# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_ral1710BSNQ
_audit_block_doi                 10.5517/ccdc.csd.cc20996v
_database_code_depnum_ccdc_archive 'CCDC 1855976'
loop_
_audit_author_name
_audit_author_address
'Anthony Willis'
;Australian National University
Australia
;
_audit_update_record             
;
2018-07-16 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_audit_creation_date             17-03-06
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1710BSNQ\Tony_ral1710BSNQ_ At 12: 2 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   15.6742(16)
_cell_length_b                   9.0717(8)
_cell_length_c                   26.436(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.398(9)
_cell_angle_gamma                90
_cell_volume                     3747.9(7)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_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 0.0181 0.0091 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 0.0311 0.0180 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 -3.0029 0.5091 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 0.0492 0.0322 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

# Given Formula = C42 H48 N4 Ni1 O4 
# Dc =      1.30 Fooo =   1552.00 Mu =     11.18 M =    731.58
# Found Formula = C42 H48 N4.00 Ni1 O4.00 
# Dc =      1.30 FOOO =   1552.00 Mu =     11.18 M =    731.58

_chemical_formula_sum            'C42 H48 N4 Ni O4'
_chemical_formula_moiety         'C42 H48 N4 Ni O4'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         731.58


_cell_measurement_reflns_used    3091
_cell_measurement_theta_min      3
_cell_measurement_theta_max      72
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.021
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_max          0.122

_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    1.118

# Sheldrick geometric approximatio 0.92 0.98 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro version 1.171.38.46 (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.98
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
#_diffrn_ambient_temperature 150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_measurement_method       'ω scans'


# If a reference occurs more than once, delete the author 
# and date from subsequent references. 

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2017)'

_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    'PLATON (Spek, 2008)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            24063
_reflns_number_total             7203
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_av_sigmaI/netI    0.1506

# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 7203 
# Theoretical number of reflections is about 14697 


_diffrn_reflns_theta_min         4.219
_diffrn_reflns_theta_max         71.836
_diffrn_measured_fraction_theta_max 0.979

_diffrn_reflns_theta_full        68.629
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       29
_reflns_limit_h_min              -19
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              32

_oxford_diffrn_Wilson_B_factor   3.37
_oxford_diffrn_Wilson_scale      0.11

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

_refine_diff_density_min         -0.59
_refine_diff_density_max         0.70


# 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         7202
_refine_ls_number_restraints     109
_refine_ls_number_parameters     542
_oxford_refine_ls_R_factor_ref   0.1307
_refine_ls_wR_factor_ref         0.2019
_refine_ls_goodness_of_fit_ref   0.9532
_refine_ls_shift/su_max          0.0061437
_refine_ls_shift/su_mean         0.0002418


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        7202
_refine_ls_R_factor_all          0.1307
_refine_ls_wR_factor_all         0.2019

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4277
_refine_ls_R_factor_gt           0.0810
_refine_ls_wR_factor_gt          0.1717

# 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 #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.307E+04 0.473E+04 0.307E+04 0.133E+04 357. 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               
The crystals of [Ni(C₄₂H₄₈N₄O₄)] which were supplied 
were very thin and flaky.  A segment was eventually found
which gave weak diffraction but appeared to be largely single.

The final R-factor is poor but the identity of the compound
is unambiguously established.


There is disorder in the packing of 
one arm of the [Ni(C₄₂H₄₈N₄O₄)] molecule.
Atoms O4, N4 and C36 --- C42 are each disordered over two sites.
The relative occupancies of these sites were refined appropriately.
Restraints were imposed so bond lengths and angles would 
have sensible values, 
and so adjacent sites would have similar displacement parameters
to each other.
 
H atoms were included at calculated positions
 and ride on the C atom sites to which they are respectively bonded.

 
The largest features in the
final difference electron density map are located 
randomly through the structure including near the Ni atom
and near atoms C19 --- C23 possibly indicating a small amount of
disorder of the packing of this group too.
;

# 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 0.42054(5) 0.71361(9) 0.48964(3) 0.0413 1.0000 Uani . . . . . .
O1 O 0.4483(2) 0.8096(4) 0.54970(12) 0.0459 1.0000 Uani . U . . . .
O2 O 0.3129(2) 0.7142(4) 0.51087(13) 0.0505 1.0000 Uani . . . . . .
O3 O 0.6010(3) 1.1031(4) 0.67399(13) 0.0569 1.0000 Uani . . . . . .
O4 O 0.0170(6) 0.7338(15) 0.5071(4) 0.0649 0.509(11) Uani D U P . . .
O94 O 0.0063(6) 0.7701(17) 0.4843(5) 0.0706 0.491(11) Uani D U P . . .
N1 N 0.5294(3) 0.7262(5) 0.46782(14) 0.0404 1.0000 Uani . . . . . .
N2 N 0.3901(3) 0.6061(4) 0.43151(15) 0.0418 1.0000 Uani . . . . . .
N3 N 0.6345(4) 1.1418(6) 0.78190(18) 0.0636 1.0000 Uani . . . . . .
N4 N -0.0436(9) 0.9033(13) 0.6241(4) 0.0736 0.509(11) Uani D U P . . .
N94 N 0.0035(9) 0.8658(13) 0.6198(4) 0.0737 0.491(11) Uani D U P . . .
C1 C 0.5197(3) 0.8764(5) 0.56391(18) 0.0398 1.0000 Uani . U . . . .
C2 C 0.5235(3) 0.9495(6) 0.61140(19) 0.0447 1.0000 Uani . U . . . .
C3 C 0.5945(4) 1.0273(5) 0.62873(19) 0.0457 1.0000 Uani . . . . . .
C4 C 0.6652(4) 1.0369(6) 0.60009(19) 0.0478 1.0000 Uani . . . . . .
C5 C 0.6637(3) 0.9640(5) 0.55449(19) 0.0444 1.0000 Uani . . . . . .
C6 C 0.5920(3) 0.8812(5) 0.53534(18) 0.0390 1.0000 Uani . U . . . .
C7 C 0.5947(3) 0.8030(5) 0.48795(18) 0.0402 1.0000 Uani . . . . . .
C8 C 0.5359(3) 0.6560(6) 0.4179(2) 0.0496 1.0000 Uani . . . . . .
C9 C 0.4657(3) 0.5464(6) 0.4092(2) 0.0502 1.0000 Uani . . . . . .
C10 C 0.3123(3) 0.5781(5) 0.41082(19) 0.0413 1.0000 Uani . . . . . .
C11 C 0.2377(3) 0.6236(5) 0.4340(2) 0.0445 1.0000 Uani . . . . . .
C12 C 0.1541(3) 0.5982(6) 0.4100(2) 0.0553 1.0000 Uani . . . . . .
C13 C 0.0817(4) 0.6386(7) 0.4315(3) 0.0661 1.0000 Uani . . . . . .
C14 C 0.0877(3) 0.7112(8) 0.4782(3) 0.0749 1.0000 Uani D . . . . .
C15 C 0.1657(4) 0.7355(7) 0.5037(2) 0.0616 1.0000 Uani . . . . . .
C16 C 0.2414(3) 0.6912(6) 0.4828(2) 0.0485 1.0000 Uani . . . . . .
C17 C 0.5340(4) 1.0831(8) 0.7069(2) 0.0639 1.0000 Uani . . . . . .
C18 C 0.5537(4) 1.1727(7) 0.7541(2) 0.0651 1.0000 Uani . . . . . .
C19 C 0.6420(5) 1.2368(8) 0.8271(2) 0.0743 1.0000 Uani . . . . . .
C20 C 0.7305(5) 1.2236(8) 0.8541(3) 0.0893 1.0000 Uani . . . . . .
C21 C 0.7473(6) 1.0679(8) 0.8698(3) 0.0910 1.0000 Uani . . . . . .
C22 C 0.7328(6) 0.9661(9) 0.8237(3) 0.1017 1.0000 Uani . . . . . .
C23 C 0.6418(5) 0.9940(8) 0.7975(2) 0.0753 1.0000 Uani . . . . . .
C24 C 0.6785(3) 0.8033(6) 0.4635(2) 0.0445 1.0000 Uani . . . . . .
C25 C 0.7371(3) 0.6924(6) 0.4770(2) 0.0539 1.0000 Uani . . . . . .
C26 C 0.8170(3) 0.6922(7) 0.4573(3) 0.0621 1.0000 Uani . . . . . .
C27 C 0.8361(4) 0.7994(8) 0.4239(3) 0.0709 1.0000 Uani . . . . . .
C28 C 0.7784(4) 0.9080(8) 0.4099(3) 0.0715 1.0000 Uani . . . . . .
C29 C 0.6986(4) 0.9118(6) 0.4306(2) 0.0547 1.0000 Uani . . . . . .
C30 C 0.3015(3) 0.4982(6) 0.3608(2) 0.0438 1.0000 Uani . . . . . .
C31 C 0.3010(4) 0.3480(6) 0.3584(2) 0.0601 1.0000 Uani . . . . . .
C32 C 0.2878(5) 0.2759(7) 0.3120(2) 0.0721 1.0000 Uani . . . . . .
C33 C 0.2739(5) 0.3567(7) 0.2682(2) 0.0739 1.0000 Uani . . . . . .
C34 C 0.2735(5) 0.5067(7) 0.2704(2) 0.0763 1.0000 Uani . . . . . .
C35 C 0.2868(4) 0.5800(6) 0.3170(2) 0.0628 1.0000 Uani . . . . . .
C36 C 0.0279(8) 0.801(2) 0.5556(5) 0.0675 0.509(11) Uani D U P . . .
C37 C -0.0589(7) 0.8305(15) 0.5753(4) 0.0702 0.509(11) Uani D U P . . .
C38 C -0.1197(10) 0.9816(19) 0.6351(6) 0.0965 0.509(11) Uani D U P . . .
C39 C -0.1053(13) 1.074(2) 0.6837(6) 0.1028 0.509(11) Uani D U P . . .
C40 C -0.0770(9) 0.974(3) 0.7288(7) 0.1100 0.509(11) Uani D U P . . .
C41 C 0.0024(17) 0.890(5) 0.7141(8) 0.1232 0.509(11) Uani D U P . . .
C42 C -0.020(2) 0.802(3) 0.6653(6) 0.1100 0.509(11) Uani D U P . . .
C936 C 0.0032(9) 0.8668(14) 0.5263(4) 0.0669 0.491(11) Uani D U P . . .
C937 C -0.0038(10) 0.7763(14) 0.5742(4) 0.0610 0.491(11) Uani D U P . . .
C938 C -0.0687(12) 0.965(2) 0.6222(6) 0.0878 0.491(11) Uani D U P . . .
C939 C -0.0581(16) 1.066(2) 0.6691(7) 0.1169 0.491(11) Uani D U P . . .
C940 C -0.0490(18) 0.970(3) 0.7172(7) 0.1123 0.491(11) Uani D U P . . .
C941 C 0.027(2) 0.866(5) 0.7127(9) 0.1313 0.491(11) Uani D U P . . .
C942 C 0.010(3) 0.773(3) 0.6645(7) 0.1158 0.491(11) Uani D U P . . .
H21 H 0.4760 0.9443 0.6315 0.0537 1.0000 Uiso R . . . . .
H41 H 0.7138 1.0932 0.6119 0.0574 1.0000 Uiso R . . . . .
H51 H 0.7123 0.9695 0.5352 0.0533 1.0000 Uiso R . . . . .
H81 H 0.5896 0.6076 0.4174 0.0595 1.0000 Uiso R . . . . .
H82 H 0.5310 0.7288 0.3921 0.0595 1.0000 Uiso R . . . . .
H91 H 0.4820 0.4556 0.4250 0.0602 1.0000 Uiso R . . . . .
H92 H 0.4535 0.5311 0.3738 0.0602 1.0000 Uiso R . . . . .
H121 H 0.1490 0.5512 0.3778 0.0664 1.0000 Uiso R . . . . .
H131 H 0.0272 0.6176 0.4148 0.0794 1.0000 Uiso R . . . . .
H151 H 0.1687 0.7827 0.5358 0.0740 1.0000 Uiso R . . . . .
H171 H 0.5300 0.9818 0.7156 0.0767 1.0000 Uiso R . . . . .
H172 H 0.4812 1.1148 0.6904 0.0767 1.0000 Uiso R . . . . .
H181 H 0.5534 1.2737 0.7447 0.0781 1.0000 Uiso R . . . . .
H182 H 0.5097 1.1552 0.7762 0.0781 1.0000 Uiso R . . . . .
H191 H 0.6005 1.2078 0.8495 0.0893 1.0000 Uiso R . . . . .
H192 H 0.6321 1.3363 0.8171 0.0893 1.0000 Uiso R . . . . .
H201 H 0.7341 1.2850 0.8833 0.1073 1.0000 Uiso R . . . . .
H202 H 0.7720 1.2539 0.8319 0.1073 1.0000 Uiso R . . . . .
H211 H 0.8048 1.0588 0.8837 0.1093 1.0000 Uiso R . . . . .
H212 H 0.7095 1.0408 0.8947 0.1093 1.0000 Uiso R . . . . .
H221 H 0.7374 0.8663 0.8344 0.1224 1.0000 Uiso R . . . . .
H222 H 0.7745 0.9860 0.8004 0.1224 1.0000 Uiso R . . . . .
H231 H 0.6001 0.9737 0.8209 0.0904 1.0000 Uiso R . . . . .
H232 H 0.6327 0.9313 0.7689 0.0904 1.0000 Uiso R . . . . .
H251 H 0.7227 0.6166 0.4996 0.0647 1.0000 Uiso R . . . . .
H261 H 0.8578 0.6180 0.4670 0.0746 1.0000 Uiso R . . . . .
H271 H 0.8903 0.7987 0.4101 0.0851 1.0000 Uiso R . . . . .
H281 H 0.7925 0.9811 0.3862 0.0859 1.0000 Uiso R . . . . .
H291 H 0.6592 0.9888 0.4218 0.0656 1.0000 Uiso R . . . . .
H311 H 0.3097 0.2920 0.3887 0.0721 1.0000 Uiso R . . . . .
H321 H 0.2883 0.1713 0.3106 0.0866 1.0000 Uiso R . . . . .
H331 H 0.2647 0.3080 0.2364 0.0887 1.0000 Uiso R . . . . .
H341 H 0.2641 0.5623 0.2401 0.0915 1.0000 Uiso R . . . . .
H351 H 0.2857 0.6846 0.3184 0.0754 1.0000 Uiso R . . . . .
H361 H 0.0576 0.8920 0.5529 0.0810 0.509 Uiso R . . . . .
H362 H 0.0600 0.7379 0.5784 0.0810 0.509 Uiso R . . . . .
H371 H -0.0883 0.7401 0.5793 0.0843 0.509 Uiso R . . . . .
H372 H -0.0920 0.8923 0.5524 0.0843 0.509 Uiso R . . . . .
H381 H -0.1642 0.9125 0.6393 0.1159 0.509 Uiso R . . . . .
H382 H -0.1361 1.0453 0.6075 0.1159 0.509 Uiso R . . . . .
H391 H -0.1571 1.1220 0.6903 0.1230 0.509 Uiso R . . . . .
H392 H -0.0622 1.1452 0.6794 0.1230 0.509 Uiso R . . . . .
H401 H -0.0635 1.0317 0.7583 0.1325 0.509 Uiso R . . . . .
H402 H -0.1213 0.9064 0.7351 0.1325 0.509 Uiso R . . . . .
H411 H 0.0213 0.8247 0.7408 0.1485 0.509 Uiso R . . . . .
H412 H 0.0467 0.9584 0.7085 0.1485 0.509 Uiso R . . . . .
H421 H -0.0670 0.7380 0.6702 0.1325 0.509 Uiso R . . . . .
H422 H 0.0277 0.7449 0.6572 0.1325 0.509 Uiso R . . . . .
H9361 H 0.0539 0.9246 0.5297 0.0802 0.491 Uiso R . . . . .
H9362 H -0.0451 0.9298 0.5212 0.0802 0.491 Uiso R . . . . .
H9371 H -0.0577 0.7280 0.5721 0.0733 0.491 Uiso R . . . . .
H9372 H 0.0406 0.7048 0.5764 0.0733 0.491 Uiso R . . . . .
H9381 H -0.1194 0.9080 0.6237 0.1053 0.491 Uiso R . . . . .
H9382 H -0.0732 1.0241 0.5925 0.1053 0.491 Uiso R . . . . .
H9391 H -0.1070 1.1273 0.6700 0.1401 0.491 Uiso R . . . . .
H9392 H -0.0085 1.1248 0.6673 0.1401 0.491 Uiso R . . . . .
H9401 H -0.0391 1.0311 0.7463 0.1353 0.491 Uiso R . . . . .
H9402 H -0.0997 0.9143 0.7200 0.1353 0.491 Uiso R . . . . .
H9411 H 0.0337 0.8039 0.7416 0.1582 0.491 Uiso R . . . . .
H9412 H 0.0783 0.9224 0.7105 0.1582 0.491 Uiso R . . . . .
H9421 H -0.0415 0.7196 0.6665 0.1395 0.491 Uiso R . . . . .
H9422 H 0.0562 0.7051 0.6620 0.1395 0.491 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.56(5)
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 . 1.834(3) yes
Ni1 . O2 . 1.818(4) yes
Ni1 . N1 . 1.846(4) yes
Ni1 . N2 . 1.851(4) yes
O1 . C1 . 1.302(6) yes
O2 . C16 . 1.313(6) yes
O3 . C3 . 1.377(6) yes
O3 . C17 . 1.427(7) yes
O4 . C14 . 1.408(8) yes
O4 . C36 . 1.418(9) yes
O94 . C14 . 1.403(8) yes
O94 . C936 . 1.419(9) yes
N1 . C7 . 1.316(6) yes
N1 . C8 . 1.476(6) yes
N2 . C9 . 1.467(7) yes
N2 . C10 . 1.323(6) yes
N3 . C18 . 1.442(8) yes
N3 . C19 . 1.470(7) yes
N3 . C23 . 1.405(8) yes
N4 . C37 . 1.453(9) yes
N4 . C38 . 1.438(9) yes
N4 . C42 . 1.451(9) yes
N94 . C937 . 1.450(9) yes
N94 . C938 . 1.448(9) yes
N94 . C942 . 1.451(9) yes
C1 . C2 . 1.417(7) yes
C1 . C6 . 1.410(7) yes
C2 . C3 . 1.366(7) yes
C2 . H21 . 0.950 no
C3 . C4 . 1.392(8) yes
C4 . C5 . 1.374(7) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.413(7) yes
C5 . H51 . 0.950 no
C6 . C7 . 1.443(7) yes
C7 . C24 . 1.507(7) yes
C8 . C9 . 1.488(7) yes
C8 . H81 . 0.950 no
C8 . H82 . 0.950 no
C9 . H91 . 0.950 no
C9 . H92 . 0.950 no
C10 . C11 . 1.421(7) yes
C10 . C30 . 1.505(7) yes
C11 . C12 . 1.430(7) yes
C11 . C16 . 1.426(7) yes
C12 . C13 . 1.358(8) yes
C12 . H121 . 0.950 no
C13 . C14 . 1.397(9) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.367(8) yes
C15 . C16 . 1.406(8) yes
C15 . H151 . 0.950 no
C17 . C18 . 1.501(8) yes
C17 . H171 . 0.950 no
C17 . H172 . 0.950 no
C18 . H181 . 0.950 no
C18 . H182 . 0.950 no
C19 . C20 . 1.516(9) yes
C19 . H191 . 0.950 no
C19 . H192 . 0.950 no
C20 . C21 . 1.490(9) yes
C20 . H201 . 0.950 no
C20 . H202 . 0.950 no
C21 . C22 . 1.533(9) yes
C21 . H211 . 0.950 no
C21 . H212 . 0.950 no
C22 . C23 . 1.557(10) yes
C22 . H221 . 0.950 no
C22 . H222 . 0.950 no
C23 . H231 . 0.950 no
C23 . H232 . 0.950 no
C24 . C25 . 1.391(7) yes
C24 . C29 . 1.367(8) yes
C25 . C26 . 1.391(8) yes
C25 . H251 . 0.950 no
C26 . C27 . 1.362(9) yes
C26 . H261 . 0.950 no
C27 . C28 . 1.369(9) yes
C27 . H271 . 0.950 no
C28 . C29 . 1.403(8) yes
C28 . H281 . 0.950 no
C29 . H291 . 0.950 no
C30 . C31 . 1.364(7) yes
C30 . C35 . 1.379(7) yes
C31 . C32 . 1.392(8) yes
C31 . H311 . 0.950 no
C32 . C33 . 1.373(9) yes
C32 . H321 . 0.950 no
C33 . C34 . 1.363(9) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.401(8) yes
C34 . H341 . 0.950 no
C35 . H351 . 0.950 no
C36 . C37 . 1.517(9) yes
C36 . H361 . 0.950 no
C36 . H362 . 0.950 no
C37 . H371 . 0.950 no
C37 . H372 . 0.950 no
C38 . C39 . 1.535(9) yes
C38 . H381 . 0.950 no
C38 . H382 . 0.950 no
C39 . C40 . 1.535(9) yes
C39 . H391 . 0.950 no
C39 . H392 . 0.950 no
C40 . C41 . 1.534(9) yes
C40 . H401 . 0.950 no
C40 . H402 . 0.950 no
C41 . C42 . 1.539(9) yes
C41 . C940 . 1.09(4) yes
C41 . H411 . 0.950 no
C41 . H412 . 0.950 no
C42 . H421 . 0.950 no
C42 . H422 . 0.950 no
C936 . C937 . 1.520(9) yes
C936 . H9361 . 0.950 no
C936 . H9362 . 0.950 no
C937 . H9371 . 0.950 no
C937 . H9372 . 0.950 no
C938 . C939 . 1.540(9) yes
C938 . H9381 . 0.950 no
C938 . H9382 . 0.950 no
C939 . C940 . 1.537(9) yes
C939 . H9391 . 0.950 no
C939 . H9392 . 0.950 no
C940 . C941 . 1.536(9) yes
C940 . H9401 . 0.950 no
C940 . H9402 . 0.950 no
C941 . C942 . 1.539(9) yes
C941 . H9411 . 0.950 no
C941 . H9412 . 0.950 no
C942 . H9421 . 0.950 no
C942 . H9422 . 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 . 84.03(15) yes
O1 . Ni1 . N1 . 94.42(16) yes
O2 . Ni1 . N1 . 176.26(18) yes
O1 . Ni1 . N2 . 176.16(18) yes
O2 . Ni1 . N2 . 94.10(17) yes
N1 . Ni1 . N2 . 87.64(18) yes
Ni1 . O1 . C1 . 127.8(3) yes
Ni1 . O2 . C16 . 126.7(3) yes
C3 . O3 . C17 . 117.3(4) yes
C14 . O4 . C36 . 120.5(10) yes
C14 . O94 . C936 . 114.3(10) yes
Ni1 . N1 . C7 . 128.0(4) yes
Ni1 . N1 . C8 . 112.4(3) yes
C7 . N1 . C8 . 119.0(4) yes
Ni1 . N2 . C9 . 111.3(3) yes
Ni1 . N2 . C10 . 128.0(4) yes
C9 . N2 . C10 . 120.7(4) yes
C18 . N3 . C19 . 108.1(5) yes
C18 . N3 . C23 . 112.5(5) yes
C19 . N3 . C23 . 108.7(5) yes
C37 . N4 . C38 . 108.7(9) yes
C37 . N4 . C42 . 113.1(12) yes
C38 . N4 . C42 . 109.1(13) yes
C937 . N94 . C938 . 111.8(10) yes
C937 . N94 . C942 . 110.3(12) yes
C938 . N94 . C942 . 109.6(13) yes
O1 . C1 . C2 . 116.8(5) yes
O1 . C1 . C6 . 124.6(4) yes
C2 . C1 . C6 . 118.6(4) yes
C1 . C2 . C3 . 121.1(5) yes
C1 . C2 . H21 . 119.4 no
C3 . C2 . H21 . 119.4 no
O3 . C3 . C2 . 123.6(5) yes
O3 . C3 . C4 . 115.6(4) yes
C2 . C3 . C4 . 120.8(5) yes
C3 . C4 . C5 . 119.1(5) yes
C3 . C4 . H41 . 120.5 no
C5 . C4 . H41 . 120.5 no
C4 . C5 . C6 . 122.0(5) yes
C4 . C5 . H51 . 119.0 no
C6 . C5 . H51 . 119.0 no
C5 . C6 . C1 . 118.3(5) yes
C5 . C6 . C7 . 119.8(5) yes
C1 . C6 . C7 . 121.9(4) yes
C6 . C7 . N1 . 122.5(5) yes
C6 . C7 . C24 . 117.2(4) yes
N1 . C7 . C24 . 120.2(4) yes
N1 . C8 . C9 . 109.0(4) yes
N1 . C8 . H81 . 109.6 no
C9 . C8 . H81 . 109.6 no
N1 . C8 . H82 . 109.6 no
C9 . C8 . H82 . 109.6 no
H81 . C8 . H82 . 109.5 no
C8 . C9 . N2 . 107.6(4) yes
C8 . C9 . H91 . 109.9 no
N2 . C9 . H91 . 109.9 no
C8 . C9 . H92 . 109.9 no
N2 . C9 . H92 . 109.9 no
H91 . C9 . H92 . 109.5 no
N2 . C10 . C11 . 121.9(5) yes
N2 . C10 . C30 . 119.6(5) yes
C11 . C10 . C30 . 118.5(4) yes
C10 . C11 . C12 . 121.3(5) yes
C10 . C11 . C16 . 122.5(4) yes
C12 . C11 . C16 . 116.2(5) yes
C11 . C12 . C13 . 122.6(6) yes
C11 . C12 . H121 . 118.7 no
C13 . C12 . H121 . 118.7 no
C12 . C13 . C14 . 119.7(5) yes
C12 . C13 . H131 . 120.1 no
C14 . C13 . H131 . 120.2 no
O4 . C14 . C13 . 123.1(7) yes
O94 . C14 . C13 . 106.3(7) yes
O4 . C14 . C15 . 114.9(8) yes
O94 . C14 . C15 . 131.9(7) yes
C13 . C14 . C15 . 120.5(5) yes
C14 . C15 . C16 . 120.7(6) yes
C14 . C15 . H151 . 119.6 no
C16 . C15 . H151 . 119.7 no
C11 . C16 . C15 . 120.2(5) yes
C11 . C16 . O2 . 123.6(5) yes
C15 . C16 . O2 . 116.2(5) yes
O3 . C17 . C18 . 108.9(5) yes
O3 . C17 . H171 . 109.6 no
C18 . C17 . H171 . 109.6 no
O3 . C17 . H172 . 109.6 no
C18 . C17 . H172 . 109.6 no
H171 . C17 . H172 . 109.5 no
C17 . C18 . N3 . 115.8(5) yes
C17 . C18 . H181 . 107.9 no
N3 . C18 . H181 . 107.9 no
C17 . C18 . H182 . 107.9 no
N3 . C18 . H182 . 107.9 no
H181 . C18 . H182 . 109.5 no
N3 . C19 . C20 . 110.4(6) yes
N3 . C19 . H191 . 109.2 no
C20 . C19 . H191 . 109.2 no
N3 . C19 . H192 . 109.2 no
C20 . C19 . H192 . 109.2 no
H191 . C19 . H192 . 109.5 no
C19 . C20 . C21 . 110.0(6) yes
C19 . C20 . H201 . 109.3 no
C21 . C20 . H201 . 109.3 no
C19 . C20 . H202 . 109.3 no
C21 . C20 . H202 . 109.4 no
H201 . C20 . H202 . 109.5 no
C20 . C21 . C22 . 109.7(6) yes
C20 . C21 . H211 . 109.4 no
C22 . C21 . H211 . 109.4 no
C20 . C21 . H212 . 109.4 no
C22 . C21 . H212 . 109.4 no
H211 . C21 . H212 . 109.5 no
C21 . C22 . C23 . 109.3(7) yes
C21 . C22 . H221 . 109.5 no
C23 . C22 . H221 . 109.5 no
C21 . C22 . H222 . 109.5 no
C23 . C22 . H222 . 109.5 no
H221 . C22 . H222 . 109.5 no
C22 . C23 . N3 . 109.7(6) yes
C22 . C23 . H231 . 109.4 no
N3 . C23 . H231 . 109.4 no
C22 . C23 . H232 . 109.4 no
N3 . C23 . H232 . 109.4 no
H231 . C23 . H232 . 109.5 no
C7 . C24 . C25 . 118.0(5) yes
C7 . C24 . C29 . 121.7(5) yes
C25 . C24 . C29 . 120.2(5) yes
C24 . C25 . C26 . 120.1(6) yes
C24 . C25 . H251 . 120.0 no
C26 . C25 . H251 . 120.0 no
C25 . C26 . C27 . 119.4(6) yes
C25 . C26 . H261 . 120.3 no
C27 . C26 . H261 . 120.3 no
C26 . C27 . C28 . 121.0(6) yes
C26 . C27 . H271 . 119.5 no
C28 . C27 . H271 . 119.5 no
C27 . C28 . C29 . 120.2(6) yes
C27 . C28 . H281 . 119.9 no
C29 . C28 . H281 . 119.9 no
C28 . C29 . C24 . 119.1(6) yes
C28 . C29 . H291 . 120.4 no
C24 . C29 . H291 . 120.4 no
C10 . C30 . C31 . 121.4(5) yes
C10 . C30 . C35 . 118.6(5) yes
C31 . C30 . C35 . 119.9(5) yes
C30 . C31 . C32 . 120.7(6) yes
C30 . C31 . H311 . 119.7 no
C32 . C31 . H311 . 119.6 no
C31 . C32 . C33 . 119.7(6) yes
C31 . C32 . H321 . 120.1 no
C33 . C32 . H321 . 120.1 no
C32 . C33 . C34 . 119.8(6) yes
C32 . C33 . H331 . 120.1 no
C34 . C33 . H331 . 120.1 no
C33 . C34 . C35 . 120.7(6) yes
C33 . C34 . H341 . 119.6 no
C35 . C34 . H341 . 119.6 no
C34 . C35 . C30 . 119.2(5) yes
C34 . C35 . H351 . 120.4 no
C30 . C35 . H351 . 120.4 no
O4 . C36 . C37 . 109.7(9) yes
O4 . C36 . H361 . 109.4 no
C37 . C36 . H361 . 109.4 no
O4 . C36 . H362 . 109.4 no
C37 . C36 . H362 . 109.4 no
H361 . C36 . H362 . 109.5 no
C36 . C37 . N4 . 107.1(10) yes
C36 . C37 . H371 . 110.1 no
N4 . C37 . H371 . 110.1 no
C36 . C37 . H372 . 110.0 no
N4 . C37 . H372 . 110.1 no
H371 . C37 . H372 . 109.5 no
N4 . C38 . C39 . 111.5(10) yes
N4 . C38 . H381 . 109.0 no
C39 . C38 . H381 . 109.0 no
N4 . C38 . H382 . 108.9 no
C39 . C38 . H382 . 109.0 no
H381 . C38 . H382 . 109.5 no
C38 . C39 . C40 . 110.1(12) yes
C38 . C39 . H391 . 109.3 no
C40 . C39 . H391 . 109.3 no
C38 . C39 . H392 . 109.3 no
C40 . C39 . H392 . 109.3 no
H391 . C39 . H392 . 109.5 no
C39 . C40 . C41 . 106.7(13) yes
C39 . C40 . H401 . 110.2 no
C41 . C40 . H401 . 110.2 no
C39 . C40 . H402 . 110.2 no
C41 . C40 . H402 . 110.1 no
H401 . C40 . H402 . 109.5 no
C40 . C41 . C42 . 109.3(14) yes
C40 . C41 . H411 . 109.6 no
C42 . C41 . H411 . 109.6 no
C40 . C41 . H412 . 109.4 no
C42 . C41 . H412 . 109.5 no
H411 . C41 . H412 . 109.5 no
C41 . C42 . N4 . 109.1(13) yes
C41 . C42 . H421 . 109.5 no
N4 . C42 . H421 . 109.7 no
C41 . C42 . H422 . 109.6 no
N4 . C42 . H422 . 109.5 no
H421 . C42 . H422 . 109.5 no
O94 . C936 . C937 . 109.1(11) yes
O94 . C936 . H9361 . 109.6 no
C937 . C936 . H9361 . 109.5 no
O94 . C936 . H9362 . 109.6 no
C937 . C936 . H9362 . 109.6 no
H9361 . C936 . H9362 . 109.5 no
C936 . C937 . N94 . 112.5(10) yes
C936 . C937 . H9371 . 108.7 no
N94 . C937 . H9371 . 108.7 no
C936 . C937 . H9372 . 108.7 no
N94 . C937 . H9372 . 108.7 no
H9371 . C937 . H9372 . 109.5 no
N94 . C938 . C939 . 111.5(10) yes
N94 . C938 . H9381 . 109.0 no
C939 . C938 . H9381 . 109.0 no
N94 . C938 . H9382 . 108.9 no
C939 . C938 . H9382 . 108.9 no
H9381 . C938 . H9382 . 109.5 no
C938 . C939 . C940 . 109.2(13) yes
C938 . C939 . H9391 . 109.5 no
C940 . C939 . H9391 . 109.6 no
C938 . C939 . H9392 . 109.6 no
C940 . C939 . H9392 . 109.5 no
H9391 . C939 . H9392 . 109.5 no
C939 . C940 . C41 . 110(2) yes
C939 . C940 . C941 . 107.8(15) yes
C939 . C940 . H9401 . 109.9 no
C941 . C940 . H9401 . 109.8 no
C939 . C940 . H9402 . 109.8 no
C941 . C940 . H9402 . 110.0 no
H9401 . C940 . H9402 . 109.5 no
C940 . C941 . C942 . 108.4(15) yes
C940 . C941 . H9411 . 109.7 no
C942 . C941 . H9411 . 109.7 no
C940 . C941 . H9412 . 109.8 no
C942 . C941 . H9412 . 109.8 no
H9411 . C941 . H9412 . 109.5 no
C941 . C942 . N94 . 110.5(14) yes
C941 . C942 . H9421 . 109.3 no
N94 . C942 . H9421 . 109.1 no
C941 . C942 . H9422 . 109.2 no
N94 . C942 . H9422 . 109.2 no
H9421 . C942 . H9422 . 109.5 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C1 -168.5(4) . . . . no
N1 Ni1 O1 C1 8.1(4) . . . . no
O1 Ni1 O2 C16 163.1(4) . . . . no
N2 Ni1 O2 C16 -20.3(4) . . . . no
O1 Ni1 N1 C7 -9.8(5) . . . . no
O1 Ni1 N1 C8 179.3(3) . . . . no
N2 Ni1 N1 C7 173.4(4) . . . . no
N2 Ni1 N1 C8 2.5(3) . . . . no
O2 Ni1 N2 C9 -164.7(3) . . . . no
O2 Ni1 N2 C10 13.7(4) . . . . no
N1 Ni1 N2 C9 18.6(3) . . . . no
N1 Ni1 N2 C10 -163.0(4) . . . . no
Ni1 O1 C1 C2 176.7(3) . . . . no
Ni1 O1 C1 C6 -2.9(7) . . . . no
Ni1 O2 C16 C11 17.5(7) . . . . no
Ni1 O2 C16 C15 -163.4(4) . . . . no
C17 O3 C3 C2 8.1(7) . . . . no
C17 O3 C3 C4 -173.4(5) . . . . no
C3 O3 C17 C18 179.2(5) . . . . no
C36 O4 C14 C13 176.4(11) . . . . no
C36 O4 C14 C15 10.4(16) . . . . no
C14 O4 C36 C37 172.5(11) . . . . no
Ni1 N1 C7 C6 6.4(7) . . . . no
Ni1 N1 C7 C24 -178.0(4) . . . . no
C8 N1 C7 C6 176.8(4) . . . . no
C8 N1 C7 C24 -7.6(7) . . . . no
Ni1 N1 C8 C9 -22.5(5) . . . . no
C7 N1 C8 C9 165.7(4) . . . . no
Ni1 N2 C9 C8 -34.7(5) . . . . no
C10 N2 C9 C8 146.8(4) . . . . no
Ni1 N2 C10 C11 -3.8(7) . . . . no
Ni1 N2 C10 C30 175.0(3) . . . . no
C9 N2 C10 C11 174.4(4) . . . . no
C9 N2 C10 C30 -6.7(7) . . . . no
C19 N3 C18 C17 -178.8(5) . . . . no
C23 N3 C18 C17 -58.7(7) . . . . no
C18 N3 C19 C20 -172.6(5) . . . . no
C23 N3 C19 C20 64.9(7) . . . . no
C18 N3 C23 C22 175.9(5) . . . . no
C19 N3 C23 C22 -64.2(7) . . . . no
C38 N4 C37 C36 158.5(12) . . . . no
C42 N4 C37 C36 -80.0(19) . . . . no
C37 N4 C38 C39 -174.3(12) . . . . no
C42 N4 C38 C39 61.7(19) . . . . no
C37 N4 C42 C41 175.1(17) . . . . no
C38 N4 C42 C41 -64(2) . . . . no
O1 C1 C2 C3 -177.5(5) . . . . no
C6 C1 C2 C3 2.1(7) . . . . no
O1 C1 C6 C5 177.0(4) . . . . no
O1 C1 C6 C7 -3.8(7) . . . . no
C2 C1 C6 C5 -2.6(7) . . . . no
C2 C1 C6 C7 176.6(4) . . . . no
C1 C2 C3 O3 178.5(5) . . . . no
C1 C2 C3 C4 0.0(8) . . . . no
O3 C3 C4 C5 179.9(4) . . . . no
C2 C3 C4 C5 -1.6(8) . . . . no
C3 C4 C5 C6 1.0(8) . . . . no
C4 C5 C6 C1 1.1(7) . . . . no
C4 C5 C6 C7 -178.1(5) . . . . no
C1 C6 C7 N1 2.0(7) . . . . no
C1 C6 C7 C24 -173.8(4) . . . . no
C5 C6 C7 N1 -178.8(4) . . . . no
C5 C6 C7 C24 5.4(7) . . . . no
N1 C7 C24 C25 -87.2(6) . . . . no
N1 C7 C24 C29 95.4(6) . . . . no
C6 C7 C24 C25 88.7(6) . . . . no
C6 C7 C24 C29 -88.7(6) . . . . no
N1 C8 C9 N2 35.9(5) . . . . no
N2 C10 C11 C12 177.2(5) . . . . no
N2 C10 C11 C16 -5.3(7) . . . . no
C30 C10 C11 C12 -1.7(7) . . . . no
C30 C10 C11 C16 175.8(5) . . . . no
N2 C10 C30 C31 86.6(6) . . . . no
N2 C10 C30 C35 -97.3(6) . . . . no
C11 C10 C30 C31 -94.5(6) . . . . no
C11 C10 C30 C35 81.6(6) . . . . no
C10 C11 C12 C13 179.1(5) . . . . no
C16 C11 C12 C13 1.4(8) . . . . no
C10 C11 C16 O2 -1.6(8) . . . . no
C10 C11 C16 C15 179.3(5) . . . . no
C12 C11 C16 O2 176.0(5) . . . . no
C12 C11 C16 C15 -3.1(7) . . . . no
C11 C12 C13 C14 1.7(9) . . . . no
C12 C13 C14 O4 -168.6(8) . . . . no
C12 C13 C14 C15 -3.3(10) . . . . no
O4 C14 C15 C16 168.1(8) . . . . no
C13 C14 C15 C16 1.6(10) . . . . no
C14 C15 C16 O2 -177.5(6) . . . . no
C14 C15 C16 C11 1.6(9) . . . . no
O3 C17 C18 N3 -57.0(7) . . . . no
N3 C19 C20 C21 -59.5(8) . . . . no
C19 C20 C21 C22 54.2(9) . . . . no
C20 C21 C22 C23 -53.7(9) . . . . no
C21 C22 C23 N3 59.6(7) . . . . no
C7 C24 C25 C26 -176.9(5) . . . . no
C29 C24 C25 C26 0.5(8) . . . . no
C7 C24 C29 C28 178.6(5) . . . . no
C25 C24 C29 C28 1.3(8) . . . . no
C24 C25 C26 C27 -1.6(10) . . . . no
C25 C26 C27 C28 0.8(11) . . . . no
C26 C27 C28 C29 1.1(11) . . . . no
C27 C28 C29 C24 -2.1(10) . . . . no
C10 C30 C31 C32 177.6(6) . . . . no
C35 C30 C31 C32 1.5(9) . . . . no
C10 C30 C35 C34 -177.7(6) . . . . no
C31 C30 C35 C34 -1.5(9) . . . . no
C30 C31 C32 C33 -0.9(11) . . . . no
C31 C32 C33 C34 0.3(12) . . . . no
C32 C33 C34 C35 -0.3(12) . . . . no
C33 C34 C35 C30 0.9(11) . . . . no
O4 C36 C37 N4 -178.2(12) . . . . no
N4 C38 C39 C40 -58.6(18) . . . . no
C38 C39 C40 C41 55(2) . . . . no
C39 C40 C41 C42 -58(3) . . . . no
C40 C41 C42 N4 63(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
Ni1 C3 3.906(5) . 2_676 no
Ni1 C4 3.474(5) . 2_676 no
Ni1 C5 3.380(5) . 2_676 no
Ni1 C6 3.737(5) . 2_676 no
Ni1 C9 3.894(5) . 2_666 no
O1 O2 2.444(5) . . no
O1 N1 2.701(5) . . no
O1 C7 2.917(6) . . no
O2 N2 2.686(5) . . no
O2 C10 2.918(6) . . no
O3 C35 3.369(7) . 2_676 no
O3 N3 2.882(6) . . no
O4 C26 3.327(11) . 1_455 no
O94 C936 3.31(2) . 2_576 no
O94 C27 3.014(13) . 1_455 no
O94 C26 3.080(11) . 1_455 no
N1 N2 2.560(6) . . no
N1 C1 2.897(6) . . no
N1 C9 2.413(7) . . no
N2 C4 3.439(7) . 2_676 no
N2 C8 2.384(7) . . no
N2 C16 2.890(7) . . no
C4 C38 3.464(17) . 1_655 no
C4 C10 3.524(7) . 2_676 no
C4 C11 3.581(7) . 2_676 no
C5 C25 3.457(7) . . no
C5 C29 3.395(7) . . no
C8 C25 3.426(7) . . no
C8 C29 3.445(8) . . no
C9 C31 3.343(8) . . no
C9 C35 3.585(8) . . no
C12 C31 3.577(8) . . no
C12 C35 3.344(8) . . no
C15 C937 3.381(16) . . no
C21 C26 3.424(10) . 4_565 no
C936 C936 2.786(17) . 2_576 no



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 06/03/17 at 12:58:34
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT O(4,OCC) N(4,OCC) C(36,OCC) UNTIL C(42) 
CONT O(94,OCC) N(94,OCC) C(936,OCC) UNTIL C(942) 
EQUIV O(4,OCC) N(4,OCC) C(36,OCC) UNTIL C(42) 
CONT O(94,OCC) N(94,OCC) C(936,OCC) UNTIL C(942) 
WEIGHT -1 O(94,OCC) N(94,OCC) C(936,OCC) UNTIL C(942) 
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 ( 8,X'S) H( 81,X'S) H( 82,X'S) 
RIDE C ( 9,X'S) H( 91,X'S) H( 92,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 ( 17,X'S) H( 171,X'S) H( 172,X'S) 
RIDE C ( 18,X'S) H( 181,X'S) H( 182,X'S) 
RIDE C ( 19,X'S) H( 191,X'S) H( 192,X'S) 
RIDE C ( 20,X'S) H( 201,X'S) H( 202,X'S) 
RIDE C ( 21,X'S) H( 211,X'S) H( 212,X'S) 
RIDE C ( 22,X'S) H( 221,X'S) H( 222,X'S) 
RIDE C ( 23,X'S) H( 231,X'S) H( 232,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) 
RIDE C ( 31,X'S) H( 311,X'S) 
RIDE C ( 32,X'S) H( 321,X'S) 
RIDE C ( 33,X'S) H( 331,X'S) 
RIDE C ( 34,X'S) H( 341,X'S) 
RIDE C ( 35,X'S) H( 351,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 ( 936,X'S) H( 9361,X'S) H( 9362,X'S) 
RIDE C ( 937,X'S) H( 9371,X'S) H( 9372,X'S) 
RIDE C ( 938,X'S) H( 9381,X'S) H( 9382,X'S) 
RIDE C ( 939,X'S) H( 9391,X'S) H( 9392,X'S) 
RIDE C ( 940,X'S) H( 9401,X'S) H( 9402,X'S) 
RIDE C ( 941,X'S) H( 9411,X'S) H( 9412,X'S) 
RIDE C ( 942,X'S) H( 9421,X'S) H( 9422,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 06/03/17 at 12:58:34
#
#LIST     16                                                                    
DIST 0.0, .01 =  MEAN  C(14) TO O(4), C(14) TO O(94) 
DIST 0.0, .01 =  MEAN  O(4) TO C(36), O(94) TO C(936) 
DIST 0.0, .01 =  MEAN  C(36) TO C(37), C(936) TO C(937) 
DIST 1.45, .01 =    C(37) TO N(4), C(937) TO N(94) 
DIST 1.45, .01 =    N(4) TO C(38), N(94) TO C(938) 
DIST 1.54, .01 =    C(38) TO C(39), C(938) TO C(939) 
DIST 1.54, .01 =    C(39) TO C(40), C(939) TO C(940) 
DIST 1.54, .01 =    C(40) TO C(41), C(940) TO C(941) 
DIST 1.54, .01 =    C(41) TO C(42), C(941) TO C(942) 
DIST 1.45, .01 =    N(4) TO C(42), N(94) TO C(942) 
REM 
ANGLE 109, 2 = C(37) TO N(4) TO C(38) 
ANGLE 109, 2 = C(37) TO N(4) TO C(42) 
ANGLE 109, 2 = C(38) TO N(4) TO C(42) 
ANGLE 109, 2 = N(4) TO C(38) TO C(39) 
ANGLE 109, 2 = C(38) TO C(39) TO C(40) 
ANGLE 109, 2 = C(39) TO C(40) TO C(41) 
ANGLE 109, 2 = C(40) TO C(41) TO C(42) 
ANGLE 109, 2 = C(41) TO C(42) TO N(4) 
REM 
ANGLE 109, 2 = C(937) TO N(94) TO C(938) 
ANGLE 109, 2 = C(937) TO N(94) TO C(942) 
ANGLE 109, 2 = C(938) TO N(94) TO C(942) 
ANGLE 109, 2 = N(94) TO C(938) TO C(939) 
ANGLE 109, 2 = C(938) TO C(939) TO C(940) 
ANGLE 109, 2 = C(939) TO C(940) TO C(941) 
ANGLE 109, 2 = C(940) TO C(941) TO C(942) 
ANGLE 109, 2 = C(941) TO C(942) TO N(94) 
REM 
U(IJ) 0.0, .02 = C(38) TO C(938) 
U(IJ) 0.0, .02 = C(39) TO C(939) 
U(IJ) 0.0, .02 = C(40) TO C(940) 
U(IJ) 0.0, .02 = C(41) TO C(941) 
U(IJ) 0.0, .02 = C(42) TO C(942) 
REM 
U(IJ) 0.0, .02 = O(4) TO O(94) 
U(IJ) 0.0, .02 = C(36) TO C(936) 
U(IJ) 0.0, .02 = C(37) TO C(937) 
U(IJ) 0.0, .02 = N(4) TO N(94) 
REM 
U(IJ) 0.0, .01 = C(1) TO O(1) 
U(IJ) 0.0, .01 = C(1) TO C(2) 
U(IJ) 0.0, .01 = C(1) TO C(6) 
REM 
LIMIT C(40,X) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-15 2 8 x .



