# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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data_(R)-MOF-4a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C22 H12 Cu O6), 2(C5 N1 H5), H2 O, 2(C3 H7 N O), H2 O '
_chemical_formula_sum            'C38 H40 Cu N4 O10'
_chemical_formula_weight         776.28

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           trigonal
_symmetry_space_group_name_H-M   'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2" '

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

_cell_length_a                   8.89960(10)
_cell_length_b                   8.89960(10)
_cell_length_c                   39.5773(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2714.68(11)
_cell_formula_units_Z            3
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    17087
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1215
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8780
_exptl_absorpt_correction_T_max  0.8780
_exptl_absorpt_process_details   'NUMBAS; Rigaku, 2005'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            26777
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.51
_reflns_number_total             4148
_reflns_number_gt                3949
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0738P)^2^+2.0276P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_number_reflns         4148
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1453
_refine_ls_wR_factor_gt          0.1377
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.124
_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
C4 C 0.6697(4) 0.2309(4) 0.27020(7) 0.0218(5) Uani 1 1 d . . .
H1 H 0.588(5) 0.196(5) 0.2550(9) 0.022(8) Uiso 1 1 d . . .
C3 C 0.8155(4) 0.2185(4) 0.26491(7) 0.0206(5) Uani 1 1 d . . .
C2 C 0.9471(4) 0.2781(4) 0.29033(7) 0.0205(5) Uani 1 1 d . . .
C1 C 0.9294(4) 0.3485(4) 0.32045(7) 0.0196(5) Uani 1 1 d . . .
C10 C 0.7756(4) 0.3566(4) 0.32618(7) 0.0198(5) Uani 1 1 d . . .
C9 C 0.7450(4) 0.4225(4) 0.35674(8) 0.0276(6) Uani 1 1 d . . .
H5 H 0.834(6) 0.470(6) 0.3746(11) 0.040(11) Uiso 1 1 d . . .
C8 C 0.5951(5) 0.4234(5) 0.36172(8) 0.0336(7) Uani 1 1 d . . .
H4 H 0.592(7) 0.482(7) 0.3803(13) 0.061(15) Uiso 1 1 d . . .
C7 C 0.4632(4) 0.3618(5) 0.33663(9) 0.0337(8) Uani 1 1 d . . .
H3 H 0.354(6) 0.364(5) 0.3379(11) 0.041(11) Uiso 1 1 d . . .
C6 C 0.4897(4) 0.3023(4) 0.30653(8) 0.0271(6) Uani 1 1 d . . .
H2 H 0.401(5) 0.263(5) 0.2904(9) 0.024(8) Uiso 1 1 d . . .
C5 C 0.6442(4) 0.2977(4) 0.30066(7) 0.0221(6) Uani 1 1 d . . .
C11 C 0.8339(4) 0.1434(4) 0.23223(7) 0.0248(6) Uani 1 1 d . . .
C12 C 0.9673(5) 0.3638(5) 0.15992(8) 0.0345(7) Uani 1 1 d . . .
H6 H 1.0141 0.3334 0.1785 0.041 Uiso 1 1 calc R . .
C13 C 1.0590(5) 0.5326(5) 0.14755(10) 0.0416(9) Uani 1 1 d . . .
H7 H 1.1682 0.6140 0.1569 0.050 Uiso 1 1 calc R . .
C14 C 0.9885(5) 0.5795(5) 0.12144(9) 0.0415(9) Uani 1 1 d . . .
H8 H 1.0457 0.6951 0.1131 0.050 Uiso 1 1 calc R . .
C15 C 0.8316(6) 0.4540(5) 0.10740(10) 0.0435(9) Uani 1 1 d . . .
H9 H 0.7816 0.4818 0.0889 0.052 Uiso 1 1 calc R . .
C16 C 0.7501(5) 0.2884(5) 0.12083(9) 0.0358(7) Uani 1 1 d . . .
H10 H 0.6429 0.2034 0.1113 0.043 Uiso 1 1 calc R . .
C17 C 0.2152(6) 0.0675(6) 0.08081(12) 0.0539(11) Uani 1 1 d . . .
H11 H 0.1485 -0.0185 0.0645 0.065 Uiso 1 1 calc R . .
C18 C 0.0876(9) 0.2391(10) 0.0598(2) 0.110(3) Uani 1 1 d . . .
H12 H 0.0410 0.1588 0.0407 0.165 Uiso 1 1 calc R . .
H13 H 0.1529 0.3585 0.0514 0.165 Uiso 1 1 calc R . .
H14 H -0.0082 0.2260 0.0741 0.165 Uiso 1 1 calc R . .
C19 C 0.3027(11) 0.3376(8) 0.1080(2) 0.113(3) Uani 1 1 d . . .
H15 H 0.2544 0.4141 0.1115 0.169 Uiso 1 1 calc R . .
H16 H 0.4250 0.4070 0.1015 0.169 Uiso 1 1 calc R . .
H17 H 0.2931 0.2749 0.1290 0.169 Uiso 1 1 calc R . .
O1 O 1.0923(3) 0.2677(3) 0.28527(5) 0.0269(5) Uani 1 1 d . . .
H18 H 1.0839 0.2170 0.2669 0.040 Uiso 1 1 calc R . .
O2 O 0.9673(3) 0.1317(3) 0.22695(5) 0.0316(5) Uani 1 1 d . . .
O3 O 0.7102(3) 0.0978(3) 0.21141(5) 0.0301(5) Uani 1 1 d . . .
O4 O 0.2952(4) 0.0274(5) 0.09839(9) 0.0578(8) Uani 1 1 d . . .
O5 O 0.4117(5) 0.0000 0.1667 0.0480(10) Uani 1 2 d S . .
H19 H 0.374(5) 0.006(5) 0.1479(8) 0.015(8) Uiso 1 1 d . . .
O6 O 1.0527(8) 0.0000 0.1667 0.0750(16) Uani 1 2 d S . .
N1 N 0.8165(4) 0.2426(3) 0.14691(6) 0.0276(6) Uani 1 1 d . . .
N2 N 0.1978(6) 0.2020(6) 0.07876(15) 0.0786(16) Uani 1 1 d . . .
Cu1 Cu 0.67573(6) 0.0000 0.1667 0.02583(15) Uani 1 2 d S . .
