# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Feng Luo'
_publ_contact_author_address     
;
nankai university
Tianjin
300071
CHINA
;

_publ_contact_author_email       'LUOFENG 123456@MAIL.NANKAI.EDU.CN'

_publ_section_title              
;
Unprecedented (3, 4)-connected Metal-organic
Frameworks (MOFs) with 3-fold Interpenetration and Considerable
Solvent-accessible Void Space
;
loop_
_publ_author_name
'Feng Luo'
'S. Batten'
'Jimin Zheng'

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 641708'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H48 Cu3 N12 O23'
_chemical_formula_weight         1639.84

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           Rhombohedral
_symmetry_space_group_name_H-M   R-3

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

_cell_length_a                   18.604(3)
_cell_length_b                   18.604(3)
_cell_length_c                   19.756(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5921.7(17)
_cell_formula_units_Z            3
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    13310
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.50

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2505
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9265
_exptl_absorpt_correction_T_max  0.9631
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'rigaku r-axis rapid IP area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18919
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3010
_reflns_number_gt                2311
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAXIS-RAPID Auto(Rigaku, 2004)'
_computing_cell_refinement       'RAXIS-RAPID Auto(Rigaku, 2004)'
_computing_data_reduction        'CrystalStructure(Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.1119P)^2^+4.9780P] 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    refu
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3010
_refine_ls_number_parameters     193
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1745
_refine_ls_wR_factor_gt          0.1616
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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
C1 C 0.4004(2) 0.55666(19) 0.00059(16) 0.0299(7) Uani 1 1 d . . .
C2 C 0.36564(19) 0.61358(18) -0.00279(17) 0.0285(6) Uani 1 1 d . . .
C3 C 0.28033(19) 0.58118(19) -0.00290(17) 0.0307(7) Uani 1 1 d . . .
H3 H 0.2448 0.5240 -0.0031 0.037 Uiso 1 1 calc R . .
C4 C 0.5238(3) 0.5482(3) 0.1440(2) 0.0616(13) Uani 1 1 d . . .
H4 H 0.5556 0.6013 0.1262 0.074 Uiso 1 1 calc R . .
C5 C 0.5158(3) 0.5393(3) 0.2134(2) 0.0681(15) Uani 1 1 d . . .
H5 H 0.5415 0.5857 0.2413 0.097(19) Uiso 1 1 calc R . .
C6 C 0.4699(2) 0.4619(2) 0.24086(18) 0.0407(8) Uani 1 1 d . . .
C7 C 0.4337(3) 0.3965(3) 0.19655(19) 0.0548(11) Uani 1 1 d . . .