#===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_ral1702BSNQ
_audit_block_doi                 10.5517/ccdc.csd.cc20998x
_database_code_depnum_ccdc_archive 'CCDC 1855978'
loop_
_audit_author_name
_audit_author_address
'Anthony Willis'
;Australian National University
Australia
;
_audit_update_record             
;
2018-07-16 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_audit_creation_date             17-01-18
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1702BSNQ\Tony_ral1702BSNQ_ At 12: 9 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   12.8742(1)
_cell_length_b                   9.3175(1)
_cell_length_c                   25.5985(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.4790(7)
_cell_angle_gamma                90
_cell_volume                     3037.11(5)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'

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 0.0181 0.0091 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 0.0311 0.0180 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 -3.0029 0.5091 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 0.0492 0.0322 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 0.3331 0.5567 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 = C31 H36 N2 Ni1 O8 S1 
# Dc =      1.43 Fooo =   1376.00 Mu =     20.18 M =    655.41
# Found Formula = C31 H36 N2 Ni1 O8 S1 
# Dc =      1.43 FOOO =   1376.00 Mu =     20.18 M =    655.41

_chemical_formula_sum            'C31 H36 N2 Ni O8 S'
_chemical_formula_moiety         'C29 H24 N2 Ni O4, C2 H6 O S, 3(H2 O)'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         655.41


_cell_measurement_reflns_used    26974
_cell_measurement_theta_min      3
_cell_measurement_theta_max      74
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.092
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_max          0.187

_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    2.018

# Sheldrick geometric approximatio 0.76 0.83 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro version 1.171.38.43 (Rigaku Oxford Diffraction, 2016)
(Release 29 April 2016; compiled 27 May 2016,16:53)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_T_max  0.83
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
#_diffrn_ambient_temperature 150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_measurement_method       'ω scans'


# If a reference occurs more than once, delete the author 
# and date from subsequent references. 

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'

_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    'PLATON (Spek, 2008)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            44751
_reflns_number_total             6155
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.0340

# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6155 
# Theoretical number of reflections is about 12304 


_diffrn_reflns_theta_min         3.491
_diffrn_reflns_theta_max         73.851
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        73.851
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -16
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              31

_oxford_diffrn_Wilson_B_factor   1.79
_oxford_diffrn_Wilson_scale      0.11

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

_refine_diff_density_min         -0.26
_refine_diff_density_max         0.37


# 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         6155
_refine_ls_number_restraints     3
_refine_ls_number_parameters     413
_oxford_refine_ls_R_factor_ref   0.0313
_refine_ls_wR_factor_ref         0.0794
_refine_ls_goodness_of_fit_ref   0.9963
_refine_ls_shift/su_max          0.0062995
_refine_ls_shift/su_mean         0.0003569


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6155
_refine_ls_R_factor_all          0.0313
_refine_ls_wR_factor_all         0.0794

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5799
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_gt          0.0783

# 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    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 + 1.88P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               

The H atoms were all located in a difference map, but 
those bonded to C
 were repositioned geometrically. 
The H atoms were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98Å, O---H = 0.83Å) 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
and the displacement parameters were held fixed. 
Finally the positions of the H atoms bonded to O were also allowed 
to refine freely, but with restraints on O---H angle and H---O---H
angle for O8 only.
 

The largest features in the
final difference electron density map are located 
near O8 and then midway between bonded C atoms.
The former might suggest some disorder in the H atom positions about O8.
;

# 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 0.830485(17) 0.74316(2) 0.389244(8) 0.0172 1.0000 Uani . . . . . .
S1 S 0.31988(3) 0.10513(4) 0.301613(15) 0.0284 1.0000 Uani . . . . . .
O1 O 0.81379(7) 0.71768(11) 0.45874(4) 0.0208 1.0000 Uani . . . . . .
O2 O 0.69048(7) 0.69830(11) 0.37774(4) 0.0219 1.0000 Uani . . . . . .
O3 O 0.90721(8) 0.55431(12) 0.63452(4) 0.0247 1.0000 Uani . . . . . .
O4 O 0.33747(8) 0.74574(12) 0.30630(4) 0.0246 1.0000 Uani . . . . . .
O5 O 0.30358(8) 0.25808(11) 0.28052(4) 0.0268 1.0000 Uani . . . . . .
O6 O 0.29490(9) 0.47793(14) 0.35052(4) 0.0287 1.0000 Uani . . . . . .
O7 O 0.54997(14) 0.62221(18) 0.56640(6) 0.0529 1.0000 Uani . . . . . .
O8 O 0.59443(14) 0.5932(3) 0.46554(7) 0.0885 1.0000 Uani D . . . . .
N1 N 0.96849(9) 0.81010(13) 0.40754(4) 0.0204 1.0000 Uani . . . . . .
N2 N 0.83966(9) 0.74206(12) 0.31606(5) 0.0198 1.0000 Uani . . . . . .
C1 C 0.88853(10) 0.68850(15) 0.49796(5) 0.0181 1.0000 Uani . . . . . .
C2 C 0.85818(10) 0.63890(15) 0.54545(5) 0.0195 1.0000 Uani . . . . . .
C3 C 0.93291(11) 0.60398(15) 0.58806(5) 0.0201 1.0000 Uani . . . . . .
C4 C 1.04053(11) 0.61664(16) 0.58510(5) 0.0230 1.0000 Uani . . . . . .
C5 C 1.07067(10) 0.66862(16) 0.53964(5) 0.0219 1.0000 Uani . . . . . .
C6 C 0.99728(10) 0.70902(15) 0.49535(5) 0.0189 1.0000 Uani . . . . . .
C7 C 1.03148(10) 0.78256(15) 0.45134(5) 0.0189 1.0000 Uani . . . . . .
C8 C 1.00192(11) 0.91008(17) 0.36854(6) 0.0263 1.0000 Uani . . . . . .
C9 C 1.02234(12) 0.8321(2) 0.31865(6) 0.0328 1.0000 Uani . . . . . .
C10 C 0.94671(11) 0.70736(18) 0.30520(6) 0.0261 1.0000 Uani . . . . . .
C11 C 0.76192(11) 0.75150(14) 0.27708(5) 0.0183 1.0000 Uani . . . . . .
C12 C 0.65332(11) 0.76151(14) 0.28565(5) 0.0184 1.0000 Uani . . . . . .
C13 C 0.57262(11) 0.79533(16) 0.24365(5) 0.0220 1.0000 Uani . . . . . .
C14 C 0.46807(11) 0.79266(16) 0.24916(5) 0.0231 1.0000 Uani . . . . . .
C15 C 0.44021(11) 0.75148(15) 0.29808(5) 0.0201 1.0000 Uani . . . . . .
C16 C 0.51596(11) 0.71948(15) 0.34023(5) 0.0203 1.0000 Uani . . . . . .
C17 C 0.62350(11) 0.72734(14) 0.33553(5) 0.0182 1.0000 Uani . . . . . .
C18 C 1.14433(10) 0.83069(15) 0.45855(5) 0.0196 1.0000 Uani . . . . . .
C19 C 1.17710(11) 0.95421(16) 0.48663(6) 0.0245 1.0000 Uani . . . . . .
C20 C 1.28270(12) 0.99130(18) 0.49541(6) 0.0300 1.0000 Uani . . . . . .
C21 C 1.35630(12) 0.90245(19) 0.47730(6) 0.0328 1.0000 Uani . . . . . .
C22 C 1.32448(12) 0.77832(19) 0.44986(7) 0.0325 1.0000 Uani . . . . . .
C23 C 1.21848(12) 0.74356(16) 0.43960(6) 0.0262 1.0000 Uani . . . . . .
C24 C 0.78195(10) 0.74697(15) 0.22065(5) 0.0186 1.0000 Uani . . . . . .
C25 C 0.82674(12) 0.86302(16) 0.19810(6) 0.0241 1.0000 Uani . . . . . .
C26 C 0.84286(12) 0.85773(17) 0.14557(6) 0.0262 1.0000 Uani . . . . . .
C27 C 0.81548(11) 0.73649(17) 0.11549(5) 0.0241 1.0000 Uani . . . . . .
C28 C 0.77104(11) 0.62026(17) 0.13768(6) 0.0261 1.0000 Uani . . . . . .
C29 C 0.75350(11) 0.62599(16) 0.18997(5) 0.0237 1.0000 Uani . . . . . .
C30 C 0.44690(12) 0.10249(19) 0.33961(7) 0.0338 1.0000 Uani . . . . . .
C31 C 0.24541(15) 0.0943(2) 0.35471(9) 0.0530 1.0000 Uani . . . . . .
H1 H 0.8454(16) 0.549(2) 0.6340(8) 0.0367 1.0000 Uiso . . . . . .
H2 H 0.2973(17) 0.756(2) 0.2791(9) 0.0380 1.0000 Uiso . . . . . .
H3 H 0.3033(17) 0.554(3) 0.3384(9) 0.0434 1.0000 Uiso . . . . . .
H4 H 0.3032(16) 0.416(2) 0.3261(9) 0.0436 1.0000 Uiso . . . . . .
H5 H 0.597(2) 0.580(3) 0.5902(11) 0.0785 1.0000 Uiso . . . . . .
H6 H 0.510(2) 0.568(3) 0.5598(13) 0.0796 1.0000 Uiso . . . . . .
H7 H 0.646(2) 0.624(4) 0.4556(12) 0.1318 1.0000 Uiso D . . . . .
H8 H 0.595(3) 0.610(4) 0.4965(8) 0.1330 1.0000 Uiso D . . . . .
H21 H 0.7872 0.6288 0.5475 0.0225 1.0000 Uiso R . . . . .
H41 H 1.0913 0.5900 0.6143 0.0281 1.0000 Uiso R . . . . .
H51 H 1.1425 0.6769 0.5378 0.0256 1.0000 Uiso R . . . . .
H81 H 1.0642 0.9628 0.3839 0.0308 1.0000 Uiso R . . . . .
H82 H 0.9442 0.9786 0.3593 0.0307 1.0000 Uiso R . . . . .
H91 H 1.0923 0.7960 0.3230 0.0396 1.0000 Uiso R . . . . .
H92 H 1.0160 0.8996 0.2895 0.0387 1.0000 Uiso R . . . . .
H101 H 0.9708 0.6239 0.3269 0.0298 1.0000 Uiso R . . . . .
H102 H 0.9450 0.6809 0.2682 0.0306 1.0000 Uiso R . . . . .
H131 H 0.5906 0.8211 0.2106 0.0265 1.0000 Uiso R . . . . .
H141 H 0.4168 0.8197 0.2206 0.0278 1.0000 Uiso R . . . . .
H161 H 0.4959 0.6943 0.3729 0.0249 1.0000 Uiso R . . . . .
H191 H 1.1274 1.0115 0.4997 0.0283 1.0000 Uiso R . . . . .
H201 H 1.3034 1.0764 0.5140 0.0363 1.0000 Uiso R . . . . .
H211 H 1.4284 0.9254 0.4837 0.0385 1.0000 Uiso R . . . . .
H221 H 1.3746 0.7163 0.4384 0.0400 1.0000 Uiso R . . . . .
H231 H 1.1965 0.6612 0.4208 0.0310 1.0000 Uiso R . . . . .
H251 H 0.8454 0.9457 0.2183 0.0284 1.0000 Uiso R . . . . .
H261 H 0.8720 0.9360 0.1304 0.0317 1.0000 Uiso R . . . . .
H271 H 0.8269 0.7343 0.0810 0.0278 1.0000 Uiso R . . . . .
H281 H 0.7533 0.5371 0.1177 0.0310 1.0000 Uiso R . . . . .
H291 H 0.7223 0.5479 0.2053 0.0291 1.0000 Uiso R . . . . .
H301 H 0.4960 0.1147 0.3153 0.0510 1.0000 Uiso R . . . . .
H302 H 0.4498 0.1801 0.3649 0.0504 1.0000 Uiso R . . . . .
H303 H 0.4560 0.0107 0.3572 0.0511 1.0000 Uiso R . . . . .
H311 H 0.1739 0.1125 0.3397 0.0796 1.0000 Uiso R . . . . .
H312 H 0.2717 0.1663 0.3809 0.0799 1.0000 Uiso R . . . . .
H313 H 0.2542 -0.0011 0.3681 0.0787 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       37(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          3.24(3)
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 . 1.8385(9) yes
Ni1 . O2 . 1.8313(9) yes
Ni1 . N1 . 1.8761(11) yes
Ni1 . N2 . 1.8944(12) yes
S1 . O5 . 1.5274(11) yes
S1 . C30 . 1.7754(16) yes
S1 . C31 . 1.778(2) yes
O1 . C1 . 1.3126(16) yes
O2 . C17 . 1.3075(16) yes
O3 . C3 . 1.3618(16) yes
O3 . H1 . 0.79(2) no
O4 . C15 . 1.3707(17) yes
O4 . H2 . 0.81(2) no
O6 . H3 . 0.79(2) no
O6 . H4 . 0.87(2) no
O7 . H5 . 0.88(3) no
O7 . H6 . 0.72(3) no
O8 . H7 . 0.802(18) no
O8 . H8 . 0.807(18) no
N1 . C7 . 1.3087(18) yes
N1 . C8 . 1.4752(17) yes
N2 . C10 . 1.4813(17) yes
N2 . C11 . 1.3079(18) yes
C1 . C2 . 1.4086(18) yes
C1 . C6 . 1.4244(18) yes
C2 . C3 . 1.3827(18) yes
C2 . H21 . 0.928 no
C3 . C4 . 1.4036(19) yes
C4 . C5 . 1.3684(19) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.4156(18) yes
C5 . H51 . 0.936 no
C6 . C7 . 1.4417(18) yes
C7 . C18 . 1.5056(17) yes
C8 . C9 . 1.526(2) yes
C8 . H81 . 0.972 no
C8 . H82 . 0.982 no
C9 . C10 . 1.522(2) yes
C9 . H91 . 0.953 no
C9 . H92 . 0.970 no
C10 . H101 . 0.979 no
C10 . H102 . 0.975 no
C11 . C12 . 1.4500(19) yes
C11 . C24 . 1.5048(18) yes
C12 . C13 . 1.4160(19) yes
C12 . C17 . 1.4226(18) yes
C13 . C14 . 1.3742(19) yes
C13 . H131 . 0.940 no
C14 . C15 . 1.4058(19) yes
C14 . H141 . 0.943 no
C15 . C16 . 1.3763(19) yes
C16 . C17 . 1.4091(19) yes
C16 . H161 . 0.941 no
C18 . C19 . 1.389(2) yes
C18 . C23 . 1.394(2) yes
C19 . C20 . 1.389(2) yes
C19 . H191 . 0.932 no
C20 . C21 . 1.388(2) yes
C20 . H201 . 0.942 no
C21 . C22 . 1.384(2) yes
C21 . H211 . 0.944 no
C22 . C23 . 1.389(2) yes
C22 . H221 . 0.945 no
C23 . H231 . 0.927 no
C24 . C25 . 1.3905(19) yes
C24 . C29 . 1.392(2) yes
C25 . C26 . 1.3914(19) yes
C25 . H251 . 0.939 no
C26 . C27 . 1.383(2) yes
C26 . H261 . 0.931 no
C27 . C28 . 1.385(2) yes
C27 . H271 . 0.917 no
C28 . C29 . 1.3911(19) yes
C28 . H281 . 0.938 no
C29 . H291 . 0.944 no
C30 . H301 . 0.956 no
C30 . H302 . 0.966 no
C30 . H303 . 0.965 no
C31 . H311 . 0.959 no
C31 . H312 . 0.973 no
C31 . H313 . 0.954 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 . 82.72(4) yes
O1 . Ni1 . N1 . 92.46(5) yes
O2 . Ni1 . N1 . 171.67(5) yes
O1 . Ni1 . N2 . 171.65(5) yes
O2 . Ni1 . N2 . 92.48(5) yes
N1 . Ni1 . N2 . 93.08(5) yes
O5 . S1 . C30 . 105.91(7) yes
O5 . S1 . C31 . 105.16(8) yes
C30 . S1 . C31 . 97.89(9) yes
Ni1 . O1 . C1 . 126.13(8) yes
Ni1 . O2 . C17 . 126.81(9) yes
C3 . O3 . H1 . 112.1(14) no
C15 . O4 . H2 . 111.9(15) no
H3 . O6 . H4 . 106(2) no
H5 . O7 . H6 . 104(3) no
H7 . O8 . H8 . 110.6(10) no
Ni1 . N1 . C7 . 126.37(10) yes
Ni1 . N1 . C8 . 113.64(9) yes
C7 . N1 . C8 . 119.87(11) yes
Ni1 . N2 . C10 . 112.47(9) yes
Ni1 . N2 . C11 . 127.00(10) yes
C10 . N2 . C11 . 119.99(12) yes
O1 . C1 . C2 . 117.56(12) yes
O1 . C1 . C6 . 123.44(12) yes
C2 . C1 . C6 . 118.96(12) yes
C1 . C2 . C3 . 120.58(12) yes
C1 . C2 . H21 . 118.9 no
C3 . C2 . H21 . 120.5 no
C2 . C3 . O3 . 122.58(12) yes
C2 . C3 . C4 . 121.01(12) yes
O3 . C3 . C4 . 116.40(12) yes
C3 . C4 . C5 . 118.78(12) yes
C3 . C4 . H41 . 120.3 no
C5 . C4 . H41 . 120.9 no
C4 . C5 . C6 . 122.40(12) yes
C4 . C5 . H51 . 118.6 no
C6 . C5 . H51 . 119.0 no
C1 . C6 . C5 . 118.12(12) yes
C1 . C6 . C7 . 121.07(12) yes
C5 . C6 . C7 . 120.50(12) yes
C6 . C7 . N1 . 122.73(12) yes
C6 . C7 . C18 . 116.50(12) yes
N1 . C7 . C18 . 120.75(12) yes
N1 . C8 . C9 . 111.66(13) yes
N1 . C8 . H81 . 110.5 no
C9 . C8 . H81 . 110.2 no
N1 . C8 . H82 . 106.8 no
C9 . C8 . H82 . 109.0 no
H81 . C8 . H82 . 108.6 no
C8 . C9 . C10 . 111.69(12) yes
C8 . C9 . H91 . 110.3 no
C10 . C9 . H91 . 108.6 no
C8 . C9 . H92 . 109.3 no
C10 . C9 . H92 . 110.0 no
H91 . C9 . H92 . 106.8 no
C9 . C10 . N2 . 111.88(13) yes
C9 . C10 . H101 . 109.8 no
N2 . C10 . H101 . 107.0 no
C9 . C10 . H102 . 109.6 no
N2 . C10 . H102 . 110.4 no
H101 . C10 . H102 . 108.1 no
N2 . C11 . C12 . 122.37(12) yes
N2 . C11 . C24 . 120.69(12) yes
C12 . C11 . C24 . 116.91(12) yes
C11 . C12 . C13 . 121.02(12) yes
C11 . C12 . C17 . 121.02(12) yes
C13 . C12 . C17 . 117.81(12) yes
C12 . C13 . C14 . 122.55(13) yes
C12 . C13 . H131 . 119.3 no
C14 . C13 . H131 . 118.2 no
C13 . C14 . C15 . 118.61(13) yes
C13 . C14 . H141 . 120.0 no
C15 . C14 . H141 . 121.4 no
C14 . C15 . O4 . 121.75(12) yes
C14 . C15 . C16 . 120.87(13) yes
O4 . C15 . C16 . 117.35(12) yes
C15 . C16 . C17 . 120.89(12) yes
C15 . C16 . H161 . 119.7 no
C17 . C16 . H161 . 119.4 no
C12 . C17 . C16 . 119.13(12) yes
C12 . C17 . O2 . 123.76(12) yes
C16 . C17 . O2 . 117.08(12) yes
C7 . C18 . C19 . 121.61(12) yes
C7 . C18 . C23 . 118.82(12) yes
C19 . C18 . C23 . 119.43(13) yes
C18 . C19 . C20 . 120.35(14) yes
C18 . C19 . H191 . 119.2 no
C20 . C19 . H191 . 120.5 no
C19 . C20 . C21 . 119.84(14) yes
C19 . C20 . H201 . 119.3 no
C21 . C20 . H201 . 120.9 no
C20 . C21 . C22 . 120.16(14) yes
C20 . C21 . H211 . 120.6 no
C22 . C21 . H211 . 119.2 no
C21 . C22 . C23 . 119.99(15) yes
C21 . C22 . H221 . 120.3 no
C23 . C22 . H221 . 119.7 no
C18 . C23 . C22 . 120.17(14) yes
C18 . C23 . H231 . 119.4 no
C22 . C23 . H231 . 120.5 no
C11 . C24 . C25 . 121.13(12) yes
C11 . C24 . C29 . 119.76(12) yes
C25 . C24 . C29 . 119.10(12) yes
C24 . C25 . C26 . 120.25(14) yes
C24 . C25 . H251 . 119.8 no
C26 . C25 . H251 . 119.9 no
C25 . C26 . C27 . 120.32(14) yes
C25 . C26 . H261 . 120.2 no
C27 . C26 . H261 . 119.5 no
C26 . C27 . C28 . 119.81(13) yes
C26 . C27 . H271 . 119.4 no
C28 . C27 . H271 . 120.8 no
C27 . C28 . C29 . 120.01(14) yes
C27 . C28 . H281 . 120.3 no
C29 . C28 . H281 . 119.7 no
C24 . C29 . C28 . 120.50(13) yes
C24 . C29 . H291 . 118.9 no
C28 . C29 . H291 . 120.6 no
S1 . C30 . H301 . 106.6 no
S1 . C30 . H302 . 107.3 no
H301 . C30 . H302 . 112.4 no
S1 . C30 . H303 . 107.8 no
H301 . C30 . H303 . 111.2 no
H302 . C30 . H303 . 111.2 no
S1 . C31 . H311 . 106.1 no
S1 . C31 . H312 . 108.4 no
H311 . C31 . H312 . 111.8 no
S1 . C31 . H313 . 106.2 no
H311 . C31 . H313 . 111.4 no
H312 . C31 . H313 . 112.6 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 . H1 . O6 2_666 166(2) 0.80(2) 1.92(2) 2.702(2) yes
O4 . H2 . O5 3_555 173(2) 0.81(2) 1.85(2) 2.657(2) yes
O6 . H3 . O4 . 175(2) 0.79(2) 2.04(2) 2.827(2) yes
O6 . H4 . O5 . 168(2) 0.87(2) 1.88(2) 2.735(2) yes
O7 . H5 . O6 2_666 169(3) 0.89(3) 1.98(3) 2.851(2) yes
O7 . H6 . O8 2_666 173(3) 0.72(3) 2.06(3) 2.776(2) yes
O8 . H7 . O1 . 160(3) 0.80(2) 2.32(2) 3.081(2) yes
O8 . H7 . O2 . 136(3) 0.80(2) 2.26(2) 2.891(2) yes
O8 . H8 . O7 . 161(3) 0.81(2) 1.97(2) 2.739(2) yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C1 158.15(12) . . . . no
N1 Ni1 O1 C1 -28.68(12) . . . . no
O1 Ni1 O2 C17 159.79(11) . . . . no
N2 Ni1 O2 C17 -27.06(11) . . . . no
O1 Ni1 N1 C7 24.19(12) . . . . no
O1 Ni1 N1 C8 -151.79(10) . . . . no
N2 Ni1 N1 C7 -149.57(12) . . . . no
N2 Ni1 N1 C8 34.45(10) . . . . no
O2 Ni1 N2 C10 -153.25(10) . . . . no
O2 Ni1 N2 C11 18.29(12) . . . . no
N1 Ni1 N2 C10 32.96(10) . . . . no
N1 Ni1 N2 C11 -155.51(12) . . . . no
Ni1 O1 C1 C2 -164.97(10) . . . . no
Ni1 O1 C1 C6 17.21(19) . . . . no
Ni1 O2 C17 C12 19.04(19) . . . . no
Ni1 O2 C17 C16 -162.94(10) . . . . no
Ni1 N1 C7 C6 -8.1(2) . . . . no
Ni1 N1 C7 C18 173.56(10) . . . . no
C8 N1 C7 C6 167.71(13) . . . . no
C8 N1 C7 C18 -10.68(19) . . . . no
Ni1 N1 C8 C9 -73.51(13) . . . . no
C7 N1 C8 C9 110.22(14) . . . . no
Ni1 N2 C10 C9 -73.81(13) . . . . no
C11 N2 C10 C9 113.99(14) . . . . no
Ni1 N2 C11 C12 -1.38(19) . . . . no
Ni1 N2 C11 C24 -179.13(9) . . . . no
C10 N2 C11 C12 169.59(13) . . . . no
C10 N2 C11 C24 -8.17(19) . . . . no
O1 C1 C2 C3 178.96(13) . . . . no
C6 C1 C2 C3 -3.1(2) . . . . no
O1 C1 C6 C5 -177.75(13) . . . . no
O1 C1 C6 C7 8.7(2) . . . . no
C2 C1 C6 C5 4.5(2) . . . . no
C2 C1 C6 C7 -169.09(13) . . . . no
C1 C2 C3 O3 -179.33(13) . . . . no
C1 C2 C3 C4 -0.2(2) . . . . no
O3 C3 C4 C5 -178.78(13) . . . . no
C2 C3 C4 C5 2.0(2) . . . . no
C3 C4 C5 C6 -0.5(2) . . . . no
C4 C5 C6 C1 -2.7(2) . . . . no
C4 C5 C6 C7 170.87(14) . . . . no
C1 C6 C7 N1 -13.2(2) . . . . no
C1 C6 C7 C18 165.27(12) . . . . no
C5 C6 C7 N1 173.42(13) . . . . no
C5 C6 C7 C18 -8.13(19) . . . . no
N1 C7 C18 C19 99.07(16) . . . . no
N1 C7 C18 C23 -85.37(17) . . . . no
C6 C7 C18 C19 -79.42(17) . . . . no
C6 C7 C18 C23 96.14(15) . . . . no
N1 C8 C9 C10 35.16(17) . . . . no
C8 C9 C10 N2 38.09(17) . . . . no
N2 C11 C12 C13 169.44(13) . . . . no
N2 C11 C12 C17 -15.3(2) . . . . no
C24 C11 C12 C13 -12.73(19) . . . . no
C24 C11 C12 C17 162.58(12) . . . . no
N2 C11 C24 C25 -73.24(18) . . . . no
N2 C11 C24 C29 108.02(15) . . . . no
C12 C11 C24 C25 108.88(15) . . . . no
C12 C11 C24 C29 -69.86(17) . . . . no
C11 C12 C13 C14 173.80(13) . . . . no
C17 C12 C13 C14 -1.7(2) . . . . no
C11 C12 C17 O2 6.6(2) . . . . no
C11 C12 C17 C16 -171.42(12) . . . . no
C13 C12 C17 O2 -177.97(13) . . . . no
C13 C12 C17 C16 4.04(19) . . . . no
C12 C13 C14 C15 -1.5(2) . . . . no
C13 C14 C15 O4 -179.68(13) . . . . no
C13 C14 C15 C16 2.3(2) . . . . no
O4 C15 C16 C17 -177.96(12) . . . . no
C14 C15 C16 C17 0.1(2) . . . . no
C15 C16 C17 O2 178.54(13) . . . . no
C15 C16 C17 C12 -3.3(2) . . . . no
C7 C18 C19 C20 176.05(13) . . . . no
C23 C18 C19 C20 0.5(2) . . . . no
C7 C18 C23 C22 -174.11(14) . . . . no
C19 C18 C23 C22 1.6(2) . . . . no
C18 C19 C20 C21 -1.8(2) . . . . no
C19 C20 C21 C22 1.0(2) . . . . no
C20 C21 C22 C23 1.1(3) . . . . no
C21 C22 C23 C18 -2.4(2) . . . . no
C11 C24 C25 C26 -178.82(13) . . . . no
C29 C24 C25 C26 -0.1(2) . . . . no
C11 C24 C29 C28 179.73(13) . . . . no
C25 C24 C29 C28 1.0(2) . . . . no
C24 C25 C26 C27 -0.7(2) . . . . no
C25 C26 C27 C28 0.5(2) . . . . no
C26 C27 C28 C29 0.4(2) . . . . no
C27 C28 C29 C24 -1.1(2) . . . . 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
Ni1 C28 3.7767(16) . 3_655 no
Ni1 C4 3.7558(15) . 2_766 no
S1 O4 3.3572(12) . 1_545 no
S1 C15 3.6479(15) . 1_545 no
S1 O4 3.4352(11) . 3_545 no
O1 O2 2.4252(14) . . no
O1 C20 3.2716(19) . 2_776 no
O1 N1 2.6825(15) . . no
O1 C7 2.9004(16) . . no
O1 O8 3.082(2) . . no
O1 C19 3.3567(18) . 2_776 no
O2 O8 2.891(2) . . no
O2 C11 2.9035(16) . . no
O2 C26 3.2457(19) . 3_645 no
O2 N2 2.6911(15) . . no
O3 C14 3.2528(17) . 4_565 no
O3 C10 3.3176(19) . 2_766 no
O3 O6 2.7021(16) . 2_666 no
O4 O6 2.8269(17) . . no
O4 O5 2.6571(14) . 3_555 no
O6 O7 2.851(2) . 2_666 no
O7 O8 2.776(3) . 2_666 no
O7 O8 2.739(2) . . no
N1 N2 2.7370(16) . . no
N1 C1 2.8989(17) . . no
N1 C10 2.7643(19) . . no
N2 C17 2.9018(18) . . no
N2 C8 2.7914(19) . . no
C1 C19 3.471(2) . 2_776 no
C1 C5 3.525(2) . 2_766 no
C5 C27 3.5610(19) . 4_565 no
C5 C23 3.479(2) . . no
C5 C19 3.369(2) . . no
C8 C23 3.463(2) . . no
C8 C19 3.519(2) . . no
C10 C25 3.280(2) . . no
C13 C29 3.278(2) . . no
C15 C30 3.436(2) . 1_565 no
C17 C26 3.496(2) . 3_645 no
C17 C25 3.583(2) . 3_645 no
C26 C30 3.581(2) . 3_655 no
C27 C30 3.347(2) . 3_655 no
C28 C30 3.596(2) . 3_655 no



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 18/01/17 at 12:24:59
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT H(1,X'S) UNTIL H(8) 
CONT EXTPARAM 
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   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,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   (  23,X'S) H   ( 231,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) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 18/01/17 at 12:24:59
#
#LIST     16                                                                    
DIST 0.83, .02 = H(7) TO O(8) 
DIST 0.83, .02 = H(8) TO O(8) 
ANGLE 109.5 1.0 = H(7) TO O(8) TO H(8) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


#===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_ral1704SNQ
_audit_block_doi                 10.5517/ccdc.csd.cc20999y
_database_code_depnum_ccdc_archive 'CCDC 1855979'
loop_
_audit_author_name
_audit_author_address
'Anthony Willis'
;Australian National University
Australia
;
_audit_update_record             
;
2018-07-16 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_audit_creation_date             17-01-19
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1704SNQ\Tony_ral1704SNQ_da At 11:32 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   14.6486(1)
_cell_length_b                   8.8879(1)
_cell_length_c                   31.2974(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.8126(8)
_cell_angle_gamma                90
_cell_volume                     4072.74(7)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_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 0.0181 0.0091 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'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 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 -3.0029 0.5091 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 0.0492 0.0322 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

# Given Formula = C44 H52 Cl2 N4 Ni1 O4 
# Dc =      1.35 Fooo =   1752.00 Mu =     22.72 M =    830.54
# Found Formula = C44 H52 Cl2 N4 Ni1 O4 
# Dc =      1.35 FOOO =   1752.00 Mu =     22.72 M =    830.54

_chemical_formula_sum            'C44 H52 Cl2 N4 Ni O4'
_chemical_formula_moiety         'C43 H50 N4 Ni O4, C H2 Cl2'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         830.54


_cell_measurement_reflns_used    28937
_cell_measurement_theta_min      4
_cell_measurement_theta_max      74
_cell_measurement_temperature    150

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.018
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_max          0.356

_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1752
_exptl_absorpt_coefficient_mu    2.272

# Sheldrick geometric approximatio 0.84 0.96 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro version 1.171.38.43 (Rigaku Oxford Diffraction, 2016)
(Release 29 April 2016; compiled 27 May 2016,16:53)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_T_max  0.96
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
#_diffrn_ambient_temperature 150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_measurement_method       'ω scans'


# If a reference occurs more than once, delete the author 
# and date from subsequent references. 

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'

_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    'PLATON (Spek, 2008)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            61919
_reflns_number_total             8211
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0481

# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8211 
# Theoretical number of reflections is about 16486 


_diffrn_reflns_theta_min         3.018
_diffrn_reflns_theta_max         73.799
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        73.799
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_reflns_limit_h_min              -18
_reflns_limit_h_max              18
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              38

_oxford_diffrn_Wilson_B_factor   2.14
_oxford_diffrn_Wilson_scale      0.13

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

_refine_diff_density_min         -1.54
_refine_diff_density_max         0.89


# 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         8211
_refine_ls_number_restraints     0
_refine_ls_number_parameters     496
_oxford_refine_ls_R_factor_ref   0.0556
_refine_ls_wR_factor_ref         0.1397
_refine_ls_goodness_of_fit_ref   0.9957
_refine_ls_shift/su_max          0.0035838
_refine_ls_shift/su_mean         0.0002933


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8211
_refine_ls_R_factor_all          0.0556
_refine_ls_wR_factor_all         0.1397

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7518
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_gt          0.1360

# 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 #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² + 5.50P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               

The H atoms were all located in a difference map, but 
were repositioned geometrically. 
The H atoms were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98Å) 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
and the displacement parameters were held fixed. 


