# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_ral1605X
_database_code_depnum_ccdc_archive 'CCDC 1838238'
_audit_update_record             
;
2018-04-19 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_audit_creation_date             16-05-30
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1605X\Tony_ral1605X_data\r At 12:15 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   11.1634(2)
_cell_length_b                   20.7999(3)
_cell_length_c                   8.9866(1)
_cell_angle_alpha                90
_cell_angle_beta                 112.1248(18)
_cell_angle_gamma                90
_cell_volume                     1933.02(6)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-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 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C20 H20 N2 Ni1 O4 
# Dc =      1.41 Fooo =    936.00 Mu =     10.31 M =    411.10
# Found Formula = C20 H24 N2 Ni1 O6 
# Dc =      1.54 FOOO =    936.00 Mu =     10.45 M =    447.13

_chemical_formula_sum            'C20 H24 N2 Ni1 O6'
_chemical_formula_moiety         'C20 H20 N2 Ni O4, 2(H2 O)'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         447.13


_cell_measurement_reflns_used    15436
_cell_measurement_theta_min      4
_cell_measurement_theta_max      30
_cell_measurement_temperature    150

_exptl_crystal_description       lath
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.078
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_max          0.427

_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    1.045

# Sheldrick geometric approximatio 0.81 0.92 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_T_max  0.92
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2015)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2015)'
_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            21241
_reflns_number_total             4958
_diffrn_reflns_av_R_equivalents  0.020
# Number of reflections without Friedels Law is 4958 
# Number of reflections with Friedels Law is 2643 
# Theoretical number of reflections is about 2776 


_diffrn_reflns_theta_min         3.538
_diffrn_reflns_theta_max         29.829
_diffrn_measured_fraction_theta_max 0.923

_diffrn_reflns_theta_full        27.637
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -15
_reflns_limit_h_max              13
_reflns_limit_k_min              -29
_reflns_limit_k_max              29
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   1.13
_oxford_diffrn_Wilson_scale      0.16

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

_refine_diff_density_min         -0.45
_refine_diff_density_max         0.53


# 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         4958
_refine_ls_number_restraints     1
_refine_ls_number_parameters     282
_oxford_refine_ls_R_factor_ref   0.0228
_refine_ls_wR_factor_ref         0.0555
_refine_ls_goodness_of_fit_ref   1.0075
_refine_ls_shift/su_max          0.0044372
_refine_ls_shift/su_mean         0.0002618


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4958
_refine_ls_R_factor_all          0.0228
_refine_ls_wR_factor_all         0.0555

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4809
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_gt          0.0545

_refine_ls_abs_structure_Flack   0.004(12)
_refine_ls_abs_structure_details 'Flack (1983), 2315 Friedel-pairs'
# 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 ad


_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) + ( 0.02P)² + 2.65P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               
The compound is enantiomerically pure.
Its absolute configuration has been determined 
by refinement of the Flack parameter
and is in agreement with the configuration expected
on the basis of 
the synthetic precursors.
The final value of the Flack parameter is 0.004(12) and 
the final value of the Hooft parameter is 0.002(6).


All of the H atoms were located in difference electron density maps, 
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 = 0.83 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints
except for those bonded to O which were allowed to refine freely.


Most of the largest features in the
final difference electron density map 
are located midway between bonded atoms or near the Ni atoms.


The structure presents some pseudo-symmetry.
Structure checking programs such as ADDSYM within PLATON
suggest that there might be an extra centre of symmetry
 and that the space group could be C2/c.  
As the compound is chiral, an inversion symmetry operation is not an option.
Furthermore, if the space group were to be C2/c, then
reflections h0l: l=2n+1 would need to be systematically extinct.
In fact reflections h0l:l=2n+1 have an average I/σ(I) of 134
(cf. reflections h0l:l=2n with an average I/σ(I) of 386),
so this reflection class is a long way from being absent
and clearly no c-glide is present.


;

# 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 1.0000 0.45317(5) 1.0000 0.0134 1.0000 Uani S T . . . .
Ni2 Ni 0.5000 0.52195(5) 0.5000 0.0136 1.0000 Uani S T . . . .
O1 O 0.9406(2) 0.38671(10) 0.8561(3) 0.0206 1.0000 Uani . . . . . .
O2 O 0.82528(18) 0.28032(10) 0.3562(2) 0.0213 1.0000 Uani . . . . . .
O3 O 0.53599(19) 0.58846(10) 0.6469(3) 0.0177 1.0000 Uani . . . . . .
O4 O 0.69639(19) 0.69515(10) 1.1488(2) 0.0219 1.0000 Uani . . . . . .
O5 O 0.6697(2) 0.79899(11) 0.9680(3) 0.0292 1.0000 Uani . . . . . .
O6 O 0.83370(19) 0.17700(11) 0.5392(2) 0.0245 1.0000 Uani . . . . . .
N1 N 0.93296(19) 0.51775(13) 0.8500(3) 0.0147 1.0000 Uani . . . . . .
N2 N 0.53461(18) 0.45740(13) 0.6516(3) 0.0163 1.0000 Uani . . . . . .
C1 C 0.8968(3) 0.39094(14) 0.6984(4) 0.0152 1.0000 Uani . . . . . .
C2 C 0.8785(2) 0.33347(15) 0.6106(3) 0.0165 1.0000 Uani . . . . . .
C3 C 0.8399(2) 0.33453(14) 0.4440(3) 0.0156 1.0000 Uani . . . . . .
C4 C 0.8151(3) 0.39309(15) 0.3615(3) 0.0211 1.0000 Uani . . . . . .
C5 C 0.8288(2) 0.44935(17) 0.4463(3) 0.0202 1.0000 Uani . . . . . .
C6 C 0.8694(2) 0.45023(16) 0.6148(3) 0.0167 1.0000 Uani . . . . . .
C7 C 0.8829(3) 0.51060(13) 0.6961(3) 0.0178 1.0000 Uani . . . . . .
C8 C 0.93676(18) 0.58124(9) 0.92652(19) 0.0151 1.0000 Uani . . . . . .
C9 C 0.9266(2) 0.64034(15) 0.8230(3) 0.0197 1.0000 Uani . . . . . .
C10 C 0.93774(18) 0.70076(9) 0.9262(2) 0.0190 1.0000 Uani . . . . . .
C11 C 0.5905(2) 0.58433(14) 0.8043(4) 0.0141 1.0000 Uani . . . . . .
C12 C 0.6173(2) 0.64188(14) 0.8934(3) 0.0162 1.0000 Uani . . . . . .
C13 C 0.6716(2) 0.64070(14) 1.0580(3) 0.0177 1.0000 Uani . . . . . .
C14 C 0.7023(3) 0.58224(15) 1.1421(3) 0.0224 1.0000 Uani . . . . . .
C15 C 0.6767(2) 0.52611(17) 1.0565(3) 0.0230 1.0000 Uani . . . . . .
C16 C 0.6208(2) 0.52502(16) 0.8871(3) 0.0165 1.0000 Uani . . . . . .
C17 C 0.5883(2) 0.46470(13) 0.8054(4) 0.0175 1.0000 Uani . . . . . .
C18 C 0.48893(18) 0.39342(9) 0.5785(2) 0.0165 1.0000 Uani . . . . . .
C19 C 0.5501(3) 0.33445(15) 0.6793(3) 0.0220 1.0000 Uani . . . . . .
C20 C 0.4929(2) 0.27367(10) 0.5814(2) 0.0226 1.0000 Uani . . . . . .
H1 H 0.836(3) 0.2532(15) 0.404(4) 0.0321 1.0000 Uiso . . . . . .
H2 H 0.687(3) 0.7307(15) 1.088(4) 0.0341 1.0000 Uiso . . . . . .
H3 H 0.625(3) 0.8270(17) 0.971(4) 0.0440 1.0000 Uiso . . . . . .
H4 H 0.654(3) 0.7888(16) 0.858(4) 0.0437 1.0000 Uiso . . . . . .
H5 H 0.815(3) 0.1802(16) 0.605(4) 0.0373 1.0000 Uiso . . . . . .
H6 H 0.897(3) 0.1558(16) 0.567(3) 0.0370 1.0000 Uiso . . . . . .
H21 H 0.8951 0.2944 0.6647 0.0197 1.0000 Uiso R . . . . .
H41 H 0.7921 0.3938 0.2462 0.0253 1.0000 Uiso R . . . . .
H51 H 0.8115 0.4885 0.3912 0.0249 1.0000 Uiso R . . . . .
H71 H 0.8494 0.5477 0.6318 0.0196 1.0000 Uiso R . . . . .
H81 H 0.8664 0.5815 0.9635 0.0166 1.0000 Uiso R . . . . .
H91 H 0.8429 0.6420 0.7309 0.0240 1.0000 Uiso R . . . . .
H92 H 0.9983 0.6391 0.7844 0.0235 1.0000 Uiso R . . . . .
H101 H 0.8661 0.7017 0.9594 0.0214 1.0000 Uiso R . . . . .
H102 H 0.9323 0.7387 0.8630 0.0226 1.0000 Uiso R . . . . .
H121 H 0.5980 0.6809 0.8390 0.0189 1.0000 Uiso R . . . . .
H141 H 0.7413 0.5836 1.2562 0.0271 1.0000 Uiso R . . . . .
H151 H 0.6955 0.4875 1.1105 0.0277 1.0000 Uiso R . . . . .
H171 H 0.6033 0.4273 0.8705 0.0200 1.0000 Uiso R . . . . .
H181 H 0.3961 0.3925 0.5530 0.0189 1.0000 Uiso R . . . . .
H191 H 0.5330 0.3343 0.7800 0.0253 1.0000 Uiso R . . . . .
H192 H 0.6442 0.3356 0.7087 0.0251 1.0000 Uiso R . . . . .
H201 H 0.5350 0.2365 0.6445 0.0266 1.0000 Uiso R . . . . .
H202 H 0.4020 0.2708 0.5622 0.0259 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.461(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . N1 3_757 1.850(2) yes
Ni1 . O1 3_757 1.837(2) yes
Ni1 . O1 . 1.837(2) yes
Ni1 . N1 . 1.850(2) yes
Ni2 . O3 3_656 1.849(2) yes
Ni2 . N2 3_656 1.847(3) yes
Ni2 . O3 . 1.849(2) yes
Ni2 . N2 . 1.847(3) yes
O1 . C1 . 1.317(3) yes
O2 . C3 . 1.351(3) yes
O2 . H1 . 0.69(3) no
O3 . C11 . 1.315(3) yes
O4 . C13 . 1.362(3) yes
O4 . H2 . 0.90(3) no
O5 . H3 . 0.77(4) no
O5 . H4 . 0.96(3) no
O6 . H5 . 0.70(3) no
O6 . H6 . 0.79(3) no
N1 . C7 . 1.290(3) yes
N1 . C8 . 1.482(3) yes
N2 . C17 . 1.292(3) yes
N2 . C18 . 1.487(3) yes
C1 . C2 . 1.404(4) yes
C1 . C6 . 1.416(4) yes
C2 . C3 . 1.393(3) yes
C2 . H21 . 0.929 no
C3 . C4 . 1.398(4) yes
C4 . C5 . 1.373(4) yes
C4 . H41 . 0.969 no
C5 . C6 . 1.407(3) yes
C5 . H51 . 0.934 no
C6 . C7 . 1.432(4) yes
C7 . H71 . 0.952 no
C8 . C8 3_757 1.528(3) yes
C8 . C9 . 1.520(3) yes
C8 . H81 . 0.962 no
C9 . C10 . 1.539(3) yes
C9 . H91 . 0.988 no
C9 . H92 . 0.985 no
C10 . C10 3_757 1.517(4) yes
C10 . H101 . 0.953 no
C10 . H102 . 0.961 no
C11 . C12 . 1.408(4) yes
C11 . C16 . 1.414(4) yes
C12 . C13 . 1.372(3) yes
C12 . H121 . 0.929 no
C13 . C14 . 1.404(4) yes
C14 . C15 . 1.368(5) yes
C14 . H141 . 0.951 no
C15 . C16 . 1.412(3) yes
C15 . H151 . 0.922 no
C16 . C17 . 1.430(4) yes
C17 . H171 . 0.949 no
C18 . C18 3_656 1.521(3) yes
C18 . C19 . 1.525(3) yes
C18 . H181 . 0.974 no
C19 . C20 . 1.535(3) yes
C19 . H191 . 0.992 no
C19 . H192 . 0.983 no
C20 . C20 3_656 1.530(4) yes
C20 . H201 . 0.969 no
C20 . H202 . 0.965 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
N1 3_757 Ni1 . O1 3_757 95.38(8) yes
N1 3_757 Ni1 . O1 . 177.19(11) yes
O1 3_757 Ni1 . O1 . 82.42(13) yes
N1 3_757 Ni1 . N1 . 86.87(15) yes
O1 3_757 Ni1 . N1 . 177.19(11) yes
O1 . Ni1 . N1 . 95.38(8) yes
O3 3_656 Ni2 . N2 3_656 95.08(8) yes
O3 3_656 Ni2 . O3 . 83.12(13) yes
N2 3_656 Ni2 . O3 . 178.00(11) yes
O3 3_656 Ni2 . N2 . 178.00(11) yes
N2 3_656 Ni2 . N2 . 86.74(15) yes
O3 . Ni2 . N2 . 95.08(8) yes
Ni1 . O1 . C1 . 126.61(18) yes
C3 . O2 . H1 . 111(3) no
Ni2 . O3 . C11 . 127.38(18) yes
C13 . O4 . H2 . 111.5(20) no
H3 . O5 . H4 . 110(3) no
H5 . O6 . H6 . 108(3) no
Ni1 . N1 . C7 . 126.2(2) yes
Ni1 . N1 . C8 . 112.07(14) yes
C7 . N1 . C8 . 121.7(2) yes
Ni2 . N2 . C17 . 126.0(2) yes
Ni2 . N2 . C18 . 112.53(14) yes
C17 . N2 . C18 . 121.5(2) yes
O1 . C1 . C2 . 117.7(3) yes
O1 . C1 . C6 . 123.2(2) yes
C2 . C1 . C6 . 119.1(2) yes
C1 . C2 . C3 . 120.7(3) yes
C1 . C2 . H21 . 119.5 no
C3 . C2 . H21 . 119.8 no
C2 . C3 . O2 . 122.3(2) yes
C2 . C3 . C4 . 120.2(2) yes
O2 . C3 . C4 . 117.5(2) yes
C3 . C4 . C5 . 119.3(2) yes
C3 . C4 . H41 . 120.0 no
C5 . C4 . H41 . 120.7 no
C4 . C5 . C6 . 122.1(3) yes
C4 . C5 . H51 . 119.4 no
C6 . C5 . H51 . 118.5 no
C1 . C6 . C5 . 118.5(3) yes
C1 . C6 . C7 . 122.2(2) yes
C5 . C6 . C7 . 119.3(3) yes
C6 . C7 . N1 . 124.6(3) yes
C6 . C7 . H71 . 117.4 no
N1 . C7 . H71 . 118.0 no
C8 3_757 C8 . N1 . 104.88(12) yes
C8 3_757 C8 . C9 . 111.14(14) yes
N1 . C8 . C9 . 117.00(16) yes
C8 3_757 C8 . H81 . 108.1 no
N1 . C8 . H81 . 106.3 no
C9 . C8 . H81 . 109.0 no
C8 . C9 . C10 . 108.73(17) yes
C8 . C9 . H91 . 111.6 no
C10 . C9 . H91 . 108.2 no
C8 . C9 . H92 . 108.2 no
C10 . C9 . H92 . 109.9 no
H91 . C9 . H92 . 110.1 no
C9 . C10 . C10 3_757 111.47(14) yes
C9 . C10 . H101 . 108.5 no
C10 3_757 C10 . H101 . 109.1 no
C9 . C10 . H102 . 110.0 no
C10 3_757 C10 . H102 . 110.5 no
H101 . C10 . H102 . 107.2 no
O3 . C11 . C12 . 118.0(2) yes
O3 . C11 . C16 . 123.0(2) yes
C12 . C11 . C16 . 119.0(2) yes
C11 . C12 . C13 . 120.7(3) yes
C11 . C12 . H121 . 119.0 no
C13 . C12 . H121 . 120.3 no
C12 . C13 . O4 . 122.6(3) yes
C12 . C13 . C14 . 121.0(3) yes
O4 . C13 . C14 . 116.4(2) yes
C13 . C14 . C15 . 118.6(2) yes
C13 . C14 . H141 . 118.3 no
C15 . C14 . H141 . 123.1 no
C14 . C15 . C16 . 122.3(3) yes
C14 . C15 . H151 . 119.4 no
C16 . C15 . H151 . 118.3 no
C11 . C16 . C15 . 118.3(3) yes
C11 . C16 . C17 . 122.1(2) yes
C15 . C16 . C17 . 119.4(3) yes
C16 . C17 . N2 . 125.3(3) yes
C16 . C17 . H171 . 116.8 no
N2 . C17 . H171 . 117.8 no
C18 3_656 C18 . N2 . 105.15(13) yes
C18 3_656 C18 . C19 . 110.99(15) yes
N2 . C18 . C19 . 117.08(17) yes
C18 3_656 C18 . H181 . 108.2 no
N2 . C18 . H181 . 106.3 no
C19 . C18 . H181 . 108.8 no
C18 . C19 . C20 . 109.01(18) yes
C18 . C19 . H191 . 110.3 no
C20 . C19 . H191 . 109.8 no
C18 . C19 . H192 . 109.6 no
C20 . C19 . H192 . 110.2 no
H191 . C19 . H192 . 107.9 no
C19 . C20 . C20 3_656 112.19(15) yes
C19 . C20 . H201 . 108.4 no
C20 3_656 C20 . H201 . 111.0 no
C19 . C20 . H202 . 109.6 no
C20 3_656 C20 . H202 . 108.0 no
H201 . C20 . H202 . 107.5 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
O2 . H1 . O6 . 170(4) 0.69(3) 2.00(3) 2.686(3) yes
O4 . H2 . O5 . 179(3) 0.90(3) 1.75(3) 2.651(4) yes
O5 . H3 . O1 2_455 151(3) 0.77(3) 2.29(3) 2.990(4) yes
O5 . H3 . O1 4_657 143(3) 0.77(3) 2.31(3) 2.968(4) yes
O5 . H4 . O2 4_656 163(3) 0.97(3) 2.03(3) 2.961(4) yes
O6 . H5 . O4 4_647 169(3) 0.70(3) 2.29(3) 2.971(3) yes
O6 . H6 . O3 2_545 167(4) 0.79(3) 2.01(3) 2.790(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
N1 Ni1 O1 C1 14.6(3) . . . . no
O1 Ni1 O1 C1 -167.1(3) 3_757 . . . no
O1 Ni1 N1 C7 -9.7(3) . . . . no
O1 Ni1 N1 C8 167.65(17) . . . . no
N1 Ni1 N1 C7 168.6(3) 3_757 . . . no
N1 Ni1 N1 C8 -14.04(17) 3_757 . . . no
N2 Ni2 O3 C11 10.7(2) . . . . no
O3 Ni2 O3 C11 -170.2(3) 3_656 . . . no
O3 Ni2 N2 C17 -10.5(2) . . . . no
O3 Ni2 N2 C18 167.29(16) . . . . no
N2 Ni2 N2 C17 168.6(2) 3_656 . . . no
N2 Ni2 N2 C18 -13.56(16) 3_656 . . . no
Ni1 O1 C1 C2 168.4(2) . . . . no
Ni1 O1 C1 C6 -10.7(5) . . . . no
Ni2 O3 C11 C12 175.60(19) . . . . no
Ni2 O3 C11 C16 -5.6(4) . . . . no
C7 N1 C8 C8 -145.5(3) . . . 3_757 no
Ni1 N1 C7 C6 0.8(5) . . . . no
C8 N1 C7 C6 -176.3(3) . . . . no
Ni1 N1 C8 C9 160.69(16) . . . . no
Ni1 N1 C8 C8 37.0(2) . . . 3_757 no
C7 N1 C8 C9 -21.9(4) . . . . no
C18 N2 C17 C16 -172.0(2) . . . . no
Ni2 N2 C18 C19 159.61(19) . . . . no
Ni2 N2 C18 C18 35.9(2) . . . 3_656 no
C17 N2 C18 C19 -22.5(3) . . . . no
C17 N2 C18 C18 -146.2(2) . . . 3_656 no
Ni2 N2 C17 C16 5.7(4) . . . . no
C2 C1 C6 C7 178.5(3) . . . . no
C6 C1 C2 C3 3.1(4) . . . . no
O1 C1 C2 C3 -176.1(3) . . . . no
C2 C1 C6 C5 -2.1(4) . . . . no
O1 C1 C6 C5 177.0(3) . . . . no
O1 C1 C6 C7 -2.4(5) . . . . no
C1 C2 C3 C4 -1.9(4) . . . . no
C1 C2 C3 O2 177.9(3) . . . . no
O2 C3 C4 C5 180.0(3) . . . . no
C2 C3 C4 C5 -0.2(4) . . . . no
C3 C4 C5 C6 1.1(4) . . . . no
C4 C5 C6 C1 0.0(4) . . . . no
C4 C5 C6 C7 179.4(3) . . . . no
C5 C6 C7 N1 -171.8(3) . . . . no
C1 C6 C7 N1 7.6(5) . . . . no
N1 C8 C8 N1 -45.6(2) . . 3_757 3_757 no
N1 C8 C9 C10 -177.84(19) . . . . no
C8 C8 C9 C10 -57.4(2) 3_757 . . . no
C9 C8 C8 C9 59.7(2) . . 3_757 3_757 no
N1 C8 C8 C9 -172.93(18) . . 3_757 3_757 no
C9 C8 C8 N1 -172.93(18) . . 3_757 3_757 no
C8 C9 C10 C10 56.6(2) . . . 3_757 no
C9 C10 C10 C9 -57.3(2) . . 3_757 3_757 no
O3 C11 C12 C13 178.7(2) . . . . no
C16 C11 C12 C13 -0.2(4) . . . . no
O3 C11 C16 C15 -178.7(2) . . . . no
O3 C11 C16 C17 -3.2(4) . . . . no
C12 C11 C16 C15 0.1(4) . . . . no
C12 C11 C16 C17 175.6(2) . . . . no
C11 C12 C13 O4 -178.5(2) . . . . no
C11 C12 C13 C14 0.2(4) . . . . no
O4 C13 C14 C15 178.6(3) . . . . no
C12 C13 C14 C15 -0.1(4) . . . . no
C13 C14 C15 C16 0.1(4) . . . . no
C14 C15 C16 C11 -0.1(4) . . . . no
C14 C15 C16 C17 -175.7(3) . . . . no
C11 C16 C17 N2 3.1(4) . . . . no
C15 C16 C17 N2 178.6(3) . . . . no
N2 C18 C19 C20 -178.5(2) . . . . no
C18 C18 C19 C20 -57.8(3) 3_656 . . . no
N2 C18 C18 N2 -44.0(2) . . 3_656 3_656 no
N2 C18 C18 C19 -171.5(2) . . 3_656 3_656 no
C19 C18 C18 N2 -171.5(2) . . 3_656 3_656 no
C19 C18 C18 C19 61.0(3) . . 3_656 3_656 no
C18 C19 C20 C20 54.7(3) . . . 3_656 no
C19 C20 C20 C19 -54.4(3) . . 3_656 3_656 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 O5 3.790(2) . 2_545 no
Ni1 O5 3.790(2) . 4_647 no
Ni2 C7 3.970(3) . 3_656 no
Ni2 C7 3.970(3) . . no
Ni2 O6 3.803(2) . 4_656 no
Ni2 O6 3.803(2) . 2_455 no
O1 O5 2.991(3) . 2_545 no
O1 N1 2.727(3) . . no
O1 O5 2.968(3) . 4_647 no
O1 O1 2.422(4) . 3_757 no
O1 C7 2.903(3) . . no
O2 O5 2.961(3) . 4_646 no
O2 C2 3.392(3) . 3_756 no
O2 O6 2.686(3) . . no
O3 C17 2.893(4) . . no
O3 O6 2.790(3) . 2_455 no
O3 O6 3.184(3) . 4_656 no
O3 N2 2.727(3) . . no
O3 O3 2.453(4) . 3_656 no
O4 O6 2.971(3) . 4_657 no
O4 O5 2.651(3) . . no
O5 C12 3.343(4) . . no
O5 C13 3.389(4) . . no
O6 C2 3.319(4) . . no
O6 C3 3.394(4) . . no
N1 C8 2.386(3) . 3_757 no
N1 N1 2.543(4) . 3_757 no
N1 C1 2.926(4) . . no
N2 C18 2.389(3) . 3_656 no
N2 N2 2.537(4) . 3_656 no
N2 C11 2.932(4) . . no
C1 C4 3.455(5) . 3_756 no
C2 C4 3.557(4) . 3_756 no
C2 C3 3.359(3) . 3_756 no
C3 C3 3.329(3) . 3_756 no
C5 C5 3.573(3) . 3_756 no
C8 C11 3.599(3) . . no
C11 C14 3.479(4) . 3_657 no
C12 C13 3.414(3) . 3_657 no
C13 C13 3.572(3) . 3_657 no
C15 C16 3.543(3) . 3_657 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 30/05/16 at 14:05:31
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT H(1,X'S) UNTIL H(6) 
CONT ENANTIO 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,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) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 30/05/16 at 14:05:31
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

_vrf_PLAT111_ral1605X            
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry       
RESPONSE: ...
The structure does present some pseudo-symmetry.
ADDSYM suggests that there might be an extra centre of symmetry
 and that the space group could be C2/c.  
As the compound is chiral, an inversion symmetry operation is not an option.
Furthermore, if the space group were to be C2/c, then
reflections h0l: l=2n+1 would need to be systematically extinct.
In fact reflections h0l:l=2n+1 have an average I/sig(I) of 134
(cf. reflections h0l:l=2n with an average I/sig(I) of 386),
so this reflection class is a long way from being absent
and clearly no c-glide is present.

;


#===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_ral1502SN
_database_code_depnum_ccdc_archive 'CCDC 1838520'
_audit_update_record             
;
2018-04-20 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_audit_creation_date             15-07-21
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1502SN\Tony_ral1502SN_data At 12: 6 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.1282(2)
_cell_length_b                   11.3329(4)
_cell_length_c                   18.5868(5)
_cell_angle_alpha                105.604(3)
_cell_angle_beta                 100.863(2)
_cell_angle_gamma                98.646(2)
_cell_volume                     1777.19(10)

_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

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            2

# Given Formula = C17.50 H24 Cl1.50 N2 Ni0.50 O2 
# Dc =      0.70 Fooo =    792.00 Mu =     16.07 M =    753.86
# Found Formula = C35 H47 Cl3 N4 Ni1 O4 
# Dc =      1.41 FOOO =    792.00 Mu =     32.15 M =   1505.70

_chemical_formula_sum            'C35 H47 Cl3 N4 Ni1 O4'
_chemical_formula_moiety         'C34 H46 N4 Ni O4, C H Cl3'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         752.85


_cell_measurement_reflns_used    10403
_cell_measurement_theta_min      4
_cell_measurement_theta_max      72
_cell_measurement_temperature    150

_exptl_crystal_description       lath
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.028
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_max          0.292

_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    3.215

# Sheldrick geometric approximatio 0.81 0.91 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.91
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_radiation_source         'Supernova (Cu) X-ray Source'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
;
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2015)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2015)'
_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            21131
_reflns_number_total             6997
_diffrn_reflns_av_R_equivalents  0.033
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6997 
# Theoretical number of reflections is about 14069 


_diffrn_reflns_theta_min         4.147
_diffrn_reflns_theta_max         72.391
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        72.391
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_reflns_limit_h_min              -11
_reflns_limit_h_max              10
_reflns_limit_k_min              -14
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   2.15
_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         -0.45
_refine_diff_density_max         0.48


# 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         6997
_refine_ls_number_restraints     6
_refine_ls_number_parameters     460
_oxford_refine_ls_R_factor_ref   0.0496
_refine_ls_wR_factor_ref         0.1029
_refine_ls_goodness_of_fit_ref   1.0258
_refine_ls_shift/su_max          0.0056653
_refine_ls_shift/su_mean         0.0003190


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6997
_refine_ls_R_factor_all          0.0496
_refine_ls_wR_factor_all         0.1029

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6628
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_gt          0.1009

# 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 syn
_refine_ls_abs_structure_details 
;
The enantiomer has been assigned by reference to an unchanging chiral
centre in the synthetic procedure.
;


_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) + ( 0.01P)² + 3.96P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               

The compound is enantiomerically pure.
The structure was, however, initially solved in centrosymmetric 
space group P\=1, and refined well. 
Disorder was found in the vicinity of the chiral centres 
(i.e. at C8, C9, C18 and C19), as was expected.
All other atoms were well-behaved.
This suggested that the space group should be P1,
 with two [Ni(C₃₄H₄₆N₄O₄)]
molecules and two chloroform molecules,
with all atoms, apart from those of the disorder, being related to
corresponding atoms by an inversion centre.
This model was set up, with the disordered atom sites been chosen to give
R-configurations at C8 and C9 of the first molecule
and at C108 and C109 of the second, and, to complete chair-conformations
of the cyclohexane rings, with C18 and C19 for molecule 1 and C118 and C119
for molecule 2. 
Constraints were imposed during the refinement to maintain the inversion
relationships of all other atoms.




The H atoms away from the chiral section of the molecule 
were all located in a difference map whilst still in 
space group P\=1, but 
 were repositioned geometrically. 
These 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.
The H atoms of the chiral section of the molecule were added at
calculated positions in the P1 structure and ride on the 
atoms to which they are bonded.



The largest features in the
final difference electron density map are located 
near the coordinating N atom, near chloroform Cl atoms
and within the terminal C₅H₁₀N groups, but all are small.
;

