# 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/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_ral1108a
_database_code_depnum_ccdc_archive 'CCDC 1017431'
_audit_update_record             
;
2014-08-01 deposited with the CCDC.
2014-12-18 downloaded from the CCDC.
;
_audit_creation_date             12-09-14
_audit_creation_method           CRYSTALS_ver_14.11

_oxford_structure_analysis_title '9131637 ral1108aslow'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   31.9069(3)
_cell_length_b                   15.0731(2)
_cell_length_c                   20.8035(2)
_cell_angle_alpha                90
_cell_angle_beta                 125.4699(6)
_cell_angle_gamma                90
_cell_volume                     8148.40(17)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C44 H54 N4 Ni1 O6 S1 
# Dc =      1.35 Fooo =   3440.00 Mu =      5.81 M =    825.71
# Found Formula = C44 H54 N4 Ni1 O5.00 S1.00 
# Dc =      1.32 FOOO =   3440.00 Mu =      5.78 M =    809.71

_chemical_formula_sum            'C44 H54 N4 Ni O5 S'
_chemical_formula_moiety         'C42 H48 N4 Ni O4, C2 H6 O S'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         809.71


_cell_measurement_reflns_used    53359
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    200

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.160
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_max          0.380

_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3440
_exptl_absorpt_coefficient_mu    0.578

# Sheldrick geometric approximatio 0.90 0.91 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 5 5 0.090
5 -5 -5 0.080
3 3 -3 0.090
-3 -3 3 0.050
1 0 0 0.210
-1 0 0 0.170
1 0 -1 0.130
-1 0 1 0.090
4 -4 4 0.130


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 2.0 deg at rate 250 sec/frame,
crystal-detector distance 28mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            89506
_reflns_number_total             9323
_diffrn_reflns_av_R_equivalents  0.038
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 9323 
# Theoretical number of reflections is about 18683 


_diffrn_reflns_theta_min         2.564
_diffrn_reflns_theta_max         27.481
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        27.481
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -41
_reflns_limit_h_max              33
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              26

_oxford_diffrn_Wilson_B_factor   2.51
_oxford_diffrn_Wilson_scale      17.22

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.69
_refine_diff_density_max         1.33


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         9323
_refine_ls_number_restraints     41
_refine_ls_number_parameters     533
_oxford_refine_ls_R_factor_ref   0.0497
_refine_ls_wR_factor_ref         0.1121
_refine_ls_goodness_of_fit_ref   0.9815
_refine_ls_shift/su_max          0.0138235
_refine_ls_shift/su_mean         0.0008230


# The values computed from all data 
_oxford_reflns_number_all        9323
_refine_ls_R_factor_all          0.0497
_refine_ls_wR_factor_all         0.1121

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7886
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_gt          0.1027

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² +12.69P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
# start Validation Reply Form
_vrf_PUBL024_GLOBAL              
;
PROBLEM: The number of authors is greater than 5.
RESPONSE: KD prepared all compounds with advice and guidance by CR and SFR.
ACW collected, solved, refined and prepared cif files for the three compounds.
AG and J-LM provided help and guidance to KJD for the FRET experiments and 
performed analysis and interpreatation on the FRET data. JB and SFR advised 
KJD on mass spectrometry and DNA binding studies. KJD, JB & SFR analysed and
interpreted mass spec and binding study data. SFR wrote the manuscript with input
from all contributing authors.
;
_vrf_PLAT430_ral1108a            
;
PROBLEM: Short Inter D...A Contact S1 .. O203 .. 2.31 Ang.
RESPONSE: The short contact experienced here is part of a DMSO solvate molecule
severely disordered over two sites. No distances or angle data is used. 
;
_refine_special_details          
;
H atoms of the nickel moiety were all observed in difference electron density
maps but were 
included at calculated positions.
They were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints.
H atoms of the solvate molecule were included at calculated positions
and ride on the atom sites to which they are bonded.


