# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2010


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Yoshikawa, Hirofumi'
_publ_contact_author_email       yoshikawah@mbox.chem.nagoya-u.ac.jp

_publ_section_title              
;
Two 3D Coordination Assemblies
with Same Cluster Configuration
Showing Different Magnetic Behaviors: A Ferromagnetic
{[CN)8Co2(DMF)8][NO3]}n and A Paramagnetic
{(CN)8Cu2(py)8}n
;
loop_
_publ_author_name
H.Yoshikawa
C.Zhang

data_2
#TrackingRef '- CIF.cif'

_database_code_depnum_ccdc_archive 'CCDC 752235'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H40 Cu2 N16 W'
_chemical_formula_sum            'C48 H40 Cu2 N16 W'
_chemical_formula_weight         1151.9

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   19.873(3)
_cell_length_b                   19.873(3)
_cell_length_c                   12.5477(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4955.6(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8042
_cell_measurement_theta_min      3.2438
_cell_measurement_theta_max      25.3491

_exptl_crystal_description       block
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2144
_exptl_absorpt_coefficient_mu    3.215
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4455
_exptl_absorpt_correction_T_max  0.6800
_exptl_absorpt_process_details   'SADABS(Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23821
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         25.35
_reflns_number_total             2277
_reflns_number_gt                2170
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_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^)+(0.0022P)^2^+53.5706P] 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         2277
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0951
_refine_ls_goodness_of_fit_ref   1.292
_refine_ls_restrained_S_all      1.292
_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
W1 W 0.5000 0.7500 1.1250 0.01945(16) Uani 1 4 d S . .
Cu2 Cu 0.5000 0.5000 1.0000 0.0325(3) Uani 1 2 d S . .
N1 N 0.4708(3) 0.5438(3) 0.8216(5) 0.0405(16) Uani 1 1 d . . .
N2 N 0.3981(3) 0.4884(3) 1.0385(5) 0.0381(15) Uani 1 1 d . . .
N3 N 0.4972(3) 0.5917(3) 1.0538(5) 0.0337(14) Uani 1 1 d . . .
N4 N 0.5974(3) 0.7421(3) 0.9080(5) 0.0316(14) Uani 1 1 d . . .
C1 C 0.4973(3) 0.6472(3) 1.0796(5) 0.0218(14) Uani 1 1 d . . .
C4 C 0.3538(4) 0.5398(4) 1.0341(6) 0.045(2) Uani 1 1 d . . .
H4 H 0.3702 0.5834 1.0169 0.054 Uiso 1 1 calc R . .
C5 C 0.4582(4) 0.5209(4) 0.6355(7) 0.051(2) Uani 1 1 d . . .
H5 H 0.4584 0.4886 0.5797 0.061 Uiso 1 1 calc R . .
C6 C 0.4447(5) 0.5876(5) 0.6133(7) 0.058(2) Uani 1 1 d . . .
H6 H 0.4363 0.6024 0.5425 0.070 Uiso 1 1 calc R . .
C7 C 0.4439(5) 0.6320(5) 0.6979(8) 0.066(3) Uani 1 1 d . . .
H7 H 0.4344 0.6783 0.6867 0.079 Uiso 1 1 calc R . .
C8 C 0.4571(5) 0.6082(4) 0.7988(7) 0.056(2) Uani 1 1 d . . .
H8 H 0.4564 0.6395 0.8560 0.067 Uiso 1 1 calc R . .
C9 C 0.4712(4) 0.5016(4) 0.7384(6) 0.045(2) Uani 1 1 d . . .
H9 H 0.4811 0.4555 0.7513 0.054 Uiso 1 1 calc R . .
C12 C 0.5640(3) 0.7460(3) 0.9840(5) 0.0229(14) Uani 1 1 d . . .
C13 C 0.3725(4) 0.4272(4) 1.0637(6) 0.045(2) Uani 1 1 d . . .
H13 H 0.4024 0.3900 1.0686 0.054 Uiso 1 1 calc R . .
C14 C 0.3048(5) 0.4166(4) 1.0827(7) 0.054(2) Uani 1 1 d . . .
H14 H 0.2888 0.3727 1.0989 0.064 Uiso 1 1 calc R . .
C15 C 0.2616(5) 0.4691(5) 1.0781(8) 0.058(2) Uani 1 1 d . . .
H15 H 0.2150 0.4627 1.0915 0.070 Uiso 1 1 calc R . .
C16 C 0.2867(4) 0.5326(5) 1.0533(7) 0.055(2) Uani 1 1 d . . .
H16 H 0.2574 0.5704 1.0497 0.066 Uiso 1 1 calc R . .