H20 H 0.9891 -0.0757 0.1522 0.039 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C4 0.0236(14) 0.0218(13) 0.0184(13) -0.0022(10) -0.0047(11) 0.0101(11)
C3 0.0243(14) 0.0178(12) 0.0155(12) 0.0002(10) 0.0020(10) 0.0072(10)
C2 0.0188(13) 0.0208(13) 0.0209(13) 0.0025(10) 0.0023(10) 0.0092(11)
C1 0.0191(13) 0.0220(13) 0.0162(12) -0.0001(10) -0.0030(10) 0.0091(11)
C10 0.0203(13) 0.0228(13) 0.0172(12) -0.0020(10) -0.0024(10) 0.0116(11)
C9 0.0301(16) 0.0377(17) 0.0199(14) -0.0087(12) -0.0058(12) 0.0207(14)
C8 0.0354(17) 0.048(2) 0.0238(15) -0.0121(14) -0.0018(12) 0.0258(15)
C7 0.0289(16) 0.048(2) 0.0331(16) -0.0097(14) -0.0023(12) 0.0255(15)
C6 0.0236(14) 0.0329(15) 0.0284(15) -0.0056(12) -0.0061(12) 0.0169(12)
C5 0.0223(14) 0.0253(14) 0.0195(13) -0.0027(11) -0.0037(11) 0.0126(12)
C11 0.0294(15) 0.0241(14) 0.0173(13) -0.0015(11) 0.0033(11) 0.0107(12)
C12 0.0376(18) 0.0379(19) 0.0236(15) 0.0023(13) -0.0064(13) 0.0154(16)
C13 0.044(2) 0.0359(19) 0.0351(18) 0.0012(14) -0.0054(15) 0.0123(16)
C14 0.054(2) 0.0316(17) 0.0374(19) 0.0082(14) 0.0033(16) 0.0203(16)
C15 0.056(2) 0.0369(19) 0.042(2) 0.0074(15) -0.0085(17) 0.0270(18)
C16 0.0427(19) 0.0355(17) 0.0311(16) -0.0009(13) -0.0088(14) 0.0211(16)
C17 0.041(2) 0.049(2) 0.059(3) 0.0136(19) 0.0033(19) 0.013(2)
C18 0.074(4) 0.079(5) 0.156(7) 0.069(5) -0.001(4) 0.023(4)
C19 0.155(8) 0.047(3) 0.117(6) -0.001(3) 0.064(5) 0.036(4)
O1 0.0235(10) 0.0356(12) 0.0238(10) -0.0045(9) 0.0010(8) 0.0165(9)
O2 0.0375(12) 0.0404(14) 0.0230(10) -0.0031(9) 0.0023(8) 0.0241(11)
O3 0.0325(12) 0.0359(11) 0.0174(9) -0.0067(8) -0.0022(9) 0.0137(10)
O4 0.0537(19) 0.067(2) 0.063(2) -0.0051(17) 0.0013(15) 0.0382(18)
O5 0.0421(16) 0.073(3) 0.039(2) -0.012(2) -0.0059(10) 0.0365(15)
O6 0.093(3) 0.090(4) 0.041(2) -0.021(3) -0.0105(13) 0.045(2)
N1 0.0334(14) 0.0295(13) 0.0230(12) -0.0003(10) -0.0001(10) 0.0180(11)
N2 0.062(3) 0.053(2) 0.136(4) 0.033(3) 0.056(3) 0.040(2)
Cu1 0.0344(2) 0.0256(3) 0.0146(2) -0.00359(17) -0.00179(8) 0.01280(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
C4 C3 1.372(4) . ?
C4 C5 1.412(4) . ?
C4 H1 0.87(4) . ?
C3 C2 1.430(4) . ?
C3 C11 1.502(4) . ?
C2 O1 1.355(3) . ?
C2 C1 1.392(4) . ?
C1 C10 1.425(4) . ?
C1 C1 1.491(5) 5_765 ?
C10 C9 1.428(4) . ?
C10 C5 1.432(4) . ?
C9 C8 1.352(5) . ?
C9 H5 0.98(4) . ?
C8 C7 1.422(5) . ?
C8 H4 0.91(6) . ?
C7 C6 1.371(4) . ?
C7 H3 0.98(4) . ?
C6 C5 1.414(4) . ?
C6 H2 0.93(4) . ?
C11 O2 1.260(4) . ?
C11 O3 1.269(4) . ?
C12 N1 1.335(4) . ?
C12 C13 1.392(5) . ?
C12 H6 0.9500 . ?
C13 C14 1.377(5) . ?
C13 H7 0.9500 . ?
C14 C15 1.395(6) . ?
C14 H8 0.9500 . ?
C15 C16 1.383(5) . ?
C15 H9 0.9500 . ?
C16 N1 1.350(4) . ?
C16 H10 0.9500 . ?
C17 O4 1.171(6) . ?
C17 N2 1.284(6) . ?
C17 H11 0.9500 . ?
C18 N2 1.399(8) . ?
C18 H12 0.9800 . ?
C18 H13 0.9800 . ?
C18 H14 0.9800 . ?
C19 N2 1.594(9) . ?
C19 H15 0.9800 . ?
C19 H16 0.9800 . ?
C19 H17 0.9800 . ?
O1 H18 0.8400 . ?
O3 Cu1 1.9287(19) . ?
O5 Cu1 2.349(4) . ?
O5 H19 0.83(3) . ?
O6 H20 0.8500 . ?
N1 Cu1 2.034(3) . ?
Cu1 O3 1.9288(19) 4 ?
Cu1 N1 2.034(3) 4 ?

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
C3 C4 C5 121.5(3) . . ?
C3 C4 H1 121(2) . . ?
C5 C4 H1 117(2) . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 C11 119.0(3) . . ?
C2 C3 C11 121.3(3) . . ?
O1 C2 C1 118.9(3) . . ?
O1 C2 C3 120.2(3) . . ?
C1 C2 C3 120.9(3) . . ?
C2 C1 C10 119.1(2) . . ?
C2 C1 C1 120.9(3) . 5_765 ?
C10 C1 C1 119.9(3) . 5_765 ?
C1 C10 C9 122.7(3) . . ?
C1 C10 C5 119.9(3) . . ?
C9 C10 C5 117.4(3) . . ?
C8 C9 C10 121.1(3) . . ?
C8 C9 H5 119(3) . . ?
C10 C9 H5 120(3) . . ?
C9 C8 C7 121.5(3) . . ?
C9 C8 H4 116(3) . . ?
C7 C8 H4 122(3) . . ?
C6 C7 C8 119.2(3) . . ?
C6 C7 H3 115(3) . . ?
C8 C7 H3 126(3) . . ?
C7 C6 C5 120.7(3) . . ?
C7 C6 H2 118(2) . . ?
C5 C6 H2 122(2) . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 C10 118.8(3) . . ?
C6 C5 C10 120.1(3) . . ?
O2 C11 O3 124.7(3) . . ?
O2 C11 C3 119.8(3) . . ?
O3 C11 C3 115.6(3) . . ?
N1 C12 C13 123.2(3) . . ?
N1 C12 H6 118.4 . . ?
C13 C12 H6 118.4 . . ?
C14 C13 C12 118.7(4) . . ?
C14 C13 H7 120.6 . . ?
C12 C13 H7 120.6 . . ?
C13 C14 C15 118.8(3) . . ?
C13 C14 H8 120.6 . . ?
C15 C14 H8 120.6 . . ?
C16 C15 C14 118.8(3) . . ?
C16 C15 H9 120.6 . . ?
C14 C15 H9 120.6 . . ?
N1 C16 C15 122.7(3) . . ?
N1 C16 H10 118.6 . . ?
C15 C16 H10 118.6 . . ?
