# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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 1479971'
_audit_update_record             
;
2016-05-15 deposited with the CCDC.
2016-11-07 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 H26 Cu N4 O8'
_chemical_formula_weight         610.07

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           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.2276(5)
_cell_length_b                   11.6453(6)
_cell_length_c                   12.8446(7)
_cell_angle_alpha                89.7710(10)
_cell_angle_beta                 76.7720(10)
_cell_angle_gamma                76.6840(10)
_cell_volume                     1305.78(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.63
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             630
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.874
_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            6715
_diffrn_reflns_av_R_equivalents  0.0124
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4577
_reflns_number_gt                4074
_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)+(0.0483P)²+0.7396P] 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         4577
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0859
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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 -0.11123(3) 0.36085(2) 0.46862(2) 0.02196(10) Uani 1 1 d . . .
N1 N -0.2460(2) 0.34262(15) 0.61491(14) 0.0229(4) Uani 1 1 d . . .
O1 O 0.06877(17) 0.28906(14) 0.51918(13) 0.0306(4) Uani 1 1 d . . .
C1 C -0.3907(3) 0.40773(19) 0.63639(18) 0.0264(5) Uani 1 1 d . . .
H1A H -0.4205 0.4606 0.5865 0.032 Uiso 1 1 calc R . .
O1W O -0.3894(2) 0.41035(17) 1.04279(17) 0.0545(5) Uani 1 1 d . . .
H1WA H -0.4096 0.3458 1.0241 0.065 Uiso 1 1 d R . .
H1WB H -0.4550 0.4369 1.1008 0.065 Uiso 1 1 d R . .
O2 O 0.18852(19) 0.43574(14) 0.49070(15) 0.0377(4) Uani 1 1 d . . .
N2 N 0.0155(2) -0.62186(16) 1.32022(15) 0.0250(4) Uani 1 1 d . . .
C2 C -0.4966(3) 0.3997(2) 0.72888(19) 0.0301(5) Uani 1 1 d . . .
H2A H -0.5957 0.4468 0.7413 0.036 Uiso 1 1 calc R . .
O2W O 1.0222(3) 0.0180(2) 0.38665(17) 0.0741(8) Uani 1 1 d . . .
H2WA H 1.0472 0.0800 0.4017 0.089 Uiso 1 1 d R . .
H2WB H 0.9280 0.0362 0.3851 0.089 Uiso 1 1 d R . .
O3 O 0.70802(18) 0.38143(14) 0.40374(13) 0.0283(4) Uani 1 1 d . . .
N3 N -0.1602(2) 0.06552(16) 0.82961(15) 0.0297(4) Uani 1 1 d . . .
H3B H -0.1152 0.0601 0.7627 0.036 Uiso 1 1 calc R . .
C3 C -0.4542(3) 0.3213(2) 0.80268(18) 0.0289(5) Uani 1 1 d . . .
H3A H -0.5244 0.3147 0.8658 0.035 Uiso 1 1 calc R . .
C4 C -0.3052(3) 0.25195(19) 0.78213(18) 0.0246(5) Uani 1 1 d . . .
O4 O 0.7623(2) 0.18680(15) 0.40830(16) 0.0419(4) Uani 1 1 d . . .
N4 N 0.0398(2) -0.33782(17) 1.04894(16) 0.0329(5) Uani 1 1 d . . .
H13A H 0.1367 -0.3685 1.0305 0.039 Uiso 1 1 calc R . .
O5 O -0.3377(2) 0.18683(15) 0.95902(13) 0.0421(5) Uani 1 1 d . . .
C5 C -0.2041(3) 0.26626(19) 0.68749(18) 0.0250(5) Uani 1 1 d . . .
H5A H -0.1037 0.2214 0.6738 0.030 Uiso 1 1 calc R . .
O6 O -0.1827(2) -0.3595(2) 1.1535(2) 0.0838(9) Uani 1 1 d . . .
C6 C -0.2670(3) 0.1651(2) 0.86497(18) 0.0280(5) Uani 1 1 d . . .
C7 C -0.1135(3) -0.0322(2) 0.89103(18) 0.0278(5) Uani 1 1 d . . .
C8 C -0.2022(3) -0.0552(2) 0.9874(2) 0.0459(7) Uani 1 1 d . . .
H8A H -0.2957 -0.0033 1.0167 0.055 Uiso 1 1 calc R . .
C9 C -0.1531(3) -0.1544(2) 1.0406(2) 0.0469(7) Uani 1 1 d . . .
H9A H -0.2130 -0.1679 1.1061 0.056 Uiso 1 1 calc R . .
C10 C -0.0159(3) -0.2340(2) 0.99762(18) 0.0288(5) Uani 1 1 d . . .
C11 C 0.0721(3) -0.2109(2) 0.9015(2) 0.0343(6) Uani 1 1 d . . .
H11A H 0.1649 -0.2635 0.8716 0.041 Uiso 1 1 calc R . .
C12 C 0.0247(3) -0.1109(2) 0.84913(19) 0.0345(6) Uani 1 1 d . . .
H12A H 0.0864 -0.0962 0.7848 0.041 Uiso 1 1 calc R . .
C13 C -0.0442(3) -0.3927(2) 1.1235(2) 0.0396(6) Uani 1 1 d . . .
C14 C 0.0384(3) -0.4995(2) 1.16965(19) 0.0307(5) Uani 1 1 d . . .
C15 C 0.1787(3) -0.5740(2) 1.1214(2) 0.0382(6) Uani 1 1 d . . .
H15A H 0.2345 -0.5577 1.0553 0.046 Uiso 1 1 calc R . .
C16 C 0.2335(3) -0.6727(2) 1.1736(2) 0.0377(6) Uani 1 1 d . . .
H16A H 0.3262 -0.7245 1.1424 0.045 Uiso 1 1 calc R . .
C17 C 0.1501(3) -0.6940(2) 1.27193(19) 0.0306(5) Uani 1 1 d . . .
H17A H 0.1883 -0.7607 1.3063 0.037 Uiso 1 1 calc R . .
C18 C -0.0388(3) -0.5282(2) 1.26788(18) 0.0267(5) Uani 1 1 d . . .
H18A H -0.1339 -0.4797 1.2994 0.032 Uiso 1 1 calc R . .
C19 C 0.1840(2) 0.33367(19) 0.51293(17) 0.0232(5) Uani 1 1 d . . .
C20 C 0.3266(3) 0.2479(2) 0.53275(19) 0.0292(5) Uani 1 1 d . . .
H20A H 0.4036 0.2909 0.5373 0.035 Uiso 1 1 calc R . .
H20B H 0.3003 0.2114 0.6003 0.035 Uiso 1 1 calc R . .
C21 C 0.3913(2) 0.15258(19) 0.44264(19) 0.0262(5) Uani 1 1 d . . .
C22 C 0.3462(3) 0.0466(2) 0.4543(2) 0.0356(6) Uani 1 1 d . . .
H22A H 0.2802 0.0344 0.5176 0.043 Uiso 1 1 calc R . .
C23 C 0.3980(3) -0.0408(2) 0.3732(3) 0.0473(7) Uani 1 1 d . . .
H23A H 0.3675 -0.1116 0.3823 0.057 Uiso 1 1 calc R . .
C24 C 0.4944(3) -0.0232(3) 0.2796(3) 0.0546(8) Uani 1 1 d . . .
H24A H 0.5272 -0.0810 0.2241 0.066 Uiso 1 1 calc R . .
C25 C 0.5427(3) 0.0808(3) 0.2679(2) 0.0448(7) Uani 1 1 d . . .
H25A H 0.6101 0.0915 0.2047 0.054 Uiso 1 1 calc R . .
C26 C 0.4929(2) 0.1699(2) 0.34866(19) 0.0283(5) Uani 1 1 d . . .
C27 C 0.5511(3) 0.2808(2) 0.3340(2) 0.0300(5) Uani 1 1 d . . .
H27A H 0.4675 0.3478 0.3640 0.036 Uiso 1 1 calc R . .
H27B H 0.5839 0.2912 0.2580 0.036 Uiso 1 1 calc R . .
C28 C 0.6844(2) 0.2808(2) 0.38631(17) 0.0249(5) 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
Cu1 O1 1.9311(15) . ?
Cu1 O3 1.9962(15) 1_455 ?
Cu1 N2 2.0314(18) 1_564 ?
Cu1 N1 2.0425(18) . ?
Cu1 O2 2.3355(16) 2_566 ?
N1 C1 1.341(3) . ?
N1 C5 1.345(3) . ?
O1 C19 1.273(3) . ?
C1 C2 1.373(3) . ?
O2 C19 1.229(3) . ?
O2 Cu1 2.3354(16) 2_566 ?
N2 C18 1.337(3) . ?
N2 C17 1.343(3) . ?
N2 Cu1 2.0314(18) 1_546 ?
C2 C3 1.372(3) . ?
O3 C28 1.270(3) . ?
O3 Cu1 1.9961(15) 1_655 ?
N3 C6 1.340(3) . ?
N3 C7 1.423(3) . ?
C3 C4 1.392(3) . ?
C4 C5 1.388(3) . ?
C4 C6 1.509(3) . ?
O4 C28 1.234(3) . ?
N4 C13 1.345(3) . ?
N4 C10 1.422(3) . ?
O5 C6 1.231(3) . ?
O6 C13 1.216(3) . ?
C7 C12 1.381(3) . ?
C7 C8 1.382(3) . ?
C8 C9 1.378(4) . ?
C9 C10 1.382(3) . ?
C10 C11 1.377(3) . ?
C11 C12 1.375(3) . ?
C13 C14 1.497(3) . ?
C14 C18 1.381(3) . ?
C14 C15 1.390(3) . ?
C15 C16 1.381(3) . ?
C16 C17 1.374(3) . ?
C19 C20 1.530(3) . ?
C20 C21 1.522(3) . ?
C21 C22 1.387(3) . ?
