# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1528477'
_audit_update_record             
;
2017-01-19 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   9.6743(3)
_cell_length_b                   5.6824(2)
_cell_length_c                   30.9646(9)
_cell_angle_alpha                90
_cell_angle_beta                 91.293(2)
_cell_angle_gamma                90
_cell_volume                     1701.79(5)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_int_tables_number      4
# 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
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,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'
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'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2
_chemical_formula_moiety         'C40 H36 N2 Ni1 O7'

# Given Formula = C40 H20 Cu0.50 N4 Ni2 O8 
# Dc =      1.63 Fooo =    748.00 Mu =     14.74 M =    833.81
# Found Formula = C40 H36 N2 Ni1 O7 
# Dc =      1.40 FOOO =    748.00 Mu =      6.25 M =    715.44

_chemical_formula_sum            'C40 H36 N2 Ni1 O7'
_chemical_compound_source        ?
_chemical_formula_weight         715.44


_cell_measurement_reflns_used    274
_cell_measurement_theta_min      15
_cell_measurement_theta_max      30
_cell_measurement_temperature    294

_exptl_crystal_description       bar
_exptl_crystal_colour            'light blue'

_diffrn_ambient_temperature      294
_exptl_crystal_size_min          0.132
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_max          0.552

_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             748
_exptl_absorpt_coefficient_mu    0.625

# Sheldrick geometric approximatio 0.88 0.92 
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_T_max  0.92
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21296
_reflns_number_total             6936
_diffrn_reflns_av_R_equivalents  0.026
# Number of reflections without Friedels Law is 6936 
# Number of reflections with Friedels Law is 3853 
# Theoretical number of reflections is about 3514 


_diffrn_reflns_theta_min         0.658
_diffrn_reflns_theta_max         26.463
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        25.934
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       38
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -7
_reflns_limit_k_max              6
_reflns_limit_l_min              0
_reflns_limit_l_max              38


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

_refine_diff_density_min         -0.32
_refine_diff_density_max         0.56


# 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 
_refine_ls_number_reflns         5527
_refine_ls_number_restraints     7
_refine_ls_number_parameters     452
_refine_ls_wR_factor_ref         0.0734
_refine_ls_goodness_of_fit_ref   1.0736
_refine_ls_shift/su_max          0.0015887
_refine_ls_shift/su_mean         0.0000464


# The values computed with all filters except I/sigma 
_refine_ls_R_factor_all          0.0468
_refine_ls_wR_factor_all         0.0787

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5527
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_gt          0.0734

_refine_ls_abs_structure_Flack   0.015(13)
_refine_ls_abs_structure_details 'Flack (1983), 3083 Friedel-pairs'


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.98 2.47 0.771 
;