O4 C17 N2 134.1(6) . . ?
O4 C17 H11 112.9 . . ?
N2 C17 H11 112.9 . . ?
N2 C18 H12 109.5 . . ?
N2 C18 H13 109.5 . . ?
H12 C18 H13 109.5 . . ?
N2 C18 H14 109.5 . . ?
H12 C18 H14 109.5 . . ?
H13 C18 H14 109.5 . . ?
N2 C19 H15 109.5 . . ?
N2 C19 H16 109.5 . . ?
H15 C19 H16 109.5 . . ?
N2 C19 H17 109.5 . . ?
H15 C19 H17 109.5 . . ?
H16 C19 H17 109.5 . . ?
C2 O1 H18 109.5 . . ?
C11 O3 Cu1 131.1(2) . . ?
Cu1 O5 H19 116(3) . . ?
C12 N1 C16 117.8(3) . . ?
C12 N1 Cu1 123.1(2) . . ?
C16 N1 Cu1 119.0(2) . . ?
C17 N2 C18 132.8(6) . . ?
C17 N2 C19 111.2(6) . . ?
C18 N2 C19 115.1(6) . . ?
O3 Cu1 O3 172.35(15) . 4 ?
O3 Cu1 N1 90.68(10) . 4 ?
O3 Cu1 N1 89.97(10) 4 4 ?
O3 Cu1 N1 89.97(10) . . ?
O3 Cu1 N1 90.68(10) 4 . ?
N1 Cu1 N1 170.21(16) 4 . ?
O3 Cu1 O5 86.18(8) . . ?
O3 Cu1 O5 86.18(8) 4 . ?
N1 Cu1 O5 94.89(8) 4 . ?
N1 Cu1 O5 94.89(8) . . ?

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
C5 C4 C3 C2 -1.5(5) . . . . ?
C5 C4 C3 C11 178.9(3) . . . . ?
C4 C3 C2 O1 -179.5(3) . . . . ?
C11 C3 C2 O1 0.0(4) . . . . ?
C4 C3 C2 C1 0.1(4) . . . . ?
C11 C3 C2 C1 179.6(3) . . . . ?
O1 C2 C1 C10 -178.8(3) . . . . ?
C3 C2 C1 C10 1.7(4) . . . . ?
O1 C2 C1 C1 2.8(4) . . . 5_765 ?
C3 C2 C1 C1 -176.8(2) . . . 5_765 ?
C2 C1 C10 C9 178.3(3) . . . . ?
C1 C1 C10 C9 -3.2(4) 5_765 . . . ?
C2 C1 C10 C5 -1.9(5) . . . . ?
C1 C1 C10 C5 176.6(2) 5_765 . . . ?
C1 C10 C9 C8 -178.0(3) . . . . ?
C5 C10 C9 C8 2.2(5) . . . . ?
C10 C9 C8 C7 -1.1(6) . . . . ?
C9 C8 C7 C6 -0.9(6) . . . . ?
C8 C7 C6 C5 1.6(5) . . . . ?
C3 C4 C5 C6 -177.0(3) . . . . ?
C3 C4 C5 C10 1.3(5) . . . . ?
C7 C6 C5 C4 177.7(3) . . . . ?
C7 C6 C5 C10 -0.4(5) . . . . ?
C1 C10 C5 C4 0.5(4) . . . . ?
C9 C10 C5 C4 -179.7(3) . . . . ?
C1 C10 C5 C6 178.7(3) . . . . ?
C9 C10 C5 C6 -1.5(4) . . . . ?
C4 C3 C11 O2 179.7(3) . . . . ?
C2 C3 C11 O2 0.2(4) . . . . ?
C4 C3 C11 O3 0.7(4) . . . . ?
C2 C3 C11 O3 -178.8(3) . . . . ?
N1 C12 C13 C14 2.5(6) . . . . ?
C12 C13 C14 C15 -2.8(6) . . . . ?
C13 C14 C15 C16 1.8(6) . . . . ?
C14 C15 C16 N1 -0.3(6) . . . . ?
O2 C11 O3 Cu1 -0.1(5) . . . . ?
C13 C12 N1 C16 -1.0(5) . . . . ?
C13 C12 N1 Cu1 -176.4(3) . . . . ?
C15 C16 N1 C12 0.0(6) . . . . ?
C15 C16 N1 Cu1 175.5(3) . . . . ?
O4 C17 N2 C18 -172.2(7) . . . . ?
O4 C17 N2 C19 -3.4(8) . . . . ?
C11 O3 Cu1 N1 85.2(3) . . . 4 ?
C11 O3 Cu1 N1 -85.0(3) . . . . ?
C12 N1 Cu1 O3 45.5(3) . . . . ?
C16 N1 Cu1 O3 -129.9(3) . . . . ?
C12 N1 Cu1 O3 -142.2(3) . . . 4 ?
C16 N1 Cu1 O3 42.5(3) . . . 4 ?
C12 N1 Cu1 O5 131.6(3) . . . . ?
C16 N1 Cu1 O5 -43.7(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H18 O2 0.84 1.83 2.585(3) 148.1 .
O5 H19 O4 0.83(3) 2.12(3) 2.948(4) 176(3) .
O6 H20 O2 0.850 2.170 2.921(4) 146.9(3) 4

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.109


_database_code_depnum_ccdc_archive 'CCDC 954513'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_(R)-MOF-4b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C39 H31 Cu N3 O6), (C1.50 H3.50 N0.50 O0.50), 0.5(H2 O) '
_chemical_formula_sum            'C40.50 H35.50 Cu N3.50 O7'
_chemical_formula_weight         746.76

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           orthorhombic
_symmetry_space_group_name_H-M   'C 2 2 21'

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

_cell_length_a                   22.934(4)
_cell_length_b                   30.885(5)
_cell_length_c                   10.5055(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7441(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11291
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3104
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8825
_exptl_absorpt_correction_T_max  0.9686
_exptl_absorpt_process_details   'NUMBAS; Rigaku, 2005'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'RAPID-F IP'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_reflns_number            30654
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8488
_reflns_number_gt                7765
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0838P)^2^+6.1466P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.028(15)
_refine_ls_number_reflns         8488
_refine_ls_number_parameters     503
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0535
_refine_ls_wR_factor_ref         0.1539
_refine_ls_wR_factor_gt          0.1495
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

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 0.23140(10) 0.14655(8) -0.0805(2) 0.0162(5) Uani 1 1 d . . .
C2 C 0.18475(11) 0.14187(8) 0.0011(2) 0.0174(5) Uani 1 1 d . . .
C3 C 0.14057(10) 0.17444(8) 0.0110(2) 0.0178(5) Uani 1 1 d . . .
C4 C 0.14640(10) 0.21103(8) -0.0622(2) 0.0177(5) Uani 1 1 d . . .
H32 H 0.1179 0.2332 -0.0549 0.021 Uiso 1 1 calc R . .
C5 C 0.19335(10) 0.21683(8) -0.1481(2) 0.0182(5) Uani 1 1 d . . .