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
W1 0.01534(18) 0.01534(18) 0.0277(3) 0.000 0.000 0.000
Cu2 0.0454(8) 0.0144(6) 0.0378(7) -0.0042(5) 0.0000(6) -0.0004(5)
N1 0.055(4) 0.023(3) 0.044(4) -0.002(3) -0.001(3) 0.001(3)
N2 0.050(4) 0.026(3) 0.038(4) -0.005(3) -0.004(3) 0.001(3)
N3 0.050(4) 0.015(3) 0.036(4) -0.001(3) -0.002(3) 0.000(3)
N4 0.027(3) 0.038(3) 0.030(3) 0.001(3) 0.005(3) 0.003(3)
C1 0.017(3) 0.028(4) 0.021(3) 0.005(3) 0.000(3) -0.001(3)
C4 0.050(5) 0.037(4) 0.047(5) -0.003(4) -0.008(4) 0.005(4)
C5 0.070(6) 0.045(5) 0.036(5) -0.007(4) 0.004(4) -0.001(4)
C6 0.075(6) 0.064(6) 0.035(5) 0.013(5) -0.003(5) -0.002(5)
C7 0.106(8) 0.038(5) 0.054(6) 0.007(5) -0.011(6) 0.012(5)
C8 0.096(7) 0.028(4) 0.045(5) -0.001(4) -0.005(5) 0.009(5)
C9 0.082(6) 0.021(4) 0.033(4) -0.002(3) 0.016(4) 0.003(4)
C12 0.020(3) 0.019(3) 0.030(4) 0.001(3) -0.002(3) 0.000(3)
C13 0.052(5) 0.036(4) 0.047(5) -0.001(4) 0.002(4) -0.003(4)
C14 0.062(6) 0.048(5) 0.051(5) -0.006(4) 0.008(5) -0.009(4)
C15 0.046(5) 0.056(6) 0.073(7) -0.006(5) 0.006(5) -0.006(5)
C16 0.050(5) 0.054(6) 0.060(6) -0.010(5) -0.007(5) 0.018(4)