The largest features in the
final difference electron density map are located 
within the region of the disordered solvate molecule..
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.297237(9) 0.289308(16) 0.483093(13) 0.0286 1.0000 Uani . . . . . .
S1 S 0.45819(8) 0.37777(18) 0.63513(14) 0.0871 0.489(3) Uani D U P . . .
S2 S 0.49338(8) 0.32366(19) 0.6277(2) 0.1339 0.511(3) Uani D U P . . .
O1 O 0.34837(5) 0.22510(9) 0.56834(8) 0.0337 1.0000 Uani . . . . . .
O2 O 0.33194(5) 0.38495(9) 0.54782(8) 0.0375 1.0000 Uani . . . . . .
O3 O 0.43969(5) -0.02377(9) 0.73205(8) 0.0357 1.0000 Uani . . . . . .
O4 O 0.37012(6) 0.68238(10) 0.63998(9) 0.0411 1.0000 Uani . . . . . .
N1 N 0.26119(6) 0.19117(11) 0.42207(9) 0.0295 1.0000 Uani . . . . . .
N2 N 0.24847(6) 0.35760(11) 0.39869(9) 0.0304 1.0000 Uani . . . . . .
N3 N 0.43148(6) -0.00845(12) 0.87172(9) 0.0343 1.0000 Uani . . . . . .
N4 N 0.49021(7) 0.71351(12) 0.83754(11) 0.0412 1.0000 Uani . . . . . .
C1 C 0.35269(7) 0.13879(12) 0.57667(11) 0.0291 1.0000 Uani . . . . . .
C2 C 0.39450(7) 0.10528(13) 0.65017(11) 0.0326 1.0000 Uani . . . . . .
C3 C 0.40087(7) 0.01494(13) 0.66288(11) 0.0317 1.0000 Uani . . . . . .
C4 C 0.36664(8) -0.04547(14) 0.60319(12) 0.0361 1.0000 Uani . . . . . .
C5 C 0.32607(8) -0.01330(13) 0.53241(12) 0.0348 1.0000 Uani . . . . . .
C6 C 0.31755(7) 0.07881(13) 0.51712(11) 0.0302 1.0000 Uani . . . . . .
C7 C 0.27273(7) 0.10854(13) 0.44356(11) 0.0312 1.0000 Uani . . . . . .
C8 C 0.20960(7) 0.21371(13) 0.34901(11) 0.0309 1.0000 Uani . . . . . .
C9 C 0.21391(7) 0.30793(13) 0.32416(10) 0.0311 1.0000 Uani . . . . . .
C10 C 0.24389(7) 0.44346(13) 0.39695(11) 0.0325 1.0000 Uani . . . . . .
C11 C 0.27698(7) 0.50197(13) 0.46049(11) 0.0313 1.0000 Uani . . . . . .
C12 C 0.26773(8) 0.59448(14) 0.45173(12) 0.0373 1.0000 Uani . . . . . .
C13 C 0.29861(8) 0.65254(14) 0.51131(12) 0.0390 1.0000 Uani . . . . . .
C14 C 0.34144(8) 0.61952(13) 0.58371(12) 0.0345 1.0000 Uani . . . . . .
C15 C 0.35186(8) 0.53014(14) 0.59477(11) 0.0360 1.0000 Uani . . . . . .
C16 C 0.32001(7) 0.46906(13) 0.53364(11) 0.0315 1.0000 Uani . . . . . .
C17 C 0.18654(7) 0.14622(13) 0.28317(11) 0.0341 1.0000 Uani . . . . . .
C18 C 0.21375(9) 0.11058(15) 0.25606(13) 0.0440 1.0000 Uani . . . . . .
C19 C 0.19005(12) 0.05192(17) 0.19318(15) 0.0590 1.0000 Uani . . . . . .
C20 C 0.13916(13) 0.02876(18) 0.15700(16) 0.0709 1.0000 Uani . . . . . .
C21 C 0.11223(11) 0.06300(19) 0.18342(17) 0.0668 1.0000 Uani . . . . . .
C22 C 0.13550(8) 0.12135(16) 0.24658(14) 0.0480 1.0000 Uani . . . . . .
C23 C 0.23254(7) 0.31380(13) 0.27173(11) 0.0318 1.0000 Uani . . . . . .
C24 C 0.28414(8) 0.32070(15) 0.30130(13) 0.0390 1.0000 Uani . . . . . .
C25 C 0.29907(10) 0.32532(16) 0.25056(15) 0.0474 1.0000 Uani . . . . . .
C26 C 0.26270(11) 0.32309(18) 0.16974(15) 0.0529 1.0000 Uani . . . . . .
C27 C 0.21140(11) 0.31619(19) 0.13978(14) 0.0544 1.0000 Uani . . . . . .
C28 C 0.19642(9) 0.31238(16) 0.19025(12) 0.0429 1.0000 Uani . . . . . .
C29 C 0.47102(7) 0.03094(14) 0.80120(11) 0.0360 1.0000 Uani . . . . . .
C30 C 0.44485(8) 0.06269(14) 0.83865(12) 0.0363 1.0000 Uani . . . . . .
C31 C 0.38209(9) -0.04856(18) 0.81043(13) 0.0477 1.0000 Uani . . . . . .
C32 C 0.36814(11) -0.12417(19) 0.84200(16) 0.0561 1.0000 Uani . . . . . .
C33 C 0.36655(10) -0.0938(2) 0.91005(15) 0.0541 1.0000 Uani . . . . . .
C34 C 0.41672(9) -0.0478(2) 0.97201(14) 0.0532 1.0000 Uani . . . . . .
C35 C 0.42877(8) 0.02549(16) 0.93529(12) 0.0429 1.0000 Uani . . . . . .
C36 C 0.41672(9) 0.65278(15) 0.71224(12) 0.0427 1.0000 Uani . . . . . .
C37 C 0.44041(9) 0.73355(14) 0.76437(13) 0.0411 1.0000 Uani . . . . . .
C38 C 0.51770(9) 0.79578(14) 0.87753(13) 0.0423 1.0000 Uani . . . . . .
C39 C 0.57081(10) 0.77713(17) 0.95126(15) 0.0515 1.0000 Uani . . . . . .
C40 C 0.56796(12) 0.71832(19) 1.00759(15) 0.0654 1.0000 Uani . . . . . .
C41 C 0.53723(14) 0.6353(2) 0.96457(16) 0.0795 1.0000 Uani . . . . . .
C42 C 0.48490(11) 0.65893(18) 0.89042(14) 0.0621 1.0000 Uani . . . . . .
O101 O 0.5035(4) 0.4377(6) 0.6666(7) 0.1446 0.489(3) Uani D U P . . .
C102 C 0.4279(3) 0.3820(5) 0.5332(4) 0.0875 0.489(3) Uani D U P . . .
C103 C 0.4713(3) 0.2830(5) 0.6430(6) 0.1116 0.489(3) Uani D U P . . .
C201 C 0.4758(8) 0.4237(11) 0.6584(13) 0.2544 0.511(3) Uani D U P . . .
C202 C 0.4395(3) 0.2875(6) 0.5423(5) 0.1101 0.511(3) Uani D U P . . .
O203 O 0.5087(2) 0.2520(4) 0.6873(4) 0.1313 0.511(3) Uani D U P . . .
H21 H 0.4170 0.1456 0.6897 0.0380 1.0000 Uiso R . . . . .
H41 H 0.3720 -0.1069 0.6131 0.0425 1.0000 Uiso R . . . . .
H51 H 0.3025 -0.0532 0.4925 0.0411 1.0000 Uiso R . . . . .
H71 H 0.2491 0.0636 0.4067 0.0354 1.0000 Uiso R . . . . .
H81 H 0.1867 0.2181 0.3657 0.0353 1.0000 Uiso R . . . . .
H91 H 0.1796 0.3344 0.2951 0.0353 1.0000 Uiso R . . . . .
H101 H 0.2161 0.4699 0.3480 0.0378 1.0000 Uiso R . . . . .
H121 H 0.2389 0.6156 0.4018 0.0446 1.0000 Uiso R . . . . .
H131 H 0.2921 0.7141 0.5050 0.0462 1.0000 Uiso R . . . . .
H151 H 0.3802 0.5083 0.6435 0.0423 1.0000 Uiso R . . . . .
H181 H 0.2482 0.1263 0.2808 0.0519 1.0000 Uiso R . . . . .
H191 H 0.2094 0.0291 0.1762 0.0700 1.0000 Uiso R . . . . .
H201 H 0.1230 -0.0107 0.1144 0.0835 1.0000 Uiso R . . . . .
H211 H 0.0781 0.0467 0.1591 0.0793 1.0000 Uiso R . . . . .
H221 H 0.1170 0.1441 0.2649 0.0563 1.0000 Uiso R . . . . .
H241 H 0.3085 0.3222 0.3554 0.0463 1.0000 Uiso R . . . . .
H251 H 0.3341 0.3299 0.2720 0.0559 1.0000 Uiso R . . . . .
H261 H 0.2730 0.3259 0.1360 0.0622 1.0000 Uiso R . . . . .
H271 H 0.1863 0.3143 0.0844 0.0645 1.0000 Uiso R . . . . .
H281 H 0.1609 0.3080 0.1699 0.0502 1.0000 Uiso R . . . . .
H291 H 0.5007 -0.0067 0.8402 0.0422 1.0000 Uiso R . . . . .
H292 H 0.4838 0.0821 0.7888 0.0420 1.0000 Uiso R . . . . .
H301 H 0.4693 0.1029 0.8818 0.0433 1.0000 Uiso R . . . . .
H302 H 0.4137 0.0985 0.8003 0.0427 1.0000 Uiso R . . . . .
H311 H 0.3540 -0.0021 0.7880 0.0559 1.0000 Uiso R . . . . .
H312 H 0.3839 -0.0701 0.7682 0.0562 1.0000 Uiso R . . . . .
H321 H 0.3939 -0.1710 0.8616 0.0667 1.0000 Uiso R . . . . .
H322 H 0.3339 -0.1482 0.7987 0.0670 1.0000 Uiso R . . . . .
H331 H 0.3606 -0.1441 0.9336 0.0639 1.0000 Uiso R . . . . .
H332 H 0.3384 -0.0501 0.8902 0.0641 1.0000 Uiso R . . . . .
H341 H 0.4146 -0.0227 1.0147 0.0631 1.0000 Uiso R . . . . .
H342 H 0.4444 -0.0924 0.9961 0.0629 1.0000 Uiso R . . . . .
H351 H 0.4615 0.0532 0.9753 0.0502 1.0000 Uiso R . . . . .
H352 H 0.4018 0.0719 0.9143 0.0502 1.0000 Uiso R . . . . .
H361 H 0.4405 0.6278 0.7021 0.0499 1.0000 Uiso R . . . . .
H362 H 0.4086 0.6081 0.7374 0.0498 1.0000 Uiso R . . . . .
H371 H 0.4456 0.7782 0.7356 0.0480 1.0000 Uiso R . . . . .
H372 H 0.4168 0.7571 0.7751 0.0476 1.0000 Uiso R . . . . .
H381 H 0.4976 0.8290 0.8914 0.0498 1.0000 Uiso R . . . . .
H382 H 0.5209 0.8308 0.8408 0.0499 1.0000 Uiso R . . . . .
H391 H 0.5878 0.8340 0.9761 0.0606 1.0000 Uiso R . . . . .
H392 H 0.5906 0.7470 0.9365 0.0606 1.0000 Uiso R . . . . .
H401 H 0.6027 0.7022 1.0516 0.0780 1.0000 Uiso R . . . . .
H402 H 0.5514 0.7508 1.0273 0.0780 1.0000 Uiso R . . . . .
H411 H 0.5327 0.6000 0.9980 0.0941 1.0000 Uiso R . . . . .
H412 H 0.5562 0.6012 0.9492 0.0941 1.0000 Uiso R . . . . .
H421 H 0.4649 0.6906 0.9052 0.0738 1.0000 Uiso R . . . . .
H422 H 0.4665 0.6052 0.8628 0.0738 1.0000 Uiso R . . . . .
H1021 H 0.3981 0.3455 0.5073 0.1048 0.489 Uiso R . . . . .
H1022 H 0.4510 0.3614 0.5215 0.1048 0.489 Uiso R . . . . .
H1023 H 0.4183 0.4415 0.5154 0.1048 0.489 Uiso R . . . . .
H1031 H 0.4411 0.2485 0.6220 0.1339 0.489 Uiso R . . . . .
H1032 H 0.4956 0.2689 0.6972 0.1339 0.489 Uiso R . . . . .
H1033 H 0.4857 0.2705 0.6148 0.1339 0.489 Uiso R . . . . .
H2011 H 0.4660 0.4697 0.6210 0.3056 0.511 Uiso R . . . . .
H2012 H 0.5045 0.4425 0.7087 0.3056 0.511 Uiso R . . . . .
H2013 H 0.4479 0.4103 0.6613 0.3056 0.511 Uiso R . . . . .
H2021 H 0.4282 0.3310 0.5024 0.1325 0.511 Uiso R . . . . .
H2022 H 0.4467 0.2337 0.5266 0.1325 0.511 Uiso R . . . . .
H2023 H 0.4132 0.2773 0.5499 0.1325 0.511 Uiso R . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.2764(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
#     do we want this?????????????????
Ni1 . O1 . 1.8400(13) yes
Ni1 . O2 . 1.8404(14) yes
Ni1 . N1 . 1.8515(16) yes
Ni1 . N2 . 1.8419(15) yes
Ni1 . Ni1 4_556 3.6669(5) yes
S1 . S2 . 1.466(3) yes
S1 . O101 . 1.495(8) yes
S1 . C102 . 1.749(7) yes
S1 . C103 . 1.470(8) yes
S2 . C201 . 1.847(14) yes
S2 . C202 . 1.693(8) yes
S2 . O203 . 1.496(7) yes
O1 . C1 . 1.309(2) yes
O2 . C16 . 1.307(2) yes
O3 . C3 . 1.370(2) yes
O3 . C29 . 1.442(2) yes
O4 . C14 . 1.365(2) yes
O4 . C36 . 1.441(2) yes
N1 . C7 . 1.302(3) yes
N1 . C8 . 1.494(2) yes
N2 . C9 . 1.482(2) yes
N2 . C10 . 1.301(3) yes
N3 . C30 . 1.465(3) yes
N3 . C31 . 1.464(3) yes
N3 . C35 . 1.467(3) yes
N4 . C37 . 1.458(3) yes
N4 . C38 . 1.467(3) yes
N4 . C42 . 1.460(3) yes
C1 . C2 . 1.416(3) yes
C1 . C6 . 1.413(3) yes
C2 . C3 . 1.380(3) yes
C2 . H21 . 0.935 no
C3 . C4 . 1.411(3) yes
C4 . C5 . 1.366(3) yes
C4 . H41 . 0.942 no
C5 . C6 . 1.415(3) yes
C5 . H51 . 0.944 no
C6 . C7 . 1.431(3) yes
C7 . H71 . 0.971 no
C8 . C9 . 1.544(3) yes
C8 . C17 . 1.511(3) yes
C8 . H81 . 0.975 no
C9 . C23 . 1.518(3) yes
C9 . H91 . 0.977 no
C10 . C11 . 1.421(3) yes
C10 . H101 . 0.967 no
C11 . C12 . 1.415(3) yes
C11 . C16 . 1.422(3) yes
C12 . C13 . 1.362(3) yes
C12 . H121 . 0.957 no
C13 . C14 . 1.412(3) yes
C13 . H131 . 0.943 no
C14 . C15 . 1.375(3) yes
C15 . C16 . 1.413(3) yes
C15 . H151 . 0.944 no
C17 . C18 . 1.389(3) yes
C17 . C22 . 1.390(3) yes
C18 . C19 . 1.384(3) yes
C18 . H181 . 0.935 no
C19 . C20 . 1.381(4) yes
C19 . H191 . 0.936 no
C20 . C21 . 1.362(5) yes
C20 . H201 . 0.936 no
C21 . C22 . 1.385(4) yes
C21 . H211 . 0.929 no
C22 . H221 . 0.933 no
C23 . C24 . 1.387(3) yes
C23 . C28 . 1.391(3) yes
C24 . C25 . 1.389(3) yes
C24 . H241 . 0.926 no
C25 . C26 . 1.382(3) yes
C25 . H251 . 0.934 no
C26 . C27 . 1.376(4) yes
C26 . H261 . 0.934 no
C27 . C28 . 1.384(3) yes
C27 . H271 . 0.948 no
C28 . H281 . 0.954 no
C29 . C30 . 1.513(3) yes
C29 . H291 . 0.993 no
C29 . H292 . 0.975 no
C30 . H301 . 0.984 no
C30 . H302 . 0.999 no
C31 . C32 . 1.506(3) yes
C31 . H311 . 1.013 no
C31 . H312 . 0.969 no
C32 . C33 . 1.516(3) yes
C32 . H321 . 0.976 no
C32 . H322 . 0.997 no
C33 . C34 . 1.520(3) yes
C33 . H331 . 0.979 no
C33 . H332 . 0.990 no
C34 . C35 . 1.514(3) yes
C34 . H341 . 1.002 no
C34 . H342 . 0.984 no
C35 . H351 . 0.973 no
C35 . H352 . 0.992 no
C36 . C37 . 1.509(3) yes
C36 . H361 . 0.976 no
C36 . H362 . 0.976 no
C37 . H371 . 0.977 no
C37 . H372 . 0.968 no
C38 . C39 . 1.512(3) yes
C38 . H381 . 0.980 no
C38 . H382 . 0.982 no
C39 . C40 . 1.513(4) yes
C39 . H391 . 0.985 no
C39 . H392 . 0.962 no
C40 . C41 . 1.520(4) yes
C40 . H401 . 0.973 no
C40 . H402 . 0.969 no
C41 . C42 . 1.518(4) yes
C41 . H411 . 0.950 no
C41 . H412 . 0.980 no
C42 . H421 . 0.978 no
C42 . H422 . 0.969 no
C102 . H1021 . 0.950 no
C102 . H1022 . 0.950 no
C102 . H1023 . 0.950 no
C103 . H1031 . 0.950 no
C103 . H1032 . 0.950 no
C103 . H1033 . 0.950 no
C201 . H2011 . 0.950 no
C201 . H2012 . 0.950 no
C201 . H2013 . 0.950 no
C202 . H2021 . 0.950 no
C202 . H2022 . 0.950 no
C202 . H2023 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Ni1 . O2 . 83.47(6) yes
O1 . Ni1 . N1 . 95.23(6) yes
O2 . Ni1 . N1 . 176.48(7) yes
O1 . Ni1 . N2 . 177.18(7) yes
O2 . Ni1 . N2 . 94.39(7) yes
N1 . Ni1 . N2 . 87.01(7) yes
Ni1 4_556 Ni1 . O1 . 90.74(5) yes
Ni1 4_556 Ni1 . O2 . 108.99(5) yes
Ni1 4_556 Ni1 . N1 . 67.70(5) yes
Ni1 4_556 Ni1 . N2 . 91.70(5) yes
O101 . S1 . C102 . 102.8(5) yes
O101 . S1 . C103 . 113.4(5) yes
C102 . S1 . C103 . 95.2(5) yes
C201 . S2 . C202 . 107.4(7) yes
C201 . S2 . O203 . 108.8(8) yes
C202 . S2 . O203 . 106.3(5) yes
Ni1 . O1 . C1 . 128.07(12) yes
Ni1 . O2 . C16 . 128.45(12) yes
C3 . O3 . C29 . 119.02(15) yes
C14 . O4 . C36 . 116.90(16) yes
Ni1 . N1 . C7 . 126.12(13) yes
Ni1 . N1 . C8 . 113.28(12) yes
C7 . N1 . C8 . 119.47(16) yes
Ni1 . N2 . C9 . 114.78(12) yes
Ni1 . N2 . C10 . 127.00(14) yes
C9 . N2 . C10 . 118.05(16) yes
C30 . N3 . C31 . 110.67(16) yes
C30 . N3 . C35 . 110.71(17) yes
C31 . N3 . C35 . 109.42(16) yes
C37 . N4 . C38 . 110.34(17) yes
C37 . N4 . C42 . 111.77(19) yes
C38 . N4 . C42 . 109.98(18) yes
O1 . C1 . C2 . 117.27(17) yes
O1 . C1 . C6 . 123.42(17) yes
C2 . C1 . C6 . 119.30(17) yes
C1 . C2 . C3 . 120.05(18) yes
C1 . C2 . H21 . 118.6 no
C3 . C2 . H21 . 121.3 no
C2 . C3 . O3 . 124.37(18) yes
C2 . C3 . C4 . 121.04(18) yes
O3 . C3 . C4 . 114.58(17) yes
C3 . C4 . C5 . 119.01(19) yes
C3 . C4 . H41 . 119.5 no
C5 . C4 . H41 . 121.5 no
C4 . C5 . C6 . 121.91(19) yes
C4 . C5 . H51 . 119.6 no
C6 . C5 . H51 . 118.5 no
C5 . C6 . C1 . 118.66(17) yes
C5 . C6 . C7 . 119.34(18) yes
C1 . C6 . C7 . 121.95(17) yes
C6 . C7 . N1 . 125.07(18) yes
C6 . C7 . H71 . 117.5 no
N1 . C7 . H71 . 117.4 no
N1 . C8 . C9 . 106.87(15) yes
N1 . C8 . C17 . 116.02(16) yes
C9 . C8 . C17 . 114.01(15) yes
N1 . C8 . H81 . 105.3 no
C9 . C8 . H81 . 106.7 no
C17 . C8 . H81 . 107.2 no
C8 . C9 . N2 . 105.73(14) yes
C8 . C9 . C23 . 116.24(16) yes
N2 . C9 . C23 . 111.00(15) yes
C8 . C9 . H91 . 107.2 no
N2 . C9 . H91 . 109.1 no
C23 . C9 . H91 . 107.3 no
N2 . C10 . C11 . 125.50(17) yes
N2 . C10 . H101 . 117.4 no
C11 . C10 . H101 . 117.1 no
C10 . C11 . C12 . 120.32(17) yes
C10 . C11 . C16 . 120.91(18) yes
C12 . C11 . C16 . 118.77(18) yes
C11 . C12 . C13 . 121.94(19) yes
C11 . C12 . H121 . 117.7 no
C13 . C12 . H121 . 120.4 no
C12 . C13 . C14 . 119.03(19) yes
C12 . C13 . H131 . 121.4 no
C14 . C13 . H131 . 119.6 no
C13 . C14 . O4 . 114.98(18) yes
C13 . C14 . C15 . 120.95(19) yes
O4 . C14 . C15 . 124.07(18) yes
C14 . C15 . C16 . 120.66(18) yes
C14 . C15 . H151 . 120.7 no
C16 . C15 . H151 . 118.7 no
C11 . C16 . C15 . 118.64(18) yes
C11 . C16 . O2 . 123.62(17) yes
C15 . C16 . O2 . 117.74(17) yes
C8 . C17 . C18 . 122.56(18) yes
C8 . C17 . C22 . 118.52(19) yes
C18 . C17 . C22 . 118.9(2) yes
C17 . C18 . C19 . 120.2(2) yes
C17 . C18 . H181 . 119.5 no
C19 . C18 . H181 . 120.3 no
C18 . C19 . C20 . 120.1(3) yes
C18 . C19 . H191 . 118.2 no
C20 . C19 . H191 . 121.7 no
C19 . C20 . C21 . 120.1(2) yes
C19 . C20 . H201 . 120.2 no
C21 . C20 . H201 . 119.7 no
C20 . C21 . C22 . 120.5(3) yes
C20 . C21 . H211 . 119.7 no
C22 . C21 . H211 . 119.8 no
C17 . C22 . C21 . 120.2(3) yes
C17 . C22 . H221 . 119.6 no
C21 . C22 . H221 . 120.2 no
C9 . C23 . C24 . 123.00(17) yes
C9 . C23 . C28 . 118.79(18) yes
C24 . C23 . C28 . 118.21(19) yes
C23 . C24 . C25 . 120.6(2) yes
C23 . C24 . H241 . 119.0 no
C25 . C24 . H241 . 120.4 no
C24 . C25 . C26 . 120.5(2) yes
C24 . C25 . H251 . 118.9 no
C26 . C25 . H251 . 120.6 no
C25 . C26 . C27 . 119.4(2) yes
C25 . C26 . H261 . 120.0 no
C27 . C26 . H261 . 120.6 no
C26 . C27 . C28 . 120.2(2) yes
C26 . C27 . H271 . 119.9 no
C28 . C27 . H271 . 119.9 no
C23 . C28 . C27 . 121.1(2) yes
C23 . C28 . H281 . 118.2 no
C27 . C28 . H281 . 120.7 no
O3 . C29 . C30 . 115.12(16) yes
O3 . C29 . H291 . 105.5 no
C30 . C29 . H291 . 108.2 no
O3 . C29 . H292 . 110.0 no
C30 . C29 . H292 . 109.1 no
H291 . C29 . H292 . 108.6 no
C29 . C30 . N3 . 114.11(17) yes
C29 . C30 . H301 . 106.4 no
N3 . C30 . H301 . 108.3 no
C29 . C30 . H302 . 110.6 no
N3 . C30 . H302 . 110.2 no
H301 . C30 . H302 . 106.9 no
N3 . C31 . C32 . 112.0(2) yes
N3 . C31 . H311 . 109.5 no
C32 . C31 . H311 . 108.5 no
N3 . C31 . H312 . 109.1 no
C32 . C31 . H312 . 109.3 no
H311 . C31 . H312 . 108.4 no
C31 . C32 . C33 . 111.0(2) yes
C31 . C32 . H321 . 109.8 no
C33 . C32 . H321 . 107.8 no
C31 . C32 . H322 . 109.0 no
C33 . C32 . H322 . 109.9 no
H321 . C32 . H322 . 109.3 no
C32 . C33 . C34 . 109.88(19) yes
C32 . C33 . H331 . 110.8 no
C34 . C33 . H331 . 110.1 no
C32 . C33 . H332 . 108.9 no
C34 . C33 . H332 . 107.6 no
H331 . C33 . H332 . 109.5 no
C33 . C34 . C35 . 110.9(2) yes
C33 . C34 . H341 . 110.2 no
C35 . C34 . H341 . 109.8 no
C33 . C34 . H342 . 108.2 no
C35 . C34 . H342 . 109.8 no
H341 . C34 . H342 . 107.9 no
C34 . C35 . N3 . 111.43(19) yes
C34 . C35 . H351 . 110.0 no
N3 . C35 . H351 . 109.0 no
C34 . C35 . H352 . 109.1 no
N3 . C35 . H352 . 109.8 no
H351 . C35 . H352 . 107.4 no
O4 . C36 . C37 . 106.45(17) yes
O4 . C36 . H361 . 110.8 no
C37 . C36 . H361 . 109.8 no
O4 . C36 . H362 . 109.9 no
C37 . C36 . H362 . 110.4 no
H361 . C36 . H362 . 109.4 no
C36 . C37 . N4 . 111.77(18) yes
C36 . C37 . H371 . 107.9 no
N4 . C37 . H371 . 108.2 no
C36 . C37 . H372 . 109.2 no
N4 . C37 . H372 . 110.9 no
H371 . C37 . H372 . 108.7 no
N4 . C38 . C39 . 111.55(19) yes
N4 . C38 . H381 . 108.7 no
C39 . C38 . H381 . 109.7 no
N4 . C38 . H382 . 108.1 no
C39 . C38 . H382 . 109.2 no
H381 . C38 . H382 . 109.6 no
C38 . C39 . C40 . 111.0(2) yes
C38 . C39 . H391 . 108.8 no
C40 . C39 . H391 . 111.4 no
C38 . C39 . H392 . 108.7 no
C40 . C39 . H392 . 108.5 no
H391 . C39 . H392 . 108.3 no
C39 . C40 . C41 . 109.5(2) yes
C39 . C40 . H401 . 109.2 no
C41 . C40 . H401 . 110.0 no
C39 . C40 . H402 . 108.9 no
C41 . C40 . H402 . 110.0 no
H401 . C40 . H402 . 109.3 no
C40 . C41 . C42 . 111.0(2) yes
C40 . C41 . H411 . 110.5 no
C42 . C41 . H411 . 109.3 no
C40 . C41 . H412 . 108.3 no
C42 . C41 . H412 . 108.4 no
H411 . C41 . H412 . 109.4 no
C41 . C42 . N4 . 111.0(2) yes
C41 . C42 . H421 . 109.1 no
N4 . C42 . H421 . 110.1 no
C41 . C42 . H422 . 109.6 no
N4 . C42 . H422 . 108.6 no
H421 . C42 . H422 . 108.3 no

