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

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

data_cmpd3_exp_140_tsb19_p
_database_code_depnum_ccdc_archive 'CCDC 1984622'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_audit_creation_date             2020-02-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
N,N'-Bis-(4'-(hydroxybenzophenylidene))ethylenediaminenickel(II)
_chemical_formula_moiety         'C28 H22 N2 Ni O4, C3 H7 N O'
_chemical_formula_sum            'C31 H29 N3 Ni O5'
_chemical_formula_weight         582.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C31H29N3NiO5
_chemical_oxdiff_usercomment     'TSB 19_P from DMF'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.5896(2)
_cell_length_b                   17.1222(3)
_cell_length_c                   13.0803(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.082(2)
_cell_angle_gamma                90
_cell_volume                     2709.28(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16667
_cell_measurement_temperature    294
_cell_measurement_theta_max      28.9920
_cell_measurement_theta_min      1.9730
_shelx_estimated_absorpt_T_max   0.832
_shelx_estimated_absorpt_T_min   0.750
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.48a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cubeoctahedron
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method 'from DMF solvent'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60527
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         1.987
_diffrn_ambient_temperature      294
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 110.00   0.50   10.00    --   20.00  54.00   0.00  368
  2  ω    -74.00 110.00   0.50   10.00    --   20.00  54.00-180.00  368
  3  ω    -74.00 110.00   0.50   10.00    --   20.00  54.00  90.00  368
  4  ω    -74.00 110.00   0.50   10.00    --   20.00  54.00 150.00  368
  5  ω    -74.00 110.00   0.50   10.00    --   20.00  54.00 -60.00  368
  6  ω    -74.00 110.00   0.50   10.00    --   20.00  54.00 -30.00  368
  7  ω    -74.00  -4.00   0.50   10.00    --   20.00  54.00  60.00  140
  8  ω    -74.00 110.00   0.50   10.00    --   20.00  54.00-120.00  368
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0004505000
_diffrn_orient_matrix_UB_12      -0.0008972000
_diffrn_orient_matrix_UB_13      -0.0543756000
_diffrn_orient_matrix_UB_21      0.0504146000
_diffrn_orient_matrix_UB_22      0.0211800000
_diffrn_orient_matrix_UB_23      0.0125123000
_diffrn_orient_matrix_UB_31      0.0299630000
_diffrn_orient_matrix_UB_32      -0.0355418000
_diffrn_orient_matrix_UB_33      0.0087663000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5190
_reflns_number_total             7293
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.07
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_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         0.511
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.056
_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     414
_refine_ls_number_reflns         7293
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0421
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0577P)²+1.0442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1214
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N2P-C1PA = N2P-C1PB
 1.48 with sigma of 0.02
 N2-C1A = N2-C1B
 1.48 with sigma of 0.02
 C1A-C1PA = C1B-C1PB
 1.51 with sigma of 0.02
 N2-C1PA = N2-C1PB
 2.4 with sigma of 0.04
 N2P-C1A = N2P-C1B
 2.4 with sigma of 0.04
 N3D-C4D \\sim N3D-C5D
 with sigma of 0.02
 N3M-C4M \\sim N3M-C5M
 with sigma of 0.02
3. Restrained planarity
 C2D, O3AA, N3D, C4D, C5D
 with sigma of 0.1
 C2M, O4AA, N3M, C4M, C5M
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C2D \\sim O3AA \\sim N3D \\sim C4D \\sim C5D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C2M \\sim O4AA \\sim N3M \\sim C4M \\sim C5M: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C2D, O3AA, N3D, C4D, C5D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2M, O4AA, N3M, C4M, C5M
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1PA)=Sof(H1PA)=Sof(H1PB)=1-FVAR(1)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1PB)=Sof(H1PC)=Sof(H1PD)=FVAR(1)
 Sof(C2D)=Sof(H2D)=Sof(O3AA)=Sof(N3D)=Sof(C4D)=Sof(H4DA)=Sof(H4DB)=Sof(H4DC)=
 Sof(C5D)=Sof(H5DA)=Sof(H5DB)=Sof(H5DC)=1-FVAR(2)
 Sof(C2M)=Sof(H2M)=Sof(O4AA)=Sof(N3M)=Sof(C4M)=Sof(H4MA)=Sof(H4MB)=Sof(H4MC)=
 Sof(C5M)=Sof(H5MA)=Sof(H5MB)=Sof(H5MC)=FVAR(2)
7.a Free rotating group:
 C2D(O3AA,N3D,C4D,C5D), C2M(O4AA,N3M,C4M,C5M)
7.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1PA(H1PA,H1PB), C1PB(H1PC,H1PD)
7.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C5(H5), C5P(H5P), C6(H6), C6P(H6P), C8(H8), C8P(H8P), C9(H9),
 C9P(H9P), C11P(H11P), C12(H12), C12P(H12P), C13(H13), C13P(H13P), C14(H14),
 C14P(H14P), C2D(H2D), C2M(H2M)
7.d Idealised Me refined as rotating group:
 C4D(H4DA,H4DB,H4DC), C5D(H5DA,H5DB,H5DC), C4M(H4MA,H4MB,H4MC), C5M(H5MA,H5MB,
 H5MC)
7.e Idealised tetrahedral OH refined as rotating group:
 O17(H17), O17P(H17P)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 1.04129(2) 1.01330(2) 0.19207(2) 0.04101(9) Uani 1 1 d . . . . .
O16 O 1.13122(11) 1.08987(8) 0.26628(13) 0.0516(4) Uani 1 1 d . . . . .
O16P O 0.92843(11) 1.08155(9) 0.19326(14) 0.0531(4) Uani 1 1 d . . . . .
O17 O 1.52636(15) 0.70486(10) 0.17106(16) 0.0650(5) Uani 1 1 d . . . . .
H17 H 1.529028 0.670178 0.214929 0.097 Uiso 1 1 calc GR . . . .
O17P O 0.6190(2) 0.66684(13) -0.11364(18) 0.0891(7) Uani 1 1 d . . . . .
H17P H 0.630472 0.628091 -0.075311 0.134 Uiso 1 1 calc GR . . . .
N2 N 1.15678(14) 0.94830(10) 0.18683(14) 0.0435(4) Uani 1 1 d D . . . .
N2P N 0.94559(14) 0.93632(10) 0.12027(15) 0.0484(4) Uani 1 1 d D . . . .
C11 C 1.42202(18) 1.02999(14) 0.3444(2) 0.0558(6) Uani 1 1 d . . . . .
H11 H 1.467501 0.988935 0.336552 0.067 Uiso 1 1 calc R . . . .
C1A C 1.1192(8) 0.8859(7) 0.1041(9) 0.055(2) Uani 0.484(13) 1 d D . P A 3
H1AA H 1.169464 0.841744 0.118906 0.066 Uiso 0.484(13) 1 calc R . P A 3
H1AB H 1.115742 0.905966 0.033881 0.066 Uiso 0.484(13) 1 calc R . P A 3
C1B C 1.1150(8) 0.8714(5) 0.1403(7) 0.0468(18) Uani 0.516(13) 1 d D . P A 4
H1BA H 1.106703 0.836050 0.195499 0.056 Uiso 0.516(13) 1 calc R . P A 4
H1BB H 1.166285 0.848351 0.105542 0.056 Uiso 0.516(13) 1 calc R . P A 4
C1PA C 1.0055(5) 0.8618(4) 0.1103(9) 0.055(2) Uani 0.484(13) 1 d D . P A 3
H1PA H 0.966540 0.833638 0.046592 0.066 Uiso 0.484(13) 1 calc R . P A 3
H1PB H 1.011138 0.828524 0.171505 0.066 Uiso 0.484(13) 1 calc R . P A 3
C1PB C 1.0060(4) 0.8855(4) 0.0615(6) 0.0468(15) Uani 0.516(13) 1 d D . P A 4
H1PC H 0.966869 0.836774 0.040067 0.056 Uiso 0.516(13) 1 calc R . P A 4
H1PD H 1.015121 0.911865 -0.001122 0.056 Uiso 0.516(13) 1 calc R . P A 4
C3 C 1.26251(16) 0.95619(12) 0.23365(16) 0.0414(4) Uani 1 1 d . . . . .
C3P C 0.83819(16) 0.93185(12) 0.10127(16) 0.0417(4) Uani 1 1 d . . . . .
C4 C 1.34027(16) 0.89256(12) 0.22235(17) 0.0430(4) Uani 1 1 d . . . . .
C4P C 0.77861(16) 0.86109(12) 0.04725(17) 0.0436(5) Uani 1 1 d . . . . .
C5 C 1.37807(18) 0.88799(13) 0.13303(19) 0.0492(5) Uani 1 1 d . . . . .
H5 H 1.360134 0.927381 0.082190 0.059 Uiso 1 1 calc R . . . .
C5P C 0.71718(19) 0.86515(14) -0.05829(18) 0.0532(5) Uani 1 1 d . . . . .
H5P H 0.711720 0.912348 -0.094581 0.064 Uiso 1 1 calc R . . . .
C6 C 1.44227(17) 0.82571(13) 0.11786(19) 0.0501(5) Uani 1 1 d . . . . .
H6 H 1.468139 0.823759 0.057854 0.060 Uiso 1 1 calc R . . . .
C6P C 0.6640(2) 0.79996(16) -0.1102(2) 0.0628(6) Uani 1 1 d . . . . .
H6P H 0.622972 0.803590 -0.181121 0.075 Uiso 1 1 calc R . . . .
C7 C 1.46775(16) 0.76625(12) 0.19278(19) 0.0473(5) Uani 1 1 d . . . . .
C7P C 0.6711(2) 0.72956(15) -0.0578(2) 0.0586(6) Uani 1 1 d . . . . .
C8 C 1.43264(18) 0.77100(13) 0.28341(19) 0.0502(5) Uani 1 1 d . . . . .
H8 H 1.451577 0.731920 0.334626 0.060 Uiso 1 1 calc R . . . .
C8P C 0.7310(3) 0.72468(15) 0.0476(2) 0.0673(7) Uani 1 1 d . . . . .
H8P H 0.735413 0.677500 0.083792 0.081 Uiso 1 1 calc R . . . .
C9 C 1.36939(17) 0.83362(13) 0.29854(18) 0.0483(5) Uani 1 1 d . . . . .
H9 H 1.346093 0.836464 0.359986 0.058 Uiso 1 1 calc R . . . .
C9P C 0.7842(2) 0.78999(14) 0.0994(2) 0.0622(6) Uani 1 1 d . . . . .
H9P H 0.824599 0.786256 0.170512 0.075 Uiso 1 1 calc R . . . .
C10 C 1.30671(16) 1.02445(12) 0.29624(17) 0.0426(4) Uani 1 1 d . . . . .
C10P C 0.77355(16) 0.99454(12) 0.12919(16) 0.0408(4) Uani 1 1 d . . . . .
C11P C 0.65820(18) 0.98514(14) 0.11207(19) 0.0499(5) Uani 1 1 d . . . . .
H11P H 0.625918 0.937564 0.086571 0.060 Uiso 1 1 calc R . . . .
C12 C 1.4682(2) 1.09415(15) 0.4021(2) 0.0644(7) Uani 1 1 d . . . . .
H12 H 1.544173 1.096541 0.432983 0.077 Uiso 1 1 calc R . . . .
C12P C 0.59273(18) 1.04366(16) 0.1318(2) 0.0575(6) Uani 1 1 d . . . . .
H12P H 0.517282 1.035657 0.120370 0.069 Uiso 1 1 calc R . . . .
C13 C 1.40103(19) 1.15550(15) 0.4140(2) 0.0575(6) Uani 1 1 d . . . . .
H13 H 1.432225 1.199082 0.453428 0.069 Uiso 1 1 calc R . . . .
C13P C 0.63977(19) 1.11502(15) 0.1688(2) 0.0595(6) Uani 1 1 d . . . . .
H13P H 0.595464 1.155228 0.181650 0.071 Uiso 1 1 calc R . . . .
C14 C 1.28889(18) 1.15276(13) 0.36837(19) 0.0518(5) Uani 1 1 d . . . . .
H14 H 1.245264 1.194568 0.377526 0.062 Uiso 1 1 calc R . . . .
C14P C 0.75139(18) 1.12680(14) 0.1868(2) 0.0565(6) Uani 1 1 d . . . . .
H14P H 0.781406 1.175314 0.210715 0.068 Uiso 1 1 calc R . . . .
C15 C 1.23865(16) 1.08777(12) 0.30789(17) 0.0429(4) Uani 1 1 d . . . . .
C15P C 0.82141(16) 1.06676(12) 0.16983(17) 0.0437(5) Uani 1 1 d . . . . .
C2D C 0.6333(4) 0.4774(3) -0.0059(4) 0.103(2) Uani 0.603(6) 1 d . U P B 1
H2D H 0.561103 0.465392 -0.043930 0.124 Uiso 0.603(6) 1 calc R . P B 1
O3AA O 0.6681(7) 0.5419(3) -0.0202(6) 0.196(5) Uani 0.603(6) 1 d G U P B 1
N3D N 0.6910(3) 0.4215(2) 0.0607(3) 0.0783(17) Uani 0.603(6) 1 d DG U P B 1
C4D C 0.6427(5) 0.3464(3) 0.0724(6) 0.122(3) Uani 0.603(6) 1 d DG U P B 1
H4DA H 0.633502 0.342243 0.142646 0.182 Uiso 0.603(6) 1 calc GR . P B 1
H4DB H 0.690540 0.305472 0.061600 0.182 Uiso 0.603(6) 1 calc GR . P B 1
H4DC H 0.572007 0.341802 0.020755 0.182 Uiso 0.603(6) 1 calc GR . P B 1
C5D C 0.8043(4) 0.4358(4) 0.1227(5) 0.151(4) Uani 0.603(6) 1 d DG U P B 1
H5DA H 0.851512 0.436633 0.076368 0.226 Uiso 0.603(6) 1 calc GR . P B 1
H5DB H 0.827639 0.394964 0.174413 0.226 Uiso 0.603(6) 1 calc GR . P B 1
H5DC H 0.808472 0.485134 0.158428 0.226 Uiso 0.603(6) 1 calc GR . P B 1
C2M C 0.7338(5) 0.4897(3) 0.0577(5) 0.090(3) Uani 0.397(6) 1 d . U P B 2
H2M H 0.807210 0.503619 0.066807 0.108 Uiso 0.397(6) 1 calc R . P B 2
O4AA O 0.6633(6) 0.5368(3) 0.0130(7) 0.113(3) Uani 0.397(6) 1 d G U P B 2
N3M N 0.7141(4) 0.4186(3) 0.0954(5) 0.065(2) Uani 0.397(6) 1 d DG U P B 2
C4M C 0.8034(6) 0.3666(4) 0.1475(7) 0.098(3) Uani 0.397(6) 1 d DG U P B 2
H4MA H 0.871474 0.385368 0.137097 0.148 Uiso 0.397(6) 1 calc GR . P B 2
H4MB H 0.788366 0.315148 0.117722 0.148 Uiso 0.397(6) 1 calc GR . P B 2
H4MC H 0.809534 0.364622 0.222294 0.148 Uiso 0.397(6) 1 calc GR . P B 2
C5M C 0.6017(5) 0.3926(4) 0.0843(10) 0.123(5) Uani 0.397(6) 1 d DG U P B 2
H5MA H 0.553263 0.437032 0.073279 0.184 Uiso 0.397(6) 1 calc GR . P B 2
H5MB H 0.598523 0.365718 0.147778 0.184 Uiso 0.397(6) 1 calc GR . P B 2
H5MC H 0.578965 0.357986 0.024520 0.184 Uiso 0.397(6) 1 calc GR . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni O16 1.8258(14) . ?
Ni O16P 1.8431(15) . ?
Ni N2 1.8474(17) . ?
Ni N2P 1.8559(17) . ?
O16 C15 1.311(2) . ?
O16P C15P 1.321(2) . ?
O17 H17 0.8200 . ?
O17 C7 1.359(3) . ?
O17P H17P 0.8200 . ?
O17P C7P 1.361(3) . ?
N2 C1A 1.502(10) . ?
N2 C1B 1.484(9) . ?
N2 C3 1.309(2) . ?
N2P C1PA 1.506(6) . ?
N2P C1PB 1.500(6) . ?
N2P C3P 1.308(3) . ?
C11 H11 0.9300 . ?
C11 C10 1.416(3) . ?
C11 C12 1.368(3) . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C1A C1PA 1.513(12) . ?
C1B H1BA 0.9700 . ?
C1B H1BB 0.9700 . ?
C1B C1PB 1.490(10) . ?
C1PA H1PA 0.9700 . ?
C1PA H1PB 0.9700 . ?
C1PB H1PC 0.9700 . ?
C1PB H1PD 0.9700 . ?
C3 C4 1.499(3) . ?
C3 C10 1.447(3) . ?
C3P C4P 1.495(3) . ?
C3P C10P 1.453(3) . ?
C4 C5 1.380(3) . ?
C4 C9 1.394(3) . ?
C4P C5P 1.385(3) . ?
C4P C9P 1.388(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.385(3) . ?
C5P H5P 0.9300 . ?
C5P C6P 1.380(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.388(3) . ?
C6P H6P 0.9300 . ?
C6P C7P 1.377(4) . ?
C7 C8 1.378(3) . ?
C7P C8P 1.379(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.382(3) . ?
C8P H8P 0.9300 . ?
C8P C9P 1.381(3) . ?
C9 H9 0.9300 . ?
C9P H9P 0.9300 . ?
C10 C15 1.416(3) . ?
C10P C11P 1.416(3) . ?
C10P C15P 1.413(3) . ?
C11P H11P 0.9300 . ?
C11P C12P 1.366(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.385(4) . ?
C12P H12P 0.9300 . ?
C12P C13P 1.386(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.373(3) . ?
C13P H13P 0.9300 . ?
C13P C14P 1.374(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.410(3) . ?
C14P H14P 0.9300 . ?
C14P C15P 1.411(3) . ?
C2D H2D 0.9300 . ?
C2D O3AA 1.2217 . ?
C2D N3D 1.3607 . ?
N3D C4D 1.4488 . ?
N3D C5D 1.4523 . ?
C4D H4DA 0.9600 . ?
C4D H4DB 0.9600 . ?
C4D H4DC 0.9600 . ?
C5D H5DA 0.9600 . ?
C5D H5DB 0.9600 . ?
C5D H5DC 0.9600 . ?
C2M H2M 0.9300 . ?
C2M O4AA 1.2217 . ?
C2M N3M 1.3611 . ?
N3M C4M 1.4485 . ?
N3M C5M 1.4523 . ?
C4M H4MA 0.9600 . ?
C4M H4MB 0.9600 . ?
C4M H4MC 0.9600 . ?
C5M H5MA 0.9600 . ?
C5M H5MB 0.9600 . ?
C5M H5MC 0.9600 . ?