_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
W1 C1 2.121(7) 14_567 ?
W1 C1 2.121(7) . ?
W1 C1 2.121(7) 12_768 ?
W1 C1 2.121(7) 7_564 ?
W1 C12 2.180(7) 14_567 ?
W1 C12 2.180(7) 7_564 ?
W1 C12 2.180(7) 12_768 ?
W1 C12 2.180(7) . ?
Cu2 N3 1.944(5) 9_667 ?
Cu2 N3 1.944(5) . ?
Cu2 N2 2.095(6) . ?
Cu2 N2 2.095(6) 9_667 ?
Cu2 N1 2.471(6) 9_667 ?
Cu2 N1 2.471(6) . ?
N1 C8 1.339(9) . ?
N1 C9 1.340(9) . ?
N2 C4 1.351(9) . ?
N2 C13 1.354(9) . ?
N3 C1 1.151(8) . ?
N4 C12 1.166(8) . ?
C4 C16 1.362(11) . ?
C4 H4 0.9500 . ?
C5 C9 1.372(11) . ?
C5 C6 1.380(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.381(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.376(12) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C13 C14 1.382(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.352(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.393(12) . ?
C15 H15 0.9500 . ?
C16 H16 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
C1 W1 C1 94.14(9) 14_567 . ?
C1 W1 C1 148.8(3) 14_567 12_768 ?
C1 W1 C1 94.14(9) . 12_768 ?
C1 W1 C1 94.14(9) 14_567 7_564 ?
C1 W1 C1 148.8(3) . 7_564 ?
C1 W1 C1 94.14(9) 12_768 7_564 ?
C1 W1 C12 76.2(2) 14_567 14_567 ?
C1 W1 C12 69.8(2) . 14_567 ?
C1 W1 C12 78.6(2) 12_768 14_567 ?
C1 W1 C12 141.3(2) 7_564 14_567 ?
C1 W1 C12 69.8(2) 14_567 7_564 ?
C1 W1 C12 78.6(2) . 7_564 ?
C1 W1 C12 141.3(2) 12_768 7_564 ?
C1 W1 C12 76.2(2) 7_564 7_564 ?
C12 W1 C12 131.2(2) 14_567 7_564 ?
C1 W1 C12 78.6(2) 14_567 12_768 ?
C1 W1 C12 141.3(2) . 12_768 ?
C1 W1 C12 76.2(2) 12_768 12_768 ?
C1 W1 C12 69.8(2) 7_564 12_768 ?
C12 W1 C12 71.5(3) 14_567 12_768 ?
C12 W1 C12 131.2(2) 7_564 12_768 ?
C1 W1 C12 141.3(2) 14_567 . ?
C1 W1 C12 76.2(2) . . ?
C1 W1 C12 69.8(2) 12_768 . ?
C1 W1 C12 78.6(2) 7_564 . ?
C12 W1 C12 131.2(2) 14_567 . ?
C12 W1 C12 71.5(3) 7_564 . ?
C12 W1 C12 131.2(2) 12_768 . ?
N3 Cu2 N3 180.000(1) 9_667 . ?
N3 Cu2 N2 90.2(2) 9_667 . ?
N3 Cu2 N2 89.8(2) . . ?
N3 Cu2 N2 89.8(2) 9_667 9_667 ?
N3 Cu2 N2 90.2(2) . 9_667 ?
N2 Cu2 N2 180.00(9) . 9_667 ?
N3 Cu2 N1 88.7(2) 9_667 9_667 ?
N3 Cu2 N1 91.3(2) . 9_667 ?
N2 Cu2 N1 88.8(2) . 9_667 ?
N2 Cu2 N1 91.2(2) 9_667 9_667 ?
N3 Cu2 N1 91.3(2) 9_667 . ?
N3 Cu2 N1 88.7(2) . . ?
N2 Cu2 N1 91.2(2) . . ?
N2 Cu2 N1 88.8(2) 9_667 . ?
N1 Cu2 N1 180.000(1) 9_667 . ?
C8 N1 C9 115.7(7) . . ?
C8 N1 Cu2 125.3(5) . . ?
C9 N1 Cu2 118.9(5) . . ?
C4 N2 C13 116.4(7) . . ?
C4 N2 Cu2 122.5(5) . . ?
C13 N2 Cu2 121.0(5) . . ?
C1 N3 Cu2 175.7(6) . . ?
N3 C1 W1 178.4(6) . . ?
N2 C4 C16 123.4(8) . . ?
N2 C4 H4 118.3 . . ?
C16 C4 H4 118.3 . . ?
C9 C5 C6 119.7(8) . . ?
C9 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C7 117.4(8) . . ?