#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
S1 O2 3.324(3) . . no
S1 C201 3.59(2) . 5_656 no
O1 C8 3.304(3) . 4_556 no
O1 C202 3.39(1) . . no
O1 C103 3.389(9) . . no
O2 C102 3.25(1) . . no
O2 C8 3.446(3) . 4_556 no
O2 C7 3.448(3) . 4_556 no
O2 N1 3.563(3) . 4_556 no
O3 C29 3.400(3) . 5_656 no
O3 O3 3.469(4) . 5_656 no
O101 C21 3.28(2) . 8 no
O101 C201 3.31(3) . 5_656 no
O203 O203 2.97(2) . 5_656 no
O203 C103 3.24(2) . 5_656 no
O203 C29 3.376(6) . 5_656 no
O203 C30 3.400(7) . 5_656 no
N2 C1 3.550(4) . 4_556 no
N2 C6 3.565(4) . 4_556 no
C5 C11 3.380(4) . 4_556 no
C5 C12 3.422(4) . 4_556 no
C5 C10 3.472(4) . 4_556 no
C6 C10 3.349(4) . 4_556 no
C6 C33 3.391(5) . 6_554 no
C6 C11 3.525(4) . 4_556 no
C7 C33 3.452(5) . 6_554 no
C7 C16 3.461(4) . 4_556 no
C7 C11 3.599(4) . 4_556 no
C19 C25 3.562(4) . 7_545 no
C19 C24 3.568(4) . 7_545 no
C20 C25 3.548(4) . 7_545 no
C25 C32 3.578(4) . 6_554 no
C29 C29 3.540(6) . 5_656 no
C201 C201 3.17(5) . 5_656 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ni1 O1 C1 C2 . . . . -176.7(2) no
Ni1 O1 C1 C6 . . . . 2.1(4) no
Ni1 O2 C16 C11 . . . . -2.8(4) no
Ni1 O2 C16 C15 . . . . 177.1(2) no
Ni1 N1 C7 C6 . . . . -4.1(4) no
Ni1 N1 C8 C9 . . . . 30.1(3) no
Ni1 N1 C8 C17 . . . . 158.5(2) no
Ni1 N2 C9 C8 . . . . 30.1(2) no
Ni1 N2 C9 C23 . . . . -96.8(2) no
Ni1 N2 C10 C11 . . . . 1.5(4) no
O1 Ni1 O2 C16 . . . . -177.8(2) no
O1 Ni1 N1 C7 . . . . 2.6(3) no
O1 Ni1 N1 C8 . . . . 170.2(2) no
O1 C1 C2 C3 . . . . 179.4(3) no
O1 C1 C6 C5 . . . . 179.8(3) no
O1 C1 C6 C7 . . . . -2.9(4) no
O2 Ni1 O1 C1 . . . . 175.1(2) no
O2 Ni1 N2 C9 . . . . 171.6(2) no
O2 Ni1 N2 C10 . . . . -3.4(3) no
O2 C16 C11 C10 . . . . -0.4(4) no
O2 C16 C11 C12 . . . . 180.0(3) no
O2 C16 C15 C14 . . . . -180.0(3) no
O3 C3 C2 C1 . . . . -179.3(3) no
O3 C3 C4 C5 . . . . 178.9(3) no
O3 C29 C30 N3 . . . . 65.3(2) no
O4 C14 C13 C12 . . . . -179.9(3) no
O4 C14 C15 C16 . . . . 179.5(3) no
O4 C36 C37 N4 . . . . -175.6(3) no
N1 Ni1 O1 C1 . . . . -1.6(2) no
N1 Ni1 N2 C9 . . . . -11.6(2) no
N1 Ni1 N2 C10 . . . . 173.4(3) no
N1 C7 C6 C1 . . . . 4.0(5) no
N1 C7 C6 C5 . . . . -178.6(3) no
N1 C8 C9 N2 . . . . -36.6(3) no
N1 C8 C9 C23 . . . . 87.1(2) no
N1 C8 C17 C18 . . . . -49.6(3) no
N1 C8 C17 C22 . . . . 132.7(2) no
N2 Ni1 O2 C16 . . . . 4.1(2) no
N2 Ni1 N1 C7 . . . . -179.1(3) no
N2 Ni1 N1 C8 . . . . -11.5(2) no
N2 C9 C8 C17 . . . . -166.1(2) no
N2 C9 C23 C24 . . . . 31.4(3) no
N2 C9 C23 C28 . . . . -148.5(2) no
N2 C10 C11 C12 . . . . -179.3(3) no
N2 C10 C11 C16 . . . . 1.0(5) no
N3 C31 C32 C33 . . . . 57.2(3) no
N3 C35 C34 C33 . . . . -57.3(3) no
N4 C38 C39 C40 . . . . -57.0(4) no
N4 C42 C41 C40 . . . . 57.7(4) no
C1 C2 C3 C4 . . . . 0.9(4) no
C1 C6 C5 C4 . . . . 1.0(5) no
C2 C1 C6 C5 . . . . -1.5(4) no
C2 C1 C6 C7 . . . . 175.9(3) no
C2 C3 O3 C29 . . . . 11.5(4) no
C2 C3 C4 C5 . . . . -1.3(5) no
C3 O3 C29 C30 . . . . 72.9(3) no
C3 C2 C1 C6 . . . . 0.5(4) no
C3 C4 C5 C6 . . . . 0.3(5) no
C4 C3 O3 C29 . . . . -168.7(2) no
C4 C5 C6 C7 . . . . -176.4(3) no
C6 C7 N1 C8 . . . . -171.1(3) no
C7 N1 C8 C9 . . . . -161.3(2) no
C7 N1 C8 C17 . . . . -32.9(4) no
C8 C9 N2 C10 . . . . -154.5(2) no
C8 C9 C23 C24 . . . . -89.5(2) no
C8 C9 C23 C28 . . . . 90.7(2) no
C8 C17 C18 C19 . . . . -177.1(2) no
C8 C17 C22 C21 . . . . 176.8(2) no
C9 N2 C10 C11 . . . . -173.3(3) no
C9 C8 C17 C18 . . . . 75.2(2) no
C9 C8 C17 C22 . . . . -102.5(3) no
C9 C23 C24 C25 . . . . 179.6(2) no
C9 C23 C28 C27 . . . . -179.0(2) no
C10 N2 C9 C23 . . . . 78.7(3) no
C10 C11 C12 C13 . . . . -180.0(3) no
C10 C11 C16 C15 . . . . 179.7(3) no
C11 C12 C13 C14 . . . . 0.7(5) no
C11 C16 C15 C14 . . . . -0.0(4) no
C12 C11 C16 C15 . . . . 0.0(4) no
C12 C13 C14 C15 . . . . -0.6(5) no
C13 C12 C11 C16 . . . . -0.4(5) no
C13 C14 O4 C36 . . . . -174.6(3) no
C13 C14 C15 C16 . . . . 0.3(5) no
C14 O4 C36 C37 . . . . -179.0(3) no
C15 C14 O4 C36 . . . . 6.1(4) no
C17 C8 C9 C23 . . . . -42.5(2) no
C17 C18 C19 C20 . . . . 0.2(4) no
C17 C22 C21 C20 . . . . 0.6(4) no
C18 C17 C22 C21 . . . . -1.0(4) no
C18 C19 C20 C21 . . . . -0.5(4) no
C19 C18 C17 C22 . . . . 0.6(3) no
C19 C20 C21 C22 . . . . 0.1(4) no
C23 C24 C25 C26 . . . . -0.0(4) no
C23 C28 C27 C26 . . . . -1.2(4) no
C24 C23 C28 C27 . . . . 1.1(3) no
C24 C25 C26 C27 . . . . -0.0(4) no
C25 C24 C23 C28 . . . . -0.5(3) no
C25 C26 C27 C28 . . . . 0.6(4) no
C29 C30 N3 C31 . . . . -84.2(2) no
C29 C30 N3 C35 . . . . 154.3(1) no
C30 N3 C31 C32 . . . . 178.0(2) no
C30 N3 C35 C34 . . . . -178.1(2) no
C31 N3 C35 C34 . . . . 59.6(2) no
C31 C32 C33 C34 . . . . -52.9(3) no
C32 C31 N3 C35 . . . . -59.7(3) no
C32 C33 C34 C35 . . . . 53.1(3) no
C36 C37 N4 C38 . . . . 166.2(3) no
C36 C37 N4 C42 . . . . -71.1(3) no
C37 N4 C38 C39 . . . . -176.7(3) no
C37 N4 C42 C41 . . . . 177.4(2) no
C38 N4 C42 C41 . . . . -59.7(3) no
C38 C39 C40 C41 . . . . 53.4(4) no
C39 C38 N4 C42 . . . . 59.6(3) no
C39 C40 C41 C42 . . . . -53.8(5) no

