# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Satoshi Takamizawa'

_publ_contact_author_email       STAKA@YOKOHAMA-CU.AC.JP

_publ_section_title              
;
Guest replacement
in a flexible single-crystal host by mixing surrounding gas
;
loop_
_publ_author_name
'Satoshi Takamizawa'
'Ryosuke Miyake'

# Attachment 'B904160E-revised-2 cif.txt'

data_71206y1
_database_code_depnum_ccdc_archive 'CCDC 722494'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
[Cu2(bza)4(pyz)]n 1.6(CH3OH)
;
_chemical_name_common            '(Cu2(bza)4(pyz))n 1.6(CH3OH)'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33.56 H30.24 Cu2 N2 O9.56'
_chemical_formula_weight         741.56

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.6996(16)
_cell_length_b                   9.9844(16)
_cell_length_c                   10.7765(17)
_cell_angle_alpha                70.417(3)
_cell_angle_beta                 65.104(2)
_cell_angle_gamma                62.126(2)
_cell_volume                     824.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    90
_cell_measurement_reflns_used    1517
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      27.09

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             386
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5237
_exptl_absorpt_correction_T_max  0.9355
_exptl_absorpt_process_details   
;
TWINABS; sheldrick, 2007
;

_exptl_special_details           
;
Since the crystal was sealed in glass capillary with the vapor mixture
(acetonitirile and methanol), although the crystal was
considered to be in saturated inclusion state,
the adsorption amount (methanol) should be decreased
because of a decrease of the inner vapor pressure
by cooling to the measurement temperature.
;

_diffrn_ambient_temperature      90
_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 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5559
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         27.51
_reflns_number_total             3746
_reflns_number_gt                3353
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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^)+(0.0538P)^2^+0.3999P] 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         3746
_refine_ls_number_parameters     218
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.0991
_refine_ls_wR_factor_gt          0.0953
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.6457(3) 0.6070(3) 0.3002(2) 0.0346(6) Uani 1 1 d . . .
Cu1 Cu 0.36996(4) 0.48766(4) 0.50545(4) 0.01426(11) Uani 1 1 d . . .
O3 O 0.2612(2) 0.6911(3) 0.5574(2) 0.0271(5) Uani 1 1 d . . .
O4 O 0.4833(2) 0.7138(2) 0.5485(2) 0.0271(5) Uani 1 1 d . . .
O2 O 0.4254(2) 0.5826(2) 0.3086(2) 0.0230(4) Uani 1 1 d . . .
N1 N 0.1433(3) 0.4926(2) 0.5065(2) 0.0154(4) Uani 1 1 d . . .
C8 C 0.3313(3) 0.7620(3) 0.5703(3) 0.0161(5) Uani 1 1 d . . .
C9 C 0.22496(18) 0.91445(15) 0.61697(17) 0.0173(5) Uani 1 1 d G . .
C10 C 0.05546(19) 0.96917(19) 0.6483(2) 0.0211(6) Uani 1 1 d G . .
H10 H 0.0081 0.9137 0.6334 0.025 Uiso 1 1 calc R . .
C11 C -0.04481(15) 1.1051(2) 0.7013(2) 0.0262(6) Uani 1 1 d G . .
H11 H -0.1607 1.1425 0.7227 0.031 Uiso 1 1 calc R . .
C12 C 0.0244(2) 1.18628(16) 0.72306(19) 0.0272(6) Uani 1 1 d G . .
H12 H -0.0441 1.2792 0.7593 0.033 Uiso 1 1 calc R . .
C13 C 0.1939(2) 1.13156(19) 0.6918(2) 0.0254(6) Uani 1 1 d G . .
H13 H 0.2412 1.1871 0.7066 0.030 Uiso 1 1 calc R . .
C14 C 0.29419(15) 0.99564(19) 0.6387(2) 0.0196(5) Uani 1 1 d G . .
H14 H 0.4100 0.9582 0.6173 0.024 Uiso 1 1 calc R . .
C1 C 0.5433(3) 0.6259(3) 0.2466(3) 0.0185(5) Uani 1 1 d . . .
C2 C 0.5637(3) 0.7047(2) 0.09925(15) 0.0214(6) Uani 1 1 d G . .
C3 C 0.4752(2) 0.7024(2) 0.02719(18) 0.0248(6) Uani 1 1 d G . .
H3 H 0.4027 0.6491 0.0714 0.030 Uiso 1 1 calc R . .
C4 C 0.4929(3) 0.7780(3) -0.10949(18) 0.0313(7) Uani 1 1 d G . .
H4 H 0.4324 0.7764 -0.1587 0.038 Uiso 1 1 calc R . .
C5 C 0.5990(3) 0.8560(3) -0.17411(16) 0.0338(7) Uani 1 1 d G . .
H5 H 0.6110 0.9077 -0.2675 0.041 Uiso 1 1 calc R . .
C6 C 0.6874(3) 0.8583(3) -0.1020(2) 0.0432(9) Uani 1 1 d G . .
H6 H 0.7599 0.9116 -0.1462 0.052 Uiso 1 1 calc R . .
C7 C 0.6698(3) 0.7827(3) 0.03463(19) 0.0395(9) Uani 1 1 d G . .
H7 H 0.7303 0.7843 0.0839 0.047 Uiso 1 1 calc R . .
C15 C -0.0041(3) 0.5683(3) 0.5896(3) 0.0170(5) Uani 1 1 d . . .
H15 H -0.0110 0.6179 0.6546 0.020 Uiso 1 1 calc R . .
C16 C 0.1471(3) 0.4240(3) 0.4172(3) 0.0163(5) Uani 1 1 d . . .
H16 H 0.2501 0.3687 0.3571 0.020 Uiso 1 1 calc R . .
C1S C 0.0835(17) 0.661(2) 0.9639(16) 0.040(4) Uani 0.375(8) 1 d PD A 1
H1S1 H 0.0314 0.7730 0.9513 0.060 Uiso 0.375(8) 1 calc PR A 1
H1S2 H 0.2028 0.6285 0.9378 0.060 Uiso 0.375(8) 1 calc PR A 1
H1S3 H 0.0408 0.6171 1.0614 0.060 Uiso 0.375(8) 1 calc PR A 1
O1S O 0.0483(7) 0.6068(8) 0.8787(7) 0.033(2) Uani 0.375(8) 1 d PD A 1
H1S H -0.0535 0.6463 0.8916 0.050 Uiso 0.375(8) 1 calc PR A 1
C2S C 0.1423(14) 0.6683(18) 0.9439(13) 0.035(3) Uani 0.404(8) 1 d PD B 2
H2S1 H 0.1048 0.7739 0.9567 0.053 Uiso 0.404(8) 1 calc PR B 2
H2S2 H 0.0755 0.6647 0.8985 0.053 Uiso 0.404(8) 1 calc PR B 2
H2S3 H 0.2580 0.6340 0.8858 0.053 Uiso 0.404(8) 1 calc PR B 2
O2S O 0.1261(9) 0.5711(7) 1.0739(6) 0.042(2) Uani 0.404(8) 1 d PD B 2
H2S H 0.1776 0.5792 1.1153 0.063 Uiso 0.404(8) 1 calc PR B 2