# 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 0.74863(4) 0.29407(13) 0.765445(11) 0.0449 1.0000 Uani . U . . . .
N1 N 0.5960(3) 0.5227(5) 0.78417(7) 0.0437 1.0000 Uani . . . . . .
N2 N 0.5780(3) 0.1477(5) 0.73257(8) 0.0482 1.0000 Uani . . . . . .
O1 O 0.9010(2) 0.4351(5) 0.80510(7) 0.0515 1.0000 Uani . . . . . .
O2 O 0.7717(2) 0.1602(4) 0.83188(6) 0.0471 1.0000 Uani . U . . . .
O3 O 0.5896(3) 0.6469(5) 1.08992(8) 0.0624 1.0000 Uani . . . . . .
O4 O 0.8001(2) 0.5001(5) 0.71421(7) 0.0527 1.0000 Uani . . . . . .
O5 O 0.9058(3) 0.2318(5) 0.67458(8) 0.0630 1.0000 Uani . . . . . .
O6 O 0.1731(3) 0.6604(5) 0.51646(8) 0.0647 1.0000 Uani . . . . . .
O7 O 0.8793(3) 0.0183(5) 0.74748(8) 0.0675 1.0000 Uani . . . . . .
C1 C 0.8730(3) 0.2951(8) 0.83543(8) 0.0432 1.0000 Uani . . . . . .
C2 C 0.9648(3) 0.2931(9) 0.87627(8) 0.0489 1.0000 Uani . . . . . .
C3 C 1.1048(4) 0.4066(8) 0.86858(12) 0.0691 1.0000 Uani . . . . . .
C4 C 0.8925(3) 0.4065(6) 0.91364(9) 0.0434 1.0000 Uani . . . . . .
C5 C 0.8251(4) 0.6258(6) 0.90913(10) 0.0516 1.0000 Uani . . . . . .
C6 C 0.7552(4) 0.7238(6) 0.94194(10) 0.0511 1.0000 Uani . . . . . .
C7 C 0.7477(3) 0.6138(5) 0.98258(9) 0.0412 1.0000 Uani . . . . . .
C8 C 0.6686(3) 0.6993(6) 1.01657(10) 0.0463 1.0000 Uani . . . . . .
C9 C 0.6646(3) 0.5845(6) 1.05507(10) 0.0477 1.0000 Uani . . . . . .
C10 C 0.7449(3) 0.3791(6) 1.06140(10) 0.0521 1.0000 Uani . . . . . .
C11 C 0.8210(3) 0.2911(8) 1.02934(9) 0.0491 1.0000 Uani . . . . . .
C12 C 0.8232(3) 0.4000(5) 0.98842(9) 0.0396 1.0000 Uani . . . . . .
C13 C 0.8932(3) 0.3012(7) 0.95327(8) 0.0421 1.0000 Uani . . . . . .
C14 C 0.4971(4) 0.8370(8) 1.08557(13) 0.0707 1.0000 Uani . . . . . .
C15 C 0.8630(3) 0.4329(7) 0.68108(10) 0.0459 1.0000 Uani . . . . . .
C16 C 0.8859(3) 0.6195(7) 0.64671(10) 0.0493 1.0000 Uani . . . . . .
C17 C 1.0122(4) 0.5656(9) 0.61964(12) 0.0766 1.0000 Uani . . . . . .
C18 C 0.7574(3) 0.6544(6) 0.61850(9) 0.0447 1.0000 Uani . . . . . .
C19 C 0.7476(3) 0.8589(6) 0.59291(11) 0.0513 1.0000 Uani . . . . . .
C20 C 0.6363(4) 0.9004(7) 0.56629(11) 0.0541 1.0000 Uani . . . . . .
C21 C 0.5242(3) 0.7424(5) 0.56450(9) 0.0430 1.0000 Uani . . . . . .
C22 C 0.4023(3) 0.7864(8) 0.53871(9) 0.0494 1.0000 Uani . . . . . .
C23 C 0.2957(3) 0.6346(7) 0.53878(10) 0.0499 1.0000 Uani . . . . . .
C24 C 0.3052(3) 0.4260(6) 0.56371(11) 0.0507 1.0000 Uani . . . . . .
C25 C 0.4184(3) 0.3786(6) 0.58836(11) 0.0490 1.0000 Uani . . . . . .
C26 C 0.5315(3) 0.5360(6) 0.58963(9) 0.0410 1.0000 Uani . . . . . .
C27 C 0.6511(3) 0.4972(6) 0.61630(9) 0.0431 1.0000 Uani . . . . . .
C28 C 0.1532(4) 0.8725(8) 0.49293(14) 0.0810 1.0000 Uani . . . . . .
C29 C 0.6069(4) 0.7047(6) 0.81007(10) 0.0531 1.0000 Uani . . . . . .
C30 C 0.4958(4) 0.8372(9) 0.82297(11) 0.0684 1.0000 Uani . . . . . .
C31 C 0.3671(4) 0.7817(11) 0.80729(12) 0.0740 1.0000 Uani . . . . . .
C32 C 0.3497(4) 0.5930(8) 0.77865(12) 0.0616 1.0000 Uani . . . . . .
C33 C 0.2206(4) 0.5183(10) 0.75852(16) 0.0836 1.0000 Uani . . . . . .
C34 C 0.2134(4) 0.3442(11) 0.73063(15) 0.0849 1.0000 Uani . . . . . .
C35 C 0.3320(4) 0.2091(7) 0.71995(11) 0.0621 1.0000 Uani . . . . . .
C36 C 0.3325(5) 0.0152(9) 0.69150(12) 0.0758 1.0000 Uani . . . . . .
C37 C 0.4500(5) -0.1025(8) 0.68430(12) 0.0741 1.0000 Uani . . . . . .
C38 C 0.5716(4) -0.0343(7) 0.70595(11) 0.0617 1.0000 Uani . . . . . .
C39 C 0.4603(3) 0.2688(8) 0.73948(8) 0.0470 1.0000 Uani . . . . . .
C40 C 0.4681(3) 0.4669(6) 0.76820(9) 0.0470 1.0000 Uani . . . . . .
H21 H 0.9773 0.1281 0.8839 0.0557 1.0000 Uiso R . . . . .
H31 H 1.1662 0.3841 0.8934 0.1016 1.0000 Uiso R . . . . .
H32 H 1.0937 0.5725 0.8642 0.1013 1.0000 Uiso R . . . . .
H33 H 1.1493 0.3418 0.8445 0.1015 1.0000 Uiso R . . . . .
H51 H 0.8273 0.7036 0.8836 0.0593 1.0000 Uiso R . . . . .
H61 H 0.7094 0.8655 0.9369 0.0582 1.0000 Uiso R . . . . .
H71 H 0.8586 -0.1205 0.7467 0.0980 1.0000 Uiso R . . . . .
H72 H 0.8942 0.0633 0.7215 0.0969 1.0000 Uiso R . . . . .
H81 H 0.6212 0.8343 1.0129 0.0532 1.0000 Uiso R . . . . .
H101 H 0.7418 0.3050 1.0885 0.0588 1.0000 Uiso R . . . . .
H111 H 0.8718 0.1588 1.0340 0.0556 1.0000 Uiso R . . . . .
H131 H 0.9404 0.1559 0.9569 0.0472 1.0000 Uiso R . . . . .
H141 H 0.5510 0.9724 1.0794 0.1024 1.0000 Uiso R . . . . .
H142 H 0.4348 0.8065 1.0620 0.1023 1.0000 Uiso R . . . . .
H143 H 0.4483 0.8539 1.1118 0.1023 1.0000 Uiso R . . . . .