H7 H 0.4019 0.3427 0.2129 0.078(16) Uiso 1 1 calc R . .
C8 C 0.4444(3) 0.4104(2) 0.12816(19) 0.0514(10) Uani 1 1 d . . .
H8 H 0.4194 0.3652 0.0989 0.079(16) Uiso 1 1 calc R . .
C9 C 0.4559(3) 0.4418(2) 0.31541(18) 0.0474(9) Uani 1 1 d . . .
C10 C 0.4949(2) 0.5002(2) 0.42956(19) 0.0380(8) Uani 1 1 d . . .
C11 C 0.5091(3) 0.5687(2) 0.46648(19) 0.0483(9) Uani 1 1 d . . .
H11 H 0.5154 0.6156 0.4442 0.079(16) Uiso 1 1 calc R . .
C12 C 0.4858(3) 0.4310(3) 0.46379(19) 0.0488(10) Uani 1 1 d . . .
H12 H 0.4762 0.3842 0.4396 0.080(16) Uiso 1 1 calc R . .
Cu1 Cu 0.5000 0.5000 0.0000 0.0270(2) Uani 1 2 d S . .
H2 H 0.514(4) 0.559(3) 0.341(3) 0.09(2) Uiso 1 1 d D . .
N1 N 0.48894(18) 0.48584(17) 0.10218(15) 0.0337(6) Uani 1 1 d . . .
N2 N 0.4944(2) 0.5059(2) 0.35835(17) 0.0437(8) Uani 1 1 d D . .
O1 O 0.35405(15) 0.48028(14) -0.00062(13) 0.0388(6) Uani 1 1 d . . .
O2 O 0.47928(13) 0.59172(14) 0.00489(11) 0.0322(5) Uani 1 1 d . . .
O3 O 0.4114(3) 0.3702(2) 0.33325(16) 0.0926(15) Uani 1 1 d . . .
O4 O 0.3333 0.6667 0.1667 0.188(9) Uani 1 6 d S A 1
O5 O 0.3333 0.6667 0.8022(18) 0.204(13) Uani 0.50 3 d SP B 1
O4' O 0.316(3) 0.745(2) 0.1664(7) 0.153(9) Uani 0.33 1 d P . 2
O5' O 0.3614(15) 0.7526(14) 0.8038(16) 0.095(9) Uani 0.17 1 d P C 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
C1 0.0335(16) 0.0334(16) 0.0270(15) -0.0029(12) -0.0024(12) 0.0199(14)
C2 0.0299(15) 0.0279(15) 0.0309(16) -0.0009(12) -0.0011(12) 0.0169(13)
C3 0.0292(15) 0.0256(15) 0.0359(17) -0.0003(12) -0.0001(12) 0.0125(12)
C4 0.099(4) 0.038(2) 0.0284(19) 0.0022(16) -0.003(2) 0.020(2)
C5 0.112(4) 0.040(2) 0.028(2) -0.0020(17) -0.002(2) 0.020(2)
C6 0.048(2) 0.0420(19) 0.0280(16) 0.0005(15) -0.0022(15) 0.0198(17)
C7 0.074(3) 0.037(2) 0.0328(19) 0.0011(16) 0.0028(19) 0.0123(19)
C8 0.070(3) 0.038(2) 0.0299(18) -0.0051(15) 0.0002(18) 0.0147(19)
C9 0.061(2) 0.045(2) 0.0266(17) 0.0027(15) -0.0030(16) 0.0198(19)
C10 0.0401(18) 0.048(2) 0.0230(16) 0.0049(14) -0.0016(13) 0.0196(15)
C11 0.068(3) 0.046(2) 0.0292(18) 0.0038(16) -0.0060(17) 0.028(2)
C12 0.072(3) 0.046(2) 0.0282(18) -0.0013(15) -0.0048(17) 0.030(2)
Cu1 0.0337(3) 0.0333(3) 0.0213(3) -0.00091(19) -0.00068(19) 0.0222(2)
N1 0.0447(16) 0.0392(15) 0.0222(13) 0.0012(11) 0.0008(11) 0.0248(13)
N2 0.0550(19) 0.0443(18) 0.0238(15) 0.0041(12) -0.0010(12) 0.0187(15)
O1 0.0390(13) 0.0291(12) 0.0504(15) -0.0041(10) -0.0064(11) 0.0186(10)
O2 0.0314(12) 0.0342(12) 0.0362(12) 0.0000(9) 0.0000(9) 0.0203(10)
O3 0.144(4) 0.0457(19) 0.0348(16) 0.0055(14) -0.0031(19) 0.007(2)
O4 0.262(14) 0.262(14) 0.041(7) 0.000 0.000 0.131(7)
O5 0.192(18) 0.192(18) 0.23(4) 0.000 0.000 0.096(9)
O4' 0.24(2) 0.24(4) 0.030(5) -0.004(9) -0.003(7) 0.16(3)
O5' 0.096(17) 0.063(14) 0.14(3) -0.011(14) 0.023(16) 0.052(13)