C21 C26 1.394(3) . ?
C22 C23 1.380(4) . ?
C23 C24 1.368(5) . ?
C24 C25 1.380(4) . ?
C25 C26 1.391(3) . ?
C26 C27 1.504(3) . ?
C27 C28 1.530(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
O1 Cu1 O3 161.73(7) . 1_455 ?
O1 Cu1 N2 92.28(7) . 1_564 ?
O3 Cu1 N2 87.51(7) 1_455 1_564 ?
O1 Cu1 N1 89.82(7) . . ?
O3 Cu1 N1 90.09(7) 1_455 . ?
N2 Cu1 N1 177.54(7) 1_564 . ?
O1 Cu1 O2 111.94(7) . 2_566 ?
O3 Cu1 O2 86.29(6) 1_455 2_566 ?
N2 Cu1 O2 93.80(7) 1_564 2_566 ?
N1 Cu1 O2 86.59(7) . 2_566 ?
C1 N1 C5 118.14(19) . . ?
C1 N1 Cu1 116.41(14) . . ?
C5 N1 Cu1 125.32(15) . . ?
C19 O1 Cu1 124.78(14) . . ?
N1 C1 C2 122.8(2) . . ?
C19 O2 Cu1 151.20(16) . 2_566 ?
C18 N2 C17 117.60(19) . . ?
C18 N2 Cu1 116.59(15) . 1_546 ?
C17 N2 Cu1 125.78(15) . 1_546 ?
C3 C2 C1 119.1(2) . . ?
C28 O3 Cu1 109.32(14) . 1_655 ?
C6 N3 C7 126.87(19) . . ?
C2 C3 C4 119.3(2) . . ?
C5 C4 C3 118.2(2) . . ?
C5 C4 C6 125.0(2) . . ?
C3 C4 C6 116.8(2) . . ?
C13 N4 C10 126.4(2) . . ?
N1 C5 C4 122.4(2) . . ?
O5 C6 N3 123.8(2) . . ?
O5 C6 C4 119.3(2) . . ?
N3 C6 C4 116.84(19) . . ?
C12 C7 C8 118.5(2) . . ?
C12 C7 N3 117.9(2) . . ?
C8 C7 N3 123.5(2) . . ?
C9 C8 C7 120.6(2) . . ?
C8 C9 C10 120.8(2) . . ?
C11 C10 C9 118.5(2) . . ?
C11 C10 N4 118.4(2) . . ?
C9 C10 N4 123.1(2) . . ?
C12 C11 C10 120.9(2) . . ?
C11 C12 C7 120.8(2) . . ?
O6 C13 N4 122.7(2) . . ?
O6 C13 C14 119.6(2) . . ?
N4 C13 C14 117.7(2) . . ?
C18 C14 C15 117.9(2) . . ?
C18 C14 C13 115.3(2) . . ?
C15 C14 C13 126.7(2) . . ?
C16 C15 C14 118.6(2) . . ?
C17 C16 C15 119.7(2) . . ?
N2 C17 C16 122.4(2) . . ?
N2 C18 C14 123.8(2) . . ?
O2 C19 O1 125.5(2) . . ?
O2 C19 C20 119.8(2) . . ?
O1 C19 C20 114.61(19) . . ?
C21 C20 C19 110.51(18) . . ?
C22 C21 C26 119.5(2) . . ?
C22 C21 C20 118.9(2) . . ?
C26 C21 C20 121.6(2) . . ?
C23 C22 C21 120.9(3) . . ?
C24 C23 C22 119.9(3) . . ?
C23 C24 C25 119.7(3) . . ?
C24 C25 C26 121.4(3) . . ?
C25 C26 C21 118.5(2) . . ?
C25 C26 C27 119.9(2) . . ?
C21 C26 C27 121.6(2) . . ?
C26 C27 C28 113.91(19) . . ?
O4 C28 O3 123.8(2) . . ?
O4 C28 C27 120.3(2) . . ?
O3 C28 C27 115.9(2) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.434
_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-3
_database_code_depnum_ccdc_archive 'CCDC 1479973'
_audit_update_record             
;
2016-05-15 deposited with the CCDC.
2016-11-07 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 H32 Cu N4 O8'
_chemical_formula_weight         616.12

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   '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                   9.0062(6)
_cell_length_b                   19.4623(14)
_cell_length_c                   16.0701(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.4420(10)
_cell_angle_gamma                90.00
_cell_volume                     2808.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      25.04

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1284
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_T_max  0.912
_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            14228
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.04
_reflns_number_total             4966
_reflns_number_gt                3445
_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)+(0.0615P)²+2.3080P] 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         4966
_refine_ls_number_parameters     370
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1306
_refine_ls_wR_factor_gt          0.1160
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.051
_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
Cu1 Cu -0.68577(5) 0.02798(2) 0.76174(3) 0.03018(17) Uani 1 1 d . . .
O1 O -0.4886(3) -0.00572(14) 0.74972(18) 0.0360(7) Uani 1 1 d . . .
N1 N -0.6032(3) 0.08360(16) 0.8631(2) 0.0321(8) Uani 1 1 d . . .
C1 C -0.6627(5) 0.1451(2) 0.8768(3) 0.0449(12) Uani 1 1 d . . .
H1A H -0.7467 0.1585 0.8434 0.054 Uiso 1 1 calc R . .
O1W O -0.6922(3) 0.12940(14) 0.68834(19) 0.0466(8) Uani 1 1 d . . .
H1WA H -0.7521 0.1481 0.6516 0.056 Uiso 1 1 d R . .
H1WB H -0.6045 0.1414 0.6786 0.056 Uiso 1 1 d R . .
O2 O -0.4092(3) 0.07797(16) 0.6704(2) 0.0522(8) Uani 1 1 d . . .
N2 N -0.2376(4) 0.47738(16) 0.8461(2) 0.0353(8) Uani 1 1 d . . .
C2 C -0.6068(5) 0.1892(2) 0.9370(3) 0.0432(11) Uani 1 1 d . . .
H2A H -0.6511 0.2318 0.9434 0.052 Uiso 1 1 calc R . .
O2W O -0.6736(5) 0.3804(3) 0.9797(3) 0.1214(19) Uani 1 1 d . . .
H2WA H -0.6124 0.3492 0.9965 0.146 Uiso 1 1 d R . .
H2WB H -0.7499 0.3732 1.0065 0.146 Uiso 1 1 d R . .
O3 O 0.1771(3) -0.05456(17) 0.8782(2) 0.0587(9) Uani 1 1 d . . .
C3 C -0.4832(4) 0.17015(19) 0.9890(3) 0.0320(9) Uani 1 1 d . . .
N3 N -0.3219(4) 0.19989(16) 1.1129(2) 0.0376(8) Uani 1 1 d . . .
H3A H -0.2798 0.1607 1.1070 0.045 Uiso 1 1 calc R . .
O4 O 0.1145(3) 0.03499(14) 0.79833(18) 0.0360(7) Uani 1 1 d . . .
N4 N -0.1716(4) 0.33306(17) 1.1069(2) 0.0389(9) Uani 1 1 d . . .
H4B H -0.2624 0.3463 1.0973 0.047 Uiso 1 1 calc R . .
C4 C -0.4236(5) 0.1063(2) 0.9765(3) 0.0407(11) Uani 1 1 d . . .
H4A H -0.3420 0.0910 1.0106 0.049 Uiso 1 1 calc R . .
O5 O -0.4778(3) 0.27964(14) 1.0540(2) 0.0482(8) Uani 1 1 d . . .
C5 C -0.4852(5) 0.0651(2) 0.9135(3) 0.0400(10) Uani 1 1 d . . .
H5A H -0.4426 0.0223 0.9055 0.048 Uiso 1 1 calc R . .
O6 O 0.0606(3) 0.34426(18) 1.0666(2) 0.0579(9) Uani 1 1 d . . .
C6 C -0.4263(4) 0.2212(2) 1.0547(3) 0.0352(10) Uani 1 1 d . . .
C7 C -0.2780(4) 0.2416(2) 1.1862(3) 0.0343(10) Uani 1 1 d . . .
H7A H -0.3602 0.2731 1.1948 0.041 Uiso 1 1 calc R . .
C8 C -0.2563(6) 0.1958(2) 1.2630(3) 0.0574(14) Uani 1 1 d . . .
H8A H -0.3475 0.1707 1.2699 0.069 Uiso 1 1 calc R . .
H8B H -0.1781 0.1627 1.2552 0.069 Uiso 1 1 calc R . .
C9 C -0.2151(7) 0.2381(3) 1.3409(3) 0.0694(16) Uani 1 1 d . . .
H9A H -0.2950 0.2700 1.3502 0.083 Uiso 1 1 calc R . .
H9B H -0.2016 0.2081 1.3890 0.083 Uiso 1 1 calc R . .
C10 C -0.0724(7) 0.2776(3) 1.3307(3) 0.0690(16) Uani 1 1 d . . .
H10A H -0.0467 0.3047 1.3803 0.083 Uiso 1 1 calc R . .
H10B H 0.0083 0.2456 1.3236 0.083 Uiso 1 1 calc R . .
C11 C -0.0927(6) 0.3242(2) 1.2556(3) 0.0527(13) Uani 1 1 d . . .
H11A H 0.0000 0.3481 1.2488 0.063 Uiso 1 1 calc R . .
H11B H -0.1679 0.3583 1.2653 0.063 Uiso 1 1 calc R . .
C12 C -0.1393(4) 0.2849(2) 1.1754(3) 0.0353(10) Uani 1 1 d . . .
H12A H -0.0577 0.2546 1.1618 0.042 Uiso 1 1 calc R . .
C13 C -0.0729(4) 0.3580(2) 1.0584(3) 0.0361(10) Uani 1 1 d . . .
C14 C -0.1335(5) 0.4037(2) 0.9882(3) 0.0358(10) Uani 1 1 d . . .