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
O1 0.0328(12) 0.0666(16) 0.0200(11) 0.0098(10) -0.0131(9) -0.0385(12)
Cu1 0.01066(16) 0.02047(17) 0.01542(16) -0.00211(11) -0.00501(11) -0.00877(12)
O3 0.0140(9) 0.0353(11) 0.0408(13) -0.0217(10) -0.0070(8) -0.0077(9)
O4 0.0138(9) 0.0207(10) 0.0501(14) -0.0091(9) -0.0114(9) -0.0060(8)
O2 0.0223(10) 0.0380(11) 0.0159(10) 0.0025(8) -0.0081(8) -0.0202(9)
N1 0.0141(10) 0.0193(11) 0.0156(11) 0.0010(9) -0.0067(8) -0.0095(9)
C8 0.0162(12) 0.0199(13) 0.0136(12) 0.0013(10) -0.0060(9) -0.0097(10)
C9 0.0184(13) 0.0184(13) 0.0157(12) 0.0017(10) -0.0062(10) -0.0099(11)
C10 0.0176(13) 0.0212(13) 0.0249(15) -0.0009(11) -0.0064(11) -0.0102(11)
C11 0.0200(14) 0.0207(13) 0.0286(16) 0.0004(11) -0.0057(12) -0.0054(12)
C12 0.0341(16) 0.0148(13) 0.0256(15) 0.0006(11) -0.0078(12) -0.0079(12)
C13 0.0372(17) 0.0198(13) 0.0249(16) 0.0025(11) -0.0149(13) -0.0152(13)
C14 0.0214(13) 0.0210(13) 0.0189(14) 0.0030(10) -0.0098(11) -0.0113(11)
C1 0.0178(12) 0.0230(14) 0.0180(13) -0.0031(10) -0.0063(10) -0.0102(11)
C2 0.0239(14) 0.0241(14) 0.0184(13) -0.0005(11) -0.0067(11) -0.0130(12)
C3 0.0255(14) 0.0305(15) 0.0220(15) -0.0004(11) -0.0094(12) -0.0147(13)
C4 0.0381(18) 0.0407(18) 0.0225(15) 0.0027(13) -0.0164(13) -0.0203(15)
C5 0.049(2) 0.0394(18) 0.0183(15) 0.0066(13) -0.0140(14) -0.0254(16)
C6 0.060(2) 0.063(2) 0.0255(17) 0.0093(16) -0.0144(16) -0.050(2)
C7 0.056(2) 0.063(2) 0.0216(16) 0.0076(15) -0.0158(15) -0.047(2)
C15 0.0167(12) 0.0221(13) 0.0161(13) -0.0026(10) -0.0060(10) -0.0103(11)
C16 0.0133(11) 0.0204(13) 0.0166(12) -0.0024(10) -0.0033(9) -0.0092(10)
C1S 0.029(8) 0.049(7) 0.050(8) -0.029(6) -0.019(7) 0.000(6)
O1S 0.021(3) 0.048(4) 0.031(4) -0.016(3) -0.005(2) -0.010(3)
C2S 0.024(7) 0.043(6) 0.032(5) -0.005(4) -0.007(5) -0.011(6)
O2S 0.060(5) 0.036(4) 0.029(3) -0.008(3) -0.010(3) -0.019(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.261(3) . ?
O1 Cu1 1.961(2) 2_666 ?
Cu1 O3 1.953(2) . ?
Cu1 O4 1.954(2) 2_666 ?
Cu1 O1 1.961(2) 2_666 ?
Cu1 O2 1.9638(19) . ?
Cu1 N1 2.172(2) . ?
Cu1 Cu1 2.5983(7) 2_666 ?
O3 C8 1.256(3) . ?
O4 C8 1.258(3) . ?
O4 Cu1 1.954(2) 2_666 ?
O2 C1 1.252(3) . ?
N1 C15 1.335(3) . ?
N1 C16 1.335(3) . ?
C8 C9 1.497(3) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C10 H10 0.9500 . ?
C11 C12 1.3900 . ?
C11 H11 0.9500 . ?
C12 C13 1.3900 . ?
C12 H12 0.9500 . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C1 C2 1.491(3) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 C7 1.3900 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C15 C16 1.385(3) 2_566 ?
C15 H15 0.9500 . ?
C16 C15 1.385(3) 2_566 ?
C16 H16 0.9500 . ?
C1S O1S 1.419(12) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O1S H1S 0.8400 . ?
C2S O2S 1.405(13) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
O2S H2S 0.8400 . ?

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 O1 Cu1 122.68(18) . 2_666 ?
O3 Cu1 O4 169.15(7) . 2_666 ?
O3 Cu1 O1 89.73(11) . 2_666 ?
O4 Cu1 O1 89.33(11) 2_666 2_666 ?
O3 Cu1 O2 89.76(9) . . ?
O4 Cu1 O2 89.10(10) 2_666 . ?
O1 Cu1 O2 169.00(7) 2_666 . ?
O3 Cu1 N1 92.63(8) . . ?
O4 Cu1 N1 98.21(8) 2_666 . ?
O1 Cu1 N1 98.50(8) 2_666 . ?
O2 Cu1 N1 92.50(8) . . ?
O3 Cu1 Cu1 82.51(6) . 2_666 ?
O4 Cu1 Cu1 86.64(6) 2_666 2_666 ?
O1 Cu1 Cu1 84.96(6) 2_666 2_666 ?
O2 Cu1 Cu1 84.08(5) . 2_666 ?
N1 Cu1 Cu1 174.04(6) . 2_666 ?
C8 O3 Cu1 125.41(17) . . ?
C8 O4 Cu1 120.49(17) . 2_666 ?
C1 O2 Cu1 123.73(17) . . ?
C15 N1 C16 117.3(2) . . ?
C15 N1 Cu1 122.58(17) . . ?
C16 N1 Cu1 120.05(18) . . ?
O3 C8 O4 124.9(2) . . ?
O3 C8 C9 117.3(2) . . ?
O4 C8 C9 117.8(2) . . ?
C10 C9 C14 120.0 . . ?
C10 C9 C8 119.76(14) . . ?
C14 C9 C8 120.07(14) . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
O2 C1 O1 124.5(3) . . ?
O2 C1 C2 117.5(2) . . ?
O1 C1 C2 118.0(2) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 120.23(15) . . ?
C7 C2 C1 119.77(15) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
N1 C15 C16 121.2(2) . 2_566 ?
N1 C15 H15 119.4 . . ?
C16 C15 H15 119.4 2_566 . ?
N1 C16 C15 121.5(2) . 2_566 ?
N1 C16 H16 119.3 . . ?
C15 C16 H16 119.3 2_566 . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C2S O2S H2S 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.090

