . ?
C5 Mo1 C8 99.85(9) . . ?
C3 Mo1 C8 73.98(9) . . ?
C4 Mo1 C8 145.27(9) . . ?
C2 Mo1 C8 77.35(9) . . ?
C1 Mo1 C8 70.17(8) . . ?
C5 Mo1 C6 76.30(9) . . ?
C3 Mo1 C6 135.08(9) . . ?
C4 Mo1 C6 72.32(9) . . ?
C2 Mo1 C6 128.35(8) . . ?
C1 Mo1 C6 72.75(9) . . ?
C8 Mo1 C6 142.40(9) . . ?
C5 Mo1 C7 147.48(9) . . ?
C3 Mo1 C7 142.00(8) . . ?
C4 Mo1 C7 100.00(9) . . ?
C2 Mo1 C7 70.35(8) . . ?
C1 Mo1 C7 80.67(9) . . ?
C8 Mo1 C7 92.15(9) . . ?
C6 Mo1 C7 75.84(9) . . ?
N1 Cu2 N1 180.00(8) . 2_757 ?
N1 Cu2 O2 87.94(8) . . ?
N1 Cu2 O2 92.06(8) 2_757 . ?
N1 Cu2 O2 92.06(8) . 2_757 ?
N1 Cu2 O2 87.94(8) 2_757 2_757 ?
O2 Cu2 O2 180.0000(10) . 2_757 ?
N1 Cu2 O1 87.31(8) . . ?
N1 Cu2 O1 92.69(8) 2_757 . ?
O2 Cu2 O1 90.50(8) . . ?
O2 Cu2 O1 89.50(8) 2_757 . ?
N1 Cu2 O1 92.69(8) . 2_757 ?
N1 Cu2 O1 87.31(8) 2_757 2_757 ?
O2 Cu2 O1 89.50(8) . 2_757 ?
O2 Cu2 O1 90.50(8) 2_757 2_757 ?
O1 Cu2 O1 180 . 2_757 ?
O3 Cu3 O5 172.31(7) . . ?
O3 Cu3 N3 89.39(8) . 2_656 ?
O5 Cu3 N3 90.40(8) . 2_656 ?
O3 Cu3 N9 89.23(7) . . ?
O5 Cu3 N9 90.52(7) . . ?
N3 Cu3 N9 176.35(8) 2_656 . ?
O3 Cu3 N2 98.13(7) . . ?
O5 Cu3 N2 89.56(7) . . ?
N3 Cu3 N2 90.70(7) 2_656 . ?
N9 Cu3 N2 92.83(7) . . ?
O3 Cu3 O4 89.83(7) . . ?
O5 Cu3 O4 82.49(7) . . ?
N3 Cu3 O4 86.94(7) 2_656 . ?
N9 Cu3 O4 89.68(7) . . ?
N2 Cu3 O4 171.69(7) . . ?
N1 C1 Mo1 176.3(2) . . ?
C1 N1 Cu2 176.3(2) . . ?
N8 C8 Mo1 177.8(2) . . ?
N3 C3 Mo1 176.2(2) . . ?
C3 N3 Cu3 166.20(19) . 2_656 ?
N5 C5 Mo1 179.7(2) . . ?
N7 C7 Mo1 176.4(2) . . ?
N2 C2 Mo1 178.8(2) . . ?
C2 N2 Cu3 165.7(2) . . ?
N4 C4 Mo1 177.7(2) . . ?
N6 C6 Mo1 178.6(2) . . ?
C11 O1 Cu2 125.17(18) . . ?
O1 C11 N11 124.3(2) . . ?
O1 C11 H11 123.2(17) . . ?
N11 C11 H11 112.5(17) . . ?
C11 N11 C12 120.7(3) . . ?
C11 N11 C13 122.3(2) . . ?
C12 N11 C13 116.9(2) . . ?
N11 C13 H13C 109.5 . . ?
N11 C13 H13B 109.5 . . ?
H13C C13 H13B 109.5 . . ?
N11 C13 H13A 109.5 . . ?
H13C C13 H13A 109.5 . . ?
H13B C13 H13A 109.5 . . ?
N11 C12 H12B 109.5 . . ?
N11 C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C12 H12A 109.5 . . ?
H12B C12 H12A 109.5 . . ?
H12C C12 H12A 109.5 . . ?
C21 O2 Cu2 125.51(18) . . ?
O2 C21 N21 123.9(3) . . ?
O2 C21 H21 122.2(18) . . ?
N21 C21 H21 113.7(18) . . ?
C21 N21 C22 121.4(2) . . ?
C21 N21 C23 121.7(2) . . ?
C22 N21 C23 116.9(2) . . ?
N21 C23 H23C 109.5 . . ?
N21 C23 H23B 109.5 . . ?
H23C C23 H23B 109.5 . . ?
N21 C23 H23A 109.5 . . ?
H23C C23 H23A 109.5 . . ?
H23B C23 H23A 109.5 . . ?
N21 C22 H22A 109.5 . . ?
N21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C31 O3 Cu3 117.66(16) . . ?
O3 C31 N31 123.2(2) . . ?
O3 C31 H31 121.6(18) . . ?
N31 C31 H31 115.0(17) . . ?
C31 N31 C32 121.3(2) . . ?
C31 N31 C33 121.1(2) . . ?
C32 N31 C33 117.5(2) . . ?
N31 C32 H32A 109.5 . . ?
N31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N31 C33 H33A 109.5 . . ?
N31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
N31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33C C33 H33B 109.5 . . ?