# 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 0.62346(5) 0.51259(4) 0.43318(2) 0.0162 1.0000 Uani . . . . . .
Ni101 Ni 0.37654(5) 0.48741(4) 0.56682(2) 0.0162 1.0000 Uani . . . . . .
Cl1 Cl 0.82066(11) 0.45379(8) 0.25663(6) 0.0488 1.0000 Uani . . . . . .
Cl2 Cl 0.73297(9) 0.18401(7) 0.21622(4) 0.0364 1.0000 Uani . . . . . .
Cl3 Cl 0.53817(9) 0.32114(8) 0.14613(5) 0.0396 1.0000 Uani . . . . . .
Cl101 Cl 0.17934(11) 0.54621(8) 0.74337(6) 0.0488 1.0000 Uani . . . . . .
Cl102 Cl 0.26703(9) 0.81599(7) 0.78378(4) 0.0364 1.0000 Uani . . . . . .
Cl103 Cl 0.46183(9) 0.67886(8) 0.85387(5) 0.0396 1.0000 Uani . . . . . .
O1 O 0.6421(2) 0.34758(16) 0.39995(10) 0.0202 1.0000 Uani . . . . . .
O2 O 0.4816(2) 0.46903(16) 0.34009(10) 0.0215 1.0000 Uani . . . . . .
O3 O 0.7919(2) -0.03325(17) 0.40843(10) 0.0239 1.0000 Uani . . . . . .
O4 O 0.0766(2) 0.50204(19) 0.14869(11) 0.0284 1.0000 Uani . . . . . .
O101 O 0.3579(2) 0.65242(16) 0.60005(10) 0.0202 1.0000 Uani . . . . . .
O102 O 0.5184(2) 0.53097(16) 0.65991(10) 0.0215 1.0000 Uani . . . . . .
O103 O 0.2081(2) 1.03325(17) 0.59157(10) 0.0239 1.0000 Uani . . . . . .
O104 O 0.9234(2) 0.49796(19) 0.85131(11) 0.0284 1.0000 Uani . . . . . .
N1 N 0.7645(3) 0.55174(19) 0.52630(13) 0.0216 1.0000 Uani . . . . . .
N2 N 0.6007(3) 0.6768(2) 0.46463(13) 0.0244 1.0000 Uani . . . . . .
N3 N 0.7506(3) -0.2621(2) 0.21769(13) 0.0264 1.0000 Uani . . . . . .
N4 N -0.1235(3) 0.2201(2) -0.01127(14) 0.0300 1.0000 Uani . . . . . .
N101 N 0.2355(3) 0.44826(19) 0.47370(13) 0.0216 1.0000 Uani . . . . . .
N102 N 0.3993(3) 0.3232(2) 0.53537(13) 0.0244 1.0000 Uani . . . . . .
N103 N 0.2494(3) 1.2621(2) 0.78231(13) 0.0264 1.0000 Uani . . . . . .
N104 N 1.1235(3) 0.7799(2) 1.01127(14) 0.0300 1.0000 Uani . . . . . .
C1 C 0.7239(3) 0.2887(2) 0.43805(14) 0.0169 1.0000 Uani . . . . . .
C2 C 0.7104(3) 0.1586(2) 0.40334(14) 0.0189 1.0000 Uani . . . . . .
C3 C 0.7944(3) 0.0914(2) 0.44012(14) 0.0191 1.0000 Uani . . . . . .
C4 C 0.8929(3) 0.1486(2) 0.51372(14) 0.0208 1.0000 Uani . . . . . .
C5 C 0.9054(3) 0.2740(2) 0.54784(14) 0.0199 1.0000 Uani . . . . . .
C6 C 0.8230(3) 0.3468(2) 0.51155(14) 0.0181 1.0000 Uani . . . . . .
C7 C 0.8386(3) 0.4765(2) 0.55166(15) 0.0221 1.0000 Uani . . . . . .
C8 C 0.8124(6) 0.6889(4) 0.5637(3) 0.0174 1.0000 Uani . . . . . .
C9 C 0.6665(6) 0.7357(4) 0.5503(3) 0.0171 1.0000 Uani . . . . . .
C10 C 0.5065(3) 0.7270(2) 0.42795(15) 0.0227 1.0000 Uani . . . . . .
C11 C 0.4026(3) 0.6654(2) 0.35541(14) 0.0195 1.0000 Uani . . . . . .
C12 C 0.3015(3) 0.7311(3) 0.32325(16) 0.0254 1.0000 Uani . . . . . .
C13 C 0.1951(3) 0.6758(3) 0.25544(16) 0.0270 1.0000 Uani . . . . . .
C14 C 0.1858(3) 0.5488(3) 0.21607(15) 0.0229 1.0000 Uani . . . . . .
C15 C 0.2825(3) 0.4812(2) 0.24483(15) 0.0212 1.0000 Uani . . . . . .
C16 C 0.3933(3) 0.5376(2) 0.31498(14) 0.0183 1.0000 Uani . . . . . .
C17 C 0.8908(3) 0.7324(2) 0.64932(15) 0.0247 1.0000 Uani . . . . . .
C18 C 0.9165(7) 0.8730(5) 0.6828(3) 0.0280 1.0000 Uani . . . . . .
C19 C 0.7714(7) 0.9219(5) 0.6650(3) 0.0286 1.0000 Uani . . . . . .
C20 C 0.7008(3) 0.8809(2) 0.57717(15) 0.0250 1.0000 Uani . . . . . .
C21 C 0.7207(3) -0.0888(2) 0.32806(15) 0.0233 1.0000 Uani . . . . . .
C22 C 0.7800(3) -0.2084(3) 0.30074(15) 0.0262 1.0000 Uani . . . . . .
C23 C 0.5899(4) -0.3087(3) 0.17966(18) 0.0334 1.0000 Uani . . . . . .
C24 C 0.5712(4) -0.3839(3) 0.09572(18) 0.0394 1.0000 Uani . . . . . .
C25 C 0.6521(4) -0.3070(3) 0.05396(17) 0.0378 1.0000 Uani . . . . . .
C26 C 0.8177(4) -0.2559(3) 0.09706(18) 0.0376 1.0000 Uani . . . . . .
C27 C 0.8272(3) -0.1826(3) 0.18039(16) 0.0274 1.0000 Uani . . . . . .
C28 C 0.0475(3) 0.3701(3) 0.10853(16) 0.0292 1.0000 Uani . . . . . .
C29 C -0.0904(3) 0.3468(3) 0.04257(16) 0.0315 1.0000 Uani . . . . . .
C30 C -0.2222(4) 0.2169(3) -0.08389(18) 0.0420 1.0000 Uani . . . . . .
C31 C -0.2513(5) 0.0906(4) -0.1440(2) 0.0502 1.0000 Uani . . . . . .
C32 C -0.3195(5) -0.0126(4) -0.1158(2) 0.0572 1.0000 Uani . . . . . .
C33 C -0.2230(6) -0.0049(4) -0.0378(2) 0.0646 1.0000 Uani . . . . . .
C34 C -0.1950(5) 0.1259(4) 0.0188(2) 0.0473 1.0000 Uani . . . . . .
C35 C 0.6660(3) 0.3251(3) 0.23070(16) 0.0277 1.0000 Uani . . . . . .
C101 C 0.2761(3) 0.7113(2) 0.56195(14) 0.0169 1.0000 Uani . . . . . .
C102 C 0.2896(3) 0.8414(2) 0.59666(14) 0.0189 1.0000 Uani . . . . . .
C103 C 0.2056(3) 0.9086(2) 0.55988(14) 0.0191 1.0000 Uani . . . . . .
C104 C 0.1071(3) 0.8514(2) 0.48628(14) 0.0208 1.0000 Uani . . . . . .
C105 C 0.0946(3) 0.7260(2) 0.45216(14) 0.0199 1.0000 Uani . . . . . .
C106 C 0.1770(3) 0.6532(2) 0.48845(14) 0.0181 1.0000 Uani . . . . . .
C107 C 0.1614(3) 0.5235(2) 0.44834(15) 0.0221 1.0000 Uani . . . . . .
C108 C 0.2453(6) 0.3251(4) 0.4188(3) 0.0165 1.0000 Uani . . . . . .
C109 C 0.2669(5) 0.2418(4) 0.4699(3) 0.0166 1.0000 Uani . . . . . .
C110 C 0.4935(3) 0.2730(2) 0.57205(15) 0.0227 1.0000 Uani . . . . . .
C111 C 0.5974(3) 0.3346(2) 0.64459(14) 0.0195 1.0000 Uani . . . . . .
C112 C 0.6985(3) 0.2689(3) 0.67675(16) 0.0254 1.0000 Uani . . . . . .
C113 C 0.8049(3) 0.3242(3) 0.74456(16) 0.0270 1.0000 Uani . . . . . .
C114 C 0.8142(3) 0.4512(3) 0.78393(15) 0.0229 1.0000 Uani . . . . . .
C115 C 0.7175(3) 0.5188(2) 0.75517(15) 0.0212 1.0000 Uani . . . . . .
C116 C 0.6067(3) 0.4624(2) 0.68502(14) 0.0183 1.0000 Uani . . . . . .
C117 C 0.1092(3) 0.2676(2) 0.35068(15) 0.0247 1.0000 Uani . . . . . .
C118 C 0.1350(7) 0.1401(5) 0.3048(3) 0.0270 1.0000 Uani . . . . . .
C119 C 0.1597(6) 0.0542(4) 0.3547(3) 0.0267 1.0000 Uani . . . . . .
C120 C 0.2992(3) 0.1191(2) 0.42283(15) 0.0250 1.0000 Uani . . . . . .
C121 C 0.2793(3) 1.0888(2) 0.67194(15) 0.0233 1.0000 Uani . . . . . .
C122 C 0.2200(3) 1.2084(3) 0.69926(15) 0.0262 1.0000 Uani . . . . . .
C123 C 0.4101(4) 1.3087(3) 0.82034(18) 0.0334 1.0000 Uani . . . . . .
C124 C 0.4288(4) 1.3839(3) 0.90428(18) 0.0394 1.0000 Uani . . . . . .
C125 C 0.3479(4) 1.3070(3) 0.94604(17) 0.0378 1.0000 Uani . . . . . .
C126 C 0.1823(4) 1.2559(3) 0.90294(18) 0.0376 1.0000 Uani . . . . . .
C127 C 0.1728(3) 1.1826(3) 0.81961(16) 0.0274 1.0000 Uani . . . . . .
C128 C 0.9525(3) 0.6299(3) 0.89147(16) 0.0292 1.0000 Uani . . . . . .
C129 C 1.0904(3) 0.6532(3) 0.95743(16) 0.0315 1.0000 Uani . . . . . .
C130 C 1.2222(4) 0.7831(3) 1.08389(18) 0.0420 1.0000 Uani . . . . . .
C131 C 1.2513(5) 0.9094(4) 1.1440(2) 0.0502 1.0000 Uani . . . . . .
C132 C 1.3195(5) 1.0126(4) 1.1158(2) 0.0572 1.0000 Uani . . . . . .
C133 C 1.2230(6) 1.0049(4) 1.0378(2) 0.0646 1.0000 Uani . . . . . .
C134 C 1.1950(5) 0.8741(4) 0.9812(2) 0.0473 1.0000 Uani . . . . . .
C135 C 0.3340(3) 0.6749(3) 0.76930(16) 0.0277 1.0000 Uani . . . . . .
H21 H 0.6439 0.1200 0.3558 0.0219 1.0000 Uiso R . . . . .
H41 H 0.9462 0.1017 0.5390 0.0244 1.0000 Uiso R . . . . .
H51 H 0.9711 0.3146 0.5974 0.0225 1.0000 Uiso R . . . . .
H71 H 0.9080 0.5096 0.6009 0.0276 1.0000 Uiso R . . . . .
H81 H 0.8789 0.7227 0.5372 0.0209 1.0000 Uiso R . . . . .
H91 H 0.5995 0.7047 0.5776 0.0204 1.0000 Uiso R . . . . .
H101 H 0.5050 0.8113 0.4516 0.0270 1.0000 Uiso R . . . . .
H121 H 0.3086 0.8157 0.3499 0.0298 1.0000 Uiso R . . . . .
H131 H 0.1282 0.7192 0.2345 0.0322 1.0000 Uiso R . . . . .
H151 H 0.2760 0.3979 0.2187 0.0250 1.0000 Uiso R . . . . .
H171 H 0.9866 0.7084 0.6559 0.0296 1.0000 Uiso R . . . . .
H172 H 0.8285 0.6937 0.6757 0.0296 1.0000 Uiso R . . . . .
H181 H 0.9528 0.8953 0.7370 0.0339 1.0000 Uiso R . . . . .
H182 H 0.9910 0.9112 0.6618 0.0339 1.0000 Uiso R . . . . .
H191 H 0.7953 1.0108 0.6843 0.0343 1.0000 Uiso R . . . . .
H192 H 0.6994 0.8896 0.6895 0.0343 1.0000 Uiso R . . . . .
H201 H 0.7709 0.9128 0.5517 0.0300 1.0000 Uiso R . . . . .
H202 H 0.6093 0.9103 0.5669 0.0300 1.0000 Uiso R . . . . .
H211 H 0.7454 -0.0310 0.2990 0.0269 1.0000 Uiso R . . . . .
H212 H 0.6101 -0.1099 0.3207 0.0272 1.0000 Uiso R . . . . .
H221 H 0.8936 -0.1865 0.3200 0.0311 1.0000 Uiso R . . . . .
H222 H 0.7373 -0.2701 0.3229 0.0309 1.0000 Uiso R . . . . .
H231 H 0.5429 -0.3608 0.2064 0.0401 1.0000 Uiso R . . . . .
H232 H 0.5426 -0.2372 0.1803 0.0400 1.0000 Uiso R . . . . .
H241 H 0.6170 -0.4568 0.0927 0.0468 1.0000 Uiso R . . . . .
H242 H 0.4642 -0.4118 0.0691 0.0467 1.0000 Uiso R . . . . .
H251 H 0.6438 -0.3569 0.0019 0.0460 1.0000 Uiso R . . . . .
H252 H 0.6027 -0.2357 0.0528 0.0461 1.0000 Uiso R . . . . .
H261 H 0.8659 -0.3280 0.0965 0.0460 1.0000 Uiso R . . . . .
H262 H 0.8690 -0.2006 0.0732 0.0462 1.0000 Uiso R . . . . .
H271 H 0.9326 -0.1518 0.2092 0.0329 1.0000 Uiso R . . . . .
H272 H 0.7804 -0.1113 0.1800 0.0330 1.0000 Uiso R . . . . .
H281 H 0.0255 0.3222 0.1439 0.0347 1.0000 Uiso R . . . . .
H282 H 0.1354 0.3491 0.0887 0.0346 1.0000 Uiso R . . . . .
H291 H -0.0690 0.4071 0.0153 0.0374 1.0000 Uiso R . . . . .
H292 H -0.1787 0.3619 0.0639 0.0373 1.0000 Uiso R . . . . .
H301 H -0.3208 0.2326 -0.0737 0.0493 1.0000 Uiso R . . . . .
H302 H -0.1746 0.2816 -0.1028 0.0493 1.0000 Uiso R . . . . .
H311 H -0.3155 0.0898 -0.1918 0.0610 1.0000 Uiso R . . . . .
H312 H -0.1525 0.0743 -0.1544 0.0607 1.0000 Uiso R . . . . .
H321 H -0.4230 -0.0042 -0.1096 0.0691 1.0000 Uiso R . . . . .
H322 H -0.3270 -0.0940 -0.1512 0.0695 1.0000 Uiso R . . . . .
H331 H -0.2777 -0.0649 -0.0173 0.0773 1.0000 Uiso R . . . . .
H332 H -0.1283 -0.0272 -0.0444 0.0770 1.0000 Uiso R . . . . .
H341 H -0.2948 0.1438 0.0260 0.0570 1.0000 Uiso R . . . . .
H342 H -0.1327 0.1315 0.0693 0.0567 1.0000 Uiso R . . . . .
H351 H 0.6143 0.3316 0.2717 0.0331 1.0000 Uiso R . . . . .
H1021 H 0.3561 0.8800 0.6442 0.0219 1.0000 Uiso R . . . . .
H1041 H 0.0538 0.8983 0.4610 0.0244 1.0000 Uiso R . . . . .
H1051 H 0.0289 0.6854 0.4026 0.0225 1.0000 Uiso R . . . . .
H1071 H 0.0920 0.4904 0.3991 0.0276 1.0000 Uiso R . . . . .
H1081 H 0.3344 0.3383 0.4001 0.0198 1.0000 Uiso R . . . . .
H1091 H 0.1782 0.2253 0.4884 0.0200 1.0000 Uiso R . . . . .
H1101 H 0.4950 0.1887 0.5484 0.0270 1.0000 Uiso R . . . . .
H1121 H 0.6914 0.1843 0.6501 0.0298 1.0000 Uiso R . . . . .
H1131 H 0.8718 0.2808 0.7655 0.0322 1.0000 Uiso R . . . . .
H1151 H 0.7240 0.6021 0.7813 0.0250 1.0000 Uiso R . . . . .
H1171 H 0.0184 0.2554 0.3681 0.0296 1.0000 Uiso R . . . . .
H1172 H 0.1012 0.3210 0.3192 0.0296 1.0000 Uiso R . . . . .
H1181 H 0.2224 0.1545 0.2850 0.0320 1.0000 Uiso R . . . . .
H1182 H 0.0480 0.1000 0.2633 0.0320 1.0000 Uiso R . . . . .
H1191 H 0.0717 0.0374 0.3736 0.0320 1.0000 Uiso R . . . . .
H1192 H 0.1772 -0.0224 0.3248 0.0320 1.0000 Uiso R . . . . .
H1201 H 0.3152 0.0662 0.4542 0.0300 1.0000 Uiso R . . . . .
H1202 H 0.3874 0.1365 0.4041 0.0300 1.0000 Uiso R . . . . .
H1211 H 0.2546 1.0310 0.7010 0.0269 1.0000 Uiso R . . . . .
H1212 H 0.3899 1.1099 0.6793 0.0272 1.0000 Uiso R . . . . .
H1221 H 0.1064 1.1865 0.6800 0.0311 1.0000 Uiso R . . . . .
H1222 H 0.2627 1.2701 0.6771 0.0309 1.0000 Uiso R . . . . .
H1231 H 0.4571 1.3608 0.7936 0.0401 1.0000 Uiso R . . . . .
H1232 H 0.4574 1.2372 0.8197 0.0400 1.0000 Uiso R . . . . .
H1241 H 0.3830 1.4568 0.9073 0.0468 1.0000 Uiso R . . . . .
H1242 H 0.5358 1.4118 0.9309 0.0467 1.0000 Uiso R . . . . .
H1251 H 0.3562 1.3569 0.9981 0.0460 1.0000 Uiso R . . . . .
H1252 H 0.3973 1.2357 0.9472 0.0461 1.0000 Uiso R . . . . .
H1261 H 0.1341 1.3280 0.9035 0.0460 1.0000 Uiso R . . . . .
H1262 H 0.1310 1.2006 0.9268 0.0462 1.0000 Uiso R . . . . .
H1271 H 0.0674 1.1518 0.7908 0.0329 1.0000 Uiso R . . . . .
H1272 H 0.2196 1.1113 0.8200 0.0330 1.0000 Uiso R . . . . .
H1281 H 0.9745 0.6778 0.8561 0.0347 1.0000 Uiso R . . . . .
H1282 H 0.8646 0.6509 0.9113 0.0346 1.0000 Uiso R . . . . .
H1291 H 1.0690 0.5929 0.9847 0.0374 1.0000 Uiso R . . . . .
H1292 H 1.1787 0.6381 0.9361 0.0373 1.0000 Uiso R . . . . .
H1301 H 1.3208 0.7674 1.0737 0.0493 1.0000 Uiso R . . . . .
H1302 H 1.1746 0.7184 1.1028 0.0493 1.0000 Uiso R . . . . .
H1311 H 1.3155 0.9102 1.1918 0.0610 1.0000 Uiso R . . . . .
H1312 H 1.1525 0.9257 1.1544 0.0607 1.0000 Uiso R . . . . .
H1321 H 1.4230 1.0042 1.1096 0.0691 1.0000 Uiso R . . . . .
H1322 H 1.3270 1.0940 1.1512 0.0695 1.0000 Uiso R . . . . .
H1331 H 1.2777 1.0649 1.0173 0.0773 1.0000 Uiso R . . . . .
H1332 H 1.1283 1.0272 1.0444 0.0770 1.0000 Uiso R . . . . .
H1341 H 1.2948 0.8562 0.9740 0.0570 1.0000 Uiso R . . . . .
H1342 H 1.1327 0.8685 0.9307 0.0567 1.0000 Uiso R . . . . .
H1351 H 0.3857 0.6684 0.7283 0.0331 1.0000 Uiso R . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.892(19)
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 . Ni101 . 3.6917(9) yes
Ni1 . O1 . 1.8495(17) yes
Ni1 . O2 . 1.8490(18) yes
Ni1 . N1 . 1.851(2) yes
Ni1 . N2 . 1.851(2) yes
Ni101 . O101 . 1.8495(17) yes
Ni101 . O102 . 1.8490(18) yes
Ni101 . N101 . 1.851(2) yes
Ni101 . N102 . 1.851(2) yes
Cl1 . C35 . 1.761(3) yes
Cl2 . C35 . 1.769(3) yes
Cl3 . C35 . 1.758(3) yes
Cl101 . C135 . 1.761(3) yes
Cl102 . C135 . 1.769(3) yes
Cl103 . C135 . 1.758(3) yes
O1 . C1 . 1.307(3) yes
O2 . C16 . 1.308(3) yes
O3 . C3 . 1.371(3) yes
O3 . C21 . 1.434(3) yes
O4 . C14 . 1.363(3) yes
O4 . C28 . 1.438(3) yes
O101 . C101 . 1.307(3) yes
O102 . C116 . 1.308(3) yes
O103 . C103 . 1.371(3) yes
O103 . C121 . 1.434(3) yes
O104 . C114 . 1.363(3) yes
O104 . C128 . 1.438(3) yes
N1 . C7 . 1.295(3) yes
N1 . C8 . 1.481(5) yes
N2 . C9 . 1.513(5) yes
N2 . C10 . 1.289(3) yes
N3 . C22 . 1.454(3) yes
N3 . C23 . 1.451(4) yes
N3 . C27 . 1.453(4) yes
N4 . C29 . 1.462(4) yes
N4 . C30 . 1.463(4) yes
N4 . C34 . 1.459(4) yes
N101 . C107 . 1.295(3) yes
N101 . C108 . 1.517(5) yes
N102 . C109 . 1.517(5) yes
N102 . C110 . 1.289(3) yes
N103 . C122 . 1.454(3) yes
N103 . C123 . 1.451(4) yes
N103 . C127 . 1.453(4) yes
N104 . C129 . 1.462(4) yes
N104 . C130 . 1.463(4) yes
N104 . C134 . 1.459(4) yes
C1 . C2 . 1.418(3) yes
C1 . C6 . 1.410(3) yes
C2 . C3 . 1.376(3) yes
C2 . H21 . 0.922 no
C3 . C4 . 1.409(4) yes
C4 . C5 . 1.368(4) yes
C4 . H41 . 0.932 no
C5 . C6 . 1.413(3) yes
C5 . H51 . 0.950 no
C6 . C7 . 1.430(3) yes
C7 . H71 . 0.951 no
C8 . C9 . 1.508(7) yes
C8 . C17 . 1.526(5) yes
C8 . H81 . 0.950 no
C9 . C20 . 1.550(5) yes
C9 . H91 . 0.950 no
C10 . C11 . 1.420(4) yes
C10 . H101 . 0.942 no
C11 . C12 . 1.414(4) yes
C11 . C16 . 1.423(3) yes
C12 . C13 . 1.362(4) yes
C12 . H121 . 0.940 no
C13 . C14 . 1.409(4) yes
C13 . H131 . 0.933 no
C14 . C15 . 1.377(4) yes
C15 . C16 . 1.411(4) yes
C15 . H151 . 0.926 no
C17 . C18 . 1.510(6) yes
C17 . H171 . 0.950 no
C17 . H172 . 0.950 no
C18 . C19 . 1.524(9) yes
C18 . H181 . 0.950 no
C18 . H182 . 0.950 no
C19 . C20 . 1.551(6) yes
C19 . H191 . 0.950 no
C19 . H192 . 0.950 no
C20 . H201 . 0.950 no
C20 . H202 . 0.950 no
C21 . C22 . 1.530(3) yes
C21 . H211 . 0.982 no
C21 . H212 . 0.976 no
C22 . H221 . 1.000 no
C22 . H222 . 0.972 no
C23 . C24 . 1.526(4) yes
C23 . H231 . 0.970 no
C23 . H232 . 0.972 no
C24 . C25 . 1.514(5) yes
C24 . H241 . 0.975 no
C24 . H242 . 0.969 no
C25 . C26 . 1.514(5) yes
C25 . H251 . 0.963 no
C25 . H252 . 0.986 no
C26 . C27 . 1.527(4) yes
C26 . H261 . 0.984 no
C26 . H262 . 0.974 no
C27 . H271 . 0.969 no
C27 . H272 . 0.970 no
C28 . C29 . 1.517(4) yes
C28 . H281 . 0.989 no
C28 . H282 . 0.979 no
C29 . H291 . 0.973 no
C29 . H292 . 0.981 no
C30 . C31 . 1.511(5) yes
C30 . H301 . 0.986 no
C30 . H302 . 0.975 no
C31 . C32 . 1.504(6) yes
C31 . H311 . 0.965 no
C31 . H312 . 0.991 no
C32 . C33 . 1.520(6) yes
C32 . H321 . 0.987 no
C32 . H322 . 0.963 no
C33 . C34 . 1.521(5) yes
C33 . H331 . 0.982 no
C33 . H332 . 0.956 no
C34 . H341 . 0.988 no
C34 . H342 . 0.982 no
C35 . H351 . 0.961 no
C101 . C102 . 1.418(3) yes
C101 . C106 . 1.410(3) yes
C102 . C103 . 1.376(3) yes
C102 . H1021 . 0.922 no
C103 . C104 . 1.409(4) yes
C104 . C105 . 1.368(4) yes
C104 . H1041 . 0.932 no
C105 . C106 . 1.413(3) yes
C105 . H1051 . 0.950 no
C106 . C107 . 1.430(3) yes
C107 . H1071 . 0.951 no
C108 . C109 . 1.516(7) yes
C108 . C117 . 1.514(5) yes
C108 . H1081 . 0.950 no
C109 . C120 . 1.534(5) yes
C109 . H1091 . 0.950 no
C110 . C111 . 1.420(4) yes
C110 . H1101 . 0.942 no
C111 . C112 . 1.414(4) yes
C111 . C116 . 1.423(3) yes
C112 . C113 . 1.362(4) yes
C112 . H1121 . 0.940 no
C113 . C114 . 1.409(4) yes
C113 . H1131 . 0.933 no
C114 . C115 . 1.377(4) yes
C115 . C116 . 1.411(4) yes
C115 . H1151 . 0.926 no
C117 . C118 . 1.544(6) yes
C117 . H1171 . 0.950 no
C117 . H1172 . 0.950 no
C118 . C119 . 1.528(8) yes
C118 . H1181 . 0.950 no
C118 . H1182 . 0.950 no
C119 . C120 . 1.542(5) yes
C119 . H1191 . 0.950 no
C119 . H1192 . 0.950 no
C120 . H1201 . 0.950 no
C120 . H1202 . 0.950 no
C121 . C122 . 1.530(3) yes
C121 . H1211 . 0.982 no
C121 . H1212 . 0.976 no
C122 . H1221 . 1.000 no
C122 . H1222 . 0.972 no
C123 . C124 . 1.526(4) yes
C123 . H1231 . 0.970 no
C123 . H1232 . 0.972 no
C124 . C125 . 1.514(5) yes
C124 . H1241 . 0.975 no
C124 . H1242 . 0.969 no
C125 . C126 . 1.514(5) yes
C125 . H1251 . 0.963 no
C125 . H1252 . 0.986 no
C126 . C127 . 1.527(4) yes
C126 . H1261 . 0.984 no
C126 . H1262 . 0.974 no
C127 . H1271 . 0.969 no
C127 . H1272 . 0.970 no
C128 . C129 . 1.517(4) yes
C128 . H1281 . 0.989 no
C128 . H1282 . 0.979 no
C129 . H1291 . 0.973 no
C129 . H1292 . 0.981 no
C130 . C131 . 1.511(5) yes
C130 . H1301 . 0.986 no
C130 . H1302 . 0.975 no
C131 . C132 . 1.504(6) yes
C131 . H1311 . 0.965 no
C131 . H1312 . 0.991 no
C132 . C133 . 1.520(6) yes
C132 . H1321 . 0.987 no
C132 . H1322 . 0.963 no
C133 . C134 . 1.521(5) yes
C133 . H1331 . 0.982 no
C133 . H1332 . 0.956 no
C134 . H1341 . 0.988 no
C134 . H1342 . 0.982 no
C135 . H1351 . 0.961 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
Ni101 . Ni1 . O1 . 99.69(6) yes
Ni101 . Ni1 . O2 . 101.77(6) yes
O1 . Ni1 . O2 . 83.74(7) yes
Ni101 . Ni1 . N1 . 77.79(7) yes
O1 . Ni1 . N1 . 94.87(8) yes
O2 . Ni1 . N1 . 178.47(9) yes
Ni101 . Ni1 . N2 . 80.24(8) yes
O1 . Ni1 . N2 . 178.65(9) yes
O2 . Ni1 . N2 . 94.94(9) yes
N1 . Ni1 . N2 . 86.43(9) yes
Ni1 . Ni101 . O101 . 99.69(6) yes
Ni1 . Ni101 . O102 . 101.77(6) yes
O101 . Ni101 . O102 . 83.74(7) yes
Ni1 . Ni101 . N101 . 77.79(7) yes
O101 . Ni101 . N101 . 94.87(8) yes
O102 . Ni101 . N101 . 178.47(9) yes
Ni1 . Ni101 . N102 . 80.24(8) yes
O101 . Ni101 . N102 . 178.65(9) yes
O102 . Ni101 . N102 . 94.94(9) yes
N101 . Ni101 . N102 . 86.43(9) yes
Ni1 . O1 . C1 . 127.54(16) yes
Ni1 . O2 . C16 . 127.78(16) yes
C3 . O3 . C21 . 117.17(19) yes
C14 . O4 . C28 . 118.5(2) yes
Ni101 . O101 . C101 . 127.54(16) yes
Ni101 . O102 . C116 . 127.78(16) yes
C103 . O103 . C121 . 117.17(19) yes
C114 . O104 . C128 . 118.5(2) yes
Ni1 . N1 . C7 . 126.76(18) yes
Ni1 . N1 . C8 . 111.6(2) yes
C7 . N1 . C8 . 120.4(3) yes
Ni1 . N2 . C9 . 110.8(2) yes
Ni1 . N2 . C10 . 126.44(19) yes
C9 . N2 . C10 . 120.0(3) yes
C22 . N3 . C23 . 113.9(2) yes
C22 . N3 . C27 . 114.1(2) yes
C23 . N3 . C27 . 111.8(2) yes
C29 . N4 . C30 . 109.2(3) yes
C29 . N4 . C34 . 112.6(3) yes
C30 . N4 . C34 . 110.0(3) yes
Ni101 . N101 . C107 . 126.76(18) yes
Ni101 . N101 . C108 . 111.2(2) yes
C107 . N101 . C108 . 120.2(3) yes
Ni101 . N102 . C109 . 111.5(2) yes
Ni101 . N102 . C110 . 126.44(19) yes
C109 . N102 . C110 . 120.5(3) yes
C122 . N103 . C123 . 113.9(2) yes
C122 . N103 . C127 . 114.1(2) yes
C123 . N103 . C127 . 111.8(2) yes
C129 . N104 . C130 . 109.2(3) yes
C129 . N104 . C134 . 112.6(3) yes
C130 . N104 . C134 . 110.0(3) yes
O1 . C1 . C2 . 117.7(2) yes
O1 . C1 . C6 . 123.9(2) yes
C2 . C1 . C6 . 118.5(2) yes
C1 . C2 . C3 . 120.6(2) yes
C1 . C2 . H21 . 118.6 no
C3 . C2 . H21 . 120.8 no
C2 . C3 . O3 . 123.6(2) yes
C2 . C3 . C4 . 121.2(2) yes
O3 . C3 . C4 . 115.2(2) yes
C3 . C4 . C5 . 118.5(2) yes
C3 . C4 . H41 . 120.6 no
C5 . C4 . H41 . 120.8 no
C4 . C5 . C6 . 122.0(2) yes
C4 . C5 . H51 . 120.0 no
C6 . C5 . H51 . 117.9 no
C5 . C6 . C1 . 119.2(2) yes
C5 . C6 . C7 . 118.9(2) yes
C1 . C6 . C7 . 121.9(2) yes
C6 . C7 . N1 . 124.9(2) yes
C6 . C7 . H71 . 117.4 no
N1 . C7 . H71 . 117.7 no
N1 . C8 . C9 . 104.1(4) yes
N1 . C8 . C17 . 116.4(4) yes
C9 . C8 . C17 . 110.6(4) yes
N1 . C8 . H81 . 108.5 no
C9 . C8 . H81 . 108.5 no
C17 . C8 . H81 . 108.6 no
N2 . C9 . C8 . 103.0(4) yes
N2 . C9 . C20 . 114.1(3) yes
C8 . C9 . C20 . 110.4(4) yes
N2 . C9 . H91 . 109.7 no
C8 . C9 . H91 . 109.7 no
C20 . C9 . H91 . 109.7 no
N2 . C10 . C11 . 125.6(2) yes
N2 . C10 . H101 . 117.4 no
C11 . C10 . H101 . 117.0 no
C10 . C11 . C12 . 119.4(2) yes
C10 . C11 . C16 . 121.9(2) yes
C12 . C11 . C16 . 118.7(2) yes
C11 . C12 . C13 . 122.3(3) yes
C11 . C12 . H121 . 118.4 no
C13 . C12 . H121 . 119.3 no
C12 . C13 . C14 . 118.7(2) yes
C12 . C13 . H131 . 122.1 no
C14 . C13 . H131 . 119.2 no
C13 . C14 . O4 . 114.5(2) yes
C13 . C14 . C15 . 121.1(2) yes
O4 . C14 . C15 . 124.4(2) yes
C14 . C15 . C16 . 120.6(2) yes
C14 . C15 . H151 . 120.8 no
C16 . C15 . H151 . 118.6 no
C11 . C16 . C15 . 118.6(2) yes
C11 . C16 . O2 . 123.2(2) yes
C15 . C16 . O2 . 118.2(2) yes
C8 . C17 . C18 . 111.2(3) yes
C8 . C17 . H171 . 109.0 no
C18 . C17 . H171 . 109.0 no
C8 . C17 . H172 . 109.1 no
C18 . C17 . H172 . 109.1 no
H171 . C17 . H172 . 109.5 no
C17 . C18 . C19 . 112.6(5) yes
C17 . C18 . H181 . 108.7 no
C19 . C18 . H181 . 108.7 no
C17 . C18 . H182 . 108.7 no
C19 . C18 . H182 . 108.6 no
H181 . C18 . H182 . 109.5 no
C18 . C19 . C20 . 111.1(4) yes
C18 . C19 . H191 . 109.1 no
C20 . C19 . H191 . 109.1 no
C18 . C19 . H192 . 109.0 no
C20 . C19 . H192 . 109.1 no
H191 . C19 . H192 . 109.5 no
C9 . C20 . C19 . 105.9(3) yes
C9 . C20 . H201 . 110.4 no
C19 . C20 . H201 . 110.4 no
C9 . C20 . H202 . 110.3 no
C19 . C20 . H202 . 110.4 no
H201 . C20 . H202 . 109.5 no
O3 . C21 . C22 . 106.9(2) yes
O3 . C21 . H211 . 110.9 no
C22 . C21 . H211 . 110.6 no
O3 . C21 . H212 . 109.7 no
C22 . C21 . H212 . 109.7 no
H211 . C21 . H212 . 108.9 no
C21 . C22 . N3 . 115.1(2) yes
C21 . C22 . H221 . 107.6 no
N3 . C22 . H221 . 105.8 no
C21 . C22 . H222 . 108.9 no
N3 . C22 . H222 . 110.0 no
H221 . C22 . H222 . 109.3 no
N3 . C23 . C24 . 110.2(3) yes
N3 . C23 . H231 . 109.2 no
C24 . C23 . H231 . 110.2 no
N3 . C23 . H232 . 108.3 no
C24 . C23 . H232 . 107.8 no
H231 . C23 . H232 . 111.0 no
C23 . C24 . C25 . 111.3(3) yes
C23 . C24 . H241 . 110.3 no
C25 . C24 . H241 . 106.6 no
C23 . C24 . H242 . 110.9 no
C25 . C24 . H242 . 108.9 no
H241 . C24 . H242 . 108.9 no
C24 . C25 . C26 . 109.9(3) yes
C24 . C25 . H251 . 110.4 no
C26 . C25 . H251 . 111.0 no
C24 . C25 . H252 . 108.3 no
C26 . C25 . H252 . 108.4 no
H251 . C25 . H252 . 108.8 no
C25 . C26 . C27 . 109.8(3) yes
C25 . C26 . H261 . 107.3 no
C27 . C26 . H261 . 108.9 no
C25 . C26 . H262 . 110.7 no
C27 . C26 . H262 . 109.0 no
H261 . C26 . H262 . 110.9 no
C26 . C27 . N3 . 110.5(2) yes
C26 . C27 . H271 . 110.7 no
N3 . C27 . H271 . 108.2 no
C26 . C27 . H272 . 107.9 no
N3 . C27 . H272 . 110.9 no
H271 . C27 . H272 . 108.6 no
O4 . C28 . C29 . 105.1(2) yes
O4 . C28 . H281 . 109.2 no
C29 . C28 . H281 . 111.3 no
O4 . C28 . H282 . 110.2 no
C29 . C28 . H282 . 110.3 no
H281 . C28 . H282 . 110.7 no
C28 . C29 . N4 . 112.6(2) yes
C28 . C29 . H291 . 107.7 no
N4 . C29 . H291 . 109.0 no
C28 . C29 . H292 . 108.7 no
N4 . C29 . H292 . 110.2 no
H291 . C29 . H292 . 108.6 no
N4 . C30 . C31 . 111.7(3) yes
N4 . C30 . H301 . 107.7 no
C31 . C30 . H301 . 108.2 no
N4 . C30 . H302 . 109.3 no
C31 . C30 . H302 . 109.5 no
H301 . C30 . H302 . 110.5 no
C30 . C31 . C32 . 111.1(3) yes
C30 . C31 . H311 . 111.0 no
C32 . C31 . H311 . 111.0 no
C30 . C31 . H312 . 108.6 no
C32 . C31 . H312 . 107.8 no
H311 . C31 . H312 . 107.2 no
C31 . C32 . C33 . 110.4(3) yes
C31 . C32 . H321 . 110.0 no
C33 . C32 . H321 . 107.8 no
C31 . C32 . H322 . 111.5 no
C33 . C32 . H322 . 108.6 no
H321 . C32 . H322 . 108.3 no
C32 . C33 . C34 . 111.0(4) yes
C32 . C33 . H331 . 108.7 no
C34 . C33 . H331 . 108.6 no
C32 . C33 . H332 . 108.9 no
C34 . C33 . H332 . 110.5 no
H331 . C33 . H332 . 109.1 no
C33 . C34 . N4 . 111.0(3) yes
C33 . C34 . H341 . 108.2 no
N4 . C34 . H341 . 108.1 no
C33 . C34 . H342 . 111.5 no
N4 . C34 . H342 . 110.3 no
H341 . C34 . H342 . 107.6 no
Cl2 . C35 . Cl1 . 109.98(16) yes
Cl2 . C35 . Cl3 . 109.79(15) yes
Cl1 . C35 . Cl3 . 110.00(16) yes
Cl2 . C35 . H351 . 107.5 no
Cl1 . C35 . H351 . 109.7 no
Cl3 . C35 . H351 . 109.8 no
O101 . C101 . C102 . 117.7(2) yes
O101 . C101 . C106 . 123.9(2) yes
C102 . C101 . C106 . 118.5(2) yes
C101 . C102 . C103 . 120.6(2) yes
C101 . C102 . H1021 . 118.6 no
C103 . C102 . H1021 . 120.8 no
C102 . C103 . O103 . 123.6(2) yes
C102 . C103 . C104 . 121.2(2) yes
O103 . C103 . C104 . 115.2(2) yes
C103 . C104 . C105 . 118.5(2) yes
C103 . C104 . H1041 . 120.6 no
C105 . C104 . H1041 . 120.8 no
C104 . C105 . C106 . 122.0(2) yes
C104 . C105 . H1051 . 120.0 no
C106 . C105 . H1051 . 117.9 no
C105 . C106 . C101 . 119.2(2) yes
C105 . C106 . C107 . 118.9(2) yes
C101 . C106 . C107 . 121.9(2) yes
C106 . C107 . N101 . 124.9(2) yes
C106 . C107 . H1071 . 117.4 no
N101 . C107 . H1071 . 117.7 no
N101 . C108 . C109 . 103.6(4) yes
N101 . C108 . C117 . 114.9(3) yes
C109 . C108 . C117 . 112.4(4) yes
N101 . C108 . H1081 . 108.6 no
C109 . C108 . H1081 . 108.6 no
C117 . C108 . H1081 . 108.5 no
N102 . C109 . C108 . 102.0(4) yes
N102 . C109 . C120 . 114.8(3) yes
C108 . C109 . C120 . 108.5(4) yes
N102 . C109 . H1091 . 110.4 no
C108 . C109 . H1091 . 110.4 no
C120 . C109 . H1091 . 110.4 no
N102 . C110 . C111 . 125.6(2) yes
N102 . C110 . H1101 . 117.4 no
C111 . C110 . H1101 . 117.0 no
C110 . C111 . C112 . 119.4(2) yes
C110 . C111 . C116 . 121.9(2) yes
C112 . C111 . C116 . 118.7(2) yes
C111 . C112 . C113 . 122.3(3) yes
C111 . C112 . H1121 . 118.4 no
C113 . C112 . H1121 . 119.3 no
C112 . C113 . C114 . 118.7(2) yes
C112 . C113 . H1131 . 122.1 no
C114 . C113 . H1131 . 119.2 no
C113 . C114 . O104 . 114.5(2) yes
C113 . C114 . C115 . 121.1(2) yes
O104 . C114 . C115 . 124.4(2) yes
C114 . C115 . C116 . 120.6(2) yes
C114 . C115 . H1151 . 120.8 no
C116 . C115 . H1151 . 118.6 no
C111 . C116 . C115 . 118.6(2) yes
C111 . C116 . O102 . 123.2(2) yes
C115 . C116 . O102 . 118.2(2) yes
C108 . C117 . C118 . 107.4(3) yes
C108 . C117 . H1171 . 109.9 no
C118 . C117 . H1171 . 110.0 no
C108 . C117 . H1172 . 110.0 no
C118 . C117 . H1172 . 110.1 no
H1171 . C117 . H1172 . 109.5 no
C117 . C118 . C119 . 112.0(5) yes
C117 . C118 . H1181 . 108.8 no
C119 . C118 . H1181 . 108.9 no
C117 . C118 . H1182 . 108.8 no
C119 . C118 . H1182 . 108.8 no
H1181 . C118 . H1182 . 109.5 no
C118 . C119 . C120 . 109.3(4) yes
C118 . C119 . H1191 . 109.5 no
C120 . C119 . H1191 . 109.5 no
C118 . C119 . H1192 . 109.5 no
C120 . C119 . H1192 . 109.5 no
H1191 . C119 . H1192 . 109.5 no
C119 . C120 . C109 . 108.1(3) yes
C119 . C120 . H1201 . 109.8 no
C109 . C120 . H1201 . 109.8 no
C119 . C120 . H1202 . 109.8 no
C109 . C120 . H1202 . 109.8 no
H1201 . C120 . H1202 . 109.5 no
O103 . C121 . C122 . 106.9(2) yes
O103 . C121 . H1211 . 110.9 no
C122 . C121 . H1211 . 110.6 no
O103 . C121 . H1212 . 109.7 no
C122 . C121 . H1212 . 109.7 no
H1211 . C121 . H1212 . 108.9 no
C121 . C122 . N103 . 115.1(2) yes
C121 . C122 . H1221 . 107.6 no
N103 . C122 . H1221 . 105.8 no
C121 . C122 . H1222 . 108.9 no
N103 . C122 . H1222 . 110.0 no
H1221 . C122 . H1222 . 109.3 no
N103 . C123 . C124 . 110.2(3) yes
N103 . C123 . H1231 . 109.2 no
C124 . C123 . H1231 . 110.2 no
N103 . C123 . H1232 . 108.3 no
C124 . C123 . H1232 . 107.8 no
H1231 . C123 . H1232 . 111.0 no
C123 . C124 . C125 . 111.3(3) yes
C123 . C124 . H1241 . 110.3 no
C125 . C124 . H1241 . 106.6 no
C123 . C124 . H1242 . 110.9 no
C125 . C124 . H1242 . 108.9 no
H1241 . C124 . H1242 . 108.9 no
C124 . C125 . C126 . 109.9(3) yes
C124 . C125 . H1251 . 110.4 no
C126 . C125 . H1251 . 111.0 no
C124 . C125 . H1252 . 108.3 no
C126 . C125 . H1252 . 108.4 no
H1251 . C125 . H1252 . 108.8 no
C125 . C126 . C127 . 109.8(3) yes
C125 . C126 . H1261 . 107.3 no
C127 . C126 . H1261 . 108.9 no
C125 . C126 . H1262 . 110.7 no
C127 . C126 . H1262 . 109.0 no
H1261 . C126 . H1262 . 110.9 no
C126 . C127 . N103 . 110.5(2) yes
C126 . C127 . H1271 . 110.7 no
N103 . C127 . H1271 . 108.2 no
C126 . C127 . H1272 . 107.9 no
N103 . C127 . H1272 . 110.9 no
H1271 . C127 . H1272 . 108.6 no
O104 . C128 . C129 . 105.1(2) yes
O104 . C128 . H1281 . 109.2 no
C129 . C128 . H1281 . 111.3 no
O104 . C128 . H1282 . 110.2 no
C129 . C128 . H1282 . 110.3 no
H1281 . C128 . H1282 . 110.7 no
C128 . C129 . N104 . 112.6(2) yes
C128 . C129 . H1291 . 107.7 no
N104 . C129 . H1291 . 109.0 no
C128 . C129 . H1292 . 108.7 no
N104 . C129 . H1292 . 110.2 no
H1291 . C129 . H1292 . 108.6 no
N104 . C130 . C131 . 111.7(3) yes
N104 . C130 . H1301 . 107.7 no
C131 . C130 . H1301 . 108.2 no
N104 . C130 . H1302 . 109.3 no
C131 . C130 . H1302 . 109.5 no
H1301 . C130 . H1302 . 110.5 no
C130 . C131 . C132 . 111.1(3) yes
C130 . C131 . H1311 . 111.0 no
C132 . C131 . H1311 . 111.0 no
C130 . C131 . H1312 . 108.6 no
C132 . C131 . H1312 . 107.8 no
H1311 . C131 . H1312 . 107.2 no
C131 . C132 . C133 . 110.4(3) yes
C131 . C132 . H1321 . 110.0 no
C133 . C132 . H1321 . 107.8 no
C131 . C132 . H1322 . 111.5 no
C133 . C132 . H1322 . 108.6 no
H1321 . C132 . H1322 . 108.3 no
C132 . C133 . C134 . 111.0(4) yes
C132 . C133 . H1331 . 108.7 no
C134 . C133 . H1331 . 108.6 no
C132 . C133 . H1332 . 108.9 no
C134 . C133 . H1332 . 110.5 no
H1331 . C133 . H1332 . 109.1 no
C133 . C134 . N104 . 111.0(3) yes
C133 . C134 . H1341 . 108.2 no
N104 . C134 . H1341 . 108.1 no
C133 . C134 . H1342 . 111.5 no
N104 . C134 . H1342 . 110.3 no
H1341 . C134 . H1342 . 107.6 no
Cl102 . C135 . Cl101 . 109.98(16) yes
Cl102 . C135 . Cl103 . 109.79(15) yes
Cl101 . C135 . Cl103 . 110.00(16) yes
Cl102 . C135 . H1351 . 107.5 no
Cl101 . C135 . H1351 . 109.7 no
Cl103 . C135 . H1351 . 109.8 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 -175.2(2) . . . . no
N1 Ni1 O1 C1 4.1(2) . . . . no
O1 Ni1 O2 C16 174.8(2) . . . . no
N2 Ni1 O2 C16 -4.9(2) . . . . no
O1 Ni1 N1 C7 -1.4(3) . . . . no
O1 Ni1 N1 C8 165.6(3) . . . . no
N2 Ni1 N1 C7 178.2(3) . . . . no
N2 Ni1 N1 C8 -14.7(3) . . . . no
O2 Ni1 N2 C9 163.4(3) . . . . no
O2 Ni1 N2 C10 2.6(3) . . . . no
N1 Ni1 N2 C9 -16.0(3) . . . . no
N1 Ni1 N2 C10 -176.8(3) . . . . no
O102 Ni101 N102 C110 -2.6(3) . . . . no
N101 Ni101 N102 C109 -17.6(3) . . . . no
N101 Ni101 N102 C110 176.8(3) . . . . no
N102 Ni101 O102 C116 4.9(2) . . . . no
O101 Ni101 N101 C107 1.4(3) . . . . no
O101 Ni101 N101 C108 165.8(3) . . . . no
N102 Ni101 N101 C107 -178.2(3) . . . . no
O102 Ni101 O101 C101 175.2(2) . . . . no
N101 Ni101 O101 C101 -4.1(2) . . . . no
O101 Ni101 O102 C116 -174.8(2) . . . . no
N102 Ni101 N101 C108 -13.8(3) . . . . no
O102 Ni101 N102 C109 163.1(2) . . . . no
Ni1 O1 C1 C6 -4.8(4) . . . . no
Ni1 O1 C1 C2 174.62(18) . . . . no
Ni1 O2 C16 C11 5.2(4) . . . . no
Ni1 O2 C16 C15 -174.04(18) . . . . no
C21 O3 C3 C4 -166.7(2) . . . . no
C3 O3 C21 C22 160.4(2) . . . . no
C21 O3 C3 C2 12.0(4) . . . . no
C28 O4 C14 C13 -173.5(2) . . . . no
C28 O4 C14 C15 7.2(4) . . . . no
C14 O4 C28 C29 173.4(2) . . . . no
Ni101 O101 C101 C102 -174.62(18) . . . . no
Ni101 O101 C101 C106 4.8(4) . . . . no
Ni101 O102 C116 C111 -5.2(4) . . . . no
Ni101 O102 C116 C115 174.04(18) . . . . no
C103 O103 C121 C122 -160.4(2) . . . . no
C121 O103 C103 C104 166.7(2) . . . . no
C121 O103 C103 C102 -12.0(4) . . . . no
C128 O104 C114 C115 -7.2(4) . . . . no
C114 O104 C128 C129 -173.4(2) . . . . no
C128 O104 C114 C113 173.5(2) . . . . no
Ni1 N1 C8 C17 163.0(3) . . . . no
C7 N1 C8 C9 -151.0(3) . . . . no
Ni1 N1 C7 C6 -0.6(4) . . . . no
C8 N1 C7 C6 -166.6(3) . . . . no
Ni1 N1 C8 C9 41.1(4) . . . . no
C7 N1 C8 C17 -29.1(5) . . . . no
Ni1 N2 C9 C8 41.4(4) . . . . no
Ni1 N2 C9 C20 161.1(3) . . . . no
C10 N2 C9 C8 -156.4(3) . . . . no
C10 N2 C9 C20 -36.8(5) . . . . no
Ni1 N2 C10 C11 -0.7(4) . . . . no
C9 N2 C10 C11 -159.9(3) . . . . no
C23 N3 C27 C26 -60.8(3) . . . . no
C27 N3 C22 C21 64.2(3) . . . . no
C22 N3 C23 C24 -169.8(3) . . . . no
C23 N3 C22 C21 -65.8(3) . . . . no
C22 N3 C27 C26 168.2(3) . . . . no
C27 N3 C23 C24 59.1(3) . . . . no
C34 N4 C29 C28 75.7(3) . . . . no
C30 N4 C29 C28 -161.9(3) . . . . no
C34 N4 C30 C31 -60.2(4) . . . . no
C29 N4 C34 C33 -178.2(3) . . . . no
C29 N4 C30 C31 175.9(3) . . . . no
C30 N4 C34 C33 59.8(4) . . . . no
Ni101 N101 C107 C106 0.6(4) . . . . no
C108 N101 C107 C106 -162.5(3) . . . . no
Ni101 N101 C108 C109 41.1(4) . . . . no
Ni101 N101 C108 C117 164.0(3) . . . . no
C107 N101 C108 C109 -153.4(3) . . . . no
C107 N101 C108 C117 -30.4(5) . . . . no
C110 N102 C109 C108 -149.9(3) . . . . no
C110 N102 C109 C120 -32.8(5) . . . . no
Ni101 N102 C109 C120 160.5(3) . . . . no
Ni101 N102 C109 C108 43.5(4) . . . . no
Ni101 N102 C110 C111 0.7(4) . . . . no
C109 N102 C110 C111 -163.8(3) . . . . no
C127 N103 C122 C121 -64.2(3) . . . . no
C122 N103 C127 C126 -168.2(3) . . . . no
C122 N103 C123 C124 169.8(3) . . . . no
C127 N103 C123 C124 -59.1(3) . . . . no
C123 N103 C122 C121 65.8(3) . . . . no
C123 N103 C127 C126 60.8(3) . . . . no
C129 N104 C134 C133 178.2(3) . . . . no
C130 N104 C129 C128 161.9(3) . . . . no
C134 N104 C129 C128 -75.7(3) . . . . no
C130 N104 C134 C133 -59.8(4) . . . . no
C134 N104 C130 C131 60.2(4) . . . . no
C129 N104 C130 C131 -175.9(3) . . . . no
O1 C1 C6 C7 1.8(4) . . . . no
O1 C1 C6 C5 179.6(2) . . . . no
O1 C1 C2 C3 179.4(2) . . . . no
C6 C1 C2 C3 -1.2(4) . . . . no
C2 C1 C6 C5 0.2(4) . . . . no
C2 C1 C6 C7 -177.6(3) . . . . no
C1 C2 C3 O3 -177.0(2) . . . . no
C1 C2 C3 C4 1.6(4) . . . . no
C2 C3 C4 C5 -1.0(4) . . . . no
O3 C3 C4 C5 177.8(2) . . . . no
C3 C4 C5 C6 0.0(4) . . . . no
C4 C5 C6 C1 0.4(4) . . . . no
C4 C5 C6 C7 178.2(3) . . . . no
C1 C6 C7 N1 1.0(4) . . . . no
C5 C6 C7 N1 -176.8(3) . . . . no
C17 C8 C9 C20 61.6(5) . . . . no
N1 C8 C9 N2 -50.5(4) . . . . no
N1 C8 C9 C20 -172.7(3) . . . . no
C17 C8 C9 N2 -176.2(3) . . . . no
C9 C8 C17 C18 -54.6(5) . . . . no
N1 C8 C17 C18 -173.0(4) . . . . no
N2 C9 C20 C19 -178.2(4) . . . . no
C8 C9 C20 C19 -62.8(5) . . . . no
N2 C10 C11 C16 -0.3(4) . . . . no
N2 C10 C11 C12 177.6(3) . . . . no
C10 C11 C12 C13 -177.3(3) . . . . no
C10 C11 C16 O2 -2.1(4) . . . . no
C10 C11 C16 C15 177.2(3) . . . . no
C16 C11 C12 C13 0.6(4) . . . . no
C12 C11 C16 C15 -0.7(4) . . . . no
C12 C11 C16 O2 -179.9(3) . . . . no
C11 C12 C13 C14 -0.1(5) . . . . no
C12 C13 C14 O4 -179.7(3) . . . . no
C12 C13 C14 C15 -0.4(4) . . . . no
C13 C14 C15 C16 0.3(4) . . . . no
O4 C14 C15 C16 179.5(3) . . . . no
C14 C15 C16 O2 179.5(2) . . . . no
C14 C15 C16 C11 0.2(4) . . . . no
C8 C17 C18 C19 51.8(5) . . . . no
C17 C18 C19 C20 -55.7(6) . . . . no
C18 C19 C20 C9 59.3(5) . . . . no
O3 C21 C22 N3 -165.8(2) . . . . no
N3 C23 C24 C25 -55.8(4) . . . . no
C23 C24 C25 C26 54.3(4) . . . . no
C24 C25 C26 C27 -54.9(4) . . . . no
C25 C26 C27 N3 58.1(3) . . . . no
O4 C28 C29 N4 171.8(2) . . . . no
N4 C30 C31 C32 56.7(4) . . . . no
C30 C31 C32 C33 -52.1(5) . . . . no
C31 C32 C33 C34 52.3(5) . . . . no
C32 C33 C34 N4 -56.5(5) . . . . no
O101 C101 C102 C103 -179.4(2) . . . . no
C106 C101 C102 C103 1.2(4) . . . . no
O101 C101 C106 C105 -179.6(2) . . . . no
O101 C101 C106 C107 -1.8(4) . . . . no
C102 C101 C106 C105 -0.2(4) . . . . no
C102 C101 C106 C107 177.6(3) . . . . no
C101 C102 C103 O103 177.0(2) . . . . no
C101 C102 C103 C104 -1.6(4) . . . . no
O103 C103 C104 C105 -177.8(2) . . . . no
C102 C103 C104 C105 1.0(4) . . . . no
C103 C104 C105 C106 0.0(4) . . . . no
C104 C105 C106 C101 -0.4(4) . . . . no
C104 C105 C106 C107 -178.2(3) . . . . no
C101 C106 C107 N101 -1.0(4) . . . . no
C105 C106 C107 N101 176.8(3) . . . . no
N101 C108 C109 N102 -51.2(4) . . . . no
N101 C108 C109 C120 -172.8(3) . . . . no
C117 C108 C109 N102 -175.8(3) . . . . no
C117 C108 C109 C120 62.7(5) . . . . no
N101 C108 C117 C118 -176.4(4) . . . . no
C109 C108 C117 C118 -58.3(5) . . . . no
N102 C109 C120 C119 -174.8(3) . . . . no
C108 C109 C120 C119 -61.5(4) . . . . no
N102 C110 C111 C112 -177.6(3) . . . . no
N102 C110 C111 C116 0.3(4) . . . . no
C110 C111 C112 C113 177.3(3) . . . . no
C116 C111 C112 C113 -0.6(4) . . . . no
C110 C111 C116 O102 2.1(4) . . . . no
C110 C111 C116 C115 -177.2(3) . . . . no
C112 C111 C116 O102 179.9(3) . . . . no
C112 C111 C116 C115 0.7(4) . . . . no
C111 C112 C113 C114 0.1(4) . . . . no
C112 C113 C114 O104 179.7(3) . . . . no
C112 C113 C114 C115 0.4(4) . . . . no
O104 C114 C115 C116 -179.5(3) . . . . no
C113 C114 C115 C116 -0.3(4) . . . . no
C114 C115 C116 O102 -179.5(2) . . . . no
C114 C115 C116 C111 -0.2(4) . . . . no
C108 C117 C118 C119 56.3(5) . . . . no
C117 C118 C119 C120 -58.8(6) . . . . no
C118 C119 C120 C109 60.2(5) . . . . no
O103 C121 C122 N103 165.8(2) . . . . no
N103 C123 C124 C125 55.8(4) . . . . no
C123 C124 C125 C126 -54.3(4) . . . . no
C124 C125 C126 C127 54.9(4) . . . . no
C125 C126 C127 N103 -58.1(3) . . . . no
O104 C128 C129 N104 -171.8(2) . . . . no
N104 C130 C131 C132 -56.7(4) . . . . no
C130 C131 C132 C133 52.1(5) . . . . no
C131 C132 C133 C134 -52.3(5) . . . . no
C132 C133 C134 N104 56.5(5) . . . . 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 Ni101 3.6919(6) . . no
Ni1 Cl1 3.9829(11) . . no
Ni1 N101 3.764(3) . . no
Ni1 N102 3.839(3) . . no
Ni1 C35 3.915(3) . . no
Ni1 C108 3.694(5) . . no
Ni101 C135 3.915(3) . . no
Ni101 Cl101 3.9829(11) . . no
Ni101 N1 3.764(3) . . no
Ni101 C9 3.681(5) . . no
Ni101 N2 3.839(3) . . no
Cl2 C2 3.607(3) . . no
Cl102 C18 3.632(6) . 1_455 no
Cl102 C102 3.607(3) . . no
Cl3 C132 3.598(5) . 1_444 no
Cl3 C15 3.633(3) . . no
Cl103 C115 3.633(3) . . no
Cl103 C32 3.598(5) . 1_666 no
O1 C35 3.139(3) . . no
O1 O2 2.469(3) . . no
O1 C7 2.897(3) . . no
O1 N1 2.725(3) . . no
O2 C10 2.891(3) . . no
O2 N2 2.727(3) . . no
O2 C35 3.156(3) . . no
O2 C108 3.297(6) . . no
O101 C135 3.139(3) . . no
O101 C9 3.215(6) . . no
O101 C107 2.897(3) . . no
O101 O102 2.469(3) . . no
O101 N101 2.725(3) . . no
O102 N102 2.727(3) . . no
O102 C135 3.156(3) . . no
O102 C110 2.891(3) . . no
N1 N2 2.534(4) . . no
N1 O1 2.725(3) . . no
N1 C1 2.919(3) . . no
N1 C9 2.357(6) . . no
N2 C16 2.927(3) . . no
N2 O2 2.727(3) . . no
N2 C8 2.364(6) . . no
N101 C109 2.384(5) . . no
N101 N102 2.534(4) . . no
N101 C101 2.919(3) . . no
N101 O101 2.725(3) . . no
N102 C108 2.357(6) . . no
N102 C116 2.927(3) . . no
C1 C110 3.572(4) . . no
C2 Cl2 3.607(3) . . no
C5 C112 3.325(4) . . no
C6 C111 3.520(4) . . no
C6 C110 3.469(4) . . no
C7 C111 3.504(4) . . no
C7 C116 3.569(4) . . no
C9 C101 3.585(6) . . no
C10 C106 3.469(4) . . no
C10 C101 3.572(4) . . no
C11 C106 3.520(4) . . no
C11 C107 3.504(4) . . no
C12 C105 3.325(4) . . no
C16 C107 3.569(4) . . no
C132 Cl3 3.598(5) . 1_666 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
C9 . H91 . O101 . 153 0.950 2.34 3.214(5) yes
C35 . H351 . O1 . 145 0.961 2.30 3.139(5) yes
C35 . H351 . O2 . 139 0.961 2.36 3.156(5) yes
C108 . H1081 . O2 . 145 0.950 2.47 3.297(5) yes
C135 . H1351 . O101 . 145 0.961 2.30 3.139(5) yes
C135 . H1351 . O102 . 139 0.961 2.36 3.156(5) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 21/07/15 at 17:15:06
#
#LIST     12                                                                    
BLOCK SCALE  NI(1,X'S,U'S) UNTIL C(135) 
EQUIV  NI(1,X) NI(101,X) 
WEIGHT -1 NI(101,X) 
EQUIV  NI(1,Y) NI(101,Y) 
WEIGHT -1 NI(101,Y) 
EQUIV  NI(1,Z) NI(101,Z) 
WEIGHT -1 NI(101,Z) 
EQUIV  NI(1,U[11]) NI(101,U[11]) 
EQUIV  NI(1,U[22]) NI(101,U[22]) 
EQUIV  NI(1,U[33]) NI(101,U[33]) 
EQUIV  NI(1,U[12]) NI(101,U[12]) 
EQUIV  NI(1,U[13]) NI(101,U[13]) 
EQUIV  NI(1,U[23]) NI(101,U[23]) 
EQUIV  CL(1,X) CL(101,X) 
WEIGHT -1 CL(101,X) 
EQUIV  CL(1,Y) CL(101,Y) 
WEIGHT -1 CL(101,Y) 
EQUIV  CL(1,Z) CL(101,Z) 
WEIGHT -1 CL(101,Z) 
EQUIV  CL(1,U[11]) CL(101,U[11]) 
EQUIV  CL(1,U[22]) CL(101,U[22]) 
EQUIV  CL(1,U[33]) CL(101,U[33]) 
EQUIV  CL(1,U[12]) CL(101,U[12]) 
EQUIV  CL(1,U[13]) CL(101,U[13]) 
EQUIV  CL(1,U[23]) CL(101,U[23]) 
EQUIV  CL(2,X) CL(102,X) 
WEIGHT -1 CL(102,X) 
EQUIV  CL(2,Y) CL(102,Y) 
WEIGHT -1 CL(102,Y) 
EQUIV  CL(2,Z) CL(102,Z) 
WEIGHT -1 CL(102,Z) 
EQUIV  CL(2,U[11]) CL(102,U[11]) 
EQUIV  CL(2,U[22]) CL(102,U[22]) 
EQUIV  CL(2,U[33]) CL(102,U[33]) 
EQUIV  CL(2,U[12]) CL(102,U[12]) 
EQUIV  CL(2,U[13]) CL(102,U[13]) 
EQUIV  CL(2,U[23]) CL(102,U[23]) 
EQUIV  CL(3,X) CL(103,X) 
WEIGHT -1 CL(103,X) 
EQUIV  CL(3,Y) CL(103,Y) 
WEIGHT -1 CL(103,Y) 
EQUIV  CL(3,Z) CL(103,Z) 
WEIGHT -1 CL(103,Z) 
EQUIV  CL(3,U[11]) CL(103,U[11]) 
EQUIV  CL(3,U[22]) CL(103,U[22]) 
EQUIV  CL(3,U[33]) CL(103,U[33]) 
EQUIV  CL(3,U[12]) CL(103,U[12]) 
EQUIV  CL(3,U[13]) CL(103,U[13]) 
EQUIV  CL(3,U[23]) CL(103,U[23]) 
EQUIV  O(1,X) O(101,X) 
WEIGHT -1 O(101,X) 
EQUIV  O(1,Y) O(101,Y) 
WEIGHT -1 O(101,Y) 
EQUIV  O(1,Z) O(101,Z) 
WEIGHT -1 O(101,Z) 
EQUIV  O(1,U[11]) O(101,U[11]) 
EQUIV  O(1,U[22]) O(101,U[22]) 
EQUIV  O(1,U[33]) O(101,U[33]) 
EQUIV  O(1,U[12]) O(101,U[12]) 
EQUIV  O(1,U[13]) O(101,U[13]) 
EQUIV  O(1,U[23]) O(101,U[23]) 
EQUIV  O(2,X) O(102,X) 
WEIGHT -1 O(102,X) 
EQUIV  O(2,Y) O(102,Y) 
WEIGHT -1 O(102,Y) 
EQUIV  O(2,Z) O(102,Z) 
WEIGHT -1 O(102,Z) 
EQUIV  O(2,U[11]) O(102,U[11]) 
EQUIV  O(2,U[22]) O(102,U[22]) 
EQUIV  O(2,U[33]) O(102,U[33]) 
EQUIV  O(2,U[12]) O(102,U[12]) 
EQUIV  O(2,U[13]) O(102,U[13]) 
EQUIV  O(2,U[23]) O(102,U[23]) 
EQUIV  O(3,X) O(103,X) 
WEIGHT -1 O(103,X) 
EQUIV  O(3,Y) O(103,Y) 
WEIGHT -1 O(103,Y) 
EQUIV  O(3,Z) O(103,Z) 
WEIGHT -1 O(103,Z) 
EQUIV  O(3,U[11]) O(103,U[11]) 
EQUIV  O(3,U[22]) O(103,U[22]) 
EQUIV  O(3,U[33]) O(103,U[33]) 
EQUIV  O(3,U[12]) O(103,U[12]) 
EQUIV  O(3,U[13]) O(103,U[13]) 
EQUIV  O(3,U[23]) O(103,U[23]) 
EQUIV  O(4,X) O(104,X) 
WEIGHT -1 O(104,X) 
EQUIV  O(4,Y) O(104,Y) 
WEIGHT -1 O(104,Y) 
EQUIV  O(4,Z) O(104,Z) 
WEIGHT -1 O(104,Z) 
EQUIV  O(4,U[11]) O(104,U[11]) 
EQUIV  O(4,U[22]) O(104,U[22]) 
EQUIV  O(4,U[33]) O(104,U[33]) 
EQUIV  O(4,U[12]) O(104,U[12]) 
EQUIV  O(4,U[13]) O(104,U[13]) 
EQUIV  O(4,U[23]) O(104,U[23]) 
EQUIV  N(1,X) N(101,X) 
WEIGHT -1 N(101,X) 
EQUIV  N(1,Y) N(101,Y) 
WEIGHT -1 N(101,Y) 
EQUIV  N(1,Z) N(101,Z) 
WEIGHT -1 N(101,Z) 
EQUIV  N(1,U[11]) N(101,U[11]) 
EQUIV  N(1,U[22]) N(101,U[22]) 
EQUIV  N(1,U[33]) N(101,U[33]) 
EQUIV  N(1,U[12]) N(101,U[12]) 
EQUIV  N(1,U[13]) N(101,U[13]) 
EQUIV  N(1,U[23]) N(101,U[23]) 
EQUIV  N(2,X) N(102,X) 
WEIGHT -1 N(102,X) 
EQUIV  N(2,Y) N(102,Y) 
WEIGHT -1 N(102,Y) 
EQUIV  N(2,Z) N(102,Z) 
WEIGHT -1 N(102,Z) 
EQUIV  N(2,U[11]) N(102,U[11]) 
EQUIV  N(2,U[22]) N(102,U[22]) 
EQUIV  N(2,U[33]) N(102,U[33]) 
EQUIV  N(2,U[12]) N(102,U[12]) 
EQUIV  N(2,U[13]) N(102,U[13]) 
EQUIV  N(2,U[23]) N(102,U[23]) 
EQUIV  N(3,X) N(103,X) 
WEIGHT -1 N(103,X) 
EQUIV  N(3,Y) N(103,Y) 
WEIGHT -1 N(103,Y) 
EQUIV  N(3,Z) N(103,Z) 
WEIGHT -1 N(103,Z) 
EQUIV  N(3,U[11]) N(103,U[11]) 
EQUIV  N(3,U[22]) N(103,U[22]) 
EQUIV  N(3,U[33]) N(103,U[33]) 
EQUIV  N(3,U[12]) N(103,U[12]) 
EQUIV  N(3,U[13]) N(103,U[13]) 
EQUIV  N(3,U[23]) N(103,U[23]) 
EQUIV  N(4,X) N(104,X) 
WEIGHT -1 N(104,X) 
EQUIV  N(4,Y) N(104,Y) 
WEIGHT -1 N(104,Y) 
EQUIV  N(4,Z) N(104,Z) 
WEIGHT -1 N(104,Z) 
EQUIV  N(4,U[11]) N(104,U[11]) 
EQUIV  N(4,U[22]) N(104,U[22]) 
EQUIV  N(4,U[33]) N(104,U[33]) 
EQUIV  N(4,U[12]) N(104,U[12]) 
EQUIV  N(4,U[13]) N(104,U[13]) 
EQUIV  N(4,U[23]) N(104,U[23]) 
EQUIV  C(1,X) C(101,X) 
WEIGHT -1 C(101,X) 
EQUIV  C(1,Y) C(101,Y) 
WEIGHT -1 C(101,Y) 
EQUIV  C(1,Z) C(101,Z) 
WEIGHT -1 C(101,Z) 
EQUIV  C(1,U[11]) C(101,U[11]) 
EQUIV  C(1,U[22]) C(101,U[22]) 
EQUIV  C(1,U[33]) C(101,U[33]) 
EQUIV  C(1,U[12]) C(101,U[12]) 
EQUIV  C(1,U[13]) C(101,U[13]) 
EQUIV  C(1,U[23]) C(101,U[23]) 
EQUIV  C(2,U[11]) C(102,U[11]) 
EQUIV  C(2,U[22]) C(102,U[22]) 
EQUIV  C(2,U[33]) C(102,U[33]) 
EQUIV  C(2,U[12]) C(102,U[12]) 
EQUIV  C(2,U[13]) C(102,U[13]) 
EQUIV  C(2,U[23]) C(102,U[23]) 
EQUIV  C(3,X) C(103,X) 
WEIGHT -1 C(103,X) 
EQUIV  C(3,Y) C(103,Y) 
WEIGHT -1 C(103,Y) 
EQUIV  C(3,Z) C(103,Z) 
WEIGHT -1 C(103,Z) 
EQUIV  C(3,U[11]) C(103,U[11]) 
EQUIV  C(3,U[22]) C(103,U[22]) 
EQUIV  C(3,U[33]) C(103,U[33]) 
EQUIV  C(3,U[12]) C(103,U[12]) 
EQUIV  C(3,U[13]) C(103,U[13]) 
EQUIV  C(3,U[23]) C(103,U[23]) 
EQUIV  C(4,U[11]) C(104,U[11]) 
EQUIV  C(4,U[22]) C(104,U[22]) 
EQUIV  C(4,U[33]) C(104,U[33]) 
EQUIV  C(4,U[12]) C(104,U[12]) 
EQUIV  C(4,U[13]) C(104,U[13]) 
EQUIV  C(4,U[23]) C(104,U[23]) 
EQUIV  C(5,U[11]) C(105,U[11]) 
EQUIV  C(5,U[22]) C(105,U[22]) 
EQUIV  C(5,U[33]) C(105,U[33]) 
EQUIV  C(5,U[12]) C(105,U[12]) 
EQUIV  C(5,U[13]) C(105,U[13]) 
EQUIV  C(5,U[23]) C(105,U[23]) 
EQUIV  C(6,X) C(106,X) 
WEIGHT -1 C(106,X) 
EQUIV  C(6,Y) C(106,Y) 
WEIGHT -1 C(106,Y) 
EQUIV  C(6,Z) C(106,Z) 
WEIGHT -1 C(106,Z) 
EQUIV  C(6,U[11]) C(106,U[11]) 
EQUIV  C(6,U[22]) C(106,U[22]) 
EQUIV  C(6,U[33]) C(106,U[33]) 
EQUIV  C(6,U[12]) C(106,U[12]) 
EQUIV  C(6,U[13]) C(106,U[13]) 
EQUIV  C(6,U[23]) C(106,U[23]) 
EQUIV  C(7,U[11]) C(107,U[11]) 
EQUIV  C(7,U[22]) C(107,U[22]) 
EQUIV  C(7,U[33]) C(107,U[33]) 
EQUIV  C(7,U[12]) C(107,U[12]) 
EQUIV  C(7,U[13]) C(107,U[13]) 
EQUIV  C(7,U[23]) C(107,U[23]) 
EQUIV  C(10,U[11]) C(110,U[11]) 
EQUIV  C(10,U[22]) C(110,U[22]) 
EQUIV  C(10,U[33]) C(110,U[33]) 
EQUIV  C(10,U[12]) C(110,U[12]) 
EQUIV  C(10,U[13]) C(110,U[13]) 
EQUIV  C(10,U[23]) C(110,U[23]) 
EQUIV  C(11,X) C(111,X) 
WEIGHT -1 C(111,X) 
EQUIV  C(11,Y) C(111,Y) 
WEIGHT -1 C(111,Y) 
EQUIV  C(11,Z) C(111,Z) 
WEIGHT -1 C(111,Z) 
EQUIV  C(11,U[11]) C(111,U[11]) 
EQUIV  C(11,U[22]) C(111,U[22]) 
EQUIV  C(11,U[33]) C(111,U[33]) 
EQUIV  C(11,U[12]) C(111,U[12]) 
EQUIV  C(11,U[13]) C(111,U[13]) 
EQUIV  C(11,U[23]) C(111,U[23]) 
EQUIV  C(12,U[11]) C(112,U[11]) 
EQUIV  C(12,U[22]) C(112,U[22]) 
EQUIV  C(12,U[33]) C(112,U[33]) 
EQUIV  C(12,U[12]) C(112,U[12]) 
EQUIV  C(12,U[13]) C(112,U[13]) 
EQUIV  C(12,U[23]) C(112,U[23]) 
EQUIV  C(13,U[11]) C(113,U[11]) 
EQUIV  C(13,U[22]) C(113,U[22]) 
EQUIV  C(13,U[33]) C(113,U[33]) 
EQUIV  C(13,U[12]) C(113,U[12]) 
EQUIV  C(13,U[13]) C(113,U[13]) 
EQUIV  C(13,U[23]) C(113,U[23]) 
EQUIV  C(14,X) C(114,X) 
WEIGHT -1 C(114,X) 
EQUIV  C(14,Y) C(114,Y) 
WEIGHT -1 C(114,Y) 
EQUIV  C(14,Z) C(114,Z) 
WEIGHT -1 C(114,Z) 
EQUIV  C(14,U[11]) C(114,U[11]) 
EQUIV  C(14,U[22]) C(114,U[22]) 
EQUIV  C(14,U[33]) C(114,U[33]) 
EQUIV  C(14,U[12]) C(114,U[12]) 
EQUIV  C(14,U[13]) C(114,U[13]) 
EQUIV  C(14,U[23]) C(114,U[23]) 
EQUIV  C(15,U[11]) C(115,U[11]) 
EQUIV  C(15,U[22]) C(115,U[22]) 
EQUIV  C(15,U[33]) C(115,U[33]) 
EQUIV  C(15,U[12]) C(115,U[12]) 
EQUIV  C(15,U[13]) C(115,U[13]) 
EQUIV  C(15,U[23]) C(115,U[23]) 
EQUIV  C(16,X) C(116,X) 
WEIGHT -1 C(116,X) 
EQUIV  C(16,Y) C(116,Y) 
WEIGHT -1 C(116,Y) 
EQUIV  C(16,Z) C(116,Z) 
WEIGHT -1 C(116,Z) 
EQUIV  C(16,U[11]) C(116,U[11]) 
EQUIV  C(16,U[22]) C(116,U[22]) 
EQUIV  C(16,U[33]) C(116,U[33]) 
EQUIV  C(16,U[12]) C(116,U[12]) 
EQUIV  C(16,U[13]) C(116,U[13]) 
EQUIV  C(16,U[23]) C(116,U[23]) 
EQUIV  C(17,U[11]) C(117,U[11]) 
EQUIV  C(17,U[22]) C(117,U[22]) 
EQUIV  C(17,U[33]) C(117,U[33]) 
EQUIV  C(17,U[12]) C(117,U[12]) 
EQUIV  C(17,U[13]) C(117,U[13]) 
EQUIV  C(17,U[23]) C(117,U[23]) 
EQUIV  C(20,U[11]) C(120,U[11]) 
EQUIV  C(20,U[22]) C(120,U[22]) 
EQUIV  C(20,U[33]) C(120,U[33]) 
EQUIV  C(20,U[12]) C(120,U[12]) 
EQUIV  C(20,U[13]) C(120,U[13]) 
EQUIV  C(20,U[23]) C(120,U[23]) 
EQUIV  C(21,U[11]) C(121,U[11]) 
EQUIV  C(21,U[22]) C(121,U[22]) 
EQUIV  C(21,U[33]) C(121,U[33]) 
EQUIV  C(21,U[12]) C(121,U[12]) 
EQUIV  C(21,U[13]) C(121,U[13]) 
EQUIV  C(21,U[23]) C(121,U[23]) 
EQUIV  C(22,U[11]) C(122,U[11]) 
EQUIV  C(22,U[22]) C(122,U[22]) 
EQUIV  C(22,U[33]) C(122,U[33]) 
EQUIV  C(22,U[12]) C(122,U[12]) 
EQUIV  C(22,U[13]) C(122,U[13]) 
EQUIV  C(22,U[23]) C(122,U[23]) 
EQUIV  C(23,U[11]) C(123,U[11]) 
EQUIV  C(23,U[22]) C(123,U[22]) 
EQUIV  C(23,U[33]) C(123,U[33]) 
EQUIV  C(23,U[12]) C(123,U[12]) 
EQUIV  C(23,U[13]) C(123,U[13]) 
EQUIV  C(23,U[23]) C(123,U[23]) 
EQUIV  C(24,U[11]) C(124,U[11]) 
EQUIV  C(24,U[22]) C(124,U[22]) 
EQUIV  C(24,U[33]) C(124,U[33]) 
EQUIV  C(24,U[12]) C(124,U[12]) 
EQUIV  C(24,U[13]) C(124,U[13]) 
EQUIV  C(24,U[23]) C(124,U[23]) 
EQUIV  C(25,U[11]) C(125,U[11]) 
EQUIV  C(25,U[22]) C(125,U[22]) 
EQUIV  C(25,U[33]) C(125,U[33]) 
EQUIV  C(25,U[12]) C(125,U[12]) 
EQUIV  C(25,U[13]) C(125,U[13]) 
EQUIV  C(25,U[23]) C(125,U[23]) 
EQUIV  C(26,U[11]) C(126,U[11]) 
EQUIV  C(26,U[22]) C(126,U[22]) 
EQUIV  C(26,U[33]) C(126,U[33]) 
EQUIV  C(26,U[12]) C(126,U[12]) 
EQUIV  C(26,U[13]) C(126,U[13]) 
EQUIV  C(26,U[23]) C(126,U[23]) 
EQUIV  C(27,U[11]) C(127,U[11]) 
EQUIV  C(27,U[22]) C(127,U[22]) 
EQUIV  C(27,U[33]) C(127,U[33]) 
EQUIV  C(27,U[12]) C(127,U[12]) 
EQUIV  C(27,U[13]) C(127,U[13]) 
EQUIV  C(27,U[23]) C(127,U[23]) 
EQUIV  C(28,U[11]) C(128,U[11]) 
EQUIV  C(28,U[22]) C(128,U[22]) 
EQUIV  C(28,U[33]) C(128,U[33]) 
EQUIV  C(28,U[12]) C(128,U[12]) 
EQUIV  C(28,U[13]) C(128,U[13]) 
EQUIV  C(28,U[23]) C(128,U[23]) 
EQUIV  C(29,U[11]) C(129,U[11]) 
EQUIV  C(29,U[22]) C(129,U[22]) 
EQUIV  C(29,U[33]) C(129,U[33]) 
EQUIV  C(29,U[12]) C(129,U[12]) 
EQUIV  C(29,U[13]) C(129,U[13]) 
EQUIV  C(29,U[23]) C(129,U[23]) 
EQUIV  C(30,U[11]) C(130,U[11]) 
EQUIV  C(30,U[22]) C(130,U[22]) 
EQUIV  C(30,U[33]) C(130,U[33]) 
EQUIV  C(30,U[12]) C(130,U[12]) 
EQUIV  C(30,U[13]) C(130,U[13]) 
EQUIV  C(30,U[23]) C(130,U[23]) 
EQUIV  C(31,U[11]) C(131,U[11]) 
EQUIV  C(31,U[22]) C(131,U[22]) 
EQUIV  C(31,U[33]) C(131,U[33]) 
EQUIV  C(31,U[12]) C(131,U[12]) 
EQUIV  C(31,U[13]) C(131,U[13]) 
EQUIV  C(31,U[23]) C(131,U[23]) 
EQUIV  C(32,U[11]) C(132,U[11]) 
EQUIV  C(32,U[22]) C(132,U[22]) 
EQUIV  C(32,U[33]) C(132,U[33]) 
EQUIV  C(32,U[12]) C(132,U[12]) 
EQUIV  C(32,U[13]) C(132,U[13]) 
EQUIV  C(32,U[23]) C(132,U[23]) 
EQUIV  C(33,U[11]) C(133,U[11]) 
EQUIV  C(33,U[22]) C(133,U[22]) 
EQUIV  C(33,U[33]) C(133,U[33]) 
EQUIV  C(33,U[12]) C(133,U[12]) 
EQUIV  C(33,U[13]) C(133,U[13]) 
EQUIV  C(33,U[23]) C(133,U[23]) 
EQUIV  C(34,U[11]) C(134,U[11]) 
EQUIV  C(34,U[22]) C(134,U[22]) 
EQUIV  C(34,U[33]) C(134,U[33]) 
EQUIV  C(34,U[12]) C(134,U[12]) 
EQUIV  C(34,U[13]) C(134,U[13]) 
EQUIV  C(34,U[23]) C(134,U[23]) 
EQUIV  C(35,U[11]) C(135,U[11]) 
EQUIV  C(35,U[22]) C(135,U[22]) 
EQUIV  C(35,U[33]) C(135,U[33]) 
EQUIV  C(35,U[12]) C(135,U[12]) 
EQUIV  C(35,U[13]) C(135,U[13]) 
EQUIV  C(35,U[23]) C(135,U[23]) 
RIDE C   (   2,X'S) H   (  21,X'S) C(102,X'S) H(1021,X'S) 
WEIGHT -1 C(102,X'S) H(1021,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) C(104,X'S) H(1041,X'S) 
WEIGHT -1  C(104,X'S) H(1041,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) C(105,X'S) H(1051,X'S) 
WEIGHT -1  C(105,X'S) H(1051,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) C(107,X'S) H(1071,X'S) 
WEIGHT -1  C(107,X'S) H(1071,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) C(110,X'S) H(1101,X'S) 
WEIGHT -1  C(110,X'S) H(1101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) C(112,X'S) H(1121,X'S) 
WEIGHT -1  C(112,X'S) H(1121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) C(113,X'S) H(1131,X'S) 
WEIGHT -1  C(113,X'S) H(1131,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) C(115,X'S) H(1151,X'S) 
WEIGHT -1  C(115,X'S) H(1151,X'S) 
RIDE C(  21,X'S) H   ( 211,X'S) H( 212,X'S) C(121,X'S) H(1211,X'S) H(1212,X'S) 
WEIGHT -1  C(121,X'S) H(1211,X'S) H(1212,X'S) 
RIDE C(  22,X'S) H   ( 221,X'S) H( 222,X'S) C(122,X'S) H(1221,X'S) H(1222,X'S) 
WEIGHT -1  C(122,X'S) H(1221,X'S) H(1222,X'S) 
RIDE C(  23,X'S) H   ( 231,X'S) H( 232,X'S) C(123,X'S) H(1231,X'S) H(1232,X'S) 
WEIGHT -1  C(123,X'S) H(1231,X'S) H(1232,X'S) 
RIDE C(  24,X'S) H   ( 241,X'S) H( 242,X'S) C(124,X'S) H(1241,X'S) H(1242,X'S) 
WEIGHT -1  C(124,X'S) H(1241,X'S) H(1242,X'S) 
RIDE C(  25,X'S) H   ( 251,X'S) H( 252,X'S) C(125,X'S) H(1251,X'S) H(1252,X'S) 
WEIGHT -1  C(125,X'S) H(1251,X'S) H(1252,X'S) 
RIDE C(  26,X'S) H   ( 261,X'S) H( 262,X'S) C(126,X'S) H(1261,X'S) H(1262,X'S) 
WEIGHT -1  C(126,X'S) H(1261,X'S) H(1262,X'S) 
RIDE C(  27,X'S) H   ( 271,X'S) H( 272,X'S) C(127,X'S) H(1271,X'S) H(1272,X'S) 
WEIGHT -1  C(127,X'S) H(1271,X'S) H(1272,X'S) 
RIDE C(  28,X'S) H   ( 281,X'S) H( 282,X'S) C(128,X'S) H(1281,X'S) H(1282,X'S) 
WEIGHT -1  C(128,X'S) H(1281,X'S) H(1282,X'S) 
RIDE C(  29,X'S) H   ( 291,X'S) H( 292,X'S) C(129,X'S) H(1291,X'S) H(1292,X'S) 
WEIGHT -1  C(129,X'S) H(1291,X'S) H(1292,X'S) 
RIDE C(  30,X'S) H   ( 301,X'S) H( 302,X'S) C(130,X'S) H(1301,X'S) H(1302,X'S) 
WEIGHT -1  C(130,X'S) H(1301,X'S) H(1302,X'S) 
RIDE C(  31,X'S) H   ( 311,X'S) H( 312,X'S) C(131,X'S) H(1311,X'S) H(1312,X'S) 
WEIGHT -1  C(131,X'S) H(1311,X'S) H(1312,X'S) 
RIDE C(  32,X'S) H   ( 321,X'S) H( 322,X'S) C(132,X'S) H(1321,X'S) H(1322,X'S) 
WEIGHT -1  C(132,X'S) H(1321,X'S) H(1322,X'S) 
RIDE C(  33,X'S) H   ( 331,X'S) H( 332,X'S) C(133,X'S) H(1331,X'S) H(1332,X'S) 
WEIGHT -1  C(133,X'S) H(1331,X'S) H(1332,X'S) 
RIDE C(  34,X'S) H   ( 341,X'S) H( 342,X'S) C(134,X'S) H(1341,X'S) H(1342,X'S) 
WEIGHT -1  C(134,X'S) H(1341,X'S) H(1342,X'S) 
RIDE C(  35,X'S) H   ( 351,X'S) C(135,X'S) H(1351,X'S) 
WEIGHT -1  C(135,X'S) H(1351,X'S) 
RIDE C(8,X'S) H(81,X'S) 
RIDE C(9,X'S) H(91,X'S) 
RIDE C(17,X'S) H(171,X'S) H(172,X'S) C(117,X'S) H(1171,X'S) H(1172,X'S) 
WEIGHT -1  C(117,X'S) H(1171,X'S) H(1172,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) C(120,X'S) H(1201,X'S) H(1202,X'S) 
WEIGHT -1  C(120,X'S) H(1201,X'S) H(1202,X'S) 
RIDE C(108,X'S) H(1081,X'S) 
RIDE C(109,X'S) H(1091,X'S) 
RIDE C(118,X'S) H(1181,X'S) H(1182,X'S) 
RIDE C(119,X'S) H(1191,X'S) H(1192,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 21/07/15 at 17:15:06
#
#LIST     16                                                                    
ORIGIN  .0001 X 
ORIGIN  .0001 Y 
ORIGIN  .0001 Z 
NO 
END                                                                             
;