The largest features in the
final difference electron density map are located 
near the Cl atoms of the solvate and then midway between bonded C atoms.
The former might suggest some disorder of solvate molecules
with the possible presence of acetone or water instead of dichloromethane.
;

# 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 0.55409(2) 0.53788(4) 0.779471(10) 0.0148 1.0000 Uani . . . . . .
Cl1 Cl 0.86133(6) 0.32979(11) 0.70753(3) 0.0613 1.0000 Uani . . . . . .
Cl2 Cl 0.89100(11) 0.63584(12) 0.73663(5) 0.1096 1.0000 Uani . . . . . .
O1 O 0.67027(10) 0.56345(17) 0.80215(4) 0.0210 1.0000 Uani . . . . . .
O2 O 0.60639(10) 0.56183(17) 0.72643(4) 0.0189 1.0000 Uani . . . . . .
O3 O 0.89723(11) 0.6959(2) 0.90767(5) 0.0317 1.0000 Uani . . . . . .
O4 O 0.64423(10) 0.35446(18) 0.58790(4) 0.0229 1.0000 Uani . . . . . .
N1 N 0.50636(12) 0.46696(18) 0.83117(5) 0.0172 1.0000 Uani . . . . . .
N2 N 0.43647(11) 0.56235(19) 0.75537(5) 0.0163 1.0000 Uani . . . . . .
N3 N 1.07377(13) 0.5055(2) 0.88709(6) 0.0276 1.0000 Uani . . . . . .
N4 N 0.79805(12) 0.3800(2) 0.52047(6) 0.0244 1.0000 Uani . . . . . .
C1 C 0.69389(14) 0.5738(2) 0.84273(6) 0.0177 1.0000 Uani . . . . . .
C2 C 0.78239(14) 0.6296(2) 0.85290(7) 0.0215 1.0000 Uani . . . . . .
C3 C 0.81379(15) 0.6409(2) 0.89497(7) 0.0241 1.0000 Uani . . . . . .
C4 C 0.75837(16) 0.5958(3) 0.92853(7) 0.0284 1.0000 Uani . . . . . .
C5 C 0.67305(16) 0.5415(3) 0.91911(7) 0.0252 1.0000 Uani . . . . . .
C6 C 0.63739(14) 0.5292(2) 0.87656(6) 0.0181 1.0000 Uani . . . . . .
C7 C 0.54681(14) 0.4689(2) 0.86897(6) 0.0170 1.0000 Uani . . . . . .
C8 C 0.41573(14) 0.3952(2) 0.82574(6) 0.0206 1.0000 Uani . . . . . .
C9 C 0.34227(15) 0.5141(3) 0.81761(7) 0.0241 1.0000 Uani . . . . . .
C10 C 0.37450(14) 0.6319(2) 0.78604(6) 0.0205 1.0000 Uani . . . . . .
C11 C 0.40909(13) 0.5334(2) 0.71631(6) 0.0161 1.0000 Uani . . . . . .
C12 C 0.47259(13) 0.4833(2) 0.68480(6) 0.0159 1.0000 Uani . . . . . .
C13 C 0.44001(14) 0.4163(2) 0.64627(6) 0.0187 1.0000 Uani . . . . . .
C14 C 0.49777(14) 0.3739(2) 0.61483(6) 0.0201 1.0000 Uani . . . . . .
C15 C 0.59186(14) 0.4021(2) 0.62060(6) 0.0183 1.0000 Uani . . . . . .
C16 C 0.62651(14) 0.4704(2) 0.65743(6) 0.0177 1.0000 Uani . . . . . .
C17 C 0.56829(13) 0.5073(2) 0.69122(6) 0.0161 1.0000 Uani . . . . . .
C18 C 0.96421(16) 0.7193(3) 0.87595(9) 0.0337 1.0000 Uani . . . . . .
C19 C 1.00422(16) 0.5750(3) 0.85896(8) 0.0306 1.0000 Uani . . . . . .
C20 C 1.11792(17) 0.3841(3) 0.86397(9) 0.0379 1.0000 Uani . . . . . .
C21 C 1.19461(19) 0.3133(4) 0.89082(11) 0.0462 1.0000 Uani . . . . . .
C22 C 1.1584(2) 0.2508(3) 0.93204(11) 0.0469 1.0000 Uani . . . . . .
C23 C 1.1070(2) 0.3733(3) 0.95539(9) 0.0407 1.0000 Uani . . . . . .
C24 C 1.03438(18) 0.4457(3) 0.92619(8) 0.0336 1.0000 Uani . . . . . .
C25 C 0.50012(14) 0.4034(2) 0.90685(6) 0.0197 1.0000 Uani . . . . . .
C26 C 0.51826(17) 0.2567(3) 0.91961(7) 0.0284 1.0000 Uani . . . . . .
C27 C 0.47678(19) 0.1969(3) 0.95498(8) 0.0330 1.0000 Uani . . . . . .
C28 C 0.41773(17) 0.2846(3) 0.97830(7) 0.0306 1.0000 Uani . . . . . .
C29 C 0.39930(16) 0.4308(3) 0.96562(7) 0.0286 1.0000 Uani . . . . . .
C30 C 0.43980(15) 0.4910(3) 0.92986(7) 0.0227 1.0000 Uani . . . . . .
C31 C 0.31108(13) 0.5578(2) 0.70307(6) 0.0174 1.0000 Uani . . . . . .
C32 C 0.24361(15) 0.4584(3) 0.71586(7) 0.0244 1.0000 Uani . . . . . .
C33 C 0.15247(16) 0.4890(3) 0.70570(8) 0.0309 1.0000 Uani . . . . . .
C34 C 0.12831(16) 0.6165(3) 0.68257(8) 0.0319 1.0000 Uani . . . . . .
C35 C 0.19526(16) 0.7138(3) 0.66911(7) 0.0283 1.0000 Uani . . . . . .
C36 C 0.28665(15) 0.6851(2) 0.67925(7) 0.0217 1.0000 Uani . . . . . .
C37 C 0.74174(15) 0.3564(3) 0.59466(7) 0.0258 1.0000 Uani . . . . . .
C38 C 0.78678(15) 0.2818(3) 0.55731(7) 0.0257 1.0000 Uani . . . . . .
C39 C 0.71304(18) 0.3986(4) 0.49592(8) 0.0385 1.0000 Uani . . . . . .
C40 C 0.7240(2) 0.5068(4) 0.45870(9) 0.0466 1.0000 Uani . . . . . .
C41 C 0.7990(3) 0.4534(3) 0.43001(9) 0.0535 1.0000 Uani . . . . . .
C42 C 0.8857(3) 0.4316(4) 0.45632(12) 0.0601 1.0000 Uani . . . . . .
C43 C 0.8703(2) 0.3240(4) 0.49350(10) 0.0481 1.0000 Uani . . . . . .
C44 C 0.8274(2) 0.4728(3) 0.74251(9) 0.0413 1.0000 Uani . . . . . .
H21 H 0.8193 0.6596 0.8308 0.0259 1.0000 Uiso R . . . . .
H41 H 0.7803 0.6026 0.9566 0.0346 1.0000 Uiso R . . . . .
H51 H 0.6372 0.5118 0.9415 0.0299 1.0000 Uiso R . . . . .
H81 H 0.4012 0.3347 0.8503 0.0243 1.0000 Uiso R . . . . .
H82 H 0.4182 0.3297 0.8011 0.0248 1.0000 Uiso R . . . . .
H91 H 0.3272 0.5629 0.8443 0.0289 1.0000 Uiso R . . . . .
H92 H 0.2879 0.4646 0.8060 0.0289 1.0000 Uiso R . . . . .
H101 H 0.4097 0.7085 0.8011 0.0239 1.0000 Uiso R . . . . .
H102 H 0.3228 0.6796 0.7715 0.0241 1.0000 Uiso R . . . . .
H131 H 0.3763 0.3975 0.6425 0.0217 1.0000 Uiso R . . . . .
H141 H 0.4759 0.3273 0.5898 0.0246 1.0000 Uiso R . . . . .
H161 H 0.6896 0.4899 0.6607 0.0219 1.0000 Uiso R . . . . .
H181 H 1.0135 0.7783 0.8899 0.0405 1.0000 Uiso R . . . . .
H182 H 0.9379 0.7791 0.8525 0.0397 1.0000 Uiso R . . . . .
H191 H 1.0347 0.6028 0.8326 0.0369 1.0000 Uiso R . . . . .
H192 H 0.9549 0.5025 0.8522 0.0371 1.0000 Uiso R . . . . .
H201 H 1.1422 0.4230 0.8370 0.0449 1.0000 Uiso R . . . . .
H202 H 1.0734 0.3043 0.8569 0.0451 1.0000 Uiso R . . . . .
H211 H 1.2403 0.3902 0.8978 0.0548 1.0000 Uiso R . . . . .
H212 H 1.2238 0.2349 0.8746 0.0557 1.0000 Uiso R . . . . .
H221 H 1.2083 0.2127 0.9509 0.0559 1.0000 Uiso R . . . . .
H222 H 1.1165 0.1684 0.9249 0.0555 1.0000 Uiso R . . . . .
H231 H 1.1491 0.4499 0.9653 0.0492 1.0000 Uiso R . . . . .
H232 H 1.0775 0.3316 0.9799 0.0487 1.0000 Uiso R . . . . .
H241 H 1.0064 0.5305 0.9417 0.0400 1.0000 Uiso R . . . . .
H242 H 0.9870 0.3709 0.9184 0.0400 1.0000 Uiso R . . . . .
H261 H 0.5586 0.1975 0.9044 0.0346 1.0000 Uiso R . . . . .
H271 H 0.4882 0.0974 0.9627 0.0406 1.0000 Uiso R . . . . .
H281 H 0.3916 0.2449 1.0022 0.0371 1.0000 Uiso R . . . . .
H291 H 0.3591 0.4900 0.9813 0.0343 1.0000 Uiso R . . . . .
H301 H 0.4268 0.5881 0.9215 0.0276 1.0000 Uiso R . . . . .
H321 H 0.2595 0.3705 0.7305 0.0294 1.0000 Uiso R . . . . .
H331 H 0.1080 0.4223 0.7144 0.0371 1.0000 Uiso R . . . . .
H341 H 0.0669 0.6373 0.6760 0.0384 1.0000 Uiso R . . . . .
H351 H 0.1783 0.7994 0.6530 0.0346 1.0000 Uiso R . . . . .
H361 H 0.3312 0.7500 0.6700 0.0272 1.0000 Uiso R . . . . .
H371 H 0.7579 0.2999 0.6208 0.0311 1.0000 Uiso R . . . . .
H372 H 0.7621 0.4635 0.5973 0.0296 1.0000 Uiso R . . . . .
H381 H 0.8476 0.2495 0.5676 0.0307 1.0000 Uiso R . . . . .
H382 H 0.7515 0.1931 0.5487 0.0315 1.0000 Uiso R . . . . .
H391 H 0.6661 0.4371 0.5153 0.0464 1.0000 Uiso R . . . . .
H392 H 0.6964 0.2992 0.4844 0.0461 1.0000 Uiso R . . . . .
H401 H 0.7407 0.6072 0.4696 0.0556 1.0000 Uiso R . . . . .
H402 H 0.6668 0.5121 0.4427 0.0568 1.0000 Uiso R . . . . .
H411 H 0.8090 0.5276 0.4074 0.0641 1.0000 Uiso R . . . . .
H412 H 0.7805 0.3570 0.4176 0.0642 1.0000 Uiso R . . . . .
H421 H 0.9055 0.5265 0.4681 0.0715 1.0000 Uiso R . . . . .
H422 H 0.9331 0.3944 0.4390 0.0723 1.0000 Uiso R . . . . .
H431 H 0.9260 0.3133 0.5107 0.0585 1.0000 Uiso R . . . . .
H432 H 0.8539 0.2233 0.4819 0.0582 1.0000 Uiso R . . . . .
H441 H 0.8381 0.4369 0.7717 0.0512 1.0000 Uiso R . . . . .
H442 H 0.7630 0.4962 0.7368 0.0504 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.99(3)
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 . 1.8372(15) yes
Ni1 . O2 . 1.8625(14) yes
Ni1 . N1 . 1.8909(17) yes
Ni1 . N2 . 1.8716(17) yes
Cl1 . C44 . 1.760(3) yes
Cl2 . C44 . 1.736(3) yes
O1 . C1 . 1.309(2) yes
O2 . C17 . 1.312(2) yes
O3 . C3 . 1.364(3) yes
O3 . C18 . 1.433(3) yes
O4 . C15 . 1.365(2) yes
O4 . C37 . 1.437(3) yes
N1 . C7 . 1.306(3) yes
N1 . C8 . 1.478(3) yes
N2 . C10 . 1.477(2) yes
N2 . C11 . 1.300(3) yes
N3 . C19 . 1.462(3) yes
N3 . C20 . 1.461(3) yes
N3 . C24 . 1.469(3) yes
N4 . C38 . 1.459(3) yes
N4 . C39 . 1.452(3) yes
N4 . C43 . 1.462(3) yes
C1 . C2 . 1.415(3) yes
C1 . C6 . 1.421(3) yes
C2 . C3 . 1.385(3) yes
C2 . H21 . 0.930 no
C3 . C4 . 1.406(3) yes
C4 . C5 . 1.363(3) yes
C4 . H41 . 0.927 no
C5 . C6 . 1.419(3) yes
C5 . H51 . 0.927 no
C6 . C7 . 1.444(3) yes
C7 . C25 . 1.505(3) yes
C8 . C9 . 1.524(3) yes
C8 . H81 . 0.967 no
C8 . H82 . 0.967 no
C9 . C10 . 1.525(3) yes
C9 . H91 . 0.974 no
C9 . H92 . 0.970 no
C10 . H101 . 0.966 no
C10 . H102 . 0.969 no
C11 . C12 . 1.447(3) yes
C11 . C31 . 1.497(3) yes
C12 . C13 . 1.414(3) yes
C12 . C17 . 1.426(3) yes
C13 . C14 . 1.371(3) yes
C13 . H131 . 0.952 no
C14 . C15 . 1.407(3) yes
C14 . H141 . 0.933 no
C15 . C16 . 1.385(3) yes
C16 . C17 . 1.418(3) yes
C16 . H161 . 0.942 no
C18 . C19 . 1.514(4) yes
C18 . H181 . 0.984 no
C18 . H182 . 0.976 no
C19 . H191 . 0.983 no
C19 . H192 . 0.986 no
C20 . C21 . 1.518(4) yes
C20 . H201 . 0.988 no
C20 . H202 . 0.984 no
C21 . C22 . 1.516(4) yes
C21 . H211 . 0.976 no
C21 . H212 . 0.970 no
C22 . C23 . 1.523(4) yes
C22 . H221 . 0.985 no
C22 . H222 . 0.977 no
C23 . C24 . 1.523(3) yes
C23 . H231 . 0.963 no
C23 . H232 . 0.966 no
C24 . H241 . 0.992 no
C24 . H242 . 0.986 no
C25 . C26 . 1.388(3) yes
C25 . C30 . 1.395(3) yes
C26 . C27 . 1.385(3) yes
C26 . H261 . 0.933 no
C27 . C28 . 1.389(4) yes
C27 . H271 . 0.931 no
C28 . C29 . 1.382(4) yes
C28 . H281 . 0.922 no
C29 . C30 . 1.390(3) yes
C29 . H291 . 0.941 no
C30 . H301 . 0.921 no
C31 . C32 . 1.394(3) yes
C31 . C36 . 1.395(3) yes
C32 . C33 . 1.390(3) yes
C32 . H321 . 0.932 no
C33 . C34 . 1.384(4) yes
C33 . H331 . 0.928 no
C34 . C35 . 1.383(4) yes
C34 . H341 . 0.935 no
C35 . C36 . 1.390(3) yes
C35 . H351 . 0.941 no
C36 . H361 . 0.925 no
C37 . C38 . 1.513(3) yes
C37 . H371 . 0.983 no
C37 . H372 . 0.999 no
C38 . H381 . 0.980 no
C38 . H382 . 0.976 no
C39 . C40 . 1.522(4) yes
C39 . H391 . 0.992 no
C39 . H392 . 0.981 no
C40 . C41 . 1.517(4) yes
C40 . H401 . 0.984 no
C40 . H402 . 0.964 no
C41 . C42 . 1.504(6) yes
C41 . H411 . 0.982 no
C41 . H412 . 0.976 no
C42 . C43 . 1.528(4) yes
C42 . H421 . 0.961 no
C42 . H422 . 0.954 no
C43 . H431 . 0.968 no
C43 . H432 . 0.993 no
C44 . H441 . 0.976 no
C44 . H442 . 0.976 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 . 85.87(6) yes
O1 . Ni1 . N1 . 94.23(7) yes
O2 . Ni1 . N1 . 167.03(7) yes
O1 . Ni1 . N2 . 166.18(7) yes
O2 . Ni1 . N2 . 91.54(7) yes
N1 . Ni1 . N2 . 91.31(7) yes
Ni1 . O1 . C1 . 126.63(13) yes
Ni1 . O2 . C17 . 122.02(13) yes
C3 . O3 . C18 . 118.50(18) yes
C15 . O4 . C37 . 117.73(16) yes
Ni1 . N1 . C7 . 126.95(14) yes
Ni1 . N1 . C8 . 113.62(13) yes
C7 . N1 . C8 . 119.33(17) yes
Ni1 . N2 . C10 . 111.32(12) yes
Ni1 . N2 . C11 . 127.49(14) yes
C10 . N2 . C11 . 121.07(17) yes
C19 . N3 . C20 . 109.0(2) yes
C19 . N3 . C24 . 111.70(18) yes
C20 . N3 . C24 . 109.7(2) yes
C38 . N4 . C39 . 111.70(18) yes
C38 . N4 . C43 . 110.79(19) yes
C39 . N4 . C43 . 111.0(2) yes
O1 . C1 . C2 . 117.06(18) yes
O1 . C1 . C6 . 124.14(18) yes
C2 . C1 . C6 . 118.78(18) yes
C1 . C2 . C3 . 120.9(2) yes
C1 . C2 . H21 . 119.0 no
C3 . C2 . H21 . 120.1 no
C2 . C3 . O3 . 124.8(2) yes
C2 . C3 . C4 . 120.5(2) yes
O3 . C3 . C4 . 114.69(19) yes
C3 . C4 . C5 . 119.1(2) yes
C3 . C4 . H41 . 119.9 no
C5 . C4 . H41 . 121.0 no
C4 . C5 . C6 . 122.5(2) yes
C4 . C5 . H51 . 118.3 no
C6 . C5 . H51 . 119.1 no
C1 . C6 . C5 . 118.17(19) yes
C1 . C6 . C7 . 122.34(18) yes
C5 . C6 . C7 . 119.47(19) yes
C6 . C7 . N1 . 122.82(18) yes
C6 . C7 . C25 . 116.89(17) yes
N1 . C7 . C25 . 120.27(18) yes
N1 . C8 . C9 . 110.30(17) yes
N1 . C8 . H81 . 111.6 no
C9 . C8 . H81 . 110.2 no
N1 . C8 . H82 . 107.2 no
C9 . C8 . H82 . 109.2 no
H81 . C8 . H82 . 108.3 no
C8 . C9 . C10 . 110.67(17) yes
C8 . C9 . H91 . 110.1 no
C10 . C9 . H91 . 109.5 no
C8 . C9 . H92 . 108.4 no
C10 . C9 . H92 . 109.7 no
H91 . C9 . H92 . 108.4 no
C9 . C10 . N2 . 110.04(17) yes
C9 . C10 . H101 . 109.8 no
N2 . C10 . H101 . 106.4 no
C9 . C10 . H102 . 110.6 no
N2 . C10 . H102 . 111.4 no
H101 . C10 . H102 . 108.5 no
N2 . C11 . C12 . 121.05(18) yes
N2 . C11 . C31 . 119.74(17) yes
C12 . C11 . C31 . 119.17(17) yes
C11 . C12 . C13 . 120.26(18) yes
C11 . C12 . C17 . 120.55(17) yes
C13 . C12 . C17 . 119.12(18) yes
C12 . C13 . C14 . 121.91(19) yes
C12 . C13 . H131 . 118.8 no
C14 . C13 . H131 . 119.3 no
C13 . C14 . C15 . 118.92(18) yes
C13 . C14 . H141 . 121.4 no
C15 . C14 . H141 . 119.7 no
C14 . C15 . O4 . 114.84(17) yes
C14 . C15 . C16 . 121.10(18) yes
O4 . C15 . C16 . 124.04(18) yes
C15 . C16 . C17 . 120.59(18) yes
C15 . C16 . H161 . 120.2 no
C17 . C16 . H161 . 119.2 no
C12 . C17 . C16 . 118.19(18) yes
C12 . C17 . O2 . 124.30(18) yes
C16 . C17 . O2 . 117.51(18) yes
O3 . C18 . C19 . 113.7(2) yes
O3 . C18 . H181 . 106.2 no
C19 . C18 . H181 . 108.7 no
O3 . C18 . H182 . 109.8 no
C19 . C18 . H182 . 110.2 no
H181 . C18 . H182 . 108.1 no
C18 . C19 . N3 . 114.6(2) yes
C18 . C19 . H191 . 105.9 no
N3 . C19 . H191 . 106.6 no
C18 . C19 . H192 . 109.9 no
N3 . C19 . H192 . 110.2 no
H191 . C19 . H192 . 109.4 no
N3 . C20 . C21 . 111.3(2) yes
N3 . C20 . H201 . 110.0 no
C21 . C20 . H201 . 109.8 no
N3 . C20 . H202 . 110.0 no
C21 . C20 . H202 . 107.4 no
H201 . C20 . H202 . 108.3 no
C20 . C21 . C22 . 110.5(2) yes
C20 . C21 . H211 . 108.8 no
C22 . C21 . H211 . 108.8 no
C20 . C21 . H212 . 109.7 no
C22 . C21 . H212 . 110.8 no
H211 . C21 . H212 . 108.1 no
C21 . C22 . C23 . 109.8(2) yes
C21 . C22 . H221 . 111.3 no
C23 . C22 . H221 . 109.0 no
C21 . C22 . H222 . 108.3 no
C23 . C22 . H222 . 109.2 no
H221 . C22 . H222 . 109.2 no
C22 . C23 . C24 . 111.1(2) yes
C22 . C23 . H231 . 109.8 no
C24 . C23 . H231 . 108.8 no
C22 . C23 . H232 . 110.3 no
C24 . C23 . H232 . 108.5 no
H231 . C23 . H232 . 108.3 no
C23 . C24 . N3 . 111.6(2) yes
C23 . C24 . H241 . 108.6 no
N3 . C24 . H241 . 108.2 no
C23 . C24 . H242 . 109.6 no
N3 . C24 . H242 . 109.2 no
H241 . C24 . H242 . 109.6 no
C7 . C25 . C26 . 120.17(19) yes
C7 . C25 . C30 . 120.16(19) yes
C26 . C25 . C30 . 119.66(19) yes
C25 . C26 . C27 . 120.4(2) yes
C25 . C26 . H261 . 120.1 no
C27 . C26 . H261 . 119.5 no
C26 . C27 . C28 . 120.0(2) yes
C26 . C27 . H271 . 119.5 no
C28 . C27 . H271 . 120.5 no
C27 . C28 . C29 . 119.7(2) yes
C27 . C28 . H281 . 119.5 no
C29 . C28 . H281 . 120.7 no
C28 . C29 . C30 . 120.6(2) yes
C28 . C29 . H291 . 119.7 no
C30 . C29 . H291 . 119.7 no
C25 . C30 . C29 . 119.6(2) yes
C25 . C30 . H301 . 120.3 no
C29 . C30 . H301 . 120.1 no
C11 . C31 . C32 . 120.74(18) yes
C11 . C31 . C36 . 119.51(18) yes
C32 . C31 . C36 . 119.68(19) yes
C31 . C32 . C33 . 119.6(2) yes
C31 . C32 . H321 . 120.3 no
C33 . C32 . H321 . 120.1 no
C32 . C33 . C34 . 120.5(2) yes
C32 . C33 . H331 . 119.0 no
C34 . C33 . H331 . 120.4 no
C33 . C34 . C35 . 119.9(2) yes
C33 . C34 . H341 . 120.3 no
C35 . C34 . H341 . 119.8 no
C34 . C35 . C36 . 120.2(2) yes
C34 . C35 . H351 . 119.3 no
C36 . C35 . H351 . 120.5 no
C31 . C36 . C35 . 120.0(2) yes
C31 . C36 . H361 . 120.2 no
C35 . C36 . H361 . 119.8 no
O4 . C37 . C38 . 109.66(17) yes
O4 . C37 . H371 . 109.2 no
C38 . C37 . H371 . 108.7 no
O4 . C37 . H372 . 108.4 no
C38 . C37 . H372 . 110.2 no
H371 . C37 . H372 . 110.7 no
C37 . C38 . N4 . 114.27(19) yes
C37 . C38 . H381 . 106.7 no
N4 . C38 . H381 . 108.1 no
C37 . C38 . H382 . 109.1 no
N4 . C38 . H382 . 109.7 no
H381 . C38 . H382 . 108.8 no
N4 . C39 . C40 . 111.6(2) yes
N4 . C39 . H391 . 108.3 no
C40 . C39 . H391 . 110.1 no
N4 . C39 . H392 . 106.9 no
C40 . C39 . H392 . 108.6 no
H391 . C39 . H392 . 111.4 no
C39 . C40 . C41 . 110.6(3) yes
C39 . C40 . H401 . 109.8 no
C41 . C40 . H401 . 108.2 no
C39 . C40 . H402 . 108.5 no
C41 . C40 . H402 . 110.0 no
H401 . C40 . H402 . 109.8 no
C40 . C41 . C42 . 109.3(2) yes
C40 . C41 . H411 . 110.1 no
C42 . C41 . H411 . 109.8 no
C40 . C41 . H412 . 108.2 no
C42 . C41 . H412 . 109.0 no
H411 . C41 . H412 . 110.4 no
C41 . C42 . C43 . 110.8(3) yes
C41 . C42 . H421 . 109.6 no
C43 . C42 . H421 . 107.9 no
C41 . C42 . H422 . 110.6 no
C43 . C42 . H422 . 110.1 no
H421 . C42 . H422 . 107.8 no
C42 . C43 . N4 . 110.7(2) yes
C42 . C43 . H431 . 110.1 no
N4 . C43 . H431 . 108.9 no
C42 . C43 . H432 . 109.1 no
N4 . C43 . H432 . 110.3 no
H431 . C43 . H432 . 107.7 no
Cl1 . C44 . Cl2 . 111.95(16) yes
Cl1 . C44 . H441 . 107.8 no
Cl2 . C44 . H441 . 107.6 no
Cl1 . C44 . H442 . 109.3 no
Cl2 . C44 . H442 . 108.8 no
H441 . C44 . H442 . 111.5 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C1 174.14(16) . . . . no
N1 Ni1 O1 C1 -18.87(16) . . . . no
O1 Ni1 O2 C17 156.00(15) . . . . no
N2 Ni1 O2 C17 -37.60(15) . . . . no
O1 Ni1 N1 C7 10.41(17) . . . . no
O1 Ni1 N1 C8 -165.87(13) . . . . no
N2 Ni1 N1 C7 -156.92(17) . . . . no
N2 Ni1 N1 C8 26.80(13) . . . . no
O2 Ni1 N2 C10 -149.22(13) . . . . no
O2 Ni1 N2 C11 26.72(17) . . . . no
N1 Ni1 N2 C10 43.44(13) . . . . no
N1 Ni1 N2 C11 -140.62(17) . . . . no
Ni1 O1 C1 C2 -164.85(13) . . . . no
Ni1 O1 C1 C6 16.8(3) . . . . no
Ni1 O2 C17 C12 27.6(2) . . . . no
Ni1 O2 C17 C16 -152.59(13) . . . . no
C18 O3 C3 C2 -11.7(3) . . . . no
C18 O3 C3 C4 169.0(2) . . . . no
C3 O3 C18 C19 -72.3(3) . . . . no
C37 O4 C15 C14 -169.76(18) . . . . no
C37 O4 C15 C16 8.9(3) . . . . no
C15 O4 C37 C38 172.88(18) . . . . no
Ni1 N1 C7 C6 0.4(3) . . . . no
Ni1 N1 C7 C25 -178.17(13) . . . . no
C8 N1 C7 C6 176.49(17) . . . . no
C8 N1 C7 C25 -2.1(3) . . . . no
Ni1 N1 C8 C9 -74.15(17) . . . . no
C7 N1 C8 C9 109.3(2) . . . . no
Ni1 N2 C10 C9 -79.09(17) . . . . no
C11 N2 C10 C9 104.7(2) . . . . no
Ni1 N2 C11 C12 -3.5(3) . . . . no
Ni1 N2 C11 C31 178.87(13) . . . . no
C10 N2 C11 C12 172.04(16) . . . . no
C10 N2 C11 C31 -5.5(3) . . . . no
C20 N3 C19 C18 -170.0(2) . . . . no
C24 N3 C19 C18 68.7(3) . . . . no
C19 N3 C20 C21 176.8(2) . . . . no
C24 N3 C20 C21 -60.6(3) . . . . no
C19 N3 C24 C23 180.0(2) . . . . no
C20 N3 C24 C23 59.1(3) . . . . no
C39 N4 C38 C37 -77.7(3) . . . . no
C43 N4 C38 C37 158.1(2) . . . . no
C38 N4 C39 C40 177.4(2) . . . . no
C43 N4 C39 C40 -58.5(3) . . . . no
C38 N4 C43 C42 -176.8(2) . . . . no
C39 N4 C43 C42 58.5(3) . . . . no
O1 C1 C2 C3 -178.45(17) . . . . no
C6 C1 C2 C3 0.0(3) . . . . no
O1 C1 C6 C5 177.69(19) . . . . no
O1 C1 C6 C7 -0.7(3) . . . . no
C2 C1 C6 C5 -0.6(3) . . . . no
C2 C1 C6 C7 -179.01(17) . . . . no
C1 C2 C3 O3 -178.70(18) . . . . no
C1 C2 C3 C4 0.5(3) . . . . no
O3 C3 C4 C5 179.0(2) . . . . no
C2 C3 C4 C5 -0.4(3) . . . . no
C3 C4 C5 C6 -0.3(4) . . . . no
C4 C5 C6 C1 0.8(3) . . . . no
C4 C5 C6 C7 179.3(2) . . . . no
C1 C6 C7 N1 -8.1(3) . . . . no
C1 C6 C7 C25 170.55(17) . . . . no
C5 C6 C7 N1 173.6(2) . . . . no
C5 C6 C7 C25 -7.8(3) . . . . no
N1 C7 C25 C26 95.6(2) . . . . no
N1 C7 C25 C30 -85.8(2) . . . . no
C6 C7 C25 C26 -83.1(2) . . . . no
C6 C7 C25 C30 95.6(2) . . . . no
N1 C8 C9 C10 43.2(2) . . . . no
C8 C9 C10 N2 31.7(2) . . . . no
N2 C11 C12 C13 163.87(18) . . . . no
N2 C11 C12 C17 -19.2(3) . . . . no
C31 C11 C12 C13 -18.5(3) . . . . no
C31 C11 C12 C17 158.43(17) . . . . no
N2 C11 C31 C32 -74.6(2) . . . . no
N2 C11 C31 C36 102.5(2) . . . . no
C12 C11 C31 C32 107.7(2) . . . . no
C12 C11 C31 C36 -75.1(2) . . . . no
C11 C12 C13 C14 176.89(17) . . . . no
C17 C12 C13 C14 -0.1(3) . . . . no
C11 C12 C17 O2 6.4(3) . . . . no
C11 C12 C17 C16 -173.48(17) . . . . no
C13 C12 C17 O2 -176.65(17) . . . . no
C13 C12 C17 C16 3.5(3) . . . . no
C12 C13 C14 C15 -1.9(3) . . . . no
C13 C14 C15 O4 179.25(16) . . . . no
C13 C14 C15 C16 0.5(3) . . . . no
O4 C15 C16 C17 -175.63(17) . . . . no
C14 C15 C16 C17 3.0(3) . . . . no
C15 C16 C17 O2 175.20(17) . . . . no
C15 C16 C17 C12 -5.0(3) . . . . no
O3 C18 C19 N3 -78.5(3) . . . . no
N3 C20 C21 C22 58.9(3) . . . . no
C20 C21 C22 C23 -54.1(3) . . . . no
C21 C22 C23 C24 52.8(3) . . . . no
C22 C23 C24 N3 -55.9(3) . . . . no
C7 C25 C26 C27 178.7(2) . . . . no
C30 C25 C26 C27 0.1(3) . . . . no
C7 C25 C30 C29 -178.0(2) . . . . no
C26 C25 C30 C29 0.7(3) . . . . no
C25 C26 C27 C28 -1.0(4) . . . . no
C26 C27 C28 C29 1.2(4) . . . . no
C27 C28 C29 C30 -0.4(4) . . . . no
C28 C29 C30 C25 -0.6(3) . . . . no
C11 C31 C32 C33 175.5(2) . . . . no
C36 C31 C32 C33 -1.6(3) . . . . no
C11 C31 C36 C35 -175.93(19) . . . . no
C32 C31 C36 C35 1.3(3) . . . . no
C31 C32 C33 C34 0.7(4) . . . . no
C32 C33 C34 C35 0.5(4) . . . . no
C33 C34 C35 C36 -0.9(4) . . . . no
C34 C35 C36 C31 0.0(3) . . . . no
O4 C37 C38 N4 82.6(2) . . . . no
N4 C39 C40 C41 56.8(3) . . . . no
C39 C40 C41 C42 -54.9(3) . . . . no
C40 C41 C42 C43 55.5(3) . . . . no
C41 C42 C43 N4 -57.7(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
O1 O2 2.5203(18) . . no
O1 C7 2.931(2) . . no
O1 C44 3.115(3) . . no
O1 N1 2.732(2) . . no
O2 C44 3.355(3) . . no
O2 C11 2.909(2) . . no
O2 N2 2.676(2) . . no
O2 C8 3.394(2) . 3_656 no
O3 N3 3.174(2) . . no
O3 C24 3.040(3) . . no
O4 C39 3.105(3) . . no
O4 N4 3.144(2) . . no
N1 C10 2.775(3) . . no
N1 N2 2.691(2) . . no
N1 C1 2.918(3) . . no
N2 C8 2.682(2) . . no
N2 C17 2.871(2) . . no
C1 C36 3.536(3) . 3_646 no
C2 C19 3.285(3) . . no
C5 C30 3.473(3) . . no
C5 C26 3.399(4) . . no
C8 C30 3.376(3) . . no
C8 C26 3.482(3) . . no
C8 C17 3.497(3) . 3_646 no
C9 C32 3.491(3) . . no
C10 C16 3.491(3) . 3_656 no
C10 C36 3.575(3) . . no
C10 C32 3.258(3) . . no
C10 C17 3.508(3) . 3_656 no
C13 C36 3.459(3) . . no
C14 C26 3.574(3) . 3_656 no
C35 C41 3.443(4) . 2_666 no




_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/01/17 at 12:21:12
#
#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   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,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) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,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   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/01/17 at 12:21:12
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


#===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_ral1709ASNQ
_audit_block_doi                 10.5517/ccdc.csd.cc20997w
_database_code_depnum_ccdc_archive 'CCDC 1855977'
loop_
_audit_author_name
_audit_author_address
'Anthony Willis'
;Australian National University
Australia
;
_audit_update_record             
;
2018-07-16 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_audit_creation_date             17-02-15
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1709ASNQ\Tony_ral1709ASNQ_ At 11:44 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.9443(2)
_cell_length_b                   10.8213(2)
_cell_length_c                   15.0907(3)
_cell_angle_alpha                90.9180(16)
_cell_angle_beta                 95.2472(16)
_cell_angle_gamma                94.9377(15)
_cell_volume                     1610.64(5)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

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 0.0181 0.0091 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 0.0311 0.0180 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 -3.0029 0.5091 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 0.0492 0.0322 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 0.3331 0.5567 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            2

# Given Formula = C33 H38 N2 Ni1 O7 S1 
# Dc =      1.37 Fooo =    732.00 Mu =     18.87 M =    665.45
# Found Formula = C33.00 H38 N2 Ni1 O7 S2 
# Dc =      1.44 FOOO =    732.00 Mu =     25.04 M =    697.52

_chemical_formula_sum            'C33 H38 N2 Ni O7 S2'
_chemical_formula_moiety         ' C29 H24 N2 Ni O4, 2(C2 H6 O S), H2 O '
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         697.52


_cell_measurement_reflns_used    21373
_cell_measurement_theta_min      3
_cell_measurement_theta_max      74
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.065
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_max          0.292

_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             732.000
_exptl_absorpt_coefficient_mu    2.504

# Sheldrick geometric approximatio 0.76 0.85 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro version 1.171.38.43 (Rigaku Oxford Diffraction, 2016)
(Release 29 April 2016; compiled 27 May 2016,16:53)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.85
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
#_diffrn_ambient_temperature 150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_measurement_method       'ω scans'


# If a reference occurs more than once, delete the author 
# and date from subsequent references. 

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'

_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    'PLATON (Spek, 2008)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            32422
_reflns_number_total             6529
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.0233
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6529 
# Theoretical number of reflections is about 13048 


_diffrn_reflns_theta_min         2.941
_diffrn_reflns_theta_max         73.838
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        73.838
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -13
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_oxford_diffrn_Wilson_B_factor   2.15
_oxford_diffrn_Wilson_scale      0.07

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

_refine_diff_density_min         -0.92
_refine_diff_density_max         1.07


# 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         6529
_refine_ls_number_restraints     33
_refine_ls_number_parameters     451
_oxford_refine_ls_R_factor_ref   0.0388
_refine_ls_wR_factor_ref         0.0970
_refine_ls_goodness_of_fit_ref   1.0076
_refine_ls_shift/su_max          0.0025843
_refine_ls_shift/su_mean         0.0001025


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6529
_refine_ls_R_factor_all          0.0388
_refine_ls_wR_factor_all         0.0970

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6390
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_gt          0.0967

# 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    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 + 1.82P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               
There is disorder in the packing of the [Ni(C₂₉H₂₄N₂O₄)] molecule so
the methyl group appears to be attached to either C8 or C9.
Two sites were used for each of C8, C9 and C23 (the corresponding sites being
named C98, C99 and C923).
Methyl C23 is bonded to C8, whereas C923 is bonded to C99.  
The relative occupancies of these sites were refined appropriately.
Restraints were imposed so corresponding bond lengths should tend
to be equal and so adjacent sites would have similar displacement parameters
to each other.
 
A subsequent difference electron map showed a peak close to S1
which suggested that this dimethylsulfoxide molecule was disordered
to a small extent, with the 2 C atoms and O atom being common to each
orientation, but with S atom sites on each side of the plane
described by those atoms.  This additional S site was included with 
an isotropic displacement parameter 
and the relative occupancies of the S sites were refined.  Restraints were 
applied so S---X distances for the minor S site 
would tend towards expected values.





H atoms away from the disorder were observed in a difference map 
and those bonded to C were positioned geometrically. 
The H atoms away from the disorder
were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98Å, O---H = 0.83Å) 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
and the displacement parameters were held fixed. 
Finally the positions of the H atoms bonded to O were allowed 
to refine with distance restraints.
H atoms of the disordered atoms were maintained at calculated positions
 and ride on the C atom sites to which they are respectively bonded.

