# 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        'Daofeng Sun'
_publ_contact_author_email       DFSUN@SDU.EDU.CN

_publ_section_title              
;
Construction of Copper Metal-Organic Supramolecules
Based on Paddlewheel SBU through Altering the Substituent Positions
of New Flexible Carboxylate Ligands
;
loop_
_publ_author_name
'Daofeng Sun'
'Fangna Dai'
'Dongliang Gao'
'Haiyan He'
'Xiaoliang Qiu'
;
Fei Ye
;

# Attachment '2-revised.cif'

data_test2
_database_code_depnum_ccdc_archive 'CCDC 714741'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H72 Cu2 N4 O16'
_chemical_formula_weight         1256.32

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   P21/c

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

_cell_length_a                   15.5453(11)
_cell_length_b                   10.0554(7)
_cell_length_c                   21.4858(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.182(4)
_cell_angle_gamma                90.00
_cell_volume                     3087.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2041
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      20.35

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9280
_exptl_absorpt_correction_T_max  0.9630
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13531
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         23.78
_reflns_number_total             4700
_reflns_number_gt                3292
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 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+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         4700
_refine_ls_number_parameters     379
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1746
_refine_ls_wR_factor_gt          0.1488
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002

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
Cu Cu 0.51809(4) 0.61974(5) -0.01589(3) 0.0327(2) Uani 1 1 d . . .
O1 O 0.4835(2) 0.6754(3) 0.05849(18) 0.0466(9) Uani 1 1 d . . .
O2 O 0.4507(2) 0.4731(3) 0.08515(16) 0.0424(9) Uani 1 1 d . . .
O3 O 0.3252(2) 0.5476(4) 0.14653(17) 0.0463(9) Uani 1 1 d . . .
O4 O 0.1594(2) 0.4164(4) -0.09351(18) 0.0483(9) Uani 1 1 d . . .
O5 O 0.3543(2) 0.4079(3) -0.05324(17) 0.0419(8) Uani 1 1 d . . .
O6 O 0.3868(2) 0.6116(3) -0.08074(18) 0.0494(9) Uani 1 1 d . . .
O7 O 0.5539(3) 0.8094(3) -0.04434(18) 0.0478(9) Uani 1 1 d . . .
N1 N 0.6565(3) 0.9168(4) -0.0765(3) 0.0596(14) Uani 1 1 d . . .
C1 C 0.4658(3) 0.5948(5) 0.0966(2) 0.0348(12) Uani 1 1 d . . .
C2 C 0.4678(4) 0.6504(5) 0.1614(2) 0.0411(12) Uani 1 1 d . . .
C3 C 0.5426(4) 0.7273(5) 0.1999(3) 0.0556(15) Uani 1 1 d . . .
H3A H 0.5905 0.7414 0.1849 0.067 Uiso 1 1 calc R . .
C4 C 0.5493(5) 0.7844(6) 0.2600(3) 0.0679(18) Uani 1 1 d . . .
H4A H 0.6018 0.8338 0.2859 0.082 Uiso 1 1 calc R . .
C5 C 0.4784(5) 0.7674(6) 0.2810(3) 0.0697(19) Uani 1 1 d . . .
H5A H 0.4812 0.8084 0.3205 0.084 Uiso 1 1 calc R . .
C6 C 0.4023(5) 0.6899(6) 0.2442(3) 0.0560(15) Uani 1 1 d . . .
H6A H 0.3543 0.6785 0.2592 0.067 Uiso 1 1 calc R . .
C7 C 0.3967(4) 0.6287(5) 0.1847(2) 0.0389(12) Uani 1 1 d . . .
C8 C 0.2397(4) 0.5540(6) 0.1557(3) 0.0567(15) Uani 1 1 d . . .
H8A H 0.2162 0.6445 0.1494 0.068 Uiso 1 1 calc R . .
H8B H 0.2494 0.5259 0.2012 0.068 Uiso 1 1 calc R . .
C9 C 0.1710(4) 0.4637(5) 0.1047(3) 0.0476(14) Uani 1 1 d . . .
C14 C 0.1494(4) 0.4841(5) 0.0353(3) 0.0467(13) Uani 1 1 d . . .
C13 C 0.0910(4) 0.3950(5) -0.0121(3) 0.0476(14) Uani 1 1 d . . .
C12 C 0.0491(4) 0.2902(6) 0.0091(3) 0.0550(15) Uani 1 1 d . . .
C11 C 0.0675(4) 0.2765(6) 0.0763(3) 0.0583(16) Uani 1 1 d . . .
H11A H 0.0376 0.2090 0.0897 0.070 Uiso 1 1 calc R . .
C10 C 0.1288(4) 0.3592(6) 0.1255(3) 0.0544(15) Uani 1 1 d . . .
C17 C 0.1885(4) 0.6036(6) 0.0124(3) 0.0565(15) Uani 1 1 d . . .
H17A H 0.2449 0.5787 0.0071 0.085 Uiso 1 1 calc R . .
H17B H 0.2020 0.6729 0.0456 0.085 Uiso 1 1 calc R . .
H17C H 0.1433 0.6349 -0.0301 0.085 Uiso 1 1 calc R . .
C16 C -0.0141(5) 0.1896(7) -0.0401(4) 0.0748(19) Uani 1 1 d . . .
H16A H 0.0226 0.1331 -0.0562 0.112 Uiso 1 1 calc R . .
H16B H -0.0602 0.2353 -0.0777 0.112 Uiso 1 1 calc R . .
H16C H -0.0447 0.1367 -0.0178 0.112 Uiso 1 1 calc R . .
C15 C 0.1479(5) 0.3330(7) 0.1989(4) 0.086(2) Uani 1 1 d . . .
H15A H 0.1063 0.2651 0.2018 0.129 Uiso 1 1 calc R . .
H15B H 0.1381 0.4132 0.2195 0.129 Uiso 1 1 calc R . .
H15C H 0.2115 0.3041 0.2220 0.129 Uiso 1 1 calc R . .
C18 C 0.0715(4) 0.4124(6) -0.0853(3) 0.0549(15) Uani 1 1 d . . .
H18A H 0.0336 0.3391 -0.1112 0.066 Uiso 1 1 calc R . .
H18B H 0.0372 0.4945 -0.1019 0.066 Uiso 1 1 calc R . .
C19 C 0.1597(4) 0.4655(5) -0.1524(3) 0.0461(13) Uani 1 1 d . . .
C20 C 0.0806(4) 0.4740(7) -0.2118(3) 0.0652(17) Uani 1 1 d . . .
H20A H 0.0234 0.4447 -0.2126 0.078 Uiso 1 1 calc R . .
C21 C 0.0853(5) 0.5257(8) -0.2705(3) 0.081(2) Uani 1 1 d . . .
H21A H 0.0317 0.5299 -0.3103 0.097 Uiso 1 1 calc R . .
C22 C 0.1678(6) 0.5698(8) -0.2698(3) 0.083(2) Uani 1 1 d . . .
H22A H 0.1712 0.6038 -0.3090 0.099 Uiso 1 1 calc R . .
C23 C 0.2465(4) 0.5641(7) -0.2108(3) 0.0631(17) Uani 1 1 d . . .
H23A H 0.3029 0.5949 -0.2108 0.076 Uiso 1 1 calc R . .
C24 C 0.2446(4) 0.5140(5) -0.1513(3) 0.0451(13) Uani 1 1 d . . .
C25 C 0.3342(3) 0.5112(5) -0.0900(2) 0.0387(12) Uani 1 1 d . . .
C26 C 0.6263(4) 0.8136(5) -0.0556(3) 0.0518(14) Uani 1 1 d . . .
H26A H 0.6616 0.7361 -0.0484 0.062 Uiso 1 1 calc R . .
C27 C 0.6064(7) 1.0400(10) -0.0904(5) 0.123(3) Uiso 1 1 d . . .
H27A H 0.5596 1.0388 -0.1358 0.185 Uiso 1 1 calc R . .
H27B H 0.6491 1.1120 -0.0857 0.185 Uiso 1 1 calc R . .
H27C H 0.5769 1.0520 -0.0591 0.185 Uiso 1 1 calc R . .
C28 C 0.7417(6) 0.9150(9) -0.0904(5) 0.123(4) Uani 1 1 d . . .
H28A H 0.7684 0.8274 -0.0823 0.184 Uiso 1 1 calc R . .
H28B H 0.7861 0.9774 -0.0612 0.184 Uiso 1 1 calc R . .
H28C H 0.7264 0.9392 -0.1368 0.184 Uiso 1 1 calc R . .
N01 N 0.7479(4) 1.0084(6) 0.1082(3) 0.0819(17) Uani 1 1 d D . .
C01 C 0.7931(7) 0.8993(10) 0.1085(5) 0.131(4) Uani 1 1 d D . .
H01A H 0.7747 0.8124 0.1116 0.157 Uiso 1 1 calc R . .
C03 C 0.6550(7) 1.0036(14) 0.1066(5) 0.175(6) Uani 1 1 d . . .
H03A H 0.6346 0.9127 0.1032 0.263 Uiso 1 1 calc R . .
H03B H 0.6135 1.0526 0.0682 0.263 Uiso 1 1 calc R . .
H03C H 0.6546 1.0421 0.1474 0.263 Uiso 1 1 calc R . .
C04 C 0.7947(14) 1.1294(11) 0.1112(9) 0.380(18) Uani 1 1 d D . .
H04A H 0.8553 1.1121 0.1111 0.570 Uiso 1 1 calc R . .
H04B H 0.8016 1.1759 0.1520 0.570 Uiso 1 1 calc R . .
H04C H 0.7590 1.1830 0.0727 0.570 Uiso 1 1 calc R . .
O01 O 0.8728(8) 0.941(2) 0.1034(8) 0.52(2) Uani 1 1 d 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
Cu O1 1.957(3) . ?
Cu O6 1.968(3) . ?
Cu O2 1.972(3) 3_665 ?
Cu O5 1.975(3) 3_665 ?
Cu O7 2.141(3) . ?
Cu Cu 2.6237(11) 3_665 ?
O1 C1 1.257(6) . ?
O2 C1 1.252(6) . ?
O2 Cu 1.972(3) 3_665 ?
O3 C7 1.362(6) . ?
O3 C8 1.420(6) . ?
O4 C19 1.360(6) . ?
O4 C18 1.446(6) . ?
O5 C25 1.267(6) . ?
O5 Cu 1.975(3) 3_665 ?
O6 C25 1.265(6) . ?
O7 C26 1.241(6) . ?
N1 C26 1.291(7) . ?
N1 C27 1.432(10) . ?
N1 C28 1.468(8) . ?
C1 C2 1.490(7) . ?
C2 C3 1.370(7) . ?
C2 C7 1.399(7) . ?
C3 C4 1.381(8) . ?
C3 H3A 0.9300 . ?
C4 C5 1.355(9) . ?
C4 H4A 0.9300 . ?
C5 C6 1.377(8) . ?
C5 H5A 0.9300 . ?
C6 C7 1.389(7) . ?
C6 H6A 0.9300 . ?
C8 C9 1.499(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.401(8) . ?
C9 C14 1.408(7) . ?
C14 C13 1.392(7) . ?
C14 C17 1.514(7) . ?
C13 C12 1.407(8) . ?
C13 C18 1.490(8) . ?
C12 C11 1.364(8) . ?
C12 C16 1.513(8) . ?
C11 C10 1.386(8) . ?
C11 H11A 0.9300 . ?
C10 C15 1.508(8) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.384(7) . ?
C19 C24 1.398(7) . ?
C20 C21 1.393(9) . ?
C20 H20A 0.9300 . ?
C21 C22 1.350(9) . ?
C21 H21A 0.9300 . ?
C22 C23 1.373(9) . ?
C22 H22A 0.9300 . ?
C23 C24 1.385(7) . ?
C23 H23A 0.9300 . ?
C24 C25 1.493(7) . ?
C26 H26A 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
N01 C01 1.302(9) . ?
N01 C04 1.406(12) . ?
N01 C03 1.432(10) . ?
C01 O01 1.352(14) . ?
C01 H01A 0.9300 . ?
C03 H03A 0.9600 . ?
C03 H03B 0.9600 . ?
C03 H03C 0.9600 . ?
C04 H04A 0.9600 . ?
C04 H04B 0.9600 . ?
C04 H04C 0.9600 . ?