# start Validation Reply Form 
_vrf_PLAT111_ral1502SN           
; 
PROBLEM: ADDSYM Detects New (Pseudo)Centre of Symmetry.   
RESPONSE: This is an enantiomerically pure compound which is in a 
pseudo-centrosymmetric structure.  Details are given in _refine_special_details
of the cif. 
;
_vrf_PLAT113_ral1502SN           
; 
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space group.   P-1 Check  
RESPONSE: This is an enantiomerically pure compound which is in a 
pseudo-centrosymmetric structure.  Details are given in _refine_special_details
of the cif. 
;
# end Validation Reply Form





#===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_ral1404SN
_database_code_depnum_ccdc_archive 'CCDC 1838240'
_audit_update_record             
;
2018-04-19 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_audit_creation_date             14-09-08
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1404SN\Tony_ral1404SN_data At 12: 7 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   15.2582(2)
_cell_length_b                   5.6873(1)
_cell_length_c                   26.0174(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.6233(12)
_cell_angle_gamma                90
_cell_volume                     2203.16(6)

_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 = C26 H22 N2 Ni1 O3 S1 
# Dc =      1.51 Fooo =   1072.00 Mu =     24.22 M =    501.25
# Found Formula = C26 H22 N2 Ni1 O4 S1 
# Dc =      1.56 FOOO =   1072.00 Mu =     24.77 M =    517.25

_chemical_formula_sum            'C26 H22 N2 Ni O4 S'
_chemical_formula_moiety         'C24 H16 N2 Ni O3, C2 H6 O S'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         517.25


_cell_measurement_reflns_used    11739
_cell_measurement_theta_min      3
_cell_measurement_theta_max      72
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.035
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_max          0.283

_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    2.477

# Sheldrick geometric approximatio 0.67 0.92 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.92
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2' ####
_diffrn_radiation_source         
'Supernova (Cu) X-ray Source' ################
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_cell_refinement       
;
CrysAlisPro

;
_computing_data_reduction        
;
CrysAlisPro

;
_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            25587
_reflns_number_total             4294
_diffrn_reflns_av_R_equivalents  0.033
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 4294 
# Theoretical number of reflections is about 8650 


_diffrn_reflns_theta_min         3.095
_diffrn_reflns_theta_max         71.906
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        71.906
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -18
_reflns_limit_h_max              18
_reflns_limit_k_min              0
_reflns_limit_k_max              7
_reflns_limit_l_min              0
_reflns_limit_l_max              32

_oxford_diffrn_Wilson_B_factor   2.37
_oxford_diffrn_Wilson_scale      0.16

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

_refine_diff_density_min         -0.37
_refine_diff_density_max         0.47


# 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         4294
_refine_ls_number_restraints     0
_refine_ls_number_parameters     373
_oxford_refine_ls_R_factor_ref   0.0344
_refine_ls_wR_factor_ref         0.0889
_refine_ls_goodness_of_fit_ref   1.0042
_refine_ls_shift/su_max          0.0026742
_refine_ls_shift/su_mean         0.0002662