H161 H 0.9034 0.7653 0.6621 0.0571 1.0000 Uiso R . . . . .
H171 H 1.0226 0.6889 0.5990 0.1121 1.0000 Uiso R . . . . .
H172 H 1.0939 0.5519 0.6377 0.1123 1.0000 Uiso R . . . . .
H173 H 0.9971 0.4174 0.6054 0.1131 1.0000 Uiso R . . . . .
H191 H 0.8157 0.9675 0.5955 0.0580 1.0000 Uiso R . . . . .
H201 H 0.6340 1.0379 0.5507 0.0617 1.0000 Uiso R . . . . .
H221 H 0.3960 0.9240 0.5234 0.0564 1.0000 Uiso R . . . . .
H241 H 0.2332 0.3266 0.5634 0.0578 1.0000 Uiso R . . . . .
H251 H 0.4223 0.2416 0.6047 0.0555 1.0000 Uiso R . . . . .
H271 H 0.6572 0.3617 0.6315 0.0494 1.0000 Uiso R . . . . .
H281 H 0.1619 1.0009 0.5116 0.1193 1.0000 Uiso R . . . . .
H282 H 0.2211 0.8776 0.4714 0.1197 1.0000 Uiso R . . . . .
H283 H 0.0642 0.8683 0.4804 0.1195 1.0000 Uiso R . . . . .
H291 H 0.6950 0.7469 0.8197 0.0617 1.0000 Uiso R . . . . .
H301 H 0.5072 0.9612 0.8415 0.0799 1.0000 Uiso R . . . . .
H311 H 0.2929 0.8701 0.8153 0.0859 1.0000 Uiso R . . . . .
H331 H 0.1420 0.5969 0.7654 0.0972 1.0000 Uiso R . . . . .
H341 H 0.1308 0.3103 0.7176 0.0989 1.0000 Uiso R . . . . .
H361 H 0.2511 -0.0254 0.6777 0.0897 1.0000 Uiso R . . . . .
H371 H 0.4505 -0.2279 0.6657 0.0843 1.0000 Uiso R . . . . .
H381 H 0.6536 -0.1191 0.7011 0.0709 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
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 . 2.060(3) yes
Ni1 . N2 . 2.092(3) yes
Ni1 . O1 . 2.059(2) yes
Ni1 . O2 . 2.200(2) yes
Ni1 . O4 . 2.042(2) yes
Ni1 . O7 . 2.096(3) yes
N1 . C29 . 1.311(4) yes
N1 . C40 . 1.359(4) yes
N2 . C38 . 1.323(5) yes
N2 . C39 . 1.351(5) yes
O1 . C1 . 1.265(4) yes
O2 . C1 . 1.247(4) yes
O3 . C9 . 1.361(4) yes
O3 . C14 . 1.407(5) yes
O4 . C15 . 1.263(4) yes
O5 . C15 . 1.234(4) yes
O6 . C23 . 1.368(4) yes
O6 . C28 . 1.419(5) yes
O7 . H71 . 0.814 no
O7 . H72 . 0.859 no
C1 . C2 . 1.529(3) yes
C2 . C3 . 1.524(5) yes
C2 . C4 . 1.510(4) yes
C2 . H21 . 0.974 no
C3 . H31 . 0.970 no
C3 . H32 . 0.958 no
C3 . H33 . 0.944 no
C4 . C5 . 1.411(5) yes
C4 . C13 . 1.365(4) yes
C5 . C6 . 1.353(5) yes
C5 . H51 . 0.907 no
C6 . C7 . 1.409(4) yes
C6 . H61 . 0.930 no
C7 . C8 . 1.402(4) yes
C7 . C12 . 1.427(4) yes
C8 . C9 . 1.360(4) yes
C8 . H81 . 0.900 no
C9 . C10 . 1.413(5) yes
C10 . C11 . 1.346(5) yes
C10 . H101 . 0.941 no
C11 . C12 . 1.411(4) yes
C11 . H111 . 0.908 no
C12 . C13 . 1.411(4) yes
C13 . H131 . 0.949 no
C14 . H141 . 0.951 no
C14 . H142 . 0.953 no
C14 . H143 . 0.952 no
C15 . C16 . 1.522(5) yes
C16 . C17 . 1.528(4) yes
C16 . C18 . 1.516(4) yes
C16 . H161 . 0.969 no
C17 . H171 . 0.955 no
C17 . H172 . 0.960 no
C17 . H173 . 0.960 no
C18 . C19 . 1.408(5) yes
C18 . C27 . 1.363(4) yes
C19 . C20 . 1.363(5) yes
C19 . H191 . 0.905 no
C20 . C21 . 1.408(4) yes
C20 . H201 . 0.919 no
C21 . C22 . 1.431(4) yes
C21 . C26 . 1.408(4) yes
C22 . C23 . 1.344(5) yes
C22 . H221 . 0.915 no
C23 . C24 . 1.416(5) yes
C24 . C25 . 1.348(4) yes
C24 . H241 . 0.897 no
C25 . C26 . 1.414(4) yes
C25 . H251 . 0.929 no
C26 . C27 . 1.423(4) yes
C27 . H271 . 0.904 no
C28 . H281 . 0.934 no
C28 . H282 . 0.947 no
C28 . H283 . 0.938 no
C29 . C30 . 1.379(5) yes
C29 . H291 . 0.928 no
C30 . C31 . 1.363(5) yes
C30 . H301 . 0.914 no
C31 . C32 . 1.399(7) yes
C31 . H311 . 0.915 no
C32 . C33 . 1.447(5) yes
C32 . C40 . 1.395(5) yes
C33 . C34 . 1.314(7) yes
C33 . H331 . 0.911 no
C34 . C35 . 1.426(6) yes
C34 . H341 . 0.908 no
C35 . C36 . 1.411(6) yes
C35 . C39 . 1.410(4) yes
C36 . C37 . 1.342(6) yes
C36 . H361 . 0.918 no
C37 . C38 . 1.395(5) yes
C37 . H371 . 0.917 no
C38 . H381 . 0.943 no
C39 . C40 . 1.436(5) yes
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 . Ni1 . N2 . 79.91(11) yes
N1 . Ni1 . O1 . 95.43(10) yes
N2 . Ni1 . O1 . 172.34(10) yes
N1 . Ni1 . O2 . 90.75(9) yes
N2 . Ni1 . O2 . 112.32(9) yes
O1 . Ni1 . O2 . 61.37(8) yes
N1 . Ni1 . O4 . 92.64(10) yes
N2 . Ni1 . O4 . 93.06(10) yes
O1 . Ni1 . O4 . 93.23(9) yes
O2 . Ni1 . O4 . 154.58(9) yes
N1 . Ni1 . O7 . 170.58(11) yes
N2 . Ni1 . O7 . 92.73(11) yes
O1 . Ni1 . O7 . 91.23(10) yes
O2 . Ni1 . O7 . 86.60(9) yes
O4 . Ni1 . O7 . 93.62(10) yes
Ni1 . N1 . C29 . 128.4(2) yes
Ni1 . N1 . C40 . 113.7(2) yes
C29 . N1 . C40 . 117.8(3) yes
Ni1 . N2 . C38 . 129.7(3) yes
Ni1 . N2 . C39 . 112.3(2) yes
C38 . N2 . C39 . 118.0(3) yes
Ni1 . O1 . C1 . 92.05(17) yes
Ni1 . O2 . C1 . 86.16(17) yes
C9 . O3 . C14 . 118.3(3) yes
Ni1 . O4 . C15 . 126.0(3) yes
C23 . O6 . C28 . 117.2(3) yes
Ni1 . O7 . H71 . 125.6 no
Ni1 . O7 . H72 . 98.1 no
