# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 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_nhbndn_sq
_database_code_depnum_ccdc_archive 'CCDC 1493817'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-08-25 downloaded from the CCDC.
;

_nottingham_internal_archive_date ?
_nottingham_internal_coll_client NHB/NRC
_nottingham_internal_coll_date   11/02/2016
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '10.0000, 40.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_name   NHBNDN
_nottingham_internal_coll_number 15629
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_user   pczcrp
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 12/02/2016
_nottingham_internal_process_user pczcrp
_nottingham_internal_refinement_date 12/02/2016
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 12/02/2016
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_solution_date 12/02/2016
_nottingham_internal_solution_user pczcrp
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?

_refine_special_details          
;
Disordered solvent dimethyformamide could not be sensibly modelled and so the 
structure was treated with PLATON SQUEEZE. This which gave an estimate of 255 
electrons per unit cell, corresponding to six dimethylformamide molecules, which 
were included in the formula and calculation of derived parameters.
;

_vrf_CHEMW03_nhbndn_sq           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: PLATON SQUEEZE was used, the removed solvents were included in the formula and calculation of derived parameters.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 0.000 -0.005 892 255 '6(C3 H7 N O)'


_audit_creation_date             2016-02-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H15 N5 Ni O9'
_chemical_formula_sum            'C48 H57 N11 Ni O15'
_chemical_formula_weight         1086.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         C48H24Ni2N2O18
_chemical_oxdiff_usercomment     
'NHBNDN #15629 GVB-894 in fomblin on micromount for NHB/NRC'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.1115(7)
_cell_length_b                   12.5077(8)
_cell_length_c                   16.1965(4)
_cell_angle_alpha                85.612(3)
_cell_angle_beta                 89.685(3)
_cell_angle_gamma                64.385(6)
_cell_volume                     2022.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4146
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.3830
_cell_measurement_theta_min      4.4180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.1555
_exptl_crystal_size_mid          0.0593
_exptl_crystal_size_min          0.0264
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14755
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.645
_diffrn_reflns_theta_min         3.933
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   19.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8292   57.0000  -90.0000 92

#__ type_ start__ end____ width___ exp.time_
  2 omega  132.00  166.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000   30.0000 34

#__ type_ start__ end____ width___ exp.time_
  3 omega  108.00  136.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
  4 omega   64.00  121.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000 -180.0000 57

#__ type_ start__ end____ width___ exp.time_
  5 omega   64.00  108.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
  6 omega   45.00  108.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  -90.0000 63

#__ type_ start__ end____ width___ exp.time_
  7 omega   35.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000    0.0000 74

#__ type_ start__ end____ width___ exp.time_
  8 omega   89.00  117.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  150.0000 28

#__ type_ start__ end____ width___ exp.time_
  9 omega   59.00  126.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000   30.0000 67

#__ type_ start__ end____ width___ exp.time_
 10 omega   97.00  159.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  -90.0000 62

#__ type_ start__ end____ width___ exp.time_
 11 omega  101.00  174.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000 -150.0000 73

#__ type_ start__ end____ width___ exp.time_
 12 omega   41.00   86.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 45

#__ type_ start__ end____ width___ exp.time_
 13 omega   30.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -30.0000 60

#__ type_ start__ end____ width___ exp.time_
 14 omega   41.00   69.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
 15 omega   31.00   66.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -120.0000 35

#__ type_ start__ end____ width___ exp.time_
 16 omega   33.00   72.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -180.0000 39

#__ type_ start__ end____ width___ exp.time_
 17 omega  -69.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   77.0000   30.0000 92

#__ type_ start__ end____ width___ exp.time_
 18 omega   34.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  120.0000 56

#__ type_ start__ end____ width___ exp.time_
 19 omega   31.00   72.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  150.0000 41

#__ type_ start__ end____ width___ exp.time_
 20 omega  -27.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8292  -57.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
 21 omega    8.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -180.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.1131412000
_diffrn_orient_matrix_UB_12      -0.0207722000
_diffrn_orient_matrix_UB_13      0.0427846000
_diffrn_orient_matrix_UB_21      0.0584979000
_diffrn_orient_matrix_UB_22      -0.1270898000
_diffrn_orient_matrix_UB_23      -0.0282580000
_diffrn_orient_matrix_UB_31      0.0862437000
_diffrn_orient_matrix_UB_32      -0.0469274000
_diffrn_orient_matrix_UB_33      0.0805084000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus tube'
_diffrn_source_type              'ROD microfocus tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5761
_reflns_number_total             7891
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7891
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0543
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0716P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1498

