# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_complex4
_database_code_depnum_ccdc_archive 'CCDC 1045910'
_audit_update_record             
;
2016-03-11 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Ni2(NO3)3(L-chloro)](H2O)0.7'
_chemical_formula_moiety         'C24 H28 Cl N7 Ni2 O10, 0.7(H2 O)'
_chemical_formula_sum            'C24 H29.40 Cl N7 Ni2 O10.70'
_chemical_formula_weight         739.98

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'
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'
Cl Cl 0.1484 0.1585 '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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_mame_Hall  '-P 2yn'

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                   10.6743(11)
_cell_length_b                   15.6272(17)
_cell_length_c                   18.068(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.609(3)
_cell_angle_gamma                90.00
_cell_volume                     2987.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4000
_cell_measurement_theta_min      1.75
_cell_measurement_theta_max      26.00

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1524
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7210
_exptl_absorpt_correction_T_max  0.8582
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36623
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         27.00
_reflns_number_total             6426
_reflns_number_gt                5272
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX-2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0557P)²+1.6707P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6426
_refine_ls_number_parameters     414
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.1044
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.046
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.57309(3) 0.860336(19) 0.133059(18) 0.03615(10) Uani 1 d . . .
Ni1 Ni 0.36272(3) 0.73117(2) 0.215136(17) 0.03579(10) Uani 1 d . . .
Cl1 Cl 0.72223(11) 0.43873(6) 0.03333(7) 0.0901(3) Uani 1 d . . .
O1 O 0.50147(15) 0.74375(10) 0.15376(9) 0.0328(3) Uani 1 d . . .
O3 O 0.39277(18) 0.89721(13) 0.08347(11) 0.0510(5) Uani 1 d . . .
O2 O 0.29090(18) 0.85720(12) 0.17558(11) 0.0458(4) Uani 1 d . . .
O4 O 0.2044(2) 0.94055(18) 0.08853(16) 0.0831(8) Uani 1 d . . .
O9 O 0.6279(2) 0.98947(13) 0.12861(12) 0.0559(5) Uani 1 d . . .
O8 O 0.54138(18) 0.94843(13) 0.22364(11) 0.0517(5) Uani 1 d . . .
O10 O 0.6006(3) 1.08076(15) 0.21575(17) 0.0884(8) Uani 1 d . . .
O6 O 0.44160(18) 0.80881(14) 0.31033(11) 0.0521(8) Uani 1 d . . .
O5 O 0.25178(18) 0.76090(14) 0.29855(11) 0.0525(5) Uani 1 d . . .
O7 O 0.3152(3) 0.8477(2) 0.38899(14) 0.0892(9) Uani 1 d . . .
O11 O 0.2358(5) 0.8588(3) -0.0703(3) 0.1086(16) Uani 0.70 d PD . .
H91 H 0.201(8) 0.890(4) -0.042(4) 0.141 Uiso 0.70 d PD . .
H92 H 0.270(7) 0.888(4) -0.100(3) 0.141 Uiso 0.70 d PD . .
N3 N 0.6258(2) 0.82493(14) 0.03062(12) 0.0400(5) Uani 1 d . . .
N4 N 0.74372(18) 0.83382(13) 0.19295(12) 0.0397(5) Uani 1 d . . .
N1 N 0.4297(2) 0.61554(14) 0.26631(12) 0.0412(5) Uani 1 d . . .
N2 N 0.2241(2) 0.67302(14) 0.14158(12) 0.0407(5) Uani 1 d . . .
N5 N 0.2964(2) 0.89922(14) 0.11691(13) 0.0446(5) Uani 1 d . . .
N7 N 0.5900(2) 1.00906(15) 0.19111(15) 0.0531(6) Uani 1 d . . .
N6 N 0.3360(2) 0.80804(17) 0.33472(13) 0.0512(6) Uani 1 d . . .
C1 C 0.5511(2) 0.67325(15) 0.12596(13) 0.0327(5) Uani 1 d . . .
C2 C 0.5797(2) 0.60105(16) 0.17086(15) 0.0391(5) Uani 1 d . . .
C3 C 0.6310(3) 0.52904(17) 0.14147(18) 0.0505(7) Uani 1 d . . .
H3 H 0.6495 0.4809 0.1712 0.061 Uiso 1 calc R . .
C4 C 0.6542(3) 0.52867(17) 0.0689(2) 0.0555(8) Uani 1 d . . .
C5 C 0.6274(3) 0.59832(19) 0.02414(17) 0.0503(7) Uani 1 d . . .
H5 H 0.6437 0.5967 -0.0251 0.060 Uiso 1 calc R . .
C6 C 0.5758(2) 0.67183(17) 0.05145(14) 0.0393(5) Uani 1 d . . .
C7 C 0.5489(3) 0.74910(19) 0.00317(14) 0.0460(6) Uani 1 d . . .
H7A H 0.5654 0.7356 -0.0470 0.055 Uiso 1 calc R . .
H7B H 0.4600 0.7634 0.0007 0.055 Uiso 1 calc R . .
C8 C 0.5939(3) 0.8960(2) -0.02322(18) 0.0632(9) Uani 1 d . . .
H8A H 0.6110 0.8787 -0.0718 0.095 Uiso 1 calc R . .
H8B H 0.6440 0.9453 -0.0073 0.095 Uiso 1 calc R . .
H8C H 0.5059 0.9100 -0.0253 0.095 Uiso 1 calc R . .
C9 C 0.7634(3) 0.80506(18) 0.03320(16) 0.0471(6) Uani 1 d . . .
H9A H 0.7862 0.8093 -0.0169 0.057 Uiso 1 calc R . .
H9B H 0.7782 0.7465 0.0499 0.057 Uiso 1 calc R . .
C10 C 0.8489(3) 0.86425(18) 0.08461(18) 0.0502(7) Uani 1 d . . .
H10A H 0.9335 0.8625 0.0706 0.060 Uiso 1 calc R . .
H10B H 0.8180 0.9225 0.0779 0.060 Uiso 1 calc R . .
C11 C 0.8545(2) 0.84021(16) 0.16514(16) 0.0430(6) Uani 1 d . . .
C12 C 0.9665(3) 0.8219(2) 0.2108(2) 0.0605(8) Uani 1 d . . .
H12 H 1.0433 0.8265 0.1920 0.073 Uiso 1 calc R . .
C13 C 0.9645(3) 0.7974(3) 0.2828(2) 0.0707(10) Uani 1 d . . .
H13 H 1.0396 0.7849 0.3131 0.085 Uiso 1 calc R . .
C14 C 0.8522(3) 0.7913(2) 0.31061(18) 0.0575(7) Uani 1 d . . .
H14 H 0.8493 0.7746 0.3597 0.069 Uiso 1 calc R . .
C15 C 0.7445(2) 0.81041(17) 0.26440(15) 0.0434(6) Uani 1 d . . .
H15 H 0.6678 0.8070 0.2833 0.052 Uiso 1 calc R . .
C16 C 0.5632(2) 0.60324(17) 0.25230(15) 0.0422(6) Uani 1 d . . .
H16A H 0.5946 0.5500 0.2753 0.051 Uiso 1 calc R . .
H16B H 0.6142 0.6493 0.2763 0.051 Uiso 1 calc R . .
C17 C 0.4342(3) 0.6169(2) 0.34909(16) 0.0564(7) Uani 1 d . . .
H17A H 0.3501 0.6237 0.3617 0.085 Uiso 1 calc R . .
H17B H 0.4859 0.6638 0.3693 0.085 Uiso 1 calc R . .
H17C H 0.4693 0.5641 0.3696 0.085 Uiso 1 calc R . .
C18 C 0.3510(3) 0.54181(17) 0.23596(17) 0.0485(6) Uani 1 d . . .
H18A H 0.3724 0.4922 0.2673 0.058 Uiso 1 calc R . .
H18B H 0.3705 0.5285 0.1863 0.058 Uiso 1 calc R . .
C19 C 0.2102(3) 0.5594(2) 0.23197(18) 0.0556(7) Uani 1 d . . .
H19A H 0.1658 0.5055 0.2344 0.067 Uiso 1 calc R . .
H19B H 0.1953 0.5934 0.2749 0.067 Uiso 1 calc R . .
C20 C 0.1577(2) 0.60565(19) 0.16222(16) 0.0477(6) Uani 1 d . . .
C21 C 0.0487(3) 0.5784(2) 0.1188(2) 0.0634(8) Uani 1 d . . .
H21 H 0.0034 0.5326 0.1345 0.076 Uiso 1 calc R . .
C22 C 0.0070(3) 0.6185(2) 0.0528(2) 0.0657(9) Uani 1 d . . .
H22 H -0.0669 0.6009 0.0237 0.079 Uiso 1 calc R . .
C23 C 0.0767(3) 0.6854(2) 0.03050(18) 0.0572(8) Uani 1 d . . .
H23 H 0.0514 0.7133 -0.0144 0.069 Uiso 1 calc R . .
C24 C 0.1842(3) 0.71038(17) 0.07540(16) 0.0469(6) Uani 1 d . . .
H24 H 0.2317 0.7551 0.0595 0.056 Uiso 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 O1 2.0296(16) . ?
Ni2 N4 2.034(2) . ?
Ni2 N3 2.079(2) . ?
Ni2 O3 2.0936(19) . ?
Ni2 O9 2.106(2) . ?
Ni2 O8 2.199(2) . ?
Ni1 O1 1.9741(15) . ?
Ni1 N2 2.064(2) . ?
Ni1 O5 2.0886(19) . ?
Ni1 N1 2.111(2) . ?
Ni1 O6 2.181(2) . ?
Ni1 O2 2.1981(18) . ?
Cl1 C4 1.743(3) . ?
O1 C1 1.348(3) . ?
O3 N5 1.261(3) . ?
O2 N5 1.255(3) . ?
O4 N5 1.229(3) . ?
O9 N7 1.286(3) . ?
O8 N7 1.262(3) . ?
O10 N7 1.205(3) . ?
O6 N6 1.263(3) . ?
O5 N6 1.274(3) . ?
O7 N6 1.205(3) . ?
N3 C8 1.486(3) . ?
N3 C7 1.489(4) . ?
N3 C9 1.497(3) . ?
N4 C15 1.341(3) . ?
N4 C11 1.348(3) . ?
N1 C18 1.487(4) . ?
N1 C17 1.490(3) . ?
N1 C16 1.492(3) . ?
N2 C24 1.348(4) . ?
N2 C20 1.349(4) . ?
C1 C2 1.399(3) . ?
C1 C6 1.406(3) . ?
C2 C3 1.387(4) . ?
C2 C16 1.505(4) . ?
C3 C4 1.367(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.363(4) . ?
C5 C6 1.392(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.495(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.525(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.496(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.390(4) . ?
C12 C13 1.359(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.362(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.361(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.520(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.496(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.381(4) . ?
C21 C22 1.368(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.374(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.371(4) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni2 N4 92.96(8) . . ?
O1 Ni2 N3 94.48(7) . . ?
N4 Ni2 N3 95.20(8) . . ?
O1 Ni2 O3 88.77(7) . . ?
N4 Ni2 O3 172.49(8) . . ?
N3 Ni2 O3 91.95(8) . . ?
O1 Ni2 O9 168.72(7) . . ?
N4 Ni2 O9 88.96(8) . . ?
N3 Ni2 O9 96.42(8) . . ?
O3 Ni2 O9 87.95(8) . . ?
O1 Ni2 O8 109.03(7) . . ?
N4 Ni2 O8 86.95(8) . . ?
N3 Ni2 O8 156.28(8) . . ?
O3 Ni2 O8 85.57(8) . . ?
O9 Ni2 O8 59.95(8) . . ?
O1 Ni1 N2 102.07(8) . . ?
O1 Ni1 O5 157.29(8) . . ?
N2 Ni1 O5 97.82(8) . . ?
O1 Ni1 N1 95.48(7) . . ?
N2 Ni1 N1 94.44(9) . . ?
O5 Ni1 N1 93.78(8) . . ?
O1 Ni1 O6 98.49(7) . . ?
N2 Ni1 O6 157.19(8) . . ?
O5 Ni1 O6 60.24(8) . . ?
N1 Ni1 O6 93.31(8) . . ?
O1 Ni1 O2 89.05(7) . . ?
N2 Ni1 O2 89.76(8) . . ?
O5 Ni1 O2 80.14(8) . . ?
N1 Ni1 O2 173.04(8) . . ?
O6 Ni1 O2 80.77(8) . . ?
C1 O1 Ni1 119.28(14) . . ?
C1 O1 Ni2 119.25(13) . . ?
Ni1 O1 Ni2 121.45(8) . . ?
N5 O3 Ni2 124.35(16) . . ?
N5 O2 Ni1 133.65(15) . . ?
C8 N3 C7 108.0(2) . . ?
C8 N3 C9 108.3(2) . . ?
C7 N3 C9 109.9(2) . . ?
C8 N3 Ni2 108.55(17) . . ?
C7 N3 Ni2 107.83(15) . . ?
C9 N3 Ni2 114.06(17) . . ?
C15 N4 C11 119.0(2) . . ?
C15 N4 Ni2 117.32(16) . . ?
C11 N4 Ni2 123.66(19) . . ?
C18 N1 C17 108.8(2) . . ?
C18 N1 C16 110.1(2) . . ?
C17 N1 C16 105.5(2) . . ?
C18 N1 Ni1 111.08(16) . . ?
C17 N1 Ni1 113.03(18) . . ?
C16 N1 Ni1 108.15(15) . . ?
C24 N2 C20 117.8(2) . . ?
C24 N2 Ni1 119.73(18) . . ?
C20 N2 Ni1 121.59(19) . . ?
O4 N5 O2 120.2(2) . . ?
O4 N5 O3 118.1(2) . . ?
O3 N5 O2 121.6(2) . . ?
O10 N7 O8 123.4(3) . . ?
O10 N7 O9 121.4(3) . . ?
O8 N7 O9 115.3(2) . . ?
O7 N6 O6 123.2(3) . . ?
O7 N6 O5 121.4(3) . . ?
O6 N6 O5 115.4(2) . . ?
O1 C1 C2 120.6(2) . . ?
O1 C1 C6 120.2(2) . . ?
C2 C1 C6 119.2(2) . . ?
C3 C2 C1 119.9(2) . . ?
C3 C2 C16 119.7(2) . . ?
C1 C2 C16 120.2(2) . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 121.0(2) . . ?
C5 C4 Cl1 119.4(2) . . ?
C3 C4 Cl1 119.6(2) . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.0(2) . . ?
C5 C6 C7 121.0(2) . . ?
C1 C6 C7 120.0(2) . . ?
N3 C7 C6 113.2(2) . . ?
N3 C7 H7A 108.9 . . ?
C6 C7 H7A 108.9 . . ?
N3 C7 H7B 108.9 . . ?
C6 C7 H7B 108.9 . . ?
H7A C7 H7B 107.8 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 113.5(2) . . ?
N3 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N3 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C11 C10 C9 112.6(2) . . ?
C11 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N4 C11 C12 119.4(3) . . ?
N4 C11 C10 117.2(2) . . ?
C12 C11 C10 123.3(2) . . ?
C13 C12 C11 120.3(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 119.9(3) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 118.1(3) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
N4 C15 C14 123.2(3) . . ?
N4 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
N1 C16 C2 114.0(2) . . ?
N1 C16 H16A 108.7 . . ?
C2 C16 H16A 108.7 . . ?
N1 C16 H16B 108.7 . . ?
C2 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C18 C19 112.6(2) . . ?
N1 C18 H18A 109.1 . . ?
C19 C18 H18A 109.1 . . ?
N1 C18 H18B 109.1 . . ?
C19 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C18 112.7(2) . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
N2 C20 C21 121.2(3) . . ?
N2 C20 C19 117.2(2) . . ?
C21 C20 C19 121.5(3) . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 118.6(3) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
C24 C23 C22 119.1(3) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
N2 C24 C23 122.9(3) . . ?
N2 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?

