# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Satoshi Takamizawa'
_publ_contact_author_email       STAKA@YOKOHAMA-CU.AC.JP

_publ_section_title              
;
Switch of channel geometry by 1D component
slide responding to slight structural stimuli of adsorbed guest
;
loop_
_publ_author_name
'Satoshi Takamizawa'
'Takamasa Akatsuka'
'Ryosuke Miyake'

# Attachment 'revised2_cif.txt'

data_60724a1_1b_298K
_database_code_depnum_ccdc_archive 'CCDC 736067'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H24 Cu2 N2 O8'
_chemical_formula_weight         691.61

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   17.998(16)
_cell_length_b                   9.697(8)
_cell_length_c                   18.903(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.339(18)
_cell_angle_gamma                90.00
_cell_volume                     3272(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    1.350
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7037
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_process_details   
;
SADABS; sheldrick, 1996
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298
_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            9009
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2903
_reflns_number_gt                2047
_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 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 > 2sigma(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)+(0.1047P)²+3.1363P] where P=(Fo²+2Fc²)/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         2903
_refine_ls_number_parameters     177
_refine_ls_number_restraints     270
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1869
_refine_ls_wR_factor_gt          0.1704
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.123
_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 0.1293(3) 0.7287(6) 0.2120(3) 0.0478(14) Uani 1 1 d U . .
C2 C 0.2037(2) 0.7286(4) 0.1883(3) 0.0548(15) Uani 1 1 d GU . .
C3 C 0.2296(3) 0.8472(4) 0.1581(3) 0.085(2) Uani 1 1 d GU . .
H3 H 0.2016 0.9279 0.1566 0.102 Uiso 1 1 calc R . .
C4 C 0.2975(3) 0.8450(5) 0.1303(3) 0.110(3) Uani 1 1 d GU . .
H4 H 0.3148 0.9244 0.1101 0.132 Uiso 1 1 calc R . .
C5 C 0.3394(2) 0.7244(6) 0.1327(3) 0.100(2) Uani 1 1 d GU . .
H5 H 0.3848 0.7229 0.1141 0.121 Uiso 1 1 calc R . .
C6 C 0.3135(2) 0.6058(5) 0.1628(3) 0.085(2) Uani 1 1 d GU . .
H6 H 0.3416 0.5251 0.1644 0.102 Uiso 1 1 calc R . .
C7 C 0.2457(3) 0.6080(4) 0.1907(3) 0.0645(17) Uani 1 1 d GU . .
H7 H 0.2283 0.5286 0.2108 0.077 Uiso 1 1 calc R . .
C8 C 0.0584(4) 0.7211(6) 0.3788(4) 0.0530(15) Uani 1 1 d U . .
C9 C 0.0979(3) 0.7173(5) 0.4518(2) 0.0607(16) Uani 1 1 d GU . .
C10 C 0.1014(3) 0.5934(4) 0.4890(3) 0.0731(19) Uani 1 1 d GU . .
H10 H 0.0767 0.5160 0.4688 0.088 Uiso 1 1 calc R . .
C11 C 0.1419(3) 0.5852(5) 0.5567(3) 0.094(2) Uani 1 1 d GU . .
H11 H 0.1442 0.5023 0.5816 0.113 Uiso 1 1 calc R . .
C12 C 0.1788(3) 0.7009(7) 0.5870(2) 0.099(2) Uani 1 1 d GU . .
H12 H 0.2059 0.6954 0.6322 0.118 Uiso 1 1 calc R . .
C13 C 0.1754(3) 0.8247(6) 0.5497(3) 0.104(3) Uani 1 1 d GU . .
H13 H 0.2001 0.9021 0.5700 0.125 Uiso 1 1 calc R . .
C14 C 0.1349(3) 0.8330(4) 0.4821(3) 0.087(2) Uani 1 1 d GU . .
H14 H 0.1326 0.9158 0.4572 0.105 Uiso 1 1 calc R . .
C15 C 0.0317(3) 0.2978(5) 0.2037(3) 0.0500(15) Uani 1 1 d U . .
H15 H 0.0547 0.3439 0.1692 0.060 Uiso 1 1 calc R . .
C16 C 0.0324(3) 0.1561(6) 0.2037(4) 0.0531(15) Uani 1 1 d U . .
H16 H 0.0566 0.1103 0.1700 0.064 Uiso 1 1 calc R . .
Cu1 Cu 0.0000 0.85959(8) 0.2500 0.0462(4) Uani 1 2 d SU . .
Cu2 Cu 0.0000 0.59227(8) 0.2500 0.0440(4) Uani 1 2 d SU . .
N1 N 0.0000 0.3715(6) 0.2500 0.0428(16) Uani 1 2 d SU . .
N2 N 0.0000 0.0826(6) 0.2500 0.0450(16) Uani 1 2 d SU . .
O1 O 0.0962(2) 0.8429(4) 0.2140(2) 0.0571(11) Uani 1 1 d U . .
O2 O 0.1030(2) 0.6154(4) 0.2287(2) 0.0547(11) Uani 1 1 d U . .
O3 O 0.0353(3) 0.6095(4) 0.3508(2) 0.0576(11) Uani 1 1 d U . .
O4 O 0.0514(3) 0.8364(4) 0.3475(2) 0.0605(12) Uani 1 1 d U . .


_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 1.252(7) . ?
C1 O1 1.261(7) . ?
C1 C2 1.466(7) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C8 O3 1.252(7) . ?
C8 O4 1.265(7) . ?
C8 C9 1.469(7) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C15 N1 1.315(6) . ?
C15 C16 1.374(8) . ?
C16 N2 1.321(7) . ?
Cu1 O1 1.946(4) 2 ?
Cu1 O1 1.946(4) . ?
Cu1 O4 1.966(5) . ?
Cu1 O4 1.966(5) 2 ?
Cu1 N2 2.163(6) 1_565 ?
Cu1 Cu2 2.592(2) . ?
Cu2 O3 1.938(5) . ?
Cu2 O3 1.938(5) 2 ?
Cu2 O2 1.960(4) 2 ?
Cu2 O2 1.960(4) . ?
Cu2 N1 2.141(6) . ?
N1 C15 1.315(6) 2 ?
N2 C16 1.321(7) 2 ?
N2 Cu1 2.163(6) 1_545 ?