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C011(H011), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C019(H019)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni01 Ni 0.35771(5) 0.55059(4) 0.90609(2) 0.02504(13) Uani 1 1 d . . . . .
O002 O 0.5609(2) 0.34747(17) 1.05446(11) 0.0321(4) Uani 1 1 d . . . . .
O003 O 0.4586(2) 0.37529(17) 0.93082(11) 0.0319(4) Uani 1 1 d . . . . .
O004 O 0.1998(2) 0.5389(2) 0.83424(12) 0.0388(5) Uani 1 1 d . . . . .
O005 O 0.1970(2) 0.7104(2) 0.85118(12) 0.0409(5) Uani 1 1 d . . . . .
O006 O 0.8552(2) 0.3695(2) 0.63576(12) 0.0425(5) Uani 1 1 d . . . . .
O007 O 1.2014(2) 0.3676(3) 0.26959(12) 0.0489(6) Uani 1 1 d . . . . .
O008 O 0.8485(2) 0.7046(3) 0.16656(13) 0.0498(6) Uani 1 1 d . . . . .
N009 N 0.4625(2) 0.5369(2) 0.79752(12) 0.0297(5) Uani 1 1 d . . . . .
N00A N 1.2458(2) 0.5542(2) 0.01093(13) 0.0313(5) Uani 1 1 d . . . . .
O00B O 0.4729(2) 0.6504(3) 0.50812(13) 0.0569(7) Uani 1 1 d . . . . .
N00C N 1.0254(2) 0.5395(3) 0.22035(13) 0.0379(6) Uani 1 1 d . . . . .
N00D N 0.6658(2) 0.5165(2) 0.57491(13) 0.0353(5) Uani 1 1 d . . . . .
N00E N 0.1417(3) 0.6508(3) 0.82076(15) 0.0441(6) Uani 1 1 d . . . . .
C00F C 0.5136(3) 0.3150(2) 0.99655(15) 0.0267(5) Uani 1 1 d . . . . .
O00G O 0.0359(3) 0.6998(3) 0.78058(19) 0.0733(9) Uani 1 1 d . . . . .
C00H C 0.4572(3) 0.0408(3) 0.96862(16) 0.0296(5) Uani 1 1 d . . . . .
C00I C 0.4508(3) 0.1567(2) 0.95718(16) 0.0310(5) Uani 1 1 d . . . . .
H00I H 0.3955 0.2111 0.9139 0.037 Uiso 1 1 calc R . . . .
C00J C 0.5235(3) 0.1912(2) 1.00785(16) 0.0303(6) Uani 1 1 d . . . . .
C00K C 0.8800(3) 0.5264(3) 0.35986(16) 0.0362(6) Uani 1 1 d . . . . .
C00L C 0.5947(3) 0.5231(3) 0.65069(16) 0.0342(6) Uani 1 1 d . . . . .
C00M C 0.6733(3) 0.6045(3) 0.43476(16) 0.0400(7) Uani 1 1 d . . . . .
C00N C 0.8067(3) 0.5219(3) 0.43068(16) 0.0354(6) Uani 1 1 d . . . . .
C00O C 1.0117(3) 0.4396(3) 0.35456(17) 0.0391(7) Uani 1 1 d . . . . .
C00P C 0.5162(3) 0.4352(3) 0.75998(16) 0.0331(6) Uani 1 1 d . . . . .
H00P H 0.5066 0.3680 0.7847 0.040 Uiso 1 1 calc R . . . .
C00Q C 1.1911(3) 0.4766(3) 0.01988(16) 0.0360(6) Uani 1 1 d . . . . .
H00Q H 1.2031 0.4249 -0.0226 0.043 Uiso 1 1 calc R . . . .
C00R C 0.5847(3) 0.4231(3) 0.68703(17) 0.0375(6) Uani 1 1 d . . . . .
H00R H 0.6234 0.3493 0.6627 0.045 Uiso 1 1 calc R . . . .
C00S C 0.4759(3) 0.6311(3) 0.76189(16) 0.0350(6) Uani 1 1 d . . . . .
H00S H 0.4392 0.7032 0.7883 0.042 Uiso 1 1 calc R . . . .
C00T C 0.8944(3) 0.6267(3) 0.22248(17) 0.0390(7) Uani 1 1 d . . . . .
C00U C 1.1013(3) 0.5439(3) 0.14881(16) 0.0390(7) Uani 1 1 d . . . . .
C00V C 0.7993(3) 0.4351(3) 0.57448(16) 0.0355(6) Uani 1 1 d . . . . .
C00W C 0.5935(3) 0.5961(3) 0.50656(17) 0.0413(7) Uani 1 1 d . . . . .
C00X C 0.8709(3) 0.4327(3) 0.49627(16) 0.0356(6) Uani 1 1 d . . . . .
C00Y C 0.5406(3) 0.6283(3) 0.68845(17) 0.0382(6) Uani 1 1 d . . . . .
H00Y H 0.5476 0.6971 0.6646 0.046 Uiso 1 1 calc R . . . .
C00Z C 1.0722(3) 0.3523(3) 0.41771(18) 0.0398(7) Uani 1 1 d . . . . .
H00Z H 1.1613 0.2938 0.4128 0.048 Uiso 1 1 calc R . . . .
C010 C 1.1190(3) 0.4687(3) 0.08725(17) 0.0377(6) Uani 1 1 d . . . . .
H010 H 1.0822 0.4127 0.0913 0.045 Uiso 1 1 calc R . . . .
C011 C 0.3909(3) -0.1093(3) 0.92876(18) 0.0351(6) Uani 1 1 d . . . . .
H011 H 0.3398 -0.1330 0.8940 0.042 Uiso 1 1 calc R . . . .
C012 C 0.8179(3) 0.6199(3) 0.29680(16) 0.0390(7) Uani 1 1 d . . . . .
C013 C 1.0891(3) 0.4415(3) 0.27996(16) 0.0411(7) Uani 1 1 d . . . . .
C014 C 1.2270(3) 0.6269(3) 0.07137(18) 0.0450(8) Uani 1 1 d . . . . .
H014 H 1.2641 0.6826 0.0659 0.054 Uiso 1 1 calc R . . . .
C015 C 0.3817(3) 0.0031(3) 0.91752(18) 0.0358(6) Uani 1 1 d . . . . .
H015 H 0.3240 0.0571 0.8749 0.043 Uiso 1 1 calc R . . . .
C016 C 0.6140(3) 0.6943(4) 0.37262(18) 0.0451(7) Uani 1 1 d . . . . .
H016 H 0.5238 0.7509 0.3765 0.054 Uiso 1 1 calc R . . . .
C017 C 1.0013(3) 0.3503(3) 0.48970(18) 0.0402(7) Uani 1 1 d . . . . .
H017 H 1.0438 0.2915 0.5341 0.048 Uiso 1 1 calc R . . . .
C018 C 0.6882(3) 0.7016(3) 0.30347(18) 0.0450(7) Uani 1 1 d . . . . .
H018 H 0.6478 0.7639 0.2609 0.054 Uiso 1 1 calc R . . . .
C019 C 1.1557(4) 0.6244(4) 0.14174(19) 0.0506(9) Uani 1 1 d . . . . .
H019 H 1.1448 0.6767 0.1837 0.061 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni01 O002 1.9945(18) 2_667 ?
Ni01 O003 1.993(2) . ?
Ni01 O004 2.1738(19) . ?
Ni01 O005 2.153(2) . ?
Ni01 N009 2.081(2) . ?
Ni01 N00A 2.091(2) 1_456 ?
O002 Ni01 1.9945(18) 2_667 ?
O002 C00F 1.253(3) . ?
O003 C00F 1.249(3) . ?
O004 N00E 1.263(4) . ?
O005 N00E 1.278(4) . ?
O006 C00V 1.219(4) . ?
O007 C013 1.210(4) . ?
O008 C00T 1.212(4) . ?
N009 C00P 1.342(4) . ?
N009 C00S 1.338(4) . ?
N00A Ni01 2.091(2) 1_654 ?
N00A C00Q 1.349(4) . ?
N00A C014 1.341(4) . ?
O00B C00W 1.213(4) . ?
N00C C00T 1.394(4) . ?
N00C C00U 1.441(3) . ?
N00C C013 1.419(5) . ?
N00D C00L 1.444(3) . ?
N00D C00V 1.390(4) . ?
N00D C00W 1.418(4) . ?
N00E O00G 1.227(4) . ?
C00F C00J 1.502(4) . ?
C00H C00H 1.412(6) 2_657 ?
C00H C00I 1.418(4) . ?
C00H C015 1.421(4) . ?
C00I H00I 0.9500 . ?
C00I C00J 1.369(4) . ?
C00J C011 1.420(4) 2_657 ?
C00K C00N 1.415(4) . ?
C00K C00O 1.402(5) . ?
C00K C012 1.419(5) . ?
C00L C00R 1.389(4) . ?
C00L C00Y 1.379(5) . ?
C00M C00N 1.398(5) . ?
C00M C00W 1.483(4) . ?
C00M C016 1.379(5) . ?
C00N C00X 1.421(5) . ?
C00O C00Z 1.375(5) . ?
C00O C013 1.484(4) . ?
C00P H00P 0.9500 . ?
C00P C00R 1.385(4) . ?
C00Q H00Q 0.9500 . ?
C00Q C010 1.373(4) . ?
C00R H00R 0.9500 . ?
C00S H00S 0.9500 . ?
C00S C00Y 1.381(4) . ?
C00T C012 1.488(4) . ?
C00U C010 1.378(4) . ?
C00U C019 1.379(5) . ?
C00V C00X 1.488(4) . ?
C00X C017 1.377(5) . ?
C00Y H00Y 0.9500 . ?
C00Z H00Z 0.9500 . ?
C00Z C017 1.408(4) . ?
C010 H010 0.9500 . ?
C011 C00J 1.419(4) 2_657 ?
C011 H011 0.9500 . ?
C011 C015 1.363(4) . ?
C012 C018 1.369(5) . ?
C014 H014 0.9500 . ?
C014 C019 1.391(4) . ?
C015 H015 0.9500 . ?
C016 H016 0.9500 . ?
C016 C018 1.407(4) . ?
C017 H017 0.9500 . ?
C018 H018 0.9500 . ?
C019 H019 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O002 Ni01 O004 147.90(9) 2_667 . ?
O002 Ni01 O005 87.82(9) 2_667 . ?
O002 Ni01 N009 88.62(8) 2_667 . ?
O002 Ni01 N00A 96.57(8) 2_667 1_456 ?
O003 Ni01 O002 117.37(8) . 2_667 ?
O003 Ni01 O004 94.52(9) . . ?
O003 Ni01 O005 154.72(8) . . ?
O003 Ni01 N009 89.00(9) . . ?
O003 Ni01 N00A 88.47(9) . 1_456 ?
O005 Ni01 O004 60.21(9) . . ?
N009 Ni01 O004 88.37(8) . . ?
N009 Ni01 O005 89.57(9) . . ?
N009 Ni01 N00A 174.81(9) . 1_456 ?
N00A Ni01 O004 87.32(8) 1_456 . ?
N00A Ni01 O005 90.79(9) 1_456 . ?
C00F O002 Ni01 149.76(17) . 2_667 ?
C00F O003 Ni01 130.78(16) . . ?
N00E O004 Ni01 90.96(16) . . ?
N00E O005 Ni01 91.51(18) . . ?
C00P N009 Ni01 121.68(17) . . ?
C00S N009 Ni01 120.46(19) . . ?
C00S N009 C00P 117.8(2) . . ?
C00Q N00A Ni01 118.26(18) . 1_654 ?
C014 N00A Ni01 124.36(19) . 1_654 ?
C014 N00A C00Q 117.4(2) . . ?
C00T N00C C00U 117.6(3) . . ?
C00T N00C C013 125.9(2) . . ?
C013 N00C C00U 116.4(3) . . ?
C00V N00D C00L 118.2(2) . . ?
C00V N00D C00W 124.9(2) . . ?
C00W N00D C00L 116.8(3) . . ?
O004 N00E O005 117.3(2) . . ?
O00G N00E O004 121.1(3) . . ?
O00G N00E O005 121.6(3) . . ?
O002 C00F C00J 116.4(2) . . ?
O003 C00F O002 126.7(2) . . ?
O003 C00F C00J 116.9(2) . . ?
C00H C00H C00I 119.4(3) 2_657 . ?
C00H C00H C015 118.7(3) 2_657 . ?
C00I C00H C015 121.9(3) . . ?
C00H C00I H00I 119.6 . . ?
C00J C00I C00H 120.7(3) . . ?
C00J C00I H00I 119.6 . . ?
C00I C00J C00F 120.4(3) . . ?
C00I C00J C011 119.9(2) . 2_657 ?
C011 C00J C00F 119.7(2) 2_657 . ?
C00N C00K C012 118.6(3) . . ?
C00O C00K C00N 119.2(3) . . ?
C00O C00K C012 122.2(3) . . ?
C00R C00L N00D 120.4(3) . . ?
C00Y C00L N00D 119.6(3) . . ?
C00Y C00L C00R 120.0(3) . . ?
C00N C00M C00W 119.9(3) . . ?
C016 C00M C00N 120.9(3) . . ?
C016 C00M C00W 119.2(3) . . ?
C00K C00N C00X 118.9(3) . . ?
C00M C00N C00K 119.6(3) . . ?
C00M C00N C00X 121.5(3) . . ?
C00K C00O C013 119.9(3) . . ?
C00Z C00O C00K 121.4(3) . . ?
C00Z C00O C013 118.7(3) . . ?
N009 C00P H00P 118.3 . . ?
N009 C00P C00R 123.3(3) . . ?
C00R C00P H00P 118.3 . . ?
N00A C00Q H00Q 118.3 . . ?
N00A C00Q C010 123.3(3) . . ?
C010 C00Q H00Q 118.3 . . ?
C00L C00R H00R 121.3 . . ?
C00P C00R C00L 117.5(3) . . ?
C00P C00R H00R 121.3 . . ?
N009 C00S H00S 118.5 . . ?
N009 C00S C00Y 123.0(3) . . ?
C00Y C00S H00S 118.5 . . ?
O008 C00T N00C 120.3(3) . . ?
O008 C00T C012 123.0(3) . . ?
N00C C00T C012 116.6(3) . . ?
C010 C00U N00C 120.4(3) . . ?
C010 C00U C019 119.9(3) . . ?
C019 C00U N00C 119.7(3) . . ?
O006 C00V N00D 121.4(2) . . ?
O006 C00V C00X 121.6(3) . . ?
N00D C00V C00X 117.0(3) . . ?
O00B C00W N00D 120.2(3) . . ?
O00B C00W C00M 123.6(3) . . ?
N00D C00W C00M 116.2(3) . . ?
C00N C00X C00V 119.2(3) . . ?
C017 C00X C00N 120.3(3) . . ?
C017 C00X C00V 120.3(3) . . ?
C00L C00Y C00S 118.3(3) . . ?
C00L C00Y H00Y 120.9 . . ?
C00S C00Y H00Y 120.9 . . ?
C00O C00Z H00Z 120.2 . . ?
C00O C00Z C017 119.5(3) . . ?
C017 C00Z H00Z 120.2 . . ?
C00Q C010 C00U 118.4(3) . . ?
C00Q C010 H010 120.8 . . ?
C00U C010 H010 120.8 . . ?
C00J C011 H011 119.8 2_657 . ?
C015 C011 C00J 120.3(2) . 2_657 ?
C015 C011 H011 119.8 . . ?
C00K C012 C00T 119.2(3) . . ?
C018 C012 C00K 120.4(3) . . ?
C018 C012 C00T 120.3(3) . . ?
O007 C013 N00C 120.2(2) . . ?
O007 C013 C00O 123.8(3) . . ?
N00C C013 C00O 115.9(3) . . ?
N00A C014 H014 118.5 . . ?
N00A C014 C019 123.0(3) . . ?
C019 C014 H014 118.5 . . ?
C00H C015 H015 119.5 . . ?
C011 C015 C00H 121.0(3) . . ?
C011 C015 H015 119.5 . . ?
C00M C016 H016 120.2 . . ?
C00M C016 C018 119.5(3) . . ?
C018 C016 H016 120.2 . . ?
C00X C017 C00Z 120.5(3) . . ?
C00X C017 H017 119.7 . . ?
C00Z C017 H017 119.7 . . ?
C012 C018 C016 120.8(3) . . ?
C012 C018 H018 119.6 . . ?
C016 C018 H018 119.6 . . ?
C00U C019 C014 118.0(3) . . ?
C00U C019 H019 121.0 . . ?
C014 C019 H019 121.0 . . ?