_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 1.240(4) . ?
C1 O2 1.276(4) . ?
C1 C2 1.493(4) . ?
C1 Cu1 2.549(3) . ?
C2 C3 1.388(4) . ?
C2 C3 1.392(4) 2_665 ?
C3 C2 1.392(4) 3_565 ?
C3 H3 0.9300 . ?
C4 N1 1.302(5) . ?
C4 C5 1.381(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.367(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.371(5) . ?
C6 C9 1.510(5) . ?
C7 C8 1.371(5) . ?
C7 H7 0.9300 . ?
C8 N1 1.325(5) . ?
C8 H8 0.9300 . ?
C9 O3 1.217(5) . ?
C9 N2 1.341(5) . ?
C10 C11 1.376(5) . ?
C10 C12 1.386(5) . ?
C10 N2 1.411(5) . ?
C11 C12 1.381(5) 10_666 ?
C11 H11 0.9300 . ?
C12 C11 1.381(5) 10_666 ?
C12 H12 0.9300 . ?
Cu1 O2 1.931(2) . ?
Cu1 O2 1.931(2) 10_665 ?
Cu1 N1 2.033(3) 10_665 ?
Cu1 N1 2.033(3) . ?
Cu1 C1 2.549(3) 10_665 ?
N2 H2 0.93(5) . ?
O4' O4' 1.65(2) 14_455 ?
O4' O4' 1.65(2) 15 ?

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 O2 123.3(3) . . ?
O1 C1 C2 120.8(3) . . ?
O2 C1 C2 115.8(3) . . ?
O1 C1 Cu1 76.03(18) . . ?
O2 C1 Cu1 47.45(14) . . ?
C2 C1 Cu1 162.8(2) . . ?
C3 C2 C3 120.1(3) . 2_665 ?
C3 C2 C1 119.9(3) . . ?
C3 C2 C1 119.9(3) 2_665 . ?
C2 C3 C2 119.9(3) . 3_565 ?
C2 C3 H3 120.0 . . ?
C2 C3 H3 120.0 3_565 . ?
N1 C4 C5 123.2(4) . . ?
N1 C4 H4 118.4 . . ?
C5 C4 H4 118.4 . . ?
C6 C5 C4 119.5(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 116.9(4) . . ?
C5 C6 C9 126.0(3) . . ?
C7 C6 C9 117.1(3) . . ?
C6 C7 C8 120.1(4) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
N1 C8 C7 122.4(3) . . ?
N1 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
O3 C9 N2 123.9(3) . . ?
O3 C9 C6 119.5(3) . . ?
N2 C9 C6 116.6(3) . . ?
C11 C10 C12 118.6(4) . . ?
C11 C10 N2 117.7(3) . . ?
C12 C10 N2 123.6(3) . . ?
C10 C11 C12 120.9(4) . 10_666 ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 10_666 . ?
C11 C12 C10 120.5(4) 10_666 . ?
C11 C12 H12 119.7 10_666 . ?
C10 C12 H12 119.7 . . ?
O2 Cu1 O2 180.0 . 10_665 ?
O2 Cu1 N1 89.26(10) . 10_665 ?
O2 Cu1 N1 90.74(10) 10_665 10_665 ?
O2 Cu1 N1 90.74(10) . . ?
O2 Cu1 N1 89.26(10) 10_665 . ?
N1 Cu1 N1 180.00(18) 10_665 . ?
O2 Cu1 C1 29.15(10) . . ?
O2 Cu1 C1 150.85(10) 10_665 . ?
N1 Cu1 C1 89.90(10) 10_665 . ?
N1 Cu1 C1 90.10(10) . . ?
O2 Cu1 C1 150.85(10) . 10_665 ?
O2 Cu1 C1 29.15(10) 10_665 10_665 ?
N1 Cu1 C1 90.10(10) 10_665 10_665 ?
N1 Cu1 C1 89.90(10) . 10_665 ?
C1 Cu1 C1 180.0 . 10_665 ?
C4 N1 C8 117.8(3) . . ?
C4 N1 Cu1 122.7(3) . . ?
C8 N1 Cu1 119.4(2) . . ?
C9 N2 C10 125.8(3) . . ?
C9 N2 H2 117(4) . . ?
C10 N2 H2 116(4) . . ?
C1 O2 Cu1 103.40(19) . . ?
O4' O4' O4' 120.00(3) 14_455 15 ?