 
The largest features in the
final difference electron density map are located 
near the Ni atom and within the disordered parts of the structure.
;

# 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 0.23869(3) 0.41803(3) 0.451053(19) 0.0228 1.0000 Uani . . . . . .
S1 S 0.60246(6) 0.08492(5) 0.10390(3) 0.0309 0.950(2) Uani . . P . . .
S2 S 0.04316(6) 0.21927(5) 0.02367(3) 0.0340 1.0000 Uani . . . . . .
O1 O 0.27331(14) 0.36482(11) 0.33940(8) 0.0255 1.0000 Uani . . . . . .
O2 O 0.20840(17) 0.25235(12) 0.46984(9) 0.0337 1.0000 Uani . . . . . .
O3 O 0.41626(14) 0.37298(12) 0.04977(8) 0.0259 1.0000 Uani D . . . . .
O4 O 0.11686(15) -0.12344(12) 0.60813(9) 0.0286 1.0000 Uani D . . . . .
O5 O 0.4773(2) 0.13839(15) 0.06264(11) 0.0489 1.0000 Uani D . . . . .
O6 O 0.01433(19) 0.13257(15) 0.09792(10) 0.0446 1.0000 Uani . . . . . .
O7 O 0.03695(17) 0.21510(15) 0.27390(10) 0.0361 1.0000 Uani D . . . . .
N1 N 0.2746(2) 0.58520(15) 0.42855(11) 0.0352 1.0000 Uani D . . . . .
N2 N 0.2017(2) 0.46691(14) 0.56396(11) 0.0316 1.0000 Uani D . . . . .
C1 C 0.31532(17) 0.43255(16) 0.27439(11) 0.0192 1.0000 Uani . . . . . .
C2 C 0.34339(18) 0.36865(16) 0.19699(11) 0.0202 1.0000 Uani . . . . . .
C3 C 0.38345(17) 0.43182(16) 0.12379(11) 0.0200 1.0000 Uani . . . . . .
C4 C 0.39225(19) 0.56216(17) 0.12387(12) 0.0235 1.0000 Uani . . . . . .
C5 C 0.36875(18) 0.62532(16) 0.19971(12) 0.0217 1.0000 Uani . . . . . .
C6 C 0.33240(17) 0.56449(16) 0.27759(11) 0.0185 1.0000 Uani . . . . . .
C7 C 0.31303(19) 0.63662(16) 0.35653(12) 0.0228 1.0000 Uani . . . . . .
C8 C 0.2878(5) 0.6606(3) 0.5163(2) 0.0257 0.571(8) Uani D U P . . .
C9 C 0.1769(6) 0.6015(4) 0.5669(3) 0.0334 0.571(8) Uani D U P . . .
C10 C 0.17800(19) 0.39650(17) 0.63128(11) 0.0223 1.0000 Uani . . . . . .
C11 C 0.16539(17) 0.26297(16) 0.62436(11) 0.0194 1.0000 Uani . . . . . .
C12 C 0.13437(18) 0.19159(17) 0.69895(11) 0.0215 1.0000 Uani . . . . . .
C13 C 0.11698(18) 0.06491(17) 0.69573(12) 0.0227 1.0000 Uani . . . . . .
C14 C 0.13068(18) 0.00186(16) 0.61500(12) 0.0214 1.0000 Uani . . . . . .
C15 C 0.1619(2) 0.06742(17) 0.54114(12) 0.0244 1.0000 Uani . . . . . .
C16 C 0.17967(19) 0.19791(17) 0.54322(11) 0.0226 1.0000 Uani . . . . . .
C17 C 0.3363(2) 0.77534(16) 0.35316(12) 0.0236 1.0000 Uani . . . . . .
C18 C 0.2315(2) 0.84288(18) 0.32077(15) 0.0311 1.0000 Uani . . . . . .
C19 C 0.2487(2) 0.97165(19) 0.32050(15) 0.0335 1.0000 Uani . . . . . .
C20 C 0.3712(2) 1.03324(17) 0.35320(13) 0.0321 1.0000 Uani . . . . . .
C21 C 0.4771(2) 0.96627(19) 0.38429(14) 0.0342 1.0000 Uani . . . . . .
C22 C 0.4607(2) 0.83734(18) 0.38375(13) 0.0307 1.0000 Uani . . . . . .
C23 C 0.4237(5) 0.6589(5) 0.5686(4) 0.0386 0.571(8) Uani D U P . . .
C24 C 0.16144(19) 0.45139(16) 0.72131(11) 0.0212 1.0000 Uani . . . . . .
C25 C 0.27135(19) 0.46011(18) 0.78571(12) 0.0262 1.0000 Uani . . . . . .
C26 C 0.2545(2) 0.49485(18) 0.87277(12) 0.0275 1.0000 Uani . . . . . .
C27 C 0.1279(2) 0.52098(17) 0.89548(12) 0.0265 1.0000 Uani . . . . . .
C28 C 0.0187(2) 0.51487(19) 0.83107(13) 0.0300 1.0000 Uani . . . . . .
C29 C 0.0357(2) 0.48011(18) 0.74405(12) 0.0280 1.0000 Uani . . . . . .
C30 C 0.6526(3) 0.1745(2) 0.20383(17) 0.0474 1.0000 Uani D . . . . .
C31 C 0.5431(3) -0.0553(2) 0.15189(15) 0.0400 1.0000 Uani D . . . . .
C32 C 0.1618(2) 0.1500(2) -0.03876(15) 0.0379 1.0000 Uani . . . . . .
C33 C -0.0996(3) 0.1952(3) -0.05751(18) 0.0503 1.0000 Uani . . . . . .
C98 C 0.2014(7) 0.6615(4) 0.4920(3) 0.0307 0.429(8) Uani D U P . . .
C99 C 0.2466(7) 0.6038(5) 0.5793(3) 0.0276 0.429(8) Uani D U P . . .
C923 C 0.3938(6) 0.6312(6) 0.6064(5) 0.0390 0.429(8) Uani D U P . . .
S91 S 0.5225(9) 0.1140(8) 0.1591(6) 0.032(3) 0.050(2) Uiso D . P . . .
H1 H 0.427(3) 0.3015(16) 0.0595(18) 0.0398 1.0000 Uiso D . . . . .
H2 H 0.070(2) -0.152(2) 0.6470(15) 0.0422 1.0000 Uiso D . . . . .
H3 H 0.039(3) 0.198(3) 0.2224(12) 0.0543 1.0000 Uiso D . . . . .
H4 H 0.110(2) 0.250(3) 0.293(2) 0.0544 1.0000 Uiso D . . . . .
H21 H 0.3351 0.2814 0.1961 0.0237 1.0000 Uiso R . . . . .
H41 H 0.4159 0.6038 0.0736 0.0281 1.0000 Uiso R . . . . .
H51 H 0.3780 0.7124 0.2009 0.0257 1.0000 Uiso R . . . . .
H81 H 0.2708 0.7440 0.5042 0.0302 0.571 Uiso R . . . . .
H91 H 0.1841 0.6329 0.6265 0.0397 0.571 Uiso R . . . . .
H92 H 0.0901 0.6142 0.5386 0.0397 0.571 Uiso R . . . . .
H121 H 0.1241 0.2333 0.7530 0.0261 1.0000 Uiso R . . . . .
H131 H 0.0947 0.0211 0.7457 0.0270 1.0000 Uiso R . . . . .
H151 H 0.1716 0.0250 0.4878 0.0293 1.0000 Uiso R . . . . .
H181 H 0.1482 0.8024 0.2993 0.0377 1.0000 Uiso R . . . . .
H191 H 0.1772 1.0169 0.2984 0.0404 1.0000 Uiso R . . . . .
H201 H 0.3814 1.1212 0.3548 0.0389 1.0000 Uiso R . . . . .
H211 H 0.5612 1.0064 0.4066 0.0415 1.0000 Uiso R . . . . .
H221 H 0.5334 0.7924 0.4041 0.0370 1.0000 Uiso R . . . . .
H231 H 0.4921 0.6967 0.5354 0.0458 0.571 Uiso R . . . . .
H232 H 0.4234 0.7032 0.6234 0.0458 0.571 Uiso R . . . . .
H233 H 0.4413 0.5755 0.5800 0.0458 0.571 Uiso R . . . . .
H251 H 0.3562 0.4422 0.7709 0.0314 1.0000 Uiso R . . . . .
H261 H 0.3288 0.4999 0.9152 0.0330 1.0000 Uiso R . . . . .
H271 H 0.1164 0.5426 0.9543 0.0320 1.0000 Uiso R . . . . .
H281 H -0.0666 0.5340 0.8463 0.0363 1.0000 Uiso R . . . . .
H291 H -0.0387 0.4748 0.7005 0.0346 1.0000 Uiso R . . . . .
H301 H 0.6840 0.2564 0.1879 0.0711 1.0000 Uiso R . . . . .
H302 H 0.7231 0.1373 0.2382 0.0709 1.0000 Uiso R . . . . .
H303 H 0.5722 0.1769 0.2358 0.0714 1.0000 Uiso R . . . . .
H311 H 0.5118 -0.1144 0.1051 0.0599 1.0000 Uiso R . . . . .
H312 H 0.6149 -0.0860 0.1898 0.0601 1.0000 Uiso R . . . . .
H313 H 0.4694 -0.0384 0.1848 0.0597 1.0000 Uiso R . . . . .
H321 H 0.2425 0.1405 -0.0001 0.0566 1.0000 Uiso R . . . . .
H322 H 0.1841 0.2038 -0.0863 0.0568 1.0000 Uiso R . . . . .
H323 H 0.1242 0.0699 -0.0618 0.0561 1.0000 Uiso R . . . . .
H331 H -0.1777 0.2215 -0.0326 0.0745 1.0000 Uiso R . . . . .
H332 H -0.0824 0.2432 -0.1087 0.0744 1.0000 Uiso R . . . . .
H333 H -0.1160 0.1087 -0.0743 0.0738 1.0000 Uiso R . . . . .
H981 H 0.2310 0.7473 0.4913 0.0364 0.429 Uiso R . . . . .
H982 H 0.1058 0.6507 0.4788 0.0364 0.429 Uiso R . . . . .
H991 H 0.1973 0.6352 0.6244 0.0337 0.429 Uiso R . . . . .
H9231 H 0.4164 0.5929 0.6613 0.0468 0.429 Uiso R . . . . .
H9232 H 0.4146 0.7184 0.6130 0.0468 0.429 Uiso R . . . . .
H9233 H 0.4445 0.5997 0.5620 0.0468 0.429 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.76(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 . 1.8434(12) yes
Ni1 . O2 . 1.8232(13) yes
Ni1 . N1 . 1.8563(17) yes
Ni1 . N2 . 1.8541(16) yes
S1 . O5 . 1.5055(17) yes
S1 . C30 . 1.788(2) yes
S1 . C31 . 1.770(2) yes
S2 . O6 . 1.5047(17) yes
S2 . C32 . 1.781(2) yes
S2 . C33 . 1.787(3) yes
O1 . C1 . 1.311(2) yes
O2 . C16 . 1.306(2) yes
O3 . C3 . 1.356(2) yes
O3 . H1 . 0.803(16) no
O4 . C14 . 1.352(2) yes
O4 . H2 . 0.828(17) no
O5 . S91 . 1.518(9) yes
O7 . H3 . 0.800(17) no
O7 . H4 . 0.811(17) no
N1 . C7 . 1.302(2) yes
N1 . C8 . 1.533(3) yes
N1 . C98 . 1.527(5) yes
N2 . C9 . 1.498(4) yes
N2 . C10 . 1.306(2) yes
N2 . C99 . 1.517(5) yes
C1 . C2 . 1.410(2) yes
C1 . C6 . 1.423(2) yes
C2 . C3 . 1.380(2) yes
C2 . H21 . 0.941 no
C3 . C4 . 1.406(3) yes
C4 . C5 . 1.372(3) yes
C4 . H41 . 0.927 no
C5 . C6 . 1.417(2) yes
C5 . H51 . 0.939 no
C6 . C7 . 1.450(2) yes
C7 . C17 . 1.501(2) yes
C8 . C9 . 1.503(5) yes
C8 . C23 . 1.503(5) yes
C8 . H81 . 0.950 no
C9 . H91 . 0.950 no
C9 . H92 . 0.950 no
C10 . C11 . 1.441(2) yes
C10 . C24 . 1.502(2) yes
C11 . C12 . 1.417(2) yes
C11 . C16 . 1.427(2) yes
C12 . C13 . 1.366(3) yes
C12 . H121 . 0.943 no
C13 . C14 . 1.410(2) yes
C13 . H131 . 0.932 no
C14 . C15 . 1.376(2) yes
C15 . C16 . 1.407(2) yes
C15 . H151 . 0.937 no
C17 . C18 . 1.382(3) yes
C17 . C22 . 1.391(3) yes
C18 . C19 . 1.389(3) yes
C18 . H181 . 0.931 no
C19 . C20 . 1.383(3) yes
C19 . H191 . 0.937 no
C20 . C21 . 1.380(3) yes
C20 . H201 . 0.949 no
C21 . C22 . 1.391(3) yes
C21 . H211 . 0.940 no
C22 . H221 . 0.937 no
C23 . H231 . 0.950 no
C23 . H232 . 0.950 no
C23 . H233 . 0.950 no
C24 . C25 . 1.390(3) yes
C24 . C29 . 1.385(3) yes
C25 . C26 . 1.390(3) yes
C25 . H251 . 0.928 no
C26 . C27 . 1.385(3) yes
C26 . H261 . 0.930 no
C27 . C28 . 1.386(3) yes
C27 . H271 . 0.934 no
C28 . C29 . 1.390(3) yes
C28 . H281 . 0.937 no
C29 . H291 . 0.941 no
C30 . S91 . 1.496(9) yes
C30 . H301 . 0.956 no
C30 . H302 . 0.955 no
C30 . H303 . 0.972 no
C31 . S91 . 1.863(9) yes
C31 . H311 . 0.956 no
C31 . H312 . 0.960 no
C31 . H313 . 0.950 no
C32 . H321 . 0.963 no
C32 . H322 . 0.960 no
C32 . H323 . 0.961 no
C33 . H331 . 0.956 no
C33 . H332 . 0.958 no
C33 . H333 . 0.962 no
C98 . C99 . 1.515(6) yes
C98 . H981 . 0.950 no
C98 . H982 . 0.950 no
C99 . C923 . 1.486(7) yes
C99 . H991 . 0.950 no
C923 . H9231 . 0.950 no
C923 . H9232 . 0.950 no
C923 . H9233 . 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 . 83.37(6) yes
O1 . Ni1 . N1 . 94.55(6) yes
O2 . Ni1 . N1 . 177.62(7) yes
O1 . Ni1 . N2 . 178.33(6) yes
O2 . Ni1 . N2 . 95.00(6) yes
N1 . Ni1 . N2 . 87.09(7) yes
O5 . S1 . C30 . 105.59(11) yes
O5 . S1 . C31 . 105.22(12) yes
C30 . S1 . C31 . 98.82(12) yes
O6 . S2 . C32 . 106.48(11) yes
O6 . S2 . C33 . 106.05(12) yes
C32 . S2 . C33 . 97.20(12) yes
Ni1 . O1 . C1 . 127.74(11) yes
Ni1 . O2 . C16 . 128.11(12) yes
C3 . O3 . H1 . 110.7(19) no
C14 . O4 . H2 . 109.4(19) no
H3 . O7 . H4 . 109(3) no
Ni1 . N1 . C7 . 128.88(13) yes
Ni1 . N1 . C8 . 109.61(15) yes
C7 . N1 . C8 . 120.00(18) yes
Ni1 . N1 . C98 . 108.9(2) yes
C7 . N1 . C98 . 118.6(2) yes
Ni1 . N2 . C9 . 111.0(2) yes
Ni1 . N2 . C10 . 127.80(13) yes
C9 . N2 . C10 . 120.4(2) yes
Ni1 . N2 . C99 . 109.4(2) yes
C10 . N2 . C99 . 120.2(2) yes
O1 . C1 . C2 . 116.87(15) yes
O1 . C1 . C6 . 124.01(15) yes
C2 . C1 . C6 . 119.12(15) yes
C1 . C2 . C3 . 121.19(16) yes
C1 . C2 . H21 . 118.7 no
C3 . C2 . H21 . 120.1 no
C2 . C3 . O3 . 122.51(16) yes
C2 . C3 . C4 . 120.28(16) yes
O3 . C3 . C4 . 117.21(15) yes
C3 . C4 . C5 . 118.93(16) yes
C3 . C4 . H41 . 119.7 no
C5 . C4 . H41 . 121.3 no
C4 . C5 . C6 . 122.69(16) yes
C4 . C5 . H51 . 119.3 no
C6 . C5 . H51 . 118.0 no
C1 . C6 . C5 . 117.59(15) yes
C1 . C6 . C7 . 122.41(15) yes
C5 . C6 . C7 . 120.00(15) yes
C6 . C7 . N1 . 122.27(16) yes
C6 . C7 . C17 . 117.98(15) yes
N1 . C7 . C17 . 119.74(16) yes
N1 . C8 . C9 . 104.0(3) yes
N1 . C8 . C23 . 113.8(3) yes
C9 . C8 . C23 . 111.0(5) yes
N1 . C8 . H81 . 109.3 no
C9 . C8 . H81 . 109.4 no
C23 . C8 . H81 . 109.3 no
C8 . C9 . N2 . 102.7(3) yes
C8 . C9 . H91 . 111.3 no
N2 . C9 . H91 . 111.2 no
C8 . C9 . H92 . 111.1 no
N2 . C9 . H92 . 111.0 no
H91 . C9 . H92 . 109.5 no
N2 . C10 . C11 . 122.76(16) yes
N2 . C10 . C24 . 121.29(16) yes
C11 . C10 . C24 . 115.94(15) yes
C10 . C11 . C12 . 120.13(15) yes
C10 . C11 . C16 . 122.19(15) yes
C12 . C11 . C16 . 117.66(15) yes
C11 . C12 . C13 . 122.84(16) yes
C11 . C12 . H121 . 118.7 no
C13 . C12 . H121 . 118.5 no
C12 . C13 . C14 . 118.90(16) yes
C12 . C13 . H131 . 120.5 no
C14 . C13 . H131 . 120.6 no
C13 . C14 . O4 . 121.60(16) yes
C13 . C14 . C15 . 120.21(16) yes
O4 . C14 . C15 . 118.17(16) yes
C14 . C15 . C16 . 121.62(16) yes
C14 . C15 . H151 . 119.9 no
C16 . C15 . H151 . 118.5 no
C11 . C16 . C15 . 118.77(16) yes
C11 . C16 . O2 . 123.82(16) yes
C15 . C16 . O2 . 117.41(16) yes
C7 . C17 . C18 . 119.41(17) yes
C7 . C17 . C22 . 121.20(17) yes
C18 . C17 . C22 . 119.38(17) yes
C17 . C18 . C19 . 120.49(19) yes
C17 . C18 . H181 . 120.2 no
C19 . C18 . H181 . 119.3 no
C18 . C19 . C20 . 120.0(2) yes
C18 . C19 . H191 . 120.1 no
C20 . C19 . H191 . 119.9 no
C19 . C20 . C21 . 119.76(18) yes
C19 . C20 . H201 . 119.6 no
C21 . C20 . H201 . 120.6 no
C20 . C21 . C22 . 120.38(19) yes
C20 . C21 . H211 . 121.0 no
C22 . C21 . H211 . 118.6 no
C17 . C22 . C21 . 119.92(19) yes
C17 . C22 . H221 . 120.1 no
C21 . C22 . H221 . 119.9 no
C8 . C23 . H231 . 109.5 no
C8 . C23 . H232 . 109.5 no
H231 . C23 . H232 . 109.5 no
C8 . C23 . H233 . 109.4 no
H231 . C23 . H233 . 109.5 no
H232 . C23 . H233 . 109.5 no
C10 . C24 . C25 . 118.89(16) yes
C10 . C24 . C29 . 121.11(16) yes
C25 . C24 . C29 . 119.59(16) yes
C24 . C25 . C26 . 120.15(18) yes
C24 . C25 . H251 . 120.2 no
C26 . C25 . H251 . 119.7 no
C25 . C26 . C27 . 119.97(17) yes
C25 . C26 . H261 . 119.2 no
C27 . C26 . H261 . 120.8 no
C26 . C27 . C28 . 120.05(17) yes
C26 . C27 . H271 . 119.8 no
C28 . C27 . H271 . 120.1 no
C27 . C28 . C29 . 119.89(18) yes
C27 . C28 . H281 . 120.0 no
C29 . C28 . H281 . 120.1 no
C28 . C29 . C24 . 120.32(18) yes
C28 . C29 . H291 . 119.9 no
C24 . C29 . H291 . 119.8 no
S1 . C30 . H301 . 108.3 no
S1 . C30 . H302 . 109.9 no
H301 . C30 . H302 . 110.1 no
S1 . C30 . H303 . 106.7 no
H301 . C30 . H303 . 110.2 no
H302 . C30 . H303 . 111.5 no
S1 . C31 . H311 . 108.7 no
S1 . C31 . H312 . 109.8 no
H311 . C31 . H312 . 110.3 no
S1 . C31 . H313 . 107.8 no
H311 . C31 . H313 . 109.3 no
H312 . C31 . H313 . 110.9 no
S2 . C32 . H321 . 108.6 no
S2 . C32 . H322 . 108.9 no
H321 . C32 . H322 . 109.2 no
S2 . C32 . H323 . 110.1 no
H321 . C32 . H323 . 109.2 no
H322 . C32 . H323 . 110.7 no
S2 . C33 . H331 . 108.9 no
S2 . C33 . H332 . 109.2 no
H331 . C33 . H332 . 109.6 no
S2 . C33 . H333 . 110.3 no
H331 . C33 . H333 . 108.9 no
H332 . C33 . H333 . 109.9 no
N1 . C98 . C99 . 99.6(4) yes
N1 . C98 . H981 . 111.8 no
C99 . C98 . H981 . 111.8 no
N1 . C98 . H982 . 111.9 no
C99 . C98 . H982 . 112.0 no
H981 . C98 . H982 . 109.5 no
N2 . C99 . C98 . 103.7(4) yes
N2 . C99 . C923 . 114.4(5) yes
C98 . C99 . C923 . 113.1(6) yes
N2 . C99 . H991 . 108.5 no
C98 . C99 . H991 . 108.5 no
C923 . C99 . H991 . 108.5 no
C99 . C923 . H9231 . 109.5 no
C99 . C923 . H9232 . 109.5 no
H9231 . C923 . H9232 . 109.5 no
C99 . C923 . H9233 . 109.4 no
H9231 . C923 . H9233 . 109.5 no
H9232 . C923 . H9233 . 109.5 no
C31 . S91 . O5 . 100.4(5) yes
C31 . S91 . C30 . 106.6(5) yes
O5 . S91 . C30 . 121.4(6) yes
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 . H1 . O5 . 168(3) 0.80(2) 1.88(2) 2.666(4) yes
O4 . H2 . O7 2_556 177(3) 0.83(2) 1.78(2) 2.605(4) yes
O7 . H3 . O6 . 169(3) 0.80(2) 1.98(2) 2.771(4) yes
O7 . H4 . O1 . 169(3) 0.81(2) 2.03(2) 2.827(4) yes


loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C1 -175.83(16) . . . . no
N1 Ni1 O1 C1 3.01(16) . . . . no
O1 Ni1 O2 C16 176.56(18) . . . . no
N2 Ni1 O2 C16 -3.81(19) . . . . no
O1 Ni1 N1 C7 -1.1(2) . . . . no
O1 Ni1 N1 C8 -166.9(2) . . . . no
N2 Ni1 N1 C7 179.2(2) . . . . no
N2 Ni1 N1 C8 13.5(2) . . . . no
O2 Ni1 N2 C9 -163.5(3) . . . . no
O2 Ni1 N2 C10 6.4(2) . . . . no
N1 Ni1 N2 C9 17.7(3) . . . . no
N1 Ni1 N2 C10 -172.5(2) . . . . no
Ni1 O1 C1 C2 175.74(12) . . . . no
Ni1 O1 C1 C6 -4.9(3) . . . . no
Ni1 O2 C16 C11 0.7(3) . . . . no
Ni1 O2 C16 C15 -179.40(14) . . . . no
Ni1 N1 C7 C6 1.1(3) . . . . no
Ni1 N1 C7 C17 179.97(15) . . . . no
C8 N1 C7 C6 165.5(3) . . . . no
C8 N1 C7 C17 -15.6(3) . . . . no
Ni1 N1 C8 C9 -40.8(3) . . . . no
Ni1 N1 C8 C23 80.1(3) . . . . no
C7 N1 C8 C9 152.0(3) . . . . no
C7 N1 C8 C23 -87.1(3) . . . . no
Ni1 N2 C9 C8 -43.9(4) . . . . no
C10 N2 C9 C8 145.4(3) . . . . no
Ni1 N2 C10 C11 -5.7(3) . . . . no
Ni1 N2 C10 C24 174.64(14) . . . . no
C9 N2 C10 C11 163.3(3) . . . . no
C9 N2 C10 C24 -16.4(4) . . . . no
O1 C1 C2 C3 177.66(16) . . . . no
C6 C1 C2 C3 -1.8(3) . . . . no
O1 C1 C6 C5 -175.36(16) . . . . no
O1 C1 C6 C7 4.2(3) . . . . no
C2 C1 C6 C5 4.0(2) . . . . no
C2 C1 C6 C7 -176.43(17) . . . . no
C1 C2 C3 O3 177.35(16) . . . . no
C1 C2 C3 C4 -2.4(3) . . . . no
O3 C3 C4 C5 -175.66(16) . . . . no
C2 C3 C4 C5 4.1(3) . . . . no
C3 C4 C5 C6 -1.7(3) . . . . no
C4 C5 C6 C1 -2.4(3) . . . . no
C4 C5 C6 C7 178.09(17) . . . . no
C1 C6 C7 N1 -2.2(3) . . . . no
C1 C6 C7 C17 178.86(16) . . . . no
C5 C6 C7 N1 177.33(18) . . . . no
C5 C6 C7 C17 -1.6(3) . . . . no
N1 C7 C17 C18 -92.4(2) . . . . no
N1 C7 C17 C22 86.3(2) . . . . no
C6 C7 C17 C18 86.5(2) . . . . no
C6 C7 C17 C22 -94.8(2) . . . . no
N1 C8 C9 N2 52.1(4) . . . . no
C23 C8 C9 N2 -70.7(4) . . . . no
N2 C10 C11 C12 -177.53(18) . . . . no
N2 C10 C11 C16 0.8(3) . . . . no
C24 C10 C11 C12 2.1(2) . . . . no
C24 C10 C11 C16 -179.53(17) . . . . no
N2 C10 C24 C25 -98.7(2) . . . . no
N2 C10 C24 C29 88.6(2) . . . . no
C11 C10 C24 C25 81.6(2) . . . . no
C11 C10 C24 C29 -91.1(2) . . . . no
C10 C11 C12 C13 177.91(17) . . . . no
C16 C11 C12 C13 -0.5(3) . . . . no
C10 C11 C16 O2 1.8(3) . . . . no
C10 C11 C16 C15 -178.12(17) . . . . no
C12 C11 C16 O2 -179.81(18) . . . . no
C12 C11 C16 C15 0.3(3) . . . . no
C11 C12 C13 C14 0.2(3) . . . . no
C12 C13 C14 O4 178.89(17) . . . . no
C12 C13 C14 C15 0.4(3) . . . . no
O4 C14 C15 C16 -179.18(17) . . . . no
C13 C14 C15 C16 -0.7(3) . . . . no
C14 C15 C16 O2 -179.63(18) . . . . no
C14 C15 C16 C11 0.3(3) . . . . no
C7 C17 C18 C19 177.23(19) . . . . no
C22 C17 C18 C19 -1.5(3) . . . . no
C7 C17 C22 C21 -176.51(18) . . . . no
C18 C17 C22 C21 2.2(3) . . . . no
C17 C18 C19 C20 -0.3(3) . . . . no
C18 C19 C20 C21 1.4(3) . . . . no
C19 C20 C21 C22 -0.7(3) . . . . no
C20 C21 C22 C17 -1.1(3) . . . . no
C10 C24 C25 C26 -171.43(17) . . . . no
C29 C24 C25 C26 1.4(3) . . . . no
C10 C24 C29 C28 171.27(18) . . . . no
C25 C24 C29 C28 -1.4(3) . . . . no
C24 C25 C26 C27 -0.1(3) . . . . no
C25 C26 C27 C28 -1.3(3) . . . . no
C26 C27 C28 C29 1.3(3) . . . . no
C27 C28 C29 C24 0.1(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
Ni1 O7 3.7505(16) . . no
Ni1 C23 3.565(5) . 2_666 no
Ni1 C923 3.911(6) . 2_666 no
S1 O5 3.4490(17) . 2_655 no
S2 C27 3.657(2) . 2_566 no
S91 C20 3.503(9) . 1_545 no
S91 O3 3.469(9) . . no
S91 C2 3.475(9) . . no
O1 N1 2.718(2) . . no
O1 C23 3.233(5) . 2_666 no
O1 O7 2.828(2) . . no
O1 C923 3.333(6) . 2_666 no
O1 O2 2.4386(18) . . no
O1 C7 2.938(2) . . no
O2 N2 2.711(2) . . no
O2 C10 2.925(2) . . no
O3 O5 2.667(2) . . no
O3 C26 3.340(2) . 1_554 no
O4 O7 2.605(2) . 2_556 no
O4 C9 3.149(5) . 1_545 no
O4 C8 3.359(4) . 1_545 no
O4 C99 3.359(6) . 1_545 no
O4 C98 3.110(5) . 1_545 no
O5 C31 3.330(3) . 2_655 no
O5 C32 3.376(3) . . no
O6 O7 2.771(2) . . no
O7 C13 3.333(2) . 2_556 no
O7 C28 3.409(3) . 2_566 no
O7 C14 3.327(2) . 2_556 no
N1 N2 2.556(2) . . no
N1 C1 2.910(2) . . no
N1 C99 2.325(5) . . no
N1 C9 2.392(5) . . no
N2 C8 2.344(4) . . no
N2 C98 2.385(5) . . no
N2 C16 2.910(2) . . no
C1 C23 3.567(6) . 2_666 no
C1 C923 3.393(7) . 2_666 no
C4 C25 3.525(3) . 2_666 no
C5 C22 3.575(3) . . no
C5 C18 3.408(3) . . no
C8 C22 3.287(4) . . no
C9 C29 3.365(5) . . no
C12 C29 3.429(3) . . no
C12 C25 3.299(3) . . no
C14 C15 3.591(3) . 2_556 no
C15 C15 3.527(3) . 2_556 no
C17 C23 3.566(6) . . no
C18 C98 3.290(5) . . no
C21 C21 3.537(3) . 2_676 no
C22 C23 3.447(6) . . no
C24 C923 3.493(7) . . no
C25 C923 3.551(7) . . no
C25 C99 3.502(5) . . no
C29 C99 3.598(6) . . no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 15/02/17 at 14:24:44
#
#LIST     12                                                                    
BLOCK SCALE X'S, NI(1,U'S) UNTIL C(7) 
CONT C(8,U'S,OCC) UNTIL C(9) 
CONT C(10,U'S) UNTIL C(22)  C(23,U'S,OCC) 
CONT C(24,U'S) UNTIL C(33) C(98,U'S,OCC) UNTIL C(923) 
CONT H(1,X'S) UNTIL H(4) 
CONT S(91,U[ISO],OCC) S(1,OCC) 
EQUIV S(1,OCC) S(91,OCC) 
WEIGHT -1 S(91,OCC) 
EQUIV C(8,OCC) C(9,OCC) C(23,OCC) 
CONT  C(98,OCC) C(99,OCC) C(923,OCC) 
WEIGHT -1  C(98,OCC) C(99,OCC) C(923,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(8,X'S) H(81,X'S) 
RIDE C(9,X'S) H(91,X'S) H(92,X'S) 
RIDE C(23,X'S) H(231,X'S) H(232,X'S) H(233,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 ( 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) 
RIDE C(98,X'S) H(981,X'S) H(982,X'S) 
RIDE C(99,X'S) H(991,X'S) 
RIDE C(923,X'S) H(9231,X'S) H(9232,X'S) H(9233,X'S) 
RIDE C(30,X'S) H(301,X'S) H(302,X'S) H(303,X'S) 
RIDE C(31,X'S) H(311,X'S) H(312,X'S) H(313,X'S) 
RIDE C(32,X'S) H(321,X'S) H(322,X'S) H(323,X'S) 
RIDE C(33,X'S) H(331,X'S) H(332,X'S) H(333,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 15/02/17 at 14:24:44
#
#LIST     16                                                                    
DIST 0.0, .01 = MEAN N(1) TO C(8), N(1) TO C(98) 
DIST 0.0, .01 = MEAN N(2) TO C(9), N(2) TO C(99) 
DIST 0.0, .01 = MEAN C(8) TO C(9), C(98) TO C(99) 
DIST 0.0, .01 = MEAN C(8) TO C(23), C(99) TO C(923) 
REM 
U(IJ) 0.0, .02 = C(8) TO C(98) 
U(IJ) 0.0, .02 = C(9) TO C(99) 
U(IJ) 0.0, .02 = C(23) TO C(923) 
REM 
DIST 0.82, .02 = O(3) TO H(1) 
DIST 0.82, .02 = O(4) TO H(2) 
DIST 0.82, .02 = O(7) TO H(3) 
DIST 0.82, .02 = O(7) TO H(4) 
REM 
DIST 1.50, .02 = S(91) TO O(5) 
DIST 1.78, .02 = S(91) TO C(30), S(91) TO C(31) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


#===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_ral1701ESNQ
_audit_block_doi                 10.5517/ccdc.csd.cc2099bz
_database_code_depnum_ccdc_archive 'CCDC 1855980'
loop_
_audit_author_name
_audit_author_address
'Anthony Willis'
;Australian National University
Australia
;
_audit_update_record             
;
2018-07-16 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_audit_creation_date             17-01-16
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1701ESNQ\Tony_ral1701ESNQ_ At 11:48 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   10.5477(5)
_cell_length_b                   15.4745(6)
_cell_length_c                   16.5986(8)
_cell_angle_alpha                88.093(3)
_cell_angle_beta                 83.802(4)
_cell_angle_gamma                70.576(4)
_cell_volume                     2540.1(2)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

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 0.0181 0.0091 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 0.0311 0.0180 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 -3.0029 0.5091 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 0.0492 0.0322 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            2

# Given Formula = C56 H74 N6 Ni1 O6 
# Dc =      1.29 Fooo =   1056.00 Mu =     10.00 M =    985.95
# Found Formula = C56 H74 N6 Ni1 O6 
# Dc =      1.29 FOOO =   1056.00 Mu =     10.00 M =    985.95

_chemical_formula_sum            'C56 H74 N6 Ni O6'
_chemical_formula_moiety         'C56 H74 N6 Ni O6'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         985.95


_cell_measurement_reflns_used    5970
_cell_measurement_theta_min      3
_cell_measurement_theta_max      73
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.025
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_max          0.298

_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1056
_exptl_absorpt_coefficient_mu    1.000

# Sheldrick geometric approximatio 0.82 0.98 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro version 1.171.38.43 (Rigaku Oxford Diffraction, 2016)
(Release 29 April 2016; compiled 27 May 2016,16:53)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.98
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
#_diffrn_ambient_temperature 150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_measurement_method       'ω scans'


# If a reference occurs more than once, delete the author 
# and date from subsequent references. 

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2016)'

_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    'PLATON (Spek, 2008)'
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            28016
_reflns_number_total             9968
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.0854

# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 9968 
# Theoretical number of reflections is about 20594 


_diffrn_reflns_theta_min         3.028
_diffrn_reflns_theta_max         73.893
_diffrn_measured_fraction_theta_max 0.968

_diffrn_reflns_theta_full        72.699
_diffrn_measured_fraction_theta_full 0.980


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -19
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              20

_oxford_diffrn_Wilson_B_factor   3.49
_oxford_diffrn_Wilson_scale      0.20

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

_refine_diff_density_min         -0.63
_refine_diff_density_max         0.77


# 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         9967
_refine_ls_number_restraints     0
_refine_ls_number_parameters     622
_oxford_refine_ls_R_factor_ref   0.0910
_refine_ls_wR_factor_ref         0.1766
_refine_ls_goodness_of_fit_ref   0.9641
_refine_ls_shift/su_max          0.0021065
_refine_ls_shift/su_mean         0.0003594


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9967
_refine_ls_R_factor_all          0.0910
_refine_ls_wR_factor_all         0.1766

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6999
_refine_ls_R_factor_gt           0.0638
_refine_ls_wR_factor_gt          0.1534

# 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 #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 + 2.40P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               

The H atoms were all located in a difference map, but 
 were repositioned geometrically. 
The H atoms were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98Å) 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
and the displacement parameters were held fixed. 
 