#------------------------------------------------------------------------------



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 14/09/12 at 14:41:04
#
#LIST     12                                                                    
BLOCK SCALE X'S, NI(1,U'S) S(1,OCC,U'S) UNTIL S(2) 
CONT O(1,U'S) UNTIL O(4) N(1,U'S) UNTIL C(42) 
CONT O(101,U'S,OCC) C(102,U'S,OCC) UNTIL C(202) O(203,U'S,OCC) 
EQUIV S(1,OCC) S(2,OCC) O(101,OCC) C(102,OCC) UNTIL C(202) O(203,OCC) 
WEIGHT -1 S(2,OCC) C(201,OCC) UNTIL C(202) O(203,OCC) 
RIDE C ( 2,X'S) H( 21,X'S) 
RIDE C ( 4,X'S) H( 41,X'S) 
RIDE C ( 5,X'S) H( 51,X'S) 
RIDE C ( 7,X'S) H( 71,X'S) 
RIDE C ( 8,X'S) H( 81,X'S) 
RIDE C ( 9,X'S) H( 91,X'S) 
RIDE C ( 10,X'S) H( 101,X'S) 
RIDE C ( 12,X'S) H( 121,X'S) 
RIDE C ( 13,X'S) H( 131,X'S) 
RIDE C ( 15,X'S) H( 151,X'S) 
RIDE C ( 18,X'S) H( 181,X'S) 
RIDE C ( 19,X'S) H( 191,X'S) 
RIDE C ( 20,X'S) H( 201,X'S) 
RIDE C ( 21,X'S) H( 211,X'S) 
RIDE C ( 22,X'S) H( 221,X'S) 
RIDE C ( 24,X'S) H( 241,X'S) 
RIDE C ( 25,X'S) H( 251,X'S) 
RIDE C ( 26,X'S) H( 261,X'S) 
RIDE C ( 27,X'S) H( 271,X'S) 
RIDE C ( 28,X'S) H( 281,X'S) 
RIDE C ( 29,X'S) H( 291,X'S) H( 292,X'S) 
RIDE C ( 30,X'S) H( 301,X'S) H( 302,X'S) 
RIDE C ( 31,X'S) H( 311,X'S) H( 312,X'S) 
RIDE C ( 32,X'S) H( 321,X'S) H( 322,X'S) 
RIDE C ( 33,X'S) H( 331,X'S) H( 332,X'S) 
RIDE C ( 34,X'S) H( 341,X'S) H( 342,X'S) 
RIDE C ( 35,X'S) H( 351,X'S) H( 352,X'S) 
RIDE C ( 36,X'S) H( 361,X'S) H( 362,X'S) 
RIDE C ( 37,X'S) H( 371,X'S) H( 372,X'S) 
RIDE C ( 38,X'S) H( 381,X'S) H( 382,X'S) 
RIDE C ( 39,X'S) H( 391,X'S) H( 392,X'S) 
RIDE C ( 40,X'S) H( 401,X'S) H( 402,X'S) 
RIDE C ( 41,X'S) H( 411,X'S) H( 412,X'S) 
RIDE C ( 42,X'S) H( 421,X'S) H( 422,X'S) 
RIDE C(102,X'S) H(1021,X'S) H(1022,X'S) H(1023,X'S) 
RIDE C(103,X'S) H(1031,X'S) H(1032,X'S) H(1033,X'S) 
RIDE C(201,X'S) H(2011,X'S) H(2012,X'S) H(2013,X'S) 
RIDE C(202,X'S) H(2021,X'S) H(2022,X'S) H(2023,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 14/09/12 at 14:41:04
#
#LIST     16                                                                    
REM 
DIST 1.70, .02 = S(1) TO O(101) 
DIST 1.80, .02 = S(1) TO C(102), S(1) TO C(103) 
ANGLE 100, 2. = C(102) TO S(1) TO C(103) 
ANGLE 103, 2. = O(101) TO S(1) TO C(102), O(101) TO S(1) TO C(103) 
REM 
DIST 1.70, .02 = S(2) TO O(203) 
DIST 1.80, .02 = S(2) TO C(202), S(2) TO C(201) 
ANGLE 100, 2. = C(202) TO S(2) TO C(201) 
ANGLE 103, 2. = C(201) TO S(2) TO O(203), C(202) TO S(2) TO O(203) 
REM 
VIBR 0.0, .01 = S(1) TO O(101), S(1) TO C(102) 
VIBR 0.0, .01 = S(2) TO C(201), S(2) TO C(202), S(2) TO O(203) 
U(IJ) 0.0, .02 = O(101) TO C(201), C(102) TO C(202) 
U(IJ) 0.0, .005 =  C(103) TO O(203) 
U(IJ) 0.0, .03 = S(1) TO C(103) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_ral1107
_database_code_depnum_ccdc_archive 'CCDC 1017432'
_audit_update_record             
;
2014-08-01 deposited with the CCDC.
2014-12-18 downloaded from the CCDC.
;
_audit_creation_date             12-09-13
_audit_creation_method           CRYSTALS_ver_14.11

_oxford_structure_analysis_title '9131447 ral1107 - squeezed'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   20.0562(7)
_cell_length_b                   10.1772(2)
_cell_length_c                   22.9552(7)
_cell_angle_alpha                90
_cell_angle_beta                 112.4092(13)
_cell_angle_gamma                90
_cell_volume                     4331.7(2)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C46 H58 N4 Ni1 O6 S1 
# Dc =      1.31 Fooo =   1616.00 Mu =      5.49 M =    853.77
# Found Formula = C44 H52 N4 Ni1 O4 
# Dc =      1.16 FOOO =   1616.00 Mu =      4.91 M =    759.63

_chemical_formula_sum            'C44 H52 N4 Ni O4'
_chemical_formula_moiety         'C44 H52 N4 Ni O4'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         759.63


_cell_measurement_reflns_used    52417
_cell_measurement_theta_min      3
_cell_measurement_theta_max      25
_cell_measurement_temperature    200

_exptl_crystal_description       lath
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.040
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.420

_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.491

# Sheldrick geometric approximatio 0.94 0.98 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.728 # 0.981*8.17/11.01; 0.94 
_exptl_absorpt_correction_T_max  0.981 # 0.98 
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 1.6 deg at rate 240 sec/frame,
crystal-detector distance 30mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      200
_diffrn_reflns_number            63136
_reflns_number_total             7680
_diffrn_reflns_av_R_equivalents  0.118 # scalepack 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7680 
# Theoretical number of reflections is about 15434 


_diffrn_reflns_theta_min         2.634
_diffrn_reflns_theta_max         25.101
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        25.101
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              -23
_reflns_limit_h_max              22
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              27

_oxford_diffrn_Wilson_B_factor   2.56
_oxford_diffrn_Wilson_scale      47.90

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.56
_refine_diff_density_max         0.79


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         7679
_refine_ls_number_restraints     0
_refine_ls_number_parameters     478
_oxford_refine_ls_R_factor_ref   0.0854
_refine_ls_wR_factor_ref         0.1475
_refine_ls_goodness_of_fit_ref   0.9693
_refine_ls_shift/su_max          0.0004726
_refine_ls_shift/su_mean         0.0000995


# The values computed from all data 
_oxford_reflns_number_all        7679
_refine_ls_R_factor_all          0.0854
_refine_ls_wR_factor_all         0.1475

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5282
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_gt          0.1275

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² + 5.99P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.500 314 59 ' '
2 0.000 0.500 0.000 314 59 ' '
_platon_squeeze_details          
;
disordered dmso
;
_refine_special_details          
;
SQUEEZE was used to account for the electron density arising
from a highly-disordered solvate molecule.

All H atoms of the nickel species were observed 
in difference electron density maps, but were 
included at calculated positions.
They were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints.


