# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_am020204
_database_code_depnum_ccdc_archive 'CCDC 1021588'
_audit_update_record             
;
2014-11-24 deposited with the CCDC.
2014-12-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23.70 H49.40 Cu2 F6 N8 O13 S2'
_chemical_formula_weight         959.71

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.3134(8)
_cell_length_b                   12.3928(9)
_cell_length_c                   16.8732(13)
_cell_angle_alpha                93.869(9)
_cell_angle_beta                 97.990(10)
_cell_angle_gamma                90.512(10)
_cell_volume                     1923.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      30.4

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             991
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7981
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_process_details   '(Coppens et al., 1965)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(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  'Stoe IPDS'
_diffrn_measurement_method       'φ oscillation scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         50-200
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  15
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22273
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.67
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8190
_reflns_number_gt                5256
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.1022P)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         8190
_refine_ls_number_parameters     506
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0612
_refine_ls_wR_factor_ref         0.1561
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_restrained_S_all      0.902
_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 0.43817(5) 0.08591(4) 0.21824(3) 0.03154(15) Uani 1 1 d . . .
Cu2 Cu 0.33241(5) 0.41738(4) -0.21586(3) 0.03161(15) Uani 1 1 d . . .
S3 S 0.80958(12) 0.14205(9) 0.32759(7) 0.0353(2) Uani 1 1 d . . .
S4 S 0.64745(12) 0.35820(9) -0.33897(7) 0.0390(3) Uani 1 1 d . . .
C1 C 0.1776(5) 0.2147(4) 0.1752(3) 0.0347(9) Uani 1 1 d . . .
H1A H 0.1410 0.1713 0.2156 0.042 Uiso 1 1 calc R . .
H1B H 0.0926 0.2364 0.1381 0.042 Uiso 1 1 calc R . .
C2 C 0.2532(5) 0.3174(3) 0.2185(3) 0.0357(10) Uani 1 1 d . . .
H2A H 0.2581 0.3712 0.1781 0.043 Uiso 1 1 calc R . .
H2B H 0.1907 0.3475 0.2571 0.043 Uiso 1 1 calc R . .
C3 C 0.4058(5) 0.3065(4) 0.2638(3) 0.0394(10) Uani 1 1 d . . .
H3A H 0.4771 0.3132 0.2259 0.047 Uiso 1 1 calc R . .
H3B H 0.4247 0.3670 0.3056 0.047 Uiso 1 1 calc R . .
C4 C 0.3399(6) 0.1886(4) 0.3684(3) 0.0438(11) Uani 1 1 d . . .
H4A H 0.2379 0.2057 0.3491 0.053 Uiso 1 1 calc R . .
H4B H 0.3750 0.2407 0.4143 0.053 Uiso 1 1 calc R . .
C5 C 0.3466(5) 0.0734(4) 0.3967(3) 0.0400(10) Uani 1 1 d . . .
H5A H 0.4493 0.0521 0.4074 0.048 Uiso 1 1 calc R . .
H5B H 0.3056 0.0728 0.4478 0.048 Uiso 1 1 calc R . .
C6 C 0.2645(5) -0.0093(4) 0.3362(3) 0.0406(10) Uani 1 1 d . . .
H6A H 0.2495 -0.0764 0.3629 0.049 Uiso 1 1 calc R . .
H6B H 0.1680 0.0192 0.3168 0.049 Uiso 1 1 calc R . .
C7 C 0.2484(5) -0.0987(4) 0.1991(3) 0.0399(10) Uani 1 1 d . . .
H7A H 0.1977 -0.1569 0.2224 0.048 Uiso 1 1 calc R . .
H7B H 0.3108 -0.1337 0.1623 0.048 Uiso 1 1 calc R . .
C8 C 0.1348(5) -0.0325(4) 0.1500(3) 0.0386(10) Uani 1 1 d . . .
H8A H 0.0822 0.0102 0.1882 0.046 Uiso 1 1 calc R . .
H8B H 0.0636 -0.0839 0.1183 0.046 Uiso 1 1 calc R . .
C9 C 0.1855(5) 0.0454(4) 0.0925(3) 0.0356(9) Uani 1 1 d . . .
H9A H 0.2461 0.0045 0.0575 0.043 Uiso 1 1 calc R . .
H9B H 0.0988 0.0691 0.0576 0.043 Uiso 1 1 calc R . .
C10 C 0.3270(4) 0.2030(3) 0.0639(3) 0.0319(9) Uani 1 1 d . . .
H10A H 0.3860 0.1517 0.0352 0.038 Uiso 1 1 calc R . .
H10B H 0.3928 0.2623 0.0897 0.038 Uiso 1 1 calc R . .
C11 C 0.2146(4) 0.2514(4) 0.0012(3) 0.0353(10) Uani 1 1 d . . .
H11A H 0.1592 0.3079 0.0274 0.042 Uiso 1 1 calc R . .
H11B H 0.1457 0.1943 -0.0251 0.042 Uiso 1 1 calc R . .
C12 C 0.2959(4) 0.3008(3) -0.0613(3) 0.0323(9) Uani 1 1 d . . .
H12A H 0.3694 0.3532 -0.0327 0.039 Uiso 1 1 calc R . .
H12B H 0.3486 0.2423 -0.0871 0.039 Uiso 1 1 calc R . .
C13 C 0.0916(5) 0.2854(3) -0.1733(3) 0.0332(9) Uani 1 1 d . . .
H13A H 0.0363 0.3275 -0.2147 0.040 Uiso 1 1 calc R . .
H13B H 0.0234 0.2634 -0.1370 0.040 Uiso 1 1 calc R . .
C14 C 0.1473(5) 0.1825(3) -0.2149(3) 0.0342(9) Uani 1 1 d . . .
H14A H 0.0662 0.1502 -0.2536 0.041 Uiso 1 1 calc R . .
H14B H 0.1725 0.1300 -0.1737 0.041 Uiso 1 1 calc R . .
C15 C 0.2797(5) 0.1953(3) -0.2601(3) 0.0379(10) Uani 1 1 d . . .
H15A H 0.3695 0.1901 -0.2217 0.046 Uiso 1 1 calc R . .
H15B H 0.2783 0.1348 -0.3016 0.046 Uiso 1 1 calc R . .
C16 C 0.1614(5) 0.3093(4) -0.3666(3) 0.0416(11) Uani 1 1 d . . .
H16A H 0.0688 0.2897 -0.3482 0.050 Uiso 1 1 calc R . .
H16B H 0.1760 0.2579 -0.4121 0.050 Uiso 1 1 calc R . .
C17 C 0.1521(5) 0.4238(4) -0.3948(3) 0.0439(12) Uani 1 1 d . . .
H17A H 0.0861 0.4231 -0.4462 0.053 Uiso 1 1 calc R . .
H17B H 0.2494 0.4476 -0.4048 0.053 Uiso 1 1 calc R . .
C18 C 0.0974(5) 0.5053(4) -0.3339(3) 0.0390(10) Uani 1 1 d . . .
H18A H 0.0673 0.5718 -0.3606 0.047 Uiso 1 1 calc R . .
H18B H 0.0112 0.4742 -0.3148 0.047 Uiso 1 1 calc R . .
C19 C 0.1499(5) 0.5975(4) -0.1977(3) 0.0408(11) Uani 1 1 d . . .
H19A H 0.0892 0.6554 -0.2216 0.049 Uiso 1 1 calc R . .
H19B H 0.2310 0.6327 -0.1605 0.049 Uiso 1 1 calc R . .
C20 C 0.0574(5) 0.5302(4) -0.1488(3) 0.0376(10) Uani 1 1 d . . .
H20A H 0.0013 0.5812 -0.1180 0.045 Uiso 1 1 calc R . .
H20B H -0.0133 0.4861 -0.1873 0.045 Uiso 1 1 calc R . .
C21 C 0.1367(5) 0.4544(3) -0.0902(3) 0.0354(9) Uani 1 1 d . . .
H21A H 0.2131 0.4971 -0.0545 0.043 Uiso 1 1 calc R . .
H21B H 0.0667 0.4287 -0.0562 0.043 Uiso 1 1 calc R . .
C31 C 0.8959(6) 0.1061(5) 0.4249(3) 0.0531(13) Uani 1 1 d . . .
C41 C 0.6850(7) 0.3897(6) -0.4374(3) 0.0599(15) Uani 1 1 d . . .
N1 N 0.2702(4) 0.1450(3) 0.1291(2) 0.0299(7) Uani 1 1 d . . .
N2 N 0.4292(4) 0.2013(3) 0.3031(2) 0.0325(8) Uani 1 1 d . . .
H2 H 0.5237 0.2074 0.3295 0.039 Uiso 1 1 calc R . .
N3 N 0.3436(4) -0.0357(3) 0.2657(2) 0.0355(8) Uani 1 1 d . . .
H3 H 0.4177 -0.0816 0.2835 0.043 Uiso 1 1 calc R . .
N4 N 0.2059(4) 0.3574(3) -0.1261(2) 0.0284(7) Uani 1 1 d . . .
N5 N 0.2838(4) 0.3000(3) -0.2994(2) 0.0337(8) Uani 1 1 d . . .
H5 H 0.3658 0.2950 -0.3251 0.040 Uiso 1 1 calc R . .
N6 N 0.2112(4) 0.5342(3) -0.2633(2) 0.0357(8) Uani 1 1 d . . .
H6 H 0.2755 0.5813 -0.2816 0.043 Uiso 1 1 calc R . .
N16 N 0.6288(4) 0.0506(3) 0.1276(2) 0.0386(9) Uani 1 1 d . . .
N26 N 0.5711(4) 0.4516(3) -0.1309(2) 0.0387(9) Uani 1 1 d . . .
O1 O 0.5304(4) -0.0162(3) 0.14334(19) 0.0409(7) Uani 1 1 d . . .
O2 O 0.7219(4) 0.0193(3) 0.0875(2) 0.0570(10) Uani 1 1 d . . .
O3 O 0.6203(4) 0.1466(3) 0.1554(2) 0.0434(8) Uani 1 1 d . . .
O4 O 0.5373(3) 0.3572(3) -0.16217(19) 0.0400(7) Uani 1 1 d . . .
O5 O 0.4679(4) 0.5217(3) -0.1427(2) 0.0428(8) Uani 1 1 d . . .
O6 O 0.6882(4) 0.4777(3) -0.0930(2) 0.0571(10) Uani 1 1 d . . .
O7 O 0.6978(4) 0.0579(3) 0.3080(2) 0.0494(9) Uani 1 1 d . . .
O8 O 0.9261(4) 0.1377(4) 0.2795(2) 0.0569(10) Uani 1 1 d . . .
O9 O 0.7513(3) 0.2484(2) 0.3418(2) 0.0404(7) Uani 1 1 d . . .
O10 O 0.5784(4) 0.2523(3) -0.3507(3) 0.0552(10) Uani 1 1 d . . .
O11 O 0.7883(4) 0.3638(4) -0.2920(3) 0.0738(14) Uani 1 1 d . . .
O12 O 0.5487(4) 0.4424(3) -0.3203(3) 0.0548(10) Uani 1 1 d . . .
O51 O 0.8624(6) 0.2089(5) 0.0376(4) 0.0663(17) Uani 0.70 1 d P A 1
C51 C 0.7374(7) 0.2495(5) -0.0043(4) 0.0370(14) Uani 0.70 1 d P A 1
H51A H 0.6896 0.2975 0.0321 0.055 Uiso 0.70 1 calc PR A 1
H51B H 0.6713 0.1894 -0.0262 0.055 Uiso 0.70 1 calc PR A 1
H51C H 0.7632 0.2901 -0.0483 0.055 Uiso 0.70 1 calc PR A 1
O52 O 0.8425(15) 0.2904(13) -0.0383(10) 0.072(4) Uani 0.30 1 d P B 2
F1 F 1.0020(4) 0.1746(4) 0.4558(2) 0.0865(13) Uani 1 1 d . . .
F2 F 0.8037(4) 0.1015(3) 0.47751(19) 0.0719(11) Uani 1 1 d . . .
F3 F 0.9557(5) 0.0070(3) 0.4174(2) 0.0838(13) Uani 1 1 d . . .
F4 F 0.7879(6) 0.3254(5) -0.4619(3) 0.1125(18) Uani 1 1 d . . .
F5 F 0.7377(5) 0.4905(4) -0.4366(2) 0.0868(13) Uani 1 1 d . . .