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 Cu O6 92.78(15) . . ?
O1 Cu O2 168.35(14) . 3_665 ?
O6 Cu O2 86.59(15) . 3_665 ?
O1 Cu O5 86.76(15) . 3_665 ?
O6 Cu O5 168.90(14) . 3_665 ?
O2 Cu O5 91.62(14) 3_665 3_665 ?
O1 Cu O7 99.45(14) . . ?
O6 Cu O7 98.54(14) . . ?
O2 Cu O7 92.15(13) 3_665 . ?
O5 Cu O7 92.47(14) 3_665 . ?
O1 Cu Cu 83.91(10) . 3_665 ?
O6 Cu Cu 82.95(10) . 3_665 ?
O2 Cu Cu 84.47(10) 3_665 3_665 ?
O5 Cu Cu 85.97(10) 3_665 3_665 ?
O7 Cu Cu 176.22(10) . 3_665 ?
C1 O1 Cu 123.3(3) . . ?
C1 O2 Cu 121.9(3) . 3_665 ?
C7 O3 C8 118.4(4) . . ?
C19 O4 C18 118.2(4) . . ?
C25 O5 Cu 120.8(3) . 3_665 ?
C25 O6 Cu 124.8(3) . . ?
C26 O7 Cu 116.3(3) . . ?
C26 N1 C27 121.7(6) . . ?
C26 N1 C28 122.9(5) . . ?
C27 N1 C28 115.4(6) . . ?
O2 C1 O1 125.1(4) . . ?
O2 C1 C2 118.9(4) . . ?
O1 C1 C2 115.9(4) . . ?
C3 C2 C7 118.4(5) . . ?
C3 C2 C1 118.5(5) . . ?
C7 C2 C1 123.2(5) . . ?
C2 C3 C4 122.2(6) . . ?
C2 C3 H3A 118.9 . . ?
C4 C3 H3A 118.9 . . ?
C5 C4 C3 119.2(6) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
C4 C5 C6 120.5(6) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
C5 C6 C7 120.6(6) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
O3 C7 C6 124.1(5) . . ?
O3 C7 C2 116.7(4) . . ?
C6 C7 C2 119.1(5) . . ?
O3 C8 C9 107.9(4) . . ?
O3 C8 H8A 110.1 . . ?
C9 C8 H8A 110.1 . . ?
O3 C8 H8B 110.1 . . ?
C9 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 C14 120.0(5) . . ?
C10 C9 C8 120.6(5) . . ?
C14 C9 C8 119.4(5) . . ?
C13 C14 C9 119.8(5) . . ?
C13 C14 C17 120.1(5) . . ?
C9 C14 C17 120.1(5) . . ?
C14 C13 C12 119.8(5) . . ?
C14 C13 C18 120.0(5) . . ?
C12 C13 C18 120.2(5) . . ?
C11 C12 C13 119.2(6) . . ?
C11 C12 C16 118.8(6) . . ?
C13 C12 C16 122.0(6) . . ?
C12 C11 C10 122.7(5) . . ?
C12 C11 H11A 118.6 . . ?
C10 C11 H11A 118.6 . . ?
C11 C10 C9 118.3(5) . . ?
C11 C10 C15 119.0(6) . . ?
C9 C10 C15 122.7(6) . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C18 C13 108.8(4) . . ?
O4 C18 H18A 109.9 . . ?
C13 C18 H18A 109.9 . . ?
O4 C18 H18B 109.9 . . ?
C13 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
O4 C19 C20 123.6(5) . . ?
O4 C19 C24 117.4(5) . . ?
C20 C19 C24 119.0(5) . . ?
C19 C20 C21 120.9(6) . . ?
C19 C20 H20A 119.5 . . ?
C21 C20 H20A 119.5 . . ?
C22 C21 C20 120.0(6) . . ?
C22 C21 H21A 120.0 . . ?
C20 C21 H21A 120.0 . . ?
C21 C22 C23 119.7(6) . . ?
C21 C22 H22A 120.2 . . ?
C23 C22 H22A 120.2 . . ?
C22 C23 C24 122.1(6) . . ?
C22 C23 H23A 118.9 . . ?
C24 C23 H23A 118.9 . . ?
C23 C24 C19 118.3(5) . . ?
C23 C24 C25 118.0(5) . . ?
C19 C24 C25 123.7(5) . . ?
O6 C25 O5 124.8(5) . . ?
O6 C25 C24 116.4(4) . . ?
O5 C25 C24 118.8(5) . . ?
O7 C26 N1 125.3(5) . . ?
O7 C26 H26A 117.3 . . ?
N1 C26 H26A 117.3 . . ?
N1 C27 H27A 109.5 . . ?
N1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N1 C28 H28A 109.5 . . ?
N1 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N1 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C01 N01 C04 117.4(11) . . ?
C01 N01 C03 120.6(9) . . ?
C04 N01 C03 121.9(11) . . ?
N01 C01 O01 104.5(12) . . ?
N01 C01 H01A 127.7 . . ?
O01 C01 H01A 127.7 . . ?
N01 C03 H03A 109.5 . . ?
N01 C03 H03B 109.5 . . ?
H03A C03 H03B 109.5 . . ?
N01 C03 H03C 109.5 . . ?
H03A C03 H03C 109.5 . . ?
H03B C03 H03C 109.5 . . ?
N01 C04 H04A 109.5 . . ?
N01 C04 H04B 109.5 . . ?
H04A C04 H04B 109.5 . . ?
N01 C04 H04C 109.5 . . ?
H04A C04 H04C 109.5 . . ?
H04B C04 H04C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        23.78
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.085