The largest features in the
final difference electron density map are located 
randomly through the structure.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.73891(2) 0.62896(4) 0.27910(2) 0.0321 1.0000 Uani . . . . . .
O1 O 0.66669(12) 0.5496(2) 0.29805(10) 0.0349 1.0000 Uani . . . . . .
O2 O 0.79783(13) 0.5891(2) 0.36124(11) 0.0404 1.0000 Uani . . . . . .
O3 O 0.42703(14) 0.4751(3) 0.28364(12) 0.0548 1.0000 Uani . . . . . .
O4 O 0.98623(14) 0.6523(2) 0.56156(11) 0.0431 1.0000 Uani . . . . . .
N1 N 0.68092(16) 0.6676(3) 0.19642(13) 0.0326 1.0000 Uani . . . . . .
N2 N 0.81021(15) 0.7166(3) 0.26319(12) 0.0331 1.0000 Uani . . . . . .
N3 N 0.34172(19) 0.3692(4) 0.44815(16) 0.0593 1.0000 Uani . . . . . .
N4 N 0.9057(2) 0.4421(4) 0.68529(17) 0.0621 1.0000 Uani . . . . . .
C1 C 0.59705(19) 0.5534(3) 0.26453(16) 0.0341 1.0000 Uani . . . . . .
C2 C 0.5497(2) 0.5088(4) 0.29224(17) 0.0385 1.0000 Uani . . . . . .
C3 C 0.4762(2) 0.5115(4) 0.25945(18) 0.0430 1.0000 Uani . . . . . .
C4 C 0.4470(2) 0.5567(4) 0.19695(17) 0.0455 1.0000 Uani . . . . . .
C5 C 0.4915(2) 0.6004(4) 0.16955(17) 0.0420 1.0000 Uani . . . . . .
C6 C 0.56697(19) 0.6017(3) 0.20186(16) 0.0352 1.0000 Uani . . . . . .
C7 C 0.6112(2) 0.6553(3) 0.17112(17) 0.0382 1.0000 Uani . . . . . .
C8 C 0.71610(19) 0.7407(3) 0.15946(15) 0.0343 1.0000 Uani . . . . . .
C9 C 0.79878(19) 0.7283(3) 0.19553(15) 0.0330 1.0000 Uani . . . . . .
C10 C 0.86876(19) 0.7649(3) 0.30504(15) 0.0339 1.0000 Uani . . . . . .
C11 C 0.89284(19) 0.7432(3) 0.37088(16) 0.0341 1.0000 Uani . . . . . .
C12 C 0.9565(2) 0.8038(4) 0.41229(17) 0.0412 1.0000 Uani . . . . . .
C13 C 0.9857(2) 0.7745(4) 0.47503(17) 0.0421 1.0000 Uani . . . . . .
C14 C 0.9526(2) 0.6783(4) 0.49858(16) 0.0366 1.0000 Uani . . . . . .
C15 C 0.89069(19) 0.6163(4) 0.46003(16) 0.0379 1.0000 Uani . . . . . .
C16 C 0.85798(19) 0.6484(3) 0.39535(15) 0.0341 1.0000 Uani . . . . . .
C17 C 0.69265(19) 0.7012(3) 0.09086(16) 0.0349 1.0000 Uani . . . . . .
C18 C 0.6709(2) 0.5743(4) 0.06886(17) 0.0418 1.0000 Uani . . . . . .
C19 C 0.6521(2) 0.5439(4) 0.00618(19) 0.0517 1.0000 Uani . . . . . .
C20 C 0.6555(2) 0.6379(5) -0.03566(19) 0.0588 1.0000 Uani . . . . . .
C21 C 0.6782(2) 0.7634(5) -0.01467(19) 0.0566 1.0000 Uani . . . . . .
C22 C 0.6970(2) 0.7941(4) 0.04891(17) 0.0431 1.0000 Uani . . . . . .
C23 C 0.83498(18) 0.6151(3) 0.17634(15) 0.0335 1.0000 Uani . . . . . .
C24 C 0.8294(2) 0.4852(4) 0.19359(18) 0.0456 1.0000 Uani . . . . . .
C25 C 0.8653(2) 0.3858(4) 0.1766(2) 0.0550 1.0000 Uani . . . . . .
C26 C 0.9073(2) 0.4129(5) 0.1429(2) 0.0571 1.0000 Uani . . . . . .
C27 C 0.9116(2) 0.5398(5) 0.1244(2) 0.0591 1.0000 Uani . . . . . .
C28 C 0.8757(2) 0.6406(4) 0.14069(17) 0.0455 1.0000 Uani . . . . . .
C29 C 0.4523(2) 0.4369(5) 0.3483(2) 0.0588 1.0000 Uani . . . . . .
C30 C 0.3861(2) 0.4128(6) 0.3629(2) 0.0675 1.0000 Uani . . . . . .
C31 C 0.4067(2) 0.3834(6) 0.4327(2) 0.0741 1.0000 Uani . . . . . .
C32 C 0.3074(3) 0.2398(5) 0.4271(2) 0.0672 1.0000 Uani . . . . . .
C33 C 0.2395(3) 0.2259(6) 0.4410(2) 0.0704 1.0000 Uani . . . . . .
C34 C 0.2562(3) 0.2440(5) 0.5101(2) 0.0675 1.0000 Uani . . . . . .
C35 C 0.2947(3) 0.3729(6) 0.5325(3) 0.0866 1.0000 Uani . . . . . .
C36 C 0.3605(3) 0.3823(6) 0.5158(2) 0.0819 1.0000 Uani . . . . . .
C37 C 0.9559(2) 0.5508(4) 0.58756(16) 0.0421 1.0000 Uani . . . . . .
C38 C 1.0041(2) 0.5362(4) 0.65632(16) 0.0443 1.0000 Uani . . . . . .
C39 C 0.9783(2) 0.4265(4) 0.68763(18) 0.0492 1.0000 Uani . . . . . .
C41 C 0.8088(4) 0.3288(11) 0.7074(4) 0.1519 1.0000 Uani . . . . . .
C42 C 0.8014(4) 0.4455(12) 0.7466(4) 0.1540 1.0000 Uani . . . . . .
C43 C 0.8235(4) 0.5704(9) 0.7221(4) 0.1436 1.0000 Uani . . . . . .
C44 C 0.8998(3) 0.5531(6) 0.7231(3) 0.0824 1.0000 Uani . . . . . .
C40 C 0.8851(3) 0.3201(6) 0.7089(3) 0.0877 1.0000 Uani . . . . . .
H21 H 0.5680 0.4762 0.3318 0.0460 1.0000 Uiso R . . . . .
H41 H 0.3975 0.5576 0.1753 0.0550 1.0000 Uiso R . . . . .
H51 H 0.4728 0.6308 0.1286 0.0498 1.0000 Uiso R . . . . .
H71 H 0.5876 0.6874 0.1292 0.0450 1.0000 Uiso R . . . . .
H81 H 0.7043 0.8335 0.1601 0.0406 1.0000 Uiso R . . . . .
H91 H 0.8212 0.8093 0.1898 0.0398 1.0000 Uiso R . . . . .
H101 H 0.8989 0.8129 0.2901 0.0407 1.0000 Uiso R . . . . .
H121 H 0.9792 0.8669 0.3960 0.0486 1.0000 Uiso R . . . . .
H131 H 1.0272 0.8174 0.5018 0.0504 1.0000 Uiso R . . . . .
H151 H 0.8688 0.5531 0.4762 0.0457 1.0000 Uiso R . . . . .
H181 H 0.6682 0.5109 0.0966 0.0500 1.0000 Uiso R . . . . .
H191 H 0.6369 0.4602 -0.0088 0.0623 1.0000 Uiso R . . . . .
H201 H 0.6422 0.6151 -0.0784 0.0709 1.0000 Uiso R . . . . .
H211 H 0.6799 0.8300 -0.0427 0.0686 1.0000 Uiso R . . . . .
H221 H 0.7126 0.8789 0.0635 0.0519 1.0000 Uiso R . . . . .
H241 H 0.8020 0.4653 0.2170 0.0546 1.0000 Uiso R . . . . .
H251 H 0.8602 0.2982 0.1875 0.0658 1.0000 Uiso R . . . . .
H261 H 0.9319 0.3457 0.1322 0.0690 1.0000 Uiso R . . . . .
H271 H 0.9374 0.5585 0.1013 0.0708 1.0000 Uiso R . . . . .
H281 H 0.8777 0.7278 0.1277 0.0543 1.0000 Uiso R . . . . .
H291 H 0.4798 0.5084 0.3760 0.0708 1.0000 Uiso R . . . . .
H292 H 0.4806 0.3580 0.3560 0.0707 1.0000 Uiso R . . . . .
H301 H 0.3555 0.4933 0.3514 0.0808 1.0000 Uiso R . . . . .
H302 H 0.3587 0.3398 0.3368 0.0813 1.0000 Uiso R . . . . .
H311 H 0.4365 0.4589 0.4575 0.0895 1.0000 Uiso R . . . . .
H312 H 0.4373 0.3046 0.4444 0.0893 1.0000 Uiso R . . . . .
H321 H 0.3415 0.1698 0.4507 0.0805 1.0000 Uiso R . . . . .
H322 H 0.2944 0.2252 0.3814 0.0812 1.0000 Uiso R . . . . .
H331 H 0.2041 0.2902 0.4172 0.0841 1.0000 Uiso R . . . . .
H332 H 0.2195 0.1376 0.4271 0.0839 1.0000 Uiso R . . . . .
H341 H 0.2860 0.1715 0.5327 0.0807 1.0000 Uiso R . . . . .
H342 H 0.2116 0.2419 0.5177 0.0812 1.0000 Uiso R . . . . .
H351 H 0.3063 0.3853 0.5780 0.1042 1.0000 Uiso R . . . . .
H352 H 0.2617 0.4427 0.5079 0.1039 1.0000 Uiso R . . . . .
H361 H 0.3844 0.4667 0.5286 0.0986 1.0000 Uiso R . . . . .
H362 H 0.3942 0.3097 0.5372 0.0979 1.0000 Uiso R . . . . .
H371 H 0.9540 0.4666 0.5664 0.0508 1.0000 Uiso R . . . . .
H372 H 0.9075 0.5763 0.5836 0.0507 1.0000 Uiso R . . . . .
H381 H 1.0530 0.5150 0.6600 0.0530 1.0000 Uiso R . . . . .
H382 H 1.0047 0.6203 0.6770 0.0529 1.0000 Uiso R . . . . .
H391 H 1.0129 0.4195 0.7318 0.0586 1.0000 Uiso R . . . . .
H392 H 0.9793 0.3436 0.6663 0.0584 1.0000 Uiso R . . . . .
H411 H 0.7978 0.2469 0.7251 0.1820 1.0000 Uiso R . . . . .
H412 H 0.7747 0.3387 0.6643 0.1821 1.0000 Uiso R . . . . .
H421 H 0.8323 0.4322 0.7908 0.1847 1.0000 Uiso R . . . . .
H422 H 0.7505 0.4530 0.7428 0.1851 1.0000 Uiso R . . . . .
H431 H 0.8231 0.6443 0.7491 0.1721 1.0000 Uiso R . . . . .
H432 H 0.7906 0.5885 0.6804 0.1718 1.0000 Uiso R . . . . .
H441 H 0.9328 0.5435 0.7669 0.0986 1.0000 Uiso R . . . . .
H442 H 0.9135 0.6335 0.7065 0.0990 1.0000 Uiso R . . . . .
H401 H 0.9185 0.3051 0.7532 0.1047 1.0000 Uiso R . . . . .
H402 H 0.8896 0.2462 0.6826 0.1054 1.0000 Uiso R . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.17313(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . O1 . 1.849(2) yes
Ni1 . O2 . 1.849(2) yes
Ni1 . N1 . 1.851(3) yes
Ni1 . N2 . 1.836(3) yes
O1 . C1 . 1.313(4) yes
O2 . C16 . 1.309(4) yes
O3 . C3 . 1.356(4) yes
O3 . C29 . 1.428(5) yes
O4 . C14 . 1.368(4) yes
O4 . C37 . 1.439(4) yes
N1 . C7 . 1.300(5) yes
N1 . C8 . 1.492(4) yes
N2 . C9 . 1.486(4) yes
N2 . C10 . 1.298(4) yes
N3 . C31 . 1.483(5) yes
N3 . C32 . 1.479(6) yes
N3 . C36 . 1.457(5) yes
N4 . C39 . 1.446(5) yes
N4 . C44 . 1.457(7) yes
N4 . C40 . 1.475(6) yes
C1 . C2 . 1.405(5) yes
C1 . C6 . 1.419(5) yes
C2 . C3 . 1.375(5) yes
C2 . H21 . 0.904 no
C3 . C4 . 1.405(5) yes
C4 . C5 . 1.348(5) yes
C4 . H41 . 0.925 no
C5 . C6 . 1.410(5) yes
C5 . H51 . 0.923 no
C6 . C7 . 1.434(5) yes
C7 . H71 . 0.954 no
C8 . C9 . 1.551(5) yes
C8 . C17 . 1.516(5) yes
C8 . H81 . 0.976 no
C9 . C23 . 1.514(5) yes
C9 . H91 . 0.972 no
C10 . C11 . 1.418(5) yes
C10 . H101 . 0.938 no
C11 . C12 . 1.410(5) yes
C11 . C16 . 1.426(5) yes
C12 . C13 . 1.365(5) yes
C12 . H121 . 0.943 no
C13 . C14 . 1.401(5) yes
C13 . H131 . 0.933 no
C14 . C15 . 1.374(5) yes
C15 . C16 . 1.414(5) yes
C15 . H151 . 0.932 no
C17 . C18 . 1.394(5) yes
C17 . C22 . 1.376(5) yes
C18 . C19 . 1.376(5) yes
C18 . H181 . 0.923 no
C19 . C20 . 1.375(6) yes
C19 . H191 . 0.926 no
C20 . C21 . 1.380(7) yes
C20 . H201 . 0.941 no
C21 . C22 . 1.397(5) yes
C21 . H211 . 0.945 no
C22 . H221 . 0.935 no
C23 . C24 . 1.397(5) yes
C23 . C28 . 1.384(5) yes
C24 . C25 . 1.382(6) yes
C24 . H241 . 0.926 no
C25 . C26 . 1.371(6) yes
C25 . H251 . 0.942 no
C26 . C27 . 1.372(6) yes
C26 . H261 . 0.930 no
C27 . C28 . 1.383(6) yes
C27 . H271 . 0.892 no
C28 . H281 . 0.943 no
C29 . C30 . 1.509(6) yes
C29 . H291 . 0.986 no
C29 . H292 . 0.960 no
C30 . C31 . 1.523(6) yes
C30 . H301 . 0.997 no
C30 . H302 . 0.981 no
C31 . H311 . 1.006 no
C31 . H312 . 0.983 no
C32 . C33 . 1.519(6) yes
C32 . H321 . 0.993 no
C32 . H322 . 0.990 no
C33 . C34 . 1.503(6) yes
C33 . H331 . 0.967 no
C33 . H332 . 0.986 no
C34 . C35 . 1.509(7) yes
C34 . H341 . 0.966 no
C34 . H342 . 0.976 no
C35 . C36 . 1.512(7) yes
C35 . H351 . 0.987 no
C35 . H352 . 0.989 no
C36 . H361 . 0.973 no
C36 . H362 . 0.996 no
C37 . C38 . 1.511(5) yes
C37 . H371 . 0.979 no
C37 . H372 . 0.975 no
C38 . C39 . 1.521(5) yes
C38 . H381 . 0.977 no
C38 . H382 . 0.977 no
C39 . H391 . 0.989 no
C39 . H392 . 0.980 no
C41 . C42 . 1.533(13) yes
C41 . C40 . 1.519(10) yes
C41 . H411 . 0.988 no
C41 . H412 . 0.970 no
C42 . C43 . 1.523(11) yes
C42 . H421 . 0.976 no
C42 . H422 . 0.993 no
C43 . C44 . 1.532(8) yes
C43 . H431 . 0.976 no
C43 . H432 . 0.951 no
C44 . H441 . 0.976 no
C44 . H442 . 0.984 no
C40 . H401 . 0.994 no
C40 . H402 . 0.989 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Ni1 . O2 . 85.28(10) yes
O1 . Ni1 . N1 . 95.25(11) yes
O2 . Ni1 . N1 . 179.11(12) yes
O1 . Ni1 . N2 . 176.43(12) yes
O2 . Ni1 . N2 . 93.78(11) yes
N1 . Ni1 . N2 . 85.73(12) yes
Ni1 . O1 . C1 . 127.1(2) yes
Ni1 . O2 . C16 . 126.4(2) yes
C3 . O3 . C29 . 118.4(3) yes
C14 . O4 . C37 . 117.5(3) yes
Ni1 . N1 . C7 . 125.9(2) yes
Ni1 . N1 . C8 . 116.1(2) yes
C7 . N1 . C8 . 117.1(3) yes
Ni1 . N2 . C9 . 115.2(2) yes
Ni1 . N2 . C10 . 126.2(2) yes
C9 . N2 . C10 . 118.6(3) yes
C31 . N3 . C32 . 110.5(4) yes
C31 . N3 . C36 . 110.7(4) yes
C32 . N3 . C36 . 109.2(4) yes
C39 . N4 . C44 . 111.9(4) yes
C39 . N4 . C40 . 108.2(4) yes
C44 . N4 . C40 . 109.6(4) yes
O1 . C1 . C2 . 118.5(3) yes
O1 . C1 . C6 . 123.4(3) yes
C2 . C1 . C6 . 118.1(3) yes
C1 . C2 . C3 . 120.9(3) yes
C1 . C2 . H21 . 119.1 no
C3 . C2 . H21 . 119.9 no
C2 . C3 . O3 . 124.4(3) yes
C2 . C3 . C4 . 120.6(4) yes
O3 . C3 . C4 . 114.9(3) yes
C3 . C4 . C5 . 119.4(4) yes
C3 . C4 . H41 . 119.8 no
C5 . C4 . H41 . 120.8 no
C4 . C5 . C6 . 121.8(3) yes
C4 . C5 . H51 . 120.2 no
C6 . C5 . H51 . 118.0 no
C1 . C6 . C5 . 119.1(3) yes
C1 . C6 . C7 . 121.8(3) yes
C5 . C6 . C7 . 119.1(3) yes
C6 . C7 . N1 . 125.3(3) yes
C6 . C7 . H71 . 117.8 no
N1 . C7 . H71 . 116.9 no
N1 . C8 . C9 . 107.3(3) yes
N1 . C8 . C17 . 115.6(3) yes
C9 . C8 . C17 . 112.2(3) yes
N1 . C8 . H81 . 107.7 no
C9 . C8 . H81 . 106.7 no
C17 . C8 . H81 . 106.9 no
C8 . C9 . N2 . 105.8(3) yes
C8 . C9 . C23 . 116.1(3) yes
N2 . C9 . C23 . 110.1(3) yes
C8 . C9 . H91 . 108.4 no
N2 . C9 . H91 . 108.4 no
C23 . C9 . H91 . 107.9 no
N2 . C10 . C11 . 125.1(3) yes
N2 . C10 . H101 . 117.0 no
C11 . C10 . H101 . 117.8 no
C10 . C11 . C12 . 120.2(3) yes
C10 . C11 . C16 . 120.4(3) yes
C12 . C11 . C16 . 119.0(3) yes
C11 . C12 . C13 . 122.0(3) yes
C11 . C12 . H121 . 118.7 no
C13 . C12 . H121 . 119.3 no
C12 . C13 . C14 . 119.0(3) yes
C12 . C13 . H131 . 120.6 no
C14 . C13 . H131 . 120.4 no
C13 . C14 . O4 . 115.3(3) yes
C13 . C14 . C15 . 121.2(3) yes
O4 . C14 . C15 . 123.5(3) yes
C14 . C15 . C16 . 120.9(3) yes
C14 . C15 . H151 . 120.6 no
C16 . C15 . H151 . 118.5 no
C11 . C16 . C15 . 118.0(3) yes
C11 . C16 . O2 . 123.7(3) yes
C15 . C16 . O2 . 118.3(3) yes
C8 . C17 . C18 . 123.5(3) yes
C8 . C17 . C22 . 117.9(3) yes
C18 . C17 . C22 . 118.5(3) yes
C17 . C18 . C19 . 120.7(4) yes
C17 . C18 . H181 . 119.3 no
C19 . C18 . H181 . 120.0 no
C18 . C19 . C20 . 120.5(4) yes
C18 . C19 . H191 . 121.0 no
C20 . C19 . H191 . 118.5 no
C19 . C20 . C21 . 119.8(4) yes
C19 . C20 . H201 . 119.1 no
C21 . C20 . H201 . 121.1 no
C20 . C21 . C22 . 119.6(4) yes
C20 . C21 . H211 . 121.2 no
C22 . C21 . H211 . 119.1 no
C21 . C22 . C17 . 120.9(4) yes
C21 . C22 . H221 . 120.0 no
C17 . C22 . H221 . 119.1 no
C9 . C23 . C24 . 122.6(3) yes
C9 . C23 . C28 . 119.1(3) yes
C24 . C23 . C28 . 118.3(4) yes
C23 . C24 . C25 . 120.5(4) yes
C23 . C24 . H241 . 120.0 no
C25 . C24 . H241 . 119.5 no
C24 . C25 . C26 . 120.7(4) yes
C24 . C25 . H251 . 119.9 no
C26 . C25 . H251 . 119.5 no
C25 . C26 . C27 . 119.2(4) yes
C25 . C26 . H261 . 120.2 no
C27 . C26 . H261 . 120.6 no
C26 . C27 . C28 . 121.0(4) yes
C26 . C27 . H271 . 120.2 no
C28 . C27 . H271 . 118.8 no
C23 . C28 . C27 . 120.4(4) yes
C23 . C28 . H281 . 118.0 no
C27 . C28 . H281 . 121.6 no
O3 . C29 . C30 . 106.4(3) yes
O3 . C29 . H291 . 111.0 no
C30 . C29 . H291 . 107.5 no
O3 . C29 . H292 . 111.7 no
C30 . C29 . H292 . 109.4 no
H291 . C29 . H292 . 110.7 no
C29 . C30 . C31 . 110.9(4) yes
C29 . C30 . H301 . 108.3 no
C31 . C30 . H301 . 109.4 no
C29 . C30 . H302 . 108.8 no
C31 . C30 . H302 . 111.0 no
H301 . C30 . H302 . 108.4 no
C30 . C31 . N3 . 111.1(4) yes
C30 . C31 . H311 . 108.1 no
N3 . C31 . H311 . 108.9 no
C30 . C31 . H312 . 109.8 no
N3 . C31 . H312 . 111.6 no
H311 . C31 . H312 . 107.1 no
N3 . C32 . C33 . 111.0(4) yes
N3 . C32 . H321 . 108.9 no
C33 . C32 . H321 . 107.7 no
N3 . C32 . H322 . 112.4 no
C33 . C32 . H322 . 108.1 no
H321 . C32 . H322 . 108.5 no
C32 . C33 . C34 . 110.6(4) yes
C32 . C33 . H331 . 110.0 no
C34 . C33 . H331 . 109.5 no
C32 . C33 . H332 . 107.7 no
C34 . C33 . H332 . 110.6 no
H331 . C33 . H332 . 108.3 no
C33 . C34 . C35 . 110.2(4) yes
C33 . C34 . H341 . 108.4 no
C35 . C34 . H341 . 110.5 no
C33 . C34 . H342 . 109.6 no
C35 . C34 . H342 . 110.1 no
H341 . C34 . H342 . 108.0 no
C34 . C35 . C36 . 110.5(5) yes
C34 . C35 . H351 . 110.9 no
C36 . C35 . H351 . 112.6 no
C34 . C35 . H352 . 106.6 no
C36 . C35 . H352 . 105.5 no
H351 . C35 . H352 . 110.5 no
C35 . C36 . N3 . 111.7(4) yes
C35 . C36 . H361 . 110.9 no
N3 . C36 . H361 . 107.4 no
C35 . C36 . H362 . 108.8 no
N3 . C36 . H362 . 108.0 no
H361 . C36 . H362 . 110.0 no
O4 . C37 . C38 . 107.5(3) yes
O4 . C37 . H371 . 111.5 no
C38 . C37 . H371 . 108.7 no
O4 . C37 . H372 . 109.5 no
C38 . C37 . H372 . 109.9 no
H371 . C37 . H372 . 109.8 no
C37 . C38 . C39 . 111.6(3) yes
C37 . C38 . H381 . 109.5 no
C39 . C38 . H381 . 107.9 no
C37 . C38 . H382 . 107.9 no
C39 . C38 . H382 . 110.9 no
H381 . C38 . H382 . 109.0 no
C38 . C39 . N4 . 114.9(3) yes
C38 . C39 . H391 . 107.8 no
N4 . C39 . H391 . 110.3 no
C38 . C39 . H392 . 108.8 no
N4 . C39 . H392 . 106.8 no
H391 . C39 . H392 . 108.1 no
C42 . C41 . C40 . 110.8(7) yes
C42 . C41 . H411 . 108.9 no
C40 . C41 . H411 . 108.9 no
C42 . C41 . H412 . 109.2 no
C40 . C41 . H412 . 110.0 no
H411 . C41 . H412 . 109.0 no
C41 . C42 . C43 . 108.8(6) yes
C41 . C42 . H421 . 109.8 no
C43 . C42 . H421 . 109.9 no
C41 . C42 . H422 . 109.5 no
C43 . C42 . H422 . 109.7 no
H421 . C42 . H422 . 109.1 no
C42 . C43 . C44 . 109.2(6) yes
C42 . C43 . H431 . 109.5 no
C44 . C43 . H431 . 109.1 no
C42 . C43 . H432 . 110.3 no
C44 . C43 . H432 . 110.0 no
H431 . C43 . H432 . 108.7 no
C43 . C44 . N4 . 112.8(6) yes
C43 . C44 . H441 . 108.0 no
N4 . C44 . H441 . 111.1 no
C43 . C44 . H442 . 108.9 no
N4 . C44 . H442 . 108.4 no
H441 . C44 . H442 . 107.6 no
C41 . C40 . N4 . 111.3(6) yes
C41 . C40 . H401 . 108.1 no
N4 . C40 . H401 . 109.4 no
C41 . C40 . H402 . 110.8 no
N4 . C40 . H402 . 108.2 no
H401 . C40 . H402 . 108.9 no