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4294
_refine_ls_R_factor_all          0.0344
_refine_ls_wR_factor_all         0.0889

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4044
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_gt          0.0871

# 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    refxyz #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 1.60P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
The largest features in the
final difference electron density map are located 
near the Ni atom and
midway between bonded atoms.
;

# 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 0.359802(17) 0.21408(5) 0.657325(11) 0.0213 1.0000 Uani . . . . . .
S1 S 0.12414(3) 0.04936(8) 0.490293(19) 0.0333 1.0000 Uani . . . . . .
O1 O 0.23670(8) 0.2111(2) 0.63314(5) 0.0265 1.0000 Uani . . . . . .
O2 O 0.35697(8) -0.0517(2) 0.61648(5) 0.0256 1.0000 Uani . . . . . .
O3 O -0.06313(8) 0.4851(3) 0.59587(5) 0.0296 1.0000 Uani . . . . . .
O4 O 0.10059(10) -0.0525(3) 0.43558(6) 0.0417 1.0000 Uani . . . . . .
N1 N 0.36199(9) 0.4858(3) 0.69712(5) 0.0218 1.0000 Uani . . . . . .
N2 N 0.48344(9) 0.2099(3) 0.68048(5) 0.0225 1.0000 Uani . . . . . .
C1 C 0.17905(11) 0.3713(3) 0.64024(6) 0.0222 1.0000 Uani . . . . . .
C2 C 0.08772(11) 0.3398(3) 0.61582(7) 0.0238 1.0000 Uani . . . . . .
C3 C 0.02437(11) 0.5089(3) 0.61993(6) 0.0238 1.0000 Uani . . . . . .
C4 C 0.04837(12) 0.7154(3) 0.64952(7) 0.0255 1.0000 Uani . . . . . .
C5 C 0.13588(12) 0.7462(3) 0.67463(7) 0.0247 1.0000 Uani . . . . . .
C6 C 0.20355(11) 0.5773(3) 0.67117(6) 0.0224 1.0000 Uani . . . . . .
C7 C 0.29291(11) 0.6227(3) 0.69774(6) 0.0230 1.0000 Uani . . . . . .
C8 C 0.44945(11) 0.5474(3) 0.72528(6) 0.0230 1.0000 Uani . . . . . .
C9 C 0.51642(11) 0.3947(3) 0.71631(6) 0.0242 1.0000 Uani . . . . . .
C10 C 0.53916(11) 0.0643(3) 0.66514(7) 0.0246 1.0000 Uani . . . . . .
C11 C 0.51558(11) -0.1259(3) 0.62993(6) 0.0238 1.0000 Uani . . . . . .
C12 C 0.58524(12) -0.2785(3) 0.61800(7) 0.0253 1.0000 Uani . . . . . .
C13 C 0.67813(13) -0.2400(4) 0.63765(8) 0.0323 1.0000 Uani . . . . . .
C14 C 0.74168(13) -0.3947(4) 0.62747(8) 0.0353 1.0000 Uani . . . . . .
C15 C 0.71629(13) -0.5970(4) 0.59756(8) 0.0346 1.0000 Uani . . . . . .
C16 C 0.62686(13) -0.6363(4) 0.57652(8) 0.0323 1.0000 Uani . . . . . .
C17 C 0.56006(12) -0.4779(3) 0.58578(7) 0.0271 1.0000 Uani . . . . . .
C18 C 0.46727(13) -0.5202(3) 0.56397(7) 0.0294 1.0000 Uani . . . . . .
C19 C 0.40241(12) -0.3757(3) 0.57436(7) 0.0284 1.0000 Uani . . . . . .
C20 C 0.42402(11) -0.1755(3) 0.60793(7) 0.0237 1.0000 Uani . . . . . .
C21 C 0.47166(12) 0.7382(3) 0.75897(7) 0.0266 1.0000 Uani . . . . . .
C22 C 0.56068(13) 0.7781(4) 0.78291(7) 0.0311 1.0000 Uani . . . . . .
C23 C 0.62733(12) 0.6264(4) 0.77410(8) 0.0344 1.0000 Uani . . . . . .
C24 C 0.60583(12) 0.4339(4) 0.74146(8) 0.0325 1.0000 Uani . . . . . .
C25 C 0.23724(19) 0.1440(5) 0.50002(10) 0.0516 1.0000 Uani . . . . . .
C26 C 0.14229(17) -0.1942(4) 0.53412(9) 0.0405 1.0000 Uani . . . . . .
H3 H -0.0698(17) 0.348(5) 0.5843(10) 0.0444 1.0000 Uiso . . . . . .
H21 H 0.0738(14) 0.206(4) 0.5986(8) 0.0281 1.0000 Uiso . . . . . .
H41 H -0.0007(14) 0.832(4) 0.6505(8) 0.0305 1.0000 Uiso . . . . . .
H51 H 0.1527(14) 0.885(4) 0.6936(8) 0.0291 1.0000 Uiso . . . . . .
H71 H 0.3032(14) 0.770(4) 0.7187(8) 0.0276 1.0000 Uiso . . . . . .
H101 H 0.6020(14) 0.091(4) 0.6800(8) 0.0286 1.0000 Uiso . . . . . .
H131 H 0.6984(15) -0.099(4) 0.6573(9) 0.0385 1.0000 Uiso . . . . . .
H141 H 0.7992(17) -0.357(5) 0.6390(9) 0.0415 1.0000 Uiso . . . . . .
H151 H 0.7575(17) -0.704(4) 0.5912(9) 0.0416 1.0000 Uiso . . . . . .
H161 H 0.6056(15) -0.771(4) 0.5549(9) 0.0386 1.0000 Uiso . . . . . .
H181 H 0.4521(15) -0.660(4) 0.5415(9) 0.0341 1.0000 Uiso . . . . . .
H191 H 0.3415(15) -0.402(4) 0.5604(8) 0.0337 1.0000 Uiso . . . . . .
H211 H 0.4297(15) 0.845(4) 0.7665(8) 0.0322 1.0000 Uiso . . . . . .
H221 H 0.5770(15) 0.913(4) 0.8071(9) 0.0377 1.0000 Uiso . . . . . .
H231 H 0.6856(16) 0.652(5) 0.7913(9) 0.0411 1.0000 Uiso . . . . . .
H241 H 0.6508(16) 0.332(4) 0.7364(9) 0.0397 1.0000 Uiso . . . . . .
H251 H 0.256(2) 0.186(6) 0.5356(14) 0.0764 1.0000 Uiso . . . . . .
H252 H 0.268(2) 0.012(6) 0.4916(13) 0.0765 1.0000 Uiso . . . . . .
H253 H 0.238(2) 0.278(6) 0.4775(13) 0.0767 1.0000 Uiso . . . . . .
H261 H 0.1712(19) -0.143(5) 0.5668(12) 0.0604 1.0000 Uiso . . . . . .
H262 H 0.088(2) -0.259(5) 0.5325(12) 0.0613 1.0000 Uiso . . . . . .
H263 H 0.178(2) -0.296(5) 0.5183(11) 0.0604 1.0000 Uiso . . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.92(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 . 1.8460(12) yes
Ni1 . O2 . 1.8430(12) yes
Ni1 . N1 . 1.8563(15) yes
Ni1 . N2 . 1.8508(14) yes
S1 . O4 . 1.5058(15) yes
S1 . C25 . 1.772(3) yes
S1 . C26 . 1.777(2) yes
O1 . C1 . 1.307(2) yes
O2 . C20 . 1.300(2) yes
O3 . C3 . 1.352(2) yes
O3 . H3 . 0.83(3) no
N1 . C7 . 1.313(2) yes
N1 . C8 . 1.419(2) yes
N2 . C9 . 1.422(2) yes
N2 . C10 . 1.310(2) yes
C1 . C2 . 1.411(2) yes
C1 . C6 . 1.424(2) yes
C2 . C3 . 1.384(2) yes
C2 . H21 . 0.89(2) no
C3 . C4 . 1.408(3) yes
C4 . C5 . 1.364(3) yes
C4 . H41 . 1.00(2) no
C5 . C6 . 1.428(2) yes
C5 . H51 . 0.94(2) no
C6 . C7 . 1.411(2) yes
C7 . H71 . 0.99(2) no
C8 . C9 . 1.399(2) yes
C8 . C21 . 1.390(3) yes
C9 . C24 . 1.396(2) yes
C10 . C11 . 1.412(2) yes
C10 . H101 . 0.96(2) no
C11 . C12 . 1.457(2) yes
C11 . C20 . 1.418(2) yes
C12 . C13 . 1.415(3) yes
C12 . C17 . 1.413(3) yes
C13 . C14 . 1.377(3) yes
C13 . H131 . 0.96(2) no
C14 . C15 . 1.396(3) yes
C14 . H141 . 0.89(2) no
C15 . C16 . 1.373(3) yes
C15 . H151 . 0.91(3) no
C16 . C17 . 1.419(2) yes
C16 . H161 . 0.97(2) no
C17 . C18 . 1.426(3) yes
C18 . C19 . 1.358(3) yes
C18 . H181 . 0.98(2) no
C19 . C20 . 1.429(3) yes
C19 . H191 . 0.93(2) no
C21 . C22 . 1.384(3) yes
C21 . H211 . 0.93(2) no
C22 . C23 . 1.390(3) yes
C22 . H221 . 0.99(2) no
C23 . C24 . 1.380(3) yes
C23 . H231 . 0.92(2) no
C24 . H241 . 0.93(2) no
C25 . H251 . 0.94(3) no
C25 . H252 . 0.93(3) no
C25 . H253 . 0.96(3) no
C26 . H261 . 0.92(3) no
C26 . H262 . 0.90(3) no
C26 . H263 . 0.95(3) 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 . 84.38(5) yes
O1 . Ni1 . N1 . 95.20(6) yes
O2 . Ni1 . N1 . 178.73(6) yes
O1 . Ni1 . N2 . 178.45(6) yes
O2 . Ni1 . N2 . 94.07(6) yes
N1 . Ni1 . N2 . 86.35(6) yes
O4 . S1 . C25 . 105.99(11) yes
O4 . S1 . C26 . 106.15(10) yes
C25 . S1 . C26 . 97.74(12) yes
Ni1 . O1 . C1 . 127.68(11) yes
Ni1 . O2 . C20 . 128.50(11) yes
C3 . O3 . H3 . 106.9(18) no
Ni1 . N1 . C7 . 125.71(12) yes
Ni1 . N1 . C8 . 113.18(11) yes
C7 . N1 . C8 . 120.95(15) yes
Ni1 . N2 . C9 . 113.18(11) yes
Ni1 . N2 . C10 . 126.30(12) yes
C9 . N2 . C10 . 120.44(15) yes
O1 . C1 . C2 . 118.46(16) yes
O1 . C1 . C6 . 123.47(15) yes
C2 . C1 . C6 . 118.07(15) yes
C1 . C2 . C3 . 120.98(16) yes
C1 . C2 . H21 . 116.2(14) no
C3 . C2 . H21 . 122.8(14) no
C2 . C3 . O3 . 122.05(16) yes
C2 . C3 . C4 . 121.27(16) yes
O3 . C3 . C4 . 116.67(15) yes
C3 . C4 . C5 . 118.65(16) yes
C3 . C4 . H41 . 117.3(13) no
C5 . C4 . H41 . 124.0(13) no
C4 . C5 . C6 . 121.96(16) yes
C4 . C5 . H51 . 119.2(13) no
C6 . C5 . H51 . 118.8(13) no
C5 . C6 . C1 . 119.02(15) yes
C5 . C6 . C7 . 118.73(16) yes
C1 . C6 . C7 . 122.24(15) yes
C6 . C7 . N1 . 125.29(16) yes
C6 . C7 . H71 . 116.3(12) no
N1 . C7 . H71 . 118.4(12) no
N1 . C8 . C9 . 113.55(15) yes
N1 . C8 . C21 . 126.20(16) yes
C9 . C8 . C21 . 120.24(16) yes
N2 . C9 . C8 . 113.66(14) yes
N2 . C9 . C24 . 126.52(16) yes
C8 . C9 . C24 . 119.82(16) yes
N2 . C10 . C11 . 126.27(16) yes
N2 . C10 . H101 . 115.5(13) no
C11 . C10 . H101 . 118.2(13) no
C10 . C11 . C12 . 120.00(15) yes
C10 . C11 . C20 . 120.22(15) yes
C12 . C11 . C20 . 119.72(16) yes
C11 . C12 . C13 . 123.42(17) yes
C11 . C12 . C17 . 119.22(16) yes
C13 . C12 . C17 . 117.36(16) yes
C12 . C13 . C14 . 121.58(19) yes
C12 . C13 . H131 . 120.0(14) no
C14 . C13 . H131 . 118.4(14) no
C13 . C14 . C15 . 120.83(19) yes
C13 . C14 . H141 . 117.8(17) no
C15 . C14 . H141 . 121.3(16) no
C14 . C15 . C16 . 119.14(18) yes
C14 . C15 . H151 . 122.0(15) no
C16 . C15 . H151 . 118.8(16) no
C15 . C16 . C17 . 121.13(19) yes
C15 . C16 . H161 . 122.6(14) no
C17 . C16 . H161 . 116.2(14) no
C16 . C17 . C12 . 119.85(17) yes
C16 . C17 . C18 . 120.85(18) yes
C12 . C17 . C18 . 119.28(16) yes
C17 . C18 . C19 . 121.47(18) yes
C17 . C18 . H181 . 117.2(13) no
C19 . C18 . H181 . 121.3(13) no
C18 . C19 . C20 . 121.53(17) yes
C18 . C19 . H191 . 122.3(14) no
C20 . C19 . H191 . 116.2(14) no
C19 . C20 . C11 . 118.73(15) yes
C19 . C20 . O2 . 116.80(15) yes
C11 . C20 . O2 . 124.47(16) yes
C8 . C21 . C22 . 119.47(17) yes
C8 . C21 . H211 . 123.9(14) no
C22 . C21 . H211 . 116.7(14) no
C21 . C22 . C23 . 120.37(18) yes
C21 . C22 . H221 . 120.0(13) no
C23 . C22 . H221 . 119.6(13) no
C22 . C23 . C24 . 120.63(17) yes
C22 . C23 . H231 . 119.3(16) no
C24 . C23 . H231 . 120.0(16) no
C9 . C24 . C23 . 119.44(17) yes
C9 . C24 . H241 . 120.6(15) no
C23 . C24 . H241 . 119.9(15) no
S1 . C25 . H251 . 107.4(20) no
S1 . C25 . H252 . 104(2) no
H251 . C25 . H252 . 112(3) no
S1 . C25 . H253 . 107.4(19) no
H251 . C25 . H253 . 111(3) no
H252 . C25 . H253 . 115(3) no
S1 . C26 . H261 . 108.8(19) no
S1 . C26 . H262 . 105.9(19) no
H261 . C26 . H262 . 115(3) no
S1 . C26 . H263 . 102.8(17) no
H261 . C26 . H263 . 113(2) no
H262 . C26 . H263 . 110(3) 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 . H3 . O4 2_556 170(3) 0.83(3) 1.79(3) 2.616(3) 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 -172.82(14) . . . . no
N1 Ni1 O1 C1 5.98(14) . . . . no
O1 Ni1 O2 C20 176.76(15) . . . . no
N2 Ni1 O2 C20 -3.21(15) . . . . no
O1 Ni1 N1 C7 -6.85(15) . . . . no
O1 Ni1 N1 C8 177.76(11) . . . . no
N2 Ni1 N1 C7 173.09(15) . . . . no
N2 Ni1 N1 C8 -2.30(11) . . . . no
O2 Ni1 N2 C9 -178.64(11) . . . . no
O2 Ni1 N2 C10 4.61(16) . . . . no
N1 Ni1 N2 C9 2.57(12) . . . . no
N1 Ni1 N2 C10 -174.19(16) . . . . no
Ni1 O1 C1 C2 176.67(12) . . . . no
Ni1 O1 C1 C6 -3.0(2) . . . . no
Ni1 O2 C20 C11 0.5(3) . . . . no
Ni1 O2 C20 C19 179.83(12) . . . . no
Ni1 N1 C7 C6 5.0(2) . . . . no
C8 N1 C7 C6 -179.95(15) . . . . no
Ni1 N1 C8 C9 1.55(18) . . . . no
Ni1 N1 C8 C21 -178.69(14) . . . . no
C7 N1 C8 C9 -174.09(15) . . . . no
C7 N1 C8 C21 5.7(3) . . . . no
Ni1 N2 C9 C8 -2.32(18) . . . . no
Ni1 N2 C9 C24 178.21(15) . . . . no
C10 N2 C9 C8 174.65(15) . . . . no
C10 N2 C9 C24 -4.8(3) . . . . no
Ni1 N2 C10 C11 -3.5(3) . . . . no
C9 N2 C10 C11 179.97(16) . . . . no
O1 C1 C2 C3 -176.95(15) . . . . no
C6 C1 C2 C3 2.7(2) . . . . no
O1 C1 C6 C5 177.42(15) . . . . no
O1 C1 C6 C7 -1.3(3) . . . . no
C2 C1 C6 C5 -2.2(2) . . . . no
C2 C1 C6 C7 179.06(15) . . . . no
C1 C2 C3 O3 178.43(15) . . . . no
C1 C2 C3 C4 -1.4(3) . . . . no
O3 C3 C4 C5 179.74(16) . . . . no
C2 C3 C4 C5 -0.4(3) . . . . no
C3 C4 C5 C6 0.8(3) . . . . no
C4 C5 C6 C1 0.5(3) . . . . no
C4 C5 C6 C7 179.24(16) . . . . no
C1 C6 C7 N1 0.2(3) . . . . no
C5 C6 C7 N1 -178.54(16) . . . . no
N1 C8 C9 N2 0.5(2) . . . . no
N1 C8 C9 C24 179.98(16) . . . . no
C21 C8 C9 N2 -179.29(15) . . . . no
C21 C8 C9 C24 0.2(3) . . . . no
N1 C8 C21 C22 -178.72(17) . . . . no
C9 C8 C21 C22 1.0(3) . . . . no
N2 C9 C24 C23 178.05(18) . . . . no
C8 C9 C24 C23 -1.4(3) . . . . no
N2 C10 C11 C12 -177.77(17) . . . . no
N2 C10 C11 C20 -0.6(3) . . . . no
C10 C11 C12 C13 -3.8(3) . . . . no
C10 C11 C12 C17 175.37(16) . . . . no
C20 C11 C12 C13 179.08(17) . . . . no
C20 C11 C12 C17 -1.8(2) . . . . no
C10 C11 C20 O2 2.2(3) . . . . no
C10 C11 C20 C19 -177.15(16) . . . . no
C12 C11 C20 O2 179.38(16) . . . . no
C12 C11 C20 C19 0.0(3) . . . . no
C11 C12 C13 C14 176.86(18) . . . . no
C17 C12 C13 C14 -2.3(3) . . . . no
C11 C12 C17 C16 -176.04(17) . . . . no
C11 C12 C17 C18 2.5(3) . . . . no
C13 C12 C17 C16 3.1(3) . . . . no
C13 C12 C17 C18 -178.36(17) . . . . no
C12 C13 C14 C15 -0.5(3) . . . . no
C13 C14 C15 C16 2.5(3) . . . . no
C14 C15 C16 C17 -1.6(3) . . . . no
C15 C16 C17 C12 -1.3(3) . . . . no
C15 C16 C17 C18 -179.77(19) . . . . no
C12 C17 C18 C19 -1.4(3) . . . . no
C16 C17 C18 C19 177.11(18) . . . . no
C17 C18 C19 C20 -0.5(3) . . . . no
C18 C19 C20 O2 -178.28(16) . . . . no
C18 C19 C20 C11 1.1(3) . . . . no
C8 C21 C22 C23 -1.1(3) . . . . no
C21 C22 C23 C24 -0.1(3) . . . . no
C22 C23 C24 C9 1.3(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 C7 3.7321(17) . 1_545 no
Ni1 C18 3.5514(19) . 1_565 no
Ni1 C19 3.3374(18) . 1_565 no
Ni1 C20 3.9006(17) . 1_565 no
Ni1 C21 3.9063(18) . 1_545 no
S1 O3 3.4627(16) . 2_566 no
O1 C5 3.354(2) . 1_545 no
O1 C7 2.900(2) . . no
O1 N1 2.7341(19) . . no
O1 O2 2.4773(17) . . no
O2 C7 3.124(2) . 1_545 no
O2 C25 3.367(3) . . no
O2 N2 2.7029(19) . . no
O2 C10 2.868(2) . . no
O3 O4 2.616(2) . 2_556 no
O3 C15 3.408(2) . 1_465 no
O3 C22 3.359(2) . 3_546 no
O3 C14 3.329(2) . 1_465 no
O4 C2 3.322(2) . 2_556 no
O4 C4 3.398(2) . 2_566 no
O4 C3 3.355(2) . 2_556 no
N1 C9 2.357(2) . . no
N1 C20 3.309(2) . 1_565 no
N1 N2 2.537(2) . . no
N1 C1 2.933(2) . . no
N2 C18 3.358(2) . 1_565 no
N2 C8 2.361(2) . . no
N2 C17 3.442(2) . 1_565 no
N2 C21 3.400(2) . 1_545 no
N2 C20 2.905(2) . . no
C3 C26 3.582(3) . 1_565 no
C3 C22 3.351(3) . 3_546 no
C3 C21 3.495(2) . 3_546 no
C5 C8 3.591(2) . 3_556 no
C7 C20 3.581(2) . 1_565 no
C8 C20 3.382(2) . 1_565 no
C8 C11 3.423(2) . 1_565 no
C9 C11 3.532(2) . 1_565 no
C9 C12 3.503(2) . 1_565 no
C10 C17 3.381(2) . 1_565 no
C10 C22 3.421(3) . 1_545 no
C10 C21 3.400(2) . 1_545 no
C10 C18 3.529(2) . 1_565 no
C10 C16 3.370(3) . 1_565 no
C12 C24 3.557(3) . 1_545 no



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 08/09/14 at 12:42:04
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT NI   (    1 ,X'S,U'S)  UNTIL C    (   26 ) 
CONT H    (   21 ,X'S)  UNTIL H    (    3 ) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 08/09/14 at 12:42:04
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


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

data_ral1406X
_database_code_depnum_ccdc_archive 'CCDC 1838241'
_audit_update_record             
;
2018-04-19 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_audit_creation_date             14-09-22
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1406X\Tony_ral1406X_data\r At 17:16 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   12.2000(4)
_cell_length_b                   15.0224(5)
_cell_length_c                   15.4129(6)
_cell_angle_alpha                74.102(3)
_cell_angle_beta                 71.068(3)
_cell_angle_gamma                69.971(3)
_cell_volume                     2467.88(16)

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


_cell_formula_units_Z            2 # 6

# Given Formula = C20 H14 N2 Ni1 O4 
# Dc =      1.64 Fooo =   1268.00 Mu =     12.10 M =   1215.16
# Found Formula = C20 H14.67 N2 Ni1 O4.33 

# Dc =      1.66 FOOO =   1268.00 Mu =     12.13 M =   1233.17

_chemical_formula_sum            'C60 H44 N6 Ni3 O13'
_chemical_formula_moiety         '3(C20 H14 N2 Ni O4), H2 O'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         1233.18 # 411.06


_cell_measurement_reflns_used    8873
_cell_measurement_theta_min      2
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.037
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_max          0.337

_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1268
_exptl_absorpt_coefficient_mu    1.213

# Sheldrick geometric approximatio 0.83 0.96 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  0.96
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2014)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2014)'
_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            43351
_reflns_number_total             12285
_diffrn_reflns_av_R_equivalents  0.066
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 12285 
# Theoretical number of reflections is about 28752 


_diffrn_reflns_theta_min         1.838
_diffrn_reflns_theta_max         29.984
_diffrn_measured_fraction_theta_max 0.854

_diffrn_reflns_theta_full        26.490
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -15
_reflns_limit_h_max              16
_reflns_limit_k_min              -19
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              21

_oxford_diffrn_Wilson_B_factor   1.45
_oxford_diffrn_Wilson_scale      1.81

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

_refine_diff_density_min         -1.53
_refine_diff_density_max         1.50


# 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         12283
_refine_ls_number_restraints     0
_refine_ls_number_parameters     739
_oxford_refine_ls_R_factor_ref   0.1142
_refine_ls_wR_factor_ref         0.1061
_refine_ls_goodness_of_fit_ref   1.0221
_refine_ls_shift/su_max          0.0080350
_refine_ls_shift/su_mean         0.0001258


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        12283
_refine_ls_R_factor_all          0.1142
_refine_ls_wR_factor_all         0.1061

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7756
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_gt          0.0823

# 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) + ( 0.02P)² + 3.33P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
The largest features in the
final difference electron density map are located 
randomly through the structure.
;