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 124.6(6) . . ?
O2 C1 C2 117.8(5) . . ?
O1 C1 C2 117.6(5) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 119.5(3) . . ?
C7 C2 C1 120.3(3) . . ?
C2 C3 C4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C2 120.0 . . ?
O3 C8 O4 124.0(6) . . ?
O3 C8 C9 118.0(5) . . ?
O4 C8 C9 118.0(5) . . ?
C10 C9 C14 120.0 . . ?
C10 C9 C8 118.8(4) . . ?
C14 C9 C8 121.1(4) . . ?
C11 C10 C9 120.0 . . ?
C10 C11 C12 120.0 . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C14 120.0 . . ?
C13 C14 C9 120.0 . . ?
N1 C15 C16 123.2(6) . . ?
N2 C16 C15 122.4(6) . . ?
O1 Cu1 O1 170.5(2) 2 . ?
O1 Cu1 O4 89.8(2) 2 . ?
O1 Cu1 O4 89.1(2) . . ?
O1 Cu1 O4 89.1(2) 2 2 ?
O1 Cu1 O4 89.8(2) . 2 ?
O4 Cu1 O4 166.9(2) . 2 ?
O1 Cu1 N2 94.77(11) 2 1_565 ?
O1 Cu1 N2 94.77(11) . 1_565 ?
O4 Cu1 N2 96.56(12) . 1_565 ?
O4 Cu1 N2 96.56(12) 2 1_565 ?
O1 Cu1 Cu2 85.23(11) 2 . ?
O1 Cu1 Cu2 85.23(11) . . ?
O4 Cu1 Cu2 83.44(12) . . ?
O4 Cu1 Cu2 83.44(12) 2 . ?
N2 Cu1 Cu2 180.000(1) 1_565 . ?
O3 Cu2 O3 170.1(2) . 2 ?
O3 Cu2 O2 89.34(19) . 2 ?
O3 Cu2 O2 89.53(19) 2 2 ?
O3 Cu2 O2 89.53(19) . . ?
O3 Cu2 O2 89.34(19) 2 . ?
O2 Cu2 O2 166.9(2) 2 . ?
O3 Cu2 N1 94.94(12) . . ?
O3 Cu2 N1 94.94(12) 2 . ?
O2 Cu2 N1 96.57(11) 2 . ?
O2 Cu2 N1 96.57(11) . . ?
O3 Cu2 Cu1 85.06(12) . . ?
O3 Cu2 Cu1 85.06(12) 2 . ?
O2 Cu2 Cu1 83.43(11) 2 . ?
O2 Cu2 Cu1 83.43(11) . . ?
N1 Cu2 Cu1 180.000(1) . . ?
C15 N1 C15 114.2(6) 2 . ?
C15 N1 Cu2 122.9(3) 2 . ?
C15 N1 Cu2 122.9(3) . . ?
C16 N2 C16 114.7(7) 2 . ?
C16 N2 Cu1 122.7(3) 2 1_545 ?
C16 N2 Cu1 122.7(3) . 1_545 ?
C1 O1 Cu1 121.9(4) . . ?
C1 O2 Cu2 123.3(4) . . ?
C8 O3 Cu2 122.6(4) . . ?
C8 O4 Cu1 123.2(4) . . ?