# Attachment '3-revised.cif'

data_dv
_database_code_depnum_ccdc_archive 'CCDC 714742'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H84 Cu2 N6 O18'
_chemical_formula_weight         1448.53

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.568(2)
_cell_length_b                   14.124(3)
_cell_length_c                   14.562(5)
_cell_angle_alpha                111.999(5)
_cell_angle_beta                 96.899(5)
_cell_angle_gamma                111.303(4)
_cell_volume                     1793.1(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1450
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      19.87

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9364
_exptl_absorpt_correction_T_max  0.9364
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6751
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         21.92
_reflns_number_total             4337
_reflns_number_gt                3152
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1167P)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         4337
_refine_ls_number_parameters     449
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1899
_refine_ls_wR_factor_gt          0.1487
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.007
_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
Cu Cu 0.99404(7) 0.58892(6) 0.49286(5) 0.0332(3) Uani 1 1 d . . .
O1 O 0.8444(4) 0.4759(3) 0.3611(3) 0.0426(11) Uani 1 1 d . . .
O2 O 0.8579(5) 0.3262(3) 0.3729(3) 0.0542(12) Uani 1 1 d . . .
O3 O 0.7274(4) 0.4239(3) 0.1633(3) 0.0467(11) Uani 1 1 d . . .
O4 O 1.2564(5) 0.6283(4) 0.2814(3) 0.0521(12) Uani 1 1 d . . .
O5 O 1.1411(4) 0.5833(4) 0.4228(3) 0.0473(11) Uani 1 1 d . . .
O6 O 1.1496(5) 0.4316(4) 0.4323(3) 0.0518(12) Uani 1 1 d . . .
N N 0.9965(5) 0.7434(4) 0.4908(4) 0.0386(12) Uani 1 1 d . . .
C1 C 0.8043(6) 0.3708(5) 0.3269(4) 0.0374(15) Uani 1 1 d . . .
C2 C 0.6866(7) 0.2895(5) 0.2296(5) 0.0424(16) Uani 1 1 d . . .
C3 C 0.6083(8) 0.1789(6) 0.2138(5) 0.0560(19) Uani 1 1 d . . .
H3A H 0.6336 0.1585 0.2644 0.067 Uiso 1 1 calc R . .
C4 C 0.4960(9) 0.0985(7) 0.1280(6) 0.078(3) Uani 1 1 d . . .
H4A H 0.4461 0.0253 0.1206 0.094 Uiso 1 1 calc R . .
C5 C 0.4582(9) 0.1280(7) 0.0523(6) 0.077(2) Uani 1 1 d . . .
H5A H 0.3808 0.0745 -0.0061 0.093 Uiso 1 1 calc R . .
C6 C 0.5331(8) 0.2347(6) 0.0624(6) 0.063(2) Uani 1 1 d . . .
H6A H 0.5075 0.2527 0.0101 0.076 Uiso 1 1 calc R . .
C7 C 0.6482(7) 0.3175(5) 0.1505(5) 0.0430(16) Uani 1 1 d . . .
C8 C 0.7235(7) 0.4428(6) 0.0717(5) 0.0524(18) Uani 1 1 d . . .
H8A H 0.6392 0.4518 0.0518 0.063 Uiso 1 1 calc R . .
H8B H 0.7225 0.3790 0.0141 0.063 Uiso 1 1 calc R . .
C9 C 0.8550(8) 0.5496(6) 0.1005(5) 0.0477(17) Uani 1 1 d . . .
C10 C 0.8473(8) 0.6470(6) 0.1026(5) 0.0559(19) Uani 1 1 d . . .
C11 C 0.9737(9) 0.7445(6) 0.1347(6) 0.061(2) Uani 1 1 d . . .
H11A H 0.9687 0.8093 0.1359 0.073 Uiso 1 1 calc R . .
C12 C 1.1062(8) 0.7502(6) 0.1648(5) 0.0559(19) Uani 1 1 d . . .
C13 C 1.1127(7) 0.6521(6) 0.1608(5) 0.0478(17) Uani 1 1 d . . .
C14 C 0.9884(7) 0.5512(5) 0.1280(5) 0.0448(17) Uani 1 1 d . . .
C15 C 0.7069(8) 0.6485(7) 0.0685(7) 0.077(2) Uani 1 1 d . . .
H15A H 0.7222 0.7258 0.0891 0.116 Uiso 1 1 calc R . .
H15B H 0.6415 0.6151 0.1004 0.116 Uiso 1 1 calc R . .
H15C H 0.6682 0.6057 -0.0055 0.116 Uiso 1 1 calc R . .
C16 C 1.2406(9) 0.8614(7) 0.2024(8) 0.096(3) Uani 1 1 d . . .
H16A H 1.2177 0.9134 0.1846 0.143 Uiso 1 1 calc R . .
H16B H 1.3096 0.8462 0.1700 0.143 Uiso 1 1 calc R . .
H16C H 1.2790 0.8946 0.2763 0.143 Uiso 1 1 calc R . .
C17 C 0.9983(7) 0.4456(5) 0.1232(5) 0.0500(18) Uani 1 1 d . . .
H17A H 1.0806 0.4430 0.1028 0.075 Uiso 1 1 calc R . .
H17B H 0.9145 0.3793 0.0734 0.075 Uiso 1 1 calc R . .
H17C H 1.0062 0.4473 0.1902 0.075 Uiso 1 1 calc R . .
C18 C 1.2554(8) 0.6518(6) 0.1937(6) 0.0571(19) Uani 1 1 d . . .
H18A H 1.2659 0.5938 0.1374 0.068 Uiso 1 1 calc R . .
H18B H 1.3331 0.7253 0.2124 0.068 Uiso 1 1 calc R . .
C19 C 1.3440(7) 0.5833(6) 0.3010(5) 0.0457(16) Uani 1 1 d . . .
C20 C 1.4611(7) 0.5932(7) 0.2650(6) 0.062(2) Uani 1 1 d . . .
H20A H 1.4828 0.6319 0.2251 0.075 Uiso 1 1 calc R . .
C21 C 1.5452(9) 0.5458(8) 0.2882(7) 0.080(3) Uani 1 1 d . . .
H21A H 1.6244 0.5535 0.2644 0.096 Uiso 1 1 calc R . .
C22 C 1.5155(9) 0.4880(8) 0.3451(7) 0.080(3) Uani 1 1 d . . .
H22A H 1.5733 0.4561 0.3600 0.096 Uiso 1 1 calc R . .
C23 C 1.3997(8) 0.4775(7) 0.3799(5) 0.059(2) Uani 1 1 d . . .
H23A H 1.3794 0.4368 0.4182 0.070 Uiso 1 1 calc R . .
C24 C 1.3108(6) 0.5238(5) 0.3616(5) 0.0416(16) Uani 1 1 d . . .
C25 C 1.1912(6) 0.5114(5) 0.4083(4) 0.0347(14) Uani 1 1 d . . .
C26 C 0.9790(9) 0.7584(6) 0.4066(5) 0.068(2) Uani 1 1 d . . .
H26A H 0.9636 0.6992 0.3432 0.082 Uiso 1 1 calc R . .
C27 C 0.9825(10) 0.8578(6) 0.4086(6) 0.077(3) Uani 1 1 d . . .
H27A H 0.9725 0.8647 0.3474 0.092 Uiso 1 1 calc R . .
C28 C 1.0003(6) 0.9462(5) 0.4987(5) 0.0385(15) Uani 1 1 d . . .
C29 C 1.0175(10) 0.9305(6) 0.5838(5) 0.082(3) Uani 1 1 d . . .
H29A H 1.0310 0.9878 0.6479 0.099 Uiso 1 1 calc R . .
C30 C 1.0154(10) 0.8287(6) 0.5766(5) 0.084(3) Uani 1 1 d . . .
H30A H 1.0283 0.8213 0.6374 0.101 Uiso 1 1 calc R . .
N01 N 0.9623(11) 0.8635(7) 0.8601(6) 0.100(3) Uani 1 1 d . . .
N02 N 1.5350(11) 0.8428(7) 0.5120(8) 0.120(3) Uani 1 1 d . . .
C06 C 1.4103(14) 0.8598(10) 0.5210(11) 0.150(5) Uani 1 1 d . . .
H06A H 1.3509 0.8349 0.4533 0.224 Uiso 1 1 calc R . .
H06B H 1.4378 0.9392 0.5626 0.224 Uiso 1 1 calc R . .
H06C H 1.3588 0.8167 0.5532 0.224 Uiso 1 1 calc R . .
C05 C 1.585(2) 0.8006(14) 0.5767(12) 0.216(9) Uani 1 1 d . . .
H05A H 1.5136 0.7259 0.5597 0.324 Uiso 1 1 calc R . .
H05B H 1.6028 0.8509 0.6481 0.324 Uiso 1 1 calc R . .
H05C H 1.6707 0.7967 0.5657 0.324 Uiso 1 1 calc R . .
C03 C 1.063(2) 0.8241(18) 0.8609(16) 0.258(11) Uani 1 1 d . . .
H03A H 1.1162 0.8520 0.9312 0.386 Uiso 1 1 calc R . .
H03B H 1.1254 0.8502 0.8240 0.386 Uiso 1 1 calc R . .
H03C H 1.0167 0.7423 0.8280 0.386 Uiso 1 1 calc R . .
C02 C 0.844(2) 0.7842(19) 0.8718(16) 0.299(14) Uani 1 1 d . . .
H02A H 0.8731 0.7361 0.8921 0.448 Uiso 1 1 calc R . .
H02B H 0.7697 0.7384 0.8071 0.448 Uiso 1 1 calc R . .
H02C H 0.8104 0.8246 0.9241 0.448 Uiso 1 1 calc R . .
O02 O 1.5708(17) 0.8865(10) 0.3807(10) 0.206(7) Uani 1 1 d . . .
O01 O 1.0985(19) 1.0008(14) 0.8416(12) 0.253(8) Uani 1 1 d D . .
O03 O 0.3777(11) 0.1141(10) -0.2015(7) 0.201(5) Uani 1 1 d . . .
C04 C 1.593(2) 0.8589(14) 0.4427(15) 0.169(8) Uani 1 1 d . . .
H04A H 1.6722 0.8444 0.4434 0.203 Uiso 1 1 calc R . .
C01 C 0.976(3) 0.9627(19) 0.8497(18) 0.40(3) Uani 1 1 d D . .
H01A H 0.9097 0.9918 0.8491 0.479 Uiso 1 1 calc R . .