F6 F 0.5673(5) 0.3811(5) -0.4919(2) 0.1049(17) 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 N2 1.965(4) . ?
Cu1 N3 2.006(3) . ?
Cu1 O1 2.010(4) . ?
Cu1 N1 2.182(3) . ?
Cu1 O3 2.270(3) . ?
Cu1 O7 2.708(4) . ?
Cu2 N5 1.960(4) . ?
Cu2 N6 1.987(4) . ?
Cu2 O5 2.028(3) . ?
Cu2 O4 2.157(3) . ?
Cu2 N4 2.206(3) . ?
S3 O8 1.442(3) . ?
S3 O9 1.447(3) . ?
S3 O7 1.456(3) . ?
S3 C31 1.812(5) . ?
S4 O11 1.434(4) . ?
S4 O12 1.445(4) . ?
S4 O10 1.445(4) . ?
S4 C41 1.811(6) . ?
C1 N1 1.485(6) . ?
C1 C2 1.537(6) . ?
C2 C3 1.530(6) . ?
C3 N2 1.506(5) . ?
C4 N2 1.486(6) . ?
C4 C5 1.536(6) . ?
C5 C6 1.518(7) . ?
C6 N3 1.503(6) . ?
C7 N3 1.501(6) . ?
C7 C8 1.530(6) . ?
C8 C9 1.531(5) . ?
C9 N1 1.508(5) . ?
C10 N1 1.506(5) . ?
C10 C11 1.537(5) . ?
C11 C12 1.537(5) . ?
C12 N4 1.499(5) . ?
C13 N4 1.488(5) . ?
C13 C14 1.543(6) . ?
C14 C15 1.549(6) . ?
C15 N5 1.498(5) . ?
C16 N5 1.503(5) . ?
C16 C17 1.526(6) . ?
C17 C18 1.534(7) . ?
C18 N6 1.502(6) . ?
C19 N6 1.493(6) . ?
C19 C20 1.548(6) . ?
C20 C21 1.529(5) . ?
C21 N4 1.501(6) . ?
C31 F2 1.321(6) . ?
C31 F1 1.323(7) . ?
C31 F3 1.358(7) . ?
C41 F6 1.328(7) . ?
C41 F5 1.336(8) . ?
C41 F4 1.343(8) . ?
N16 O2 1.221(5) . ?
N16 O3 1.256(5) . ?
N16 O1 1.296(5) . ?
N26 O6 1.215(5) . ?
N26 O4 1.269(5) . ?
N26 O5 1.305(5) . ?
O51 C51 1.392(8) . ?

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 Cu1 N3 99.79(15) . . ?
N2 Cu1 O1 157.30(14) . . ?
N3 Cu1 O1 92.44(14) . . ?
N2 Cu1 N1 97.86(14) . . ?
N3 Cu1 N1 105.22(13) . . ?
O1 Cu1 N1 97.25(13) . . ?
N2 Cu1 O3 101.99(13) . . ?
N3 Cu1 O3 149.32(14) . . ?
O1 Cu1 O3 60.36(13) . . ?
N1 Cu1 O3 92.94(11) . . ?
N2 Cu1 O7 80.68(13) . . ?
N3 Cu1 O7 92.90(13) . . ?
O1 Cu1 O7 79.67(13) . . ?
N1 Cu1 O7 161.77(11) . . ?
O3 Cu1 O7 69.81(11) . . ?
N5 Cu2 N6 100.19(15) . . ?
N5 Cu2 O5 155.02(15) . . ?
N6 Cu2 O5 93.71(14) . . ?
N5 Cu2 O4 97.95(14) . . ?
N6 Cu2 O4 151.50(13) . . ?
O5 Cu2 O4 62.13(13) . . ?
N5 Cu2 N4 97.90(13) . . ?
N6 Cu2 N4 103.61(13) . . ?
O5 Cu2 N4 98.88(13) . . ?
O4 Cu2 N4 95.41(11) . . ?
O8 S3 O9 115.3(2) . . ?
O8 S3 O7 116.0(3) . . ?
O9 S3 O7 113.1(2) . . ?
O8 S3 C31 103.5(2) . . ?
O9 S3 C31 105.1(2) . . ?
O7 S3 C31 101.6(2) . . ?
O11 S4 O12 116.0(3) . . ?
O11 S4 O10 115.7(3) . . ?
O12 S4 O10 112.5(2) . . ?
O11 S4 C41 103.0(3) . . ?
O12 S4 C41 102.3(3) . . ?
O10 S4 C41 105.1(3) . . ?
N1 C1 C2 115.0(3) . . ?
C3 C2 C1 117.8(3) . . ?
N2 C3 C2 113.7(3) . . ?
N2 C4 C5 111.8(4) . . ?
C6 C5 C4 113.0(4) . . ?
N3 C6 C5 112.3(4) . . ?
N3 C7 C8 115.2(4) . . ?
C7 C8 C9 118.6(4) . . ?
N1 C9 C8 117.3(4) . . ?
N1 C10 C11 117.2(3) . . ?
C10 C11 C12 108.2(3) . . ?
N4 C12 C11 116.7(3) . . ?
N4 C13 C14 115.2(3) . . ?
C13 C14 C15 117.5(3) . . ?
N5 C15 C14 113.8(4) . . ?
N5 C16 C17 111.5(4) . . ?
C16 C17 C18 112.8(4) . . ?
N6 C18 C17 112.1(4) . . ?
N6 C19 C20 114.8(4) . . ?
C21 C20 C19 117.8(4) . . ?
N4 C21 C20 116.8(4) . . ?
F2 C31 F1 107.9(5) . . ?
F2 C31 F3 107.6(5) . . ?
F1 C31 F3 106.9(5) . . ?
F2 C31 S3 112.6(4) . . ?
F1 C31 S3 112.2(4) . . ?
F3 C31 S3 109.4(4) . . ?
F6 C41 F5 107.4(5) . . ?
F6 C41 F4 109.1(6) . . ?
F5 C41 F4 105.4(5) . . ?
F6 C41 S4 112.3(4) . . ?
F5 C41 S4 111.4(5) . . ?
F4 C41 S4 111.0(4) . . ?
C1 N1 C10 112.4(3) . . ?
C1 N1 C9 109.7(3) . . ?
C10 N1 C9 109.3(3) . . ?
C1 N1 Cu1 105.5(2) . . ?
C10 N1 Cu1 114.5(2) . . ?
C9 N1 Cu1 105.0(2) . . ?
C4 N2 C3 113.5(4) . . ?
C4 N2 Cu1 121.4(3) . . ?
C3 N2 Cu1 108.0(3) . . ?
C7 N3 C6 111.4(4) . . ?
C7 N3 Cu1 108.0(2) . . ?
C6 N3 Cu1 118.4(3) . . ?
C13 N4 C12 112.5(3) . . ?
C13 N4 C21 109.4(3) . . ?
C12 N4 C21 109.9(3) . . ?
C13 N4 Cu2 104.9(2) . . ?
C12 N4 Cu2 113.5(2) . . ?
C21 N4 Cu2 106.4(2) . . ?
C15 N5 C16 112.9(3) . . ?
C15 N5 Cu2 108.7(3) . . ?
C16 N5 Cu2 121.4(3) . . ?
C19 N6 C18 111.7(4) . . ?
C19 N6 Cu2 108.8(2) . . ?
C18 N6 Cu2 118.7(3) . . ?
O2 N16 O3 123.8(4) . . ?
O2 N16 O1 120.3(4) . . ?
O3 N16 O1 115.9(4) . . ?
O6 N26 O4 124.7(4) . . ?
O6 N26 O5 121.0(4) . . ?
O4 N26 O5 114.3(4) . . ?
N16 O1 Cu1 97.0(3) . . ?
N16 O3 Cu1 86.3(2) . . ?
N26 O4 Cu2 89.2(2) . . ?
N26 O5 Cu2 94.0(3) . . ?
S3 O7 Cu1 124.04(18) . . ?

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
N1 C1 C2 C3 -44.2(5) . . . . ?
C1 C2 C3 N2 -35.3(6) . . . . ?
N2 C4 C5 C6 -71.8(5) . . . . ?
C4 C5 C6 N3 74.3(5) . . . . ?
N3 C7 C8 C9 72.1(6) . . . . ?
C7 C8 C9 N1 -70.0(6) . . . . ?
N1 C10 C11 C12 -177.0(4) . . . . ?
C10 C11 C12 N4 -177.2(4) . . . . ?
N4 C13 C14 C15 -45.2(5) . . . . ?
C13 C14 C15 N5 -34.5(6) . . . . ?
N5 C16 C17 C18 -71.4(5) . . . . ?
C16 C17 C18 N6 74.7(5) . . . . ?
N6 C19 C20 C21 73.0(5) . . . . ?
C19 C20 C21 N4 -69.0(6) . . . . ?
O8 S3 C31 F2 -177.5(5) . . . . ?
O9 S3 C31 F2 61.1(5) . . . . ?
O7 S3 C31 F2 -56.9(5) . . . . ?
O8 S3 C31 F1 60.5(5) . . . . ?
O9 S3 C31 F1 -60.8(5) . . . . ?
O7 S3 C31 F1 -178.8(4) . . . . ?
O8 S3 C31 F3 -58.0(5) . . . . ?
O9 S3 C31 F3 -179.3(4) . . . . ?
O7 S3 C31 F3 62.6(4) . . . . ?
O11 S4 C41 F6 175.5(5) . . . . ?
O12 S4 C41 F6 -63.7(6) . . . . ?
O10 S4 C41 F6 53.9(6) . . . . ?
O11 S4 C41 F5 -64.0(5) . . . . ?
O12 S4 C41 F5 56.7(5) . . . . ?
O10 S4 C41 F5 174.4(4) . . . . ?
O11 S4 C41 F4 53.1(6) . . . . ?
O12 S4 C41 F4 173.8(5) . . . . ?
O10 S4 C41 F4 -68.5(5) . . . . ?
C2 C1 N1 C10 -60.3(4) . . . . ?
C2 C1 N1 C9 177.8(3) . . . . ?
C2 C1 N1 Cu1 65.1(3) . . . . ?
C11 C10 N1 C1 -56.9(5) . . . . ?
C11 C10 N1 C9 65.3(5) . . . . ?
C11 C10 N1 Cu1 -177.3(3) . . . . ?
C8 C9 N1 C1 -63.7(5) . . . . ?
C8 C9 N1 C10 172.5(4) . . . . ?
C8 C9 N1 Cu1 49.3(4) . . . . ?
N2 Cu1 N1 C1 -23.1(2) . . . . ?
N3 Cu1 N1 C1 79.3(3) . . . . ?
O1 Cu1 N1 C1 173.9(2) . . . . ?
O3 Cu1 N1 C1 -125.6(2) . . . . ?
O7 Cu1 N1 C1 -107.2(4) . . . . ?
N2 Cu1 N1 C10 101.0(3) . . . . ?
N3 Cu1 N1 C10 -156.5(3) . . . . ?
O1 Cu1 N1 C10 -62.0(3) . . . . ?
O3 Cu1 N1 C10 -1.5(3) . . . . ?
O7 Cu1 N1 C10 17.0(6) . . . . ?
N2 Cu1 N1 C9 -139.0(3) . . . . ?
N3 Cu1 N1 C9 -36.6(3) . . . . ?
O1 Cu1 N1 C9 57.9(3) . . . . ?
O3 Cu1 N1 C9 118.4(3) . . . . ?
O7 Cu1 N1 C9 136.9(4) . . . . ?
C5 C4 N2 C3 170.1(4) . . . . ?
C5 C4 N2 Cu1 38.8(5) . . . . ?
C2 C3 N2 C4 -65.5(5) . . . . ?
C2 C3 N2 Cu1 72.1(4) . . . . ?
N3 Cu1 N2 C4 -11.9(3) . . . . ?
O1 Cu1 N2 C4 -133.6(4) . . . . ?
N1 Cu1 N2 C4 95.1(3) . . . . ?
O3 Cu1 N2 C4 -170.2(3) . . . . ?
O7 Cu1 N2 C4 -103.3(3) . . . . ?
N3 Cu1 N2 C3 -145.5(3) . . . . ?
O1 Cu1 N2 C3 92.9(4) . . . . ?
N1 Cu1 N2 C3 -38.4(3) . . . . ?
O3 Cu1 N2 C3 56.3(3) . . . . ?
O7 Cu1 N2 C3 123.2(3) . . . . ?
C8 C7 N3 C6 75.9(4) . . . . ?