C15 C -0.0436(5) 0.4185(4) 0.9263(4) 0.096(2) Uani 1 1 d U . .
H15A H 0.0552 0.4041 0.9308 0.115 Uiso 1 1 calc R . .
C16 C -0.0988(6) 0.4546(4) 0.8570(4) 0.096(2) Uani 1 1 d U . .
H16A H -0.0350 0.4635 0.8155 0.115 Uiso 1 1 calc R . .
C17 C -0.3187(6) 0.4626(3) 0.9061(3) 0.079(2) Uani 1 1 d . . .
H17A H -0.4169 0.4777 0.9011 0.095 Uiso 1 1 calc R . .
C18 C -0.2728(6) 0.4263(3) 0.9772(3) 0.0738(18) Uani 1 1 d . . .
H18A H -0.3394 0.4176 1.0174 0.089 Uiso 1 1 calc R . .
C19 C -0.3907(4) 0.0240(2) 0.7095(2) 0.0321(9) Uani 1 1 d . . .
C20 C -0.2430(4) -0.0137(2) 0.7083(3) 0.0380(10) Uani 1 1 d . . .
H20A H -0.2304 -0.0280 0.6514 0.046 Uiso 1 1 calc R . .
H20B H -0.1633 0.0182 0.7246 0.046 Uiso 1 1 calc R . .
C21 C -0.2272(4) -0.0756(2) 0.7639(3) 0.0364(10) Uani 1 1 d . . .
C22 C -0.2938(5) -0.1367(2) 0.7349(4) 0.0538(13) Uani 1 1 d . . .
H22A H -0.3408 -0.1383 0.6813 0.065 Uiso 1 1 calc R . .
C23 C -0.2913(6) -0.1942(3) 0.7838(5) 0.0764(19) Uani 1 1 d . . .
H23A H -0.3365 -0.2344 0.7635 0.092 Uiso 1 1 calc R . .
C24 C -0.2222(6) -0.1927(3) 0.8629(5) 0.077(2) Uani 1 1 d . . .
H24A H -0.2220 -0.2315 0.8967 0.092 Uiso 1 1 calc R . .
C25 C -0.1534(5) -0.1336(3) 0.8919(4) 0.0638(15) Uani 1 1 d . . .
H25A H -0.1043 -0.1333 0.9450 0.077 Uiso 1 1 calc R . .
C26 C -0.1550(4) -0.0741(2) 0.8442(3) 0.0384(10) Uani 1 1 d . . .
C27 C -0.0730(5) -0.0112(2) 0.8782(3) 0.0466(12) Uani 1 1 d . . .
H27A H -0.0709 -0.0111 0.9386 0.056 Uiso 1 1 calc R . .
H27B H -0.1249 0.0298 0.8576 0.056 Uiso 1 1 calc R . .
C28 C 0.0870(4) -0.0105(2) 0.8513(3) 0.0351(10) 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
Cu1 O1 1.917(3) . ?
Cu1 O4 1.940(3) 1_455 ?
Cu1 N1 2.048(3) . ?
Cu1 N2 2.065(3) 2_446 ?
Cu1 O1W 2.298(3) . ?
O1 C19 1.273(5) . ?
N1 C5 1.333(5) . ?
N1 C1 1.337(5) . ?
C1 C2 1.360(6) . ?
O2 C19 1.228(5) . ?
N2 C17 1.286(6) . ?
N2 C16 1.326(6) . ?
N2 Cu1 2.065(3) 2_456 ?
C2 C3 1.389(5) . ?
O3 C28 1.235(5) . ?
C3 C4 1.375(5) . ?
C3 C6 1.510(5) . ?
N3 C6 1.341(5) . ?
N3 C7 1.458(5) . ?
O4 C28 1.266(5) . ?
O4 Cu1 1.940(3) 1_655 ?
N4 C13 1.319(5) . ?
N4 C12 1.458(5) . ?
C4 C5 1.375(6) . ?
O5 C6 1.228(5) . ?
O6 C13 1.228(5) . ?
C7 C8 1.522(6) . ?
C7 C12 1.528(5) . ?
C8 C9 1.521(7) . ?
C9 C10 1.517(7) . ?
C10 C11 1.508(6) . ?
C11 C12 1.529(6) . ?
C13 C14 1.504(5) . ?
C14 C18 1.328(6) . ?
C14 C15 1.362(7) . ?
C15 C16 1.377(7) . ?
C17 C18 1.379(7) . ?
C19 C20 1.520(5) . ?
C20 C21 1.501(6) . ?
C21 C22 1.396(6) . ?
C21 C26 1.399(6) . ?
C22 C23 1.367(8) . ?
C23 C24 1.371(9) . ?
C24 C25 1.371(8) . ?
C25 C26 1.389(6) . ?
C26 C27 1.510(6) . ?
C27 C28 1.536(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O4 160.48(12) . 1_455 ?
O1 Cu1 N1 88.79(12) . . ?
O4 Cu1 N1 90.57(12) 1_455 . ?
O1 Cu1 N2 90.24(13) . 2_446 ?
O4 Cu1 N2 91.75(12) 1_455 2_446 ?
N1 Cu1 N2 175.71(14) . 2_446 ?
O1 Cu1 O1W 103.24(11) . . ?
O4 Cu1 O1W 96.20(11) 1_455 . ?
N1 Cu1 O1W 86.99(12) . . ?
N2 Cu1 O1W 89.17(12) 2_446 . ?
C19 O1 Cu1 125.4(3) . . ?
C5 N1 C1 116.9(3) . . ?
C5 N1 Cu1 124.3(3) . . ?
C1 N1 Cu1 118.6(3) . . ?
N1 C1 C2 123.3(4) . . ?
C17 N2 C16 114.2(4) . . ?
C17 N2 Cu1 124.3(3) . 2_456 ?
C16 N2 Cu1 121.4(3) . 2_456 ?
C1 C2 C3 119.7(4) . . ?
C4 C3 C2 117.2(4) . . ?
C4 C3 C6 125.6(3) . . ?
C2 C3 C6 117.2(3) . . ?
C6 N3 C7 121.6(3) . . ?
C28 O4 Cu1 112.9(2) . 1_655 ?
C13 N4 C12 125.4(3) . . ?
C5 C4 C3 119.6(4) . . ?
N1 C5 C4 123.2(4) . . ?
O5 C6 N3 122.4(4) . . ?
O5 C6 C3 119.8(4) . . ?
N3 C6 C3 117.8(3) . . ?
N3 C7 C8 109.8(3) . . ?
N3 C7 C12 112.9(3) . . ?
C8 C7 C12 111.1(3) . . ?
C9 C8 C7 111.0(4) . . ?
C10 C9 C8 109.9(5) . . ?
C11 C10 C9 109.8(4) . . ?
C10 C11 C12 112.5(4) . . ?
N4 C12 C7 108.9(3) . . ?
N4 C12 C11 110.0(3) . . ?
C7 C12 C11 110.7(4) . . ?
O6 C13 N4 123.7(4) . . ?
O6 C13 C14 120.3(4) . . ?
N4 C13 C14 116.0(4) . . ?
C18 C14 C15 116.1(4) . . ?
C18 C14 C13 125.5(4) . . ?
C15 C14 C13 118.1(4) . . ?
C14 C15 C16 120.1(5) . . ?
N2 C16 C15 123.7(5) . . ?
N2 C17 C18 125.8(4) . . ?
C14 C18 C17 120.0(5) . . ?
O2 C19 O1 125.2(4) . . ?
O2 C19 C20 119.4(4) . . ?
O1 C19 C20 115.4(4) . . ?
C21 C20 C19 115.0(3) . . ?
C22 C21 C26 118.9(4) . . ?
C22 C21 C20 117.7(4) . . ?
C26 C21 C20 123.3(4) . . ?
C23 C22 C21 121.1(5) . . ?
C22 C23 C24 120.1(5) . . ?
C25 C24 C23 119.6(5) . . ?
C24 C25 C26 121.8(6) . . ?
C25 C26 C21 118.4(4) . . ?
C25 C26 C27 119.5(5) . . ?
C21 C26 C27 122.0(4) . . ?
C26 C27 C28 110.4(3) . . ?
O3 C28 O4 124.2(4) . . ?
O3 C28 C27 120.1(4) . . ?
O4 C28 C27 115.6(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.068
####################################################################### 
# 
# 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 1479974'
_audit_update_record             
;
2016-05-15 deposited with the CCDC.
2016-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H58 N8 Ni2 O13'
_chemical_formula_weight         1168.52

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           Orthorhombic
_symmetry_space_group_name_H-M   'P b c n'

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

_cell_length_a                   18.4470(2)
_cell_length_b                   21.0140(3)
_cell_length_c                   28.7750(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11154.5(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.42
_cell_measurement_theta_max      25.21

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4880
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_T_max  0.921
_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            55277
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         25.21
_reflns_number_total             10023
_reflns_number_gt                6200
_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)+(0.0576P)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         10023
_refine_ls_number_parameters     712
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1240
_refine_ls_wR_factor_gt          0.1084
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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 0.09088(2) 0.26001(2) -0.055312(14) 0.03153(13) Uani 1 1 d . . .
N1 N 0.06404(15) 0.32418(14) -0.10956(9) 0.0345(7) Uani 1 1 d . . .
O1 O -0.00284(12) 0.21066(12) -0.06929(8) 0.0408(6) Uani 1 1 d . . .
C1 C 0.0106(2) 0.31468(18) -0.13969(14) 0.0512(11) Uani 1 1 d . . .
H1A H -0.0100 0.2744 -0.1415 0.061 Uiso 1 1 calc R . .
O1W O 0.11563(12) 0.20537(10) 0.00285(7) 0.0335(6) Uani 1 1 d . . .
H1WA H 0.0940 0.1876 0.0255 0.040 Uiso 1 1 d R . .
H1WB H 0.1609 0.2041 0.0083 0.040 Uiso 1 1 d R . .