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

# Replace last . with number of unfound hydrogen 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 0.38743(4) 0.45707(3) 0.49469(3) 0.0247 1.0000 Uani . . . . . .
Ni2 Ni 0.48623(4) 0.16925(3) 0.37724(3) 0.0221 1.0000 Uani . . . . . .
Ni3 Ni 0.69373(4) 0.01328(3) 0.05188(3) 0.0232 1.0000 Uani . . . . . .
O1 O 0.2979(2) 0.53939(18) 0.41327(18) 0.0321 1.0000 Uani . . . . . .
O2 O 0.2605(2) 0.51482(18) 0.58402(17) 0.0306 1.0000 Uani . . . . . .
O3 O 0.1508(3) 0.6863(2) 0.3197(2) 0.0474 1.0000 Uani . . . . . .
O4 O 0.0582(3) 0.6167(2) 0.6877(2) 0.0481 1.0000 Uani . . . . . .
O5 O 0.6275(2) 0.08545(17) 0.32493(16) 0.0257 1.0000 Uani . . . . . .
O6 O 0.4739(2) 0.21318(17) 0.25459(16) 0.0251 1.0000 Uani . . . . . .
O7 O 0.8244(2) -0.01626(18) 0.21838(16) 0.0314 1.0000 Uani . . . . . .
O8 O 0.4864(2) 0.25598(18) 0.06803(17) 0.0325 1.0000 Uani . . . . . .
O9 O 0.7051(2) 0.11760(17) 0.08811(16) 0.0247 1.0000 Uani . . . . . .
O10 O 0.5475(2) 0.03167(17) 0.13986(16) 0.0273 1.0000 Uani . . . . . .
O11 O 0.6848(2) 0.27244(19) 0.15830(17) 0.0350 1.0000 Uani . . . . . .
O12 O 0.3461(2) 0.08525(18) 0.27114(17) 0.0332 1.0000 Uani . . . . . .
O13 O 0.0510(3) 0.5710(4) 0.5096(3) 0.1343 1.0000 Uani . . . . . .
N1 N 0.5133(3) 0.4010(2) 0.4025(2) 0.0251 1.0000 Uani . . . . . .
N2 N 0.4736(3) 0.3728(2) 0.5789(2) 0.0243 1.0000 Uani . . . . . .
N3 N 0.5016(3) 0.1233(2) 0.49905(19) 0.0218 1.0000 Uani . . . . . .
N4 N 0.3430(3) 0.2552(2) 0.4278(2) 0.0233 1.0000 Uani . . . . . .
N5 N 0.8400(3) -0.0016(2) -0.03832(19) 0.0221 1.0000 Uani . . . . . .
N6 N 0.6794(3) -0.0915(2) 0.01799(19) 0.0241 1.0000 Uani . . . . . .
C1 C 0.3337(4) 0.5564(3) 0.3208(3) 0.0294 1.0000 Uani . . . . . .
C2 C 0.2574(4) 0.6329(3) 0.2716(3) 0.0353 1.0000 Uani . . . . . .
C3 C 0.2893(4) 0.6525(3) 0.1761(3) 0.0378 1.0000 Uani . . . . . .
C4 C 0.3955(4) 0.5991(3) 0.1243(3) 0.0392 1.0000 Uani . . . . . .
C5 C 0.4711(4) 0.5252(3) 0.1697(3) 0.0355 1.0000 Uani . . . . . .
C6 C 0.4420(3) 0.5032(3) 0.2686(3) 0.0280 1.0000 Uani . . . . . .
C7 C 0.5248(3) 0.4268(3) 0.3124(3) 0.0271 1.0000 Uani . . . . . .
C8 C 0.6049(3) 0.3253(2) 0.4385(3) 0.0247 1.0000 Uani . . . . . .
C9 C 0.5848(3) 0.3128(2) 0.5348(3) 0.0243 1.0000 Uani . . . . . .
C10 C 0.4365(3) 0.3623(3) 0.6696(3) 0.0287 1.0000 Uani . . . . . .
C11 C 0.3263(3) 0.4169(3) 0.7209(3) 0.0270 1.0000 Uani . . . . . .
C12 C 0.2965(4) 0.3955(3) 0.8198(3) 0.0346 1.0000 Uani . . . . . .
C13 C 0.1910(4) 0.4450(3) 0.8710(3) 0.0393 1.0000 Uani . . . . . .
C14 C 0.1107(4) 0.5198(3) 0.8267(3) 0.0415 1.0000 Uani . . . . . .
C15 C 0.1367(4) 0.5428(3) 0.7311(3) 0.0334 1.0000 Uani . . . . . .
C16 C 0.2453(3) 0.4908(3) 0.6751(3) 0.0276 1.0000 Uani . . . . . .
C17 C 0.7076(3) 0.2677(3) 0.3872(3) 0.0300 1.0000 Uani . . . . . .
C18 C 0.7906(4) 0.2006(3) 0.4324(3) 0.0381 1.0000 Uani . . . . . .
C19 C 0.7724(4) 0.1909(3) 0.5273(3) 0.0374 1.0000 Uani . . . . . .
C20 C 0.6701(4) 0.2460(3) 0.5791(3) 0.0330 1.0000 Uani . . . . . .
C21 C 0.7081(3) 0.0237(2) 0.3676(2) 0.0229 1.0000 Uani . . . . . .
C22 C 0.8133(3) -0.0308(3) 0.3121(3) 0.0265 1.0000 Uani . . . . . .
C23 C 0.9033(3) -0.0970(3) 0.3502(3) 0.0322 1.0000 Uani . . . . . .
C24 C 0.8918(3) -0.1133(3) 0.4464(3) 0.0331 1.0000 Uani . . . . . .
C25 C 0.7903(3) -0.0634(3) 0.5023(3) 0.0300 1.0000 Uani . . . . . .
C26 C 0.6969(3) 0.0060(3) 0.4644(2) 0.0240 1.0000 Uani . . . . . .
C27 C 0.5929(3) 0.0568(3) 0.5248(2) 0.0249 1.0000 Uani . . . . . .
C28 C 0.4027(3) 0.1700(3) 0.5661(2) 0.0242 1.0000 Uani . . . . . .
C29 C 0.3155(3) 0.2424(3) 0.5275(2) 0.0244 1.0000 Uani . . . . . .
C30 C 0.2729(3) 0.3244(3) 0.3815(2) 0.0256 1.0000 Uani . . . . . .
C31 C 0.2925(3) 0.3449(3) 0.2825(2) 0.0238 1.0000 Uani . . . . . .
C32 C 0.2099(3) 0.4264(3) 0.2429(3) 0.0309 1.0000 Uani . . . . . .
C33 C 0.2253(4) 0.4502(3) 0.1486(3) 0.0327 1.0000 Uani . . . . . .
C34 C 0.3204(3) 0.3924(3) 0.0907(3) 0.0303 1.0000 Uani . . . . . .
C35 C 0.3993(3) 0.3125(3) 0.1279(3) 0.0265 1.0000 Uani . . . . . .
C36 C 0.3900(3) 0.2885(2) 0.2245(2) 0.0245 1.0000 Uani . . . . . .
C37 C 0.3872(3) 0.1486(3) 0.6624(3) 0.0295 1.0000 Uani . . . . . .
C38 C 0.2869(4) 0.2003(3) 0.7182(3) 0.0310 1.0000 Uani . . . . . .
C39 C 0.1994(4) 0.2731(3) 0.6800(3) 0.0342 1.0000 Uani . . . . . .
C40 C 0.2130(4) 0.2940(3) 0.5848(3) 0.0312 1.0000 Uani . . . . . .
C41 C 0.7865(3) 0.1657(2) 0.0460(2) 0.0223 1.0000 Uani . . . . . .
C42 C 0.7741(3) 0.2480(3) 0.0809(3) 0.0273 1.0000 Uani . . . . . .
C43 C 0.8525(4) 0.3040(3) 0.0372(3) 0.0302 1.0000 Uani . . . . . .
C44 C 0.9487(4) 0.2792(3) -0.0388(3) 0.0327 1.0000 Uani . . . . . .
C45 C 0.9665(3) 0.1979(3) -0.0708(3) 0.0288 1.0000 Uani . . . . . .
C46 C 0.8857(3) 0.1401(3) -0.0288(2) 0.0246 1.0000 Uani . . . . . .
C47 C 0.9083(3) 0.0561(3) -0.0660(2) 0.0253 1.0000 Uani . . . . . .
C48 C 0.8680(3) -0.0806(3) -0.0836(2) 0.0273 1.0000 Uani . . . . . .
C49 C 0.7803(3) -0.1291(3) -0.0531(2) 0.0270 1.0000 Uani . . . . . .
C50 C 0.5862(3) -0.1254(3) 0.0493(3) 0.0270 1.0000 Uani . . . . . .
C51 C 0.4818(3) -0.0942(3) 0.1191(2) 0.0260 1.0000 Uani . . . . . .
C52 C 0.3883(4) -0.1394(3) 0.1461(3) 0.0313 1.0000 Uani . . . . . .
C53 C 0.2848(4) -0.1097(3) 0.2125(3) 0.0332 1.0000 Uani . . . . . .
C54 C 0.2712(4) -0.0326(3) 0.2539(3) 0.0317 1.0000 Uani . . . . . .
C55 C 0.3594(3) 0.0124(3) 0.2288(2) 0.0269 1.0000 Uani . . . . . .
C56 C 0.4680(3) -0.0161(3) 0.1599(2) 0.0252 1.0000 Uani . . . . . .
C57 C 0.9705(4) -0.1090(3) -0.1542(3) 0.0315 1.0000 Uani . . . . . .
C58 C 0.9807(4) -0.1854(3) -0.1938(3) 0.0375 1.0000 Uani . . . . . .
C59 C 0.8925(4) -0.2324(3) -0.1641(3) 0.0386 1.0000 Uani . . . . . .
C60 C 0.7921(4) -0.2050(3) -0.0935(3) 0.0351 1.0000 Uani . . . . . .
H31 H 0.2370 0.7023 0.1461 0.0446 1.0000 Uiso R . . . . .
H41 H 0.4152 0.6133 0.0588 0.0466 1.0000 Uiso R . . . . .
H51 H 0.5432 0.4878 0.1366 0.0422 1.0000 Uiso R . . . . .
H71 H 0.5932 0.3923 0.2733 0.0328 1.0000 Uiso R . . . . .
H101 H 0.4865 0.3138 0.7037 0.0331 1.0000 Uiso R . . . . .
H121 H 0.3510 0.3467 0.8496 0.0418 1.0000 Uiso R . . . . .
H131 H 0.1722 0.4297 0.9360 0.0470 1.0000 Uiso R . . . . .
H141 H 0.0388 0.5543 0.8616 0.0496 1.0000 Uiso R . . . . .
H171 H 0.7209 0.2740 0.3233 0.0357 1.0000 Uiso R . . . . .
H181 H 0.8592 0.1613 0.3990 0.0458 1.0000 Uiso R . . . . .
H191 H 0.8309 0.1467 0.5566 0.0445 1.0000 Uiso R . . . . .
H201 H 0.6577 0.2395 0.6435 0.0397 1.0000 Uiso R . . . . .
H231 H 0.9726 -0.1311 0.3122 0.0387 1.0000 Uiso R . . . . .
H241 H 0.9513 -0.1609 0.4728 0.0403 1.0000 Uiso R . . . . .
H251 H 0.7814 -0.0758 0.5664 0.0354 1.0000 Uiso R . . . . .
H271 H 0.5898 0.0419 0.5877 0.0299 1.0000 Uiso R . . . . .
H301 H 0.2042 0.3643 0.4144 0.0311 1.0000 Uiso R . . . . .
H321 H 0.1449 0.4631 0.2831 0.0368 1.0000 Uiso R . . . . .
H331 H 0.1723 0.5046 0.1219 0.0391 1.0000 Uiso R . . . . .
H341 H 0.3304 0.4080 0.0267 0.0356 1.0000 Uiso R . . . . .
H371 H 0.4452 0.0992 0.6887 0.0347 1.0000 Uiso R . . . . .
H381 H 0.2772 0.1861 0.7829 0.0364 1.0000 Uiso R . . . . .
H391 H 0.1311 0.3072 0.7189 0.0409 1.0000 Uiso R . . . . .
H401 H 0.1535 0.3420 0.5598 0.0362 1.0000 Uiso R . . . . .
H431 H 0.8405 0.3585 0.0590 0.0355 1.0000 Uiso R . . . . .
H441 H 1.0001 0.3176 -0.0668 0.0387 1.0000 Uiso R . . . . .
H451 H 1.0304 0.1800 -0.1202 0.0342 1.0000 Uiso R . . . . .
H471 H 0.9787 0.0418 -0.1139 0.0297 1.0000 Uiso R . . . . .
H501 H 0.5865 -0.1736 0.0227 0.0312 1.0000 Uiso R . . . . .
H521 H 0.3971 -0.1897 0.1191 0.0382 1.0000 Uiso R . . . . .
H531 H 0.2238 -0.1395 0.2294 0.0401 1.0000 Uiso R . . . . .
H541 H 0.2007 -0.0118 0.2990 0.0378 1.0000 Uiso R . . . . .
H571 H 1.0317 -0.0782 -0.1756 0.0370 1.0000 Uiso R . . . . .
H581 H 1.0477 -0.2041 -0.2404 0.0447 1.0000 Uiso R . . . . .
H591 H 0.8998 -0.2832 -0.1910 0.0457 1.0000 Uiso R . . . . .
H601 H 0.7326 -0.2370 -0.0735 0.0421 1.0000 Uiso R . . . . .
H3 H 0.1263 0.6664 0.3749 0.0710 1.0000 Uiso R . . . . .
H4 H 0.0767 0.6228 0.6302 0.0722 1.0000 Uiso R . . . . .
H7 H 0.7651 0.0246 0.2041 0.0470 1.0000 Uiso R . . . . .
H8 H 0.5300 0.2095 0.0930 0.0486 1.0000 Uiso R . . . . .
H11 H 0.6475 0.2336 0.1805 0.0532 1.0000 Uiso R . . . . .
H12 H 0.4078 0.1025 0.2527 0.0499 1.0000 Uiso R . . . . .
H13 H 0.0835 0.5267 0.4818 0.2016 1.0000 Uiso R . . . . .
H14 H 0.1193 0.5628 0.5121 0.2018 1.0000 Uiso R . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.8018(11)
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 . Ni1 2_666 3.4741(10) yes
Ni1 . O1 . 1.847(2) yes
Ni1 . O2 . 1.843(3) yes
Ni1 . N1 . 1.855(3) yes
Ni1 . N2 . 1.862(3) yes
Ni2 . O5 . 1.836(2) yes
Ni2 . O6 . 1.861(2) yes
Ni2 . N3 . 1.862(3) yes
Ni2 . N4 . 1.857(3) yes
Ni3 . O9 . 1.862(2) yes
Ni3 . O10 . 1.842(2) yes
Ni3 . N5 . 1.859(3) yes
Ni3 . N6 . 1.866(3) yes
O1 . C1 . 1.326(4) yes
O2 . C16 . 1.317(4) yes
O3 . C2 . 1.367(5) yes
O3 . H3 . 0.812 no
O4 . C15 . 1.370(5) yes
O4 . H4 . 0.827 no
O5 . C21 . 1.312(4) yes
O6 . C36 . 1.331(4) yes
O7 . C22 . 1.368(4) yes
O7 . H7 . 0.821 no
O8 . C35 . 1.370(4) yes
O8 . H8 . 0.806 no
O9 . C41 . 1.321(4) yes
O10 . C56 . 1.309(4) yes
O11 . C42 . 1.367(4) yes
O11 . H11 . 0.797 no
O12 . C55 . 1.361(4) yes
O12 . H12 . 0.817 no
O13 . H13 . 0.806 no
O13 . H14 . 0.812 no
N1 . C7 . 1.309(4) yes
N1 . C8 . 1.426(4) yes
N2 . C9 . 1.420(4) yes
N2 . C10 . 1.304(4) yes
N3 . C27 . 1.305(4) yes
N3 . C28 . 1.423(4) yes
N4 . C29 . 1.436(4) yes
N4 . C30 . 1.305(4) yes
N5 . C47 . 1.300(4) yes
N5 . C48 . 1.425(4) yes
N6 . C49 . 1.422(5) yes
N6 . C50 . 1.301(4) yes
C1 . C2 . 1.418(5) yes
C1 . C6 . 1.404(5) yes
C2 . C3 . 1.370(5) yes
C3 . C4 . 1.389(6) yes
C3 . H31 . 0.924 no
C4 . C5 . 1.365(6) yes
C4 . H41 . 0.939 no
C5 . C6 . 1.419(5) yes
C5 . H51 . 0.936 no
C6 . C7 . 1.420(5) yes
C7 . H71 . 0.937 no
C8 . C9 . 1.394(5) yes
C8 . C17 . 1.391(5) yes
C9 . C20 . 1.387(5) yes
C10 . C11 . 1.420(5) yes
C10 . H101 . 0.935 no
C11 . C12 . 1.418(5) yes
C11 . C16 . 1.406(5) yes
C12 . C13 . 1.356(6) yes
C12 . H121 . 0.933 no
C13 . C14 . 1.397(6) yes
C13 . H131 . 0.933 no
C14 . C15 . 1.373(5) yes
C14 . H141 . 0.929 no
C15 . C16 . 1.424(5) yes
C17 . C18 . 1.378(5) yes
C17 . H171 . 0.928 no
C18 . C19 . 1.380(6) yes
C18 . H181 . 0.929 no
C19 . C20 . 1.374(5) yes
C19 . H191 . 0.936 no
C20 . H201 . 0.936 no
C21 . C22 . 1.415(5) yes
C21 . C26 . 1.411(5) yes
C22 . C23 . 1.374(5) yes
C23 . C24 . 1.403(5) yes
C23 . H231 . 0.931 no
C24 . C25 . 1.365(5) yes
C24 . H241 . 0.938 no
C25 . C26 . 1.417(5) yes
C25 . H251 . 0.931 no
C26 . C27 . 1.421(5) yes
C27 . H271 . 0.925 no
C28 . C29 . 1.390(5) yes
C28 . C37 . 1.392(5) yes
C29 . C40 . 1.392(5) yes
C30 . C31 . 1.427(5) yes
C30 . H301 . 0.930 no
C31 . C32 . 1.426(5) yes
C31 . C36 . 1.402(5) yes
C32 . C33 . 1.364(5) yes
C32 . H321 . 0.941 no
C33 . C34 . 1.399(5) yes
C33 . H331 . 0.940 no
C34 . C35 . 1.373(5) yes
C34 . H341 . 0.927 no
C35 . C36 . 1.409(5) yes
C37 . C38 . 1.369(5) yes
C37 . H371 . 0.937 no
C38 . C39 . 1.392(5) yes
C38 . H381 . 0.937 no
C39 . C40 . 1.380(5) yes
C39 . H391 . 0.932 no
C40 . H401 . 0.931 no
C41 . C42 . 1.422(5) yes
C41 . C46 . 1.400(5) yes
C42 . C43 . 1.379(5) yes
C43 . C44 . 1.391(5) yes
C43 . H431 . 0.917 no
C44 . C45 . 1.365(5) yes
C44 . H441 . 0.921 no
C45 . C46 . 1.417(5) yes
C45 . H451 . 0.918 no
C46 . C47 . 1.432(5) yes
C47 . H471 . 0.937 no
C48 . C49 . 1.384(5) yes
C48 . C57 . 1.392(5) yes
C49 . C60 . 1.389(5) yes
C50 . C51 . 1.407(5) yes
C50 . H501 . 0.922 no
C51 . C52 . 1.415(5) yes
C51 . C56 . 1.414(5) yes
C52 . C53 . 1.367(5) yes
C52 . H521 . 0.918 no
C53 . C54 . 1.406(5) yes
C53 . H531 . 0.928 no
C54 . C55 . 1.360(5) yes
C54 . H541 . 0.932 no
C55 . C56 . 1.419(5) yes
C57 . C58 . 1.394(5) yes
C57 . H571 . 0.934 no
C58 . C59 . 1.374(6) yes
C58 . H581 . 0.914 no
C59 . C60 . 1.374(5) yes
C59 . H591 . 0.931 no
C60 . H601 . 0.931 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
Ni1 2_666 Ni1 . O1 . 112.87(8) yes
Ni1 2_666 Ni1 . O2 . 99.94(8) yes
O1 . Ni1 . O2 . 83.82(11) yes
Ni1 2_666 Ni1 . N1 . 80.54(9) yes
O1 . Ni1 . N1 . 94.76(12) yes
O2 . Ni1 . N1 . 178.58(12) yes
Ni1 2_666 Ni1 . N2 . 68.66(9) yes
O1 . Ni1 . N2 . 178.25(12) yes
O2 . Ni1 . N2 . 95.12(12) yes
N1 . Ni1 . N2 . 86.29(13) yes
O5 . Ni2 . O6 . 83.67(10) yes
O5 . Ni2 . N3 . 95.11(12) yes
O6 . Ni2 . N3 . 178.78(12) yes
O5 . Ni2 . N4 . 178.86(12) yes
O6 . Ni2 . N4 . 95.20(12) yes
N3 . Ni2 . N4 . 86.02(13) yes
O9 . Ni3 . O10 . 83.97(10) yes
O9 . Ni3 . N5 . 95.00(12) yes
O10 . Ni3 . N5 . 178.38(12) yes
O9 . Ni3 . N6 . 178.68(12) yes
O10 . Ni3 . N6 . 94.75(12) yes
N5 . Ni3 . N6 . 86.28(13) yes
Ni1 . O1 . C1 . 127.0(2) yes
Ni1 . O2 . C16 . 126.8(2) yes
C2 . O3 . H3 . 118.3 no
C15 . O4 . H4 . 114.7 no
Ni2 . O5 . C21 . 127.0(2) yes
Ni2 . O6 . C36 . 126.3(2) yes
C22 . O7 . H7 . 110.9 no
C35 . O8 . H8 . 114.3 no
Ni3 . O9 . C41 . 126.4(2) yes
Ni3 . O10 . C56 . 126.9(2) yes
C42 . O11 . H11 . 111.4 no
C55 . O12 . H12 . 109.9 no
H13 . O13 . H14 . 82.4 no
Ni1 . N1 . C7 . 126.3(3) yes
Ni1 . N1 . C8 . 113.2(2) yes
C7 . N1 . C8 . 120.5(3) yes
Ni1 . N2 . C9 . 112.9(2) yes
Ni1 . N2 . C10 . 125.9(3) yes
C9 . N2 . C10 . 121.1(3) yes
Ni2 . N3 . C27 . 126.0(3) yes
Ni2 . N3 . C28 . 113.5(2) yes
C27 . N3 . C28 . 120.5(3) yes
Ni2 . N4 . C29 . 113.2(2) yes
Ni2 . N4 . C30 . 126.4(3) yes
C29 . N4 . C30 . 120.4(3) yes
Ni3 . N5 . C47 . 126.2(3) yes
Ni3 . N5 . C48 . 112.9(2) yes
C47 . N5 . C48 . 120.7(3) yes
Ni3 . N6 . C49 . 112.6(2) yes
Ni3 . N6 . C50 . 125.9(3) yes
C49 . N6 . C50 . 121.3(3) yes
O1 . C1 . C2 . 117.9(4) yes
O1 . C1 . C6 . 124.2(3) yes
C2 . C1 . C6 . 117.9(4) yes
C1 . C2 . O3 . 119.9(4) yes
C1 . C2 . C3 . 120.2(4) yes
O3 . C2 . C3 . 119.9(4) yes
C2 . C3 . C4 . 122.0(4) yes
C2 . C3 . H31 . 118.1 no
C4 . C3 . H31 . 119.9 no
C3 . C4 . C5 . 119.2(4) yes
C3 . C4 . H41 . 120.5 no
C5 . C4 . H41 . 120.2 no
C4 . C5 . C6 . 120.6(4) yes
C4 . C5 . H51 . 121.1 no
C6 . C5 . H51 . 118.3 no
C5 . C6 . C1 . 120.1(4) yes
C5 . C6 . C7 . 118.4(4) yes
C1 . C6 . C7 . 121.5(3) yes
C6 . C7 . N1 . 125.5(4) yes
C6 . C7 . H71 . 116.9 no
N1 . C7 . H71 . 117.6 no
N1 . C8 . C9 . 113.4(3) yes
N1 . C8 . C17 . 126.5(3) yes
C9 . C8 . C17 . 120.0(3) yes
N2 . C9 . C8 . 114.1(3) yes
N2 . C9 . C20 . 125.9(3) yes
C8 . C9 . C20 . 120.1(3) yes
N2 . C10 . C11 . 125.8(3) yes
N2 . C10 . H101 . 116.9 no
C11 . C10 . H101 . 117.3 no
C10 . C11 . C12 . 119.5(3) yes
C10 . C11 . C16 . 121.0(3) yes
C12 . C11 . C16 . 119.5(4) yes
C11 . C12 . C13 . 121.1(4) yes
C11 . C12 . H121 . 119.0 no
C13 . C12 . H121 . 119.9 no
C12 . C13 . C14 . 120.1(4) yes
C12 . C13 . H131 . 120.2 no
C14 . C13 . H131 . 119.7 no
C13 . C14 . C15 . 120.4(4) yes
C13 . C14 . H141 . 120.3 no
C15 . C14 . H141 . 119.3 no
C14 . C15 . O4 . 120.3(4) yes
C14 . C15 . C16 . 120.9(4) yes
O4 . C15 . C16 . 118.7(3) yes
C15 . C16 . C11 . 117.9(3) yes
C15 . C16 . O2 . 116.9(3) yes
C11 . C16 . O2 . 125.2(3) yes
C8 . C17 . C18 . 119.2(4) yes
C8 . C17 . H171 . 120.9 no
C18 . C17 . H171 . 119.9 no
C17 . C18 . C19 . 120.5(4) yes
C17 . C18 . H181 . 120.0 no
C19 . C18 . H181 . 119.5 no
C18 . C19 . C20 . 120.9(4) yes
C18 . C19 . H191 . 119.5 no
C20 . C19 . H191 . 119.5 no
C9 . C20 . C19 . 119.2(4) yes
C9 . C20 . H201 . 119.8 no
C19 . C20 . H201 . 121.0 no
O5 . C21 . C22 . 117.2(3) yes
O5 . C21 . C26 . 125.2(3) yes
C22 . C21 . C26 . 117.6(3) yes
C21 . C22 . O7 . 118.4(3) yes
C21 . C22 . C23 . 121.5(3) yes
O7 . C22 . C23 . 120.1(3) yes
C22 . C23 . C24 . 120.4(4) yes
C22 . C23 . H231 . 120.1 no
C24 . C23 . H231 . 119.5 no
C23 . C24 . C25 . 119.6(4) yes
C23 . C24 . H241 . 120.3 no
C25 . C24 . H241 . 120.1 no
C24 . C25 . C26 . 121.1(4) yes
C24 . C25 . H251 . 119.5 no
C26 . C25 . H251 . 119.4 no
C25 . C26 . C21 . 119.8(3) yes
C25 . C26 . C27 . 119.3(3) yes
C21 . C26 . C27 . 120.8(3) yes
C26 . C27 . N3 . 125.6(3) yes
C26 . C27 . H271 . 117.3 no
N3 . C27 . H271 . 117.1 no
N3 . C28 . C29 . 113.7(3) yes
N3 . C28 . C37 . 126.3(3) yes
C29 . C28 . C37 . 119.9(3) yes
N4 . C29 . C28 . 113.6(3) yes
N4 . C29 . C40 . 126.2(3) yes
C28 . C29 . C40 . 120.2(3) yes
N4 . C30 . C31 . 125.2(3) yes
N4 . C30 . H301 . 118.8 no
C31 . C30 . H301 . 116.0 no
C30 . C31 . C32 . 117.8(3) yes
C30 . C31 . C36 . 122.1(3) yes
C32 . C31 . C36 . 120.1(3) yes
C31 . C32 . C33 . 120.3(4) yes
C31 . C32 . H321 . 118.7 no
C33 . C32 . H321 . 121.0 no
C32 . C33 . C34 . 119.8(4) yes
C32 . C33 . H331 . 120.8 no
C34 . C33 . H331 . 119.4 no
C33 . C34 . C35 . 120.6(4) yes
C33 . C34 . H341 . 119.9 no
C35 . C34 . H341 . 119.5 no
C34 . C35 . O8 . 117.8(3) yes
C34 . C35 . C36 . 121.2(4) yes
O8 . C35 . C36 . 121.0(3) yes
C35 . C36 . C31 . 117.9(3) yes
C35 . C36 . O6 . 117.6(3) yes
C31 . C36 . O6 . 124.4(3) yes
C28 . C37 . C38 . 119.6(4) yes
C28 . C37 . H371 . 120.2 no
C38 . C37 . H371 . 120.3 no
C37 . C38 . C39 . 120.8(4) yes
C37 . C38 . H381 . 119.3 no
C39 . C38 . H381 . 119.9 no
C38 . C39 . C40 . 120.1(4) yes
C38 . C39 . H391 . 119.9 no
C40 . C39 . H391 . 120.0 no
C29 . C40 . C39 . 119.4(4) yes
C29 . C40 . H401 . 120.9 no
C39 . C40 . H401 . 119.7 no
O9 . C41 . C42 . 117.5(3) yes
O9 . C41 . C46 . 124.8(3) yes
C42 . C41 . C46 . 117.7(3) yes
C41 . C42 . O11 . 120.6(3) yes
C41 . C42 . C43 . 120.4(3) yes
O11 . C42 . C43 . 119.0(3) yes
C42 . C43 . C44 . 121.2(4) yes
C42 . C43 . H431 . 118.9 no
C44 . C43 . H431 . 119.9 no
C43 . C44 . C45 . 119.7(4) yes
C43 . C44 . H441 . 119.8 no
C45 . C44 . H441 . 120.5 no
C44 . C45 . C46 . 120.4(4) yes
C44 . C45 . H451 . 120.7 no
C46 . C45 . H451 . 118.9 no
C45 . C46 . C41 . 120.5(3) yes
C45 . C46 . C47 . 117.9(3) yes
C41 . C46 . C47 . 121.6(3) yes
C46 . C47 . N5 . 125.4(3) yes
C46 . C47 . H471 . 116.7 no
N5 . C47 . H471 . 117.9 no
N5 . C48 . C49 . 113.9(3) yes
N5 . C48 . C57 . 126.1(4) yes
C49 . C48 . C57 . 120.0(4) yes
N6 . C49 . C48 . 114.2(3) yes
N6 . C49 . C60 . 125.0(4) yes
C48 . C49 . C60 . 120.7(4) yes
N6 . C50 . C51 . 126.3(4) yes
N6 . C50 . H501 . 117.9 no
C51 . C50 . H501 . 115.8 no
C50 . C51 . C52 . 119.4(4) yes
C50 . C51 . C56 . 120.5(3) yes
C52 . C51 . C56 . 120.0(4) yes
C51 . C52 . C53 . 120.9(4) yes
C51 . C52 . H521 . 119.9 no
C53 . C52 . H521 . 119.2 no
C52 . C53 . C54 . 119.2(4) yes
C52 . C53 . H531 . 120.3 no
C54 . C53 . H531 . 120.5 no
C53 . C54 . C55 . 121.0(4) yes
C53 . C54 . H541 . 119.7 no
C55 . C54 . H541 . 119.3 no
O12 . C55 . C54 . 120.3(3) yes
O12 . C55 . C56 . 118.3(3) yes
C54 . C55 . C56 . 121.5(4) yes
C55 . C56 . C51 . 117.3(3) yes
C55 . C56 . O10 . 117.3(3) yes
C51 . C56 . O10 . 125.4(3) yes
C48 . C57 . C58 . 118.4(4) yes
C48 . C57 . H571 . 121.8 no
C58 . C57 . H571 . 119.8 no
C57 . C58 . C59 . 121.3(4) yes
C57 . C58 . H581 . 118.5 no
C59 . C58 . H581 . 120.2 no
C58 . C59 . C60 . 120.2(4) yes
C58 . C59 . H591 . 120.8 no
C60 . C59 . H591 . 119.0 no
C49 . C60 . C59 . 119.4(4) yes
C49 . C60 . H601 . 120.6 no
C59 . C60 . H601 . 120.0 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 . H3 . O13 . 160 0.81 2.29 3.066(6) yes
O4 . H4 . O13 . 142 0.83 2.35 3.040(6) yes
O7 . H7 . O9 . 142 0.82 2.11 2.806(6) yes
O8 . H8 . O9 . 148 0.81 2.10 2.814(6) yes
O8 . H8 . O10 . 136 0.81 2.52 3.148(6) yes
O11 . H11 . O6 . 145 0.80 2.14 2.825(6) yes
O12 . H12 . O6 . 141 0.82 2.09 2.777(6) yes
O13 . H14 . O1 . 136 0.81 2.19 2.830(6) yes
O13 . H14 . O2 . 153 0.81 2.16 2.909(6) 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 169.9(3) . . . . no
N1 Ni1 O1 C1 -10.1(4) . . . . no
O1 Ni1 O2 C16 174.3(3) . . . . no
N2 Ni1 O2 C16 -4.3(3) . . . . no
O1 Ni1 N1 C7 5.3(4) . . . . no
O1 Ni1 N1 C8 -177.0(3) . . . . no
N2 Ni1 N1 C7 -176.0(4) . . . . no
N2 Ni1 N1 C8 1.6(3) . . . . no
O2 Ni1 N2 C9 -179.3(3) . . . . no
O2 Ni1 N2 C10 5.3(4) . . . . no
N1 Ni1 N2 C9 0.7(3) . . . . no
N1 Ni1 N2 C10 -174.8(4) . . . . no
O5 Ni2 N3 C27 3.5(4) . . . . no
O5 Ni2 N3 C28 -178.2(3) . . . . no
N4 Ni2 N3 C27 -176.4(4) . . . . no
N4 Ni2 N3 C28 1.9(3) . . . . no
O6 Ni2 N4 C29 178.1(3) . . . . no
O6 Ni2 N4 C30 -4.8(4) . . . . no
N3 Ni2 N4 C29 -1.9(3) . . . . no
N3 Ni2 N4 C30 175.3(4) . . . . no
O5 Ni2 O6 C36 -174.4(3) . . . . no
N4 Ni2 O6 C36 5.5(3) . . . . no
O6 Ni2 O5 C21 175.1(3) . . . . no
N3 Ni2 O5 C21 -5.0(3) . . . . no
O10 Ni3 N6 C50 4.0(3) . . . . no
N6 Ni3 N5 C48 -1.3(3) . . . . no
O10 Ni3 N6 C49 179.8(2) . . . . no
O9 Ni3 N5 C48 178.5(2) . . . . no
N6 Ni3 N5 C47 173.0(3) . . . . no
O9 Ni3 N5 C47 -7.3(3) . . . . no
N5 Ni3 O9 C41 9.0(3) . . . . no
O9 Ni3 O10 C56 177.4(3) . . . . no
O10 Ni3 O9 C41 -169.8(3) . . . . no
N5 Ni3 N6 C49 1.0(3) . . . . no
N6 Ni3 O10 C56 -2.9(3) . . . . no
N5 Ni3 N6 C50 -174.7(3) . . . . no
Ni1 O1 C1 C6 9.7(6) . . . . no
Ni1 O1 C1 C2 -170.7(3) . . . . no
Ni1 O2 C16 C11 1.6(6) . . . . no
Ni1 O2 C16 C15 -176.9(3) . . . . no
Ni2 O5 C21 C26 4.3(5) . . . . no
Ni2 O5 C21 C22 -177.2(3) . . . . no
Ni2 O6 C36 C31 -3.2(5) . . . . no
Ni2 O6 C36 C35 177.4(3) . . . . no
Ni3 O9 C41 C46 -6.4(5) . . . . no
Ni3 O9 C41 C42 175.4(3) . . . . no
Ni3 O10 C56 C51 2.3(5) . . . . no
Ni3 O10 C56 C55 -178.2(2) . . . . no
Ni1 N1 C8 C9 -3.6(4) . . . . no
C7 N1 C8 C17 -4.7(6) . . . . no
Ni1 N1 C8 C17 177.5(3) . . . . no
Ni1 N1 C7 C6 0.0(6) . . . . no
C8 N1 C7 C6 -177.5(4) . . . . no
C7 N1 C8 C9 174.2(4) . . . . no
C10 N2 C9 C8 172.8(4) . . . . no
C10 N2 C9 C20 -7.1(6) . . . . no
C9 N2 C10 C11 -178.8(4) . . . . no
Ni1 N2 C9 C20 177.2(3) . . . . no
Ni1 N2 C10 C11 -3.7(6) . . . . no
Ni1 N2 C9 C8 -2.9(4) . . . . no
C27 N3 C28 C29 176.9(4) . . . . no
C27 N3 C28 C37 -4.0(6) . . . . no
Ni2 N3 C28 C37 177.6(4) . . . . no
Ni2 N3 C27 C26 -1.1(6) . . . . no
C28 N3 C27 C26 -179.3(4) . . . . no
Ni2 N3 C28 C29 -1.6(5) . . . . no
Ni2 N4 C30 C31 1.8(6) . . . . no
C30 N4 C29 C40 4.7(7) . . . . no
C30 N4 C29 C28 -175.9(4) . . . . no
Ni2 N4 C29 C40 -178.0(4) . . . . no
Ni2 N4 C29 C28 1.5(4) . . . . no
C29 N4 C30 C31 178.8(4) . . . . no
C48 N5 C47 C46 176.8(3) . . . . no
C47 N5 C48 C57 5.0(6) . . . . no
C47 N5 C48 C49 -173.4(3) . . . . no
Ni3 N5 C48 C57 179.6(3) . . . . no
Ni3 N5 C47 C46 3.0(6) . . . . no
Ni3 N5 C48 C49 1.3(4) . . . . no
C50 N6 C49 C48 175.4(4) . . . . no
Ni3 N6 C49 C60 -178.0(3) . . . . no
C50 N6 C49 C60 -2.0(6) . . . . no
Ni3 N6 C50 C51 -4.6(6) . . . . no
Ni3 N6 C49 C48 -0.6(4) . . . . no
C49 N6 C50 C51 179.9(4) . . . . no
C2 C1 C6 C7 178.6(4) . . . . no
O1 C1 C2 O3 0.0(7) . . . . no
O1 C1 C2 C3 -179.0(4) . . . . no
C2 C1 C6 C5 -1.4(7) . . . . no
O1 C1 C6 C7 -1.7(7) . . . . no
C6 C1 C2 C3 0.7(7) . . . . no
O1 C1 C6 C5 178.3(4) . . . . no
C6 C1 C2 O3 179.7(4) . . . . no
C1 C2 C3 C4 0.2(8) . . . . no
O3 C2 C3 C4 -178.8(4) . . . . no
C2 C3 C4 C5 -0.5(8) . . . . no
C3 C4 C5 C6 -0.2(7) . . . . no
C4 C5 C6 C1 1.1(7) . . . . no
C4 C5 C6 C7 -178.8(4) . . . . no
C5 C6 C7 N1 176.7(4) . . . . no
C1 C6 C7 N1 -3.3(7) . . . . no
C17 C8 C9 C20 3.1(6) . . . . no
N1 C8 C17 C18 176.8(4) . . . . no
C17 C8 C9 N2 -176.8(3) . . . . no
N1 C8 C9 N2 4.2(5) . . . . no
N1 C8 C9 C20 -175.9(4) . . . . no
C9 C8 C17 C18 -2.1(6) . . . . no
C8 C9 C20 C19 -1.8(6) . . . . no
N2 C9 C20 C19 178.2(4) . . . . no
N2 C10 C11 C12 178.3(4) . . . . no
N2 C10 C11 C16 -0.6(7) . . . . no
C10 C11 C12 C13 -178.8(4) . . . . no
C12 C11 C16 C15 1.3(6) . . . . no
C10 C11 C16 O2 1.7(7) . . . . no
C16 C11 C12 C13 0.2(7) . . . . no
C12 C11 C16 O2 -177.2(4) . . . . no
C10 C11 C16 C15 -179.8(4) . . . . no
C11 C12 C13 C14 -1.4(7) . . . . no
C12 C13 C14 C15 1.2(8) . . . . no
C13 C14 C15 O4 -179.5(4) . . . . no
C13 C14 C15 C16 0.4(7) . . . . no
C14 C15 C16 O2 177.1(4) . . . . no
C14 C15 C16 C11 -1.6(7) . . . . no
O4 C15 C16 O2 -3.0(6) . . . . no
O4 C15 C16 C11 178.3(4) . . . . no
C8 C17 C18 C19 -0.3(7) . . . . no
C17 C18 C19 C20 1.6(7) . . . . no
C18 C19 C20 C9 -0.6(7) . . . . no
O5 C21 C22 O7 -0.2(5) . . . . no
O5 C21 C22 C23 179.7(4) . . . . no
C22 C21 C26 C27 -179.0(4) . . . . no
C22 C21 C26 C25 1.0(6) . . . . no
C26 C21 C22 C23 -1.7(6) . . . . no
O5 C21 C26 C25 179.5(4) . . . . no
C26 C21 C22 O7 178.5(3) . . . . no
O5 C21 C26 C27 -0.4(6) . . . . no
O7 C22 C23 C24 -179.1(4) . . . . no
C21 C22 C23 C24 1.0(6) . . . . no
C22 C23 C24 C25 0.4(6) . . . . no
C23 C24 C25 C26 -1.1(6) . . . . no
C24 C25 C26 C21 0.4(6) . . . . no
C24 C25 C26 C27 -179.7(4) . . . . no
C21 C26 C27 N3 -1.2(7) . . . . no
C25 C26 C27 N3 178.9(4) . . . . no
N3 C28 C29 C40 179.6(4) . . . . no
C37 C28 C29 N4 -179.1(4) . . . . no
N3 C28 C29 N4 0.1(5) . . . . no
C37 C28 C29 C40 0.4(6) . . . . no
N3 C28 C37 C38 179.8(4) . . . . no
C29 C28 C37 C38 -1.1(6) . . . . no
C28 C29 C40 C39 0.5(7) . . . . no
N4 C29 C40 C39 180.0(4) . . . . no
N4 C30 C31 C36 2.3(7) . . . . no
N4 C30 C31 C32 -176.9(4) . . . . no
C30 C31 C32 C33 179.0(4) . . . . no
C32 C31 C36 C35 -3.0(6) . . . . no
C30 C31 C36 O6 -1.5(6) . . . . no
C30 C31 C36 C35 177.8(4) . . . . no
C36 C31 C32 C33 -0.2(6) . . . . no
C32 C31 C36 O6 177.7(4) . . . . no
C31 C32 C33 C34 2.1(7) . . . . no
C32 C33 C34 C35 -0.8(7) . . . . no
C33 C34 C35 O8 176.5(4) . . . . no
C33 C34 C35 C36 -2.6(7) . . . . no
O8 C35 C36 O6 4.8(6) . . . . no
C34 C35 C36 C31 4.4(6) . . . . no
C34 C35 C36 O6 -176.2(4) . . . . no
O8 C35 C36 C31 -174.6(4) . . . . no
C28 C37 C38 C39 0.9(7) . . . . no
C37 C38 C39 C40 0.0(7) . . . . no
C38 C39 C40 C29 -0.7(7) . . . . no
O9 C41 C42 O11 3.5(5) . . . . no
O9 C41 C42 C43 -176.8(4) . . . . no
C46 C41 C42 O11 -174.9(3) . . . . no
C46 C41 C42 C43 4.9(6) . . . . no
O9 C41 C46 C45 178.4(3) . . . . no
O9 C41 C46 C47 -0.9(6) . . . . no
C42 C41 C46 C45 -3.3(5) . . . . no
C42 C41 C46 C47 177.4(3) . . . . no
O11 C42 C43 C44 176.6(4) . . . . no
C41 C42 C43 C44 -3.2(7) . . . . no
C42 C43 C44 C45 -0.2(7) . . . . no
C43 C44 C45 C46 1.8(7) . . . . no
C44 C45 C46 C41 0.1(6) . . . . no
C44 C45 C46 C47 179.4(4) . . . . no
C41 C46 C47 N5 2.7(6) . . . . no
C45 C46 C47 N5 -176.6(4) . . . . no
N5 C48 C49 N6 -0.4(5) . . . . no
N5 C48 C49 C60 177.1(4) . . . . no
C57 C48 C49 N6 -178.8(4) . . . . no
C57 C48 C49 C60 -1.3(6) . . . . no
N5 C48 C57 C58 -177.0(4) . . . . no
C49 C48 C57 C58 1.2(6) . . . . no
N6 C49 C60 C59 177.7(4) . . . . no
C48 C49 C60 C59 0.4(6) . . . . no
N6 C50 C51 C52 -179.4(4) . . . . no
N6 C50 C51 C56 2.8(6) . . . . no
C50 C51 C52 C53 -178.8(4) . . . . no
C56 C51 C52 C53 -1.0(6) . . . . no
C50 C51 C56 O10 -1.5(6) . . . . no
C50 C51 C56 C55 179.0(4) . . . . no
C52 C51 C56 O10 -179.3(4) . . . . no
C52 C51 C56 C55 1.2(5) . . . . no
C51 C52 C53 C54 0.4(7) . . . . no
C52 C53 C54 C55 -0.1(7) . . . . no
C53 C54 C55 O12 -178.4(4) . . . . no
C53 C54 C55 C56 0.3(6) . . . . no
O12 C55 C56 O10 -1.7(5) . . . . no
O12 C55 C56 C51 177.8(3) . . . . no
C54 C55 C56 O10 179.6(4) . . . . no
C54 C55 C56 C51 -0.9(5) . . . . no
C48 C57 C58 C59 -0.3(7) . . . . no
C57 C58 C59 C60 -0.6(7) . . . . no
C58 C59 C60 C49 0.5(7) . . . . 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 Ni2 4.7673(6) . . no
Ni1 O13 3.824(5) . . no
Ni1 N4 3.709(3) . . no
Ni1 C29 3.490(4) . . no
Ni1 C30 3.790(4) . . no
Ni1 C40 3.500(5) . . no
Ni1 C8 3.725(3) . 2_666 no
Ni1 C9 3.481(3) . 2_666 no
Ni1 C10 3.884(4) . 2_666 no
Ni1 Ni1 3.4741(7) . 2_666 no
Ni1 N1 3.659(3) . 2_666 no
Ni1 N2 3.290(3) . 2_666 no
Ni2 C17 3.555(4) . . no
Ni2 N1 3.741(3) . . no
Ni2 C7 3.875(4) . . no
Ni2 C25 3.918(4) . 2_656 no
Ni2 O12 3.408(3) . . no
Ni2 O11 3.750(3) . . no
Ni2 C8 3.593(4) . . no
Ni2 C27 3.638(4) . 2_656 no
Ni2 C26 3.854(4) . 2_656 no
Ni3 C51 3.624(4) . 2_655 no
Ni3 C50 3.874(4) . 2_655 no
Ni3 C53 3.887(4) . 2_655 no
Ni3 O8 3.678(3) . . no
Ni3 O7 3.297(3) . . no
Ni3 C52 3.379(5) . 2_655 no
O1 C20 3.415(5) . 2_666 no
O1 C9 3.393(5) . 2_666 no
O1 O2 2.465(4) . . no
O1 O3 2.719(4) . . no
O1 O13 2.830(5) . . no
O1 N1 2.724(4) . . no
O1 C7 2.895(5) . . no
O2 N2 2.734(4) . . no
O2 O13 2.908(5) . . no
O2 O4 2.680(4) . . no
O2 C10 2.900(5) . . no
O2 C8 3.234(4) . 2_666 no
O3 O13 3.067(5) . . no
O4 O13 3.041(5) . . no
O4 C59 3.338(5) . 1_466 no
O4 C32 3.326(6) . 2_566 no
O5 O6 2.467(4) . . no
O5 N3 2.729(4) . . no
O5 C27 2.900(4) . . no
O5 O7 2.665(4) . . no
O6 O12 2.778(4) . . no
O6 N4 2.746(4) . . no
O6 O11 2.825(4) . . no
O6 C30 2.916(4) . . no
O6 O8 2.734(3) . . no
O7 C38 3.267(5) . 2_656 no
O7 C41 3.271(4) . . no
O7 O9 2.806(3) . . no
O7 C47 3.312(4) . 2_755 no
O7 C57 3.373(6) . 2_755 no
O8 O10 3.148(4) . . no
O8 O9 2.814(4) . . no
O8 C4 3.383(5) . 2_665 no
O8 C41 3.377(5) . . no
O9 C47 2.908(4) . . no
O9 O11 2.730(4) . . no
O9 N5 2.743(4) . . no
O9 O10 2.478(4) . . no
O10 C50 2.890(5) . . no
O10 N6 2.729(4) . . no
O10 O12 2.663(4) . . no
O11 C36 3.346(5) . . no
O12 C25 3.324(5) . 2_656 no
O12 C36 3.130(4) . . no
O12 Ni2 3.408(3) . . no
O13 O13 2.931(7) . 2_566 no
N1 C9 2.357(5) . . no
N1 N2 2.542(4) . . no
N1 C1 2.918(6) . . no
N2 C16 2.912(5) . . no
N2 O2 2.734(4) . . no
N2 C8 2.360(5) . . no
N3 C29 2.356(5) . . no
N3 N4 2.537(5) . . no
N3 C27 3.427(5) . 2_656 no
N3 C26 3.419(6) . 2_656 no
N3 C21 2.908(4) . . no
N4 O6 2.746(4) . . no
N4 C36 2.927(4) . . no
N4 C28 2.364(5) . . no
N5 O9 2.743(4) . . no
N5 C53 3.282(6) . 2_655 no
N5 N6 2.546(5) . . no
N5 C49 2.357(5) . . no
N5 C41 2.924(4) . . no
N6 C48 2.356(5) . . no
N6 C51 3.439(5) . 2_655 no
N6 C56 2.901(5) . . no
C1 C10 3.477(7) . 2_666 no
C1 C32 3.467(7) . . no
C2 C32 3.508(6) . . no
C3 C33 3.546(7) . . no
C3 C52 3.589(7) . 1_565 no
C4 C33 3.417(7) . . no
C5 C12 3.493(7) . 2_666 no
C6 C31 3.386(6) . . no
C6 C32 3.567(6) . . no
C6 C10 3.348(6) . 2_666 no
C6 C11 3.491(6) . 2_666 no
C7 C16 3.507(6) . 2_666 no
C7 C10 3.454(6) . 2_666 no
C7 C11 3.276(6) . 2_666 no
C8 C16 3.574(6) . 2_666 no
C9 C28 3.431(6) . . no
C10 C38 3.312(6) . . no
C10 C6 3.348(6) . 2_666 no
C10 C39 3.525(7) . . no
C10 C37 3.499(6) . . no
C11 C39 3.336(7) . . no
C11 C38 3.461(6) . . no
C16 C39 3.479(6) . . no
C18 C27 3.488(6) . . no
C18 C26 3.351(6) . . no
C19 C27 3.460(7) . . no
C19 C54 3.552(6) . 2_656 no
C20 C53 3.404(6) . 2_656 no
C20 C54 3.538(6) . 2_656 no
C21 C37 3.366(5) . 2_656 no
C21 C28 3.392(5) . 2_656 no
C22 C37 3.351(6) . 2_656 no
C22 C38 3.369(6) . 2_656 no
C23 C40 3.479(6) . 2_656 no
C23 C39 3.480(6) . 2_656 no
C24 C29 3.548(6) . 2_656 no
C24 C40 3.567(6) . 2_656 no
C25 C29 3.542(6) . 2_656 no
C26 C28 3.456(6) . 2_656 no
C34 C60 3.515(6) . 2_655 no
C35 C60 3.492(7) . 2_655 no
C37 C56 3.511(6) . 2_656 no
C42 C57 3.447(7) . 2_755 no
C43 C57 3.435(6) . 2_755 no
C43 C58 3.390(7) . 2_755 no
C44 C57 3.517(6) . 2_755 no
C44 C48 3.542(6) . 2_755 no
C45 C48 3.351(6) . 2_755 no
C45 C57 3.590(6) . 2_755 no
C46 C47 3.477(6) . 2_755 no
C47 C53 3.529(6) . 2_655 no
C47 C46 3.477(6) . 2_755 no
C47 C47 3.237(5) . 2_755 no
C48 C53 3.352(6) . 2_655 no
C48 C54 3.337(6) . 2_655 no
C49 C55 3.415(5) . 2_655 no
C49 C54 3.460(6) . 2_655 no
C50 C56 3.467(5) . 2_655 no
C54 C57 3.526(7) . 2_655 no
C55 C60 3.416(6) . 2_655 no



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 22/09/14 at 12:10:35
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE O   (   3,X'S) H   (   3,X'S) 
RIDE O   (   4,X'S) H   (   4,X'S) 
RIDE O   (   7,X'S) H   (   7,X'S) 
RIDE O   (   8,X'S) H   (   8,X'S) 
RIDE O   (  11,X'S) H   (  11,X'S) 
RIDE O   (  12,X'S) H   (  12,X'S) 
RIDE O   (  13,X'S) H   (  13,X'S) H   (  14,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  17,X'S) H   ( 171,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   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  27,X'S) H   ( 271,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   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 22/09/14 at 12:10:35
#
#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
1 0 0 x .
0 1 1 x .