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
O16 Ni O16P 84.62(6) . . ?
O16 Ni N2 94.23(7) . . ?
O16 Ni N2P 177.45(8) . . ?
O16P Ni N2 177.23(8) . . ?
O16P Ni N2P 93.48(7) . . ?
N2 Ni N2P 87.74(7) . . ?
C15 O16 Ni 128.13(13) . . ?
C15P O16P Ni 128.01(13) . . ?
C7 O17 H17 109.5 . . ?
C7P O17P H17P 109.5 . . ?
C1A N2 Ni 111.2(4) . . ?
C1B N2 Ni 110.9(4) . . ?
C3 N2 Ni 128.99(15) . . ?
C3 N2 C1A 119.2(4) . . ?
C3 N2 C1B 118.8(4) . . ?
C1PA N2P Ni 112.0(2) . . ?
C1PB N2P Ni 108.7(2) . . ?
C3P N2P Ni 129.05(15) . . ?
C3P N2P C1PA 116.8(3) . . ?
C3P N2P C1PB 120.9(2) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C12 C11 C10 121.7(2) . . ?
N2 C1A H1AA 110.6 . . ?
N2 C1A H1AB 110.6 . . ?
N2 C1A C1PA 105.6(7) . . ?
H1AA C1A H1AB 108.8 . . ?
C1PA C1A H1AA 110.6 . . ?
C1PA C1A H1AB 110.6 . . ?
N2 C1B H1BA 110.3 . . ?
N2 C1B H1BB 110.3 . . ?
N2 C1B C1PB 107.1(6) . . ?
H1BA C1B H1BB 108.6 . . ?
C1PB C1B H1BA 110.3 . . ?
C1PB C1B H1BB 110.3 . . ?
N2P C1PA C1A 106.2(7) . . ?
N2P C1PA H1PA 110.5 . . ?
N2P C1PA H1PB 110.5 . . ?
C1A C1PA H1PA 110.5 . . ?
C1A C1PA H1PB 110.5 . . ?
H1PA C1PA H1PB 108.7 . . ?
N2P C1PB H1PC 111.0 . . ?
N2P C1PB H1PD 111.0 . . ?
C1B C1PB N2P 103.9(6) . . ?
C1B C1PB H1PC 111.0 . . ?
C1B C1PB H1PD 111.0 . . ?
H1PC C1PB H1PD 109.0 . . ?
N2 C3 C4 119.07(18) . . ?
N2 C3 C10 122.01(19) . . ?
C10 C3 C4 118.92(17) . . ?
N2P C3P C4P 119.61(19) . . ?
N2P C3P C10P 122.04(18) . . ?
C10P C3P C4P 118.33(17) . . ?
C5 C4 C3 120.82(18) . . ?
C5 C4 C9 118.7(2) . . ?
C9 C4 C3 120.3(2) . . ?
C5P C4P C3P 119.93(19) . . ?
C5P C4P C9P 118.2(2) . . ?
C9P C4P C3P 121.85(19) . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.1(2) . . ?
C6 C5 H5 119.5 . . ?
C4P C5P H5P 119.6 . . ?
C6P C5P C4P 120.7(2) . . ?
C6P C5P H5P 119.6 . . ?
C5 C6 H6 120.2 . . ?
C5 C6 C7 119.6(2) . . ?
C7 C6 H6 120.2 . . ?
C5P C6P H6P 119.8 . . ?
C7P C6P C5P 120.5(2) . . ?
C7P C6P H6P 119.8 . . ?
O17 C7 C6 116.9(2) . . ?
O17 C7 C8 123.23(19) . . ?
C8 C7 C6 119.9(2) . . ?
O17P C7P C6P 117.9(2) . . ?
O17P C7P C8P 122.5(3) . . ?
C6P C7P C8P 119.5(2) . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.3(2) . . ?
C9 C8 H8 119.9 . . ?
C7P C8P H8P 120.1 . . ?
C7P C8P C9P 119.9(2) . . ?
C9P C8P H8P 120.1 . . ?
C4 C9 H9 119.8 . . ?
C8 C9 C4 120.5(2) . . ?
C8 C9 H9 119.8 . . ?
C4P C9P H9P 119.4 . . ?
C8P C9P C4P 121.1(2) . . ?
C8P C9P H9P 119.4 . . ?
C11 C10 C3 119.46(19) . . ?
C15 C10 C11 118.50(19) . . ?
C15 C10 C3 122.00(18) . . ?
C11P C10P C3P 119.84(19) . . ?
C15P C10P C3P 122.05(18) . . ?
C15P C10P C11P 118.07(19) . . ?
C10P C11P H11P 118.9 . . ?
C12P C11P C10P 122.2(2) . . ?
C12P C11P H11P 118.9 . . ?
C11 C12 H12 120.3 . . ?
C11 C12 C13 119.4(2) . . ?
C13 C12 H12 120.3 . . ?
C11P C12P H12P 120.3 . . ?
C11P C12P C13P 119.4(2) . . ?
C13P C12P H12P 120.3 . . ?
C12 C13 H13 119.6 . . ?
C14 C13 C12 120.8(2) . . ?
C14 C13 H13 119.6 . . ?
C12P C13P H13P 119.8 . . ?
C14P C13P C12P 120.5(2) . . ?
C14P C13P H13P 119.8 . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.2(2) . . ?
C15 C14 H14 119.4 . . ?
C13P C14P H14P 119.3 . . ?
C13P C14P C15P 121.3(2) . . ?
C15P C14P H14P 119.3 . . ?
O16 C15 C10 124.18(18) . . ?
O16 C15 C14 117.53(19) . . ?
C14 C15 C10 118.29(18) . . ?
O16P C15P C10P 123.79(19) . . ?
O16P C15P C14P 117.73(19) . . ?
C14P C15P C10P 118.47(19) . . ?
O3AA C2D H2D 117.2 . . ?
O3AA C2D N3D 125.6 . . ?
N3D C2D H2D 117.2 . . ?
C2D N3D C4D 121.7 . . ?
C2D N3D C5D 120.5 . . ?
C4D N3D C5D 117.8 . . ?
N3D C4D H4DA 109.5 . . ?
N3D C4D H4DB 109.5 . . ?
N3D C4D H4DC 109.5 . . ?
H4DA C4D H4DB 109.5 . . ?
H4DA C4D H4DC 109.5 . . ?
H4DB C4D H4DC 109.5 . . ?
N3D C5D H5DA 109.5 . . ?
N3D C5D H5DB 109.5 . . ?
N3D C5D H5DC 109.5 . . ?
H5DA C5D H5DB 109.5 . . ?
H5DA C5D H5DC 109.5 . . ?
H5DB C5D H5DC 109.5 . . ?
O4AA C2M H2M 117.2 . . ?
O4AA C2M N3M 125.7 . . ?
N3M C2M H2M 117.2 . . ?
C2M N3M C4M 121.7 . . ?
C2M N3M C5M 120.5 . . ?
C4M N3M C5M 117.8 . . ?
N3M C4M H4MA 109.5 . . ?
N3M C4M H4MB 109.5 . . ?
N3M C4M H4MC 109.5 . . ?
H4MA C4M H4MB 109.5 . . ?
H4MA C4M H4MC 109.5 . . ?
H4MB C4M H4MC 109.5 . . ?
N3M C5M H5MA 109.5 . . ?
N3M C5M H5MB 109.5 . . ?
N3M C5M H5MC 109.5 . . ?
H5MA C5M H5MB 109.5 . . ?
H5MA C5M H5MC 109.5 . . ?
H5MB C5M H5MC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O17 H17 O16P 0.82 1.92 2.715(2) 164.1 2_745 yes
O17P H17P O3AA 0.82 1.65 2.456(5) 165.9 . yes
O17P H17P O4AA 0.82 1.92 2.739(6) 177.6 . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni O16 C15 C10 4.1(3) . . . . ?
Ni O16 C15 C14 -175.64(16) . . . . ?
Ni O16P C15P C10P -6.1(3) . . . . ?
Ni O16P C15P C14P 173.71(17) . . . . ?
Ni N2 C1A C1PA -38.6(11) . . . . ?
Ni N2 C1B C1PB 31.6(9) . . . . ?
Ni N2 C3 C4 176.35(15) . . . . ?
Ni N2 C3 C10 -3.5(3) . . . . ?
Ni N2P C1PA C1A -31.2(11) . . . . ?
Ni N2P C1PB C1B 44.4(8) . . . . ?
Ni N2P C3P C4P -176.11(15) . . . . ?
Ni N2P C3P C10P 5.1(3) . . . . ?
O16 Ni O16P C15P -166.0(2) . . . . ?
O16 Ni N2 C1A -163.8(5) . . . . ?
O16 Ni N2 C1B 173.5(4) . . . . ?
O16 Ni N2 C3 6.8(2) . . . . ?
O16P Ni O16 C15 175.6(2) . . . . ?
O16P Ni N2P C1PA -174.4(5) . . . . ?
O16P Ni N2P C1PB 154.6(4) . . . . ?
O16P Ni N2P C3P -11.9(2) . . . . ?
O17 C7 C8 C9 -177.3(2) . . . . ?
O17P C7P C8P C9P 178.5(3) . . . . ?
N2 Ni O16 C15 -7.0(2) . . . . ?
N2 Ni N2P C1PA 8.1(5) . . . . ?
N2 Ni N2P C1PB -22.9(4) . . . . ?
N2 Ni N2P C3P 170.6(2) . . . . ?
N2 C1A C1PA N2P 43.1(13) . . . . ?
N2 C1B C1PB N2P -47.8(10) . . . . ?
N2 C3 C4 C5 81.8(3) . . . . ?
N2 C3 C4 C9 -93.5(3) . . . . ?
N2 C3 C10 C11 -179.5(2) . . . . ?
N2 C3 C10 C15 -1.9(3) . . . . ?
N2P Ni O16P C15P 12.3(2) . . . . ?
N2P Ni N2 C1A 17.8(5) . . . . ?
N2P Ni N2 C1B -4.9(4) . . . . ?
N2P Ni N2 C3 -171.6(2) . . . . ?
N2P C3P C4P C5P -105.6(3) . . . . ?
N2P C3P C4P C9P 73.3(3) . . . . ?
N2P C3P C10P C11P -176.7(2) . . . . ?
N2P C3P C10P C15P 5.7(3) . . . . ?
C11 C10 C15 O16 179.3(2) . . . . ?
C11 C10 C15 C14 -1.0(3) . . . . ?
C11 C12 C13 C14 -0.3(4) . . . . ?
C1A N2 C3 C4 -13.7(6) . . . . ?
C1A N2 C3 C10 166.4(6) . . . . ?
C1B N2 C3 C4 10.6(5) . . . . ?
C1B N2 C3 C10 -169.3(5) . . . . ?
C1PA N2P C3P C4P -14.3(6) . . . . ?
C1PA N2P C3P C10P 166.9(5) . . . . ?
C1PB N2P C3P C4P 18.8(5) . . . . ?
C1PB N2P C3P C10P -160.0(4) . . . . ?
C3 N2 C1A C1PA 149.8(7) . . . . ?
C3 N2 C1B C1PB -160.2(6) . . . . ?
C3 C4 C5 C6 -174.4(2) . . . . ?
C3 C4 C9 C8 173.91(19) . . . . ?
C3 C10 C15 O16 1.7(3) . . . . ?
C3 C10 C15 C14 -178.6(2) . . . . ?
C3P N2P C1PA C1A 164.0(7) . . . . ?
C3P N2P C1PB C1B -147.7(5) . . . . ?
C3P C4P C5P C6P 178.3(2) . . . . ?
C3P C4P C9P C8P -178.4(2) . . . . ?
C3P C10P C11P C12P -176.6(2) . . . . ?
C3P C10P C15P O16P -5.2(3) . . . . ?
C3P C10P C15P C14P 174.9(2) . . . . ?
C4 C3 C10 C11 0.6(3) . . . . ?
C4 C3 C10 C15 178.18(19) . . . . ?
C4 C5 C6 C7 1.0(3) . . . . ?
C4P C3P C10P C11P 4.6(3) . . . . ?
C4P C3P C10P C15P -173.06(19) . . . . ?
C4P C5P C6P C7P 0.0(4) . . . . ?
C5 C4 C9 C8 -1.5(3) . . . . ?
C5 C6 C7 O17 176.8(2) . . . . ?
C5 C6 C7 C8 -2.4(3) . . . . ?
C5P C4P C9P C8P 0.5(4) . . . . ?
C5P C6P C7P O17P -178.6(2) . . . . ?
C5P C6P C7P C8P 0.7(4) . . . . ?
C6 C7 C8 C9 1.9(3) . . . . ?
C6P C7P C8P C9P -0.8(4) . . . . ?
C7 C8 C9 C4 0.1(3) . . . . ?
C7P C8P C9P C4P 0.2(4) . . . . ?
C9 C4 C5 C6 1.0(3) . . . . ?
C9P C4P C5P C6P -0.6(4) . . . . ?
C10 C11 C12 C13 0.0(4) . . . . ?
C10 C3 C4 C5 -98.3(2) . . . . ?
C10 C3 C4 C9 86.4(2) . . . . ?
C10P C3P C4P C5P 73.2(3) . . . . ?
C10P C3P C4P C9P -107.9(3) . . . . ?
C10P C11P C12P C13P 0.6(4) . . . . ?
C11P C10P C15P O16P 177.1(2) . . . . ?
C11P C10P C15P C14P -2.7(3) . . . . ?
C11P C12P C13P C14P -0.7(4) . . . . ?
C12 C11 C10 C3 178.3(2) . . . . ?
C12 C11 C10 C15 0.7(4) . . . . ?
C12 C13 C14 C15 -0.1(4) . . . . ?
C12P C13P C14P C15P -1.0(4) . . . . ?
C13 C14 C15 O16 -179.5(2) . . . . ?
C13 C14 C15 C10 0.8(4) . . . . ?
C13P C14P C15P O16P -177.2(2) . . . . ?
C13P C14P C15P C10P 2.7(4) . . . . ?
C15P C10P C11P C12P 1.2(3) . . . . ?
O3AA C2D N3D C4D 180.0 . . . . ?
O3AA C2D N3D C5D 0.0 . . . . ?
O4AA C2M N3M C4M 180.0 . . . . ?
O4AA C2M N3M C5M 0.0 . . . . ?