Ni2 Ni -0.35787(2) 0.24268(2) -0.063641(14) 0.02977(13) Uani 1 1 d . . .
N2 N -0.41486(16) 0.30961(14) -0.10604(10) 0.0361(7) Uani 1 1 d . . .
O2 O -0.00930(15) 0.15032(15) -0.00594(10) 0.0677(9) Uani 1 1 d . . .
C2 C -0.0157(2) 0.36162(19) -0.16831(16) 0.0622(13) Uani 1 1 d . . .
H2A H -0.0525 0.3523 -0.1894 0.075 Uiso 1 1 calc R . .
O3 O -0.29209(13) 0.18179(11) -0.02669(8) 0.0386(6) Uani 1 1 d . . .
N3 N -0.32476(16) 0.18470(14) -0.11985(9) 0.0337(7) Uani 1 1 d . . .
C3 C 0.01198(19) 0.42252(17) -0.16604(12) 0.0363(9) Uani 1 1 d . . .
O4 O -0.31347(12) 0.19321(11) 0.04979(8) 0.0366(6) Uani 1 1 d . . .
N4 N -0.15071(16) 0.18974(15) -0.40432(10) 0.0386(8) Uani 1 1 d . . .
C4 C 0.0676(2) 0.43229(19) -0.13478(13) 0.0467(11) Uani 1 1 d . . .
H4A H 0.0888 0.4723 -0.1319 0.056 Uiso 1 1 calc R . .
O5 O -0.45238(12) 0.19396(11) -0.05927(8) 0.0374(6) Uani 1 1 d . . .
N5 N 0.01558(17) 0.52883(14) -0.19934(11) 0.0452(9) Uani 1 1 d . . .
H5B H 0.0576 0.5313 -0.1865 0.054 Uiso 1 1 calc R . .
C5 C 0.0912(2) 0.38286(19) -0.10816(13) 0.0488(11) Uani 1 1 d . . .
H5A H 0.1291 0.3906 -0.0875 0.059 Uiso 1 1 calc R . .
O6 O -0.47329(13) 0.17937(11) 0.01676(8) 0.0400(6) Uani 1 1 d . . .
N6 N -0.48452(18) 0.50372(16) -0.20050(12) 0.0543(10) Uani 1 1 d . . .
H6A H -0.4382 0.5008 -0.1980 0.065 Uiso 1 1 calc R . .
C6 C -0.0211(2) 0.47451(19) -0.19521(14) 0.0429(10) Uani 1 1 d . . .
O7 O -0.75142(13) 0.16980(12) 0.00099(9) 0.0451(7) Uani 1 1 d . . .
N7 N -0.27090(17) -0.00769(14) -0.22105(10) 0.0436(8) Uani 1 1 d . . .
H7C H -0.3169 -0.0033 -0.2177 0.052 Uiso 1 1 calc R . .
C7 C -0.0115(2) 0.58476(16) -0.22454(13) 0.0489(11) Uani 1 1 d . . .
H7A H -0.0646 0.5846 -0.2232 0.059 Uiso 1 1 calc R . .
O8 O -0.76486(12) 0.20392(12) 0.07367(8) 0.0394(6) Uani 1 1 d . . .
N8 N -0.23764(16) -0.00840(15) -0.32033(10) 0.0440(8) Uani 1 1 d . . .
H8C H -0.1921 -0.0103 -0.3265 0.053 Uiso 1 1 calc R . .
C8 C 0.0160(3) 0.64483(18) -0.20034(16) 0.0640(13) Uani 1 1 d . . .
H8A H 0.0686 0.6446 -0.2002 0.077 Uiso 1 1 calc R . .
H8B H -0.0004 0.6449 -0.1683 0.077 Uiso 1 1 calc R . .
O9 O -0.08141(15) 0.46602(13) -0.21270(11) 0.0623(9) Uani 1 1 d . . .
C9 C -0.0109(3) 0.70513(19) -0.22455(16) 0.0840(18) Uani 1 1 d . . .
H9A H -0.0633 0.7076 -0.2221 0.101 Uiso 1 1 calc R . .
H9B H 0.0094 0.7422 -0.2093 0.101 Uiso 1 1 calc R . .
O10 O -0.59047(15) 0.45566(14) -0.18457(11) 0.0685(9) Uani 1 1 d . . .
C10 C -0.5144(4) 0.6782(2) -0.22562(18) 0.126(3) Uani 1 1 d . . .
H10A H -0.4974 0.7159 -0.2095 0.151 Uiso 1 1 calc R . .
H10B H -0.5670 0.6797 -0.2265 0.151 Uiso 1 1 calc R . .
O11 O -0.16244(16) 0.03780(14) -0.20825(12) 0.0713(10) Uani 1 1 d . . .
C11 C -0.4907(3) 0.6200(2) -0.19952(16) 0.0737(15) Uani 1 1 d . . .
H11A H -0.5120 0.6204 -0.1687 0.088 Uiso 1 1 calc R . .
H11B H -0.4384 0.6205 -0.1961 0.088 Uiso 1 1 calc R . .
O12 O -0.33734(14) 0.05313(13) -0.32650(10) 0.0572(8) Uani 1 1 d . . .
C12 C -0.5136(2) 0.55911(17) -0.22501(13) 0.0487(11) Uani 1 1 d . . .
H12A H -0.5667 0.5565 -0.2252 0.058 Uiso 1 1 calc R . .
C13 C -0.5241(2) 0.45768(19) -0.18188(14) 0.0428(10) Uani 1 1 d . . .
C14 C -0.4838(2) 0.40522(18) -0.15699(13) 0.0396(9) Uani 1 1 d . . .
C15 C -0.5204(2) 0.3672(2) -0.12678(17) 0.0739(16) Uani 1 1 d . . .
H15A H -0.5700 0.3727 -0.1226 0.089 Uiso 1 1 calc R . .
C16 C -0.4843(2) 0.3208(2) -0.10234(16) 0.0692(15) Uani 1 1 d . . .
H16A H -0.5110 0.2958 -0.0819 0.083 Uiso 1 1 calc R . .
C17 C -0.3804(2) 0.3458(2) -0.13527(18) 0.0838(19) Uani 1 1 d . . .
H17A H -0.3310 0.3389 -0.1391 0.101 Uiso 1 1 calc R . .
C18 C -0.4122(2) 0.3936(2) -0.16096(19) 0.0881(19) Uani 1 1 d . . .
H18A H -0.3842 0.4180 -0.1811 0.106 Uiso 1 1 calc R . .
C19 C -0.3565(2) 0.1282(2) -0.12539(13) 0.0491(11) Uani 1 1 d . . .
H19A H -0.4001 0.1211 -0.1101 0.059 Uiso 1 1 calc R . .
C20 C -0.3288(2) 0.07986(19) -0.15225(14) 0.0519(11) Uani 1 1 d . . .
H20A H -0.3531 0.0412 -0.1543 0.062 Uiso 1 1 calc R . .
C21 C -0.2650(2) 0.08894(18) -0.17598(12) 0.0367(9) Uani 1 1 d . . .
C22 C -0.2325(2) 0.14732(19) -0.17138(14) 0.0513(11) Uani 1 1 d . . .
H22A H -0.1898 0.1561 -0.1873 0.062 Uiso 1 1 calc R . .
C23 C -0.2633(2) 0.19290(19) -0.14321(14) 0.0508(11) Uani 1 1 d . . .
H23A H -0.2396 0.2318 -0.1403 0.061 Uiso 1 1 calc R . .
C24 C -0.2284(2) 0.03676(19) -0.20350(13) 0.0416(10) Uani 1 1 d . . .
C25 C -0.2449(2) -0.06394(17) -0.24591(12) 0.0387(9) Uani 1 1 d . . .
H25A H -0.1917 -0.0640 -0.2452 0.046 Uiso 1 1 calc R . .
C26 C -0.2722(2) -0.12336(18) -0.22090(14) 0.0561(12) Uani 1 1 d . . .
H26A H -0.3247 -0.1218 -0.2189 0.067 Uiso 1 1 calc R . .
H26B H -0.2531 -0.1240 -0.1895 0.067 Uiso 1 1 calc R . .
C27 C -0.2495(3) -0.1842(2) -0.24603(17) 0.0795(16) Uani 1 1 d . . .
H27A H -0.1971 -0.1879 -0.2458 0.095 Uiso 1 1 calc R . .
H27B H -0.2695 -0.2209 -0.2301 0.095 Uiso 1 1 calc R . .
C28 C -0.2767(3) -0.1828(2) -0.29591(17) 0.0781(15) Uani 1 1 d . . .
H28A H -0.2606 -0.2208 -0.3120 0.094 Uiso 1 1 calc R . .
H28B H -0.3293 -0.1825 -0.2960 0.094 Uiso 1 1 calc R . .
C29 C -0.2488(2) -0.12451(19) -0.32102(14) 0.0585(12) Uani 1 1 d . . .
H29A H -0.2680 -0.1241 -0.3524 0.070 Uiso 1 1 calc R . .
H29B H -0.1963 -0.1269 -0.3231 0.070 Uiso 1 1 calc R . .
C30 C -0.2699(2) -0.06268(17) -0.29658(12) 0.0399(9) Uani 1 1 d . . .
H30A H -0.3227 -0.0583 -0.2973 0.048 Uiso 1 1 calc R . .
C31 C -0.2729(2) 0.04405(18) -0.33330(13) 0.0401(9) Uani 1 1 d . . .
C32 C -0.2277(2) 0.09407(18) -0.35810(12) 0.0375(9) Uani 1 1 d . . .
C33 C -0.1610(2) 0.0827(2) -0.37656(18) 0.0772(17) Uani 1 1 d . . .
H33A H -0.1401 0.0425 -0.3741 0.093 Uiso 1 1 calc R . .
C34 C -0.1246(2) 0.1311(2) -0.39899(17) 0.0747(16) Uani 1 1 d . . .
H34A H -0.0790 0.1222 -0.4111 0.090 Uiso 1 1 calc R . .