C6 C 0.19845(11) 0.25468(8) -0.2231(2) 0.0211(6) Uani 1 1 d . . .
H33 H 0.1705 0.2771 -0.2138 0.025 Uiso 1 1 calc R . .
C7 C 0.24304(12) 0.25961(9) -0.3090(3) 0.0271(7) Uani 1 1 d . . .
H34 H 0.2464 0.2854 -0.3578 0.033 Uiso 1 1 calc R . .
C8 C 0.28405(11) 0.22554(9) -0.3238(3) 0.0242(6) Uani 1 1 d . . .
H35 H 0.3143 0.2283 -0.3850 0.029 Uiso 1 1 calc R . .
C9 C 0.28075(10) 0.18916(8) -0.2520(3) 0.0213(5) Uani 1 1 d . . .
H36 H 0.3090 0.1670 -0.2630 0.026 Uiso 1 1 calc R . .
C10 C 0.23546(10) 0.18366(8) -0.1598(2) 0.0166(5) Uani 1 1 d . . .
C11 C 0.27634(10) 0.11128(8) -0.0861(2) 0.0167(5) Uani 1 1 d . . .
C12 C 0.32567(10) 0.11399(8) -0.0134(2) 0.0152(5) Uani 1 1 d . . .
C13 C 0.36761(10) 0.08005(8) -0.0115(2) 0.0162(5) Uani 1 1 d . . .
C14 C 0.35925(10) 0.04472(8) -0.0885(2) 0.0168(5) Uani 1 1 d . . .
H37 H 0.3876 0.0223 -0.0899 0.020 Uiso 1 1 calc R . .
C15 C 0.30876(11) 0.04116(8) -0.1663(2) 0.0179(5) Uani 1 1 d . . .
C16 C 0.29952(10) 0.00368(7) -0.2460(3) 0.0203(5) Uani 1 1 d . . .
H38 H 0.3276 -0.0190 -0.2471 0.024 Uiso 1 1 calc R . .
C17 C 0.25088(12) 0.00065(9) -0.3193(3) 0.0250(6) Uani 1 1 d . . .
H39 H 0.2461 -0.0235 -0.3742 0.030 Uiso 1 1 calc R . .
C18 C 0.20738(11) 0.03299(9) -0.3149(2) 0.0232(6) Uani 1 1 d . . .
H40 H 0.1728 0.0298 -0.3638 0.028 Uiso 1 1 calc R . .
C19 C 0.21500(10) 0.06938(8) -0.2395(3) 0.0210(5) Uani 1 1 d . . .
H41 H 0.1858 0.0912 -0.2380 0.025 Uiso 1 1 calc R . .
C20 C 0.26643(10) 0.07448(8) -0.1639(2) 0.0167(5) Uani 1 1 d . . .
C21 C 0.08746(11) 0.16897(9) 0.0936(2) 0.0199(6) Uani 1 1 d . . .
C22 C 0.19784(15) 0.10857(12) 0.2023(3) 0.0413(9) Uani 1 1 d . . .
H42 H 0.2386 0.1179 0.2079 0.062 Uiso 1 1 calc R . .
H43 H 0.1933 0.0806 0.2453 0.062 Uiso 1 1 calc R . .
H44 H 0.1727 0.1301 0.2433 0.062 Uiso 1 1 calc R . .
C23 C 0.41941(10) 0.07859(8) 0.0773(2) 0.0169(5) Uani 1 1 d . . .
C24 C 0.36738(11) 0.18347(9) 0.0149(3) 0.0232(6) Uani 1 1 d . . .
H45 H 0.4018 0.1711 -0.0268 0.035 Uiso 1 1 calc R . .
H46 H 0.3798 0.2029 0.0835 0.035 Uiso 1 1 calc R . .
H47 H 0.3444 0.1998 -0.0475 0.035 Uiso 1 1 calc R . .
C28 C -0.06007(13) 0.15450(10) 0.0402(3) 0.0342(8) Uani 1 1 d . . .
H51 H -0.0253 0.1378 0.0398 0.041 Uiso 1 1 calc R . .
C29 C -0.10473(16) 0.14292(13) -0.0417(4) 0.0476(9) Uani 1 1 d . . .
H52 H -0.1005 0.1191 -0.0983 0.057 Uiso 1 1 calc R . .
C30 C -0.15572(14) 0.16688(12) -0.0389(3) 0.0397(9) Uani 1 1 d . . .
H53 H -0.1872 0.1595 -0.0935 0.048 Uiso 1 1 calc R . .
C31 C -0.16057(13) 0.20092(11) 0.0419(3) 0.0346(8) Uani 1 1 d . . .
H54 H -0.1952 0.2177 0.0447 0.041 Uiso 1 1 calc R . .
C32 C -0.11383(12) 0.21057(10) 0.1204(3) 0.0282(7) Uani 1 1 d . . .
H55 H -0.1174 0.2343 0.1774 0.034 Uiso 1 1 calc R . .
C25 C 0.04221(12) 0.29901(9) 0.1924(3) 0.0238(6) Uani 1 1 d . . .
H48 H 0.0726 0.2835 0.1511 0.029 Uiso 1 1 calc R . .
C26 C 0.04398(14) 0.34425(9) 0.1898(3) 0.0298(7) Uani 1 1 d . . .
H49 H 0.0748 0.3589 0.1474 0.036 Uiso 1 1 calc R . .
C27 C 0.0000 0.36746(12) 0.2500 0.0305(9) Uani 1 2 d S . .
H50 H 0.0000 0.3982 0.2500 0.037 Uiso 1 2 calc SR . .
C33 C 0.50235(13) 0.20653(8) 0.1417(2) 0.0230(5) Uani 1 1 d . . .
H56 H 0.5044 0.1909 0.0639 0.028 Uiso 1 1 calc R . .
C34 C 0.50187(14) 0.25177(8) 0.1366(3) 0.0289(6) Uani 1 1 d . . .
H57 H 0.5028 0.2667 0.0575 0.035 Uiso 1 1 calc R . .
C35 C 0.5000 0.27392(11) 0.2500 0.0304(9) Uani 1 2 d S . .
H58 H 0.5000 0.3047 0.2500 0.036 Uiso 1 2 calc SR . .
C36 C 0.61730(11) 0.12420(9) 0.1441(3) 0.0235(6) Uani 1 1 d . . .
H59 H 0.6192 0.1456 0.2089 0.028 Uiso 1 1 calc R . .
C37 C 0.66605(12) 0.11736(10) 0.0670(3) 0.0270(7) Uani 1 1 d . . .
H60 H 0.7001 0.1345 0.0775 0.032 Uiso 1 1 calc R . .
C38 C 0.66408(12) 0.08558(10) -0.0243(3) 0.0267(7) Uani 1 1 d . . .
H61 H 0.6971 0.0800 -0.0764 0.032 Uiso 1 1 calc R . .
C39 C 0.61330(12) 0.06183(9) -0.0393(3) 0.0272(7) Uani 1 1 d . . .