_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
Cu O2 1.962(4) 2_766 ?
Cu O5 1.968(4) . ?
Cu O1 1.968(4) . ?
Cu O6 1.972(4) 2_766 ?
Cu N 2.185(5) . ?
Cu Cu 2.6426(13) 2_766 ?
O1 C1 1.253(7) . ?
O2 C1 1.286(7) . ?
O2 Cu 1.962(4) 2_766 ?
O3 C7 1.354(7) . ?
O3 C8 1.454(7) . ?
O4 C19 1.358(7) . ?
O4 C18 1.434(7) . ?
O5 C25 1.269(7) . ?
O6 C25 1.249(7) . ?
O6 Cu 1.972(4) 2_766 ?
N C30 1.301(8) . ?
N C26 1.322(8) . ?
C1 C2 1.480(8) . ?
C2 C3 1.388(8) . ?
C2 C7 1.413(8) . ?
C3 C4 1.364(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.381(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.364(10) . ?
C5 H5A 0.9300 . ?
C6 C7 1.399(9) . ?
C6 H6A 0.9300 . ?
C8 C9 1.498(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.396(9) . ?
C9 C14 1.408(9) . ?
C10 C11 1.390(10) . ?
C10 C15 1.517(10) . ?
C11 C12 1.380(10) . ?
C11 H11A 0.9300 . ?
C12 C13 1.391(9) . ?
C12 C16 1.527(10) . ?
C13 C14 1.402(9) . ?
C13 C18 1.528(9) . ?
C14 C17 1.509(8) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.383(9) . ?
C19 C24 1.423(8) . ?
C20 C21 1.372(10) . ?
C20 H20A 0.9300 . ?
C21 C22 1.352(11) . ?
C21 H21A 0.9300 . ?
C22 C23 1.361(10) . ?
C22 H22A 0.9300 . ?
C23 C24 1.377(9) . ?
C23 H23A 0.9300 . ?
C24 C25 1.492(8) . ?
C26 C27 1.381(9) . ?
C26 H26A 0.9300 . ?
C27 C28 1.363(9) . ?
C27 H27A 0.9300 . ?
C28 C29 1.341(9) . ?
C28 C28 1.509(11) 2_776 ?
C29 C30 1.392(9) . ?
C29 H29A 0.9300 . ?
C30 H30A 0.9300 . ?
N01 C03 1.366(17) . ?
N01 C02 1.42(2) . ?
N01 C01 1.42(2) . ?
N02 C04 1.291(17) . ?
N02 C05 1.430(16) . ?
N02 C06 1.435(15) . ?
C06 H06A 0.9600 . ?
C06 H06B 0.9600 . ?
C06 H06C 0.9600 . ?
C05 H05A 0.9600 . ?
C05 H05B 0.9600 . ?
C05 H05C 0.9600 . ?
C03 H03A 0.9600 . ?
C03 H03B 0.9600 . ?
C03 H03C 0.9600 . ?
C02 H02A 0.9600 . ?
C02 H02B 0.9600 . ?
C02 H02C 0.9600 . ?
O02 C04 1.14(2) . ?
O01 C01 1.25(2) . ?
C04 H04A 0.9300 . ?
C01 H01A 0.9300 . ?