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
O1 C1 C2 C3 -179.9(2) . . . . ?
C6 C1 C2 C3 -0.5(4) . . . . ?
O1 C1 C2 C16 -3.9(3) . . . . ?
C6 C1 C2 C16 175.5(2) . . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
C16 C2 C3 C4 -175.6(3) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C2 C3 C4 Cl1 178.4(2) . . . . ?
C3 C4 C5 C6 0.2(5) . . . . ?
Cl1 C4 C5 C6 -178.5(2) . . . . ?
C4 C5 C6 C1 -0.3(4) . . . . ?
C4 C5 C6 C7 178.6(3) . . . . ?
O1 C1 C6 C5 179.9(2) . . . . ?
C2 C1 C6 C5 0.4(4) . . . . ?
O1 C1 C6 C7 0.9(3) . . . . ?
C2 C1 C6 C7 -178.5(2) . . . . ?
C8 N3 C7 C6 178.0(2) . . . . ?
C9 N3 C7 C6 60.0(3) . . . . ?
C5 C6 C7 N3 -116.1(3) . . . . ?
C1 C6 C7 N3 62.9(3) . . . . ?
C8 N3 C9 C10 82.5(3) . . . . ?
C7 N3 C9 C10 -159.7(2) . . . . ?
N3 C9 C10 C11 79.3(3) . . . . ?
C15 N4 C11 C12 0.4(4) . . . . ?
C15 N4 C11 C10 178.4(2) . . . . ?
C9 C10 C11 N4 -54.6(3) . . . . ?
C9 C10 C11 C12 123.4(3) . . . . ?
N4 C11 C12 C13 0.3(5) . . . . ?
C10 C11 C12 C13 -177.6(3) . . . . ?
C11 C12 C13 C14 -0.5(6) . . . . ?
C12 C13 C14 C15 -0.1(6) . . . . ?
C11 N4 C15 C14 -1.0(4) . . . . ?
C13 C14 C15 N4 0.8(5) . . . . ?
C18 N1 C16 C2 63.4(3) . . . . ?
C17 N1 C16 C2 -179.3(2) . . . . ?
C3 C2 C16 N1 -120.4(3) . . . . ?
C1 C2 C16 N1 63.6(3) . . . . ?
C17 N1 C18 C19 78.2(3) . . . . ?
C16 N1 C18 C19 -166.6(2) . . . . ?
N1 C18 C19 C20 84.5(3) . . . . ?
C24 N2 C20 C21 -3.2(4) . . . . ?
C24 N2 C20 C19 174.0(2) . . . . ?
C18 C19 C20 N2 -45.6(4) . . . . ?
C18 C19 C20 C21 131.7(3) . . . . ?
N2 C20 C21 C22 1.3(5) . . . . ?
C19 C20 C21 C22 -175.8(3) . . . . ?
C20 C21 C22 C23 0.8(5) . . . . ?
C21 C22 C23 C24 -0.9(5) . . . . ?
C20 N2 C24 C23 3.1(4) . . . . ?
C22 C23 C24 N2 -1.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.063
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex1
_database_code_depnum_ccdc_archive 'CCDC 1045911'
_audit_update_record             
;
2016-03-11 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Ni2(NO3)3(l-methyl)]'
_chemical_formula_moiety         'C25 H31 N7 Ni2 O10'
_chemical_formula_sum            'C25 H31 N7 Ni2 O10'
_chemical_formula_weight         706.95

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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   10.6333(13)
_cell_length_b                   15.630(2)
_cell_length_c                   18.033(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.823(2)
_cell_angle_gamma                90.00
_cell_volume                     2969.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3000
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      25.60