_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.846
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cmpd13_exp_139_tsb5_p
_database_code_depnum_ccdc_archive 'CCDC 1984624'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_audit_creation_date             2020-02-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
N-(4-(hydroxybenzophenylidene))-N'-salicylidineethylenediaminenickel(II)
_chemical_formula_moiety         'C22 H18 N2 Ni O3, 0.5(H2 O)'
_chemical_formula_sum            'C22 H19 N2 Ni O3.50'
_chemical_formula_weight         426.10
_chemical_melting_point          ?
_chemical_oxdiff_formula         C22H19N2NiO3.5
_chemical_oxdiff_usercomment     'TSB 5_P from DMSO/water'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.3061(3)
_cell_length_b                   20.2032(5)
_cell_length_c                   9.6204(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.606(3)
_cell_angle_gamma                90
_cell_volume                     1919.58(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11958
_cell_measurement_temperature    294.0
_cell_measurement_theta_max      27.5640
_cell_measurement_theta_min      2.0400
_shelx_estimated_absorpt_T_max   0.950
_shelx_estimated_absorpt_T_min   0.625
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.48a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             884
_exptl_crystal_recrystallization_method 'From DMSO-water'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            40482
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.016
_diffrn_ambient_temperature      294.0
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 110.00   0.50    5.00    --   20.00  54.00 -60.00  368
  2  ω    -74.00 110.00   0.50    5.00    --   20.00  54.00 -60.00  368
  3  ω    -74.00 110.00   0.50    5.00    --   20.00  54.00 -90.00  368
  4  ω    -74.00 110.00   0.50    5.00    --   20.00  54.00  30.00  368
  5  ω    -74.00 110.00   0.50    5.00    --   20.00  54.00-180.00  368
  6  ω    -74.00 110.00   0.50    5.00    --   20.00  54.00  90.00  368
  7  ω    -74.00  71.00   0.50    5.00    --   20.00  54.00   0.00  290
  8  ω    -74.00 110.00   0.50    5.00    --   20.00  54.00 150.00  368
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0035215000
_diffrn_orient_matrix_UB_12      -0.0097179000
_diffrn_orient_matrix_UB_13      0.0719000000
_diffrn_orient_matrix_UB_21      -0.0713477000
_diffrn_orient_matrix_UB_22      0.0031213000
_diffrn_orient_matrix_UB_23      -0.0162383000
_diffrn_orient_matrix_UB_31      -0.0076427000
_diffrn_orient_matrix_UB_32      -0.0335665000
_diffrn_orient_matrix_UB_33      -0.0221580000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3718
_reflns_number_total             4762
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_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         0.264
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4762
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0327
_refine_ls_restrained_S_all      1.050
_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)+(0.0392P)²+0.5205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0868
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.01
 H1WA-H1WB
 1.34 with sigma of 0.04
3. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C16(H16A,H16B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C13(H13),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
4.c Idealised tetrahedral OH refined as rotating group:
 O2AA(H2AA)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.46761(2) 0.44971(2) 0.62929(3) 0.04013(8) Uani 1 1 d . . . . .
O1 O 0.63152(13) 0.46532(6) 0.76402(16) 0.0502(3) Uani 1 1 d . . . . .
O2 O 0.55566(11) 0.37701(6) 0.58454(13) 0.0401(3) Uani 1 1 d . . . . .
O2AA O 0.65663(12) 0.19767(7) 0.32878(15) 0.0516(3) Uani 1 1 d . . . . .
H2AA H 0.623548 0.173448 0.259286 0.077 Uiso 1 1 calc GR . . . .
N1 N 0.38411(16) 0.52265(8) 0.67911(19) 0.0501(4) Uani 1 1 d . . . . .
N2 N 0.29968(14) 0.42698(8) 0.50359(17) 0.0421(3) Uani 1 1 d . . . . .
C1 C 0.2489(2) 0.53475(10) 0.5792(3) 0.0616(6) Uani 1 1 d . . . . .
H1A H 0.255712 0.561629 0.498017 0.074 Uiso 1 1 calc R . . . .
H1B H 0.192601 0.557823 0.628830 0.074 Uiso 1 1 calc R . . . .
C2 C 0.4324(2) 0.56205(10) 0.7862(2) 0.0564(5) Uani 1 1 d . . . . .
H2 H 0.376516 0.595959 0.800323 0.068 Uiso 1 1 calc R . . . .
C3 C 0.5649(2) 0.55802(10) 0.8852(2) 0.0535(5) Uani 1 1 d . . . . .
C4 C 0.6045(3) 0.60447(12) 0.9986(3) 0.0704(6) Uani 1 1 d . . . . .
H4 H 0.543285 0.636660 1.008597 0.084 Uiso 1 1 calc R . . . .
C5 C 0.7312(3) 0.60309(13) 1.0941(3) 0.0770(7) Uani 1 1 d . . . . .
H5 H 0.756043 0.634280 1.168044 0.092 Uiso 1 1 calc R . . . .
C6 C 0.8221(3) 0.55516(12) 1.0803(2) 0.0659(6) Uani 1 1 d . . . . .
H6 H 0.907985 0.553925 1.146055 0.079 Uiso 1 1 calc R . . . .
C7 C 0.7870(2) 0.50909(11) 0.9702(2) 0.0559(5) Uani 1 1 d . . . . .
H7 H 0.849655 0.477164 0.962792 0.067 Uiso 1 1 calc R . . . .
C8 C 0.6581(2) 0.50960(9) 0.8691(2) 0.0470(4) Uani 1 1 d . . . . .
C9 C 0.51007(16) 0.33534(8) 0.47551(18) 0.0360(4) Uani 1 1 d . . . . .
C10 C 0.60231(16) 0.28982(9) 0.44864(19) 0.0395(4) Uani 1 1 d . . . . .
H10 H 0.692634 0.291970 0.503255 0.047 Uiso 1 1 calc R . . . .
C11 C 0.56244(17) 0.24187(9) 0.34311(19) 0.0402(4) Uani 1 1 d . . . . .
C12 C 0.42741(18) 0.23926(10) 0.2573(2) 0.0481(4) Uani 1 1 d . . . . .
H12 H 0.399996 0.207825 0.184108 0.058 Uiso 1 1 calc R . . . .
C13 C 0.33682(17) 0.28349(10) 0.2826(2) 0.0469(4) Uani 1 1 d . . . . .
H13 H 0.247222 0.281093 0.225811 0.056 Uiso 1 1 calc R . . . .
C14 C 0.37263(16) 0.33262(9) 0.39063(18) 0.0386(4) Uani 1 1 d . . . . .
C15 C 0.27027(16) 0.37559(9) 0.41763(19) 0.0395(4) Uani 1 1 d . . . . .
C16 C 0.18871(19) 0.46813(10) 0.5266(3) 0.0544(5) Uani 1 1 d . . . . .
H16A H 0.151493 0.447818 0.598223 0.065 Uiso 1 1 calc R . . . .
H16B H 0.116773 0.472856 0.436671 0.065 Uiso 1 1 calc R . . . .
C17 C 0.12560(16) 0.35525(9) 0.3528(2) 0.0414(4) Uani 1 1 d . . . . .
C18 C 0.0703(2) 0.31182(11) 0.4306(2) 0.0587(5) Uani 1 1 d . . . . .
H18 H 0.120949 0.298092 0.522332 0.070 Uiso 1 1 calc R . . . .
C19 C -0.0604(2) 0.28855(13) 0.3727(3) 0.0687(6) Uani 1 1 d . . . . .
H19 H -0.097094 0.259301 0.425951 0.082 Uiso 1 1 calc R . . . .
C20 C -0.1351(2) 0.30799(11) 0.2396(3) 0.0617(6) Uani 1 1 d . . . . .
H20 H -0.222627 0.291945 0.201428 0.074 Uiso 1 1 calc R . . . .
C21 C -0.0828(2) 0.35075(13) 0.1615(3) 0.0651(6) Uani 1 1 d . . . . .
H21 H -0.134840 0.364004 0.069904 0.078 Uiso 1 1 calc R . . . .
C22 C 0.0486(2) 0.37509(12) 0.2174(2) 0.0598(5) Uani 1 1 d . . . . .
H22 H 0.083919 0.404587 0.163500 0.072 Uiso 1 1 calc R . . . .
O1W O 0.8735(4) 0.3946(2) 0.7418(5) 0.0905(12) Uani 0.5 1 d D . P . .
H1WA H 0.799(4) 0.411(3) 0.741(8) 0.136 Uiso 0.5 1 d DR . P . .
H1WB H 0.879(7) 0.3532(6) 0.747(9) 0.136 Uiso 0.5 1 d DR . P . .