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 Cu O5 89.21(19) 2_766 . ?
O2 Cu O1 168.14(16) 2_766 . ?
O5 Cu O1 90.29(18) . . ?
O2 Cu O6 88.4(2) 2_766 2_766 ?
O5 Cu O6 167.98(16) . 2_766 ?
O1 Cu O6 89.61(19) . 2_766 ?
O2 Cu N 93.17(18) 2_766 . ?
O5 Cu N 96.55(17) . . ?
O1 Cu N 98.66(17) . . ?
O6 Cu N 95.35(17) 2_766 . ?
O2 Cu Cu 82.91(12) 2_766 2_766 ?
O5 Cu Cu 83.08(12) . 2_766 ?
O1 Cu Cu 85.26(12) . 2_766 ?
O6 Cu Cu 84.94(12) 2_766 2_766 ?
N Cu Cu 176.07(14) . 2_766 ?
C1 O1 Cu 122.9(4) . . ?
C1 O2 Cu 125.2(4) . 2_766 ?
C7 O3 C8 118.1(5) . . ?
C19 O4 C18 117.4(5) . . ?
C25 O5 Cu 124.5(4) . . ?
C25 O6 Cu 122.6(4) . 2_766 ?
C30 N C26 115.4(5) . . ?
C30 N Cu 119.9(4) . . ?
C26 N Cu 124.7(4) . . ?
O1 C1 O2 123.7(6) . . ?
O1 C1 C2 120.5(5) . . ?
O2 C1 C2 115.8(5) . . ?
C3 C2 C7 117.1(6) . . ?
C3 C2 C1 119.0(5) . . ?
C7 C2 C1 123.9(5) . . ?
C4 C3 C2 123.4(6) . . ?
C4 C3 H3A 118.3 . . ?
C2 C3 H3A 118.3 . . ?
C3 C4 C5 118.6(7) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
C6 C5 C4 120.6(7) . . ?
C6 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
C5 C6 C7 120.9(7) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
O3 C7 C6 123.2(6) . . ?
O3 C7 C2 117.6(5) . . ?
C6 C7 C2 119.2(6) . . ?
O3 C8 C9 106.3(5) . . ?
O3 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
O3 C8 H8B 110.5 . . ?
C9 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
C10 C9 C14 120.0(6) . . ?
C10 C9 C8 121.4(6) . . ?
C14 C9 C8 118.6(6) . . ?
C11 C10 C9 118.1(7) . . ?
C11 C10 C15 119.5(7) . . ?
C9 C10 C15 122.4(7) . . ?
C12 C11 C10 123.5(7) . . ?
C12 C11 H11A 118.2 . . ?
C10 C11 H11A 118.2 . . ?
C11 C12 C13 117.8(6) . . ?
C11 C12 C16 120.6(7) . . ?
C13 C12 C16 121.5(7) . . ?
C12 C13 C14 121.0(6) . . ?
C12 C13 C18 121.0(6) . . ?
C14 C13 C18 118.1(6) . . ?
C13 C14 C9 119.5(6) . . ?
C13 C14 C17 119.9(6) . . ?
C9 C14 C17 120.6(6) . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 C18 C13 107.0(5) . . ?
O4 C18 H18A 110.3 . . ?
C13 C18 H18A 110.3 . . ?
O4 C18 H18B 110.3 . . ?
C13 C18 H18B 110.3 . . ?
H18A C18 H18B 108.6 . . ?
O4 C19 C20 123.0(6) . . ?
O4 C19 C24 117.0(5) . . ?
C20 C19 C24 120.0(6) . . ?
C21 C20 C19 119.7(7) . . ?
C21 C20 H20A 120.2 . . ?
C19 C20 H20A 120.2 . . ?
C22 C21 C20 121.5(7) . . ?
C22 C21 H21A 119.2 . . ?
C20 C21 H21A 119.2 . . ?
C21 C22 C23 118.8(7) . . ?
C21 C22 H22A 120.6 . . ?
C23 C22 H22A 120.6 . . ?
C22 C23 C24 123.5(6) . . ?
C22 C23 H23A 118.2 . . ?
C24 C23 H23A 118.2 . . ?
C23 C24 C19 116.4(6) . . ?
C23 C24 C25 118.6(6) . . ?
C19 C24 C25 124.9(5) . . ?
O6 C25 O5 124.8(5) . . ?
O6 C25 C24 116.9(5) . . ?
O5 C25 C24 118.3(5) . . ?
N C26 C27 123.0(6) . . ?
N C26 H26A 118.5 . . ?
C27 C26 H26A 118.5 . . ?
C28 C27 C26 121.2(6) . . ?
C28 C27 H27A 119.4 . . ?
C26 C27 H27A 119.4 . . ?
C29 C28 C27 115.6(6) . . ?
C29 C28 C28 122.8(7) . 2_776 ?
C27 C28 C28 121.6(7) . 2_776 ?
C28 C29 C30 120.3(6) . . ?
C28 C29 H29A 119.9 . . ?
C30 C29 H29A 119.9 . . ?
N C30 C29 124.5(6) . . ?
N C30 H30A 117.7 . . ?
C29 C30 H30A 117.7 . . ?
C03 N01 C02 104.8(15) . . ?
C03 N01 C01 126.8(16) . . ?
C02 N01 C01 128.4(15) . . ?
C04 N02 C05 122.3(17) . . ?
C04 N02 C06 119.8(15) . . ?
C05 N02 C06 117.7(13) . . ?
N02 C06 H06A 109.5 . . ?
N02 C06 H06B 109.5 . . ?
H06A C06 H06B 109.5 . . ?
N02 C06 H06C 109.5 . . ?
H06A C06 H06C 109.5 . . ?
H06B C06 H06C 109.5 . . ?
N02 C05 H05A 109.5 . . ?
N02 C05 H05B 109.5 . . ?
H05A C05 H05B 109.5 . . ?
N02 C05 H05C 109.5 . . ?
H05A C05 H05C 109.5 . . ?
H05B C05 H05C 109.5 . . ?
N01 C03 H03A 109.5 . . ?
N01 C03 H03B 109.5 . . ?
H03A C03 H03B 109.5 . . ?
N01 C03 H03C 109.5 . . ?
H03A C03 H03C 109.5 . . ?
H03B C03 H03C 109.5 . . ?
N01 C02 H02A 109.5 . . ?
N01 C02 H02B 109.5 . . ?
H02A C02 H02B 109.5 . . ?
N01 C02 H02C 109.5 . . ?
H02A C02 H02C 109.5 . . ?
H02B C02 H02C 109.5 . . ?
O02 C04 N02 135(3) . . ?
O02 C04 H04A 112.3 . . ?
N02 C04 H04A 112.3 . . ?
O01 C01 N01 102.5(16) . . ?
O01 C01 H01A 128.8 . . ?
N01 C01 H01A 128.8 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        21.92
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.134

# Attachment '1-revised.cif'

data_test
_database_code_depnum_ccdc_archive 'CCDC 721690'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H60 Cu2 N4 O12 S4'
_chemical_formula_weight         1236.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.4913(9)
_cell_length_b                   11.0159(9)
_cell_length_c                   12.4366(10)
_cell_angle_alpha                89.1180(10)
_cell_angle_beta                 89.0410(10)
_cell_angle_gamma                79.8570(10)
_cell_volume                     1414.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3218
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.22

_exptl_crystal_description       block
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             642
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8306
_exptl_absorpt_correction_T_max  0.8689
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8377
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         27.57
_reflns_number_total             6148
_reflns_number_gt                4928
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0950P)²+0.3744P] 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         6148
_refine_ls_number_parameters     341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1535
_refine_ls_wR_factor_gt          0.1396
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.028
_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
Cu1 Cu 0.44597(3) 0.48183(3) -0.09174(3) 0.03188(13) Uani 1 1 d . . .
S1 S 0.35853(9) 0.32948(8) 0.33956(7) 0.0500(2) Uani 1 1 d . . .
S2 S 0.65956(9) 0.15519(7) 0.24660(6) 0.0426(2) Uani 1 1 d . . .
O1 O 0.3070(2) 0.4462(2) 0.00494(18) 0.0469(5) Uani 1 1 d . . .
O2 O 0.3962(2) 0.4767(2) 0.16248(17) 0.0419(5) Uani 1 1 d . . .
O3 O 0.6263(2) 0.33866(18) 0.08830(17) 0.0392(5) Uani 1 1 d . . .
O4 O 0.5355(2) 0.31079(19) -0.06863(17) 0.0445(5) Uani 1 1 d . . .
O5 O 0.3390(2) 0.4503(2) -0.23038(18) 0.0489(6) Uani 1 1 d . . .
O6 O 0.9495(6) -0.1700(5) 0.3859(6) 0.154(2) Uani 1 1 d . . .
N1 N 0.2436(3) 0.5221(3) -0.3849(2) 0.0584(8) Uani 1 1 d . . .
N2 N 1.0163(5) -0.1516(6) 0.2167(7) 0.125(2) Uani 1 1 d . . .
C1 C 0.3106(3) 0.4425(3) 0.1061(2) 0.0357(6) Uani 1 1 d . . .
C2 C 0.2035(3) 0.3900(3) 0.1622(2) 0.0361(6) Uani 1 1 d . . .
C3 C 0.0896(3) 0.3915(3) 0.1057(3) 0.0495(8) Uani 1 1 d . . .
H3A H 0.0822 0.4277 0.0376 0.059 Uiso 1 1 calc R . .
C4 C -0.0120(4) 0.3415(4) 0.1468(3) 0.0598(10) Uani 1 1 d . . .
H4A H -0.0883 0.3461 0.1087 0.072 Uiso 1 1 calc R . .
C5 C 0.0023(4) 0.2839(4) 0.2471(3) 0.0607(10) Uani 1 1 d . . .
H5A H -0.0645 0.2477 0.2760 0.073 Uiso 1 1 calc R . .
C6 C 0.1137(4) 0.2797(4) 0.3041(3) 0.0522(9) Uani 1 1 d . . .
H6A H 0.1211 0.2405 0.3711 0.063 Uiso 1 1 calc R . .
C7 C 0.2159(3) 0.3327(3) 0.2642(3) 0.0374(6) Uani 1 1 d . . .
C8 C 0.3652(4) 0.1915(3) 0.4217(3) 0.0532(9) Uani 1 1 d . . .
H8A H 0.2896 0.1991 0.4687 0.064 Uiso 1 1 calc R . .
H8B H 0.3667 0.1204 0.3764 0.064 Uiso 1 1 calc R . .
C9 C 0.4854(4) 0.1757(3) 0.4870(3) 0.0469(8) Uani 1 1 d . . .
C10 C 0.4763(4) 0.2317(4) 0.5870(3) 0.0580(10) Uani 1 1 d . . .
H10A H 0.3977 0.2782 0.6090 0.070 Uiso 1 1 calc R . .
C11 C 0.5811(5) 0.2198(4) 0.6542(3) 0.0691(12) Uani 1 1 d . . .
H11A H 0.5733 0.2590 0.7203 0.083 Uiso 1 1 calc R . .
C12 C 0.6961(5) 0.1504(4) 0.6234(3) 0.0688(12) Uani 1 1 d . . .
H12A H 0.7667 0.1409 0.6689 0.083 Uiso 1 1 calc R . .
C13 C 0.7075(4) 0.0934(4) 0.5230(3) 0.0588(10) Uani 1 1 d . . .
H13A H 0.7862 0.0461 0.5023 0.071 Uiso 1 1 calc R . .
C14 C 0.6034(4) 0.1063(3) 0.4539(3) 0.0465(8) Uani 1 1 d . . .
C15 C 0.6236(4) 0.0423(3) 0.3468(3) 0.0510(8) Uani 1 1 d . . .
H15A H 0.5462 0.0114 0.3273 0.061 Uiso 1 1 calc R . .
H15B H 0.6949 -0.0267 0.3508 0.061 Uiso 1 1 calc R . .
C16 C 0.6632(3) 0.0727(3) 0.1250(2) 0.0322(6) Uani 1 1 d . . .
C17 C 0.6906(3) -0.0560(3) 0.1260(3) 0.0418(7) Uani 1 1 d . . .
H17A H 0.7066 -0.0979 0.1912 0.050 Uiso 1 1 calc R . .
C18 C 0.6944(3) -0.1226(3) 0.0326(3) 0.0457(8) Uani 1 1 d . . .
H18A H 0.7135 -0.2083 0.0355 0.055 Uiso 1 1 calc R . .
C19 C 0.6702(3) -0.0627(3) -0.0648(3) 0.0476(8) Uani 1 1 d . . .
H19A H 0.6739 -0.1072 -0.1281 0.057 Uiso 1 1 calc R . .
C20 C 0.6406(3) 0.0639(3) -0.0670(3) 0.0413(7) Uani 1 1 d . . .
H20A H 0.6222 0.1042 -0.1326 0.050 Uiso 1 1 calc R . .
C21 C 0.6371(3) 0.1344(3) 0.0260(2) 0.0321(6) Uani 1 1 d . . .
C22 C 0.5972(3) 0.2716(3) 0.0142(2) 0.0329(6) Uani 1 1 d . . .
C23 C 0.3294(4) 0.5204(3) -0.3091(3) 0.0493(8) Uani 1 1 d . . .
H23A H 0.3867 0.5758 -0.3152 0.059 Uiso 1 1 calc R . .
C24 C 0.1481(5) 0.4430(5) -0.3785(5) 0.0877(16) Uani 1 1 d . . .
H24A H 0.1696 0.3835 -0.3216 0.132 Uiso 1 1 calc R . .
H24B H 0.1465 0.4012 -0.4455 0.132 Uiso 1 1 calc R . .
H24C H 0.0644 0.4917 -0.3642 0.132 Uiso 1 1 calc R . .
C25 C 0.2367(7) 0.6078(5) -0.4751(4) 0.102(2) Uani 1 1 d . . .
H25A H 0.1508 0.6552 -0.4790 0.153 Uiso 1 1 calc R . .
H25B H 0.2570 0.5627 -0.5404 0.153 Uiso 1 1 calc R . .
H25C H 0.2977 0.6621 -0.4655 0.153 Uiso 1 1 calc R . .
C26 C 0.9674(10) -0.1088(11) 0.3074(10) 0.160(4) Uiso 1 1 d . . .
H26A H 0.9439 -0.0236 0.3126 0.192 Uiso 1 1 calc R . .
C27 C 1.0645(11) -0.2668(12) 0.1859(10) 0.204(5) Uiso 1 1 d . . .
H27A H 1.0566 -0.3232 0.2443 0.306 Uiso 1 1 calc R . .
H27B H 1.1542 -0.2723 0.1662 0.306 Uiso 1 1 calc R . .
H27C H 1.0173 -0.2873 0.1254 0.306 Uiso 1 1 calc R . .
C28 C 1.0197(13) -0.0624(12) 0.1324(10) 0.234(6) Uiso 1 1 d . . .
H28A H 0.9847 0.0183 0.1587 0.351 Uiso 1 1 calc R . .
H28B H 0.9690 -0.0810 0.0733 0.351 Uiso 1 1 calc R . .
H28C H 1.1076 -0.0645 0.1087 0.351 Uiso 1 1 calc R . .