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 169.3(5) . . . . ?
O1 C1 C2 C3 -10.6(7) . . . . ?
O2 C1 C2 C7 -5.5(8) . . . . ?
O1 C1 C2 C7 174.6(5) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C1 C2 C3 C4 -174.9(5) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C1 C2 C7 C6 174.8(5) . . . . ?
O3 C8 C9 C10 -6.4(7) . . . . ?
O4 C8 C9 C10 175.3(4) . . . . ?
O3 C8 C9 C14 170.1(5) . . . . ?
O4 C8 C9 C14 -8.2(7) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C8 C9 C10 C11 176.5(5) . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C9 0.0 . . . . ?
C10 C9 C14 C13 0.0 . . . . ?
C8 C9 C14 C13 -176.4(5) . . . . ?
N1 C15 C16 N2 1.2(9) . . . . ?
O1 Cu1 Cu2 O3 -81.4(2) 2 . . . ?
O1 Cu1 Cu2 O3 98.6(2) . . . . ?
O4 Cu1 Cu2 O3 8.97(18) . . . . ?
O4 Cu1 Cu2 O3 -171.03(18) 2 . . . ?
N2 Cu1 Cu2 O3 160(97) 1_565 . . . ?
O1 Cu1 Cu2 O3 98.6(2) 2 . . 2 ?
O1 Cu1 Cu2 O3 -81.4(2) . . . 2 ?
O4 Cu1 Cu2 O3 -171.03(18) . . . 2 ?
O4 Cu1 Cu2 O3 8.97(18) 2 . . 2 ?
N2 Cu1 Cu2 O3 -20(42) 1_565 . . 2 ?
O1 Cu1 Cu2 O2 8.54(18) 2 . . 2 ?
O1 Cu1 Cu2 O2 -171.46(18) . . . 2 ?
O4 Cu1 Cu2 O2 98.87(19) . . . 2 ?
O4 Cu1 Cu2 O2 -81.13(19) 2 . . 2 ?
N2 Cu1 Cu2 O2 -110(100) 1_565 . . 2 ?
O1 Cu1 Cu2 O2 -171.46(18) 2 . . . ?
O1 Cu1 Cu2 O2 8.54(18) . . . . ?
O4 Cu1 Cu2 O2 -81.13(19) . . . . ?
O4 Cu1 Cu2 O2 98.87(19) 2 . . . ?
N2 Cu1 Cu2 O2 70(43) 1_565 . . . ?
O1 Cu1 Cu2 N1 20(100) 2 . . . ?
O1 Cu1 Cu2 N1 -160(100) . . . . ?
O4 Cu1 Cu2 N1 111(100) . . . . ?
O4 Cu1 Cu2 N1 -69(100) 2 . . . ?
N2 Cu1 Cu2 N1 0(58) 1_565 . . . ?
C16 C15 N1 C15 -0.6(4) . . . 2 ?
C16 C15 N1 Cu2 179.4(4) . . . . ?
O3 Cu2 N1 C15 49.8(4) . . . 2 ?
O3 Cu2 N1 C15 -130.2(4) 2 . . 2 ?
O2 Cu2 N1 C15 -40.1(4) 2 . . 2 ?
O2 Cu2 N1 C15 139.9(4) . . . 2 ?
Cu1 Cu2 N1 C15 -52(100) . . . 2 ?
O3 Cu2 N1 C15 -130.2(4) . . . . ?
O3 Cu2 N1 C15 49.8(4) 2 . . . ?
O2 Cu2 N1 C15 139.9(4) 2 . . . ?
O2 Cu2 N1 C15 -40.1(4) . . . . ?
Cu1 Cu2 N1 C15 128(100) . . . . ?
C15 C16 N2 C16 -0.6(4) . . . 2 ?
C15 C16 N2 Cu1 179.4(4) . . . 1_545 ?
O2 C1 O1 Cu1 4.0(9) . . . . ?
C2 C1 O1 Cu1 -176.1(4) . . . . ?
O1 Cu1 O1 C1 -9.3(5) 2 . . . ?
O4 Cu1 O1 C1 74.1(5) . . . . ?
O4 Cu1 O1 C1 -92.8(5) 2 . . . ?
N2 Cu1 O1 C1 170.7(5) 1_565 . . . ?
Cu2 Cu1 O1 C1 -9.3(5) . . . . ?
O1 C1 O2 Cu2 7.8(9) . . . . ?
C2 C1 O2 Cu2 -172.1(4) . . . . ?
O3 Cu2 O2 C1 -96.2(5) . . . . ?
O3 Cu2 O2 C1 74.0(5) 2 . . . ?
O2 Cu2 O2 C1 -11.1(5) 2 . . . ?
N1 Cu2 O2 C1 168.9(5) . . . . ?
Cu1 Cu2 O2 C1 -11.1(5) . . . . ?
O4 C8 O3 Cu2 10.4(9) . . . . ?
C9 C8 O3 Cu2 -167.8(4) . . . . ?
O3 Cu2 O3 C8 -12.8(5) 2 . . . ?
O2 Cu2 O3 C8 -96.3(5) 2 . . . ?
O2 Cu2 O3 C8 70.6(5) . . . . ?
N1 Cu2 O3 C8 167.2(5) . . . . ?
Cu1 Cu2 O3 C8 -12.8(5) . . . . ?
O3 C8 O4 Cu1 2.0(9) . . . . ?
C9 C8 O4 Cu1 -179.9(4) . . . . ?
O1 Cu1 O4 C8 76.5(5) 2 . . . ?
O1 Cu1 O4 C8 -94.0(5) . . . . ?
O4 Cu1 O4 C8 -8.7(5) 2 . . . ?
N2 Cu1 O4 C8 171.3(5) 1_565 . . . ?
Cu2 Cu1 O4 C8 -8.7(5) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.049
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.115

#===END

data_61104a1_1b_2(acetone)_90K
_database_code_depnum_ccdc_archive 'CCDC 736068'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H36 Cu2 N2 O10'
_chemical_formula_weight         807.79

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           Monoclinic
_symmetry_space_group_name_H-M   C2/m