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 4.2(5) . . . . ?
O2 C1 C2 C3 -175.6(3) . . . . ?
Cu1 C1 C2 C3 172.1(6) . . . . ?
O1 C1 C2 C3 -178.5(3) . . . 2_665 ?
O2 C1 C2 C3 1.6(5) . . . 2_665 ?
Cu1 C1 C2 C3 -10.6(10) . . . 2_665 ?
C3 C2 C3 C2 -0.3(7) 2_665 . . 3_565 ?
C1 C2 C3 C2 176.9(2) . . . 3_565 ?
N1 C4 C5 C6 0.5(9) . . . . ?
C4 C5 C6 C7 -0.1(7) . . . . ?
C4 C5 C6 C9 179.4(5) . . . . ?
C5 C6 C7 C8 0.0(7) . . . . ?
C9 C6 C7 C8 -179.6(4) . . . . ?
C6 C7 C8 N1 -0.1(7) . . . . ?
C5 C6 C9 O3 177.7(5) . . . . ?
C7 C6 C9 O3 -2.7(7) . . . . ?
C5 C6 C9 N2 -2.2(7) . . . . ?
C7 C6 C9 N2 177.3(4) . . . . ?
C12 C10 C11 C12 0.0(7) . . . 10_666 ?
N2 C10 C11 C12 -177.1(4) . . . 10_666 ?
C11 C10 C12 C11 0.0(7) . . . 10_666 ?
N2 C10 C12 C11 176.9(4) . . . 10_666 ?
O1 C1 Cu1 O2 -175.7(3) . . . . ?
C2 C1 Cu1 O2 15.0(7) . . . . ?
O1 C1 Cu1 O2 4.3(3) . . . 10_665 ?
O2 C1 Cu1 O2 180.0 . . . 10_665 ?
C2 C1 Cu1 O2 -165.0(7) . . . 10_665 ?
O1 C1 Cu1 N1 95.7(2) . . . 10_665 ?
O2 C1 Cu1 N1 -88.7(2) . . . 10_665 ?
C2 C1 Cu1 N1 -73.7(8) . . . 10_665 ?
O1 C1 Cu1 N1 -84.3(2) . . . . ?
O2 C1 Cu1 N1 91.3(2) . . . . ?
C2 C1 Cu1 N1 106.3(8) . . . . ?
O1 C1 Cu1 C1 -91(58) . . . 10_665 ?
O2 C1 Cu1 C1 85(58) . . . 10_665 ?
C2 C1 Cu1 C1 100(58) . . . 10_665 ?
C5 C4 N1 C8 -0.6(7) . . . . ?
C5 C4 N1 Cu1 179.2(4) . . . . ?
C7 C8 N1 C4 0.4(7) . . . . ?
C7 C8 N1 Cu1 -179.4(4) . . . . ?
O2 Cu1 N1 C4 -44.9(4) . . . . ?
O2 Cu1 N1 C4 135.1(4) 10_665 . . . ?
N1 Cu1 N1 C4 -74(100) 10_665 . . . ?
C1 Cu1 N1 C4 -74.1(4) . . . . ?
C1 Cu1 N1 C4 105.9(4) 10_665 . . . ?
O2 Cu1 N1 C8 134.9(3) . . . . ?
O2 Cu1 N1 C8 -45.1(3) 10_665 . . . ?
N1 Cu1 N1 C8 106(100) 10_665 . . . ?
C1 Cu1 N1 C8 105.7(3) . . . . ?
C1 Cu1 N1 C8 -74.3(3) 10_665 . . . ?
O3 C9 N2 C10 5.2(7) . . . . ?
C6 C9 N2 C10 -174.9(3) . . . . ?
C11 C10 N2 C9 -156.2(4) . . . . ?
C12 C10 N2 C9 26.9(6) . . . . ?
O1 C1 O2 Cu1 5.1(4) . . . . ?
C2 C1 O2 Cu1 -175.1(2) . . . . ?
O2 Cu1 O2 C1 -89(58) 10_665 . . . ?
N1 Cu1 O2 C1 91.1(2) 10_665 . . . ?
N1 Cu1 O2 C1 -88.9(2) . . . . ?
C1 Cu1 O2 C1 180.0 10_665 . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.097

# Attachment '1a.cif'

data_070312am
_database_code_depnum_ccdc_archive 'CCDC 641751'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H16 Cu N4 O6'
_chemical_formula_weight         519.95