C35 C -0.2164(2) 0.1985(2) -0.38853(16) 0.0616(13) Uani 1 1 d . . .
H35A H -0.2376 0.2382 -0.3929 0.074 Uiso 1 1 calc R . .
C36 C -0.2560(2) 0.1528(2) -0.36590(16) 0.0606(13) Uani 1 1 d . . .
H36A H -0.3027 0.1621 -0.3558 0.073 Uiso 1 1 calc R . .
C37 C -0.0343(2) 0.1714(2) -0.04299(14) 0.0428(10) Uani 1 1 d . . .
C38 C -0.1085(2) 0.1484(2) -0.06032(14) 0.0538(12) Uani 1 1 d . . .
H38A H -0.1428 0.1830 -0.0567 0.065 Uiso 1 1 calc R . .
H38B H -0.1046 0.1396 -0.0933 0.065 Uiso 1 1 calc R . .
C39 C -0.1389(2) 0.09110(19) -0.03724(15) 0.0477(11) Uani 1 1 d . . .
C40 C -0.1246(3) 0.0303(3) -0.0563(2) 0.0900(18) Uani 1 1 d . . .
H40A H -0.0968 0.0271 -0.0832 0.108 Uiso 1 1 calc R . .
C41 C -0.1512(4) -0.0244(3) -0.0358(3) 0.116(3) Uani 1 1 d . . .
H41A H -0.1435 -0.0639 -0.0496 0.139 Uiso 1 1 calc R . .
C42 C -0.1885(4) -0.0200(3) 0.0047(3) 0.111(2) Uani 1 1 d . . .
H42A H -0.2048 -0.0568 0.0193 0.134 Uiso 1 1 calc R . .
C43 C -0.2025(3) 0.0378(2) 0.0241(2) 0.0799(16) Uani 1 1 d . . .
H43A H -0.2284 0.0399 0.0518 0.096 Uiso 1 1 calc R . .
C44 C -0.1788(2) 0.09315(18) 0.00345(14) 0.0443(10) Uani 1 1 d . . .
C45 C -0.1987(2) 0.1546(2) 0.02684(14) 0.0521(11) Uani 1 1 d . . .
H45A H -0.1640 0.1870 0.0178 0.063 Uiso 1 1 calc R . .
H45B H -0.1950 0.1490 0.0602 0.063 Uiso 1 1 calc R . .
C46 C -0.27513(19) 0.17809(16) 0.01520(13) 0.0341(9) Uani 1 1 d . . .
C47 C -0.49074(19) 0.17691(17) -0.02510(13) 0.0344(9) Uani 1 1 d . . .
C48 C -0.5659(2) 0.1515(2) -0.03683(14) 0.0570(12) Uani 1 1 d . . .
H48A H -0.6007 0.1853 -0.0317 0.068 Uiso 1 1 calc R . .
H48B H -0.5669 0.1412 -0.0697 0.068 Uiso 1 1 calc R . .
C49 C -0.59051(19) 0.09428(19) -0.01040(14) 0.0420(10) Uani 1 1 d . . .
C50 C -0.5752(2) 0.0350(3) -0.0283(2) 0.0749(16) Uani 1 1 d . . .
H50A H -0.5496 0.0322 -0.0561 0.090 Uiso 1 1 calc R . .
C51 C -0.5961(4) -0.0195(3) -0.0067(3) 0.111(3) Uani 1 1 d . . .
H51A H -0.5844 -0.0588 -0.0196 0.134 Uiso 1 1 calc R . .
C52 C -0.6333(4) -0.0168(3) 0.0327(3) 0.109(3) Uani 1 1 d . . .
H52A H -0.6484 -0.0541 0.0471 0.131 Uiso 1 1 calc R . .
C53 C -0.6494(3) 0.0412(3) 0.05218(18) 0.0740(15) Uani 1 1 d . . .
H53A H -0.6751 0.0426 0.0800 0.089 Uiso 1 1 calc R . .
C54 C -0.62829(19) 0.09784(18) 0.03131(14) 0.0388(9) Uani 1 1 d . . .
C55 C -0.6512(2) 0.1596(2) 0.05328(14) 0.0507(11) Uani 1 1 d . . .
H55A H -0.6183 0.1930 0.0434 0.061 Uiso 1 1 calc R . .
H55B H -0.6472 0.1558 0.0868 0.061 Uiso 1 1 calc R . .
C56 C -0.72813(19) 0.17864(16) 0.04090(14) 0.0355(9) 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 O4 2.026(2) 3 ?
Ni1 O1 2.056(2) . ?
Ni1 O6 2.063(2) 3 ?
Ni1 O1W 2.080(2) . ?
Ni1 N1 2.121(3) . ?
Ni1 N4 2.179(3) 4_554 ?
N1 C1 1.328(4) . ?
N1 C5 1.332(4) . ?
O1 C37 1.261(4) . ?
C1 C2 1.374(5) . ?
O1W Ni2 2.119(2) 3 ?
Ni2 O5 2.026(2) . ?
Ni2 O3 2.059(2) . ?
Ni2 O8 2.070(2) 3 ?
Ni2 N3 2.115(3) . ?
Ni2 O1W 2.119(2) 3_455 ?
Ni2 N2 2.138(3) . ?
N2 C17 1.300(5) . ?
N2 C16 1.307(5) . ?
O2 C37 1.243(4) . ?
C2 C3 1.379(5) . ?
O3 C46 1.248(4) . ?
N3 C23 1.330(4) . ?
N3 C19 1.332(4) . ?
C3 C4 1.380(5) . ?
C3 C6 1.507(5) . ?
O4 C46 1.262(4) . ?
O4 Ni1 2.026(2) 3_455 ?
N4 C35 1.308(5) . ?
N4 C34 1.332(5) . ?
N4 Ni1 2.179(3) 4_554 ?
C4 C5 1.363(5) . ?
O5 C47 1.263(4) . ?
N5 C6 1.333(5) . ?
N5 C7 1.469(4) . ?
O6 C47 1.248(4) . ?
O6 Ni1 2.063(2) 3_455 ?
N6 C13 1.325(5) . ?
N6 C12 1.463(4) . ?
C6 O9 1.233(4) . ?
O7 C56 1.240(4) . ?
N7 C24 1.320(5) . ?
N7 C25 1.463(4) . ?
C7 C7 1.526(8) 4_554 ?
C7 C8 1.529(5) . ?
O8 C56 1.277(4) . ?
O8 Ni2 2.070(2) 3_455 ?
N8 C31 1.333(4) . ?
N8 C30 1.457(4) . ?
C8 C9 1.529(5) . ?
C9 C9 1.519(10) 4_554 ?
O10 C13 1.228(4) . ?
C10 C11 1.501(6) . ?
C10 C10 1.501(12) 4_454 ?
O11 C24 1.224(4) . ?
C11 C12 1.535(5) . ?
O12 C31 1.220(4) . ?
C12 C12 1.523(8) 4_454 ?
C13 C14 1.510(5) . ?
C14 C18 1.347(5) . ?
C14 C15 1.360(5) . ?
C15 C16 1.374(5) . ?
C17 C18 1.380(6) . ?
C19 C20 1.375(5) . ?
C20 C21 1.373(5) . ?
C21 C22 1.372(5) . ?
C21 C24 1.512(5) . ?
C22 C23 1.377(5) . ?
C25 C26 1.527(5) . ?
C25 C30 1.529(5) . ?
C26 C27 1.528(6) . ?
C27 C28 1.521(6) . ?
C28 C29 1.513(6) . ?
C29 C30 1.528(5) . ?
C31 C32 1.519(5) . ?
C32 C36 1.359(5) . ?
C32 C33 1.362(5) . ?
C33 C34 1.379(5) . ?
C35 C36 1.370(5) . ?
C37 C38 1.534(5) . ?
C38 C39 1.486(6) . ?
C39 C44 1.384(5) . ?
C39 C40 1.415(6) . ?
C40 C41 1.383(8) . ?
C41 C42 1.356(9) . ?
C42 C43 1.361(7) . ?
C43 C44 1.377(5) . ?
C44 C45 1.501(5) . ?
C45 C46 1.531(5) . ?
C47 C48 1.524(5) . ?
C48 C49 1.493(5) . ?
C49 C50 1.377(6) . ?
C49 C54 1.390(5) . ?
C50 C51 1.360(8) . ?
C51 C52 1.326(9) . ?
C52 C53 1.374(8) . ?
C53 C54 1.389(6) . ?
C54 C55 1.504(5) . ?
C55 C56 1.517(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 O1 172.98(10) 3 . ?
O4 Ni1 O6 99.09(10) 3 3 ?
O1 Ni1 O6 86.22(10) . 3 ?
O4 Ni1 O1W 90.78(9) 3 . ?
O1 Ni1 O1W 93.65(9) . . ?
O6 Ni1 O1W 91.96(9) 3 . ?
O4 Ni1 N1 87.28(10) 3 . ?
O1 Ni1 N1 88.87(11) . . ?
O6 Ni1 N1 82.48(10) 3 . ?
O1W Ni1 N1 173.74(10) . . ?
O4 Ni1 N4 85.96(11) 3 4_554 ?
O1 Ni1 N4 88.84(11) . 4_554 ?
O6 Ni1 N4 174.82(11) 3 4_554 ?
O1W Ni1 N4 86.77(10) . 4_554 ?
N1 Ni1 N4 99.02(11) . 4_554 ?
C1 N1 C5 116.0(3) . . ?
C1 N1 Ni1 123.9(3) . . ?
C5 N1 Ni1 118.6(2) . . ?
C37 O1 Ni1 126.8(2) . . ?
N1 C1 C2 123.1(4) . . ?
Ni1 O1W Ni2 115.50(10) . 3 ?
O5 Ni2 O3 99.27(10) . . ?
O5 Ni2 O8 174.75(10) . 3 ?
O3 Ni2 O8 85.44(10) . 3 ?