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
Ni01 O002 C00F O003 -26.8(6) 2_667 . . . ?
Ni01 O002 C00F C00J 153.5(3) 2_667 . . . ?
Ni01 O003 C00F O002 -28.1(4) . . . . ?
Ni01 O003 C00F C00J 151.56(19) . . . . ?
Ni01 O004 N00E O005 0.6(2) . . . . ?
Ni01 O004 N00E O00G -178.8(3) . . . . ?
Ni01 O005 N00E O004 -0.6(3) . . . . ?
Ni01 O005 N00E O00G 178.8(3) . . . . ?
Ni01 N009 C00P C00R 178.9(2) . . . . ?
Ni01 N009 C00S C00Y -177.9(2) . . . . ?
Ni01 N00A C00Q C010 178.1(2) 1_654 . . . ?
Ni01 N00A C014 C019 -177.8(3) 1_654 . . . ?
O002 C00F C00J C00I 166.1(3) . . . . ?
O002 C00F C00J C011 -14.1(4) . . . 2_657 ?
O003 C00F C00J C00I -13.5(4) . . . . ?
O003 C00F C00J C011 166.2(3) . . . 2_657 ?
O006 C00V C00X C00N -171.3(3) . . . . ?
O006 C00V C00X C017 4.1(4) . . . . ?
O008 C00T C012 C00K -179.2(3) . . . . ?
O008 C00T C012 C018 2.0(5) . . . . ?
N009 C00P C00R C00L -1.6(5) . . . . ?
N009 C00S C00Y C00L -0.5(5) . . . . ?
N00A C00Q C010 C00U 0.1(5) . . . . ?
N00A C014 C019 C00U -0.5(6) . . . . ?
N00C C00T C012 C00K -0.7(4) . . . . ?
N00C C00T C012 C018 -179.5(3) . . . . ?
N00C C00U C010 C00Q 179.5(3) . . . . ?
N00C C00U C019 C014 -179.3(3) . . . . ?
N00D C00L C00R C00P 179.5(3) . . . . ?
N00D C00L C00Y C00S -178.5(3) . . . . ?
N00D C00V C00X C00N 8.0(4) . . . . ?
N00D C00V C00X C017 -176.6(3) . . . . ?
C00H C00H C00I C00J -2.0(5) 2_657 . . . ?
C00H C00H C015 C011 0.3(5) 2_657 . . . ?
C00H C00I C00J C00F -178.5(2) . . . . ?
C00H C00I C00J C011 1.7(4) . . . 2_657 ?
C00I C00H C015 C011 179.0(3) . . . . ?
C00J C011 C015 C00H 0.0(5) 2_657 . . . ?
C00K C00N C00X C00V 173.6(3) . . . . ?
C00K C00N C00X C017 -1.7(4) . . . . ?
C00K C00O C00Z C017 -0.5(5) . . . . ?
C00K C00O C013 O007 -177.5(3) . . . . ?
C00K C00O C013 N00C 4.8(4) . . . . ?
C00K C012 C018 C016 -0.2(5) . . . . ?
C00L N00D C00V O006 1.0(4) . . . . ?
C00L N00D C00V C00X -178.4(2) . . . . ?
C00L N00D C00W O00B -12.9(5) . . . . ?
C00L N00D C00W C00M 168.9(3) . . . . ?
C00M C00N C00X C00V -6.5(4) . . . . ?
C00M C00N C00X C017 178.2(3) . . . . ?
C00M C016 C018 C012 0.7(5) . . . . ?
C00N C00K C00O C00Z -1.9(4) . . . . ?
C00N C00K C00O C013 178.7(3) . . . . ?
C00N C00K C012 C00T 179.2(3) . . . . ?
C00N C00K C012 C018 -2.0(4) . . . . ?
C00N C00M C00W O00B -166.8(3) . . . . ?
C00N C00M C00W N00D 11.4(4) . . . . ?
C00N C00M C016 C018 1.1(5) . . . . ?
C00N C00X C017 C00Z -0.7(5) . . . . ?
C00O C00K C00N C00M -176.9(3) . . . . ?
C00O C00K C00N C00X 3.0(4) . . . . ?
C00O C00K C012 C00T -0.1(4) . . . . ?
C00O C00K C012 C018 178.7(3) . . . . ?
C00O C00Z C017 C00X 1.9(5) . . . . ?
C00P N009 C00S C00Y 0.7(4) . . . . ?
C00Q N00A C014 C019 0.6(5) . . . . ?
C00R C00L C00Y C00S -0.7(4) . . . . ?
C00S N009 C00P C00R 0.4(4) . . . . ?
C00T N00C C00U C010 -101.3(4) . . . . ?
C00T N00C C00U C019 78.2(4) . . . . ?
C00T N00C C013 O007 176.2(3) . . . . ?
C00T N00C C013 C00O -6.1(4) . . . . ?
C00T C012 C018 C016 178.6(3) . . . . ?
C00U N00C C00T O008 -1.8(4) . . . . ?
C00U N00C C00T C012 179.7(3) . . . . ?
C00U N00C C013 O007 0.5(4) . . . . ?
C00U N00C C013 C00O 178.3(2) . . . . ?
C00V N00D C00L C00R -58.3(4) . . . . ?
C00V N00D C00L C00Y 119.5(3) . . . . ?
C00V N00D C00W O00B 168.3(3) . . . . ?
C00V N00D C00W C00M -10.0(5) . . . . ?
C00V C00X C017 C00Z -176.0(3) . . . . ?
C00W N00D C00L C00R 122.8(3) . . . . ?
C00W N00D C00L C00Y -59.4(4) . . . . ?
C00W N00D C00V O006 179.8(3) . . . . ?
C00W N00D C00V C00X 0.5(4) . . . . ?
C00W C00M C00N C00K 176.5(3) . . . . ?
C00W C00M C00N C00X -3.5(5) . . . . ?
C00W C00M C016 C018 -178.7(3) . . . . ?
C00Y C00L C00R C00P 1.7(4) . . . . ?
C00Z C00O C013 O007 3.1(5) . . . . ?
C00Z C00O C013 N00C -174.6(3) . . . . ?
C010 C00U C019 C014 0.3(6) . . . . ?
C012 C00K C00N C00M 3.8(4) . . . . ?
C012 C00K C00N C00X -176.3(3) . . . . ?
C012 C00K C00O C00Z 177.4(3) . . . . ?
C012 C00K C00O C013 -2.0(4) . . . . ?
C013 N00C C00T O008 -177.4(3) . . . . ?
C013 N00C C00T C012 4.0(4) . . . . ?
C013 N00C C00U C010 74.7(4) . . . . ?
C013 N00C C00U C019 -105.7(4) . . . . ?
C013 C00O C00Z C017 178.9(3) . . . . ?
C014 N00A C00Q C010 -0.4(5) . . . . ?
C015 C00H C00I C00J 179.3(3) . . . . ?
C016 C00M C00N C00K -3.4(5) . . . . ?
C016 C00M C00N C00X 176.7(3) . . . . ?
C016 C00M C00W O00B 13.0(5) . . . . ?
C016 C00M C00W N00D -168.7(3) . . . . ?
C019 C00U C010 C00Q -0.1(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2 0 -5 0.0773 -1.9916 0.0049 -4.9979 0.0114 0.0241 -0.5744
2 0 5 0.0773 1.9916 -0.0049 4.9979 -0.0114 -0.0241 0.5744
0 2 2 0.0444 -0.0063 2.4941 2.0018 0.0346 -0.3739 0.0436
0 -2 -2 0.0444 0.0063 -2.4941 -2.0018 -0.0346 0.3739 -0.0436
5 5 -5 0.0299 4.9924 4.5062 -4.9937 -0.8721 -0.1395 -0.1829
-5 -5 5 0.0299 -4.9924 -4.5062 4.9937 0.8721 0.1395 0.1829
1 -2 -1 0.0254 1.0031 -1.9951 -1.0017 -0.1149 0.3405 0.0995
-1 2 1 0.0254 -1.0031 1.9951 1.0017 0.1149 -0.3405 -0.0995
0 2 3 0.0295 -0.0075 2.4927 3.0014 0.0775 -0.4020 0.1240
0 -2 -3 0.0295 0.0075 -2.4927 -3.0014 -0.0775 0.4020 -0.1240
3 4 -1 0.0132 2.9910 3.9993 -0.9957 -0.4641 -0.3052 -0.0099
-3 -4 1 0.0132 -2.9910 -3.9993 0.9957 0.4641 0.3052 0.0099