H62 H 0.6107 0.0400 -0.1027 0.033 Uiso 1 1 calc R . .
C40 C 0.56624(12) 0.07063(9) 0.0401(3) 0.0234(6) Uani 1 1 d . . .
H63 H 0.5315 0.0541 0.0307 0.028 Uiso 1 1 calc R . .
O1 O 0.18152(8) 0.10422(6) 0.07079(18) 0.0230(4) Uani 1 1 d . . .
O2 O 0.06111(7) 0.20448(6) 0.12033(17) 0.0210(4) Uani 1 1 d . . .
O3 O 0.07151(9) 0.13284(6) 0.1306(2) 0.0319(5) Uani 1 1 d . . .
O4 O 0.33241(8) 0.14923(6) 0.06694(17) 0.0195(4) Uani 1 1 d . . .
O5 O 0.44515(7) 0.11438(6) 0.10581(16) 0.0168(4) Uani 1 1 d . . .
O6 O 0.43473(8) 0.04286(6) 0.12045(19) 0.0248(4) Uani 1 1 d . . .
O7 O 0.5000 0.02209(10) -0.2500 0.0494(9) Uani 1 2 d S . .
H31 H 0.4778(14) 0.0117(11) -0.212(3) 0.038(11) Uiso 1 1 d . . .
N2 N -0.06375(10) 0.18811(7) 0.1199(2) 0.0219(5) Uani 1 1 d . . .
N1 N 0.0000 0.27644(9) 0.2500 0.0204(6) Uani 1 2 d S . .
N3 N 0.5000 0.18430(9) 0.2500 0.0185(6) Uani 1 2 d S . .
N4 N 0.56817(9) 0.10163(7) 0.12972(19) 0.0175(5) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.200874(13) 0.2500 0.01736(9) Uani 1 2 d S . .
Cu2 Cu 0.5000 0.111438(12) 0.2500 0.01469(8) Uani 1 2 d S . .
C42 C 0.0820(4) 0.0478(4) 0.1720(9) 0.112(5) Uani 0.50 1 d PDU A -1
H67 H 0.1162 0.0437 0.2215 0.135 Uiso 0.50 1 calc PR A -1
N5 N 0.0825(4) 0.0411(3) 0.0422(10) 0.146(5) Uani 0.50 1 d PDU A -1
C43 C 0.0424(5) 0.0607(5) -0.0484(10) 0.234(9) Uani 0.50 1 d PDU A -1
H64 H 0.0501 0.0493 -0.1338 0.351 Uiso 0.50 1 calc PR A -1
H65 H 0.0478 0.0922 -0.0485 0.351 Uiso 0.50 1 calc PR A -1
H66 H 0.0022 0.0539 -0.0239 0.351 Uiso 0.50 1 calc PR A -1
C44 C 0.1258(5) 0.0148(5) -0.0208(15) 0.198(8) Uani 0.50 1 d PDU A -1
H68 H 0.1557 0.0335 -0.0584 0.298 Uiso 0.50 1 calc PR A -1
H69 H 0.1071 -0.0023 -0.0881 0.298 Uiso 0.50 1 calc PR A -1
H70 H 0.1439 -0.0047 0.0411 0.298 Uiso 0.50 1 calc PR A -1
O11 O 0.0345(6) 0.0596(3) 0.2234(10) 0.336(12) Uani 0.50 1 d PD A -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 0.0122(10) 0.0182(10) 0.0181(11) -0.0044(10) -0.0028(9) 0.0025(9)
C2 0.0202(11) 0.0180(10) 0.0141(11) 0.0011(9) -0.0025(9) 0.0014(9)
C3 0.0125(10) 0.0239(12) 0.0171(11) -0.0015(10) 0.0013(9) 0.0036(10)
C4 0.0141(10) 0.0195(11) 0.0194(12) -0.0028(10) -0.0011(9) 0.0043(9)
C5 0.0149(10) 0.0217(11) 0.0180(12) -0.0008(10) -0.0029(9) 0.0015(9)
C6 0.0220(11) 0.0196(11) 0.0217(14) -0.0001(10) 0.0009(10) 0.0024(9)
C7 0.0232(12) 0.0270(13) 0.0312(14) 0.0077(12) -0.0001(12) -0.0022(11)
C8 0.0172(11) 0.0304(13) 0.0251(13) 0.0046(12) 0.0020(10) 0.0002(11)
C9 0.0154(9) 0.0288(11) 0.0197(11) 0.0043(13) 0.0017(12) 0.0011(9)
C10 0.0125(10) 0.0220(11) 0.0154(11) 0.0001(10) -0.0015(9) -0.0008(9)
C11 0.0130(10) 0.0204(11) 0.0165(11) 0.0014(10) 0.0015(9) 0.0034(9)
C12 0.0149(10) 0.0148(10) 0.0158(11) -0.0013(9) 0.0002(9) 0.0022(9)
C13 0.0170(10) 0.0163(10) 0.0154(11) 0.0026(9) 0.0015(9) 0.0016(9)
C14 0.0153(10) 0.0164(10) 0.0188(11) 0.0025(10) 0.0023(9) 0.0009(9)
C15 0.0183(11) 0.0189(11) 0.0165(11) 0.0015(10) 0.0002(9) 0.0005(9)
C16 0.0232(10) 0.0175(10) 0.0203(11) -0.0009(12) -0.0029(12) 0.0013(9)
C17 0.0301(14) 0.0241(12) 0.0209(13) -0.0041(11) -0.0013(11) -0.0047(11)
C18 0.0197(12) 0.0308(13) 0.0190(13) -0.0025(11) -0.0077(10) -0.0038(11)
C19 0.0174(10) 0.0238(11) 0.0220(12) -0.0005(12) 0.0002(11) 0.0013(9)
C20 0.0136(10) 0.0217(11) 0.0149(11) 0.0011(10) 0.0016(9) 0.0001(9)
C21 0.0170(10) 0.0262(12) 0.0163(12) 0.0006(10) 0.0018(10) 0.0040(10)
C22 0.0394(17) 0.055(2) 0.0292(15) 0.0109(15) -0.0017(14) 0.0065(16)
C23 0.0153(10) 0.0166(10) 0.0189(11) 0.0062(10) 0.0012(9) 0.0004(9)
C24 0.0202(11) 0.0199(11) 0.0296(14) -0.0045(11) -0.0061(11) 0.0000(10)
C28 0.0282(14) 0.0354(15) 0.0390(17) -0.0132(14) -0.0052(13) 0.0014(12)
C29 0.0477(19) 0.0517(19) 0.0435(19) -0.0202(17) -0.0130(16) 0.0038(17)
C30 0.0319(15) 0.0529(19) 0.0342(17) -0.0052(16) -0.0138(14) -0.0021(15)
C31 0.0255(13) 0.0446(17) 0.0335(16) 0.0081(14) -0.0060(13) 0.0039(13)