C8 C7 N3 Cu1 -55.7(4) . . . . ?
C5 C6 N3 C7 -168.1(3) . . . . ?
C5 C6 N3 Cu1 -42.1(4) . . . . ?
N2 Cu1 N3 C7 140.7(3) . . . . ?
O1 Cu1 N3 C7 -58.5(3) . . . . ?
N1 Cu1 N3 C7 39.7(3) . . . . ?
O3 Cu1 N3 C7 -84.5(4) . . . . ?
O7 Cu1 N3 C7 -138.2(3) . . . . ?
N2 Cu1 N3 C6 13.1(3) . . . . ?
O1 Cu1 N3 C6 173.9(3) . . . . ?
N1 Cu1 N3 C6 -87.9(3) . . . . ?
O3 Cu1 N3 C6 147.8(3) . . . . ?
O7 Cu1 N3 C6 94.1(3) . . . . ?
C14 C13 N4 C12 -58.3(4) . . . . ?
C14 C13 N4 C21 179.2(3) . . . . ?
C14 C13 N4 Cu2 65.4(3) . . . . ?
C11 C12 N4 C13 -58.1(5) . . . . ?
C11 C12 N4 C21 64.1(5) . . . . ?
C11 C12 N4 Cu2 -176.9(3) . . . . ?
C20 C21 N4 C13 -63.9(4) . . . . ?
C20 C21 N4 C12 172.0(3) . . . . ?
C20 C21 N4 Cu2 48.8(4) . . . . ?
N5 Cu2 N4 C13 -23.3(3) . . . . ?
N6 Cu2 N4 C13 79.3(3) . . . . ?
O5 Cu2 N4 C13 175.3(2) . . . . ?
O4 Cu2 N4 C13 -122.1(2) . . . . ?
N5 Cu2 N4 C12 99.9(3) . . . . ?
N6 Cu2 N4 C12 -157.5(3) . . . . ?
O5 Cu2 N4 C12 -61.5(3) . . . . ?
O4 Cu2 N4 C12 1.1(3) . . . . ?
N5 Cu2 N4 C21 -139.2(3) . . . . ?
N6 Cu2 N4 C21 -36.6(3) . . . . ?
O5 Cu2 N4 C21 59.4(3) . . . . ?
O4 Cu2 N4 C21 122.0(3) . . . . ?
C14 C15 N5 C16 -66.1(5) . . . . ?
C14 C15 N5 Cu2 71.7(4) . . . . ?
C17 C16 N5 C15 169.4(4) . . . . ?
C17 C16 N5 Cu2 37.7(5) . . . . ?
N6 Cu2 N5 C15 -144.0(3) . . . . ?
O5 Cu2 N5 C15 93.3(4) . . . . ?
O4 Cu2 N5 C15 58.1(3) . . . . ?
N4 Cu2 N5 C15 -38.5(3) . . . . ?
N6 Cu2 N5 C16 -10.4(3) . . . . ?
O5 Cu2 N5 C16 -133.2(3) . . . . ?
O4 Cu2 N5 C16 -168.4(3) . . . . ?
N4 Cu2 N5 C16 95.0(3) . . . . ?
C20 C19 N6 C18 74.9(4) . . . . ?
C20 C19 N6 Cu2 -58.1(4) . . . . ?
C17 C18 N6 C19 -169.8(3) . . . . ?
C17 C18 N6 Cu2 -41.9(4) . . . . ?
N5 Cu2 N6 C19 141.6(3) . . . . ?
O5 Cu2 N6 C19 -59.2(3) . . . . ?
O4 Cu2 N6 C19 -89.7(4) . . . . ?
N4 Cu2 N6 C19 40.8(3) . . . . ?
N5 Cu2 N6 C18 12.4(3) . . . . ?
O5 Cu2 N6 C18 171.5(3) . . . . ?
O4 Cu2 N6 C18 141.1(3) . . . . ?
N4 Cu2 N6 C18 -88.4(3) . . . . ?
O2 N16 O1 Cu1 173.9(3) . . . . ?
O3 N16 O1 Cu1 -6.6(4) . . . . ?
N2 Cu1 O1 N16 -38.4(4) . . . . ?
N3 Cu1 O1 N16 -161.3(2) . . . . ?
N1 Cu1 O1 N16 93.0(2) . . . . ?
O3 Cu1 O1 N16 3.8(2) . . . . ?
O7 Cu1 O1 N16 -68.8(2) . . . . ?
O2 N16 O3 Cu1 -174.7(4) . . . . ?
O1 N16 O3 Cu1 5.8(3) . . . . ?
N2 Cu1 O3 N16 160.8(2) . . . . ?
N3 Cu1 O3 N16 26.5(4) . . . . ?
O1 Cu1 O3 N16 -3.9(2) . . . . ?
N1 Cu1 O3 N16 -100.5(2) . . . . ?
O7 Cu1 O3 N16 85.5(2) . . . . ?
O6 N26 O4 Cu2 -175.1(4) . . . . ?
O5 N26 O4 Cu2 4.9(3) . . . . ?
N5 Cu2 O4 N26 160.8(2) . . . . ?
N6 Cu2 O4 N26 31.6(4) . . . . ?
O5 Cu2 O4 N26 -3.3(2) . . . . ?
N4 Cu2 O4 N26 -100.5(2) . . . . ?
O6 N26 O5 Cu2 174.8(4) . . . . ?
O4 N26 O5 Cu2 -5.2(3) . . . . ?
N5 Cu2 O5 N26 -37.0(4) . . . . ?
N6 Cu2 O5 N26 -161.0(2) . . . . ?
O4 Cu2 O5 N26 3.2(2) . . . . ?
N4 Cu2 O5 N26 94.6(2) . . . . ?
O8 S3 O7 Cu1 -99.7(3) . . . . ?
O9 S3 O7 Cu1 36.8(3) . . . . ?
C31 S3 O7 Cu1 148.9(3) . . . . ?
N2 Cu1 O7 S3 -57.1(3) . . . . ?
N3 Cu1 O7 S3 -156.6(3) . . . . ?
O1 Cu1 O7 S3 111.5(3) . . . . ?
N1 Cu1 O7 S3 29.7(6) . . . . ?
O3 Cu1 O7 S3 49.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.929
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.929
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.826
_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/. 
# 
# Audit and citation data items have may 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_am050406
_database_code_depnum_ccdc_archive 'CCDC 1021589'
_audit_update_record             
;
2014-08-28 deposited with the CCDC.
2014-12-05 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 H60 N6 Ni2 O10'
_chemical_formula_weight         758.24

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                   8.6958(13)
_cell_length_b                   8.7403(13)
_cell_length_c                   12.3998(19)
_cell_angle_alpha                102.060(18)
_cell_angle_beta                 105.113(18)
_cell_angle_gamma                94.828(18)
_cell_volume                     880.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    7998
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      30.4

_exptl_crystal_description       cube
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             406
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7265
_exptl_absorpt_correction_T_max  0.8433
_exptl_absorpt_process_details   '(Coppens et al., 1965)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(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  'Stoe IPDS'
_diffrn_measurement_method       'φ oscillation scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         50-200
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  8
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15881
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.40
_diffrn_reflns_theta_max         30.42
_reflns_number_total             4836
_reflns_number_gt                4373
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0725P)²+0.2519P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4836
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1150
_refine_ls_wR_factor_gt          0.1117
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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 0.00373(2) 0.16065(2) 0.784761(16) 0.01956(8) Uani 1 1 d . . .
C1 C 0.1179(2) -0.1373(2) 0.84169(14) 0.0251(3) Uani 1 1 d . . .
H1A H 0.0025 -0.1826 0.8154 0.030 Uiso 1 1 calc R . .
H1B H 0.1734 -0.1939 0.8984 0.030 Uiso 1 1 calc R . .
C2 C 0.1857(2) -0.1700(2) 0.73818(15) 0.0264(3) Uani 1 1 d . . .
H2A H 0.2977 -0.1146 0.7622 0.032 Uiso 1 1 calc R . .
H2B H 0.1898 -0.2848 0.7159 0.032 Uiso 1 1 calc R . .
C3 C 0.0911(2) -0.1193(2) 0.63240(14) 0.0254(3) Uani 1 1 d . . .
H3A H 0.1357 -0.1578 0.5677 0.030 Uiso 1 1 calc R . .
H3B H -0.0224 -0.1702 0.6102 0.030 Uiso 1 1 calc R . .
C4 C 0.2427(2) 0.1309(2) 0.63265(15) 0.0281(3) Uani 1 1 d . . .
H4A H 0.2394 0.0941 0.5508 0.034 Uiso 1 1 calc R . .
H4B H 0.3380 0.0965 0.6797 0.034 Uiso 1 1 calc R . .
C5 C 0.2620(2) 0.3108(2) 0.66394(16) 0.0314(4) Uani 1 1 d . . .
H5A H 0.1579 0.3442 0.6298 0.038 Uiso 1 1 calc R . .
H5B H 0.3420 0.3524 0.6293 0.038 Uiso 1 1 calc R . .
C6 C 0.3159(2) 0.3849(3) 0.79393(17) 0.0331(4) Uani 1 1 d . . .
H6A H 0.4104 0.3388 0.8302 0.040 Uiso 1 1 calc R . .
H6B H 0.3497 0.5000 0.8072 0.040 Uiso 1 1 calc R . .
C7 C 0.2526(2) 0.3919(2) 0.97708(15) 0.0304(4) Uani 1 1 d . . .
H7B H 0.1620 0.3946 1.0116 0.036 Uiso 1 1 calc R . .
H7A H 0.3197 0.4973 1.0060 0.036 Uiso 1 1 calc R . .
C8 C 0.3545(2) 0.2675(3) 1.01606(15) 0.0308(4) Uani 1 1 d . . .
H8A H 0.4681 0.3041 1.0226 0.037 Uiso 1 1 calc R . .
H8B H 0.3486 0.2624 1.0939 0.037 Uiso 1 1 calc R . .
C9 C 0.3074(2) 0.1006(2) 0.93876(15) 0.0268(3) Uani 1 1 d . . .
H9A H 0.3425 0.1000 0.8689 0.032 Uiso 1 1 calc R . .
H9B H 0.3685 0.0289 0.9797 0.032 Uiso 1 1 calc R . .
C10 C 0.08354(19) 0.0436(2) 1.01029(14) 0.0231(3) Uani 1 1 d . . .
H10A H 0.0869 0.1563 1.0473 0.028 Uiso 1 1 calc R . .
H10B H 0.1622 -0.0008 1.0642 0.028 Uiso 1 1 calc R . .
C20 C -0.3344(2) -0.0221(2) 0.70994(15) 0.0265(3) Uani 1 1 d . . .
C21 C -0.4532(2) -0.1532(3) 0.6194(2) 0.0436(5) Uani 1 1 d . . .
H21A H -0.4856 -0.2350 0.6557 0.065 Uiso 1 1 calc R . .
H21B H -0.4025 -0.1995 0.5608 0.065 Uiso 1 1 calc R . .
H21C H -0.5484 -0.1097 0.5833 0.065 Uiso 1 1 calc R . .
C30 C -0.1494(2) 0.4185(2) 0.68200(17) 0.0318(4) Uani 1 1 d . . .
C31 C -0.2245(4) 0.4835(3) 0.5799(2) 0.0535(7) Uani 1 1 d . . .
H31A H -0.3407 0.4466 0.5530 0.080 Uiso 1 1 calc R . .
H31B H -0.1762 0.4465 0.5178 0.080 Uiso 1 1 calc R . .
H31C H -0.2052 0.5993 0.6026 0.080 Uiso 1 1 calc R . .
N1 N 0.13327(16) 0.03371(18) 0.90173(11) 0.0206(3) Uani 1 1 d . . .
N2 N 0.09490(16) 0.05471(18) 0.65077(12) 0.0215(3) Uani 1 1 d . . .
H2 H 0.0157 0.0624 0.5861 0.026 Uiso 1 1 calc R . .
N3 N 0.18746(19) 0.3599(2) 0.85015(13) 0.0270(3) Uani 1 1 d . . .
H3 H 0.1306 0.4439 0.8402 0.032 Uiso 1 1 calc R . .
O1 O -0.12218(17) 0.27404(18) 0.89519(11) 0.0273(3) Uani 1 1 d . . .
H33 H -0.124(4) 0.358(5) 0.871(3) 0.063(10) Uiso 1 1 d . . .
H32 H -0.208(4) 0.216(5) 0.863(3) 0.063(10) Uiso 1 1 d . . .
