# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-1
_database_code_depnum_ccdc_archive 'CCDC 1005163'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H24 Co N4 O10'
_chemical_formula_weight         671.47

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/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                   27.913(2)
_cell_length_b                   9.7024(7)
_cell_length_c                   22.8070(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.5180(10)
_cell_angle_gamma                90.00
_cell_volume                     5821.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.55
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            PURPLE
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2760
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14220
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5137
_reflns_number_gt                4313
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0688P)²+7.2501P] 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         5137
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1220
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.395779(13) 0.01648(3) 0.108360(15) 0.03081(13) Uani 1 1 d . . .
N1 N 0.41914(9) 0.0399(2) 0.03291(11) 0.0381(5) Uani 1 1 d . . .
O1 O 0.40077(12) -0.2128(3) 0.10246(13) 0.0948(11) Uani 1 1 d . . .
C1 C 0.44982(12) 0.1439(3) 0.02995(14) 0.0515(8) Uani 1 1 d . . .
H1A H 0.4618 0.2039 0.0635 0.062 Uiso 1 1 calc R . .
O1W O 0.45700(10) 0.0338(2) 0.30135(10) 0.0609(6) Uani 1 1 d . . .
H1WA H 0.4336 -0.0135 0.2758 0.073 Uiso 1 1 d R . .
H1WB H 0.4789 0.0523 0.2841 0.073 Uiso 1 1 d R . .
N2 N 0.18187(9) -0.5003(2) -0.56956(11) 0.0390(5) Uani 1 1 d . . .
C2 C 0.46392(15) 0.1636(4) -0.02133(16) 0.0637(10) Uani 1 1 d . . .
H2A H 0.4853 0.2365 -0.0223 0.076 Uiso 1 1 calc R . .
O2 O 0.40902(16) -0.1106(3) 0.18771(13) 0.1222(16) Uani 1 1 d . . .
O2W O 0.55096(11) -0.4221(3) 0.50108(12) 0.0903(9) Uani 1 1 d . . .
H2WA H 0.5760 -0.4325 0.5344 0.108 Uiso 1 1 d R . .
H2WB H 0.5491 -0.3372 0.4915 0.108 Uiso 1 1 d R . .
N3 N 0.39776(8) -0.1196(2) -0.12059(10) 0.0370(5) Uani 1 1 d . . .
H3B H 0.4066 -0.0988 -0.1522 0.044 Uiso 1 1 calc R . .
O3 O 0.49232(8) -0.3828(2) 0.38334(9) 0.0507(5) Uani 1 1 d . . .
C3 C 0.44672(13) 0.0763(3) -0.07142(14) 0.0508(8) Uani 1 1 d . . .
H3A H 0.4559 0.0901 -0.1066 0.061 Uiso 1 1 calc R . .
O4 O 0.47432(9) -0.6060(2) 0.38294(9) 0.0531(5) Uani 1 1 d . . .
C4 C 0.41538(10) -0.0328(3) -0.06875(12) 0.0342(6) Uani 1 1 d . . .
N4 N 0.27892(9) -0.4093(3) -0.42115(11) 0.0509(7) Uani 1 1 d . . .
H4A H 0.3068 -0.3634 -0.4127 0.061 Uiso 1 1 calc R . .
O5 O 0.43395(9) -0.8369(2) 0.16926(9) 0.0545(6) Uani 1 1 d . . .
C5 C 0.40260(10) -0.0472(3) -0.01497(12) 0.0361(6) Uani 1 1 d . . .
H5A H 0.3818 -0.1201 -0.0124 0.043 Uiso 1 1 calc R . .
O6 O 0.37413(8) -0.7270(3) 0.09711(11) 0.0704(8) Uani 1 1 d . . .
C6 C 0.36808(10) -0.2336(3) -0.12620(12) 0.0354(6) Uani 1 1 d . . .
O7 O 0.35936(8) -0.2844(2) -0.08170(9) 0.0475(5) Uani 1 1 d . . .
C7 C 0.34510(9) -0.2895(3) -0.19079(12) 0.0356(6) Uani 1 1 d . . .
C8 C 0.33395(9) -0.4345(3) -0.20101(12) 0.0360(6) Uani 1 1 d . . .
O8 O 0.21682(9) -0.4787(3) -0.38459(11) 0.0735(8) Uani 1 1 d . . .
C9 C 0.34987(11) -0.5350(3) -0.15345(14) 0.0451(7) Uani 1 1 d . . .
H9A H 0.3680 -0.5075 -0.1130 0.054 Uiso 1 1 calc R . .
C10 C 0.33912(13) -0.6714(3) -0.16569(16) 0.0563(8) Uani 1 1 d . . .
H10A H 0.3500 -0.7355 -0.1336 0.068 Uiso 1 1 calc R . .
C11 C 0.31190(13) -0.7156(4) -0.22610(18) 0.0623(9) Uani 1 1 d . . .
H11A H 0.3046 -0.8087 -0.2341 0.075 Uiso 1 1 calc R . .
C12 C 0.29615(12) -0.6226(3) -0.27288(16) 0.0521(8) Uani 1 1 d . . .
H12A H 0.2781 -0.6528 -0.3129 0.063 Uiso 1 1 calc R . .
C13 C 0.30659(10) -0.4803(3) -0.26221(13) 0.0391(6) Uani 1 1 d . . .
C14 C 0.29130(10) -0.3826(3) -0.31176(13) 0.0427(7) Uani 1 1 d . . .
C15 C 0.30409(11) -0.2465(3) -0.30083(13) 0.0472(7) Uani 1 1 d . . .
H15A H 0.2952 -0.1841 -0.3336 0.057 Uiso 1 1 calc R . .
C16 C 0.33070(11) -0.2008(3) -0.23998(13) 0.0435(7) Uani 1 1 d . . .
H16A H 0.3387 -0.1078 -0.2332 0.052 Uiso 1 1 calc R . .
C17 C 0.25848(11) -0.4274(4) -0.37549(13) 0.0487(7) Uani 1 1 d . . .
C18 C 0.25668(11) -0.4623(4) -0.48210(13) 0.0474(7) Uani 1 1 d . . .
C19 C 0.28441(13) -0.5340(5) -0.51061(19) 0.0848(14) Uani 1 1 d . . .
H19A H 0.3192 -0.5453 -0.4911 0.102 Uiso 1 1 calc R . .
C20 C 0.26069(14) -0.5902(6) -0.56882(19) 0.0944(16) Uani 1 1 d . . .
H20A H 0.2793 -0.6392 -0.5889 0.113 Uiso 1 1 calc R . .
C21 C 0.20984(12) -0.5728(4) -0.59615(15) 0.0583(9) Uani 1 1 d . . .
H21A H 0.1938 -0.6128 -0.6348 0.070 Uiso 1 1 calc R . .
C22 C 0.20551(10) -0.4446(3) -0.51371(12) 0.0411(6) Uani 1 1 d . . .
H22A H 0.1866 -0.3916 -0.4954 0.049 Uiso 1 1 calc R . .
C23 C 0.40976(11) -0.2169(4) 0.15927(17) 0.0585(9) Uani 1 1 d . . .
C24 C 0.42005(10) -0.3535(3) 0.19232(12) 0.0391(6) Uani 1 1 d . . .
C25 C 0.44025(9) -0.3599(3) 0.25669(12) 0.0354(6) Uani 1 1 d . . .
H25A H 0.4470 -0.2792 0.2801 0.042 Uiso 1 1 calc R . .
C26 C 0.45043(9) -0.4872(2) 0.28615(12) 0.0294(5) Uani 1 1 d . . .
C27 C 0.47304(10) -0.4985(3) 0.35516(12) 0.0352(6) Uani 1 1 d . . .
C28 C 0.44102(9) -0.6072(3) 0.25154(11) 0.0314(5) Uani 1 1 d . . .
H28A H 0.4484 -0.6922 0.2714 0.038 Uiso 1 1 calc R . .
C29 C 0.42058(9) -0.6008(3) 0.18724(12) 0.0344(6) Uani 1 1 d . . .
C30 C 0.40877(11) -0.7285(3) 0.14874(13) 0.0446(7) Uani 1 1 d . . .
C31 C 0.41015(10) -0.4741(3) 0.15819(12) 0.0392(6) Uani 1 1 d . . .
H31A H 0.3963 -0.4699 0.1151 0.047 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
Co1 O5 2.024(2) 1_565 ?
Co1 N1 2.046(2) . ?
Co1 N2 2.056(2) 4_554 ?
Co1 O2 2.118(3) . ?
Co1 O1 2.236(3) . ?
Co1 C23 2.515(3) . ?
N1 C5 1.335(3) . ?
N1 C1 1.340(3) . ?
O1 C23 1.235(4) . ?
C1 C2 1.366(4) . ?
N2 C22 1.337(3) . ?
N2 C21 1.337(4) . ?
N2 Co1 2.056(2) 4_544 ?
C2 C3 1.373(4) . ?
O2 C23 1.222(5) . ?
N3 C6 1.362(3) . ?
N3 C4 1.401(3) . ?
O3 C27 1.316(3) . ?
C3 C4 1.387(4) . ?
O4 C27 1.214(3) . ?
C4 C5 1.394(4) . ?
N4 C17 1.356(4) . ?
N4 C18 1.416(4) . ?
O5 C30 1.265(4) . ?
O5 Co1 2.024(2) 1_545 ?
O6 C30 1.249(4) . ?
C6 O7 1.223(3) . ?
C6 C7 1.498(3) . ?
C7 C16 1.363(4) . ?
C7 C8 1.443(4) . ?
C8 C9 1.415(4) . ?
C8 C13 1.420(4) . ?
O8 C17 1.217(4) . ?
C9 C10 1.366(4) . ?
C10 C11 1.400(5) . ?
C11 C12 1.354(5) . ?
C12 C13 1.415(4) . ?
C13 C14 1.426(4) . ?
C14 C15 1.369(4) . ?
C14 C17 1.501(4) . ?
C15 C16 1.409(4) . ?
C18 C19 1.358(5) . ?
C18 C22 1.379(4) . ?
C19 C20 1.382(5) . ?
C20 C21 1.357(5) . ?
C23 C24 1.504(4) . ?
C24 C31 1.381(4) . ?
C24 C25 1.387(4) . ?
C25 C26 1.389(3) . ?
C26 C28 1.382(3) . ?
C26 C27 1.491(4) . ?
C28 C29 1.386(4) . ?
C29 C31 1.381(4) . ?
C29 C30 1.490(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
O5 Co1 N1 104.86(9) 1_565 . ?
O5 Co1 N2 126.05(10) 1_565 4_554 ?
N1 Co1 N2 103.48(9) . 4_554 ?
O5 Co1 O2 85.48(9) 1_565 . ?
N1 Co1 O2 140.31(15) . . ?
N2 Co1 O2 100.35(13) 4_554 . ?
O5 Co1 O1 135.33(11) 1_565 . ?
N1 Co1 O1 90.92(9) . . ?
N2 Co1 O1 88.47(10) 4_554 . ?
O2 Co1 O1 58.37(11) . . ?
O5 Co1 C23 110.54(11) 1_565 . ?
N1 Co1 C23 116.37(12) . . ?
N2 Co1 C23 96.10(9) 4_554 . ?
O2 Co1 C23 29.01(12) . . ?
O1 Co1 C23 29.40(11) . . ?
C5 N1 C1 119.2(2) . . ?
C5 N1 Co1 119.83(17) . . ?
C1 N1 Co1 120.97(18) . . ?
C23 O1 Co1 87.9(3) . . ?
N1 C1 C2 121.4(3) . . ?
C22 N2 C21 117.9(3) . . ?
C22 N2 Co1 119.46(18) . 4_544 ?
C21 N2 Co1 122.5(2) . 4_544 ?
C1 C2 C3 120.3(3) . . ?
C23 O2 Co1 93.8(2) . . ?
C6 N3 C4 126.8(2) . . ?
C2 C3 C4 119.0(3) . . ?
C3 C4 C5 117.7(2) . . ?
C3 C4 N3 118.1(2) . . ?
C5 C4 N3 124.2(2) . . ?
C17 N4 C18 123.2(2) . . ?
C30 O5 Co1 103.33(18) . 1_545 ?
N1 C5 C4 122.4(2) . . ?
O7 C6 N3 122.2(2) . . ?
O7 C6 C7 122.1(2) . . ?
N3 C6 C7 115.7(2) . . ?
C16 C7 C8 119.6(2) . . ?
C16 C7 C6 119.5(2) . . ?
C8 C7 C6 120.7(2) . . ?
C9 C8 C13 117.8(3) . . ?
C9 C8 C7 123.5(2) . . ?
C13 C8 C7 118.7(2) . . ?
C10 C9 C8 121.3(3) . . ?
C9 C10 C11 120.5(3) . . ?
C12 C11 C10 119.9(3) . . ?
C11 C12 C13 121.4(3) . . ?
C12 C13 C8 119.1(3) . . ?
C12 C13 C14 121.5(3) . . ?
C8 C13 C14 119.4(3) . . ?
C15 C14 C13 120.4(3) . . ?
C15 C14 C17 119.6(3) . . ?
C13 C14 C17 119.9(3) . . ?
C14 C15 C16 120.2(3) . . ?
C7 C16 C15 121.7(3) . . ?
O8 C17 N4 123.1(3) . . ?
O8 C17 C14 121.5(3) . . ?
N4 C17 C14 115.4(2) . . ?
C19 C18 C22 118.0(3) . . ?
C19 C18 N4 121.5(3) . . ?
C22 C18 N4 120.4(3) . . ?
C18 C19 C20 119.7(3) . . ?
C21 C20 C19 119.0(3) . . ?
N2 C21 C20 122.5(3) . . ?
N2 C22 C18 122.9(3) . . ?
O2 C23 O1 119.7(3) . . ?
O2 C23 C24 120.8(3) . . ?
O1 C23 C24 119.5(4) . . ?
O2 C23 Co1 57.16(18) . . ?
O1 C23 Co1 62.7(2) . . ?
C24 C23 Co1 177.3(3) . . ?
C31 C24 C25 119.5(2) . . ?
C31 C24 C23 119.7(3) . . ?
C25 C24 C23 120.8(3) . . ?
C24 C25 C26 119.8(2) . . ?
C28 C26 C25 120.2(2) . . ?
C28 C26 C27 118.3(2) . . ?
C25 C26 C27 121.5(2) . . ?
O4 C27 O3 122.8(3) . . ?
O4 C27 C26 122.9(2) . . ?
O3 C27 C26 114.3(2) . . ?
C26 C28 C29 120.0(2) . . ?
C31 C29 C28 119.6(2) . . ?
C31 C29 C30 119.2(2) . . ?
C28 C29 C30 121.2(3) . . ?
O6 C30 O5 121.2(3) . . ?
O6 C30 C29 119.7(3) . . ?
O5 C30 C29 119.1(3) . . ?
C29 C31 C24 120.9(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.057
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-2
_database_code_depnum_ccdc_archive 'CCDC 1005164'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H32 N6 Ni O11'
_chemical_formula_weight         855.45