_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
Cu1 O1 1.963(2) . ?
Cu1 O4 1.971(2) . ?
Cu1 O2 1.982(2) 2_665 ?
Cu1 O3 1.990(2) 2_665 ?
Cu1 O5 2.139(2) . ?
Cu1 Cu1 2.6320(7) 2_665 ?
S1 C7 1.774(3) . ?
S1 C8 1.810(3) . ?
S2 C16 1.773(3) . ?
S2 C15 1.828(3) . ?
O1 C1 1.259(4) . ?
O2 C1 1.261(4) . ?
O2 Cu1 1.982(2) 2_665 ?
O3 C22 1.264(3) . ?
O3 Cu1 1.990(2) 2_665 ?
O4 C22 1.256(4) . ?
O5 C23 1.232(4) . ?
O6 C26 1.210(11) . ?
N1 C23 1.312(4) . ?
N1 C24 1.439(6) . ?
N1 C25 1.449(5) . ?
N2 C26 1.292(11) . ?
N2 C27 1.339(12) . ?
N2 C28 1.431(12) . ?
C1 C2 1.508(4) . ?
C2 C3 1.393(5) . ?
C2 C7 1.405(4) . ?
C3 C4 1.371(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.390(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.370(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.390(5) . ?
C6 H6A 0.9300 . ?
C8 C9 1.494(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.391(5) . ?
C9 C14 1.395(5) . ?
C10 C11 1.379(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.362(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.400(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.388(5) . ?
C13 H13A 0.9300 . ?
C14 C15 1.511(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.396(4) . ?
C16 C21 1.405(4) . ?
C17 C18 1.379(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.376(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.375(4) . ?
C19 H19A 0.9300 . ?
C20 C21 1.399(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.501(4) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?

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 Cu1 O4 88.37(10) . . ?
O1 Cu1 O2 168.57(9) . 2_665 ?
O4 Cu1 O2 90.16(10) . 2_665 ?
O1 Cu1 O3 90.80(10) . 2_665 ?
O4 Cu1 O3 168.44(9) . 2_665 ?
O2 Cu1 O3 88.37(9) 2_665 2_665 ?
O1 Cu1 O5 91.50(10) . . ?
O4 Cu1 O5 97.69(9) . . ?
O2 Cu1 O5 99.93(9) 2_665 . ?
O3 Cu1 O5 93.85(9) 2_665 . ?
O1 Cu1 Cu1 82.07(7) . 2_665 ?
O4 Cu1 Cu1 82.99(6) . 2_665 ?
O2 Cu1 Cu1 86.51(6) 2_665 2_665 ?
O3 Cu1 Cu1 85.48(6) 2_665 2_665 ?
O5 Cu1 Cu1 173.52(7) . 2_665 ?
C7 S1 C8 102.98(16) . . ?
C16 S2 C15 102.40(15) . . ?
C1 O1 Cu1 125.7(2) . . ?
C1 O2 Cu1 119.50(19) . 2_665 ?
C22 O3 Cu1 120.96(19) . 2_665 ?
C22 O4 Cu1 124.99(19) . . ?
C23 O5 Cu1 121.9(2) . . ?
C23 N1 C24 121.0(4) . . ?
C23 N1 C25 121.5(4) . . ?
C24 N1 C25 117.4(4) . . ?
C26 N2 C27 131.4(10) . . ?
C26 N2 C28 115.7(9) . . ?
C27 N2 C28 112.8(10) . . ?
O1 C1 O2 125.6(3) . . ?
O1 C1 C2 115.9(3) . . ?
O2 C1 C2 118.5(3) . . ?
C3 C2 C7 118.8(3) . . ?
C3 C2 C1 117.4(3) . . ?
C7 C2 C1 123.7(3) . . ?
C4 C3 C2 122.6(3) . . ?
C4 C3 H3A 118.7 . . ?
C2 C3 H3A 118.7 . . ?
C3 C4 C5 118.0(3) . . ?
C3 C4 H4A 121.0 . . ?
C5 C4 H4A 121.0 . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 H5A 119.6 . . ?
C4 C5 H5A 119.6 . . ?
C5 C6 C7 121.5(3) . . ?
C5 C6 H6A 119.3 . . ?
C7 C6 H6A 119.3 . . ?
C6 C7 C2 118.3(3) . . ?
C6 C7 S1 121.2(3) . . ?
C2 C7 S1 120.5(2) . . ?
C9 C8 S1 108.2(2) . . ?
C9 C8 H8A 110.1 . . ?
S1 C8 H8A 110.1 . . ?
C9 C8 H8B 110.1 . . ?
S1 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 C14 119.2(3) . . ?
C10 C9 C8 117.2(3) . . ?
C14 C9 C8 123.6(3) . . ?
C11 C10 C9 121.5(4) . . ?
C11 C10 H10A 119.3 . . ?
C9 C10 H10A 119.3 . . ?
C12 C11 C10 119.7(4) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C11 C12 C13 119.7(4) . . ?
C11 C12 H12A 120.2 . . ?
C13 C12 H12A 120.2 . . ?
C14 C13 C12 121.1(4) . . ?
C14 C13 H13A 119.4 . . ?
C12 C13 H13A 119.4 . . ?
C13 C14 C9 118.7(3) . . ?
C13 C14 C15 117.9(3) . . ?
C9 C14 C15 123.3(3) . . ?
C14 C15 S2 107.7(2) . . ?
C14 C15 H15A 110.2 . . ?
S2 C15 H15A 110.2 . . ?
C14 C15 H15B 110.2 . . ?
S2 C15 H15B 110.2 . . ?
H15A C15 H15B 108.5 . . ?
C17 C16 C21 118.5(3) . . ?
C17 C16 S2 120.3(2) . . ?
C21 C16 S2 121.2(2) . . ?
C18 C17 C16 121.6(3) . . ?
C18 C17 H17A 119.2 . . ?
C16 C17 H17A 119.2 . . ?
C19 C18 C17 120.3(3) . . ?
C19 C18 H18A 119.9 . . ?
C17 C18 H18A 119.9 . . ?
C20 C19 C18 118.9(3) . . ?
C20 C19 H19A 120.6 . . ?
C18 C19 H19A 120.6 . . ?
C19 C20 C21 122.4(3) . . ?
C19 C20 H20A 118.8 . . ?
C21 C20 H20A 118.8 . . ?
C20 C21 C16 118.4(3) . . ?
C20 C21 C22 117.5(3) . . ?
C16 C21 C22 124.0(2) . . ?
O4 C22 O3 124.9(3) . . ?
O4 C22 C21 117.0(3) . . ?
O3 C22 C21 118.1(2) . . ?
O5 C23 N1 124.3(3) . . ?
O5 C23 H23A 117.9 . . ?
N1 C23 H23A 117.9 . . ?
N1 C24 H24A 109.5 . . ?
N1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N1 C25 H25A 109.5 . . ?
N1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O6 C26 N2 125.6(11) . . ?
O6 C26 H26A 117.2 . . ?
N2 C26 H26A 117.2 . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N2 C28 H28A 109.5 . . ?
N2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.939
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.939
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.086