O20 O -0.18858(15) -0.01884(16) 0.70939(11) 0.0258(3) Uani 1 1 d . . .
O21 O -0.38666(16) 0.0717(2) 0.77885(13) 0.0358(3) Uani 1 1 d . . .
O30 O -0.11530(17) 0.27913(17) 0.66072(11) 0.0282(3) Uani 1 1 d . . .
O31 O -0.1225(2) 0.50679(19) 0.78115(14) 0.0451(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
Ni1 O20 2.0644(15) . ?
Ni1 N2 2.1009(14) . ?
Ni1 O1 2.1102(13) . ?
Ni1 N3 2.1235(17) . ?
Ni1 O30 2.1272(13) . ?
Ni1 N1 2.1528(14) . ?
C1 N1 1.502(2) . ?
C1 C2 1.532(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.528(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N2 1.486(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N2 1.488(2) . ?
C4 C5 1.523(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.535(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N3 1.486(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N3 1.484(2) . ?
C7 C8 1.536(3) . ?
C7 H7B 0.9900 . ?
C7 H7A 0.9900 . ?
C8 C9 1.525(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N1 1.491(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N1 1.5058(19) . ?
C10 C10 1.515(3) 2_557 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C20 O21 1.257(2) . ?
C20 O20 1.268(2) . ?
C20 C21 1.516(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C30 O31 1.259(3) . ?
C30 O30 1.269(2) . ?
C30 C31 1.511(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N2 H2 0.9300 . ?
N3 H3 0.9300 . ?
O1 H33 0.85(4) . ?
O1 H32 0.81(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
O20 Ni1 N2 84.74(6) . . ?
O20 Ni1 O1 90.47(6) . . ?
N2 Ni1 O1 169.59(5) . . ?
O20 Ni1 N3 173.66(5) . . ?
N2 Ni1 N3 95.13(6) . . ?
O1 Ni1 N3 88.60(6) . . ?
O20 Ni1 O30 85.72(6) . . ?
N2 Ni1 O30 82.83(5) . . ?
O1 Ni1 O30 87.60(5) . . ?
N3 Ni1 O30 87.98(6) . . ?
O20 Ni1 N1 94.39(6) . . ?
N2 Ni1 N1 93.09(5) . . ?
O1 Ni1 N1 96.50(5) . . ?
N3 Ni1 N1 91.94(6) . . ?
O30 Ni1 N1 175.90(5) . . ?
N1 C1 C2 115.76(14) . . ?
N1 C1 H1A 108.3 . . ?
C2 C1 H1A 108.3 . . ?
N1 C1 H1B 108.3 . . ?
C2 C1 H1B 108.3 . . ?
H1A C1 H1B 107.4 . . ?
C3 C2 C1 115.19(13) . . ?
C3 C2 H2A 108.5 . . ?
C1 C2 H2A 108.5 . . ?
C3 C2 H2B 108.5 . . ?
C1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
N2 C3 C2 113.54(14) . . ?
N2 C3 H3A 108.9 . . ?
C2 C3 H3A 108.9 . . ?
N2 C3 H3B 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
N2 C4 C5 113.27(14) . . ?
N2 C4 H4A 108.9 . . ?
C5 C4 H4A 108.9 . . ?
N2 C4 H4B 108.9 . . ?
C5 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C4 C5 C6 114.03(16) . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N3 C6 C5 113.02(16) . . ?
N3 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
N3 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
N3 C7 C8 112.85(15) . . ?
N3 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
N3 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
H7B C7 H7A 107.8 . . ?
C9 C8 C7 116.21(15) . . ?
C9 C8 H8A 108.2 . . ?
C7 C8 H8A 108.2 . . ?
C9 C8 H8B 108.2 . . ?
C7 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?
N1 C9 C8 116.71(14) . . ?
N1 C9 H9A 108.1 . . ?
C8 C9 H9A 108.1 . . ?
N1 C9 H9B 108.1 . . ?
C8 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
N1 C10 C10 113.28(17) . 2_557 ?
N1 C10 H10A 108.9 . . ?
C10 C10 H10A 108.9 2_557 . ?
N1 C10 H10B 108.9 . . ?
C10 C10 H10B 108.9 2_557 . ?
H10A C10 H10B 107.7 . . ?
O21 C20 O20 125.81(18) . . ?
O21 C20 C21 118.40(16) . . ?
O20 C20 C21 115.78(16) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O31 C30 O30 124.90(18) . . ?
O31 C30 C31 118.09(19) . . ?
O30 C30 C31 117.00(19) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C9 N1 C1 107.57(13) . . ?
C9 N1 C10 106.26(13) . . ?
C1 N1 C10 108.86(13) . . ?
C9 N1 Ni1 108.74(10) . . ?
C1 N1 Ni1 110.02(10) . . ?
C10 N1 Ni1 115.08(10) . . ?
C3 N2 C4 111.29(13) . . ?
C3 N2 Ni1 115.01(10) . . ?
C4 N2 Ni1 121.26(11) . . ?
C3 N2 H2 101.9 . . ?
C4 N2 H2 101.9 . . ?
Ni1 N2 H2 101.9 . . ?
C7 N3 C6 112.01(15) . . ?
C7 N3 Ni1 111.45(12) . . ?
C6 N3 Ni1 122.10(13) . . ?
C7 N3 H3 102.8 . . ?
C6 N3 H3 102.8 . . ?
Ni1 N3 H3 102.8 . . ?
Ni1 O1 H33 96(2) . . ?
Ni1 O1 H32 96(2) . . ?
H33 O1 H32 109(3) . . ?
C20 O20 Ni1 129.87(13) . . ?
C30 O30 Ni1 125.88(13) . . ?

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
N1 C1 C2 C3 -69.8(2) . . . . ?
C1 C2 C3 N2 65.9(2) . . . . ?
N2 C4 C5 C6 74.9(2) . . . . ?
C4 C5 C6 N3 -71.7(2) . . . . ?
N3 C7 C8 C9 -30.5(2) . . . . ?
C7 C8 C9 N1 -48.1(2) . . . . ?
C8 C9 N1 C1 -171.94(14) . . . . ?
C8 C9 N1 C10 -55.48(18) . . . . ?
C8 C9 N1 Ni1 68.94(16) . . . . ?
C2 C1 N1 C9 -57.13(17) . . . . ?
C2 C1 N1 C10 -171.88(14) . . . . ?
C2 C1 N1 Ni1 61.16(16) . . . . ?
C10 C10 N1 C9 -170.62(17) 2_557 . . . ?
C10 C10 N1 C1 -55.0(2) 2_557 . . . ?
C10 C10 N1 Ni1 69.0(2) 2_557 . . . ?
O20 Ni1 N1 C9 157.61(11) . . . . ?
N2 Ni1 N1 C9 72.65(11) . . . . ?
O1 Ni1 N1 C9 -111.41(11) . . . . ?
N3 Ni1 N1 C9 -22.59(11) . . . . ?
O30 Ni1 N1 C9 66.2(7) . . . . ?
O20 Ni1 N1 C1 40.04(11) . . . . ?
N2 Ni1 N1 C1 -44.92(11) . . . . ?
O1 Ni1 N1 C1 131.02(10) . . . . ?
N3 Ni1 N1 C1 -140.17(11) . . . . ?
O30 Ni1 N1 C1 -51.3(7) . . . . ?
O20 Ni1 N1 C10 -83.36(12) . . . . ?
N2 Ni1 N1 C10 -168.31(12) . . . . ?
O1 Ni1 N1 C10 7.62(12) . . . . ?
N3 Ni1 N1 C10 96.44(12) . . . . ?
O30 Ni1 N1 C10 -174.7(7) . . . . ?
C2 C3 N2 C4 83.92(16) . . . . ?
C2 C3 N2 Ni1 -58.87(16) . . . . ?
C5 C4 N2 C3 -173.30(14) . . . . ?
C5 C4 N2 Ni1 -33.18(18) . . . . ?
O20 Ni1 N2 C3 -48.40(11) . . . . ?
O1 Ni1 N2 C3 -111.3(3) . . . . ?
N3 Ni1 N2 C3 137.96(11) . . . . ?
O30 Ni1 N2 C3 -134.73(12) . . . . ?
N1 Ni1 N2 C3 45.73(11) . . . . ?
O20 Ni1 N2 C4 172.85(12) . . . . ?
O1 Ni1 N2 C4 109.9(3) . . . . ?
N3 Ni1 N2 C4 -0.79(13) . . . . ?
O30 Ni1 N2 C4 86.52(13) . . . . ?
N1 Ni1 N2 C4 -93.02(12) . . . . ?
C8 C7 N3 C6 -69.8(2) . . . . ?
C8 C7 N3 Ni1 70.93(17) . . . . ?
C5 C6 N3 C7 164.25(17) . . . . ?
C5 C6 N3 Ni1 28.3(2) . . . . ?
O20 Ni1 N3 C7 138.3(4) . . . . ?
N2 Ni1 N3 C7 -133.12(12) . . . . ?
O1 Ni1 N3 C7 56.61(12) . . . . ?
O30 Ni1 N3 C7 144.26(12) . . . . ?
N1 Ni1 N3 C7 -39.84(12) . . . . ?
O20 Ni1 N3 C6 -85.5(5) . . . . ?
N2 Ni1 N3 C6 3.08(15) . . . . ?
O1 Ni1 N3 C6 -167.18(14) . . . . ?
O30 Ni1 N3 C6 -79.53(14) . . . . ?
N1 Ni1 N3 C6 96.36(14) . . . . ?
O21 C20 O20 Ni1 -17.6(3) . . . . ?
C21 C20 O20 Ni1 163.24(16) . . . . ?
N2 Ni1 O20 C20 -152.34(16) . . . . ?
O1 Ni1 O20 C20 18.40(16) . . . . ?
N3 Ni1 O20 C20 -63.2(5) . . . . ?
O30 Ni1 O20 C20 -69.16(16) . . . . ?
N1 Ni1 O20 C20 114.95(16) . . . . ?
O31 C30 O30 Ni1 -2.6(3) . . . . ?
C31 C30 O30 Ni1 176.00(17) . . . . ?
O20 Ni1 O30 C30 127.14(17) . . . . ?
N2 Ni1 O30 C30 -147.63(17) . . . . ?
O1 Ni1 O30 C30 36.48(17) . . . . ?
N3 Ni1 O30 C30 -52.20(17) . . . . ?
N1 Ni1 O30 C30 -141.2(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O31 0.93 2.28 3.080(2) 143.3 .
O1 H33 O31 0.85(4) 1.88(4) 2.709(2) 164(3) .
O1 H32 O21 0.81(4) 1.84(4) 2.649(2) 172(4) .

_diffrn_measured_fraction_theta_max 0.905
_diffrn_reflns_theta_full        30.42
_diffrn_measured_fraction_theta_full 0.905
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_am130906
_database_code_depnum_ccdc_archive 'CCDC 1021590'
_audit_update_record             
;
2014-08-28 deposited with the CCDC.
2014-12-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H52 F12 N6 O12 S4'
_chemical_formula_weight         996.98

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   10.3354(8)
_cell_length_b                   17.2802(9)
_cell_length_c                   11.9040(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.109(10)
_cell_angle_gamma                90.00
_cell_volume                     2120.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      30.4

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1036
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8718
_exptl_absorpt_correction_T_max  0.9408
_exptl_absorpt_process_details   '(Coppens et al., 1965)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(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  'Stoe IPDS'
_diffrn_measurement_method       'φ oscillation scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         50-200
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  7
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33989
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         30.00
_reflns_number_total             6158
_reflns_number_gt                4590
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.1000P)²+0.6904P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6158
_refine_ls_number_parameters     279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.1944
_refine_ls_wR_factor_gt          0.1748
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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
S20 S 0.79238(5) 0.09366(3) 0.69416(4) 0.04674(16) Uani 1 1 d . . .
S30 S 0.16626(6) 0.41861(3) 0.72638(6) 0.05497(18) Uani 1 1 d . . .
N1 N 0.58222(17) 0.33675(9) 0.60150(14) 0.0402(3) Uani 1 1 d . . .
H1C H 0.533(3) 0.2952(18) 0.625(3) 0.062(8) Uiso 1 1 d . . .
C10 C 0.4890(2) 0.40051(11) 0.56702(17) 0.0421(4) Uani 1 1 d . . .
H10A H 0.4508 0.4207 0.6351 0.051 Uiso 1 1 calc R . .