H71 . O7 . H72 . 107.9 no
O1 . C1 . O2 . 120.1(2) yes
O1 . C1 . C2 . 119.3(3) yes
O2 . C1 . C2 . 120.6(3) yes
C1 . C2 . C3 . 111.7(3) yes
C1 . C2 . C4 . 111.1(3) yes
C3 . C2 . C4 . 111.6(3) yes
C1 . C2 . H21 . 106.0 no
C3 . C2 . H21 . 109.9 no
C4 . C2 . H21 . 106.3 no
C2 . C3 . H31 . 110.5 no
C2 . C3 . H32 . 110.0 no
H31 . C3 . H32 . 107.9 no
C2 . C3 . H33 . 112.4 no
H31 . C3 . H33 . 107.0 no
H32 . C3 . H33 . 108.9 no
C2 . C4 . C5 . 121.5(3) yes
C2 . C4 . C13 . 120.6(3) yes
C5 . C4 . C13 . 118.0(3) yes
C4 . C5 . C6 . 121.8(3) yes
C4 . C5 . H51 . 119.8 no
C6 . C5 . H51 . 118.4 no
C5 . C6 . C7 . 121.7(3) yes
C5 . C6 . H61 . 118.4 no
C7 . C6 . H61 . 119.9 no
C6 . C7 . C8 . 123.9(3) yes
C6 . C7 . C12 . 117.0(3) yes
C8 . C7 . C12 . 119.1(3) yes
C7 . C8 . C9 . 121.3(3) yes
C7 . C8 . H81 . 119.1 no
C9 . C8 . H81 . 119.7 no
O3 . C9 . C8 . 126.6(3) yes
O3 . C9 . C10 . 114.0(3) yes
C8 . C9 . C10 . 119.4(3) yes
C9 . C10 . C11 . 120.9(3) yes
C9 . C10 . H101 . 117.7 no
C11 . C10 . H101 . 121.4 no
C10 . C11 . C12 . 121.3(3) yes
C10 . C11 . H111 . 119.7 no
C12 . C11 . H111 . 119.1 no
C7 . C12 . C11 . 118.0(3) yes
C7 . C12 . C13 . 119.6(3) yes
C11 . C12 . C13 . 122.4(3) yes
C12 . C13 . C4 . 121.7(3) yes
C12 . C13 . H131 . 119.5 no
C4 . C13 . H131 . 118.7 no
O3 . C14 . H141 . 106.8 no
O3 . C14 . H142 . 108.9 no
H141 . C14 . H142 . 109.5 no
O3 . C14 . H143 . 108.8 no
H141 . C14 . H143 . 111.9 no
H142 . C14 . H143 . 110.8 no
O4 . C15 . O5 . 125.6(4) yes
O4 . C15 . C16 . 116.0(3) yes
O5 . C15 . C16 . 118.4(3) yes
C15 . C16 . C17 . 112.0(3) yes
C15 . C16 . C18 . 111.3(3) yes
C17 . C16 . C18 . 111.5(3) yes
C15 . C16 . H161 . 106.1 no
C17 . C16 . H161 . 108.0 no
C18 . C16 . H161 . 107.7 no
C16 . C17 . H171 . 108.5 no
C16 . C17 . H172 . 110.8 no
H171 . C17 . H172 . 110.5 no
C16 . C17 . H173 . 108.2 no
H171 . C17 . H173 . 110.7 no
H172 . C17 . H173 . 108.1 no
C16 . C18 . C19 . 118.4(3) yes
C16 . C18 . C27 . 123.4(3) yes
C19 . C18 . C27 . 118.2(3) yes
C18 . C19 . C20 . 121.7(3) yes
C18 . C19 . H191 . 118.2 no
C20 . C19 . H191 . 120.0 no
C19 . C20 . C21 . 120.7(3) yes
C19 . C20 . H201 . 118.3 no
C21 . C20 . H201 . 120.9 no
C20 . C21 . C22 . 122.3(3) yes
C20 . C21 . C26 . 118.7(3) yes
C22 . C21 . C26 . 119.0(3) yes
C21 . C22 . C23 . 120.6(4) yes
C21 . C22 . H221 . 118.8 no
C23 . C22 . H221 . 120.5 no
O6 . C23 . C22 . 125.9(3) yes
O6 . C23 . C24 . 114.2(3) yes
C22 . C23 . C24 . 119.8(3) yes
C23 . C24 . C25 . 121.2(3) yes
C23 . C24 . H241 . 118.7 no
C25 . C24 . H241 . 120.1 no
C24 . C25 . C26 . 120.5(3) yes
C24 . C25 . H251 . 119.9 no
C26 . C25 . H251 . 119.6 no
C25 . C26 . C21 . 118.8(3) yes
C25 . C26 . C27 . 122.5(3) yes
C21 . C26 . C27 . 118.7(3) yes
C26 . C27 . C18 . 122.0(3) yes
C26 . C27 . H271 . 118.5 no
C18 . C27 . H271 . 119.5 no
O6 . C28 . H281 . 109.7 no
O6 . C28 . H282 . 107.5 no
H281 . C28 . H282 . 111.0 no
O6 . C28 . H283 . 107.7 no
H281 . C28 . H283 . 110.2 no
H282 . C28 . H283 . 110.7 no
N1 . C29 . C30 . 123.7(3) yes
N1 . C29 . H291 . 117.4 no
C30 . C29 . H291 . 118.8 no
C29 . C30 . C31 . 118.8(4) yes
C29 . C30 . H301 . 121.3 no
C31 . C30 . H301 . 119.9 no
C30 . C31 . C32 . 119.9(4) yes
C30 . C31 . H311 . 119.5 no
C32 . C31 . H311 . 120.6 no
C31 . C32 . C33 . 126.0(4) yes
C31 . C32 . C40 . 116.9(3) yes
C33 . C32 . C40 . 117.1(4) yes
C32 . C33 . C34 . 122.4(4) yes
C32 . C33 . H331 . 118.1 no
C34 . C33 . H331 . 119.4 no
C33 . C34 . C35 . 121.8(3) yes
C33 . C34 . H341 . 119.1 no
C35 . C34 . H341 . 119.1 no
C34 . C35 . C36 . 125.4(4) yes
C34 . C35 . C39 . 118.5(4) yes
C36 . C35 . C39 . 116.1(4) yes
C35 . C36 . C37 . 120.5(3) yes
C35 . C36 . H361 . 118.2 no
C37 . C36 . H361 . 121.2 no
C36 . C37 . C38 . 119.3(4) yes
C36 . C37 . H371 . 120.6 no
C38 . C37 . H371 . 120.1 no
C37 . C38 . N2 . 122.9(4) yes
C37 . C38 . H381 . 119.0 no
N2 . C38 . H381 . 118.0 no
C35 . C39 . N2 . 123.1(4) yes
C35 . C39 . C40 . 119.2(3) yes
N2 . C39 . C40 . 117.7(3) yes
C39 . C40 . C32 . 120.9(3) yes
C39 . C40 . N1 . 116.3(3) yes
C32 . C40 . N1 . 122.8(3) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O7 . H71 . O4 1_545 157.39(8) 0.814 2.440 3.207(5) yes
O7 . H72 . O5 . 163.26(13) 0.859 1.746 2.581(5) yes
O7 . H72 . C15 . 135.17(10) 0.859 2.460 3.129(5) yes
C29 . H291 . O2 1_565 124.12(10) 0.928 2.489 3.107(5) yes
C30 . H301 . O3 2_657 142.75(11) 0.914 2.566 3.340(5) yes
C34 . H341 . O5 1_455 174.91(11) 0.908 2.564 3.469(5) yes