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7577
_exptl_absorpt_correction_T_max  0.8893
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20601
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.30
_reflns_number_total             5383
_reflns_number_gt                3902
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX-2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0580P)²+1.9779P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5383
_refine_ls_number_parameters     400
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.1316
_refine_ls_wR_factor_gt          0.1178
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
Ni2 Ni 0.92245(4) 0.63741(3) 0.36564(3) 0.03360(17) Uani 1 1 d . . .
Ni1 Ni 1.12742(5) 0.76739(3) 0.28209(3) 0.03367(16) Uani 1 1 d . . .
O1 O 0.9914(2) 0.75392(16) 0.34481(14) 0.0314(6) Uani 1 1 d . . .
O3 O 1.1054(3) 0.6024(2) 0.41515(15) 0.0454(7) Uani 1 1 d . . .
O2 O 1.2040(3) 0.64286(18) 0.32141(16) 0.0424(7) Uani 1 1 d . . .
O4 O 1.2929(3) 0.5575(2) 0.4061(2) 0.0739(11) Uani 1 1 d . . .
O8 O 0.9562(3) 0.55040(19) 0.27497(16) 0.0469(7) Uani 1 1 d . . .
O9 O 0.8704(3) 0.50802(19) 0.36989(17) 0.0494(8) Uani 1 1 d . . .
O10 O 0.9042(4) 0.4167(2) 0.2844(2) 0.0832(12) Uani 1 1 d . . .
O6 O 1.0461(3) 0.6899(2) 0.18682(16) 0.0505(8) Uani 1 1 d . . .
O5 O 1.2364(3) 0.7379(2) 0.19723(17) 0.0490(8) Uani 1 1 d . . .
O7 O 1.1702(4) 0.6506(3) 0.1069(2) 0.0881(13) Uani 1 1 d . . .
N3 N 0.8706(3) 0.6721(2) 0.46903(17) 0.0388(8) Uani 1 1 d . . .
N4 N 0.7500(3) 0.6642(2) 0.30645(19) 0.0379(8) Uani 1 1 d . . .
N1 N 1.0584(3) 0.8828(2) 0.23147(18) 0.0396(8) Uani 1 1 d . . .
N2 N 1.2670(3) 0.8255(2) 0.35507(17) 0.0357(8) Uani 1 1 d . . .
N5 N 1.2012(3) 0.6002(2) 0.3803(2) 0.0416(8) Uani 1 1 d . . .
N7 N 0.9097(3) 0.4890(2) 0.3085(2) 0.0507(10) Uani 1 1 d . . .
N6 N 1.1505(4) 0.6908(3) 0.16153(19) 0.0495(10) Uani 1 1 d . . .
C1 C 0.9411(3) 0.8244(2) 0.3736(2) 0.0308(8) Uani 1 1 d . . .
C2 C 0.9128(4) 0.8972(3) 0.3295(2) 0.0380(9) Uani 1 1 d . . .
C3 C 0.8633(4) 0.9685(3) 0.3601(3) 0.0496(11) Uani 1 1 d . . .
H3 H 0.8435 1.0163 0.3301 0.059 Uiso 1 1 calc R . .
C4 C 0.8421(4) 0.9711(3) 0.4347(3) 0.0554(13) Uani 1 1 d . . .
C5 C 0.8703(4) 0.8986(3) 0.4770(3) 0.0488(12) Uani 1 1 d . . .
H5 H 0.8552 0.8984 0.5266 0.059 Uiso 1 1 calc R . .
C6 C 0.9204(4) 0.8256(3) 0.4481(2) 0.0366(9) Uani 1 1 d . . .
C7 C 0.9468(4) 0.7476(3) 0.4959(2) 0.0443(11) Uani 1 1 d . . .
H7A H 1.0361 0.7333 0.4985 0.053 Uiso 1 1 calc R . .
H7B H 0.9306 0.7610 0.5463 0.053 Uiso 1 1 calc R . .
C8 C 0.9043(5) 0.6016(3) 0.5226(3) 0.0634(14) Uani 1 1 d . . .
H8A H 0.9925 0.5878 0.5239 0.095 Uiso 1 1 calc R . .
H8B H 0.8536 0.5523 0.5072 0.095 Uiso 1 1 calc R . .
H8C H 0.8886 0.6190 0.5716 0.095 Uiso 1 1 calc R . .
C9 C 0.7330(4) 0.6910(3) 0.4657(2) 0.0460(11) Uani 1 1 d . . .
H9A H 0.7178 0.7494 0.4487 0.055 Uiso 1 1 calc R . .
H9B H 0.7100 0.6869 0.5158 0.055 Uiso 1 1 calc R . .
C10 C 0.6476(4) 0.6320(3) 0.4147(3) 0.0521(12) Uani 1 1 d . . .
H10A H 0.6796 0.5740 0.4208 0.063 Uiso 1 1 calc R . .
H10B H 0.5630 0.6330 0.4291 0.063 Uiso 1 1 calc R . .
C11 C 0.6405(4) 0.6572(3) 0.3353(3) 0.0430(10) Uani 1 1 d . . .
C12 C 0.5262(4) 0.6759(3) 0.2902(3) 0.0593(13) Uani 1 1 d . . .
H12 H 0.4497 0.6702 0.3093 0.071 Uiso 1 1 calc R . .
C13 C 0.5268(5) 0.7024(4) 0.2180(3) 0.0696(15) Uani 1 1 d . . .
H13 H 0.4509 0.7153 0.1881 0.083 Uiso 1 1 calc R . .
C14 C 0.6395(4) 0.7100(3) 0.1897(3) 0.0567(13) Uani 1 1 d . . .
H14 H 0.6420 0.7287 0.1410 0.068 Uiso 1 1 calc R . .
C15 C 0.7479(4) 0.6890(3) 0.2355(2) 0.0422(10) Uani 1 1 d . . .
H15 H 0.8246 0.6922 0.2163 0.051 Uiso 1 1 calc R . .
C16 C 0.9258(4) 0.8962(3) 0.2479(2) 0.0421(10) Uani 1 1 d . . .
H16A H 0.8723 0.8511 0.2239 0.050 Uiso 1 1 calc R . .
H16B H 0.8946 0.9502 0.2260 0.050 Uiso 1 1 calc R . .
C17 C 1.0510(5) 0.8818(3) 0.1483(2) 0.0550(12) Uani 1 1 d . . .
H17A H 1.0117 0.9336 0.1281 0.082 Uiso 1 1 calc R . .
H17B H 1.0015 0.8335 0.1285 0.082 Uiso 1 1 calc R . .
H17C H 1.1350 0.8775 0.1347 0.082 Uiso 1 1 calc R . .
C18 C 1.1400(4) 0.9560(3) 0.2608(3) 0.0465(11) Uani 1 1 d . . .
H18A H 1.1224 0.9699 0.3108 0.056 Uiso 1 1 calc R . .
H18B H 1.1185 1.0055 0.2293 0.056 Uiso 1 1 calc R . .
C19 C 1.2813(4) 0.9373(3) 0.2637(3) 0.0505(12) Uani 1 1 d . . .
H19A H 1.2944 0.9027 0.2207 0.061 Uiso 1 1 calc R . .
H19B H 1.3265 0.9907 0.2605 0.061 Uiso 1 1 calc R . .
C20 C 1.3345(4) 0.8917(3) 0.3332(2) 0.0434(10) Uani 1 1 d . . .
C21 C 1.4467(4) 0.9173(3) 0.3752(3) 0.0561(13) Uani 1 1 d . . .
H21 H 1.4933 0.9620 0.3584 0.067 Uiso 1 1 calc R . .
C22 C 1.4895(5) 0.8778(3) 0.4408(3) 0.0609(14) Uani 1 1 d . . .
H22 H 1.5658 0.8942 0.4686 0.073 Uiso 1 1 calc R . .
C23 C 1.4177(4) 0.8128(3) 0.4656(3) 0.0537(12) Uani 1 1 d . . .
H23 H 1.4431 0.7857 0.5111 0.064 Uiso 1 1 calc R . .
C24 C 1.3083(4) 0.7893(3) 0.4213(2) 0.0433(10) Uani 1 1 d . . .
H24 H 1.2598 0.7457 0.4382 0.052 Uiso 1 1 calc R . .
C25 C 0.7857(6) 1.0493(3) 0.4673(4) 0.0839(19) Uani 1 1 d . . .
H25A H 0.7589 1.0348 0.5144 0.126 Uiso 1 1 calc R . .
H25B H 0.7140 1.0690 0.4334 0.126 Uiso 1 1 calc R . .
H25C H 0.8484 1.0938 0.4747 0.126 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 O1 2.017(3) . ?
Ni2 N4 2.035(3) . ?
Ni2 N3 2.087(3) . ?
Ni2 O3 2.100(3) . ?
Ni2 O9 2.101(3) . ?
Ni2 O8 2.194(3) . ?
Ni1 O1 1.965(2) . ?
Ni1 N2 2.057(3) . ?
Ni1 O5 2.093(3) . ?
Ni1 N1 2.108(3) . ?
Ni1 O6 2.182(3) . ?
Ni1 O2 2.190(3) . ?
O1 C1 1.359(4) . ?
O3 N5 1.268(4) . ?
O2 N5 1.257(4) . ?
O4 N5 1.220(4) . ?
O8 N7 1.270(4) . ?
O9 N7 1.271(4) . ?
O10 N7 1.209(5) . ?
O6 N6 1.256(4) . ?
O5 N6 1.278(5) . ?
O7 N6 1.211(5) . ?
N3 C8 1.476(5) . ?
N3 C7 1.476(5) . ?
N3 C9 1.486(5) . ?
N4 C15 1.333(5) . ?
N4 C11 1.343(5) . ?
N1 C18 1.488(5) . ?
N1 C17 1.492(5) . ?
N1 C16 1.495(5) . ?
N2 C24 1.341(5) . ?
N2 C20 1.348(5) . ?
C1 C6 1.390(5) . ?
C1 C2 1.397(6) . ?
C2 C3 1.380(6) . ?
C2 C16 1.497(5) . ?
C3 C4 1.394(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(7) . ?
C4 C25 1.515(6) . ?
C5 C6 1.390(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.497(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.513(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.477(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.398(6) . ?
C12 C13 1.367(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.364(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.525(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.485(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.383(6) . ?
C21 C22 1.357(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.381(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.369(6) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni2 N4 92.37(12) . . ?
O1 Ni2 N3 94.54(12) . . ?
N4 Ni2 N3 94.96(13) . . ?
O1 Ni2 O3 88.56(11) . . ?
N4 Ni2 O3 173.17(12) . . ?
N3 Ni2 O3 91.72(12) . . ?
O1 Ni2 O9 168.51(11) . . ?
N4 Ni2 O9 89.64(12) . . ?
N3 Ni2 O9 96.56(13) . . ?
O3 Ni2 O9 88.14(12) . . ?
O1 Ni2 O8 108.68(10) . . ?
N4 Ni2 O8 87.92(12) . . ?
N3 Ni2 O8 156.49(12) . . ?
O3 Ni2 O8 85.38(11) . . ?
O9 Ni2 O8 60.07(11) . . ?
O1 Ni1 N2 101.68(11) . . ?
O1 Ni1 O5 157.17(12) . . ?
N2 Ni1 O5 98.16(13) . . ?
O1 Ni1 N1 95.79(11) . . ?
N2 Ni1 N1 94.43(13) . . ?
O5 Ni1 N1 93.81(12) . . ?
O1 Ni1 O6 98.62(11) . . ?
N2 Ni1 O6 157.42(12) . . ?
O5 Ni1 O6 60.13(12) . . ?
N1 Ni1 O6 93.25(12) . . ?
O1 Ni1 O2 89.35(10) . . ?
N2 Ni1 O2 88.93(12) . . ?
O5 Ni1 O2 79.79(11) . . ?
N1 Ni1 O2 173.15(11) . . ?
O6 Ni1 O2 81.48(11) . . ?
C1 O1 Ni1 119.5(2) . . ?
C1 O1 Ni2 119.2(2) . . ?
Ni2 O1 Ni1 121.24(12) . . ?
N5 O3 Ni2 123.8(2) . . ?
N5 O2 Ni1 134.0(2) . . ?
N7 O8 Ni2 90.0(2) . . ?
N7 O9 Ni2 94.2(2) . . ?
N6 O6 Ni1 90.2(2) . . ?
N6 O5 Ni1 93.8(2) . . ?
C8 N3 C7 107.9(3) . . ?
C8 N3 C9 108.9(3) . . ?
C7 N3 C9 110.4(3) . . ?
C8 N3 Ni2 108.7(3) . . ?
C7 N3 Ni2 107.5(2) . . ?
C9 N3 Ni2 113.2(2) . . ?
C15 N4 C11 119.5(4) . . ?
C15 N4 Ni2 117.3(3) . . ?
C11 N4 Ni2 123.2(3) . . ?
C18 N1 C17 108.3(3) . . ?
C18 N1 C16 110.0(3) . . ?
C17 N1 C16 106.2(3) . . ?
C18 N1 Ni1 110.6(3) . . ?
C17 N1 Ni1 113.2(3) . . ?
C16 N1 Ni1 108.5(2) . . ?
C24 N2 C20 117.5(4) . . ?
C24 N2 Ni1 120.2(3) . . ?
C20 N2 Ni1 121.2(3) . . ?
O4 N5 O2 120.2(3) . . ?
O4 N5 O3 118.7(4) . . ?
O3 N5 O2 121.1(3) . . ?
O10 N7 O8 122.6(4) . . ?
O10 N7 O9 121.7(4) . . ?
O8 N7 O9 115.7(4) . . ?
O7 N6 O6 123.3(4) . . ?
O7 N6 O5 121.2(4) . . ?
O6 N6 O5 115.5(3) . . ?
O1 C1 C6 120.1(4) . . ?
O1 C1 C2 120.5(3) . . ?
C6 C1 C2 119.3(4) . . ?
C3 C2 C1 119.6(4) . . ?
C3 C2 C16 119.5(4) . . ?
C1 C2 C16 120.7(4) . . ?
C2 C3 C4 122.0(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C5 C4 C3 117.3(4) . . ?
C5 C4 C25 121.1(5) . . ?
C3 C4 C25 121.5(5) . . ?
C4 C5 C6 122.2(4) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C5 119.5(4) . . ?
C1 C6 C7 120.3(4) . . ?
C5 C6 C7 120.2(4) . . ?
N3 C7 C6 114.2(3) . . ?
N3 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 . . ?
N3 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 114.2(4) . . ?
N3 C9 H9A 108.7 . . ?
C10 C9 H9A 108.7 . . ?
N3 C9 H9B 108.7 . . ?
C10 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C11 C10 C9 112.0(4) . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N4 C11 C12 119.3(4) . . ?
N4 C11 C10 117.6(4) . . ?
C12 C11 C10 123.0(4) . . ?
C13 C12 C11 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 119.9(5) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 117.6(5) . . ?
C15 C14 H14 121.2 . . ?
C13 C14 H14 121.2 . . ?
N4 C15 C14 123.6(4) . . ?
N4 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
N1 C16 C2 114.3(3) . . ?
N1 C16 H16A 108.7 . . ?
C2 C16 H16A 108.7 . . ?
N1 C16 H16B 108.7 . . ?
C2 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C18 C19 112.9(4) . . ?
N1 C18 H18A 109.0 . . ?
C19 C18 H18A 109.0 . . ?
N1 C18 H18B 109.0 . . ?
C19 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C18 112.4(3) . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
N2 C20 C21 121.0(4) . . ?
N2 C20 C19 117.3(4) . . ?
C21 C20 C19 121.7(4) . . ?
C22 C21 C20 120.5(5) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 118.8(5) . . ?
C21 C22 H22 120.6 . . ?
C23 C22 H22 120.6 . . ?
C24 C23 C22 118.2(4) . . ?
C24 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
N2 C24 C23 123.7(4) . . ?
N2 C24 H24 118.1 . . ?
C23 C24 H24 118.1 . . ?
C4 C25 H25A 109.5 . . ?
C4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