# start Validation Reply Form
_vrf_PLAT417_ral1406X            
;
PROBLEM: Short Inter D-H..H-D     H4       ..H14       ..       2.09 Ang.  
RESPONSE: There is possibly disordering of the H-bonding 
to/from the water molecule.
;
# end Validation Reply Form

#===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_ral1403SN
_database_code_depnum_ccdc_archive 'CCDC 1838521'
_audit_update_record             
;
2018-04-20 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_audit_creation_date             14-09-05
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1403SN\Tony_ral1403SN_data At 16:53 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   8.1684(1)
_cell_length_b                   20.6438(3)
_cell_length_c                   21.0440(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.3335(14)
_cell_angle_gamma                90
_cell_volume                     3501.60(8)

_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 H44 N4 Ni1 O4 
# Dc =      1.38 Fooo =   1536.00 Mu =     11.96 M =    727.55
# Found Formula = C42 H44 N4 Ni1 O4 
# Dc =      1.38 FOOO =   1536.00 Mu =     11.96 M =    727.55

_chemical_formula_sum            'C42 H44 N4 Ni O4'
_chemical_formula_moiety         'C42 H44 N4 Ni O4'
_chemical_compound_source        ?
_chemical_formula_weight         727.55


_cell_measurement_reflns_used    11492
_cell_measurement_theta_min      4
_cell_measurement_theta_max      72
_cell_measurement_temperature    150

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.049
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_max          0.207

_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    1.196

# Sheldrick geometric approximatio 0.89 0.94 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.94
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2' ####
_diffrn_radiation_source         
'Supernova (Cu) X-ray Source' ################
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_cell_refinement       
;
CrysAlisPro

;
_computing_data_reduction        
;
CrysAlisPro

;
_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            48784
_reflns_number_total             6875
_diffrn_reflns_av_R_equivalents  0.055
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6875 
# Theoretical number of reflections is about 13774 


_diffrn_reflns_theta_min         3.018
_diffrn_reflns_theta_max         72.018
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        72.018
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -10
_reflns_limit_h_max              9
_reflns_limit_k_min              0
_reflns_limit_k_max              25
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   2.14
_oxford_diffrn_Wilson_scale      0.10

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

_refine_diff_density_min         -0.33
_refine_diff_density_max         0.33


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         6875
_refine_ls_number_restraints     0
_refine_ls_number_parameters     460
_oxford_refine_ls_R_factor_ref   0.0428
_refine_ls_wR_factor_ref         0.0906
_refine_ls_goodness_of_fit_ref   0.9847
_refine_ls_shift/su_max          0.0022854
_refine_ls_shift/su_mean         0.0000660


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6875
_refine_ls_R_factor_all          0.0428
_refine_ls_wR_factor_all         0.0906

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5841
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_gt          0.0848

# 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) + ( 0.04P)² + 1.56P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
The largest features in the
final difference electron density map are located 
midway between bonded atoms.
;

# 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 0.74454(3) 0.500133(12) 0.506800(12) 0.0207 1.0000 Uani . . . . . .
O1 O 0.81095(14) 0.48552(5) 0.42833(5) 0.0240 1.0000 Uani . . . . . .
O2 O 0.64894(14) 0.41987(5) 0.49143(5) 0.0245 1.0000 Uani . . . . . .
O3 O 1.04769(16) 0.52776(6) 0.24089(6) 0.0326 1.0000 Uani . . . . . .
O4 O 0.36656(15) 0.22652(6) 0.52801(6) 0.0305 1.0000 Uani . . . . . .
N1 N 0.85238(16) 0.57905(6) 0.52230(6) 0.0214 1.0000 Uani . . . . . .
N2 N 0.66398(16) 0.51574(6) 0.58343(6) 0.0218 1.0000 Uani . . . . . .
N3 N 0.94280(18) 0.40984(7) 0.11312(7) 0.0282 1.0000 Uani . . . . . .
N4 N 0.43875(19) 0.09894(7) 0.41748(7) 0.0301 1.0000 Uani . . . . . .
C1 C 0.88880(19) 0.52568(8) 0.39599(7) 0.0217 1.0000 Uani . . . . . .
C2 C 0.9221(2) 0.50542(8) 0.33535(8) 0.0242 1.0000 Uani . . . . . .
C3 C 1.0055(2) 0.54529(8) 0.29881(8) 0.0262 1.0000 Uani . . . . . .
C4 C 1.0554(2) 0.60813(8) 0.32012(8) 0.0297 1.0000 Uani . . . . . .
C5 C 1.0230(2) 0.62833(8) 0.37869(8) 0.0281 1.0000 Uani . . . . . .
C6 C 0.9421(2) 0.58842(8) 0.41840(8) 0.0237 1.0000 Uani . . . . . .
C7 C 0.9166(2) 0.61196(8) 0.47909(8) 0.0238 1.0000 Uani . . . . . .
C8 C 0.8317(2) 0.60674(7) 0.58178(7) 0.0218 1.0000 Uani . . . . . .
C9 C 0.7108(2) 0.57729(7) 0.61017(7) 0.0221 1.0000 Uani . . . . . .
C10 C 0.59279(19) 0.47172(8) 0.61476(7) 0.0227 1.0000 Uani . . . . . .
C11 C 0.5414(2) 0.40948(8) 0.59093(8) 0.0229 1.0000 Uani . . . . . .
C12 C 0.4564(2) 0.36768(8) 0.62831(8) 0.0260 1.0000 Uani . . . . . .
C13 C 0.4011(2) 0.30790(8) 0.60738(8) 0.0272 1.0000 Uani . . . . . .
C14 C 0.4278(2) 0.28647(8) 0.54613(8) 0.0247 1.0000 Uani . . . . . .
C15 C 0.5105(2) 0.32506(8) 0.50811(8) 0.0243 1.0000 Uani . . . . . .
C16 C 0.57039(19) 0.38695(7) 0.52963(7) 0.0217 1.0000 Uani . . . . . .
C17 C 0.9298(2) 0.65928(8) 0.61373(8) 0.0237 1.0000 Uani . . . . . .
C18 C 1.0870(2) 0.67666(8) 0.59880(8) 0.0269 1.0000 Uani . . . . . .
C19 C 1.1751(2) 0.72753(9) 0.63025(9) 0.0320 1.0000 Uani . . . . . .
C20 C 1.1121(2) 0.76141(9) 0.67813(9) 0.0367 1.0000 Uani . . . . . .
C21 C 0.9658(2) 0.74230(9) 0.69653(9) 0.0324 1.0000 Uani . . . . . .
C22 C 0.8722(2) 0.69025(8) 0.66619(8) 0.0249 1.0000 Uani . . . . . .
C23 C 0.7199(2) 0.66777(8) 0.68694(8) 0.0248 1.0000 Uani . . . . . .
C24 C 0.6491(2) 0.70112(8) 0.73452(8) 0.0296 1.0000 Uani . . . . . .
C25 C 0.5041(2) 0.68103(9) 0.75326(9) 0.0332 1.0000 Uani . . . . . .
C26 C 0.4187(2) 0.62830(8) 0.72241(8) 0.0300 1.0000 Uani . . . . . .
C27 C 0.4826(2) 0.59424(8) 0.67578(8) 0.0263 1.0000 Uani . . . . . .
C28 C 0.6384(2) 0.61120(8) 0.65914(7) 0.0231 1.0000 Uani . . . . . .
C29 C 0.9925(2) 0.46497(8) 0.21759(8) 0.0286 1.0000 Uani . . . . . .
C30 C 1.0525(2) 0.45401(9) 0.15384(9) 0.0340 1.0000 Uani . . . . . .
C31 C 1.0001(3) 0.40207(10) 0.05104(9) 0.0385 1.0000 Uani . . . . . .
C32 C 0.8858(3) 0.35820(10) 0.00576(9) 0.0416 1.0000 Uani . . . . . .
C33 C 0.8722(3) 0.29249(10) 0.03704(10) 0.0396 1.0000 Uani . . . . . .
C34 C 0.8144(3) 0.30187(9) 0.10185(10) 0.0384 1.0000 Uani . . . . . .
C35 C 0.9329(2) 0.34642(9) 0.14408(9) 0.0330 1.0000 Uani . . . . . .
C36 C 0.4029(2) 0.20360(8) 0.46741(9) 0.0309 1.0000 Uani . . . . . .
C37 C 0.3387(2) 0.13488(9) 0.45704(10) 0.0356 1.0000 Uani . . . . . .
C38 C 0.3794(3) 0.03196(9) 0.40883(10) 0.0399 1.0000 Uani . . . . . .
C39 C 0.4915(3) -0.00795(10) 0.37268(11) 0.0465 1.0000 Uani . . . . . .
C40 C 0.5086(3) 0.02302(10) 0.30857(10) 0.0428 1.0000 Uani . . . . . .
C41 C 0.5602(3) 0.09338(10) 0.31864(9) 0.0421 1.0000 Uani . . . . . .
C42 C 0.4405(3) 0.12904(9) 0.35433(9) 0.0378 1.0000 Uani . . . . . .
H21 H 0.8891 0.4637 0.3208 0.0286 1.0000 Uiso R . . . . .
H41 H 1.1116 0.6355 0.2949 0.0360 1.0000 Uiso R . . . . .
H51 H 1.0550 0.6700 0.3923 0.0339 1.0000 Uiso R . . . . .
H71 H 0.9473 0.6549 0.4893 0.0288 1.0000 Uiso R . . . . .
H101 H 0.5772 0.4815 0.6572 0.0263 1.0000 Uiso R . . . . .
H121 H 0.4370 0.3828 0.6688 0.0303 1.0000 Uiso R . . . . .
H131 H 0.3411 0.2810 0.6325 0.0336 1.0000 Uiso R . . . . .
H151 H 0.5293 0.3118 0.4671 0.0280 1.0000 Uiso R . . . . .
H181 H 1.1345 0.6527 0.5694 0.0316 1.0000 Uiso R . . . . .
H191 H 1.2789 0.7381 0.6198 0.0374 1.0000 Uiso R . . . . .
H201 H 1.1700 0.7965 0.6984 0.0436 1.0000 Uiso R . . . . .
H211 H 0.9284 0.7645 0.7314 0.0390 1.0000 Uiso R . . . . .
H241 H 0.7020 0.7383 0.7533 0.0347 1.0000 Uiso R . . . . .
H251 H 0.4608 0.7032 0.7861 0.0405 1.0000 Uiso R . . . . .
H261 H 0.3125 0.6169 0.7328 0.0358 1.0000 Uiso R . . . . .
H271 H 0.4206 0.5610 0.6537 0.0318 1.0000 Uiso R . . . . .
H291 H 1.0347 0.4323 0.2490 0.0338 1.0000 Uiso R . . . . .
H292 H 0.8707 0.4642 0.2108 0.0330 1.0000 Uiso R . . . . .
H301 H 1.0501 0.4957 0.1321 0.0401 1.0000 Uiso R . . . . .
H302 H 1.1671 0.4375 0.1617 0.0411 1.0000 Uiso R . . . . .
H311 H 1.0045 0.4453 0.0325 0.0457 1.0000 Uiso R . . . . .
H312 H 1.1148 0.3826 0.0585 0.0457 1.0000 Uiso R . . . . .
H321 H 0.9299 0.3535 -0.0345 0.0516 1.0000 Uiso R . . . . .
H322 H 0.7767 0.3789 -0.0038 0.0495 1.0000 Uiso R . . . . .
H331 H 0.9822 0.2724 0.0438 0.0477 1.0000 Uiso R . . . . .
H332 H 0.7956 0.2638 0.0084 0.0488 1.0000 Uiso R . . . . .
H341 H 0.7040 0.3228 0.0946 0.0453 1.0000 Uiso R . . . . .
H342 H 0.8069 0.2593 0.1246 0.0467 1.0000 Uiso R . . . . .
H351 H 1.0461 0.3263 0.1523 0.0393 1.0000 Uiso R . . . . .
H352 H 0.8927 0.3528 0.1851 0.0399 1.0000 Uiso R . . . . .
H361 H 0.5251 0.2034 0.4689 0.0356 1.0000 Uiso R . . . . .
H362 H 0.3497 0.2318 0.4326 0.0367 1.0000 Uiso R . . . . .
H371 H 0.3488 0.1134 0.4986 0.0433 1.0000 Uiso R . . . . .
H372 H 0.2204 0.1356 0.4368 0.0434 1.0000 Uiso R . . . . .
H381 H 0.3803 0.0132 0.4521 0.0474 1.0000 Uiso R . . . . .
H382 H 0.2624 0.0320 0.3848 0.0478 1.0000 Uiso R . . . . .
H391 H 0.6015 -0.0098 0.3996 0.0552 1.0000 Uiso R . . . . .
H392 H 0.4468 -0.0524 0.3663 0.0562 1.0000 Uiso R . . . . .
H401 H 0.5896 -0.0011 0.2878 0.0518 1.0000 Uiso R . . . . .
H402 H 0.4013 0.0217 0.2799 0.0500 1.0000 Uiso R . . . . .
H411 H 0.6730 0.0952 0.3443 0.0504 1.0000 Uiso R . . . . .
H412 H 0.5625 0.1149 0.2766 0.0507 1.0000 Uiso R . . . . .
H421 H 0.4755 0.1733 0.3608 0.0455 1.0000 Uiso R . . . . .
H422 H 0.3259 0.1297 0.3292 0.0445 1.0000 Uiso R . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.41(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 . 1.8447(11) yes
Ni1 . O2 . 1.8378(11) yes
Ni1 . N1 . 1.8557(13) yes
Ni1 . N2 . 1.8659(13) yes
O1 . C1 . 1.3019(19) yes
O2 . C16 . 1.2989(19) yes
O3 . C3 . 1.3678(19) yes
O3 . C29 . 1.432(2) yes
O4 . C14 . 1.3659(19) yes
O4 . C36 . 1.435(2) yes
N1 . C7 . 1.311(2) yes
N1 . C8 . 1.4109(19) yes
N2 . C9 . 1.4168(19) yes
N2 . C10 . 1.313(2) yes
N3 . C30 . 1.456(2) yes
N3 . C31 . 1.466(2) yes
N3 . C35 . 1.470(2) yes
N4 . C37 . 1.460(2) yes
N4 . C38 . 1.467(2) yes
N4 . C42 . 1.469(2) yes
C1 . C2 . 1.411(2) yes
C1 . C6 . 1.423(2) yes
C2 . C3 . 1.379(2) yes
C2 . H21 . 0.940 no
C3 . C4 . 1.411(2) yes
C4 . C5 . 1.367(2) yes
C4 . H41 . 0.943 no
C5 . C6 . 1.411(2) yes
C5 . H51 . 0.932 no
C6 . C7 . 1.413(2) yes
C7 . H71 . 0.936 no
C8 . C9 . 1.376(2) yes
C8 . C17 . 1.447(2) yes
C9 . C28 . 1.449(2) yes
C10 . C11 . 1.418(2) yes
C10 . H101 . 0.944 no
C11 . C12 . 1.422(2) yes
C11 . C16 . 1.427(2) yes
C12 . C13 . 1.363(2) yes
C12 . H121 . 0.945 no
C13 . C14 . 1.413(2) yes
C13 . H131 . 0.955 no
C14 . C15 . 1.381(2) yes
C15 . C16 . 1.416(2) yes
C15 . H151 . 0.942 no
C17 . C18 . 1.417(2) yes
C17 . C22 . 1.420(2) yes
C18 . C19 . 1.380(2) yes
C18 . H181 . 0.925 no
C19 . C20 . 1.392(3) yes
C19 . H191 . 0.936 no
C20 . C21 . 1.373(3) yes
C20 . H201 . 0.930 no
C21 . C22 . 1.410(2) yes
C21 . H211 . 0.956 no
C22 . C23 . 1.459(2) yes
C23 . C24 . 1.414(2) yes
C23 . C28 . 1.423(2) yes
C24 . C25 . 1.372(3) yes
C24 . H241 . 0.936 no
C25 . C26 . 1.395(2) yes
C25 . H251 . 0.944 no
C26 . C27 . 1.377(2) yes
C26 . H261 . 0.958 no
C27 . C28 . 1.417(2) yes
C27 . H271 . 0.931 no
C29 . C30 . 1.518(2) yes
C29 . H291 . 0.967 no
C29 . H292 . 0.982 no
C30 . H301 . 0.973 no
C30 . H302 . 0.985 no
C31 . C32 . 1.520(3) yes
C31 . H311 . 0.978 no
C31 . H312 . 1.008 no
C32 . C33 . 1.520(3) yes
C32 . H321 . 0.977 no
C32 . H322 . 0.980 no
C33 . C34 . 1.526(3) yes
C33 . H331 . 0.979 no
C33 . H332 . 0.992 no
C34 . C35 . 1.515(3) yes
C34 . H341 . 0.989 no
C34 . H342 . 1.008 no
C35 . H351 . 1.003 no
C35 . H352 . 0.982 no
C36 . C37 . 1.516(2) yes
C36 . H361 . 0.994 no
C36 . H362 . 0.980 no
C37 . H371 . 0.972 no
C37 . H372 . 0.990 no
C38 . C39 . 1.524(3) yes
C38 . H381 . 0.988 no
C38 . H382 . 1.006 no
C39 . C40 . 1.520(3) yes
C39 . H391 . 0.983 no
C39 . H392 . 0.988 no
C40 . C41 . 1.518(3) yes
C40 . H401 . 0.986 no
C40 . H402 . 0.980 no
C41 . C42 . 1.517(3) yes
C41 . H411 . 0.990 no
C41 . H412 . 0.994 no
C42 . H421 . 0.960 no
C42 . H422 . 0.998 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(5) yes
O1 . Ni1 . N1 . 95.78(5) yes
O2 . Ni1 . N1 . 176.84(5) yes
O1 . Ni1 . N2 . 176.43(5) yes
O2 . Ni1 . N2 . 96.22(5) yes
N1 . Ni1 . N2 . 85.43(6) yes
Ni1 . O1 . C1 . 127.11(10) yes
Ni1 . O2 . C16 . 126.97(10) yes
C3 . O3 . C29 . 115.70(13) yes
C14 . O4 . C36 . 115.31(13) yes
Ni1 . N1 . C7 . 124.40(11) yes
Ni1 . N1 . C8 . 112.95(10) yes
C7 . N1 . C8 . 121.63(14) yes
Ni1 . N2 . C9 . 112.82(10) yes
Ni1 . N2 . C10 . 124.17(11) yes
C9 . N2 . C10 . 122.30(14) yes
C30 . N3 . C31 . 109.77(14) yes
C30 . N3 . C35 . 111.68(15) yes
C31 . N3 . C35 . 110.24(14) yes
C37 . N4 . C38 . 110.21(14) yes
C37 . N4 . C42 . 112.91(15) yes
C38 . N4 . C42 . 109.75(15) yes
O1 . C1 . C2 . 117.80(14) yes
O1 . C1 . C6 . 123.76(14) yes
C2 . C1 . C6 . 118.44(14) yes
C1 . C2 . C3 . 120.84(15) yes
C1 . C2 . H21 . 118.6 no
C3 . C2 . H21 . 120.5 no
C2 . C3 . O3 . 123.87(15) yes
C2 . C3 . C4 . 120.97(15) yes
O3 . C3 . C4 . 115.16(14) yes
C3 . C4 . C5 . 118.61(15) yes
C3 . C4 . H41 . 120.8 no
C5 . C4 . H41 . 120.5 no
C4 . C5 . C6 . 122.24(16) yes
C4 . C5 . H51 . 118.3 no
C6 . C5 . H51 . 119.5 no
C1 . C6 . C5 . 118.86(15) yes
C1 . C6 . C7 . 122.04(15) yes
C5 . C6 . C7 . 119.10(15) yes
C6 . C7 . N1 . 125.68(15) yes
C6 . C7 . H71 . 117.4 no
N1 . C7 . H71 . 116.9 no
N1 . C8 . C9 . 113.81(14) yes
N1 . C8 . C17 . 125.36(14) yes
C9 . C8 . C17 . 120.77(14) yes
N2 . C9 . C8 . 112.98(14) yes
N2 . C9 . C28 . 126.92(14) yes
C8 . C9 . C28 . 119.99(14) yes
N2 . C10 . C11 . 125.42(15) yes
N2 . C10 . H101 . 117.8 no
C11 . C10 . H101 . 116.8 no
C10 . C11 . C12 . 119.82(14) yes
C10 . C11 . C16 . 122.16(14) yes
C12 . C11 . C16 . 118.01(14) yes
C11 . C12 . C13 . 122.47(15) yes
C11 . C12 . H121 . 117.8 no
C13 . C12 . H121 . 119.7 no
C12 . C13 . C14 . 119.10(15) yes
C12 . C13 . H131 . 121.4 no
C14 . C13 . H131 . 119.5 no
C13 . C14 . O4 . 115.76(14) yes
C13 . C14 . C15 . 120.69(15) yes
O4 . C14 . C15 . 123.55(15) yes
C14 . C15 . C16 . 120.76(15) yes
C14 . C15 . H151 . 122.1 no
C16 . C15 . H151 . 117.2 no
C11 . C16 . C15 . 118.95(14) yes
C11 . C16 . O2 . 124.05(14) yes
C15 . C16 . O2 . 117.00(14) yes
C8 . C17 . C18 . 122.68(15) yes
C8 . C17 . C22 . 118.05(15) yes
C18 . C17 . C22 . 119.00(15) yes
C17 . C18 . C19 . 120.46(16) yes
C17 . C18 . H181 . 120.4 no
C19 . C18 . H181 . 119.1 no
C18 . C19 . C20 . 120.31(17) yes
C18 . C19 . H191 . 119.1 no
C20 . C19 . H191 . 120.6 no
C19 . C20 . C21 . 120.05(16) yes
C19 . C20 . H201 . 120.2 no
C21 . C20 . H201 . 119.7 no
C20 . C21 . C22 . 121.62(16) yes
C20 . C21 . H211 . 118.7 no
C22 . C21 . H211 . 119.7 no
C17 . C22 . C21 . 118.11(15) yes
C17 . C22 . C23 . 119.70(14) yes
C21 . C22 . C23 . 122.19(15) yes
C22 . C23 . C24 . 121.59(15) yes
C22 . C23 . C28 . 120.21(14) yes
C24 . C23 . C28 . 118.20(15) yes
C23 . C24 . C25 . 121.88(16) yes
C23 . C24 . H241 . 119.0 no
C25 . C24 . H241 . 119.2 no
C24 . C25 . C26 . 119.46(16) yes
C24 . C25 . H251 . 120.5 no
C26 . C25 . H251 . 120.0 no
C25 . C26 . C27 . 120.75(16) yes
C25 . C26 . H261 . 119.2 no
C27 . C26 . H261 . 120.0 no
C26 . C27 . C28 . 120.62(15) yes
C26 . C27 . H271 . 119.6 no
C28 . C27 . H271 . 119.8 no
C9 . C28 . C23 . 118.10(14) yes
C9 . C28 . C27 . 122.87(15) yes
C23 . C28 . C27 . 118.73(14) yes
O3 . C29 . C30 . 107.98(13) yes
O3 . C29 . H291 . 109.8 no
C30 . C29 . H291 . 111.7 no
O3 . C29 . H292 . 108.6 no
C30 . C29 . H292 . 109.5 no
H291 . C29 . H292 . 109.2 no
C29 . C30 . N3 . 110.96(14) yes
C29 . C30 . H301 . 107.4 no
N3 . C30 . H301 . 108.3 no
C29 . C30 . H302 . 109.7 no
N3 . C30 . H302 . 111.1 no
H301 . C30 . H302 . 109.3 no
N3 . C31 . C32 . 111.82(16) yes
N3 . C31 . H311 . 107.0 no
C32 . C31 . H311 . 110.7 no
N3 . C31 . H312 . 109.1 no
C32 . C31 . H312 . 108.7 no
H311 . C31 . H312 . 109.4 no
C31 . C32 . C33 . 109.93(17) yes
C31 . C32 . H321 . 109.1 no
C33 . C32 . H321 . 110.5 no
C31 . C32 . H322 . 108.3 no
C33 . C32 . H322 . 110.6 no
H321 . C32 . H322 . 108.4 no
C32 . C33 . C34 . 109.20(15) yes
C32 . C33 . H331 . 108.1 no
C34 . C33 . H331 . 109.5 no
C32 . C33 . H332 . 110.7 no
C34 . C33 . H332 . 111.3 no
H331 . C33 . H332 . 108.0 no
C33 . C34 . C35 . 109.89(16) yes
C33 . C34 . H341 . 108.9 no
C35 . C34 . H341 . 107.8 no
C33 . C34 . H342 . 111.5 no
C35 . C34 . H342 . 109.4 no
H341 . C34 . H342 . 109.3 no
C34 . C35 . N3 . 110.87(15) yes
C34 . C35 . H351 . 109.5 no
N3 . C35 . H351 . 109.3 no
C34 . C35 . H352 . 108.9 no
N3 . C35 . H352 . 108.7 no
H351 . C35 . H352 . 109.6 no
O4 . C36 . C37 . 108.65(14) yes
O4 . C36 . H361 . 108.9 no
C37 . C36 . H361 . 108.9 no
O4 . C36 . H362 . 109.7 no
C37 . C36 . H362 . 110.4 no
H361 . C36 . H362 . 110.3 no
C36 . C37 . N4 . 110.18(14) yes
C36 . C37 . H371 . 108.7 no
N4 . C37 . H371 . 107.9 no
C36 . C37 . H372 . 109.7 no
N4 . C37 . H372 . 111.1 no
H371 . C37 . H372 . 109.2 no
N4 . C38 . C39 . 111.00(16) yes
N4 . C38 . H381 . 107.6 no
C39 . C38 . H381 . 109.4 no
N4 . C38 . H382 . 109.2 no
C39 . C38 . H382 . 110.4 no
H381 . C38 . H382 . 109.1 no
C38 . C39 . C40 . 111.41(18) yes
C38 . C39 . H391 . 107.5 no
C40 . C39 . H391 . 108.7 no
C38 . C39 . H392 . 109.3 no
C40 . C39 . H392 . 110.8 no
H391 . C39 . H392 . 109.0 no
C39 . C40 . C41 . 110.00(16) yes
C39 . C40 . H401 . 110.3 no
C41 . C40 . H401 . 110.8 no
C39 . C40 . H402 . 109.4 no
C41 . C40 . H402 . 108.3 no
H401 . C40 . H402 . 108.0 no
C40 . C41 . C42 . 110.30(16) yes
C40 . C41 . H411 . 108.9 no
C42 . C41 . H411 . 109.3 no
C40 . C41 . H412 . 110.4 no
C42 . C41 . H412 . 109.3 no
H411 . C41 . H412 . 108.6 no
C41 . C42 . N4 . 110.13(16) yes
C41 . C42 . H421 . 109.3 no
N4 . C42 . H421 . 108.7 no
C41 . C42 . H422 . 111.6 no
N4 . C42 . H422 . 109.9 no
H421 . C42 . H422 . 107.1 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 175.00(13) . . . . no
N1 Ni1 O1 C1 -7.81(13) . . . . no
O1 Ni1 O2 C16 176.52(13) . . . . no
N2 Ni1 O2 C16 -6.91(13) . . . . no
O1 Ni1 N1 C7 12.28(14) . . . . no
O1 Ni1 N1 C8 -179.13(10) . . . . no
N2 Ni1 N1 C7 -164.34(14) . . . . no
N2 Ni1 N1 C8 4.25(11) . . . . no
O2 Ni1 N2 C9 -178.31(10) . . . . no
O2 Ni1 N2 C10 11.21(13) . . . . no
N1 Ni1 N2 C9 4.40(11) . . . . no
N1 Ni1 N2 C10 -166.09(13) . . . . no
Ni1 O1 C1 C2 -177.50(11) . . . . no
Ni1 O1 C1 C6 2.7(2) . . . . no
Ni1 O2 C16 C11 1.7(2) . . . . no
Ni1 O2 C16 C15 -178.43(11) . . . . no
C29 O3 C3 C2 2.9(2) . . . . no
C29 O3 C3 C4 -177.82(14) . . . . no
C3 O3 C29 C30 -179.30(14) . . . . no
C36 O4 C14 C13 -176.45(14) . . . . no
C36 O4 C14 C15 3.8(2) . . . . no
C14 O4 C36 C37 175.54(14) . . . . no
Ni1 N1 C7 C6 -12.4(2) . . . . no
C8 N1 C7 C6 179.98(16) . . . . no
Ni1 N1 C8 C9 -12.40(17) . . . . no
Ni1 N1 C8 C17 164.88(13) . . . . no
C7 N1 C8 C9 156.54(15) . . . . no
C7 N1 C8 C17 -26.2(2) . . . . no
Ni1 N2 C9 C8 -12.39(16) . . . . no
Ni1 N2 C9 C28 163.62(13) . . . . no
C10 N2 C9 C8 158.30(15) . . . . no
C10 N2 C9 C28 -25.7(2) . . . . no
Ni1 N2 C10 C11 -11.0(2) . . . . no
C9 N2 C10 C11 179.44(15) . . . . no
C31 N3 C30 C29 177.88(15) . . . . no
C35 N3 C30 C29 -59.55(18) . . . . no
C30 N3 C31 C32 -177.93(16) . . . . no
C35 N3 C31 C32 58.6(2) . . . . no
C30 N3 C35 C34 178.33(15) . . . . no
C31 N3 C35 C34 -59.4(2) . . . . no
C38 N4 C37 C36 178.53(15) . . . . no
C42 N4 C37 C36 -58.3(2) . . . . no
C37 N4 C38 C39 -175.01(16) . . . . no
C42 N4 C38 C39 60.0(2) . . . . no
C37 N4 C42 C41 174.17(16) . . . . no
C38 N4 C42 C41 -62.5(2) . . . . no
O1 C1 C2 C3 -179.38(15) . . . . no
C6 C1 C2 C3 0.5(2) . . . . no
O1 C1 C6 C5 -178.90(15) . . . . no
O1 C1 C6 C7 1.1(3) . . . . no
C2 C1 C6 C5 1.3(2) . . . . no
C2 C1 C6 C7 -178.74(15) . . . . no
C1 C2 C3 O3 177.27(15) . . . . no
C1 C2 C3 C4 -1.9(3) . . . . no
O3 C3 C4 C5 -177.69(15) . . . . no
C2 C3 C4 C5 1.6(2) . . . . no
C3 C4 C5 C6 0.2(2) . . . . no
C4 C5 C6 C1 -1.6(2) . . . . no
C4 C5 C6 C7 178.37(16) . . . . no
C1 C6 C7 N1 4.2(3) . . . . no
C5 C6 C7 N1 -175.79(16) . . . . no
N1 C8 C9 N2 15.95(19) . . . . no
N1 C8 C9 C28 -160.36(14) . . . . no
C17 C8 C9 N2 -161.47(14) . . . . no
C17 C8 C9 C28 22.2(2) . . . . no
N1 C8 C17 C18 -18.8(2) . . . . no
N1 C8 C17 C22 167.34(15) . . . . no
C9 C8 C17 C18 158.34(16) . . . . no
C9 C8 C17 C22 -15.6(2) . . . . no
N2 C9 C28 C23 170.15(15) . . . . no
N2 C9 C28 C27 -16.2(2) . . . . no
C8 C9 C28 C23 -14.1(2) . . . . no
C8 C9 C28 C27 159.52(16) . . . . no
N2 C10 C11 C12 -176.18(15) . . . . no
N2 C10 C11 C16 3.1(3) . . . . no
C10 C11 C12 C13 178.64(16) . . . . no
C16 C11 C12 C13 -0.7(2) . . . . no
C10 C11 C16 O2 2.0(3) . . . . no
C10 C11 C16 C15 -177.89(15) . . . . no
C12 C11 C16 O2 -178.74(15) . . . . no
C12 C11 C16 C15 1.4(2) . . . . no
C11 C12 C13 C14 -0.4(3) . . . . no
C12 C13 C14 O4 -178.97(15) . . . . no
C12 C13 C14 C15 0.8(2) . . . . no
O4 C14 C15 C16 179.72(15) . . . . no
C13 C14 C15 C16 0.0(3) . . . . no
C14 C15 C16 O2 179.04(15) . . . . no
C14 C15 C16 C11 -1.1(2) . . . . no
C8 C17 C18 C19 179.43(16) . . . . no
C22 C17 C18 C19 -6.7(2) . . . . no
C8 C17 C22 C21 -178.73(15) . . . . no
C8 C17 C22 C23 1.2(2) . . . . no
C18 C17 C22 C21 7.2(2) . . . . no
C18 C17 C22 C23 -172.92(15) . . . . no
C17 C18 C19 C20 1.5(3) . . . . no
C18 C19 C20 C21 3.3(3) . . . . no
C19 C20 C21 C22 -2.7(3) . . . . no
C20 C21 C22 C17 -2.6(3) . . . . no
C20 C21 C22 C23 177.51(17) . . . . no
C17 C22 C23 C24 -173.55(16) . . . . no
C17 C22 C23 C28 6.2(2) . . . . no
C21 C22 C23 C24 6.4(3) . . . . no
C21 C22 C23 C28 -173.83(16) . . . . no
C22 C23 C24 C25 178.59(16) . . . . no
C28 C23 C24 C25 -1.2(2) . . . . no
C22 C23 C28 C9 -0.1(2) . . . . no
C22 C23 C28 C27 -173.97(15) . . . . no
C24 C23 C28 C9 179.71(14) . . . . no
C24 C23 C28 C27 5.8(2) . . . . no
C23 C24 C25 C26 -3.4(3) . . . . no
C24 C25 C26 C27 3.4(3) . . . . no
C25 C26 C27 C28 1.4(3) . . . . no
C26 C27 C28 C9 -179.57(15) . . . . no
C26 C27 C28 C23 -6.0(2) . . . . no
O3 C29 C30 N3 -152.41(14) . . . . no
N3 C31 C32 C33 -57.3(2) . . . . no
C31 C32 C33 C34 55.7(3) . . . . no
C32 C33 C34 C35 -56.9(2) . . . . no
C33 C34 C35 N3 59.1(2) . . . . no
O4 C36 C37 N4 -151.17(14) . . . . no
N4 C38 C39 C40 -55.4(2) . . . . no
C38 C39 C40 C41 52.2(3) . . . . no
C39 C40 C41 C42 -54.4(2) . . . . no
C40 C41 C42 N4 59.9(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 Ni1 3.9587(4) . 2_666 no
Ni1 Ni1 4.2293(4) . 2_766 no
Ni1 O1 3.6779(12) . 2_766 no
Ni1 O2 3.6191(12) . 2_666 no
Ni1 N1 3.8134(13) . 2_766 no
Ni1 N2 3.5767(13) . 2_666 no
Ni1 C1 3.3840(16) . 2_766 no
Ni1 C2 3.9406(17) . 2_766 no
Ni1 C5 3.8680(17) . 2_766 no
Ni1 C6 3.3263(17) . 2_766 no
Ni1 C7 3.5830(17) . 2_766 no
Ni1 C10 3.4911(15) . 2_666 no
Ni1 C11 3.4072(17) . 2_666 no
Ni1 C16 3.4640(15) . 2_666 no
O1 O2 2.4334(15) . . no
O1 N1 2.7452(16) . . no
O1 C7 2.898(2) . . no
O1 N1 3.0810(17) . 2_766 no
O1 C7 3.375(2) . 2_766 no
O1 C10 3.3923(19) . 2_666 no
O1 C27 3.400(2) . 2_666 no
O2 C9 3.3424(19) . 2_666 no
O2 C10 2.9117(18) . . no
O2 N2 2.7574(16) . . no
O2 N2 3.0783(17) . 2_666 no
N1 N2 2.5246(18) . . no
N1 C1 2.9367(19) . . no
N1 C9 2.335(2) . . no
N1 C1 3.305(2) . 2_766 no
N2 C16 2.9418(19) . . no
N2 C8 2.329(2) . . no
N2 C16 3.4473(19) . 2_666 no
C1 C8 3.544(2) . 2_766 no
C1 C12 3.548(2) . 2_666 no
C2 C8 3.363(2) . 2_766 no
C2 C9 3.479(2) . 2_766 no
C3 C10 3.502(2) . 2_766 no
C4 C11 3.533(2) . 2_766 no
C4 C10 3.402(2) . 2_766 no
C5 C11 3.597(2) . 2_766 no
C5 C16 3.574(2) . 2_766 no
C6 C13 3.499(2) . 2_666 no
C6 C12 3.368(2) . 2_666 no
C7 C18 2.988(2) . . no
C7 C12 3.512(2) . 2_666 no
C7 C13 3.354(2) . 2_666 no
C7 C14 3.480(2) . 2_666 no
C8 C15 3.415(2) . 2_666 no
C9 C16 3.505(2) . 2_666 no
C9 C15 3.474(2) . 2_666 no
C10 C27 3.038(2) . . no
C18 C26 3.580(2) . 1_655 no
C19 C25 3.548(3) . 1_655 no
C19 C26 3.266(2) . 1_655 no



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 05/09/14 at 17:20:58
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 05/09/14 at 17:20:58
#
#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_ral1405X
_database_code_depnum_ccdc_archive 'CCDC 1838523'
_audit_update_record             
;
2018-04-20 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_audit_creation_date             14-09-19
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1405X\Tony_ral1405X_data\r At 11:26 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   10.1567(3)
_cell_length_b                   8.5596(4)
_cell_length_c                   33.2575(13)
_cell_angle_alpha                90
_cell_angle_beta                 98.602(3)
_cell_angle_gamma                90
_cell_volume                     2858.79(19)

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


_cell_formula_units_Z            4

# Given Formula = C30 H40 N4 Ni1 O5 
# Dc =      1.38 Fooo =   1272.00 Mu =      7.25 M =    595.38
# Found Formula = C30 H42 N4 Ni1 O5 
# Dc =      1.39 FOOO =   1272.00 Mu =      7.25 M =    597.40

_chemical_formula_sum            'C30 H42 N4 Ni O5'
_chemical_formula_moiety         'C30 H40 N4 Ni O4, H2 O'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         597.40


_cell_measurement_reflns_used    8919
_cell_measurement_theta_min      2
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            brown-green
_exptl_crystal_size_min          0.039
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_max          0.325

_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    0.725

# Sheldrick geometric approximatio 0.83 0.97 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  0.97
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33d (release 23-04-2014 CrysAlis171 .NET)
(compiled Apr 23 2014,17:37:27)
;
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2014)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2014)'
_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            41210
_reflns_number_total             8148
_diffrn_reflns_av_R_equivalents  0.087
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8148 
# Theoretical number of reflections is about 17998 


_diffrn_reflns_theta_min         2.030
_diffrn_reflns_theta_max         30.855
_diffrn_measured_fraction_theta_max 0.905

_diffrn_reflns_theta_full        28.052
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       46
_reflns_limit_h_min              -14
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              46

_oxford_diffrn_Wilson_B_factor   1.09
_oxford_diffrn_Wilson_scale      0.74

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

_refine_diff_density_min         -1.28
_refine_diff_density_max         1.34


# 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         8148
_refine_ls_number_restraints     0
_refine_ls_number_parameters     362
_oxford_refine_ls_R_factor_ref   0.1120
_refine_ls_wR_factor_ref         0.1063
_refine_ls_goodness_of_fit_ref   1.0196
_refine_ls_shift/su_max          0.0006288
_refine_ls_shift/su_mean         0.0000317


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8148
_refine_ls_R_factor_all          0.1120
_refine_ls_wR_factor_all         0.1063

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5248
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_gt          0.0840

# 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) + ( 0.02P)² + 2.23P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
;
The largest features in the
final difference electron density map are located 
randomly through the structure.
;