#===END

data_71227y1
_database_code_depnum_ccdc_archive 'CCDC 722495'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
[Cu2(bza)4(pyz)]n 0.5(CH3CN) 1.3(CH3OH)

;
_chemical_name_common            '(Cu2(bza)4(pyz))n 0.5(CH3CN) 1.3(CH3OH)'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34.32 H30.76 Cu2 N2.50 O9.32'
_chemical_formula_weight         754.38

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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.6836(14)
_cell_length_b                   10.1691(14)
_cell_length_c                   10.6629(16)
_cell_angle_alpha                71.897(4)
_cell_angle_beta                 64.393(3)
_cell_angle_gamma                63.142(3)
_cell_volume                     836.0(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    90
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             386
_exptl_absorpt_coefficient_mu    1.330
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6182
_exptl_absorpt_correction_T_max  0.9612
_exptl_absorpt_process_details   
;
SADABS, scheldrick, 1996
;

_exptl_special_details           
;
Since the crystal was sealed in glass capillary with the vapor mixture
(acetonitirile and methanol), although the crystal was
considered to be in saturated inclusion state,
the adsorption amount (acetonitirile and methanol) should be decreased
because of a decrease of the inner vapor pressure
by cooling to the measurement temperature.
;

_diffrn_ambient_temperature      90
_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 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6204
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         28.33
_reflns_number_total             4092
_reflns_number_gt                3032
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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^)+(0.0667P)^2^+0.1783P] 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         4092
_refine_ls_number_parameters     270
_refine_ls_number_restraints     107
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1360
_refine_ls_wR_factor_gt          0.1247
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.024
_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
C1 C 0.9562(4) -0.1272(4) 0.2530(4) 0.0273(8) Uani 1 1 d . . .
C2 C 0.9375(4) -0.2068(4) 0.3986(4) 0.0321(8) Uani 1 1 d . . .
C3 C 1.0223(5) -0.2038(4) 0.4746(4) 0.0348(9) Uani 1 1 d . . .
H3 H 1.0941 -0.1502 0.4325 0.042 Uiso 1 1 calc R . .
C4 C 1.0036(5) -0.2772(5) 0.6091(5) 0.0440(10) Uani 1 1 d . . .
H4 H 1.0615 -0.2730 0.6596 0.053 Uiso 1 1 calc R . .
C5 C 0.9019(5) -0.3566(5) 0.6713(5) 0.0460(11) Uani 1 1 d . . .
H5 H 0.8899 -0.4083 0.7641 0.055 Uiso 1 1 calc R . .
C6 C 0.8170(6) -0.3604(7) 0.5968(5) 0.0595(14) Uani 1 1 d . . .
H6 H 0.7456 -0.4144 0.6394 0.071 Uiso 1 1 calc R . .
C7 C 0.8347(6) -0.2877(6) 0.4635(5) 0.0529(13) Uani 1 1 d . . .
H7 H 0.7761 -0.2922 0.4138 0.063 Uiso 1 1 calc R . .
C8 C 0.8308(4) 0.2548(4) 0.0783(3) 0.0239(7) Uani 1 1 d . . .
C9 C 0.7267(4) 0.4060(4) 0.1197(3) 0.0234(7) Uani 1 1 d . . .
C10 C 0.5579(4) 0.4637(4) 0.1464(4) 0.0314(8) Uani 1 1 d . . .
H10 H 0.5091 0.4074 0.1351 0.038 Uiso 1 1 calc R . .
C11 C 0.4608(5) 0.6015(5) 0.1889(5) 0.0456(11) Uani 1 1 d . . .
H11 H 0.3460 0.6411 0.2047 0.055 Uiso 1 1 calc R . .
C12 C 0.5308(5) 0.6823(5) 0.2086(6) 0.0512(12) Uani 1 1 d . . .
H12 H 0.4630 0.7752 0.2426 0.061 Uiso 1 1 calc R . .
C13 C 0.6990(5) 0.6281(4) 0.1790(5) 0.0402(10) Uani 1 1 d . . .
H13 H 0.7473 0.6856 0.1891 0.048 Uiso 1 1 calc R . .
C14 C 0.7966(4) 0.4909(4) 0.1348(4) 0.0280(8) Uani 1 1 d . . .
H14 H 0.9122 0.4540 0.1146 0.034 Uiso 1 1 calc R . .
C15 C 0.4960(4) 0.0644(4) 0.0938(4) 0.0260(8) Uani 1 1 d . . .
H15 H 0.4888 0.1111 0.1622 0.031 Uiso 1 1 calc R . .
C16 C 0.6475(4) -0.0730(4) -0.0866(4) 0.0280(8) Uani 1 1 d . . .
H16 H 0.7509 -0.1264 -0.1496 0.034 Uiso 1 1 calc R . .
Cu1 Cu 0.87010(5) -0.01304(5) 0.00602(5) 0.02396(15) Uani 1 1 d . . .
N1 N 0.6439(3) -0.0079(3) 0.0068(3) 0.0235(6) Uani 1 1 d . . .
O1 O 0.8539(3) -0.1088(3) 0.1995(3) 0.0365(7) Uani 1 1 d . . .
O2 O 0.7600(3) 0.1841(3) 0.0664(3) 0.0381(7) Uani 1 1 d . . .
O3 O 0.9833(3) 0.2070(3) 0.0564(3) 0.0297(6) Uani 1 1 d . . .
O4 O 1.0746(3) -0.0828(3) 0.1909(3) 0.0327(6) Uani 1 1 d . . .
C1S C 0.357(3) 0.823(2) 0.5531(15) 0.086(3) Uani 0.374(8) 1 d PDU A -3
H1S1 H 0.2501 0.8756 0.6198 0.129 Uiso 0.374(8) 1 calc PR A -3
H1S2 H 0.4425 0.7858 0.5946 0.129 Uiso 0.374(8) 1 calc PR A -3
H1S3 H 0.3509 0.7389 0.5316 0.129 Uiso 0.374(8) 1 calc PR A -3
O1S O 0.3951(16) 0.9228(15) 0.4267(13) 0.086(3) Uani 0.374(8) 1 d PDU A -3
H1S H 0.3156 0.9634 0.3970 0.130 Uiso 0.374(8) 1 calc PR A -3
C2S C 0.473(3) 0.971(3) 0.4728(18) 0.086(3) Uani 0.281(7) 1 d PDU B -2
H2S1 H 0.5314 0.8975 0.4078 0.129 Uiso 0.281(7) 1 calc PR B -2
H2S2 H 0.5396 1.0297 0.4520 0.129 Uiso 0.281(7) 1 calc PR B -2
H2S3 H 0.3666 1.0370 0.4620 0.129 Uiso 0.281(7) 1 calc PR B -2
O2S O 0.448(2) 0.8957(17) 0.6140(16) 0.085(3) Uani 0.281(7) 1 d PDU B -2
H2S H 0.3848 0.9582 0.6702 0.127 Uiso 0.281(7) 1 calc PR B -2
C3S C 0.421(2) 0.7327(19) 0.519(3) 0.087(3) Uani 0.253(7) 1 d PDU C -1
C4S C 0.472(3) 0.576(2) 0.511(3) 0.087(3) Uani 0.253(7) 1 d PDU C -1
H4S1 H 0.4052 0.5666 0.4686 0.131 Uiso 0.253(7) 1 calc PR C -1
H4S2 H 0.4562 0.5186 0.6050 0.131 Uiso 0.253(7) 1 calc PR C -1
H4S3 H 0.5886 0.5376 0.4521 0.131 Uiso 0.253(7) 1 calc PR C -1
N1S N 0.395(3) 0.8539(19) 0.526(3) 0.085(3) Uani 0.253(7) 1 d PDU C -1