C32 0.0245(12) 0.0294(13) 0.0305(14) 0.0013(13) 0.0000(11) 0.0012(11)
C25 0.0219(12) 0.0222(12) 0.0275(13) 0.0037(11) 0.0001(11) 0.0016(10)
C26 0.0343(15) 0.0225(13) 0.0327(15) 0.0054(12) 0.0016(13) -0.0045(12)
C27 0.044(2) 0.0195(15) 0.0280(18) 0.000 -0.005(2) 0.000
C33 0.0232(11) 0.0268(11) 0.0190(11) 0.0013(10) 0.0012(12) -0.0040(13)
C34 0.0214(11) 0.0285(12) 0.0368(14) 0.0122(11) -0.0026(14) -0.0059(13)
C35 0.0294(17) 0.0131(14) 0.049(2) 0.000 0.001(2) 0.000
C36 0.0191(12) 0.0307(13) 0.0209(13) 0.0012(11) 0.0027(10) -0.0044(10)
C37 0.0169(11) 0.0372(15) 0.0269(14) -0.0011(13) 0.0043(11) -0.0024(11)
C38 0.0188(11) 0.0368(15) 0.0244(13) 0.0060(12) 0.0062(11) 0.0041(11)
C39 0.0292(13) 0.0272(13) 0.0251(13) -0.0031(12) 0.0069(11) 0.0039(12)
C40 0.0200(12) 0.0234(12) 0.0268(13) -0.0021(11) 0.0016(11) 0.0021(10)
O1 0.0222(8) 0.0209(9) 0.0257(9) 0.0084(8) 0.0050(8) 0.0049(7)
O2 0.0174(8) 0.0266(9) 0.0191(8) 0.0016(8) 0.0040(7) 0.0056(7)
O3 0.0270(10) 0.0228(9) 0.0458(12) 0.0069(9) 0.0121(9) 0.0020(8)
O4 0.0183(8) 0.0189(8) 0.0213(9) -0.0038(7) -0.0009(7) 0.0013(7)
O5 0.0124(7) 0.0174(7) 0.0205(9) -0.0015(7) -0.0019(7) -0.0015(6)
O6 0.0222(8) 0.0190(8) 0.0333(10) 0.0023(8) -0.0128(8) -0.0011(7)
O7 0.0477(16) 0.0257(13) 0.075(2) 0.000 0.0412(19) 0.000
N2 0.0198(10) 0.0274(11) 0.0184(10) 0.0021(9) -0.0010(9) 0.0010(9)
N1 0.0219(13) 0.0200(12) 0.0193(13) 0.000 0.0031(15) 0.000
N3 0.0194(12) 0.0164(12) 0.0198(13) 0.000 0.0025(15) 0.000
N4 0.0141(9) 0.0219(10) 0.0166(10) -0.0016(9) 0.0003(8) 0.0038(8)
Cu1 0.01366(16) 0.02151(18) 0.01691(18) 0.000 0.00163(19) 0.000
Cu2 0.01175(16) 0.01646(16) 0.01586(18) 0.000 -0.00055(18) 0.000
C42 0.059(6) 0.114(9) 0.163(10) 0.020(8) 0.020(7) 0.024(6)
N5 0.101(7) 0.106(7) 0.231(11) 0.005(8) -0.021(8) -0.059(6)
C43 0.302(16) 0.153(12) 0.246(15) -0.060(12) 0.006(13) -0.054(12)
C44 0.223(13) 0.198(14) 0.174(12) -0.026(11) 0.042(12) -0.112(10)
O11 0.69(3) 0.120(6) 0.194(14) -0.023(9) 0.05(2) -0.218(11)

_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 C2 1.379(3) . ?
C1 C10 1.420(3) . ?
C1 C11 1.501(3) . ?
C2 O1 1.376(3) . ?
C2 C3 1.431(3) . ?
C3 C4 1.373(4) . ?
C3 C21 1.505(3) . ?
C4 C5 1.416(3) . ?
C5 C10 1.413(3) . ?
C5 C6 1.415(3) . ?
C6 C7 1.372(4) . ?
C7 C8 1.420(4) . ?
C8 C9 1.356(4) . ?
C9 C10 1.430(4) . ?
C11 C12 1.367(3) . ?
C11 C20 1.418(4) . ?
C12 O4 1.386(3) . ?
C12 C13 1.423(3) . ?
C13 C14 1.372(3) . ?
C13 C23 1.511(3) . ?
C14 C15 1.422(3) . ?
C15 C20 1.415(3) . ?
C15 C16 1.444(3) . ?
C16 C17 1.359(4) . ?
C17 C18 1.413(4) . ?
C18 C19 1.386(4) . ?
C19 C20 1.431(3) . ?
C21 O3 1.237(3) . ?
C21 O2 1.283(3) . ?
C22 O1 1.437(4) . ?
C23 O6 1.244(3) . ?
C23 O5 1.289(3) . ?
C24 O4 1.435(3) . ?
C28 N2 1.336(4) . ?
C28 C29 1.385(5) . ?
C29 C30 1.384(5) . ?
C30 C31 1.356(5) . ?
C31 C32 1.384(4) . ?
C32 N2 1.342(4) . ?
C25 N1 1.338(3) . ?
C25 C26 1.398(4) . ?
C26 C27 1.390(4) . ?
C27 C26 1.390(4) 4 ?
C33 N3 1.330(3) . ?
C33 C34 1.398(3) . ?
C34 C35 1.374(3) . ?
C35 C34 1.374(3) 4_655 ?
C36 N4 1.334(3) . ?
C36 C37 1.397(4) . ?
C37 C38 1.373(4) . ?
C38 C39 1.385(4) . ?
C39 C40 1.391(4) . ?
C40 N4 1.343(3) . ?
O2 Cu1 1.9577(17) . ?
O5 Cu2 1.9711(17) . ?
N2 Cu1 2.040(2) . ?
N1 C25 1.338(3) 4 ?
N1 Cu1 2.334(3) . ?
N3 C33 1.330(3) 4_655 ?
N3 Cu2 2.250(3) . ?
N4 Cu2 2.033(2) . ?
Cu1 O2 1.9577(17) 4 ?
Cu1 N2 2.040(2) 4 ?
Cu2 O5 1.9711(17) 4_655 ?
Cu2 N4 2.033(2) 4_655 ?
C42 O11 1.268(13) . ?
C42 N5 1.380(14) . ?
N5 C44 1.442(12) . ?
N5 C43 1.457(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C10 120.0(2) . . ?
C2 C1 C11 118.8(2) . . ?
C10 C1 C11 121.2(2) . . ?
O1 C2 C1 117.5(2) . . ?
O1 C2 C3 121.2(2) . . ?
C1 C2 C3 121.4(2) . . ?
C4 C3 C2 118.0(2) . . ?
C4 C3 C21 119.6(2) . . ?
C2 C3 C21 122.4(2) . . ?
C3 C4 C5 122.3(2) . . ?
C10 C5 C6 119.6(2) . . ?
C10 C5 C4 118.9(2) . . ?
C6 C5 C4 121.5(2) . . ?