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.4576(4)
_cell_length_b                   11.7570(6)
_cell_length_c                   17.2174(8)
_cell_angle_alpha                83.1940(10)
_cell_angle_beta                 80.7120(10)
_cell_angle_gamma                77.6280(10)
_cell_volume                     1838.47(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.06
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             884
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9359
_diffrn_reflns_av_R_equivalents  0.0114
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6402
_reflns_number_gt                5620
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0454P)²+3.0526P] 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         6402
_refine_ls_number_parameters     569
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1128
_refine_ls_wR_factor_gt          0.1091
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -1.14851(4) 0.89018(3) 0.27635(2) 0.02290(11) Uani 1 1 d . . .
O1 O -1.2492(2) 1.06168(16) 0.27706(12) 0.0281(4) Uani 1 1 d . . .
N1 N -0.9407(2) 0.9359(2) 0.24947(14) 0.0261(5) Uani 1 1 d . . .
C1 C -0.9231(3) 1.0472(3) 0.24190(17) 0.0298(6) Uani 1 1 d . . .
H1A H -1.0050 1.1060 0.2522 0.036 Uiso 1 1 calc R . .
O1W O -1.3536(2) 0.84121(18) 0.29239(14) 0.0410(6) Uani 1 1 d . . .
H1WA H -1.4246 0.8994 0.2928 0.049 Uiso 1 1 d R . .
H1WB H -1.3777 0.7899 0.3283 0.049 Uiso 1 1 d R . .
O2 O -1.4808(2) 1.04767(18) 0.32198(17) 0.0498(7) Uani 1 1 d . . .
N2 N 0.1446(3) 0.1074(2) -0.15048(14) 0.0297(5) Uani 1 1 d . . .
C2 C -0.7891(3) 1.0778(3) 0.2195(2) 0.0379(7) Uani 1 1 d . . .
H2A H -0.7805 1.1556 0.2170 0.045 Uiso 1 1 calc R . .
O2W O -1.0690(2) 0.71192(17) 0.27683(14) 0.0395(5) Uani 1 1 d . . .
H2WA H -0.9929 0.6590 0.2801 0.047 Uiso 1 1 d R . .
H2WB H -1.1235 0.6878 0.2504 0.047 Uiso 1 1 d R . .
O3 O -1.8557(2) 1.39415(18) 0.30283(16) 0.0453(6) Uani 1 1 d . . .
N3 N -1.1275(4) 0.8843(3) 0.39843(17) 0.0660(11) Uani 1 1 d . C .
C3 C -0.6668(3) 0.9918(3) 0.2007(2) 0.0390(8) Uani 1 1 d . . .
H3A H -0.5754 1.0107 0.1845 0.047 Uiso 1 1 calc R . .
O4 O -1.8101(2) 1.57230(18) 0.30236(17) 0.0505(7) Uani 1 1 d . . .
C4 C -0.6838(3) 0.8778(3) 0.20666(18) 0.0308(6) Uani 1 1 d . . .
N4 N -0.5675(3) 0.7826(2) 0.18509(16) 0.0361(6) Uani 1 1 d . . .
H4A H -0.4884 0.7702 0.2061 0.043 Uiso 1 1 calc R . .
O5 O -1.2830(2) 1.60163(18) 0.29707(14) 0.0393(5) Uani 1 1 d . . .
N5 N -0.0917(3) 0.2691(2) 0.00526(15) 0.0400(7) Uani 1 1 d . . .
H5B H -0.1665 0.2898 -0.0195 0.048 Uiso 1 1 calc R . .
C5 C -0.8212(3) 0.8537(3) 0.23305(18) 0.0311(6) Uani 1 1 d . . .
H5A H -0.8310 0.7760 0.2397 0.037 Uiso 1 1 calc R . .
O6 O -1.1298(2) 1.43749(19) 0.33181(14) 0.0374(5) Uani 1 1 d . . .
N6 N -0.8487(5) 0.7199(5) 0.5166(2) 0.140(3) Uani 1 1 d . . .
H6A H -0.8421 0.6949 0.5651 0.168 Uiso 1 1 calc R A 1
C6 C -0.5823(3) 0.7119(3) 0.13160(18) 0.0327(7) Uani 1 1 d . . .
O7 O -0.6891(2) 0.7344(2) 0.09630(14) 0.0464(6) Uani 1 1 d . . .
C7 C -0.4622(3) 0.6068(3) 0.11818(17) 0.0300(6) Uani 1 1 d . . .
O8 O -0.0022(3) 0.2952(2) 0.11459(15) 0.0537(7) Uani 1 1 d . . .
C8 C -0.4955(3) 0.4980(3) 0.10598(16) 0.0278(6) Uani 1 1 d . . .
C9 C -0.6400(3) 0.4798(3) 0.10942(18) 0.0377(7) Uani 1 1 d . . .
H9A H -0.7180 0.5422 0.1184 0.045 Uiso 1 1 calc R . .
O9 O -0.6949(4) 0.7710(4) 0.4083(2) 0.1223(19) Uani 1 1 d . . .
C10 C -0.6677(4) 0.3740(3) 0.0999(2) 0.0453(8) Uani 1 1 d . . .
H10A H -0.7635 0.3651 0.1015 0.054 Uiso 1 1 calc R . .
C11 C -0.5516(4) 0.2778(3) 0.0877(2) 0.0475(9) Uani 1 1 d . . .
H11A H -0.5706 0.2054 0.0811 0.057 Uiso 1 1 calc R . .
C12 C -0.4116(4) 0.2908(3) 0.08556(18) 0.0376(7) Uani 1 1 d . . .
H12A H -0.3360 0.2260 0.0790 0.045 Uiso 1 1 calc R . .
C13 C -0.3777(3) 0.4003(3) 0.09297(16) 0.0288(6) Uani 1 1 d . . .
C14 C -0.2315(3) 0.4153(3) 0.09048(17) 0.0301(6) Uani 1 1 d . . .
C15 C -0.2046(3) 0.5205(3) 0.10385(19) 0.0370(7) Uani 1 1 d . . .
H15A H -0.1090 0.5286 0.1039 0.044 Uiso 1 1 calc R . .
C16 C -0.3203(3) 0.6162(3) 0.11754(19) 0.0353(7) Uani 1 1 d . . .
H16A H -0.3000 0.6873 0.1263 0.042 Uiso 1 1 calc R . .
C17 C -0.0990(3) 0.3197(3) 0.07313(18) 0.0342(7) Uani 1 1 d . . .
C18 C 0.0254(3) 0.1861(3) -0.02889(18) 0.0329(7) Uani 1 1 d . . .
C19 C 0.1219(4) 0.1067(3) 0.0130(2) 0.0476(9) Uani 1 1 d . . .
H19A H 0.1148 0.1057 0.0676 0.057 Uiso 1 1 calc R . .
C20 C 0.2292(4) 0.0290(3) -0.0289(2) 0.0513(10) Uani 1 1 d . . .
H20A H 0.2965 -0.0248 -0.0025 0.062 Uiso 1 1 calc R . .
C21 C 0.2371(3) 0.0309(3) -0.10933(19) 0.0378(7) Uani 1 1 d . . .
H21A H 0.3095 -0.0230 -0.1362 0.045 Uiso 1 1 calc R . .
C22 C 0.0419(3) 0.1832(3) -0.10984(18) 0.0340(7) Uani 1 1 d . . .
H22A H -0.0226 0.2373 -0.1378 0.041 Uiso 1 1 calc R . .
C23 C -1.2193(6) 0.9449(6) 0.4530(3) 0.140(4) Uani 1 1 d . . .
H23A H -1.2783 1.0157 0.4384 0.169 Uiso 1 1 calc R B 1
C24 C -1.2265(8) 0.9006(7) 0.5338(4) 0.0497(13) Uani 0.505(3) 1 d P C 1
H24A H -1.3104 0.9213 0.5696 0.060 Uiso 0.505(3) 1 calc PR C 1
C24' C -1.1605(8) 0.9760(7) 0.5256(4) 0.0497(13) Uani 0.495(3) 1 d P C 2
H24B H -1.2062 1.0413 0.5523 0.060 Uiso 0.495(3) 1 calc PR C 2
C25 C -1.1047(8) 0.8263(7) 0.5567(4) 0.0481(13) Uani 0.505(3) 1 d P C 1
H25A H -1.0913 0.8129 0.6096 0.058 Uiso 0.505(3) 1 calc PR C 1
C25' C -1.0366(8) 0.9015(7) 0.5486(4) 0.0481(13) Uani 0.495(3) 1 d P C 2
H25B H -1.0126 0.9011 0.5989 0.058 Uiso 0.495(3) 1 calc PR C 2
C26 C -1.0024(7) 0.7719(6) 0.4988(4) 0.0355(11) Uani 0.505(3) 1 d P C 1
C26' C -0.9499(7) 0.8283(6) 0.4956(4) 0.0355(11) Uani 0.495(3) 1 d P C 2
C27 C -1.0089(5) 0.8127(4) 0.4215(2) 0.0752(16) Uani 1 1 d . . .
H27A H -0.9285 0.7900 0.3839 0.090 Uiso 1 1 calc R C 1
C28 C -0.7180(6) 0.7068(6) 0.4665(3) 0.115(3) Uani 1 1 d . C .
C29 C -0.6082(6) 0.5990(6) 0.4873(2) 0.102(3) Uani 1 1 d . . .
C30 C -0.4652(6) 0.6133(6) 0.4894(2) 0.091(2) Uani 1 1 d . . .
C31 C -0.4506(8) 0.7048(7) 0.4912(4) 0.0403(15) Uani 0.50 1 d P . .
H31A H -0.5265 0.7692 0.4869 0.048 Uiso 0.50 1 calc PR C .
C32 C -0.3160(9) 0.7150(7) 0.5002(5) 0.059(2) Uani 0.50 1 d P C .
H32A H -0.2952 0.7890 0.4992 0.071 Uiso 0.50 1 calc PR . .
C33 C -0.2064(8) 0.6164(8) 0.5109(5) 0.055(2) Uani 0.50 1 d P . .
H33A H -0.1130 0.6253 0.5159 0.083 Uiso 0.50 1 calc PR C .
C34 C -0.7656(7) 0.4894(6) 0.4861(4) 0.0393(15) Uani 0.50 1 d P . .
H34A H -0.8335 0.5575 0.4764 0.059 Uiso 0.50 1 calc PR C .
C35 C -0.6438(6) 0.4886(6) 0.4970(2) 0.091(2) Uani 1 1 d . . .
C41 C -1.3822(3) 1.1048(2) 0.29990(16) 0.0249(6) Uani 1 1 d . . .
C42 C -1.4237(3) 1.2350(2) 0.30129(16) 0.0220(5) Uani 1 1 d . . .
C43 C -1.5704(3) 1.2888(2) 0.30284(16) 0.0237(6) Uani 1 1 d . . .
H43A H -1.6403 1.2437 0.3034 0.028 Uiso 1 1 calc R . .
C44 C -1.6125(3) 1.4091(2) 0.30359(16) 0.0224(6) Uani 1 1 d . . .
C45 C -1.7690(3) 1.4670(2) 0.30337(18) 0.0284(6) Uani 1 1 d . . .
C46 C -1.5090(3) 1.4764(2) 0.30605(16) 0.0228(6) Uani 1 1 d . . .
H46A H -1.5374 1.5570 0.3072 0.027 Uiso 1 1 calc R . .
C47 C -1.3632(3) 1.4228(2) 0.30681(15) 0.0211(5) Uani 1 1 d . . .
C48 C -1.2501(3) 1.4931(2) 0.31219(17) 0.0265(6) Uani 1 1 d . . .
C49 C -1.3213(3) 1.3025(2) 0.30295(15) 0.0225(6) Uani 1 1 d . . .
H49A H -1.2232 1.2670 0.3015 0.027 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
Ni1 O1 2.0375(18) . ?
Ni1 O2W 2.069(2) . ?
Ni1 O1W 2.107(2) . ?
Ni1 N1 2.113(2) . ?
Ni1 N3 2.135(3) . ?
Ni1 N2 2.158(2) 2_465 ?
O1 C41 1.269(3) . ?
N1 C5 1.335(4) . ?
N1 C1 1.343(4) . ?
C1 C2 1.375(4) . ?
O2 C41 1.248(3) . ?
N2 C22 1.335(4) . ?
N2 C21 1.338(4) . ?
N2 Ni1 2.158(2) 2_465 ?
C2 C3 1.386(4) . ?
O3 C45 1.309(3) . ?
N3 C23 1.332(5) . ?
N3 C27 1.336(4) . ?
C3 C4 1.373(4) . ?
O4 C45 1.214(3) . ?
C4 C5 1.384(4) . ?
C4 N4 1.428(4) . ?
N4 C6 1.353(4) . ?
O5 C48 1.254(3) . ?
N5 C17 1.359(4) . ?
N5 C18 1.410(4) . ?
O6 C48 1.260(3) . ?
N6 C28 1.379(7) . ?
N6 C26' 1.466(7) . ?
N6 C26 1.516(7) . ?
C6 O7 1.227(4) . ?
C6 C7 1.500(4) . ?
C7 C16 1.369(4) . ?
C7 C8 1.428(4) . ?
O8 C17 1.216(4) . ?
C8 C9 1.419(4) . ?
C8 C13 1.428(4) . ?
C9 C10 1.358(5) . ?
O9 C28 1.200(7) . ?
C10 C11 1.407(5) . ?
C11 C12 1.359(5) . ?
C12 C13 1.417(4) . ?
C13 C14 1.425(4) . ?
C14 C15 1.366(4) . ?
C14 C17 1.509(4) . ?
C15 C16 1.404(4) . ?
C18 C22 1.381(4) . ?
C18 C19 1.383(4) . ?
C19 C20 1.382(5) . ?
C20 C21 1.372(5) . ?
C23 C24 1.423(8) . ?
C23 C24' 1.557(10) . ?
C24 C25 1.371(10) . ?
C24' C25' 1.387(10) . ?
C25 C26 1.383(9) . ?
C25' C26' 1.374(10) . ?
C26 C27 1.366(7) . ?
C26' C27 1.517(8) . ?
C28 C29 1.504(6) . ?
C29 C35 1.395(9) . ?
C29 C30 1.404(9) . ?
C30 C31 1.118(9) . ?
C30 C35 1.427(6) 2_466 ?
C31 C32 1.338(11) . ?
C32 C33 1.396(11) . ?
C33 C34 1.320(11) 2_466 ?
C34 C35 1.194(8) . ?
C34 C33 1.320(11) 2_466 ?
C35 C30 1.427(6) 2_466 ?
C41 C42 1.499(4) . ?
C42 C49 1.382(4) . ?
C42 C43 1.393(4) . ?
C43 C44 1.386(4) . ?
C44 C46 1.392(4) . ?
C44 C45 1.491(4) . ?
C46 C47 1.389(4) . ?
C47 C49 1.391(4) . ?
C47 C48 1.506(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
O1 Ni1 O2W 173.71(8) . . ?
O1 Ni1 O1W 90.17(8) . . ?
O2W Ni1 O1W 83.55(8) . . ?
O1 Ni1 N1 91.18(8) . . ?
O2W Ni1 N1 95.05(8) . . ?
O1W Ni1 N1 174.79(9) . . ?
O1 Ni1 N3 90.30(11) . . ?
O2W Ni1 N3 90.73(12) . . ?
O1W Ni1 N3 97.11(13) . . ?
N1 Ni1 N3 87.91(13) . . ?
O1 Ni1 N2 92.35(9) . 2_465 ?
O2W Ni1 N2 87.24(9) . 2_465 ?
O1W Ni1 N2 88.40(9) . 2_465 ?
N1 Ni1 N2 86.52(9) . 2_465 ?
N3 Ni1 N2 173.88(11) . 2_465 ?
C41 O1 Ni1 128.53(18) . . ?
C5 N1 C1 117.1(2) . . ?
C5 N1 Ni1 120.13(19) . . ?
C1 N1 Ni1 122.53(19) . . ?
N1 C1 C2 122.7(3) . . ?
C22 N2 C21 117.1(3) . . ?
C22 N2 Ni1 119.26(19) . 2_465 ?
C21 N2 Ni1 123.6(2) . 2_465 ?
C1 C2 C3 119.4(3) . . ?
C23 N3 C27 117.4(3) . . ?
C23 N3 Ni1 126.8(3) . . ?
C27 N3 Ni1 115.9(2) . . ?
C4 C3 C2 118.5(3) . . ?
C3 C4 C5 118.6(3) . . ?
C3 C4 N4 123.5(3) . . ?
C5 C4 N4 117.9(3) . . ?
C6 N4 C4 119.8(2) . . ?
C17 N5 C18 126.9(3) . . ?
N1 C5 C4 123.6(3) . . ?
C28 N6 C26' 112.1(5) . . ?
C28 N6 C26 129.6(4) . . ?
C26' N6 C26 35.1(3) . . ?
O7 C6 N4 120.7(3) . . ?
O7 C6 C7 122.7(3) . . ?
N4 C6 C7 116.6(3) . . ?
C16 C7 C8 120.2(3) . . ?
C16 C7 C6 119.4(3) . . ?
C8 C7 C6 120.4(3) . . ?
C9 C8 C7 123.6(3) . . ?
C9 C8 C13 117.8(3) . . ?
C7 C8 C13 118.5(3) . . ?
C10 C9 C8 121.9(3) . . ?
C9 C10 C11 120.1(3) . . ?
C12 C11 C10 119.9(3) . . ?
C11 C12 C13 121.8(3) . . ?
C12 C13 C14 122.4(3) . . ?
C12 C13 C8 118.4(3) . . ?
C14 C13 C8 119.2(3) . . ?
C15 C14 C13 120.3(3) . . ?
C15 C14 C17 116.2(3) . . ?
C13 C14 C17 123.5(3) . . ?
C14 C15 C16 120.5(3) . . ?
C7 C16 C15 121.1(3) . . ?
O8 C17 N5 122.8(3) . . ?
O8 C17 C14 122.1(3) . . ?
N5 C17 C14 115.0(3) . . ?
C22 C18 C19 118.3(3) . . ?
C22 C18 N5 117.0(3) . . ?
C19 C18 N5 124.7(3) . . ?
C20 C19 C18 117.8(3) . . ?
C21 C20 C19 120.3(3) . . ?
N2 C21 C20 122.4(3) . . ?
N2 C22 C18 124.1(3) . . ?
N3 C23 C24 119.6(5) . . ?
N3 C23 C24' 119.6(5) . . ?
C24 C23 C24' 46.0(4) . . ?
C25 C24 C23 117.3(6) . . ?
C25' C24' C23 116.8(6) . . ?
C24 C25 C26 118.1(6) . . ?
C26' C25' C24' 118.8(6) . . ?
C27 C26 C25 118.9(5) . . ?
C27 C26 N6 113.8(5) . . ?
C25 C26 N6 119.4(6) . . ?
C25' C26' N6 125.1(6) . . ?
C25' C26' C27 118.6(5) . . ?
N6 C26' C27 108.1(5) . . ?
N3 C27 C26 121.9(4) . . ?
N3 C27 C26' 121.9(4) . . ?
C26 C27 C26' 35.9(4) . . ?
O9 C28 N6 123.8(4) . . ?
O9 C28 C29 121.9(5) . . ?
N6 C28 C29 114.2(5) . . ?
C35 C29 C30 121.5(5) . . ?
C35 C29 C28 121.1(6) . . ?
C30 C29 C28 117.1(7) . . ?
C31 C30 C29 116.4(6) . . ?
C31 C30 C35 124.4(8) . 2_466 ?
C29 C30 C35 118.2(7) . 2_466 ?
C30 C31 C32 115.2(8) . . ?
C31 C32 C33 121.1(8) . . ?
C34 C33 C32 120.4(7) 2_466 . ?
C35 C34 C33 113.0(7) . 2_466 ?
C34 C35 C29 113.8(6) . . ?
C34 C35 C30 125.6(8) . 2_466 ?
C29 C35 C30 120.2(6) . 2_466 ?
O2 C41 O1 125.4(2) . . ?
O2 C41 C42 117.5(2) . . ?
O1 C41 C42 117.1(2) . . ?
C49 C42 C43 119.4(2) . . ?
C49 C42 C41 121.9(2) . . ?
C43 C42 C41 118.7(2) . . ?
C44 C43 C42 120.2(2) . . ?
C43 C44 C46 120.1(2) . . ?
C43 C44 C45 120.3(2) . . ?
C46 C44 C45 119.6(2) . . ?
O4 C45 O3 123.8(3) . . ?
O4 C45 C44 122.4(3) . . ?
O3 C45 C44 113.7(2) . . ?
C47 C46 C44 119.8(2) . . ?
C46 C47 C49 119.6(2) . . ?
C46 C47 C48 120.9(2) . . ?
C49 C47 C48 119.5(2) . . ?
O5 C48 O6 125.4(3) . . ?
O5 C48 C47 117.6(2) . . ?
O6 C48 C47 117.0(2) . . ?
C42 C49 C47 120.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.063
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-3
_database_code_depnum_ccdc_archive 'CCDC 1005165'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H22 Cu N4 O9'
_chemical_formula_weight         658.07

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   'C 2/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                   27.413(4)
_cell_length_b                   10.0478(16)
_cell_length_c                   20.669(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.821(3)
_cell_angle_gamma                90.00
_cell_volume                     5477.4(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.54
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2696
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8599
_exptl_absorpt_correction_T_max  0.8812
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13469
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4774
_reflns_number_gt                3829
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0646P)²+12.1060P] 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         4774
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1147
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
Cu1 Cu -0.092418(15) 0.10345(4) 0.103348(19) 0.02535(14) Uani 1 1 d . . .
O1 O -0.08810(9) 0.2729(2) 0.14591(12) 0.0351(6) Uani 1 1 d . . .
N1 N -0.02286(10) 0.1150(3) 0.08931(13) 0.0274(6) Uani 1 1 d . . .
C1 C -0.01613(14) 0.1633(3) 0.03178(16) 0.0316(8) Uani 1 1 d . . .
H1A H -0.0433 0.2029 0.0008 0.038 Uiso 1 1 calc R . .
O1W O -0.05084(18) 0.5560(5) -0.00582(17) 0.1101(16) Uani 1 1 d . . .
H1WA H -0.0667 0.5502 0.0241 0.132 Uiso 1 1 d R . .
H1WB H -0.0609 0.4929 -0.0336 0.132 Uiso 1 1 d R . .
N2 N 0.33128(11) -0.6024(3) 0.57367(14) 0.0299(6) Uani 1 1 d . . .
C2 C 0.02979(15) 0.1558(4) 0.01758(17) 0.0376(9) Uani 1 1 d . . .
H2A H 0.0332 0.1883 -0.0231 0.045 Uiso 1 1 calc R . .
O2 O -0.10751(12) 0.4022(3) 0.05581(13) 0.0540(8) Uani 1 1 d . . .
N3 N 0.10235(10) -0.0172(3) 0.17217(14) 0.0310(7) Uani 1 1 d . . .
H3B H 0.1035 -0.0023 0.2135 0.037 Uiso 1 1 calc R . .
O3 O -0.09156(8) 0.9039(2) 0.09803(11) 0.0276(5) Uani 1 1 d . . .
C3 C 0.07107(14) 0.1000(4) 0.06354(17) 0.0353(8) Uani 1 1 d . . .
H3A H 0.1027 0.0974 0.0551 0.042 Uiso 1 1 calc R . .
O4 O -0.07427(9) 0.9727(2) 0.20253(11) 0.0311(5) Uani 1 1 d . . .
N4 N 0.23160(11) -0.4515(3) 0.43671(15) 0.0406(8) Uani 1 1 d . . .
H4A H 0.2000 -0.4682 0.4190 0.049 Uiso 1 1 calc R . .
C4 C 0.06412(13) 0.0482(3) 0.12244(16) 0.0275(7) Uani 1 1 d . . .
O5 O -0.02710(11) 0.6582(3) 0.39089(12) 0.0462(7) Uani 1 1 d . . .
C5 C 0.01659(13) 0.0591(3) 0.13351(16) 0.0284(7) Uani 1 1 d . . .
H5A H 0.0120 0.0259 0.1735 0.034 Uiso 1 1 calc R . .
O6 O -0.03904(12) 0.4416(3) 0.37171(13) 0.0520(8) Uani 1 1 d . . .
C6 C 0.13753(14) -0.1021(4) 0.15972(19) 0.0370(9) Uani 1 1 d . . .
O7 O 0.14481(12) -0.1174(3) 0.10448(14) 0.0596(9) Uani 1 1 d . . .
C7 C 0.16696(12) -0.1759(4) 0.22151(17) 0.0327(8) Uani 1 1 d . . .
C8 C 0.18606(14) -0.1054(4) 0.27975(19) 0.0375(9) Uani 1 1 d . . .
H8A H 0.1807 -0.0140 0.2800 0.045 Uiso 1 1 calc R . .
O8 O 0.29576(13) -0.3192(4) 0.4286(2) 0.1099(18) Uani 1 1 d . . .
C9 C 0.21327(14) -0.1682(4) 0.33850(19) 0.0390(9) Uani 1 1 d . . .
H9A H 0.2268 -0.1178 0.3770 0.047 Uiso 1 1 calc R . .
C10 C 0.22032(13) -0.3030(4) 0.34043(18) 0.0368(9) Uani 1 1 d . . .
C11 C 0.20108(13) -0.3809(4) 0.28151(19) 0.0351(8) Uani 1 1 d . . .
C12 C 0.20828(16) -0.5212(4) 0.2807(2) 0.0465(10) Uani 1 1 d . . .
H12A H 0.2259 -0.5644 0.3199 0.056 Uiso 1 1 calc R . .
C13 C 0.18995(17) -0.5921(4) 0.2241(3) 0.0556(12) Uani 1 1 d . . .
H13A H 0.1947 -0.6838 0.2248 0.067 Uiso 1 1 calc R . .
C14 C 0.16378(16) -0.5298(5) 0.1643(2) 0.0514(11) Uani 1 1 d . . .
H14A H 0.1512 -0.5804 0.1257 0.062 Uiso 1 1 calc R . .
C15 C 0.15655(14) -0.3958(4) 0.1621(2) 0.0417(9) Uani 1 1 d . . .
H15A H 0.1394 -0.3558 0.1217 0.050 Uiso 1 1 calc R . .
C16 C 0.17468(12) -0.3159(4) 0.22029(18) 0.0332(8) Uani 1 1 d . . .
C17 C 0.25299(15) -0.3586(4) 0.4055(2) 0.0488(11) Uani 1 1 d . . .
C18 C 0.25569(13) -0.5235(4) 0.49517(18) 0.0326(8) Uani 1 1 d . . .
C19 C 0.22656(14) -0.5952(4) 0.5283(2) 0.0384(9) Uani 1 1 d . . .
H19A H 0.1914 -0.5925 0.5135 0.046 Uiso 1 1 calc R . .
C20 C 0.25056(14) -0.6704(4) 0.58321(19) 0.0379(9) Uani 1 1 d . . .
H20A H 0.2316 -0.7191 0.6060 0.045 Uiso 1 1 calc R . .
C21 C 0.30251(13) -0.6737(4) 0.60455(18) 0.0343(8) Uani 1 1 d . . .
H21A H 0.3183 -0.7266 0.6412 0.041 Uiso 1 1 calc R . .
C22 C 0.30844(13) -0.5292(4) 0.52019(17) 0.0328(8) Uani 1 1 d . . .
H22A H 0.3283 -0.4803 0.4988 0.039 Uiso 1 1 calc R . .
C23 C -0.09401(12) 0.3852(3) 0.11740(17) 0.0286(8) Uani 1 1 d . . .
C24 C -0.08288(11) 0.5024(3) 0.16464(16) 0.0228(7) Uani 1 1 d . . .
C25 C -0.06659(12) 0.4796(3) 0.23373(16) 0.0264(7) Uani 1 1 d . . .
H25A H -0.0637 0.3929 0.2502 0.032 Uiso 1 1 calc R . .
C26 C -0.05472(12) 0.5853(3) 0.27767(16) 0.0245(7) Uani 1 1 d . . .
C27 C -0.03827(13) 0.5666(4) 0.35253(18) 0.0332(8) Uani 1 1 d . . .
C28 C -0.05864(12) 0.7142(3) 0.25290(16) 0.0240(7) Uani 1 1 d . . .
H28A H -0.0496 0.7852 0.2826 0.029 Uiso 1 1 calc R . .
C29 C -0.07579(11) 0.7386(3) 0.18451(15) 0.0224(7) Uani 1 1 d . . .
C30 C -0.08096(12) 0.8796(3) 0.16044(16) 0.0224(7) Uani 1 1 d . . .
C31 C -0.08803(12) 0.6318(3) 0.14025(16) 0.0224(7) Uani 1 1 d . . .
H31A H -0.0997 0.6472 0.0942 0.027 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 1.906(2) . ?
Cu1 O3 2.008(2) 1_545 ?
Cu1 N1 2.009(3) . ?
Cu1 N2 2.013(3) 8_445 ?
Cu1 O4 2.371(2) 1_545 ?
Cu1 C30 2.520(3) 1_545 ?
O1 C23 1.262(4) . ?
N1 C5 1.334(4) . ?
N1 C1 1.343(4) . ?
C1 C2 1.370(5) . ?
N2 C22 1.333(4) . ?
N2 C21 1.348(4) . ?
N2 Cu1 2.013(3) 8_546 ?
C2 C3 1.382(5) . ?
O2 C23 1.237(4) . ?
N3 C6 1.363(4) . ?
N3 C4 1.414(4) . ?
O3 C30 1.267(4) . ?
O3 Cu1 2.008(2) 1_565 ?
C3 C4 1.384(5) . ?
O4 C30 1.256(4) . ?
O4 Cu1 2.371(2) 1_565 ?
N4 C17 1.356(5) . ?
N4 C18 1.409(5) . ?
C4 C5 1.387(5) . ?
O5 C27 1.199(4) . ?
O6 C27 1.320(5) . ?
C6 O7 1.221(4) . ?
C6 C7 1.507(5) . ?
C7 C8 1.372(5) . ?
C7 C16 1.423(5) . ?
C8 C9 1.391(5) . ?
O8 C17 1.206(5) . ?
C9 C10 1.367(5) . ?
C10 C11 1.423(5) . ?
C10 C17 1.505(5) . ?
C11 C12 1.425(5) . ?
C11 C16 1.432(5) . ?
C12 C13 1.344(6) . ?
C13 C14 1.397(6) . ?
C14 C15 1.360(6) . ?
C15 C16 1.419(5) . ?
C18 C19 1.387(5) . ?
C18 C22 1.398(5) . ?
C19 C20 1.373(5) . ?
C20 C21 1.372(5) . ?
C23 C24 1.507(4) . ?
C24 C31 1.388(4) . ?
C24 C25 1.394(4) . ?
C25 C26 1.378(5) . ?
C26 C28 1.386(4) . ?
C26 C27 1.501(5) . ?
C28 C29 1.385(4) . ?
C29 C31 1.391(4) . ?
C29 C30 1.495(4) . ?
C30 Cu1 2.520(3) 1_565 ?