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
C1 0.0160(15) 0.0352(19) 0.031(2) -0.0157(16) -0.0063(14) -0.0042(14)
C2 0.0213(17) 0.045(2) 0.028(2) -0.0138(17) -0.0057(15) -0.0077(16)
C3 0.0310(19) 0.037(2) 0.042(2) -0.0072(18) -0.0181(17) -0.0105(17)
C4 0.042(2) 0.056(3) 0.038(3) -0.008(2) -0.021(2) -0.013(2)
C5 0.040(2) 0.063(3) 0.029(2) -0.007(2) -0.0083(18) -0.018(2)
C6 0.055(3) 0.099(4) 0.035(3) -0.003(3) -0.008(2) -0.050(3)
C7 0.045(3) 0.100(4) 0.030(2) -0.007(2) -0.009(2) -0.046(3)
C8 0.0159(14) 0.0378(19) 0.0214(17) -0.0078(15) -0.0078(13) -0.0092(14)
C9 0.0181(15) 0.0311(18) 0.0218(18) -0.0045(14) -0.0077(13) -0.0087(14)
C10 0.0212(16) 0.034(2) 0.038(2) -0.0066(17) -0.0093(16) -0.0093(15)
C11 0.0256(19) 0.037(2) 0.070(3) -0.008(2) -0.017(2) -0.0063(17)
C12 0.040(2) 0.030(2) 0.081(4) -0.017(2) -0.022(2) -0.0033(19)
C13 0.043(2) 0.033(2) 0.053(3) -0.0075(19) -0.021(2) -0.0158(18)
C14 0.0256(17) 0.035(2) 0.027(2) 0.0000(16) -0.0119(15) -0.0145(16)
C15 0.0150(14) 0.0370(19) 0.033(2) -0.0169(16) -0.0070(14) -0.0088(14)
C16 0.0118(14) 0.040(2) 0.035(2) -0.0208(17) -0.0040(13) -0.0061(14)
Cu1 0.00982(19) 0.0392(3) 0.0306(3) -0.01450(18) -0.00758(15) -0.00870(16)
N1 0.0099(11) 0.0357(17) 0.0304(17) -0.0135(13) -0.0073(11) -0.0068(11)
O1 0.0209(12) 0.0685(19) 0.0288(15) -0.0117(13) -0.0080(11) -0.0213(13)
O2 0.0149(11) 0.0490(16) 0.0616(19) -0.0304(14) -0.0141(12) -0.0055(11)
O3 0.0139(11) 0.0401(14) 0.0400(16) -0.0139(12) -0.0083(10) -0.0097(10)
O4 0.0257(13) 0.0462(16) 0.0353(15) -0.0017(12) -0.0162(11) -0.0180(12)
C1S 0.086(3) 0.086(3) 0.086(3) -0.0124(9) -0.0295(12) -0.0314(12)
O1S 0.086(3) 0.086(3) 0.086(3) -0.0125(9) -0.0292(11) -0.0314(12)
C2S 0.086(3) 0.086(3) 0.086(3) -0.0123(9) -0.0294(12) -0.0314(12)
O2S 0.085(3) 0.085(3) 0.085(3) -0.0125(9) -0.0294(12) -0.0314(12)
C3S 0.086(3) 0.087(3) 0.086(3) -0.0124(9) -0.0297(12) -0.0319(12)
C4S 0.087(3) 0.088(3) 0.087(3) -0.0123(10) -0.0301(13) -0.0322(13)
N1S 0.086(3) 0.085(3) 0.085(3) -0.0124(8) -0.0295(11) -0.0315(12)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O4 1.258(4) . ?
C1 O1 1.264(4) . ?
C1 C2 1.485(5) . ?
C2 C7 1.393(6) . ?
C2 C3 1.394(5) . ?
C3 C4 1.371(6) . ?
C4 C5 1.372(6) . ?
C5 C6 1.386(6) . ?
C6 C7 1.359(6) . ?
C8 O2 1.257(4) . ?
C8 O3 1.263(4) . ?
C8 C9 1.487(5) . ?
C9 C10 1.391(4) . ?
C9 C14 1.392(4) . ?
C10 C11 1.374(5) . ?
C11 C12 1.383(6) . ?
C12 C13 1.382(6) . ?
C13 C14 1.375(5) . ?
C15 N1 1.333(4) . ?
C15 C16 1.386(4) 2_655 ?
C16 N1 1.339(4) . ?
C16 C15 1.386(4) 2_655 ?
Cu1 O3 1.954(3) 2_755 ?
Cu1 O1 1.959(3) . ?
Cu1 O2 1.962(3) . ?
Cu1 O4 1.968(3) 2_755 ?
Cu1 N1 2.164(2) . ?
Cu1 Cu1 2.5922(8) 2_755 ?
O3 Cu1 1.954(3) 2_755 ?
O4 Cu1 1.968(3) 2_755 ?
C1S O1S 1.4296(10) . ?
C2S O2S 1.4300(10) . ?
C3S N1S 1.1613(10) . ?
C3S C4S 1.4613(10) . ?