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           Rhombohedral
_symmetry_space_group_name_H-M   R-3

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

_cell_length_a                   18.5943(16)
_cell_length_b                   18.5943(16)
_cell_length_c                   19.761(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5916.9(12)
_cell_formula_units_Z            9
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    11240
_cell_measurement_theta_min      1.63
_cell_measurement_theta_max      26.39

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      NONE
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2385
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9256
_exptl_absorpt_correction_T_max  0.9659
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'rigaku r-axis rapid IP area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11240
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         26.39
_reflns_number_total             2717
_reflns_number_gt                1753
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAXIS-RAPID Auto(Rigaku, 2004)'
_computing_cell_refinement       'RAXIS-RAPID Auto(Rigaku, 2004)'
_computing_data_reduction        'CrystalStructure(Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.1105P)^2^+7.4660P] 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    refu
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2717
_refine_ls_number_parameters     165
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.2007
_refine_ls_wR_factor_gt          0.1714
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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 0.5558(3) 0.1560(3) 0.9927(2) 0.0304(11) Uani 1 1 d . . .
C2 C 0.6134(3) 0.2480(3) 0.9913(3) 0.0360(12) Uani 1 1 d . . .
C3 C 0.6990(3) 0.2804(3) 0.9912(3) 0.0363(12) Uani 1 1 d . . .
H3 H 0.7206 0.2448 0.9909 0.044 Uiso 1 1 calc R . .
C8 C 0.4089(3) -0.0395(4) 0.8721(3) 0.0503(15) Uani 1 1 d . . .
H8 H 0.3635 -0.0611 0.9011 0.060 Uiso 1 1 calc R . .
C7 C 0.3952(3) -0.0423(4) 0.8042(3) 0.0557(17) Uani 1 1 d . . .
H7 H 0.3412 -0.0645 0.7881 0.067 Uiso 1 1 calc R . .
C4 C 0.5477(3) 0.0222(4) 0.8557(3) 0.0551(17) Uani 1 1 d . . .
H4 H 0.6010 0.0450 0.8734 0.066 Uiso 1 1 calc R . .
C5 C 0.5389(4) 0.0208(4) 0.7864(3) 0.0590(19) Uani 1 1 d . . .
H5 H 0.5852 0.0421 0.7584 0.071 Uiso 1 1 calc R . .
C6 C 0.4602(3) -0.0126(3) 0.7592(2) 0.0376(12) Uani 1 1 d . . .
C9 C 0.4405(4) -0.0179(4) 0.6844(2) 0.0460(14) Uani 1 1 d . . .
C10 C 0.4998(3) 0.0041(3) 0.5707(2) 0.0363(12) Uani 1 1 d . . .
C11 C 0.5677(3) 0.0597(4) 0.5341(3) 0.0465(14) Uani 1 1 d . . .
H11 H 0.6139 0.1005 0.5569 0.056 Uiso 1 1 calc R . .
C12 C 0.5691(3) 0.0567(4) 0.4637(2) 0.0461(14) Uani 1 1 d . . .
H12 H 0.6159 0.0950 0.4399 0.055 Uiso 1 1 calc R . .
Cu1 Cu 0.5000 0.0000 1.0000 0.0263(3) Uani 1 2 d S . .
H2 H 0.558(4) 0.041(4) 0.657(3) 0.054(18) Uiso 1 1 d . . .
N1 N 0.4843(2) -0.0073(2) 0.89861(19) 0.0316(10) Uani 1 1 d . . .
N2 N 0.5044(3) 0.0096(3) 0.6419(2) 0.0425(12) Uani 1 1 d . . .
O1 O 0.5915(2) 0.11200(19) 0.99152(16) 0.0317(8) Uani 1 1 d . . .
O2 O 0.4795(2) 0.1260(2) 0.99553(18) 0.0395(9) Uani 1 1 d . . .
O3 O 0.3686(3) -0.0469(4) 0.6668(2) 0.097(2) Uani 1 1 d . . .