C7 C6 C5 121.3(2) . . ?
C6 C7 C8 118.9(3) . . ?
C9 C8 C7 121.1(2) . . ?
C8 C9 C10 121.0(2) . . ?
C5 C10 C1 119.3(2) . . ?
C5 C10 C9 118.0(2) . . ?
C1 C10 C9 122.7(2) . . ?
C12 C11 C20 120.2(2) . . ?
C12 C11 C1 120.1(2) . . ?
C20 C11 C1 119.6(2) . . ?
C11 C12 O4 118.7(2) . . ?
C11 C12 C13 121.5(2) . . ?
O4 C12 C13 119.6(2) . . ?
C14 C13 C12 118.9(2) . . ?
C14 C13 C23 116.7(2) . . ?
C12 C13 C23 124.2(2) . . ?
C13 C14 C15 121.0(2) . . ?
C20 C15 C14 119.5(2) . . ?
C20 C15 C16 119.5(2) . . ?
C14 C15 C16 121.0(2) . . ?
C17 C16 C15 120.3(2) . . ?
C16 C17 C18 120.8(2) . . ?
C19 C18 C17 120.2(2) . . ?
C18 C19 C20 120.7(2) . . ?
C15 C20 C11 118.9(2) . . ?
C15 C20 C19 118.4(2) . . ?
C11 C20 C19 122.7(2) . . ?
O3 C21 O2 124.2(2) . . ?
O3 C21 C3 121.5(2) . . ?
O2 C21 C3 114.3(2) . . ?
O6 C23 O5 123.1(2) . . ?
O6 C23 C13 118.3(2) . . ?
O5 C23 C13 118.6(2) . . ?
N2 C28 C29 122.9(3) . . ?
C30 C29 C28 118.3(3) . . ?
C31 C30 C29 119.8(3) . . ?
C30 C31 C32 118.4(3) . . ?
N2 C32 C31 123.3(3) . . ?
N1 C25 C26 123.4(3) . . ?
C27 C26 C25 119.0(3) . . ?
C26 C27 C26 117.9(4) . 4 ?
N3 C33 C34 123.2(2) . . ?
C35 C34 C33 117.7(2) . . ?
C34 C35 C34 120.3(3) 4_655 . ?
N4 C36 C37 122.1(3) . . ?
C38 C37 C36 119.1(3) . . ?
C37 C38 C39 119.1(3) . . ?
C38 C39 C40 118.7(3) . . ?
N4 C40 C39 122.3(2) . . ?
C2 O1 C22 114.7(2) . . ?
C21 O2 Cu1 116.16(16) . . ?
C12 O4 C24 114.14(19) . . ?
C23 O5 Cu2 115.57(15) . . ?
C28 N2 C32 117.2(2) . . ?
C28 N2 Cu1 121.65(19) . . ?
C32 N2 Cu1 120.75(19) . . ?
C25 N1 C25 117.2(3) 4 . ?
C25 N1 Cu1 121.41(15) 4 . ?
C25 N1 Cu1 121.41(15) . . ?
C33 N3 C33 117.8(3) 4_655 . ?
C33 N3 Cu2 121.09(14) 4_655 . ?
C33 N3 Cu2 121.08(14) . . ?
C36 N4 C40 118.7(2) . . ?
C36 N4 Cu2 120.09(18) . . ?
C40 N4 Cu2 121.09(17) . . ?
O2 Cu1 O2 173.47(11) . 4 ?
O2 Cu1 N2 87.94(8) . 4 ?
O2 Cu1 N2 93.33(8) 4 4 ?
O2 Cu1 N2 93.33(8) . . ?
O2 Cu1 N2 87.94(8) 4 . ?
N2 Cu1 N2 157.71(13) 4 . ?
O2 Cu1 N1 86.74(6) . . ?
O2 Cu1 N1 86.74(6) 4 . ?
N2 Cu1 N1 101.15(7) 4 . ?
N2 Cu1 N1 101.15(7) . . ?
O5 Cu2 O5 174.72(10) 4_655 . ?
O5 Cu2 N4 91.14(8) 4_655 4_655 ?
O5 Cu2 N4 89.64(8) . 4_655 ?
O5 Cu2 N4 89.64(8) 4_655 . ?
O5 Cu2 N4 91.14(8) . . ?
N4 Cu2 N4 162.86(12) 4_655 . ?
O5 Cu2 N3 87.36(5) 4_655 . ?
O5 Cu2 N3 87.36(5) . . ?
N4 Cu2 N3 98.57(6) 4_655 . ?
N4 Cu2 N3 98.57(6) . . ?
O11 C42 N5 118.2(10) . . ?
C42 N5 C44 123.0(10) . . ?
C42 N5 C43 125.2(9) . . ?
C44 N5 C43 111.7(9) . . ?

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
C10 C1 C2 O1 176.7(2) . . . . ?
C11 C1 C2 O1 -1.6(3) . . . . ?
C10 C1 C2 C3 -1.9(4) . . . . ?
C11 C1 C2 C3 179.9(2) . . . . ?
O1 C2 C3 C4 -179.5(2) . . . . ?
C1 C2 C3 C4 -1.0(4) . . . . ?
O1 C2 C3 C21 -2.1(4) . . . . ?
C1 C2 C3 C21 176.4(2) . . . . ?
C2 C3 C4 C5 1.7(4) . . . . ?
C21 C3 C4 C5 -175.8(2) . . . . ?
C3 C4 C5 C10 0.5(4) . . . . ?
C3 C4 C5 C6 179.7(2) . . . . ?
C10 C5 C6 C7 1.2(4) . . . . ?
C4 C5 C6 C7 -178.0(2) . . . . ?
C5 C6 C7 C8 1.1(4) . . . . ?
C6 C7 C8 C9 -2.1(4) . . . . ?
C7 C8 C9 C10 0.7(4) . . . . ?
C6 C5 C10 C1 177.4(2) . . . . ?
C4 C5 C10 C1 -3.4(4) . . . . ?
C6 C5 C10 C9 -2.5(4) . . . . ?
C4 C5 C10 C9 176.7(2) . . . . ?
C2 C1 C10 C5 4.1(4) . . . . ?
C11 C1 C10 C5 -177.7(2) . . . . ?
C2 C1 C10 C9 -176.0(2) . . . . ?
C11 C1 C10 C9 2.2(4) . . . . ?
C8 C9 C10 C5 1.6(4) . . . . ?
C8 C9 C10 C1 -178.3(2) . . . . ?
C2 C1 C11 C12 -94.5(3) . . . . ?
C10 C1 C11 C12 87.2(3) . . . . ?
C2 C1 C11 C20 83.4(3) . . . . ?
C10 C1 C11 C20 -94.8(3) . . . . ?
C20 C11 C12 O4 -176.4(2) . . . . ?
C1 C11 C12 O4 1.5(3) . . . . ?
C20 C11 C12 C13 -1.2(4) . . . . ?
C1 C11 C12 C13 176.6(2) . . . . ?
C11 C12 C13 C14 2.7(4) . . . . ?