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
O4 C1 O1 124.3(4) . . ?
O4 C1 C2 117.1(3) . . ?
O1 C1 C2 118.5(3) . . ?
C7 C2 C3 117.8(4) . . ?
C7 C2 C1 120.8(3) . . ?
C3 C2 C1 121.4(3) . . ?
C4 C3 C2 121.0(4) . . ?
C3 C4 C5 120.5(4) . . ?
C4 C5 C6 119.1(4) . . ?
C7 C6 C5 120.7(4) . . ?
C6 C7 C2 121.0(4) . . ?
O2 C8 O3 124.7(3) . . ?
O2 C8 C9 117.2(3) . . ?
O3 C8 C9 118.1(3) . . ?
C10 C9 C14 118.9(3) . . ?
C10 C9 C8 120.6(3) . . ?
C14 C9 C8 120.4(3) . . ?
C11 C10 C9 120.7(3) . . ?
C10 C11 C12 119.8(4) . . ?
C13 C12 C11 120.1(4) . . ?
C14 C13 C12 120.1(4) . . ?
C13 C14 C9 120.3(3) . . ?
N1 C15 C16 121.4(3) . 2_655 ?
N1 C16 C15 121.6(3) . 2_655 ?
O3 Cu1 O1 88.71(12) 2_755 . ?
O3 Cu1 O2 169.48(9) 2_755 . ?
O1 Cu1 O2 90.51(12) . . ?
O3 Cu1 O4 89.59(11) 2_755 2_755 ?
O1 Cu1 O4 169.36(9) . 2_755 ?
O2 Cu1 O4 89.25(12) . 2_755 ?
O3 Cu1 N1 98.32(10) 2_755 . ?
O1 Cu1 N1 98.86(10) . . ?
O2 Cu1 N1 92.17(10) . . ?
O4 Cu1 N1 91.78(10) 2_755 . ?
O3 Cu1 Cu1 86.81(7) 2_755 2_755 ?
O1 Cu1 Cu1 85.28(7) . 2_755 ?
O2 Cu1 Cu1 82.66(7) . 2_755 ?
O4 Cu1 Cu1 84.14(7) 2_755 2_755 ?
N1 Cu1 Cu1 173.44(8) . 2_755 ?
C15 N1 C16 117.0(3) . . ?
C15 N1 Cu1 122.6(2) . . ?
C16 N1 Cu1 120.3(2) . . ?
C1 O1 Cu1 122.6(2) . . ?
C8 O2 Cu1 125.2(2) . . ?
C8 O3 Cu1 120.6(2) . 2_755 ?
C1 O4 Cu1 123.6(2) . 2_755 ?
N1S C3S C4S 173.7(13) . . ?

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
O4 C1 C2 C7 -165.7(4) . . . . ?
O1 C1 C2 C7 14.1(6) . . . . ?
O4 C1 C2 C3 14.0(5) . . . . ?
O1 C1 C2 C3 -166.3(3) . . . . ?
C7 C2 C3 C4 -0.6(6) . . . . ?
C1 C2 C3 C4 179.7(4) . . . . ?
C2 C3 C4 C5 0.7(6) . . . . ?
C3 C4 C5 C6 -0.7(7) . . . . ?
C4 C5 C6 C7 0.5(8) . . . . ?
C5 C6 C7 C2 -0.5(8) . . . . ?
C3 C2 C7 C6 0.5(7) . . . . ?
C1 C2 C7 C6 -179.8(4) . . . . ?
O2 C8 C9 C10 1.2(5) . . . . ?
O3 C8 C9 C10 -179.4(3) . . . . ?
O2 C8 C9 C14 -179.9(3) . . . . ?
O3 C8 C9 C14 -0.5(5) . . . . ?
C14 C9 C10 C11 -0.9(6) . . . . ?
C8 C9 C10 C11 178.0(4) . . . . ?
C9 C10 C11 C12 -1.5(7) . . . . ?
C10 C11 C12 C13 3.2(7) . . . . ?
C11 C12 C13 C14 -2.5(7) . . . . ?
C12 C13 C14 C9 0.0(6) . . . . ?
C10 C9 C14 C13 1.6(5) . . . . ?
C8 C9 C14 C13 -177.2(3) . . . . ?
C16 C15 N1 C16 -0.7(6) 2_655 . . . ?
C16 C15 N1 Cu1 176.3(3) 2_655 . . . ?
C15 C16 N1 C15 0.7(6) 2_655 . . . ?
C15 C16 N1 Cu1 -176.3(3) 2_655 . . . ?
O3 Cu1 N1 C15 150.5(3) 2_755 . . . ?
O1 Cu1 N1 C15 60.6(3) . . . . ?
O2 Cu1 N1 C15 -30.3(3) . . . . ?
O4 Cu1 N1 C15 -119.6(3) 2_755 . . . ?
Cu1 Cu1 N1 C15 -68.2(8) 2_755 . . . ?
O3 Cu1 N1 C16 -32.6(3) 2_755 . . . ?
O1 Cu1 N1 C16 -122.6(3) . . . . ?
O2 Cu1 N1 C16 146.5(3) . . . . ?
O4 Cu1 N1 C16 57.2(3) 2_755 . . . ?
Cu1 Cu1 N1 C16 108.6(7) 2_755 . . . ?
O4 C1 O1 Cu1 2.3(5) . . . . ?
C2 C1 O1 Cu1 -177.4(2) . . . . ?
O3 Cu1 O1 C1 86.8(3) 2_755 . . . ?
O2 Cu1 O1 C1 -82.7(3) . . . . ?
O4 Cu1 O1 C1 5.9(8) 2_755 . . . ?
N1 Cu1 O1 C1 -175.0(3) . . . . ?
Cu1 Cu1 O1 C1 -0.1(3) 2_755 . . . ?
O3 C8 O2 Cu1 -1.9(5) . . . . ?
C9 C8 O2 Cu1 177.4(2) . . . . ?
O3 Cu1 O2 C8 0.4(8) 2_755 . . . ?
O1 Cu1 O2 C8 86.0(3) . . . . ?
O4 Cu1 O2 C8 -83.3(3) 2_755 . . . ?
N1 Cu1 O2 C8 -175.1(3) . . . . ?
Cu1 Cu1 O2 C8 0.8(3) 2_755 . . . ?
O2 C8 O3 Cu1 2.0(5) . . . 2_755 ?
C9 C8 O3 Cu1 -177.4(2) . . . 2_755 ?
O1 C1 O4 Cu1 -3.9(5) . . . 2_755 ?
C2 C1 O4 Cu1 175.8(2) . . . 2_755 ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.099