C5 C6 H6 121.3 . . ?
C7 C6 H6 121.3 . . ?
C8 C7 C6 119.1(8) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
N1 C8 C7 124.3(8) . . ?
N1 C8 H8 117.9 . . ?
C7 C8 H8 117.9 . . ?
N1 C9 C5 123.8(7) . . ?
N1 C9 H9 118.1 . . ?
C5 C9 H9 118.1 . . ?
N4 C12 W1 178.0(6) . . ?
N2 C13 C14 122.8(8) . . ?
N2 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C15 C14 C13 119.5(8) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 118.8(8) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C4 C16 C15 119.0(8) . . ?
C4 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Cu2 N1 C8 176.4(7) 9_667 . . . ?
N3 Cu2 N1 C8 -3.6(7) . . . . ?
N2 Cu2 N1 C8 86.2(7) . . . . ?
N2 Cu2 N1 C8 -93.8(7) 9_667 . . . ?
N1 Cu2 N1 C8 45(100) 9_667 . . . ?
N3 Cu2 N1 C9 -6.7(6) 9_667 . . . ?
N3 Cu2 N1 C9 173.3(6) . . . . ?
N2 Cu2 N1 C9 -97.0(6) . . . . ?
N2 Cu2 N1 C9 83.0(6) 9_667 . . . ?
N1 Cu2 N1 C9 -139(93) 9_667 . . . ?
N3 Cu2 N2 C4 -147.6(6) 9_667 . . . ?
N3 Cu2 N2 C4 32.4(6) . . . . ?
N2 Cu2 N2 C4 1(100) 9_667 . . . ?
N1 Cu2 N2 C4 123.7(6) 9_667 . . . ?
N1 Cu2 N2 C4 -56.3(6) . . . . ?
N3 Cu2 N2 C13 28.8(6) 9_667 . . . ?
N3 Cu2 N2 C13 -151.2(6) . . . . ?
N2 Cu2 N2 C13 178(100) 9_667 . . . ?
N1 Cu2 N2 C13 -59.9(6) 9_667 . . . ?
N1 Cu2 N2 C13 120.1(6) . . . . ?
N3 Cu2 N3 C1 49(100) 9_667 . . . ?
N2 Cu2 N3 C1 -127(8) . . . . ?
N2 Cu2 N3 C1 53(8) 9_667 . . . ?
N1 Cu2 N3 C1 144(8) 9_667 . . . ?
N1 Cu2 N3 C1 -36(8) . . . . ?
Cu2 N3 C1 W1 -40(27) . . . . ?
C1 W1 C1 N3 167(21) 14_567 . . . ?
C1 W1 C1 N3 -43(21) 12_768 . . . ?
C1 W1 C1 N3 62(21) 7_564 . . . ?
C12 W1 C1 N3 -120(21) 14_567 . . . ?
C12 W1 C1 N3 98(21) 7_564 . . . ?
C12 W1 C1 N3 -117(21) 12_768 . . . ?
C12 W1 C1 N3 25(21) . . . . ?
C13 N2 C4 C16 -0.2(12) . . . . ?
Cu2 N2 C4 C16 176.4(6) . . . . ?
C9 C5 C6 C7 -1.1(14) . . . . ?
C5 C6 C7 C8 0.7(15) . . . . ?
C9 N1 C8 C7 0.0(14) . . . . ?
Cu2 N1 C8 C7 177.0(8) . . . . ?
C6 C7 C8 N1 -0.1(16) . . . . ?
C8 N1 C9 C5 -0.5(13) . . . . ?
Cu2 N1 C9 C5 -177.7(7) . . . . ?
C6 C5 C9 N1 1.1(14) . . . . ?
C1 W1 C12 N4 -64(17) 14_567 . . . ?
C1 W1 C12 N4 16(17) . . . . ?
C1 W1 C12 N4 115(17) 12_768 . . . ?
C1 W1 C12 N4 -146(17) 7_564 . . . ?
C12 W1 C12 N4 62(17) 14_567 . . . ?
C12 W1 C12 N4 -67(17) 7_564 . . . ?
C12 W1 C12 N4 164(17) 12_768 . . . ?
C4 N2 C13 C14 1.0(12) . . . . ?
Cu2 N2 C13 C14 -175.6(6) . . . . ?
N2 C13 C14 C15 -1.2(13) . . . . ?
C13 C14 C15 C16 0.5(14) . . . . ?
N2 C4 C16 C15 -0.4(14) . . . . ?
C14 C15 C16 C4 0.2(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.742
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.118