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 0.036(3) 0.025(2) 0.028(2) -0.0005(19) 0.002(2) 0.014(2)
C2 0.029(3) 0.025(3) 0.052(3) 0.002(2) 0.003(2) 0.012(2)
C3 0.030(3) 0.029(3) 0.053(3) 0.002(2) 0.001(2) 0.017(2)
C8 0.030(3) 0.077(4) 0.029(3) 0.004(3) 0.004(2) 0.015(3)
C7 0.031(3) 0.093(5) 0.030(3) 0.000(3) -0.005(2) 0.021(3)
C4 0.030(3) 0.088(5) 0.030(3) -0.001(3) -0.002(2) 0.016(3)
C5 0.034(3) 0.102(5) 0.020(3) 0.003(3) 0.006(2) 0.017(3)
C6 0.039(3) 0.049(3) 0.023(2) -0.002(2) -0.001(2) 0.021(3)
C9 0.043(3) 0.067(4) 0.025(3) -0.004(3) -0.005(2) 0.026(3)
C10 0.044(3) 0.050(3) 0.020(2) -0.004(2) -0.005(2) 0.027(3)
C11 0.044(3) 0.056(4) 0.029(3) -0.010(3) -0.007(2) 0.017(3)
C12 0.045(3) 0.054(3) 0.024(2) -0.003(2) 0.003(2) 0.013(3)
Cu1 0.0334(5) 0.0226(5) 0.0192(4) 0.0007(3) 0.0011(3) 0.0113(4)
N1 0.038(2) 0.034(2) 0.019(2) 0.0006(16) 0.0021(17) 0.0157(19)
N2 0.039(3) 0.064(3) 0.022(2) -0.005(2) -0.004(2) 0.024(2)
O1 0.0348(19) 0.0241(17) 0.0345(17) 0.0014(14) 0.0014(14) 0.0133(15)
O2 0.0271(19) 0.0315(19) 0.055(2) -0.0011(16) 0.0042(16) 0.0110(15)
O3 0.043(3) 0.184(6) 0.031(2) -0.010(3) -0.0043(19) 0.033(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
C1 O2 1.239(6) . ?
C1 O1 1.287(5) . ?
C1 C2 1.497(7) . ?
C2 C3 1.384(7) 3_665 ?
C2 C3 1.392(6) . ?
C3 C2 1.384(7) 2_655 ?
C3 H3 0.9300 . ?
C8 N1 1.326(6) . ?
C8 C7 1.363(7) . ?
C8 H8 0.9300 . ?
C7 C6 1.374(7) . ?
C7 H7 0.9300 . ?
C4 N1 1.328(7) . ?
C4 C5 1.378(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(8) . ?
C5 H5 0.9300 . ?
C6 C9 1.515(7) . ?
C9 O3 1.216(7) . ?
C9 N2 1.330(7) . ?
C10 C11 1.371(7) . ?
C10 C12 1.390(7) 10_656 ?
C10 N2 1.411(6) . ?
C11 C12 1.393(7) . ?
C11 H11 0.9300 . ?
C12 C10 1.390(7) 10_656 ?
C12 H12 0.9300 . ?
Cu1 O1 1.928(3) . ?
Cu1 O1 1.928(3) 10_657 ?
Cu1 N1 2.019(4) . ?
Cu1 N1 2.019(4) 10_657 ?
N2 H2 0.92(6) . ?