#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O1 C9 3.334(4) . 3_645 no
O1 C25 3.570(5) . 3_655 no
O2 C8 3.574(4) . 3_645 no
O3 C40 3.402(7) . 4_454 no
O4 C7 3.411(4) . 4_565 no
O4 C5 3.506(5) . 4_565 no
C1 C10 3.532(5) . 3_645 no
C10 C39 3.583(6) . 2_766 no
C15 C34 3.565(7) . 2_666 no
C19 C34 3.579(7) . 4_554 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ni1 O1 C1 C2 . . . . -167.8(3) no
Ni1 O1 C1 C6 . . . . 11.4(5) no
Ni1 O2 C16 C11 . . . . -9.0(5) no
Ni1 O2 C16 C15 . . . . 171.4(3) no
Ni1 N1 C7 C6 . . . . -4.1(5) no
Ni1 N1 C8 C9 . . . . 16.6(3) no
Ni1 N1 C8 C17 . . . . 142.6(2) no
Ni1 N2 C9 C8 . . . . 33.6(3) no
Ni1 N2 C9 C23 . . . . -92.6(3) no
Ni1 N2 C10 C11 . . . . 9.0(5) no
O1 Ni1 O2 C16 . . . . -156.6(3) no
O1 Ni1 N1 C7 . . . . 9.2(3) no
O1 Ni1 N1 C8 . . . . 177.9(2) no
O1 C1 C2 C3 . . . . 179.5(3) no
O1 C1 C6 C5 . . . . 179.3(3) no
O1 C1 C6 C7 . . . . -2.5(5) no
O2 Ni1 O1 C1 . . . . 167.7(3) no
O2 Ni1 N2 C9 . . . . 158.4(2) no
O2 Ni1 N2 C10 . . . . -19.9(3) no
O2 C16 C11 C10 . . . . -9.0(6) no
O2 C16 C11 C12 . . . . 178.2(4) no
O2 C16 C15 C14 . . . . -177.9(4) no
O3 C3 C2 C1 . . . . -177.3(4) no
O3 C3 C4 C5 . . . . 177.2(4) no
O3 C29 C30 C31 . . . . -174.8(4) no
O4 C14 C13 C12 . . . . 178.4(4) no
O4 C14 C15 C16 . . . . 179.3(4) no
O4 C37 C38 C39 . . . . -177.6(3) no
N1 Ni1 O1 C1 . . . . -13.0(3) no
N1 Ni1 N2 C9 . . . . -20.9(2) no
N1 Ni1 N2 C10 . . . . 160.8(3) no
N1 C7 C6 C1 . . . . -1.3(5) no
N1 C7 C6 C5 . . . . 176.9(4) no
N1 C8 C9 N2 . . . . -29.8(3) no
N1 C8 C9 C23 . . . . 92.6(4) no
N1 C8 C17 C18 . . . . -31.0(5) no
N1 C8 C17 C22 . . . . 152.7(3) no
N2 Ni1 O2 C16 . . . . 20.0(3) no
N2 Ni1 N1 C7 . . . . -167.4(3) no
N2 Ni1 N1 C8 . . . . 1.3(3) no
N2 C9 C8 C17 . . . . -157.8(3) no
N2 C9 C23 C24 . . . . 45.0(4) no
N2 C9 C23 C28 . . . . -134.6(3) no
N2 C10 C11 C12 . . . . -178.2(4) no
N2 C10 C11 C16 . . . . 9.1(6) no
N3 C31 C30 C29 . . . . 175.9(4) no
N3 C32 C33 C34 . . . . -57.5(5) no
N3 C36 C35 C34 . . . . 57.9(6) no
N4 C39 C38 C37 . . . . -58.6(5) no
N4 C40 C41 C42 . . . . -58.0(8) no
N4 C44 C43 C42 . . . . 58.6(8) no
C1 C2 C3 C4 . . . . 1.3(6) no
C1 C6 C5 C4 . . . . 1.2(6) no
C2 C1 C6 C5 . . . . -1.4(5) no
C2 C1 C6 C7 . . . . 176.8(3) no
C2 C3 O3 C29 . . . . 3.0(6) no
C2 C3 C4 C5 . . . . -1.5(6) no
C3 O3 C29 C30 . . . . 175.5(4) no
C3 C2 C1 C6 . . . . 0.2(5) no
C3 C4 C5 C6 . . . . 0.2(6) no
C4 C3 O3 C29 . . . . -175.6(4) no
C4 C5 C6 C7 . . . . -177.0(4) no
C6 C7 N1 C8 . . . . -172.7(3) no
C7 N1 C8 C9 . . . . -173.7(3) no
C7 N1 C8 C17 . . . . -47.6(4) no
C8 C9 N2 C10 . . . . -148.0(3) no
C8 C9 C23 C24 . . . . -75.2(4) no
C8 C9 C23 C28 . . . . 105.3(4) no
C8 C17 C18 C19 . . . . -178.2(4) no
C8 C17 C22 C21 . . . . 178.2(4) no
C9 N2 C10 C11 . . . . -169.2(3) no
C9 C8 C17 C18 . . . . 92.4(4) no
C9 C8 C17 C22 . . . . -83.9(4) no
C9 C23 C24 C25 . . . . -177.9(3) no
C9 C23 C28 C27 . . . . 177.6(3) no
C10 N2 C9 C23 . . . . 85.8(4) no
C10 C11 C12 C13 . . . . -172.8(4) no
C10 C11 C16 C15 . . . . 170.5(4) no
C11 C12 C13 C14 . . . . 2.0(6) no
C11 C16 C15 C14 . . . . 2.5(6) no
C12 C11 C16 C15 . . . . -2.2(5) no
C12 C13 C14 C15 . . . . -1.8(7) no
C13 C12 C11 C16 . . . . -0.0(6) no
C13 C14 O4 C37 . . . . -177.7(4) no
C13 C14 C15 C16 . . . . -0.5(6) no
C14 O4 C37 C38 . . . . 177.3(3) no
C15 C14 O4 C37 . . . . 2.4(6) no
C17 C8 C9 C23 . . . . -35.4(4) no
C17 C18 C19 C20 . . . . 1.0(6) no
C17 C22 C21 C20 . . . . -0.5(6) no
C18 C17 C22 C21 . . . . 1.7(6) no
C18 C19 C20 C21 . . . . 0.3(6) no
C19 C18 C17 C22 . . . . -2.0(6) no
C19 C20 C21 C22 . . . . -0.5(6) no
C23 C24 C25 C26 . . . . 0.4(5) no
C23 C28 C27 C26 . . . . 0.3(5) no
C24 C23 C28 C27 . . . . -1.9(5) no
C24 C25 C26 C27 . . . . -2.0(5) no
C25 C24 C23 C28 . . . . 1.6(5) no
C25 C26 C27 C28 . . . . 1.7(5) no
C30 C31 N3 C32 . . . . 76.7(5) no
C30 C31 N3 C36 . . . . -162.2(5) no
C31 N3 C32 C33 . . . . -178.3(3) no
C31 N3 C36 C35 . . . . 178.0(5) no
C32 N3 C36 C35 . . . . -60.1(6) no
C32 C33 C34 C35 . . . . 54.1(6) no
C33 C32 N3 C36 . . . . 59.8(5) no
C33 C34 C35 C36 . . . . -54.0(6) no
C38 C39 N4 C40 . . . . 171.8(4) no
C38 C39 N4 C44 . . . . -67.3(5) no
C39 N4 C40 C41 . . . . -179.6(5) no
C39 N4 C44 C43 . . . . -179.2(5) no
C40 N4 C44 C43 . . . . -59.1(6) no
C40 C41 C42 C43 . . . . 56.4(8) no
C41 C40 N4 C44 . . . . 58.1(6) no
C41 C42 C43 C44 . . . . -55.5(7) no
#------------------------------------------------------------------------------