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

# Replace last . with number of unfound hydrogen 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 0.43024(3) 0.33410(4) 0.502661(11) 0.0167 1.0000 Uani . . . . . .
O1 O 0.58281(17) 0.2342(2) 0.52886(5) 0.0177 1.0000 Uani . . . . . .
O2 O 0.41388(17) 0.4201(2) 0.55342(6) 0.0192 1.0000 Uani . . . . . .
O3 O 0.80956(17) 0.1519(2) 0.57381(6) 0.0228 1.0000 Uani . . . . . .
O4 O 0.42740(18) 0.5103(2) 0.62930(6) 0.0249 1.0000 Uani . . . . . .
O5 O 0.5761(2) 0.2070(3) 0.62037(7) 0.0434 1.0000 Uani . . . . . .
N1 N 0.4356(2) 0.2378(3) 0.45296(7) 0.0178 1.0000 Uani . . . . . .
N2 N 0.2877(2) 0.4455(3) 0.47525(7) 0.0191 1.0000 Uani . . . . . .
N3 N 1.0743(2) 0.1482(3) 0.66237(7) 0.0234 1.0000 Uani . . . . . .
N4 N 0.6749(2) 0.6297(3) 0.68264(7) 0.0238 1.0000 Uani . . . . . .
C1 C 0.6571(2) 0.1341(3) 0.51276(8) 0.0172 1.0000 Uani . . . . . .
C2 C 0.7784(3) 0.0805(3) 0.53629(8) 0.0181 1.0000 Uani . . . . . .
C3 C 0.8550(3) -0.0329(3) 0.52176(9) 0.0216 1.0000 Uani . . . . . .
C4 C 0.8170(3) -0.0988(3) 0.48294(9) 0.0223 1.0000 Uani . . . . . .
C5 C 0.7054(3) -0.0454(3) 0.45901(9) 0.0217 1.0000 Uani . . . . . .
C6 C 0.6270(3) 0.0724(3) 0.47306(8) 0.0182 1.0000 Uani . . . . . .
C7 C 0.5162(3) 0.1295(3) 0.44530(9) 0.0201 1.0000 Uani . . . . . .
C8 C 0.3268(3) 0.2830(3) 0.42034(9) 0.0218 1.0000 Uani . . . . . .
C9 C 0.2824(3) 0.4429(3) 0.43101(8) 0.0220 1.0000 Uani . . . . . .
C10 C 0.2032(3) 0.5285(3) 0.49095(9) 0.0203 1.0000 Uani . . . . . .
C11 C 0.2054(3) 0.5557(3) 0.53356(9) 0.0200 1.0000 Uani . . . . . .
C12 C 0.1015(3) 0.6447(4) 0.54585(9) 0.0247 1.0000 Uani . . . . . .
C13 C 0.1035(3) 0.6834(4) 0.58548(10) 0.0281 1.0000 Uani . . . . . .
C14 C 0.2113(3) 0.6381(3) 0.61464(9) 0.0252 1.0000 Uani . . . . . .
C15 C 0.3151(3) 0.5543(3) 0.60321(9) 0.0205 1.0000 Uani . . . . . .
C16 C 0.3147(2) 0.5048(3) 0.56208(9) 0.0182 1.0000 Uani . . . . . .
C17 C 0.9323(3) 0.1031(4) 0.59759(9) 0.0247 1.0000 Uani . . . . . .
C18 C 0.9635(3) 0.2112(4) 0.63354(9) 0.0274 1.0000 Uani . . . . . .
C19 C 1.1999(3) 0.1450(4) 0.64589(10) 0.0360 1.0000 Uani . . . . . .
C20 C 1.3076(3) 0.0632(5) 0.67521(11) 0.0451 1.0000 Uani . . . . . .
C21 C 1.3276(3) 0.1419(4) 0.71650(10) 0.0419 1.0000 Uani . . . . . .
C22 C 1.1952(3) 0.1564(5) 0.73215(10) 0.0437 1.0000 Uani . . . . . .
C23 C 1.0911(3) 0.2343(4) 0.70074(10) 0.0394 1.0000 Uani . . . . . .
C24 C 0.4358(3) 0.5628(4) 0.67050(9) 0.0267 1.0000 Uani . . . . . .
C25 C 0.5719(3) 0.5225(4) 0.69266(9) 0.0262 1.0000 Uani . . . . . .
C26 C 0.8067(3) 0.5574(4) 0.69108(10) 0.0287 1.0000 Uani . . . . . .
C27 C 0.9118(3) 0.6638(4) 0.67834(10) 0.0351 1.0000 Uani . . . . . .
C28 C 0.9130(3) 0.8221(4) 0.69891(10) 0.0373 1.0000 Uani . . . . . .
C29 C 0.7737(3) 0.8924(4) 0.69213(10) 0.0370 1.0000 Uani . . . . . .
C30 C 0.6732(3) 0.7774(4) 0.70471(10) 0.0320 1.0000 Uani . . . . . .
H31 H 0.9333 -0.0651 0.5378 0.0259 1.0000 Uiso R . . . . .
H41 H 0.8686 -0.1789 0.4740 0.0264 1.0000 Uiso R . . . . .
H51 H 0.6793 -0.0873 0.4329 0.0257 1.0000 Uiso R . . . . .
H71 H 0.5025 0.0828 0.4190 0.0231 1.0000 Uiso R . . . . .
H81 H 0.2542 0.2094 0.4196 0.0253 1.0000 Uiso R . . . . .
H82 H 0.3578 0.2827 0.3942 0.0262 1.0000 Uiso R . . . . .
H91 H 0.3421 0.5219 0.4231 0.0259 1.0000 Uiso R . . . . .
H92 H 0.1923 0.4667 0.4177 0.0254 1.0000 Uiso R . . . . .
H101 H 0.1347 0.5777 0.4729 0.0236 1.0000 Uiso R . . . . .
H121 H 0.0311 0.6773 0.5255 0.0297 1.0000 Uiso R . . . . .
H131 H 0.0348 0.7397 0.5934 0.0334 1.0000 Uiso R . . . . .
H141 H 0.2126 0.6651 0.6420 0.0295 1.0000 Uiso R . . . . .
H171 H 0.9212 -0.0034 0.6069 0.0298 1.0000 Uiso R . . . . .
H172 H 1.0015 0.1054 0.5803 0.0294 1.0000 Uiso R . . . . .
H181 H 0.8865 0.2192 0.6474 0.0326 1.0000 Uiso R . . . . .
H182 H 0.9860 0.3151 0.6244 0.0328 1.0000 Uiso R . . . . .
H191 H 1.2260 0.2520 0.6403 0.0426 1.0000 Uiso R . . . . .
H192 H 1.1867 0.0859 0.6203 0.0429 1.0000 Uiso R . . . . .
H201 H 1.3890 0.0654 0.6638 0.0546 1.0000 Uiso R . . . . .
H202 H 1.2799 -0.0467 0.6784 0.0538 1.0000 Uiso R . . . . .
H211 H 1.3898 0.0832 0.7356 0.0497 1.0000 Uiso R . . . . .
H212 H 1.3643 0.2443 0.7138 0.0501 1.0000 Uiso R . . . . .
H221 H 1.2055 0.2180 0.7568 0.0521 1.0000 Uiso R . . . . .
H222 H 1.1642 0.0529 0.7377 0.0516 1.0000 Uiso R . . . . .
H231 H 1.0060 0.2362 0.7112 0.0469 1.0000 Uiso R . . . . .
H232 H 1.1179 0.3421 0.6964 0.0473 1.0000 Uiso R . . . . .
H241 H 0.3663 0.5112 0.6834 0.0314 1.0000 Uiso R . . . . .
H242 H 0.4202 0.6759 0.6705 0.0316 1.0000 Uiso R . . . . .
H251 H 0.5684 0.5264 0.7220 0.0310 1.0000 Uiso R . . . . .
H252 H 0.5945 0.4165 0.6853 0.0313 1.0000 Uiso R . . . . .
H261 H 0.8279 0.5351 0.7204 0.0331 1.0000 Uiso R . . . . .
H262 H 0.8049 0.4586 0.6760 0.0345 1.0000 Uiso R . . . . .
H271 H 0.9979 0.6163 0.6847 0.0417 1.0000 Uiso R . . . . .
H272 H 0.8939 0.6787 0.6491 0.0419 1.0000 Uiso R . . . . .
H281 H 0.9419 0.8076 0.7280 0.0446 1.0000 Uiso R . . . . .
H282 H 0.9759 0.8906 0.6887 0.0448 1.0000 Uiso R . . . . .
H291 H 0.7716 0.9880 0.7078 0.0438 1.0000 Uiso R . . . . .
H292 H 0.7488 0.9169 0.6634 0.0434 1.0000 Uiso R . . . . .
H301 H 0.6943 0.7592 0.7341 0.0380 1.0000 Uiso R . . . . .
H302 H 0.5840 0.8216 0.6993 0.0376 1.0000 Uiso R . . . . .
H1 H 0.6085 0.1932 0.5999 0.0653 1.0000 Uiso R . . . . .
H2 H 0.5227 0.2761 0.6146 0.0652 1.0000 Uiso R . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.256(3)

loop_
_oxford_twin_element_scale_factors
0.9704(5)
0.0296(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 . 1.8674(17) yes
Ni1 . O2 . 1.8717(19) yes
Ni1 . N1 . 1.855(2) yes
Ni1 . N2 . 1.855(2) yes
O1 . C1 . 1.308(3) yes
O2 . C16 . 1.308(3) yes
O3 . C2 . 1.383(3) yes
O3 . C17 . 1.435(3) yes
O4 . C15 . 1.378(3) yes
O4 . C24 . 1.432(3) yes
O5 . H1 . 0.807 no
O5 . H2 . 0.807 no
N1 . C7 . 1.287(3) yes
N1 . C8 . 1.480(3) yes
N2 . C9 . 1.464(3) yes
N2 . C10 . 1.283(3) yes
N3 . C18 . 1.468(3) yes
N3 . C19 . 1.462(4) yes
N3 . C23 . 1.461(4) yes
N4 . C25 . 1.466(4) yes
N4 . C26 . 1.463(4) yes
N4 . C30 . 1.463(4) yes
C1 . C2 . 1.433(4) yes
C1 . C6 . 1.413(4) yes
C2 . C3 . 1.376(4) yes
C3 . C4 . 1.409(4) yes
C3 . H31 . 0.930 no
C4 . C5 . 1.363(4) yes
C4 . H41 . 0.938 no
C5 . C6 . 1.407(4) yes
C5 . H51 . 0.941 no
C6 . C7 . 1.431(4) yes
C7 . H71 . 0.953 no
C8 . C9 . 1.500(4) yes
C8 . H81 . 0.968 no
C8 . H82 . 0.969 no
C9 . H91 . 0.971 no
C9 . H92 . 0.977 no
C10 . C11 . 1.433(4) yes
C10 . H101 . 0.948 no
C11 . C12 . 1.410(4) yes
C11 . C16 . 1.416(4) yes
C12 . C13 . 1.356(4) yes
C12 . H121 . 0.949 no
C13 . C14 . 1.404(4) yes
C13 . H131 . 0.918 no
C14 . C15 . 1.375(4) yes
C14 . H141 . 0.937 no
C15 . C16 . 1.431(4) yes
C17 . C18 . 1.507(4) yes
C17 . H171 . 0.975 no
C17 . H172 . 0.973 no
C18 . H181 . 0.966 no
C18 . H182 . 0.979 no
C19 . C20 . 1.523(4) yes
C19 . H191 . 0.980 no
C19 . H192 . 0.981 no
C20 . C21 . 1.515(5) yes
C20 . H201 . 0.960 no
C20 . H202 . 0.992 no
C21 . C22 . 1.518(5) yes
C21 . H211 . 0.967 no
C21 . H212 . 0.962 no
C22 . C23 . 1.524(4) yes
C22 . H221 . 0.966 no
C22 . H222 . 0.967 no
C23 . H231 . 0.980 no
C23 . H232 . 0.979 no
C24 . C25 . 1.506(4) yes
C24 . H241 . 0.984 no
C24 . H242 . 0.981 no
C25 . H251 . 0.984 no
C25 . H252 . 0.976 no
C26 . C27 . 1.512(4) yes
C26 . H261 . 0.986 no
C26 . H262 . 0.981 no
C27 . C28 . 1.517(5) yes
C27 . H271 . 0.958 no
C27 . H272 . 0.969 no
C28 . C29 . 1.523(4) yes
C28 . H281 . 0.976 no
C28 . H282 . 0.965 no
C29 . C30 . 1.521(4) yes
C29 . H291 . 0.973 no
C29 . H292 . 0.975 no
C30 . H301 . 0.982 no
C30 . H302 . 0.973 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 . 86.49(8) yes
O1 . Ni1 . N1 . 94.55(9) yes
O2 . Ni1 . N1 . 175.42(9) yes
O1 . Ni1 . N2 . 175.35(9) yes
O2 . Ni1 . N2 . 94.17(9) yes
N1 . Ni1 . N2 . 85.16(10) yes
Ni1 . O1 . C1 . 126.73(17) yes
Ni1 . O2 . C16 . 126.30(17) yes
C2 . O3 . C17 . 115.6(2) yes
C15 . O4 . C24 . 116.2(2) yes
H1 . O5 . H2 . 104.5 no
Ni1 . N1 . C7 . 126.92(19) yes
Ni1 . N1 . C8 . 114.74(18) yes
C7 . N1 . C8 . 118.1(2) yes
Ni1 . N2 . C9 . 113.22(17) yes
Ni1 . N2 . C10 . 127.2(2) yes
C9 . N2 . C10 . 119.4(2) yes
C18 . N3 . C19 . 112.9(2) yes
C18 . N3 . C23 . 111.3(2) yes
C19 . N3 . C23 . 110.0(2) yes
C25 . N4 . C26 . 110.8(2) yes
C25 . N4 . C30 . 111.4(2) yes
C26 . N4 . C30 . 110.4(2) yes
O1 . C1 . C2 . 119.2(2) yes
O1 . C1 . C6 . 124.8(2) yes
C2 . C1 . C6 . 116.0(2) yes
C1 . C2 . O3 . 114.4(2) yes
C1 . C2 . C3 . 121.3(3) yes
O3 . C2 . C3 . 124.3(2) yes
C2 . C3 . C4 . 120.8(3) yes
C2 . C3 . H31 . 119.2 no
C4 . C3 . H31 . 119.9 no
C3 . C4 . C5 . 119.4(3) yes
C3 . C4 . H41 . 119.6 no
C5 . C4 . H41 . 121.0 no
C4 . C5 . C6 . 120.6(3) yes
C4 . C5 . H51 . 120.4 no
C6 . C5 . H51 . 119.0 no
C1 . C6 . C5 . 121.6(2) yes
C1 . C6 . C7 . 121.0(3) yes
C5 . C6 . C7 . 117.4(3) yes
C6 . C7 . N1 . 125.5(3) yes
C6 . C7 . H71 . 116.2 no
N1 . C7 . H71 . 118.3 no
N1 . C8 . C9 . 106.4(2) yes
N1 . C8 . H81 . 109.4 no
C9 . C8 . H81 . 110.2 no
N1 . C8 . H82 . 110.5 no
C9 . C8 . H82 . 111.4 no
H81 . C8 . H82 . 108.8 no
C8 . C9 . N2 . 106.5(2) yes
C8 . C9 . H91 . 110.5 no
N2 . C9 . H91 . 109.4 no
C8 . C9 . H92 . 112.1 no
N2 . C9 . H92 . 110.1 no
H91 . C9 . H92 . 108.2 no
N2 . C10 . C11 . 125.4(2) yes
N2 . C10 . H101 . 117.4 no
C11 . C10 . H101 . 117.2 no
C10 . C11 . C12 . 118.2(2) yes
C10 . C11 . C16 . 120.5(2) yes
C12 . C11 . C16 . 121.2(3) yes
C11 . C12 . C13 . 120.7(3) yes
C11 . C12 . H121 . 118.0 no
C13 . C12 . H121 . 121.3 no
C12 . C13 . C14 . 120.0(3) yes
C12 . C13 . H131 . 120.4 no
C14 . C13 . H131 . 119.6 no
C13 . C14 . C15 . 120.3(3) yes
C13 . C14 . H141 . 119.9 no
C15 . C14 . H141 . 119.8 no
O4 . C15 . C14 . 124.4(3) yes
O4 . C15 . C16 . 113.9(2) yes
C14 . C15 . C16 . 121.7(3) yes
C15 . C16 . C11 . 116.0(2) yes
C15 . C16 . O2 . 118.8(2) yes
C11 . C16 . O2 . 125.1(3) yes
O3 . C17 . C18 . 108.7(2) yes
O3 . C17 . H171 . 108.4 no
C18 . C17 . H171 . 110.0 no
O3 . C17 . H172 . 108.2 no
C18 . C17 . H172 . 111.9 no
H171 . C17 . H172 . 109.5 no
C17 . C18 . N3 . 110.0(2) yes
C17 . C18 . H181 . 109.4 no
N3 . C18 . H181 . 108.1 no
C17 . C18 . H182 . 110.0 no
N3 . C18 . H182 . 110.2 no
H181 . C18 . H182 . 109.1 no
N3 . C19 . C20 . 110.6(3) yes
N3 . C19 . H191 . 109.3 no
C20 . C19 . H191 . 111.3 no
N3 . C19 . H192 . 108.7 no
C20 . C19 . H192 . 108.0 no
H191 . C19 . H192 . 108.8 no
C19 . C20 . C21 . 111.2(3) yes
C19 . C20 . H201 . 108.5 no
C21 . C20 . H201 . 110.1 no
C19 . C20 . H202 . 108.4 no
C21 . C20 . H202 . 109.0 no
H201 . C20 . H202 . 109.6 no
C20 . C21 . C22 . 110.0(3) yes
C20 . C21 . H211 . 110.5 no
C22 . C21 . H211 . 110.0 no
C20 . C21 . H212 . 108.7 no
C22 . C21 . H212 . 109.4 no
H211 . C21 . H212 . 108.2 no
C21 . C22 . C23 . 111.1(3) yes
C21 . C22 . H221 . 110.3 no
C23 . C22 . H221 . 108.5 no
C21 . C22 . H222 . 108.7 no
C23 . C22 . H222 . 108.6 no
H221 . C22 . H222 . 109.6 no
C22 . C23 . N3 . 110.9(3) yes
C22 . C23 . H231 . 108.8 no
N3 . C23 . H231 . 109.0 no
C22 . C23 . H232 . 109.5 no
N3 . C23 . H232 . 110.2 no
H231 . C23 . H232 . 108.5 no
O4 . C24 . C25 . 108.4(2) yes
O4 . C24 . H241 . 109.4 no
C25 . C24 . H241 . 110.5 no
O4 . C24 . H242 . 108.8 no
C25 . C24 . H242 . 111.3 no
H241 . C24 . H242 . 108.4 no
C24 . C25 . N4 . 112.3(2) yes
C24 . C25 . H251 . 108.1 no
N4 . C25 . H251 . 109.7 no
C24 . C25 . H252 . 108.8 no
N4 . C25 . H252 . 108.8 no
H251 . C25 . H252 . 109.0 no
N4 . C26 . C27 . 110.8(3) yes
N4 . C26 . H261 . 109.3 no
C27 . C26 . H261 . 109.5 no
N4 . C26 . H262 . 108.7 no
C27 . C26 . H262 . 109.6 no
H261 . C26 . H262 . 108.8 no
C26 . C27 . C28 . 111.7(3) yes
C26 . C27 . H271 . 110.0 no
C28 . C27 . H271 . 109.5 no
C26 . C27 . H272 . 109.0 no
C28 . C27 . H272 . 108.8 no
H271 . C27 . H272 . 107.8 no
C27 . C28 . C29 . 110.0(3) yes
C27 . C28 . H281 . 108.3 no
C29 . C28 . H281 . 109.4 no
C27 . C28 . H282 . 110.2 no
C29 . C28 . H282 . 110.9 no
H281 . C28 . H282 . 108.0 no
C28 . C29 . C30 . 110.5(3) yes
C28 . C29 . H291 . 110.3 no
C30 . C29 . H291 . 109.1 no
C28 . C29 . H292 . 109.3 no
C30 . C29 . H292 . 108.8 no
H291 . C29 . H292 . 108.8 no
C29 . C30 . N4 . 111.2(3) yes
C29 . C30 . H301 . 108.7 no
N4 . C30 . H301 . 110.2 no
C29 . C30 . H302 . 109.9 no
N4 . C30 . H302 . 108.8 no
H301 . C30 . H302 . 107.8 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
O5 . H1 . O1 . 145 0.81 2.36 3.063(4) yes
O5 . H1 . O3 . 145 0.81 2.36 3.056(4) yes
O5 . H2 . O2 . 139 0.81 2.49 3.147(4) yes
O5 . H2 . O4 . 151 0.81 2.31 3.041(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 176.0(2) . . . . no
N1 Ni1 O1 C1 0.5(2) . . . . no
O1 Ni1 O2 C16 -174.0(2) . . . . no
N2 Ni1 O2 C16 10.6(2) . . . . no
O1 Ni1 N1 C7 5.8(3) . . . . no
O1 Ni1 N1 C8 179.87(18) . . . . no
N2 Ni1 N1 C7 -178.9(3) . . . . no
N2 Ni1 N1 C8 -4.79(19) . . . . no
O2 Ni1 N2 C9 165.82(18) . . . . no
O2 Ni1 N2 C10 -9.4(3) . . . . no
N1 Ni1 N2 C9 -18.75(19) . . . . no
N1 Ni1 N2 C10 166.0(3) . . . . no
Ni1 O1 C1 C2 173.80(18) . . . . no
Ni1 O1 C1 C6 -6.3(4) . . . . no
Ni1 O2 C16 C11 -4.6(4) . . . . no
Ni1 O2 C16 C15 176.67(18) . . . . no
C17 O3 C2 C1 -178.5(2) . . . . no
C17 O3 C2 C3 1.5(4) . . . . no
C2 O3 C17 C18 169.8(2) . . . . no
C24 O4 C15 C14 -2.7(4) . . . . no
C24 O4 C15 C16 177.3(2) . . . . no
C15 O4 C24 C25 -172.4(2) . . . . no
Ni1 N1 C7 C6 -6.6(4) . . . . no
C8 N1 C7 C6 179.5(3) . . . . no
Ni1 N1 C8 C9 25.7(3) . . . . no
C7 N1 C8 C9 -159.6(3) . . . . no
Ni1 N2 C9 C8 36.8(3) . . . . no
C10 N2 C9 C8 -147.5(3) . . . . no
Ni1 N2 C10 C11 2.2(4) . . . . no
C9 N2 C10 C11 -172.8(3) . . . . no
C19 N3 C18 C17 66.1(3) . . . . no
C23 N3 C18 C17 -169.6(2) . . . . no
C18 N3 C19 C20 -174.1(3) . . . . no
C23 N3 C19 C20 61.0(3) . . . . no
C18 N3 C23 C22 173.3(3) . . . . no
C19 N3 C23 C22 -60.8(3) . . . . no
C26 N4 C25 C24 -158.1(3) . . . . no
C30 N4 C25 C24 78.7(3) . . . . no
C25 N4 C26 C27 176.5(2) . . . . no
C30 N4 C26 C27 -59.7(3) . . . . no
C25 N4 C30 C29 -176.2(2) . . . . no
C26 N4 C30 C29 60.4(3) . . . . no
O1 C1 C2 O3 -4.7(3) . . . . no
O1 C1 C2 C3 175.4(2) . . . . no
C6 C1 C2 O3 175.5(2) . . . . no
C6 C1 C2 C3 -4.6(4) . . . . no
O1 C1 C6 C5 -174.2(2) . . . . no
O1 C1 C6 C7 6.8(4) . . . . no
C2 C1 C6 C5 5.7(4) . . . . no
C2 C1 C6 C7 -173.3(3) . . . . no
O3 C2 C3 C4 -179.3(3) . . . . no
C1 C2 C3 C4 0.7(4) . . . . no
C2 C3 C4 C5 2.3(4) . . . . no
C3 C4 C5 C6 -1.2(4) . . . . no
C4 C5 C6 C1 -3.0(4) . . . . no
C4 C5 C6 C7 176.1(3) . . . . no
C1 C6 C7 N1 0.0(4) . . . . no
C5 C6 C7 N1 -179.1(3) . . . . no
N1 C8 C9 N2 -38.0(3) . . . . no
N2 C10 C11 C12 -177.4(3) . . . . no
N2 C10 C11 C16 7.6(4) . . . . no
C10 C11 C12 C13 -175.3(3) . . . . no
C16 C11 C12 C13 -0.2(5) . . . . no
C10 C11 C16 O2 -6.2(4) . . . . no
C10 C11 C16 C15 172.6(2) . . . . no
C12 C11 C16 O2 178.9(3) . . . . no
C12 C11 C16 C15 -2.4(4) . . . . no
C11 C12 C13 C14 1.6(5) . . . . no
C12 C13 C14 C15 -0.1(5) . . . . no
C13 C14 C15 O4 177.2(3) . . . . no
C13 C14 C15 C16 -2.7(4) . . . . no
O4 C15 C16 O2 2.7(3) . . . . no
O4 C15 C16 C11 -176.1(2) . . . . no
C14 C15 C16 O2 -177.3(2) . . . . no
C14 C15 C16 C11 3.9(4) . . . . no
O3 C17 C18 N3 169.6(2) . . . . no
N3 C19 C20 C21 -57.5(4) . . . . no
C19 C20 C21 C22 52.8(4) . . . . no
C20 C21 C22 C23 -52.4(4) . . . . no
C21 C22 C23 N3 57.0(4) . . . . no
O4 C24 C25 N4 77.0(3) . . . . no
N4 C26 C27 C28 56.6(3) . . . . no
C26 C27 C28 C29 -52.9(4) . . . . no
C27 C28 C29 C30 52.7(3) . . . . no
C28 C29 C30 N4 -57.1(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 C5 3.187(3) . 2_656 no
Ni1 O1 3.8379(18) . 2_666 no
Ni1 O2 3.3608(18) . 2_666 no
Ni1 N2 3.417(2) . 2_666 no
Ni1 C3 3.872(3) . 2_656 no
Ni1 C4 3.309(3) . 2_656 no
Ni1 C10 3.880(3) . 2_666 no
Ni1 C6 3.638(3) . 2_656 no
Ni1 C9 3.886(3) . 2_666 no
Ni1 C16 3.862(2) . 2_666 no
O1 O2 2.562(2) . . no
O1 O3 2.647(3) . . no
O1 O5 3.063(3) . . no
O1 N1 2.735(3) . . no
O1 C7 2.902(3) . . no
O1 C6 3.375(3) . 2_656 no
O1 N2 3.053(3) . 2_666 no
O1 C9 3.278(3) . 2_666 no
O1 C10 3.116(3) . 2_666 no
O2 C9 3.268(3) . 2_666 no
O2 O4 2.623(3) . . no
O2 O5 3.147(3) . . no
O2 N2 2.730(3) . . no
O2 C10 2.903(4) . . no
O3 O5 3.056(3) . . no
O4 N4 3.029(3) . . no
O4 O5 3.040(3) . . no
N1 N2 2.510(3) . . no
N1 C1 2.910(3) . . no
N1 C9 2.387(4) . . no
N2 C8 2.376(4) . . no
N2 C16 2.904(4) . . no
C1 C11 3.467(4) . 2_666 no
C1 C7 3.297(4) . 2_656 no
C1 C10 3.228(4) . 2_666 no
C1 C6 3.476(4) . 2_656 no
C2 C10 3.480(4) . 2_666 no
C3 C4 3.543(4) . 2_756 no
C3 C3 3.516(4) . 2_756 no
C3 C8 3.573(4) . 2_656 no
C6 C6 3.576(4) . 2_656 no
C7 C16 3.597(4) . 2_666 no
C10 C12 3.484(4) . 2_566 no

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 19/09/14 at 12:23:38
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE O   (   5,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 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) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,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   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 19/09/14 at 12:23:38
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# start Validation Reply Form
_vrf_PLAT922_ral1405X            
;
PROBLEM: wR2 in the CIF and FCF Differ by ...............     0.0079 Check 
RESPONSE:  a twinning correction was applied and the fcf listing / checkcif
have a mis-match.
;
# end Validation Reply Form

#===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_ral1503X
_database_code_depnum_ccdc_archive 'CCDC 1838522'
_audit_update_record             
;
2018-04-20 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_audit_creation_date             15-07-10
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1503X\Tony_ral1503X_data\r At 17:27 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   8.1440(1)
_cell_length_b                   11.8552(2)
_cell_length_c                   15.6018(3)
_cell_angle_alpha                93.0064(17)
_cell_angle_beta                 90.4792(16)
_cell_angle_gamma                90.5565(15)
_cell_volume                     1504.13(4)

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


_cell_formula_units_Z            2

# Given Formula = C42 H48 N4 Ni1 O4 
# Dc =      1.62 Fooo =    684.00 Mu =      7.04 M =    731.58
# Found Formula = C34 H42 N4 Ni1 O5 
# Dc =      1.43 FOOO =    684.00 Mu =      6.95 M =    645.44

_chemical_formula_sum            'C34 H42 N4 Ni1 O5'
_chemical_formula_moiety         'C34 H40 N4 Ni O4, H2 O'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         645.44


_cell_measurement_reflns_used    15941
_cell_measurement_theta_min      2
_cell_measurement_theta_max      31
_cell_measurement_temperature    150

_exptl_crystal_description       prism
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.084
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_max          0.317

_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    0.695

# Sheldrick geometric approximatio 0.92 0.94 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_T_max  0.94
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2015)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2015)'
_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            30197
_reflns_number_total             8260
_diffrn_reflns_av_R_equivalents  0.022
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8260 
# Theoretical number of reflections is about 19123 


_diffrn_reflns_theta_min         1.720
_diffrn_reflns_theta_max         30.965
_diffrn_measured_fraction_theta_max 0.864

_diffrn_reflns_theta_full        27.748
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              -16
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   1.37
_oxford_diffrn_Wilson_scale      0.10

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

_refine_diff_density_min         -0.45
_refine_diff_density_max         0.49


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         8259
_refine_ls_number_restraints     0
_refine_ls_number_parameters     403
_oxford_refine_ls_R_factor_ref   0.0359
_refine_ls_wR_factor_ref         0.0738
_refine_ls_goodness_of_fit_ref   1.0034
_refine_ls_shift/su_max          0.0023207
_refine_ls_shift/su_mean         0.0000780


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8259
_refine_ls_R_factor_all          0.0359
_refine_ls_wR_factor_all         0.0738

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7316
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_gt          0.0695

# 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) + ( 0.03P)² + 0.81P] 
 ,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 = 0.83 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints
except for those bonded to O which were allowed to refine freely.


The largest features in the
final difference electron density map are located 
midway between bonded atoms.
;

# 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 0.696839(19) 0.524915(13) 0.531727(10) 0.0154 1.0000 Uani . . . . . .
O1 O 0.74026(12) 0.66067(8) 0.48527(6) 0.0213 1.0000 Uani . . . . . .
O2 O 0.57162(11) 0.61208(7) 0.60610(6) 0.0196 1.0000 Uani . . . . . .
O3 O 1.05532(11) 0.76692(8) 0.18957(6) 0.0213 1.0000 Uani . . . . . .
O4 O 0.27741(13) 0.51395(8) 0.90945(6) 0.0262 1.0000 Uani . . . . . .
O5 O 0.61384(19) 0.86275(10) 0.57927(9) 0.0432 1.0000 Uani . . . . . .
N1 N 0.82107(13) 0.44027(9) 0.45318(7) 0.0164 1.0000 Uani . . . . . .
N2 N 0.65445(13) 0.39029(9) 0.58273(7) 0.0161 1.0000 Uani . . . . . .
N3 N 1.41879(13) 0.81602(9) 0.13511(7) 0.0179 1.0000 Uani . . . . . .
N4 N 0.21549(13) 0.31292(9) 1.07760(7) 0.0178 1.0000 Uani . . . . . .
C1 C 0.82042(15) 0.67870(11) 0.41508(8) 0.0180 1.0000 Uani . . . . . .
C2 C 0.82519(17) 0.79030(11) 0.38679(9) 0.0223 1.0000 Uani . . . . . .
C3 C 0.90493(17) 0.81459(11) 0.31299(9) 0.0215 1.0000 Uani . . . . . .
C4 C 0.98408(15) 0.72982(11) 0.26283(8) 0.0182 1.0000 Uani . . . . . .
C5 C 0.98319(15) 0.62103(11) 0.28825(8) 0.0184 1.0000 Uani . . . . . .
C6 C 0.90162(15) 0.59345(10) 0.36507(8) 0.0172 1.0000 Uani . . . . . .
C7 C 0.89875(15) 0.47901(11) 0.38767(8) 0.0180 1.0000 Uani . . . . . .
C8 C 0.81910(15) 0.32301(10) 0.46799(8) 0.0178 1.0000 Uani . . . . . .
C9 C 0.72433(15) 0.29541(10) 0.53818(8) 0.0181 1.0000 Uani . . . . . .
C10 C 0.57405(15) 0.37947(10) 0.65406(8) 0.0175 1.0000 Uani . . . . . .
C11 C 0.49915(15) 0.46881(10) 0.70294(8) 0.0165 1.0000 Uani . . . . . .
C12 C 0.42403(15) 0.44335(11) 0.78213(8) 0.0185 1.0000 Uani . . . . . .
C13 C 0.35001(16) 0.52676(11) 0.83108(8) 0.0195 1.0000 Uani . . . . . .
C14 C 0.34384(16) 0.63766(11) 0.80217(9) 0.0205 1.0000 Uani . . . . . .
C15 C 0.41402(15) 0.66374(11) 0.72632(8) 0.0190 1.0000 Uani . . . . . .
C16 C 0.49831(15) 0.58080(10) 0.67517(8) 0.0161 1.0000 Uani . . . . . .
C17 C 0.89923(18) 0.23866(11) 0.41972(9) 0.0241 1.0000 Uani . . . . . .
C18 C 0.88235(19) 0.12728(12) 0.44096(10) 0.0278 1.0000 Uani . . . . . .
C19 C 0.78530(19) 0.09906(12) 0.50977(10) 0.0272 1.0000 Uani . . . . . .
C20 C 0.70613(18) 0.18270(11) 0.55829(9) 0.0235 1.0000 Uani . . . . . .
C21 C 1.16944(16) 0.69336(11) 0.14620(9) 0.0202 1.0000 Uani . . . . . .
C22 C 1.27736(16) 0.76301(11) 0.09003(8) 0.0200 1.0000 Uani . . . . . .
C23 C 1.52078(17) 0.87196(12) 0.07239(9) 0.0234 1.0000 Uani . . . . . .
C24 C 1.67264(18) 0.92624(13) 0.11430(11) 0.0298 1.0000 Uani . . . . . .
C25 C 1.62586(19) 1.01194(13) 0.18581(11) 0.0332 1.0000 Uani . . . . . .
C26 C 1.51290(18) 0.95606(13) 0.24836(10) 0.0294 1.0000 Uani . . . . . .
C27 C 1.36691(16) 0.89967(12) 0.20186(9) 0.0223 1.0000 Uani . . . . . .
C28 C 0.28822(17) 0.40464(11) 0.94364(9) 0.0230 1.0000 Uani . . . . . .
C29 C 0.22248(16) 0.41869(11) 1.03403(8) 0.0205 1.0000 Uani . . . . . .
C30 C 0.07547(17) 0.24281(12) 1.04702(9) 0.0225 1.0000 Uani . . . . . .
C31 C 0.06877(19) 0.13188(12) 1.09162(10) 0.0284 1.0000 Uani . . . . . .
C32 C 0.06259(17) 0.15168(13) 1.18887(9) 0.0264 1.0000 Uani . . . . . .
C33 C 0.20383(17) 0.22939(13) 1.21840(9) 0.0251 1.0000 Uani . . . . . .
C34 C 0.20129(17) 0.33720(12) 1.17013(8) 0.0213 1.0000 Uani . . . . . .
H1 H 0.638(3) 0.797(2) 0.5702(16) 0.0649 1.0000 Uiso . . . . . .
H2 H 0.506(3) 0.866(2) 0.5605(16) 0.0665 1.0000 Uiso . . . . . .
H21 H 0.7723 0.8477 0.4197 0.0276 1.0000 Uiso R . . . . .
H31 H 0.9062 0.8890 0.2942 0.0265 1.0000 Uiso R . . . . .
H51 H 1.0363 0.5626 0.2560 0.0226 1.0000 Uiso R . . . . .
H71 H 0.9581 0.4273 0.3513 0.0223 1.0000 Uiso R . . . . .
H101 H 0.5656 0.3067 0.6761 0.0213 1.0000 Uiso R . . . . .
H121 H 0.4282 0.3688 0.7997 0.0217 1.0000 Uiso R . . . . .
H141 H 0.2911 0.6938 0.8362 0.0245 1.0000 Uiso R . . . . .
H151 H 0.4089 0.7370 0.7072 0.0232 1.0000 Uiso R . . . . .
H171 H 0.9651 0.2571 0.3731 0.0291 1.0000 Uiso R . . . . .
H181 H 0.9392 0.0698 0.4093 0.0338 1.0000 Uiso R . . . . .
H191 H 0.7730 0.0237 0.5244 0.0335 1.0000 Uiso R . . . . .
H201 H 0.6408 0.1630 0.6041 0.0279 1.0000 Uiso R . . . . .
H211 H 1.2372 0.6553 0.1882 0.0232 1.0000 Uiso R . . . . .
H212 H 1.1084 0.6365 0.1118 0.0236 1.0000 Uiso R . . . . .
H221 H 1.2103 0.8206 0.0640 0.0237 1.0000 Uiso R . . . . .
H222 H 1.3194 0.7120 0.0442 0.0240 1.0000 Uiso R . . . . .
H231 H 1.4552 0.9305 0.0460 0.0277 1.0000 Uiso R . . . . .
H232 H 1.5522 0.8160 0.0275 0.0270 1.0000 Uiso R . . . . .
H241 H 1.7365 0.9627 0.0712 0.0365 1.0000 Uiso R . . . . .
H242 H 1.7406 0.8686 0.1380 0.0353 1.0000 Uiso R . . . . .
H251 H 1.7234 1.0417 0.2160 0.0396 1.0000 Uiso R . . . . .
H252 H 1.5679 1.0754 0.1605 0.0393 1.0000 Uiso R . . . . .
H261 H 1.4731 1.0112 0.2909 0.0349 1.0000 Uiso R . . . . .
H262 H 1.5736 0.8982 0.2780 0.0344 1.0000 Uiso R . . . . .
H271 H 1.2998 0.9572 0.1764 0.0269 1.0000 Uiso R . . . . .
H272 H 1.2983 0.8610 0.2425 0.0264 1.0000 Uiso R . . . . .
H281 H 0.4025 0.3804 0.9447 0.0268 1.0000 Uiso R . . . . .
H282 H 0.2234 0.3503 0.9084 0.0277 1.0000 Uiso R . . . . .
H291 H 0.2955 0.4711 1.0674 0.0245 1.0000 Uiso R . . . . .
H292 H 0.1135 0.4525 1.0323 0.0248 1.0000 Uiso R . . . . .
H301 H -0.0271 0.2846 1.0578 0.0273 1.0000 Uiso R . . . . .
H302 H 0.0836 0.2279 0.9851 0.0269 1.0000 Uiso R . . . . .
H311 H 0.1664 0.0882 1.0763 0.0338 1.0000 Uiso R . . . . .
H312 H -0.0272 0.0894 1.0703 0.0348 1.0000 Uiso R . . . . .
H321 H 0.0687 0.0803 1.2167 0.0321 1.0000 Uiso R . . . . .
H322 H -0.0416 0.1868 1.2044 0.0307 1.0000 Uiso R . . . . .
H331 H 0.1986 0.2488 1.2798 0.0300 1.0000 Uiso R . . . . .
H332 H 0.3074 0.1918 1.2080 0.0296 1.0000 Uiso R . . . . .
H341 H 0.2922 0.3873 1.1891 0.0264 1.0000 Uiso R . . . . .
H342 H 0.0992 0.3772 1.1822 0.0263 1.0000 Uiso R . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.217(17)
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 . 1.8320(9) yes
Ni1 . O2 . 1.8354(9) yes
Ni1 . N1 . 1.8557(11) yes
Ni1 . N2 . 1.8512(10) yes
O1 . C1 . 1.3056(15) yes
O2 . C16 . 1.3052(15) yes
O3 . C4 . 1.3768(15) yes
O3 . C21 . 1.4305(15) yes
O4 . C13 . 1.3775(15) yes
O4 . C28 . 1.4302(15) yes
O5 . H1 . 0.81(3) no
O5 . H2 . 0.92(3) no
N1 . C7 . 1.3077(16) yes
N1 . C8 . 1.4211(16) yes
N2 . C9 . 1.4175(16) yes
N2 . C10 . 1.3072(16) yes
N3 . C22 . 1.4637(16) yes
N3 . C23 . 1.4691(16) yes
N3 . C27 . 1.4676(17) yes
N4 . C29 . 1.4582(16) yes
N4 . C30 . 1.4662(16) yes
N4 . C34 . 1.4629(16) yes
C1 . C2 . 1.4169(18) yes
C1 . C6 . 1.4165(17) yes
C2 . C3 . 1.3689(18) yes
C2 . H21 . 0.941 no
C3 . C4 . 1.4059(18) yes
C3 . H31 . 0.944 no
C4 . C5 . 1.3690(18) yes
C5 . C6 . 1.4265(17) yes
C5 . H51 . 0.945 no
C6 . C7 . 1.4196(17) yes
C7 . H71 . 0.952 no
C8 . C9 . 1.3960(18) yes
C8 . C17 . 1.3910(18) yes
C9 . C20 . 1.3952(17) yes
C10 . C11 . 1.4181(17) yes
C10 . H101 . 0.947 no
C11 . C12 . 1.4283(17) yes
C11 . C16 . 1.4181(17) yes
C12 . C13 . 1.3654(18) yes
C12 . H121 . 0.939 no
C13 . C14 . 1.4133(18) yes
C14 . C15 . 1.3671(18) yes
C14 . H141 . 0.940 no
C15 . C16 . 1.4195(17) yes
C15 . H151 . 0.934 no
C17 . C18 . 1.3840(19) yes
C17 . H171 . 0.942 no
C18 . C19 . 1.391(2) yes
C18 . H181 . 0.947 no
C19 . C20 . 1.3834(19) yes
C19 . H191 . 0.939 no
C20 . H201 . 0.933 no
C21 . C22 . 1.5156(17) yes
C21 . H211 . 0.983 no
C21 . H212 . 0.970 no
C22 . H221 . 0.981 no
C22 . H222 . 0.978 no
C23 . C24 . 1.516(2) yes
C23 . H231 . 0.985 no
C23 . H232 . 0.976 no
C24 . C25 . 1.522(2) yes
C24 . H241 . 0.970 no
C24 . H242 . 0.970 no
C25 . C26 . 1.519(2) yes
C25 . H251 . 0.974 no
C25 . H252 . 0.991 no
C26 . C27 . 1.5186(19) yes
C26 . H261 . 0.967 no
C26 . H262 . 0.983 no
C27 . H271 . 0.977 no
C27 . H272 . 0.977 no
C28 . C29 . 1.5143(18) yes
C28 . H281 . 0.977 no
C28 . H282 . 0.974 no
C29 . H291 . 0.982 no
C29 . H292 . 0.978 no
C30 . C31 . 1.5206(19) yes
C30 . H301 . 0.986 no
C30 . H302 . 0.977 no
C31 . C32 . 1.524(2) yes
C31 . H311 . 0.977 no
C31 . H312 . 0.973 no
C32 . C33 . 1.520(2) yes
C32 . H321 . 0.973 no
C32 . H322 . 0.975 no
C33 . C34 . 1.5174(19) yes
C33 . H331 . 0.975 no
C33 . H332 . 0.969 no
C34 . H341 . 0.979 no
C34 . H342 . 0.975 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 . 83.07(4) yes
O1 . Ni1 . N1 . 95.17(4) yes
O2 . Ni1 . N1 . 177.81(4) yes
O1 . Ni1 . N2 . 177.84(4) yes
O2 . Ni1 . N2 . 95.44(4) yes
N1 . Ni1 . N2 . 86.35(5) yes
Ni1 . O1 . C1 . 127.78(8) yes
Ni1 . O2 . C16 . 127.47(8) yes
C4 . O3 . C21 . 117.37(10) yes
C13 . O4 . C28 . 116.49(10) yes
H1 . O5 . H2 . 104(2) no
Ni1 . N1 . C7 . 125.93(9) yes
Ni1 . N1 . C8 . 112.99(8) yes
C7 . N1 . C8 . 121.01(11) yes
Ni1 . N2 . C9 . 113.20(8) yes
Ni1 . N2 . C10 . 125.69(9) yes
C9 . N2 . C10 . 121.08(11) yes
C22 . N3 . C23 . 108.58(10) yes
C22 . N3 . C27 . 111.35(10) yes
C23 . N3 . C27 . 109.33(10) yes
C29 . N4 . C30 . 111.19(10) yes
C29 . N4 . C34 . 109.49(10) yes
C30 . N4 . C34 . 109.35(10) yes
O1 . C1 . C2 . 117.94(11) yes
O1 . C1 . C6 . 124.08(11) yes
C2 . C1 . C6 . 117.98(11) yes
C1 . C2 . C3 . 120.88(12) yes
C1 . C2 . H21 . 118.8 no
C3 . C2 . H21 . 120.4 no
C2 . C3 . C4 . 121.18(12) yes
C2 . C3 . H31 . 120.3 no
C4 . C3 . H31 . 118.5 no
C3 . C4 . O3 . 114.32(11) yes
C3 . C4 . C5 . 119.74(12) yes
O3 . C4 . C5 . 125.93(12) yes
C4 . C5 . C6 . 120.25(12) yes
C4 . C5 . H51 . 121.4 no
C6 . C5 . H51 . 118.3 no
C5 . C6 . C1 . 119.97(11) yes
C5 . C6 . C7 . 118.51(11) yes
C1 . C6 . C7 . 121.47(11) yes
C6 . C7 . N1 . 125.32(12) yes
C6 . C7 . H71 . 116.2 no
N1 . C7 . H71 . 118.5 no
N1 . C8 . C9 . 113.63(11) yes
N1 . C8 . C17 . 126.30(12) yes
C9 . C8 . C17 . 120.07(12) yes
N2 . C9 . C8 . 113.72(11) yes
N2 . C9 . C20 . 126.40(12) yes
C8 . C9 . C20 . 119.88(12) yes
N2 . C10 . C11 . 125.31(11) yes
N2 . C10 . H101 . 118.3 no
C11 . C10 . H101 . 116.4 no
C10 . C11 . C12 . 118.10(11) yes
C10 . C11 . C16 . 121.70(11) yes
C12 . C11 . C16 . 120.20(11) yes
C11 . C12 . C13 . 120.03(11) yes
C11 . C12 . H121 . 118.6 no
C13 . C12 . H121 . 121.4 no
O4 . C13 . C12 . 125.69(12) yes
O4 . C13 . C14 . 114.38(11) yes
C12 . C13 . C14 . 119.93(12) yes
C13 . C14 . C15 . 120.99(12) yes
C13 . C14 . H141 . 118.9 no
C15 . C14 . H141 . 120.1 no
C14 . C15 . C16 . 120.97(12) yes
C14 . C15 . H151 . 120.8 no
C16 . C15 . H151 . 118.3 no
C15 . C16 . C11 . 117.76(11) yes
C15 . C16 . O2 . 118.31(11) yes
C11 . C16 . O2 . 123.93(11) yes
C8 . C17 . C18 . 119.59(13) yes
C8 . C17 . H171 . 120.3 no
C18 . C17 . H171 . 120.1 no
C17 . C18 . C19 . 120.56(13) yes
C17 . C18 . H181 . 119.8 no
C19 . C18 . H181 . 119.6 no
C18 . C19 . C20 . 120.07(13) yes
C18 . C19 . H191 . 121.0 no
C20 . C19 . H191 . 118.9 no
C9 . C20 . C19 . 119.81(13) yes
C9 . C20 . H201 . 120.7 no
C19 . C20 . H201 . 119.5 no
O3 . C21 . C22 . 108.57(10) yes
O3 . C21 . H211 . 110.1 no
C22 . C21 . H211 . 110.1 no
O3 . C21 . H212 . 108.7 no
C22 . C21 . H212 . 110.7 no
H211 . C21 . H212 . 108.6 no
C21 . C22 . N3 . 113.99(11) yes
C21 . C22 . H221 . 109.1 no
N3 . C22 . H221 . 110.1 no
C21 . C22 . H222 . 107.3 no
N3 . C22 . H222 . 107.6 no
H221 . C22 . H222 . 108.4 no
N3 . C23 . C24 . 111.52(12) yes
N3 . C23 . H231 . 108.8 no
C24 . C23 . H231 . 109.2 no
N3 . C23 . H232 . 108.6 no
C24 . C23 . H232 . 110.1 no
H231 . C23 . H232 . 108.5 no
C23 . C24 . C25 . 110.82(12) yes
C23 . C24 . H241 . 109.3 no
C25 . C24 . H241 . 110.2 no
C23 . C24 . H242 . 109.6 no
C25 . C24 . H242 . 109.2 no
H241 . C24 . H242 . 107.7 no
C24 . C25 . C26 . 109.48(12) yes
C24 . C25 . H251 . 110.7 no
C26 . C25 . H251 . 109.8 no
C24 . C25 . H252 . 109.0 no
C26 . C25 . H252 . 109.3 no
H251 . C25 . H252 . 108.6 no
C25 . C26 . C27 . 111.03(13) yes
C25 . C26 . H261 . 110.5 no
C27 . C26 . H261 . 108.9 no
C25 . C26 . H262 . 109.5 no
C27 . C26 . H262 . 108.5 no
H261 . C26 . H262 . 108.4 no
C26 . C27 . N3 . 111.74(11) yes
C26 . C27 . H271 . 109.4 no
N3 . C27 . H271 . 109.9 no
C26 . C27 . H272 . 110.1 no
N3 . C27 . H272 . 108.0 no
H271 . C27 . H272 . 107.6 no
O4 . C28 . C29 . 105.40(10) yes
O4 . C28 . H281 . 110.1 no
C29 . C28 . H281 . 110.4 no
O4 . C28 . H282 . 109.9 no
C29 . C28 . H282 . 111.7 no
H281 . C28 . H282 . 109.3 no
C28 . C29 . N4 . 113.05(11) yes
C28 . C29 . H291 . 108.3 no
N4 . C29 . H291 . 108.0 no
C28 . C29 . H292 . 109.2 no
N4 . C29 . H292 . 110.2 no
H291 . C29 . H292 . 108.0 no
N4 . C30 . C31 . 111.36(11) yes
N4 . C30 . H301 . 109.2 no
C31 . C30 . H301 . 109.5 no
N4 . C30 . H302 . 109.4 no
C31 . C30 . H302 . 109.8 no
H301 . C30 . H302 . 107.4 no
C30 . C31 . C32 . 111.42(12) yes
C30 . C31 . H311 . 108.8 no
C32 . C31 . H311 . 109.3 no
C30 . C31 . H312 . 108.2 no
C32 . C31 . H312 . 110.9 no
H311 . C31 . H312 . 108.1 no
C31 . C32 . C33 . 109.20(11) yes
C31 . C32 . H321 . 110.5 no
C33 . C32 . H321 . 110.5 no
C31 . C32 . H322 . 109.0 no
C33 . C32 . H322 . 109.7 no
H321 . C32 . H322 . 107.9 no
C32 . C33 . C34 . 110.44(11) yes
C32 . C33 . H331 . 111.4 no
C34 . C33 . H331 . 109.0 no
C32 . C33 . H332 . 109.8 no
C34 . C33 . H332 . 108.9 no
H331 . C33 . H332 . 107.2 no
C33 . C34 . N4 . 111.16(11) yes
C33 . C34 . H341 . 110.5 no
N4 . C34 . H341 . 108.5 no
C33 . C34 . H342 . 109.4 no
N4 . C34 . H342 . 109.6 no
H341 . C34 . H342 . 107.6 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
O5 . H1 . O1 . 151(2) 0.81(3) 2.21(3) 2.9420(19) yes
O5 . H1 . O2 . 143(2) 0.81(3) 2.36(3) 3.0394(19) 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 -173.02(11) . . . . no
N1 Ni1 O1 C1 5.66(11) . . . . no
O1 Ni1 O2 C16 -172.06(11) . . . . no
N2 Ni1 O2 C16 6.37(11) . . . . no
O1 Ni1 N1 C7 -2.89(11) . . . . no
O1 Ni1 N1 C8 -179.97(9) . . . . no
N2 Ni1 N1 C7 178.64(11) . . . . no
N2 Ni1 N1 C8 1.56(9) . . . . no
O2 Ni1 N2 C9 175.85(8) . . . . no
O2 Ni1 N2 C10 -6.46(11) . . . . no
N1 Ni1 N2 C9 -2.89(9) . . . . no
N1 Ni1 N2 C10 174.81(11) . . . . no
Ni1 O1 C1 C2 173.84(9) . . . . no
Ni1 O1 C1 C6 -5.56(18) . . . . no
Ni1 O2 C16 C11 -2.50(18) . . . . no
Ni1 O2 C16 C15 176.78(8) . . . . no
C21 O3 C4 C3 165.69(11) . . . . no
C21 O3 C4 C5 -15.24(18) . . . . no
C4 O3 C21 C22 -159.31(10) . . . . no
C28 O4 C13 C12 3.14(19) . . . . no
C28 O4 C13 C14 -176.75(11) . . . . no
C13 O4 C28 C29 171.86(11) . . . . no
Ni1 N1 C7 C6 0.0(2) . . . . no
C8 N1 C7 C6 176.88(12) . . . . no
Ni1 N1 C8 C9 0.11(13) . . . . no
Ni1 N1 C8 C17 179.53(11) . . . . no
C7 N1 C8 C9 -177.13(11) . . . . no
C7 N1 C8 C17 2.3(2) . . . . no
Ni1 N2 C9 C8 3.66(13) . . . . no
Ni1 N2 C9 C20 -176.31(11) . . . . no
C10 N2 C9 C8 -174.16(11) . . . . no
C10 N2 C9 C20 5.9(2) . . . . no
Ni1 N2 C10 C11 2.84(18) . . . . no
C9 N2 C10 C11 -179.63(12) . . . . no
C23 N3 C22 C21 174.91(11) . . . . no
C27 N3 C22 C21 -64.67(14) . . . . no
C22 N3 C23 C24 -178.45(11) . . . . no
C27 N3 C23 C24 59.89(14) . . . . no
C22 N3 C27 C26 -179.38(11) . . . . no
C23 N3 C27 C26 -59.41(14) . . . . no
C30 N4 C29 C28 -76.63(13) . . . . no
C34 N4 C29 C28 162.43(11) . . . . no
C29 N4 C30 C31 179.40(11) . . . . no
C34 N4 C30 C31 -59.58(14) . . . . no
C29 N4 C34 C33 -176.63(11) . . . . no
C30 N4 C34 C33 61.32(14) . . . . no
O1 C1 C2 C3 -178.97(12) . . . . no
C6 C1 C2 C3 0.47(19) . . . . no
O1 C1 C6 C5 178.67(12) . . . . no
O1 C1 C6 C7 1.20(19) . . . . no
C2 C1 C6 C5 -0.73(18) . . . . no
C2 C1 C6 C7 -178.21(12) . . . . no
C1 C2 C3 C4 0.2(2) . . . . no
C2 C3 C4 O3 178.53(12) . . . . no
C2 C3 C4 C5 -0.6(2) . . . . no
O3 C4 C5 C6 -178.69(11) . . . . no
C3 C4 C5 C6 0.33(19) . . . . no
C4 C5 C6 C1 0.34(18) . . . . no
C4 C5 C6 C7 177.89(12) . . . . no
C1 C6 C7 N1 1.7(2) . . . . no
C5 C6 C7 N1 -175.87(12) . . . . no
N1 C8 C9 N2 -2.42(15) . . . . no
N1 C8 C9 C20 177.55(12) . . . . no
C17 C8 C9 N2 178.13(12) . . . . no
C17 C8 C9 C20 -1.91(19) . . . . no
N1 C8 C17 C18 -178.42(13) . . . . no
C9 C8 C17 C18 1.0(2) . . . . no
N2 C9 C20 C19 -178.51(13) . . . . no
C8 C9 C20 C19 1.5(2) . . . . no
N2 C10 C11 C12 -176.45(12) . . . . no
N2 C10 C11 C16 3.3(2) . . . . no
C10 C11 C12 C13 -179.78(12) . . . . no
C16 C11 C12 C13 0.49(18) . . . . no
C10 C11 C16 O2 -3.51(19) . . . . no
C10 C11 C16 C15 177.22(11) . . . . no
C12 C11 C16 O2 176.22(11) . . . . no
C12 C11 C16 C15 -3.06(18) . . . . no
C11 C12 C13 O4 -178.14(12) . . . . no
C11 C12 C13 C14 1.74(19) . . . . no
O4 C13 C14 C15 178.56(12) . . . . no
C12 C13 C14 C15 -1.3(2) . . . . no
C13 C14 C15 C16 -1.4(2) . . . . no
C14 C15 C16 O2 -175.81(12) . . . . no
C14 C15 C16 C11 3.51(18) . . . . no
C8 C17 C18 C19 0.4(2) . . . . no
C17 C18 C19 C20 -0.8(2) . . . . no
C18 C19 C20 C9 -0.2(2) . . . . no
O3 C21 C22 N3 84.78(13) . . . . no
N3 C23 C24 C25 -58.05(16) . . . . no
C23 C24 C25 C26 53.74(17) . . . . no
C24 C25 C26 C27 -53.28(16) . . . . no
C25 C26 C27 N3 57.19(16) . . . . no
O4 C28 C29 N4 176.71(10) . . . . no
N4 C30 C31 C32 56.47(15) . . . . no
C30 C31 C32 C33 -52.94(16) . . . . no
C31 C32 C33 C34 54.14(15) . . . . no
C32 C33 C34 N4 -59.53(15) . . . . 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 C11 3.9863(13) . 2_666 no
Ni1 O2 3.3953(9) . 2_666 no
Ni1 N1 3.9476(11) . 2_766 no
Ni1 N2 3.5416(11) . 2_666 no
Ni1 C6 3.9362(12) . 2_766 no
Ni1 C7 3.5172(12) . 2_766 no
Ni1 C10 3.8523(12) . 2_666 no
Ni1 C16 3.7373(12) . 2_666 no
O1 O2 2.4318(13) . . no
O1 O5 2.9419(16) . . no
O1 N1 2.7226(14) . . no
O1 C7 2.8924(16) . . no
O1 C10 3.3584(16) . 2_666 no
O2 O5 3.0394(15) . . no
O2 N2 2.7276(14) . . no
O2 C10 2.8952(15) . . no
O3 C27 2.9725(16) . . no
O3 N3 3.1438(14) . . no
O5 C20 3.383(2) . 2_666 no
O5 C19 3.3529(19) . 1_565 no
N1 C16 3.2689(16) . 2_666 no
N1 C7 3.4498(16) . 2_766 no
N1 N2 2.5365(15) . . no
N1 C1 2.9189(17) . . no
N1 C9 2.3577(16) . . no
N2 C8 2.3559(16) . . no
N2 C16 2.9228(16) . . no
C1 C11 3.5659(17) . 2_666 no
C1 C8 3.4442(17) . 2_766 no
C1 C10 3.4323(17) . 2_666 no
C1 C17 3.5227(19) . 2_766 no
C5 C12 3.5481(17) . 2_666 no
C6 C9 3.5959(17) . 2_766 no
C6 C12 3.5027(17) . 2_666 no
C6 C8 3.5390(17) . 2_766 no
C6 C11 3.4838(17) . 2_666 no
C7 C16 3.4278(17) . 2_666 no
C7 C15 3.4699(18) . 2_666 no
C7 C11 3.5967(17) . 2_666 no
C8 C15 3.5748(18) . 2_666 no
C11 C1 3.5659(17) . 2_666 no
C15 C33 3.4350(19) . 2_667 no
C15 C34 3.5133(18) . 2_667 no
C16 C34 3.5163(18) . 2_667 no
C22 C30 3.5653(19) . 2_666 no