# Attachment '- CIF.cif'

data_1
#TrackingRef '- CIF.cif'

_database_code_depnum_ccdc_archive 'CCDC 752236'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C32H56Co2N16O8W
_chemical_formula_sum            'C32 H56 Co2 N16 O8 W'
_chemical_formula_weight         1094.63

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'
Co Co 0.3494 0.9721 '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'
W W -0.8490 6.8722 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   12.1408(2)
_cell_length_b                   12.1408(2)
_cell_length_c                   34.7802(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5126.57(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8753
_cell_measurement_theta_min      3.26
_cell_measurement_theta_max      27.39

_exptl_crystal_description       prism
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2207
_exptl_absorpt_coefficient_mu    2.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6203
_exptl_absorpt_correction_T_max  0.7197
_exptl_absorpt_process_details   'SADABS(Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13769
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         27.39
_reflns_number_total             2906
_reflns_number_gt                2602
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_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^)+(0.0256P)^2^+3.2884P] 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         2906
_refine_ls_number_parameters     135
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0536
_refine_ls_wR_factor_gt          0.0524
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.064
_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
W1 W -0.5000 -0.2500 0.1250 0.01581(7) Uani 1 4 d S . .
Co1 Co -0.7500 -0.2500 0.2500 0.01830(10) Uani 1 2 d S . .
O1 O -0.81940(14) -0.40515(14) 0.24468(5) 0.0272(4) Uani 1 1 d . . .
O2 O -0.86629(14) -0.18006(14) 0.21158(5) 0.0259(4) Uani 1 1 d . . .
C3 C -0.6657(2) -0.2894(2) 0.10687(7) 0.0223(5) Uani 1 1 d . . .
N2 N -0.90226(19) -0.0874(2) 0.15606(7) 0.0337(5) Uani 1 1 d . . .
C2 C -0.59973(19) -0.27525(19) 0.17543(7) 0.0197(5) Uani 1 1 d . . .
N4 N -0.95318(19) -0.53364(18) 0.24674(8) 0.0358(6) Uani 1 1 d U . .
C1 C -0.9154(2) -0.4340(2) 0.25146(7) 0.0252(5) Uani 1 1 d U . .
H1A H -0.9650 -0.3796 0.2607 0.030 Uiso 1 1 calc R . .
N3 N -0.64848(17) -0.28372(17) 0.20331(6) 0.0227(4) Uani 1 1 d . . .
N1 N -0.75241(19) -0.3104(2) 0.09644(7) 0.0384(6) Uani 1 1 d . . .
C4 C -0.8813(3) -0.6207(3) 0.23323(16) 0.0874(16) Uani 1 1 d U . .
H4A H -0.8087 -0.5898 0.2271 0.131 Uiso 1 1 calc R . .
H4B H -0.9129 -0.6543 0.2101 0.131 Uiso 1 1 calc R . .
H4C H -0.8735 -0.6767 0.2533 0.131 Uiso 1 1 calc R . .
C5 C -1.0198(2) -0.1062(3) 0.15608(9) 0.0465(8) Uani 1 1 d . . .
H5A H -1.0409 -0.1442 0.1798 0.070 Uiso 1 1 calc R . .
H5B H -1.0398 -0.1518 0.1339 0.070 Uiso 1 1 calc R . .
H5C H -1.0583 -0.0355 0.1545 0.070 Uiso 1 1 calc R . .
C6 C -1.0655(2) -0.5634(3) 0.25710(10) 0.0443(8) Uani 1 1 d U . .
H6A H -1.1047 -0.4979 0.2663 0.066 Uiso 1 1 calc R . .
H6B H -1.0641 -0.6191 0.2775 0.066 Uiso 1 1 calc R . .
H6C H -1.1035 -0.5932 0.2345 0.066 Uiso 1 1 calc R . .
C7 C -0.8367(2) -0.1253(2) 0.18315(7) 0.0289(6) Uani 1 1 d . . .
H7A H -0.7604 -0.1094 0.1808 0.035 Uiso 1 1 calc R . .
C8 C -0.8573(3) -0.0287(3) 0.12293(9) 0.0595(11) Uani 1 1 d . . .
H8A H -0.7778 -0.0189 0.1263 0.089 Uiso 1 1 calc R . .
H8B H -0.8927 0.0436 0.1208 0.089 Uiso 1 1 calc R . .
H8C H -0.8712 -0.0713 0.0995 0.089 Uiso 1 1 calc R . .