_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_nhbnfr_sq
_database_code_depnum_ccdc_archive 'CCDC 1493815'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-08-25 downloaded from the CCDC.
;
_nottingham_internal_coll_name   NHBNFR
_nottingham_internal_coll_number 16240
_nottingham_internal_coll_client NHB/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 20.00, 80.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pczcrp
_nottingham_internal_coll_date   18/06/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 19/06/2016
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 19/06/2016
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 19/06/2016
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 19/06/2016
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          
;
Disordered solvent dimethylformamide and water could not be 
sensibly modelled and so the structure was processed using 
PLATON SQUEEZE, which gave an estimate 856 e- of per cell, 
corresponding to about four water molecules and twenty 
dimethylformamide molecules per unit cell. These molecules 
were included in the sum formula and the calculation of 
derived parameters. The nitrate group is disordered over 
two positions and the occupancies were refined competitively, 
converging to a ratio of 0.31:0.69. Enhanced rigid bond and 
similarity restraints were applied to the thermal parameters 
of the disordered atoms.
;
_vrf_CHEMW03_nhbnfr_sq           
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: PLATON SQUEEZE was used, the removed solvents were included in the formula and calculation of derived parameters.
;
_audit_creation_date             2016-06-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H26 N8 Ni O12'
_chemical_formula_sum            'C90 H174 N28 Ni O36'
_chemical_formula_weight         2283.27
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C48H24O12N4Ni2
_chemical_oxdiff_usercomment     
'NHBNFR 16240 GVB-1074 IN FOMBLIN FILM ON MICROMOUNT FOR CRP/NRC'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   19.5137(6)
_cell_length_b                   19.5137(6)
_cell_length_c                   22.1533(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8435.7(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5227
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.1190
_cell_measurement_theta_min      5.1250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.596
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             9808
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 4 -5 0.0667
0 -4 5 0.0667
-5 1 0 0.0772
5 -1 0 0.0772
1 5 5 0.0788
-1 -5 -5 0.0458
-6 10 4 0.0961
4 -11 -6 0.0464
9 4 9 0.0907
10 4 -8 0.0758
9 5 -9 0.0763
-10 -4 8 0.0741

_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.125
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0003 3.9939 -5.0013 -0.4033 0.0828 -0.2277
0.0003 -3.9939 5.0013 0.4033 -0.0828 0.2277
-4.9995 0.9930 -0.0018 0.1452 -0.0233 -0.3746
4.9995 -0.9930 0.0018 -0.1452 0.0233 0.3746
0.9848 5.0023 5.0076 -0.1092 -0.5196 -0.0100
-0.9848 -5.0023 -5.0076 0.1092 0.5196 0.0100
-6.0192 9.9897 4.0065 -0.1336 -0.6700 -0.6750
4.0243 -10.9932 -6.0097 0.1880 0.8378 0.5360
8.9779 4.0162 9.0140 -0.2185 -0.7310 0.6424
9.9991 4.0044 -7.9987 -0.9147 0.1982 0.3984
8.9991 5.0018 -8.9993 -0.9663 0.2101 0.2780
-9.9991 -4.0044 7.9987 0.9147 -0.1982 -0.3984