####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1528478'
_audit_update_record             
;
2017-01-19 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   9.2260(7)
_cell_length_b                   5.9603(5)
_cell_length_c                   30.784(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.522(5)
_cell_angle_gamma                90
_cell_volume                     1692.21(16)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_int_tables_number      4
# 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
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,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'
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
_chemical_formula_moiety         'C39 H38 N2 Ni1 O7'

# Given Formula = C30 N6 Ni3 O6 
# Dc =      1.41 Fooo =    740.00 Mu =     16.98 M =    716.50
# Found Formula = C39 H38 N2 Ni1 O7 
# Dc =      1.38 FOOO =    740.00 Mu =      6.27 M =    705.45

_chemical_formula_sum            'C39 H38 N2 Ni1 O7'
_chemical_compound_source        ?
_chemical_formula_weight         705.45


_cell_measurement_reflns_used    218
_cell_measurement_theta_min      15
_cell_measurement_theta_max      20
_cell_measurement_temperature    295

_exptl_crystal_description       prism
_exptl_crystal_colour            blue

_diffrn_ambient_temperature      295
_exptl_crystal_size_min          0.110
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             740
_exptl_absorpt_coefficient_mu    0.627

# Sheldrick geometric approximatio 0.90 0.93 
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_T_max  0.93
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25416
_reflns_number_total             8811
_diffrn_reflns_av_R_equivalents  0.083
# Number of reflections without Friedels Law is 8811 
# Number of reflections with Friedels Law is 5174 
# Theoretical number of reflections is about 4783 


_diffrn_reflns_theta_min         0.662
_diffrn_reflns_theta_max         29.656
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        29.062
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       42
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -8
_reflns_limit_k_max              8
_reflns_limit_l_min              0
_reflns_limit_l_max              42


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

_refine_diff_density_min         -0.95
_refine_diff_density_max         1.73


# 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 
_refine_ls_number_reflns         4596
_refine_ls_number_restraints     1
_refine_ls_number_parameters     443
_refine_ls_wR_factor_ref         0.0717
_refine_ls_goodness_of_fit_ref   0.9916
_refine_ls_shift/su_max          0.0008745
_refine_ls_shift/su_mean         0.0000250


# The values computed with all filters except I/sigma 
_refine_ls_R_factor_all          0.1366
_refine_ls_wR_factor_all         0.0866

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4596
_refine_ls_R_factor_gt           0.0588
_refine_ls_wR_factor_gt          0.0717

_refine_ls_abs_structure_Flack   -0.006(14)
_refine_ls_abs_structure_details 'Flack (1983), 3637 Friedel-pairs'


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 4.25 3.74 3.12 
;