_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
Ni O1 1.8389(13) . ?
Ni O2 1.8412(12) . ?
Ni N1 1.8378(16) . ?
Ni N2 1.8635(15) . ?
O1 C8 1.319(2) . ?
O2 C9 1.322(2) . ?
O2AA H2AA 0.8200 . ?
O2AA C11 1.355(2) . ?
N1 C1 1.469(3) . ?
N1 C2 1.284(3) . ?
N2 C15 1.308(2) . ?
N2 C16 1.481(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C16 1.508(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.427(3) . ?
C3 C4 1.408(3) . ?
C3 C8 1.410(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.365(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.380(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.378(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.405(3) . ?
C9 C10 1.399(2) . ?
C9 C14 1.420(2) . ?
C10 H10 0.9300 . ?
C10 C11 1.378(2) . ?
C11 C12 1.402(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.363(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.408(3) . ?
C14 C15 1.446(2) . ?
C15 C17 1.500(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.378(3) . ?
C17 C22 1.377(3) . ?
C18 H18 0.9300 . ?
C18 C19 1.385(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.350(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.353(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.396(3) . ?
C22 H22 0.9300 . ?
O1W H1WA 0.836(10) . ?
O1W H1WB 0.839(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni O2 83.50(5) . . ?
O1 Ni N2 174.51(6) . . ?
O2 Ni N2 94.59(6) . . ?
N1 Ni O1 94.76(7) . . ?
N1 Ni O2 178.21(6) . . ?
N1 Ni N2 87.11(7) . . ?
C8 O1 Ni 127.16(13) . . ?
C9 O2 Ni 127.33(11) . . ?
C11 O2AA H2AA 109.5 . . ?
C1 N1 Ni 112.95(13) . . ?
C2 N1 Ni 127.08(15) . . ?
C2 N1 C1 119.97(17) . . ?
C15 N2 Ni 127.62(12) . . ?
C15 N2 C16 119.40(15) . . ?
C16 N2 Ni 112.23(12) . . ?
N1 C1 H1A 110.3 . . ?
N1 C1 H1B 110.3 . . ?
N1 C1 C16 107.06(16) . . ?
H1A C1 H1B 108.6 . . ?
C16 C1 H1A 110.3 . . ?
C16 C1 H1B 110.3 . . ?
N1 C2 H2 117.3 . . ?
N1 C2 C3 125.32(19) . . ?
C3 C2 H2 117.3 . . ?
C4 C3 C2 119.3(2) . . ?
C4 C3 C8 119.5(2) . . ?
C8 C3 C2 121.20(19) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 C3 121.2(2) . . ?
C5 C4 H4 119.4 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.6(2) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.8(2) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.5 . . ?
C6 C7 C8 121.0(2) . . ?
C8 C7 H7 119.5 . . ?
O1 C8 C3 123.81(18) . . ?
O1 C8 C7 118.27(18) . . ?
C7 C8 C3 117.91(18) . . ?
O2 C9 C10 117.32(14) . . ?
O2 C9 C14 123.43(15) . . ?
C10 C9 C14 119.17(15) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 C9 121.53(15) . . ?
C11 C10 H10 119.2 . . ?
O2AA C11 C10 117.83(15) . . ?
O2AA C11 C12 122.34(16) . . ?
C10 C11 C12 119.81(16) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 119.04(17) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 H13 118.5 . . ?
C12 C13 C14 123.05(16) . . ?
C14 C13 H13 118.5 . . ?
C9 C14 C15 122.19(16) . . ?
C13 C14 C9 117.37(16) . . ?
C13 C14 C15 120.34(15) . . ?
N2 C15 C14 122.76(15) . . ?
N2 C15 C17 120.25(15) . . ?
C14 C15 C17 116.76(15) . . ?
N2 C16 C1 106.84(16) . . ?
N2 C16 H16A 110.4 . . ?
N2 C16 H16B 110.4 . . ?
C1 C16 H16A 110.4 . . ?
C1 C16 H16B 110.4 . . ?
H16A C16 H16B 108.6 . . ?
C18 C17 C15 117.69(16) . . ?
C22 C17 C15 123.35(17) . . ?
C22 C17 C18 118.88(17) . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.2(2) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.5(2) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.21(19) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 119.8 . . ?
C20 C21 C22 120.4(2) . . ?
C22 C21 H21 119.8 . . ?
C17 C22 C21 119.7(2) . . ?
C17 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
H1WA O1W H1WB 116(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2AA H2AA O2 0.82 1.92 2.7354(18) 173.6 4_565 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni O1 C8 C3 -7.2(3) . . . . ?
Ni O1 C8 C7 173.49(14) . . . . ?
Ni O2 C9 C10 170.02(11) . . . . ?
Ni O2 C9 C14 -13.2(2) . . . . ?
Ni N1 C1 C16 32.9(2) . . . . ?
Ni N1 C2 C3 2.7(3) . . . . ?
Ni N2 C15 C14 -10.1(2) . . . . ?
Ni N2 C15 C17 164.24(13) . . . . ?
Ni N2 C16 C1 30.4(2) . . . . ?
O1 Ni O2 C9 -172.69(14) . . . . ?
O1 Ni N1 C1 171.85(15) . . . . ?
O1 Ni N1 C2 -6.95(19) . . . . ?
O2 Ni O1 C8 -170.45(16) . . . . ?
O2 Ni N2 C15 -0.87(16) . . . . ?
O2 Ni N2 C16 169.05(13) . . . . ?
O2 C9 C10 C11 176.03(16) . . . . ?
O2 C9 C14 C13 -176.82(16) . . . . ?
O2 C9 C14 C15 -0.3(3) . . . . ?
O2AA C11 C12 C13 176.87(18) . . . . ?
N1 Ni O1 C8 9.16(16) . . . . ?
N1 Ni N2 C15 179.68(16) . . . . ?
N1 Ni N2 C16 -10.41(14) . . . . ?
N1 C1 C16 N2 -39.2(2) . . . . ?
N1 C2 C3 C4 -179.7(2) . . . . ?
N1 C2 C3 C8 2.2(3) . . . . ?
N2 Ni O2 C9 12.49(14) . . . . ?
N2 Ni N1 C1 -13.32(15) . . . . ?
N2 Ni N1 C2 167.88(19) . . . . ?
N2 C15 C17 C18 -88.9(2) . . . . ?
N2 C15 C17 C22 94.5(2) . . . . ?
C1 N1 C2 C3 -176.0(2) . . . . ?
C2 N1 C1 C16 -148.2(2) . . . . ?
C2 C3 C4 C5 -178.8(2) . . . . ?
C2 C3 C8 O1 0.2(3) . . . . ?
C2 C3 C8 C7 179.48(19) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C4 C3 C8 O1 -177.99(19) . . . . ?
C4 C3 C8 C7 1.3(3) . . . . ?
C4 C5 C6 C7 0.7(4) . . . . ?
C5 C6 C7 C8 0.0(4) . . . . ?
C6 C7 C8 O1 178.30(19) . . . . ?
C6 C7 C8 C3 -1.0(3) . . . . ?
C8 C3 C4 C5 -0.6(4) . . . . ?
C9 C10 C11 O2AA -176.80(16) . . . . ?
C9 C10 C11 C12 1.8(3) . . . . ?
C9 C14 C15 N2 12.2(3) . . . . ?
C9 C14 C15 C17 -162.31(16) . . . . ?
C10 C9 C14 C13 -0.1(2) . . . . ?
C10 C9 C14 C15 176.44(16) . . . . ?
C10 C11 C12 C13 -1.7(3) . . . . ?
C11 C12 C13 C14 0.7(3) . . . . ?
C12 C13 C14 C9 0.2(3) . . . . ?
C12 C13 C14 C15 -176.42(18) . . . . ?
C13 C14 C15 N2 -171.37(17) . . . . ?
C13 C14 C15 C17 14.1(2) . . . . ?
C14 C9 C10 C11 -0.9(3) . . . . ?
C14 C15 C17 C18 85.8(2) . . . . ?
C14 C15 C17 C22 -90.8(2) . . . . ?
C15 N2 C16 C1 -158.79(18) . . . . ?
C15 C17 C18 C19 -176.5(2) . . . . ?
C15 C17 C22 C21 176.2(2) . . . . ?
C16 N2 C15 C14 -179.39(17) . . . . ?
C16 N2 C15 C17 -5.0(3) . . . . ?
C17 C18 C19 C20 0.1(4) . . . . ?
C18 C17 C22 C21 -0.4(3) . . . . ?
C18 C19 C20 C21 -0.3(4) . . . . ?
C19 C20 C21 C22 0.1(4) . . . . ?
C20 C21 C22 C17 0.2(4) . . . . ?
C22 C17 C18 C19 0.2(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mitegen mount with Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.335
_oxdiff_exptl_absorpt_empirical_full_min 0.860
####################################################################### 
# 
# 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_ral1606SN
_database_code_depnum_ccdc_archive 'CCDC 1988291'
loop_
_audit_author_name
_audit_author_address
'Anthony Willis'
;Australian National University
Australia
;
_audit_update_record             
;
2020-03-05 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_audit_creation_date             16-06-07
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1606SN\Tony_ral1606SN_form At 15: 9 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   10.6471(4)
_cell_length_b                   26.9276(13)
_cell_length_c                   28.5309(16)
_cell_angle_alpha                65.563(5)
_cell_angle_beta                 84.047(4)
_cell_angle_gamma                83.883(3)
_cell_volume                     7388.6(7)