O5 Ni2 N3 90.28(10) . . ?
O3 Ni2 N3 82.35(10) . . ?
O8 Ni2 N3 88.07(11) 3 . ?
O5 Ni2 O1W 90.60(9) . 3_455 ?
O3 Ni2 O1W 91.70(9) . 3_455 ?
O8 Ni2 O1W 91.56(9) 3 3_455 ?
N3 Ni2 O1W 174.05(10) . 3_455 ?
O5 Ni2 N2 86.82(11) . . ?
O3 Ni2 N2 173.27(10) . . ?
O8 Ni2 N2 88.36(10) 3 . ?
N3 Ni2 N2 94.85(11) . . ?
O1W Ni2 N2 91.08(10) 3_455 . ?
C17 N2 C16 115.3(4) . . ?
C17 N2 Ni2 120.9(3) . . ?
C16 N2 Ni2 123.6(3) . . ?
C1 C2 C3 120.5(4) . . ?
C46 O3 Ni2 133.3(2) . . ?
C23 N3 C19 115.4(3) . . ?
C23 N3 Ni2 123.9(3) . . ?
C19 N3 Ni2 118.5(2) . . ?
C2 C3 C4 116.4(4) . . ?
C2 C3 C6 119.7(3) . . ?
C4 C3 C6 123.8(3) . . ?
C46 O4 Ni1 132.2(2) . 3_455 ?
C35 N4 C34 115.2(3) . . ?
C35 N4 Ni1 124.0(3) . 4_554 ?
C34 N4 Ni1 120.3(3) . 4_554 ?
C5 C4 C3 119.4(4) . . ?
C47 O5 Ni2 132.3(2) . . ?
C6 N5 C7 123.8(3) . . ?
N1 C5 C4 124.6(4) . . ?
C47 O6 Ni1 133.8(2) . 3_455 ?
C13 N6 C12 125.0(3) . . ?
O9 C6 N5 123.1(4) . . ?
O9 C6 C3 119.2(4) . . ?
N5 C6 C3 117.7(3) . . ?
C24 N7 C25 124.3(3) . . ?
N5 C7 C7 112.3(3) . 4_554 ?
N5 C7 C8 108.8(3) . . ?
C7 C7 C8 110.2(3) 4_554 . ?
C56 O8 Ni2 124.2(2) . 3_455 ?
C31 N8 C30 125.4(3) . . ?
C7 C8 C9 111.6(3) . . ?
C9 C9 C8 110.7(4) 4_554 . ?
C11 C10 C10 111.4(5) . 4_454 ?
C10 C11 C12 111.1(4) . . ?
N6 C12 C12 109.5(3) . 4_454 ?
N6 C12 C11 109.4(3) . . ?
C12 C12 C11 111.1(3) 4_454 . ?
O10 C13 N6 123.3(4) . . ?
O10 C13 C14 119.7(4) . . ?
N6 C13 C14 117.0(3) . . ?
C18 C14 C15 115.8(4) . . ?
C18 C14 C13 125.0(4) . . ?
C15 C14 C13 119.2(4) . . ?
C14 C15 C16 120.2(4) . . ?
N2 C16 C15 124.1(4) . . ?
N2 C17 C18 124.4(4) . . ?
C14 C18 C17 120.2(4) . . ?
N3 C19 C20 124.3(4) . . ?
C21 C20 C19 119.6(4) . . ?
C22 C21 C20 116.8(3) . . ?
C22 C21 C24 120.2(3) . . ?
C20 C21 C24 122.9(4) . . ?
C21 C22 C23 119.9(4) . . ?
N3 C23 C22 124.0(4) . . ?
O11 C24 N7 124.1(4) . . ?
O11 C24 C21 119.3(4) . . ?
N7 C24 C21 116.6(3) . . ?
N7 C25 C26 108.8(3) . . ?
N7 C25 C30 110.7(3) . . ?
C26 C25 C30 111.3(3) . . ?
C25 C26 C27 111.8(3) . . ?
C28 C27 C26 109.8(4) . . ?
C29 C28 C27 110.8(4) . . ?
C28 C29 C30 112.4(3) . . ?
N8 C30 C29 110.2(3) . . ?
N8 C30 C25 109.7(3) . . ?
C29 C30 C25 110.3(3) . . ?
O12 C31 N8 124.0(4) . . ?
O12 C31 C32 120.1(4) . . ?
N8 C31 C32 115.9(3) . . ?
C36 C32 C33 116.3(4) . . ?
C36 C32 C31 119.7(3) . . ?
C33 C32 C31 123.9(4) . . ?
C32 C33 C34 119.5(4) . . ?
N4 C34 C33 124.1(4) . . ?
N4 C35 C36 124.1(4) . . ?
C32 C36 C35 120.7(4) . . ?
O2 C37 O1 125.2(4) . . ?
O2 C37 C38 119.8(4) . . ?
O1 C37 C38 114.9(4) . . ?
C39 C38 C37 116.5(4) . . ?
C44 C39 C40 117.1(4) . . ?
C44 C39 C38 123.6(4) . . ?
C40 C39 C38 119.2(4) . . ?
C41 C40 C39 121.3(6) . . ?
C42 C41 C40 119.3(6) . . ?
C41 C42 C43 120.7(6) . . ?
C42 C43 C44 121.1(6) . . ?
C43 C44 C39 120.5(4) . . ?
C43 C44 C45 117.1(4) . . ?
C39 C44 C45 122.4(4) . . ?
C44 C45 C46 113.9(3) . . ?
O3 C46 O4 127.3(3) . . ?
O3 C46 C45 117.6(3) . . ?
O4 C46 C45 115.1(3) . . ?
O6 C47 O5 126.5(3) . . ?
O6 C47 C48 117.6(3) . . ?
O5 C47 C48 115.9(3) . . ?
C49 C48 C47 116.5(3) . . ?
C50 C49 C54 118.3(4) . . ?
C50 C49 C48 118.4(4) . . ?
C54 C49 C48 123.3(4) . . ?
C51 C50 C49 122.2(6) . . ?
C52 C51 C50 120.0(6) . . ?
C51 C52 C53 119.9(6) . . ?
C52 C53 C54 121.5(6) . . ?
C53 C54 C49 117.9(4) . . ?
C53 C54 C55 118.6(4) . . ?
C49 C54 C55 123.4(4) . . ?
C54 C55 C56 113.0(3) . . ?
O7 C56 O8 124.2(3) . . ?
O7 C56 C55 120.1(3) . . ?
O8 C56 C55 115.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.21
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.421
_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-5
_database_code_depnum_ccdc_archive 'CCDC 1479975'
_audit_update_record             
;
2016-05-15 deposited with the CCDC.
2016-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H34 Cu3 N4 O12'
_chemical_formula_weight         905.29

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   5.7315(19)
_cell_length_b                   8.915(3)
_cell_length_c                   18.554(6)
_cell_angle_alpha                76.760(6)
_cell_angle_beta                 81.312(6)
_cell_angle_gamma                82.111(6)
_cell_volume                     907.0(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.14
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             461
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.776
_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            4639
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0948
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3176
_reflns_number_gt                2398
_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)+(0.1706P)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         3176
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0855
_refine_ls_wR_factor_ref         0.2399
_refine_ls_wR_factor_gt          0.2207
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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 -0.01873(14) 0.57981(9) 0.42031(4) 0.0206(3) Uani 1 1 d . . .
C1 C 0.1035(17) 0.7031(11) 0.2576(5) 0.046(2) Uani 1 1 d . . .
H1A H -0.0400 0.7643 0.2637 0.056 Uiso 1 1 calc R . .
O1 O 0.4123(9) 0.7030(6) 0.4377(3) 0.0289(12) Uani 1 1 d . . .
N1 N 0.1784(11) 0.6029(7) 0.3162(3) 0.0257(13) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.5000 0.5000 0.0221(4) Uani 1 2 d S . .
O2 O 0.7716(9) 0.7593(6) 0.3791(3) 0.0283(12) Uani 1 1 d . . .
C2 C 0.2305(19) 0.7189(12) 0.1884(5) 0.055(3) Uani 1 1 d . . .
H2A H 0.1738 0.7918 0.1488 0.066 Uiso 1 1 calc R . .
N2 N 0.5215(17) 0.5927(11) 0.0487(4) 0.064(3) Uani 1 1 d . . .
O3 O 0.8006(9) 1.3837(5) 0.4059(3) 0.0273(12) Uani 1 1 d . . .
C3 C 0.4434(15) 0.6277(10) 0.1765(4) 0.0368(19) Uani 1 1 d . . .
O4 O 1.1013(10) 1.2050(6) 0.4362(4) 0.0393(14) Uani 1 1 d . . .
C4 C 0.5206(17) 0.5272(12) 0.2376(5) 0.049(2) Uani 1 1 d . . .
H4A H 0.6651 0.4662 0.2332 0.059 Uiso 1 1 calc R . .
O5 O 0.7569(15) 0.7241(12) 0.0889(4) 0.081(3) Uani 1 1 d . . .
C5 C 0.3851(16) 0.5165(11) 0.3052(5) 0.043(2) Uani 1 1 d . . .
H5A H 0.4393 0.4454 0.3458 0.051 Uiso 1 1 calc R . .
O6 O 0.2083(8) 0.4379(5) 0.4794(3) 0.0194(10) Uani 1 1 d . . .
H6A H 0.2348 0.3410 0.4810 0.023 Uiso 1 1 d R . .
C6 C 0.5877(18) 0.6510(12) 0.1007(5) 0.049(2) Uani 1 1 d . . .
C7 C 0.645(2) 0.6241(16) -0.0277(6) 0.075(4) Uani 1 1 d . . .
H7A H 0.5464 0.6999 -0.0597 0.091 Uiso 1 1 calc R . .
H7B H 0.7917 0.6670 -0.0280 0.091 Uiso 1 1 calc R . .