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9272
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.397
_diffrn_reflns_theta_min         4.532
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      6.00  35.00   1.00   20.00    --  -38.50  77.00 -60.00   29
  2  ω    -70.00  17.00   1.00   20.00    --  -38.50  77.00 150.00   87
  3  ω     73.00 172.00   1.00   80.00    --  104.50  77.00-180.00   99
  4  ω     81.00 163.00   1.00   80.00    --  104.50  77.00 150.00   82
  5  ω    136.00 163.00   1.00   80.00    --  104.50  77.00 -90.00   27
  6  ω     83.00 126.00   1.00   80.00    --  104.50  77.00 -90.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0395204000
_diffrn_orient_matrix_UB_12      -0.0526642000
_diffrn_orient_matrix_UB_13      0.0385825000
_diffrn_orient_matrix_UB_21      -0.0048600000
_diffrn_orient_matrix_UB_22      -0.0479910000
_diffrn_orient_matrix_UB_23      -0.0548759000
_diffrn_orient_matrix_UB_31      0.0681818000
_diffrn_orient_matrix_UB_32      -0.0338903000
_diffrn_orient_matrix_UB_33      0.0184559000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Agilent diffraction microfocus sealed tube'
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                3408
_reflns_number_total             3635
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3635
_refine_ls_number_restraints     489
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0745
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1119P)²+23.4050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2036
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.83(9) 0.17(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(N6A)=1-FVAR(1)
 Sof(O4)=Sof(O5)=Sof(O6)=Sof(N6)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C13(H13), C14(H14), C15(H15)
6.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.7500 1.14491(7) 0.3750 0.0387(5) Uani 1 2 d S TU P . .
O1 O 0.6702(2) 0.8278(2) 0.4490(2) 0.0375(11) Uani 1 1 d . U . . .
O2 O 0.6739(3) 0.4644(2) 0.4530(2) 0.0343(10) Uani 1 1 d . U . . .
O3 O 0.6443(3) 1.1438(3) 0.3648(3) 0.0519(13) Uani 1 1 d . U . . .
N1 N 0.7500 1.0395(4) 0.3750 0.0437(19) Uani 1 2 d S TU P A .
N2 N 0.7500 0.8246(3) 0.3750 0.0315(16) Uani 1 2 d S TU P . .
N3 N 0.7500 0.4661(3) 0.3750 0.0252(14) Uani 1 2 d S TU P . .
N4 N 0.7500 0.2514(4) 0.3750 0.0365(16) Uani 1 2 d S TU P . .
N5 N 0.5386(4) 1.1815(5) 0.3867(5) 0.079(2) Uani 1 1 d . U . . .
C1 C 0.7072(4) 1.0049(3) 0.3403(4) 0.0480(18) Uani 1 1 d . U . . .
H1 H 0.6758 1.0298 0.3158 0.058 Uiso 1 1 calc R . . A .
C2 C 0.7061(4) 0.9334(3) 0.3381(4) 0.0468(17) Uani 1 1 d . U . . .
H2 H 0.6758 0.9097 0.3117 0.056 Uiso 1 1 calc R . . . .
C3 C 0.7500 0.8988(4) 0.3750 0.039(2) Uani 1 2 d S TU P . .
C4 C 0.7059(3) 0.7919(3) 0.4168(3) 0.0287(12) Uani 1 1 d . U . . .
C5 C 0.7082(3) 0.7170(3) 0.4166(3) 0.0216(11) Uani 1 1 d . U . . .
C6 C 0.6676(3) 0.6815(3) 0.4570(3) 0.0278(12) Uani 1 1 d . U . . .
H6 H 0.6393 0.7059 0.4844 0.033 Uiso 1 1 calc R . . . .
C7 C 0.6678(3) 0.6104(3) 0.4576(3) 0.0279(12) Uani 1 1 d . U . . .
H7 H 0.6401 0.5863 0.4858 0.033 Uiso 1 1 calc R . . . .
C8 C 0.7082(3) 0.5744(3) 0.4171(3) 0.0204(10) Uani 1 1 d . U . . .
C9 C 0.7500 0.6092(4) 0.3750 0.0227(15) Uani 1 2 d S TU P . .
C10 C 0.7500 0.6815(3) 0.3750 0.0232(15) Uani 1 2 d S TU P . .
C11 C 0.7081(3) 0.4984(3) 0.4165(3) 0.0269(12) Uani 1 1 d . U . . .
C12 C 0.7500 0.3932(4) 0.3750 0.0267(16) Uani 1 2 d S TU P . .
C13 C 0.7072(3) 0.3578(3) 0.3362(3) 0.0349(13) Uani 1 1 d . U . . .
H13 H 0.6775 0.3813 0.3094 0.042 Uiso 1 1 calc R . . . .
C14 C 0.7092(4) 0.2865(3) 0.3378(3) 0.0337(13) Uani 1 1 d . U . . .
H14 H 0.6802 0.2617 0.3112 0.040 Uiso 1 1 calc R . . . .
C15 C 0.6036(4) 1.1750(4) 0.3977(5) 0.054(2) Uani 1 1 d . U . . .
H15 H 0.6211 1.1955 0.4334 0.065 Uiso 1 1 calc R . . . .
C16 C 0.4950(6) 1.2217(7) 0.4274(6) 0.084(3) Uani 1 1 d . U . . .
H16A H 0.4660 1.1907 0.4511 0.125 Uiso 1 1 calc GR . . . .
H16B H 0.4659 1.2525 0.4036 0.125 Uiso 1 1 calc GR . . . .
H16C H 0.5238 1.2487 0.4547 0.125 Uiso 1 1 calc GR . . . .
C17 C 0.5077(7) 1.1425(9) 0.3361(7) 0.107(4) Uani 1 1 d . U . . .
H17A H 0.5039 1.1723 0.3006 0.160 Uiso 1 1 calc GR . . . .
H17B H 0.4620 1.1266 0.3478 0.160 Uiso 1 1 calc GR . . . .
H17C H 0.5367 1.1030 0.3264 0.160 Uiso 1 1 calc GR . . . .
O4 O 0.7608(13) 1.1529(14) 0.4720(10) 0.054(4) Uani 0.315(12) 1 d . U . A 1
O5 O 0.7571(18) 1.1193(18) 0.5620(15) 0.070(4) Uani 0.315(12) 1 d . U . A 1
O6 O 0.6879(14) 1.0852(13) 0.4975(11) 0.072(3) Uani 0.315(12) 1 d . U . A 1
N6 N 0.728(2) 1.1159(19) 0.5110(18) 0.065(4) Uani 0.315(12) 1 d . U . A 1
O4A O 0.7249(7) 1.1435(7) 0.4646(5) 0.062(2) Uani 0.685(12) 1 d . U . A 2
O5A O 0.8171(7) 1.1557(7) 0.5088(5) 0.083(3) Uani 0.685(12) 1 d . U . A 2
O6A O 0.7260(8) 1.1151(8) 0.5580(6) 0.069(3) Uani 0.685(12) 1 d . U . A 2
N6A N 0.7520(10) 1.1311(7) 0.5102(7) 0.067(3) Uani 0.685(12) 1 d . U . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O3 2.075(6) . ?
Ni1 O3 2.075(6) 5_655 ?
Ni1 N1 2.058(7) . ?
Ni1 N4 2.078(7) 1_565 ?
Ni1 O4 2.16(2) . ?
Ni1 O4 2.16(2) 5_655 ?
Ni1 O4A 2.046(9) 5_655 ?
Ni1 O4A 2.046(9) . ?
O1 C4 1.219(7) . ?
O2 C11 1.241(7) . ?
O3 C15 1.239(10) . ?
N1 C1 1.320(9) 5_655 ?
N1 C1 1.320(9) . ?
N2 C3 1.448(9) . ?
N2 C4 1.417(7) . ?
N2 C4 1.417(7) 5_655 ?
N3 C11 1.382(7) 5_655 ?
N3 C11 1.383(6) . ?
N3 C12 1.424(9) . ?
N4 Ni1 2.078(7) 1_545 ?
N4 C14 1.335(8) . ?
N4 C14 1.335(8) 5_655 ?
N5 C15 1.296(12) . ?
N5 C16 1.468(13) . ?
N5 C17 1.483(17) . ?
C1 H1 0.9500 . ?
C1 C2 1.397(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.364(9) . ?
C3 C2 1.364(10) 5_655 ?
C4 C5 1.461(7) . ?
C5 C6 1.381(8) . ?
C5 C10 1.413(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.384(8) . ?
C8 C9 1.414(6) . ?
C8 C11 1.482(7) . ?
C9 C8 1.414(6) 5_655 ?
C9 C10 1.412(9) . ?
C10 C5 1.413(6) 5_655 ?
C12 C13 1.383(8) 5_655 ?
C12 C13 1.383(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.392(9) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O4 N6 1.30(4) . ?
O5 N6 1.27(6) . ?
O6 N6 1.02(4) . ?
O4A N6A 1.16(2) . ?
O5A N6A 1.36(2) . ?
O6A N6A 1.22(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ni1 O3 178.8(3) . 5_655 ?
O3 Ni1 N4 90.59(14) . 1_565 ?
O3 Ni1 N4 90.59(14) 5_655 1_565 ?
O3 Ni1 O4 101.9(7) 5_655 5_655 ?
O3 Ni1 O4 78.2(7) . 5_655 ?
O3 Ni1 O4 78.2(7) 5_655 . ?
O3 Ni1 O4 101.9(7) . . ?
N1 Ni1 O3 89.41(14) . . ?
N1 Ni1 O3 89.41(14) . 5_655 ?
N1 Ni1 N4 180.0 . 1_565 ?
N1 Ni1 O4 94.1(7) . . ?
N1 Ni1 O4 94.1(7) . 5_655 ?
N4 Ni1 O4 85.9(7) 1_565 5_655 ?
N4 Ni1 O4 85.9(7) 1_565 . ?
O4 Ni1 O4 171.8(15) . 5_655 ?
O4A Ni1 O3 97.6(4) 5_655 . ?
O4A Ni1 O3 82.4(4) . . ?
O4A Ni1 O3 97.6(4) . 5_655 ?
O4A Ni1 O3 82.4(4) 5_655 5_655 ?
O4A Ni1 N1 89.2(4) . . ?
O4A Ni1 N1 89.2(4) 5_655 . ?
O4A Ni1 N4 90.8(4) 5_655 1_565 ?
O4A Ni1 N4 90.8(4) . 1_565 ?
O4A Ni1 O4A 178.4(8) 5_655 . ?
C15 O3 Ni1 124.7(6) . . ?
C1 N1 Ni1 120.7(4) . . ?
C1 N1 Ni1 120.7(4) 5_655 . ?
C1 N1 C1 118.6(8) 5_655 . ?
C4 N2 C3 116.8(3) 5_655 . ?
C4 N2 C3 116.8(3) . . ?
C4 N2 C4 126.4(6) . 5_655 ?
C11 N3 C11 125.7(7) 5_655 . ?
C11 N3 C12 117.1(3) . . ?
C11 N3 C12 117.1(3) 5_655 . ?
C14 N4 Ni1 120.8(4) . 1_545 ?
C14 N4 Ni1 120.8(4) 5_655 1_545 ?
C14 N4 C14 118.4(7) . 5_655 ?
C15 N5 C16 120.3(10) . . ?
C15 N5 C17 119.3(10) . . ?
C16 N5 C17 120.1(10) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.7(8) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 121.2 . . ?
C3 C2 C1 117.6(8) . . ?
C3 C2 H2 121.2 . . ?
C2 C3 N2 119.7(4) 5_655 . ?
C2 C3 N2 119.7(4) . . ?
C2 C3 C2 120.6(8) . 5_655 ?
O1 C4 N2 118.1(5) . . ?
O1 C4 C5 126.4(6) . . ?
N2 C4 C5 115.5(5) . . ?
C6 C5 C4 118.9(5) . . ?
C6 C5 C10 120.5(5) . . ?
C10 C5 C4 120.6(5) . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.5(5) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.1(6) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 C9 120.9(5) . . ?
C7 C8 C11 120.9(5) . . ?
C9 C8 C11 118.3(5) . . ?
C8 C9 C8 122.7(7) . 5_655 ?
C10 C9 C8 118.7(3) . 5_655 ?
C10 C9 C8 118.7(3) . . ?
C5 C10 C5 121.3(6) . 5_655 ?
C9 C10 C5 119.4(3) . . ?
C9 C10 C5 119.4(3) . 5_655 ?
O2 C11 N3 120.5(5) . . ?
O2 C11 C8 121.9(5) . . ?
N3 C11 C8 117.5(5) . . ?
C13 C12 N3 120.0(4) 5_655 . ?
C13 C12 N3 120.0(4) . . ?
C13 C12 C13 120.0(8) 5_655 . ?
C12 C13 H13 121.1 . . ?
C12 C13 C14 117.9(6) . . ?
C14 C13 H13 121.1 . . ?
N4 C14 C13 122.9(6) . . ?
N4 C14 H14 118.5 . . ?
C13 C14 H14 118.5 . . ?
O3 C15 N5 124.4(10) . . ?
O3 C15 H15 117.8 . . ?
N5 C15 H15 117.8 . . ?
N5 C16 H16A 109.5 . . ?
N5 C16 H16B 109.5 . . ?
N5 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
N5 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N6 O4 Ni1 125(3) . . ?
O5 N6 O4 110(4) . . ?
O6 N6 O4 120(4) . . ?
O6 N6 O5 129(4) . . ?
N6A O4A Ni1 137.3(14) . . ?
O4A N6A O5A 109.4(17) . . ?
O4A N6A O6A 128(2) . . ?
O6A N6A O5A 120.0(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O3 C15 N5 170.6(8) . . . . ?
Ni1 N1 C1 C2 178.9(6) . . . . ?
Ni1 N4 C14 C13 179.8(5) 1_545 . . . ?
Ni1 O4 N6 O5 163(3) . . . . ?
Ni1 O4 N6 O6 -10(5) . . . . ?
Ni1 O4A N6A O5A 39(2) . . . . ?
Ni1 O4A N6A O6A -158.4(15) . . . . ?
O1 C4 C5 C6 -1.1(11) . . . . ?
O1 C4 C5 C10 177.3(5) . . . . ?
N1 C1 C2 C3 2.1(12) . . . . ?
N2 C4 C5 C6 178.8(5) . . . . ?
N2 C4 C5 C10 -2.8(9) . . . . ?
N3 C12 C13 C14 179.9(5) . . . . ?
C1 N1 C1 C2 -1.1(6) 5_655 . . . ?
C1 C2 C3 N2 179.0(6) . . . . ?
C1 C2 C3 C2 -1.0(6) . . . 5_655 ?
C3 N2 C4 O1 1.3(7) . . . . ?
C3 N2 C4 C5 -178.6(4) . . . . ?
C4 N2 C3 C2 89.2(5) . . . 5_655 ?
C4 N2 C3 C2 89.2(5) 5_655 . . . ?
C4 N2 C3 C2 -90.8(5) 5_655 . . 5_655 ?
C4 N2 C3 C2 -90.8(5) . . . . ?
C4 N2 C4 O1 -178.7(7) 5_655 . . . ?
C4 N2 C4 C5 1.4(4) 5_655 . . . ?
C4 C5 C6 C7 179.1(6) . . . . ?
C4 C5 C10 C5 1.5(4) . . . 5_655 ?
C4 C5 C10 C9 -178.5(4) . . . . ?
C5 C6 C7 C8 -0.8(10) . . . . ?
C6 C5 C10 C5 179.9(7) . . . 5_655 ?
C6 C5 C10 C9 -0.1(7) . . . . ?
C6 C7 C8 C9 0.4(9) . . . . ?
C6 C7 C8 C11 -179.0(6) . . . . ?
C7 C8 C9 C8 -179.8(6) . . . 5_655 ?
C7 C8 C9 C10 0.2(6) . . . . ?
C7 C8 C11 O2 -2.2(10) . . . . ?
C7 C8 C11 N3 -179.8(5) . . . . ?
C8 C9 C10 C5 -0.3(4) 5_655 . . 5_655 ?
C8 C9 C10 C5 -0.3(4) . . . . ?
C8 C9 C10 C5 179.7(4) 5_655 . . . ?
C8 C9 C10 C5 179.7(4) . . . 5_655 ?
C9 C8 C11 O2 178.4(5) . . . . ?
C9 C8 C11 N3 0.8(8) . . . . ?
C10 C5 C6 C7 0.7(10) . . . . ?
C11 N3 C11 O2 -178.0(7) 5_655 . . . ?
C11 N3 C11 C8 -0.4(4) 5_655 . . . ?
C11 N3 C12 C13 -85.8(4) . . . 5_655 ?
C11 N3 C12 C13 94.2(4) 5_655 . . 5_655 ?
C11 N3 C12 C13 -85.8(4) 5_655 . . . ?
C11 N3 C12 C13 94.2(4) . . . . ?
C11 C8 C9 C8 -0.4(4) . . . 5_655 ?
C11 C8 C9 C10 179.6(4) . . . . ?
C12 N3 C11 O2 1.9(7) . . . . ?
C12 N3 C11 C8 179.6(4) . . . . ?
C12 C13 C14 N4 0.3(10) . . . . ?
C13 C12 C13 C14 -0.1(5) 5_655 . . . ?
C14 N4 C14 C13 -0.2(5) 5_655 . . . ?
C16 N5 C15 O3 -177.7(10) . . . . ?
C17 N5 C15 O3 8.2(18) . . . . ?