H10B H 0.4175 0.3786 0.5170 0.051 Uiso 1 1 calc R . .
O22 O 0.72470(19) 0.16404(11) 0.66766(18) 0.0655(5) Uani 1 1 d . . .
N3 N 0.5182(2) 0.15005(10) 0.50129(17) 0.0514(4) Uani 1 1 d . . .
H3C H 0.5669 0.1228 0.4530 0.062 Uiso 1 1 calc R . .
H3D H 0.5729 0.1651 0.5617 0.062 Uiso 1 1 calc R . .
C6 C 0.4181(3) 0.09680(13) 0.5431(3) 0.0600(6) Uani 1 1 d . . .
H6B H 0.4623 0.0499 0.5742 0.072 Uiso 1 1 calc R . .
H6A H 0.3592 0.0805 0.4782 0.072 Uiso 1 1 calc R . .
N2 N 0.4550(2) 0.23917(10) 0.73125(17) 0.0509(4) Uani 1 1 d . . .
H2C H 0.387(3) 0.2689(19) 0.731(3) 0.070(9) Uiso 1 1 d . . .
C1 C 0.6656(2) 0.35617(13) 0.70671(19) 0.0500(5) Uani 1 1 d . . .
H1A H 0.6967 0.4102 0.7023 0.060 Uiso 1 1 calc R . .
H1B H 0.7422 0.3216 0.7129 0.060 Uiso 1 1 calc R . .
C11 C 0.5492(2) 0.46704(10) 0.50691(18) 0.0433(4) Uani 1 1 d . . .
H11A H 0.5741 0.4499 0.4321 0.052 Uiso 1 1 calc R . .
H11B H 0.6283 0.4851 0.5511 0.052 Uiso 1 1 calc R . .
O20 O 0.7253(2) 0.02633(12) 0.6552(2) 0.0826(7) Uani 1 1 d . . .
C9 C 0.6588(2) 0.30797(12) 0.50883(18) 0.0470(4) Uani 1 1 d . . .
H9A H 0.7186 0.2668 0.5384 0.056 Uiso 1 1 calc R . .
H9B H 0.7120 0.3509 0.4818 0.056 Uiso 1 1 calc R . .
C4 C 0.4127(3) 0.15770(13) 0.7393(2) 0.0601(6) Uani 1 1 d . . .
H4B H 0.3575 0.1523 0.8035 0.072 Uiso 1 1 calc R . .
H4A H 0.4898 0.1243 0.7543 0.072 Uiso 1 1 calc R . .
O31 O 0.0885(2) 0.43249(12) 0.81959(17) 0.0711(5) Uani 1 1 d . . .
C8 C 0.5728(3) 0.27601(13) 0.41032(19) 0.0548(5) Uani 1 1 d . . .
H8A H 0.5319 0.3201 0.3682 0.066 Uiso 1 1 calc R . .
H8B H 0.6285 0.2486 0.3589 0.066 Uiso 1 1 calc R . .
C7 C 0.4668(3) 0.22113(13) 0.4417(2) 0.0561(5) Uani 1 1 d . . .
H7B H 0.4086 0.2487 0.4908 0.067 Uiso 1 1 calc R . .
H7A H 0.4147 0.2055 0.3724 0.067 Uiso 1 1 calc R . .
F21 F 0.9994(2) 0.16202(13) 0.6294(2) 0.0981(7) Uani 1 1 d . . .
C2 C 0.5894(3) 0.34675(14) 0.8101(2) 0.0578(6) Uani 1 1 d . . .
H2A H 0.5131 0.3816 0.8031 0.069 Uiso 1 1 calc R . .
H2B H 0.6445 0.3630 0.8773 0.069 Uiso 1 1 calc R . .
C5 C 0.3371(3) 0.13040(15) 0.6321(3) 0.0651(7) Uani 1 1 d . . .
H5B H 0.2738 0.0908 0.6527 0.078 Uiso 1 1 calc R . .
H5A H 0.2873 0.1748 0.5989 0.078 Uiso 1 1 calc R . .
O30 O 0.2391(2) 0.34908(14) 0.7363(2) 0.0876(7) Uani 1 1 d . . .
C3 C 0.5428(3) 0.26423(14) 0.82784(19) 0.0601(6) Uani 1 1 d . . .
H3B H 0.6184 0.2290 0.8363 0.072 Uiso 1 1 calc R . .
H3A H 0.4967 0.2616 0.8978 0.072 Uiso 1 1 calc R . .
O32 O 0.2322(2) 0.48454(12) 0.6874(2) 0.0809(6) Uani 1 1 d . . .
F22 F 0.8873(3) 0.1032(2) 0.5000(2) 0.1387(12) Uani 1 1 d . . .
F20 F 1.0053(2) 0.03886(15) 0.6231(3) 0.1381(12) Uani 1 1 d . . .
F31 F -0.0396(3) 0.4543(2) 0.5978(3) 0.1322(11) Uani 1 1 d . . .
O21 O 0.8506(3) 0.09100(18) 0.80441(19) 0.0950(8) Uani 1 1 d . . .
C20 C 0.9289(3) 0.09954(19) 0.6077(3) 0.0721(7) Uani 1 1 d . . .
F30 F -0.0200(3) 0.33331(17) 0.6364(3) 0.1239(9) Uani 1 1 d . . .
C30 C 0.0448(4) 0.3974(2) 0.6120(3) 0.0845(9) Uani 1 1 d . . .
F32 F 0.1016(3) 0.38684(19) 0.5176(2) 0.1321(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
S20 O21 1.405(2) . ?
S20 O20 1.415(2) . ?
S20 O22 1.4269(18) . ?
S20 C20 1.808(3) . ?
S30 O30 1.418(2) . ?
S30 O32 1.423(2) . ?
S30 O31 1.4362(19) . ?
S30 C30 1.821(4) . ?
N1 C9 1.489(3) . ?
N1 C10 1.501(2) . ?
N1 C1 1.506(3) . ?
N1 H1C 0.93(3) . ?
C10 C11 1.512(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
N3 C6 1.496(3) . ?
N3 C7 1.497(3) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
C6 C5 1.512(4) . ?
C6 H6B 0.9900 . ?
C6 H6A 0.9900 . ?
N2 C3 1.478(4) . ?
N2 C4 1.479(3) . ?
N2 H2C 0.87(3) . ?
C1 C2 1.517(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C11 C11 1.529(4) 3_666 ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C9 C8 1.524(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C4 C5 1.522(4) . ?
C4 H4B 0.9900 . ?
C4 H4A 0.9900 . ?
C8 C7 1.516(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C7 H7B 0.9900 . ?
C7 H7A 0.9900 . ?
F21 C20 1.318(4) . ?
C2 C3 1.524(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C5 H5B 0.9900 . ?
C5 H5A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 H3A 0.9900 . ?
F22 C20 1.324(4) . ?
F20 C20 1.318(4) . ?
F31 C30 1.318(5) . ?
F30 C30 1.336(4) . ?
C30 F32 1.318(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
O21 S20 O20 116.50(16) . . ?
O21 S20 O22 113.89(16) . . ?
O20 S20 O22 114.04(13) . . ?
O21 S20 C20 103.54(16) . . ?
O20 S20 C20 104.08(15) . . ?
O22 S20 C20 102.50(14) . . ?
O30 S30 O32 116.23(15) . . ?
O30 S30 O31 113.59(14) . . ?
O32 S30 O31 115.23(13) . . ?
O30 S30 C30 102.98(18) . . ?
O32 S30 C30 103.77(17) . . ?
O31 S30 C30 102.55(16) . . ?
C9 N1 C10 114.05(15) . . ?
C9 N1 C1 112.81(17) . . ?
C10 N1 C1 112.43(15) . . ?
C9 N1 H1C 106.9(18) . . ?
C10 N1 H1C 107.0(19) . . ?
C1 N1 H1C 102.7(19) . . ?
N1 C10 C11 114.19(16) . . ?
N1 C10 H10A 108.7 . . ?
C11 C10 H10A 108.7 . . ?
N1 C10 H10B 108.7 . . ?
C11 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C6 N3 C7 115.6(2) . . ?
C6 N3 H3C 108.4 . . ?
C7 N3 H3C 108.4 . . ?
C6 N3 H3D 108.4 . . ?
C7 N3 H3D 108.4 . . ?
H3C N3 H3D 107.4 . . ?
N3 C6 C5 115.30(19) . . ?
N3 C6 H6B 108.4 . . ?
C5 C6 H6B 108.4 . . ?
N3 C6 H6A 108.4 . . ?
C5 C6 H6A 108.4 . . ?
H6B C6 H6A 107.5 . . ?
C3 N2 C4 113.4(2) . . ?
C3 N2 H2C 106(2) . . ?
C4 N2 H2C 109(2) . . ?
N1 C1 C2 110.56(19) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C10 C11 C11 108.9(2) . 3_666 ?
C10 C11 H11A 109.9 . . ?
C11 C11 H11A 109.9 3_666 . ?
C10 C11 H11B 109.9 . . ?
C11 C11 H11B 109.9 3_666 . ?
H11A C11 H11B 108.3 . . ?
N1 C9 C8 112.29(19) . . ?
N1 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
N1 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
N2 C4 C5 112.1(2) . . ?
N2 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
N2 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
H4B C4 H4A 107.9 . . ?
C7 C8 C9 115.43(18) . . ?
C7 C8 H8A 108.4 . . ?
C9 C8 H8A 108.4 . . ?
C7 C8 H8B 108.4 . . ?
C9 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
N3 C7 C8 113.1(2) . . ?
N3 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
N3 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
H7B C7 H7A 107.8 . . ?
C1 C2 C3 113.61(19) . . ?
C1 C2 H2A 108.8 . . ?
C3 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C6 C5 C4 115.5(2) . . ?
C6 C5 H5B 108.4 . . ?
C4 C5 H5B 108.4 . . ?
C6 C5 H5A 108.4 . . ?
C4 C5 H5A 108.4 . . ?
H5B C5 H5A 107.5 . . ?
N2 C3 C2 110.40(19) . . ?
N2 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 . . ?
N2 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 . . ?
H3B C3 H3A 108.1 . . ?
F21 C20 F20 107.9(3) . . ?
F21 C20 F22 106.7(3) . . ?
F20 C20 F22 108.8(3) . . ?
F21 C20 S20 112.2(2) . . ?
F20 C20 S20 111.1(3) . . ?
F22 C20 S20 110.0(2) . . ?
F32 C30 F31 108.9(3) . . ?
F32 C30 F30 109.4(3) . . ?
F31 C30 F30 108.0(3) . . ?
F32 C30 S30 109.9(3) . . ?
F31 C30 S30 111.1(3) . . ?
F30 C30 S30 109.5(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
C9 N1 C10 C11 -51.2(2) . . . . ?
C1 N1 C10 C11 78.9(2) . . . . ?
C7 N3 C6 C5 -63.6(3) . . . . ?
C9 N1 C1 C2 -152.27(18) . . . . ?
C10 N1 C1 C2 77.1(2) . . . . ?
N1 C10 C11 C11 -171.2(2) . . . 3_666 ?
C10 N1 C9 C8 -59.7(2) . . . . ?
C1 N1 C9 C8 170.48(17) . . . . ?
C3 N2 C4 C5 -172.5(2) . . . . ?
N1 C9 C8 C7 -47.1(3) . . . . ?
C6 N3 C7 C8 175.0(2) . . . . ?
C9 C8 C7 N3 -60.9(3) . . . . ?
N1 C1 C2 C3 62.1(3) . . . . ?
N3 C6 C5 C4 -59.0(3) . . . . ?
N2 C4 C5 C6 88.4(3) . . . . ?
C4 N2 C3 C2 176.2(2) . . . . ?
C1 C2 C3 N2 -61.2(3) . . . . ?
O21 S20 C20 F21 -60.8(3) . . . . ?
O20 S20 C20 F21 176.9(2) . . . . ?
O22 S20 C20 F21 57.9(3) . . . . ?
O21 S20 C20 F20 60.0(3) . . . . ?
O20 S20 C20 F20 -62.2(3) . . . . ?
O22 S20 C20 F20 178.7(2) . . . . ?
O21 S20 C20 F22 -179.4(3) . . . . ?
O20 S20 C20 F22 58.4(3) . . . . ?
O22 S20 C20 F22 -60.7(3) . . . . ?
O30 S30 C30 F32 -64.9(3) . . . . ?
O32 S30 C30 F32 56.6(3) . . . . ?