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

_cell_length_a                   17.757(3)
_cell_length_b                   9.6260(16)
_cell_length_c                   10.8050(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.603(4)
_cell_angle_gamma                90.00
_cell_volume                     1838.1(5)
_cell_formula_units_Z            2
_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          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6685
_exptl_absorpt_correction_T_max  0.9089
_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            6902
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         28.36
_reflns_number_total             2430
_reflns_number_gt                1738
_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 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 > 2sigma(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)+(0.0548P)²+2.6405P] where P=(Fo²+2Fc²)/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         2430
_refine_ls_number_parameters     188
_refine_ls_number_restraints     275
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1401
_refine_ls_wR_factor_gt          0.1282
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.096
_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 0.3658(2) 1.0000 0.0604(4) 0.0246(8) Uani 1 2 d SU . .
C2 C 0.2893(2) 1.0000 0.1067(4) 0.0252(8) Uani 1 2 d SU . .
C3 C 0.25371(16) 0.8755(3) 0.1293(3) 0.0318(7) Uani 1 1 d U . .
H3 H 0.2771 0.7900 0.1117 0.038 Uiso 1 1 calc R . .
C4 C 0.18450(17) 0.8753(3) 0.1770(3) 0.0409(8) Uani 1 1 d U . .
H4 H 0.1602 0.7899 0.1919 0.049 Uiso 1 1 calc R . .
C5 C 0.1504(2) 1.0000 0.2032(5) 0.0428(11) Uani 1 2 d SU . .
H5 H 0.1037 1.0000 0.2392 0.051 Uiso 1 2 calc SR . .
C7 C 0.5669(3) 0.9318(5) 0.3619(6) 0.0309(12) Uani 0.50 1 d PDU . -1
C8 C 0.5906(3) 1.0335(5) 0.4459(6) 0.0387(15) Uani 0.50 1 d PDU . -1
H8 H 0.5942 1.1270 0.4188 0.046 Uiso 0.50 1 calc PR . -1
C9 C 0.6092(3) 1.0005(13) 0.5697(5) 0.0455(11) Uani 1 2 d SDU . -1
C10 C 0.6030(4) 0.8647(6) 0.6098(6) 0.0441(15) Uani 0.50 1 d PDU . -1
H10 H 0.6155 0.8424 0.6950 0.053 Uiso 0.50 1 calc PR . -1
H9 H 0.6263 1.0705 0.6275 0.053 Uiso 0.50 1 d PR . -1
C11 C 0.5787(4) 0.7617(6) 0.5265(6) 0.0418(15) Uani 0.50 1 d PDU . -1
H11 H 0.5741 0.6686 0.5541 0.050 Uiso 0.50 1 calc PR . -1
C12 C 0.5611(3) 0.7951(6) 0.4024(5) 0.0360(13) Uani 0.50 1 d PDU . -1
H12 H 0.5451 0.7244 0.3445 0.043 Uiso 0.50 1 calc PR . -1
C13 C 0.46131(16) 0.5714(3) 0.0769(3) 0.0374(8) Uani 1 1 d U . .
H13 H 0.4329 0.6196 0.1334 0.045 Uiso 1 1 calc R . .
C1S C 0.3154(4) 0.5637(9) 0.3437(7) 0.0556(19) Uani 0.50 1 d PU A -1
C2S C 0.2591(4) 0.492(5) 0.2530(7) 0.070(3) Uani 0.50 1 d PU A -1
H2S1 H 0.2833 0.4665 0.1786 0.104 Uiso 0.50 1 calc PR A -1
H2S2 H 0.2166 0.5549 0.2297 0.104 Uiso 0.50 1 calc PR A -1
H2S3 H 0.2404 0.4083 0.2914 0.104 Uiso 0.50 1 calc PR A -1
C3S C 0.2891(6) 0.6193(10) 0.4547(9) 0.080(3) Uani 0.50 1 d PU A -1
H3S1 H 0.3309 0.6669 0.5035 0.121 Uiso 0.50 1 calc PR A -1
H3S2 H 0.2704 0.5436 0.5041 0.121 Uiso 0.50 1 calc PR A -1
H3S3 H 0.2481 0.6855 0.4325 0.121 Uiso 0.50 1 calc PR A -1
Cu1 Cu 0.4950(2) 0.86724(5) -0.0213(3) 0.0254(6) Uani 0.50 1 d PDU . -1
N1 N 0.5000 0.6432(3) 0.0000 0.0430(10) Uani 1 2 d SU . .
O1 O 0.39577(13) 0.88578(19) 0.0442(3) 0.0478(7) Uani 1 1 d DU . .
O2 O 0.5301(3) 0.8645(5) 0.1526(5) 0.0285(13) Uani 0.50 1 d PDU . .
C6 C 0.5452(4) 0.9645(6) 0.2307(7) 0.0253(17) Uani 0.50 1 d PU . -1
O1S O 0.3790(4) 0.5793(8) 0.3185(6) 0.086(2) Uani 0.50 1 d PU A -1
O3 O 0.5408(3) 1.0919(6) 0.1948(5) 0.0260(13) Uani 0.50 1 d PU . -1


_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 O1 1.242(3) 6_575 ?
C1 O1 1.242(3) . ?
C1 C2 1.492(5) . ?
C2 C3 1.387(3) 6_575 ?
C2 C3 1.387(3) . ?
C3 C4 1.378(4) . ?
C4 C5 1.385(4) . ?
C5 C4 1.385(4) 6_575 ?
C7 C8 1.372(7) . ?
C7 C12 1.394(7) . ?
C7 C6 1.467(10) . ?
C8 C9 1.384(7) . ?
C9 C10 1.385(12) . ?
C10 C11 1.379(8) . ?
C11 C12 1.385(8) . ?
C13 N1 1.324(3) . ?
C13 C13 1.374(5) 6_565 ?
C1S O1S 1.197(9) . ?
C1S C3S 1.433(12) . ?
C1S C2S 1.50(2) . ?
Cu1 O2 1.921(6) . ?
Cu1 O1 1.971(5) . ?
Cu1 O1 1.987(5) 2_655 ?
Cu1 N1 2.169(3) . ?
N1 C13 1.324(3) 2_655 ?
N1 Cu1 2.169(3) 2_655 ?
O1 Cu1 1.987(5) 2_655 ?
O2 O3 0.636(5) 6_575 ?
O2 C6 1.292(7) . ?
O2 C6 1.857(8) 6_575 ?
C6 O3 1.286(9) . ?
C6 O2 1.857(8) 6_575 ?
O3 O2 0.636(5) 6_575 ?

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
O1 C1 O1 124.6(4) 6_575 . ?
O1 C1 C2 117.66(19) 6_575 . ?
O1 C1 C2 117.66(19) . . ?
C3 C2 C3 119.4(4) 6_575 . ?
C3 C2 C1 120.28(19) 6_575 . ?
C3 C2 C1 120.28(19) . . ?
C4 C3 C2 120.4(3) . . ?
C3 C4 C5 119.9(3) . . ?
C4 C5 C4 120.0(4) 6_575 . ?
C8 C7 C12 119.5(5) . . ?
C8 C7 C6 121.4(5) . . ?
C12 C7 C6 119.1(5) . . ?
C7 C8 C9 120.3(6) . . ?
C8 C9 C10 120.0(7) . . ?
C11 C10 C9 120.3(5) . . ?
C10 C11 C12 119.4(5) . . ?
C11 C12 C7 120.5(5) . . ?
N1 C13 C13 121.51(16) . 6_565 ?
O1S C1S C3S 122.4(8) . . ?
O1S C1S C2S 119.6(8) . . ?
C3S C1S C2S 117.9(8) . . ?
O2 Cu1 O2 177.9(3) 2_655 . ?
O2 Cu1 O1 98.8(3) 2_655 . ?
O2 Cu1 O1 82.3(2) . . ?
O2 Cu1 O1 95.2(3) 2_655 2_655 ?
O2 Cu1 O1 84.0(2) . 2_655 ?
O1 Cu1 O1 162.69(13) . 2_655 ?
O2 Cu1 N1 95.2(2) 2_655 . ?
O2 Cu1 N1 82.90(17) . . ?
O1 Cu1 N1 94.61(14) . . ?
O1 Cu1 N1 94.15(13) 2_655 . ?
C13 N1 C13 117.0(3) . 2_655 ?
C13 N1 Cu1 118.10(19) . 2_655 ?
C13 N1 Cu1 124.6(2) 2_655 2_655 ?
C13 N1 Cu1 124.6(2) . . ?
C13 N1 Cu1 118.10(19) 2_655 . ?
Cu1 N1 Cu1 12.62(12) 2_655 . ?
C1 O1 Cu1 122.8(2) . . ?
C1 O1 Cu1 122.3(2) . 2_655 ?
Cu1 O1 Cu1 13.84(13) . 2_655 ?
O3 O2 C6 7.8(7) 6_575 . ?
O3 O2 Cu1 137.2(10) 6_575 2_655 ?
C6 O2 Cu1 130.7(6) . 2_655 ?
O3 O2 C6 21.2(7) 6_575 6_575 ?
C6 O2 C6 14.2(3) . 6_575 ?
Cu1 O2 C6 116.5(4) 2_655 6_575 ?
O3 O2 Cu1 137.6(9) 6_575 . ?
C6 O2 Cu1 131.0(6) . . ?
C6 O2 Cu1 116.8(4) 6_575 . ?
O3 C6 O2 120.7(8) . . ?
O3 C6 C7 119.9(5) . . ?
O2 C6 C7 119.3(6) . . ?
O2 C6 O2 110.6(8) . 6_575 ?
C7 C6 O2 130.0(5) . 6_575 ?
O2 O3 C6 148.5(10) 6_575 . ?