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 O3 156.52(10) . 1_545 ?
O1 Cu1 N1 94.19(11) . . ?
O3 Cu1 N1 91.38(10) 1_545 . ?
O1 Cu1 N2 94.23(11) . 8_445 ?
O3 Cu1 N2 90.28(10) 1_545 8_445 ?
N1 Cu1 N2 154.79(11) . 8_445 ?
O1 Cu1 O4 97.13(9) . 1_545 ?
O3 Cu1 O4 59.41(8) 1_545 1_545 ?
N1 Cu1 O4 99.98(10) . 1_545 ?
N2 Cu1 O4 102.49(10) 8_445 1_545 ?
O1 Cu1 C30 126.69(10) . 1_545 ?
O3 Cu1 C30 29.85(9) 1_545 1_545 ?
N1 Cu1 C30 96.73(10) . 1_545 ?
N2 Cu1 C30 97.16(10) 8_445 1_545 ?
O4 Cu1 C30 29.57(9) 1_545 1_545 ?
C23 O1 Cu1 126.8(2) . . ?
C5 N1 C1 118.5(3) . . ?
C5 N1 Cu1 120.1(2) . . ?
C1 N1 Cu1 120.9(2) . . ?
N1 C1 C2 121.7(3) . . ?
C22 N2 C21 118.9(3) . . ?
C22 N2 Cu1 118.0(2) . 8_546 ?
C21 N2 Cu1 123.1(2) . 8_546 ?
C1 C2 C3 120.2(3) . . ?
C6 N3 C4 125.2(3) . . ?
C30 O3 Cu1 98.06(18) . 1_565 ?
C2 C3 C4 118.3(3) . . ?
C30 O4 Cu1 81.80(18) . 1_565 ?
C17 N4 C18 126.8(3) . . ?
C3 C4 C5 118.4(3) . . ?
C3 C4 N3 124.2(3) . . ?
C5 C4 N3 117.4(3) . . ?
N1 C5 C4 122.9(3) . . ?
O7 C6 N3 124.1(3) . . ?
O7 C6 C7 122.9(3) . . ?
N3 C6 C7 113.0(3) . . ?
C8 C7 C16 120.2(3) . . ?
C8 C7 C6 118.5(3) . . ?
C16 C7 C6 121.3(3) . . ?
C7 C8 C9 121.2(4) . . ?
C10 C9 C8 120.8(4) . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 C17 116.1(4) . . ?
C11 C10 C17 123.5(4) . . ?
C10 C11 C12 122.3(3) . . ?
C10 C11 C16 119.1(3) . . ?
C12 C11 C16 118.6(4) . . ?
C13 C12 C11 120.9(4) . . ?
C12 C13 C14 120.8(4) . . ?
C15 C14 C13 120.6(4) . . ?
C14 C15 C16 121.2(4) . . ?
C15 C16 C7 123.7(3) . . ?
C15 C16 C11 117.8(3) . . ?
C7 C16 C11 118.5(3) . . ?
O8 C17 N4 122.5(4) . . ?
O8 C17 C10 120.6(4) . . ?
N4 C17 C10 116.9(3) . . ?
C19 C18 C22 118.2(3) . . ?
C19 C18 N4 119.5(3) . . ?
C22 C18 N4 122.3(3) . . ?
C20 C19 C18 118.9(3) . . ?
C21 C20 C19 120.0(3) . . ?
N2 C21 C20 121.7(3) . . ?
N2 C22 C18 122.3(3) . . ?
O2 C23 O1 124.6(3) . . ?
O2 C23 C24 120.6(3) . . ?
O1 C23 C24 114.7(3) . . ?
C31 C24 C25 119.9(3) . . ?
C31 C24 C23 121.0(3) . . ?
C25 C24 C23 119.1(3) . . ?
C26 C25 C24 120.0(3) . . ?
C25 C26 C28 119.8(3) . . ?
C25 C26 C27 122.3(3) . . ?
C28 C26 C27 118.0(3) . . ?
O5 C27 O6 123.7(3) . . ?
O5 C27 C26 122.5(3) . . ?
O6 C27 C26 113.8(3) . . ?
C29 C28 C26 120.9(3) . . ?
C28 C29 C31 119.2(3) . . ?
C28 C29 C30 118.9(3) . . ?
C31 C29 C30 121.9(3) . . ?
O4 C30 O3 120.7(3) . . ?
O4 C30 C29 119.5(3) . . ?
O3 C30 C29 119.8(3) . . ?
O4 C30 Cu1 68.63(17) . 1_565 ?
O3 C30 Cu1 52.09(15) . 1_565 ?
C29 C30 Cu1 171.9(2) . 1_565 ?
C24 C31 C29 120.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.94
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.072
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-4
_database_code_depnum_ccdc_archive 'CCDC 1005166'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H24 N4 O10 Zn'
_chemical_formula_weight         677.91

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/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                   27.781(2)
_cell_length_b                   10.0395(8)
_cell_length_c                   22.2588(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.2150(10)
_cell_angle_gamma                90.00
_cell_volume                     5862.4(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.55
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2784
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14524
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5161
_reflns_number_gt                4363
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0529P)²+5.8748P] 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         5161
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0959
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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
Zn1 Zn 0.101420(9) -0.00636(2) -0.113162(11) 0.02316(10) Uani 1 1 d . . .
O1 O 0.10458(8) 0.24623(18) -0.09013(9) 0.0484(5) Uani 1 1 d . . .
N1 N 0.17907(7) 0.00745(18) -0.07535(9) 0.0280(4) Uani 1 1 d . . .
C1 C 0.20581(10) 0.0831(3) -0.10217(13) 0.0459(7) Uani 1 1 d . . .
H1A H 0.1891 0.1236 -0.1410 0.055 Uiso 1 1 calc R . .
O1W O -0.04894(7) 0.4109(2) -0.50076(8) 0.0521(5) Uani 1 1 d . . .
H1WA H -0.0598 0.4090 -0.4692 0.063 Uiso 1 1 d R . .
H1WB H -0.0552 0.4878 -0.5174 0.063 Uiso 1 1 d R . .
O2 O 0.08092(7) 0.13316(16) -0.17952(8) 0.0402(4) Uani 1 1 d . . .
N2 N 0.07799(7) -0.02955(19) -0.03686(9) 0.0272(4) Uani 1 1 d . . .
C2 C 0.25700(11) 0.1027(4) -0.07423(15) 0.0735(12) Uani 1 1 d . . .
H2A H 0.2751 0.1528 -0.0947 0.088 Uiso 1 1 calc R . .
O2W O 0.05031(15) -0.0278(3) -0.29376(13) 0.1038(12) Uani 1 1 d . . .
H2WA H 0.0658 0.0206 -0.2619 0.125 Uiso 1 1 d R . .
H2WB H 0.0198 -0.0378 -0.2941 0.125 Uiso 1 1 d R . .
O3 O 0.01034(7) 0.38702(16) -0.38240(8) 0.0385(4) Uani 1 1 d . . .
C3 C 0.28149(11) 0.0477(4) -0.01546(15) 0.0667(10) Uani 1 1 d . . .
H3A H 0.3161 0.0625 0.0048 0.080 Uiso 1 1 calc R . .
O4 O 0.02641(7) 0.60418(17) -0.38409(8) 0.0423(4) Uani 1 1 d . . .
C4 C 0.25435(10) -0.0288(3) 0.01277(12) 0.0368(6) Uani 1 1 d . . .
O5 O 0.07392(6) 0.84048(15) -0.17003(7) 0.0327(4) Uani 1 1 d . . .
N5 N 0.27722(8) -0.0835(2) 0.07416(9) 0.0390(5) Uani 1 1 d . . .
H5B H 0.3050 -0.1282 0.0818 0.047 Uiso 1 1 calc R . .
C5 C 0.20308(9) -0.0491(2) -0.01946(10) 0.0292(5) Uani 1 1 d . . .
H5A H 0.1847 -0.1044 -0.0014 0.035 Uiso 1 1 calc R . .
O6 O 0.12930(6) 0.72791(16) -0.09221(7) 0.0350(4) Uani 1 1 d . . .
N6 N 0.39505(7) -0.3807(2) 0.37760(9) 0.0321(5) Uani 1 1 d . . .
H6A H 0.4024 -0.4021 0.3442 0.039 Uiso 1 1 calc R . .
C6 C 0.25698(10) -0.0682(3) 0.12115(12) 0.0454(7) Uani 1 1 d . . .
C7 C 0.28952(9) -0.1174(3) 0.18564(11) 0.0380(6) Uani 1 1 d . . .
C8 C 0.30617(9) -0.0247(3) 0.23685(12) 0.0350(6) Uani 1 1 d . . .
C9 C 0.29763(11) 0.1139(3) 0.22745(14) 0.0492(7) Uani 1 1 d . . .
H9A H 0.2799 0.1454 0.1869 0.059 Uiso 1 1 calc R . .
C10 C 0.31444(12) 0.2011(3) 0.27566(16) 0.0559(8) Uani 1 1 d . . .
H10A H 0.3083 0.2916 0.2682 0.067 Uiso 1 1 calc R . .
C11 C 0.34139(12) 0.1557(3) 0.33742(14) 0.0505(7) Uani 1 1 d . . .
H11A H 0.3531 0.2164 0.3706 0.061 Uiso 1 1 calc R . .
C12 C 0.35036(10) 0.0235(3) 0.34875(13) 0.0396(6) Uani 1 1 d . . .
H12A H 0.3680 -0.0050 0.3899 0.048 Uiso 1 1 calc R . .
O13 O 0.21536(9) -0.0190(3) 0.11288(10) 0.0793(9) Uani 1 1 d . . .
C13 C 0.33336(9) -0.0719(3) 0.29927(11) 0.0307(5) Uani 1 1 d . . .
O14 O 0.35909(7) -0.22038(18) 0.42020(8) 0.0400(4) Uani 1 1 d . . .
C14 C 0.34260(9) -0.2127(2) 0.30820(11) 0.0307(5) Uani 1 1 d . . .
C15 C 0.32651(10) -0.2966(3) 0.25702(12) 0.0391(6) Uani 1 1 d . . .
H15A H 0.3332 -0.3873 0.2630 0.047 Uiso 1 1 calc R . .
C16 C 0.30015(10) -0.2492(3) 0.19574(12) 0.0418(6) Uani 1 1 d . . .
H16A H 0.2899 -0.3085 0.1618 0.050 Uiso 1 1 calc R . .
C17 C 0.36635(9) -0.2700(2) 0.37358(11) 0.0297(5) Uani 1 1 d . . .
C18 C 0.41403(9) -0.4643(2) 0.43088(11) 0.0281(5) Uani 1 1 d . . .
C19 C 0.44416(11) -0.5717(3) 0.42683(12) 0.0418(6) Uani 1 1 d . . .
H19A H 0.4519 -0.5866 0.3898 0.050 Uiso 1 1 calc R . .
C20 C 0.46239(12) -0.6556(3) 0.47783(13) 0.0490(7) Uani 1 1 d . . .
H20A H 0.4824 -0.7283 0.4754 0.059 Uiso 1 1 calc R . .
C21 C 0.04889(10) -0.1322(2) -0.03231(12) 0.0375(6) Uani 1 1 d . . .
H21A H 0.0360 -0.1891 -0.0669 0.045 Uiso 1 1 calc R . .
C22 C 0.09602(9) 0.0532(2) 0.01261(10) 0.0276(5) Uani 1 1 d . . .
H22A H 0.1160 0.1251 0.0090 0.033 Uiso 1 1 calc R . .
C23 C 0.08885(9) 0.2424(2) -0.14904(12) 0.0314(5) Uani 1 1 d . . .
C24 C 0.07951(8) 0.3690(2) -0.18626(10) 0.0251(5) Uani 1 1 d . . .
C25 C 0.05906(8) 0.3720(2) -0.25250(10) 0.0252(5) Uani 1 1 d . . .
H25A H 0.0513 0.2928 -0.2753 0.030 Uiso 1 1 calc R . .
C26 C 0.05023(8) 0.4934(2) -0.28437(10) 0.0230(5) Uani 1 1 d . . .
C27 C 0.02818(9) 0.5008(2) -0.35479(11) 0.0278(5) Uani 1 1 d . . .
C28 C 0.06146(8) 0.6115(2) -0.25026(10) 0.0233(5) Uani 1 1 d . . .
H28A H 0.0551 0.6926 -0.2716 0.028 Uiso 1 1 calc R . .
C29 C 0.08227(8) 0.6088(2) -0.18427(10) 0.0227(5) Uani 1 1 d . . .
C30 C 0.09645(8) 0.7332(2) -0.14591(10) 0.0254(5) Uani 1 1 d . . .
C31 C 0.09111(9) 0.4878(2) -0.15327(11) 0.0247(5) Uani 1 1 d . . .
H31A H 0.1052 0.4860 -0.1091 0.030 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
Zn1 O5 1.9782(15) 1_545 ?
Zn1 O2 1.9785(16) . ?
Zn1 N2 2.0222(19) . ?
Zn1 N1 2.046(2) . ?
O1 C23 1.239(3) . ?
N1 C5 1.330(3) . ?
N1 C1 1.333(3) . ?
C1 C2 1.366(4) . ?
C1 H1A 0.9300 . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8500 . ?
O2 C23 1.270(3) . ?
N2 C21 1.335(3) . ?
N2 C22 1.338(3) . ?
C2 C3 1.376(4) . ?
C2 H2A 0.9300 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8501 . ?
O3 C27 1.315(3) . ?
C3 C4 1.366(4) . ?
C3 H3A 0.9300 . ?
O4 C27 1.218(3) . ?
C4 C5 1.383(3) . ?
C4 N5 1.415(3) . ?
O5 C30 1.272(3) . ?
O5 Zn1 1.9783(15) 1_565 ?
N5 C6 1.350(3) . ?
N5 H5B 0.8600 . ?
C5 H5A 0.9300 . ?
O6 C30 1.244(3) . ?
N6 C17 1.354(3) . ?
N6 C18 1.406(3) . ?
N6 H6A 0.8600 . ?
C6 O13 1.214(3) . ?
C6 C7 1.506(3) . ?
C7 C16 1.359(4) . ?
C7 C8 1.425(4) . ?
C8 C9 1.416(4) . ?
C8 C13 1.426(3) . ?
C9 C10 1.344(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.407(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.358(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.419(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.439(3) . ?
O14 C17 1.226(3) . ?
C14 C15 1.368(3) . ?
C14 C17 1.501(3) . ?
C15 C16 1.402(3) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C18 C19 1.386(3) . ?
C18 C22 1.387(3) 4_545 ?
C19 C20 1.370(4) . ?
C19 H19A 0.9300 . ?
C20 C21 1.369(4) 4_545 ?
C20 H20A 0.9300 . ?
C21 C20 1.369(4) 4 ?
C21 H21A 0.9300 . ?
C22 C18 1.386(3) 4 ?
C22 H22A 0.9300 . ?
C23 C24 1.493(3) . ?
C24 C31 1.382(3) . ?
C24 C25 1.395(3) . ?
C25 C26 1.390(3) . ?
C25 H25A 0.9300 . ?
C26 C28 1.387(3) . ?
C26 C27 1.485(3) . ?
C28 C29 1.391(3) . ?
C28 H28A 0.9300 . ?
C29 C31 1.379(3) . ?
C29 C30 1.491(3) . ?
C31 H31A 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
O5 Zn1 O2 96.71(7) 1_545 . ?
O5 Zn1 N2 106.53(7) 1_545 . ?
O2 Zn1 N2 127.98(8) . . ?
O5 Zn1 N1 116.67(7) 1_545 . ?
O2 Zn1 N1 105.34(7) . . ?
N2 Zn1 N1 104.45(8) . . ?
C5 N1 C1 118.7(2) . . ?
C5 N1 Zn1 119.48(16) . . ?
C1 N1 Zn1 121.46(16) . . ?
N1 C1 C2 121.9(2) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
H1WA O1W H1WB 107.7 . . ?
C23 O2 Zn1 104.83(14) . . ?
C21 N2 C22 119.3(2) . . ?
C21 N2 Zn1 121.55(16) . . ?
C22 N2 Zn1 118.87(15) . . ?
C1 C2 C3 119.3(3) . . ?
C1 C2 H2A 120.3 . . ?
C3 C2 H2A 120.3 . . ?
H2WA O2W H2WB 107.7 . . ?
C4 C3 C2 119.2(3) . . ?
C4 C3 H3A 120.4 . . ?
C2 C3 H3A 120.4 . . ?
C3 C4 C5 118.3(2) . . ?
C3 C4 N5 121.5(2) . . ?
C5 C4 N5 120.2(2) . . ?
C30 O5 Zn1 110.80(13) . 1_565 ?
C6 N5 C4 122.4(2) . . ?
C6 N5 H5B 118.8 . . ?
C4 N5 H5B 118.8 . . ?
N1 C5 C4 122.4(2) . . ?
N1 C5 H5A 118.8 . . ?
C4 C5 H5A 118.8 . . ?
C17 N6 C18 126.53(19) . . ?
C17 N6 H6A 116.7 . . ?
C18 N6 H6A 116.7 . . ?
O13 C6 N5 123.2(2) . . ?
O13 C6 C7 121.4(2) . . ?
N5 C6 C7 115.4(2) . . ?
C16 C7 C8 120.5(2) . . ?
C16 C7 C6 120.4(3) . . ?
C8 C7 C6 118.9(2) . . ?
C9 C8 C7 121.9(2) . . ?
C9 C8 C13 118.7(2) . . ?
C7 C8 C13 119.4(2) . . ?
C10 C9 C8 121.7(3) . . ?
C10 C9 H9A 119.2 . . ?
C8 C9 H9A 119.2 . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 H10A 119.9 . . ?
C11 C10 H10A 119.9 . . ?
C12 C11 C10 120.2(3) . . ?
C12 C11 H11A 119.9 . . ?
C10 C11 H11A 119.9 . . ?
C11 C12 C13 121.5(3) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C8 117.8(2) . . ?
C12 C13 C14 123.9(2) . . ?
C8 C13 C14 118.3(2) . . ?
C15 C14 C13 119.7(2) . . ?
C15 C14 C17 119.4(2) . . ?
C13 C14 C17 120.8(2) . . ?
C14 C15 C16 121.6(3) . . ?
C14 C15 H15A 119.2 . . ?
C16 C15 H15A 119.2 . . ?
C7 C16 C15 120.4(3) . . ?
C7 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
O14 C17 N6 122.3(2) . . ?
O14 C17 C14 121.5(2) . . ?
N6 C17 C14 116.1(2) . . ?
C19 C18 C22 117.7(2) . 4_545 ?
C19 C18 N6 118.4(2) . . ?
C22 C18 N6 123.9(2) 4_545 . ?
C20 C19 C18 119.4(2) . . ?
C20 C19 H19A 120.3 . . ?
C18 C19 H19A 120.3 . . ?
C21 C20 C19 119.9(2) 4_545 . ?
C21 C20 H20A 120.0 4_545 . ?
C19 C20 H20A 120.0 . . ?
N2 C21 C20 121.4(2) . 4 ?
N2 C21 H21A 119.3 . . ?
C20 C21 H21A 119.3 4 . ?
N2 C22 C18 122.3(2) . 4 ?
N2 C22 H22A 118.8 . . ?
C18 C22 H22A 118.8 4 . ?
O1 C23 O2 122.1(2) . . ?
O1 C23 C24 119.8(2) . . ?
O2 C23 C24 118.1(2) . . ?
C31 C24 C25 119.1(2) . . ?
C31 C24 C23 118.19(19) . . ?
C25 C24 C23 122.7(2) . . ?
C26 C25 C24 120.0(2) . . ?
C26 C25 H25A 120.0 . . ?
C24 C25 H25A 120.0 . . ?
C28 C26 C25 120.0(2) . . ?
C28 C26 C27 118.33(18) . . ?
C25 C26 C27 121.67(19) . . ?
O4 C27 O3 123.2(2) . . ?
O4 C27 C26 122.6(2) . . ?
O3 C27 C26 114.22(19) . . ?
C26 C28 C29 120.13(19) . . ?
C26 C28 H28A 119.9 . . ?
C29 C28 H28A 119.9 . . ?
C31 C29 C28 119.30(19) . . ?
C31 C29 C30 118.79(19) . . ?
C28 C29 C30 121.90(19) . . ?
O6 C30 O5 123.1(2) . . ?
O6 C30 C29 119.11(19) . . ?
O5 C30 C29 117.83(18) . . ?
C29 C31 C24 121.5(2) . . ?
C29 C31 H31A 119.3 . . ?
C24 C31 H31A 119.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Zn1 N1 C5 -91.09(18) 1_545 . . . ?
O2 Zn1 N1 C5 163.04(17) . . . . ?
N2 Zn1 N1 C5 26.19(19) . . . . ?
O5 Zn1 N1 C1 95.8(2) 1_545 . . . ?
O2 Zn1 N1 C1 -10.1(2) . . . . ?
N2 Zn1 N1 C1 -146.9(2) . . . . ?
C5 N1 C1 C2 0.7(4) . . . . ?
Zn1 N1 C1 C2 173.9(3) . . . . ?
O5 Zn1 O2 C23 170.02(16) 1_545 . . . ?
N2 Zn1 O2 C23 52.93(19) . . . . ?
N1 Zn1 O2 C23 -69.92(17) . . . . ?
O5 Zn1 N2 C21 -1.0(2) 1_545 . . . ?
O2 Zn1 N2 C21 111.75(19) . . . . ?
N1 Zn1 N2 C21 -125.04(19) . . . . ?
O5 Zn1 N2 C22 172.78(17) 1_545 . . . ?
O2 Zn1 N2 C22 -74.5(2) . . . . ?
N1 Zn1 N2 C22 48.73(19) . . . . ?
N1 C1 C2 C3 -2.8(6) . . . . ?
C1 C2 C3 C4 2.0(6) . . . . ?
C2 C3 C4 C5 0.7(5) . . . . ?
C2 C3 C4 N5 -177.6(3) . . . . ?
C3 C4 N5 C6 128.4(4) . . . . ?
C5 C4 N5 C6 -49.9(4) . . . . ?
C1 N1 C5 C4 2.2(4) . . . . ?
Zn1 N1 C5 C4 -171.12(19) . . . . ?
C3 C4 C5 N1 -2.9(4) . . . . ?
N5 C4 C5 N1 175.4(2) . . . . ?
C4 N5 C6 O13 7.9(5) . . . . ?
C4 N5 C6 C7 -172.4(2) . . . . ?
O13 C6 C7 C16 114.2(4) . . . . ?
N5 C6 C7 C16 -65.5(4) . . . . ?
O13 C6 C7 C8 -61.7(4) . . . . ?
N5 C6 C7 C8 118.6(3) . . . . ?
C16 C7 C8 C9 177.3(3) . . . . ?
C6 C7 C8 C9 -6.8(4) . . . . ?
C16 C7 C8 C13 -1.2(4) . . . . ?
C6 C7 C8 C13 174.8(2) . . . . ?
C7 C8 C9 C10 -178.4(3) . . . . ?
C13 C8 C9 C10 0.0(4) . . . . ?
C8 C9 C10 C11 0.1(5) . . . . ?
C9 C10 C11 C12 -0.3(5) . . . . ?
C10 C11 C12 C13 0.4(4) . . . . ?
C11 C12 C13 C8 -0.3(4) . . . . ?
C11 C12 C13 C14 178.7(3) . . . . ?
C9 C8 C13 C12 0.1(3) . . . . ?
C7 C8 C13 C12 178.5(2) . . . . ?
C9 C8 C13 C14 -179.0(2) . . . . ?
C7 C8 C13 C14 -0.5(3) . . . . ?
C12 C13 C14 C15 -177.3(2) . . . . ?
C8 C13 C14 C15 1.7(3) . . . . ?
C12 C13 C14 C17 7.1(4) . . . . ?
C8 C13 C14 C17 -173.9(2) . . . . ?
C13 C14 C15 C16 -1.3(4) . . . . ?
C17 C14 C15 C16 174.4(2) . . . . ?
C8 C7 C16 C15 1.7(4) . . . . ?
C6 C7 C16 C15 -174.2(2) . . . . ?
C14 C15 C16 C7 -0.4(4) . . . . ?
C18 N6 C17 O14 9.7(4) . . . . ?
C18 N6 C17 C14 -168.8(2) . . . . ?
C15 C14 C17 O14 -143.7(3) . . . . ?
C13 C14 C17 O14 31.9(3) . . . . ?
C15 C14 C17 N6 34.8(3) . . . . ?
C13 C14 C17 N6 -149.6(2) . . . . ?
C17 N6 C18 C19 -178.1(2) . . . . ?
C17 N6 C18 C22 2.6(4) . . . 4_545 ?
C22 C18 C19 C20 0.3(4) 4_545 . . . ?
N6 C18 C19 C20 -179.0(3) . . . . ?
C18 C19 C20 C21 -0.5(5) . . . 4_545 ?
C22 N2 C21 C20 -0.8(4) . . . 4 ?
Zn1 N2 C21 C20 172.9(2) . . . 4 ?
C21 N2 C22 C18 0.6(4) . . . 4 ?
Zn1 N2 C22 C18 -173.27(18) . . . 4 ?
Zn1 O2 C23 O1 -2.1(3) . . . . ?
Zn1 O2 C23 C24 176.89(17) . . . . ?
O1 C23 C24 C31 2.9(3) . . . . ?
O2 C23 C24 C31 -176.1(2) . . . . ?
O1 C23 C24 C25 -176.2(2) . . . . ?
O2 C23 C24 C25 4.8(3) . . . . ?
C31 C24 C25 C26 -0.5(3) . . . . ?
C23 C24 C25 C26 178.6(2) . . . . ?
C24 C25 C26 C28 -0.4(3) . . . . ?
C24 C25 C26 C27 -179.6(2) . . . . ?
C28 C26 C27 O4 10.8(4) . . . . ?
C25 C26 C27 O4 -170.0(2) . . . . ?
C28 C26 C27 O3 -168.5(2) . . . . ?
C25 C26 C27 O3 10.7(3) . . . . ?
C25 C26 C28 C29 1.0(3) . . . . ?
C27 C26 C28 C29 -179.8(2) . . . . ?
C26 C28 C29 C31 -0.6(3) . . . . ?
C26 C28 C29 C30 178.0(2) . . . . ?
Zn1 O5 C30 O6 3.5(3) 1_565 . . . ?
Zn1 O5 C30 C29 -176.77(15) 1_565 . . . ?
C31 C29 C30 O6 22.7(3) . . . . ?
C28 C29 C30 O6 -156.0(2) . . . . ?
C31 C29 C30 O5 -157.1(2) . . . . ?
C28 C29 C30 O5 24.2(3) . . . . ?
C28 C29 C31 C24 -0.3(3) . . . . ?
C30 C29 C31 C24 -179.0(2) . . . . ?
C25 C24 C31 C29 0.9(3) . . . . ?
C23 C24 C31 C29 -178.3(2) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.053
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-5
_database_code_depnum_ccdc_archive 'CCDC 1005167'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H26 Cd N4 O11'
_chemical_formula_weight         742.96