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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni -3.0029 0.5091 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C42 H48 N4 Ni1 O4 
# Dc =      1.32 Fooo =   3104.00 Mu =     11.34 M =   2926.31
# Found Formula = C42 H48 N4 Ni1 O4 
# Dc =      1.32 FOOO =   3104.00 Mu =     11.34 M =   2926.33

_chemical_formula_sum            'C42 H48 N4 Ni1 O4'
_chemical_formula_moiety         'C42 H48 N4 Ni O4'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         731.58


_cell_measurement_reflns_used    8212
_cell_measurement_theta_min      4
_cell_measurement_theta_max      71
_cell_measurement_temperature    150

_exptl_crystal_description       lath
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.032
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_max          0.306

_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3104
_exptl_absorpt_coefficient_mu    1.134

# Sheldrick geometric approximatio 0.92 0.96 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_T_max  0.96
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2' ####
_diffrn_radiation_source         
'Supernova (Cu) X-ray Source' ################
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2015)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2015)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            52284
_reflns_number_total             27960
_diffrn_reflns_av_R_equivalents  0.056
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 27960 
# Theoretical number of reflections is about 58816 


_diffrn_reflns_theta_min         3.143
_diffrn_reflns_theta_max         71.935
_diffrn_measured_fraction_theta_max 0.964

#_diffrn_reflns_theta_full         62.463 
#_diffrn_measured_fraction_theta_full 0.993 
_diffrn_reflns_theta_full        67.2
_diffrn_measured_fraction_theta_full 0.99


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       33
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              -29
_reflns_limit_k_max              33
_reflns_limit_l_min              0
_reflns_limit_l_max              35

_oxford_diffrn_Wilson_B_factor   2.83
_oxford_diffrn_Wilson_scale      0.41

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

_refine_diff_density_min         -0.76
_refine_diff_density_max         1.36


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         27958
_refine_ls_number_restraints     0
_refine_ls_number_parameters     1838
_oxford_refine_ls_R_factor_ref   0.1262
_refine_ls_wR_factor_ref         0.1945
_refine_ls_goodness_of_fit_ref   0.9802
_refine_ls_shift/su_max          0.0036647
_refine_ls_shift/su_mean         0.0003162


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        27958
_refine_ls_R_factor_all          0.1262
_refine_ls_wR_factor_all         0.1945

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                18592 # 20106 
_refine_ls_R_factor_gt           0.0968
_refine_ls_wR_factor_gt          0.1772

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.149E+04 0.213E+04 0.115E+04 316. 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               



Hydrogen atoms 
were included at calculated positions 
and ride on the atoms to which they were bonded. 
 
The program PLATON was used to examine the structure and its data,
and it suggested a twinning operation which 
would aid the refinement.
Application of this twinning correction within CRYSTALS
gave a significant improvement in the agreement factors.