_iucr_refine_instruction_details_constraints 
;
#
# Punched on 13/09/12 at 16:27:23
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 13/09/12 at 16:27:23
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# 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_ral1102_relabel2
_database_code_depnum_ccdc_archive 'CCDC 1017433'
_audit_update_record             
;
2014-08-01 deposited with the CCDC.
2014-12-18 downloaded from the CCDC.
;
_audit_creation_date             14-01-23
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title '7111529 ral1102'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H22 N2 Ni O4, 2(H2 O)'

# Given Formula = C28 H26 N2 Ni1 O6 
# Dc =      1.46 Fooo =   1136.00 Mu =      8.29 M =    545.23
# Found Formula = C28 H26 N2 Ni1 O6 
# Dc =      1.46 FOOO =   1136.00 Mu =      8.29 M =    545.23

_chemical_formula_sum            'C28 H26 N2 Ni O6'
_chemical_compound_source        'from U of Wollongong'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            brown

_diffrn_ambient_temperature      200

_cell_length_a                   8.3098(1)
_cell_length_b                   28.7045(6)
_cell_length_c                   10.4088(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.0868(12)
_cell_angle_gamma                90
_cell_volume                     2482.35(8)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_int_tables_number      14

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .
_symmetry_space_group_name_Hall  '-P 2ybc '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4
_chemical_formula_weight         545.23


_cell_measurement_reflns_used    117964
_cell_measurement_theta_min      3
_cell_measurement_theta_max      25
_cell_measurement_temperature    200
_exptl_crystal_size_min          0.060
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_max          0.410

_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.829

# Sheldrick geometric approximatio 0.81 0.95 
# Absorption correction 

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.170
-1 0 0 0.240
0 1 0 0.150
0 -1 0 0.100
0 0 1 0.010
1 2 0 0.140
-1 -2 0 0.157
-1 -5 -3 0.043
1 5 3 0.029
0 -1 -1 0.056


_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_process_details   
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents   0.047

# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'
_diffrn_special_details          
;
CCD data collecting conditions-
phi and omega scans of width 0.5 deg at rate 42 sec/frame,
crystal-detector distance 45mm,
multiple scan sets so over 90 percent of data collected with 4-fold  
redundancy or more.
;

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35296
_reflns_number_total             4362
_diffrn_reflns_av_R_equivalents  0.067
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 4362 
# Theoretical number of reflections is about 8737 


_diffrn_reflns_theta_min         2.552
_diffrn_reflns_theta_max         24.992
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        24.992
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -9
_reflns_limit_h_max              9
_reflns_limit_k_min              0
_reflns_limit_k_max              34
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   2.36
_oxford_diffrn_Wilson_scale      8.20

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.38
_refine_diff_density_max         0.49


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         4362
_refine_ls_number_restraints     0
_refine_ls_number_parameters     352
_oxford_refine_ls_R_factor_ref   0.0480
_refine_ls_wR_factor_ref         0.0933
_refine_ls_goodness_of_fit_ref   1.0147
_refine_ls_shift/su_max          0.0023567
_refine_ls_shift/su_mean         0.0004775


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4362
_refine_ls_R_factor_all          0.0480
_refine_ls_wR_factor_all         0.0933

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3613
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_gt          0.0880


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 2.49P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
The largest features in the
final difference electron density map are located 
near the Ni atom.
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.24634(4) 0.583000(11) 0.37191(3) 0.0312 1.0000 Uani . . . . . .
O1 O 0.1081(2) 0.57507(6) 0.23342(17) 0.0384 1.0000 Uani . . . . . .
O2 O 0.37891(19) 0.54334(6) 0.28013(16) 0.0352 1.0000 Uani . . . . . .
O3 O -0.3519(2) 0.59485(8) -0.0361(2) 0.0504 1.0000 Uani . . . . . .
O4 O 0.8555(2) 0.46233(7) 0.1701(2) 0.0427 1.0000 Uani . . . . . .
O51 O -0.2045(3) 0.53582(8) -0.1946(2) 0.0522 1.0000 Uani . . . . . .
O52 O 0.6903(3) 0.42140(10) -0.0089(2) 0.0645 1.0000 Uani . . . . . .
N1 N 0.1072(2) 0.62009(7) 0.4656(2) 0.0325 1.0000 Uani . . . . . .
N2 N 0.3940(2) 0.59303(7) 0.5027(2) 0.0336 1.0000 Uani . . . . . .
C1 C -0.0326(3) 0.59544(9) 0.2131(3) 0.0328 1.0000 Uani . . . . . .
C2 C -0.1155(3) 0.58605(9) 0.0975(3) 0.0353 1.0000 Uani . . . . . .
C3 C -0.2657(3) 0.60459(9) 0.0730(3) 0.0370 1.0000 Uani . . . . . .
C4 C -0.3378(3) 0.63470(9) 0.1620(3) 0.0399 1.0000 Uani . . . . . .
C5 C -0.2580(3) 0.64429(9) 0.2742(3) 0.0357 1.0000 Uani . . . . . .
C6 C -0.1053(3) 0.62540(8) 0.3040(2) 0.0316 1.0000 Uani . . . . . .
C7 C -0.0336(3) 0.63447(9) 0.4267(3) 0.0338 1.0000 Uani . . . . . .
C8 C 0.1656(3) 0.62846(9) 0.6002(2) 0.0357 1.0000 Uani . . . . . .
C9 C 0.3499(3) 0.63103(9) 0.5923(3) 0.0366 1.0000 Uani . . . . . .
C10 C 0.5340(3) 0.57367(9) 0.5177(2) 0.0339 1.0000 Uani . . . . . .
C11 C 0.6042(3) 0.54220(8) 0.4298(2) 0.0305 1.0000 Uani . . . . . .
C12 C 0.7607(3) 0.52632(9) 0.4555(3) 0.0355 1.0000 Uani . . . . . .
C13 C 0.8426(3) 0.49957(9) 0.3702(3) 0.0370 1.0000 Uani . . . . . .
C14 C 0.7670(3) 0.48755(9) 0.2535(3) 0.0335 1.0000 Uani . . . . . .
C15 C 0.6108(3) 0.50155(9) 0.2259(2) 0.0327 1.0000 Uani . . . . . .
C16 C 0.5266(3) 0.52964(8) 0.3123(2) 0.0312 1.0000 Uani . . . . . .
C17 C 0.0884(3) 0.66764(9) 0.6753(3) 0.0371 1.0000 Uani . . . . . .
C18 C 0.0837(3) 0.71380(10) 0.6356(3) 0.0433 1.0000 Uani . . . . . .
C19 C 0.0159(4) 0.74779(10) 0.7114(3) 0.0495 1.0000 Uani . . . . . .
C20 C -0.0494(4) 0.73621(11) 0.8276(3) 0.0532 1.0000 Uani . . . . . .
C21 C -0.0455(5) 0.69101(12) 0.8685(3) 0.0639 1.0000 Uani . . . . . .
C22 C 0.0223(4) 0.65661(11) 0.7929(3) 0.0532 1.0000 Uani . . . . . .
C23 C 0.4204(3) 0.67636(10) 0.5441(3) 0.0398 1.0000 Uani . . . . . .
C24 C 0.3722(3) 0.69666(10) 0.4283(3) 0.0453 1.0000 Uani . . . . . .
C25 C 0.4334(4) 0.73880(11) 0.3887(3) 0.0541 1.0000 Uani . . . . . .
C26 C 0.5488(4) 0.76120(13) 0.4632(4) 0.0658 1.0000 Uani . . . . . .
C27 C 0.6037(4) 0.74113(13) 0.5742(4) 0.0674 1.0000 Uani . . . . . .
C28 C 0.5405(4) 0.69860(11) 0.6159(3) 0.0522 1.0000 Uani . . . . . .
H21 H -0.0701 0.5664 0.0372 0.0418 1.0000 Uiso R . . . . .
H31 H -0.303(5) 0.5776(13) -0.080(4) 0.0762 1.0000 Uiso . . . . . .
H41 H 0.800(4) 0.4552(12) 0.103(3) 0.0630 1.0000 Uiso . . . . . .
H42 H -0.4384 0.6462 0.1460 0.0473 1.0000 Uiso R . . . . .
H51 H -0.3040 0.6635 0.3333 0.0426 1.0000 Uiso R . . . . .
H71 H -0.0953 0.6523 0.4855 0.0412 1.0000 Uiso R . . . . .
H81 H 0.1409 0.6002 0.6465 0.0427 1.0000 Uiso R . . . . .
H91 H 0.3972 0.6239 0.6726 0.0435 1.0000 Uiso R . . . . .
H101 H 0.5935 0.5809 0.5940 0.0403 1.0000 Uiso R . . . . .
H121 H 0.8093 0.5342 0.5322 0.0424 1.0000 Uiso R . . . . .
H131 H 0.9469 0.4910 0.3867 0.0437 1.0000 Uiso R . . . . .
H151 H 0.5628 0.4927 0.1489 0.0383 1.0000 Uiso R . . . . .
H181 H 0.1260 0.7222 0.5584 0.0515 1.0000 Uiso R . . . . .
H191 H 0.0150 0.7789 0.6823 0.0603 1.0000 Uiso R . . . . .
H201 H -0.0980 0.7581 0.8762 0.0639 1.0000 Uiso R . . . . .
H211 H -0.0899 0.6831 0.9465 0.0774 1.0000 Uiso R . . . . .
H221 H 0.0219 0.6253 0.8195 0.0648 1.0000 Uiso R . . . . .
H241 H 0.2958 0.6815 0.3752 0.0543 1.0000 Uiso R . . . . .
H251 H 0.3953 0.7516 0.3082 0.0652 1.0000 Uiso R . . . . .
H261 H 0.5921 0.7908 0.4377 0.0793 1.0000 Uiso R . . . . .
H271 H 0.6864 0.7559 0.6250 0.0808 1.0000 Uiso R . . . . .
H281 H 0.5793 0.6833 0.6921 0.0624 1.0000 Uiso R . . . . .
H511 H -0.120(5) 0.5313(14) -0.182(4) 0.0773 1.0000 Uiso . . . . . .
H512 H -0.245(5) 0.5085(14) -0.212(4) 0.0775 1.0000 Uiso . . . . . .
H521 H 0.594(5) 0.4166(15) -0.017(4) 0.0969 1.0000 Uiso . . . . . .
H522 H 0.712(5) 0.4267(16) -0.083(5) 0.0980 1.0000 Uiso . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3833(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . O1 . 1.8403(17) yes
Ni1 . O2 . 1.8607(17) yes
Ni1 . N1 . 1.862(2) yes
Ni1 . N2 . 1.838(2) yes
O1 . C1 . 1.321(3) yes
O2 . C16 . 1.325(3) yes
O3 . C3 . 1.359(3) yes
O3 . H31 . 0.79(4) no
O4 . C14 . 1.358(3) yes
O4 . H41 . 0.85(3) no
O51 . H511 . 0.72(4) no
O51 . H512 . 0.87(4) no
O52 . H521 . 0.82(4) no
O52 . H522 . 0.81(5) no
N1 . C7 . 1.298(3) yes
N1 . C8 . 1.494(3) yes
N2 . C9 . 1.485(3) yes
N2 . C10 . 1.296(3) yes
C1 . C2 . 1.402(4) yes
C1 . C6 . 1.422(4) yes
C2 . C3 . 1.377(4) yes
C2 . H21 . 0.929 no
C3 . C4 . 1.409(4) yes
C4 . C5 . 1.360(4) yes
C4 . H42 . 0.911 no
C5 . C6 . 1.409(3) yes
C5 . H51 . 0.914 no
C6 . C7 . 1.423(4) yes
C7 . H71 . 0.955 no
C8 . C9 . 1.537(4) yes
C8 . C17 . 1.518(4) yes
C8 . H81 . 0.967 no
C9 . C23 . 1.516(4) yes
C9 . H91 . 0.940 no
C10 . C11 . 1.419(4) yes
C10 . H101 . 0.951 no
C11 . C12 . 1.399(3) yes
C11 . C16 . 1.418(3) yes
C12 . C13 . 1.365(4) yes
C12 . H121 . 0.917 no
C13 . C14 . 1.400(4) yes
C13 . H131 . 0.915 no
C14 . C15 . 1.383(3) yes
C15 . C16 . 1.405(4) yes
C15 . H151 . 0.924 no
C17 . C18 . 1.388(4) yes
C17 . C22 . 1.389(4) yes
C18 . C19 . 1.381(4) yes
C18 . H181 . 0.915 no
C19 . C20 . 1.375(4) yes
C19 . H191 . 0.943 no
C20 . C21 . 1.366(5) yes
C20 . H201 . 0.907 no
C21 . C22 . 1.388(4) yes
C21 . H211 . 0.927 no
C22 . H221 . 0.941 no
C23 . C24 . 1.391(4) yes
C23 . C28 . 1.391(4) yes
C24 . C25 . 1.379(4) yes
C24 . H241 . 0.941 no
C25 . C26 . 1.381(5) yes
C25 . H251 . 0.964 no
C26 . C27 . 1.362(5) yes
C26 . H261 . 0.963 no
C27 . C28 . 1.401(5) yes
C27 . H271 . 0.957 no
C28 . H281 . 0.958 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Ni1 . O2 . 83.63(7) yes
O1 . Ni1 . N1 . 95.53(8) yes
O2 . Ni1 . N1 . 177.09(9) yes
O1 . Ni1 . N2 . 176.00(9) yes
O2 . Ni1 . N2 . 94.74(8) yes
N1 . Ni1 . N2 . 86.28(9) yes
Ni1 . O1 . C1 . 127.47(17) yes
Ni1 . O2 . C16 . 127.29(16) yes
C3 . O3 . H31 . 110(3) no
C14 . O4 . H41 . 111(2) no
H511 . O51 . H512 . 104(4) no
H521 . O52 . H522 . 100(4) no
Ni1 . N1 . C7 . 125.70(18) yes
Ni1 . N1 . C8 . 112.92(15) yes
C7 . N1 . C8 . 121.1(2) yes
Ni1 . N2 . C9 . 114.26(16) yes
Ni1 . N2 . C10 . 127.39(18) yes
C9 . N2 . C10 . 118.1(2) yes
O1 . C1 . C2 . 118.1(2) yes
O1 . C1 . C6 . 123.2(2) yes
C2 . C1 . C6 . 118.7(2) yes
C1 . C2 . C3 . 120.9(2) yes
C1 . C2 . H21 . 119.8 no
C3 . C2 . H21 . 119.2 no
C2 . C3 . O3 . 122.4(2) yes
C2 . C3 . C4 . 120.7(2) yes
O3 . C3 . C4 . 116.8(2) yes
C3 . C4 . C5 . 118.9(2) yes
C3 . C4 . H42 . 120.2 no
C5 . C4 . H42 . 120.9 no
C4 . C5 . C6 . 122.2(2) yes
C4 . C5 . H51 . 119.8 no
C6 . C5 . H51 . 118.0 no
C1 . C6 . C5 . 118.6(2) yes
C1 . C6 . C7 . 122.2(2) yes
C5 . C6 . C7 . 119.2(2) yes
C6 . C7 . N1 . 125.5(2) yes
C6 . C7 . H71 . 116.9 no
N1 . C7 . H71 . 117.6 no
N1 . C8 . C9 . 105.3(2) yes
N1 . C8 . C17 . 118.0(2) yes
C9 . C8 . C17 . 115.0(2) yes
N1 . C8 . H81 . 105.3 no
C9 . C8 . H81 . 106.7 no
C17 . C8 . H81 . 105.6 no
C8 . C9 . N2 . 104.9(2) yes
C8 . C9 . C23 . 116.8(2) yes
N2 . C9 . C23 . 108.8(2) yes
C8 . C9 . H91 . 110.0 no
N2 . C9 . H91 . 107.2 no
C23 . C9 . H91 . 108.8 no
N2 . C10 . C11 . 125.1(2) yes
N2 . C10 . H101 . 117.3 no
C11 . C10 . H101 . 117.7 no
C10 . C11 . C12 . 118.4(2) yes
C10 . C11 . C16 . 122.1(2) yes
C12 . C11 . C16 . 119.2(2) yes
C11 . C12 . C13 . 122.1(2) yes
C11 . C12 . H121 . 118.6 no
C13 . C12 . H121 . 119.3 no
C12 . C13 . C14 . 118.8(2) yes
C12 . C13 . H131 . 120.8 no
C14 . C13 . H131 . 120.3 no
C13 . C14 . O4 . 116.5(2) yes
C13 . C14 . C15 . 120.8(2) yes
O4 . C14 . C15 . 122.7(2) yes
C14 . C15 . C16 . 120.7(2) yes
C14 . C15 . H151 . 119.2 no
C16 . C15 . H151 . 120.1 no
C11 . C16 . C15 . 118.3(2) yes
C11 . C16 . O2 . 123.1(2) yes
C15 . C16 . O2 . 118.6(2) yes
C8 . C17 . C18 . 124.3(2) yes
C8 . C17 . C22 . 117.6(2) yes
C18 . C17 . C22 . 118.1(3) yes
C17 . C18 . C19 . 120.9(3) yes
C17 . C18 . H181 . 120.2 no
C19 . C18 . H181 . 118.9 no
C18 . C19 . C20 . 120.2(3) yes
C18 . C19 . H191 . 119.1 no
C20 . C19 . H191 . 120.7 no
C19 . C20 . C21 . 119.7(3) yes
C19 . C20 . H201 . 120.7 no
C21 . C20 . H201 . 119.5 no
C20 . C21 . C22 . 120.4(3) yes
C20 . C21 . H211 . 119.9 no
C22 . C21 . H211 . 119.6 no
C17 . C22 . C21 . 120.6(3) yes
C17 . C22 . H221 . 118.7 no
C21 . C22 . H221 . 120.7 no
C9 . C23 . C24 . 122.6(2) yes
C9 . C23 . C28 . 119.6(3) yes
C24 . C23 . C28 . 117.8(3) yes
C23 . C24 . C25 . 121.6(3) yes
C23 . C24 . H241 . 119.7 no
C25 . C24 . H241 . 118.7 no
C24 . C25 . C26 . 119.8(3) yes
C24 . C25 . H251 . 118.6 no
C26 . C25 . H251 . 121.6 no
C25 . C26 . C27 . 119.8(3) yes
C25 . C26 . H261 . 121.0 no
C27 . C26 . H261 . 119.2 no
C26 . C27 . C28 . 120.7(3) yes
C26 . C27 . H271 . 120.4 no
C28 . C27 . H271 . 118.9 no
C27 . C28 . C23 . 120.2(3) yes
C27 . C28 . H281 . 122.4 no
C23 . C28 . H281 . 117.4 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O3 . H31 . O51 . 174(4) 0.79(4) 1.89(4) 2.678(4) yes
O4 . H41 . O52 . 160(3) 0.85(3) 1.76(3) 2.577(4) yes
O51 . H511 . O4 2_665 163(4) 0.72(4) 2.21(4) 2.907(4) yes
O51 . H512 . O2 2_565 164(4) 0.87(4) 1.98(4) 2.830(4) yes
O52 . H521 . O3 2_565 159(4) 0.82(4) 2.12(5) 2.897(4) yes
O52 . H522 . O1 2_665 147(4) 0.81(5) 2.19(5) 2.903(4) yes
O52 . H522 . O2 2_665 147(4) 0.81(5) 2.34(4) 3.043(4) yes