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'
Cd Cd -0.8075 1.2024 '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                   10.0186(6)
_cell_length_b                   10.2419(6)
_cell_length_c                   14.6114(8)
_cell_angle_alpha                90.7530(10)
_cell_angle_beta                 93.9340(10)
_cell_angle_gamma                90.7470(10)
_cell_volume                     1495.46(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.99
_cell_measurement_theta_max      28.48

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11175
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         28.48
_reflns_number_total             7471
_reflns_number_gt                6702
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0392P)²+0.8674P] 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         7471
_refine_ls_number_parameters     424
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0747
_refine_ls_wR_factor_gt          0.0719
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd -0.076444(14) 0.326839(14) 0.836244(10) 0.01852(5) Uani 1 1 d . . .
O1 O -0.06075(15) 0.07928(15) 0.82011(12) 0.0284(3) Uani 1 1 d . . .
N1 N 0.15588(17) 0.31943(17) 0.85845(13) 0.0229(4) Uani 1 1 d . . .
C1 C 0.2228(2) 0.4169(2) 0.90407(16) 0.0261(4) Uani 1 1 d . . .
H1A H 0.1751 0.4780 0.9358 0.031 Uiso 1 1 calc R . .
O1W O -0.09364(16) 0.29120(16) 0.99465(11) 0.0297(3) Uani 1 1 d . . .
H1WA H -0.0462 0.2946 1.0452 0.036 Uiso 1 1 d R . .
H1WB H -0.1752 0.2962 1.0068 0.036 Uiso 1 1 d R . .
O2 O -0.25840(16) 0.17068(14) 0.82490(12) 0.0300(4) Uani 1 1 d . . .
N2 N -0.0816(2) 0.3377(2) 0.67569(13) 0.0295(4) Uani 1 1 d . . .
C2 C 0.3600(2) 0.4295(2) 0.90539(17) 0.0285(5) Uani 1 1 d . . .
H2A H 0.4041 0.4963 0.9396 0.034 Uiso 1 1 calc R . .
O2W O -0.88309(17) -0.03269(19) 0.94519(14) 0.0402(4) Uani 1 1 d . . .
H2WA H -0.8256 0.0237 0.9662 0.048 Uiso 1 1 d R . .
H2WB H -0.9212 -0.0025 0.8963 0.048 Uiso 1 1 d R . .
O3 O -0.63902(17) -0.05608(17) 0.91052(14) 0.0374(4) Uani 1 1 d . . .
N3 N 0.43788(18) 0.15470(18) 0.75593(13) 0.0241(4) Uani 1 1 d . . .
H3B H 0.5236 0.1623 0.7628 0.029 Uiso 1 1 calc R . .
C3 C 0.4320(2) 0.3426(2) 0.85577(16) 0.0269(5) Uani 1 1 d . . .
H3A H 0.5244 0.3514 0.8549 0.032 Uiso 1 1 calc R . .
O3W O 0.0138(2) -0.0673(3) 0.66095(18) 0.0833(10) Uani 1 1 d . . .
H3WA H -0.0212 -0.0253 0.7036 0.100 Uiso 1 1 d R . .
H3WB H 0.0930 -0.0379 0.6575 0.100 Uiso 1 1 d R . .
O4 O -0.64176(17) -0.26520(16) 0.95192(13) 0.0352(4) Uani 1 1 d . . .
C4 C 0.3638(2) 0.2419(2) 0.80723(14) 0.0206(4) Uani 1 1 d . . .
N4 N 0.8923(2) -0.2228(2) 0.51661(14) 0.0366(5) Uani 1 1 d . . .
H4A H 0.9155 -0.1753 0.5642 0.044 Uiso 1 1 calc R . .
C5 C 0.2254(2) 0.2312(2) 0.81258(15) 0.0222(4) Uani 1 1 d . . .
H5A H 0.1798 0.1609 0.7835 0.027 Uiso 1 1 calc R . .
O5 O -0.24672(16) -0.52355(15) 0.83801(12) 0.0305(4) Uani 1 1 d . . .
O6 O -0.05093(16) -0.42588(16) 0.86825(13) 0.0320(4) Uani 1 1 d . . .
C6 C 0.3879(2) 0.0598(2) 0.69677(16) 0.0264(4) Uani 1 1 d . . .
O7 O 0.26837(17) 0.04158(19) 0.67842(14) 0.0417(5) Uani 1 1 d . . .
C7 C 0.4906(2) -0.0215(2) 0.65352(15) 0.0253(4) Uani 1 1 d . . .
O8 O 0.7130(2) -0.3111(2) 0.43328(14) 0.0474(5) Uani 1 1 d . . .
C8 C 0.4763(2) -0.1606(2) 0.65044(15) 0.0243(4) Uani 1 1 d . . .
C9 C 0.3767(2) -0.2298(2) 0.69580(16) 0.0310(5) Uani 1 1 d . . .
H9A H 0.3143 -0.1833 0.7269 0.037 Uiso 1 1 calc R . .
C10 C 0.3709(3) -0.3622(3) 0.69454(18) 0.0394(6) Uani 1 1 d . . .
H10A H 0.3054 -0.4053 0.7253 0.047 Uiso 1 1 calc R . .
C11 C 0.4630(3) -0.4350(3) 0.64723(19) 0.0415(6) Uani 1 1 d . . .
H11A H 0.4586 -0.5257 0.6470 0.050 Uiso 1 1 calc R . .
C12 C 0.5588(3) -0.3725(2) 0.60167(18) 0.0360(6) Uani 1 1 d . . .
H12A H 0.6185 -0.4215 0.5699 0.043 Uiso 1 1 calc R . .
C13 C 0.5693(2) -0.2343(2) 0.60160(15) 0.0260(4) Uani 1 1 d . . .
C14 C 0.6719(2) -0.1670(2) 0.55726(16) 0.0288(5) Uani 1 1 d . . .
C15 C 0.6846(2) -0.0339(2) 0.56446(17) 0.0325(5) Uani 1 1 d . . .
H15A H 0.7539 0.0086 0.5372 0.039 Uiso 1 1 calc R . .
C16 C 0.5935(2) 0.0391(2) 0.61282(17) 0.0309(5) Uani 1 1 d . . .
H16A H 0.6033 0.1294 0.6172 0.037 Uiso 1 1 calc R . .
C17 C 0.7597(2) -0.2415(2) 0.49608(17) 0.0317(5) Uani 1 1 d . . .
C18 C 0.0191(2) 0.2969(3) 0.62702(16) 0.0335(5) Uani 1 1 d . . .
H18A H 0.1022 0.2834 0.6575 0.040 Uiso 1 1 calc R . .
C19 C 0.0042(2) 0.2740(3) 0.53298(16) 0.0317(5) Uani 1 1 d . . .
C20 C -0.1198(3) 0.2953(3) 0.48839(19) 0.0465(7) Uani 1 1 d . . .
H20A H -0.1334 0.2810 0.4254 0.056 Uiso 1 1 calc R . .
C21 C -0.2231(3) 0.3380(4) 0.5388(2) 0.0514(8) Uani 1 1 d . . .
H21A H -0.3072 0.3527 0.5101 0.062 Uiso 1 1 calc R . .
C22 C -0.2002(3) 0.3586(3) 0.63191(18) 0.0386(6) Uani 1 1 d . . .
H22A H -0.2698 0.3881 0.6653 0.046 Uiso 1 1 calc R . .
C23 C -0.1851(2) 0.07201(19) 0.82918(14) 0.0202(4) Uani 1 1 d . . .
C24 C -0.2485(2) -0.05814(19) 0.84859(14) 0.0191(4) Uani 1 1 d . . .
C25 C -0.3776(2) -0.0582(2) 0.87728(14) 0.0207(4) Uani 1 1 d . . .
H25A H -0.4206 0.0208 0.8847 0.025 Uiso 1 1 calc R . .
C26 C -0.4436(2) -0.1741(2) 0.89519(14) 0.0202(4) Uani 1 1 d . . .
C27 C -0.5843(2) -0.1707(2) 0.92243(15) 0.0230(4) Uani 1 1 d . . .
C28 C -0.3786(2) -0.2919(2) 0.88452(14) 0.0201(4) Uani 1 1 d . . .
H28A H -0.4233 -0.3701 0.8941 0.024 Uiso 1 1 calc R . .
C29 C -0.2470(2) -0.29358(19) 0.85966(14) 0.0191(4) Uani 1 1 d . . .
C30 C -0.1765(2) -0.4222(2) 0.85462(14) 0.0212(4) Uani 1 1 d . . .
C31 C -0.1817(2) -0.17612(19) 0.84131(14) 0.0204(4) Uani 1 1 d . . .
H31A H -0.0939 -0.1767 0.8243 0.024 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
Cd1 O5 2.3091(16) 1_565 ?
Cd1 N1 2.3303(18) . ?
Cd1 N2 2.3470(19) . ?
Cd1 O1W 2.3655(16) . ?
Cd1 O2 2.4050(16) . ?
Cd1 O1 2.5512(16) . ?
Cd1 O6 2.5756(16) 1_565 ?
O1 C23 1.264(3) . ?
N1 C1 1.339(3) . ?
N1 C5 1.347(3) . ?
C1 C2 1.378(3) . ?
O2 C23 1.256(3) . ?
N2 C22 1.331(3) . ?
N2 C18 1.341(3) . ?
C2 C3 1.382(3) . ?
O3 C27 1.311(3) . ?
N3 C6 1.360(3) . ?
N3 C4 1.410(3) . ?
C3 C4 1.389(3) . ?
O4 C27 1.218(3) . ?
C4 C5 1.396(3) . ?
N4 C17 1.352(3) . ?
N4 C19 1.408(3) 2_656 ?
O5 C30 1.258(3) . ?
O5 Cd1 2.3091(16) 1_545 ?
O6 C30 1.261(3) . ?
O6 Cd1 2.5756(16) 1_545 ?
C6 O7 1.220(3) . ?
C6 C7 1.500(3) . ?
C7 C16 1.371(3) . ?
C7 C8 1.430(3) . ?
O8 C17 1.218(3) . ?
C8 C9 1.422(3) . ?
C8 C13 1.429(3) . ?
C9 C10 1.357(4) . ?
C10 C11 1.406(4) . ?
C11 C12 1.362(4) . ?
C12 C13 1.418(3) . ?
C13 C14 1.427(3) . ?
C14 C15 1.369(3) . ?
C14 C17 1.505(3) . ?
C15 C16 1.408(3) . ?
C18 C19 1.388(3) . ?
C19 C20 1.383(3) . ?
C19 N4 1.408(3) 2_656 ?
C20 C21 1.383(4) . ?
C21 C22 1.377(4) . ?
C23 C24 1.507(3) . ?
C24 C25 1.387(3) . ?
C24 C31 1.395(3) . ?
C25 C26 1.389(3) . ?
C26 C28 1.390(3) . ?
C26 C27 1.491(3) . ?
C28 C29 1.392(3) . ?
C29 C31 1.400(3) . ?
C29 C30 1.506(3) . ?

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
O5 Cd1 N1 139.63(6) 1_565 . ?
O5 Cd1 N2 90.27(7) 1_565 . ?
N1 Cd1 N2 95.47(7) . . ?
O5 Cd1 O1W 89.85(6) 1_565 . ?
N1 Cd1 O1W 89.72(6) . . ?
N2 Cd1 O1W 171.82(6) . . ?
O5 Cd1 O2 83.35(5) 1_565 . ?
N1 Cd1 O2 136.35(6) . . ?
N2 Cd1 O2 90.35(7) . . ?
O1W Cd1 O2 81.54(6) . . ?
O5 Cd1 O1 136.05(5) 1_565 . ?
N1 Cd1 O1 84.17(6) . . ?
N2 Cd1 O1 88.00(6) . . ?
O1W Cd1 O1 86.24(6) . . ?
O2 Cd1 O1 52.77(5) . . ?
O5 Cd1 O6 53.33(5) 1_565 1_565 ?
N1 Cd1 O6 86.30(6) . 1_565 ?
N2 Cd1 O6 96.73(7) . 1_565 ?
O1W Cd1 O6 89.90(6) . 1_565 ?
O2 Cd1 O6 135.95(5) . 1_565 ?
O1 Cd1 O6 169.73(5) . 1_565 ?
C23 O1 Cd1 88.28(12) . . ?
C1 N1 C5 118.74(18) . . ?
C1 N1 Cd1 119.68(14) . . ?
C5 N1 Cd1 120.54(14) . . ?
N1 C1 C2 122.0(2) . . ?
C23 O2 Cd1 95.21(13) . . ?
C22 N2 C18 118.7(2) . . ?
C22 N2 Cd1 116.68(16) . . ?
C18 N2 Cd1 123.02(16) . . ?
C1 C2 C3 119.8(2) . . ?
C6 N3 C4 126.73(18) . . ?
C2 C3 C4 118.8(2) . . ?
C3 C4 C5 118.35(19) . . ?
C3 C4 N3 118.34(19) . . ?
C5 C4 N3 123.31(19) . . ?
C17 N4 C19 125.8(2) . 2_656 ?
N1 C5 C4 122.18(19) . . ?
C30 O5 Cd1 98.47(13) . 1_545 ?
C30 O6 Cd1 85.98(12) . 1_545 ?
O7 C6 N3 123.3(2) . . ?
O7 C6 C7 121.5(2) . . ?
N3 C6 C7 115.25(19) . . ?
C16 C7 C8 120.6(2) . . ?
C16 C7 C6 119.4(2) . . ?
C8 C7 C6 119.9(2) . . ?
C9 C8 C13 118.2(2) . . ?
C9 C8 C7 123.3(2) . . ?
C13 C8 C7 118.4(2) . . ?
C10 C9 C8 121.3(2) . . ?
C9 C10 C11 120.6(2) . . ?
C12 C11 C10 120.0(2) . . ?
C11 C12 C13 121.4(2) . . ?
C12 C13 C14 122.4(2) . . ?
C12 C13 C8 118.5(2) . . ?
C14 C13 C8 119.1(2) . . ?
C15 C14 C13 120.5(2) . . ?
C15 C14 C17 119.6(2) . . ?
C13 C14 C17 119.7(2) . . ?
C14 C15 C16 120.5(2) . . ?
C7 C16 C15 120.7(2) . . ?
O8 C17 N4 124.0(2) . . ?
O8 C17 C14 121.8(2) . . ?
N4 C17 C14 114.2(2) . . ?
N2 C18 C19 122.7(2) . . ?
C20 C19 C18 118.1(2) . . ?
C20 C19 N4 119.5(2) . 2_656 ?
C18 C19 N4 122.3(2) . 2_656 ?
C19 C20 C21 119.0(2) . . ?
C22 C21 C20 119.3(2) . . ?
N2 C22 C21 122.2(2) . . ?
O2 C23 O1 122.21(19) . . ?
O2 C23 C24 118.26(19) . . ?
O1 C23 C24 119.50(18) . . ?
C25 C24 C31 119.47(18) . . ?
C25 C24 C23 117.61(18) . . ?
C31 C24 C23 122.90(18) . . ?
C24 C25 C26 121.12(19) . . ?
C25 C26 C28 119.22(19) . . ?
C25 C26 C27 119.62(18) . . ?
C28 C26 C27 121.12(18) . . ?
O4 C27 O3 124.0(2) . . ?
O4 C27 C26 123.17(19) . . ?
O3 C27 C26 112.81(18) . . ?
C26 C28 C29 120.50(18) . . ?
C28 C29 C31 119.70(18) . . ?
C28 C29 C30 119.15(18) . . ?
C31 C29 C30 121.14(18) . . ?
O5 C30 O6 122.16(19) . . ?
O5 C30 C29 117.99(18) . . ?
O6 C30 C29 119.84(18) . . ?
C24 C31 C29 119.88(18) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        28.48
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.074
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-6
_database_code_depnum_ccdc_archive 'CCDC 1005168'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H28 Co N4 O12'
_chemical_formula_weight         707.50