#===END

data_40418s1
_database_code_depnum_ccdc_archive 'CCDC 722496'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
[Cu2(bza)4(pyz)]n 2.0(CH3CN)
;
_chemical_name_common            '(Cu2(bza)4(pyz))n 2.0(CH3CN)'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H30 Cu2 N4 O8'
_chemical_formula_weight         773.74

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'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.674(4)
_cell_length_b                   10.558(4)
_cell_length_c                   10.644(5)
_cell_angle_alpha                84.420(10)
_cell_angle_beta                 62.980(7)
_cell_angle_gamma                63.864(7)
_cell_volume                     862.2(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    90
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             396
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_T_max  0.9266
_exptl_absorpt_process_details   
;
SADABS; sheldrick, 1996
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90
_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 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5594
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         26.72
_reflns_number_total             3621
_reflns_number_gt                2660
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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^)+(0.0995P)^2^+1.9268P] 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         3621
_refine_ls_number_parameters     256
_refine_ls_number_restraints     332
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0749
_refine_ls_wR_factor_ref         0.2032
_refine_ls_wR_factor_gt          0.1922
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.065
_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
C1 C 0.5824(7) 0.7584(7) 1.0885(7) 0.0279(9) Uani 1 1 d U . .
C2 C 0.6495(8) 0.6083(7) 1.1181(7) 0.0291(9) Uani 1 1 d U . .
C3 C 0.5693(8) 0.5249(7) 1.1215(7) 0.0322(10) Uani 1 1 d U . .
H3 H 0.4684 0.5651 1.1082 0.039 Uiso 1 1 calc R . .
C4 C 0.6368(9) 0.3832(7) 1.1442(7) 0.0368(11) Uani 1 1 d U . .
H4 H 0.5823 0.3265 1.1464 0.044 Uiso 1 1 calc R . .
C5 C 0.7856(9) 0.3247(7) 1.1638(7) 0.0398(11) Uani 1 1 d U . .
H5 H 0.8328 0.2277 1.1783 0.048 Uiso 1 1 calc R . .
C6 C 0.8625(9) 0.4055(7) 1.1621(7) 0.0372(11) Uani 1 1 d U . .
H6 H 0.9623 0.3650 1.1770 0.045 Uiso 1 1 calc R . .
C7 C 0.7970(8) 0.5481(7) 1.1388(7) 0.0317(10) Uani 1 1 d U . .
H7 H 0.8527 0.6036 1.1371 0.038 Uiso 1 1 calc R . .
C8 C 0.7076(8) 0.8663(7) 0.7487(7) 0.0314(9) Uani 1 1 d U . .
C9 C 0.8348(8) 0.7862(7) 0.6050(7) 0.0332(9) Uani 1 1 d U . .
C10 C 0.7964(9) 0.7032(7) 0.5441(7) 0.0354(11) Uani 1 1 d U . .
H10 H 0.6904 0.6964 0.5953 0.042 Uiso 1 1 calc R . .
C11 C 0.9152(9) 0.6299(8) 0.4070(8) 0.0401(11) Uani 1 1 d U . .
H11 H 0.8896 0.5731 0.3652 0.048 Uiso 1 1 calc R . .
C12 C 1.0673(9) 0.6396(8) 0.3331(8) 0.0413(12) Uani 1 1 d U . .
H12 H 1.1467 0.5895 0.2401 0.050 Uiso 1 1 calc R . .
C13 C 1.1073(9) 0.7214(7) 0.3920(8) 0.0397(11) Uani 1 1 d U . .
H13 H 1.2131 0.7283 0.3400 0.048 Uiso 1 1 calc R . .
C14 C 0.9907(9) 0.7935(7) 0.5284(7) 0.0355(10) Uani 1 1 d U . .
H14 H 1.0183 0.8487 0.5699 0.043 Uiso 1 1 calc R . .
C15 C 0.0962(7) 1.0504(6) 0.8964(6) 0.0247(10) Uani 1 1 d U . .
H15 H 0.1625 1.0878 0.8213 0.030 Uiso 1 1 calc R . .
C16 C 0.0550(7) 0.9391(6) 1.0956(6) 0.0249(10) Uani 1 1 d U . .
H16 H 0.0899 0.8956 1.1655 0.030 Uiso 1 1 calc R . .
C1SA C 0.588(2) 0.1191(19) 0.510(2) 0.058(3) Uani 0.482(9) 1 d PDU . .
C2SA C 0.513(3) 0.028(2) 0.511(2) 0.060(3) Uani 0.482(9) 1 d PDU . .
H1SA H 0.5630 -0.0598 0.5474 0.090 Uiso 0.482(9) 1 calc PR . .
H2SA H 0.5370 0.0061 0.4134 0.090 Uiso 0.482(9) 1 calc PR . .
H3SA H 0.3872 0.0771 0.5713 0.090 Uiso 0.482(9) 1 calc PR . .
C1SB C 0.594(2) 0.2932(17) 0.4862(19) 0.058(3) Uani 0.518(9) 1 d PDU . .
C2SB C 0.517(2) 0.4466(15) 0.501(2) 0.062(3) Uani 0.518(9) 1 d PDU . .
H1SB H 0.5901 0.4770 0.4176 0.094 Uiso 0.518(9) 1 calc PR . .
H2SB H 0.5083 0.4827 0.5869 0.094 Uiso 0.518(9) 1 calc PR . .
H3SB H 0.4013 0.4842 0.5075 0.094 Uiso 0.518(9) 1 calc PR . .
Cu1 Cu 0.37675(9) 0.98812(8) 0.99188(8) 0.0227(2) Uani 1 1 d U . .
N1 N 0.1527(6) 0.9890(5) 0.9916(5) 0.0244(8) Uani 1 1 d U . .
N1SA N 0.629(2) 0.202(2) 0.524(2) 0.060(3) Uani 0.482(9) 1 d PDU . .
N1SB N 0.664(2) 0.1707(16) 0.4663(18) 0.060(2) Uani 0.518(9) 1 d PDU . .
O1 O 0.4500(5) 0.8058(4) 1.0665(4) 0.0276(8) Uani 1 1 d U . .
O2 O 0.6636(5) 0.8269(5) 1.0807(5) 0.0295(8) Uani 1 1 d U . .
O3 O 0.5530(5) 0.8863(5) 0.8004(5) 0.0312(8) Uani 1 1 d U . .
O4 O 0.7637(5) 0.9106(5) 0.8133(4) 0.0301(8) Uani 1 1 d U . .