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
O1 C1 C2 C3 -179.1(4) . . . . ?
C6 C1 C2 C3 -0.9(6) . . . . ?
O1 C1 C2 C16 5.9(6) . . . . ?
C6 C1 C2 C16 -175.9(4) . . . . ?
C1 C2 C3 C4 1.1(7) . . . . ?
C16 C2 C3 C4 176.1(4) . . . . ?
C2 C3 C4 C5 -1.2(7) . . . . ?
C2 C3 C4 C25 -179.0(5) . . . . ?
C3 C4 C5 C6 1.3(7) . . . . ?
C25 C4 C5 C6 179.1(5) . . . . ?
O1 C1 C6 C5 179.2(3) . . . . ?
C2 C1 C6 C5 1.0(6) . . . . ?
O1 C1 C6 C7 -3.3(5) . . . . ?
C2 C1 C6 C7 178.4(4) . . . . ?
C4 C5 C6 C1 -1.2(6) . . . . ?
C4 C5 C6 C7 -178.7(4) . . . . ?
C8 N3 C7 C6 -178.4(3) . . . . ?
C9 N3 C7 C6 -59.5(4) . . . . ?
C1 C6 C7 N3 -60.9(5) . . . . ?
C5 C6 C7 N3 116.5(4) . . . . ?
C8 N3 C9 C10 -82.2(5) . . . . ?
C7 N3 C9 C10 159.5(4) . . . . ?
N3 C9 C10 C11 -80.4(5) . . . . ?
C15 N4 C11 C12 0.2(6) . . . . ?
C15 N4 C11 C10 -178.2(4) . . . . ?
C9 C10 C11 N4 55.2(5) . . . . ?
C9 C10 C11 C12 -123.1(5) . . . . ?
N4 C11 C12 C13 -1.2(7) . . . . ?
C10 C11 C12 C13 177.1(5) . . . . ?
C11 C12 C13 C14 0.6(8) . . . . ?
C12 C13 C14 C15 1.0(8) . . . . ?
C11 N4 C15 C14 1.5(6) . . . . ?
C13 C14 C15 N4 -2.0(7) . . . . ?
C18 N1 C16 C2 -64.3(4) . . . . ?
C17 N1 C16 C2 178.7(4) . . . . ?
C3 C2 C16 N1 121.3(4) . . . . ?
C1 C2 C16 N1 -63.7(5) . . . . ?
C17 N1 C18 C19 -78.6(4) . . . . ?
C16 N1 C18 C19 165.8(3) . . . . ?
N1 C18 C19 C20 -84.7(5) . . . . ?
C24 N2 C20 C21 4.3(6) . . . . ?
C24 N2 C20 C19 -173.9(4) . . . . ?
C18 C19 C20 N2 45.3(5) . . . . ?
C18 C19 C20 C21 -132.9(4) . . . . ?
C19 C20 C21 C22 176.1(4) . . . . ?
C20 C21 C22 C23 -1.3(7) . . . . ?
C21 C22 C23 C24 2.1(7) . . . . ?
C20 N2 C24 C23 -3.5(6) . . . . ?
C22 C23 C24 N2 0.3(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.30
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.670
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.096
####################################################################### 
# 
# 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_complex2
_database_code_depnum_ccdc_archive 'CCDC 1045912'
_audit_update_record             
;
2016-03-11 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Ni2(NO3)3(L-isopropyl)](H2O)0.80'
_chemical_formula_moiety         'C27 H35 N7 Ni2 O10, 0.8(H2 O)'
_chemical_formula_sum            'C27 H36.60 N7 Ni2 O10.80'
_chemical_formula_weight         749.41

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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   10.6714(16)
_cell_length_b                   16.421(2)
_cell_length_c                   18.430(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.785(2)
_cell_angle_gamma                90.00
_cell_volume                     3213.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4000
_cell_measurement_theta_min      1.70
_cell_measurement_theta_max      25.20