The largest features in the
final difference electron density map are located 
near Ni atoms.
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.27714(10) 0.91082(4) 0.31594(4) 0.0277 1.0000 Uani . . . . . .
Ni2 Ni 0.62376(10) 0.59456(4) 0.18714(4) 0.0276 1.0000 Uani . . . . . .
Ni3 Ni 0.89931(10) 0.68170(4) 0.58071(4) 0.0282 1.0000 Uani . . . . . .
Ni4 Ni 0.26275(10) 0.81723(4) 0.91716(4) 0.0270 1.0000 Uani . . . . . .
O1 O 0.4042(4) 0.91654(18) 0.35178(18) 0.0345 1.0000 Uani . . . . . .
O2 O 0.4004(4) 0.87436(19) 0.29038(19) 0.0379 1.0000 Uani . . . . . .
O3 O 0.0092(5) 0.90091(18) 0.45568(18) 0.0369 1.0000 Uani . . . . . .
O4 O 0.0814(5) 0.98150(18) 0.16268(18) 0.0359 1.0000 Uani . . . . . .
O5 O 0.7224(4) 0.6266(2) 0.21448(19) 0.0363 1.0000 Uani . . . . . .
O6 O 0.7695(4) 0.58972(19) 0.14799(18) 0.0332 1.0000 Uani . . . . . .
O7 O 0.3748(5) 0.52517(18) 0.34160(17) 0.0378 1.0000 Uani . . . . . .
O8 O 0.4076(5) 0.6092(2) 0.05007(19) 0.0414 1.0000 Uani . . . . . .
O9 O 0.8014(4) 0.6620(2) 0.54306(19) 0.0383 1.0000 Uani . . . . . .
O10 O 0.7622(4) 0.72852(19) 0.5833(2) 0.0372 1.0000 Uani . . . . . .
O11 O 1.0709(5) 0.5084(2) 0.6412(2) 0.0477 1.0000 Uani . . . . . .
O12 O 1.1818(4) 0.7998(2) 0.5904(2) 0.0448 1.0000 Uani . . . . . .
O13 O 0.1586(4) 0.76710(19) 0.91650(19) 0.0374 1.0000 Uani . . . . . .
O14 O 0.1250(4) 0.84001(18) 0.94938(18) 0.0330 1.0000 Uani . . . . . .
O15 O 0.5888(5) 0.6859(2) 0.9430(2) 0.0547 1.0000 Uani . . . . . .
O16 O 0.3689(5) 0.99271(19) 0.84690(19) 0.0418 1.0000 Uani . . . . . .
N1 N 0.1541(5) 0.9433(2) 0.34755(19) 0.0250 1.0000 Uani . . . . . .
N2 N 0.1547(5) 0.90744(19) 0.27591(19) 0.0265 1.0000 Uani . . . . . .
N3 N -0.0974(7) 0.8190(3) 0.4315(3) 0.0502 1.0000 Uani . . . . . .
N4 N 0.1043(6) 1.0913(2) 0.1628(2) 0.0380 1.0000 Uani . . . . . .
N5 N 0.4794(5) 0.5979(2) 0.2296(2) 0.0281 1.0000 Uani . . . . . .
N6 N 0.5269(4) 0.5656(2) 0.15505(19) 0.0258 1.0000 Uani . . . . . .
N7 N 0.4496(6) 0.4163(2) 0.3370(2) 0.0392 1.0000 Uani . . . . . .
N8 N 0.2083(7) 0.6800(3) 0.0826(3) 0.0553 1.0000 Uani . . . . . .
N9 N 1.0334(5) 0.6314(2) 0.5792(2) 0.0329 1.0000 Uani . . . . . .
N10 N 0.9991(5) 0.7062(2) 0.6154(2) 0.0292 1.0000 Uani . . . . . .
N11 N 0.9776(6) 0.5277(3) 0.7338(2) 0.0420 1.0000 Uani . . . . . .
N12 N 1.3111(6) 0.7840(3) 0.4991(3) 0.0487 1.0000 Uani . . . . . .
N13 N 0.4025(5) 0.7897(2) 0.8884(2) 0.0292 1.0000 Uani . . . . . .
N14 N 0.3629(5) 0.8707(2) 0.91603(19) 0.0272 1.0000 Uani . . . . . .
N15 N 0.6852(6) 0.7331(3) 1.0100(3) 0.0592 1.0000 Uani . . . . . .
N16 N 0.3452(5) 0.9613(2) 0.7615(2) 0.0394 1.0000 Uani . . . . . .
C1 C 0.3982(6) 0.9417(3) 0.3818(2) 0.0306 1.0000 Uani . . . . . .
C2 C 0.5132(7) 0.9430(3) 0.4033(3) 0.0420 1.0000 Uani . . . . . .
C3 C 0.5182(7) 0.9701(3) 0.4333(3) 0.0465 1.0000 Uani . . . . . .
C4 C 0.4114(7) 0.9980(3) 0.4453(3) 0.0460 1.0000 Uani . . . . . .
C5 C 0.2967(7) 0.9965(3) 0.4269(3) 0.0425 1.0000 Uani . . . . . .
C6 C 0.2871(6) 0.9694(3) 0.3947(3) 0.0303 1.0000 Uani . . . . . .
C7 C 0.1636(6) 0.9665(2) 0.3779(2) 0.0250 1.0000 Uani . . . . . .
C8 C 0.0243(6) 0.9354(3) 0.3370(2) 0.0291 1.0000 Uani . . . . . .
C9 C 0.0328(6) 0.9372(3) 0.2828(2) 0.0296 1.0000 Uani . . . . . .
C10 C 0.1656(6) 0.8864(2) 0.2420(2) 0.0275 1.0000 Uani . . . . . .
C11 C 0.2828(6) 0.8592(2) 0.2305(3) 0.0312 1.0000 Uani . . . . . .
C12 C 0.2899(7) 0.8377(3) 0.1929(3) 0.0414 1.0000 Uani . . . . . .
C13 C 0.3980(7) 0.8108(3) 0.1822(3) 0.0461 1.0000 Uani . . . . . .
C14 C 0.5040(7) 0.8036(3) 0.2097(3) 0.0465 1.0000 Uani . . . . . .
C15 C 0.5010(7) 0.8250(3) 0.2450(3) 0.0423 1.0000 Uani . . . . . .
C16 C 0.3932(6) 0.8539(3) 0.2577(3) 0.0323 1.0000 Uani . . . . . .
C17 C 0.0514(6) 0.9899(3) 0.4002(2) 0.0303 1.0000 Uani . . . . . .
C18 C 0.0236(7) 1.0458(3) 0.3813(3) 0.0413 1.0000 Uani . . . . . .
C19 C -0.0770(8) 1.0678(3) 0.4036(3) 0.0521 1.0000 Uani . . . . . .
C20 C -0.1506(8) 1.0328(3) 0.4446(3) 0.0510 1.0000 Uani . . . . . .
C21 C -0.1235(7) 0.9771(3) 0.4638(3) 0.0413 1.0000 Uani . . . . . .
C22 C -0.0245(6) 0.9549(3) 0.4413(2) 0.0327 1.0000 Uani . . . . . .
C23 C -0.0763(9) 0.8618(3) 0.4911(3) 0.0513 1.0000 Uani . . . . . .
C24 C -0.0573(10) 0.8117(4) 0.4826(4) 0.0654 1.0000 Uani . . . . . .
C25 C -0.2285(10) 0.8196(4) 0.4311(4) 0.0776 1.0000 Uani . . . . . .
C26 C -0.2645(11) 0.8309(5) 0.3793(5) 0.0853 1.0000 Uani . . . . . .
C27 C -0.2075(10) 0.7854(4) 0.3623(4) 0.0705 1.0000 Uani . . . . . .
C28 C -0.0714(11) 0.7775(5) 0.3691(5) 0.0880 1.0000 Uani . . . . . .
C29 C -0.0417(10) 0.7703(4) 0.4225(5) 0.0793 1.0000 Uani . . . . . .
C30 C 0.0523(6) 0.8893(3) 0.2125(3) 0.0332 1.0000 Uani . . . . . .
C31 C -0.0121(7) 0.8426(3) 0.2254(3) 0.0385 1.0000 Uani . . . . . .
C32 C -0.1166(8) 0.8446(4) 0.1995(3) 0.0495 1.0000 Uani . . . . . .
C33 C -0.1567(7) 0.8930(3) 0.1607(3) 0.0473 1.0000 Uani . . . . . .
C34 C -0.0919(7) 0.9403(3) 0.1463(3) 0.0400 1.0000 Uani . . . . . .
C35 C 0.0123(6) 0.9378(3) 0.1728(3) 0.0327 1.0000 Uani . . . . . .
C36 C 0.0442(8) 1.0320(3) 0.1228(3) 0.0432 1.0000 Uani . . . . . .
C37 C 0.1286(8) 1.0751(3) 0.1196(3) 0.0441 1.0000 Uani . . . . . .
C38 C 0.0965(7) 1.1510(3) 0.1456(3) 0.0425 1.0000 Uani . . . . . .
C39 C 0.0573(8) 1.1667(3) 0.1907(3) 0.0505 1.0000 Uani . . . . . .
C40 C 0.1435(9) 1.1391(3) 0.2339(3) 0.0547 1.0000 Uani . . . . . .
C41 C 0.1587(8) 1.0779(3) 0.2487(3) 0.0502 1.0000 Uani . . . . . .
C42 C 0.1976(7) 1.0657(3) 0.2017(3) 0.0427 1.0000 Uani . . . . . .
C51 C 0.6901(6) 0.6463(3) 0.2489(3) 0.0319 1.0000 Uani . . . . . .
C52 C 0.7817(7) 0.6710(3) 0.2628(3) 0.0408 1.0000 Uani . . . . . .
C53 C 0.7582(7) 0.6899(3) 0.2999(3) 0.0444 1.0000 Uani . . . . . .
C54 C 0.6408(8) 0.6856(3) 0.3270(3) 0.0466 1.0000 Uani . . . . . .
C55 C 0.5461(7) 0.6625(3) 0.3147(3) 0.0351 1.0000 Uani . . . . . .
C56 C 0.5663(7) 0.6427(3) 0.2755(3) 0.0348 1.0000 Uani . . . . . .
C57 C 0.4660(6) 0.6184(2) 0.2639(3) 0.0316 1.0000 Uani . . . . . .
C58 C 0.3742(6) 0.5711(3) 0.2217(3) 0.0340 1.0000 Uani . . . . . .
C59 C 0.3908(6) 0.5752(3) 0.1672(3) 0.0320 1.0000 Uani . . . . . .
C60 C 0.5628(6) 0.5425(2) 0.1243(2) 0.0263 1.0000 Uani . . . . . .
C61 C 0.6944(6) 0.5389(3) 0.1045(2) 0.0286 1.0000 Uani . . . . . .
C62 C 0.7307(6) 0.5120(3) 0.0715(3) 0.0356 1.0000 Uani . . . . . .
C63 C 0.8516(7) 0.5103(3) 0.0509(3) 0.0412 1.0000 Uani . . . . . .
C64 C 0.9422(7) 0.5368(3) 0.0620(3) 0.0448 1.0000 Uani . . . . . .
C65 C 0.9108(6) 0.5632(3) 0.0936(3) 0.0396 1.0000 Uani . . . . . .
C66 C 0.7870(6) 0.5649(3) 0.1172(3) 0.0297 1.0000 Uani . . . . . .
C67 C 0.3391(6) 0.6190(3) 0.2926(2) 0.0316 1.0000 Uani . . . . . .
C68 C 0.2662(7) 0.6681(3) 0.2800(3) 0.0433 1.0000 Uani . . . . . .
C69 C 0.1482(8) 0.6696(4) 0.3068(3) 0.0560 1.0000 Uani . . . . . .
C70 C 0.1070(7) 0.6223(4) 0.3459(4) 0.0562 1.0000 Uani . . . . . .
C71 C 0.1794(7) 0.5733(4) 0.3590(3) 0.0472 1.0000 Uani . . . . . .