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 123.6(4) . . ?
O2 C1 C2 121.3(4) . . ?
O1 C1 C2 115.1(4) . . ?
C3 C2 C3 120.0(5) 3_665 . ?
C3 C2 C1 119.7(4) 3_665 . ?
C3 C2 C1 120.3(4) . . ?
C2 C3 C2 120.0(5) 2_655 . ?
C2 C3 H3 120.0 2_655 . ?
C2 C3 H3 120.0 . . ?
N1 C8 C7 122.8(5) . . ?
N1 C8 H8 118.6 . . ?
C7 C8 H8 118.6 . . ?
C8 C7 C6 120.8(5) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
N1 C4 C5 123.6(5) . . ?
N1 C4 H4 118.2 . . ?
C5 C4 H4 118.2 . . ?
C4 C5 C6 119.0(5) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C7 C6 C5 116.7(5) . . ?
C7 C6 C9 118.0(5) . . ?
C5 C6 C9 125.2(5) . . ?
O3 C9 N2 124.2(5) . . ?
O3 C9 C6 119.0(5) . . ?
N2 C9 C6 116.8(5) . . ?
C11 C10 C12 118.9(5) . 10_656 ?
C11 C10 N2 118.1(5) . . ?
C12 C10 N2 123.0(5) 10_656 . ?
C10 C11 C12 121.6(5) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C10 C12 C11 119.5(5) 10_656 . ?
C10 C12 H12 120.3 10_656 . ?
C11 C12 H12 120.3 . . ?
O1 Cu1 O1 180.000(1) . 10_657 ?
O1 Cu1 N1 90.36(14) . . ?
O1 Cu1 N1 89.64(14) 10_657 . ?
O1 Cu1 N1 89.64(14) . 10_657 ?
O1 Cu1 N1 90.36(14) 10_657 10_657 ?
N1 Cu1 N1 180.000(1) . 10_657 ?
C8 N1 C4 117.0(4) . . ?
C8 N1 Cu1 120.4(3) . . ?
C4 N1 Cu1 122.5(3) . . ?
C9 N2 C10 126.3(5) . . ?
C9 N2 H2 121(4) . . ?
C10 N2 H2 112(4) . . ?
C1 O1 Cu1 103.2(3) . . ?

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 -1.9(8) . . . 3_665 ?
O1 C1 C2 C3 178.8(5) . . . 3_665 ?
O2 C1 C2 C3 177.2(5) . . . . ?
O1 C1 C2 C3 -2.1(7) . . . . ?
C3 C2 C3 C2 0.5(11) 3_665 . . 2_655 ?
C1 C2 C3 C2 -178.6(3) . . . 2_655 ?
N1 C8 C7 C6 1.3(10) . . . . ?
N1 C4 C5 C6 0.2(10) . . . . ?
C8 C7 C6 C5 -1.0(9) . . . . ?
C8 C7 C6 C9 179.8(6) . . . . ?
C4 C5 C6 C7 0.3(9) . . . . ?
C4 C5 C6 C9 179.4(6) . . . . ?
C7 C6 C9 O3 1.0(9) . . . . ?
C5 C6 C9 O3 -178.1(7) . . . . ?
C7 C6 C9 N2 -178.6(6) . . . . ?
C5 C6 C9 N2 2.4(9) . . . . ?
C12 C10 C11 C12 0.0(10) 10_656 . . . ?
N2 C10 C11 C12 177.8(5) . . . . ?
C10 C11 C12 C10 0.0(10) . . . 10_656 ?
C7 C8 N1 C4 -0.7(9) . . . . ?
C7 C8 N1 Cu1 176.8(5) . . . . ?
C5 C4 N1 C8 0.0(9) . . . . ?
C5 C4 N1 Cu1 -177.4(5) . . . . ?
O1 Cu1 N1 C8 -135.3(4) . . . . ?
O1 Cu1 N1 C8 44.7(4) 10_657 . . . ?
N1 Cu1 N1 C8 -44.4(13) 10_657 . . . ?
O1 Cu1 N1 C4 42.0(4) . . . . ?
O1 Cu1 N1 C4 -138.0(4) 10_657 . . . ?
N1 Cu1 N1 C4 132.9(12) 10_657 . . . ?
O3 C9 N2 C10 -5.3(11) . . . . ?
C6 C9 N2 C10 174.2(5) . . . . ?
C11 C10 N2 C9 156.5(6) . . . . ?
C12 C10 N2 C9 -25.8(8) 10_656 . . . ?
O2 C1 O1 Cu1 -3.0(6) . . . . ?
C2 C1 O1 Cu1 176.3(3) . . . . ?
O1 Cu1 O1 C1 3(7) 10_657 . . . ?
N1 Cu1 O1 C1 87.5(3) . . . . ?
N1 Cu1 O1 C1 -92.5(3) 10_657 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.39
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.416
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.192