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_absorpt_coefficient_mu    1.240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7387
_exptl_absorpt_correction_T_max  0.8263
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22065
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         25.30
_reflns_number_total             5826
_reflns_number_gt                4948
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX-2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0512P)²+1.8744P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5826
_refine_ls_number_parameters     434
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0940
_refine_ls_wR_factor_gt          0.0887
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.11813(3) 0.245887(19) 0.270799(16) 0.03425(10) Uani 1 d . . .
Ni2 Ni -0.08715(3) 0.124811(19) 0.358472(18) 0.03782(11) Uani 1 d . . .
O1 O -0.01889(15) 0.23542(9) 0.33463(9) 0.0323(4) Uani 1 d . . .
O2 O 0.18891(18) 0.12413(11) 0.30810(10) 0.0463(4) Uani 1 d . . .
O3 O 0.09334(17) 0.09111(12) 0.40408(10) 0.0475(5) Uani 1 d . . .
O4 O 0.2800(2) 0.04773(15) 0.39262(14) 0.0744(7) Uani 1 d . . .
O5 O 0.22688(17) 0.21812(13) 0.18500(10) 0.0509(5) Uani 1 d . . .
O6 O 0.03493(17) 0.17840(13) 0.18009(10) 0.0511(5) Uani 1 d . . .
O7 O 0.1454(3) 0.1514(2) 0.09030(13) 0.0923(9) Uani 1 d . . .
O8 O -0.05232(18) 0.03397(13) 0.27208(11) 0.0523(7) Uani 1 d . . .
O9 O -0.13793(19) 0.00188(12) 0.36863(12) 0.0556(5) Uani 1 d . . .
O10 O -0.1026(3) -0.09206(14) 0.29086(16) 0.0849(8) Uani 1 d . . .
N1 N 0.05697(19) 0.35823(13) 0.22330(10) 0.0373(5) Uani 1 d . . .
N2 N 0.25639(19) 0.29788(13) 0.34130(11) 0.0367(5) Uani 1 d . . .
N3 N -0.1398(2) 0.15900(13) 0.45952(12) 0.0450(5) Uani 1 d . . .
N4 N -0.2584(2) 0.14893(14) 0.30135(15) 0.0484(6) Uani 1 d . . .
N5 N 0.1885(2) 0.08691(13) 0.36728(13) 0.0438(5) Uani 1 d . . .
N6 N 0.1356(2) 0.18067(17) 0.14957(13) 0.0532(6) Uani 1 d . . .
N7 N -0.0971(2) -0.02151(15) 0.30895(14) 0.0516(6) Uani 1 d . . .
C1 C -0.0652(2) 0.30361(14) 0.36383(12) 0.0313(5) Uani 1 d . . .
C2 C -0.0892(2) 0.30512(15) 0.43708(13) 0.0358(5) Uani 1 d . . .
C3 C -0.1355(2) 0.37607(15) 0.46573(13) 0.0383(6) Uani 1 d . . .
H3 H -0.1523 0.3762 0.5143 0.046 Uiso 1 calc R . .
C4 C -0.1575(2) 0.44618(15) 0.42544(14) 0.0378(6) Uani 1 d . . .
C5 C -0.1351(2) 0.44254(15) 0.35259(14) 0.0389(6) Uani 1 d . . .
H5 H -0.1509 0.4885 0.3236 0.047 Uiso 1 calc R . .
C6 C -0.0903(2) 0.37327(15) 0.32159(13) 0.0343(5) Uani 1 d . . .
C7 C -0.0750(2) 0.37242(16) 0.24099(13) 0.0383(6) Uani 1 d . . .
H7A H -0.1286 0.3301 0.2179 0.046 Uiso 1 calc R . .
H7B H -0.1040 0.4241 0.2201 0.046 Uiso 1 calc R . .
C8 C 0.0514(3) 0.3597(2) 0.14228(14) 0.0523(7) Uani 1 d . . .
H8A H 0.1341 0.3503 0.1277 0.078 Uiso 1 calc R . .
H8B H 0.0212 0.4118 0.1246 0.078 Uiso 1 calc R . .
H8C H -0.0047 0.3178 0.1223 0.078 Uiso 1 calc R . .
C9 C 0.1406(3) 0.42548(17) 0.25223(15) 0.0451(6) Uani 1 d . . .
H9A H 0.1229 0.4378 0.3016 0.054 Uiso 1 calc R . .
H9B H 0.1220 0.4738 0.2228 0.054 Uiso 1 calc R . .
C10 C 0.2805(3) 0.4053(2) 0.25251(15) 0.0511(7) Uani 1 d . . .
H10A H 0.2931 0.3741 0.2091 0.061 Uiso 1 calc R . .
H10B H 0.3280 0.4555 0.2509 0.061 Uiso 1 calc R . .
C11 C 0.3294(2) 0.35748(17) 0.31872(14) 0.0419(6) Uani 1 d . . .
C12 C 0.4430(3) 0.3778(2) 0.35855(17) 0.0553(8) Uani 1 d . . .
H12 H 0.4940 0.4181 0.3418 0.066 Uiso 1 calc R . .
C13 C 0.4793(3) 0.3379(2) 0.42277(18) 0.0582(8) Uani 1 d . . .
H13 H 0.5562 0.3497 0.4490 0.070 Uiso 1 calc R . .
C14 C 0.4011(3) 0.28110(19) 0.44744(16) 0.0523(7) Uani 1 d . . .
H14 H 0.4219 0.2554 0.4920 0.063 Uiso 1 calc R . .
C15 C 0.2912(3) 0.26212(16) 0.40572(14) 0.0412(6) Uani 1 d . . .
H15 H 0.2386 0.2228 0.4228 0.049 Uiso 1 calc R . .
C16 C -0.0635(3) 0.23161(16) 0.48488(14) 0.0441(6) Uani 1 d . . .
H16A H 0.0251 0.2179 0.4865 0.053 Uiso 1 calc R . .
H16B H -0.0812 0.2451 0.5341 0.053 Uiso 1 calc R . .
C17 C -0.1093(4) 0.09258(19) 0.51312(17) 0.0653(9) Uani 1 d . . .
H17A H -0.1626 0.0466 0.5006 0.098 Uiso 1 calc R . .
H17B H -0.1229 0.1113 0.5610 0.098 Uiso 1 calc R . .
H17C H -0.0228 0.0769 0.5124 0.098 Uiso 1 calc R . .
C18 C -0.2772(3) 0.17818(19) 0.45669(18) 0.0572(8) Uani 1 d . . .
H18A H -0.2912 0.2330 0.4379 0.069 Uiso 1 calc R . .
H18B H -0.3020 0.1771 0.5059 0.069 Uiso 1 calc R . .
C19 C -0.3616(3) 0.1192(2) 0.4093(2) 0.0689(10) Uani 1 d . . .
H19A H -0.3292 0.0643 0.4167 0.083 Uiso 1 calc R . .
H19B H -0.4458 0.1205 0.4248 0.083 Uiso 1 calc R . .
C20 C -0.3687(3) 0.13943(18) 0.3301(2) 0.0577(8) Uani 1 d . . .
C21 C -0.4820(3) 0.1521(2) 0.2868(3) 0.0786(12) Uani 1 d . . .
H21 H -0.5583 0.1442 0.3061 0.094 Uiso 1 calc R . .
C22 C -0.4808(3) 0.1761(3) 0.2162(3) 0.0905(14) Uani 1 d . . .
H22 H -0.5561 0.1853 0.1874 0.109 Uiso 1 calc R . .
C23 C -0.3686(3) 0.1865(2) 0.1877(2) 0.0739(10) Uani 1 d . . .
H23 H -0.3661 0.2033 0.1397 0.089 Uiso 1 calc R . .
C24 C -0.2596(3) 0.17160(18) 0.23190(18) 0.0526(7) Uani 1 d . . .
H24 H -0.1831 0.1776 0.2124 0.063 Uiso 1 calc R . .
C25 C -0.2021(3) 0.52567(16) 0.45692(15) 0.0463(6) Uani 1 d . . .
H25 H -0.1480 0.5687 0.4403 0.056 Uiso 1 calc R . .
C26 C -0.1871(3) 0.52884(19) 0.53890(16) 0.0572(8) Uani 1 d . . .
H26A H -0.2048 0.5830 0.5547 0.086 Uiso 1 calc R . .
H26B H -0.1023 0.5144 0.5566 0.086 Uiso 1 calc R . .
H26C H -0.2447 0.4912 0.5577 0.086 Uiso 1 calc R . .
C27 C -0.3341(3) 0.5461(2) 0.42642(19) 0.0714(10) Uani 1 d . . .
H27A H -0.3523 0.6016 0.4378 0.107 Uiso 1 calc R . .
H27B H -0.3922 0.5107 0.4475 0.107 Uiso 1 calc R . .
H27C H -0.3423 0.5389 0.3745 0.107 Uiso 1 calc R . .
O11 O 0.2496(5) 0.1419(3) 0.5564(3) 0.1260(17) Uani 0.80 d PD . .
H91 H 0.230(7) 0.120(4) 0.515(4) 0.164 Uiso 0.80 d PD . .
H92 H 0.230(7) 0.110(4) 0.589(3) 0.164 Uiso 0.80 d PD . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.9744(15) . ?
Ni1 N2 2.051(2) . ?
Ni1 O5 2.1037(18) . ?
Ni1 N1 2.117(2) . ?
Ni1 O6 2.1242(19) . ?
Ni1 O2 2.2217(19) . ?
Ni2 O1 2.0217(16) . ?
Ni2 N4 2.054(2) . ?
Ni2 N3 2.076(2) . ?
Ni2 O3 2.0967(19) . ?
Ni2 O9 2.103(2) . ?
Ni2 O8 2.240(2) . ?
O1 C1 1.357(3) . ?
O2 N5 1.251(3) . ?
O3 N5 1.278(3) . ?
O4 N5 1.223(3) . ?
O5 N6 1.275(3) . ?
O6 N6 1.262(3) . ?
O7 N6 1.208(3) . ?
O8 N7 1.259(3) . ?
O9 N7 1.282(3) . ?
O10 N7 1.205(3) . ?
N1 C9 1.485(3) . ?
N1 C8 1.489(3) . ?
N1 C7 1.495(3) . ?
N2 C15 1.343(3) . ?
N2 C11 1.343(3) . ?
N3 C17 1.485(4) . ?
N3 C16 1.492(4) . ?
N3 C18 1.496(4) . ?
N4 C24 1.332(4) . ?
N4 C20 1.347(3) . ?
C1 C6 1.394(3) . ?
C1 C2 1.399(3) . ?
C2 C3 1.390(3) . ?
C2 C16 1.503(3) . ?
C3 C4 1.377(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(3) . ?
C4 C25 1.524(3) . ?
C5 C6 1.380(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.511(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.528(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.500(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.392(4) . ?
C12 C13 1.374(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.360(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.372(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.534(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.490(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.397(5) . ?
C21 C22 1.360(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.365(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.373(4) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C27 1.501(4) . ?
C25 C26 1.504(4) . ?
C25 H25 0.9800 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N2 100.80(7) . . ?
O1 Ni1 O5 157.95(8) . . ?
N2 Ni1 O5 98.64(8) . . ?
O1 Ni1 N1 96.10(7) . . ?
N2 Ni1 N1 94.09(8) . . ?
O5 Ni1 N1 92.78(8) . . ?
O1 Ni1 O6 98.49(7) . . ?
N2 Ni1 O6 158.84(8) . . ?
O5 Ni1 O6 60.91(7) . . ?
N1 Ni1 O6 92.42(8) . . ?
O1 Ni1 O2 89.22(6) . . ?
N2 Ni1 O2 88.75(8) . . ?
O5 Ni1 O2 80.88(8) . . ?
N1 Ni1 O2 173.39(7) . . ?
O6 Ni1 O2 82.89(8) . . ?
O1 Ni2 N4 92.11(8) . . ?
O1 Ni2 N3 95.05(7) . . ?
N4 Ni2 N3 95.76(10) . . ?
O1 Ni2 O3 89.30(7) . . ?
N4 Ni2 O3 172.10(8) . . ?
N3 Ni2 O3 91.86(8) . . ?
O1 Ni2 O9 169.51(7) . . ?
N4 Ni2 O9 90.38(9) . . ?
N3 Ni2 O9 94.84(8) . . ?
O3 Ni2 O9 86.88(8) . . ?
O1 Ni2 O8 110.77(7) . . ?
N4 Ni2 O8 88.10(8) . . ?
N3 Ni2 O8 153.77(8) . . ?
O3 Ni2 O8 84.13(7) . . ?
O9 Ni2 O8 59.12(8) . . ?
C1 O1 Ni1 119.07(14) . . ?
C1 O1 Ni2 120.09(13) . . ?
Ni1 O1 Ni2 120.83(7) . . ?
N5 O2 Ni1 132.73(15) . . ?
N5 O3 Ni2 123.23(16) . . ?
N6 O5 Ni1 92.20(14) . . ?
N6 O6 Ni1 91.63(15) . . ?
N7 O8 Ni2 89.94(15) . . ?
N7 O9 Ni2 95.65(15) . . ?
C9 N1 C8 108.1(2) . . ?
C9 N1 C7 110.6(2) . . ?
C8 N1 C7 105.84(19) . . ?
C9 N1 Ni1 110.52(15) . . ?
C8 N1 Ni1 114.09(17) . . ?
C7 N1 Ni1 107.67(15) . . ?
C15 N2 C11 118.4(2) . . ?
C15 N2 Ni1 119.69(18) . . ?
C11 N2 Ni1 120.65(17) . . ?
C17 N3 C16 107.6(2) . . ?
C17 N3 C18 109.0(2) . . ?
C16 N3 C18 110.2(2) . . ?
C17 N3 Ni2 109.71(17) . . ?
C16 N3 Ni2 107.99(15) . . ?
C18 N3 Ni2 112.25(19) . . ?
C24 N4 C20 119.1(3) . . ?
C24 N4 Ni2 117.93(18) . . ?
C20 N4 Ni2 122.9(2) . . ?
O4 N5 O2 121.1(2) . . ?
O4 N5 O3 118.2(2) . . ?
O2 N5 O3 120.6(2) . . ?
O7 N6 O6 123.2(3) . . ?
O7 N6 O5 121.6(2) . . ?
O6 N6 O5 115.3(2) . . ?
O10 N7 O8 123.8(3) . . ?
O10 N7 O9 120.9(3) . . ?
O8 N7 O9 115.2(2) . . ?
O1 C1 C6 120.8(2) . . ?
O1 C1 C2 120.4(2) . . ?
C6 C1 C2 118.7(2) . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 C16 120.1(2) . . ?
C1 C2 C16 120.7(2) . . ?
C4 C3 C2 122.9(2) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 116.7(2) . . ?
C3 C4 C25 123.6(2) . . ?
C5 C4 C25 119.7(2) . . ?
C6 C5 C4 122.4(2) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C1 120.0(2) . . ?
C5 C6 C7 119.4(2) . . ?
C1 C6 C7 120.5(2) . . ?
N1 C7 C6 114.4(2) . . ?
N1 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 113.0(2) . . ?
N1 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
N1 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C9 112.1(2) . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 C12 120.8(3) . . ?
N2 C11 C10 117.9(2) . . ?
C12 C11 C10 121.1(3) . . ?
C13 C12 C11 119.7(3) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C14 C13 C12 119.1(3) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 119.1(3) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
N2 C15 C14 122.7(3) . . ?
N2 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
N3 C16 C2 113.4(2) . . ?
N3 C16 H16A 108.9 . . ?
C2 C16 H16A 108.9 . . ?
N3 C16 H16B 108.9 . . ?
C2 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 113.8(2) . . ?
N3 C18 H18A 108.8 . . ?
C19 C18 H18A 108.8 . . ?
N3 C18 H18B 108.8 . . ?
C19 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C20 C19 C18 112.7(3) . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
N4 C20 C21 119.8(3) . . ?
N4 C20 C19 116.8(3) . . ?
C21 C20 C19 123.3(3) . . ?
C22 C21 C20 119.9(3) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 119.8(4) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C22 C23 C24 118.2(4) . . ?
C22 C23 H23 120.9 . . ?
C24 C23 H23 120.9 . . ?
N4 C24 C23 123.1(3) . . ?
N4 C24 H24 118.5 . . ?
C23 C24 H24 118.5 . . ?
C27 C25 C26 111.6(2) . . ?
C27 C25 C4 111.5(2) . . ?
C26 C25 C4 114.0(2) . . ?
C27 C25 H25 106.4 . . ?
C26 C25 H25 106.4 . . ?
C4 C25 H25 106.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