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 C1 C2 C3 0.6(6) 6_575 . . 6_575 ?
O1 C1 C2 C3 178.5(4) . . . 6_575 ?
O1 C1 C2 C3 -178.5(4) 6_575 . . . ?
O1 C1 C2 C3 -0.6(6) . . . . ?
C3 C2 C3 C4 -1.8(6) 6_575 . . . ?
C1 C2 C3 C4 177.3(3) . . . . ?
C2 C3 C4 C5 -0.3(6) . . . . ?
C3 C4 C5 C4 2.5(7) . . . 6_575 ?
C12 C7 C8 C9 0.4(8) . . . . ?
C6 C7 C8 C9 178.6(5) . . . . ?
C7 C8 C9 C10 -0.8(8) . . . . ?
C8 C9 C10 C11 0.4(10) . . . . ?
C9 C10 C11 C12 0.5(10) . . . . ?
C10 C11 C12 C7 -0.9(10) . . . . ?
C8 C7 C12 C11 0.4(9) . . . . ?
C6 C7 C12 C11 -177.8(6) . . . . ?
C13 C13 N1 C13 0.0 6_565 . . 2_655 ?
C13 C13 N1 Cu1 -173.88(8) 6_565 . . 2_655 ?
C13 C13 N1 Cu1 173.43(8) 6_565 . . . ?
O2 Cu1 N1 C13 -121.2(3) 2_655 . . . ?
O2 Cu1 N1 C13 59.7(3) . . . . ?
O1 Cu1 N1 C13 -21.9(2) . . . . ?
O1 Cu1 N1 C13 143.1(2) 2_655 . . . ?
O2 Cu1 N1 C13 52.1(4) 2_655 . . 2_655 ?
O2 Cu1 N1 C13 -127.0(3) . . . 2_655 ?
O1 Cu1 N1 C13 151.43(19) . . . 2_655 ?
O1 Cu1 N1 C13 -43.5(2) 2_655 . . 2_655 ?
O2 Cu1 N1 Cu1 176.3(13) 2_655 . . 2_655 ?
O2 Cu1 N1 Cu1 -2.8(10) . . . 2_655 ?
O1 Cu1 N1 Cu1 -84.4(11) . . . 2_655 ?
O1 Cu1 N1 Cu1 80.7(10) 2_655 . . 2_655 ?
O1 C1 O1 Cu1 -4.2(7) 6_575 . . . ?
C2 C1 O1 Cu1 178.1(3) . . . . ?
O1 C1 O1 Cu1 12.3(7) 6_575 . . 2_655 ?
C2 C1 O1 Cu1 -165.5(3) . . . 2_655 ?
O2 Cu1 O1 C1 -88.3(4) 2_655 . . . ?
O2 Cu1 O1 C1 93.5(3) . . . . ?
O1 Cu1 O1 C1 55.4(5) 2_655 . . . ?
N1 Cu1 O1 C1 175.6(3) . . . . ?
O2 Cu1 O1 Cu1 179.3(2) 2_655 . . 2_655 ?
O2 Cu1 O1 Cu1 1.05(17) . . . 2_655 ?
O1 Cu1 O1 Cu1 -37.0(4) 2_655 . . 2_655 ?
N1 Cu1 O1 Cu1 83.23(12) . . . 2_655 ?
O2 Cu1 O2 O3 149(10) 2_655 . . 6_575 ?
O1 Cu1 O2 O3 -89.7(14) . . . 6_575 ?
O1 Cu1 O2 O3 79.7(14) 2_655 . . 6_575 ?
N1 Cu1 O2 O3 174.7(14) . . . 6_575 ?
O2 Cu1 O2 C6 154(10) 2_655 . . . ?
O1 Cu1 O2 C6 -84.0(8) . . . . ?
O1 Cu1 O2 C6 85.4(8) 2_655 . . . ?
N1 Cu1 O2 C6 -179.7(8) . . . . ?
O2 Cu1 O2 Cu1 80(17) 2_655 . . 2_655 ?
O1 Cu1 O2 Cu1 -159(7) . . . 2_655 ?
O1 Cu1 O2 Cu1 11(7) 2_655 . . 2_655 ?
N1 Cu1 O2 Cu1 106(7) . . . 2_655 ?
O2 Cu1 O2 C6 154(10) 2_655 . . 6_575 ?
O1 Cu1 O2 C6 -84.3(5) . . . 6_575 ?
O1 Cu1 O2 C6 85.1(5) 2_655 . . 6_575 ?
N1 Cu1 O2 C6 -179.9(5) . . . 6_575 ?
O3 O2 C6 O3 147(6) 6_575 . . . ?
Cu1 O2 C6 O3 -2.0(13) 2_655 . . . ?
C6 O2 C6 O3 -2.3(4) 6_575 . . . ?
Cu1 O2 C6 O3 -3.2(12) . . . . ?
O3 O2 C6 C7 -33(5) 6_575 . . . ?
Cu1 O2 C6 C7 177.3(5) 2_655 . . . ?
C6 O2 C6 C7 177.1(11) 6_575 . . . ?
Cu1 O2 C6 C7 176.1(4) . . . . ?
O3 O2 C6 O2 149(5) 6_575 . . 6_575 ?
Cu1 O2 C6 O2 0.2(13) 2_655 . . 6_575 ?
C6 O2 C6 O2 0.000(10) 6_575 . . 6_575 ?
Cu1 O2 C6 O2 -1.0(12) . . . 6_575 ?
C8 C7 C6 O3 -7.1(9) . . . . ?
C12 C7 C6 O3 171.1(6) . . . . ?
C8 C7 C6 O2 173.5(7) . . . . ?
C12 C7 C6 O2 -8.3(10) . . . . ?
C8 C7 C6 O2 -10.0(10) . . . 6_575 ?
C12 C7 C6 O2 168.2(6) . . . 6_575 ?
O2 C6 O3 O2 12(2) . . . 6_575 ?
C7 C6 O3 O2 -167.4(19) . . . 6_575 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.085