C41 O4 Cu3 113.46(15) . . ?
O4 C41 N41 125.5(2) . . ?
O4 C41 H41 123.9(18) . . ?
N41 C41 H41 110.5(18) . . ?
C41 N41 C42 121.6(2) . . ?
C41 N41 C43 121.4(2) . . ?
C42 N41 C43 116.9(2) . . ?
N41 C42 H42A 109.5 . . ?
N41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
N41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42C C42 H42B 109.5 . . ?
N41 C43 H43C 109.5 . . ?
N41 C43 H43A 109.5 . . ?
H43C C43 H43A 109.5 . . ?
N41 C43 H43B 109.5 . . ?
H43C C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C51 O5 Cu3 122.10(17) . . ?
O5 C51 N51 123.9(3) . . ?
O5 C51 H51 124(2) . . ?
N51 C51 H51 112(2) . . ?
N51 C52 H52A 109.5 . . ?
N51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
N51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52C C52 H52B 109.5 . . ?
N51 C53 H53C 109.5 . . ?
N51 C53 H53A 109.5 . . ?
H53C C53 H53A 109.5 . . ?
N51 C53 H53B 109.5 . . ?
H53C C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 N51 C52 121.8(2) . . ?
C51 N51 C53 121.0(3) . . ?
C52 N51 C53 117.1(2) . . ?
N9 C9 C10 121.2(2) . 2_766 ?
N9 C9 H9 119.4 . . ?
C10 C9 H9 119.4 2_766 . ?
N9 C10 C9 121.8(2) . 2_766 ?
N9 C10 H10 119.1 . . ?
C9 C10 H10 119.1 2_766 . ?
C10 N9 C9 117.0(2) . . ?
C10 N9 Cu3 122.43(16) . . ?
C9 N9 Cu3 120.56(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Cu3 N2 C2 175.8(7) . . . . ?
O5 Cu3 N2 C2 -4.4(7) . . . . ?
N3 Cu3 N2 C2 -94.8(7) 2_656 . . . ?
N9 Cu3 N2 C2 86.1(7) . . . . ?
N1 Cu2 O1 C11 -153.7(2) . . . . ?
N1 Cu2 O1 C11 26.3(2) 2_757 . . . ?
O2 Cu2 O1 C11 -65.8(2) . . . . ?
O2 Cu2 O1 C11 114.2(2) 2_757 . . . ?
Cu2 O1 C11 N11 172.46(19) . . . . ?
O1 C11 N11 C12 -4.2(4) . . . . ?
O1 C11 N11 C13 179.0(3) . . . . ?
N1 Cu2 O2 C21 -153.4(2) . . . . ?
N1 Cu2 O2 C21 26.6(2) 2_757 . . . ?
O1 Cu2 O2 C21 119.3(2) . . . . ?
O1 Cu2 O2 C21 -60.7(2) 2_757 . . . ?
Cu2 O2 C21 N21 172.8(2) . . . . ?
O2 C21 N21 C22 -2.2(4) . . . . ?
O2 C21 N21 C23 177.2(3) . . . . ?
N3 Cu3 O3 C31 48.64(18) 2_656 . . . ?
N9 Cu3 O3 C31 -127.98(18) . . . . ?
N2 Cu3 O3 C31 139.26(17) . . . . ?
O4 Cu3 O3 C31 -38.30(17) . . . . ?
Cu3 O3 C31 N31 -147.1(2) . . . . ?
O3 C31 N31 C32 2.3(4) . . . . ?
O3 C31 N31 C33 -176.3(2) . . . . ?
O3 Cu3 O4 C41 137.87(16) . . . . ?
O5 Cu3 O4 C41 -42.33(16) . . . . ?
N3 Cu3 O4 C41 48.47(17) 2_656 . . . ?
N9 Cu3 O4 C41 -132.90(17) . . . . ?
Cu3 O4 C41 N41 147.8(2) . . . . ?
O4 C41 N41 C42 -2.2(4) . . . . ?
O4 C41 N41 C43 -179.2(3) . . . . ?
N3 Cu3 O5 C51 43.02(19) 2_656 . . . ?
N9 Cu3 O5 C51 -140.50(19) . . . . ?
N2 Cu3 O5 C51 -47.67(19) . . . . ?
O4 Cu3 O5 C51 129.89(19) . . . . ?
Cu3 O5 C51 N51 -157.48(19) . . . . ?
O5 C51 N51 C52 4.7(4) . . . . ?
O5 C51 N51 C53 -178.9(2) . . . . ?
C9 C10 N9 C9 0.4(4) 2_766 . . . ?
C9 C10 N9 Cu3 178.13(19) 2_766 . . . ?
C10 C9 N9 C10 -0.4(4) 2_766 . . . ?
C10 C9 N9 Cu3 -178.17(19) 2_766 . . . ?
O3 Cu3 N9 C10 -95.09(19) . . . . ?
O5 Cu3 N9 C10 92.59(19) . . . . ?
N2 Cu3 N9 C10 3.0(2) . . . . ?
O4 Cu3 N9 C10 175.07(19) . . . . ?
O3 Cu3 N9 C9 82.51(19) . . . . ?
O5 Cu3 N9 C9 -89.81(19) . . . . ?
N2 Cu3 N9 C9 -179.40(19) . . . . ?
O4 Cu3 N9 C9 -7.32(19) . . . . ?


# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_chemical_properties_physical    
'Moisture-sensitive, Heat-sensitive, Light-sensitive'
_exptl_crystal_preparation       'Magnetic properties'