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
W1 0.01821(8) 0.01821(8) 0.01101(10) 0.000 0.000 0.000
Co1 0.0206(2) 0.0205(2) 0.0138(2) 0.00052(18) 0.00202(18) -0.00352(18)
O1 0.0246(9) 0.0251(10) 0.0320(10) -0.0025(8) 0.0029(8) -0.0055(7)
O2 0.0258(10) 0.0312(10) 0.0207(9) 0.0042(7) 0.0005(7) -0.0009(7)
C3 0.0229(13) 0.0287(14) 0.0154(11) -0.0019(10) 0.0025(10) -0.0008(10)
N2 0.0301(13) 0.0420(14) 0.0289(12) 0.0121(10) -0.0009(10) 0.0025(10)
C2 0.0213(12) 0.0211(12) 0.0165(12) -0.0004(9) -0.0016(9) 0.0011(9)
N4 0.0279(12) 0.0240(12) 0.0554(16) -0.0035(11) 0.0032(11) -0.0051(9)
C1 0.0282(14) 0.0248(13) 0.0227(12) -0.0010(10) -0.0013(11) -0.0008(10)
N3 0.0262(11) 0.0234(11) 0.0186(10) 0.0007(8) 0.0020(9) -0.0025(9)
N1 0.0283(13) 0.0553(17) 0.0315(13) 0.0004(12) -0.0008(11) -0.0051(12)
C4 0.048(2) 0.034(2) 0.180(5) -0.032(3) 0.022(3) -0.0047(17)
C5 0.0379(18) 0.064(2) 0.0375(17) 0.0131(16) -0.0104(14) 0.0001(15)
C6 0.0338(17) 0.0387(17) 0.060(2) 0.0002(15) 0.0038(15) -0.0154(13)
C7 0.0249(14) 0.0313(15) 0.0306(14) 0.0050(12) 0.0009(11) 0.0006(11)
C8 0.052(2) 0.076(3) 0.051(2) 0.039(2) 0.0060(17) 0.0077(19)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C2 2.153(2) 7_344 ?
W1 C2 2.153(2) 12_566 ?
W1 C2 2.153(2) . ?
W1 C2 2.153(2) 14_545 ?
W1 C3 2.162(2) 12_566 ?
W1 C3 2.162(2) . ?
W1 C3 2.162(2) 7_344 ?
W1 C3 2.162(2) 14_545 ?
Co1 O1 2.0718(17) . ?
Co1 O1 2.0718(17) 13_345 ?
Co1 N3 2.079(2) 13_345 ?
Co1 N3 2.079(2) . ?
Co1 O2 2.1212(17) 13_345 ?
Co1 O2 2.1212(17) . ?
O1 C1 1.239(3) . ?
O2 C7 1.245(3) . ?
C3 N1 1.142(3) . ?
N2 C7 1.316(3) . ?
N2 C5 1.445(4) . ?
N2 C8 1.461(4) . ?
C2 N3 1.141(3) . ?
N4 C1 1.305(3) . ?
N4 C4 1.449(4) . ?
N4 C6 1.457(4) . ?
C1 H1A 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