O31 S30 C30 F32 176.9(3) . . . . ?
O30 S30 C30 F31 174.4(3) . . . . ?
O32 S30 C30 F31 -64.0(3) . . . . ?
O31 S30 C30 F31 56.3(3) . . . . ?
O30 S30 C30 F30 55.3(3) . . . . ?
O32 S30 C30 F30 176.8(3) . . . . ?
O31 S30 C30 F30 -62.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_am200206
_database_code_depnum_ccdc_archive 'CCDC 1021591'
_audit_update_record             
;
2014-08-28 deposited with the CCDC.
2014-12-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C83 H110 B2 N8 Ni2 O5'
_chemical_formula_weight         1438.83

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'
B B 0.0013 0.0007 '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                   11.2739(8)
_cell_length_b                   12.8908(9)
_cell_length_c                   14.9803(10)
_cell_angle_alpha                104.807(8)
_cell_angle_beta                 97.878(9)
_cell_angle_gamma                107.244(8)
_cell_volume                     1956.0(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      30.4

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             770
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8221
_exptl_absorpt_correction_T_max  0.9003
_exptl_absorpt_process_details   '(Coppens et al., 1965)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(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  'Stoe IPDS'
_diffrn_measurement_method       'φ oscillation scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         50-200
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  9
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10463
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         30.03
_reflns_number_total             10463
_reflns_number_gt                7107
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.1000P)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         10463
_refine_ls_number_parameters     453
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1290
_refine_ls_wR_factor_gt          0.1232
_refine_ls_goodness_of_fit_ref   0.805
_refine_ls_restrained_S_all      0.805
_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 0.447514(19) 0.945158(19) 0.301658(14) 0.03569(6) Uani 1 1 d . . .
C1 C 0.63331(18) 0.9001(2) 0.18574(14) 0.0547(5) Uani 1 1 d . . .
H1B H 0.6881 0.9816 0.2143 0.066 Uiso 1 1 calc R . .
H1A H 0.6518 0.8719 0.1231 0.066 Uiso 1 1 calc R . .
C2 C 0.6704(2) 0.8333(2) 0.24858(15) 0.0616(5) Uani 1 1 d . . .
H2B H 0.6103 0.7534 0.2230 0.074 Uiso 1 1 calc R . .
H2A H 0.7565 0.8316 0.2435 0.074 Uiso 1 1 calc R . .
C3 C 0.67192(19) 0.8778(2) 0.35273(14) 0.0541(5) Uani 1 1 d . . .
H3B H 0.7118 0.8364 0.3877 0.065 Uiso 1 1 calc R . .
H3A H 0.7256 0.9598 0.3777 0.065 Uiso 1 1 calc R . .
C4 C 0.4747(2) 0.74584(19) 0.36835(15) 0.0558(5) Uani 1 1 d . . .
H4A H 0.5176 0.7310 0.4235 0.067 Uiso 1 1 calc R . .
H4B H 0.4817 0.6927 0.3102 0.067 Uiso 1 1 calc R . .
C5 C 0.3342(2) 0.71984(19) 0.36927(14) 0.0568(5) Uani 1 1 d . . .
H5A H 0.3034 0.6494 0.3871 0.068 Uiso 1 1 calc R . .
H5B H 0.3258 0.7831 0.4188 0.068 Uiso 1 1 calc R . .
C6 C 0.2489(2) 0.70397(18) 0.27545(14) 0.0520(5) Uani 1 1 d . . .
H6B H 0.2679 0.6511 0.2233 0.062 Uiso 1 1 calc R . .
H6A H 0.1584 0.6695 0.2768 0.062 Uiso 1 1 calc R . .
C7 C 0.20724(18) 0.80212(19) 0.15938(13) 0.0510(5) Uani 1 1 d . . .
H7A H 0.2084 0.8781 0.1560 0.061 Uiso 1 1 calc R . .
H7B H 0.1169 0.7518 0.1446 0.061 Uiso 1 1 calc R . .
C8 C 0.2724(2) 0.7525(2) 0.08487(14) 0.0559(5) Uani 1 1 d . . .
H8B H 0.2270 0.6688 0.0596 0.067 Uiso 1 1 calc R . .
H8A H 0.2606 0.7838 0.0317 0.067 Uiso 1 1 calc R . .
C9 C 0.41442(19) 0.77370(18) 0.11616(12) 0.0490(4) Uani 1 1 d . . .
H9B H 0.4243 0.7243 0.1555 0.059 Uiso 1 1 calc R . .
H9A H 0.4463 0.7490 0.0589 0.059 Uiso 1 1 calc R . .
C10 C 0.48018(17) 0.97442(17) 0.11894(11) 0.0433(4) Uani 1 1 d . . .
H10A H 0.5347 1.0527 0.1593 0.052 Uiso 1 1 calc R . .
H10B H 0.3905 0.9714 0.1115 0.052 Uiso 1 1 calc R . .
C11 C 0.5110(2) 0.95527(19) 0.02127(13) 0.0515(5) Uani 1 1 d . . .
H11A H 0.6012 0.9600 0.0271 0.062 Uiso 1 1 calc R . .
H11B H 0.4562 0.8780 -0.0210 0.062 Uiso 1 1 calc R . .
C15 C 0.67348(17) 1.19272(17) 0.37384(12) 0.0449(4) Uani 1 1 d . . .
C16 C 0.7559(2) 1.3117(2) 0.40447(17) 0.0635(6) Uani 1 1 d . . .
H16A H 0.8107 1.3305 0.4672 0.095 Uiso 1 1 calc R . .
H16B H 0.7036 1.3606 0.4079 0.095 Uiso 1 1 calc R . .
H16C H 0.8090 1.3244 0.3590 0.095 Uiso 1 1 calc R . .
C20 C 0.33319(16) 1.07603(16) 0.36268(12) 0.0410(4) Uani 1 1 d . . .
C21 C 0.2671(2) 1.15867(19) 0.39831(15) 0.0526(4) Uani 1 1 d . . .
H21C H 0.2066 1.1592 0.3450 0.079 Uiso 1 1 calc R . .
H21B H 0.3306 1.2356 0.4284 0.079 Uiso 1 1 calc R . .
H21A H 0.2211 1.1350 0.4448 0.079 Uiso 1 1 calc R . .
C30 C 0.90012(18) 0.45171(17) 0.24931(12) 0.0460(4) Uani 1 1 d . . .
C31 C 0.8639(3) 0.3458(2) 0.18027(17) 0.0786(8) Uani 1 1 d . . .
H31A H 0.7947 0.3267 0.1280 0.094 Uiso 1 1 calc R . .
C32 C 0.9233(4) 0.2671(3) 0.1838(2) 0.1028(11) Uani 1 1 d . . .
H32A H 0.8938 0.1954 0.1351 0.123 Uiso 1 1 calc R . .
C33 C 1.0257(3) 0.2921(3) 0.2578(2) 0.0888(8) Uani 1 1 d . . .
H33A H 1.0665 0.2380 0.2611 0.107 Uiso 1 1 calc R . .
C34 C 1.0666(2) 0.3958(2) 0.32591(19) 0.0666(6) Uani 1 1 d . . .
H34A H 1.1375 0.4149 0.3769 0.080 Uiso 1 1 calc R . .
C35 C 1.00580(18) 0.47341(19) 0.32139(15) 0.0517(5) Uani 1 1 d . . .
H35A H 1.0373 0.5454 0.3698 0.062 Uiso 1 1 calc R . .
C36 C 0.79510(16) 0.54969(16) 0.13585(13) 0.0429(4) Uani 1 1 d . . .
C37 C 0.68436(18) 0.56222(19) 0.09188(15) 0.0530(5) Uani 1 1 d . . .
H37A H 0.6153 0.5558 0.1225 0.064 Uiso 1 1 calc R . .
C38 C 0.6716(2) 0.5836(2) 0.00523(17) 0.0645(6) Uani 1 1 d . . .
H38A H 0.5948 0.5917 -0.0218 0.077 Uiso 1 1 calc R . .
C39 C 0.7693(2) 0.5932(2) -0.04168(16) 0.0638(6) Uani 1 1 d . . .
H39A H 0.7607 0.6078 -0.1008 0.077 Uiso 1 1 calc R . .
C40 C 0.8807(2) 0.5811(2) -0.00070(15) 0.0564(5) Uani 1 1 d . . .
H40A H 0.9493 0.5876 -0.0318 0.068 Uiso 1 1 calc R . .
C41 C 0.89184(18) 0.55940(17) 0.08562(13) 0.0473(4) Uani 1 1 d . . .
H41A H 0.9686 0.5508 0.1119 0.057 Uiso 1 1 calc R . .
C42 C 0.67741(18) 0.48245(19) 0.26623(16) 0.0538(5) Uani 1 1 d . . .
C43 C 0.6338(2) 0.5346(2) 0.3413(2) 0.0766(7) Uani 1 1 d . . .
H43 H 0.6870 0.6072 0.3841 0.092 Uiso 1 1 calc R . .
C44 C 0.5121(3) 0.4822(3) 0.3555(3) 0.1117(10) Uani 1 1 d . . .
H44 H 0.4851 0.5198 0.4079 0.134 Uiso 1 1 calc R . .
C45 C 0.4321(3) 0.3776(3) 0.2948(3) 0.1165(12) Uani 1 1 d . . .
H45 H 0.3498 0.3430 0.3043 0.140 Uiso 1 1 calc R . .
C46 C 0.4727(3) 0.3253(4) 0.2218(3) 0.1176(14) Uani 1 1 d . . .
H46 H 0.4194 0.2521 0.1800 0.141 Uiso 1 1 calc R . .
C47 C 0.5918(3) 0.3771(3) 0.2067(2) 0.0887(9) Uani 1 1 d . . .
H47 H 0.6160 0.3388 0.1530 0.106 Uiso 1 1 calc R . .
C48 C 0.89951(17) 0.66590(18) 0.31919(13) 0.0472(4) Uani 1 1 d . . .
C49 C 0.9294(2) 0.6870(2) 0.41770(15) 0.0661(6) Uani 1 1 d . . .
H49A H 0.8986 0.6254 0.4420 0.079 Uiso 1 1 calc R . .
C50 C 1.0029(3) 0.7951(3) 0.48157(18) 0.0844(9) Uani 1 1 d . . .
H50A H 1.0218 0.8054 0.5477 0.101 Uiso 1 1 calc R . .
C51 C 1.0480(2) 0.8866(3) 0.4488(2) 0.0795(8) Uani 1 1 d . . .
H51A H 1.0982 0.9600 0.4920 0.095 Uiso 1 1 calc R . .
C52 C 1.0198(2) 0.8705(2) 0.35389(19) 0.0653(6) Uani 1 1 d . . .
H52A H 1.0496 0.9332 0.3306 0.078 Uiso 1 1 calc R . .
C53 C 0.94724(16) 0.76231(18) 0.29045(15) 0.0492(4) Uani 1 1 d . . .
H53A H 0.9294 0.7537 0.2246 0.059 Uiso 1 1 calc R . .
C61A C 0.9824(6) -0.0303(6) 0.0796(4) 0.157(2) Uani 0.50 1 d P A 1
H61A H 0.9881 -0.1069 0.0728 0.189 Uiso 0.50 1 calc PR A 1
H61B H 0.9679 -0.0008 0.1434 0.189 Uiso 0.50 1 calc PR A 1
C62 C 1.1050(5) 0.0462(7) 0.0730(5) 0.231(3) Uani 0.50 1 d P . 1
H62A H 1.1118 0.1257 0.1053 0.278 Uiso 0.50 1 calc PR . 1
H62B H 1.1739 0.0306 0.1099 0.278 Uiso 0.50 1 calc PR . 1
C63A C 0.8724(5) -0.0419(7) 0.0083(5) 0.176(3) Uani 0.50 1 d P . 1
H63A H 0.8017 -0.1125 0.0024 0.211 Uiso 0.50 1 calc PR . 1
H63B H 0.8436 0.0236 0.0307 0.211 Uiso 0.50 1 calc PR . 1
O62 O 1.1050(5) 0.0462(7) 0.0730(5) 0.231(3) Uani 0.50 1 d P . 2
C61B C 0.9824(6) -0.0303(6) 0.0796(4) 0.157(2) Uani 0.50 1 d P B 2
H61C H 0.9881 -0.1069 0.0728 0.189 Uiso 0.50 1 calc PR B 2
H61D H 0.9679 -0.0008 0.1434 0.189 Uiso 0.50 1 calc PR B 2
C63B C 0.8724(5) -0.0419(7) 0.0083(5) 0.176(3) Uani 0.50 1 d P . 2
H63C H 0.8017 -0.1125 0.0024 0.211 Uiso 0.50 1 calc PR . 2
H63D H 0.8436 0.0236 0.0307 0.211 Uiso 0.50 1 calc PR . 2
B1 B 0.81789(18) 0.53846(19) 0.24351(14) 0.0430(4) Uani 1 1 d . . .