_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.486
_oxdiff_exptl_absorpt_empirical_full_min 0.394
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.83(9)
2 0.17(9)

####################################################################### 
# 
# 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_nhbnen_sq
_database_code_depnum_ccdc_archive 'CCDC 1493816'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-08-25 downloaded from the CCDC.
;
_nottingham_internal_coll_name   NHBNEN
_nottingham_internal_coll_number 15708
_nottingham_internal_coll_client NHB/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '30.0000, 120.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczcrp
_nottingham_internal_coll_date   04/03/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 10/03/2016
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 10/03/2016
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 10/03/2016
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 10/03/2016
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          
;
Disorded solvent dimethylformamide could not be reasonably modelled and the data was 
treated PLATON SQUEEZE. This gave an estimate of 38e- per cell, corresponding to one 
dimethylformamide molecule. This molecule was included in the sum formula and calculation 
of derived parameters.
;
_vrf_CHEMW03_nhbnen_sq           
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: PLATON SQUEEZE was used, the removed solvents were included in the formula and calculation of derived parameters.
;
_audit_creation_date             2016-03-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H14 N5 Ni O9, 2(C3 H7 N O)'
_chemical_formula_sum            'C37 H35 N8 Ni O12'
_chemical_formula_weight         842.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         C48H24Ni2N2O18
_chemical_oxdiff_usercomment     
'#15708 NHBNEN GVB-933 FOMBLIM ON MICROMOUNT FOR NHB/NRC'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.8571(6)
_cell_length_b                   11.2573(7)
_cell_length_c                   16.1205(8)
_cell_angle_alpha                89.642(4)
_cell_angle_beta                 83.978(5)
_cell_angle_gamma                82.956(5)
_cell_volume                     1765.46(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6640
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.3240
_cell_measurement_theta_min      3.9680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.0891
_exptl_crystal_size_mid          0.0612
_exptl_crystal_size_min          0.0362
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14637
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.646
_diffrn_reflns_theta_min         3.957
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -94.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  150.0000 92

#__ type_ start__ end____ width___ exp.time_
  2 omega  -94.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  -90.0000 92

#__ type_ start__ end____ width___ exp.time_
  3 omega   20.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8292   38.0000 -120.0000 95

#__ type_ start__ end____ width___ exp.time_
  4 omega   83.00  123.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 40

#__ type_ start__ end____ width___ exp.time_
  5 omega  -30.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8292  -38.0000   60.0000 95

#__ type_ start__ end____ width___ exp.time_
  6 omega   30.00   91.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -60.0000 61

#__ type_ start__ end____ width___ exp.time_
  7 omega   33.00  122.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000   30.0000 89

#__ type_ start__ end____ width___ exp.time_
  8 omega   30.00   91.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   90.0000 61

#__ type_ start__ end____ width___ exp.time_
  9 omega   30.00   91.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  150.0000 61

#__ type_ start__ end____ width___ exp.time_
 10 omega   83.00  176.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 93

#__ type_ start__ end____ width___ exp.time_
 11 omega  151.00  176.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 12 omega  102.00  143.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000  120.0000 41

#__ type_ start__ end____ width___ exp.time_
 13 omega   30.00   79.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -150.0000 49

#__ type_ start__ end____ width___ exp.time_
 14 omega  131.00  167.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000    0.0000 36

#__ type_ start__ end____ width___ exp.time_
 15 omega   82.00  114.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000    0.0000 32

#__ type_ start__ end____ width___ exp.time_
 16 omega   36.00  131.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 17 omega   34.00   59.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 18 omega   89.00  130.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000 -180.0000 41

#__ type_ start__ end____ width___ exp.time_
 19 omega   38.00  136.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000 -150.0000 98