# 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 0.74562(5) 0.50021(14) 0.263001(15) 0.0333 1.0000 Uani . . . . . .
N1 N 0.5885(3) 0.7236(6) 0.28082(11) 0.0345 1.0000 Uani . . . . . .
N2 N 0.5646(3) 0.3590(6) 0.23275(10) 0.0350 1.0000 Uani . . . . . .
O1 O 0.9086(3) 0.6287(5) 0.30359(9) 0.0405 1.0000 Uani . . . . . .
O2 O 0.7668(3) 0.3677(5) 0.32915(9) 0.0431 1.0000 Uani . . . . . .
O3 O 0.5882(3) 0.8199(5) 0.59160(10) 0.0530 1.0000 Uani . . . . . .
O4 O 0.7897(3) 0.6894(5) 0.21061(9) 0.0393 1.0000 Uani . . . . . .
O5 O 0.9661(3) 0.4898(8) 0.18090(9) 0.0713 1.0000 Uani . . . . . .
O6 O 0.1746(3) 0.8923(6) 0.01219(11) 0.0588 1.0000 Uani . . . . . .
O7 O 0.8781(3) 0.2467(5) 0.24110(9) 0.0432 1.0000 Uani . . . . . .
C1 C 0.8753(3) 0.4948(10) 0.33361(10) 0.0335 1.0000 Uani . . . . . .
C2 C 0.9688(4) 0.4881(10) 0.37497(11) 0.0400 1.0000 Uani . . . . . .
C3 C 1.1163(4) 0.5936(8) 0.36822(15) 0.0539 1.0000 Uani . . . . . .
C4 C 0.8936(4) 0.5922(7) 0.41267(12) 0.0347 1.0000 Uani . . . . . .
C5 C 0.8282(5) 0.8040(7) 0.40892(15) 0.0430 1.0000 Uani . . . . . .
C6 C 0.7562(5) 0.8975(7) 0.44315(13) 0.0416 1.0000 Uani . . . . . .
C7 C 0.7480(4) 0.7865(7) 0.48320(13) 0.0370 1.0000 Uani . . . . . .
C8 C 0.6676(4) 0.8744(7) 0.51783(13) 0.0411 1.0000 Uani . . . . . .
C9 C 0.6619(5) 0.7563(7) 0.55576(14) 0.0440 1.0000 Uani . . . . . .
C10 C 0.7416(5) 0.5582(7) 0.56082(14) 0.0451 1.0000 Uani . . . . . .
C11 C 0.8179(4) 0.4702(9) 0.52830(13) 0.0451 1.0000 Uani . . . . . .
C12 C 0.8226(4) 0.5804(6) 0.48760(13) 0.0353 1.0000 Uani . . . . . .
C13 C 0.8920(4) 0.4895(10) 0.45192(11) 0.0371 1.0000 Uani . . . . . .
C14 C 0.4979(4) 1.0130(12) 0.58856(14) 0.0606 1.0000 Uani . . . . . .
C15 C 0.8871(5) 0.6571(8) 0.18339(13) 0.0436 1.0000 Uani . . . . . .
C16 C 0.9088(4) 0.8491(7) 0.15056(13) 0.0384 1.0000 Uani . . . . . .
C17 C 1.0410(5) 0.8144(10) 0.12324(15) 0.0616 1.0000 Uani . . . . . .
C18 C 0.7745(4) 0.8842(7) 0.12127(13) 0.0340 1.0000 Uani . . . . . .
C19 C 0.7621(5) 1.0857(7) 0.09818(14) 0.0404 1.0000 Uani . . . . . .
C20 C 0.6476(5) 1.1289(8) 0.07027(14) 0.0436 1.0000 Uani . . . . . .
C21 C 0.5343(4) 0.9743(9) 0.06504(11) 0.0368 1.0000 Uani . . . . . .
C22 C 0.4107(4) 1.0196(10) 0.03855(11) 0.0411 1.0000 Uani . . . . . .
C23 C 0.3015(5) 0.8648(9) 0.03546(14) 0.0478 1.0000 Uani . . . . . .
C24 C 0.3117(5) 0.6625(8) 0.05760(13) 0.0451 1.0000 Uani . . . . . .
C25 C 0.4297(5) 0.6144(7) 0.08325(14) 0.0439 1.0000 Uani . . . . . .
C26 C 0.5451(4) 0.7691(7) 0.08834(12) 0.0337 1.0000 Uani . . . . . .
C27 C 0.6674(4) 0.7333(7) 0.11638(12) 0.0350 1.0000 Uani . . . . . .
C28 C 0.1465(6) 1.1031(11) -0.0072(2) 0.0757 1.0000 Uani . . . . . .
C29 C 0.6077(5) 0.8984(8) 0.30603(14) 0.0456 1.0000 Uani . . . . . .
C30 C 0.4948(5) 1.0338(10) 0.32030(13) 0.0487 1.0000 Uani . . . . . .
C31 C 0.3577(5) 0.9766(10) 0.30661(14) 0.0526 1.0000 Uani . . . . . .
C32 C 0.3359(5) 0.7974(8) 0.27878(15) 0.0476 1.0000 Uani . . . . . .
C33 C 0.4535(4) 0.6708(7) 0.26601(12) 0.0369 1.0000 Uani . . . . . .
C34 C 0.4427(4) 0.4824(10) 0.23614(11) 0.0369 1.0000 Uani . . . . . .
C35 C 0.3172(5) 0.4269(7) 0.21227(15) 0.0501 1.0000 Uani . . . . . .
C36 C 0.3205(5) 0.2433(8) 0.18484(16) 0.0585 1.0000 Uani . . . . . .
C37 C 0.4434(5) 0.1179(8) 0.18255(15) 0.0514 1.0000 Uani . . . . . .
C38 C 0.5642(5) 0.1810(8) 0.20673(13) 0.0432 1.0000 Uani . . . . . .
C39 C 0.9898(5) 0.1311(8) 0.26386(15) 0.0518 1.0000 Uani . . . . . .
H393 H 1.0633 0.0881 0.2440 0.0781 1.0000 Uiso R . . . . .
H392 H 1.0319 0.2292 0.2856 0.0783 1.0000 Uiso R . . . . .
H391 H 0.9513 -0.0017 0.2770 0.0785 1.0000 Uiso R . . . . .
H71 H 0.9044 0.3098 0.2190 0.0653 1.0000 Uiso R . . . . .
H21 H 0.9823 0.3314 0.3818 0.0478 1.0000 Uiso R . . . . .
H131 H 0.9369 0.3539 0.4549 0.0444 1.0000 Uiso R . . . . .
H142 H 0.4457 1.0290 0.6149 0.0908 1.0000 Uiso R . . . . .
H143 H 0.4317 0.9958 0.5649 0.0907 1.0000 Uiso R . . . . .
H141 H 0.5563 1.1444 0.5841 0.0907 1.0000 Uiso R . . . . .
H61 H 0.7111 1.0370 0.4398 0.0497 1.0000 Uiso R . . . . .
H51 H 0.8327 0.8791 0.3829 0.0521 1.0000 Uiso R . . . . .
H81 H 0.6197 1.0115 0.5150 0.0485 1.0000 Uiso R . . . . .
H32 H 1.1747 0.5787 0.3943 0.0809 1.0000 Uiso R . . . . .
H33 H 1.1627 0.5166 0.3450 0.0810 1.0000 Uiso R . . . . .
H31 H 1.1057 0.7496 0.3605 0.0809 1.0000 Uiso R . . . . .
H101 H 0.7405 0.4841 0.5872 0.0552 1.0000 Uiso R . . . . .