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'
Co Co 0.3494 0.9721 '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                   10.0522(16)
_cell_length_b                   11.4431(18)
_cell_length_c                   15.205(2)
_cell_angle_alpha                96.493(3)
_cell_angle_beta                 102.803(3)
_cell_angle_gamma                105.101(2)
_cell_volume                     1619.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.40
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            PINK
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_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             730
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8304
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5671
_reflns_number_gt                4979
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.1089P)²+0.3836P] 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         5671
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.1501
_refine_ls_wR_factor_gt          0.1429
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.40212(3) 0.11698(3) 0.54724(2) 0.01878(15) Uani 1 1 d . . .
N1 N 0.4130(2) 0.0150(2) 0.65701(16) 0.0285(5) Uani 1 1 d . . .
O1 O 0.1955(2) 0.11733(19) 0.55189(16) 0.0390(5) Uani 1 1 d . . .
C1 C 0.3307(3) -0.1000(3) 0.6473(2) 0.0413(8) Uani 1 1 d . . .
H1A H 0.2661 -0.1359 0.5907 0.050 Uiso 1 1 calc R . .
O1W O 0.0341(4) 0.8317(3) 0.7992(2) 0.0841(10) Uani 1 1 d . . .
H1WA H 0.0220 0.7719 0.7567 0.101 Uiso 1 1 d R . .
H1WB H 0.0510 0.8974 0.7771 0.101 Uiso 1 1 d R . .
O2 O 0.3562(2) 0.28161(19) 0.63768(14) 0.0341(5) Uani 1 1 d . . .
N2 N 0.4171(3) -0.7704(2) 1.44354(16) 0.0287(5) Uani 1 1 d . . .
C2 C 0.3352(4) -0.1684(3) 0.7153(2) 0.0452(9) Uani 1 1 d . . .
H2A H 0.2756 -0.2486 0.7045 0.054 Uiso 1 1 calc R . .
O2W O -0.0150(5) 0.0908(5) 0.3722(3) 0.1400(19) Uani 1 1 d . . .
H2WA H -0.0824 0.0348 0.3811 0.168 Uiso 1 1 d R . .
H2WB H 0.0523 0.1129 0.4212 0.168 Uiso 1 1 d R . .
O3 O 0.1905(2) 0.5988(2) 0.80031(17) 0.0476(6) Uani 1 1 d . . .
N3 N 0.4256(3) -0.1881(2) 0.87009(17) 0.0431(7) Uani 1 1 d . . .
H3A H 0.3562 -0.2550 0.8576 0.052 Uiso 1 1 calc R . .
C3 C 0.4292(3) -0.1173(3) 0.80047(19) 0.0340(7) Uani 1 1 d . . .
O3W O -0.1122(9) 0.9313(8) 0.9187(6) 0.280(5) Uani 1 1 d . . .
H3WA H -0.1858 0.8771 0.9225 0.335 Uiso 1 1 d R . .
H3WB H -0.0695 0.8959 0.8867 0.335 Uiso 1 1 d R . .
O4 O -0.0363(3) 0.5948(2) 0.74625(18) 0.0505(6) Uani 1 1 d . . .
N4 N 0.4514(3) -0.5277(2) 1.25605(17) 0.0372(6) Uani 1 1 d . . .
H4B H 0.5130 -0.4568 1.2784 0.045 Uiso 1 1 calc R . .
C4 C 0.5185(4) 0.0007(3) 0.8114(2) 0.0420(8) Uani 1 1 d . . .
H4A H 0.5864 0.0377 0.8666 0.050 Uiso 1 1 calc R . .
O4W O 0.118(2) 1.0349(15) 0.898(2) 0.92(4) Uani 1 1 d . . .
H4WA H 0.0640 1.0528 0.9293 1.099 Uiso 1 1 d R . .
H4WB H 0.1980 1.0415 0.9346 1.099 Uiso 1 1 d R . .
O5 O -0.38620(19) 0.19672(17) 0.59708(13) 0.0271(4) Uani 1 1 d . . .
C5 C 0.5050(4) 0.0619(3) 0.7393(2) 0.0394(7) Uani 1 1 d . . .
H5A H 0.5641 0.1421 0.7481 0.047 Uiso 1 1 calc R . .
O6 O -0.3157(2) 0.03725(17) 0.55070(13) 0.0311(5) Uani 1 1 d . . .
C6 C 0.5174(4) -0.1644(3) 0.9542(2) 0.0432(8) Uani 1 1 d . . .
O7 O 0.6280(3) -0.0808(2) 0.97894(18) 0.0630(8) Uani 1 1 d . . .
C7 C 0.4763(4) -0.2563(3) 1.0145(2) 0.0416(8) Uani 1 1 d . . .
O8 O 0.2872(4) -0.6413(2) 1.12557(17) 0.0711(9) Uani 1 1 d . . .
C8 C 0.3385(4) -0.2886(3) 1.0313(2) 0.0407(8) Uani 1 1 d . . .
C9 C 0.2319(4) -0.2326(3) 1.0008(2) 0.0498(9) Uani 1 1 d . . .
H9A H 0.2501 -0.1710 0.9663 0.060 Uiso 1 1 calc R . .
C10 C 0.1034(5) -0.2657(4) 1.0203(3) 0.0659(11) Uani 1 1 d . . .
H10A H 0.0353 -0.2268 0.9991 0.079 Uiso 1 1 calc R . .
C11 C 0.0727(6) -0.3581(4) 1.0722(3) 0.0739(13) Uani 1 1 d . . .
H11A H -0.0156 -0.3808 1.0851 0.089 Uiso 1 1 calc R . .
C12 C 0.1719(5) -0.4142(4) 1.1032(3) 0.0595(10) Uani 1 1 d . . .
H12A H 0.1505 -0.4753 1.1377 0.071 Uiso 1 1 calc R . .
C13 C 0.3072(4) -0.3827(3) 1.0848(2) 0.0439(8) Uani 1 1 d . . .
C14 C 0.4157(4) -0.4372(3) 1.1201(2) 0.0444(8) Uani 1 1 d . . .
C15 C 0.5478(4) -0.3995(3) 1.1062(2) 0.0543(10) Uani 1 1 d . . .
H15A H 0.6177 -0.4345 1.1316 0.065 Uiso 1 1 calc R . .
C16 C 0.5792(4) -0.3074(3) 1.0536(2) 0.0530(10) Uani 1 1 d . . .
H16A H 0.6704 -0.2809 1.0452 0.064 Uiso 1 1 calc R . .
C17 C 0.3766(4) -0.5466(3) 1.1661(2) 0.0449(8) Uani 1 1 d . . .
C18 C 0.4368(3) -0.6134(3) 1.3154(2) 0.0312(6) Uani 1 1 d . . .
C19 C 0.3387(4) -0.7289(3) 1.2930(2) 0.0450(8) Uani 1 1 d . . .
H19A H 0.2771 -0.7566 1.2345 0.054 Uiso 1 1 calc R . .
C20 C 0.3331(3) -0.8024(3) 1.3582(2) 0.0412(8) Uani 1 1 d . . .
H20A H 0.2662 -0.8798 1.3418 0.049 Uiso 1 1 calc R . .
C21 C 0.5149(4) -0.6594(3) 1.4638(2) 0.0367(7) Uani 1 1 d . . .
H21A H 0.5771 -0.6350 1.5222 0.044 Uiso 1 1 calc R . .
C22 C 0.5277(4) -0.5796(3) 1.4022(2) 0.0374(7) Uani 1 1 d . . .
H22A H 0.5973 -0.5036 1.4194 0.045 Uiso 1 1 calc R . .
C23 C 0.2290(3) 0.2183(3) 0.60632(19) 0.0272(6) Uani 1 1 d . . .
C24 C 0.1108(3) 0.2606(2) 0.63099(19) 0.0261(6) Uani 1 1 d . . .
C25 C -0.0300(3) 0.1855(3) 0.60141(19) 0.0271(6) Uani 1 1 d . . .
H25A H -0.0504 0.1066 0.5683 0.033 Uiso 1 1 calc R . .
C26 C -0.1396(3) 0.2266(2) 0.62057(17) 0.0235(5) Uani 1 1 d . . .
C27 C -0.2918(3) 0.1466(2) 0.58672(17) 0.0212(5) Uani 1 1 d . . .
C28 C -0.1094(3) 0.3450(2) 0.66948(19) 0.0266(6) Uani 1 1 d . . .
H28A H -0.1833 0.3742 0.6807 0.032 Uiso 1 1 calc R . .
C29 C 0.0303(3) 0.4192(2) 0.70146(19) 0.0276(6) Uani 1 1 d . . .
C30 C 0.0695(3) 0.5466(3) 0.7546(2) 0.0329(7) Uani 1 1 d . . .
C31 C 0.1401(3) 0.3761(3) 0.68273(19) 0.0287(6) Uani 1 1 d . . .
H31A H 0.2341 0.4255 0.7052 0.034 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
Co1 O5 2.0129(18) 1_655 ?
Co1 O6 2.0299(19) 2_556 ?
Co1 O1 2.095(2) . ?
Co1 N1 2.142(2) . ?
Co1 N2 2.153(2) 1_564 ?
Co1 O2 2.409(2) . ?
N1 C1 1.331(4) . ?
N1 C5 1.336(4) . ?
O1 C23 1.261(4) . ?
C1 C2 1.366(4) . ?
O2 C23 1.247(3) . ?
N2 C20 1.332(4) . ?
N2 C21 1.342(4) . ?
N2 Co1 2.153(2) 1_546 ?
C2 C3 1.382(4) . ?
O3 C30 1.213(4) . ?
N3 C6 1.353(4) . ?
N3 C3 1.405(4) . ?
C3 C4 1.382(4) . ?
O4 C30 1.309(4) . ?
N4 C17 1.369(4) . ?
N4 C18 1.406(4) . ?
C4 C5 1.367(4) . ?
O5 C27 1.258(3) . ?
O5 Co1 2.0129(18) 1_455 ?
O6 C27 1.246(3) . ?
O6 Co1 2.0299(19) 2_556 ?
C6 O7 1.213(4) . ?
C6 C7 1.508(4) . ?
C7 C16 1.373(5) . ?
C7 C8 1.426(5) . ?
O8 C17 1.208(4) . ?
C8 C9 1.406(5) . ?
C8 C13 1.435(4) . ?
C9 C10 1.357(6) . ?
C10 C11 1.400(6) . ?
C11 C12 1.350(6) . ?
C12 C13 1.412(5) . ?
C13 C14 1.427(5) . ?
C14 C15 1.356(5) . ?
C14 C17 1.508(4) . ?
C15 C16 1.407(4) . ?
C18 C22 1.377(4) . ?
C18 C19 1.381(4) . ?
C19 C20 1.372(4) . ?
C21 C22 1.383(4) . ?
C23 C24 1.498(4) . ?
C24 C31 1.383(4) . ?
C24 C25 1.393(4) . ?
C25 C26 1.379(4) . ?
C26 C28 1.392(4) . ?
C26 C27 1.503(4) . ?
C28 C29 1.383(4) . ?
C29 C31 1.390(4) . ?
C29 C30 1.492(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
O5 Co1 O6 123.41(8) 1_655 2_556 ?
O5 Co1 O1 147.67(8) 1_655 . ?
O6 Co1 O1 88.90(8) 2_556 . ?
O5 Co1 N1 87.66(8) 1_655 . ?
O6 Co1 N1 93.17(9) 2_556 . ?
O1 Co1 N1 89.63(9) . . ?
O5 Co1 N2 85.74(8) 1_655 1_564 ?
O6 Co1 N2 90.63(9) 2_556 1_564 ?
O1 Co1 N2 95.86(9) . 1_564 ?
N1 Co1 N2 173.39(9) . 1_564 ?
O5 Co1 O2 90.37(7) 1_655 . ?
O6 Co1 O2 145.98(7) 2_556 . ?
O1 Co1 O2 57.54(7) . . ?
N1 Co1 O2 92.05(8) . . ?
N2 Co1 O2 87.80(8) 1_564 . ?
C1 N1 C5 115.6(2) . . ?
C1 N1 Co1 122.27(19) . . ?
C5 N1 Co1 122.08(19) . . ?
C23 O1 Co1 97.67(17) . . ?
N1 C1 C2 124.0(3) . . ?
C23 O2 Co1 83.59(16) . . ?
C20 N2 C21 116.0(2) . . ?
C20 N2 Co1 124.28(19) . 1_546 ?
C21 N2 Co1 119.75(19) . 1_546 ?
C1 C2 C3 119.4(3) . . ?
C6 N3 C3 128.3(3) . . ?
C2 C3 C4 117.5(3) . . ?
C2 C3 N3 117.8(3) . . ?
C4 C3 N3 124.7(3) . . ?
C17 N4 C18 126.1(3) . . ?
C5 C4 C3 118.6(3) . . ?
C27 O5 Co1 124.88(17) . 1_455 ?
N1 C5 C4 124.7(3) . . ?
C27 O6 Co1 157.30(18) . 2_556 ?
O7 C6 N3 123.9(3) . . ?
O7 C6 C7 121.6(3) . . ?
N3 C6 C7 114.4(3) . . ?
C16 C7 C8 121.0(3) . . ?
C16 C7 C6 116.7(3) . . ?
C8 C7 C6 122.3(3) . . ?
C9 C8 C7 124.6(3) . . ?
C9 C8 C13 117.5(3) . . ?
C7 C8 C13 117.9(3) . . ?
C10 C9 C8 122.0(3) . . ?
C9 C10 C11 120.4(4) . . ?
C12 C11 C10 119.8(4) . . ?
C11 C12 C13 121.9(4) . . ?
C12 C13 C14 122.8(3) . . ?
C12 C13 C8 118.4(4) . . ?
C14 C13 C8 118.7(3) . . ?
C15 C14 C13 121.5(3) . . ?
C15 C14 C17 120.0(3) . . ?
C13 C14 C17 118.3(3) . . ?
C14 C15 C16 120.1(4) . . ?
C7 C16 C15 120.6(4) . . ?
O8 C17 N4 124.3(3) . . ?
O8 C17 C14 121.8(3) . . ?
N4 C17 C14 113.9(3) . . ?
C22 C18 C19 117.5(3) . . ?
C22 C18 N4 117.5(3) . . ?
C19 C18 N4 125.0(3) . . ?
C20 C19 C18 119.2(3) . . ?
N2 C20 C19 124.4(3) . . ?
N2 C21 C22 123.3(3) . . ?
C18 C22 C21 119.6(3) . . ?
O2 C23 O1 121.2(3) . . ?
O2 C23 C24 121.1(3) . . ?
O1 C23 C24 117.7(2) . . ?
C31 C24 C25 119.0(2) . . ?
C31 C24 C23 120.2(2) . . ?
C25 C24 C23 120.9(2) . . ?
C26 C25 C24 120.8(2) . . ?
C25 C26 C28 119.6(2) . . ?
C25 C26 C27 120.8(2) . . ?
C28 C26 C27 119.6(2) . . ?
O6 C27 O5 125.0(2) . . ?
O6 C27 C26 118.6(2) . . ?
O5 C27 C26 116.4(2) . . ?
C29 C28 C26 120.1(2) . . ?
C28 C29 C31 119.7(2) . . ?
C28 C29 C30 122.6(3) . . ?
C31 C29 C30 117.7(2) . . ?
O3 C30 O4 124.5(3) . . ?
O3 C30 C29 121.3(3) . . ?
O4 C30 C29 114.2(3) . . ?
C24 C31 C29 120.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.092
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-7
_database_code_depnum_ccdc_archive 'CCDC 1005169'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H18 N4 Ni O6'
_chemical_formula_weight         565.17

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3'

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

_cell_length_a                   16.7246(7)
_cell_length_b                   16.7246(7)
_cell_length_c                   59.874(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     14503.8(15)
_cell_formula_units_Z            18
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      25.04

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5220
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27885
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_theta_min         1.02
_diffrn_reflns_theta_max         25.04
_reflns_number_total             5712
_reflns_number_gt                4138
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0995P)²+72.8223P] 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         5712
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.2021
_refine_ls_wR_factor_gt          0.1918
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.34317(4) 0.02116(4) 0.281142(9) 0.0269(2) Uani 1 1 d . . .
O1 O 0.4903(2) 0.0880(2) 0.27711(5) 0.0372(8) Uani 1 1 d . . .
N1 N 0.3309(3) 0.0063(3) 0.24651(7) 0.0354(10) Uani 1 1 d . . .
C1 C 0.3035(5) 0.0565(4) 0.23502(9) 0.0539(16) Uani 1 1 d . . .
H1A H 0.2883 0.0948 0.2430 0.065 Uiso 1 1 calc R . .
O2 O 0.4177(2) 0.1666(2) 0.27651(5) 0.0350(8) Uani 1 1 d . . .
N2 N 0.2979(3) -0.0087(3) -0.01725(6) 0.0373(10) Uani 1 1 d . . .
C2 C 0.2960(5) 0.0555(5) 0.21181(10) 0.0634(18) Uani 1 1 d . . .
H2A H 0.2770 0.0924 0.2046 0.076 Uiso 1 1 calc R . .
O3 O 0.2227(2) 0.0169(2) 0.28239(6) 0.0363(8) Uani 1 1 d . . .
N3 N 0.3138(4) -0.0063(4) 0.17685(8) 0.0727(17) Uani 1 1 d . . .
H3A H 0.3404 -0.0335 0.1708 0.087 Uiso 1 1 calc R . .
C3 C 0.3175(5) -0.0020(4) 0.19991(9) 0.0556(16) Uani 1 1 d . . .
O4 O 0.1245(3) -0.1275(3) 0.29199(7) 0.0548(11) Uani 1 1 d . . .
N4 N 0.3034(3) 0.0191(4) 0.05288(7) 0.0486(12) Uani 1 1 d . . .
H4B H 0.2976 0.0647 0.0575 0.058 Uiso 1 1 calc R . .
C4 C 0.3450(6) -0.0526(6) 0.21192(10) 0.084(3) Uani 1 1 d . . .
H4A H 0.3603 -0.0920 0.2045 0.101 Uiso 1 1 calc R . .
C5 C 0.3509(6) -0.0474(5) 0.23460(9) 0.069(2) Uani 1 1 d . . .
H5A H 0.3701 -0.0837 0.2421 0.083 Uiso 1 1 calc R . .
O5 O 0.2290(6) 0.0594(6) 0.16795(9) 0.146(3) Uani 1 1 d . . .
C6 C 0.2749(7) 0.0256(7) 0.16257(11) 0.088(3) Uani 1 1 d . . .
O6 O 0.3265(5) -0.0969(4) 0.06436(8) 0.108(2) Uani 1 1 d . . .
C7 C 0.2884(6) 0.0130(6) 0.13800(10) 0.077(2) Uani 1 1 d . . .
C8 C 0.3795(5) 0.0590(5) 0.12789(10) 0.0640(18) Uani 1 1 d . . .
C9 C 0.4627(5) 0.1177(6) 0.13988(12) 0.077(2) Uani 1 1 d . . .
H9A H 0.4602 0.1251 0.1552 0.093 Uiso 1 1 calc R . .
C10 C 0.5439(6) 0.1618(7) 0.12937(14) 0.100(3) Uani 1 1 d . . .
H10A H 0.5968 0.2000 0.1375 0.119 Uiso 1 1 calc R . .
C11 C 0.5513(6) 0.1519(7) 0.10640(15) 0.104(3) Uani 1 1 d . . .
H11A H 0.6085 0.1820 0.0993 0.125 Uiso 1 1 calc R . .
C12 C 0.4721(6) 0.0966(6) 0.09447(12) 0.081(2) Uani 1 1 d . . .
H12A H 0.4765 0.0912 0.0791 0.097 Uiso 1 1 calc R . .
C13 C 0.3860(5) 0.0485(5) 0.10451(10) 0.0586(16) Uani 1 1 d . . .
C14 C 0.3056(5) -0.0088(5) 0.09251(9) 0.0599(17) Uani 1 1 d . . .
C15 C 0.2217(6) -0.0517(6) 0.10255(11) 0.088(3) Uani 1 1 d . . .
H15A H 0.1691 -0.0912 0.0944 0.105 Uiso 1 1 calc R . .
C16 C 0.2148(6) -0.0355(7) 0.12571(11) 0.100(3) Uani 1 1 d . . .
H16A H 0.1568 -0.0601 0.1322 0.120 Uiso 1 1 calc R . .
C17 C 0.3125(5) -0.0328(5) 0.06856(10) 0.0628(18) Uani 1 1 d . . .
C18 C 0.3023(4) 0.0064(4) 0.02932(8) 0.0394(12) Uani 1 1 d . . .
C19 C 0.2946(6) 0.0684(5) 0.01606(9) 0.073(2) Uani 1 1 d . . .
H19A H 0.2914 0.1174 0.0224 0.087 Uiso 1 1 calc R . .
C20 C 0.2917(6) 0.0581(5) -0.00700(9) 0.071(2) Uani 1 1 d . . .
H20A H 0.2851 0.1004 -0.0157 0.085 Uiso 1 1 calc R . .
C21 C 0.3080(5) -0.0667(4) -0.00362(9) 0.0594(17) Uani 1 1 d . . .
H21A H 0.3143 -0.1136 -0.0102 0.071 Uiso 1 1 calc R . .
C22 C 0.3098(5) -0.0622(5) 0.01925(9) 0.0657(19) Uani 1 1 d . . .
H22A H 0.3160 -0.1054 0.0277 0.079 Uiso 1 1 calc R . .
C23 C 0.4919(3) 0.1636(3) 0.27610(7) 0.0315(11) Uani 1 1 d . . .
C24 C 0.5828(3) 0.2512(3) 0.27481(8) 0.0333(11) Uani 1 1 d . . .
C25 C 0.5863(3) 0.3373(3) 0.27477(8) 0.0354(11) Uani 1 1 d . . .
H25A H 0.5317 0.3393 0.2747 0.042 Uiso 1 1 calc R . .
C26 C 0.0910(3) 0.0683(3) 0.28728(8) 0.0362(11) Uani 1 1 d . . .
H26A H 0.1527 0.1147 0.2873 0.043 Uiso 1 1 calc R . .
C27 C 0.0691(3) -0.0229(3) 0.28725(8) 0.0350(11) Uani 1 1 d . . .
C28 C 0.1448(3) -0.0476(3) 0.28713(8) 0.0345(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O3 1.982(3) . ?
Ni1 N1 2.086(4) . ?
Ni1 N2 2.109(4) 6 ?
Ni1 O2 2.125(3) . ?
Ni1 O1 2.148(3) . ?
Ni1 C23 2.456(5) . ?
O1 C23 1.254(6) . ?
N1 C5 1.314(7) . ?
N1 C1 1.332(7) . ?
C1 C2 1.395(8) . ?
O2 C23 1.268(6) . ?
N2 C20 1.322(7) . ?
N2 C21 1.342(7) . ?
N2 Ni1 2.109(4) 8_544 ?
C2 C3 1.382(8) . ?
O3 C28 1.239(6) . ?
N3 C6 1.336(9) . ?
N3 C3 1.382(7) . ?
C3 C4 1.355(9) . ?
O4 C28 1.237(6) . ?
N4 C17 1.338(8) . ?
N4 C18 1.425(6) . ?
C4 C5 1.362(8) . ?
O5 C6 1.202(9) . ?
C6 C7 1.519(9) . ?
O6 C17 1.233(8) . ?
C7 C16 1.309(11) . ?
C7 C8 1.452(10) . ?
C8 C13 1.422(8) . ?
C8 C9 1.432(10) . ?
C9 C10 1.335(11) . ?
C10 C11 1.398(11) . ?
C11 C12 1.377(11) . ?
C12 C13 1.386(10) . ?
C13 C14 1.399(10) . ?
C14 C15 1.356(10) . ?
C14 C17 1.508(8) . ?
C15 C16 1.428(9) . ?
C18 C22 1.357(8) . ?
C18 C19 1.362(8) . ?
C19 C20 1.389(8) . ?
C21 C22 1.371(8) . ?
C23 C24 1.494(7) . ?
C24 C25 1.355(7) 2_655 ?
C24 C25 1.412(7) . ?
C25 C24 1.355(7) 3_665 ?
C26 C27 1.379(7) . ?
C26 C27 1.381(7) 2 ?
C27 C26 1.381(7) 3 ?
C27 C28 1.515(7) . ?