#===END

data_60723a1_1b_90K
_database_code_depnum_ccdc_archive 'CCDC 745355'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H24 Cu2 N2 O8'
_chemical_formula_weight         691.61

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   17.485(3)
_cell_length_b                   9.6876(19)
_cell_length_c                   19.213(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.432(4)
_cell_angle_gamma                90.00
_cell_volume                     3219.2(11)
_cell_formula_units_Z            4
_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          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6999
_exptl_absorpt_correction_T_max  0.9731
_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            11425
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         28.28
_reflns_number_total             3999
_reflns_number_gt                2987
_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 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 > 2sigma(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)+(0.0814P)²+0.0000P] where P=(Fo²+2Fc²)/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         3999
_refine_ls_number_parameters     201
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1462
_refine_ls_wR_factor_gt          0.1342
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.136
_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 0.1340(2) 0.7337(3) 0.2152(2) 0.0174(7) Uani 1 1 d . . .
C2 C 0.2099(2) 0.7342(4) 0.1894(2) 0.0186(7) Uani 1 1 d . . .
C3 C 0.2392(2) 0.8551(4) 0.1650(2) 0.0255(9) Uani 1 1 d . . .
H3 H 0.2123 0.9396 0.1680 0.031 Uiso 1 1 calc R . .
C4 C 0.3074(2) 0.8536(4) 0.1362(2) 0.0321(10) Uani 1 1 d . . .
H4 H 0.3272 0.9367 0.1195 0.039 Uiso 1 1 calc R . .
C5 C 0.3464(2) 0.7303(4) 0.1318(2) 0.0307(10) Uani 1 1 d . . .
H5 H 0.3921 0.7282 0.1104 0.037 Uiso 1 1 calc R . .
C6 C 0.3194(2) 0.6105(4) 0.1584(2) 0.0276(9) Uani 1 1 d . . .
H6 H 0.3472 0.5267 0.1566 0.033 Uiso 1 1 calc R . .
C7 C 0.2519(2) 0.6123(4) 0.1875(2) 0.0216(8) Uani 1 1 d . . .
H7 H 0.2339 0.5299 0.2064 0.026 Uiso 1 1 calc R . .
C8 C 0.0589(2) 0.7228(4) 0.3785(2) 0.0189(8) Uani 1 1 d . . .
C9 C 0.0985(2) 0.7176(4) 0.4518(2) 0.0202(8) Uani 1 1 d . . .
C10 C 0.1010(2) 0.5960(4) 0.4908(2) 0.0241(8) Uani 1 1 d . . .
H10 H 0.0745 0.5166 0.4707 0.029 Uiso 1 1 calc R . .
C11 C 0.1410(2) 0.5889(4) 0.5576(2) 0.0311(10) Uani 1 1 d . . .
H11 H 0.1415 0.5055 0.5836 0.037 Uiso 1 1 calc R . .
C12 C 0.1808(3) 0.7033(5) 0.5872(2) 0.0341(10) Uani 1 1 d . . .
H12 H 0.2097 0.6977 0.6331 0.041 Uiso 1 1 calc R . .
C13 C 0.1784(3) 0.8249(5) 0.5500(2) 0.0359(11) Uani 1 1 d . . .
H13 H 0.2050 0.9038 0.5705 0.043 Uiso 1 1 calc R . .
C14 C 0.1375(2) 0.8328(4) 0.4831(2) 0.0292(9) Uani 1 1 d . . .
H14 H 0.1358 0.9174 0.4580 0.035 Uiso 1 1 calc R . .
C15 C 0.0379(2) 0.3014(3) 0.2071(2) 0.0193(8) Uani 1 1 d . . .
H15 H 0.0655 0.3495 0.1756 0.023 Uiso 1 1 calc R . .
C16 C 0.0382(2) 0.1580(3) 0.2071(2) 0.0192(8) Uani 1 1 d . . .
H16 H 0.0662 0.1103 0.1757 0.023 Uiso 1 1 calc R . .
Cu1 Cu 0.0000 0.86259(6) 0.2500 0.01650(19) Uani 1 2 d SU . .
Cu2 Cu 0.0000 0.59529(6) 0.2500 0.01612(19) Uani 1 2 d SU . .
N1 N 0.0000 0.3729(4) 0.2500 0.0163(9) Uani 1 2 d SU . .
N2 N 0.0000 0.0859(4) 0.2500 0.0181(9) Uani 1 2 d SU . .
O1 O 0.09927(15) 0.8482(2) 0.21633(14) 0.0208(6) Uani 1 1 d . . .
O2 O 0.10779(15) 0.6197(2) 0.23241(15) 0.0212(6) Uani 1 1 d . . .
O3 O 0.03399(16) 0.6098(2) 0.35099(14) 0.0210(6) Uani 1 1 d . . .
O4 O 0.05340(15) 0.8382(2) 0.34741(14) 0.0216(6) Uani 1 1 d . . .