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 0.64393(5) 0.53648(3) 0.54137(3) 0.0388 1.0000 Uani . . . . . .
O1 O 0.6467(2) 0.51260(15) 0.64949(14) 0.0472 1.0000 Uani . . . . . .
O2 O 0.4912(2) 0.63208(14) 0.57319(13) 0.0413 1.0000 Uani . . . . . .
O3 O 0.7959(2) 0.38136(15) 0.89836(14) 0.0505 1.0000 Uani . . . . . .
O4 O 1.3332(2) 0.09313(15) 0.42262(16) 0.0505 1.0000 Uani . . . . . .
O5 O 0.6937(3) 0.69432(18) 0.06692(15) 0.0570 1.0000 Uani . . . . . .
O6 O 0.1508(2) 0.92365(14) 0.57063(15) 0.0462 1.0000 Uani . . . . . .
N1 N 0.8005(3) 0.43974(16) 0.51189(16) 0.0387 1.0000 Uani . . . . . .
N2 N 0.6351(3) 0.56497(16) 0.43254(16) 0.0381 1.0000 Uani . . . . . .
N3 N 0.6690(3) 0.38003(19) 1.07504(18) 0.0491 1.0000 Uani . . . . . .
N4 N 1.6020(3) 0.00762(18) 0.2947(2) 0.0492 1.0000 Uani . . . . . .
N5 N 0.7455(3) 0.6812(2) -0.11857(19) 0.0562 1.0000 Uani . . . . . .
N6 N -0.0408(3) 1.00940(19) 0.7652(2) 0.0526 1.0000 Uani . . . . . .
C1 C 0.7366(3) 0.4489(2) 0.6862(2) 0.0399 1.0000 Uani . . . . . .
C2 C 0.7184(3) 0.4492(2) 0.7714(2) 0.0443 1.0000 Uani . . . . . .
C3 C 0.8064(3) 0.3844(2) 0.8163(2) 0.0425 1.0000 Uani . . . . . .
C4 C 0.9176(3) 0.3160(2) 0.7760(2) 0.0471 1.0000 Uani . . . . . .
C5 C 0.9384(3) 0.3157(2) 0.6943(2) 0.0431 1.0000 Uani . . . . . .
C6 C 0.8508(3) 0.38204(19) 0.6455(2) 0.0379 1.0000 Uani . . . . . .
C7 C 0.8787(3) 0.38000(19) 0.5588(2) 0.0381 1.0000 Uani . . . . . .
C8 C 0.8396(3) 0.4358(2) 0.4239(2) 0.0448 1.0000 Uani . . . . . .
C9 C 0.7138(3) 0.4834(2) 0.3831(2) 0.0428 1.0000 Uani . . . . . .
C10 C 0.5669(3) 0.6425(2) 0.3999(2) 0.0381 1.0000 Uani . . . . . .
C11 C 0.4681(3) 0.71544(19) 0.44777(19) 0.0377 1.0000 Uani . . . . . .
C12 C 0.4015(3) 0.8010(2) 0.4117(2) 0.0413 1.0000 Uani . . . . . .
C13 C 0.2985(3) 0.8682(2) 0.4538(2) 0.0440 1.0000 Uani . . . . . .
C14 C 0.2574(3) 0.8537(2) 0.5342(2) 0.0405 1.0000 Uani . . . . . .
C15 C 0.3217(3) 0.7732(2) 0.5732(2) 0.0406 1.0000 Uani . . . . . .
C16 C 0.4306(3) 0.70381(19) 0.5302(2) 0.0374 1.0000 Uani . . . . . .
C17 C 0.6923(4) 0.4551(2) 0.9416(2) 0.0505 1.0000 Uani . . . . . .
C18 C 0.7147(4) 0.4486(2) 1.0301(2) 0.0526 1.0000 Uani . . . . . .
C19 C 0.6440(4) 0.4013(2) 1.1614(2) 0.0525 1.0000 Uani . . . . . .
C20 C 0.5818(4) 0.3365(3) 1.2077(2) 0.0583 1.0000 Uani . . . . . .
C21 C 0.6776(5) 0.2378(3) 1.1952(2) 0.0628 1.0000 Uani . . . . . .
C22 C 0.7159(5) 0.2162(2) 1.1059(2) 0.0624 1.0000 Uani . . . . . .
C23 C 0.7684(4) 0.2875(2) 1.0627(2) 0.0597 1.0000 Uani . . . . . .
C24 C 1.0020(3) 0.30637(19) 0.5221(2) 0.0378 1.0000 Uani . . . . . .
C25 C 0.9984(3) 0.2177(2) 0.5156(2) 0.0424 1.0000 Uani . . . . . .
C26 C 1.1113(3) 0.1487(2) 0.4823(2) 0.0454 1.0000 Uani . . . . . .
C27 C 1.2291(3) 0.1662(2) 0.4562(2) 0.0412 1.0000 Uani . . . . . .
C28 C 1.2354(3) 0.2541(2) 0.4646(2) 0.0432 1.0000 Uani . . . . . .
C29 C 1.1208(3) 0.3233(2) 0.4973(2) 0.0438 1.0000 Uani . . . . . .
C30 C 1.4645(3) 0.1029(2) 0.4118(2) 0.0506 1.0000 Uani . . . . . .
C31 C 1.5672(4) 0.0113(2) 0.3816(2) 0.0525 1.0000 Uani . . . . . .
C32 C 1.7103(4) -0.0786(2) 0.2716(3) 0.0607 1.0000 Uani . . . . . .
C33 C 1.7553(5) -0.0822(3) 0.1819(3) 0.0753 1.0000 Uani . . . . . .
C34 C 1.6387(5) -0.0691(3) 0.1325(3) 0.0714 1.0000 Uani . . . . . .
C35 C 1.5233(5) 0.0185(3) 0.1601(3) 0.0647 1.0000 Uani . . . . . .
C36 C 1.4863(4) 0.0169(2) 0.2506(2) 0.0555 1.0000 Uani . . . . . .
C37 C 0.5941(3) 0.6568(2) 0.3112(2) 0.0402 1.0000 Uani . . . . . .
C38 C 0.7229(3) 0.6561(2) 0.2794(2) 0.0457 1.0000 Uani . . . . . .
C39 C 0.7521(4) 0.6677(2) 0.1983(2) 0.0465 1.0000 Uani . . . . . .
C40 C 0.6530(4) 0.6816(2) 0.1465(2) 0.0450 1.0000 Uani . . . . . .
C41 C 0.5250(4) 0.6823(2) 0.1757(2) 0.0476 1.0000 Uani . . . . . .
C42 C 0.4960(3) 0.6699(2) 0.2584(2) 0.0435 1.0000 Uani . . . . . .
C43 C 0.5951(4) 0.7235(3) 0.0122(2) 0.0575 1.0000 Uani . . . . . .
C44 C 0.6580(4) 0.7545(3) -0.0651(2) 0.0609 1.0000 Uani . . . . . .
C45 C 0.8752(4) 0.6354(3) -0.0883(3) 0.0622 1.0000 Uani . . . . . .
C46 C 0.9617(4) 0.5571(3) -0.1443(3) 0.0689 1.0000 Uani . . . . . .
C47 C 0.9809(5) 0.5894(4) -0.2291(3) 0.0818 1.0000 Uani . . . . . .
C48 C 0.8463(5) 0.6448(4) -0.2597(3) 0.0782 1.0000 Uani . . . . . .
C49 C 0.7638(5) 0.7189(3) -0.1998(2) 0.0680 1.0000 Uani . . . . . .
C50 C 0.1113(3) 0.9135(2) 0.6543(2) 0.0483 1.0000 Uani . . . . . .
C51 C -0.0140(4) 0.9956(2) 0.6783(2) 0.0543 1.0000 Uani . . . . . .
C52 C -0.1456(5) 1.0987(3) 0.7840(3) 0.0711 1.0000 Uani . . . . . .
C53 C -0.1656(5) 1.1181(3) 0.8740(3) 0.0767 1.0000 Uani . . . . . .
C54 C -0.2071(5) 1.0450(3) 0.9205(3) 0.0801 1.0000 Uani . . . . . .
C55 C -0.1048(6) 0.9511(3) 0.8977(3) 0.0874 1.0000 Uani . . . . . .
C56 C -0.0842(5) 0.9375(3) 0.8062(3) 0.0695 1.0000 Uani . . . . . .
H21 H 0.6443 0.4937 0.7971 0.0530 1.0000 Uiso R . . . . .
H41 H 0.9753 0.2716 0.8065 0.0556 1.0000 Uiso R . . . . .
H51 H 1.0130 0.2710 0.6685 0.0518 1.0000 Uiso R . . . . .
H81 H 0.9064 0.4660 0.4113 0.0540 1.0000 Uiso R . . . . .
H82 H 0.8796 0.3729 0.4062 0.0531 1.0000 Uiso R . . . . .
H91 H 0.7347 0.4980 0.3266 0.0495 1.0000 Uiso R . . . . .
H92 H 0.6584 0.4431 0.3848 0.0503 1.0000 Uiso R . . . . .
H121 H 0.4290 0.8130 0.3584 0.0493 1.0000 Uiso R . . . . .
H131 H 0.2565 0.9237 0.4293 0.0531 1.0000 Uiso R . . . . .
H151 H 0.2954 0.7640 0.6279 0.0482 1.0000 Uiso R . . . . .
H171 H 0.6965 0.5147 0.9209 0.0610 1.0000 Uiso R . . . . .
H172 H 0.6030 0.4510 0.9345 0.0604 1.0000 Uiso R . . . . .
H181 H 0.6633 0.5077 1.0558 0.0632 1.0000 Uiso R . . . . .
H182 H 0.8119 0.4375 1.0354 0.0627 1.0000 Uiso R . . . . .
H191 H 0.7309 0.3978 1.1820 0.0625 1.0000 Uiso R . . . . .
H192 H 0.5815 0.4642 1.1678 0.0623 1.0000 Uiso R . . . . .
H201 H 0.5647 0.3519 1.2667 0.0696 1.0000 Uiso R . . . . .
H202 H 0.4937 0.3421 1.1881 0.0706 1.0000 Uiso R . . . . .
H211 H 0.7639 0.2314 1.2205 0.0751 1.0000 Uiso R . . . . .
H212 H 0.6361 0.1915 1.2201 0.0744 1.0000 Uiso R . . . . .
H221 H 0.7848 0.1543 1.0984 0.0752 1.0000 Uiso R . . . . .
H222 H 0.6332 0.2168 1.0818 0.0746 1.0000 Uiso R . . . . .
H231 H 0.8562 0.2858 1.0827 0.0721 1.0000 Uiso R . . . . .
H232 H 0.7846 0.2742 1.0040 0.0719 1.0000 Uiso R . . . . .
H251 H 0.9217 0.2054 0.5332 0.0513 1.0000 Uiso R . . . . .
H261 H 1.1069 0.0900 0.4775 0.0536 1.0000 Uiso R . . . . .
H281 H 1.3142 0.2669 0.4490 0.0515 1.0000 Uiso R . . . . .
H291 H 1.1247 0.3813 0.5026 0.0533 1.0000 Uiso R . . . . .
H301 H 1.4886 0.1191 0.4628 0.0611 1.0000 Uiso R . . . . .
H302 H 1.4665 0.1504 0.3720 0.0611 1.0000 Uiso R . . . . .
H311 H 1.6501 0.0019 0.4066 0.0628 1.0000 Uiso R . . . . .
H312 H 1.5304 -0.0374 0.3982 0.0632 1.0000 Uiso R . . . . .
H321 H 1.7872 -0.0845 0.3019 0.0726 1.0000 Uiso R . . . . .
H322 H 1.6755 -0.1302 0.2860 0.0728 1.0000 Uiso R . . . . .
H331 H 1.7924 -0.0326 0.1674 0.0897 1.0000 Uiso R . . . . .
H332 H 1.8259 -0.1401 0.1679 0.0903 1.0000 Uiso R . . . . .
H341 H 1.6700 -0.0637 0.0742 0.0862 1.0000 Uiso R . . . . .
H342 H 1.6062 -0.1220 0.1404 0.0860 1.0000 Uiso R . . . . .
H351 H 1.5538 0.0720 0.1471 0.0783 1.0000 Uiso R . . . . .
H352 H 1.4426 0.0258 0.1321 0.0776 1.0000 Uiso R . . . . .
H361 H 1.4145 0.0740 0.2670 0.0663 1.0000 Uiso R . . . . .
H362 H 1.4524 -0.0347 0.2627 0.0671 1.0000 Uiso R . . . . .
H381 H 0.7902 0.6476 0.3141 0.0550 1.0000 Uiso R . . . . .
H391 H 0.8379 0.6682 0.1780 0.0561 1.0000 Uiso R . . . . .
H411 H 0.4589 0.6901 0.1419 0.0572 1.0000 Uiso R . . . . .
H421 H 0.4099 0.6690 0.2782 0.0519 1.0000 Uiso R . . . . .
H431 H 0.5183 0.7751 0.0370 0.0692 1.0000 Uiso R . . . . .
H432 H 0.5627 0.6726 0.0009 0.0696 1.0000 Uiso R . . . . .
H441 H 0.7151 0.7916 -0.0506 0.0734 1.0000 Uiso R . . . . .
H442 H 0.5829 0.7940 -0.0948 0.0730 1.0000 Uiso R . . . . .
H451 H 0.9218 0.6821 -0.0867 0.0753 1.0000 Uiso R . . . . .
H452 H 0.8578 0.6150 -0.0318 0.0745 1.0000 Uiso R . . . . .
H461 H 1.0504 0.5304 -0.1232 0.0827 1.0000 Uiso R . . . . .
H462 H 0.9166 0.5104 -0.1441 0.0831 1.0000 Uiso R . . . . .
H471 H 1.0377 0.6305 -0.2297 0.0981 1.0000 Uiso R . . . . .
H472 H 1.0282 0.5368 -0.2656 0.0981 1.0000 Uiso R . . . . .
H481 H 0.8618 0.6719 -0.3132 0.0940 1.0000 Uiso R . . . . .
H482 H 0.7927 0.6038 -0.2651 0.0940 1.0000 Uiso R . . . . .
H491 H 0.8135 0.7637 -0.1969 0.0820 1.0000 Uiso R . . . . .
H492 H 0.6734 0.7489 -0.2195 0.0821 1.0000 Uiso R . . . . .
H501 H 0.1842 0.9124 0.6859 0.0580 1.0000 Uiso R . . . . .
H502 H 0.0892 0.8568 0.6628 0.0584 1.0000 Uiso R . . . . .
H511 H 0.0007 1.0492 0.6529 0.0644 1.0000 Uiso R . . . . .
H512 H -0.0925 0.9859 0.6595 0.0652 1.0000 Uiso R . . . . .
H521 H -0.1165 1.1457 0.7549 0.0851 1.0000 Uiso R . . . . .
H522 H -0.2320 1.0972 0.7664 0.0850 1.0000 Uiso R . . . . .
H531 H -0.2324 1.1786 0.8866 0.0922 1.0000 Uiso R . . . . .
H532 H -0.0782 1.1169 0.8913 0.0919 1.0000 Uiso R . . . . .
H541 H -0.2130 1.0553 0.9793 0.0962 1.0000 Uiso R . . . . .
H542 H -0.2957 1.0462 0.9047 0.0959 1.0000 Uiso R . . . . .
H551 H -0.0180 0.9477 0.9162 0.1050 1.0000 Uiso R . . . . .
H552 H -0.1363 0.9025 0.9247 0.1052 1.0000 Uiso R . . . . .
H561 H -0.1706 0.9400 0.7862 0.0841 1.0000 Uiso R . . . . .
H562 H -0.0157 0.8768 0.7908 0.0841 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.39(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
Ni1 . O1 . 1.822(2) yes
Ni1 . O2 . 1.829(2) yes
Ni1 . N1 . 1.854(3) yes
Ni1 . N2 . 1.850(3) yes
O1 . C1 . 1.305(3) yes
O2 . C16 . 1.313(3) yes
O3 . C3 . 1.355(4) yes
O3 . C17 . 1.438(4) yes
O4 . C27 . 1.371(4) yes
O4 . C30 . 1.434(4) yes
O5 . C40 . 1.373(4) yes
O5 . C43 . 1.404(4) yes
O6 . C14 . 1.375(4) yes
O6 . C50 . 1.425(4) yes
N1 . C7 . 1.313(4) yes
N1 . C8 . 1.472(4) yes
N2 . C9 . 1.477(4) yes
N2 . C10 . 1.311(4) yes
N3 . C18 . 1.457(5) yes
N3 . C19 . 1.457(4) yes
N3 . C23 . 1.471(4) yes
N4 . C31 . 1.447(5) yes
N4 . C32 . 1.469(4) yes
N4 . C36 . 1.453(5) yes
N5 . C44 . 1.456(5) yes
N5 . C45 . 1.452(5) yes
N5 . C49 . 1.471(5) yes
N6 . C51 . 1.449(5) yes
N6 . C52 . 1.472(4) yes
N6 . C56 . 1.460(5) yes
C1 . C2 . 1.407(5) yes
C1 . C6 . 1.421(4) yes
C2 . C3 . 1.380(4) yes
C2 . H21 . 0.926 no
C3 . C4 . 1.413(4) yes
C4 . C5 . 1.350(5) yes
C4 . H41 . 0.930 no
C5 . C6 . 1.428(4) yes
C5 . H51 . 0.931 no
C6 . C7 . 1.436(4) yes
C7 . C24 . 1.500(4) yes
C8 . C9 . 1.508(4) yes
C8 . H81 . 0.970 no
C8 . H82 . 0.965 no
C9 . H91 . 0.977 no
C9 . H92 . 0.984 no
C10 . C11 . 1.446(4) yes
C10 . C37 . 1.492(4) yes
C11 . C12 . 1.423(4) yes
C11 . C16 . 1.405(4) yes
C12 . C13 . 1.373(4) yes
C12 . H121 . 0.932 no
C13 . C14 . 1.392(5) yes
C13 . H131 . 0.929 no
C14 . C15 . 1.382(4) yes
C15 . C16 . 1.427(4) yes
C15 . H151 . 0.941 no
C17 . C18 . 1.508(5) yes
C17 . H171 . 0.987 no
C17 . H172 . 0.985 no
C18 . H181 . 0.979 no
C18 . H182 . 0.995 no
C19 . C20 . 1.517(5) yes
C19 . H191 . 0.996 no
C19 . H192 . 0.979 no
C20 . C21 . 1.532(5) yes
C20 . H201 . 0.998 no
C20 . H202 . 0.993 no
C21 . C22 . 1.513(5) yes
C21 . H211 . 1.017 no
C21 . H212 . 1.013 no
C22 . C23 . 1.518(5) yes
C22 . H221 . 0.993 no
C22 . H222 . 0.995 no
C23 . H231 . 1.009 no
C23 . H232 . 0.988 no
C24 . C25 . 1.393(4) yes
C24 . C29 . 1.381(5) yes
C25 . C26 . 1.385(4) yes
C25 . H251 . 0.907 no
C26 . C27 . 1.380(5) yes
C26 . H261 . 0.930 no
C27 . C28 . 1.397(4) yes
C28 . C29 . 1.392(4) yes
C28 . H281 . 0.925 no
C29 . H291 . 0.919 no
C30 . C31 . 1.530(4) yes
C30 . H301 . 0.974 no
C30 . H302 . 0.976 no
C31 . H311 . 0.974 no
C31 . H312 . 0.977 no
C32 . C33 . 1.511(6) yes
C32 . H321 . 0.977 no
C32 . H322 . 0.996 no
C33 . C34 . 1.506(7) yes
C33 . H331 . 0.984 no
C33 . H332 . 0.972 no
C34 . C35 . 1.534(5) yes
C34 . H341 . 0.997 no
C34 . H342 . 0.987 no
C35 . C36 . 1.512(6) yes
C35 . H351 . 0.992 no
C35 . H352 . 0.986 no
C36 . H361 . 0.977 no
C36 . H362 . 0.985 no
C37 . C38 . 1.401(5) yes
C37 . C42 . 1.386(5) yes
C38 . C39 . 1.367(5) yes
C38 . H381 . 0.935 no
C39 . C40 . 1.382(5) yes
C39 . H391 . 0.934 no
C40 . C41 . 1.381(5) yes
C41 . C42 . 1.395(5) yes
C41 . H411 . 0.917 no
C42 . H421 . 0.937 no
C43 . C44 . 1.519(5) yes
C43 . H431 . 0.992 no
C43 . H432 . 0.987 no
C44 . H441 . 1.010 no
C44 . H442 . 0.994 no
C45 . C46 . 1.525(6) yes
C45 . H451 . 1.001 no
C45 . H452 . 0.997 no
C46 . C47 . 1.493(6) yes
C46 . H461 . 0.986 no
C46 . H462 . 0.987 no
C47 . C48 . 1.524(7) yes
C47 . H471 . 1.008 no
C47 . H472 . 0.988 no
C48 . C49 . 1.511(6) yes
C48 . H481 . 0.989 no
C48 . H482 . 0.992 no
C49 . H491 . 1.003 no
C49 . H492 . 0.997 no
C50 . C51 . 1.524(4) yes
C50 . H501 . 0.972 no
C50 . H502 . 0.982 no
C51 . H511 . 0.968 no
C51 . H512 . 0.973 no
C52 . C53 . 1.512(6) yes
C52 . H521 . 0.975 no
C52 . H522 . 0.995 no
C53 . C54 . 1.506(7) yes
C53 . H531 . 0.980 no
C53 . H532 . 0.989 no
C54 . C55 . 1.524(6) yes
C54 . H541 . 0.987 no
C54 . H542 . 0.991 no
C55 . C56 . 1.523(6) yes
C55 . H551 . 0.980 no
C55 . H552 . 0.995 no
C56 . H561 . 0.992 no
C56 . H562 . 0.997 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 . 84.18(9) yes
O1 . Ni1 . N1 . 94.40(10) yes
O2 . Ni1 . N1 . 178.39(12) yes
O1 . Ni1 . N2 . 177.67(10) yes
O2 . Ni1 . N2 . 93.49(10) yes
N1 . Ni1 . N2 . 87.92(11) yes
Ni1 . O1 . C1 . 128.4(2) yes
Ni1 . O2 . C16 . 127.4(2) yes
C3 . O3 . C17 . 117.6(2) yes
C27 . O4 . C30 . 116.7(3) yes
C40 . O5 . C43 . 118.4(3) yes
C14 . O6 . C50 . 117.3(2) yes
Ni1 . N1 . C7 . 128.6(2) yes
Ni1 . N1 . C8 . 112.38(18) yes
C7 . N1 . C8 . 119.0(3) yes
Ni1 . N2 . C9 . 109.69(18) yes
Ni1 . N2 . C10 . 128.1(2) yes
C9 . N2 . C10 . 122.1(3) yes
C18 . N3 . C19 . 110.6(3) yes
C18 . N3 . C23 . 111.5(3) yes
C19 . N3 . C23 . 109.1(3) yes
C31 . N4 . C32 . 110.2(3) yes
C31 . N4 . C36 . 112.2(3) yes
C32 . N4 . C36 . 109.7(3) yes
C44 . N5 . C45 . 112.4(3) yes
C44 . N5 . C49 . 109.1(3) yes
C45 . N5 . C49 . 110.7(3) yes
C51 . N6 . C52 . 110.2(3) yes
C51 . N6 . C56 . 112.4(3) yes
C52 . N6 . C56 . 108.9(3) yes
O1 . C1 . C2 . 116.7(3) yes
O1 . C1 . C6 . 124.1(3) yes
C2 . C1 . C6 . 119.1(3) yes
C1 . C2 . C3 . 121.6(3) yes
C1 . C2 . H21 . 118.2 no
C3 . C2 . H21 . 120.2 no
C2 . C3 . O3 . 124.6(3) yes
C2 . C3 . C4 . 119.4(3) yes
O3 . C3 . C4 . 115.9(3) yes
C3 . C4 . C5 . 119.9(3) yes
C3 . C4 . H41 . 119.1 no
C5 . C4 . H41 . 121.1 no
C4 . C5 . C6 . 122.6(3) yes
C4 . C5 . H51 . 119.0 no
C6 . C5 . H51 . 118.4 no
C5 . C6 . C1 . 117.3(3) yes
C5 . C6 . C7 . 120.5(3) yes
C1 . C6 . C7 . 122.1(3) yes
C6 . C7 . N1 . 122.3(3) yes
C6 . C7 . C24 . 117.7(3) yes
N1 . C7 . C24 . 120.0(3) yes
N1 . C8 . C9 . 107.6(3) yes
N1 . C8 . H81 . 109.4 no
C9 . C8 . H81 . 110.9 no
N1 . C8 . H82 . 110.1 no
C9 . C8 . H82 . 110.9 no
H81 . C8 . H82 . 108.0 no
C8 . C9 . N2 . 106.9(3) yes
C8 . C9 . H91 . 112.0 no
N2 . C9 . H91 . 113.2 no
C8 . C9 . H92 . 108.9 no
N2 . C9 . H92 . 106.9 no
H91 . C9 . H92 . 108.7 no
N2 . C10 . C11 . 121.8(3) yes
N2 . C10 . C37 . 119.1(3) yes
C11 . C10 . C37 . 119.1(2) yes
C10 . C11 . C12 . 120.6(3) yes
C10 . C11 . C16 . 121.7(3) yes
C12 . C11 . C16 . 117.6(3) yes
C11 . C12 . C13 . 121.7(3) yes
C11 . C12 . H121 . 119.9 no
C13 . C12 . H121 . 118.4 no
C12 . C13 . C14 . 120.0(3) yes
C12 . C13 . H131 . 120.4 no
C14 . C13 . H131 . 119.6 no
C13 . C14 . O6 . 115.8(3) yes
C13 . C14 . C15 . 120.8(3) yes
O6 . C14 . C15 . 123.4(3) yes
C14 . C15 . C16 . 119.5(3) yes
C14 . C15 . H151 . 120.9 no
C16 . C15 . H151 . 119.6 no
C15 . C16 . C11 . 120.2(3) yes
C15 . C16 . O2 . 115.4(3) yes
C11 . C16 . O2 . 124.3(3) yes
O3 . C17 . C18 . 109.0(3) yes
O3 . C17 . H171 . 110.3 no
C18 . C17 . H171 . 108.6 no
O3 . C17 . H172 . 109.4 no
C18 . C17 . H172 . 110.4 no
H171 . C17 . H172 . 109.1 no
C17 . C18 . N3 . 114.5(3) yes
C17 . C18 . H181 . 108.3 no
N3 . C18 . H181 . 106.5 no
C17 . C18 . H182 . 109.3 no
N3 . C18 . H182 . 110.7 no
H181 . C18 . H182 . 107.3 no
N3 . C19 . C20 . 111.1(3) yes
N3 . C19 . H191 . 108.8 no
C20 . C19 . H191 . 110.9 no
N3 . C19 . H192 . 107.6 no
C20 . C19 . H192 . 109.5 no
H191 . C19 . H192 . 108.8 no
C19 . C20 . C21 . 109.4(3) yes
C19 . C20 . H201 . 110.5 no
C21 . C20 . H201 . 109.7 no
C19 . C20 . H202 . 110.4 no
C21 . C20 . H202 . 109.2 no
H201 . C20 . H202 . 107.6 no
C20 . C21 . C22 . 110.6(3) yes
C20 . C21 . H211 . 108.5 no
C22 . C21 . H211 . 107.5 no
C20 . C21 . H212 . 112.2 no
C22 . C21 . H212 . 108.2 no
H211 . C21 . H212 . 109.8 no
C21 . C22 . C23 . 111.4(4) yes
C21 . C22 . H221 . 110.1 no
C23 . C22 . H221 . 110.3 no
C21 . C22 . H222 . 107.8 no
C23 . C22 . H222 . 108.4 no
H221 . C22 . H222 . 108.8 no
C22 . C23 . N3 . 111.0(3) yes
C22 . C23 . H231 . 110.7 no
N3 . C23 . H231 . 109.4 no
C22 . C23 . H232 . 109.0 no
N3 . C23 . H232 . 108.2 no
H231 . C23 . H232 . 108.6 no
C7 . C24 . C25 . 119.2(3) yes
C7 . C24 . C29 . 121.8(3) yes
C25 . C24 . C29 . 119.0(3) yes
C24 . C25 . C26 . 120.1(3) yes
C24 . C25 . H251 . 119.8 no
C26 . C25 . H251 . 120.1 no
C25 . C26 . C27 . 120.7(3) yes
C25 . C26 . H261 . 119.2 no
C27 . C26 . H261 . 120.1 no
C26 . C27 . O4 . 115.6(3) yes
C26 . C27 . C28 . 119.8(3) yes
O4 . C27 . C28 . 124.7(3) yes
C27 . C28 . C29 . 119.0(3) yes
C27 . C28 . H281 . 121.1 no
C29 . C28 . H281 . 119.8 no
C28 . C29 . C24 . 121.3(3) yes
C28 . C29 . H291 . 119.1 no
C24 . C29 . H291 . 119.6 no
O4 . C30 . C31 . 108.3(3) yes
O4 . C30 . H301 . 110.6 no
C31 . C30 . H301 . 109.4 no
O4 . C30 . H302 . 110.5 no
C31 . C30 . H302 . 109.2 no
H301 . C30 . H302 . 108.9 no
C30 . C31 . N4 . 113.7(3) yes
C30 . C31 . H311 . 108.2 no
N4 . C31 . H311 . 107.2 no
C30 . C31 . H312 . 108.5 no
N4 . C31 . H312 . 109.6 no
H311 . C31 . H312 . 109.5 no
N4 . C32 . C33 . 111.6(3) yes
N4 . C32 . H321 . 109.1 no
C33 . C32 . H321 . 109.3 no
N4 . C32 . H322 . 108.2 no
C33 . C32 . H322 . 109.2 no
H321 . C32 . H322 . 109.4 no
C32 . C33 . C34 . 111.4(4) yes
C32 . C33 . H331 . 109.8 no
C34 . C33 . H331 . 107.3 no
C32 . C33 . H332 . 110.2 no
C34 . C33 . H332 . 110.1 no
H331 . C33 . H332 . 107.9 no
C33 . C34 . C35 . 109.5(4) yes
C33 . C34 . H341 . 108.8 no
C35 . C34 . H341 . 109.8 no
C33 . C34 . H342 . 109.4 no
C35 . C34 . H342 . 109.1 no
H341 . C34 . H342 . 110.3 no
C34 . C35 . C36 . 110.6(3) yes
C34 . C35 . H351 . 108.6 no
C36 . C35 . H351 . 108.6 no
C34 . C35 . H352 . 111.1 no
C36 . C35 . H352 . 109.2 no
H351 . C35 . H352 . 108.7 no
C35 . C36 . N4 . 111.2(3) yes
C35 . C36 . H361 . 109.1 no
N4 . C36 . H361 . 108.9 no
C35 . C36 . H362 . 108.0 no
N4 . C36 . H362 . 110.6 no
H361 . C36 . H362 . 109.0 no
C10 . C37 . C38 . 119.4(3) yes
C10 . C37 . C42 . 122.2(3) yes
C38 . C37 . C42 . 118.3(3) yes
C37 . C38 . C39 . 121.1(3) yes
C37 . C38 . H381 . 119.5 no
C39 . C38 . H381 . 119.4 no
C38 . C39 . C40 . 119.9(3) yes
C38 . C39 . H391 . 120.3 no
C40 . C39 . H391 . 119.8 no
C39 . C40 . O5 . 114.5(3) yes
C39 . C40 . C41 . 120.6(3) yes
O5 . C40 . C41 . 125.0(3) yes
C40 . C41 . C42 . 119.3(3) yes
C40 . C41 . H411 . 121.4 no
C42 . C41 . H411 . 119.3 no
C41 . C42 . C37 . 120.8(3) yes
C41 . C42 . H421 . 119.4 no
C37 . C42 . H421 . 119.8 no
O5 . C43 . C44 . 108.3(3) yes
O5 . C43 . H431 . 108.7 no
C44 . C43 . H431 . 110.2 no
O5 . C43 . H432 . 109.7 no
C44 . C43 . H432 . 110.6 no
H431 . C43 . H432 . 109.2 no
C43 . C44 . N5 . 115.3(3) yes
C43 . C44 . H441 . 109.1 no
N5 . C44 . H441 . 106.6 no
C43 . C44 . H442 . 107.4 no
N5 . C44 . H442 . 109.1 no
H441 . C44 . H442 . 109.2 no
N5 . C45 . C46 . 110.8(4) yes
N5 . C45 . H451 . 107.2 no
C46 . C45 . H451 . 109.2 no
N5 . C45 . H452 . 107.9 no
C46 . C45 . H452 . 113.1 no
H451 . C45 . H452 . 108.6 no
C45 . C46 . C47 . 111.6(4) yes
C45 . C46 . H461 . 108.0 no
C47 . C46 . H461 . 109.5 no
C45 . C46 . H462 . 108.6 no
C47 . C46 . H462 . 109.2 no
H461 . C46 . H462 . 109.9 no
C46 . C47 . C48 . 111.5(4) yes
C46 . C47 . H471 . 108.4 no
C48 . C47 . H471 . 107.9 no
C46 . C47 . H472 . 110.3 no
C48 . C47 . H472 . 109.8 no
H471 . C47 . H472 . 108.8 no
C47 . C48 . C49 . 111.1(4) yes
C47 . C48 . H481 . 110.2 no
C49 . C48 . H481 . 110.4 no
C47 . C48 . H482 . 109.1 no
C49 . C48 . H482 . 106.8 no
H481 . C48 . H482 . 109.1 no
C48 . C49 . N5 . 111.6(4) yes
C48 . C49 . H491 . 107.8 no
N5 . C49 . H491 . 109.0 no
C48 . C49 . H492 . 108.2 no
N5 . C49 . H492 . 109.0 no
H491 . C49 . H492 . 111.2 no
O6 . C50 . C51 . 107.1(3) yes
O6 . C50 . H501 . 109.4 no
C51 . C50 . H501 . 110.4 no
O6 . C50 . H502 . 110.1 no
C51 . C50 . H502 . 109.5 no
H501 . C50 . H502 . 110.2 no
C50 . C51 . N6 . 112.7(3) yes
C50 . C51 . H511 . 107.5 no
N6 . C51 . H511 . 109.5 no
C50 . C51 . H512 . 109.2 no
N6 . C51 . H512 . 107.4 no
H511 . C51 . H512 . 110.7 no
N6 . C52 . C53 . 110.9(4) yes
N6 . C52 . H521 . 107.9 no
C53 . C52 . H521 . 109.7 no
N6 . C52 . H522 . 108.5 no
C53 . C52 . H522 . 108.9 no
H521 . C52 . H522 . 111.0 no
C52 . C53 . C54 . 110.7(4) yes
C52 . C53 . H531 . 111.3 no
C54 . C53 . H531 . 110.3 no
C52 . C53 . H532 . 108.2 no
C54 . C53 . H532 . 107.8 no
H531 . C53 . H532 . 108.5 no
C53 . C54 . C55 . 109.6(4) yes
C53 . C54 . H541 . 110.3 no
C55 . C54 . H541 . 109.9 no
C53 . C54 . H542 . 108.7 no
C55 . C54 . H542 . 107.7 no
H541 . C54 . H542 . 110.5 no
C54 . C55 . C56 . 110.8(4) yes
C54 . C55 . H551 . 108.4 no
C56 . C55 . H551 . 108.2 no
C54 . C55 . H552 . 109.6 no
C56 . C55 . H552 . 110.3 no
H551 . C55 . H552 . 109.5 no
C55 . C56 . N6 . 111.2(4) yes
C55 . C56 . H561 . 109.6 no
N6 . C56 . H561 . 107.8 no
C55 . C56 . H562 . 111.2 no
N6 . C56 . H562 . 108.9 no
H561 . C56 . H562 . 108.1 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C1 -177.2(3) . . . . no
N1 Ni1 O1 C1 2.0(3) . . . . no
O1 Ni1 O2 C16 164.1(3) . . . . no
N2 Ni1 O2 C16 -15.7(3) . . . . no
O1 Ni1 N1 C7 -0.8(3) . . . . no
O1 Ni1 N1 C8 -178.0(2) . . . . no
N2 Ni1 N1 C7 179.0(3) . . . . no
N2 Ni1 N1 C8 1.8(2) . . . . no
O2 Ni1 N2 C9 -159.0(2) . . . . no
O2 Ni1 N2 C10 18.1(3) . . . . no
N1 Ni1 N2 C9 21.7(2) . . . . no
N1 Ni1 N2 C10 -161.2(3) . . . . no
Ni1 O1 C1 C2 176.2(2) . . . . no
Ni1 O1 C1 C6 -2.5(5) . . . . no
Ni1 O2 C16 C11 5.7(5) . . . . no
Ni1 O2 C16 C15 -173.2(2) . . . . no
C17 O3 C3 C2 -5.3(5) . . . . no
C17 O3 C3 C4 173.8(3) . . . . no
C3 O3 C17 C18 -169.1(3) . . . . no
C30 O4 C27 C26 -166.4(3) . . . . no
C30 O4 C27 C28 14.0(5) . . . . no
C27 O4 C30 C31 174.6(3) . . . . no
C43 O5 C40 C39 -169.9(3) . . . . no
C43 O5 C40 C41 9.9(5) . . . . no
C40 O5 C43 C44 166.4(3) . . . . no
C50 O6 C14 C13 -176.3(3) . . . . no
C50 O6 C14 C15 3.8(4) . . . . no
C14 O6 C50 C51 -175.8(3) . . . . no
Ni1 N1 C7 C6 0.1(5) . . . . no
Ni1 N1 C7 C24 -180.0(2) . . . . no
C8 N1 C7 C6 177.0(3) . . . . no
C8 N1 C7 C24 -3.0(4) . . . . no
Ni1 N1 C8 C9 -24.2(3) . . . . no
C7 N1 C8 C9 158.4(3) . . . . no
Ni1 N2 C9 C8 -39.4(3) . . . . no
C10 N2 C9 C8 143.3(3) . . . . no
Ni1 N2 C10 C11 -10.1(5) . . . . no
Ni1 N2 C10 C37 168.5(2) . . . . no
C9 N2 C10 C11 166.7(3) . . . . no
C9 N2 C10 C37 -14.7(5) . . . . no
C19 N3 C18 C17 -157.6(3) . . . . no
C23 N3 C18 C17 80.8(4) . . . . no
C18 N3 C19 C20 173.8(3) . . . . no
C23 N3 C19 C20 -63.1(4) . . . . no
C18 N3 C23 C22 -176.7(3) . . . . no
C19 N3 C23 C22 60.7(4) . . . . no
C32 N4 C31 C30 174.5(3) . . . . no
C36 N4 C31 C30 -63.0(4) . . . . no
C31 N4 C32 C33 -176.4(4) . . . . no
C36 N4 C32 C33 59.6(4) . . . . no
C31 N4 C36 C35 176.6(3) . . . . no
C32 N4 C36 C35 -60.5(4) . . . . no
C45 N5 C44 C43 -74.5(4) . . . . no
C49 N5 C44 C43 162.3(4) . . . . no
C44 N5 C45 C46 178.0(3) . . . . no
C49 N5 C45 C46 -59.7(4) . . . . no
C44 N5 C49 C48 -176.2(4) . . . . no
C45 N5 C49 C48 59.5(5) . . . . no
C52 N6 C51 C50 169.0(3) . . . . no
C56 N6 C51 C50 -69.3(4) . . . . no
C51 N6 C52 C53 -174.7(4) . . . . no
C56 N6 C52 C53 61.6(5) . . . . no
C51 N6 C56 C55 177.2(4) . . . . no
C52 N6 C56 C55 -60.5(5) . . . . no
O1 C1 C2 C3 179.2(3) . . . . no
C6 C1 C2 C3 -2.1(5) . . . . no
O1 C1 C6 C5 -178.7(3) . . . . no
O1 C1 C6 C7 1.2(5) . . . . no
C2 C1 C6 C5 2.7(5) . . . . no
C2 C1 C6 C7 -177.4(3) . . . . no
C1 C2 C3 O3 179.1(3) . . . . no
C1 C2 C3 C4 0.0(5) . . . . no
O3 C3 C4 C5 -177.8(3) . . . . no
C2 C3 C4 C5 1.4(5) . . . . no
C3 C4 C5 C6 -0.7(5) . . . . no
C4 C5 C6 C1 -1.4(5) . . . . no
C4 C5 C6 C7 178.7(3) . . . . no
C1 C6 C7 N1 0.0(5) . . . . no
C1 C6 C7 C24 -180.0(3) . . . . no
C5 C6 C7 N1 179.9(3) . . . . no
C5 C6 C7 C24 0.0(4) . . . . no
N1 C7 C24 C25 -102.4(4) . . . . no
N1 C7 C24 C29 80.0(4) . . . . no
C6 C7 C24 C25 77.6(4) . . . . no
C6 C7 C24 C29 -100.0(4) . . . . no
N1 C8 C9 N2 40.1(3) . . . . no
N2 C10 C11 C12 176.1(3) . . . . no
N2 C10 C11 C16 -6.3(5) . . . . no
C37 C10 C11 C12 -2.5(5) . . . . no
C37 C10 C11 C16 175.2(3) . . . . no
N2 C10 C37 C38 -61.8(4) . . . . no
N2 C10 C37 C42 117.5(4) . . . . no
C11 C10 C37 C38 116.8(3) . . . . no
C11 C10 C37 C42 -63.9(4) . . . . no
C10 C11 C12 C13 173.8(3) . . . . no
C16 C11 C12 C13 -3.9(5) . . . . no
C10 C11 C16 O2 8.6(5) . . . . no
C10 C11 C16 C15 -172.6(3) . . . . no
C12 C11 C16 O2 -173.8(3) . . . . no
C12 C11 C16 C15 5.1(5) . . . . no
C11 C12 C13 C14 0.5(5) . . . . no
C12 C13 C14 O6 -178.0(3) . . . . no
C12 C13 C14 C15 1.9(5) . . . . no
O6 C14 C15 C16 179.3(3) . . . . no
C13 C14 C15 C16 -0.6(5) . . . . no
C14 C15 C16 O2 176.0(3) . . . . no
C14 C15 C16 C11 -2.9(5) . . . . no
O3 C17 C18 N3 -78.8(4) . . . . no
N3 C19 C20 C21 59.3(4) . . . . no
C19 C20 C21 C22 -53.0(5) . . . . no
C20 C21 C22 C23 52.0(5) . . . . no
C21 C22 C23 N3 -56.0(5) . . . . no
C7 C24 C25 C26 -179.7(3) . . . . no
C29 C24 C25 C26 -2.1(5) . . . . no
C7 C24 C29 C28 178.9(3) . . . . no
C25 C24 C29 C28 1.3(5) . . . . no
C24 C25 C26 C27 0.9(5) . . . . no
C25 C26 C27 O4 -178.6(3) . . . . no
C25 C26 C27 C28 1.0(5) . . . . no
O4 C27 C28 C29 177.8(3) . . . . no
C26 C27 C28 C29 -1.8(5) . . . . no
C27 C28 C29 C24 0.6(5) . . . . no
O4 C30 C31 N4 98.3(4) . . . . no
N4 C32 C33 C34 -56.7(5) . . . . no
C32 C33 C34 C35 52.8(5) . . . . no
C33 C34 C35 C36 -53.5(5) . . . . no
C34 C35 C36 N4 58.3(4) . . . . no
C10 C37 C38 C39 179.1(3) . . . . no
C42 C37 C38 C39 -0.2(4) . . . . no
C10 C37 C42 C41 -179.5(3) . . . . no
C38 C37 C42 C41 -0.2(4) . . . . no
C37 C38 C39 C40 0.9(4) . . . . no
C38 C39 C40 O5 178.6(3) . . . . no
C38 C39 C40 C41 -1.1(4) . . . . no
O5 C40 C41 C42 -179.0(3) . . . . no
C39 C40 C41 C42 0.8(4) . . . . no
C40 C41 C42 C37 -0.1(4) . . . . no
O5 C43 C44 N5 77.5(4) . . . . no
N5 C45 C46 C47 56.3(5) . . . . no
C45 C46 C47 C48 -51.3(6) . . . . no
C46 C47 C48 C49 50.4(6) . . . . no
C47 C48 C49 N5 -54.3(6) . . . . no
O6 C50 C51 N6 -162.2(3) . . . . no
N6 C52 C53 C54 -59.4(6) . . . . no
C52 C53 C54 C55 54.3(6) . . . . no
C53 C54 C55 C56 -53.1(6) . . . . no
C54 C55 C56 N6 57.1(6) . . . . 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
Ni1 Ni1 3.9577(8) . 2_666 no
Ni1 O2 3.980(2) . 2_666 no
Ni1 N2 3.751(3) . 2_666 no
Ni1 C9 3.953(3) . 2_666 no
Ni1 C28 3.851(3) . 2_766 no
Ni1 C29 3.798(3) . 2_766 no
O1 O2 2.447(3) . . no
O1 N1 2.697(4) . . no
O1 C7 2.922(4) . . no
O2 N2 2.680(3) . . no
O2 C10 2.915(4) . . no
O2 C9 3.247(4) . 2_666 no
O3 C23 3.079(4) . . no
O3 N3 3.092(4) . . no
O4 N4 3.270(4) . . no
O4 C36 3.180(4) . . no
O5 C45 3.011(6) . . no
O5 N5 3.070(4) . . no
N1 N2 2.571(4) . . no
N1 C1 2.896(4) . . no
N1 C9 2.404(4) . . no
N2 C8 2.399(4) . . no
N2 C16 2.879(4) . . no
C1 C42 3.556(5) . 2_666 no
C2 C42 3.439(5) . 2_666 no
C5 C25 3.279(5) . . no
C8 C47 3.530(6) . 2_765 no
C8 C29 3.243(5) . . no
C9 C38 3.153(4) . . no
C12 C42 3.168(4) . . no
C14 C30 3.432(5) . 2_766 no
C14 C25 3.422(5) . 2_666 no
C15 C30 3.443(5) . 2_766 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 16/01/17 at 12:23:02
#
#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   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,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   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,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   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,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   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) H   ( 472,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 16/01/17 at 12:23:02
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
2 3 1 x .