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
O3 Ni1 N1 89.72(15) . . ?
O3 Ni1 N2 92.49(15) . 6 ?
N1 Ni1 N2 177.76(16) . 6 ?
O3 Ni1 O2 92.85(13) . . ?
N1 Ni1 O2 88.48(14) . . ?
N2 Ni1 O2 91.78(15) 6 . ?
O3 Ni1 O1 154.53(14) . . ?
N1 Ni1 O1 88.25(14) . . ?
N2 Ni1 O1 89.90(14) 6 . ?
O2 Ni1 O1 61.72(12) . . ?
O3 Ni1 C23 123.92(15) . . ?
N1 Ni1 C23 89.15(15) . . ?
N2 Ni1 C23 89.92(16) 6 . ?
O2 Ni1 C23 31.08(14) . . ?
O1 Ni1 C23 30.68(14) . . ?
C23 O1 Ni1 88.3(3) . . ?
C5 N1 C1 115.8(5) . . ?
C5 N1 Ni1 125.3(4) . . ?
C1 N1 Ni1 118.9(3) . . ?
N1 C1 C2 124.4(6) . . ?
C23 O2 Ni1 89.0(3) . . ?
C20 N2 C21 114.8(5) . . ?
C20 N2 Ni1 122.4(4) . 8_544 ?
C21 N2 Ni1 122.1(3) . 8_544 ?
C3 C2 C1 118.0(6) . . ?
C28 O3 Ni1 130.3(3) . . ?
C6 N3 C3 129.5(6) . . ?
C4 C3 N3 121.3(6) . . ?
C4 C3 C2 116.7(5) . . ?
N3 C3 C2 122.0(6) . . ?
C17 N4 C18 126.6(5) . . ?
C3 C4 C5 121.7(6) . . ?
N1 C5 C4 123.4(6) . . ?
O5 C6 N3 124.7(7) . . ?
O5 C6 C7 119.9(7) . . ?
N3 C6 C7 115.4(7) . . ?
C16 C7 C8 120.4(6) . . ?
C16 C7 C6 118.2(7) . . ?
C8 C7 C6 121.3(7) . . ?
C13 C8 C9 118.0(7) . . ?
C13 C8 C7 118.0(6) . . ?
C9 C8 C7 123.9(6) . . ?
C10 C9 C8 120.9(7) . . ?
C9 C10 C11 121.6(8) . . ?
C12 C11 C10 118.5(8) . . ?
C11 C12 C13 122.4(7) . . ?
C12 C13 C14 122.6(6) . . ?
C12 C13 C8 118.5(7) . . ?
C14 C13 C8 118.9(6) . . ?
C15 C14 C13 121.4(6) . . ?
C15 C14 C17 118.5(6) . . ?
C13 C14 C17 119.7(6) . . ?
C14 C15 C16 119.4(7) . . ?
C7 C16 C15 121.6(7) . . ?
O6 C17 N4 123.6(6) . . ?
O6 C17 C14 119.9(6) . . ?
N4 C17 C14 116.5(6) . . ?
C22 C18 C19 117.9(5) . . ?
C22 C18 N4 124.5(5) . . ?
C19 C18 N4 117.6(5) . . ?
C18 C19 C20 119.7(5) . . ?
N2 C20 C19 123.6(5) . . ?
N2 C21 C22 125.1(5) . . ?
C18 C22 C21 118.8(5) . . ?
O1 C23 O2 120.8(4) . . ?
O1 C23 C24 119.3(4) . . ?
O2 C23 C24 119.9(4) . . ?
O1 C23 Ni1 61.0(2) . . ?
O2 C23 Ni1 59.9(2) . . ?
C24 C23 Ni1 175.9(3) . . ?
C25 C24 C25 119.3(5) 2_655 . ?
C25 C24 C23 120.4(4) 2_655 . ?
C25 C24 C23 120.2(4) . . ?
C24 C25 C24 120.7(5) 3_665 . ?
C27 C26 C27 121.1(5) . 2 ?
C26 C27 C26 118.9(5) . 3 ?
C26 C27 C28 120.4(4) . . ?
C26 C27 C28 120.7(4) 3 . ?
O4 C28 O3 126.5(5) . . ?
O4 C28 C27 118.6(5) . . ?
O3 C28 C27 114.9(4) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.093






# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 92 3 ' '
2 0.000 0.000 0.127 146 21 ' '
3 0.000 1.000 0.500 1089 339 ' '
4 0.000 0.000 0.873 146 21 ' '
5 0.333 0.667 0.166 1081 339 ' '
6 0.333 0.667 0.539 147 21 ' '
7 0.333 0.667 0.794 145 21 ' '
8 0.333 0.667 0.667 88 3 ' '
9 0.667 0.333 0.833 1078 339 ' '
10 0.667 0.333 0.206 145 21 ' '
11 0.667 0.333 0.460 147 21 ' '
12 0.667 0.333 0.333 88 3 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-8
_database_code_depnum_ccdc_archive 'CCDC 1005170'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H18 Cu N4 O6'
_chemical_formula_weight         570.00

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   'R -3 c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   18.942(2)
_cell_length_b                   18.942(2)
_cell_length_c                   38.976(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12111(2)
_cell_formula_units_Z            18
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.62
_cell_measurement_theta_max      25.41

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5238
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20278
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         25.41
_reflns_number_total             2488
_reflns_number_gt                1967
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.1181P)²+156.6986P] 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         2488
_refine_ls_number_parameters     200
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0801
_refine_ls_wR_factor_ref         0.2269
_refine_ls_wR_factor_gt          0.2141
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.100
_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
Cu1 Cu 0.50914(5) 0.0000 -0.2500 0.0258(4) Uani 1 2 d S . .
O1 O 0.4288(3) -0.1139(2) -0.24465(10) 0.0322(10) Uani 1 1 d . . .
N1 N 0.5254(4) 0.0137(3) -0.19942(13) 0.0352(12) Uani 1 1 d . . .
C1 C 0.5526(6) -0.0262(5) -0.18111(17) 0.061(2) Uani 1 1 d . . .
H1A H 0.5721 -0.0562 -0.1925 0.073 Uiso 1 1 calc R . .
O2 O 0.5299(2) -0.1406(2) -0.24471(11) 0.0372(10) Uani 1 1 d . . .
C2 C 0.5535(7) -0.0254(6) -0.1460(2) 0.080(3) Uani 1 1 d U . .
H2A H 0.5713 -0.0560 -0.1340 0.096 Uiso 1 1 calc R . .
N2 N 0.4938(9) 0.0032(8) -0.0920(3) 0.039(2) Uani 0.471(11) 1 d PU . 1
H2B H 0.5235 0.0634 -0.0889 0.047 Uiso 0.471(11) 1 d PR . 1
N2' N 0.5496(8) 0.0407(7) -0.0943(3) 0.039(2) Uani 0.529(11) 1 d P . 2
H2'A H 0.5266 0.0655 -0.0852 0.047 Uiso 0.529(11) 1 calc PR . 2
C3 C 0.5281(9) 0.0208(7) -0.12863(19) 0.083(4) Uani 1 1 d . . .
O3 O 0.4811(10) -0.1151(9) -0.0777(3) 0.190(6) Uani 1 1 d . . .
C4 C 0.5016(5) 0.0628(5) -0.14730(16) 0.052(2) Uani 1 1 d . . .
H4A H 0.4847 0.0955 -0.1364 0.062 Uiso 1 1 calc R . .
C5 C 0.4994(5) 0.0572(4) -0.18238(16) 0.0453(17) Uani 1 1 d . . .
H5A H 0.4790 0.0850 -0.1948 0.054 Uiso 1 1 calc R . .
C6 C 0.4807(9) -0.0554(8) -0.0699(3) 0.036(3) Uani 0.50 1 d PU . .
C6' C 0.4011(8) -0.0298(8) 0.0716(3) 0.036(3) Uani 0.50 1 d P . .
C7 C 0.4701(9) -0.0426(8) -0.0312(3) 0.042(2) Uani 0.576(8) 1 d PU . 1
C7' C 0.4437(11) -0.0902(10) -0.0411(4) 0.042(2) Uani 0.424(8) 1 d P . 2
C8 C 0.3902(9) -0.1005(9) -0.0206(3) 0.055(3) Uani 0.576(8) 1 d PU . 1
H8A H 0.3518 -0.1401 -0.0351 0.066 Uiso 0.576(8) 1 calc PR . 1
C8' C 0.3659(13) -0.1499(13) -0.0287(5) 0.055(3) Uani 0.424(8) 1 d P . 2
H8'A H 0.3299 -0.1939 -0.0422 0.066 Uiso 0.424(8) 1 calc PR . 2
C9 C 0.3739(9) -0.0920(9) 0.0158(3) 0.046(3) Uani 0.576(8) 1 d PU . 1
H9A H 0.3229 -0.1287 0.0246 0.055 Uiso 0.576(8) 1 calc PR . 1
C9' C 0.3460(12) -0.1391(11) 0.0047(4) 0.046(3) Uani 0.424(8) 1 d P . 2
H9'A H 0.2965 -0.1784 0.0140 0.055 Uiso 0.424(8) 1 calc PR . 2
C10 C 0.4160(7) -0.0476(9) 0.0319(3) 0.087(3) Uani 1 1 d U . .
C11 C 0.5134(8) 0.0030(10) -0.0163(3) 0.097(4) Uani 1 1 d U . .
C12 C 0.4563(3) -0.1629(3) -0.24488(13) 0.0261(12) Uani 1 1 d . . .
C13 C 0.3923(3) -0.2515(3) -0.24495(14) 0.0255(12) Uani 1 1 d . . .
C14 C 0.3102(3) -0.2747(3) -0.24480(15) 0.0287(13) Uani 1 1 d . . .
H14A H 0.2947 -0.2352 -0.2446 0.034 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 1.932(4) . ?
Cu1 O1 1.932(4) 4_554 ?
Cu1 N1 1.992(5) 4_554 ?
Cu1 N1 1.992(5) . ?
O1 C12 1.271(7) . ?
N1 C1 1.318(9) . ?
N1 C5 1.330(8) . ?
C1 C2 1.367(10) . ?
O2 C12 1.239(7) . ?
C2 C3 1.371(11) . ?
N2 C6 1.327(18) . ?
N2 C3 1.533(15) . ?
N2 C6' 1.961(19) 19_655 ?
N2' C6' 1.374(16) 19_655 ?
N2' C3 1.395(12) . ?
N2' C6 1.883(18) . ?
C3 C4 1.347(10) . ?
O3 C6 1.175(15) . ?
O3 C7' 1.76(2) . ?
C4 C5 1.370(9) . ?
C6 C7' 1.31(2) . ?
C6 C7 1.557(17) . ?
C6 C6' 2.003(19) 19_655 ?
C6' N2' 1.375(16) 19_655 ?
C6' C10 1.640(16) . ?
C6' N2 1.961(19) 19_655 ?
C6' C6 2.003(19) 19_655 ?
C7 C11 1.023(18) . ?
C7 C8 1.415(19) . ?
C7 C11 1.96(2) 19_655 ?
C7 C10 1.972(19) 19_655 ?
C7' C8' 1.42(3) . ?
C7' C11 1.86(2) . ?
C8 C9 1.476(18) . ?
C8' C9' 1.40(2) . ?
C9 C10 1.034(17) . ?
C9 C11 1.95(2) 19_655 ?
C9' C10 1.89(2) . ?
C10 C11 1.320(15) 19_655 ?
C10 C7 1.972(19) 19_655 ?
C11 C10 1.320(15) 19_655 ?
C11 C11 1.35(2) 19_655 ?
C11 C9 1.95(2) 19_655 ?
C11 C7 1.96(2) 19_655 ?
C12 C13 1.500(8) . ?
C13 C14 1.380(8) 3_655 ?
C13 C14 1.390(8) . ?
C14 C13 1.380(8) 2_545 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 153.5(3) . 4_554 ?
O1 Cu1 N1 91.05(19) . 4_554 ?
O1 Cu1 N1 91.30(19) 4_554 4_554 ?
O1 Cu1 N1 91.30(19) . . ?
O1 Cu1 N1 91.06(19) 4_554 . ?
N1 Cu1 N1 169.7(3) 4_554 . ?
C12 O1 Cu1 115.6(4) . . ?
C1 N1 C5 117.3(6) . . ?
C1 N1 Cu1 122.7(4) . . ?
C5 N1 Cu1 119.6(4) . . ?
N1 C1 C2 122.7(7) . . ?
C1 C2 C3 119.8(8) . . ?
C6 N2 C3 131.9(10) . . ?
C6 N2 C6' 72.1(9) . 19_655 ?
C3 N2 C6' 93.2(9) . 19_655 ?
C6' N2' C3 134.7(10) 19_655 . ?
C6' N2' C6 74.0(8) 19_655 . ?
C3 N2' C6 104.8(9) . . ?
C4 C3 C2 117.6(7) . . ?
C4 C3 N2' 120.2(7) . . ?
C2 C3 N2' 120.0(8) . . ?
C4 C3 N2 112.9(8) . . ?
C2 C3 N2 124.6(8) . . ?
N2' C3 N2 36.9(6) . . ?
C6 O3 C7' 48.3(10) . . ?
C3 C4 C5 120.0(7) . . ?
N1 C5 C4 122.6(6) . . ?
O3 C6 C7' 89.8(13) . . ?
O3 C6 N2 123.3(13) . . ?
C7' C6 N2 143.7(13) . . ?
O3 C6 C7 117.6(12) . . ?
C7' C6 C7 34.1(8) . . ?
N2 C6 C7 119.0(10) . . ?
O3 C6 N2' 117.7(12) . . ?
C7' C6 N2' 148.8(12) . . ?
N2 C6 N2' 27.6(7) . . ?
C7 C6 N2' 114.8(9) . . ?
O3 C6 C6' 102.9(12) . 19_655 ?
C7' C6 C6' 122.3(12) . 19_655 ?
N2 C6 C6' 68.8(9) . 19_655 ?
C7 C6 C6' 95.0(9) . 19_655 ?
N2' C6 C6' 41.3(6) . 19_655 ?
N2' C6' C10 112.0(10) 19_655 . ?
N2' C6' N2 25.7(6) 19_655 19_655 ?
C10 C6' N2 100.3(8) . 19_655 ?
N2' C6' C6 64.7(8) 19_655 19_655 ?
C10 C6' C6 84.0(8) . 19_655 ?
N2 C6' C6 39.1(6) 19_655 19_655 ?
C11 C7 C8 125.7(14) . . ?
C11 C7 C6 124.7(13) . . ?
C8 C7 C6 109.5(12) . . ?
C11 C7 C11 40.1(11) . 19_655 ?
C8 C7 C11 85.7(8) . 19_655 ?
C6 C7 C11 164.8(12) . 19_655 ?
C11 C7 C10 37.7(9) . 19_655 ?
C8 C7 C10 163.3(12) . 19_655 ?
C6 C7 C10 87.2(8) . 19_655 ?
C11 C7 C10 77.6(9) 19_655 19_655 ?
C6 C7' C8' 140.5(18) . . ?
C6 C7' O3 42.0(8) . . ?
C8' C7' O3 117.4(15) . . ?
C6 C7' C11 91.2(11) . . ?
C8' C7' C11 122.6(13) . . ?
O3 C7' C11 119.1(11) . . ?
C7 C8 C9 113.4(13) . . ?
C9' C8' C7' 116.6(18) . . ?
C10 C9 C8 123.6(14) . . ?
C10 C9 C11 39.0(9) . 19_655 ?
C8 C9 C11 84.6(9) . 19_655 ?
C8' C9' C10 122.5(14) . . ?
C9 C10 C11 111.4(14) . 19_655 ?
C9 C10 C6' 126.8(12) . . ?
C11 C10 C6' 121.8(13) 19_655 . ?
C9 C10 C9' 9.1(11) . . ?
C11 C10 C9' 110.6(12) 19_655 . ?
C6' C10 C9' 127.1(9) . . ?
C9 C10 C7 139.6(12) . 19_655 ?
C11 C10 C7 28.3(8) 19_655 19_655 ?
C6' C10 C7 93.5(9) . 19_655 ?
C9' C10 C7 138.4(9) . 19_655 ?
C7 C11 C10 114.1(15) . 19_655 ?
C7 C11 C11 110.7(17) . 19_655 ?
C10 C11 C11 135(2) 19_655 19_655 ?
C7 C11 C7' 10.1(11) . . ?
C10 C11 C7' 112.3(12) 19_655 . ?
C11 C11 C7' 110.6(15) 19_655 . ?
C7 C11 C9 143.6(13) . 19_655 ?
C10 C11 C9 29.6(7) 19_655 19_655 ?
C11 C11 C9 105.3(16) 19_655 19_655 ?
C7' C11 C9 140.9(9) . 19_655 ?
C7 C11 C7 139.9(11) . 19_655 ?
C10 C11 C7 105.8(13) 19_655 19_655 ?
C11 C11 C7 29.1(10) 19_655 19_655 ?
C7' C11 C7 139.0(9) . 19_655 ?
C9 C11 C7 76.3(9) 19_655 19_655 ?
O2 C12 O1 123.7(5) . . ?
O2 C12 C13 121.5(5) . . ?
O1 C12 C13 114.8(5) . . ?
C14 C13 C14 119.8(5) 3_655 . ?
C14 C13 C12 119.9(5) 3_655 . ?
C14 C13 C12 120.3(5) . . ?
C13 C14 C13 120.2(5) 2_545 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.41
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.113
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-9
_database_code_depnum_ccdc_archive 'CCDC 1005171'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H20 N4 O8 Zn'
_chemical_formula_weight         641.88