# Attachment '4-revised.cif'

data_test3
_database_code_depnum_ccdc_archive 'CCDC 721691'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H58 Cu2 N8 O13 S4'
_chemical_formula_weight         1258.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 '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                   17.258(5)
_cell_length_b                   10.889(3)
_cell_length_c                   31.014(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.417(4)
_cell_angle_gamma                90.00
_cell_volume                     5802(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3642
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      24.91

_exptl_crystal_description       block
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2608
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8713
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16412
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.32
_diffrn_reflns_theta_max         27.41
_reflns_number_total             6437
_reflns_number_gt                4534
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 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)+(0.0649P)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         6437
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.1027
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.007
_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
Cu Cu 0.208120(18) 0.72559(3) 0.033053(9) 0.03355(11) Uani 1 1 d . . .
N3 N 0.10660(18) 0.7289(3) 0.15320(8) 0.0576(7) Uani 1 1 d . . .
N4 N 0.56136(19) 0.9030(3) 0.10421(10) 0.0674(8) Uani 1 1 d . . .
O01 O 0.5000 0.9710(7) 0.2500 0.171(3) Uani 1 2 d S . .
H01A H 0.5424 0.9186 0.2429 0.205 Uiso 0.50 1 calc PR . .
H01B H 0.5195 1.0520 0.2583 0.205 Uiso 0.50 1 calc PR . .
O1 O 0.24485(12) 0.89213(18) 0.05113(6) 0.0473(5) Uani 1 1 d . . .
O2 O 0.31366(13) 0.93549(18) -0.00466(6) 0.0504(5) Uani 1 1 d . . .
O3 O 0.19385(11) 1.1601(2) 0.43781(6) 0.0481(5) Uani 1 1 d . . .
O4 O 0.12454(12) 1.2026(2) 0.49356(6) 0.0519(6) Uani 1 1 d . . .
O5 O 0.13516(13) 0.7029(2) 0.08416(6) 0.0518(5) Uani 1 1 d . . .
O6 O 0.5577(3) 0.8691(3) 0.17592(11) 0.1264(14) Uani 1 1 d . . .
S1 S 0.30080(5) 0.98321(9) 0.13273(2) 0.0588(2) Uani 1 1 d . . .
S2 S 0.12934(5) 1.11619(8) 0.35377(2) 0.0490(2) Uani 1 1 d . . .
C1 C 0.28826(16) 0.9605(3) 0.03104(8) 0.0382(6) Uani 1 1 d . . .
C2 C 0.31023(16) 1.0828(3) 0.05132(9) 0.0411(7) Uani 1 1 d . . .
C6 C 0.3285(2) 1.1789(3) 0.02473(11) 0.0574(8) Uani 1 1 d . . .
H6 H 0.3306 1.1657 -0.0048 0.069 Uiso 1 1 calc R . .
C5 C 0.3437(3) 1.2955(3) 0.04223(14) 0.0757(11) Uani 1 1 d . . .
H5 H 0.3560 1.3611 0.0249 0.091 Uiso 1 1 calc R . .
C4 C 0.3397(2) 1.3095(4) 0.08556(14) 0.0758(11) Uani 1 1 d . . .
H4 H 0.3471 1.3880 0.0971 0.091 Uiso 1 1 calc R . .
N1 N 0.32599(18) 1.2183(3) 0.11274(9) 0.0633(8) Uani 1 1 d . . .
C3 C 0.31262(17) 1.1061(3) 0.09625(9) 0.0447(7) Uani 1 1 d . . .
C7 C 0.3332(2) 1.0523(5) 0.18535(10) 0.0796(12) Uani 1 1 d . . .
H7A H 0.3769 1.0058 0.1989 0.095 Uiso 1 1 calc R . .
H7B H 0.3508 1.1355 0.1809 0.095 Uiso 1 1 calc R . .
C8 C 0.2689(2) 1.0544(3) 0.21514(9) 0.0544(8) Uani 1 1 d . . .
C9 C 0.2707(2) 0.9757(4) 0.25065(10) 0.0678(10) Uani 1 1 d . . .
H9A H 0.3118 0.9208 0.2559 0.081 Uiso 1 1 calc R . .
C10 C 0.2124(2) 0.9785(4) 0.27800(10) 0.0660(10) Uani 1 1 d . . .
H10A H 0.2147 0.9253 0.3015 0.079 Uiso 1 1 calc R . .
C11 C 0.1500(2) 1.0593(3) 0.27113(9) 0.0532(8) Uani 1 1 d . . .
C12 C 0.1490(2) 1.1374(3) 0.23589(10) 0.0595(9) Uani 1 1 d . . .
H12A H 0.1082 1.1930 0.2307 0.071 Uiso 1 1 calc R . .
C13 C 0.2070(2) 1.1345(3) 0.20828(10) 0.0606(9) Uani 1 1 d . . .
H13A H 0.2044 1.1874 0.1847 0.073 Uiso 1 1 calc R . .
C14 C 0.0866(2) 1.0620(4) 0.30106(9) 0.0693(11) Uani 1 1 d . . .
H14A H 0.0650 0.9804 0.3038 0.083 Uiso 1 1 calc R . .
H14B H 0.0452 1.1167 0.2898 0.083 Uiso 1 1 calc R . .
C15 C 0.05115(16) 1.0940(2) 0.38581(8) 0.0374(6) Uani 1 1 d . . .
N2 N -0.01561(14) 1.0527(2) 0.36484(8) 0.0489(6) Uani 1 1 d . . .
C20 C -0.07636(19) 1.0339(3) 0.38775(11) 0.0563(8) Uani 1 1 d . . .
H20A H -0.1224 1.0055 0.3731 0.068 Uiso 1 1 calc R . .
C19 C -0.07497(19) 1.0539(3) 0.43138(11) 0.0592(9) Uani 1 1 d . . .
H19A H -0.1185 1.0384 0.4461 0.071 Uiso 1 1 calc R . .
C18 C -0.00692(18) 1.0977(3) 0.45294(9) 0.0505(8) Uani 1 1 d . . .
H18A H -0.0046 1.1131 0.4825 0.061 Uiso 1 1 calc R . .
C16 C 0.05808(16) 1.1188(2) 0.43091(8) 0.0368(6) Uani 1 1 d . . .
C17 C 0.13112(16) 1.1638(2) 0.45563(8) 0.0374(6) Uani 1 1 d . . .
C21 C 0.1547(2) 0.7200(3) 0.12283(10) 0.0516(8) Uani 1 1 d . . .
H21A H 0.2076 0.7273 0.1313 0.062 Uiso 1 1 calc R . .
C22 C 0.0237(2) 0.7210(4) 0.14255(15) 0.0847(13) Uani 1 1 d . . .
H22A H 0.0128 0.7071 0.1120 0.127 Uiso 1 1 calc R . .
H22B H -0.0003 0.7965 0.1503 0.127 Uiso 1 1 calc R . .
H22C H 0.0032 0.6543 0.1583 0.127 Uiso 1 1 calc R . .
C23 C 0.1337(4) 0.7531(5) 0.19810(13) 0.125(2) Uani 1 1 d . . .
H23A H 0.1896 0.7512 0.2016 0.188 Uiso 1 1 calc R . .
H23B H 0.1136 0.6917 0.2162 0.188 Uiso 1 1 calc R . .
H23C H 0.1159 0.8327 0.2062 0.188 Uiso 1 1 calc R . .
C24 C 0.5257(3) 0.8900(4) 0.13989(17) 0.0884(13) Uani 1 1 d . . .
H24A H 0.4717 0.8975 0.1373 0.106 Uiso 1 1 calc R . .
C25 C 0.6444(2) 0.8877(4) 0.10575(14) 0.0862(12) Uani 1 1 d . . .
H25A H 0.6667 0.8925 0.1353 0.129 Uiso 1 1 calc R . .
H25B H 0.6660 0.9513 0.0891 0.129 Uiso 1 1 calc R . .
H25C H 0.6560 0.8090 0.0940 0.129 Uiso 1 1 calc R . .
C26 C 0.5195(3) 0.9335(4) 0.06278(13) 0.0899(13) Uani 1 1 d . . .
H26A H 0.4646 0.9343 0.0656 0.135 Uiso 1 1 calc R . .
H26B H 0.5307 0.8732 0.0416 0.135 Uiso 1 1 calc R . .
H26C H 0.5356 1.0130 0.0537 0.135 Uiso 1 1 calc R . .