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
C2 W1 C2 131.57(8) 7_344 12_566 ?
C2 W1 C2 70.91(12) 7_344 . ?
C2 W1 C2 131.57(8) 12_566 . ?
C2 W1 C2 131.57(8) 7_344 14_545 ?
C2 W1 C2 70.91(12) 12_566 14_545 ?
C2 W1 C2 131.57(8) . 14_545 ?
C2 W1 C3 76.74(9) 7_344 12_566 ?
C2 W1 C3 71.50(9) 12_566 12_566 ?
C2 W1 C3 75.78(9) . 12_566 ?
C2 W1 C3 142.40(9) 14_545 12_566 ?
C2 W1 C3 142.40(9) 7_344 . ?
C2 W1 C3 76.74(9) 12_566 . ?
C2 W1 C3 71.50(9) . . ?
C2 W1 C3 75.78(9) 14_545 . ?
C3 W1 C3 94.88(3) 12_566 . ?
C2 W1 C3 71.50(9) 7_344 7_344 ?
C2 W1 C3 75.78(9) 12_566 7_344 ?
C2 W1 C3 142.40(9) . 7_344 ?
C2 W1 C3 76.74(9) 14_545 7_344 ?
C3 W1 C3 94.88(3) 12_566 7_344 ?
C3 W1 C3 146.09(12) . 7_344 ?
C2 W1 C3 75.78(9) 7_344 14_545 ?
C2 W1 C3 142.40(9) 12_566 14_545 ?
C2 W1 C3 76.74(9) . 14_545 ?
C2 W1 C3 71.50(9) 14_545 14_545 ?
C3 W1 C3 146.09(12) 12_566 14_545 ?
C3 W1 C3 94.88(3) . 14_545 ?
C3 W1 C3 94.88(3) 7_344 14_545 ?
O1 Co1 O1 180.00(4) . 13_345 ?
O1 Co1 N3 90.44(7) . 13_345 ?
O1 Co1 N3 89.56(7) 13_345 13_345 ?
O1 Co1 N3 89.56(7) . . ?
O1 Co1 N3 90.44(7) 13_345 . ?
N3 Co1 N3 180.00(7) 13_345 . ?
O1 Co1 O2 87.88(7) . 13_345 ?
O1 Co1 O2 92.12(7) 13_345 13_345 ?
N3 Co1 O2 88.94(7) 13_345 13_345 ?
N3 Co1 O2 91.06(7) . 13_345 ?
O1 Co1 O2 92.12(7) . . ?
O1 Co1 O2 87.88(7) 13_345 . ?
N3 Co1 O2 91.06(7) 13_345 . ?
N3 Co1 O2 88.94(7) . . ?
O2 Co1 O2 180.00(7) 13_345 . ?
C1 O1 Co1 128.47(17) . . ?
C7 O2 Co1 121.49(17) . . ?
N1 C3 W1 178.4(2) . . ?
C7 N2 C5 122.8(2) . . ?
C7 N2 C8 120.6(3) . . ?
C5 N2 C8 116.5(2) . . ?
N3 C2 W1 175.6(2) . . ?
C1 N4 C4 120.3(3) . . ?
C1 N4 C6 121.9(2) . . ?
C4 N4 C6 117.6(3) . . ?
O1 C1 N4 124.7(2) . . ?
O1 C1 H1A 117.7 . . ?
N4 C1 H1A 117.7 . . ?
C2 N3 Co1 162.5(2) . . ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 H6A 109.5 . . ?
N4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O2 C7 N2 125.5(3) . . ?
O2 C7 H7A 117.2 . . ?
N2 C7 H7A 117.2 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Co1 O1 C1 -92(100) 13_345 . . . ?
N3 Co1 O1 C1 33.2(2) 13_345 . . . ?
N3 Co1 O1 C1 -146.8(2) . . . . ?
O2 Co1 O1 C1 122.1(2) 13_345 . . . ?
O2 Co1 O1 C1 -57.9(2) . . . . ?
O1 Co1 O2 C7 -127.02(19) . . . . ?
O1 Co1 O2 C7 52.98(19) 13_345 . . . ?
N3 Co1 O2 C7 142.5(2) 13_345 . . . ?
N3 Co1 O2 C7 -37.5(2) . . . . ?
O2 Co1 O2 C7 9(7) 13_345 . . . ?
C2 W1 C3 N1 -172(9) 7_344 . . . ?
C2 W1 C3 N1 -27(9) 12_566 . . . ?
C2 W1 C3 N1 -170(9) . . . . ?
C2 W1 C3 N1 46(9) 14_545 . . . ?
C3 W1 C3 N1 -97(9) 12_566 . . . ?
C3 W1 C3 N1 9(9) 7_344 . . . ?
C3 W1 C3 N1 115(9) 14_545 . . . ?
C2 W1 C2 N3 31(3) 7_344 . . . ?
C2 W1 C2 N3 161(3) 12_566 . . . ?
C2 W1 C2 N3 -98(3) 14_545 . . . ?
C3 W1 C2 N3 112(3) 12_566 . . . ?
C3 W1 C2 N3 -148(3) . . . . ?
C3 W1 C2 N3 33(3) 7_344 . . . ?
C3 W1 C2 N3 -48(3) 14_545 . . . ?
Co1 O1 C1 N4 178.8(2) . . . . ?
C4 N4 C1 O1 1.0(5) . . . . ?
C6 N4 C1 O1 176.8(3) . . . . ?
W1 C2 N3 Co1 66(3) . . . . ?
O1 Co1 N3 C2 138.2(7) . . . . ?
O1 Co1 N3 C2 -41.8(7) 13_345 . . . ?
N3 Co1 N3 C2 41(24) 13_345 . . . ?
O2 Co1 N3 C2 -133.9(7) 13_345 . . . ?
O2 Co1 N3 C2 46.1(7) . . . . ?
Co1 O2 C7 N2 173.5(2) . . . . ?
C5 N2 C7 O2 -0.3(5) . . . . ?
C8 N2 C7 O2 -176.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.39
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.073