#===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_cmpd9_exp_128_tsb
_database_code_depnum_ccdc_archive 'CCDC 1922294'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_audit_creation_date             2019-06-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
N,N'-Bis-(4-(hydroxybenzophenylidene))-2-hydroxy-1,3-propylenediaminenickel(II)
_chemical_formula_moiety         'C29 H24 N2 Ni O5, 2(C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C33 H34 N4 Ni O7'
_chemical_formula_weight         657.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H34 N4 Ni O7'
_chemical_oxdiff_usercomment     TSB22
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   18.3041(4)
_cell_length_b                   8.07129(16)
_cell_length_c                   21.2716(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.144(2)
_cell_angle_gamma                90
_cell_volume                     3093.50(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15768
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      29.3430
_cell_measurement_theta_min      1.7170
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.796
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'translucent green'
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method 'from acetonitrile'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48656
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.705
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'HyPix Bantam HPC 3000'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 110.00   0.50   25.00    --   20.00  54.00  29.95  368
  2  ω    -74.00 110.00   0.50   25.00    --   20.00  54.00 -30.00  368
  3  ω    -74.00 110.00   0.50   25.00    --   20.00  54.00 -30.00  368
  4  ω    -74.00 110.00   0.50   25.00    --   20.00  54.00   1.73  368
  5  ω    -74.00 110.00   0.50   25.00    --   20.00  54.00-150.00  368
  6  ω     12.00  92.00   0.50   25.00    --   20.00  54.00-150.00  160
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0218037000
_diffrn_orient_matrix_UB_12      0.0488950000
_diffrn_orient_matrix_UB_13      -0.0239592000
_diffrn_orient_matrix_UB_21      0.0060290000
_diffrn_orient_matrix_UB_22      0.0701774000
_diffrn_orient_matrix_UB_23      0.0203063000
_diffrn_orient_matrix_UB_31      0.0322314000
_diffrn_orient_matrix_UB_32      0.0201103000
_diffrn_orient_matrix_UB_33      -0.0126918000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6297
_reflns_number_total             7953
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7953
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0448
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0457P)²+2.9016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1109
_refine_special_details          
;Backbone disorder modelled as two component via a free variable. 
Solvent acetonitriles all with distance restraints and isotropic restraints. 
The molecules are linear but with large ADPs.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 C2B-N1B = C2C-N1C = N1A-C2A
 1.15 with sigma of 0.01
 C1B-C2B = C1B-C2C = C1A-C2A
 1.46 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N1B) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(N1C)
\\sim Ueq, Uanis(C2C) \\sim Ueq: with sigma of 0.05 and sigma for terminal
atoms of 0.1
Uanis(N1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
4. Others
 Sof(H16A)=Sof(O18P)=Sof(H18P)=1-FVAR(1)
 Sof(H16)=Sof(O18)=Sof(H18)=FVAR(1)
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(N1C)=Sof(C2C)=1-FVAR(2)
 Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(N1B)=Sof(C2B)=FVAR(2)
5.a Riding coordinates:
 C16(H16), C16(H16A)
5.b Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1P(H1PA,H1PB)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C5P(H5P), C6P(H6P), C7P(H7P), C8P(H8P), C9P(H9P), C11P(H11P), C12P(H12P),
 C14P(H14P)
5.e Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1B(H1BD,H1BE,H1BF)
5.f Idealised tetrahedral OH refined as rotating group:
 O18(H18), O19(H19), O18P(H18P), O19P(H19P)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.52832(2) 0.69989(3) 0.28618(2) 0.02197(8) Uani 1 1 d . . . . .
C1 C 0.59155(14) 0.6377(3) 0.17697(10) 0.0345(5) Uani 1 1 d . . . . .
H1A H 0.631487 0.578725 0.160186 0.041 Uiso 1 1 calc R . . . .
H1B H 0.606127 0.755507 0.183049 0.041 Uiso 1 1 calc R . . . .
N2 N 0.58295(10) 0.5652(2) 0.23888(8) 0.0256(4) Uani 1 1 d . . . . .
C3 C 0.61572(11) 0.4260(3) 0.25731(10) 0.0247(4) Uani 1 1 d . . . . .
C4 C 0.65624(12) 0.3306(3) 0.21333(11) 0.0292(5) Uani 1 1 d . . . . .
C5 C 0.61834(15) 0.2174(4) 0.17097(14) 0.0484(7) Uani 1 1 d . . . . .
H5 H 0.566604 0.201005 0.169096 0.058 Uiso 1 1 calc R . . . .
C6 C 0.65627(19) 0.1273(4) 0.13101(16) 0.0620(9) Uani 1 1 d . . . . .
H6 H 0.630479 0.048015 0.102339 0.074 Uiso 1 1 calc R . . . .
C7 C 0.73113(17) 0.1527(4) 0.13296(14) 0.0513(7) Uani 1 1 d . . . . .
H7 H 0.756652 0.093103 0.104963 0.062 Uiso 1 1 calc R . . . .
C8 C 0.76843(14) 0.2638(3) 0.17518(12) 0.0397(6) Uani 1 1 d . . . . .
H8 H 0.820015 0.280823 0.176410 0.048 Uiso 1 1 calc R . . . .
C9 C 0.73203(13) 0.3521(3) 0.21635(11) 0.0315(5) Uani 1 1 d . . . . .
H9 H 0.758799 0.426823 0.246424 0.038 Uiso 1 1 calc R . . . .
C10 C 0.61656(11) 0.3554(3) 0.31977(10) 0.0239(4) Uani 1 1 d . . . . .
C11 C 0.64465(13) 0.1937(3) 0.33356(11) 0.0308(5) Uani 1 1 d . . . . .
H11 H 0.660755 0.131802 0.300549 0.037 Uiso 1 1 calc R . . . .
C12 C 0.64950(14) 0.1233(3) 0.39235(11) 0.0338(5) Uani 1 1 d . . . . .
H12 H 0.668587 0.014358 0.400032 0.041 Uiso 1 1 calc R . . . .
C13 C 0.62600(12) 0.2137(3) 0.44130(11) 0.0275(4) Uani 1 1 d . . . . .
C14 C 0.60027(11) 0.3747(3) 0.43082(10) 0.0241(4) Uani 1 1 d . . . . .
H14 H 0.586755 0.436494 0.465022 0.029 Uiso 1 1 calc R . . . .
C15 C 0.59402(11) 0.4474(2) 0.37006(10) 0.0222(4) Uani 1 1 d . . . . .
O16 O 0.56830(8) 0.60052(17) 0.36284(7) 0.0246(3) Uani 1 1 d . . . . .
C16 C 0.51979(17) 0.6252(4) 0.12911(12) 0.0460(7) Uani 1 1 d . . . . .
H16 H 0.521768 0.697957 0.092577 0.055 Uiso 0.408(5) 1 d R . P A 1
H16A H 0.513958 0.511367 0.112987 0.055 Uiso 0.592(5) 1 d R . P A 2
O18 O 0.4952(3) 0.4558(7) 0.1069(3) 0.072(2) Uani 0.408(5) 1 d . . P A 1
H18 H 0.514265 0.430524 0.075015 0.107 Uiso 0.408(5) 1 calc GR . P A 1
O19 O 0.62873(10) 0.13468(19) 0.49786(8) 0.0358(4) Uani 1 1 d . . . . .
H19 H 0.618230 0.201692 0.525146 0.054 Uiso 1 1 calc GR . . . .
C1P C 0.45352(14) 0.6693(3) 0.16007(12) 0.0400(6) Uani 1 1 d . . . . .
H1PA H 0.413400 0.713705 0.127030 0.048 Uiso 1 1 calc R . . . .
H1PB H 0.434732 0.567351 0.177648 0.048 Uiso 1 1 calc R . . . .
N2P N 0.47161(10) 0.7926(2) 0.21180(8) 0.0276(4) Uani 1 1 d . . . . .
C3P C 0.44077(12) 0.9390(3) 0.20599(10) 0.0264(4) Uani 1 1 d . . . . .
C4P C 0.39609(13) 0.9935(3) 0.14331(10) 0.0320(5) Uani 1 1 d . . . . .
C5P C 0.43124(17) 1.0374(4) 0.09317(12) 0.0493(7) Uani 1 1 d . . . . .
H5P H 0.483663 1.028727 0.097692 0.059 Uiso 1 1 calc R . . . .
C6P C 0.3894(2) 1.0944(5) 0.03591(14) 0.0713(11) Uani 1 1 d . . . . .
H6P H 0.413824 1.128202 0.002157 0.086 Uiso 1 1 calc R . . . .
C7P C 0.3136(2) 1.1020(5) 0.02799(14) 0.0699(11) Uani 1 1 d . . . . .
H7P H 0.285323 1.137349 -0.011529 0.084 Uiso 1 1 calc R . . . .
C8P C 0.27887(19) 1.0582(5) 0.07742(15) 0.0701(11) Uani 1 1 d . . . . .
H8P H 0.226319 1.064426 0.072177 0.084 Uiso 1 1 calc R . . . .
C9P C 0.31936(15) 1.0050(4) 0.13495(13) 0.0514(8) Uani 1 1 d . . . . .
H9P H 0.294462 0.976045 0.168987 0.062 Uiso 1 1 calc R . . . .
C10P C 0.44343(11) 1.0510(3) 0.25950(10) 0.0238(4) Uani 1 1 d . . . . .
C11P C 0.41817(12) 1.2167(3) 0.25020(10) 0.0279(4) Uani 1 1 d . . . . .
H11P H 0.407415 1.259213 0.207934 0.034 Uiso 1 1 calc R . . . .
C12P C 0.40865(13) 1.3180(3) 0.29989(11) 0.0292(4) Uani 1 1 d . . . . .
H12P H 0.392621 1.429320 0.292349 0.035 Uiso 1 1 calc R . . . .
C13P C 0.42310(12) 1.2536(3) 0.36214(10) 0.0254(4) Uani 1 1 d . . . . .
C14P C 0.44999(11) 1.0950(3) 0.37382(10) 0.0241(4) Uani 1 1 d . . . . .
H14P H 0.460254 1.054335 0.416371 0.029 Uiso 1 1 calc R . . . .
C15P C 0.46231(11) 0.9933(2) 0.32312(10) 0.0221(4) Uani 1 1 d . . . . .
O16P O 0.48884(8) 0.84338(18) 0.33823(7) 0.0260(3) Uani 1 1 d . . . . .
O18P O 0.5331(2) 0.7356(5) 0.07687(15) 0.0588(13) Uani 0.592(5) 1 d . . P A 2
H18P H 0.551122 0.680610 0.049789 0.088 Uiso 0.592(5) 1 calc GR . P A 2
O19P O 0.40927(10) 1.35433(18) 0.41024(7) 0.0322(4) Uani 1 1 d . . . . .
H19P H 0.413908 1.299991 0.444396 0.048 Uiso 1 1 calc GR . . . .
N1A N 0.3030(3) 0.7019(8) 0.2525(4) 0.157(3) Uani 1 1 d D U . . .
C1A C 0.2655(4) 0.9224(12) 0.3291(4) 0.200(4) Uani 1 1 d D U . . .
H1AA H 0.233549 1.003342 0.303076 0.299 Uiso 1 1 calc GR . . . .
H1AB H 0.309934 0.978160 0.351833 0.299 Uiso 1 1 calc GR . . . .
H1AC H 0.238357 0.872033 0.360028 0.299 Uiso 1 1 calc GR . . . .
C2A C 0.2874(3) 0.7927(8) 0.2874(3) 0.0871(17) Uani 1 1 d D U . . .
C1B C 0.2770(2) 0.6114(7) 0.0318(3) 0.119(2) Uani 1 1 d D U . . .
H1BA H 0.284440 0.731648 0.031931 0.179 Uiso 0.38(3) 1 calc GR . P B 1
H1BB H 0.278037 0.572668 0.075590 0.179 Uiso 0.38(3) 1 calc GR . P B 1
H1BC H 0.228933 0.584232 0.005612 0.179 Uiso 0.38(3) 1 calc GR . P B 1
H1BD H 0.237880 0.665811 0.001428 0.179 Uiso 0.62(3) 1 calc GR . P B 2
H1BE H 0.288900 0.678843 0.070543 0.179 Uiso 0.62(3) 1 calc GR . P B 2
H1BF H 0.259864 0.501883 0.042764 0.179 Uiso 0.62(3) 1 calc GR . P B 2
N1B N 0.3916(8) 0.495(4) -0.0106(10) 0.121(7) Uani 0.38(3) 1 d D U P B 1
C2B C 0.3363(9) 0.530(3) 0.0052(14) 0.152(12) Uani 0.38(3) 1 d D U P B 1
O1W O 0.59075(15) 0.7869(2) 0.47896(8) 0.0558(6) Uani 1 1 d . . . . .
H1WA H 0.580771 0.745590 0.441658 0.084 Uiso 1 1 d G . . . .
H1WB H 0.595672 0.891261 0.476213 0.084 Uiso 1 1 d G . . . .
O2W O 0.40554(13) 0.6902(2) 0.41132(11) 0.0529(6) Uani 1 1 d . . . . .
H2WA H 0.438693 0.733475 0.393013 0.079 Uiso 1 1 d G . . . .
H2WB H 0.411543 0.585699 0.413144 0.079 Uiso 1 1 d G . . . .
N1C N 0.4029(6) 0.601(3) -0.0162(4) 0.143(6) Uani 0.62(3) 1 d D U P B 2
C2C C 0.3454(5) 0.5924(17) 0.0019(4) 0.105(6) Uani 0.62(3) 1 d D U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.8837(17) . ?
Ni1 O16 1.8487(14) . ?
Ni1 N2P 1.8873(18) . ?
Ni1 O16P 1.8360(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 N2 1.475(3) . ?
C1 C16 1.517(4) . ?
N2 C3 1.301(3) . ?
C3 C4 1.504(3) . ?
C3 C10 1.443(3) . ?
C4 C5 1.381(4) . ?
C4 C9 1.388(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.364(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.388(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.415(3) . ?
C10 C15 1.422(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.362(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.399(3) . ?
C13 C14 1.387(3) . ?
C13 O19 1.355(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.406(3) . ?
C15 O16 1.322(2) . ?
C16 H16 0.9798 . ?
C16 H16A 0.9798 . ?
C16 O18 1.490(6) . ?
C16 C1P 1.521(4) . ?
C16 O18P 1.478(4) . ?
O18 H18 0.8400 . ?
O19 H19 0.8400 . ?
C1P H1PA 0.9900 . ?
C1P H1PB 0.9900 . ?
C1P N2P 1.477(3) . ?
N2P C3P 1.306(3) . ?
C3P C4P 1.502(3) . ?
C3P C10P 1.448(3) . ?
C4P C5P 1.385(4) . ?
C4P C9P 1.387(3) . ?
C5P H5P 0.9500 . ?
C5P C6P 1.397(4) . ?
C6P H6P 0.9500 . ?
C6P C7P 1.370(5) . ?
C7P H7P 0.9500 . ?
C7P C8P 1.367(5) . ?
C8P H8P 0.9500 . ?
C8P C9P 1.383(4) . ?
C9P H9P 0.9500 . ?
C10P C11P 1.418(3) . ?
C10P C15P 1.415(3) . ?
C11P H11P 0.9500 . ?
C11P C12P 1.371(3) . ?
C12P H12P 0.9500 . ?
C12P C13P 1.404(3) . ?
C13P C14P 1.378(3) . ?
C13P O19P 1.365(2) . ?
C14P H14P 0.9500 . ?
C14P C15P 1.405(3) . ?
C15P O16P 1.322(2) . ?
O18P H18P 0.8400 . ?
O19P H19P 0.8400 . ?
N1A C2A 1.117(6) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C1A C2A 1.471(7) . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
C1B H1BD 0.9800 . ?
C1B H1BE 0.9800 . ?
C1B H1BF 0.9800 . ?
C1B C2B 1.464(9) . ?
C1B C2C 1.508(8) . ?
N1B C2B 1.155(9) . ?
O1W H1WA 0.8503 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8515 . ?
O2W H2WB 0.8505 . ?
N1C C2C 1.183(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N2P 92.65(8) . . ?
O16 Ni1 N2 93.21(7) . . ?
O16 Ni1 N2P 170.15(7) . . ?
O16P Ni1 N2 171.28(7) . . ?
O16P Ni1 O16 83.02(6) . . ?
O16P Ni1 N2P 92.22(7) . . ?
H1A C1 H1B 108.0 . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
N2 C1 C16 110.9(2) . . ?
C16 C1 H1A 109.5 . . ?
C16 C1 H1B 109.5 . . ?
C1 N2 Ni1 113.47(14) . . ?
C3 N2 Ni1 126.67(15) . . ?
C3 N2 C1 119.71(17) . . ?
N2 C3 C4 120.40(19) . . ?
N2 C3 C10 123.22(18) . . ?
C10 C3 C4 116.37(18) . . ?
C5 C4 C3 119.9(2) . . ?
C5 C4 C9 119.7(2) . . ?
C9 C4 C3 120.4(2) . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.8(3) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.2(3) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.8(2) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.9(2) . . ?
C9 C8 H8 119.6 . . ?
C4 C9 H9 120.2 . . ?
C8 C9 C4 119.6(2) . . ?
C8 C9 H9 120.2 . . ?
C11 C10 C3 119.98(18) . . ?
C11 C10 C15 117.96(19) . . ?
C15 C10 C3 121.94(19) . . ?
C10 C11 H11 118.7 . . ?
C12 C11 C10 122.5(2) . . ?
C12 C11 H11 118.7 . . ?
C11 C12 H12 120.4 . . ?
C11 C12 C13 119.1(2) . . ?
C13 C12 H12 120.4 . . ?
C14 C13 C12 120.6(2) . . ?
O19 C13 C12 116.57(19) . . ?
O19 C13 C14 122.84(19) . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.62(19) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C10 119.11(18) . . ?
O16 C15 C10 123.07(19) . . ?
O16 C15 C14 117.81(18) . . ?
C15 O16 Ni1 125.84(13) . . ?
C1 C16 H16 110.1 . . ?
C1 C16 H16A 109.0 . . ?
C1 C16 C1P 110.87(19) . . ?
O18 C16 C1 116.9(3) . . ?
O18 C16 H16 110.5 . . ?
O18 C16 C1P 97.6(3) . . ?
C1P C16 H16 110.3 . . ?
C1P C16 H16A 109.0 . . ?
O18P C16 C1 103.1(3) . . ?
O18P C16 H16A 108.9 . . ?
O18P C16 C1P 115.7(2) . . ?
C16 O18 H18 109.5 . . ?
C13 O19 H19 109.5 . . ?
C16 C1P H1PA 109.0 . . ?
C16 C1P H1PB 109.0 . . ?
H1PA C1P H1PB 107.8 . . ?
N2P C1P C16 112.9(2) . . ?
N2P C1P H1PA 109.0 . . ?
N2P C1P H1PB 109.0 . . ?
C1P N2P Ni1 112.05(15) . . ?
C3P N2P Ni1 127.06(15) . . ?
C3P N2P C1P 120.17(19) . . ?
N2P C3P C4P 120.50(19) . . ?
N2P C3P C10P 122.45(19) . . ?
C10P C3P C4P 116.93(19) . . ?
C5P C4P C3P 120.3(2) . . ?
C5P C4P C9P 118.8(2) . . ?
C9P C4P C3P 120.9(2) . . ?
C4P C5P H5P 120.1 . . ?
C4P C5P C6P 119.9(3) . . ?
C6P C5P H5P 120.1 . . ?
C5P C6P H6P 119.7 . . ?
C7P C6P C5P 120.6(3) . . ?
C7P C6P H6P 119.7 . . ?
C6P C7P H7P 120.3 . . ?
C8P C7P C6P 119.5(3) . . ?
C8P C7P H7P 120.3 . . ?
C7P C8P H8P 119.6 . . ?
C7P C8P C9P 120.8(3) . . ?
C9P C8P H8P 119.6 . . ?
C4P C9P H9P 119.8 . . ?
C8P C9P C4P 120.5(3) . . ?
C8P C9P H9P 119.8 . . ?
C11P C10P C3P 120.96(19) . . ?
C15P C10P C3P 121.00(19) . . ?
C15P C10P C11P 117.56(18) . . ?
C10P C11P H11P 118.7 . . ?
C12P C11P C10P 122.5(2) . . ?
C12P C11P H11P 118.7 . . ?
C11P C12P H12P 120.7 . . ?
C11P C12P C13P 118.54(19) . . ?
C13P C12P H12P 120.7 . . ?
C14P C13P C12P 121.08(19) . . ?
O19P C13P C12P 117.21(19) . . ?
O19P C13P C14P 121.71(19) . . ?
C13P C14P H14P 119.8 . . ?
C13P C14P C15P 120.33(19) . . ?
C15P C14P H14P 119.8 . . ?
C14P C15P C10P 119.76(18) . . ?
O16P C15P C10P 123.43(18) . . ?
O16P C15P C14P 116.75(18) . . ?
C15P O16P Ni1 126.69(13) . . ?
C16 O18P H18P 109.5 . . ?
C13P O19P H19P 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
C2A C1A H1AA 109.5 . . ?
C2A C1A H1AB 109.5 . . ?
C2A C1A H1AC 109.5 . . ?
N1A C2A C1A 175.2(7) . . ?
H1BA C1B H1BB 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
H1BD C1B H1BE 109.5 . . ?
H1BD C1B H1BF 109.5 . . ?
H1BE C1B H1BF 109.5 . . ?
C2B C1B H1BA 109.5 . . ?
C2B C1B H1BB 109.5 . . ?
C2B C1B H1BC 109.5 . . ?
C2C C1B H1BD 109.5 . . ?
C2C C1B H1BE 109.5 . . ?
C2C C1B H1BF 109.5 . . ?
N1B C2B C1B 165.3(19) . . ?
H1WA O1W H1WB 109.4 . . ?
H2WA O2W H2WB 109.3 . . ?
N1C C2C C1B 169.2(12) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O19 H19 O2W 0.84 1.73 2.559(2) 170.2 3_666 yes
O19P H19P O1W 0.84 1.79 2.618(2) 168.0 3_676 yes
O1W H1WA O16 0.85 2.02 2.859(2) 166.9 . yes
O2W H2WA O16P 0.85 1.83 2.666(2) 164.9 . yes
O2W H2WB O19P 0.85 1.87 2.712(2) 170.9 1_545 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N2 C3 C4 178.84(15) . . . . ?
Ni1 N2 C3 C10 -2.0(3) . . . . ?
Ni1 N2P C3P C4P -179.01(16) . . . . ?
Ni1 N2P C3P C10P -3.2(3) . . . . ?
C1 N2 C3 C4 -5.8(3) . . . . ?
C1 N2 C3 C10 173.4(2) . . . . ?
C1 C16 C1P N2P 31.1(3) . . . . ?
N2 Ni1 O16 C15 -26.85(16) . . . . ?
N2 Ni1 N2P C1P 37.60(17) . . . . ?
N2 Ni1 N2P C3P -152.18(19) . . . . ?
N2 C1 C16 O18 -67.8(4) . . . . ?
N2 C1 C16 C1P 42.9(3) . . . . ?
N2 C1 C16 O18P 167.3(2) . . . . ?
N2 C3 C4 C5 -87.8(3) . . . . ?
N2 C3 C4 C9 94.2(3) . . . . ?
N2 C3 C10 C11 171.6(2) . . . . ?
N2 C3 C10 C15 -12.3(3) . . . . ?
C3 C4 C5 C6 -179.0(3) . . . . ?
C3 C4 C9 C8 -179.7(2) . . . . ?
C3 C10 C11 C12 177.4(2) . . . . ?
C3 C10 C15 C14 -176.30(19) . . . . ?
C3 C10 C15 O16 2.6(3) . . . . ?
C4 C3 C10 C11 -9.2(3) . . . . ?
C4 C3 C10 C15 166.91(19) . . . . ?
C4 C5 C6 C7 -1.0(5) . . . . ?
C5 C4 C9 C8 2.3(4) . . . . ?
C5 C6 C7 C8 1.5(5) . . . . ?
C6 C7 C8 C9 -0.1(4) . . . . ?
C7 C8 C9 C4 -1.8(4) . . . . ?
C9 C4 C5 C6 -0.9(4) . . . . ?
C10 C3 C4 C5 93.0(3) . . . . ?
C10 C3 C4 C9 -85.1(3) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
C10 C15 O16 Ni1 21.0(3) . . . . ?
C11 C10 C15 C14 -0.2(3) . . . . ?
C11 C10 C15 O16 178.70(19) . . . . ?
C11 C12 C13 C14 -2.0(4) . . . . ?
C11 C12 C13 O19 176.9(2) . . . . ?
C12 C13 C14 C15 3.0(3) . . . . ?
C13 C14 C15 C10 -1.9(3) . . . . ?
C13 C14 C15 O16 179.19(18) . . . . ?
C14 C15 O16 Ni1 -160.17(14) . . . . ?
C15 C10 C11 C12 1.2(3) . . . . ?
O16 Ni1 N2 C1 -158.09(16) . . . . ?
O16 Ni1 N2 C3 17.52(19) . . . . ?
O16 Ni1 O16P C15P 161.63(17) . . . . ?
C16 C1 N2 Ni1 -74.9(2) . . . . ?
C16 C1 N2 C3 109.2(2) . . . . ?
C16 C1P N2P Ni1 -73.8(2) . . . . ?
C16 C1P N2P C3P 115.2(2) . . . . ?
O18 C16 C1P N2P 153.7(3) . . . . ?
O19 C13 C14 C15 -175.8(2) . . . . ?
C1P N2P C3P C4P -9.5(3) . . . . ?
C1P N2P C3P C10P 166.3(2) . . . . ?
N2P Ni1 N2 C1 29.83(16) . . . . ?
N2P Ni1 N2 C3 -154.56(18) . . . . ?
N2P Ni1 O16P C15P -27.02(17) . . . . ?
N2P C3P C4P C5P -74.1(3) . . . . ?
N2P C3P C4P C9P 107.5(3) . . . . ?
N2P C3P C10P C11P 171.5(2) . . . . ?
N2P C3P C10P C15P -16.6(3) . . . . ?
C3P C4P C5P C6P -177.4(3) . . . . ?
C3P C4P C9P C8P 178.8(3) . . . . ?
C3P C10P C11P C12P 169.3(2) . . . . ?
C3P C10P C15P C14P -167.04(19) . . . . ?
C3P C10P C15P O16P 10.2(3) . . . . ?
C4P C3P C10P C11P -12.5(3) . . . . ?
C4P C3P C10P C15P 159.3(2) . . . . ?
C4P C5P C6P C7P -2.3(5) . . . . ?
C5P C4P C9P C8P 0.4(5) . . . . ?
C5P C6P C7P C8P 2.1(6) . . . . ?
C6P C7P C8P C9P -0.6(6) . . . . ?
C7P C8P C9P C4P -0.6(6) . . . . ?
C9P C4P C5P C6P 1.0(4) . . . . ?
C10P C3P C4P C5P 109.8(3) . . . . ?
C10P C3P C4P C9P -68.5(3) . . . . ?
C10P C11P C12P C13P -1.3(3) . . . . ?
C10P C15P O16P Ni1 16.3(3) . . . . ?
C11P C10P C15P C14P 5.1(3) . . . . ?
C11P C10P C15P O16P -177.69(19) . . . . ?
C11P C12P C13P C14P 3.4(3) . . . . ?
C11P C12P C13P O19P -176.5(2) . . . . ?
C12P C13P C14P C15P -1.1(3) . . . . ?
C13P C14P C15P C10P -3.2(3) . . . . ?
C13P C14P C15P O16P 179.37(19) . . . . ?
C14P C15P O16P Ni1 -166.42(14) . . . . ?
C15P C10P C11P C12P -2.9(3) . . . . ?
O16P Ni1 O16 C15 161.04(16) . . . . ?
O16P Ni1 N2P C1P -149.63(16) . . . . ?
O16P Ni1 N2P C3P 20.58(19) . . . . ?
O18P C16 C1P N2P -85.9(3) . . . . ?
O19P C13P C14P C15P 178.78(19) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.091
_oxdiff_exptl_absorpt_empirical_full_min 0.932
####################################################################### 
# 
# 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_cmpd6_exp_118_tsb18
_database_code_depnum_ccdc_archive 'CCDC 1922293'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_audit_creation_date             2019-06-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
N,N'-Bis-(4-((1-(2-ethyl)piperidine)oxy)benzophenylidene)-1,2-propylenediaminenickel(II)
_chemical_formula_moiety         'C43 H50 N4 Ni O4'
_chemical_formula_sum            'C43 H50 N4 Ni O4'
_chemical_formula_weight         745.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         C49H64N4NiO4
_chemical_oxdiff_usercomment     'TSB18 from Sean Pham'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.83480(19)
_cell_length_b                   12.9908(2)
_cell_length_c                   16.1427(3)
_cell_angle_alpha                67.3813(17)
_cell_angle_beta                 74.2421(15)
_cell_angle_gamma                79.8434(15)
_cell_volume                     2197.62(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23700
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      30.0920
_cell_measurement_theta_min      1.7280
_shelx_estimated_absorpt_T_max   0.914
_shelx_estimated_absorpt_T_min   0.827
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             792
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method dichloromethane/hexane
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48728
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        27.102
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.704
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'HyPix Bantam HPC 3000'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 110.00   0.50   23.00    --   20.00  54.00 -15.23  368
  2  ω    -74.00 110.00   0.50   23.00    --   20.00  54.00-150.00  368
  3  ω    -74.00 109.50   0.50   23.00    --   20.00  54.00 106.96  367
  4  ω    -62.00  76.50   0.50   23.00    --   20.00  54.00 -91.64  277
  5  ω    -74.00  57.00   0.50   23.00    --   20.00  54.00 150.00  262
  6  ω     66.00 108.00   0.50   23.00    --   20.00  54.00 150.00   84
  7  ω    -67.00 -14.00   0.50   23.00    --   20.00  54.00  30.00  106
  8  ω      7.00  33.00   0.50   23.00    --   20.00  54.00  30.00   52
  9  ω     54.00  79.50   0.50   23.00    --   20.00  54.00  30.00   51
 10  ω    -71.00  86.00   0.50   23.00    --   20.00  54.00-101.07  314
 11  ω    -73.00  74.00   0.50   23.00    --   20.00  54.00-180.00  294
 12  ω    -73.00 -18.00   0.50   23.00    --   20.00  54.00   0.00  110
 13  ω     58.00 101.00   0.50   23.00    --   20.00  54.00   0.00   86
 14  ω    -74.00  25.00   0.50   23.00    --   20.00  54.00 -30.00  198
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0171994000
_diffrn_orient_matrix_UB_12      0.0348682000
_diffrn_orient_matrix_UB_13      0.0267407000
_diffrn_orient_matrix_UB_21      0.0510173000
_diffrn_orient_matrix_UB_22      0.0294452000
_diffrn_orient_matrix_UB_23      -0.0246565000
_diffrn_orient_matrix_UB_31      -0.0317019000
_diffrn_orient_matrix_UB_32      0.0379331000
_diffrn_orient_matrix_UB_33      -0.0326004000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8124
_reflns_number_total             9563
_reflns_odcompleteness_completeness 98.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         9563
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0542P)²+0.4620P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1000
_refine_special_details          
;2 molecules of hexane removed using Bypass. Disordered piperidine 
modelled as two-component disorder using the same fragment as a 
rigid group and with RIGU restraint. The disorder about the 
ethylenediamine backbone modelled as two-component disorder with 
DFIX restraints for the minor component.,SQUEEZE
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N18B, N18}
3. Restrained distances
 N1-C2P = C2P-C1P = C1P-N3 = C1P-C1MP
 1.5 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(N18B) = Uanis(N18)
5. Rigid body (RIGU) restrains
 N18, C19, C20, C21, C22, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23B, C22B, C21B, C20B, C19B, N18B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1MP)=Sof(H1MD)=Sof(H1ME)=Sof(H1MF)=Sof(C1P)=Sof(H1P)=Sof(C2P)=Sof(H2PA)=
 Sof(H2PB)=1-FVAR(1)
 Sof(C1ME)=Sof(H1MA)=Sof(H1MB)=Sof(H1MC)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
 Sof(H18C)=Sof(H18D)=Sof(C23B)=Sof(H23E)=Sof(H23F)=Sof(C22B)=Sof(H22E)=
 Sof(H22F)=Sof(C21B)=Sof(H21E)=Sof(H21F)=Sof(C20B)=Sof(H20E)=Sof(H20F)=
 Sof(C19B)=Sof(H19E)=Sof(H19F)=Sof(N18B)=1-FVAR(2)
 Sof(H18A)=Sof(H18B)=Sof(N18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=FVAR(2)
7.a Free rotating group:
 C23B(C22B,C21B,C20B,C19B,N18B)
7.b Ternary CH refined with riding coordinates:
 C1(H1), C1P(H1P)
7.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2P(H2PA,H2PB), C17(H17A,H17B), C18(H18A,H18B), C18(H18C,H18D),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
  C17P(H17C,H17D), C18P(H18E,H18F), C19P(H19C,H19D), C20P(H20C,H20D), C21P(H21C,
 H21D), C22P(H22C,H22D), C23P(H23C,H23D), C23B(H23E,H23F), C22B(H22E,H22F),
 C21B(H21E,H21F), C20B(H20E,H20F), C19B(H19E,H19F)
7.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C15(H15),
 C6P(H6P), C7P(H7P), C8P(H8P), C9P(H9P), C10P(H10P), C12P(H12P), C13P(H13P),
 C15P(H15P)
7.e Idealised Me refined as rotating group:
 C1ME(H1MA,H1MB,H1MC), C1MP(H1MD,H1ME,H1MF)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.50373(2) 0.28617(2) 0.51215(2) 0.03196(7) Uani 1 1 d . . . . .
N1 N 0.54024(11) 0.23475(12) 0.41534(9) 0.0367(3) Uani 1 1 d D . . . .
C1ME C 0.73246(19) 0.13154(19) 0.43608(16) 0.0449(6) Uani 0.852(5) 1 d . . P A
1
H1MA H 0.711915 0.130440 0.499445 0.067 Uiso 0.852(5) 1 calc GR . P A 1
H1MB H 0.817773 0.134567 0.412263 0.067 Uiso 0.852(5) 1 calc GR . P A 1
H1MC H 0.708342 0.063678 0.435135 0.067 Uiso 0.852(5) 1 calc GR . P A 1
C1 C 0.66990(18) 0.2330(2) 0.3767(2) 0.0383(6) Uani 0.852(5) 1 d . . P A 1
H1 H 0.687103 0.231919 0.312858 0.046 Uiso 0.852(5) 1 calc R . P A 1
C2 C 0.7041(2) 0.3413(2) 0.37333(15) 0.0370(6) Uani 0.852(5) 1 d . . P A 1
H2A H 0.790656 0.339661 0.363050 0.044 Uiso 0.852(5) 1 calc R . P A 1
H2B H 0.677405 0.405260 0.322858 0.044 Uiso 0.852(5) 1 calc R . P A 1
C1MP C 0.7802(11) 0.1738(8) 0.4413(9) 0.046(3) Uani 0.148(5) 1 d D . P A 2
H1MD H 0.719779 0.123594 0.483750 0.069 Uiso 0.148(5) 1 calc GR . P A 2
H1ME H 0.837422 0.175686 0.474545 0.069 Uiso 0.148(5) 1 calc GR . P A 2
H1MF H 0.820554 0.146569 0.391119 0.069 Uiso 0.148(5) 1 calc GR . P A 2
C1P C 0.7229(9) 0.2901(8) 0.4021(6) 0.038(4) Uani 0.148(5) 1 d D . P A 2
H1P H 0.786967 0.339052 0.359757 0.045 Uiso 0.148(5) 1 calc R . P A 2
C2P C 0.6482(8) 0.2810(15) 0.3439(6) 0.050(4) Uani 0.148(5) 1 d D . P A 2
H2PA H 0.687261 0.229349 0.310834 0.060 Uiso 0.148(5) 1 calc R . P A 2
H2PB H 0.629095 0.355009 0.298732 0.060 Uiso 0.148(5) 1 calc R . P A 2
N3 N 0.64560(11) 0.35167(12) 0.46331(9) 0.0356(3) Uani 1 1 d D . . . .
C4 C 0.68935(12) 0.41251(13) 0.49353(11) 0.0336(3) Uani 1 1 d . . . . .
C5 C 0.80621(13) 0.45924(14) 0.44170(11) 0.0366(3) Uani 1 1 d . . . . .
C6 C 0.81283(14) 0.56821(14) 0.38085(12) 0.0403(4) Uani 1 1 d . . . . .
H6 H 0.743029 0.615708 0.371418 0.048 Uiso 1 1 calc R . . . .
C7 C 0.92231(15) 0.60772(15) 0.33361(13) 0.0452(4) Uani 1 1 d . . . . .
H7 H 0.927230 0.682292 0.290805 0.054 Uiso 1 1 calc R . . . .
C8 C 1.02416(14) 0.54011(16) 0.34800(13) 0.0475(4) Uani 1 1 d . . . . .
H8 H 1.098751 0.568467 0.316003 0.057 Uiso 1 1 calc R . . . .
C9 C 1.01758(14) 0.43188(16) 0.40855(13) 0.0479(4) Uani 1 1 d . . . . .
H9 H 1.087676 0.385024 0.418268 0.057 Uiso 1 1 calc R . . . .
C10 C 0.90901(14) 0.39084(15) 0.45552(13) 0.0436(4) Uani 1 1 d . . . . .
H10 H 0.904635 0.315730 0.497326 0.052 Uiso 1 1 calc R . . . .
C11 C 0.63144(12) 0.43389(13) 0.57662(11) 0.0333(3) Uani 1 1 d . . . . .
C12 C 0.68190(14) 0.50074(14) 0.60625(12) 0.0395(4) Uani 1 1 d . . . . .
H12 H 0.752675 0.533678 0.568810 0.047 Uiso 1 1 calc R . . . .
C13 C 0.63339(14) 0.51985(15) 0.68604(13) 0.0455(4) Uani 1 1 d . . . . .
H13 H 0.669330 0.565842 0.703544 0.055 Uiso 1 1 calc R . . . .
C14 C 0.52947(14) 0.47072(15) 0.74227(12) 0.0426(4) Uani 1 1 d . . . . .
C15 C 0.47604(13) 0.40671(14) 0.71603(11) 0.0361(3) Uani 1 1 d . . . . .
H15 H 0.405017 0.375016 0.754348 0.043 Uiso 1 1 calc R . . . .
C16 C 0.52487(12) 0.38713(13) 0.63298(11) 0.0321(3) Uani 1 1 d . . . . .
O16 O 0.46713(9) 0.32564(10) 0.61378(7) 0.0372(2) Uani 1 1 d . . . . .
C17 C 0.37899(16) 0.44678(19) 0.88031(13) 0.0535(5) Uani 1 1 d . . . . .
H17A H 0.389026 0.364068 0.901472 0.064 Uiso 1 1 calc R . . . .
H17B H 0.314783 0.473182 0.846614 0.064 Uiso 1 1 calc R . . . .
O17 O 0.48663(11) 0.49338(13) 0.82156(10) 0.0587(4) Uani 1 1 d . . . . .
C18 C 0.3499(2) 0.4850(3) 0.96129(19) 0.0916(9) Uani 1 1 d . . . . .
H18A H 0.418466 0.465770 0.989984 0.110 Uiso 0.679(3) 1 calc R . P B 1
H18B H 0.333171 0.567263 0.939785 0.110 Uiso 0.679(3) 1 calc R . P B 1
H18C H 0.418466 0.465770 0.989984 0.110 Uiso 0.321(3) 1 calc R . P B 2
H18D H 0.333171 0.567263 0.939785 0.110 Uiso 0.321(3) 1 calc R . P B 2
N18 N 0.24917(14) 0.43292(16) 1.02865(11) 0.0581(4) Uani 0.679(3) 1 d . U P B 1
C19 C 0.2898(4) 0.3322(4) 1.0887(3) 0.0869(13) Uani 0.679(3) 1 d . U P B 1
H19A H 0.340685 0.347748 1.121375 0.104 Uiso 0.679(3) 1 calc R . P B 1
H19B H 0.338260 0.286644 1.052719 0.104 Uiso 0.679(3) 1 calc R . P B 1
C20 C 0.1917(5) 0.2669(4) 1.1577(3) 0.1148(19) Uani 0.679(3) 1 d . U P B 1
H20A H 0.144752 0.245207 1.125641 0.138 Uiso 0.679(3) 1 calc R . P B 1
H20B H 0.224818 0.197595 1.200127 0.138 Uiso 0.679(3) 1 calc R . P B 1
C21 C 0.1145(7) 0.3328(8) 1.2112(5) 0.123(3) Uani 0.679(3) 1 d . U P B 1
H21A H 0.158452 0.345875 1.249936 0.148 Uiso 0.679(3) 1 calc R . P B 1
H21B H 0.046260 0.290404 1.252430 0.148 Uiso 0.679(3) 1 calc R . P B 1
C22 C 0.0721(6) 0.4416(6) 1.1485(4) 0.0959(17) Uani 0.679(3) 1 d . U P B 1
H22A H 0.026359 0.487687 1.184903 0.115 Uiso 0.679(3) 1 calc R . P B 1
H22B H 0.019541 0.428703 1.115733 0.115 Uiso 0.679(3) 1 calc R . P B 1
C23 C 0.1764(3) 0.5041(3) 1.0784(3) 0.0798(12) Uani 0.679(3) 1 d . U P B 1
H23A H 0.146893 0.574002 1.034208 0.096 Uiso 0.679(3) 1 calc R . P B 1
H23B H 0.224473 0.524285 1.110560 0.096 Uiso 0.679(3) 1 calc R . P B 1
C4P C 0.47158(13) 0.19109(13) 0.38870(11) 0.0354(3) Uani 1 1 d . . . . .
C5P C 0.52088(13) 0.14954(15) 0.31027(12) 0.0394(4) Uani 1 1 d . . . . .
C6P C 0.53683(15) 0.22320(16) 0.21987(12) 0.0468(4) Uani 1 1 d . . . . .
H6P H 0.515367 0.300897 0.206749 0.056 Uiso 1 1 calc R . . . .
C7P C 0.58434(17) 0.18270(18) 0.14872(13) 0.0540(5) Uani 1 1 d . . . . .
H7P H 0.595028 0.232816 0.086640 0.065 Uiso 1 1 calc R . . . .
C8P C 0.61611(17) 0.07025(18) 0.16754(14) 0.0546(5) Uani 1 1 d . . . . .
H8P H 0.649902 0.043407 0.118385 0.065 Uiso 1 1 calc R . . . .
C9P C 0.59926(16) -0.00342(17) 0.25695(13) 0.0496(4) Uani 1 1 d . . . . .
H9P H 0.620773 -0.081036 0.269619 0.060 Uiso 1 1 calc R . . . .
C10P C 0.55062(14) 0.03613(16) 0.32875(12) 0.0429(4) Uani 1 1 d . . . . .
H10P H 0.537732 -0.014679 0.390640 0.052 Uiso 1 1 calc R . . . .
C11P C 0.34963(13) 0.17713(14) 0.43435(11) 0.0362(3) Uani 1 1 d . . . . .
C12P C 0.27396(13) 0.14270(14) 0.39691(12) 0.0402(4) Uani 1 1 d . . . . .
H12P H 0.304102 0.132529 0.339466 0.048 Uiso 1 1 calc R . . . .
C13P C 0.15940(13) 0.12368(15) 0.44049(12) 0.0421(4) Uani 1 1 d . . . . .
H13P H 0.110113 0.102681 0.412952 0.050 Uiso 1 1 calc R . . . .
C14P C 0.11558(13) 0.13548(14) 0.52609(12) 0.0388(4) Uani 1 1 d . . . . .
C15P C 0.18531(13) 0.16922(14) 0.56539(12) 0.0386(4) Uani 1 1 d . . . . .
H15P H 0.154037 0.176670 0.623766 0.046 Uiso 1 1 calc R . . . .
C16P C 0.30251(13) 0.19270(13) 0.51962(11) 0.0346(3) Uani 1 1 d . . . . .
O16P O 0.36139(9) 0.22613(9) 0.56117(7) 0.0371(2) Uani 1 1 d . . . . .
C17P C -0.04767(14) 0.12953(17) 0.65152(13) 0.0490(4) Uani 1 1 d . . . . .
H17C H -0.038675 0.206965 0.644540 0.059 Uiso 1 1 calc R . . . .
H17D H -0.007421 0.076939 0.699877 0.059 Uiso 1 1 calc R . . . .
O17P O 0.00126(9) 0.11201(11) 0.56625(9) 0.0464(3) Uani 1 1 d . . . . .
C18P C -0.17652(15) 0.10914(18) 0.67684(13) 0.0499(4) Uani 1 1 d . . . . .
H18E H -0.218496 0.171070 0.634596 0.060 Uiso 1 1 calc R . . . .
H18F H -0.184553 0.038816 0.669358 0.060 Uiso 1 1 calc R . . . .
N18P N -0.23029(12) 0.10133(12) 0.77166(10) 0.0436(3) Uani 1 1 d . . . . .
C19P C -0.35112(17) 0.0706(2) 0.79467(14) 0.0592(5) Uani 1 1 d . . . . .
H19C H -0.350473 -0.000386 0.785173 0.071 Uiso 1 1 calc R . . . .
H19D H -0.396926 0.129393 0.753366 0.071 Uiso 1 1 calc R . . . .
C20P C -0.40928(18) 0.05697(19) 0.89397(14) 0.0610(5) Uani 1 1 d . . . . .
H20C H -0.490844 0.036217 0.908403 0.073 Uiso 1 1 calc R . . . .
H20D H -0.365410 -0.003949 0.935419 0.073 Uiso 1 1 calc R . . . .
C21P C -0.41128(17) 0.16360(17) 0.90984(13) 0.0540(5) Uani 1 1 d . . . . .
H21C H -0.443899 0.152109 0.975811 0.065 Uiso 1 1 calc R . . . .
H21D H -0.462446 0.222599 0.873604 0.065 Uiso 1 1 calc R . . . .
C22P C -0.28884(19) 0.19968(19) 0.88156(14) 0.0601(5) Uani 1 1 d . . . . .
H22C H -0.240753 0.145352 0.923481 0.072 Uiso 1 1 calc R . . . .
H22D H -0.291433 0.273575 0.886783 0.072 Uiso 1 1 calc R . . . .
C23P C -0.23206(17) 0.20731(16) 0.78341(13) 0.0503(4) Uani 1 1 d . . . . .
H23C H -0.276295 0.266363 0.741010 0.060 Uiso 1 1 calc R . . . .
H23D H -0.150409 0.228576 0.767282 0.060 Uiso 1 1 calc R . . . .
C23B C 0.1559(4) 0.5089(6) 1.0068(3) 0.068(2) Uani 0.321(3) 1 d . U P B 2
H23E H 0.155262 0.525814 0.941615 0.081 Uiso 0.321(3) 1 calc R . P B 2
H23F H 0.166874 0.579253 1.012867 0.081 Uiso 0.321(3) 1 calc R . P B 2
C22B C 0.0371(4) 0.4681(6) 1.0672(4) 0.075(2) Uani 0.321(3) 1 d G U P B 2
H22E H -0.026767 0.525426 1.047234 0.090 Uiso 0.321(3) 1 calc R . P B 2
H22F H 0.024331 0.398713 1.060422 0.090 Uiso 0.321(3) 1 calc R . P B 2
C21B C 0.0335(5) 0.4456(10) 1.1661(3) 0.115(6) Uani 0.321(3) 1 d G U P B 2
H21E H 0.037262 0.516602 1.174262 0.138 Uiso 0.321(3) 1 calc R . P B 2
H21F H -0.041381 0.413793 1.205250 0.138 Uiso 0.321(3) 1 calc R . P B 2
C20B C 0.1347(6) 0.3657(9) 1.1947(3) 0.105(6) Uani 0.321(3) 1 d G U P B 2
H20E H 0.124509 0.291648 1.194811 0.126 Uiso 0.321(3) 1 calc R . P B 2
H20F H 0.136003 0.356935 1.258116 0.126 Uiso 0.321(3) 1 calc R . P B 2
C19B C 0.2516(5) 0.4061(8) 1.1302(4) 0.096(3) Uani 0.321(3) 1 d G U P B 2
H19E H 0.315843 0.347636 1.147049 0.116 Uiso 0.321(3) 1 calc R . P B 2
H19F H 0.267838 0.474065 1.137321 0.116 Uiso 0.321(3) 1 calc R . P B 2
N18B N 0.24917(14) 0.43292(16) 1.02865(11) 0.0581(4) Uani 0.321(3) 1 d G U P B
2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.8466(13) . ?
Ni1 N3 1.8530(12) . ?
Ni1 O16 1.8233(10) . ?
Ni1 O16P 1.8268(10) . ?
N1 C1 1.491(2) . ?
N1 C2P 1.504(5) . ?
N1 C4P 1.3065(19) . ?
C1ME H1MA 0.9800 . ?
C1ME H1MB 0.9800 . ?
C1ME H1MC 0.9800 . ?
C1ME C1 1.508(3) . ?
C1 H1 1.0000 . ?
C1 C2 1.509(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 N3 1.476(2) . ?
C1MP H1MD 0.9800 . ?
C1MP H1ME 0.9800 . ?
C1MP H1MF 0.9800 . ?
C1MP C1P 1.510(5) . ?
C1P H1P 1.0000 . ?
C1P C2P 1.501(5) . ?
C1P N3 1.520(5) . ?
C2P H2PA 0.9900 . ?
C2P H2PB 0.9900 . ?
N3 C4 1.3072(19) . ?
C4 C5 1.503(2) . ?
C4 C11 1.437(2) . ?
C5 C6 1.379(2) . ?
C5 C10 1.390(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.386(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.378(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.371(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.413(2) . ?
C11 C16 1.418(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.358(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.403(2) . ?
C14 C15 1.368(2) . ?
C14 O17 1.3662(19) . ?
C15 H15 0.9500 . ?
C15 C16 1.409(2) . ?
C16 O16 1.3035(17) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 O17 1.436(2) . ?
C17 C18 1.506(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 H18C 0.9900 . ?
C18 H18D 0.9900 . ?
C18 N18 1.440(3) . ?
C18 N18B 1.440(3) . ?
N18 C19 1.392(4) . ?
N18 C23 1.468(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.492(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.476(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.483(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.534(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C4P C5P 1.499(2) . ?
C4P C11P 1.439(2) . ?
C5P C6P 1.386(3) . ?
C5P C10P 1.385(2) . ?
C6P H6P 0.9500 . ?
C6P C7P 1.386(2) . ?
C7P H7P 0.9500 . ?
C7P C8P 1.376(3) . ?
C8P H8P 0.9500 . ?
C8P C9P 1.374(3) . ?
C9P H9P 0.9500 . ?
C9P C10P 1.389(2) . ?
C10P H10P 0.9500 . ?
C11P C12P 1.418(2) . ?
C11P C16P 1.416(2) . ?
C12P H12P 0.9500 . ?
C12P C13P 1.364(2) . ?
C13P H13P 0.9500 . ?
C13P C14P 1.395(2) . ?
C14P C15P 1.379(2) . ?
C14P O17P 1.3641(18) . ?
C15P H15P 0.9500 . ?
C15P C16P 1.408(2) . ?
C16P O16P 1.3071(17) . ?
C17P H17C 0.9900 . ?
C17P H17D 0.9900 . ?
C17P O17P 1.429(2) . ?
C17P C18P 1.511(2) . ?
C18P H18E 0.9900 . ?
C18P H18F 0.9900 . ?
C18P N18P 1.460(2) . ?
N18P C19P 1.463(2) . ?
N18P C23P 1.456(2) . ?
C19P H19C 0.9900 . ?
C19P H19D 0.9900 . ?
C19P C20P 1.516(3) . ?
C20P H20C 0.9900 . ?
C20P H20D 0.9900 . ?
C20P C21P 1.498(3) . ?
C21P H21C 0.9900 . ?
C21P H21D 0.9900 . ?
C21P C22P 1.498(3) . ?
C22P H22C 0.9900 . ?
C22P H22D 0.9900 . ?
C22P C23P 1.515(2) . ?
C23P H23C 0.9900 . ?
C23P H23D 0.9900 . ?
C23B H23E 0.9900 . ?
C23B H23F 0.9900 . ?
C23B C22B 1.5264 . ?
C23B N18B 1.370(5) . ?
C22B H22E 0.9900 . ?
C22B H22F 0.9900 . ?
C22B C21B 1.4976 . ?
C21B H21E 0.9900 . ?
C21B H21F 0.9900 . ?
C21B C20B 1.4896 . ?
C20B H20E 0.9900 . ?
C20B H20F 0.9900 . ?
C20B C19B 1.5248 . ?
C19B H19E 0.9900 . ?
C19B H19F 0.9900 . ?
C19B N18B 1.546(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 87.62(5) . . ?
O16 Ni1 N1 175.54(6) . . ?
O16 Ni1 N3 94.68(5) . . ?
O16 Ni1 O16P 83.87(4) . . ?
O16P Ni1 N1 93.93(5) . . ?
O16P Ni1 N3 177.94(5) . . ?
C1 N1 Ni1 109.52(12) . . ?
C2P N1 Ni1 113.5(5) . . ?
C4P N1 Ni1 128.39(11) . . ?
C4P N1 C1 121.50(15) . . ?
C4P N1 C2P 115.3(5) . . ?
H1MA C1ME H1MB 109.5 . . ?
H1MA C1ME H1MC 109.5 . . ?
H1MB C1ME H1MC 109.5 . . ?
C1 C1ME H1MA 109.5 . . ?
C1 C1ME H1MB 109.5 . . ?
C1 C1ME H1MC 109.5 . . ?
N1 C1 C1ME 110.59(19) . . ?
N1 C1 H1 109.6 . . ?
N1 C1 C2 104.77(18) . . ?
C1ME C1 H1 109.6 . . ?
C1ME C1 C2 112.7(2) . . ?
C2 C1 H1 109.6 . . ?
C1 C2 H2A 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N3 C2 C1 106.18(18) . . ?
N3 C2 H2A 110.5 . . ?
N3 C2 H2B 110.5 . . ?
H1MD C1MP H1ME 109.5 . . ?
H1MD C1MP H1MF 109.5 . . ?
H1ME C1MP H1MF 109.5 . . ?
C1P C1MP H1MD 109.5 . . ?
C1P C1MP H1ME 109.5 . . ?
C1P C1MP H1MF 109.5 . . ?
C1MP C1P H1P 107.3 . . ?
C1MP C1P N3 122.1(8) . . ?
C2P C1P C1MP 105.4(12) . . ?
C2P C1P H1P 107.3 . . ?
C2P C1P N3 106.8(8) . . ?
N3 C1P H1P 107.3 . . ?
N1 C2P H2PA 111.5 . . ?
N1 C2P H2PB 111.5 . . ?
C1P C2P N1 101.5(8) . . ?
C1P C2P H2PA 111.5 . . ?
C1P C2P H2PB 111.5 . . ?
H2PA C2P H2PB 109.3 . . ?
C2 N3 Ni1 111.73(12) . . ?
C1P N3 Ni1 106.7(5) . . ?
C4 N3 Ni1 128.27(11) . . ?
C4 N3 C2 119.55(14) . . ?
C4 N3 C1P 122.0(5) . . ?
N3 C4 C5 119.29(13) . . ?
N3 C4 C11 122.39(13) . . ?
C11 C4 C5 118.29(13) . . ?
C6 C5 C4 121.13(14) . . ?
C6 C5 C10 119.80(14) . . ?
C10 C5 C4 119.07(15) . . ?
C5 C6 H6 120.3 . . ?
C5 C6 C7 119.34(16) . . ?
C7 C6 H6 120.3 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.79(17) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.86(15) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.06(16) . . ?
C10 C9 H9 120.0 . . ?
C5 C10 H10 119.9 . . ?
C9 C10 C5 120.15(17) . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C4 120.32(14) . . ?
C12 C11 C16 117.56(14) . . ?
C16 C11 C4 122.10(13) . . ?
C11 C12 H12 118.6 . . ?
C13 C12 C11 122.72(15) . . ?
C13 C12 H12 118.6 . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 119.09(15) . . ?
C14 C13 H13 120.5 . . ?
C15 C14 C13 120.50(15) . . ?
O17 C14 C13 115.55(14) . . ?
O17 C14 C15 123.93(15) . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 120.95(14) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C11 119.16(13) . . ?
O16 C16 C11 124.48(13) . . ?
O16 C16 C15 116.36(13) . . ?
C16 O16 Ni1 127.78(10) . . ?
H17A C17 H17B 108.5 . . ?
O17 C17 H17A 110.3 . . ?
O17 C17 H17B 110.3 . . ?
O17 C17 C18 107.21(15) . . ?
C18 C17 H17A 110.3 . . ?
C18 C17 H17B 110.3 . . ?
C14 O17 C17 117.49(13) . . ?
C17 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C17 C18 H18C 109.4 . . ?
C17 C18 H18D 109.4 . . ?
H18A C18 H18B 108.0 . . ?
H18C C18 H18D 108.0 . . ?
N18 C18 C17 110.99(18) . . ?
N18 C18 H18A 109.4 . . ?
N18 C18 H18B 109.4 . . ?
N18B C18 C17 110.99(18) . . ?
N18B C18 H18C 109.4 . . ?
N18B C18 H18D 109.4 . . ?
C18 N18 C23 113.6(2) . . ?
C19 N18 C18 107.8(3) . . ?
C19 N18 C23 111.5(2) . . ?
N18 C19 H19A 109.1 . . ?
N18 C19 H19B 109.1 . . ?
N18 C19 C20 112.4(3) . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 C19 111.2(5) . . ?
C21 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
C20 C21 H21A 109.6 . . ?
C20 C21 H21B 109.6 . . ?
C20 C21 C22 110.3(5) . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 H21A 109.6 . . ?
C22 C21 H21B 109.6 . . ?
C21 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C21 C22 C23 110.5(5) . . ?
H22A C22 H22B 108.1 . . ?
C23 C22 H22A 109.6 . . ?
C23 C22 H22B 109.6 . . ?
N18 C23 C22 109.7(4) . . ?
N18 C23 H23A 109.7 . . ?
N18 C23 H23B 109.7 . . ?
C22 C23 H23A 109.7 . . ?
C22 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
N1 C4P C5P 119.75(13) . . ?
N1 C4P C11P 122.29(14) . . ?
C11P C4P C5P 117.92(13) . . ?
C6P C5P C4P 120.75(15) . . ?
C10P C5P C4P 119.39(15) . . ?
C10P C5P C6P 119.86(15) . . ?
C5P C6P H6P 120.2 . . ?
C5P C6P C7P 119.53(18) . . ?
C7P C6P H6P 120.2 . . ?
C6P C7P H7P 119.8 . . ?
C8P C7P C6P 120.35(19) . . ?
C8P C7P H7P 119.8 . . ?
C7P C8P H8P 119.8 . . ?
C9P C8P C7P 120.43(17) . . ?
C9P C8P H8P 119.8 . . ?
C8P C9P H9P 120.2 . . ?
C8P C9P C10P 119.69(18) . . ?
C10P C9P H9P 120.2 . . ?
C5P C10P C9P 120.12(17) . . ?
C5P C10P H10P 119.9 . . ?
C9P C10P H10P 119.9 . . ?
C12P C11P C4P 120.77(14) . . ?
C16P C11P C4P 121.32(13) . . ?
C16P C11P C12P 117.86(14) . . ?
C11P C12P H12P 118.9 . . ?
C13P C12P C11P 122.29(15) . . ?
C13P C12P H12P 118.9 . . ?
C12P C13P H13P 120.5 . . ?
C12P C13P C14P 119.10(14) . . ?
C14P C13P H13P 120.5 . . ?
C15P C14P C13P 120.92(14) . . ?
O17P C14P C13P 115.49(13) . . ?
O17P C14P C15P 123.59(14) . . ?
C14P C15P H15P 119.8 . . ?
C14P C15P C16P 120.47(15) . . ?
C16P C15P H15P 119.8 . . ?
C15P C16P C11P 119.28(13) . . ?
O16P C16P C11P 124.41(13) . . ?
O16P C16P C15P 116.30(14) . . ?
C16P O16P Ni1 126.87(10) . . ?
H17C C17P H17D 108.6 . . ?
O17P C17P H17C 110.4 . . ?
O17P C17P H17D 110.4 . . ?
O17P C17P C18P 106.48(13) . . ?
C18P C17P H17C 110.4 . . ?
C18P C17P H17D 110.4 . . ?
C14P O17P C17P 116.53(12) . . ?
C17P C18P H18E 109.4 . . ?
C17P C18P H18F 109.4 . . ?
H18E C18P H18F 108.0 . . ?
N18P C18P C17P 111.36(14) . . ?
N18P C18P H18E 109.4 . . ?
N18P C18P H18F 109.4 . . ?
C18P N18P C19P 108.60(13) . . ?
C23P N18P C18P 111.27(14) . . ?
C23P N18P C19P 109.26(14) . . ?
N18P C19P H19C 109.5 . . ?
N18P C19P H19D 109.5 . . ?
N18P C19P C20P 110.59(16) . . ?
H19C C19P H19D 108.1 . . ?
C20P C19P H19C 109.5 . . ?
C20P C19P H19D 109.5 . . ?
C19P C20P H20C 109.6 . . ?
C19P C20P H20D 109.6 . . ?
H20C C20P H20D 108.1 . . ?
C21P C20P C19P 110.42(17) . . ?
C21P C20P H20C 109.6 . . ?
C21P C20P H20D 109.6 . . ?
C20P C21P H21C 109.7 . . ?
C20P C21P H21D 109.7 . . ?
C20P C21P C22P 109.71(16) . . ?
H21C C21P H21D 108.2 . . ?
C22P C21P H21C 109.7 . . ?
C22P C21P H21D 109.7 . . ?
C21P C22P H22C 109.4 . . ?
C21P C22P H22D 109.4 . . ?
C21P C22P C23P 111.04(16) . . ?
H22C C22P H22D 108.0 . . ?
C23P C22P H22C 109.4 . . ?
C23P C22P H22D 109.4 . . ?
N18P C23P C22P 111.35(15) . . ?
N18P C23P H23C 109.4 . . ?
N18P C23P H23D 109.4 . . ?
C22P C23P H23C 109.4 . . ?
C22P C23P H23D 109.4 . . ?
H23C C23P H23D 108.0 . . ?
H23E C23B H23F 107.7 . . ?
C22B C23B H23E 108.9 . . ?
C22B C23B H23F 108.9 . . ?
N18B C23B H23E 108.9 . . ?
N18B C23B H23F 108.9 . . ?
N18B C23B C22B 113.3(3) . . ?
C23B C22B H22E 109.6 . . ?
C23B C22B H22F 109.6 . . ?
H22E C22B H22F 108.1 . . ?
C21B C22B C23B 110.3 . . ?
C21B C22B H22E 109.6 . . ?
C21B C22B H22F 109.6 . . ?
C22B C21B H21E 109.7 . . ?
C22B C21B H21F 109.7 . . ?
H21E C21B H21F 108.2 . . ?
C20B C21B C22B 109.9 . . ?
C20B C21B H21E 109.7 . . ?
C20B C21B H21F 109.7 . . ?
C21B C20B H20E 109.3 . . ?
C21B C20B H20F 109.3 . . ?
C21B C20B C19B 111.5 . . ?
H20E C20B H20F 108.0 . . ?
C19B C20B H20E 109.3 . . ?
C19B C20B H20F 109.3 . . ?
C20B C19B H19E 109.4 . . ?
C20B C19B H19F 109.4 . . ?
C20B C19B N18B 111.3(2) . . ?
H19E C19B H19F 108.0 . . ?
N18B C19B H19E 109.4 . . ?
N18B C19B H19F 109.4 . . ?
C18 N18B C19B 115.5(3) . . ?
C23B N18B C18 104.1(3) . . ?
C23B N18B C19B 109.5(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N1 C1 C1ME 79.01(19) . . . . ?
Ni1 N1 C1 C2 -42.6(2) . . . . ?
Ni1 N1 C2P C1P 34.2(12) . . . . ?
Ni1 N1 C4P C5P -177.16(12) . . . . ?
Ni1 N1 C4P C11P 0.4(2) . . . . ?
Ni1 N3 C4 C5 -178.96(11) . . . . ?
Ni1 N3 C4 C11 3.0(2) . . . . ?
N1 Ni1 N3 C2 6.19(14) . . . . ?
N1 Ni1 N3 C1P -21.4(4) . . . . ?
N1 Ni1 N3 C4 178.31(15) . . . . ?
N1 Ni1 O16P C16P -17.64(14) . . . . ?
N1 C1 C2 N3 46.3(3) . . . . ?
N1 C4P C5P C6P -80.5(2) . . . . ?
N1 C4P C5P C10P 99.59(19) . . . . ?
N1 C4P C11P C12P 172.00(16) . . . . ?
N1 C4P C11P C16P -10.6(3) . . . . ?
C1ME C1 C2 N3 -73.9(2) . . . . ?
C1 N1 C4P C5P -6.9(3) . . . . ?
C1 N1 C4P C11P 170.66(18) . . . . ?
C1 C2 N3 Ni1 -31.4(2) . . . . ?
C1 C2 N3 C4 155.72(18) . . . . ?
C2 N3 C4 C5 -7.4(2) . . . . ?
C2 N3 C4 C11 174.58(17) . . . . ?
C1MP C1P C2P N1 81.0(11) . . . . ?
C1MP C1P N3 Ni1 -74.4(11) . . . . ?
C1MP C1P N3 C4 87.4(11) . . . . ?
C1P N3 C4 C5 23.4(5) . . . . ?
C1P N3 C4 C11 -154.6(5) . . . . ?
C2P N1 C4P C5P 23.4(8) . . . . ?
C2P N1 C4P C11P -159.0(8) . . . . ?
C2P C1P N3 Ni1 46.6(9) . . . . ?
C2P C1P N3 C4 -151.6(7) . . . . ?
N3 Ni1 N1 C1 21.32(14) . . . . ?
N3 Ni1 N1 C2P -7.8(7) . . . . ?
N3 Ni1 N1 C4P -167.53(16) . . . . ?
N3 Ni1 O16 C16 4.64(14) . . . . ?
N3 C1P C2P N1 -50.2(13) . . . . ?
N3 C4 C5 C6 98.69(19) . . . . ?
N3 C4 C5 C10 -81.1(2) . . . . ?
N3 C4 C11 C12 -179.64(15) . . . . ?
N3 C4 C11 C16 2.2(2) . . . . ?
C4 C5 C6 C7 -179.26(14) . . . . ?
C4 C5 C10 C9 179.92(15) . . . . ?
C4 C11 C12 C13 -177.27(16) . . . . ?
C4 C11 C16 C15 176.67(14) . . . . ?
C4 C11 C16 O16 -3.1(2) . . . . ?
C5 C4 C11 C12 2.3(2) . . . . ?
C5 C4 C11 C16 -175.86(14) . . . . ?
C5 C6 C7 C8 -1.1(2) . . . . ?
C6 C5 C10 C9 0.1(2) . . . . ?
C6 C7 C8 C9 1.1(3) . . . . ?
C7 C8 C9 C10 -0.4(3) . . . . ?
C8 C9 C10 C5 -0.2(3) . . . . ?
C10 C5 C6 C7 0.6(2) . . . . ?
C11 C4 C5 C6 -83.19(19) . . . . ?
C11 C4 C5 C10 96.99(18) . . . . ?
C11 C12 C13 C14 0.6(3) . . . . ?
C11 C16 O16 Ni1 -1.3(2) . . . . ?
C12 C11 C16 C15 -1.5(2) . . . . ?
C12 C11 C16 O16 178.68(15) . . . . ?
C12 C13 C14 C15 -1.6(3) . . . . ?
C12 C13 C14 O17 179.61(16) . . . . ?
C13 C14 C15 C16 1.0(3) . . . . ?
C13 C14 O17 C17 178.70(17) . . . . ?
C14 C15 C16 C11 0.6(2) . . . . ?
C14 C15 C16 O16 -179.63(15) . . . . ?
C15 C14 O17 C17 0.0(3) . . . . ?
C15 C16 O16 Ni1 178.90(10) . . . . ?
C16 C11 C12 C13 1.0(2) . . . . ?
O16 Ni1 N3 C2 -177.64(14) . . . . ?
O16 Ni1 N3 C1P 154.8(4) . . . . ?
O16 Ni1 N3 C4 -5.52(15) . . . . ?
O16 Ni1 O16P C16P 166.26(13) . . . . ?
C17 C18 N18 C19 88.5(3) . . . . ?
C17 C18 N18 C23 -147.4(3) . . . . ?
C17 C18 N18B C23B -94.3(4) . . . . ?
C17 C18 N18B C19B 145.6(4) . . . . ?
O17 C14 C15 C16 179.70(15) . . . . ?
O17 C17 C18 N18 -174.2(2) . . . . ?
O17 C17 C18 N18B -174.2(2) . . . . ?
C18 C17 O17 C14 -179.1(2) . . . . ?
C18 N18 C19 C20 -175.9(3) . . . . ?
C18 N18 C23 C22 -179.8(3) . . . . ?
N18 C19 C20 C21 -57.0(6) . . . . ?
C19 N18 C23 C22 -57.7(4) . . . . ?
C19 C20 C21 C22 54.1(8) . . . . ?
C20 C21 C22 C23 -54.2(8) . . . . ?
C21 C22 C23 N18 55.4(6) . . . . ?
C23 N18 C19 C20 58.8(4) . . . . ?
C4P N1 C1 C1ME -92.9(2) . . . . ?
C4P N1 C1 C2 145.48(19) . . . . ?
C4P N1 C2P C1P -163.2(7) . . . . ?
C4P C5P C6P C7P 178.98(15) . . . . ?
C4P C5P C10P C9P -178.32(14) . . . . ?
C4P C11P C12P C13P 176.91(16) . . . . ?
C4P C11P C16P C15P -174.81(15) . . . . ?
C4P C11P C16P O16P 3.9(3) . . . . ?
C5P C4P C11P C12P -10.4(2) . . . . ?
C5P C4P C11P C16P 167.01(15) . . . . ?
C5P C6P C7P C8P -0.4(3) . . . . ?
C6P C5P C10P C9P 1.7(2) . . . . ?
C6P C7P C8P C9P 1.1(3) . . . . ?
C7P C8P C9P C10P -0.5(3) . . . . ?
C8P C9P C10P C5P -1.0(3) . . . . ?
C10P C5P C6P C7P -1.1(2) . . . . ?
C11P C4P C5P C6P 101.84(18) . . . . ?
C11P C4P C5P C10P -78.1(2) . . . . ?
C11P C12P C13P C14P -1.8(3) . . . . ?
C11P C16P O16P Ni1 13.0(2) . . . . ?
C12P C11P C16P C15P 2.6(2) . . . . ?
C12P C11P C16P O16P -178.70(15) . . . . ?
C12P C13P C14P C15P 2.0(3) . . . . ?
C12P C13P C14P O17P -178.27(16) . . . . ?
C13P C14P C15P C16P 0.1(3) . . . . ?
C13P C14P O17P C17P -176.60(16) . . . . ?
C14P C15P C16P C11P -2.4(3) . . . . ?
C14P C15P C16P O16P 178.77(15) . . . . ?
C15P C14P O17P C17P 3.1(2) . . . . ?
C15P C16P O16P Ni1 -168.33(11) . . . . ?
C16P C11P C12P C13P -0.5(3) . . . . ?
O16P Ni1 N1 C1 -160.05(14) . . . . ?
O16P Ni1 N1 C2P 170.9(7) . . . . ?
O16P Ni1 N1 C4P 11.11(16) . . . . ?
O16P Ni1 O16 C16 -173.89(13) . . . . ?
C17P C18P N18P C19P -174.43(17) . . . . ?
C17P C18P N18P C23P 65.3(2) . . . . ?
O17P C14P C15P C16P -179.60(15) . . . . ?
O17P C17P C18P N18P 167.95(15) . . . . ?
C18P C17P O17P C14P 174.51(15) . . . . ?
C18P N18P C19P C20P 177.77(18) . . . . ?
C18P N18P C23P C22P 179.48(16) . . . . ?
N18P C19P C20P C21P 59.2(2) . . . . ?
C19P N18P C23P C22P 59.6(2) . . . . ?
C19P C20P C21P C22P -55.1(2) . . . . ?
C20P C21P C22P C23P 54.0(2) . . . . ?
C21P C22P C23P N18P -57.0(2) . . . . ?
C23P N18P C19P C20P -60.7(2) . . . . ?
C23B C22B C21B C20B -55.1 . . . . ?
C22B C23B N18B C18 177.0(4) . . . . ?
C22B C23B N18B C19B -58.9(6) . . . . ?
C22B C21B C20B C19B 53.7 . . . . ?
C21B C20B C19B N18B -53.1(3) . . . . ?
C20B C19B N18B C18 172.5(4) . . . . ?
C20B C19B N18B C23B 55.4(7) . . . . ?
N18B C23B C22B C21B 60.7(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 444.1 113.1 '2 hexane'