H111 H 0.8660 0.3360 0.5322 0.0536 1.0000 Uiso R . . . . .
H161 H 0.9206 0.9853 0.1676 0.0458 1.0000 Uiso R . . . . .
H191 H 0.8331 1.1936 0.1022 0.0486 1.0000 Uiso R . . . . .
H201 H 0.6443 1.2623 0.0549 0.0518 1.0000 Uiso R . . . . .
H271 H 0.6742 0.5976 0.1311 0.0417 1.0000 Uiso R . . . . .
H251 H 0.4345 0.4784 0.0978 0.0528 1.0000 Uiso R . . . . .
H241 H 0.2354 0.5591 0.0550 0.0538 1.0000 Uiso R . . . . .
H282 H 0.0573 1.0973 -0.0238 0.1130 1.0000 Uiso R . . . . .
H283 H 0.2219 1.1432 -0.0265 0.1131 1.0000 Uiso R . . . . .
H281 H 0.1385 1.2180 0.0144 0.1127 1.0000 Uiso R . . . . .
H171 H 1.0574 0.9445 0.1059 0.0930 1.0000 Uiso R . . . . .
H172 H 1.0283 0.6870 0.1045 0.0932 1.0000 Uiso R . . . . .
H173 H 1.1233 0.7890 0.1421 0.0932 1.0000 Uiso R . . . . .
H221 H 0.4042 1.1532 0.0238 0.0488 1.0000 Uiso R . . . . .
H351 H 0.2342 0.5140 0.2148 0.0597 1.0000 Uiso R . . . . .
H361 H 0.2384 0.2076 0.1683 0.0709 1.0000 Uiso R . . . . .
H371 H 0.4461 -0.0103 0.1650 0.0614 1.0000 Uiso R . . . . .
H381 H 0.6498 0.1000 0.2049 0.0508 1.0000 Uiso R . . . . .
H301 H 0.5132 1.1568 0.3381 0.0581 1.0000 Uiso R . . . . .
H291 H 0.7023 0.9354 0.3145 0.0548 1.0000 Uiso R . . . . .
H311 H 0.2807 1.0622 0.3157 0.0632 1.0000 Uiso R . . . . .
H321 H 0.2429 0.7618 0.2685 0.0572 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
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 . 2.054(3) yes
Ni1 . N2 . 2.069(3) yes
Ni1 . O1 . 2.076(3) yes
Ni1 . O2 . 2.188(3) yes
Ni1 . O4 . 2.018(3) yes
Ni1 . O7 . 2.068(3) yes
N1 . C29 . 1.308(5) yes
N1 . C33 . 1.352(5) yes
N2 . C34 . 1.350(5) yes
N2 . C38 . 1.329(5) yes
O1 . C1 . 1.265(5) yes
O2 . C1 . 1.260(5) yes
O3 . C9 . 1.365(5) yes
O3 . C14 . 1.422(6) yes
O4 . C15 . 1.260(5) yes
O5 . C15 . 1.238(6) yes
O6 . C23 . 1.367(5) yes
O6 . C28 . 1.412(6) yes
O7 . C39 . 1.410(5) yes
O7 . H71 . 0.820 no
C1 . C2 . 1.520(4) yes
C2 . C3 . 1.518(6) yes
C2 . C4 . 1.502(6) yes
C2 . H21 . 0.965 no
C3 . H32 . 0.959 no
C3 . H33 . 0.959 no
C3 . H31 . 0.964 no
C4 . C5 . 1.402(6) yes
C4 . C13 . 1.355(5) yes
C5 . C6 . 1.378(6) yes
C5 . H51 . 0.921 no
C6 . C7 . 1.403(6) yes
C6 . H61 . 0.934 no
C7 . C8 . 1.416(6) yes
C7 . C12 . 1.413(5) yes
C8 . C9 . 1.366(6) yes
C8 . H81 . 0.932 no
C9 . C10 . 1.397(6) yes
C10 . C11 . 1.345(6) yes
C10 . H101 . 0.925 no
C11 . C12 . 1.416(6) yes
C11 . H111 . 0.922 no
C12 . C13 . 1.395(6) yes
C13 . H131 . 0.912 no
C14 . H142 . 0.960 no
C14 . H143 . 0.943 no
C14 . H141 . 0.963 no
C15 . C16 . 1.544(6) yes
C16 . C17 . 1.514(6) yes
C16 . C18 . 1.527(5) yes
C16 . H161 . 0.971 no
C17 . H171 . 0.955 no
C17 . H172 . 0.959 no
C17 . H173 . 0.955 no
C18 . C19 . 1.399(5) yes
C18 . C27 . 1.342(6) yes
C19 . C20 . 1.368(6) yes
C19 . H191 . 0.924 no
C20 . C21 . 1.399(6) yes
C20 . H201 . 0.925 no
C21 . C22 . 1.410(5) yes
C21 . C26 . 1.420(6) yes
C22 . C23 . 1.367(7) yes
C22 . H221 . 0.918 no
C23 . C24 . 1.387(6) yes
C24 . C25 . 1.358(5) yes
C24 . H241 . 0.937 no
C25 . C26 . 1.415(6) yes
C25 . H251 . 0.926 no
C26 . C27 . 1.418(5) yes
C27 . H271 . 0.928 no
C28 . H282 . 0.959 no
C28 . H283 . 0.956 no
C28 . H281 . 0.959 no
C29 . C30 . 1.398(6) yes
C29 . H291 . 0.930 no
C30 . C31 . 1.365(6) yes
C30 . H301 . 0.927 no
C31 . C32 . 1.381(7) yes
C31 . H311 . 0.924 no
C32 . C33 . 1.388(6) yes
C32 . H321 . 0.930 no
C33 . C34 . 1.453(6) yes
C34 . C35 . 1.394(5) yes
C35 . C36 . 1.383(6) yes
C35 . H351 . 0.930 no
C36 . C37 . 1.361(6) yes
C36 . H361 . 0.925 no
C37 . C38 . 1.376(6) yes
C37 . H371 . 0.937 no
C38 . H381 . 0.929 no
C39 . H393 . 0.959 no
C39 . H392 . 0.962 no
C39 . H391 . 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
N1 . Ni1 . N2 . 79.47(14) yes
N1 . Ni1 . O1 . 96.02(12) yes
N2 . Ni1 . O1 . 169.74(12) yes
N1 . Ni1 . O2 . 91.81(12) yes
N2 . Ni1 . O2 . 108.84(11) yes
O1 . Ni1 . O2 . 61.82(10) yes
N1 . Ni1 . O4 . 90.56(12) yes
N2 . Ni1 . O4 . 92.58(12) yes
O1 . Ni1 . O4 . 96.70(11) yes
O2 . Ni1 . O4 . 158.53(10) yes
N1 . Ni1 . O7 . 171.30(13) yes
N2 . Ni1 . O7 . 91.89(13) yes
O1 . Ni1 . O7 . 92.35(11) yes
O2 . Ni1 . O7 . 90.05(11) yes
O4 . Ni1 . O7 . 90.82(11) yes
Ni1 . N1 . C29 . 126.1(3) yes
Ni1 . N1 . C33 . 114.1(3) yes
C29 . N1 . C33 . 119.6(4) yes
Ni1 . N2 . C34 . 114.1(3) yes
Ni1 . N2 . C38 . 125.8(3) yes
C34 . N2 . C38 . 119.5(4) yes
Ni1 . O1 . C1 . 91.2(2) yes
Ni1 . O2 . C1 . 86.3(2) yes
C9 . O3 . C14 . 118.4(3) yes