C8 C 0.696(2) 0.4850(18) -0.0558(7) 0.090(5) Uani 1 1 d . . .
H8A H 0.8130 0.4152 -0.0283 0.108 Uiso 1 1 calc R . .
H8B H 0.7622 0.5097 -0.1079 0.108 Uiso 1 1 calc R . .
C9 C 0.5518(13) 0.7907(8) 0.3934(4) 0.0221(15) Uani 1 1 d . . .
C10 C 0.4393(13) 0.9473(8) 0.3526(4) 0.0252(16) Uani 1 1 d . . .
H10A H 0.3167 0.9298 0.3256 0.030 Uiso 1 1 calc R . .
H10B H 0.3647 1.0074 0.3890 0.030 Uiso 1 1 calc R . .
C11 C 0.6161(14) 1.0372(8) 0.2995(4) 0.0285(17) Uani 1 1 d . . .
C12 C 0.6380(16) 1.0344(9) 0.2244(5) 0.039(2) Uani 1 1 d . . .
H12A H 0.5313 0.9835 0.2081 0.046 Uiso 1 1 calc R . .
C13 C 0.8139(19) 1.1049(11) 0.1722(5) 0.052(2) Uani 1 1 d . . .
H13A H 0.8230 1.1026 0.1220 0.062 Uiso 1 1 calc R . .
C14 C 0.9727(19) 1.1775(11) 0.1965(5) 0.049(2) Uani 1 1 d . . .
H14A H 1.0947 1.2218 0.1630 0.059 Uiso 1 1 calc R . .
C15 C 0.9523(16) 1.1855(9) 0.2715(5) 0.040(2) Uani 1 1 d . . .
H15A H 1.0594 1.2374 0.2870 0.048 Uiso 1 1 calc R . .
C16 C 0.7765(14) 1.1179(8) 0.3234(4) 0.0280(16) Uani 1 1 d . . .
C17 C 0.7602(14) 1.1233(8) 0.4043(4) 0.0276(16) Uani 1 1 d . . .
H17A H 0.8199 1.0228 0.4319 0.033 Uiso 1 1 calc R . .
H17B H 0.5948 1.1439 0.4236 0.033 Uiso 1 1 calc R . .
C18 C 0.8990(13) 1.2462(8) 0.4173(4) 0.0262(16) 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
Cu1 O2 1.944(5) 1_455 ?
Cu1 O6 1.960(4) . ?
Cu1 O6 1.993(5) 2_566 ?
Cu1 N1 2.067(6) . ?
Cu1 O3 2.235(5) 1_445 ?
Cu1 Cu1 2.9995(18) 2_566 ?
Cu1 Cu2 3.0209(11) 1_455 ?
C1 N1 1.326(10) . ?
C1 C2 1.363(13) . ?
O1 C9 1.267(8) . ?
O1 Cu2 1.957(5) . ?
N1 C5 1.337(11) . ?
Cu2 O6 1.947(4) 2_666 ?
Cu2 O6 1.947(4) . ?
Cu2 O1 1.957(5) 2_666 ?
Cu2 Cu1 3.0209(12) 2_566 ?
Cu2 Cu1 3.0210(11) 1_655 ?
O2 C9 1.253(9) . ?
O2 Cu1 1.944(5) 1_655 ?
C2 C3 1.388(13) . ?
N2 C6 1.319(12) . ?
N2 C7 1.468(12) . ?
N2 C8 1.482(14) 2_665 ?
O3 C18 1.262(9) . ?
O3 Cu1 2.235(5) 1_665 ?
C3 C4 1.366(11) . ?
C3 C6 1.504(12) . ?
O4 C18 1.245(9) . ?
C4 C5 1.362(12) . ?
O5 C6 1.208(12) . ?
O6 Cu1 1.993(5) 2_566 ?
C7 C8 1.43(2) . ?
C8 N2 1.482(14) 2_665 ?
C9 C10 1.535(9) . ?
C10 C11 1.483(11) . ?
C11 C12 1.387(11) . ?
C11 C16 1.418(10) . ?
C12 C13 1.396(13) . ?
C13 C14 1.368(14) . ?
C14 C15 1.396(13) . ?
C15 C16 1.383(12) . ?
C16 C17 1.501(10) . ?
C17 C18 1.520(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O6 163.8(2) 1_455 . ?
O2 Cu1 O6 91.2(2) 1_455 2_566 ?
O6 Cu1 O6 81.3(2) . 2_566 ?
O2 Cu1 N1 88.0(2) 1_455 . ?
O6 Cu1 N1 99.2(2) . . ?
O6 Cu1 N1 178.8(2) 2_566 . ?
O2 Cu1 O3 102.1(2) 1_455 1_445 ?
O6 Cu1 O3 91.91(18) . 1_445 ?
O6 Cu1 O3 87.36(19) 2_566 1_445 ?
N1 Cu1 O3 93.7(2) . 1_445 ?
O2 Cu1 Cu1 129.94(16) 1_455 2_566 ?
O6 Cu1 Cu1 41.05(14) . 2_566 ?
O6 Cu1 Cu1 40.23(13) 2_566 2_566 ?
N1 Cu1 Cu1 140.23(17) . 2_566 ?
O3 Cu1 Cu1 89.49(13) 1_445 2_566 ?
O2 Cu1 Cu2 77.47(15) 1_455 1_455 ?
O6 Cu1 Cu2 104.58(14) . 1_455 ?
O6 Cu1 Cu2 39.39(13) 2_566 1_455 ?
N1 Cu1 Cu2 141.19(17) . 1_455 ?
O3 Cu1 Cu2 55.73(14) 1_445 1_455 ?
Cu1 Cu1 Cu2 69.57(3) 2_566 1_455 ?
N1 C1 C2 121.9(9) . . ?
C9 O1 Cu2 126.7(5) . . ?
C1 N1 C5 117.4(7) . . ?
C1 N1 Cu1 121.2(6) . . ?
C5 N1 Cu1 121.4(5) . . ?
O6 Cu2 O6 180.0 2_666 . ?
O6 Cu2 O1 86.81(19) 2_666 2_666 ?
O6 Cu2 O1 93.19(19) . 2_666 ?
O6 Cu2 O1 93.19(19) 2_666 . ?
O6 Cu2 O1 86.81(19) . . ?
O1 Cu2 O1 180.000(2) 2_666 . ?
O6 Cu2 Cu1 139.51(14) 2_666 2_566 ?
O6 Cu2 Cu1 40.49(14) . 2_566 ?
O1 Cu2 Cu1 79.51(15) 2_666 2_566 ?
O1 Cu2 Cu1 100.49(15) . 2_566 ?
O6 Cu2 Cu1 40.49(14) 2_666 1_655 ?
O6 Cu2 Cu1 139.50(14) . 1_655 ?
O1 Cu2 Cu1 100.49(15) 2_666 1_655 ?
O1 Cu2 Cu1 79.51(15) . 1_655 ?
Cu1 Cu2 Cu1 180.0 2_566 1_655 ?
C9 O2 Cu1 130.5(5) . 1_655 ?
C1 C2 C3 120.9(8) . . ?
C6 N2 C7 120.2(8) . . ?
C6 N2 C8 125.8(8) . 2_665 ?
C7 N2 C8 113.3(8) . 2_665 ?
C18 O3 Cu1 121.6(5) . 1_665 ?
C4 C3 C2 116.5(8) . . ?
C4 C3 C6 122.8(8) . . ?
C2 C3 C6 120.5(8) . . ?
C5 C4 C3 119.7(8) . . ?
N1 C5 C4 123.5(8) . . ?
Cu2 O6 Cu1 123.1(2) . . ?
Cu2 O6 Cu1 100.1(2) . 2_566 ?
Cu1 O6 Cu1 98.7(2) . 2_566 ?
O5 C6 N2 122.0(9) . . ?
O5 C6 C3 119.5(9) . . ?
N2 C6 C3 118.5(8) . . ?
C8 C7 N2 110.6(10) . . ?
C7 C8 N2 111.0(11) . 2_665 ?
O2 C9 O1 125.7(7) . . ?
O2 C9 C10 117.6(6) . . ?
O1 C9 C10 116.7(6) . . ?
C11 C10 C9 112.2(6) . . ?
C12 C11 C16 118.2(8) . . ?
C12 C11 C10 119.3(7) . . ?
C16 C11 C10 122.3(7) . . ?
C11 C12 C13 122.5(8) . . ?
C14 C13 C12 118.6(8) . . ?
C13 C14 C15 120.3(9) . . ?
C16 C15 C14 121.5(8) . . ?
C15 C16 C11 118.8(7) . . ?
C15 C16 C17 121.1(7) . . ?
C11 C16 C17 120.0(7) . . ?
C16 C17 C18 112.9(6) . . ?
O4 C18 O3 125.2(6) . . ?
O4 C18 C17 118.1(6) . . ?
O3 C18 C17 116.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.493
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.257
####################################################################### 
# 
# 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 1479976'
_audit_update_record             
;
2016-05-15 deposited with the CCDC.
2016-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 Co N2 O6'
_chemical_formula_weight         417.27

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   '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                   16.4579(8)
_cell_length_b                   7.6329(3)
_cell_length_c                   15.1328(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.0530(10)
_cell_angle_gamma                90.00
_cell_volume                     1722.15(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.69
_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          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_T_max  0.839
_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            8275
_diffrn_reflns_av_R_equivalents  0.0105
_diffrn_reflns_av_sigmaI/netI    0.0117
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3023
_reflns_number_gt                2801
_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)+(0.0485P)²+1.0561P] 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         3023
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0799
_refine_ls_wR_factor_gt          0.0781
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
Co1 Co 0.085659(16) 0.09132(3) 0.377020(17) 0.02302(11) Uani 1 1 d . . .
O1 O -0.01169(10) 0.2647(2) 0.29314(10) 0.0380(4) Uani 1 1 d . . .
C1 C 0.17284(14) 0.4619(3) 0.40288(15) 0.0322(4) Uani 1 1 d . . .