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
O1 C1 C2 C3 179.4(2) . . . . ?
C6 C1 C2 C3 -0.8(4) . . . . ?
O1 C1 C2 C16 0.3(4) . . . . ?
C6 C1 C2 C16 -179.9(2) . . . . ?
C1 C2 C3 C4 -1.0(4) . . . . ?
C16 C2 C3 C4 178.1(3) . . . . ?
C2 C3 C4 C5 2.1(4) . . . . ?
C2 C3 C4 C25 -176.9(3) . . . . ?
C3 C4 C5 C6 -1.4(4) . . . . ?
C25 C4 C5 C6 177.6(2) . . . . ?
C4 C5 C6 C1 -0.3(4) . . . . ?
C4 C5 C6 C7 176.7(2) . . . . ?
O1 C1 C6 C5 -178.7(2) . . . . ?
C2 C1 C6 C5 1.4(4) . . . . ?
O1 C1 C6 C7 4.3(3) . . . . ?
C2 C1 C6 C7 -175.5(2) . . . . ?
C9 N1 C7 C6 -63.2(3) . . . . ?
C8 N1 C7 C6 -180.0(2) . . . . ?
C5 C6 C7 N1 119.4(3) . . . . ?
C1 C6 C7 N1 -63.7(3) . . . . ?
C8 N1 C9 C10 -78.5(3) . . . . ?
C7 N1 C9 C10 166.1(2) . . . . ?
N1 C9 C10 C11 -83.5(3) . . . . ?
C15 N2 C11 C12 4.5(4) . . . . ?
C15 N2 C11 C10 -171.2(2) . . . . ?
C9 C10 C11 N2 41.5(4) . . . . ?
C9 C10 C11 C12 -134.2(3) . . . . ?
N2 C11 C12 C13 -1.8(4) . . . . ?
C10 C11 C12 C13 173.7(3) . . . . ?
C11 C12 C13 C14 -2.2(5) . . . . ?
C12 C13 C14 C15 3.3(4) . . . . ?
C11 N2 C15 C14 -3.4(4) . . . . ?
C13 C14 C15 N2 -0.6(4) . . . . ?
C17 N3 C16 C2 -177.5(2) . . . . ?
C18 N3 C16 C2 -58.8(3) . . . . ?
C3 C2 C16 N3 119.1(3) . . . . ?
C1 C2 C16 N3 -61.8(3) . . . . ?
C17 N3 C18 C19 -80.7(3) . . . . ?
C16 N3 C18 C19 161.4(2) . . . . ?
N3 C18 C19 C20 -81.7(3) . . . . ?
C24 N4 C20 C21 1.0(4) . . . . ?
C24 N4 C20 C19 -176.2(3) . . . . ?
C18 C19 C20 N4 51.9(4) . . . . ?
C18 C19 C20 C21 -125.2(3) . . . . ?
N4 C20 C21 C22 -1.7(5) . . . . ?
C19 C20 C21 C22 175.3(4) . . . . ?
C20 C21 C22 C23 0.9(6) . . . . ?
C21 C22 C23 C24 0.5(6) . . . . ?
C20 N4 C24 C23 0.5(4) . . . . ?
C22 C23 C24 N4 -1.2(5) . . . . ?
C3 C4 C25 C27 -111.9(3) . . . . ?
C5 C4 C25 C27 69.2(3) . . . . ?
C3 C4 C25 C26 15.6(4) . . . . ?
C5 C4 C25 C26 -163.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.30
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_complex3
_database_code_depnum_ccdc_archive 'CCDC 1045913'
_audit_update_record             
;
2016-03-11 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Ni2(NO3)3)(L-t-butyl)]'
_chemical_formula_moiety         'C28 H37 N7 Ni2 O10'
_chemical_formula_sum            'C28 H37 N7 Ni2 O10'
_chemical_formula_weight         749.03

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           Monoclinic
_symmetry_space_group_name_H-M   'C c'
_symmetry_space_group_name_Hall  'C -2yc'

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

_cell_length_a                   14.1480(5)
_cell_length_b                   15.3628(5)
_cell_length_c                   17.1155(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.275(1)
_cell_angle_gamma                90.00
_cell_volume                     3466.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3000
_cell_measurement_theta_min      2.10
_cell_measurement_theta_max      33.00