Ni1 . O4 . C15 . 127.5(3) yes
C23 . O6 . C28 . 118.2(4) yes
Ni1 . O7 . C39 . 128.7(3) yes
Ni1 . O7 . H71 . 97.2 no
C39 . O7 . H71 . 114.1 no
O1 . C1 . O2 . 120.5(3) yes
O1 . C1 . C2 . 119.0(4) yes
O2 . C1 . C2 . 120.5(4) yes
C1 . C2 . C3 . 111.4(3) yes
C1 . C2 . C4 . 111.9(3) yes
C3 . C2 . C4 . 111.7(4) yes
C1 . C2 . H21 . 106.0 no
C3 . C2 . H21 . 108.7 no
C4 . C2 . H21 . 106.9 no
C2 . C3 . H32 . 109.4 no
C2 . C3 . H33 . 108.9 no
H32 . C3 . H33 . 109.1 no
C2 . C3 . H31 . 110.4 no
H32 . C3 . H31 . 110.3 no
H33 . C3 . H31 . 108.8 no
C2 . C4 . C5 . 121.0(4) yes
C2 . C4 . C13 . 121.2(4) yes
C5 . C4 . C13 . 117.7(4) yes
C4 . C5 . C6 . 121.1(4) yes
C4 . C5 . H51 . 118.7 no
C6 . C5 . H51 . 120.2 no
C5 . C6 . C7 . 121.3(4) yes
C5 . C6 . H61 . 120.0 no
C7 . C6 . H61 . 118.8 no
C6 . C7 . C8 . 121.9(4) yes
C6 . C7 . C12 . 117.2(4) yes
C8 . C7 . C12 . 120.9(4) yes
C7 . C8 . C9 . 119.1(4) yes
C7 . C8 . H81 . 120.7 no
C9 . C8 . H81 . 120.2 no
C8 . C9 . O3 . 125.4(4) yes
C8 . C9 . C10 . 119.9(4) yes
O3 . C9 . C10 . 114.6(4) yes
C9 . C10 . C11 . 122.1(4) yes
C9 . C10 . H101 . 118.9 no
C11 . C10 . H101 . 119.1 no
C10 . C11 . C12 . 120.4(5) yes
C10 . C11 . H111 . 120.0 no
C12 . C11 . H111 . 119.5 no
C11 . C12 . C7 . 117.5(4) yes
C11 . C12 . C13 . 122.8(4) yes
C7 . C12 . C13 . 119.6(4) yes
C12 . C13 . C4 . 122.9(5) yes
C12 . C13 . H131 . 118.7 no
C4 . C13 . H131 . 118.4 no
O3 . C14 . H142 . 109.3 no
O3 . C14 . H143 . 109.2 no
H142 . C14 . H143 . 109.4 no
O3 . C14 . H141 . 109.8 no
H142 . C14 . H141 . 109.7 no
H143 . C14 . H141 . 109.3 no
O4 . C15 . O5 . 126.6(4) yes
O4 . C15 . C16 . 115.4(4) yes
O5 . C15 . C16 . 118.0(4) yes
C15 . C16 . C17 . 112.5(4) yes
C15 . C16 . C18 . 111.8(3) yes
C17 . C16 . C18 . 110.1(3) yes
C15 . C16 . H161 . 106.3 no
C17 . C16 . H161 . 109.5 no
C18 . C16 . H161 . 106.4 no
C16 . C17 . H171 . 109.9 no
C16 . C17 . H172 . 110.7 no
H171 . C17 . H172 . 109.1 no
C16 . C17 . H173 . 108.9 no
H171 . C17 . H173 . 109.5 no
H172 . C17 . H173 . 108.8 no
C16 . C18 . C19 . 118.1(4) yes
C16 . C18 . C27 . 123.9(4) yes
C19 . C18 . C27 . 117.9(4) yes
C18 . C19 . C20 . 122.1(4) yes
C18 . C19 . H191 . 118.7 no
C20 . C19 . H191 . 119.1 no
C19 . C20 . C21 . 120.7(4) yes
C19 . C20 . H201 . 119.8 no
C21 . C20 . H201 . 119.6 no
C20 . C21 . C22 . 122.0(5) yes
C20 . C21 . C26 . 117.8(3) yes
C22 . C21 . C26 . 120.1(5) yes
C21 . C22 . C23 . 119.6(5) yes
C21 . C22 . H221 . 119.6 no
C23 . C22 . H221 . 120.9 no
C22 . C23 . O6 . 125.1(5) yes
C22 . C23 . C24 . 120.8(4) yes
O6 . C23 . C24 . 114.1(4) yes
C23 . C24 . C25 . 120.8(4) yes
C23 . C24 . H241 . 119.3 no
C25 . C24 . H241 . 119.9 no
C24 . C25 . C26 . 121.1(4) yes
C24 . C25 . H251 . 119.6 no
C26 . C25 . H251 . 119.4 no
C21 . C26 . C25 . 117.6(3) yes
C21 . C26 . C27 . 118.8(4) yes
C25 . C26 . C27 . 123.6(4) yes
C26 . C27 . C18 . 122.6(4) yes
C26 . C27 . H271 . 118.0 no
C18 . C27 . H271 . 119.3 no
O6 . C28 . H282 . 109.8 no
O6 . C28 . H283 . 110.9 no
H282 . C28 . H283 . 107.8 no
O6 . C28 . H281 . 111.0 no
H282 . C28 . H281 . 108.4 no
H283 . C28 . H281 . 108.8 no
N1 . C29 . C30 . 123.8(4) yes
N1 . C29 . H291 . 117.8 no
C30 . C29 . H291 . 118.4 no
C29 . C30 . C31 . 116.8(5) yes
C29 . C30 . H301 . 121.0 no
C31 . C30 . H301 . 122.2 no
C30 . C31 . C32 . 120.3(5) yes
C30 . C31 . H311 . 118.8 no
C32 . C31 . H311 . 120.9 no
C31 . C32 . C33 . 119.6(4) yes
C31 . C32 . H321 . 120.3 no
C33 . C32 . H321 . 120.1 no
C32 . C33 . N1 . 119.9(4) yes
C32 . C33 . C34 . 123.9(4) yes
N1 . C33 . C34 . 116.2(3) yes
C33 . C34 . N2 . 115.2(3) yes
C33 . C34 . C35 . 124.0(4) yes
N2 . C34 . C35 . 120.8(5) yes
C34 . C35 . C36 . 118.6(4) yes
C34 . C35 . H351 . 119.9 no
C36 . C35 . H351 . 121.6 no
C35 . C36 . C37 . 119.8(4) yes
C35 . C36 . H361 . 119.1 no
C37 . C36 . H361 . 121.0 no
C36 . C37 . C38 . 119.1(5) yes
C36 . C37 . H371 . 120.8 no
C38 . C37 . H371 . 120.1 no
C37 . C38 . N2 . 122.2(4) yes
C37 . C38 . H381 . 120.2 no
N2 . C38 . H381 . 117.6 no
O7 . C39 . H393 . 109.5 no
O7 . C39 . H392 . 109.0 no
H393 . C39 . H392 . 109.0 no
O7 . C39 . H391 . 109.7 no
H393 . C39 . H391 . 108.8 no
H392 . C39 . H391 . 110.8 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
C39 . H391 . O1 1_545 166.12(13) 0.961 2.387 3.328(6) yes
O7 . H71 . O5 . 167.07(18) 0.820 1.699 2.505(6) yes
O7 . H71 . C15 . 140.77(13) 0.820 2.346 3.025(6) yes
C30 . H301 . O3 2_656 136.91(14) 0.927 2.572 3.310(6) yes