N1 N 0.49676(14) 0.89307(14) 0.17054(9) 0.0417(3) Uani 1 1 d . . .
N2 N 0.54279(15) 0.86471(14) 0.37154(10) 0.0446(3) Uani 1 1 d . . .
H2 H 0.5594 0.9068 0.4352 0.053 Uiso 1 1 calc R . .
N3 N 0.26931(14) 0.81438(14) 0.25772(10) 0.0437(3) Uani 1 1 d . . .
H3 H 0.2206 0.8459 0.2941 0.052 Uiso 1 1 calc R . .
N5 N 0.60834(14) 1.09969(15) 0.34952(11) 0.0469(4) Uani 1 1 d . . .
O20 O 0.37959(11) 1.03084(11) 0.41836(8) 0.0418(3) Uani 1 1 d . . .
O21 O 0.34288(12) 1.05251(11) 0.27770(8) 0.0439(3) 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 N2 2.0573(16) . ?
Ni1 N3 2.0914(15) . ?
Ni1 N1 2.1126(14) . ?
Ni1 O21 2.1310(14) . ?
Ni1 N5 2.1312(16) . ?
Ni1 O20 2.1781(12) . ?
Ni1 C20 2.4833(19) . ?
C1 N1 1.497(2) . ?
C1 C2 1.525(3) . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
C2 C3 1.514(3) . ?
C2 H2B 0.9900 . ?
C2 H2A 0.9900 . ?
C3 N2 1.489(3) . ?
C3 H3B 0.9900 . ?
C3 H3A 0.9900 . ?
C4 N2 1.481(3) . ?
C4 C5 1.522(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.519(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N3 1.471(3) . ?
C6 H6B 0.9900 . ?
C6 H6A 0.9900 . ?
C7 N3 1.489(2) . ?
C7 C8 1.527(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.526(3) . ?
C8 H8B 0.9900 . ?
C8 H8A 0.9900 . ?
C9 N1 1.483(2) . ?
C9 H9B 0.9900 . ?
C9 H9A 0.9900 . ?
C10 N1 1.491(2) . ?
C10 C11 1.526(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C11 1.517(4) 2_675 ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C15 N5 1.136(2) . ?
C15 C16 1.451(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C20 O21 1.259(2) . ?
C20 O20 1.272(2) . ?
C20 C21 1.505(3) . ?
C21 H21C 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21A 0.9800 . ?
C30 C31 1.390(3) . ?
C30 C35 1.400(3) . ?
C30 B1 1.661(3) . ?
C31 C32 1.379(4) . ?
C31 H31A 0.9500 . ?
C32 C33 1.383(4) . ?
C32 H32A 0.9500 . ?
C33 C34 1.359(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.380(3) . ?
C34 H34A 0.9500 . ?
C35 H35A 0.9500 . ?
C36 C41 1.401(3) . ?
C36 C37 1.403(3) . ?
C36 B1 1.648(3) . ?
C37 C38 1.392(3) . ?
C37 H37A 0.9500 . ?
C38 C39 1.378(4) . ?
C38 H38A 0.9500 . ?
C39 C40 1.391(3) . ?
C39 H39A 0.9500 . ?
C40 C41 1.388(3) . ?
C40 H40A 0.9500 . ?
C41 H41A 0.9500 . ?
C42 C43 1.385(4) . ?
C42 C47 1.392(4) . ?
C42 B1 1.656(3) . ?
C43 C44 1.410(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.373(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.343(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.389(4) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C53 1.400(3) . ?
C48 C49 1.404(3) . ?
C48 B1 1.642(3) . ?
C49 C50 1.400(4) . ?
C49 H49A 0.9500 . ?
C50 C51 1.379(5) . ?
C50 H50A 0.9500 . ?
C51 C52 1.361(4) . ?
C51 H51A 0.9500 . ?
C52 C53 1.397(3) . ?
C52 H52A 0.9500 . ?
C53 H53A 0.9500 . ?
C61A C63A 1.464(7) . ?
C61A C62 1.473(8) . ?
C61A H61A 0.9900 . ?
C61A H61B 0.9900 . ?
C62 C63A 1.269(8) 2_755 ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63A C62 1.270(8) 2_755 ?
C63A H63A 0.9900 . ?
C63A H63B 0.9900 . ?
N2 H2 0.9300 . ?
N3 H3 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 Ni1 N3 96.91(6) . . ?
N2 Ni1 N1 96.74(6) . . ?
N3 Ni1 N1 93.41(6) . . ?
N2 Ni1 O21 160.19(5) . . ?
N3 Ni1 O21 85.10(6) . . ?
N1 Ni1 O21 102.82(5) . . ?
N2 Ni1 N5 92.00(6) . . ?
N3 Ni1 N5 169.01(7) . . ?
N1 Ni1 N5 91.90(6) . . ?
O21 Ni1 N5 84.34(6) . . ?
N2 Ni1 O20 99.05(5) . . ?
N3 Ni1 O20 88.09(6) . . ?
N1 Ni1 O20 163.84(6) . . ?
O21 Ni1 O20 61.24(5) . . ?
N5 Ni1 O20 84.16(6) . . ?
N2 Ni1 C20 129.79(6) . . ?
N3 Ni1 C20 86.50(6) . . ?
N1 Ni1 C20 133.20(6) . . ?
O21 Ni1 C20 30.46(5) . . ?
N5 Ni1 C20 82.85(6) . . ?
O20 Ni1 C20 30.79(5) . . ?
N1 C1 C2 115.37(17) . . ?
N1 C1 H1B 108.4 . . ?
C2 C1 H1B 108.4 . . ?
N1 C1 H1A 108.4 . . ?
C2 C1 H1A 108.4 . . ?
H1B C1 H1A 107.5 . . ?
C3 C2 C1 116.48(19) . . ?
C3 C2 H2B 108.2 . . ?
C1 C2 H2B 108.2 . . ?
C3 C2 H2A 108.2 . . ?
C1 C2 H2A 108.2 . . ?
H2B C2 H2A 107.3 . . ?
N2 C3 C2 113.60(16) . . ?
N2 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
N2 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
H3B C3 H3A 107.7 . . ?
N2 C4 C5 114.24(18) . . ?
N2 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
N2 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C6 C5 C4 114.46(17) . . ?
C6 C5 H5A 108.6 . . ?
C4 C5 H5A 108.6 . . ?
C6 C5 H5B 108.6 . . ?
C4 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N3 C6 C5 110.63(16) . . ?
N3 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
N3 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
H6B C6 H6A 108.1 . . ?
N3 C7 C8 113.00(17) . . ?
N3 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
N3 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 C7 117.46(15) . . ?
C9 C8 H8B 107.9 . . ?
C7 C8 H8B 107.9 . . ?
C9 C8 H8A 107.9 . . ?
C7 C8 H8A 107.9 . . ?
H8B C8 H8A 107.2 . . ?
N1 C9 C8 116.32(17) . . ?
N1 C9 H9B 108.2 . . ?
C8 C9 H9B 108.2 . . ?
N1 C9 H9A 108.2 . . ?
C8 C9 H9A 108.2 . . ?
H9B C9 H9A 107.4 . . ?
N1 C10 C11 116.86(16) . . ?
N1 C10 H10A 108.1 . . ?
C11 C10 H10A 108.1 . . ?
N1 C10 H10B 108.1 . . ?
C11 C10 H10B 108.1 . . ?
H10A C10 H10B 107.3 . . ?
C11 C11 C10 110.1(2) 2_675 . ?
C11 C11 H11A 109.6 2_675 . ?
C10 C11 H11A 109.6 . . ?
C11 C11 H11B 109.6 2_675 . ?
C10 C11 H11B 109.6 . . ?
H11A C11 H11B 108.2 . . ?
N5 C15 C16 179.5(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O21 C20 O20 120.31(17) . . ?
O21 C20 C21 119.59(16) . . ?
O20 C20 C21 120.09(16) . . ?
O21 C20 Ni1 59.10(10) . . ?
O20 C20 Ni1 61.23(9) . . ?
C21 C20 Ni1 177.82(14) . . ?
C20 C21 H21C 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21C C21 H21B 109.5 . . ?
C20 C21 H21A 109.5 . . ?
H21C C21 H21A 109.5 . . ?
H21B C21 H21A 109.5 . . ?
C31 C30 C35 113.9(2) . . ?
C31 C30 B1 120.40(17) . . ?
C35 C30 B1 125.63(17) . . ?
C32 C31 C30 123.3(2) . . ?
C32 C31 H31A 118.3 . . ?
C30 C31 H31A 118.3 . . ?
C31 C32 C33 120.3(3) . . ?
C31 C32 H32A 119.9 . . ?
C33 C32 H32A 119.9 . . ?
C34 C33 C32 118.5(3) . . ?
C34 C33 H33A 120.7 . . ?
C32 C33 H33A 120.7 . . ?
C33 C34 C35 120.4(2) . . ?
C33 C34 H34A 119.8 . . ?
C35 C34 H34A 119.8 . . ?
C34 C35 C30 123.5(2) . . ?
C34 C35 H35A 118.3 . . ?
C30 C35 H35A 118.3 . . ?
C41 C36 C37 114.98(18) . . ?
C41 C36 B1 121.54(16) . . ?
C37 C36 B1 123.16(17) . . ?
C38 C37 C36 122.7(2) . . ?
C38 C37 H37A 118.7 . . ?
C36 C37 H37A 118.7 . . ?
C39 C38 C37 120.6(2) . . ?
C39 C38 H38A 119.7 . . ?
C37 C38 H38A 119.7 . . ?
C38 C39 C40 118.7(2) . . ?
C38 C39 H39A 120.7 . . ?
C40 C39 H39A 120.7 . . ?
C41 C40 C39 120.1(2) . . ?
C41 C40 H40A 120.0 . . ?
C39 C40 H40A 120.0 . . ?
C40 C41 C36 123.06(19) . . ?
C40 C41 H41A 118.5 . . ?
C36 C41 H41A 118.5 . . ?
C43 C42 C47 115.0(2) . . ?
C43 C42 B1 124.6(2) . . ?
C47 C42 B1 120.4(2) . . ?
C42 C43 C44 121.4(3) . . ?
C42 C43 H43 119.3 . . ?
C44 C43 H43 119.3 . . ?
C45 C44 C43 121.0(3) . . ?
C45 C44 H44 119.5 . . ?
C43 C44 H44 119.5 . . ?
C46 C45 C44 118.5(3) . . ?
C46 C45 H45 120.7 . . ?
C44 C45 H45 120.7 . . ?
C45 C46 C47 120.7(4) . . ?
C45 C46 H46 119.6 . . ?
C47 C46 H46 119.6 . . ?
C46 C47 C42 123.3(4) . . ?
C46 C47 H47 118.3 . . ?
C42 C47 H47 118.3 . . ?
C53 C48 C49 114.4(2) . . ?
C53 C48 B1 122.61(17) . . ?
C49 C48 B1 123.0(2) . . ?
C50 C49 C48 122.6(3) . . ?
C50 C49 H49A 118.7 . . ?
C48 C49 H49A 118.7 . . ?
C51 C50 C49 120.2(3) . . ?
C51 C50 H50A 119.9 . . ?
C49 C50 H50A 119.9 . . ?
C52 C51 C50 119.1(2) . . ?
C52 C51 H51A 120.4 . . ?
C50 C51 H51A 120.4 . . ?
C51 C52 C53 120.4(3) . . ?
C51 C52 H52A 119.8 . . ?
C53 C52 H52A 119.8 . . ?
C52 C53 C48 123.2(2) . . ?
C52 C53 H53A 118.4 . . ?
C48 C53 H53A 118.4 . . ?
C63A C61A C62 114.2(4) . . ?
C63A C61A H61A 108.7 . . ?
C62 C61A H61A 108.7 . . ?
C63A C61A H61B 108.7 . . ?
C62 C61A H61B 108.7 . . ?
H61A C61A H61B 107.6 . . ?
C63A C62 C61A 119.0(6) 2_755 . ?