#__ type_ start__ end____ width___ exp.time_
 20 omega   62.00  121.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000 -150.0000 59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.0318280000
_diffrn_orient_matrix_UB_12      -0.0696314000
_diffrn_orient_matrix_UB_13      -0.0831302000
_diffrn_orient_matrix_UB_21      0.1539489000
_diffrn_orient_matrix_UB_22      0.0116418000
_diffrn_orient_matrix_UB_23      0.0008544000
_diffrn_orient_matrix_UB_31      0.0190318000
_diffrn_orient_matrix_UB_32      -0.1184517000
_diffrn_orient_matrix_UB_33      0.0482020000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6112
_reflns_number_total             6882
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.918
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6882
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0593
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0956P)²+1.7483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1703
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C26(H26), C16(H16), C28(H28), C17(H17), C23(H23), C20(H20),
 C4(H4), C21(H21), C2(H2), C24(H24), C12(H12), C11(H11), C32(H32), C29(H29)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C30(H30A,H30B,H30C), C33(H33A,H33B,
 H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.44020(5) 0.63482(4) 0.09579(2) 0.02425(15) Uani 1 1 d . . . . .
O5 O 0.64226(19) 0.59548(17) 0.07221(11) 0.0287(4) Uani 1 1 d . . . . .
O7 O 0.4467(2) 0.79235(17) 0.16702(12) 0.0314(4) Uani 1 1 d . . . . .
O6 O 0.6467(2) 0.49847(16) -0.04847(11) 0.0291(4) Uani 1 1 d . . . . .
O8 O 0.2509(2) 0.73375(17) 0.15078(12) 0.0325(4) Uani 1 1 d . . . . .
O4 O 0.6527(2) -0.14666(17) 0.72390(13) 0.0373(5) Uani 1 1 d . . . . .
O2 O 0.6426(2) 0.20518(18) 0.36097(12) 0.0381(5) Uani 1 1 d . . . . .
N1 N 0.4475(2) 0.53442(19) 0.20466(13) 0.0269(5) Uani 1 1 d . . . . .
O1 O 0.2994(3) 0.4671(2) 0.49273(14) 0.0498(6) Uani 1 1 d . . . . .
N4 N 0.4371(3) -0.25875(19) 0.98935(13) 0.0289(5) Uani 1 1 d . . . . .
N5 N 0.3165(3) 0.8105(2) 0.18166(15) 0.0324(5) Uani 1 1 d . . . . .
O3 O 0.2607(3) 0.0749(2) 0.83596(15) 0.0545(7) Uani 1 1 d . . . . .
O9 O 0.2587(3) 0.8960(2) 0.22289(18) 0.0529(6) Uani 1 1 d . . . . .
N3 N 0.4544(3) -0.0375(2) 0.77790(14) 0.0303(5) Uani 1 1 d . . . . .
N2 N 0.4641(3) 0.3321(2) 0.42463(14) 0.0319(5) Uani 1 1 d . . . . .
C8 C 0.4649(3) 0.1892(2) 0.56839(16) 0.0273(5) Uani 1 1 d . . . . .
C27 C 0.8574(3) 0.5185(2) 0.00441(16) 0.0265(5) Uani 1 1 d . . . . .
C14 C 0.4631(3) 0.1142(2) 0.63906(16) 0.0274(5) Uani 1 1 d . . . . .
C22 C 0.4500(3) -0.1147(2) 0.84943(16) 0.0312(6) Uani 1 1 d . . . . .
C9 C 0.5685(3) 0.1611(2) 0.50157(16) 0.0297(6) Uani 1 1 d . . . . .
C1 C 0.3414(3) 0.4780(2) 0.23540(17) 0.0309(6) Uani 1 1 d . . . . .
H1 H 0.2619 0.4846 0.2064 0.037 Uiso 1 1 calc R . . . .
C7 C 0.3641(3) 0.2892(2) 0.56612(17) 0.0310(6) Uani 1 1 d . . . . .
C13 C 0.3559(3) 0.1387(2) 0.70408(16) 0.0299(6) Uani 1 1 d . . . . .
C3 C 0.4584(3) 0.4022(2) 0.34966(16) 0.0311(6) Uani 1 1 d . . . . .
C19 C 0.5655(3) -0.0629(2) 0.71652(16) 0.0303(6) Uani 1 1 d . . . . .
C5 C 0.5596(3) 0.5239(2) 0.24632(17) 0.0328(6) Uani 1 1 d . . . . .
H5 H 0.6360 0.5628 0.2247 0.039 Uiso 1 1 calc R . . . .
C25 C 0.7032(3) 0.5387(2) 0.00907(15) 0.0256(5) Uani 1 1 d . . . . .
C26 C 0.9264(3) 0.5794(3) 0.05853(18) 0.0326(6) Uani 1 1 d . . . . .
H26 H 0.8760 0.6339 0.0986 0.039 Uiso 1 1 calc R . . . .
C16 C 0.6688(3) -0.0068(2) 0.57769(17) 0.0330(6) Uani 1 1 d . . . . .
H16 H 0.7392 -0.0718 0.5810 0.040 Uiso 1 1 calc R . . . .
C28 C 0.9318(3) 0.4393(3) -0.05399(18) 0.0332(6) Uani 1 1 d . . . . .
H28 H 0.8851 0.3977 -0.0911 0.040 Uiso 1 1 calc R . . . .
C17 C 0.6685(3) 0.0660(3) 0.50627(17) 0.0333(6) Uani 1 1 d . . . . .
H17 H 0.7381 0.0491 0.4611 0.040 Uiso 1 1 calc R . . . .
C18 C 0.3504(3) 0.0590(3) 0.77782(18) 0.0355(6) Uani 1 1 d . . . . .
C10 C 0.5651(3) 0.2321(2) 0.42377(16) 0.0311(6) Uani 1 1 d . . . . .
C15 C 0.5667(3) 0.0165(2) 0.64260(16) 0.0285(5) Uani 1 1 d . . . . .
C23 C 0.3582(3) -0.1982(3) 0.85798(18) 0.0362(6) Uani 1 1 d . . . . .
H23 H 0.2994 -0.2079 0.8161 0.043 Uiso 1 1 calc R . . . .
C6 C 0.3702(3) 0.3708(3) 0.49366(17) 0.0352(6) Uani 1 1 d . . . . .
C20 C 0.5280(3) -0.1790(3) 0.97877(17) 0.0340(6) Uani 1 1 d . . . . .
H20 H 0.5884 -0.1730 1.0204 0.041 Uiso 1 1 calc R . . . .
C4 C 0.5688(3) 0.4592(3) 0.31912(18) 0.0353(6) Uani 1 1 d . . . . .
H4 H 0.6492 0.4542 0.3473 0.042 Uiso 1 1 calc R . . . .
C21 C 0.5379(3) -0.1049(3) 0.90997(18) 0.0355(6) Uani 1 1 d . . . . .
H21 H 0.6031 -0.0490 0.9045 0.043 Uiso 1 1 calc R . . . .
C2 C 0.3423(3) 0.4107(2) 0.30753(17) 0.0315(6) Uani 1 1 d . . . . .
H2 H 0.2654 0.3714 0.3275 0.038 Uiso 1 1 calc R . . . .
N7 N 0.9903(4) 0.2550(3) 0.2444(2) 0.0596(8) Uani 1 1 d . . . . .
C24 C 0.3540(3) -0.2675(2) 0.92914(18) 0.0338(6) Uani 1 1 d . . . . .
H24 H 0.2894 -0.3238 0.9358 0.041 Uiso 1 1 calc R . . . .
C12 C 0.2571(3) 0.2357(3) 0.70033(18) 0.0354(6) Uani 1 1 d . . . . .
H12 H 0.1853 0.2506 0.7445 0.042 Uiso 1 1 calc R . . . .
C11 C 0.2618(3) 0.3128(3) 0.63137(18) 0.0352(6) Uani 1 1 d . . . . .
H11 H 0.1949 0.3809 0.6297 0.042 Uiso 1 1 calc R . . . .
N6 N 1.0487(4) -0.2510(3) 0.4245(2) 0.0675(10) Uani 1 1 d . . . . .
O11 O 0.9341(5) 0.4469(3) 0.2900(3) 0.1021(14) Uani 1 1 d . . . . .
C31 C 1.0086(5) -0.1300(4) 0.4045(4) 0.0763(13) Uani 1 1 d . . . . .
H31A H 1.0907 -0.0904 0.3889 0.114 Uiso 1 1 calc GR . . . .
H31B H 0.9551 -0.0892 0.4530 0.114 Uiso 1 1 calc GR . . . .
H31C H 0.9524 -0.1268 0.3577 0.114 Uiso 1 1 calc GR . . . .
C32 C 0.9319(5) 0.3407(5) 0.2983(4) 0.0802(14) Uani 1 1 d . . . . .
H32 H 0.8838 0.3154 0.3482 0.096 Uiso 1 1 calc R . . . .
C34 C 1.0713(7) 0.2837(5) 0.1703(3) 0.0868(17) Uani 1 1 d . . . . .
H34A H 1.0491 0.3687 0.1577 0.130 Uiso 1 1 calc GR . . . .
H34B H 1.0516 0.2350 0.1239 0.130 Uiso 1 1 calc GR . . . .
H34C H 1.1690 0.2672 0.1784 0.130 Uiso 1 1 calc GR . . . .
C30 C 1.1396(6) -0.3256(5) 0.3661(3) 0.0869(17) Uani 1 1 d . . . . .
H30A H 1.1142 -0.3091 0.3096 0.130 Uiso 1 1 calc GR . . . .
H30B H 1.1326 -0.4099 0.3794 0.130 Uiso 1 1 calc GR . . . .
H30C H 1.2342 -0.3090 0.3692 0.130 Uiso 1 1 calc GR . . . .
O10 O 0.8880(7) -0.2439(6) 0.5447(3) 0.153(3) Uani 1 1 d . . . . .
C33 C 0.9878(6) 0.1298(4) 0.2638(5) 0.095(2) Uani 1 1 d . . . . .
H33A H 1.0817 0.0917 0.2678 0.143 Uiso 1 1 calc GR . . . .
H33B H 0.9479 0.0907 0.2196 0.143 Uiso 1 1 calc GR . . . .
H33C H 0.9320 0.1220 0.3171 0.143 Uiso 1 1 calc GR . . . .
C29 C 0.9956(9) -0.2974(6) 0.4970(4) 0.122(3) Uani 1 1 d . . . . .
H29 H 1.0379 -0.3724 0.5145 0.147 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O5 1.9836(19) . ?
Ni1 O7 2.1299(19) . ?
Ni1 O6 2.0087(18) 2_665 ?
Ni1 O8 2.159(2) . ?
Ni1 N1 2.084(2) . ?
Ni1 N4 2.087(2) 1_564 ?
O5 C25 1.262(3) . ?
O7 N5 1.271(3) . ?
O6 Ni1 2.0086(18) 2_665 ?
O6 C25 1.245(3) . ?
O8 N5 1.274(3) . ?
O4 C19 1.210(4) . ?
O2 C10 1.219(4) . ?
N1 C1 1.339(4) . ?
N1 C5 1.345(4) . ?
O1 C6 1.217(4) . ?
N4 Ni1 2.087(2) 1_546 ?
N4 C20 1.342(4) . ?
N4 C24 1.346(4) . ?
N5 O9 1.219(3) . ?
O3 C18 1.217(4) . ?
N3 C22 1.440(3) . ?
N3 C19 1.400(4) . ?
N3 C18 1.398(4) . ?
N2 C3 1.442(3) . ?
N2 C10 1.407(4) . ?
N2 C6 1.406(4) . ?
C8 C14 1.414(4) . ?
C8 C9 1.413(4) . ?
C8 C7 1.410(4) . ?
C27 C25 1.503(4) . ?
C27 C26 1.393(4) . ?
C27 C28 1.387(4) . ?
C14 C13 1.411(4) . ?
C14 C15 1.412(4) . ?
C22 C23 1.380(4) . ?
C22 C21 1.384(4) . ?
C9 C17 1.371(4) . ?
C9 C10 1.485(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.385(4) . ?
C7 C6 1.482(4) . ?
C7 C11 1.382(4) . ?
C13 C18 1.485(4) . ?
C13 C12 1.377(4) . ?
C3 C4 1.376(4) . ?
C3 C2 1.384(4) . ?
C19 C15 1.485(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.383(4) . ?
C26 H26 0.9500 . ?
C26 C28 1.382(4) 2_765 ?
C16 H16 0.9500 . ?
C16 C17 1.409(4) . ?
C16 C15 1.376(4) . ?
C28 C26 1.381(4) 2_765 ?
C28 H28 0.9500 . ?
C17 H17 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.383(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.386(4) . ?
C4 H4 0.9500 . ?
C21 H21 0.9500 . ?
C2 H2 0.9500 . ?
N7 C32 1.336(7) . ?
N7 C34 1.424(6) . ?
N7 C33 1.444(5) . ?
C24 H24 0.9500 . ?
C12 H12 0.9500 . ?
C12 C11 1.407(4) . ?
C11 H11 0.9500 . ?
N6 C31 1.416(6) . ?