_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.076
_oxdiff_exptl_absorpt_empirical_full_min 0.941
####################################################################### 
# 
# 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_cmpd3_exp_131_tsb
_database_code_depnum_ccdc_archive 'CCDC 1922292'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_audit_creation_date             2019-06-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        
N,N'-Bis-(4-(hydroxybenzophenylidene))ethylenediaminenickel(II)
_chemical_name_common            ?
_chemical_formula_moiety         'C28 H22 N2 Ni O4, 2(C2 D6 O S)'
_chemical_formula_sum            'C32 H22 D12 N2 Ni O6 S2'
_chemical_formula_weight         677.51
_exptl_crystal_recrystallization_method 'From a solution of d6-DMSO'
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            'clear orange'
_diffrn_ambient_temperature      150.00(10)
_chemical_oxdiff_formula         'C32 H22 D12 N2 Ni O6 S2'
_chemical_oxdiff_usercomment     'TSB 3_P from DMSO'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.4100(2)
_cell_length_b                   9.8299(2)
_cell_length_c                   21.9572(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.1632(18)
_cell_angle_gamma                90
_cell_volume                     3486.30(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20757
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.5510
_cell_measurement_theta_min      1.8050
_shelx_estimated_absorpt_T_max   0.932
_shelx_estimated_absorpt_T_min   0.715
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            64412
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         1.702
_diffrn_ambient_environment      N~2~
_diffrn_detector                 'HyPix Bantam HPC 3000'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  79.50   0.50   10.00    --   20.00  54.00 135.93  307
  2  ω    -74.00 110.00   0.50   10.00    --   20.00  54.00   0.00  368
  3  ω    -34.50 110.00   0.50   10.00    --   20.00  54.00 -60.63  289
  4  ω    -34.50 110.00   0.50   10.00    --   20.00  54.00 -60.63  289
  5  ω    -34.50 110.00   0.50   10.00    --   20.00  54.00-120.00  289
  6  ω    -34.50 110.00   0.50   10.00    --   20.00  54.00-120.00  289
  7  ω    -34.50 110.00   0.50   10.00    --   20.00  54.00 -80.64  289
  8  ω    -74.00  23.00   0.50   10.00    --   20.00  54.00  60.00  194
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999, Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0071937000
_diffrn_orient_matrix_UB_12      -0.0697101000
_diffrn_orient_matrix_UB_13      -0.0072592000
_diffrn_orient_matrix_UB_21      0.0384213000
_diffrn_orient_matrix_UB_22      -0.0035465000
_diffrn_orient_matrix_UB_23      -0.0105614000
_diffrn_orient_matrix_UB_31      0.0200961000
_diffrn_orient_matrix_UB_32      -0.0180594000
_diffrn_orient_matrix_UB_33      0.0302055000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7826
_reflns_number_total             8956
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.205
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8956
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+2.2061P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0895
_refine_special_details          
'ByPass was used to account for solvent deuterated DMSO molecules,SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{C1AA, C501}
3. Restrained distances
 S400-O400 \\sim S500-O500
 with sigma of 0.01
 S400-C400 \\sim S500-C401
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1AA) = Uanis(C501)
Uanis(C400) = Uanis(C401)
5. Others
 Sof(S500)=Sof(O500)=Sof(C501)=Sof(D50A)=Sof(D50B)=Sof(D50C)=Sof(C401)=
 Sof(D40D)=Sof(D40E)=Sof(D40F)=1-FVAR(1)
 Sof(S400)=Sof(O400)=Sof(C400)=Sof(D40A)=Sof(D40B)=Sof(D40C)=Sof(C1AA)=
 Sof(D1AA)=Sof(D1AB)=Sof(D1AC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1P(H1PA,H1PB)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C5P(H5P), C6(H6), C6P(H6P), C7(H7), C7P(H7P), C8(H8), C8P(H8P),
 C9(H9), C9P(H9P), C11(H11), C11P(H11P), C12(H12), C12P(H12P), C14(H14),
 C14P(H14P)
6.c Idealised Me refined as rotating group:
 C400(D40A,D40B,D40C), C1AA(D1AA,D1AB,D1AC), C501(D50A,D50B,D50C), C100(D10A,
 D10B,D10C), C101(D10D,D10E,D10F), C401(D40D,D40E,D40F)
6.d Idealised tetrahedral OH refined as rotating group:
 O17(H17), O17P(H17P)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.33271(2) 0.41603(2) 0.40219(2) 0.01853(5) Uani 1 1 d . . . . .
C1 C 0.45053(10) 0.29232(19) 0.34476(7) 0.0305(3) Uani 1 1 d . . . . .
H1A H 0.431192 0.198300 0.334539 0.037 Uiso 1 1 calc R . . . .
H1B H 0.510644 0.296394 0.344087 0.037 Uiso 1 1 calc R . . . .
C1P C 0.40468(9) 0.39067(18) 0.29788(7) 0.0258(3) Uani 1 1 d . . . . .
H1PA H 0.436313 0.476392 0.297750 0.031 Uiso 1 1 calc R . . . .
H1PB H 0.396731 0.350624 0.255874 0.031 Uiso 1 1 calc R . . . .
N2 N 0.43467(7) 0.33005(13) 0.40681(6) 0.0209(2) Uani 1 1 d . . . . .
N2P N 0.32385(7) 0.41710(13) 0.31627(6) 0.0206(2) Uani 1 1 d . . . . .
C3 C 0.48632(8) 0.29010(14) 0.45587(7) 0.0198(3) Uani 1 1 d . . . . .
C3P C 0.25889(9) 0.44459(14) 0.27444(7) 0.0198(3) Uani 1 1 d . . . . .
C4 C 0.56009(9) 0.20638(15) 0.44685(7) 0.0208(3) Uani 1 1 d . . . . .
C4P C 0.26562(9) 0.45298(16) 0.20723(7) 0.0233(3) Uani 1 1 d . . . . .
C5 C 0.54789(10) 0.07023(16) 0.43023(8) 0.0283(3) Uani 1 1 d . . . . .
H5 H 0.494725 0.030232 0.427866 0.034 Uiso 1 1 calc R . . . .
C5P C 0.27571(14) 0.58027(18) 0.18210(9) 0.0379(4) Uani 1 1 d . . . . .
H5P H 0.281225 0.658571 0.207864 0.045 Uiso 1 1 calc R . . . .
C6 C 0.61370(11) -0.00733(17) 0.41706(8) 0.0313(3) Uani 1 1 d . . . . .
H6 H 0.605532 -0.100412 0.406008 0.038 Uiso 1 1 calc R . . . .
C6P C 0.27775(17) 0.5934(2) 0.11942(10) 0.0519(6) Uani 1 1 d . . . . .
H6P H 0.283751 0.680752 0.102271 0.062 Uiso 1 1 calc R . . . .
C7 C 0.69104(10) 0.05140(18) 0.42008(8) 0.0296(3) Uani 1 1 d . . . . .
H7 H 0.735395 -0.000631 0.409660 0.036 Uiso 1 1 calc R . . . .
C7P C 0.27107(15) 0.4795(2) 0.08192(9) 0.0486(5) Uani 1 1 d . . . . .
H7P H 0.272803 0.488684 0.039098 0.058 Uiso 1 1 calc R . . . .
C8 C 0.70391(9) 0.18569(17) 0.43825(8) 0.0267(3) Uani 1 1 d . . . . .
H8 H 0.757387 0.224803 0.441115 0.032 Uiso 1 1 calc R . . . .
C8P C 0.26183(12) 0.3516(2) 0.10677(8) 0.0369(4) Uani 1 1 d . . . . .
H8P H 0.257589 0.273291 0.081027 0.044 Uiso 1 1 calc R . . . .
C9 C 0.63899(9) 0.26370(16) 0.45235(7) 0.0231(3) Uani 1 1 d . . . . .
H9 H 0.648213 0.355274 0.465609 0.028 Uiso 1 1 calc R . . . .
C9P C 0.25882(10) 0.33835(17) 0.16923(7) 0.0278(3) Uani 1 1 d . . . . .
H9P H 0.252101 0.250985 0.186176 0.033 Uiso 1 1 calc R . . . .
C10 C 0.47343(8) 0.31716(15) 0.51823(7) 0.0196(3) Uani 1 1 d . . . . .
C10P C 0.17909(9) 0.47509(15) 0.29049(7) 0.0211(3) Uani 1 1 d . . . . .
C11 C 0.53393(9) 0.27947(16) 0.56988(7) 0.0232(3) Uani 1 1 d . . . . .
H11 H 0.584020 0.239204 0.562730 0.028 Uiso 1 1 calc R . . . .
C11P C 0.10743(9) 0.48216(17) 0.24341(7) 0.0263(3) Uani 1 1 d . . . . .
H11P H 0.112713 0.462628 0.201909 0.032 Uiso 1 1 calc R . . . .
C12 C 0.52289(9) 0.29895(16) 0.62990(7) 0.0256(3) Uani 1 1 d . . . . .
H12 H 0.564715 0.273087 0.663538 0.031 Uiso 1 1 calc R . . . .
C12P C 0.03101(10) 0.51624(19) 0.25595(8) 0.0310(3) Uani 1 1 d . . . . .
H12P H -0.016219 0.516925 0.223933 0.037 Uiso 1 1 calc R . . . .
C13 C 0.44844(9) 0.35794(16) 0.64064(7) 0.0221(3) Uani 1 1 d . . . . .
C13P C 0.02380(9) 0.55003(18) 0.31681(8) 0.0293(3) Uani 1 1 d . . . . .
C14 C 0.38803(9) 0.39642(15) 0.59165(7) 0.0207(3) Uani 1 1 d . . . . .
H14 H 0.338228 0.435995 0.599779 0.025 Uiso 1 1 calc R . . . .
C14P C 0.09224(9) 0.54612(18) 0.36378(7) 0.0267(3) Uani 1 1 d . . . . .
H14P H 0.086414 0.572164 0.404457 0.032 Uiso 1 1 calc R . . . .
C15 C 0.39864(8) 0.37824(14) 0.52963(7) 0.0189(3) Uani 1 1 d . . . . .
C15P C 0.17047(9) 0.50423(15) 0.35244(7) 0.0218(3) Uani 1 1 d . . . . .
O16 O 0.33758(6) 0.41742(11) 0.48643(5) 0.0222(2) Uani 1 1 d . . . . .
O16P O 0.23124(6) 0.49790(12) 0.40001(5) 0.0265(2) Uani 1 1 d . . . . .
O17 O 0.43914(7) 0.37496(13) 0.70064(5) 0.0296(2) Uani 1 1 d . . . . .
H17 H 0.392244 0.408187 0.701679 0.044 Uiso 1 1 calc GR . . . .
O17P O -0.05248(7) 0.58468(16) 0.32768(6) 0.0407(3) Uani 1 1 d . . . . .
H17P H -0.048825 0.610298 0.364555 0.061 Uiso 1 1 calc GR . . . .
S400 S 0.24772(3) 0.60755(6) 0.70596(3) 0.03452(17) Uani 0.8237(19) 1 d D . P A
1
O400 O 0.28215(17) 0.4711(3) 0.69858(13) 0.0446(6) Uani 0.8237(19) 1 d D . P A
1
C400 C 0.2085(2) 0.6077(3) 0.77583(15) 0.0623(9) Uani 0.8237(19) 1 d D . P A 1
D40A D 0.164015 0.540258 0.773339 0.093 Uiso 0.8237(19) 1 calc GR . P A 1
D40B D 0.186684 0.698103 0.782697 0.093 Uiso 0.8237(19) 1 calc GR . P A 1
D40C D 0.252990 0.584648 0.810232 0.093 Uiso 0.8237(19) 1 calc GR . P A 1
C1AA C 0.33247(18) 0.7198(3) 0.72863(15) 0.0677(7) Uani 0.8237(19) 1 d . . P A
1
D1AA D 0.368668 0.683302 0.765266 0.102 Uiso 0.8237(19) 1 calc GR . P A 1
D1AB D 0.311703 0.809275 0.738374 0.102 Uiso 0.8237(19) 1 calc GR . P A 1
D1AC D 0.363789 0.728912 0.694749 0.102 Uiso 0.8237(19) 1 calc GR . P A 1
S500 S 0.2826(3) 0.5852(4) 0.75366(18) 0.0594(12) Uani 0.1763(19) 1 d D . P A 2
O500 O 0.3007(7) 0.4608(9) 0.7236(4) 0.032(2) Uani 0.1763(19) 1 d D . P A 2
C501 C 0.33247(18) 0.7198(3) 0.72863(15) 0.0677(7) Uani 0.1763(19) 1 d . . P A
2
D50A D 0.331602 0.711249 0.684053 0.102 Uiso 0.1763(19) 1 calc GR . P A 2
D50B D 0.389952 0.721665 0.750466 0.102 Uiso 0.1763(19) 1 calc GR . P A 2
D50C D 0.304656 0.804331 0.736915 0.102 Uiso 0.1763(19) 1 calc GR . P A 2
S100 S -0.09956(2) 0.62828(4) 0.48894(2) 0.02790(9) Uani 1 1 d . . . . .
O100 O -0.03481(7) 0.63815(16) 0.44799(6) 0.0405(3) Uani 1 1 d . . . . .
C100 C -0.17943(11) 0.7445(2) 0.45741(11) 0.0421(4) Uani 1 1 d . . . . .
D10A D -0.157739 0.837538 0.461270 0.063 Uiso 1 1 calc GR . . . .
D10B D -0.225655 0.736418 0.480001 0.063 Uiso 1 1 calc GR . . . .
D10C D -0.198793 0.723255 0.413637 0.063 Uiso 1 1 calc GR . . . .
C101 C -0.15481(10) 0.47430(19) 0.46835(8) 0.0317(3) Uani 1 1 d . . . . .
D10D D -0.175087 0.472965 0.423617 0.048 Uiso 1 1 calc GR . . . .
D10E D -0.201839 0.468659 0.490240 0.048 Uiso 1 1 calc GR . . . .
D10F D -0.117916 0.396574 0.479878 0.048 Uiso 1 1 calc GR . . . .
C401 C 0.1867(8) 0.6591(15) 0.7205(6) 0.0623(9) Uani 0.1763(19) 1 d D . P A 2
D40D D 0.142049 0.593546 0.721754 0.093 Uiso 0.1763(19) 1 calc GR . P A 2
D40E D 0.187819 0.683933 0.677382 0.093 Uiso 0.1763(19) 1 calc GR . P A 2
D40F D 0.177126 0.740736 0.743821 0.093 Uiso 0.1763(19) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.8612(12) . ?
Ni1 N2P 1.8663(13) . ?
Ni1 O16 1.8374(11) . ?
Ni1 O16P 1.8424(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C1P 1.512(2) . ?
C1 N2 1.4788(19) . ?
C1P H1PA 0.9900 . ?
C1P H1PB 0.9900 . ?
C1P N2P 1.4762(18) . ?
N2 C3 1.3081(19) . ?
N2P C3P 1.3067(19) . ?
C3 C4 1.5055(18) . ?
C3 C10 1.446(2) . ?
C3P C4P 1.501(2) . ?
C3P C10P 1.4464(19) . ?
C4 C5 1.392(2) . ?
C4 C9 1.398(2) . ?
C4P C5P 1.389(2) . ?
C4P C9P 1.395(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(2) . ?
C5P H5P 0.9500 . ?
C5P C6P 1.389(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.385(2) . ?
C6P H6P 0.9500 . ?
C6P C7P 1.383(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.384(2) . ?
C7P H7P 0.9500 . ?
C7P C8P 1.390(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.391(2) . ?
C8P H8P 0.9500 . ?
C8P C9P 1.387(2) . ?
C9 H9 0.9500 . ?
C9P H9P 0.9500 . ?
C10 C11 1.418(2) . ?
C10 C15 1.4275(18) . ?
C10P C11P 1.424(2) . ?
C10P C15P 1.422(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.375(2) . ?
C11P H11P 0.9500 . ?
C11P C12P 1.372(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.409(2) . ?
C12P H12P 0.9500 . ?
C12P C13P 1.402(2) . ?
C13 C14 1.381(2) . ?
C13 O17 1.3630(18) . ?
C13P C14P 1.385(2) . ?
C13P O17P 1.3583(18) . ?
C14 H14 0.9500 . ?
C14 C15 1.414(2) . ?
C14P H14P 0.9500 . ?
C14P C15P 1.412(2) . ?
C15 O16 1.3102(17) . ?
C15P O16P 1.3122(18) . ?
O17 H17 0.8400 . ?
O17P H17P 0.8400 . ?
S400 O400 1.475(2) . ?
S400 C400 1.765(3) . ?
S400 C1AA 1.777(3) . ?
C400 D40A 0.9800 . ?
C400 D40B 0.9800 . ?
C400 D40C 0.9800 . ?
C1AA D1AA 0.9800 . ?
C1AA D1AB 0.9800 . ?
C1AA D1AC 0.9800 . ?
S500 O500 1.446(8) . ?
S500 C501 1.698(5) . ?
S500 C401 1.769(13) . ?
C501 D50A 0.9800 . ?
C501 D50B 0.9800 . ?
C501 D50C 0.9800 . ?
S100 O100 1.5112(12) . ?
S100 C100 1.7836(19) . ?
S100 C101 1.7813(18) . ?
C100 D10A 0.9800 . ?
C100 D10B 0.9800 . ?
C100 D10C 0.9800 . ?
C101 D10D 0.9800 . ?
C101 D10E 0.9800 . ?
C101 D10F 0.9800 . ?
C401 D40D 0.9800 . ?
C401 D40E 0.9800 . ?
C401 D40F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N2P 88.09(5) . . ?
O16 Ni1 N2 93.99(5) . . ?
O16 Ni1 N2P 177.91(5) . . ?
O16 Ni1 O16P 84.34(5) . . ?
O16P Ni1 N2 178.02(5) . . ?
O16P Ni1 N2P 93.58(5) . . ?
H1A C1 H1B 108.3 . . ?
C1P C1 H1A 110.0 . . ?
C1P C1 H1B 110.0 . . ?
N2 C1 H1A 110.0 . . ?
N2 C1 H1B 110.0 . . ?
N2 C1 C1P 108.63(12) . . ?
C1 C1P H1PA 110.4 . . ?
C1 C1P H1PB 110.4 . . ?
H1PA C1P H1PB 108.6 . . ?
N2P C1P C1 106.82(13) . . ?
N2P C1P H1PA 110.4 . . ?
N2P C1P H1PB 110.4 . . ?
C1 N2 Ni1 111.49(9) . . ?
C3 N2 Ni1 128.82(10) . . ?
C3 N2 C1 119.32(12) . . ?
C1P N2P Ni1 111.23(9) . . ?
C3P N2P Ni1 128.33(10) . . ?
C3P N2P C1P 120.33(13) . . ?
N2 C3 C4 118.36(12) . . ?
N2 C3 C10 122.86(12) . . ?
C10 C3 C4 118.71(12) . . ?
N2P C3P C4P 120.67(13) . . ?
N2P C3P C10P 122.20(13) . . ?
C10P C3P C4P 117.05(12) . . ?
C5 C4 C3 118.57(13) . . ?
C5 C4 C9 119.88(13) . . ?
C9 C4 C3 121.49(13) . . ?
C5P C4P C3P 118.33(14) . . ?
C5P C4P C9P 119.51(15) . . ?
C9P C4P C3P 122.11(14) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 119.97(15) . . ?
C6 C5 H5 120.0 . . ?
C4P C5P H5P 119.9 . . ?
C6P C5P C4P 120.17(17) . . ?
C6P C5P H5P 119.9 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 119.94(15) . . ?
C7 C6 H6 120.0 . . ?
C5P C6P H6P 119.9 . . ?
C7P C6P C5P 120.13(18) . . ?
C7P C6P H6P 119.9 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.20(14) . . ?
C8 C7 H7 119.9 . . ?
C6P C7P H7P 120.0 . . ?
C6P C7P C8P 120.10(17) . . ?
C8P C7P H7P 120.0 . . ?
C7 C8 H8 119.8 . . ?
C7 C8 C9 120.39(14) . . ?
C9 C8 H8 119.8 . . ?
C7P C8P H8P 120.1 . . ?
C9P C8P C7P 119.89(17) . . ?
C9P C8P H8P 120.1 . . ?
C4 C9 H9 120.2 . . ?
C8 C9 C4 119.52(14) . . ?
C8 C9 H9 120.2 . . ?
C4P C9P H9P 119.9 . . ?
C8P C9P C4P 120.18(16) . . ?
C8P C9P H9P 119.9 . . ?
C11 C10 C3 120.67(12) . . ?
C11 C10 C15 118.15(13) . . ?
C15 C10 C3 121.15(13) . . ?
C11P C10P C3P 120.04(14) . . ?
C15P C10P C3P 121.48(13) . . ?
C15P C10P C11P 118.43(13) . . ?
C10 C11 H11 118.7 . . ?
C12 C11 C10 122.54(13) . . ?
C12 C11 H11 118.7 . . ?
C10P C11P H11P 118.9 . . ?
C12P C11P C10P 122.23(15) . . ?
C12P C11P H11P 118.9 . . ?
C11 C12 H12 120.6 . . ?
C11 C12 C13 118.85(14) . . ?
C13 C12 H12 120.6 . . ?
C11P C12P H12P 120.6 . . ?
C11P C12P C13P 118.87(14) . . ?
C13P C12P H12P 120.6 . . ?
C14 C13 C12 120.44(13) . . ?
O17 C13 C12 117.42(13) . . ?
O17 C13 C14 122.14(13) . . ?
C14P C13P C12P 120.63(14) . . ?
O17P C13P C12P 117.53(14) . . ?
O17P C13P C14P 121.83(16) . . ?
C13 C14 H14 119.3 . . ?
C13 C14 C15 121.47(13) . . ?
C15 C14 H14 119.3 . . ?
C13P C14P H14P 119.3 . . ?
C13P C14P C15P 121.34(15) . . ?
C15P C14P H14P 119.3 . . ?
C14 C15 C10 118.54(13) . . ?
O16 C15 C10 124.61(13) . . ?
O16 C15 C14 116.84(12) . . ?
C14P C15P C10P 118.34(13) . . ?
O16P C15P C10P 124.21(13) . . ?
O16P C15P C14P 117.43(14) . . ?
C15 O16 Ni1 128.21(9) . . ?
C15P O16P Ni1 126.71(10) . . ?
C13 O17 H17 109.5 . . ?
C13P O17P H17P 109.5 . . ?
O400 S400 C400 107.55(16) . . ?
O400 S400 C1AA 107.43(15) . . ?
C400 S400 C1AA 98.26(15) . . ?
S400 C400 D40A 109.5 . . ?
S400 C400 D40B 109.5 . . ?
S400 C400 D40C 109.5 . . ?
D40A C400 D40B 109.5 . . ?
D40A C400 D40C 109.5 . . ?
D40B C400 D40C 109.5 . . ?
S400 C1AA D1AA 109.5 . . ?
S400 C1AA D1AB 109.5 . . ?
S400 C1AA D1AC 109.5 . . ?
D1AA C1AA D1AB 109.5 . . ?
D1AA C1AA D1AC 109.5 . . ?
D1AB C1AA D1AC 109.5 . . ?
O500 S500 C501 111.2(6) . . ?
O500 S500 C401 113.5(7) . . ?
C501 S500 C401 89.5(5) . . ?
S500 C501 D50A 109.5 . . ?
S500 C501 D50B 109.5 . . ?
S500 C501 D50C 109.5 . . ?
D50A C501 D50B 109.5 . . ?
D50A C501 D50C 109.5 . . ?
D50B C501 D50C 109.5 . . ?
O100 S100 C100 105.89(9) . . ?
O100 S100 C101 106.47(8) . . ?
C101 S100 C100 98.00(9) . . ?
S100 C100 D10A 109.5 . . ?
S100 C100 D10B 109.5 . . ?
S100 C100 D10C 109.5 . . ?
D10A C100 D10B 109.5 . . ?
D10A C100 D10C 109.5 . . ?
D10B C100 D10C 109.5 . . ?
S100 C101 D10D 109.5 . . ?
S100 C101 D10E 109.5 . . ?
S100 C101 D10F 109.5 . . ?
D10D C101 D10E 109.5 . . ?
D10D C101 D10F 109.5 . . ?
D10E C101 D10F 109.5 . . ?
S500 C401 D40D 109.5 . . ?
S500 C401 D40E 109.5 . . ?
S500 C401 D40F 109.5 . . ?
D40D C401 D40E 109.5 . . ?
D40D C401 D40F 109.5 . . ?
D40E C401 D40F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O17P H17P O100 0.84 1.83 2.659(2) 170.7 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N2 C3 C4 172.19(10) . . . . ?
Ni1 N2 C3 C10 -4.7(2) . . . . ?
Ni1 N2P C3P C4P 174.25(11) . . . . ?
Ni1 N2P C3P C10P -2.5(2) . . . . ?
C1 C1P N2P Ni1 34.30(15) . . . . ?
C1 C1P N2P C3P -149.34(14) . . . . ?
C1 N2 C3 C4 -0.2(2) . . . . ?
C1 N2 C3 C10 -177.07(14) . . . . ?
C1P C1 N2 Ni1 27.94(16) . . . . ?
C1P C1 N2 C3 -158.43(14) . . . . ?
C1P N2P C3P C4P -1.4(2) . . . . ?
C1P N2P C3P C10P -178.13(13) . . . . ?
N2 Ni1 N2P C1P -16.03(11) . . . . ?
N2 Ni1 N2P C3P 167.98(13) . . . . ?
N2 Ni1 O16 C15 4.72(13) . . . . ?
N2 C1 C1P N2P -39.34(17) . . . . ?
N2 C3 C4 C5 -75.25(19) . . . . ?
N2 C3 C4 C9 102.13(17) . . . . ?
N2 C3 C10 C11 -175.86(14) . . . . ?
N2 C3 C10 C15 6.2(2) . . . . ?
N2P Ni1 N2 C1 -7.18(11) . . . . ?
N2P Ni1 N2 C3 179.94(14) . . . . ?
N2P Ni1 O16P C15P 19.34(13) . . . . ?
N2P C3P C4P C5P -96.36(19) . . . . ?
N2P C3P C4P C9P 86.19(19) . . . . ?
N2P C3P C10P C11P -169.60(14) . . . . ?
N2P C3P C10P C15P 13.1(2) . . . . ?
C3 C4 C5 C6 175.24(15) . . . . ?
C3 C4 C9 C8 -174.30(14) . . . . ?
C3 C10 C11 C12 -177.65(14) . . . . ?
C3 C10 C15 C14 177.12(13) . . . . ?
C3 C10 C15 O16 -1.7(2) . . . . ?
C3P C4P C5P C6P -176.56(19) . . . . ?
C3P C4P C9P C8P 177.20(15) . . . . ?
C3P C10P C11P C12P -177.25(15) . . . . ?
C3P C10P C15P C14P 173.87(14) . . . . ?
C3P C10P C15P O16P -4.4(2) . . . . ?
C4 C3 C10 C11 7.3(2) . . . . ?
C4 C3 C10 C15 -170.64(13) . . . . ?
C4 C5 C6 C7 -0.5(3) . . . . ?
C4P C3P C10P C11P 13.6(2) . . . . ?
C4P C3P C10P C15P -163.72(14) . . . . ?
C4P C5P C6P C7P -1.0(4) . . . . ?
C5 C4 C9 C8 3.0(2) . . . . ?
C5 C6 C7 C8 2.3(3) . . . . ?
C5P C4P C9P C8P -0.2(2) . . . . ?
C5P C6P C7P C8P 0.4(4) . . . . ?
C6 C7 C8 C9 -1.4(3) . . . . ?
C6P C7P C8P C9P 0.4(3) . . . . ?
C7 C8 C9 C4 -1.3(2) . . . . ?
C7P C8P C9P C4P -0.5(3) . . . . ?
C9 C4 C5 C6 -2.2(2) . . . . ?
C9P C4P C5P C6P 1.0(3) . . . . ?
C10 C3 C4 C5 101.76(17) . . . . ?
C10 C3 C4 C9 -80.86(18) . . . . ?
C10 C11 C12 C13 0.4(2) . . . . ?
C10 C15 O16 Ni1 -4.2(2) . . . . ?
C10P C3P C4P C5P 80.51(19) . . . . ?
C10P C3P C4P C9P -96.94(17) . . . . ?
C10P C11P C12P C13P 2.4(3) . . . . ?
C10P C15P O16P Ni1 -14.6(2) . . . . ?
C11 C10 C15 C14 -0.9(2) . . . . ?
C11 C10 C15 O16 -179.72(14) . . . . ?
C11 C12 C13 C14 -0.5(2) . . . . ?
C11 C12 C13 O17 179.52(14) . . . . ?
C11P C10P C15P C14P -3.5(2) . . . . ?
C11P C10P C15P O16P 178.23(15) . . . . ?
C11P C12P C13P C14P -1.5(3) . . . . ?
C11P C12P C13P O17P 179.33(16) . . . . ?
C12 C13 C14 C15 0.0(2) . . . . ?
C12P C13P C14P C15P -2.0(3) . . . . ?
C13 C14 C15 C10 0.7(2) . . . . ?
C13 C14 C15 O16 179.68(13) . . . . ?
C13P C14P C15P C10P 4.4(2) . . . . ?
C13P C14P C15P O16P -177.15(15) . . . . ?
C14 C15 O16 Ni1 176.90(10) . . . . ?
C14P C15P O16P Ni1 167.06(11) . . . . ?
C15 C10 C11 C12 0.3(2) . . . . ?
C15P C10P C11P C12P 0.1(2) . . . . ?
O16 Ni1 N2 C1 172.60(11) . . . . ?
O16 Ni1 N2 C3 -0.28(14) . . . . ?
O16 Ni1 O16P C15P -160.48(13) . . . . ?
O16P Ni1 N2P C1P 165.04(10) . . . . ?
O16P Ni1 N2P C3P -10.96(14) . . . . ?
O16P Ni1 O16 C15 -176.34(13) . . . . ?
O17 C13 C14 C15 179.93(14) . . . . ?
O17P C13P C14P C15P 177.19(16) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 279.2 83.7 '2 d6-DMSO'
2 0.500 0.500 0.000 279.2 83.7 '2 d6-DMSO'