C63A C62 H62A 107.6 2_755 . ?
C61A C62 H62A 107.6 . . ?
C63A C62 H62B 107.6 2_755 . ?
C61A C62 H62B 107.6 . . ?
H62A C62 H62B 107.0 . . ?
C62 C63A C61A 113.9(6) 2_755 . ?
C62 C63A H63A 108.8 2_755 . ?
C61A C63A H63A 108.8 . . ?
C62 C63A H63B 108.8 2_755 . ?
C61A C63A H63B 108.8 . . ?
H63A C63A H63B 107.7 . . ?
C48 B1 C36 108.59(16) . . ?
C48 B1 C42 112.03(16) . . ?
C36 B1 C42 108.86(14) . . ?
C48 B1 C30 109.25(14) . . ?
C36 B1 C30 109.67(15) . . ?
C42 B1 C30 108.41(16) . . ?
C9 N1 C10 111.55(13) . . ?
C9 N1 C1 108.88(16) . . ?
C10 N1 C1 108.71(15) . . ?
C9 N1 Ni1 110.29(11) . . ?
C10 N1 Ni1 106.65(11) . . ?
C1 N1 Ni1 110.74(10) . . ?
C4 N2 C3 111.00(17) . . ?
C4 N2 Ni1 119.07(12) . . ?
C3 N2 Ni1 113.08(12) . . ?
C4 N2 H2 103.9 . . ?
C3 N2 H2 103.9 . . ?
Ni1 N2 H2 103.9 . . ?
C6 N3 C7 113.03(15) . . ?
C6 N3 Ni1 122.45(12) . . ?
C7 N3 Ni1 110.06(11) . . ?
C6 N3 H3 102.8 . . ?
C7 N3 H3 102.8 . . ?
Ni1 N3 H3 102.8 . . ?
C15 N5 Ni1 164.65(16) . . ?
C20 O20 Ni1 87.98(10) . . ?
C20 O21 Ni1 90.44(11) . . ?

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
N1 C1 C2 C3 -68.9(3) . . . . ?
C1 C2 C3 N2 68.6(3) . . . . ?
N2 C4 C5 C6 75.9(2) . . . . ?
C4 C5 C6 N3 -72.7(2) . . . . ?
N3 C7 C8 C9 -27.8(3) . . . . ?
C7 C8 C9 N1 -48.2(3) . . . . ?
N1 C10 C11 C11 179.87(19) . . . 2_675 ?
N2 Ni1 C20 O21 177.63(9) . . . . ?
N3 Ni1 C20 O21 -86.29(10) . . . . ?
N1 Ni1 C20 O21 5.11(13) . . . . ?
N5 Ni1 C20 O21 90.99(10) . . . . ?
O20 Ni1 C20 O21 -178.43(16) . . . . ?
N2 Ni1 C20 O20 -3.94(13) . . . . ?
N3 Ni1 C20 O20 92.14(10) . . . . ?
N1 Ni1 C20 O20 -176.46(9) . . . . ?
O21 Ni1 C20 O20 178.43(16) . . . . ?
N5 Ni1 C20 O20 -90.58(10) . . . . ?
N2 Ni1 C20 C21 124(3) . . . . ?
N3 Ni1 C20 C21 -140(4) . . . . ?
N1 Ni1 C20 C21 -49(4) . . . . ?
O21 Ni1 C20 C21 -54(3) . . . . ?
N5 Ni1 C20 C21 37(4) . . . . ?
O20 Ni1 C20 C21 128(4) . . . . ?
C35 C30 C31 C32 2.2(4) . . . . ?
B1 C30 C31 C32 -176.1(3) . . . . ?
C30 C31 C32 C33 -1.0(6) . . . . ?
C31 C32 C33 C34 -0.7(6) . . . . ?
C32 C33 C34 C35 0.9(5) . . . . ?
C33 C34 C35 C30 0.6(4) . . . . ?
C31 C30 C35 C34 -2.1(3) . . . . ?
B1 C30 C35 C34 176.2(2) . . . . ?
C41 C36 C37 C38 -0.5(3) . . . . ?
B1 C36 C37 C38 173.1(2) . . . . ?
C36 C37 C38 C39 0.2(4) . . . . ?
C37 C38 C39 C40 0.0(4) . . . . ?
C38 C39 C40 C41 0.2(3) . . . . ?
C39 C40 C41 C36 -0.6(3) . . . . ?
C37 C36 C41 C40 0.7(3) . . . . ?
B1 C36 C41 C40 -172.99(19) . . . . ?
C47 C42 C43 C44 1.0(4) . . . . ?
B1 C42 C43 C44 179.2(2) . . . . ?
C42 C43 C44 C45 -0.4(5) . . . . ?
C43 C44 C45 C46 0.7(5) . . . . ?
C44 C45 C46 C47 -1.5(6) . . . . ?
C45 C46 C47 C42 2.2(6) . . . . ?
C43 C42 C47 C46 -1.8(5) . . . . ?
B1 C42 C47 C46 179.8(3) . . . . ?
C53 C48 C49 C50 -1.1(3) . . . . ?
B1 C48 C49 C50 177.7(2) . . . . ?
C48 C49 C50 C51 0.7(4) . . . . ?
C49 C50 C51 C52 0.2(4) . . . . ?
C50 C51 C52 C53 -0.7(4) . . . . ?
C51 C52 C53 C48 0.3(3) . . . . ?
C49 C48 C53 C52 0.6(3) . . . . ?
B1 C48 C53 C52 -178.17(18) . . . . ?
C63A C61A C62 C63A -40.9(12) . . . 2_755 ?
C62 C61A C63A C62 38.8(12) . . . 2_755 ?
C53 C48 B1 C36 -4.6(2) . . . . ?
C49 C48 B1 C36 176.69(18) . . . . ?
C53 C48 B1 C42 -124.88(19) . . . . ?
C49 C48 B1 C42 56.4(2) . . . . ?
C53 C48 B1 C30 114.97(19) . . . . ?
C49 C48 B1 C30 -63.7(2) . . . . ?
C41 C36 B1 C48 78.2(2) . . . . ?
C37 C36 B1 C48 -95.0(2) . . . . ?
C41 C36 B1 C42 -159.57(18) . . . . ?
C37 C36 B1 C42 27.3(3) . . . . ?
C41 C36 B1 C30 -41.1(2) . . . . ?
C37 C36 B1 C30 145.73(18) . . . . ?
C43 C42 B1 C48 -1.5(3) . . . . ?
C47 C42 B1 C48 176.7(2) . . . . ?
C43 C42 B1 C36 -121.6(2) . . . . ?
C47 C42 B1 C36 56.6(3) . . . . ?
C43 C42 B1 C30 119.1(2) . . . . ?
C47 C42 B1 C30 -62.7(3) . . . . ?
C31 C30 B1 C48 -167.6(2) . . . . ?
C35 C30 B1 C48 14.3(3) . . . . ?
C31 C30 B1 C36 -48.7(3) . . . . ?
C35 C30 B1 C36 133.17(19) . . . . ?
C31 C30 B1 C42 70.1(3) . . . . ?
C35 C30 B1 C42 -108.1(2) . . . . ?
C8 C9 N1 C10 -53.9(2) . . . . ?
C8 C9 N1 C1 -173.82(16) . . . . ?
C8 C9 N1 Ni1 64.48(17) . . . . ?
C11 C10 N1 C9 -59.9(2) . . . . ?
C11 C10 N1 C1 60.2(2) . . . . ?
C11 C10 N1 Ni1 179.59(13) . . . . ?
C2 C1 N1 C9 -65.7(2) . . . . ?
C2 C1 N1 C10 172.60(17) . . . . ?
C2 C1 N1 Ni1 55.7(2) . . . . ?
N2 Ni1 N1 C9 79.38(12) . . . . ?
N3 Ni1 N1 C9 -18.00(13) . . . . ?
O21 Ni1 N1 C9 -103.74(12) . . . . ?
N5 Ni1 N1 C9 171.62(12) . . . . ?
O20 Ni1 N1 C9 -112.9(2) . . . . ?
C20 Ni1 N1 C9 -106.40(13) . . . . ?
N2 Ni1 N1 C10 -159.33(11) . . . . ?
N3 Ni1 N1 C10 103.29(11) . . . . ?
O21 Ni1 N1 C10 17.55(11) . . . . ?
N5 Ni1 N1 C10 -67.09(11) . . . . ?
O20 Ni1 N1 C10 8.4(2) . . . . ?
C20 Ni1 N1 C10 14.89(14) . . . . ?
N2 Ni1 N1 C1 -41.21(14) . . . . ?
N3 Ni1 N1 C1 -138.60(14) . . . . ?
O21 Ni1 N1 C1 135.66(13) . . . . ?
N5 Ni1 N1 C1 51.03(14) . . . . ?
O20 Ni1 N1 C1 126.49(19) . . . . ?
C20 Ni1 N1 C1 133.01(13) . . . . ?
C5 C4 N2 C3 -169.64(16) . . . . ?
C5 C4 N2 Ni1 -35.7(2) . . . . ?
C2 C3 N2 C4 79.0(2) . . . . ?
C2 C3 N2 Ni1 -57.9(2) . . . . ?
N3 Ni1 N2 C4 4.16(15) . . . . ?
N1 Ni1 N2 C4 -90.12(15) . . . . ?
O21 Ni1 N2 C4 98.9(2) . . . . ?
N5 Ni1 N2 C4 177.72(14) . . . . ?
O20 Ni1 N2 C4 93.32(14) . . . . ?
C20 Ni1 N2 C4 95.36(15) . . . . ?
N3 Ni1 N2 C3 137.20(13) . . . . ?
N1 Ni1 N2 C3 42.92(13) . . . . ?
O21 Ni1 N2 C3 -128.06(17) . . . . ?
N5 Ni1 N2 C3 -49.24(13) . . . . ?
O20 Ni1 N2 C3 -133.64(12) . . . . ?
C20 Ni1 N2 C3 -131.60(12) . . . . ?
C5 C6 N3 C7 169.18(17) . . . . ?
C5 C6 N3 Ni1 33.8(2) . . . . ?
C8 C7 N3 C6 -70.7(2) . . . . ?
C8 C7 N3 Ni1 70.22(19) . . . . ?
N2 Ni1 N3 C6 -3.79(15) . . . . ?
N1 Ni1 N3 C6 93.43(15) . . . . ?
O21 Ni1 N3 C6 -163.98(15) . . . . ?
N5 Ni1 N3 C6 -147.8(3) . . . . ?
O20 Ni1 N3 C6 -102.68(14) . . . . ?
C20 Ni1 N3 C6 -133.47(15) . . . . ?
N2 Ni1 N3 C7 -140.33(13) . . . . ?
N1 Ni1 N3 C7 -43.11(14) . . . . ?
O21 Ni1 N3 C7 59.49(13) . . . . ?
N5 Ni1 N3 C7 75.7(3) . . . . ?
O20 Ni1 N3 C7 120.78(13) . . . . ?
C20 Ni1 N3 C7 90.00(13) . . . . ?
C16 C15 N5 Ni1 -26(34) . . . . ?
N2 Ni1 N5 C15 -149.7(6) . . . . ?
N3 Ni1 N5 C15 -5.4(8) . . . . ?
N1 Ni1 N5 C15 113.5(6) . . . . ?
O21 Ni1 N5 C15 10.8(6) . . . . ?
O20 Ni1 N5 C15 -50.8(6) . . . . ?
C20 Ni1 N5 C15 -19.9(6) . . . . ?
O21 C20 O20 Ni1 1.56(16) . . . . ?
C21 C20 O20 Ni1 -178.01(16) . . . . ?
N2 Ni1 O20 C20 176.94(10) . . . . ?
N3 Ni1 O20 C20 -86.37(11) . . . . ?
N1 Ni1 O20 C20 9.3(2) . . . . ?
O21 Ni1 O20 C20 -0.91(9) . . . . ?
N5 Ni1 O20 C20 85.83(11) . . . . ?
O20 C20 O21 Ni1 -1.60(16) . . . . ?
C21 C20 O21 Ni1 177.98(15) . . . . ?
N2 Ni1 O21 C20 -5.4(2) . . . . ?
N3 Ni1 O21 C20 91.42(11) . . . . ?
N1 Ni1 O21 C20 -176.18(10) . . . . ?
N5 Ni1 O21 C20 -85.51(11) . . . . ?
O20 Ni1 O21 C20 0.92(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.915
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.915
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.061