_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 1.258(4) . ?
C1 O1 1.266(4) . ?
C1 C2 1.483(5) . ?
C2 C3 1.388(5) . ?
C2 C7 1.394(5) . ?
C3 C4 1.386(5) . ?
C4 C5 1.384(6) . ?
C5 C6 1.380(6) . ?
C6 C7 1.378(5) . ?
C8 O4 1.265(4) . ?
C8 O3 1.265(4) . ?
C8 C9 1.476(5) . ?
C9 C10 1.394(5) . ?
C9 C14 1.397(5) . ?
C10 C11 1.370(6) . ?
C11 C12 1.386(6) . ?
C12 C13 1.375(7) . ?
C13 C14 1.379(6) . ?
C15 N1 1.326(4) . ?
C15 C16 1.389(5) . ?
C16 N2 1.332(4) . ?
Cu1 O1 1.944(2) . ?
Cu1 O1 1.944(2) 2 ?
Cu1 O4 1.979(3) 2 ?
Cu1 O4 1.979(3) . ?
Cu1 N2 2.164(4) 1_565 ?
Cu1 Cu2 2.5895(9) . ?
Cu2 O3 1.949(3) 2 ?
Cu2 O3 1.949(3) . ?
Cu2 O2 1.977(3) . ?
Cu2 O2 1.977(3) 2 ?
Cu2 N1 2.155(4) . ?
N1 C15 1.326(4) 2 ?
N2 C16 1.332(4) 2 ?
N2 Cu1 2.164(4) 1_545 ?

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 124.9(3) . . ?
O2 C1 C2 117.9(3) . . ?
O1 C1 C2 117.2(3) . . ?
C3 C2 C7 118.9(4) . . ?
C3 C2 C1 120.6(3) . . ?
C7 C2 C1 120.5(3) . . ?
C4 C3 C2 120.6(3) . . ?
C5 C4 C3 119.6(4) . . ?
C6 C5 C4 120.3(4) . . ?
C7 C6 C5 120.0(3) . . ?
C6 C7 C2 120.5(4) . . ?
O4 C8 O3 124.8(4) . . ?
O4 C8 C9 118.2(3) . . ?
O3 C8 C9 117.0(3) . . ?
C10 C9 C14 118.0(4) . . ?
C10 C9 C8 121.0(3) . . ?
C14 C9 C8 121.0(3) . . ?
C11 C10 C9 121.1(4) . . ?
C10 C11 C12 120.1(4) . . ?
C13 C12 C11 119.7(4) . . ?
C12 C13 C14 120.3(4) . . ?
C13 C14 C9 120.7(4) . . ?
N1 C15 C16 121.6(3) . . ?
N2 C16 C15 121.5(3) . . ?
O1 Cu1 O1 171.78(14) . 2 ?
O1 Cu1 O4 89.84(11) . 2 ?
O1 Cu1 O4 89.18(11) 2 2 ?
O1 Cu1 O4 89.18(11) . . ?
O1 Cu1 O4 89.84(11) 2 . ?
O4 Cu1 O4 166.29(14) 2 . ?
O1 Cu1 N2 94.11(7) . 1_565 ?
O1 Cu1 N2 94.11(7) 2 1_565 ?
O4 Cu1 N2 96.85(7) 2 1_565 ?
O4 Cu1 N2 96.85(7) . 1_565 ?
O1 Cu1 Cu2 85.89(7) . . ?
O1 Cu1 Cu2 85.89(7) 2 . ?
O4 Cu1 Cu2 83.15(7) 2 . ?
O4 Cu1 Cu2 83.15(7) . . ?
N2 Cu1 Cu2 180.000(1) 1_565 . ?
O3 Cu2 O3 171.75(14) 2 . ?
O3 Cu2 O2 88.88(11) 2 . ?
O3 Cu2 O2 90.14(11) . . ?
O3 Cu2 O2 90.14(11) 2 2 ?
O3 Cu2 O2 88.88(11) . 2 ?
O2 Cu2 O2 166.29(14) . 2 ?
O3 Cu2 N1 94.13(7) 2 . ?
O3 Cu2 N1 94.13(7) . . ?
O2 Cu2 N1 96.86(7) . . ?
O2 Cu2 N1 96.86(7) 2 . ?
O3 Cu2 Cu1 85.87(7) 2 . ?
O3 Cu2 Cu1 85.87(7) . . ?
O2 Cu2 Cu1 83.14(7) . . ?
O2 Cu2 Cu1 83.14(7) 2 . ?
N1 Cu2 Cu1 180.0 . . ?
C15 N1 C15 117.1(4) . 2 ?
C15 N1 Cu2 121.5(2) . . ?
C15 N1 Cu2 121.5(2) 2 . ?
C16 N2 C16 116.8(4) . 2 ?
C16 N2 Cu1 121.6(2) . 1_545 ?
C16 N2 Cu1 121.6(2) 2 1_545 ?
C1 O1 Cu1 121.4(2) . . ?
C1 O2 Cu2 122.8(2) . . ?
C8 O3 Cu2 121.0(2) . . ?
C8 O4 Cu1 123.0(2) . . ?