H1A H 0.1189 0.4993 0.4025 0.039 Uiso 1 1 calc R . .
N1 N 0.18250(11) 0.2917(2) 0.38865(12) 0.0272(3) Uani 1 1 d . . .
O1W O 0.00214(12) -0.1170(2) 0.37044(12) 0.0483(4) Uani 1 1 d . . .
H1WA H -0.0124 -0.2091 0.3919 0.058 Uiso 1 1 d R . .
H1WB H -0.0364 -0.1018 0.3120 0.058 Uiso 1 1 d R . .
O2 O -0.10474(10) 0.4897(2) 0.23870(10) 0.0344(3) Uani 1 1 d . . .
C2 C 0.23896(17) 0.5843(3) 0.41806(19) 0.0420(5) Uani 1 1 d . . .
H2A H 0.2299 0.7016 0.4280 0.050 Uiso 1 1 calc R . .
N2 N 0.46130(13) 0.1591(3) 0.45505(14) 0.0391(4) Uani 1 1 d . . .
O3 O -0.19452(10) 0.03285(19) 0.50648(10) 0.0341(3) Uani 1 1 d . . .
C3 C 0.31884(15) 0.5294(3) 0.41824(17) 0.0397(5) Uani 1 1 d . . .
H3A H 0.3640 0.6099 0.4268 0.048 Uiso 1 1 calc R . .
O4 O -0.09930(9) -0.12111(18) 0.47217(10) 0.0288(3) Uani 1 1 d . . .
C4 C 0.33118(13) 0.3531(3) 0.40554(14) 0.0288(4) Uani 1 1 d . . .
O5 O 0.43839(12) 0.3665(2) 0.34076(15) 0.0558(5) Uani 1 1 d . . .
C5 C 0.26086(13) 0.2393(3) 0.39002(15) 0.0292(4) Uani 1 1 d . . .
H5A H 0.2683 0.1213 0.3801 0.035 Uiso 1 1 calc R . .
C6 C 0.41564(14) 0.2945(3) 0.39907(16) 0.0343(5) Uani 1 1 d . . .
C7 C 0.45910(16) 0.1073(3) 0.54733(17) 0.0408(5) Uani 1 1 d . . .
H7A H 0.4049 0.1521 0.5496 0.049 Uiso 1 1 calc R . .
H7B H 0.5101 0.1580 0.6013 0.049 Uiso 1 1 calc R . .
C8 C 0.46165(17) -0.0869(3) 0.5576(2) 0.0439(6) Uani 1 1 d . . .
H8A H 0.4660 -0.1181 0.6216 0.053 Uiso 1 1 calc R . .
H8B H 0.4066 -0.1367 0.5091 0.053 Uiso 1 1 calc R . .
C9 C -0.06909(12) 0.3692(3) 0.29832(13) 0.0240(4) Uani 1 1 d . . .
C10 C -0.09494(13) 0.3534(3) 0.38324(14) 0.0302(4) Uani 1 1 d . . .
H10A H -0.0749 0.2407 0.4145 0.036 Uiso 1 1 calc R . .
H10B H -0.0640 0.4436 0.4308 0.036 Uiso 1 1 calc R . .
C11 C -0.19495(13) 0.3704(3) 0.35309(13) 0.0248(4) Uani 1 1 d . . .
C12 C -0.23172(15) 0.5355(3) 0.34800(16) 0.0354(5) Uani 1 1 d . . .
H12A H -0.1950 0.6337 0.3614 0.042 Uiso 1 1 calc R . .
C13 C -0.32236(17) 0.5565(3) 0.32323(18) 0.0443(6) Uani 1 1 d . . .
H13A H -0.3460 0.6679 0.3212 0.053 Uiso 1 1 calc R . .
C14 C -0.37739(16) 0.4117(3) 0.30156(18) 0.0448(6) Uani 1 1 d . . .
H14A H -0.4383 0.4249 0.2852 0.054 Uiso 1 1 calc R . .
C15 C -0.34183(14) 0.2471(3) 0.30422(15) 0.0368(5) Uani 1 1 d . . .
H15A H -0.3796 0.1501 0.2879 0.044 Uiso 1 1 calc R . .
C16 C -0.25036(13) 0.2233(3) 0.33090(13) 0.0261(4) Uani 1 1 d . . .
C17 C -0.21325(15) 0.0404(3) 0.34029(14) 0.0326(4) Uani 1 1 d . . .
H17A H -0.1710 0.0362 0.3110 0.039 Uiso 1 1 calc R . .
H17B H -0.2618 -0.0399 0.3047 0.039 Uiso 1 1 calc R . .
C18 C -0.16648(13) -0.0186(2) 0.44570(14) 0.0265(4) 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
Co1 O1 2.0513(14) . ?
Co1 O2 2.0575(13) 2_545 ?
Co1 O1W 2.0763(16) . ?
Co1 O3 2.1309(14) 3_556 ?
Co1 N1 2.1616(16) . ?
Co1 O4 2.2082(13) 3_556 ?
Co1 C18 2.5003(19) 3_556 ?
O1 C9 1.264(2) . ?
C1 N1 1.337(3) . ?
C1 C2 1.378(3) . ?
N1 C5 1.342(2) . ?
O2 C9 1.247(2) . ?
O2 Co1 2.0575(13) 2 ?
C2 C3 1.379(3) . ?
N2 C6 1.346(3) . ?
N2 C7 1.467(3) . ?
N2 C8 1.468(3) 3_656 ?
O3 C18 1.254(2) . ?
O3 Co1 2.1310(14) 3_556 ?
C3 C4 1.387(3) . ?
O4 C18 1.273(2) . ?
O4 Co1 2.2081(13) 3_556 ?
C4 C5 1.385(3) . ?
C4 C6 1.502(3) . ?
O5 C6 1.225(3) . ?
C7 C8 1.489(3) . ?
C8 N2 1.468(3) 3_656 ?
C9 C10 1.520(3) . ?
C10 C11 1.516(3) . ?
C11 C12 1.386(3) . ?
C11 C16 1.395(3) . ?
C12 C13 1.385(3) . ?
C13 C14 1.377(4) . ?
C14 C15 1.380(3) . ?
C15 C16 1.395(3) . ?
C16 C17 1.506(3) . ?
C17 C18 1.517(3) . ?
C18 Co1 2.5004(19) 3_556 ?

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 Co1 O2 94.44(6) . 2_545 ?
O1 Co1 O1W 97.86(7) . . ?
O2 Co1 O1W 90.40(6) 2_545 . ?
O1 Co1 O3 164.08(6) . 3_556 ?
O2 Co1 O3 99.12(6) 2_545 3_556 ?
O1W Co1 O3 90.39(7) . 3_556 ?
O1 Co1 N1 87.11(6) . . ?
O2 Co1 N1 87.88(6) 2_545 . ?
O1W Co1 N1 174.86(7) . . ?
O3 Co1 N1 85.11(6) 3_556 . ?
O1 Co1 O4 106.50(5) . 3_556 ?
O2 Co1 O4 158.93(6) 2_545 3_556 ?
O1W Co1 O4 84.48(6) . 3_556 ?
O3 Co1 O4 60.59(5) 3_556 3_556 ?
N1 Co1 O4 95.41(6) . 3_556 ?
O1 Co1 C18 136.75(6) . 3_556 ?
O2 Co1 C18 128.75(6) 2_545 3_556 ?
O1W Co1 C18 85.53(7) . 3_556 ?
O3 Co1 C18 30.09(6) 3_556 3_556 ?
N1 Co1 C18 91.76(6) . 3_556 ?
O4 Co1 C18 30.57(6) 3_556 3_556 ?
C9 O1 Co1 141.02(13) . . ?
N1 C1 C2 123.12(19) . . ?
C1 N1 C5 117.76(17) . . ?
C1 N1 Co1 124.51(14) . . ?
C5 N1 Co1 117.47(13) . . ?
C9 O2 Co1 134.36(12) . 2 ?
C1 C2 C3 118.6(2) . . ?
C6 N2 C7 125.05(19) . . ?
C6 N2 C8 119.30(18) . 3_656 ?
C7 N2 C8 113.20(18) . 3_656 ?
C18 O3 Co1 91.48(12) . 3_556 ?
C2 C3 C4 119.4(2) . . ?
C18 O4 Co1 87.51(11) . 3_556 ?
C5 C4 C3 118.10(19) . . ?
C5 C4 C6 122.17(19) . . ?
C3 C4 C6 119.44(19) . . ?
N1 C5 C4 123.01(18) . . ?
O5 C6 N2 122.6(2) . . ?
O5 C6 C4 119.14(19) . . ?
N2 C6 C4 118.21(18) . . ?
N2 C7 C8 110.9(2) . . ?
N2 C8 C7 110.4(2) 3_656 . ?
O2 C9 O1 123.74(17) . . ?
O2 C9 C10 117.12(17) . . ?
O1 C9 C10 119.11(17) . . ?
C11 C10 C9 113.31(15) . . ?
C12 C11 C16 119.55(18) . . ?
C12 C11 C10 119.15(18) . . ?
C16 C11 C10 121.30(18) . . ?
C13 C12 C11 121.0(2) . . ?
C14 C13 C12 119.7(2) . . ?
C13 C14 C15 119.7(2) . . ?
C14 C15 C16 121.3(2) . . ?
C11 C16 C15 118.68(19) . . ?
C11 C16 C17 121.71(17) . . ?
C15 C16 C17 119.52(19) . . ?
C16 C17 C18 112.32(16) . . ?
O3 C18 O4 120.14(17) . . ?
O3 C18 C17 119.85(18) . . ?
O4 C18 C17 120.01(17) . . ?
O3 C18 Co1 58.43(10) . 3_556 ?
O4 C18 Co1 61.92(10) . 3_556 ?
C17 C18 Co1 175.45(14) . 3_556 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.050