N6 C30 1.430(6) . ?
N6 C29 1.357(8) . ?
O11 C32 1.204(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O10 C29 1.326(9) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C29 H29 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Ni1 O7 95.90(8) . . ?
O5 Ni1 O6 107.41(8) . 2_665 ?
O5 Ni1 O8 156.18(8) . . ?
O5 Ni1 N1 89.19(9) . . ?
O5 Ni1 N4 89.99(9) . 1_564 ?
O7 Ni1 O8 60.35(8) . . ?
O6 Ni1 O7 156.31(8) 2_665 . ?
O6 Ni1 O8 96.17(8) 2_665 . ?
O6 Ni1 N1 86.90(8) 2_665 . ?
O6 Ni1 N4 95.70(8) 2_665 1_564 ?
N1 Ni1 O7 89.30(8) . . ?
N1 Ni1 O8 88.72(8) . . ?
N1 Ni1 N4 177.40(9) . 1_564 ?
N4 Ni1 O7 88.33(8) 1_564 . ?
N4 Ni1 O8 91.03(9) 1_564 . ?
C25 O5 Ni1 125.29(17) . . ?
N5 O7 Ni1 92.66(14) . . ?
C25 O6 Ni1 149.39(17) . 2_665 ?
N5 O8 Ni1 91.22(16) . . ?
C1 N1 Ni1 121.36(18) . . ?
C1 N1 C5 117.7(2) . . ?
C5 N1 Ni1 120.91(19) . . ?
C20 N4 Ni1 117.60(18) . 1_546 ?
C20 N4 C24 117.7(2) . . ?
C24 N4 Ni1 124.64(19) . 1_546 ?
O7 N5 O8 115.8(2) . . ?
O9 N5 O7 121.9(2) . . ?
O9 N5 O8 122.4(3) . . ?
C19 N3 C22 117.0(2) . . ?
C18 N3 C22 117.0(2) . . ?
C18 N3 C19 126.0(2) . . ?
C10 N2 C3 117.6(2) . . ?
C6 N2 C3 117.3(2) . . ?
C6 N2 C10 125.1(2) . . ?
C9 C8 C14 118.6(2) . . ?
C7 C8 C14 119.6(3) . . ?
C7 C8 C9 121.9(2) . . ?
C26 C27 C25 120.2(2) . . ?
C28 C27 C25 120.2(2) . . ?
C28 C27 C26 119.6(3) . . ?
C13 C14 C8 118.7(2) . . ?
C13 C14 C15 121.7(2) . . ?
C15 C14 C8 119.6(3) . . ?
C23 C22 N3 120.2(3) . . ?
C23 C22 C21 119.9(3) . . ?
C21 C22 N3 120.0(3) . . ?
C8 C9 C10 119.5(2) . . ?
C17 C9 C8 120.9(2) . . ?
C17 C9 C10 119.6(3) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.1(3) . . ?
C2 C1 H1 118.5 . . ?
C8 C7 C6 119.4(3) . . ?
C11 C7 C8 120.7(2) . . ?
C11 C7 C6 119.9(3) . . ?
C14 C13 C18 119.4(2) . . ?
C12 C13 C14 120.9(2) . . ?
C12 C13 C18 119.7(3) . . ?
C4 C3 N2 120.2(3) . . ?
C4 C3 C2 119.9(2) . . ?
C2 C3 N2 119.9(3) . . ?
O4 C19 N3 120.8(2) . . ?
O4 C19 C15 123.1(3) . . ?
N3 C19 C15 116.1(2) . . ?
N1 C5 H5 118.5 . . ?
N1 C5 C4 123.0(3) . . ?
C4 C5 H5 118.5 . . ?
O5 C25 C27 116.1(2) . . ?
O6 C25 O5 125.7(3) . . ?
O6 C25 C27 118.2(2) . . ?
C27 C26 H26 120.0 . . ?
C28 C26 C27 120.0(3) 2_765 . ?
C28 C26 H26 120.0 2_765 . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C15 C16 C17 119.8(3) . . ?
C27 C28 H28 119.8 . . ?
C26 C28 C27 120.4(3) 2_765 . ?
C26 C28 H28 119.8 2_765 . ?
C9 C17 C16 120.4(3) . . ?
C9 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
O3 C18 N3 120.5(3) . . ?
O3 C18 C13 122.7(3) . . ?
N3 C18 C13 116.7(3) . . ?
O2 C10 N2 120.6(2) . . ?
O2 C10 C9 122.7(3) . . ?
N2 C10 C9 116.6(2) . . ?
C14 C15 C19 120.0(2) . . ?
C16 C15 C14 120.6(2) . . ?
C16 C15 C19 119.4(2) . . ?
C22 C23 H23 120.9 . . ?
C22 C23 C24 118.3(3) . . ?
C24 C23 H23 120.9 . . ?
O1 C6 N2 120.5(3) . . ?
O1 C6 C7 122.9(3) . . ?
N2 C6 C7 116.6(2) . . ?
N4 C20 H20 118.5 . . ?
N4 C20 C21 123.0(3) . . ?
C21 C20 H20 118.5 . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 H4 120.9 . . ?
C22 C21 C20 118.1(3) . . ?
C22 C21 H21 121.0 . . ?
C20 C21 H21 121.0 . . ?
C1 C2 H2 121.0 . . ?
C3 C2 C1 118.0(3) . . ?
C3 C2 H2 121.0 . . ?
C32 N7 C34 120.8(4) . . ?
C32 N7 C33 121.4(5) . . ?
C34 N7 C33 117.4(4) . . ?
N4 C24 C23 123.0(3) . . ?
N4 C24 H24 118.5 . . ?
C23 C24 H24 118.5 . . ?
C13 C12 H12 119.8 . . ?
C13 C12 C11 120.3(3) . . ?
C11 C12 H12 119.8 . . ?
C7 C11 C12 119.7(3) . . ?
C7 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C31 N6 C30 119.6(4) . . ?
C29 N6 C31 120.1(5) . . ?
C29 N6 C30 120.2(4) . . ?
N6 C31 H31A 109.5 . . ?
N6 C31 H31B 109.5 . . ?
N6 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N7 C32 H32 116.8 . . ?
O11 C32 N7 126.5(6) . . ?
O11 C32 H32 116.8 . . ?
N7 C34 H34A 109.5 . . ?
N7 C34 H34B 109.5 . . ?
N7 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N6 C30 H30A 109.5 . . ?
N6 C30 H30B 109.5 . . ?
N6 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N7 C33 H33A 109.5 . . ?
N7 C33 H33B 109.5 . . ?
N7 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N6 C29 H29 118.2 . . ?
O10 C29 N6 123.7(6) . . ?
O10 C29 H29 118.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O5 C25 O6 0.1(4) . . . . ?
Ni1 O5 C25 C27 -179.63(15) . . . . ?
Ni1 O7 N5 O8 0.5(2) . . . . ?
Ni1 O7 N5 O9 -179.7(3) . . . . ?
Ni1 O6 C25 O5 -87.9(4) 2_665 . . . ?
Ni1 O6 C25 C27 91.9(4) 2_665 . . . ?
Ni1 O8 N5 O7 -0.5(2) . . . . ?
Ni1 O8 N5 O9 179.7(3) . . . . ?
Ni1 N1 C1 C2 -179.9(2) . . . . ?
Ni1 N1 C5 C4 179.4(2) . . . . ?
Ni1 N4 C20 C21 178.7(2) 1_546 . . . ?
Ni1 N4 C24 C23 -177.7(2) 1_546 . . . ?
O4 C19 C15 C14 -178.7(3) . . . . ?
O4 C19 C15 C16 1.9(4) . . . . ?
N1 C1 C2 C3 0.3(4) . . . . ?
N1 C5 C4 C3 0.6(4) . . . . ?
N4 C20 C21 C22 -0.4(5) . . . . ?
N3 C22 C23 C24 -177.6(3) . . . . ?
N3 C22 C21 C20 178.5(3) . . . . ?
N3 C19 C15 C14 2.9(4) . . . . ?
N3 C19 C15 C16 -176.6(3) . . . . ?
N2 C3 C4 C5 179.0(3) . . . . ?
N2 C3 C2 C1 -179.5(2) . . . . ?
C8 C14 C13 C18 178.5(2) . . . . ?
C8 C14 C13 C12 -2.0(4) . . . . ?
C8 C14 C15 C19 -179.9(2) . . . . ?
C8 C14 C15 C16 -0.5(4) . . . . ?
C8 C9 C17 C16 0.9(4) . . . . ?
C8 C9 C10 O2 -172.3(3) . . . . ?
C8 C9 C10 N2 5.9(4) . . . . ?
C8 C7 C6 O1 -169.2(3) . . . . ?
C8 C7 C6 N2 10.3(4) . . . . ?
C8 C7 C11 C12 -0.8(5) . . . . ?
C14 C8 C9 C17 -2.6(4) . . . . ?
C14 C8 C9 C10 174.6(2) . . . . ?
C14 C8 C7 C6 177.2(2) . . . . ?
C14 C8 C7 C11 -1.5(4) . . . . ?
C14 C13 C18 O3 -179.9(3) . . . . ?
C14 C13 C18 N3 -0.1(4) . . . . ?
C14 C13 C12 C11 -0.3(5) . . . . ?
C22 N3 C19 O4 0.4(4) . . . . ?
C22 N3 C19 C15 179.0(2) . . . . ?
C22 N3 C18 O3 -0.5(4) . . . . ?
C22 N3 C18 C13 179.7(2) . . . . ?
C22 C23 C24 N4 -1.4(5) . . . . ?
C9 C8 C14 C13 -176.9(3) . . . . ?
C9 C8 C14 C15 2.4(4) . . . . ?
C9 C8 C7 C6 -3.1(4) . . . . ?
C9 C8 C7 C11 178.2(3) . . . . ?
C1 N1 C5 C4 -0.7(4) . . . . ?
C7 C8 C14 C13 2.9(4) . . . . ?
C7 C8 C14 C15 -177.9(3) . . . . ?
C7 C8 C9 C17 177.6(3) . . . . ?
C7 C8 C9 C10 -5.1(4) . . . . ?
C13 C14 C15 C19 -0.7(4) . . . . ?
C13 C14 C15 C16 178.8(3) . . . . ?
C13 C12 C11 C7 1.7(5) . . . . ?
C3 N2 C10 O2 -1.5(4) . . . . ?
C3 N2 C10 C9 -179.7(2) . . . . ?
C3 N2 C6 O1 -8.7(4) . . . . ?
C3 N2 C6 C7 171.8(3) . . . . ?
C19 N3 C22 C23 -105.5(3) . . . . ?
C19 N3 C22 C21 74.7(3) . . . . ?
C19 N3 C18 O3 -177.6(3) . . . . ?
C19 N3 C18 C13 2.6(4) . . . . ?
C5 N1 C1 C2 0.2(4) . . . . ?
C25 C27 C26 C28 -179.9(2) . . . 2_765 ?
C25 C27 C28 C26 179.9(2) . . . 2_765 ?
C26 C27 C25 O5 -11.9(4) . . . . ?
C26 C27 C25 O6 168.4(2) . . . . ?
C26 C27 C28 C26 0.1(5) . . . 2_765 ?
C28 C27 C25 O5 168.4(2) . . . . ?
C28 C27 C25 O6 -11.4(4) . . . . ?
C28 C27 C26 C28 -0.1(5) . . . 2_765 ?
C17 C9 C10 O2 4.9(4) . . . . ?
C17 C9 C10 N2 -176.9(3) . . . . ?
C17 C16 C15 C14 -1.3(4) . . . . ?
C17 C16 C15 C19 178.2(3) . . . . ?
C18 N3 C22 C23 77.1(3) . . . . ?
C18 N3 C22 C21 -102.6(3) . . . . ?
C18 N3 C19 O4 177.5(3) . . . . ?
C18 N3 C19 C15 -4.0(4) . . . . ?
C18 C13 C12 C11 179.2(3) . . . . ?
C10 N2 C3 C4 -61.9(4) . . . . ?
C10 N2 C3 C2 117.1(3) . . . . ?
C10 N2 C6 O1 169.6(3) . . . . ?
C10 N2 C6 C7 -9.8(4) . . . . ?
C10 C9 C17 C16 -176.3(3) . . . . ?
C15 C14 C13 C18 -0.8(4) . . . . ?
C15 C14 C13 C12 178.8(3) . . . . ?
C15 C16 C17 C9 1.0(4) . . . . ?
C23 C22 C21 C20 -1.3(5) . . . . ?
C6 N2 C3 C4 116.6(3) . . . . ?
C6 N2 C3 C2 -64.4(3) . . . . ?
C6 N2 C10 O2 -179.9(3) . . . . ?
C6 N2 C10 C9 1.9(4) . . . . ?
C6 C7 C11 C12 -179.5(3) . . . . ?
C20 N4 C24 C23 -0.2(4) . . . . ?
C4 C3 C2 C1 -0.5(4) . . . . ?
C21 C22 C23 C24 2.1(5) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
C24 N4 C20 C21 1.1(4) . . . . ?
C12 C13 C18 O3 0.5(5) . . . . ?
C12 C13 C18 N3 -179.6(3) . . . . ?
C11 C7 C6 O1 9.5(5) . . . . ?
C11 C7 C6 N2 -171.0(3) . . . . ?
C31 N6 C29 O10 13.1(12) . . . . ?
C34 N7 C32 O11 3.7(9) . . . . ?
C30 N6 C29 O10 -163.5(7) . . . . ?
C33 N7 C32 O11 176.1(6) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -2 5 0.0355 -0.0055 -2.0005 4.9960 -0.2762 -0.0199 0.4777
0 2 -5 0.0355 0.0055 2.0005 -4.9960 0.2762 0.0199 -0.4777
0 4 5 0.0306 -0.0015 3.9979 4.9964 -0.6938 0.0506 -0.2328
0 -4 -5 0.0306 0.0015 -3.9979 -4.9964 0.6938 -0.0506 0.2328
-5 -1 0 0.0181 -5.0007 -1.0012 0.0037 -0.0898 -0.7815 0.0236
5 1 0 0.0181 5.0007 1.0012 -0.0037 0.0898 0.7815 -0.0236

_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