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
C1 0.0240(14) 0.0357(16) 0.0318(15) 0.0035(14) -0.0192(12) -0.0129(13)
C2 0.0274(15) 0.0333(16) 0.0301(16) 0.0016(14) -0.0182(13) -0.0108(13)
C3 0.0327(17) 0.0330(18) 0.0332(18) -0.0018(15) -0.0210(14) -0.0094(15)
C4 0.0380(18) 0.0325(18) 0.0382(19) -0.0044(16) -0.0199(15) -0.0102(15)
C5 0.0386(18) 0.0344(19) 0.0375(19) -0.0030(16) -0.0191(16) -0.0058(16)
C6 0.0328(18) 0.0364(19) 0.0341(18) 0.0011(16) -0.0170(15) -0.0064(15)
C7 0.0284(17) 0.0347(18) 0.0316(18) 0.0018(16) -0.0167(14) -0.0103(15)
C8 0.0292(15) 0.0377(16) 0.0320(16) 0.0028(14) -0.0181(13) -0.0144(13)
C9 0.0330(15) 0.0375(16) 0.0339(16) 0.0014(14) -0.0209(13) -0.0133(13)
C10 0.0348(17) 0.0387(18) 0.0357(18) 0.0010(16) -0.0213(15) -0.0128(15)
C11 0.0390(18) 0.0413(19) 0.0385(19) -0.0022(17) -0.0212(16) -0.0117(16)
C12 0.0389(18) 0.0427(19) 0.0384(19) -0.0011(17) -0.0205(16) -0.0111(16)
C13 0.0366(18) 0.0425(19) 0.0383(19) -0.0002(17) -0.0193(16) -0.0130(16)
C14 0.0345(17) 0.0401(18) 0.0360(18) -0.0004(16) -0.0202(15) -0.0149(15)
C15 0.0218(18) 0.033(2) 0.032(2) 0.0071(17) -0.0205(16) -0.0145(16)
C16 0.0232(19) 0.031(2) 0.031(2) 0.0047(17) -0.0200(16) -0.0129(16)
C1SA 0.058(3) 0.061(3) 0.060(4) 0.008(3) -0.030(3) -0.026(3)
C2SA 0.060(4) 0.061(4) 0.062(4) 0.008(4) -0.033(3) -0.024(3)
C1SB 0.058(3) 0.063(3) 0.059(3) 0.005(3) -0.031(3) -0.028(3)
C2SB 0.064(4) 0.064(4) 0.058(4) 0.005(4) -0.028(3) -0.027(3)
Cu1 0.0147(3) 0.0340(4) 0.0292(4) 0.0030(3) -0.0165(3) -0.0120(3)
N1 0.0220(16) 0.0319(18) 0.0334(18) 0.0051(15) -0.0217(14) -0.0142(14)
N1SA 0.060(3) 0.063(3) 0.061(4) 0.005(3) -0.028(3) -0.029(3)
N1SB 0.059(3) 0.063(3) 0.060(4) 0.005(3) -0.029(3) -0.028(3)
O1 0.0226(15) 0.0349(17) 0.0340(17) 0.0039(14) -0.0186(13) -0.0140(14)
O2 0.0230(15) 0.0385(18) 0.0365(18) 0.0067(15) -0.0202(14) -0.0149(14)
O3 0.0291(16) 0.0413(18) 0.0316(17) 0.0008(15) -0.0185(14) -0.0172(14)
O4 0.0275(16) 0.0393(18) 0.0305(17) -0.0010(15) -0.0188(14) -0.0138(14)