#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O1 O52 2.903(3) . 2_665 no
O1 O51 3.309(3) . 2_565 no
O1 C13 3.422(3) . 1_455 no
O2 O51 2.830(3) . 2_565 no
O2 O52 3.044(3) . 2_665 no
O3 O51 2.678(3) . . no
O3 O52 2.897(3) . 2_565 no
O4 O52 2.577(3) . . no
O4 O51 2.907(3) . 2_665 no
O4 C8 3.543(3) . 2_666 no
O4 C22 3.581(4) . 2_666 no
O51 C2 3.433(4) . . no
O51 C3 3.459(4) . . no
O51 C16 3.474(3) . 2_565 no
O51 C15 3.552(4) . 2_565 no
O52 C14 3.377(4) . . no
O52 C15 3.430(3) . . no
N2 C13 3.575(3) . 2_666 no
C1 C13 3.374(4) . 1_455 no
C1 C14 3.545(4) . 1_455 no
C2 C14 3.412(4) . 1_455 no
C2 C15 3.600(4) . 1_455 no
C3 C15 3.521(4) . 1_455 no
C4 C16 3.589(4) . 1_455 no
C5 C11 3.549(4) . 1_455 no
C6 C12 3.447(4) . 1_455 no
C7 C12 3.559(4) . 1_455 no
C10 C16 3.495(3) . 2_666 no
C10 C11 3.564(4) . 2_666 no
C11 C11 3.332(5) . 2_666 no
C11 C16 3.571(3) . 2_666 no
C25 C28 3.490(4) . 4_564 no
#------------------------------------------------------------------------------
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Ni1 O1 C1 C2 . . . . 177.0(2) no
Ni1 O1 C1 C6 . . . . -4.6(4) no
Ni1 O2 C16 C11 . . . . 3.3(3) no
Ni1 O2 C16 C15 . . . . -176.4(2) no
Ni1 N1 C7 C6 . . . . -1.7(4) no
Ni1 N1 C8 C9 . . . . 34.4(2) no
Ni1 N1 C8 C17 . . . . 164.3(2) no
Ni1 N2 C9 C8 . . . . 34.6(2) no
Ni1 N2 C9 C23 . . . . -90.9(2) no
Ni1 N2 C10 C11 . . . . 3.7(4) no
O1 Ni1 O2 C16 . . . . 177.3(2) no
O1 Ni1 N1 C7 . . . . -3.4(2) no
O1 Ni1 N1 C8 . . . . 170.5(2) no
O1 C1 C2 C3 . . . . 177.2(2) no
O1 C1 C6 C5 . . . . -178.2(2) no
O1 C1 C6 C7 . . . . -2.2(4) no
O2 Ni1 O1 C1 . . . . -176.2(2) no
O2 Ni1 N2 C9 . . . . 169.4(2) no
O2 Ni1 N2 C10 . . . . -4.4(2) no
O2 C16 C11 C10 . . . . -5.2(4) no
O2 C16 C11 C12 . . . . -179.7(2) no
O2 C16 C15 C14 . . . . 178.0(2) no
O3 C3 C2 C1 . . . . -177.6(3) no
O3 C3 C4 C5 . . . . 178.0(2) no
O4 C14 C13 C12 . . . . 177.7(2) no
O4 C14 C15 C16 . . . . -176.7(2) no
N1 Ni1 O1 C1 . . . . 6.6(2) no
N1 Ni1 N2 C9 . . . . -13.3(2) no
N1 Ni1 N2 C10 . . . . 172.9(2) no
N1 C7 C6 C1 . . . . 5.5(4) no
N1 C7 C6 C5 . . . . -178.5(2) no
N1 C8 C9 N2 . . . . -41.8(2) no
N1 C8 C9 C23 . . . . 78.6(3) no
N1 C8 C17 C18 . . . . -57.1(3) no
N1 C8 C17 C22 . . . . 124.8(3) no
N2 Ni1 O2 C16 . . . . 1.0(2) no
N2 Ni1 N1 C7 . . . . 173.0(2) no
N2 Ni1 N1 C8 . . . . -13.1(2) no
N2 C9 C8 C17 . . . . -173.4(2) no
N2 C9 C23 C24 . . . . 64.8(3) no
N2 C9 C23 C28 . . . . -113.8(3) no
N2 C10 C11 C12 . . . . 176.2(2) no
N2 C10 C11 C16 . . . . 1.7(4) no
C1 C2 C3 C4 . . . . 2.0(4) no
C1 C6 C5 C4 . . . . 0.2(4) no
C2 C1 C6 C5 . . . . 0.2(4) no
C2 C1 C6 C7 . . . . 176.2(2) no
C2 C3 C4 C5 . . . . -1.6(4) no
C3 C2 C1 C6 . . . . -1.3(4) no
C3 C4 C5 C6 . . . . 0.5(4) no
C4 C5 C6 C7 . . . . -175.9(3) no
C6 C7 N1 C8 . . . . -175.1(2) no
C7 N1 C8 C9 . . . . -151.3(2) no
C7 N1 C8 C17 . . . . -21.4(3) no
C8 C9 N2 C10 . . . . -150.9(2) no
C8 C9 C23 C24 . . . . -53.5(4) no
C8 C9 C23 C28 . . . . 127.9(3) no
C8 C17 C18 C19 . . . . -177.8(3) no
C8 C17 C22 C21 . . . . 177.9(3) no
C9 N2 C10 C11 . . . . -169.9(2) no
C9 C8 C17 C18 . . . . 68.2(3) no
C9 C8 C17 C22 . . . . -109.9(3) no
C9 C23 C24 C25 . . . . 177.4(3) no
C9 C23 C28 C27 . . . . -178.3(3) no
C10 N2 C9 C23 . . . . 83.5(3) no
C10 C11 C12 C13 . . . . -173.7(2) no
C10 C11 C16 C15 . . . . 174.4(2) no
C11 C12 C13 C14 . . . . -0.2(4) no
C11 C16 C15 C14 . . . . -1.7(4) no
C12 C11 C16 C15 . . . . -0.0(3) no
C12 C13 C14 C15 . . . . -1.5(4) no
C13 C12 C11 C16 . . . . 1.0(4) no
C13 C14 C15 C16 . . . . 2.4(4) no
C17 C8 C9 C23 . . . . -53.1(3) no
C17 C18 C19 C20 . . . . -0.5(5) no
C17 C22 C21 C20 . . . . 0.6(5) no
C18 C17 C22 C21 . . . . -0.4(5) no
C18 C19 C20 C21 . . . . 0.7(5) no
C19 C18 C17 C22 . . . . 0.3(4) no
C19 C20 C21 C22 . . . . -0.7(5) no
C23 C24 C25 C26 . . . . 1.8(5) no
C23 C28 C27 C26 . . . . -0.1(5) no
C24 C23 C28 C27 . . . . 3.0(5) no
C24 C25 C26 C27 . . . . 1.2(5) no
C25 C24 C23 C28 . . . . -3.9(4) no
C25 C26 C27 C28 . . . . -2.1(5) no
#------------------------------------------------------------------------------

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 23/01/14 at 11:47:11
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT H(511,X'S) UNTIL H(522) H(31,X'S) H(41,X'S) 
RIDE C   ( 2,X'S) H   (21,X'S) 
RIDE C   ( 4,X'S) H   (42,X'S) 
RIDE C   ( 5,X'S) H   (51,X'S) 
RIDE C   ( 7,X'S) H   (71,X'S) 
RIDE C   ( 8,X'S) H   (81,X'S) 
RIDE C   ( 9,X'S) H   (91,X'S) 
RIDE C   ( 10,X'S) H   (101,X'S) 
RIDE C   ( 12,X'S) H   (121,X'S) 
RIDE C   ( 13,X'S) H   (131,X'S) 
RIDE C   ( 15,X'S) H   (151,X'S) 
RIDE C   ( 18,X'S) H   (181,X'S) 
RIDE C   ( 19,X'S) H   (191,X'S) 
RIDE C   ( 20,X'S) H   (201,X'S) 
RIDE C   ( 21,X'S) H   (211,X'S) 
RIDE C   ( 22,X'S) H   (221,X'S) 
RIDE C   ( 24,X'S) H   (241,X'S) 
RIDE C   ( 25,X'S) H   (251,X'S) 
RIDE C   ( 26,X'S) H   (261,X'S) 
RIDE C   ( 27,X'S) H   (271,X'S) 
RIDE C   ( 28,X'S) H   (281,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 23/01/14 at 11:47:11
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;



#===END