C72 C 0.2968(6) 0.5714(3) 0.3323(3) 0.0353 1.0000 Uani . . . . . .
C73 C 0.3315(8) 0.4738(3) 0.3800(3) 0.0482 1.0000 Uani . . . . . .
C74 C 0.4302(8) 0.4284(3) 0.3834(3) 0.0489 1.0000 Uani . . . . . .
C75 C 0.4703(8) 0.3568(3) 0.3523(3) 0.0508 1.0000 Uani . . . . . .
C76 C 0.4772(9) 0.3432(4) 0.3056(4) 0.0652 1.0000 Uani . . . . . .
C77 C 0.5785(10) 0.3729(3) 0.2662(4) 0.0644 1.0000 Uani . . . . . .
C78 C 0.5640(8) 0.4336(3) 0.2532(3) 0.0542 1.0000 Uani . . . . . .
C79 C 0.5554(7) 0.4437(3) 0.3022(3) 0.0469 1.0000 Uani . . . . . .
C80 C 0.4683(6) 0.5196(3) 0.1041(3) 0.0313 1.0000 Uani . . . . . .
C81 C 0.4593(7) 0.4633(3) 0.1234(3) 0.0395 1.0000 Uani . . . . . .
C82 C 0.3752(7) 0.4423(3) 0.1033(3) 0.0486 1.0000 Uani . . . . . .
C83 C 0.3034(8) 0.4777(4) 0.0639(3) 0.0526 1.0000 Uani . . . . . .
C84 C 0.3101(6) 0.5334(3) 0.0445(3) 0.0425 1.0000 Uani . . . . . .
C85 C 0.3932(6) 0.5551(3) 0.0650(3) 0.0342 1.0000 Uani . . . . . .
C86 C 0.3186(8) 0.6501(4) 0.0167(3) 0.0552 1.0000 Uani . . . . . .
C87 C 0.1984(9) 0.6560(4) 0.0448(4) 0.0670 1.0000 Uani . . . . . .
C88 C 0.2070(10) 0.7388(4) 0.0611(4) 0.0714 1.0000 Uani . . . . . .
C89 C 0.2111(11) 0.7601(4) 0.1016(5) 0.0833 1.0000 Uani . . . . . .
C90 C 0.0970(12) 0.7427(4) 0.1399(4) 0.0819 1.0000 Uani . . . . . .
C91 C 0.0939(12) 0.6827(5) 0.1618(5) 0.0951 1.0000 Uani . . . . . .
C92 C 0.0941(9) 0.6628(4) 0.1204(5) 0.0780 1.0000 Uani . . . . . .
C101 C 0.8354(6) 0.6326(3) 0.5172(3) 0.0318 1.0000 Uani . . . . . .
C102 C 0.7503(7) 0.6307(3) 0.4831(3) 0.0411 1.0000 Uani . . . . . .
C103 C 0.7755(8) 0.5999(3) 0.4555(3) 0.0468 1.0000 Uani . . . . . .
C104 C 0.8893(8) 0.5684(3) 0.4597(3) 0.0497 1.0000 Uani . . . . . .
C105 C 0.9751(8) 0.5700(3) 0.4908(3) 0.0405 1.0000 Uani . . . . . .
C106 C 0.9532(6) 0.6018(3) 0.5199(3) 0.0326 1.0000 Uani . . . . . .
C107 C 1.0466(6) 0.6006(3) 0.5536(3) 0.0333 1.0000 Uani . . . . . .
C108 C 1.1239(6) 0.6258(3) 0.6171(3) 0.0401 1.0000 Uani . . . . . .
C109 C 1.1290(7) 0.6796(3) 0.6185(3) 0.0453 1.0000 Uani . . . . . .
C110 C 0.9717(6) 0.7432(3) 0.6337(3) 0.0316 1.0000 Uani . . . . . .
C111 C 0.8517(6) 0.7749(3) 0.6272(3) 0.0303 1.0000 Uani . . . . . .
C112 C 0.8324(7) 0.8173(3) 0.6443(3) 0.0398 1.0000 Uani . . . . . .
C113 C 0.7237(7) 0.8512(3) 0.6351(4) 0.0518 1.0000 Uani . . . . . .
C114 C 0.6308(7) 0.8429(3) 0.6091(4) 0.0523 1.0000 Uani . . . . . .
C115 C 0.6453(6) 0.8025(3) 0.5919(3) 0.0441 1.0000 Uani . . . . . .
C116 C 0.7561(6) 0.7658(3) 0.6014(3) 0.0321 1.0000 Uani . . . . . .
C117 C 1.1638(7) 0.5619(3) 0.5601(3) 0.0429 1.0000 Uani . . . . . .
C118 C 1.2622(7) 0.5737(4) 0.5215(4) 0.0522 1.0000 Uani . . . . . .
C119 C 1.3712(8) 0.5376(4) 0.5300(4) 0.0655 1.0000 Uani . . . . . .
C120 C 1.3788(9) 0.4919(4) 0.5763(4) 0.0650 1.0000 Uani . . . . . .
C121 C 1.2826(8) 0.4795(4) 0.6146(4) 0.0562 1.0000 Uani . . . . . .
C122 C 1.1723(7) 0.5156(3) 0.6065(3) 0.0433 1.0000 Uani . . . . . .
C123 C 1.0802(9) 0.4673(3) 0.6927(3) 0.0541 1.0000 Uani . . . . . .
C124 C 0.9674(9) 0.4782(3) 0.7247(3) 0.0533 1.0000 Uani . . . . . .
C125 C 1.0671(8) 0.5157(4) 0.7729(4) 0.0554 1.0000 Uani . . . . . .
C126 C 1.0788(8) 0.5652(4) 0.7841(4) 0.0628 1.0000 Uani . . . . . .
C127 C 0.9496(8) 0.5850(4) 0.8010(4) 0.0611 1.0000 Uani . . . . . .
C128 C 0.8587(9) 0.5947(4) 0.7621(4) 0.0676 1.0000 Uani . . . . . .
C129 C 0.8536(8) 0.5452(4) 0.7510(4) 0.0599 1.0000 Uani . . . . . .
C130 C 1.0656(7) 0.7520(3) 0.6654(3) 0.0379 1.0000 Uani . . . . . .
C131 C 1.0462(8) 0.7303(3) 0.7186(3) 0.0471 1.0000 Uani . . . . . .
C132 C 1.1305(9) 0.7360(4) 0.7499(4) 0.0565 1.0000 Uani . . . . . .
C133 C 1.2335(9) 0.7641(4) 0.7257(4) 0.0632 1.0000 Uani . . . . . .
C134 C 1.2584(8) 0.7865(3) 0.6732(4) 0.0532 1.0000 Uani . . . . . .
C135 C 1.1705(7) 0.7801(3) 0.6426(3) 0.0395 1.0000 Uani . . . . . .
C136 C 1.2993(8) 0.8224(4) 0.5662(4) 0.0572 1.0000 Uani . . . . . .
C137 C 1.3026(8) 0.8340(3) 0.5094(3) 0.0555 1.0000 Uani . . . . . .
C138 C 1.4259(8) 0.7497(4) 0.5177(4) 0.0597 1.0000 Uani . . . . . .
C139 C 1.4326(10) 0.7004(4) 0.5062(4) 0.0734 1.0000 Uani . . . . . .
C140 C 1.4314(10) 0.7148(5) 0.4489(4) 0.0797 1.0000 Uani . . . . . .
C141 C 1.3126(10) 0.7505(5) 0.4302(5) 0.0844 1.0000 Uani . . . . . .
C142 C 1.3081(9) 0.7996(4) 0.4433(3) 0.0622 1.0000 Uani . . . . . .
C151 C 0.1865(6) 0.7281(3) 0.9011(3) 0.0318 1.0000 Uani . . . . . .
C152 C 0.0913(6) 0.6922(3) 0.9083(3) 0.0403 1.0000 Uani . . . . . .
C153 C 0.1122(7) 0.6483(3) 0.8957(3) 0.0426 1.0000 Uani . . . . . .
C154 C 0.2299(7) 0.6370(3) 0.8745(3) 0.0419 1.0000 Uani . . . . . .
C155 C 0.3247(7) 0.6712(3) 0.8673(3) 0.0371 1.0000 Uani . . . . . .
C156 C 0.3065(6) 0.7168(3) 0.8803(3) 0.0294 1.0000 Uani . . . . . .
C157 C 0.4125(6) 0.7487(3) 0.8750(3) 0.0321 1.0000 Uani . . . . . .
C158 C 0.5193(6) 0.8166(3) 0.8874(3) 0.0336 1.0000 Uani . . . . . .
C159 C 0.4770(6) 0.8736(3) 0.8816(3) 0.0353 1.0000 Uani . . . . . .
C160 C 0.3388(6) 0.9048(3) 0.9374(2) 0.0290 1.0000 Uani . . . . . .
C161 C 0.2240(6) 0.9044(3) 0.9699(3) 0.0323 1.0000 Uani . . . . . .
C162 C 0.2053(8) 0.9383(4) 0.9971(3) 0.0529 1.0000 Uani . . . . . .
C163 C 0.1012(9) 0.9381(4) 1.0287(4) 0.0636 1.0000 Uani . . . . . .
C164 C 0.0053(8) 0.9047(3) 1.0336(3) 0.0498 1.0000 Uani . . . . . .
C165 C 0.0157(7) 0.8728(3) 1.0072(3) 0.0386 1.0000 Uani . . . . . .
C166 C 0.1238(6) 0.8711(3) 0.9740(2) 0.0298 1.0000 Uani . . . . . .
C167 C 0.5428(6) 0.7312(3) 0.8566(3) 0.0405 1.0000 Uani . . . . . .
C168 C 0.5713(8) 0.7472(3) 0.8050(3) 0.0518 1.0000 Uani . . . . . .
C169 C 0.6967(9) 0.7341(4) 0.7869(4) 0.0636 1.0000 Uani . . . . . .
C170 C 0.7783(9) 0.7052(4) 0.8238(4) 0.0598 1.0000 Uani . . . . . .
C171 C 0.7511(8) 0.6883(3) 0.8762(4) 0.0538 1.0000 Uani . . . . . .
C172 C 0.6296(6) 0.7006(3) 0.8941(3) 0.0406 1.0000 Uani . . . . . .
C173 C 0.6775(8) 0.6585(4) 0.9837(4) 0.0645 1.0000 Uani . . . . . .
C174 C 0.7563(8) 0.6957(3) 0.9905(4) 0.0602 1.0000 Uani . . . . . .
C175 C 0.7633(8) 0.7788(4) 1.0012(4) 0.0683 1.0000 Uani . . . . . .
C176 C 0.6861(10) 0.8199(4) 1.0188(5) 0.0834 1.0000 Uani . . . . . .
C177 C 0.6501(13) 0.7917(6) 1.0768(5) 0.1018 1.0000 Uani . . . . . .
C178 C 0.5787(14) 0.7442(6) 1.0848(6) 0.1159 1.0000 Uani . . . . . .
C179 C 0.6545(12) 0.7054(5) 1.0643(4) 0.0893 1.0000 Uani . . . . . .
C180 C 0.4326(6) 0.9461(3) 0.9299(3) 0.0333 1.0000 Uani . . . . . .
C181 C 0.5077(7) 0.9402(3) 0.9686(3) 0.0428 1.0000 Uani . . . . . .
C182 C 0.6004(8) 0.9767(4) 0.9603(4) 0.0546 1.0000 Uani . . . . . .
C183 C 0.6114(8) 1.0207(4) 0.9131(4) 0.0537 1.0000 Uani . . . . . .
C184 C 0.5350(7) 1.0286(3) 0.8740(3) 0.0464 1.0000 Uani . . . . . .
C185 C 0.4468(7) 0.9902(3) 0.8824(3) 0.0387 1.0000 Uani . . . . . .
C186 C 0.3937(9) 1.0296(3) 0.7941(3) 0.0536 1.0000 Uani . . . . . .
C187 C 0.3096(9) 1.0155(3) 0.7623(3) 0.0552 1.0000 Uani . . . . . .
C188 C 0.2438(8) 0.9437(4) 0.7429(4) 0.0602 1.0000 Uani . . . . . .
C189 C 0.2778(8) 0.8892(4) 0.7403(4) 0.0612 1.0000 Uani . . . . . .