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8200
_exptl_absorpt_correction_T_max  0.8841
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30628
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         33.00
_reflns_number_total             10346
_reflns_number_gt                8972
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX-2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_reinfe_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0715P)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    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(9)
_refine_ls_number_reflns         10346
_refine_ls_number_parameters     429
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1117
_refine_ls_wR_factor_gt          0.1068
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
Ni1 Ni 0.10383(2) 1.091198(19) 0.918710(18) 0.03083(8) Uani 1 1 d . . .
Ni2 Ni 0.092386(18) 0.868980(18) 0.929819(17) 0.02784(7) Uani 1 1 d . . .
O1 O 0.16742(13) 0.98118(10) 0.97110(11) 0.0295(3) Uani 1 1 d . . .
O2 O -0.04704(15) 1.03573(14) 0.89412(15) 0.0432(5) Uani 1 1 d . . .
O3 O -0.02699(14) 0.91354(14) 0.96436(14) 0.0409(4) Uani 1 1 d . . .
O4 O -0.1679(2) 0.9828(2) 0.9258(3) 0.0868(12) Uani 1 1 d . . .
O5 O 0.01877(17) 1.17868(15) 0.82582(16) 0.0495(5) Uani 1 1 d . . .
O6 O 0.07126(18) 1.05993(16) 0.78821(15) 0.0498(5) Uani 1 1 d . . .
O7 O -0.0160(3) 1.1544(3) 0.6945(2) 0.0876(11) Uani 1 1 d . . .
O8 O -0.02010(15) 0.88519(14) 0.80103(13) 0.0398(4) Uani 1 1 d . . .
O9 O -0.00513(15) 0.76540(13) 0.86958(13) 0.0419(4) Uani 1 1 d . . .
O10 O -0.1217(2) 0.7776(2) 0.74577(15) 0.0652(7) Uani 1 1 d . . .
N1 N 0.24275(17) 1.15426(16) 0.93301(15) 0.0377(5) Uani 1 1 d . . .
N2 N 0.09038(19) 1.15342(16) 1.01999(16) 0.0403(5) Uani 1 1 d . . .
N3 N 0.15926(15) 0.80450(14) 1.04271(14) 0.0328(4) Uani 1 1 d . . .
N4 N 0.19359(15) 0.82927(14) 0.87592(14) 0.0339(4) Uani 1 1 d . . .
N5 N -0.08153(17) 0.97745(16) 0.92708(17) 0.0414(5) Uani 1 1 d . . .
N6 N 0.0229(2) 1.1315(2) 0.76615(19) 0.0505(7) Uani 1 1 d . . .
N7 N -0.05164(17) 0.80862(17) 0.80335(15) 0.0388(5) Uani 1 1 d . . .
C1 C 0.25384(17) 0.98460(15) 1.03954(15) 0.0291(4) Uani 1 1 d . . .
C2 C 0.26719(18) 0.93348(15) 1.11063(15) 0.0312(4) Uani 1 1 d . . .
C3 C 0.35612(19) 0.94220(17) 1.18142(16) 0.0356(5) Uani 1 1 d . . .
H3 H 0.3648 0.9069 1.2276 0.043 Uiso 1 1 calc R . .
C4 C 0.43178(19) 1.00139(18) 1.18542(17) 0.0365(5) Uani 1 1 d . . .
C5 C 0.41832(18) 1.04863(18) 1.11259(18) 0.0393(6) Uani 1 1 d . . .
H5 H 0.4691 1.0869 1.1122 0.047 Uiso 1 1 calc R . .
C6 C 0.33197(18) 1.04082(17) 1.04043(17) 0.0341(5) Uani 1 1 d . . .
C7 C 0.32487(19) 1.08746(18) 0.96129(19) 0.0377(5) Uani 1 1 d . . .
H7A H 0.3893 1.1156 0.9701 0.045 Uiso 1 1 calc R . .
H7B H 0.3134 1.0449 0.9170 0.045 Uiso 1 1 calc R . .
C8 C 0.2452(3) 1.1912(3) 0.8534(2) 0.0548(8) Uani 1 1 d . . .
H8A H 0.3123 1.2122 0.8623 0.082 Uiso 1 1 calc R . .
H8B H 0.1978 1.2384 0.8355 0.082 Uiso 1 1 calc R . .
H8C H 0.2273 1.1469 0.8110 0.082 Uiso 1 1 calc R . .
C9 C 0.2649(3) 1.2268(2) 0.9959(2) 0.0500(7) Uani 1 1 d . . .
H9A H 0.3164 1.2646 0.9892 0.060 Uiso 1 1 calc R . .
H9B H 0.2917 1.2026 1.0520 0.060 Uiso 1 1 calc R . .
C10 C 0.1706(3) 1.2801(2) 0.9859(3) 0.0568(8) Uani 1 1 d . . .
H10A H 0.1908 1.3381 1.0081 0.068 Uiso 1 1 calc R . .
H10B H 0.1301 1.2857 0.9267 0.068 Uiso 1 1 calc R . .
C11 C 0.1077(3) 1.2400(2) 1.0297(2) 0.0484(7) Uani 1 1 d . . .
C12 C 0.0704(3) 1.2869(3) 1.0815(3) 0.0672(11) Uani 1 1 d . . .
H12 H 0.0803 1.3468 1.0867 0.081 Uiso 1 1 calc R . .
C13 C 0.0189(3) 1.2452(3) 1.1253(3) 0.0714(12) Uani 1 1 d . . .
H13 H -0.0074 1.2769 1.1590 0.086 Uiso 1 1 calc R . .
C14 C 0.0068(3) 1.1574(3) 1.1188(2) 0.0622(10) Uani 1 1 d . . .
H14 H -0.0256 1.1280 1.1494 0.075 Uiso 1 1 calc R . .
C15 C 0.0440(2) 1.1125(2) 1.0654(2) 0.0463(6) Uani 1 1 d . . .
H15 H 0.0366 1.0523 1.0611 0.056 Uiso 1 1 calc R . .
C16 C 0.1875(2) 0.86966(17) 1.11257(16) 0.0340(5) Uani 1 1 d . . .
H16A H 0.2121 0.8388 1.1656 0.041 Uiso 1 1 calc R . .
H16B H 0.1272 0.9016 1.1097 0.041 Uiso 1 1 calc R . .
C17 C 0.0838(2) 0.7445(2) 1.0568(2) 0.0476(7) Uani 1 1 d . . .
H17A H 0.0608 0.7032 1.0117 0.071 Uiso 1 1 calc R . .
H17B H 0.0272 0.7776 1.0587 0.071 Uiso 1 1 calc R . .
H17C H 0.1151 0.7142 1.1089 0.071 Uiso 1 1 calc R . .
C18 C 0.2499(2) 0.75465(19) 1.04508(18) 0.0419(6) Uani 1 1 d . . .
H18A H 0.2693 0.7154 1.0927 0.050 Uiso 1 1 calc R . .
H18B H 0.3056 0.7949 1.0535 0.050 Uiso 1 1 calc R . .
C19 C 0.2337(2) 0.70167(18) 0.9654(2) 0.0445(7) Uani 1 1 d . . .
H19A H 0.2824 0.6544 0.9791 0.053 Uiso 1 1 calc R . .
H19B H 0.1664 0.6761 0.9468 0.053 Uiso 1 1 calc R . .
C20 C 0.24395(18) 0.75272(18) 0.89517(18) 0.0373(5) Uani 1 1 d . . .
C21 C 0.3028(2) 0.7247(2) 0.8501(3) 0.0530(8) Uani 1 1 d . . .
H21 H 0.3377 0.6722 0.8639 0.064 Uiso 1 1 calc R . .
C22 C 0.3098(3) 0.7738(3) 0.7856(3) 0.0599(9) Uani 1 1 d . . .
H22 H 0.3483 0.7543 0.7551 0.072 Uiso 1 1 calc R . .
C23 C 0.2588(2) 0.8534(2) 0.7661(2) 0.0500(7) Uani 1 1 d . . .
H23 H 0.2629 0.8886 0.7232 0.060 Uiso 1 1 calc R . .
C24 C 0.2017(2) 0.87774(19) 0.8134(2) 0.0405(6) Uani 1 1 d . . .
H24 H 0.1671 0.9305 0.8011 0.049 Uiso 1 1 calc R . .
C25 C 0.5274(2) 1.00958(19) 1.26516(19) 0.0421(6) Uani 1 1 d . . .
C26 C 0.5955(3) 0.9321(3) 1.2726(3) 0.0685(12) Uani 1 1 d . . .
H26A H 0.6162 0.9304 1.2250 0.103 Uiso 1 1 calc R . .
H26B H 0.5595 0.8797 1.2744 0.103 Uiso 1 1 calc R . .
H26C H 0.6543 0.9370 1.3230 0.103 Uiso 1 1 calc R . .
C27 C 0.5863(4) 1.0910(3) 1.2657(3) 0.0761(16) Uani 1 1 d . . .
H27A H 0.6432 1.0949 1.3176 0.114 Uiso 1 1 calc R . .
H27B H 0.5433 1.1408 1.2600 0.114 Uiso 1 1 calc R . .
H27C H 0.6101 1.0895 1.2198 0.114 Uiso 1 1 calc R . .
C28 C 0.4977(4) 1.0093(4) 1.3427(3) 0.0954(19) Uani 1 1 d . . .
H28A H 0.5578 1.0105 1.3924 0.143 Uiso 1 1 calc R . .
H28B H 0.4596 0.9576 1.3427 0.143 Uiso 1 1 calc R . .
H28C H 0.4571 1.0597 1.3417 0.143 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.9709(16) . ?
Ni1 N2 2.048(3) . ?
Ni1 O5 2.096(2) . ?
Ni1 N1 2.124(2) . ?
Ni1 O6 2.164(2) . ?
Ni1 O2 2.193(2) . ?
Ni2 O1 2.0133(16) . ?
Ni2 N4 2.057(2) . ?
Ni2 N3 2.070(2) . ?
Ni2 O3 2.097(2) . ?
Ni2 O9 2.113(2) . ?
Ni2 O8 2.215(2) . ?
O1 C1 1.353(3) . ?
O2 N5 1.248(3) . ?
O3 N5 1.269(3) . ?
O4 N5 1.217(4) . ?
O5 N6 1.271(4) . ?
O6 N6 1.277(4) . ?
O7 N6 1.200(4) . ?
O8 N7 1.264(3) . ?
O9 N7 1.272(3) . ?
O10 N7 1.213(3) . ?
N1 C8 1.488(4) . ?
N1 C7 1.493(3) . ?
N1 C9 1.502(4) . ?
N2 C15 1.341(4) . ?
N2 C11 1.352(4) . ?
N3 C18 1.482(4) . ?
N3 C17 1.494(4) . ?
N3 C16 1.498(3) . ?
N4 C24 1.342(4) . ?
N4 C20 1.352(3) . ?
C1 C6 1.399(3) . ?
C1 C2 1.402(3) . ?
C2 C3 1.401(3) . ?
C2 C16 1.503(3) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.394(4) . ?
C4 C25 1.539(3) . ?
C5 C6 1.392(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.503(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.521(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.490(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.385(5) . ?
C12 C13 1.379(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.358(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.392(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.532(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.487(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.393(5) . ?
C21 C22 1.369(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.398(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.386(4) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C27 1.502(5) . ?
C25 C26 1.507(5) . ?
C25 C28 1.531(7) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N2 100.51(9) . . ?
O1 Ni1 O5 159.48(9) . . ?
N2 Ni1 O5 97.97(10) . . ?
O1 Ni1 N1 95.06(8) . . ?
N2 Ni1 N1 93.20(10) . . ?
O5 Ni1 N1 92.73(9) . . ?
O1 Ni1 O6 99.81(8) . . ?
N2 Ni1 O6 157.92(9) . . ?
O5 Ni1 O6 60.72(9) . . ?
N1 Ni1 O6 93.54(10) . . ?
O1 Ni1 O2 90.34(7) . . ?
N2 Ni1 O2 87.76(9) . . ?
O5 Ni1 O2 81.52(9) . . ?
N1 Ni1 O2 174.25(8) . . ?
O6 Ni1 O2 83.55(9) . . ?
O1 Ni2 N4 92.70(8) . . ?
O1 Ni2 N3 94.47(7) . . ?
N4 Ni2 N3 96.89(9) . . ?
O1 Ni2 O3 89.86(8) . . ?
N4 Ni2 O3 170.51(8) . . ?
N3 Ni2 O3 92.02(9) . . ?
O1 Ni2 O9 169.63(7) . . ?
N4 Ni2 O9 89.73(9) . . ?
N3 Ni2 O9 95.25(8) . . ?
O3 Ni2 O9 86.18(9) . . ?
O1 Ni2 O8 110.48(7) . . ?
N4 Ni2 O8 87.29(8) . . ?
N3 Ni2 O8 154.52(8) . . ?
O3 Ni2 O8 83.25(8) . . ?
O9 Ni2 O8 59.54(8) . . ?
C1 O1 Ni1 118.72(13) . . ?
C1 O1 Ni2 122.20(13) . . ?
Ni1 O1 Ni2 118.62(8) . . ?
N5 O2 Ni1 134.84(17) . . ?
N5 O3 Ni2 121.07(18) . . ?
N6 O5 Ni1 93.58(16) . . ?
N6 O6 Ni1 90.28(19) . . ?
N7 O8 Ni2 89.91(15) . . ?
N7 O9 Ni2 94.40(15) . . ?
C8 N1 C7 106.6(2) . . ?
C8 N1 C9 107.7(3) . . ?
C7 N1 C9 110.0(2) . . ?
C8 N1 Ni1 113.38(19) . . ?
C7 N1 Ni1 107.60(16) . . ?
C9 N1 Ni1 111.41(19) . . ?
C15 N2 C11 119.6(3) . . ?
C15 N2 Ni1 119.1(2) . . ?
C11 N2 Ni1 119.7(2) . . ?
C18 N3 C17 109.8(2) . . ?
C18 N3 C16 110.2(2) . . ?
C17 N3 C16 106.5(2) . . ?
C18 N3 Ni2 111.77(18) . . ?
C17 N3 Ni2 109.54(16) . . ?
C16 N3 Ni2 108.93(15) . . ?
C24 N4 C20 119.1(2) . . ?
C24 N4 Ni2 117.89(17) . . ?
C20 N4 Ni2 122.6(2) . . ?
O4 N5 O2 119.9(3) . . ?
O4 N5 O3 119.0(3) . . ?
O2 N5 O3 121.1(2) . . ?
O7 N6 O5 121.0(3) . . ?
O7 N6 O6 123.6(4) . . ?
O5 N6 O6 115.4(3) . . ?
O10 N7 O8 122.3(3) . . ?
O10 N7 O9 121.7(3) . . ?
O8 N7 O9 116.1(2) . . ?
O1 C1 C6 119.7(2) . . ?
O1 C1 C2 121.6(2) . . ?
C6 C1 C2 118.6(2) . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 C16 119.2(2) . . ?
C1 C2 C16 121.2(2) . . ?
C4 C3 C2 122.7(2) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C3 C4 C5 116.4(2) . . ?
C3 C4 C25 120.8(3) . . ?
C5 C4 C25 122.8(2) . . ?
C6 C5 C4 122.7(2) . . ?
C6 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C5 C6 C1 119.9(2) . . ?
C5 C6 C7 120.6(2) . . ?
C1 C6 C7 119.4(2) . . ?
N1 C7 C6 114.2(2) . . ?
N1 C7 H7A 108.7 . . ?
C6 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
C6 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 111.8(3) . . ?
N1 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C11 C10 C9 112.4(3) . . ?
C11 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 C12 119.7(4) . . ?
N2 C11 C10 117.3(3) . . ?
C12 C11 C10 122.9(3) . . ?
C13 C12 C11 120.4(4) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 118.7(4) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
N2 C15 C14 121.9(4) . . ?
N2 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
N3 C16 C2 113.8(2) . . ?
N3 C16 H16A 108.8 . . ?
C2 C16 H16A 108.8 . . ?
N3 C16 H16B 108.8 . . ?
C2 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 113.7(2) . . ?
N3 C18 H18A 108.8 . . ?
C19 C18 H18A 108.8 . . ?
N3 C18 H18B 108.8 . . ?
C19 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C20 C19 C18 114.4(2) . . ?
C20 C19 H19A 108.7 . . ?
C18 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C18 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
N4 C20 C21 120.1(3) . . ?
N4 C20 C19 117.3(3) . . ?
C21 C20 C19 122.6(3) . . ?
C22 C21 C20 120.6(3) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 119.5(3) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C24 C23 C22 117.2(3) . . ?
C24 C23 H23 121.4 . . ?
C22 C23 H23 121.4 . . ?
N4 C24 C23 123.5(3) . . ?
N4 C24 H24 118.2 . . ?
C23 C24 H24 118.2 . . ?
C27 C25 C26 108.7(4) . . ?
C27 C25 C28 108.9(4) . . ?
C26 C25 C28 107.1(4) . . ?
C27 C25 C4 112.4(3) . . ?
C26 C25 C4 109.9(2) . . ?
C28 C25 C4 109.8(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