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   11.8470(4)
_cell_length_b                   16.2260(5)
_cell_length_c                   14.7859(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.5450(10)
_cell_angle_gamma                90.00
_cell_volume                     2678.51(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13361
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4707
_reflns_number_gt                4286
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0435P)²+1.5886P] 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         4707
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0752
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.002
_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
Zn1 Zn 0.261334(18) -0.550576(12) 0.276607(14) 0.01946(8) Uani 1 1 d . . .
O1 O 0.23505(14) -0.57105(9) 0.39125(10) 0.0326(3) Uani 1 1 d . . .
N1 N 0.09680(14) -0.48268(10) 0.21092(11) 0.0242(3) Uani 1 1 d . . .
C1 C 0.00772(18) -0.47799(12) 0.24181(14) 0.0276(4) Uani 1 1 d . . .
H1A H 0.0211 -0.4937 0.3050 0.033 Uiso 1 1 calc R . .
O2 O 0.12831(15) -0.68929(11) 0.36653(10) 0.0466(4) Uani 1 1 d . . .
N2 N -0.99223(17) -0.20493(12) -0.67785(12) 0.0389(5) Uani 1 1 d . . .
H2B H -1.0298 -0.1918 -0.7366 0.047 Uiso 1 1 calc R . .
C2 C -0.11381(19) -0.44980(12) 0.18581(14) 0.0288(4) Uani 1 1 d . . .
H2A H -0.1715 -0.4484 0.2157 0.035 Uiso 1 1 calc R . .
O3 O 0.23078(13) -0.87698(9) 0.64932(10) 0.0318(3) Uani 1 1 d . . .
N3 N -0.26574(14) -0.40477(11) 0.02332(12) 0.0288(4) Uani 1 1 d . . .
H3A H -0.2748 -0.4015 -0.0346 0.035 Uiso 1 1 d R . .
C3 C -0.14596(17) -0.42554(12) 0.09189(14) 0.0251(4) Uani 1 1 d . . .
O4 O 0.34867(17) -0.82939(9) 0.79190(10) 0.0450(4) Uani 1 1 d . . .
N4 N -0.78754(15) -0.25382(11) -0.38755(11) 0.0301(4) Uani 1 1 d . . .
H4B H -0.7370 -0.2152 -0.3549 0.036 Uiso 1 1 d R . .
C4 C -0.05054(18) -0.42481(13) 0.06240(14) 0.0310(5) Uani 1 1 d . . .
H4A H -0.0598 -0.4052 0.0012 0.037 Uiso 1 1 calc R . .
O5 O 0.65163(12) -0.60134(9) 0.81515(10) 0.0313(3) Uani 1 1 d . . .
C5 C 0.06694(19) -0.45354(12) 0.12262(14) 0.0292(4) Uani 1 1 d . . .
H5A H 0.1277 -0.4511 0.0960 0.035 Uiso 1 1 calc R . .
O6 O 0.58815(12) -0.51310(8) 0.69208(10) 0.0298(3) Uani 1 1 d . . .
C6 C -0.37233(18) -0.38925(13) 0.03493(14) 0.0287(4) Uani 1 1 d . . .
O7 O -0.37549(15) -0.39192(11) 0.11182(11) 0.0470(4) Uani 1 1 d . . .
C7 C -0.48386(17) -0.36891(12) -0.05922(13) 0.0258(4) Uani 1 1 d . . .
O8 O -0.8640(2) -0.37953(13) -0.37487(15) 0.0750(7) Uani 1 1 d . . .
C8 C -0.55759(16) -0.29656(12) -0.06983(13) 0.0243(4) Uani 1 1 d . . .
C9 C -0.53188(18) -0.24102(13) 0.00691(14) 0.0292(4) Uani 1 1 d . . .
H9A H -0.4693 -0.2503 0.0639 0.035 Uiso 1 1 calc R . .
C10 C -0.6032(2) -0.17211(14) -0.00567(15) 0.0340(5) Uani 1 1 d . . .
H10A H -0.5871 -0.1343 0.0443 0.041 Uiso 1 1 calc R . .
C11 C -0.70517(19) -0.15502(13) -0.09539(15) 0.0326(5) Uani 1 1 d . . .
H11A H -0.7511 -0.1078 -0.0993 0.039 Uiso 1 1 calc R . .
C12 C -0.73198(18) -0.20674(13) -0.17088(14) 0.0289(4) Uani 1 1 d . . .
H12A H -0.7957 -0.1962 -0.2268 0.035 Uiso 1 1 calc R . .
C13 C -0.65899(16) -0.27844(12) -0.16191(13) 0.0245(4) Uani 1 1 d . . .
C14 C -0.68364(18) -0.33430(13) -0.23889(14) 0.0295(4) Uani 1 1 d . . .
C15 C -0.6132(2) -0.40459(14) -0.22439(15) 0.0366(5) Uani 1 1 d . . .
H15A H -0.6304 -0.4434 -0.2734 0.044 Uiso 1 1 calc R . .
C16 C -0.51181(19) -0.42131(14) -0.13481(15) 0.0334(5) Uani 1 1 d . . .
H16A H -0.4665 -0.4689 -0.1305 0.040 Uiso 1 1 calc R . .
C17 C -0.7884(2) -0.32466(14) -0.33874(15) 0.0372(5) Uani 1 1 d . . .
C18 C -0.86066(18) -0.23935(13) -0.48494(14) 0.0300(5) Uani 1 1 d . . .
C19 C -0.96139(19) -0.28907(15) -0.54515(15) 0.0366(5) Uani 1 1 d . . .
H19A H -0.9842 -0.3355 -0.5186 0.044 Uiso 1 1 calc R . .
C20 C -1.0244(2) -0.26938(16) -0.64093(15) 0.0398(5) Uani 1 1 d . . .
H20A H -1.0880 -0.3019 -0.6773 0.048 Uiso 1 1 calc R . .
C21 C -0.8961(2) -0.15648(14) -0.62199(15) 0.0384(5) Uani 1 1 d . . .
H21A H -0.8751 -0.1110 -0.6512 0.046 Uiso 1 1 calc R . .
C22 C -0.8294(2) -0.17125(13) -0.52558(14) 0.0338(5) Uani 1 1 d . . .
H22A H -0.7673 -0.1367 -0.4911 0.041 Uiso 1 1 calc R . .
C23 C 0.20800(17) -0.63877(13) 0.41846(13) 0.0274(4) Uani 1 1 d . . .
C24 C 0.28204(16) -0.65727(11) 0.52385(13) 0.0218(4) Uani 1 1 d . . .
C25 C 0.38368(16) -0.60775(11) 0.58082(13) 0.0230(4) Uani 1 1 d . . .
H25A H 0.4011 -0.5602 0.5530 0.028 Uiso 1 1 calc R . .
C26 C 0.45850(16) -0.62707(11) 0.67644(13) 0.0208(4) Uani 1 1 d . . .
C27 C 0.57574(17) -0.57754(12) 0.73414(13) 0.0231(4) Uani 1 1 d . . .
C28 C 0.42922(16) -0.69548(11) 0.71665(13) 0.0218(4) Uani 1 1 d . . .
H28A H 0.4733 -0.7102 0.7793 0.026 Uiso 1 1 calc R . .
C29 C 0.32808(16) -0.74558(11) 0.66045(13) 0.0207(4) Uani 1 1 d . . .
C30 C 0.30144(17) -0.82111(11) 0.70347(13) 0.0233(4) Uani 1 1 d . . .
C31 C 0.25515(16) -0.72637(11) 0.56399(13) 0.0215(4) Uani 1 1 d . . .
H31A H 0.1916 -0.7601 0.5301 0.026 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
Zn1 O1 1.8530(13) . ?
Zn1 O6 1.9771(13) 3_646 ?
Zn1 O3 2.1445(14) 4_545 ?
Zn1 N1 2.1656(16) . ?
Zn1 O4 2.1814(15) 4_545 ?
Zn1 C30 2.4644(18) 4_545 ?
O1 C23 1.248(2) . ?
N1 C1 1.285(2) . ?
N1 C5 1.321(3) . ?
C1 C2 1.473(3) . ?
C1 H1A 0.9300 . ?
O2 C23 1.291(3) . ?
N2 C20 1.295(3) . ?
N2 C21 1.403(3) . ?
N2 H2B 0.8600 . ?
C2 C3 1.369(3) . ?
C2 H2A 0.9300 . ?
O3 C30 1.310(2) . ?
O3 Zn1 2.1445(14) 4_546 ?
N3 C6 1.354(3) . ?
N3 C3 1.481(2) . ?
N3 H3A 0.8284 . ?
C3 C4 1.341(3) . ?
O4 C30 1.245(2) . ?
O4 Zn1 2.1814(15) 4_546 ?
N4 C17 1.359(3) . ?
N4 C18 1.430(2) . ?
N4 H4B 0.8896 . ?
C4 C5 1.455(3) . ?
C4 H4A 0.9300 . ?
O5 C27 1.293(2) . ?
C5 H5A 0.9300 . ?
O6 C27 1.250(2) . ?
O6 Zn1 1.9772(13) 3_646 ?
C6 O7 1.151(2) . ?
C6 C7 1.601(3) . ?
C7 C16 1.354(3) . ?
C7 C8 1.440(3) . ?
O8 C17 1.249(3) . ?
C8 C9 1.400(3) . ?
C8 C13 1.513(3) . ?
C9 C10 1.376(3) . ?
C9 H9A 0.9300 . ?
C10 C11 1.491(3) . ?
C10 H10A 0.9300 . ?
C11 C12 1.347(3) . ?
C11 H11A 0.9300 . ?
C12 C13 1.429(3) . ?
C12 H12A 0.9300 . ?
C13 C14 1.407(3) . ?
C14 C15 1.387(3) . ?
C14 C17 1.587(3) . ?
C15 C16 1.485(3) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C18 C22 1.367(3) . ?
C18 C19 1.469(3) . ?
C19 C20 1.399(3) . ?
C19 H19A 0.9300 . ?
C20 H20A 0.9300 . ?
C21 C22 1.400(3) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C24 1.541(2) . ?
C24 C31 1.356(3) . ?
C24 C25 1.458(3) . ?
C25 C26 1.430(3) . ?
C25 H25A 0.9300 . ?
C26 C28 1.358(3) . ?
C26 C27 1.584(3) . ?
C28 C29 1.456(3) . ?
C28 H28A 0.9300 . ?
C29 C31 1.433(2) . ?
C29 C30 1.463(3) . ?
C30 Zn1 2.4644(18) 4_546 ?
C31 H31A 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
O1 Zn1 O6 107.09(6) . 3_646 ?
O1 Zn1 O3 132.36(6) . 4_545 ?
O6 Zn1 O3 111.48(6) 3_646 4_545 ?
O1 Zn1 N1 95.74(6) . . ?
O6 Zn1 N1 116.43(6) 3_646 . ?
O3 Zn1 N1 91.31(5) 4_545 . ?
O1 Zn1 O4 87.94(6) . 4_545 ?
O6 Zn1 O4 94.76(6) 3_646 4_545 ?
O3 Zn1 O4 62.39(5) 4_545 4_545 ?
N1 Zn1 O4 145.61(7) . 4_545 ?
O1 Zn1 C30 111.47(6) . 4_545 ?
O6 Zn1 C30 104.66(6) 3_646 4_545 ?
O3 Zn1 C30 32.07(6) 4_545 4_545 ?
N1 Zn1 C30 120.64(6) . 4_545 ?
O4 Zn1 C30 30.32(6) 4_545 4_545 ?
C23 O1 Zn1 126.33(13) . . ?
C1 N1 C5 110.49(17) . . ?
C1 N1 Zn1 126.43(13) . . ?
C5 N1 Zn1 121.92(13) . . ?
N1 C1 C2 125.68(17) . . ?
N1 C1 H1A 117.2 . . ?
C2 C1 H1A 117.2 . . ?
C20 N2 C21 120.00(18) . . ?
C20 N2 H2B 120.0 . . ?
C21 N2 H2B 120.0 . . ?
C3 C2 C1 123.18(18) . . ?
C3 C2 H2A 118.4 . . ?
C1 C2 H2A 118.4 . . ?
C30 O3 Zn1 87.54(11) . 4_546 ?
C6 N3 C3 132.58(16) . . ?
C6 N3 H3A 108.4 . . ?
C3 N3 H3A 119.1 . . ?
C4 C3 C2 110.71(18) . . ?
C4 C3 N3 119.63(17) . . ?
C2 C3 N3 129.61(18) . . ?
C30 O4 Zn1 87.51(12) . 4_546 ?
C17 N4 C18 124.34(18) . . ?
C17 N4 H4B 115.5 . . ?
C18 N4 H4B 120.1 . . ?
C3 C4 C5 122.41(18) . . ?
C3 C4 H4A 118.8 . . ?
C5 C4 H4A 118.8 . . ?
N1 C5 C4 127.19(18) . . ?
N1 C5 H5A 116.4 . . ?
C4 C5 H5A 116.4 . . ?
C27 O6 Zn1 124.58(13) . 3_646 ?
O7 C6 N3 117.27(19) . . ?
O7 C6 C7 125.23(18) . . ?
N3 C6 C7 117.50(16) . . ?
C16 C7 C8 116.74(18) . . ?
C16 C7 C6 119.41(18) . . ?
C8 C7 C6 123.84(17) . . ?
C9 C8 C7 118.47(17) . . ?
C9 C8 C13 119.74(17) . . ?
C7 C8 C13 121.77(17) . . ?
C10 C9 C8 117.14(19) . . ?
C10 C9 H9A 121.4 . . ?
C8 C9 H9A 121.4 . . ?
C9 C10 C11 123.32(19) . . ?
C9 C10 H10A 118.3 . . ?
C11 C10 H10A 118.3 . . ?
C12 C11 C10 121.18(19) . . ?
C12 C11 H11A 119.4 . . ?
C10 C11 H11A 119.4 . . ?
C11 C12 C13 117.57(18) . . ?
C11 C12 H12A 121.2 . . ?
C13 C12 H12A 121.2 . . ?
C14 C13 C12 119.60(18) . . ?
C14 C13 C8 119.36(17) . . ?
C12 C13 C8 121.02(18) . . ?
C15 C14 C13 116.95(18) . . ?
C15 C14 C17 117.89(19) . . ?
C13 C14 C17 125.11(18) . . ?
C14 C15 C16 123.6(2) . . ?
C14 C15 H15A 118.2 . . ?
C16 C15 H15A 118.2 . . ?
C7 C16 C15 121.51(19) . . ?
C7 C16 H16A 119.2 . . ?
C15 C16 H16A 119.2 . . ?
O8 C17 N4 120.5(2) . . ?
O8 C17 C14 123.6(2) . . ?
N4 C17 C14 115.79(18) . . ?
C22 C18 N4 114.43(19) . . ?
C22 C18 C19 117.53(19) . . ?
N4 C18 C19 128.0(2) . . ?
C20 C19 C18 122.6(2) . . ?
C20 C19 H19A 118.7 . . ?
C18 C19 H19A 118.7 . . ?
N2 C20 C19 118.6(2) . . ?
N2 C20 H20A 120.7 . . ?
C19 C20 H20A 120.7 . . ?
C22 C21 N2 125.0(2) . . ?
C22 C21 H21A 117.5 . . ?
N2 C21 H21A 117.5 . . ?
C18 C22 C21 116.3(2) . . ?
C18 C22 H22A 121.9 . . ?
C21 C22 H22A 121.9 . . ?
O1 C23 O2 125.63(18) . . ?
O1 C23 C24 112.14(17) . . ?
O2 C23 C24 122.23(17) . . ?
C31 C24 C25 118.19(16) . . ?
C31 C24 C23 117.80(17) . . ?
C25 C24 C23 123.90(16) . . ?
C26 C25 C24 124.71(16) . . ?
C26 C25 H25A 117.6 . . ?
C24 C25 H25A 117.6 . . ?
C28 C26 C25 116.58(17) . . ?
C28 C26 C27 119.03(16) . . ?
C25 C26 C27 124.27(16) . . ?
O6 C27 O5 123.34(17) . . ?
O6 C27 C26 112.59(16) . . ?
O5 C27 C26 124.06(16) . . ?
C26 C28 C29 119.24(16) . . ?
C26 C28 H28A 120.4 . . ?
C29 C28 H28A 120.4 . . ?
C31 C29 C28 123.61(16) . . ?
C31 C29 C30 117.97(16) . . ?
C28 C29 C30 118.39(16) . . ?
O4 C30 O3 122.55(17) . . ?
O4 C30 C29 117.40(17) . . ?
O3 C30 C29 120.05(16) . . ?
O4 C30 Zn1 62.17(10) . 4_546 ?
O3 C30 Zn1 60.39(9) . 4_546 ?
C29 C30 Zn1 178.68(13) . 4_546 ?
C24 C31 C29 117.64(16) . . ?
C24 C31 H31A 121.2 . . ?
C29 C31 H31A 121.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Zn1 O1 C23 -132.38(16) 3_646 . . . ?
O3 Zn1 O1 C23 10.6(2) 4_545 . . . ?
N1 Zn1 O1 C23 107.68(17) . . . . ?
O4 Zn1 O1 C23 -38.04(17) 4_545 . . . ?
C30 Zn1 O1 C23 -18.47(18) 4_545 . . . ?
O1 Zn1 N1 C1 -11.89(18) . . . . ?
O6 Zn1 N1 C1 -124.21(17) 3_646 . . . ?
O3 Zn1 N1 C1 120.93(17) 4_545 . . . ?
O4 Zn1 N1 C1 82.87(19) 4_545 . . . ?
C30 Zn1 N1 C1 107.25(17) 4_545 . . . ?
O1 Zn1 N1 C5 -178.38(16) . . . . ?
O6 Zn1 N1 C5 69.30(17) 3_646 . . . ?
O3 Zn1 N1 C5 -45.56(16) 4_545 . . . ?
O4 Zn1 N1 C5 -83.62(18) 4_545 . . . ?
C30 Zn1 N1 C5 -59.23(17) 4_545 . . . ?
C5 N1 C1 C2 4.0(3) . . . . ?
Zn1 N1 C1 C2 -163.76(15) . . . . ?
N1 C1 C2 C3 0.6(3) . . . . ?
C1 C2 C3 C4 -5.1(3) . . . . ?
C1 C2 C3 N3 172.44(19) . . . . ?
C6 N3 C3 C4 -169.2(2) . . . . ?
C6 N3 C3 C2 13.5(4) . . . . ?
C2 C3 C4 C5 4.9(3) . . . . ?
N3 C3 C4 C5 -172.84(19) . . . . ?
C1 N1 C5 C4 -4.2(3) . . . . ?
Zn1 N1 C5 C4 164.26(17) . . . . ?
C3 C4 C5 N1 -0.5(4) . . . . ?
C3 N3 C6 O7 0.0(4) . . . . ?
C3 N3 C6 C7 -179.84(18) . . . . ?
O7 C6 C7 C16 -127.0(2) . . . . ?
N3 C6 C7 C16 52.8(3) . . . . ?
O7 C6 C7 C8 53.7(3) . . . . ?
N3 C6 C7 C8 -126.5(2) . . . . ?
C16 C7 C8 C9 179.74(18) . . . . ?
C6 C7 C8 C9 -1.0(3) . . . . ?
C16 C7 C8 C13 -1.8(3) . . . . ?
C6 C7 C8 C13 177.48(16) . . . . ?
C7 C8 C9 C10 179.45(18) . . . . ?
C13 C8 C9 C10 1.0(3) . . . . ?
C8 C9 C10 C11 0.5(3) . . . . ?
C9 C10 C11 C12 -1.0(3) . . . . ?
C10 C11 C12 C13 -0.2(3) . . . . ?
C11 C12 C13 C14 179.95(18) . . . . ?
C11 C12 C13 C8 1.7(3) . . . . ?
C9 C8 C13 C14 179.55(18) . . . . ?
C7 C8 C13 C14 1.1(3) . . . . ?
C9 C8 C13 C12 -2.2(3) . . . . ?
C7 C8 C13 C12 179.40(17) . . . . ?
C12 C13 C14 C15 -177.15(18) . . . . ?
C8 C13 C14 C15 1.1(3) . . . . ?
C12 C13 C14 C17 0.3(3) . . . . ?
C8 C13 C14 C17 178.64(17) . . . . ?
C13 C14 C15 C16 -2.7(3) . . . . ?
C17 C14 C15 C16 179.57(19) . . . . ?
C8 C7 C16 C15 0.3(3) . . . . ?
C6 C7 C16 C15 -179.02(18) . . . . ?
C14 C15 C16 C7 2.1(3) . . . . ?
C18 N4 C17 O8 -7.1(3) . . . . ?
C18 N4 C17 C14 168.86(17) . . . . ?
C15 C14 C17 O8 50.3(3) . . . . ?
C13 C14 C17 O8 -127.2(3) . . . . ?
C15 C14 C17 N4 -125.6(2) . . . . ?
C13 C14 C17 N4 56.9(3) . . . . ?
C17 N4 C18 C22 -167.9(2) . . . . ?
C17 N4 C18 C19 10.8(3) . . . . ?
C22 C18 C19 C20 0.4(3) . . . . ?
N4 C18 C19 C20 -178.3(2) . . . . ?
C21 N2 C20 C19 -0.1(3) . . . . ?
C18 C19 C20 N2 0.2(3) . . . . ?
C20 N2 C21 C22 -0.7(3) . . . . ?
N4 C18 C22 C21 177.83(17) . . . . ?
C19 C18 C22 C21 -1.0(3) . . . . ?
N2 C21 C22 C18 1.3(3) . . . . ?
Zn1 O1 C23 O2 -45.1(3) . . . . ?
Zn1 O1 C23 C24 134.60(14) . . . . ?
O1 C23 C24 C31 175.43(17) . . . . ?
O2 C23 C24 C31 -4.8(3) . . . . ?
O1 C23 C24 C25 -8.5(3) . . . . ?
O2 C23 C24 C25 171.22(18) . . . . ?
C31 C24 C25 C26 0.6(3) . . . . ?
C23 C24 C25 C26 -175.48(18) . . . . ?
C24 C25 C26 C28 -1.9(3) . . . . ?
C24 C25 C26 C27 174.04(16) . . . . ?
Zn1 O6 C27 O5 14.5(3) 3_646 . . . ?
Zn1 O6 C27 C26 -164.54(11) 3_646 . . . ?
C28 C26 C27 O6 -175.58(17) . . . . ?
C25 C26 C27 O6 8.6(3) . . . . ?
C28 C26 C27 O5 5.4(3) . . . . ?
C25 C26 C27 O5 -170.44(18) . . . . ?
C25 C26 C28 C29 1.9(3) . . . . ?
C27 C26 C28 C29 -174.25(15) . . . . ?
C26 C28 C29 C31 -0.8(3) . . . . ?
C26 C28 C29 C30 177.19(16) . . . . ?
Zn1 O4 C30 O3 1.11(19) 4_546 . . . ?
Zn1 O4 C30 C29 -178.59(15) 4_546 . . . ?
Zn1 O3 C30 O4 -1.1(2) 4_546 . . . ?
Zn1 O3 C30 C29 178.57(15) 4_546 . . . ?
C31 C29 C30 O4 -166.38(18) . . . . ?
C28 C29 C30 O4 15.5(3) . . . . ?
C31 C29 C30 O3 13.9(3) . . . . ?
C28 C29 C30 O3 -164.20(16) . . . . ?
C31 C29 C30 Zn1 123(6) . . . 4_546 ?
C28 C29 C30 Zn1 -55(6) . . . 4_546 ?
C25 C24 C31 C29 0.6(3) . . . . ?
C23 C24 C31 C29 176.93(16) . . . . ?
C28 C29 C31 C24 -0.5(3) . . . . ?
C30 C29 C31 C24 -178.55(16) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.051
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lm-10
_database_code_depnum_ccdc_archive 'CCDC 1005172'
_audit_update_record             
;
2014-05-25 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H17 Cd Cl N4 O4'
_chemical_formula_weight         585.28

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P -3'

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

_cell_length_a                   14.1344(19)
_cell_length_b                   14.1344(19)
_cell_length_c                   20.396(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3528.9(9)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.66
_cell_measurement_theta_max      26.52