O4 C12 C13 C14 177.8(2) . . . . ?
C11 C12 C13 C23 -172.8(2) . . . . ?
O4 C12 C13 C23 2.3(4) . . . . ?
C12 C13 C14 C15 -1.9(4) . . . . ?
C23 C13 C14 C15 173.9(2) . . . . ?
C13 C14 C15 C20 -0.2(4) . . . . ?
C13 C14 C15 C16 -179.1(2) . . . . ?
C20 C15 C16 C17 0.8(4) . . . . ?
C14 C15 C16 C17 179.7(3) . . . . ?
C15 C16 C17 C18 -2.8(4) . . . . ?
C16 C17 C18 C19 2.8(4) . . . . ?
C17 C18 C19 C20 -0.8(4) . . . . ?
C14 C15 C20 C11 1.7(4) . . . . ?
C16 C15 C20 C11 -179.5(2) . . . . ?
C14 C15 C20 C19 -177.7(2) . . . . ?
C16 C15 C20 C19 1.1(4) . . . . ?
C12 C11 C20 C15 -1.0(4) . . . . ?
C1 C11 C20 C15 -178.9(2) . . . . ?
C12 C11 C20 C19 178.4(2) . . . . ?
C1 C11 C20 C19 0.5(4) . . . . ?
C18 C19 C20 C15 -1.1(4) . . . . ?
C18 C19 C20 C11 179.5(2) . . . . ?
C4 C3 C21 O3 158.4(3) . . . . ?
C2 C3 C21 O3 -18.9(4) . . . . ?
C4 C3 C21 O2 -21.4(3) . . . . ?
C2 C3 C21 O2 161.3(2) . . . . ?
C14 C13 C23 O6 -32.4(3) . . . . ?
C12 C13 C23 O6 143.2(3) . . . . ?
C14 C13 C23 O5 148.5(2) . . . . ?
C12 C13 C23 O5 -36.0(3) . . . . ?
N2 C28 C29 C30 -1.2(5) . . . . ?
C28 C29 C30 C31 0.6(6) . . . . ?
C29 C30 C31 C32 -0.3(5) . . . . ?
C30 C31 C32 N2 0.4(5) . . . . ?
N1 C25 C26 C27 0.2(4) . . . . ?
C25 C26 C27 C26 -0.08(19) . . . 4 ?
N3 C33 C34 C35 1.3(4) . . . . ?
C33 C34 C35 C34 -0.6(2) . . . 4_655 ?
N4 C36 C37 C38 -1.9(4) . . . . ?
C36 C37 C38 C39 1.5(4) . . . . ?
C37 C38 C39 C40 -0.9(4) . . . . ?
C38 C39 C40 N4 0.8(4) . . . . ?
C1 C2 O1 C22 103.9(3) . . . . ?
C3 C2 O1 C22 -77.6(3) . . . . ?
O3 C21 O2 Cu1 10.3(3) . . . . ?
C3 C21 O2 Cu1 -169.99(16) . . . . ?
C11 C12 O4 C24 -97.1(3) . . . . ?
C13 C12 O4 C24 87.7(3) . . . . ?
O6 C23 O5 Cu2 -12.4(3) . . . . ?
C13 C23 O5 Cu2 166.72(16) . . . . ?
C29 C28 N2 C32 1.3(5) . . . . ?
C29 C28 N2 Cu1 174.5(3) . . . . ?
C31 C32 N2 C28 -0.9(4) . . . . ?
C31 C32 N2 Cu1 -174.2(2) . . . . ?
C26 C25 N1 C25 -0.1(2) . . . 4 ?
C26 C25 N1 Cu1 179.9(2) . . . . ?
C34 C33 N3 C33 -0.7(2) . . . 4_655 ?
C34 C33 N3 Cu2 179.3(2) . . . . ?
C37 C36 N4 C40 1.7(4) . . . . ?
C37 C36 N4 Cu2 177.4(2) . . . . ?
C39 C40 N4 C36 -1.1(4) . . . . ?
C39 C40 N4 Cu2 -176.8(2) . . . . ?
C21 O2 Cu1 N2 67.72(18) . . . 4 ?
C21 O2 Cu1 N2 -90.00(18) . . . . ?
C21 O2 Cu1 N1 169.01(17) . . . . ?
C28 N2 Cu1 O2 56.6(2) . . . . ?
C32 N2 Cu1 O2 -130.4(2) . . . . ?
C28 N2 Cu1 O2 -129.8(2) . . . 4 ?
C32 N2 Cu1 O2 43.2(2) . . . 4 ?
C28 N2 Cu1 N2 -36.0(2) . . . 4 ?
C32 N2 Cu1 N2 136.9(2) . . . 4 ?
C28 N2 Cu1 N1 144.0(2) . . . . ?
C32 N2 Cu1 N1 -43.1(2) . . . . ?
C25 N1 Cu1 O2 167.83(15) 4 . . . ?
C25 N1 Cu1 O2 -12.17(15) . . . . ?
C25 N1 Cu1 O2 -12.17(15) 4 . . 4 ?
C25 N1 Cu1 O2 167.83(15) . . . 4 ?
C25 N1 Cu1 N2 -104.92(15) 4 . . 4 ?
C25 N1 Cu1 N2 75.08(15) . . . 4 ?
C25 N1 Cu1 N2 75.08(15) 4 . . . ?
C25 N1 Cu1 N2 -104.92(15) . . . . ?
C23 O5 Cu2 N4 -68.35(17) . . . 4_655 ?
C23 O5 Cu2 N4 94.52(17) . . . . ?
C23 O5 Cu2 N3 -166.95(16) . . . . ?
C36 N4 Cu2 O5 -41.6(2) . . . 4_655 ?
C40 N4 Cu2 O5 134.1(2) . . . 4_655 ?
C36 N4 Cu2 O5 133.2(2) . . . . ?
C40 N4 Cu2 O5 -51.2(2) . . . . ?
C36 N4 Cu2 N4 -134.3(2) . . . 4_655 ?
C40 N4 Cu2 N4 41.33(19) . . . 4_655 ?
C36 N4 Cu2 N3 45.7(2) . . . . ?
C40 N4 Cu2 N3 -138.67(19) . . . . ?
C33 N3 Cu2 O5 -42.41(15) 4_655 . . 4_655 ?
C33 N3 Cu2 O5 137.59(15) . . . 4_655 ?
C33 N3 Cu2 O5 137.59(15) 4_655 . . . ?
C33 N3 Cu2 O5 -42.41(15) . . . . ?
C33 N3 Cu2 N4 48.35(16) 4_655 . . 4_655 ?
C33 N3 Cu2 N4 -131.65(16) . . . 4_655 ?
C33 N3 Cu2 N4 -131.66(16) 4_655 . . . ?
C33 N3 Cu2 N4 48.35(16) . . . . ?
O11 C42 N5 C44 -158.9(13) . . . . ?
O11 C42 N5 C43 24(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.086

_database_code_depnum_ccdc_archive 'CCDC 954514'