_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
Cu O4 1.964(2) 6_575 ?
Cu O3 1.974(2) 4_545 ?
Cu O2 1.983(2) 7_565 ?
Cu O1 1.9844(19) . ?
Cu O5 2.130(2) . ?
Cu Cu 2.6711(8) 7_565 ?
N3 C21 1.316(4) . ?
N3 C22 1.441(5) . ?
N3 C23 1.451(5) . ?
N4 C24 1.324(5) . ?
N4 C25 1.440(5) . ?
N4 C26 1.452(5) . ?
O01 H01A 0.9700 . ?
O01 H01B 0.9700 . ?
O1 C1 1.261(3) . ?
O2 C1 1.258(3) . ?
O2 Cu 1.983(2) 7_565 ?
O3 C17 1.262(3) . ?
O3 Cu 1.9743(19) 4 ?
O4 C17 1.265(3) . ?
O4 Cu 1.964(2) 6_576 ?
O5 C21 1.229(4) . ?
O6 C24 1.221(5) . ?
S1 C3 1.777(3) . ?
S1 C7 1.836(3) . ?
S2 C15 1.766(3) . ?
S2 C14 1.827(3) . ?
C1 C2 1.506(4) . ?
C2 C6 1.387(4) . ?
C2 C3 1.413(4) . ?
C6 C5 1.396(5) . ?
C6 H6 0.9300 . ?
C5 C4 1.360(5) . ?
C5 H5 0.9300 . ?
C4 N1 1.338(5) . ?
C4 H4 0.9300 . ?
N1 C3 1.336(4) . ?
C7 C8 1.510(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C13 1.381(5) . ?
C8 C9 1.393(4) . ?
C9 C10 1.377(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.390(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.384(4) . ?
C11 C14 1.501(4) . ?
C12 C13 1.378(4) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N2 1.346(3) . ?
C15 C16 1.418(4) . ?
N2 C20 1.337(4) . ?
C20 C19 1.368(4) . ?
C20 H20A 0.9300 . ?
C19 C18 1.380(4) . ?
C19 H19A 0.9300 . ?
C18 C16 1.387(4) . ?
C18 H18A 0.9300 . ?
C16 C17 1.495(4) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Cu O3 167.46(8) 6_575 4_545 ?
O4 Cu O2 88.72(9) 6_575 7_565 ?
O3 Cu O2 90.13(9) 4_545 7_565 ?
O4 Cu O1 90.50(9) 6_575 . ?
O3 Cu O1 87.92(9) 4_545 . ?
O2 Cu O1 167.45(8) 7_565 . ?
O4 Cu O5 93.40(9) 6_575 . ?
O3 Cu O5 99.13(8) 4_545 . ?
O2 Cu O5 97.32(8) 7_565 . ?
O1 Cu O5 95.24(8) . . ?
O4 Cu Cu 82.01(6) 6_575 7_565 ?
O3 Cu Cu 85.45(6) 4_545 7_565 ?
O2 Cu Cu 85.92(6) 7_565 7_565 ?
O1 Cu Cu 81.57(6) . 7_565 ?
O5 Cu Cu 174.35(6) . 7_565 ?
C21 N3 C22 120.8(3) . . ?
C21 N3 C23 122.2(4) . . ?
C22 N3 C23 117.0(4) . . ?
C24 N4 C25 120.0(4) . . ?
C24 N4 C26 122.2(4) . . ?
C25 N4 C26 117.8(3) . . ?
H01A O01 H01B 110.2 . . ?
C1 O1 Cu 126.05(17) . . ?
C1 O2 Cu 120.99(19) . 7_565 ?
C17 O3 Cu 121.43(17) . 4 ?
C17 O4 Cu 125.99(19) . 6_576 ?
C21 O5 Cu 125.6(2) . . ?
C3 S1 C7 102.35(18) . . ?
C15 S2 C14 101.19(14) . . ?
O2 C1 O1 125.4(3) . . ?
O2 C1 C2 117.6(3) . . ?
O1 C1 C2 117.0(2) . . ?
C6 C2 C3 117.6(3) . . ?
C6 C2 C1 118.8(3) . . ?
C3 C2 C1 123.6(3) . . ?
C2 C6 C5 120.0(3) . . ?
C2 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C4 C5 C6 117.5(4) . . ?
C4 C5 H5 121.3 . . ?
C6 C5 H5 121.3 . . ?
N1 C4 C5 124.6(3) . . ?
N1 C4 H4 117.7 . . ?
C5 C4 H4 117.7 . . ?
C3 N1 C4 118.2(3) . . ?
N1 C3 C2 122.0(3) . . ?
N1 C3 S1 118.1(2) . . ?
C2 C3 S1 119.9(2) . . ?
C8 C7 S1 111.7(2) . . ?
C8 C7 H7A 109.3 . . ?
S1 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
S1 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C13 C8 C9 118.0(3) . . ?
C13 C8 C7 121.2(3) . . ?
C9 C8 C7 120.7(3) . . ?
C10 C9 C8 120.7(3) . . ?
C10 C9 H9A 119.7 . . ?
C8 C9 H9A 119.7 . . ?
C9 C10 C11 121.4(3) . . ?
C9 C10 H10A 119.3 . . ?
C11 C10 H10A 119.3 . . ?
C12 C11 C10 117.5(3) . . ?
C12 C11 C14 121.4(3) . . ?
C10 C11 C14 121.1(3) . . ?
C13 C12 C11 121.4(3) . . ?
C13 C12 H12A 119.3 . . ?
C11 C12 H12A 119.3 . . ?
C12 C13 C8 121.1(3) . . ?
C12 C13 H13A 119.5 . . ?
C8 C13 H13A 119.5 . . ?
C11 C14 S2 107.7(2) . . ?
C11 C14 H14A 110.2 . . ?
S2 C14 H14A 110.2 . . ?
C11 C14 H14B 110.2 . . ?
S2 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
N2 C15 C16 121.9(3) . . ?
N2 C15 S2 116.0(2) . . ?
C16 C15 S2 122.1(2) . . ?
C20 N2 C15 118.2(3) . . ?
N2 C20 C19 124.1(3) . . ?
N2 C20 H20A 118.0 . . ?
C19 C20 H20A 118.0 . . ?
C20 C19 C18 117.9(3) . . ?
C20 C19 H19A 121.0 . . ?
C18 C19 H19A 121.0 . . ?
C19 C18 C16 120.6(3) . . ?
C19 C18 H18A 119.7 . . ?
C16 C18 H18A 119.7 . . ?
C18 C16 C15 117.2(3) . . ?
C18 C16 C17 118.9(2) . . ?
C15 C16 C17 123.8(2) . . ?
O3 C17 O4 125.0(3) . . ?
O3 C17 C16 118.8(2) . . ?
O4 C17 C16 116.2(2) . . ?
O5 C21 N3 125.2(3) . . ?
O5 C21 H21A 117.4 . . ?
N3 C21 H21A 117.4 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O6 C24 N4 125.4(5) . . ?
O6 C24 H24A 117.3 . . ?
N4 C24 H24A 117.3 . . ?
N4 C25 H25A 109.5 . . ?
N4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N4 C26 H26A 109.5 . . ?
N4 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N4 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        27.41
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.101