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 175.4(4) . . . . ?
O1 C1 C2 C3 -2.6(6) . . . . ?
O2 C1 C2 C7 -2.8(6) . . . . ?
O1 C1 C2 C7 179.2(4) . . . . ?
C7 C2 C3 C4 2.8(6) . . . . ?
C1 C2 C3 C4 -175.3(4) . . . . ?
C2 C3 C4 C5 0.0(7) . . . . ?
C3 C4 C5 C6 -2.5(7) . . . . ?
C4 C5 C6 C7 2.0(7) . . . . ?
C5 C6 C7 C2 1.0(6) . . . . ?
C3 C2 C7 C6 -3.4(6) . . . . ?
C1 C2 C7 C6 174.8(4) . . . . ?
O4 C8 C9 C10 174.8(3) . . . . ?
O3 C8 C9 C10 -6.5(5) . . . . ?
O4 C8 C9 C14 -8.0(5) . . . . ?
O3 C8 C9 C14 170.7(4) . . . . ?
C14 C9 C10 C11 -0.6(6) . . . . ?
C8 C9 C10 C11 176.7(4) . . . . ?
C9 C10 C11 C12 -0.9(6) . . . . ?
C10 C11 C12 C13 1.6(7) . . . . ?
C11 C12 C13 C14 -1.0(7) . . . . ?
C12 C13 C14 C9 -0.5(7) . . . . ?
C10 C9 C14 C13 1.3(6) . . . . ?
C8 C9 C14 C13 -176.0(4) . . . . ?
N1 C15 C16 N2 0.3(5) . . . . ?
O1 Cu1 Cu2 O3 -79.90(11) . . . 2 ?
O1 Cu1 Cu2 O3 100.10(11) 2 . . 2 ?
O4 Cu1 Cu2 O3 10.43(10) 2 . . 2 ?
O4 Cu1 Cu2 O3 -169.57(10) . . . 2 ?
N2 Cu1 Cu2 O3 165(66) 1_565 . . 2 ?
O1 Cu1 Cu2 O3 100.10(11) . . . . ?
O1 Cu1 Cu2 O3 -79.90(11) 2 . . . ?
O4 Cu1 Cu2 O3 -169.57(10) 2 . . . ?
O4 Cu1 Cu2 O3 10.43(10) . . . . ?
N2 Cu1 Cu2 O3 -15(27) 1_565 . . . ?
O1 Cu1 Cu2 O2 9.46(11) . . . . ?
O1 Cu1 Cu2 O2 -170.54(11) 2 . . . ?
O4 Cu1 Cu2 O2 99.79(11) 2 . . . ?
O4 Cu1 Cu2 O2 -80.21(11) . . . . ?
N2 Cu1 Cu2 O2 -106(71) 1_565 . . . ?
O1 Cu1 Cu2 O2 -170.54(11) . . . 2 ?
O1 Cu1 Cu2 O2 9.46(11) 2 . . 2 ?
O4 Cu1 Cu2 O2 -80.21(11) 2 . . 2 ?
O4 Cu1 Cu2 O2 99.79(11) . . . 2 ?
N2 Cu1 Cu2 O2 74(27) 1_565 . . 2 ?
O1 Cu1 Cu2 N1 -161(100) . . . . ?
O1 Cu1 Cu2 N1 19(100) 2 . . . ?
O4 Cu1 Cu2 N1 -70(100) 2 . . . ?
O4 Cu1 Cu2 N1 110(100) . . . . ?
N2 Cu1 Cu2 N1 0(41) 1_565 . . . ?
C16 C15 N1 C15 -0.2(2) . . . 2 ?
C16 C15 N1 Cu2 179.8(2) . . . . ?
O3 Cu2 N1 C15 53.0(2) 2 . . . ?
O3 Cu2 N1 C15 -127.0(2) . . . . ?
O2 Cu2 N1 C15 -36.4(2) . . . . ?
O2 Cu2 N1 C15 143.6(2) 2 . . . ?
Cu1 Cu2 N1 C15 134(100) . . . . ?
O3 Cu2 N1 C15 -127.0(2) 2 . . 2 ?
O3 Cu2 N1 C15 53.0(2) . . . 2 ?
O2 Cu2 N1 C15 143.6(2) . . . 2 ?
O2 Cu2 N1 C15 -36.4(2) 2 . . 2 ?
Cu1 Cu2 N1 C15 -46(100) . . . 2 ?
C15 C16 N2 C16 -0.2(2) . . . 2 ?
C15 C16 N2 Cu1 179.8(2) . . . 1_545 ?
O2 C1 O1 Cu1 3.0(5) . . . . ?
C2 C1 O1 Cu1 -179.2(2) . . . . ?
O1 Cu1 O1 C1 -9.7(3) 2 . . . ?
O4 Cu1 O1 C1 -92.8(3) 2 . . . ?
O4 Cu1 O1 C1 73.5(3) . . . . ?
N2 Cu1 O1 C1 170.3(3) 1_565 . . . ?
Cu2 Cu1 O1 C1 -9.7(3) . . . . ?
O1 C1 O2 Cu2 10.0(5) . . . . ?
C2 C1 O2 Cu2 -167.8(2) . . . . ?
O3 Cu2 O2 C1 73.1(3) 2 . . . ?
O3 Cu2 O2 C1 -98.7(3) . . . . ?
O2 Cu2 O2 C1 -12.9(3) 2 . . . ?
N1 Cu2 O2 C1 167.1(3) . . . . ?
Cu1 Cu2 O2 C1 -12.9(3) . . . . ?
O4 C8 O3 Cu2 11.3(5) . . . . ?
C9 C8 O3 Cu2 -167.3(2) . . . . ?
O3 Cu2 O3 C8 -14.4(3) 2 . . . ?
O2 Cu2 O3 C8 68.7(3) . . . . ?
O2 Cu2 O3 C8 -97.6(3) 2 . . . ?
N1 Cu2 O3 C8 165.6(3) . . . . ?
Cu1 Cu2 O3 C8 -14.4(3) . . . . ?
O3 C8 O4 Cu1 2.8(5) . . . . ?
C9 C8 O4 Cu1 -178.6(2) . . . . ?
O1 Cu1 O4 C8 -96.3(3) . . . . ?
O1 Cu1 O4 C8 75.5(3) 2 . . . ?
O4 Cu1 O4 C8 -10.4(3) 2 . . . ?
N2 Cu1 O4 C8 169.6(3) 1_565 . . . ?
Cu2 Cu1 O4 C8 -10.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.035
_refine_diff_density_min         -1.702
_refine_diff_density_rms         0.135