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
O1 C1 C2 C3 -177.1(2) . . . . ?
C6 C1 C2 C3 2.3(4) . . . . ?
O1 C1 C2 C16 2.6(4) . . . . ?
C6 C1 C2 C16 -178.0(2) . . . . ?
C1 C2 C3 C4 1.6(4) . . . . ?
C16 C2 C3 C4 -178.1(3) . . . . ?
C2 C3 C4 C5 -4.2(4) . . . . ?
C2 C3 C4 C25 179.0(3) . . . . ?
C3 C4 C5 C6 3.0(4) . . . . ?
C25 C4 C5 C6 179.7(3) . . . . ?
C4 C5 C6 C1 0.8(4) . . . . ?
C4 C5 C6 C7 -174.8(3) . . . . ?
O1 C1 C6 C5 175.9(2) . . . . ?
C2 C1 C6 C5 -3.5(4) . . . . ?
O1 C1 C6 C7 -8.4(4) . . . . ?
C2 C1 C6 C7 172.2(2) . . . . ?
C8 N1 C7 C6 -178.3(3) . . . . ?
C9 N1 C7 C6 65.1(3) . . . . ?
C5 C6 C7 N1 -116.4(3) . . . . ?
C1 C6 C7 N1 67.9(3) . . . . ?
C8 N1 C9 C10 82.8(3) . . . . ?
C7 N1 C9 C10 -161.4(3) . . . . ?
N1 C9 C10 C11 83.7(4) . . . . ?
C15 N2 C11 C12 -5.0(5) . . . . ?
C15 N2 C11 C10 172.5(3) . . . . ?
C9 C10 C11 N2 -45.2(4) . . . . ?
C9 C10 C11 C12 132.2(4) . . . . ?
N2 C11 C12 C13 2.2(6) . . . . ?
C10 C11 C12 C13 -175.2(4) . . . . ?
C11 C12 C13 C14 1.5(7) . . . . ?
C12 C13 C14 C15 -2.3(6) . . . . ?
C11 N2 C15 C14 4.3(5) . . . . ?
C13 C14 C15 N2 -0.6(6) . . . . ?
C18 N3 C16 C2 58.4(3) . . . . ?
C17 N3 C16 C2 177.4(2) . . . . ?
C3 C2 C16 N3 -124.6(3) . . . . ?
C1 C2 C16 N3 55.8(3) . . . . ?
C17 N3 C18 C19 76.2(3) . . . . ?
C16 N3 C18 C19 -166.9(2) . . . . ?
N3 C18 C19 C20 81.5(3) . . . . ?
C24 N4 C20 C21 -0.4(4) . . . . ?
C24 N4 C20 C19 179.4(2) . . . . ?
C18 C19 C20 N4 -48.3(3) . . . . ?
C18 C19 C20 C21 131.4(3) . . . . ?
N4 C20 C21 C22 -0.5(5) . . . . ?
C19 C20 C21 C22 179.8(3) . . . . ?
C20 C21 C22 C23 1.1(5) . . . . ?
C21 C22 C23 C24 -1.0(5) . . . . ?
C20 N4 C24 C23 0.6(4) . . . . ?
C22 C23 C24 N4 0.1(5) . . . . ?
C3 C4 C25 C27 -165.3(4) . . . . ?
C5 C4 C25 C27 18.2(5) . . . . ?
C3 C4 C25 C26 73.6(4) . . . . ?
C5 C4 C25 C26 -103.0(4) . . . . ?
C3 C4 C25 C28 -43.9(4) . . . . ?
C5 C4 C25 C28 139.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        33.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.107