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1752
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20101
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.52
_reflns_number_total             4887
_reflns_number_gt                3880
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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)+(0.0528P)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         4887
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0987
_refine_ls_wR_factor_gt          0.0926
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd -0.23967(2) -0.457031(19) 0.150829(11) 0.02258(10) Uani 1 1 d . . .
Cl1 Cl -0.44983(7) -0.57375(7) 0.14998(4) 0.0352(2) Uani 1 1 d . . .
O1 O -0.22436(18) -0.28355(18) 0.14811(11) 0.0269(5) Uani 1 1 d . . .
O2 O -0.07131(19) -0.28749(19) 0.16088(12) 0.0318(6) Uani 1 1 d . . .
O5 O -0.3800(3) -0.3819(3) 0.49245(12) 0.0509(8) Uani 1 1 d . . .
O6 O -0.1730(4) -0.4945(4) 0.79078(14) 0.1023(17) Uani 1 1 d . . .
N1 N -0.2488(2) -0.4532(2) 0.26549(14) 0.0295(7) Uani 1 1 d . . .
N2 N -0.2412(2) -0.4491(2) 0.03651(14) 0.0257(6) Uani 1 1 d . . .
N3 N -0.2440(3) -0.4200(3) 0.46966(14) 0.0424(8) Uani 1 1 d . . .
H3A H -0.1935 -0.4272 0.4884 0.051 Uiso 1 1 d R . .
N4 N -0.2590(3) -0.4116(3) 0.83378(13) 0.0326(7) Uani 1 1 d . . .
H4B H -0.2903 -0.3750 0.8233 0.039 Uiso 1 1 d R . .
C1 C -0.1703(4) -0.4501(4) 0.30317(19) 0.0481(11) Uani 1 1 d . . .
H1A H -0.1142 -0.4555 0.2829 0.058 Uiso 1 1 calc R . .
C2 C -0.1673(4) -0.4394(4) 0.36986(18) 0.0489(12) Uani 1 1 d . . .
H2A H -0.1109 -0.4383 0.3939 0.059 Uiso 1 1 calc R . .
C3 C -0.2494(3) -0.4303(3) 0.40113(17) 0.0336(8) Uani 1 1 d . . .
C4 C -0.3310(3) -0.4314(4) 0.36279(18) 0.0404(10) Uani 1 1 d . . .
H4A H -0.3872 -0.4248 0.3817 0.048 Uiso 1 1 calc R . .
C5 C -0.3266(3) -0.4426(3) 0.29610(17) 0.0378(9) Uani 1 1 d . . .
H5A H -0.3813 -0.4428 0.2706 0.045 Uiso 1 1 calc R . .
C6 C -0.3088(3) -0.3998(3) 0.51073(17) 0.0365(9) Uani 1 1 d . . .
C7 C -0.2849(3) -0.4048(3) 0.58224(16) 0.0346(9) Uani 1 1 d . . .
C8 C -0.1867(3) -0.3232(3) 0.61203(16) 0.0326(8) Uani 1 1 d . . .
C9 C -0.1066(3) -0.2314(3) 0.5768(2) 0.0411(10) Uani 1 1 d . . .
H9A H -0.1167 -0.2243 0.5324 0.049 Uiso 1 1 calc R . .
C10 C -0.0148(4) -0.1533(4) 0.6076(2) 0.0498(11) Uani 1 1 d . . .
H10A H 0.0371 -0.0934 0.5840 0.060 Uiso 1 1 calc R . .
C11 C 0.0017(4) -0.1624(4) 0.6738(2) 0.0566(12) Uani 1 1 d . . .
H11A H 0.0638 -0.1076 0.6943 0.068 Uiso 1 1 calc R . .
C12 C -0.0715(4) -0.2503(4) 0.7090(2) 0.0460(11) Uani 1 1 d . . .
H12A H -0.0578 -0.2561 0.7530 0.055 Uiso 1 1 calc R . .
C13 C -0.1685(3) -0.3334(3) 0.67957(17) 0.0350(9) Uani 1 1 d . . .
C14 C -0.2488(3) -0.4253(3) 0.71495(17) 0.0363(9) Uani 1 1 d . . .
C15 C -0.3430(4) -0.5014(4) 0.68516(19) 0.0507(12) Uani 1 1 d . . .
H15A H -0.3953 -0.5605 0.7091 0.061 Uiso 1 1 calc R . .
C16 C -0.3612(4) -0.4907(4) 0.61859(19) 0.0490(11) Uani 1 1 d . . .
H16A H -0.4259 -0.5426 0.5989 0.059 Uiso 1 1 calc R . .
C17 C -0.2235(4) -0.4475(4) 0.78379(19) 0.0468(11) Uani 1 1 d . . .
C18 C -0.2509(3) -0.4267(3) 0.90077(16) 0.0267(7) Uani 1 1 d . . .
C19 C -0.2003(3) -0.4806(3) 0.92748(17) 0.0370(9) Uani 1 1 d . . .
H19A H -0.1683 -0.5100 0.9006 0.044 Uiso 1 1 calc R . .
C20 C -0.1987(3) -0.4894(3) -0.00549(16) 0.0344(9) Uani 1 1 d . . .
H20A H -0.1653 -0.5264 0.0117 0.041 Uiso 1 1 calc R . .
C21 C -0.2903(3) -0.3976(3) 0.01032(17) 0.0358(9) Uani 1 1 d . . .
H21A H -0.3209 -0.3684 0.0384 0.043 Uiso 1 1 calc R . .
C22 C -0.2973(3) -0.3861(3) 0.94414(17) 0.0366(9) Uani 1 1 d . . .
H22A H -0.3333 -0.3508 0.9283 0.044 Uiso 1 1 calc R . .
C23 C -0.1223(3) -0.2361(3) 0.15273(16) 0.0229(7) Uani 1 1 d . . .
C24 C -0.0583(3) -0.1134(3) 0.14925(15) 0.0214(7) Uani 1 1 d . . .
C25 C -0.1133(3) -0.0549(3) 0.14894(16) 0.0229(7) Uani 1 1 d . . .
H25A H -0.1893 -0.0917 0.1485 0.027 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
Cd1 N2 2.335(3) . ?
Cd1 N1 2.344(3) . ?
Cd1 O1 2.352(2) . ?
Cd1 O2 2.397(2) . ?
Cd1 Cl1 2.5619(10) 3_545 ?
Cd1 Cl1 2.5779(10) . ?
Cd1 C23 2.707(3) . ?
Cl1 Cd1 2.5620(10) 2_445 ?
O1 C23 1.254(4) . ?
O2 C23 1.264(4) . ?
O5 C6 1.212(5) . ?
O6 C17 1.202(5) . ?
N1 C1 1.332(5) . ?
N1 C5 1.337(5) . ?
N2 C20 1.327(4) . ?
N2 C21 1.343(4) . ?
N3 C6 1.373(5) . ?
N3 C3 1.403(4) . ?
N3 H3A 0.8599 . ?
N4 C17 1.343(5) . ?
N4 C18 1.396(4) . ?
N4 H4B 0.8598 . ?
C1 C2 1.367(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.386(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.386(5) . ?
C4 C5 1.374(5) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C6 C7 1.507(5) . ?
C7 C16 1.369(6) . ?
C7 C8 1.424(5) . ?
C8 C9 1.419(5) . ?
C8 C13 1.422(5) . ?
C9 C10 1.366(6) . ?
C9 H9A 0.9300 . ?
C10 C11 1.386(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.359(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.417(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.421(5) . ?
C14 C15 1.367(6) . ?
C14 C17 1.520(5) . ?
C15 C16 1.404(5) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C18 C22 1.386(5) . ?
C18 C19 1.390(5) . ?
C19 C20 1.374(5) 1_556 ?
C19 H19A 0.9300 . ?
C20 C19 1.374(5) 1_554 ?
C20 H20A 0.9300 . ?
C21 C22 1.369(5) 1_554 ?
C21 H21A 0.9300 . ?
C22 C21 1.369(5) 1_556 ?
C22 H22A 0.9300 . ?
C23 C24 1.504(4) . ?
C24 C25 1.386(4) 2 ?
C24 C25 1.389(4) . ?
C25 C24 1.386(4) 3 ?
C25 H25A 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
N2 Cd1 N1 173.30(10) . . ?
N2 Cd1 O1 85.69(9) . . ?
N1 Cd1 O1 88.68(9) . . ?
N2 Cd1 O2 93.78(9) . . ?
N1 Cd1 O2 85.99(9) . . ?
O1 Cd1 O2 55.38(8) . . ?
N2 Cd1 Cl1 92.37(7) . 3_545 ?
N1 Cd1 Cl1 94.31(8) . 3_545 ?
O1 Cd1 Cl1 141.82(6) . 3_545 ?
O2 Cd1 Cl1 86.82(6) . 3_545 ?
N2 Cd1 Cl1 89.36(7) . . ?
N1 Cd1 Cl1 87.85(7) . . ?
O1 Cd1 Cl1 98.22(6) . . ?
O2 Cd1 Cl1 152.97(6) . . ?
Cl1 Cd1 Cl1 119.91(4) 3_545 . ?
N2 Cd1 C23 88.52(10) . . ?
N1 Cd1 C23 88.17(10) . . ?
O1 Cd1 C23 27.58(9) . . ?
O2 Cd1 C23 27.85(9) . . ?
Cl1 Cd1 C23 114.36(7) 3_545 . ?
Cl1 Cd1 C23 125.73(8) . . ?
Cd1 Cl1 Cd1 120.08(4) 2_445 . ?
C23 O1 Cd1 92.16(19) . . ?
C23 O2 Cd1 89.8(2) . . ?
C1 N1 C5 116.5(3) . . ?
C1 N1 Cd1 121.5(3) . . ?
C5 N1 Cd1 121.7(2) . . ?
C20 N2 C21 116.3(3) . . ?
C20 N2 Cd1 127.4(2) . . ?
C21 N2 Cd1 116.3(2) . . ?
C6 N3 C3 128.5(3) . . ?
C6 N3 H3A 115.8 . . ?
C3 N3 H3A 115.8 . . ?
C17 N4 C18 127.6(3) . . ?
C17 N4 H4B 116.2 . . ?
C18 N4 H4B 116.2 . . ?
N1 C1 C2 123.8(4) . . ?
N1 C1 H1A 118.1 . . ?
C2 C1 H1A 118.1 . . ?
C1 C2 C3 119.2(4) . . ?
C1 C2 H2A 120.4 . . ?
C3 C2 H2A 120.4 . . ?
C2 C3 C4 118.0(3) . . ?
C2 C3 N3 117.6(3) . . ?
C4 C3 N3 124.4(4) . . ?
C5 C4 C3 118.4(4) . . ?
C5 C4 H4A 120.8 . . ?
C3 C4 H4A 120.8 . . ?
N1 C5 C4 124.2(3) . . ?
N1 C5 H5A 117.9 . . ?
C4 C5 H5A 117.9 . . ?
O5 C6 N3 124.4(3) . . ?
O5 C6 C7 122.5(3) . . ?
N3 C6 C7 113.1(3) . . ?
C16 C7 C8 120.2(3) . . ?
C16 C7 C6 118.1(4) . . ?
C8 C7 C6 121.7(3) . . ?
C9 C8 C13 118.8(4) . . ?
C9 C8 C7 122.3(3) . . ?
C13 C8 C7 118.9(3) . . ?
C10 C9 C8 120.5(4) . . ?
C10 C9 H9A 119.8 . . ?
C8 C9 H9A 119.8 . . ?
C9 C10 C11 120.6(4) . . ?
C9 C10 H10A 119.7 . . ?
C11 C10 H10A 119.7 . . ?
C12 C11 C10 120.8(4) . . ?
C12 C11 H11A 119.6 . . ?
C10 C11 H11A 119.6 . . ?
C11 C12 C13 120.9(4) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C12 C13 C14 122.8(3) . . ?
C12 C13 C8 118.4(4) . . ?
C14 C13 C8 118.9(4) . . ?
C15 C14 C13 120.8(3) . . ?
C15 C14 C17 119.0(4) . . ?
C13 C14 C17 119.7(4) . . ?
C14 C15 C16 120.2(4) . . ?
C14 C15 H15A 119.9 . . ?
C16 C15 H15A 119.9 . . ?
C7 C16 C15 120.9(4) . . ?
C7 C16 H16A 119.5 . . ?
C15 C16 H16A 119.5 . . ?
O6 C17 N4 123.8(4) . . ?
O6 C17 C14 119.3(4) . . ?
N4 C17 C14 116.9(4) . . ?
C22 C18 C19 117.2(3) . . ?
C22 C18 N4 118.0(3) . . ?
C19 C18 N4 124.8(3) . . ?
C20 C19 C18 118.5(3) 1_556 . ?
C20 C19 H19A 120.8 1_556 . ?
C18 C19 H19A 120.8 . . ?
N2 C20 C19 124.9(3) . 1_554 ?
N2 C20 H20A 117.6 . . ?
C19 C20 H20A 117.6 1_554 . ?
N2 C21 C22 123.0(3) . 1_554 ?
N2 C21 H21A 118.5 . . ?
C22 C21 H21A 118.5 1_554 . ?
C21 C22 C18 120.2(3) 1_556 . ?
C21 C22 H22A 119.9 1_556 . ?
C18 C22 H22A 119.9 . . ?
O1 C23 O2 122.4(3) . . ?
O1 C23 C24 118.7(3) . . ?
O2 C23 C24 118.8(3) . . ?
O1 C23 Cd1 60.26(17) . . ?
O2 C23 Cd1 62.32(17) . . ?
C24 C23 Cd1 176.4(2) . . ?
C25 C24 C25 120.0(3) 2 . ?
C25 C24 C23 120.4(3) 2 . ?
C25 C24 C23 119.6(3) . . ?
C24 C25 C24 120.0(3) 3 . ?
C24 C25 H25A 120.0 3 . ?
C24 C25 H25A 120.0 . . ?

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
N2 Cd1 Cl1 Cd1 93.69(8) . . . 2_445 ?
N1 Cd1 Cl1 Cd1 -92.40(8) . . . 2_445 ?
O1 Cd1 Cl1 Cd1 179.25(6) . . . 2_445 ?
O2 Cd1 Cl1 Cd1 -169.25(13) . . . 2_445 ?
Cl1 Cd1 Cl1 Cd1 1.33(7) 3_545 . . 2_445 ?
C23 Cd1 Cl1 Cd1 -178.60(8) . . . 2_445 ?
N2 Cd1 O1 C23 -95.1(2) . . . . ?
N1 Cd1 O1 C23 88.6(2) . . . . ?
O2 Cd1 O1 C23 2.55(18) . . . . ?
Cl1 Cd1 O1 C23 -6.7(2) 3_545 . . . ?
Cl1 Cd1 O1 C23 176.22(18) . . . . ?
N2 Cd1 O2 C23 79.6(2) . . . . ?
N1 Cd1 O2 C23 -93.7(2) . . . . ?
O1 Cd1 O2 C23 -2.52(18) . . . . ?
Cl1 Cd1 O2 C23 171.77(19) 3_545 . . . ?
Cl1 Cd1 O2 C23 -16.4(3) . . . . ?
N2 Cd1 N1 C1 -147.1(8) . . . . ?
O1 Cd1 N1 C1 -114.3(3) . . . . ?
O2 Cd1 N1 C1 -58.9(3) . . . . ?
Cl1 Cd1 N1 C1 27.6(3) 3_545 . . . ?
Cl1 Cd1 N1 C1 147.5(3) . . . . ?
C23 Cd1 N1 C1 -86.7(3) . . . . ?
N2 Cd1 N1 C5 25.9(10) . . . . ?
O1 Cd1 N1 C5 58.7(3) . . . . ?
O2 Cd1 N1 C5 114.1(3) . . . . ?
Cl1 Cd1 N1 C5 -159.4(3) 3_545 . . . ?
Cl1 Cd1 N1 C5 -39.6(3) . . . . ?
C23 Cd1 N1 C5 86.3(3) . . . . ?
N1 Cd1 N2 C20 178.4(8) . . . . ?
O1 Cd1 N2 C20 145.4(3) . . . . ?
O2 Cd1 N2 C20 90.6(3) . . . . ?
Cl1 Cd1 N2 C20 3.6(3) 3_545 . . . ?
Cl1 Cd1 N2 C20 -116.3(3) . . . . ?
C23 Cd1 N2 C20 118.0(3) . . . . ?
N1 Cd1 N2 C21 -1.4(10) . . . . ?
O1 Cd1 N2 C21 -34.3(3) . . . . ?
O2 Cd1 N2 C21 -89.1(3) . . . . ?
Cl1 Cd1 N2 C21 -176.1(3) 3_545 . . . ?
Cl1 Cd1 N2 C21 64.0(3) . . . . ?
C23 Cd1 N2 C21 -61.8(3) . . . . ?
C5 N1 C1 C2 1.5(6) . . . . ?
Cd1 N1 C1 C2 174.8(4) . . . . ?
N1 C1 C2 C3 -0.5(7) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
C1 C2 C3 N3 179.7(4) . . . . ?
C6 N3 C3 C2 173.4(4) . . . . ?
C6 N3 C3 C4 -6.3(7) . . . . ?
C2 C3 C4 C5 0.7(6) . . . . ?
N3 C3 C4 C5 -179.7(4) . . . . ?
C1 N1 C5 C4 -1.5(6) . . . . ?
Cd1 N1 C5 C4 -174.8(3) . . . . ?
C3 C4 C5 N1 0.4(6) . . . . ?
C3 N3 C6 O5 -4.0(7) . . . . ?
C3 N3 C6 C7 174.5(4) . . . . ?
O5 C6 C7 C16 68.9(6) . . . . ?
N3 C6 C7 C16 -109.7(4) . . . . ?
O5 C6 C7 C8 -110.8(5) . . . . ?
N3 C6 C7 C8 70.6(5) . . . . ?
C16 C7 C8 C9 -178.3(4) . . . . ?
C6 C7 C8 C9 1.4(6) . . . . ?
C16 C7 C8 C13 1.0(6) . . . . ?
C6 C7 C8 C13 -179.3(3) . . . . ?
C13 C8 C9 C10 -1.2(6) . . . . ?
C7 C8 C9 C10 178.1(4) . . . . ?
C8 C9 C10 C11 0.0(7) . . . . ?
C9 C10 C11 C12 1.6(7) . . . . ?
C10 C11 C12 C13 -2.0(7) . . . . ?
C11 C12 C13 C14 -178.2(4) . . . . ?
C11 C12 C13 C8 0.8(6) . . . . ?
C9 C8 C13 C12 0.8(5) . . . . ?
C7 C8 C13 C12 -178.6(4) . . . . ?
C9 C8 C13 C14 179.9(4) . . . . ?
C7 C8 C13 C14 0.5(5) . . . . ?
C12 C13 C14 C15 177.5(4) . . . . ?
C8 C13 C14 C15 -1.5(6) . . . . ?
C12 C13 C14 C17 -10.7(6) . . . . ?
C8 C13 C14 C17 170.3(3) . . . . ?
C13 C14 C15 C16 1.0(7) . . . . ?
C17 C14 C15 C16 -170.9(4) . . . . ?
C8 C7 C16 C15 -1.5(7) . . . . ?
C6 C7 C16 C15 178.7(4) . . . . ?
C14 C15 C16 C7 0.6(7) . . . . ?
C18 N4 C17 O6 -4.2(8) . . . . ?
C18 N4 C17 C14 176.5(3) . . . . ?
C15 C14 C17 O6 89.6(6) . . . . ?
C13 C14 C17 O6 -82.3(6) . . . . ?
C15 C14 C17 N4 -91.1(5) . . . . ?
C13 C14 C17 N4 97.0(5) . . . . ?
C17 N4 C18 C22 -177.4(4) . . . . ?
C17 N4 C18 C19 2.0(6) . . . . ?
C22 C18 C19 C20 -0.5(6) . . . 1_556 ?
N4 C18 C19 C20 -179.9(3) . . . 1_556 ?
C21 N2 C20 C19 1.0(6) . . . 1_554 ?
Cd1 N2 C20 C19 -178.8(3) . . . 1_554 ?
C20 N2 C21 C22 0.0(6) . . . 1_554 ?
Cd1 N2 C21 C22 179.8(3) . . . 1_554 ?
C19 C18 C22 C21 1.4(6) . . . 1_556 ?
N4 C18 C22 C21 -179.1(3) . . . 1_556 ?
Cd1 O1 C23 O2 -4.7(3) . . . . ?
Cd1 O1 C23 C24 176.1(3) . . . . ?
Cd1 O2 C23 O1 4.6(3) . . . . ?
Cd1 O2 C23 C24 -176.2(3) . . . . ?
N2 Cd1 C23 O1 83.53(19) . . . . ?
N1 Cd1 C23 O1 -90.64(19) . . . . ?
O2 Cd1 C23 O1 -175.5(3) . . . . ?
Cl1 Cd1 C23 O1 175.46(16) 3_545 . . . ?
Cl1 Cd1 C23 O1 -4.6(2) . . . . ?
N2 Cd1 C23 O2 -100.96(19) . . . . ?
N1 Cd1 C23 O2 84.9(2) . . . . ?
O1 Cd1 C23 O2 175.5(3) . . . . ?
Cl1 Cd1 C23 O2 -9.0(2) 3_545 . . . ?
Cl1 Cd1 C23 O2 170.90(15) . . . . ?
N2 Cd1 C23 C24 9(4) . . . . ?
N1 Cd1 C23 C24 -165(4) . . . . ?
O1 Cd1 C23 C24 -75(4) . . . . ?
O2 Cd1 C23 C24 110(4) . . . . ?
Cl1 Cd1 C23 C24 101(4) 3_545 . . . ?
Cl1 Cd1 C23 C24 -79(4) . . . . ?
O1 C23 C24 C25 -174.9(3) . . . 2 ?
O2 C23 C24 C25 5.9(5) . . . 2 ?
Cd1 C23 C24 C25 -102(4) . . . 2 ?
O1 C23 C24 C25 7.6(5) . . . . ?
O2 C23 C24 C25 -171.6(3) . . . . ?
Cd1 C23 C24 C25 81(4) . . . . ?
C25 C24 C25 C24 -0.9(6) 2 . . 3 ?
C23 C24 C25 C24 176.6(2) . . . 3 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.52
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.990
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.105

#==End==#