_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.099
_oxdiff_exptl_absorpt_empirical_full_min 0.903

# start Validation Reply Form
_vrf_PLAT094_exp_131_tsb         
;
PROBLEM: Ratio of Maximum / Minimum Residual Density .... 2.98 Report
RESPONSE: There is one large positive peak in the difference map between the 
sulfur atoms of the disordered deuterated DMSO molecules. This is perhaps 
indicative of a third position in the disorder model. Attempted modelling of
this lead to no better model for refinement.
;
####################################################################### 
# 
# 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_cmpd13_exp_136_tsb
_database_code_depnum_ccdc_archive 'CCDC 1922295'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2019-06-11 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_audit_creation_date             2019-06-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
N,N'-Bis-(4,4'(dihydroxybenzophenylidene))ethylenediaminenickel(II)
_chemical_formula_moiety         'C28 H22 N2 Ni O6, 4(C H4 O)'
_chemical_formula_sum            'C32 H38 N2 Ni O10'
_chemical_formula_weight         669.35
_chemical_melting_point          ?
_chemical_oxdiff_formula         C32H38N2NiO10
_chemical_oxdiff_usercomment     'TSB 9_P from DMSO/acetone/methanol'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9739(3)
_cell_length_b                   18.8657(3)
_cell_length_c                   13.1912(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.9782(17)
_cell_angle_gamma                90
_cell_volume                     3197.46(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17483
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.4310
_cell_measurement_theta_min      1.9550
_shelx_estimated_absorpt_T_max   0.835
_shelx_estimated_absorpt_T_min   0.732
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       wedge
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method 'from methanol/DMSO'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.28
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44690
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.129
_diffrn_reflns_theta_min         1.896
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'HyPix Bantam HPC 3000'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00 110.00   0.50   12.00    --   20.00  54.00 150.00  252
  2  ω    -19.50 110.00   0.50   12.00    --   20.00  54.00 -60.00  259
  3  ω    -74.00 110.00   0.50   12.00    --   20.00  54.00  90.00  368
  4  ω     -5.00  33.00   0.50   12.00    --   20.00  54.00  90.00   76
  5  ω     83.00 109.00   0.50   12.00    --   20.00  54.00  90.00   52
  6  ω    -21.00  42.00   0.50   12.00    --   20.00  54.00-180.00  126
  7  ω    -71.00 -38.00   0.50   12.00    --   20.00  54.00  30.00   66
  8  ω     -9.00 110.00   0.50   12.00    --   20.00  54.00  30.00  238
  9  ω    -58.00 -28.00   0.50   12.00    --   20.00  54.00 120.00   60
 10  ω     22.00  56.00   0.50   12.00    --   20.00  54.00 120.00   68
 11  ω    -74.00   9.00   0.50   12.00    --   20.00  54.00 150.00  166
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999, Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0181857000
_diffrn_orient_matrix_UB_12      -0.0354327000
_diffrn_orient_matrix_UB_13      0.0005196000
_diffrn_orient_matrix_UB_21      0.0082418000
_diffrn_orient_matrix_UB_22      0.0001966000
_diffrn_orient_matrix_UB_23      0.0542856000
_diffrn_orient_matrix_UB_31      -0.0514766000
_diffrn_orient_matrix_UB_32      0.0125747000
_diffrn_orient_matrix_UB_33      0.0004078000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7326
_reflns_number_total             8605
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.07
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8605
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0421
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0617P)²+2.4358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1212
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1M of O1M, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H5 of O5, H4 of O4, H6 of O6, H3 of O3, H1E of O1E,
  H1H of O1H, H1O of O1O
2.a Rotating group:
 O1M(H1M)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5A), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C16(H16),
 C18(H18), C19(H19), C23(H23), C24(H24), C26(H26), C27(H27)
2.d Idealised Me refined as rotating group:
 C1E(H1EA,H1EB,H1EC), C1O(H1OA,H1OB,H1OC), C1M(H1MA,H1MB,H1MC), C1H(H1HA,H1HB,
 H1HC)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O5(H5), O6(H6), O1E(H1E), O1O(H1O), O1H(H1H)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.34313(2) 0.24373(2) 0.53487(2) 0.02270(8) Uani 1 1 d . . . . .
O1 O 0.48605(10) 0.24168(6) 0.56422(11) 0.0275(3) Uani 1 1 d . . . . .
O2 O 0.36025(10) 0.15082(7) 0.49800(11) 0.0282(3) Uani 1 1 d . . . . .
O3 O 0.83218(11) 0.31455(8) 0.67387(14) 0.0421(4) Uani 1 1 d . . . . .
H3 H 0.841200 0.270452 0.675049 0.063 Uiso 1 1 calc GR . . . .
O4 O 0.31932(15) 0.64118(8) 0.79743(12) 0.0430(4) Uani 1 1 d . . . . .
H4 H 0.321106 0.675389 0.756960 0.064 Uiso 1 1 calc GR . . . .
O5 O -0.28587(11) 0.24644(7) 0.33093(12) 0.0336(3) Uani 1 1 d . . . . .
H5 H -0.324274 0.226660 0.368766 0.050 Uiso 1 1 calc GR . . . .
O6 O 0.27831(11) -0.08271(7) 0.38397(12) 0.0343(3) Uani 1 1 d . . . . .
H6 H 0.342924 -0.083155 0.383099 0.051 Uiso 1 1 calc GR . . . .
N1 N 0.33159(12) 0.33572(8) 0.58274(12) 0.0252(3) Uani 1 1 d . . . . .
N2 N 0.20018(12) 0.24405(8) 0.49677(12) 0.0249(3) Uani 1 1 d . . . . .
C1 C 0.22201(15) 0.35340(10) 0.59106(17) 0.0333(4) Uani 1 1 d . . . . .
H1A H 0.211074 0.405273 0.585550 0.040 Uiso 1 1 calc R . . . .
H1B H 0.203846 0.337358 0.657807 0.040 Uiso 1 1 calc R . . . .
C2 C 0.40569(14) 0.38021(9) 0.61610(13) 0.0234(3) Uani 1 1 d . . . . .
C3 C 0.37904(14) 0.45008(9) 0.66005(13) 0.0247(3) Uani 1 1 d . . . . .
C4 C 0.35711(15) 0.45304(9) 0.76008(14) 0.0263(3) Uani 1 1 d . . . . .
H4A H 0.355790 0.410473 0.798360 0.032 Uiso 1 1 calc R . . . .
C5 C 0.33707(16) 0.51728(10) 0.80501(14) 0.0304(4) Uani 1 1 d . . . . .
H5A H 0.322983 0.518638 0.873758 0.036 Uiso 1 1 calc R . . . .
C6 C 0.33774(16) 0.57955(10) 0.74875(15) 0.0303(4) Uani 1 1 d . . . . .
C7 C 0.35705(18) 0.57713(10) 0.64774(16) 0.0346(4) Uani 1 1 d . . . . .
H7 H 0.356168 0.619538 0.608808 0.042 Uiso 1 1 calc R . . . .
C8 C 0.37770(17) 0.51245(10) 0.60361(15) 0.0331(4) Uani 1 1 d . . . . .
H8 H 0.390931 0.510952 0.534600 0.040 Uiso 1 1 calc R . . . .
C9 C 0.51506(14) 0.36300(9) 0.61989(13) 0.0235(3) Uani 1 1 d . . . . .
C10 C 0.59229(15) 0.41380(10) 0.65586(14) 0.0280(4) Uani 1 1 d . . . . .
H10 H 0.570827 0.460479 0.670015 0.034 Uiso 1 1 calc R . . . .
C11 C 0.69655(16) 0.39831(10) 0.67103(16) 0.0316(4) Uani 1 1 d . . . . .
H11 H 0.746259 0.433985 0.693295 0.038 Uiso 1 1 calc R . . . .
C12 C 0.72865(15) 0.32900(11) 0.65317(15) 0.0304(4) Uani 1 1 d . . . . .
C13 C 0.65640(14) 0.27788(10) 0.61657(15) 0.0281(4) Uani 1 1 d . . . . .
H13 H 0.679429 0.231406 0.603418 0.034 Uiso 1 1 calc R . . . .
C14 C 0.54933(14) 0.29365(9) 0.59851(13) 0.0240(3) Uani 1 1 d . . . . .
C15 C 0.28685(13) 0.10465(9) 0.46516(13) 0.0233(3) Uani 1 1 d . . . . .
C16 C 0.31938(14) 0.03532(9) 0.44441(15) 0.0270(4) Uani 1 1 d . . . . .
H16 H 0.391438 0.024062 0.455297 0.032 Uiso 1 1 calc R . . . .
C17 C 0.24804(15) -0.01641(9) 0.40852(14) 0.0264(3) Uani 1 1 d . . . . .
C18 C 0.14116(15) -0.00203(10) 0.39530(15) 0.0280(4) Uani 1 1 d . . . . .
H18 H 0.092007 -0.038190 0.373731 0.034 Uiso 1 1 calc R . . . .
C19 C 0.10872(14) 0.06561(10) 0.41422(14) 0.0253(3) Uani 1 1 d . . . . .
H19 H 0.036267 0.075632 0.403879 0.030 Uiso 1 1 calc R . . . .
C20 C 0.17896(13) 0.12082(9) 0.44844(13) 0.0226(3) Uani 1 1 d . . . . .
C21 C 0.13977(14) 0.19157(9) 0.46179(13) 0.0236(3) Uani 1 1 d . . . . .
C22 C 0.02634(14) 0.20523(9) 0.42973(13) 0.0243(3) Uani 1 1 d . . . . .
C23 C -0.04871(14) 0.18208(10) 0.48821(14) 0.0278(4) Uani 1 1 d . . . . .
H23 H -0.027913 0.157366 0.550433 0.033 Uiso 1 1 calc R . . . .
C24 C -0.15361(15) 0.19484(10) 0.45632(14) 0.0279(4) Uani 1 1 d . . . . .
H24 H -0.204392 0.178209 0.496019 0.034 Uiso 1 1 calc R . . . .
C25 C -0.18405(14) 0.23194(9) 0.36629(15) 0.0260(3) Uani 1 1 d . . . . .
C26 C -0.10963(15) 0.25580(10) 0.30738(15) 0.0278(4) Uani 1 1 d . . . . .
H26 H -0.130513 0.281347 0.245900 0.033 Uiso 1 1 calc R . . . .
C27 C -0.00535(15) 0.24212(10) 0.33880(14) 0.0267(4) Uani 1 1 d . . . . .
H27 H 0.045189 0.257928 0.298240 0.032 Uiso 1 1 calc R . . . .
C28 C 0.15557(16) 0.31602(10) 0.50486(18) 0.0348(4) Uani 1 1 d . . . . .
H28A H 0.082831 0.312673 0.519233 0.042 Uiso 1 1 calc R . . . .
H28B H 0.156051 0.342323 0.439991 0.042 Uiso 1 1 calc R . . . .
O1E O 0.86593(15) 0.17659(9) 0.71262(13) 0.0501(4) Uani 1 1 d . . . . .
H1E H 0.819212 0.149051 0.685445 0.075 Uiso 1 1 calc GR . . . .
C1E C 0.8845(4) 0.1640(2) 0.8168(2) 0.0885(12) Uani 1 1 d . . . . .
H1EA H 0.820869 0.173016 0.846995 0.133 Uiso 1 1 calc GR . . . .
H1EB H 0.940027 0.195398 0.848311 0.133 Uiso 1 1 calc GR . . . .
H1EC H 0.905756 0.114489 0.828995 0.133 Uiso 1 1 calc GR . . . .
O1O O 0.47897(13) -0.08473(10) 0.37222(15) 0.0503(4) Uani 1 1 d . . . . .
H1O H 0.521356 -0.112105 0.406592 0.075 Uiso 1 1 calc GR . . . .
C1O C 0.5159(3) -0.06715(17) 0.2818(2) 0.0663(8) Uani 1 1 d . . . . .
H1OA H 0.506135 -0.107415 0.234530 0.099 Uiso 1 1 calc GR . . . .
H1OB H 0.590067 -0.055545 0.296306 0.099 Uiso 1 1 calc GR . . . .
H1OC H 0.477459 -0.026074 0.250737 0.099 Uiso 1 1 calc GR . . . .
O1M O 0.96574(18) 0.41357(14) 0.59167(19) 0.0725(6) Uani 1 1 d . . . . .
H1M H 0.930166 0.389100 0.629603 0.087 Uiso 1 1 d GR . . . .
C1M C 0.9048(3) 0.4256(2) 0.4956(3) 0.0835(11) Uani 1 1 d . . . . .
H1MA H 0.946156 0.451533 0.450958 0.125 Uiso 1 1 calc GR . . . .
H1MB H 0.843279 0.453617 0.505241 0.125 Uiso 1 1 calc GR . . . .
H1MC H 0.882792 0.380089 0.463957 0.125 Uiso 1 1 calc GR . . . .
O1H O -0.42023(13) 0.17633(10) 0.41426(14) 0.0501(4) Uani 1 1 d . . . . .
H1H H -0.464449 0.187685 0.452234 0.075 Uiso 1 1 calc GR . . . .
C1H C -0.4544(2) 0.11670(15) 0.3577(2) 0.0506(6) Uani 1 1 d . . . . .
H1HA H -0.415289 0.111896 0.299656 0.076 Uiso 1 1 calc GR . . . .
H1HB H -0.528730 0.121586 0.332311 0.076 Uiso 1 1 calc GR . . . .
H1HC H -0.443396 0.074528 0.401235 0.076 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.8413(13) . ?
Ni1 O2 1.8407(13) . ?
Ni1 N1 1.8599(15) . ?
Ni1 N2 1.8529(16) . ?
O1 C14 1.318(2) . ?
O2 C15 1.319(2) . ?
O3 H3 0.8400 . ?
O3 C12 1.361(2) . ?
O4 H4 0.8400 . ?
O4 C6 1.365(2) . ?
O5 H5 0.8400 . ?
O5 C25 1.366(2) . ?
O6 H6 0.8400 . ?
O6 C17 1.363(2) . ?
N1 C1 1.479(2) . ?
N1 C2 1.306(2) . ?
N2 C21 1.306(2) . ?
N2 C28 1.486(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C28 1.504(3) . ?
C2 C3 1.500(2) . ?
C2 C9 1.450(2) . ?
C3 C4 1.389(3) . ?
C3 C8 1.391(3) . ?
C4 H4A 0.9500 . ?
C4 C5 1.389(2) . ?
C5 H5A 0.9500 . ?
C5 C6 1.390(3) . ?
C6 C7 1.390(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.394(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.420(2) . ?
C9 C14 1.423(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.371(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.402(3) . ?
C12 C13 1.384(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.408(2) . ?
C15 C16 1.413(2) . ?
C15 C20 1.420(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(2) . ?
C17 C18 1.400(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.377(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.416(2) . ?
C20 C21 1.448(2) . ?
C21 C22 1.496(2) . ?
C22 C23 1.394(3) . ?
C22 C27 1.398(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.389(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.388(3) . ?
C25 C26 1.395(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.383(3) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
O1E H1E 0.8400 . ?
O1E C1E 1.383(4) . ?
C1E H1EA 0.9800 . ?
C1E H1EB 0.9800 . ?
C1E H1EC 0.9800 . ?
O1O H1O 0.8400 . ?
O1O C1O 1.385(4) . ?
C1O H1OA 0.9800 . ?
C1O H1OB 0.9800 . ?
C1O H1OC 0.9800 . ?
O1M H1M 0.8606 . ?
O1M C1M 1.416(4) . ?
C1M H1MA 0.9800 . ?
C1M H1MB 0.9800 . ?
C1M H1MC 0.9800 . ?
O1H H1H 0.8400 . ?
O1H C1H 1.388(3) . ?
C1H H1HA 0.9800 . ?
C1H H1HB 0.9800 . ?
C1H H1HC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N1 94.26(6) . . ?
O1 Ni1 N2 176.30(6) . . ?
O2 Ni1 O1 83.15(5) . . ?
O2 Ni1 N1 175.27(6) . . ?
O2 Ni1 N2 94.84(6) . . ?
N2 Ni1 N1 87.96(6) . . ?
C14 O1 Ni1 128.16(11) . . ?
C15 O2 Ni1 127.43(11) . . ?
C12 O3 H3 109.5 . . ?
C6 O4 H4 109.5 . . ?
C25 O5 H5 109.5 . . ?
C17 O6 H6 109.5 . . ?
C1 N1 Ni1 111.04(12) . . ?
C2 N1 Ni1 128.61(13) . . ?
C2 N1 C1 120.02(15) . . ?
C21 N2 Ni1 128.47(12) . . ?
C21 N2 C28 119.82(16) . . ?
C28 N2 Ni1 111.64(12) . . ?
N1 C1 H1A 110.3 . . ?
N1 C1 H1B 110.3 . . ?
N1 C1 C28 107.11(15) . . ?
H1A C1 H1B 108.5 . . ?
C28 C1 H1A 110.3 . . ?
C28 C1 H1B 110.3 . . ?
N1 C2 C3 119.79(16) . . ?
N1 C2 C9 122.61(15) . . ?
C9 C2 C3 117.43(15) . . ?
C4 C3 C2 119.42(15) . . ?
C4 C3 C8 119.04(16) . . ?
C8 C3 C2 121.53(16) . . ?
C3 C4 H4A 119.5 . . ?
C3 C4 C5 121.02(17) . . ?
C5 C4 H4A 119.5 . . ?
C4 C5 H5A 120.2 . . ?
C4 C5 C6 119.60(17) . . ?
C6 C5 H5A 120.2 . . ?
O4 C6 C5 117.00(18) . . ?
O4 C6 C7 123.06(18) . . ?
C5 C6 C7 119.94(17) . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 119.98(18) . . ?
C8 C7 H7 120.0 . . ?
C3 C8 C7 120.38(17) . . ?
C3 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C10 C9 C2 120.15(16) . . ?
C10 C9 C14 117.49(16) . . ?
C14 C9 C2 122.04(16) . . ?
C9 C10 H10 118.6 . . ?
C11 C10 C9 122.77(17) . . ?
C11 C10 H10 118.6 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 118.96(17) . . ?
C12 C11 H11 120.5 . . ?
O3 C12 C11 117.46(17) . . ?
O3 C12 C13 122.16(18) . . ?
C13 C12 C11 120.38(18) . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 121.08(17) . . ?
C14 C13 H13 119.5 . . ?
O1 C14 C9 123.73(16) . . ?
O1 C14 C13 117.00(16) . . ?
C13 C14 C9 119.26(16) . . ?
O2 C15 C16 116.99(15) . . ?
O2 C15 C20 124.09(15) . . ?
C16 C15 C20 118.91(16) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 C15 121.07(17) . . ?
C17 C16 H16 119.5 . . ?
O6 C17 C16 121.85(17) . . ?
O6 C17 C18 117.46(16) . . ?
C16 C17 C18 120.69(17) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 C17 118.63(17) . . ?
C19 C18 H18 120.7 . . ?
C18 C19 H19 118.7 . . ?
C18 C19 C20 122.69(17) . . ?
C20 C19 H19 118.7 . . ?
C15 C20 C21 122.32(15) . . ?
C19 C20 C15 117.94(16) . . ?
C19 C20 C21 119.71(15) . . ?
N2 C21 C20 122.55(16) . . ?
N2 C21 C22 119.19(16) . . ?
C20 C21 C22 118.21(15) . . ?
C23 C22 C21 121.67(16) . . ?
C23 C22 C27 119.07(16) . . ?
C27 C22 C21 119.26(16) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.58(17) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 120.1 . . ?
C25 C24 C23 119.81(17) . . ?
C25 C24 H24 120.1 . . ?
O5 C25 C24 122.68(17) . . ?
O5 C25 C26 117.15(17) . . ?
C24 C25 C26 120.16(17) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.78(17) . . ?
C27 C26 H26 120.1 . . ?
C22 C27 H27 119.7 . . ?
C26 C27 C22 120.59(17) . . ?
C26 C27 H27 119.7 . . ?
N2 C28 C1 107.15(15) . . ?
N2 C28 H28A 110.3 . . ?
N2 C28 H28B 110.3 . . ?
C1 C28 H28A 110.3 . . ?
C1 C28 H28B 110.3 . . ?
H28A C28 H28B 108.5 . . ?
C1E O1E H1E 109.5 . . ?
O1E C1E H1EA 109.5 . . ?
O1E C1E H1EB 109.5 . . ?
O1E C1E H1EC 109.5 . . ?
H1EA C1E H1EB 109.5 . . ?
H1EA C1E H1EC 109.5 . . ?
H1EB C1E H1EC 109.5 . . ?
C1O O1O H1O 109.5 . . ?
O1O C1O H1OA 109.5 . . ?
O1O C1O H1OB 109.5 . . ?
O1O C1O H1OC 109.5 . . ?
H1OA C1O H1OB 109.5 . . ?
H1OA C1O H1OC 109.5 . . ?
H1OB C1O H1OC 109.5 . . ?
C1M O1M H1M 109.2 . . ?
O1M C1M H1MA 109.5 . . ?
O1M C1M H1MB 109.5 . . ?
O1M C1M H1MC 109.5 . . ?
H1MA C1M H1MB 109.5 . . ?
H1MA C1M H1MC 109.5 . . ?
H1MB C1M H1MC 109.5 . . ?
C1H O1H H1H 109.5 . . ?
O1H C1H H1HA 109.5 . . ?
O1H C1H H1HB 109.5 . . ?
O1H C1H H1HC 109.5 . . ?
H1HA C1H H1HB 109.5 . . ?
H1HA C1H H1HC 109.5 . . ?
H1HB C1H H1HC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O1E 0.84 1.85 2.677(2) 165.7 . yes
O4 H4 O5 0.84 1.89 2.711(2) 164.3 3_566 yes
O5 H5 O1H 0.84 1.74 2.555(2) 163.8 . yes
O6 H6 O1O 0.84 1.79 2.630(2) 176.2 . yes
O1E H1E O6 0.84 1.92 2.757(2) 174.7 3_656 yes
O1O H1O O2 0.84 1.99 2.801(2) 163.6 3_656 yes
O1M H1M O3 0.86 2.04 2.862(3) 160.8 . yes
O1H H1H O1 0.84 1.97 2.753(2) 153.9 1_455 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 C14 C9 0.4(3) . . . . ?
Ni1 O1 C14 C13 178.95(13) . . . . ?
Ni1 O2 C15 C16 -178.13(13) . . . . ?
Ni1 O2 C15 C20 2.8(3) . . . . ?
Ni1 N1 C1 C28 -34.48(19) . . . . ?
Ni1 N1 C2 C3 -174.61(12) . . . . ?
Ni1 N1 C2 C9 0.6(3) . . . . ?
Ni1 N2 C21 C20 0.9(3) . . . . ?
Ni1 N2 C21 C22 -176.30(12) . . . . ?
Ni1 N2 C28 C1 -31.2(2) . . . . ?
O1 Ni1 O2 C15 178.07(16) . . . . ?
O1 Ni1 N1 C1 -168.71(13) . . . . ?
O1 Ni1 N1 C2 4.68(17) . . . . ?
O2 Ni1 O1 C14 178.79(16) . . . . ?
O2 Ni1 N2 C21 3.21(17) . . . . ?
O2 Ni1 N2 C28 -173.73(14) . . . . ?
O2 C15 C16 C17 -179.22(17) . . . . ?
O2 C15 C20 C19 -179.21(17) . . . . ?
O2 C15 C20 C21 3.0(3) . . . . ?
O3 C12 C13 C14 178.16(18) . . . . ?
O4 C6 C7 C8 178.5(2) . . . . ?
O5 C25 C26 C27 -179.39(16) . . . . ?
O6 C17 C18 C19 -176.51(17) . . . . ?
N1 Ni1 O1 C14 -5.19(16) . . . . ?
N1 Ni1 N2 C21 -172.97(17) . . . . ?
N1 Ni1 N2 C28 10.09(14) . . . . ?
N1 C1 C28 N2 41.3(2) . . . . ?
N1 C2 C3 C4 79.6(2) . . . . ?
N1 C2 C3 C8 -101.7(2) . . . . ?
N1 C2 C9 C10 179.29(17) . . . . ?
N1 C2 C9 C14 -7.3(3) . . . . ?
N2 Ni1 O2 C15 -5.05(16) . . . . ?
N2 Ni1 N1 C1 14.26(13) . . . . ?
N2 Ni1 N1 C2 -172.35(17) . . . . ?
N2 C21 C22 C23 -107.0(2) . . . . ?
N2 C21 C22 C27 73.1(2) . . . . ?
C1 N1 C2 C3 -1.7(3) . . . . ?
C1 N1 C2 C9 173.44(17) . . . . ?
C2 N1 C1 C28 151.48(18) . . . . ?
C2 C3 C4 C5 176.85(17) . . . . ?
C2 C3 C8 C7 -177.23(19) . . . . ?
C2 C9 C10 C11 173.18(18) . . . . ?
C2 C9 C14 O1 6.9(3) . . . . ?
C2 C9 C14 C13 -171.64(17) . . . . ?
C3 C2 C9 C10 -5.4(2) . . . . ?
C3 C2 C9 C14 167.96(16) . . . . ?
C3 C4 C5 C6 0.7(3) . . . . ?
C4 C3 C8 C7 1.5(3) . . . . ?
C4 C5 C6 O4 -178.89(18) . . . . ?
C4 C5 C6 C7 0.8(3) . . . . ?
C5 C6 C7 C8 -1.2(3) . . . . ?
C6 C7 C8 C3 0.1(3) . . . . ?
C8 C3 C4 C5 -1.9(3) . . . . ?
C9 C2 C3 C4 -95.8(2) . . . . ?
C9 C2 C3 C8 82.9(2) . . . . ?
C9 C10 C11 C12 -1.8(3) . . . . ?
C10 C9 C14 O1 -179.59(17) . . . . ?
C10 C9 C14 C13 1.9(3) . . . . ?
C10 C11 C12 O3 -176.77(19) . . . . ?
C10 C11 C12 C13 2.8(3) . . . . ?
C11 C12 C13 C14 -1.4(3) . . . . ?
C12 C13 C14 O1 -179.62(18) . . . . ?
C12 C13 C14 C9 -1.0(3) . . . . ?
C14 C9 C10 C11 -0.5(3) . . . . ?
C15 C16 C17 O6 177.15(17) . . . . ?
C15 C16 C17 C18 -2.3(3) . . . . ?
C15 C20 C21 N2 -4.8(3) . . . . ?
C15 C20 C21 C22 172.42(16) . . . . ?
C16 C15 C20 C19 1.7(3) . . . . ?
C16 C15 C20 C21 -176.12(17) . . . . ?
C16 C17 C18 C19 3.0(3) . . . . ?
C17 C18 C19 C20 -1.3(3) . . . . ?
C18 C19 C20 C15 -1.0(3) . . . . ?
C18 C19 C20 C21 176.85(17) . . . . ?
C19 C20 C21 N2 177.36(17) . . . . ?
C19 C20 C21 C22 -5.4(2) . . . . ?
C20 C15 C16 C17 -0.1(3) . . . . ?
C20 C21 C22 C23 75.7(2) . . . . ?
C20 C21 C22 C27 -104.3(2) . . . . ?
C21 N2 C28 C1 151.52(18) . . . . ?
C21 C22 C23 C24 -179.39(17) . . . . ?
C21 C22 C27 C26 -179.73(16) . . . . ?
C22 C23 C24 C25 -1.0(3) . . . . ?
C23 C22 C27 C26 0.3(3) . . . . ?
C23 C24 C25 O5 -179.76(17) . . . . ?
C23 C24 C25 C26 0.6(3) . . . . ?
C24 C25 C26 C27 0.2(3) . . . . ?
C25 C26 C27 C22 -0.7(3) . . . . ?
C27 C22 C23 C24 0.6(3) . . . . ?
C28 N2 C21 C20 177.66(17) . . . . ?
C28 N2 C21 C22 0.4(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone`'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.111
_oxdiff_exptl_absorpt_empirical_full_min 0.914