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 10/07/15 at 17:47:56
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S H(1,X'S) UNTIL H(2) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,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) 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   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 10/07/15 at 17:47:56
#
#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
0 1 0 x .


#===END
# start Validation Reply Form
_vrf_PLAT420_ral1503X            
;
PROBLEM: D-H Without Acceptor       O5       --H2             Please Check 
RESPONSE: H1 has potential H-bond contacts to both O1 and O2, 
so H2 is directed towards an empty space.
;
# end Validation Reply Form




####################################################################### 
# 
# 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_ral1604X
_database_code_depnum_ccdc_archive 'CCDC 1838239'
_audit_update_record             
;
2018-04-19 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_audit_creation_date             16-05-27
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1604X\Tony_ral1604X_data\r At 13: 0 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   11.1734(2)
_cell_length_b                   20.8139(3)
_cell_length_c                   8.9919(2)
_cell_angle_alpha                90
_cell_angle_beta                 112.121(2)
_cell_angle_gamma                90
_cell_volume                     1937.24(7)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1 '
_symmetry_space_group_name_Hall  'C 2y'

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z
-x,y,-z
-x+1/2,y+1/2,-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 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C20 H20 N2 Ni1 O4 
# Dc =      1.41 Fooo =    936.00 Mu =     10.29 M =    411.10
# Found Formula = C20 H24 N2 Ni1 O6 
# Dc =      1.53 FOOO =    936.00 Mu =     10.43 M =    447.13

_chemical_formula_sum            'C20 H24 N2 Ni O6'
_chemical_formula_moiety         'C20 H20 N2 Ni O4, 2(H2 O)'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         447.13


_cell_measurement_reflns_used    13967
_cell_measurement_theta_min      4
_cell_measurement_theta_max      30
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.106
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_max          0.358

_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    1.043

# Sheldrick geometric approximatio 0.82 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_T_max  0.90
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2015)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2015)'
_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            21728
_reflns_number_total             4879
_diffrn_reflns_av_R_equivalents  0.024
# Number of reflections without Friedels Law is 4879 
# Number of reflections with Friedels Law is 2643 
# Theoretical number of reflections is about 2809 


_diffrn_reflns_theta_min         3.535
_diffrn_reflns_theta_max         29.936
_diffrn_measured_fraction_theta_max 0.916

_diffrn_reflns_theta_full        27.610
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -15
_reflns_limit_h_max              14
_reflns_limit_k_min              -27
_reflns_limit_k_max              28
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   1.16
_oxford_diffrn_Wilson_scale      0.16

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

_refine_diff_density_min         -0.40
_refine_diff_density_max         0.67


# 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         4879
_refine_ls_number_restraints     1
_refine_ls_number_parameters     282
_oxford_refine_ls_R_factor_ref   0.0262
_refine_ls_wR_factor_ref         0.0571
_refine_ls_goodness_of_fit_ref   1.0164
_refine_ls_shift/su_max          0.0085373
_refine_ls_shift/su_mean         0.0005053


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4879
_refine_ls_R_factor_all          0.0262
_refine_ls_wR_factor_all         0.0571

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4671
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_gt          0.0542

_refine_ls_abs_structure_Flack   -0.006(13)
_refine_ls_abs_structure_details 'Flack (1983), 2236 Friedel-pairs'
# 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 ad


_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) + ( 0.02P)² + 3.00P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               
The compound is enantiomerically pure.
Its absolute configuration has been determined 
by refinement of the Flack parameter
and is in agreement with the configuration expected
on the basis of 
the synthetic precursors.
The final value of the Flack parameter is -0.007(13) and 
the final value of the Hooft parameter is -0.019(8).


All of the H atoms were located in difference electron density maps, 
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 = 0.83 Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints
except for those bonded to O which were allowed to refine freely.


Most of the largest features in the
final difference electron density map 
are located midway between bonded atoms or near the Ni atoms.


The structure presents some pseudo-symmetry.
Structure checking programs such as ADDSYM within PLATON
suggest that there might be an extra centre of symmetry
 and that the space group could be C2/c.  
As the compound is chiral, an inversion symmetry operation is not an option.
Furthermore, if the space group were to be C2/c, then
reflections h0l: l=2n+1 would need to be systematically extinct.
In fact reflections h0l:l=2n+1 have an average I/σ(I) of 134
(cf. reflections h0l:l=2n with an average I/σ(I) of 387),
so this reflection class is a long way from being absent
and clearly no c-glide is present.


;

# 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 0.0000 0.54681(5) 0.0000 0.0138 1.0000 Uani S T . . . .
Ni2 Ni 0.5000 0.47802(5) 0.5000 0.0141 1.0000 Uani S T . . . .
O1 O 0.0594(2) 0.61315(12) 0.1442(3) 0.0208 1.0000 Uani . . . . . .
O2 O 0.1749(2) 0.71977(12) 0.6439(3) 0.0217 1.0000 Uani . . . . . .
O3 O 0.4641(2) 0.41143(12) 0.3535(3) 0.0183 1.0000 Uani . . . . . .
O4 O 0.3035(2) 0.30492(12) -0.1490(3) 0.0228 1.0000 Uani . . . . . .
O5 O 0.3304(2) 0.20112(12) 0.0319(3) 0.0303 1.0000 Uani . . . . . .
O6 O 0.1666(2) 0.82302(12) 0.4608(3) 0.0244 1.0000 Uani . . . . . .
N1 N 0.0669(2) 0.48218(14) 0.1496(3) 0.0151 1.0000 Uani . . . . . .
N2 N 0.4654(2) 0.54256(15) 0.3482(3) 0.0163 1.0000 Uani . . . . . .
C1 C 0.1029(3) 0.60892(16) 0.3022(4) 0.0157 1.0000 Uani . . . . . .
C2 C 0.1215(3) 0.66635(17) 0.3895(3) 0.0179 1.0000 Uani . . . . . .
C3 C 0.1604(3) 0.66554(15) 0.5560(3) 0.0157 1.0000 Uani . . . . . .
C4 C 0.1845(3) 0.60663(17) 0.6382(4) 0.0224 1.0000 Uani . . . . . .
C5 C 0.1708(3) 0.5507(2) 0.5536(3) 0.0216 1.0000 Uani . . . . . .
C6 C 0.1309(2) 0.54966(19) 0.3858(3) 0.0170 1.0000 Uani . . . . . .
C7 C 0.1169(3) 0.48947(15) 0.3037(4) 0.0181 1.0000 Uani . . . . . .
C8 C 0.06346(19) 0.41871(10) 0.0735(2) 0.0154 1.0000 Uani . . . . . .
C9 C 0.0737(3) 0.35983(17) 0.1769(3) 0.0200 1.0000 Uani . . . . . .
C10 C 0.0623(2) 0.29939(10) 0.0738(2) 0.0198 1.0000 Uani . . . . . .
C11 C 0.4093(3) 0.41547(16) 0.1958(4) 0.0153 1.0000 Uani . . . . . .
C12 C 0.3825(3) 0.35815(16) 0.1065(3) 0.0160 1.0000 Uani . . . . . .
C13 C 0.3287(3) 0.35938(16) -0.0582(3) 0.0180 1.0000 Uani . . . . . .
C14 C 0.2974(3) 0.41774(17) -0.1422(4) 0.0226 1.0000 Uani . . . . . .
C15 C 0.3232(3) 0.47392(19) -0.0564(3) 0.0225 1.0000 Uani . . . . . .
C16 C 0.3793(2) 0.47492(18) 0.1135(3) 0.0174 1.0000 Uani . . . . . .
C17 C 0.4117(3) 0.53534(15) 0.1944(4) 0.0178 1.0000 Uani . . . . . .
C18 C 0.5110(2) 0.60662(10) 0.4212(2) 0.0172 1.0000 Uani . . . . . .
C19 C 0.4499(3) 0.66561(18) 0.3208(4) 0.0229 1.0000 Uani . . . . . .
C20 C 0.5071(2) 0.72635(11) 0.4188(3) 0.0233 1.0000 Uani . . . . . .
H1 H 0.163(3) 0.7456(16) 0.593(4) 0.0320 1.0000 Uiso . . . . . .
H2 H 0.313(3) 0.2687(16) -0.088(4) 0.0357 1.0000 Uiso . . . . . .
H3 H 0.372(3) 0.1719(18) 0.029(4) 0.0462 1.0000 Uiso . . . . . .
H4 H 0.345(3) 0.2104(18) 0.141(4) 0.0465 1.0000 Uiso . . . . . .
H5 H 0.183(3) 0.8198(18) 0.388(4) 0.0364 1.0000 Uiso . . . . . .
H6 H 0.102(3) 0.8426(17) 0.435(4) 0.0359 1.0000 Uiso . . . . . .
H21 H 0.1065 0.7054 0.3350 0.0233 1.0000 Uiso R . . . . .
H41 H 0.2064 0.6058 0.7506 0.0274 1.0000 Uiso R . . . . .
H51 H 0.1875 0.5110 0.6088 0.0270 1.0000 Uiso R . . . . .
H71 H 0.1508 0.4523 0.3662 0.0219 1.0000 Uiso R . . . . .
H81 H 0.1349 0.4185 0.0354 0.0182 1.0000 Uiso R . . . . .
H91 H 0.1581 0.3585 0.2683 0.0229 1.0000 Uiso R . . . . .
H92 H 0.0031 0.3606 0.2156 0.0232 1.0000 Uiso R . . . . .
H101 H 0.1345 0.2992 0.0392 0.0241 1.0000 Uiso R . . . . .
H102 H 0.0674 0.2616 0.1373 0.0245 1.0000 Uiso R . . . . .
H121 H 0.4030 0.3190 0.1618 0.0204 1.0000 Uiso R . . . . .
H141 H 0.2582 0.4168 -0.2539 0.0284 1.0000 Uiso R . . . . .
H151 H 0.3047 0.5130 -0.1103 0.0279 1.0000 Uiso R . . . . .
H171 H 0.3958 0.5728 0.1281 0.0199 1.0000 Uiso R . . . . .
H181 H 0.6054 0.6076 0.4467 0.0195 1.0000 Uiso R . . . . .
H191 H 0.4696 0.6648 0.2234 0.0296 1.0000 Uiso R . . . . .
H192 H 0.3550 0.6647 0.2911 0.0301 1.0000 Uiso R . . . . .
H201 H 0.4635 0.7636 0.3541 0.0275 1.0000 Uiso R . . . . .
H202 H 0.5984 0.7283 0.4375 0.0274 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.418(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . N1 3_555 1.850(3) yes
Ni1 . O1 3_555 1.839(2) yes
Ni1 . O1 . 1.839(2) yes
Ni1 . N1 . 1.850(3) yes
Ni2 . N2 3_656 1.849(3) yes
Ni2 . O3 3_656 1.849(2) yes
Ni2 . O3 . 1.849(2) yes
Ni2 . N2 . 1.849(3) yes
O1 . C1 . 1.319(4) yes
O2 . C3 . 1.352(4) yes
O2 . H1 . 0.68(3) no
O3 . C11 . 1.319(4) yes
O4 . C13 . 1.363(4) yes
O4 . H2 . 0.92(3) no
O5 . H3 . 0.77(4) no
O5 . H4 . 0.95(4) no
O6 . H5 . 0.75(3) no
O6 . H6 . 0.78(3) no
N1 . C7 . 1.293(4) yes
N1 . C8 . 1.482(3) yes
N2 . C17 . 1.293(4) yes
N2 . C18 . 1.489(3) yes
C1 . C2 . 1.402(5) yes
C1 . C6 . 1.417(5) yes
C2 . C3 . 1.393(4) yes
C2 . H21 . 0.931 no
C3 . C4 . 1.404(5) yes
C4 . C5 . 1.368(5) yes
C4 . H41 . 0.946 no
C5 . C6 . 1.403(4) yes
C5 . H51 . 0.945 no
C6 . C7 . 1.433(5) yes
C7 . H71 . 0.948 no
C8 . C8 3_555 1.532(4) yes
C8 . C9 . 1.516(4) yes
C8 . H81 . 0.980 no
C9 . C10 . 1.539(4) yes
C9 . H91 . 0.991 no
C9 . H92 . 0.975 no
C10 . C10 3_555 1.519(4) yes
C10 . H101 . 0.968 no
C10 . H102 . 0.961 no
C11 . C12 . 1.406(5) yes
C11 . C16 . 1.416(5) yes
C12 . C13 . 1.373(4) yes
C12 . H121 . 0.938 no
C13 . C14 . 1.403(5) yes
C14 . C15 . 1.370(5) yes
C14 . H141 . 0.933 no
C15 . C16 . 1.417(4) yes
C15 . H151 . 0.930 no
C16 . C17 . 1.429(5) yes
C17 . H171 . 0.957 no
C18 . C18 3_656 1.526(4) yes
C18 . C19 . 1.525(4) yes
C18 . H181 . 0.992 no
C19 . C20 . 1.536(4) yes
C19 . H191 . 0.980 no
C19 . H192 . 0.991 no
C20 . C20 3_656 1.527(4) yes
C20 . H201 . 0.982 no
C20 . H202 . 0.971 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
N1 3_555 Ni1 . O1 3_555 95.36(9) yes
N1 3_555 Ni1 . O1 . 177.30(12) yes
O1 3_555 Ni1 . O1 . 82.65(15) yes
N1 3_555 Ni1 . N1 . 86.70(17) yes
O1 3_555 Ni1 . N1 . 177.30(12) yes
O1 . Ni1 . N1 . 95.36(9) yes
N2 3_656 Ni2 . O3 3_656 95.16(9) yes
N2 3_656 Ni2 . O3 . 177.84(13) yes
O3 3_656 Ni2 . O3 . 82.88(15) yes
N2 3_656 Ni2 . N2 . 86.81(17) yes
O3 3_656 Ni2 . N2 . 177.84(13) yes
O3 . Ni2 . N2 . 95.16(9) yes
Ni1 . O1 . C1 . 126.7(2) yes
C3 . O2 . H1 . 109(3) no
Ni2 . O3 . C11 . 127.3(2) yes
C13 . O4 . H2 . 112(2) no
H3 . O5 . H4 . 109(4) no
H5 . O6 . H6 . 107(4) no
Ni1 . N1 . C7 . 126.0(2) yes
Ni1 . N1 . C8 . 112.29(16) yes
C7 . N1 . C8 . 121.7(3) yes
Ni2 . N2 . C17 . 126.1(2) yes
Ni2 . N2 . C18 . 112.57(16) yes
C17 . N2 . C18 . 121.3(3) yes
O1 . C1 . C2 . 117.6(3) yes
O1 . C1 . C6 . 123.2(3) yes
C2 . C1 . C6 . 119.2(3) yes
C1 . C2 . C3 . 120.8(3) yes
C1 . C2 . H21 . 119.3 no
C3 . C2 . H21 . 119.9 no
C2 . C3 . O2 . 122.6(3) yes
C2 . C3 . C4 . 119.8(3) yes
O2 . C3 . C4 . 117.6(2) yes
C3 . C4 . C5 . 119.4(3) yes
C3 . C4 . H41 . 119.9 no
C5 . C4 . H41 . 120.6 no
C4 . C5 . C6 . 122.3(3) yes
C4 . C5 . H51 . 119.5 no
C6 . C5 . H51 . 118.2 no
C1 . C6 . C5 . 118.4(3) yes
C1 . C6 . C7 . 121.9(2) yes
C5 . C6 . C7 . 119.7(3) yes
C6 . C7 . N1 . 125.0(3) yes
C6 . C7 . H71 . 117.8 no
N1 . C7 . H71 . 117.0 no
C8 3_555 C8 . N1 . 104.67(14) yes
C8 3_555 C8 . C9 . 111.14(16) yes
N1 . C8 . C9 . 117.05(19) yes
C8 3_555 C8 . H81 . 108.0 no
N1 . C8 . H81 . 106.4 no
C9 . C8 . H81 . 109.2 no
C8 . C9 . C10 . 108.7(2) yes
C8 . C9 . H91 . 111.0 no
C10 . C9 . H91 . 108.3 no
C8 . C9 . H92 . 108.7 no
C10 . C9 . H92 . 109.5 no
H91 . C9 . H92 . 110.5 no
C9 . C10 . C10 3_555 111.53(16) yes
C9 . C10 . H101 . 107.9 no
C10 3_555 C10 . H101 . 108.7 no
C9 . C10 . H102 . 109.8 no
C10 3_555 C10 . H102 . 110.4 no
H101 . C10 . H102 . 108.5 no
O3 . C11 . C12 . 118.2(3) yes
O3 . C11 . C16 . 122.7(3) yes
C12 . C11 . C16 . 119.1(3) yes
C11 . C12 . C13 . 120.8(3) yes
C11 . C12 . H121 . 118.6 no
C13 . C12 . H121 . 120.5 no
C12 . C13 . O4 . 122.6(3) yes
C12 . C13 . C14 . 121.1(3) yes
O4 . C13 . C14 . 116.4(3) yes
C13 . C14 . C15 . 118.6(3) yes
C13 . C14 . H141 . 118.9 no
C15 . C14 . H141 . 122.5 no
C14 . C15 . C16 . 122.2(3) yes
C14 . C15 . H151 . 119.7 no
C16 . C15 . H151 . 118.1 no
C15 . C16 . C11 . 118.2(3) yes
C15 . C16 . C17 . 119.1(3) yes
C11 . C16 . C17 . 122.6(2) yes
C16 . C17 . N2 . 125.0(3) yes
C16 . C17 . H171 . 116.7 no
N2 . C17 . H171 . 118.3 no
C18 3_656 C18 . N2 . 105.16(15) yes
C18 3_656 C18 . C19 . 110.95(17) yes
N2 . C18 . C19 . 117.25(19) yes
C18 3_656 C18 . H181 . 108.3 no
N2 . C18 . H181 . 106.1 no
C19 . C18 . H181 . 108.6 no
C18 . C19 . C20 . 109.0(2) yes
C18 . C19 . H191 . 108.3 no
C20 . C19 . H191 . 110.0 no
C18 . C19 . H192 . 109.8 no
C20 . C19 . H192 . 110.0 no
H191 . C19 . H192 . 109.7 no
C19 . C20 . C20 3_656 112.24(17) yes
C19 . C20 . H201 . 107.7 no
C20 3_656 C20 . H201 . 111.1 no
C19 . C20 . H202 . 108.5 no
C20 3_656 C20 . H202 . 108.4 no
H201 . C20 . H202 . 108.9 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
O2 . H1 . O6 . 169(4) 0.69(3) 2.01(3) 2.688(4) yes
O4 . H2 . O5 . 179(3) 0.92(3) 1.74(3) 2.653(4) yes
O5 . H3 . O1 2_545 149(3) 0.77(4) 2.31(4) 2.996(4) yes
O5 . H3 . O1 4_545 143(3) 0.77(4) 2.33(4) 2.975(4) yes
O5 . H4 . O2 4_546 164(3) 0.95(4) 2.04(4) 2.964(4) yes
O6 . H5 . O4 4_555 170(3) 0.75(3) 2.23(3) 2.970(4) yes
O6 . H6 . O3 2_455 164(3) 0.78(3) 2.03(3) 2.792(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
N1 Ni1 O1 C1 -14.9(3) . . . . no
O1 Ni1 O1 C1 167.0(3) 3_555 . . . no
O1 Ni1 N1 C7 9.7(3) . . . . no
O1 Ni1 N1 C8 -167.58(18) . . . . no
N1 Ni1 N1 C7 -168.6(3) 3_555 . . . no
N1 Ni1 N1 C8 14.17(18) 3_555 . . . no
N2 Ni2 O3 C11 -10.8(3) . . . . no
O3 Ni2 O3 C11 170.1(3) 3_656 . . . no
O3 Ni2 N2 C17 10.6(3) . . . . no
O3 Ni2 N2 C18 -167.33(18) . . . . no
N2 Ni2 N2 C17 -168.6(3) 3_656 . . . no
N2 Ni2 N2 C18 13.54(18) 3_656 . . . no
Ni1 O1 C1 C2 -168.6(2) . . . . no
Ni1 O1 C1 C6 11.3(5) . . . . no
Ni2 O3 C11 C12 -175.6(2) . . . . no
Ni2 O3 C11 C16 5.8(5) . . . . no
C7 N1 C8 C8 145.4(3) . . . 3_555 no
Ni1 N1 C7 C6 -1.0(5) . . . . no
C8 N1 C7 C6 176.1(3) . . . . no
Ni1 N1 C8 C9 -160.71(19) . . . . no
Ni1 N1 C8 C8 -37.2(2) . . . 3_555 no
C7 N1 C8 C9 21.9(4) . . . . no
C18 N2 C17 C16 172.1(3) . . . . no
Ni2 N2 C18 C19 -159.5(2) . . . . no
Ni2 N2 C18 C18 -35.8(2) . . . 3_656 no
C17 N2 C18 C19 22.5(4) . . . . no
C17 N2 C18 C18 146.2(3) . . . 3_656 no
Ni2 N2 C17 C16 -5.6(5) . . . . no
C2 C1 C6 C7 -178.5(3) . . . . no
C6 C1 C2 C3 -3.4(5) . . . . no
O1 C1 C2 C3 176.5(3) . . . . no
C2 C1 C6 C5 2.9(5) . . . . no
O1 C1 C6 C5 -177.0(3) . . . . no
O1 C1 C6 C7 1.7(5) . . . . no
C1 C2 C3 C4 1.6(5) . . . . no
C1 C2 C3 O2 -177.6(3) . . . . no
O2 C3 C4 C5 180.0(3) . . . . no
C2 C3 C4 C5 0.7(5) . . . . no
C3 C4 C5 C6 -1.2(5) . . . . no
C4 C5 C6 C1 -0.6(5) . . . . no
C4 C5 C6 C7 -179.3(3) . . . . no
C5 C6 C7 N1 171.6(3) . . . . no
C1 C6 C7 N1 -7.1(5) . . . . no
N1 C8 C8 N1 45.7(2) . . 3_555 3_555 no
N1 C8 C9 C10 177.6(2) . . . . no
C8 C8 C9 C10 57.4(3) 3_555 . . . no
C9 C8 C8 C9 -59.9(3) . . 3_555 3_555 no
N1 C8 C8 C9 172.9(2) . . 3_555 3_555 no
C9 C8 C8 N1 172.9(2) . . 3_555 3_555 no
C8 C9 C10 C10 -56.5(3) . . . 3_555 no
C9 C10 C10 C9 57.1(3) . . 3_555 3_555 no
O3 C11 C12 C13 -178.3(3) . . . . no
C16 C11 C12 C13 0.4(5) . . . . no
O3 C11 C16 C15 178.6(3) . . . . no
O3 C11 C16 C17 3.1(5) . . . . no
C12 C11 C16 C15 0.0(5) . . . . no
C12 C11 C16 C17 -175.5(3) . . . . no
C11 C12 C13 O4 178.8(3) . . . . no
C11 C12 C13 C14 -0.8(5) . . . . no
O4 C13 C14 C15 -178.8(3) . . . . no
C12 C13 C14 C15 0.8(5) . . . . no
C13 C14 C15 C16 -0.5(5) . . . . no
C14 C15 C16 C11 0.1(5) . . . . no
C14 C15 C16 C17 175.7(3) . . . . no
C11 C16 C17 N2 -3.2(5) . . . . no
C15 C16 C17 N2 -178.6(3) . . . . no
N2 C18 C19 C20 178.5(2) . . . . no
C18 C18 C19 C20 57.7(3) 3_656 . . . no
N2 C18 C18 N2 43.8(2) . . 3_656 3_656 no
N2 C18 C18 C19 171.5(2) . . 3_656 3_656 no
C19 C18 C18 N2 171.5(2) . . 3_656 3_656 no
C19 C18 C18 C19 -60.9(3) . . 3_656 3_656 no
C18 C19 C20 C20 -54.8(3) . . . 3_656 no
C19 C20 C20 C19 54.5(3) . . 3_656 3_656 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 O5 3.795(3) . 2_455 no
Ni1 O5 3.795(3) . 4_555 no
Ni2 C7 3.976(4) . . no
Ni2 O6 3.807(3) . 4_546 no
Ni2 O6 3.807(3) . 2_545 no
Ni2 C7 3.976(4) . 3_656 no
O1 O1 2.428(4) . 3_555 no
O1 N1 2.727(4) . . no
O1 O5 2.974(4) . 4_555 no
O1 O5 2.996(4) . 2_455 no
O1 C7 2.899(4) . . no
O2 O5 2.964(4) . 4_556 no
O2 O6 2.688(4) . . no
O2 C2 3.398(4) . 3_556 no
O3 O3 2.448(4) . 3_656 no
O3 C17 2.900(4) . . no
O3 O6 3.185(4) . 4_546 no
O3 N2 2.730(4) . . no
O3 O6 2.792(4) . 2_545 no
O4 O6 2.970(4) . 4_545 no
O4 O5 2.653(4) . . no
O5 C13 3.391(4) . . no
O5 C12 3.343(4) . . no
O6 C3 3.395(4) . . no
O6 C2 3.325(4) . . no
N1 C1 2.931(4) . . no
N1 N1 2.539(4) . 3_555 no
N1 C8 2.386(3) . 3_555 no
N2 N2 2.542(4) . 3_656 no
N2 C18 2.395(3) . 3_656 no
N2 C11 2.936(4) . . no
C1 C4 3.449(5) . 3_556 no
C2 C4 3.558(5) . 3_556 no
C2 C3 3.365(5) . 3_556 no
C3 C3 3.338(5) . 3_556 no
C5 C5 3.567(5) . 3_556 no
C8 C11 3.598(4) . . no
C11 C14 3.488(5) . 3_655 no
C12 C13 3.414(5) . 3_655 no
C13 C13 3.568(5) . 3_655 no
C15 C16 3.550(4) . 3_655 no




_iucr_refine_instruction_details_constraints 
;
#
# Punched on 27/05/16 at 15:02:40
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT H(1,X'S) UNTIL H(6) 
CONT ENANTIO 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,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) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 27/05/16 at 15:02:40
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

_vrf_PLAT111_ral1604X            
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry       
RESPONSE: ...
The structure does present some pseudo-symmetry.
ADDSYM suggests that there might be an extra centre of symmetry
 and that the space group could be C2/c.  
As the compound is chiral, an inversion symmetry operation is not an option.
Furthermore, if the space group were to be C2/c, then
reflections h0l: l=2n+1 would need to be systematically extinct.
In fact reflections h0l:l=2n+1 have an average I/sig(I) of 134
(cf. reflections h0l:l=2n with an average I/sig(I) of 387),
so this reflection class is a long way from being absent
and clearly no c-glide is present.

;




#===END