_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
C1 O2 1.256(7) . ?
C1 O1 1.277(7) . ?
C1 C2 1.488(9) . ?
C2 C3 1.395(8) . ?
C2 C7 1.396(8) . ?
C3 C4 1.391(9) . ?
C4 C5 1.401(9) . ?
C5 C6 1.351(10) . ?
C6 C7 1.400(9) . ?
C8 O3 1.257(7) . ?
C8 O4 1.270(7) . ?
C8 C9 1.481(9) . ?
C9 C14 1.385(9) . ?
C9 C10 1.393(9) . ?
C10 C11 1.401(9) . ?
C11 C12 1.364(10) . ?
C12 C13 1.382(10) . ?
C13 C14 1.389(9) . ?
C15 N1 1.345(7) . ?
C15 C16 1.381(7) 2_577 ?
C16 N1 1.331(7) . ?
C16 C15 1.381(7) 2_577 ?
C1SA N1SA 1.146(19) . ?
C1SA C2SA 1.435(17) . ?
C1SB N1SB 1.152(19) . ?
C1SB C2SB 1.444(17) . ?
Cu1 O1 1.962(4) . ?
Cu1 O3 1.967(4) . ?
Cu1 O2 1.968(4) 2_677 ?
Cu1 O4 1.969(4) 2_677 ?
Cu1 N1 2.165(4) . ?
Cu1 Cu1 2.5864(15) 2_677 ?
O2 Cu1 1.968(4) 2_677 ?
O4 Cu1 1.969(4) 2_677 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 124.8(6) . . ?
O2 C1 C2 118.1(5) . . ?
O1 C1 C2 117.0(5) . . ?
C3 C2 C7 119.2(6) . . ?
C3 C2 C1 120.7(5) . . ?
C7 C2 C1 120.1(5) . . ?
C4 C3 C2 120.2(6) . . ?
C3 C4 C5 119.6(6) . . ?
C6 C5 C4 120.4(7) . . ?
C5 C6 C7 120.9(6) . . ?
C2 C7 C6 119.7(6) . . ?
O3 C8 O4 123.6(6) . . ?
O3 C8 C9 119.6(5) . . ?
O4 C8 C9 116.8(5) . . ?
C14 C9 C10 119.0(6) . . ?
C14 C9 C8 121.4(6) . . ?
C10 C9 C8 119.6(6) . . ?
C9 C10 C11 119.5(6) . . ?
C12 C11 C10 120.4(6) . . ?
C11 C12 C13 120.7(7) . . ?
C12 C13 C14 119.1(7) . . ?
C9 C14 C13 121.2(6) . . ?
N1 C15 C16 122.1(5) . 2_577 ?
N1 C16 C15 121.0(5) . 2_577 ?
N1SA C1SA C2SA 171(2) . . ?
N1SB C1SB C2SB 176(2) . . ?
O1 Cu1 O3 88.00(18) . . ?
O1 Cu1 O2 170.02(15) . 2_677 ?
O3 Cu1 O2 91.21(18) . 2_677 ?
O1 Cu1 O4 90.24(18) . 2_677 ?
O3 Cu1 O4 169.46(15) . 2_677 ?
O2 Cu1 O4 88.72(18) 2_677 2_677 ?
O1 Cu1 N1 96.72(17) . . ?
O3 Cu1 N1 98.95(17) . . ?
O2 Cu1 N1 93.23(17) 2_677 . ?
O4 Cu1 N1 91.57(17) 2_677 . ?
O1 Cu1 Cu1 86.57(11) . 2_677 ?
O3 Cu1 Cu1 85.92(12) . 2_677 ?
O2 Cu1 Cu1 83.46(12) 2_677 2_677 ?
O4 Cu1 Cu1 83.60(12) 2_677 2_677 ?
N1 Cu1 Cu1 174.19(13) . 2_677 ?
C16 N1 C15 116.9(5) . . ?
C16 N1 Cu1 120.2(4) . . ?
C15 N1 Cu1 122.6(4) . . ?
C1 O1 Cu1 120.5(4) . . ?
C1 O2 Cu1 124.2(4) . 2_677 ?
C8 O3 Cu1 122.3(4) . . ?
C8 O4 Cu1 124.5(4) . 2_677 ?

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
O2 C1 C2 C3 -177.0(6) . . . . ?
O1 C1 C2 C3 -0.1(9) . . . . ?
O2 C1 C2 C7 1.1(9) . . . . ?
O1 C1 C2 C7 178.0(6) . . . . ?
C7 C2 C3 C4 -0.5(9) . . . . ?
C1 C2 C3 C4 177.7(6) . . . . ?
C2 C3 C4 C5 0.1(10) . . . . ?
C3 C4 C5 C6 0.7(10) . . . . ?
C4 C5 C6 C7 -1.0(10) . . . . ?
C3 C2 C7 C6 0.2(9) . . . . ?
C1 C2 C7 C6 -178.0(6) . . . . ?
C5 C6 C7 C2 0.6(10) . . . . ?
O3 C8 C9 C14 162.4(6) . . . . ?
O4 C8 C9 C14 -17.8(9) . . . . ?
O3 C8 C9 C10 -16.7(9) . . . . ?
O4 C8 C9 C10 163.1(6) . . . . ?
C14 C9 C10 C11 -0.4(10) . . . . ?
C8 C9 C10 C11 178.7(6) . . . . ?
C9 C10 C11 C12 -0.1(10) . . . . ?
C10 C11 C12 C13 0.1(11) . . . . ?
C11 C12 C13 C14 0.4(11) . . . . ?
C10 C9 C14 C13 0.9(10) . . . . ?
C8 C9 C14 C13 -178.2(6) . . . . ?
C12 C13 C14 C9 -0.9(10) . . . . ?
C15 C16 N1 C15 0.5(9) 2_577 . . . ?
C15 C16 N1 Cu1 174.6(4) 2_577 . . . ?
C16 C15 N1 C16 -0.5(10) 2_577 . . . ?
C16 C15 N1 Cu1 -174.4(4) 2_577 . . . ?
O1 Cu1 N1 C16 37.3(5) . . . . ?
O3 Cu1 N1 C16 126.3(4) . . . . ?
O2 Cu1 N1 C16 -141.9(4) 2_677 . . . ?
O4 Cu1 N1 C16 -53.1(5) 2_677 . . . ?
Cu1 Cu1 N1 C16 -86.8(15) 2_677 . . . ?
O1 Cu1 N1 C15 -149.0(5) . . . . ?
O3 Cu1 N1 C15 -60.0(5) . . . . ?
O2 Cu1 N1 C15 31.8(5) 2_677 . . . ?
O4 Cu1 N1 C15 120.6(5) 2_677 . . . ?
Cu1 Cu1 N1 C15 86.9(15) 2_677 . . . ?
O2 C1 O1 Cu1 8.2(8) . . . . ?
C2 C1 O1 Cu1 -168.5(4) . . . . ?
O3 Cu1 O1 C1 82.3(5) . . . . ?
O2 Cu1 O1 C1 -3.3(13) 2_677 . . . ?
O4 Cu1 O1 C1 -87.3(5) 2_677 . . . ?
N1 Cu1 O1 C1 -178.9(5) . . . . ?
Cu1 Cu1 O1 C1 -3.7(4) 2_677 . . . ?
O1 C1 O2 Cu1 -8.6(9) . . . 2_677 ?
C2 C1 O2 Cu1 168.1(4) . . . 2_677 ?
O4 C8 O3 Cu1 -0.9(9) . . . . ?
C9 C8 O3 Cu1 178.8(4) . . . . ?
O1 Cu1 O3 C8 -87.2(5) . . . . ?
O2 Cu1 O3 C8 82.8(5) 2_677 . . . ?
O4 Cu1 O3 C8 -6.7(13) 2_677 . . . ?
N1 Cu1 O3 C8 176.3(5) . . . . ?
Cu1 Cu1 O3 C8 -0.6(5) 2_677 . . . ?
O3 C8 O4 Cu1 2.6(9) . . . 2_677 ?
C9 C8 O4 Cu1 -177.2(4) . . . 2_677 ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.72
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.179
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.151