C190 C 0.3958(8) 0.8896(4) 0.7068(4) 0.0610 1.0000 Uani . . . . . .
C191 C 0.4993(8) 0.9088(5) 0.7260(5) 0.0919 1.0000 Uani . . . . . .
C192 C 0.4603(9) 0.9640(4) 0.7282(4) 0.0715 1.0000 Uani . . . . . .
H21 H 0.5879 0.9240 0.3962 0.0505 1.0000 Uiso R . . . . .
H31 H 0.5965 0.9703 0.4465 0.0559 1.0000 Uiso R . . . . .
H41 H 0.4166 1.0178 0.4659 0.0551 1.0000 Uiso R . . . . .
H51 H 0.2228 1.0143 0.4363 0.0512 1.0000 Uiso R . . . . .
H81 H -0.0340 0.9637 0.3391 0.0351 1.0000 Uiso R . . . . .
H82 H -0.0024 0.9010 0.3613 0.0351 1.0000 Uiso R . . . . .
H91 H 0.0311 0.9741 0.2581 0.0354 1.0000 Uiso R . . . . .
H92 H -0.0362 0.9200 0.2787 0.0354 1.0000 Uiso R . . . . .
H121 H 0.2176 0.8421 0.1743 0.0497 1.0000 Uiso R . . . . .
H131 H 0.4007 0.7971 0.1563 0.0554 1.0000 Uiso R . . . . .
H141 H 0.5783 0.7836 0.2037 0.0559 1.0000 Uiso R . . . . .
H151 H 0.5756 0.8205 0.2623 0.0509 1.0000 Uiso R . . . . .
H181 H 0.0735 1.0694 0.3528 0.0496 1.0000 Uiso R . . . . .
H191 H -0.0950 1.1063 0.3909 0.0625 1.0000 Uiso R . . . . .
H201 H -0.2204 1.0474 0.4596 0.0612 1.0000 Uiso R . . . . .
H211 H -0.1729 0.9537 0.4926 0.0495 1.0000 Uiso R . . . . .
H231 H -0.0594 0.8541 0.5256 0.0615 1.0000 Uiso R . . . . .
H232 H -0.1613 0.8765 0.4853 0.0615 1.0000 Uiso R . . . . .
H241 H 0.0301 0.8000 0.4844 0.0781 1.0000 Uiso R . . . . .
H242 H -0.1049 0.7845 0.5089 0.0781 1.0000 Uiso R . . . . .
H251 H -0.2678 0.8471 0.4414 0.0925 1.0000 Uiso R . . . . .
H252 H -0.2559 0.7850 0.4545 0.0925 1.0000 Uiso R . . . . .
H261 H -0.2343 0.8649 0.3557 0.1024 1.0000 Uiso R . . . . .
H262 H -0.3542 0.8328 0.3794 0.1024 1.0000 Uiso R . . . . .
H271 H -0.2462 0.7523 0.3828 0.0843 1.0000 Uiso R . . . . .
H272 H -0.2214 0.7957 0.3271 0.0843 1.0000 Uiso R . . . . .
H281 H -0.0318 0.8085 0.3442 0.1056 1.0000 Uiso R . . . . .
H282 H -0.0387 0.7458 0.3639 0.1056 1.0000 Uiso R . . . . .
H291 H 0.0475 0.7672 0.4247 0.0951 1.0000 Uiso R . . . . .
H292 H -0.0769 0.7383 0.4477 0.0951 1.0000 Uiso R . . . . .
H311 H 0.0159 0.8091 0.2521 0.0462 1.0000 Uiso R . . . . .
H321 H -0.1606 0.8126 0.2085 0.0594 1.0000 Uiso R . . . . .
H331 H -0.2294 0.8943 0.1434 0.0568 1.0000 Uiso R . . . . .
H341 H -0.1188 0.9734 0.1189 0.0480 1.0000 Uiso R . . . . .
H361 H -0.0412 1.0425 0.1299 0.0518 1.0000 Uiso R . . . . .
H362 H 0.0516 1.0284 0.0909 0.0518 1.0000 Uiso R . . . . .
H371 H 0.1150 1.1065 0.0885 0.0529 1.0000 Uiso R . . . . .
H372 H 0.2142 1.0611 0.1191 0.0529 1.0000 Uiso R . . . . .
H381 H 0.1769 1.1642 0.1309 0.0510 1.0000 Uiso R . . . . .
H382 H 0.0358 1.1670 0.1204 0.0510 1.0000 Uiso R . . . . .
H391 H 0.0593 1.2052 0.1790 0.0603 1.0000 Uiso R . . . . .
H392 H -0.0263 1.1564 0.2032 0.0603 1.0000 Uiso R . . . . .
H401 H 0.1087 1.1458 0.2630 0.0658 1.0000 Uiso R . . . . .
H402 H 0.2241 1.1537 0.2233 0.0658 1.0000 Uiso R . . . . .
H411 H 0.2219 1.0621 0.2729 0.0601 1.0000 Uiso R . . . . .
H412 H 0.0805 1.0625 0.2639 0.0601 1.0000 Uiso R . . . . .
H421 H 0.2777 1.0796 0.1874 0.0512 1.0000 Uiso R . . . . .
H422 H 0.2035 1.0273 0.2116 0.0512 1.0000 Uiso R . . . . .
H521 H 0.8633 0.6744 0.2452 0.0491 1.0000 Uiso R . . . . .
H531 H 0.8228 0.7065 0.3077 0.0533 1.0000 Uiso R . . . . .
H541 H 0.6257 0.6983 0.3537 0.0558 1.0000 Uiso R . . . . .
H551 H 0.4656 0.6598 0.3331 0.0421 1.0000 Uiso R . . . . .
H581 H 0.2956 0.5891 0.2268 0.0406 1.0000 Uiso R . . . . .
H582 H 0.3764 0.5338 0.2454 0.0406 1.0000 Uiso R . . . . .
H591 H 0.3609 0.6105 0.1440 0.0384 1.0000 Uiso R . . . . .
H592 H 0.3449 0.5483 0.1642 0.0384 1.0000 Uiso R . . . . .
H621 H 0.6687 0.4945 0.0633 0.0427 1.0000 Uiso R . . . . .
H631 H 0.8737 0.4913 0.0293 0.0494 1.0000 Uiso R . . . . .
H641 H 1.0264 0.5365 0.0473 0.0538 1.0000 Uiso R . . . . .
H651 H 0.9743 0.5812 0.1002 0.0474 1.0000 Uiso R . . . . .
H681 H 0.2959 0.7006 0.2534 0.0520 1.0000 Uiso R . . . . .
H691 H 0.0973 0.7030 0.2981 0.0673 1.0000 Uiso R . . . . .
H701 H 0.0275 0.6233 0.3640 0.0673 1.0000 Uiso R . . . . .
H711 H 0.1499 0.5411 0.3861 0.0567 1.0000 Uiso R . . . . .
H731 H 0.3175 0.4759 0.4126 0.0577 1.0000 Uiso R . . . . .
H732 H 0.2547 0.4668 0.3703 0.0577 1.0000 Uiso R . . . . .
H741 H 0.5084 0.4382 0.3893 0.0588 1.0000 Uiso R . . . . .
H742 H 0.4057 0.3962 0.4119 0.0588 1.0000 Uiso R . . . . .
H751 H 0.5475 0.3442 0.3689 0.0608 1.0000 Uiso R . . . . .
H752 H 0.4022 0.3392 0.3756 0.0608 1.0000 Uiso R . . . . .
H761 H 0.3979 0.3536 0.2905 0.0783 1.0000 Uiso R . . . . .
H762 H 0.4955 0.3049 0.3162 0.0783 1.0000 Uiso R . . . . .
H771 H 0.6589 0.3586 0.2796 0.0772 1.0000 Uiso R . . . . .
H772 H 0.5731 0.3673 0.2358 0.0772 1.0000 Uiso R . . . . .
H781 H 0.6351 0.4505 0.2317 0.0650 1.0000 Uiso R . . . . .
H782 H 0.4890 0.4489 0.2355 0.0650 1.0000 Uiso R . . . . .
H791 H 0.5429 0.4819 0.2934 0.0563 1.0000 Uiso R . . . . .
H792 H 0.6319 0.4300 0.3191 0.0563 1.0000 Uiso R . . . . .
H811 H 0.5103 0.4393 0.1503 0.0474 1.0000 Uiso R . . . . .
H821 H 0.3675 0.4040 0.1165 0.0582 1.0000 Uiso R . . . . .
H831 H 0.2474 0.4632 0.0497 0.0630 1.0000 Uiso R . . . . .
H841 H 0.2591 0.5569 0.0174 0.0510 1.0000 Uiso R . . . . .
H861 H 0.3555 0.6844 0.0019 0.0660 1.0000 Uiso R . . . . .
H862 H 0.3021 0.6397 -0.0099 0.0660 1.0000 Uiso R . . . . .
H871 H 0.1402 0.6788 0.0203 0.0802 1.0000 Uiso R . . . . .
H872 H 0.1671 0.6208 0.0629 0.0802 1.0000 Uiso R . . . . .
H881 H 0.2786 0.7499 0.0374 0.0856 1.0000 Uiso R . . . . .
H882 H 0.1318 0.7537 0.0435 0.0856 1.0000 Uiso R . . . . .
H891 H 0.2096 0.7989 0.0858 0.0999 1.0000 Uiso R . . . . .
H892 H 0.2866 0.7457 0.1191 0.0999 1.0000 Uiso R . . . . .
H901 H 0.1027 0.7541 0.1669 0.0981 1.0000 Uiso R . . . . .
H902 H 0.0217 0.7591 0.1228 0.0981 1.0000 Uiso R . . . . .
H911 H 0.1663 0.6666 0.1810 0.1138 1.0000 Uiso R . . . . .
H912 H 0.0195 0.6724 0.1839 0.1138 1.0000 Uiso R . . . . .
H921 H 0.0193 0.6774 0.1024 0.0932 1.0000 Uiso R . . . . .
H922 H 0.0955 0.6240 0.1357 0.0932 1.0000 Uiso R . . . . .
H1021 H 0.6720 0.6519 0.4795 0.0493 1.0000 Uiso R . . . . .
H1031 H 0.7152 0.5998 0.4332 0.0561 1.0000 Uiso R . . . . .
H1041 H 0.9067 0.5460 0.4410 0.0595 1.0000 Uiso R . . . . .
H1051 H 1.0533 0.5488 0.4931 0.0486 1.0000 Uiso R . . . . .
H1081 H 1.0967 0.6001 0.6502 0.0479 1.0000 Uiso R . . . . .
H1082 H 1.2053 0.6139 0.6071 0.0479 1.0000 Uiso R . . . . .
H1091 H 1.1622 0.6751 0.6498 0.0542 1.0000 Uiso R . . . . .
H1092 H 1.1816 0.7017 0.5901 0.0542 1.0000 Uiso R . . . . .
H1121 H 0.8958 0.8226 0.6626 0.0478 1.0000 Uiso R . . . . .
H1131 H 0.7124 0.8801 0.6463 0.0621 1.0000 Uiso R . . . . .
H1141 H 0.5549 0.8660 0.6033 0.0627 1.0000 Uiso R . . . . .
H1151 H 0.5808 0.7985 0.5733 0.0529 1.0000 Uiso R . . . . .
H1181 H 1.2554 0.6055 0.4902 0.0624 1.0000 Uiso R . . . . .
H1191 H 1.4391 0.5444 0.5042 0.0787 1.0000 Uiso R . . . . .
H1201 H 1.4536 0.4681 0.5818 0.0780 1.0000 Uiso R . . . . .
H1211 H 1.2899 0.4475 0.6457 0.0675 1.0000 Uiso R . . . . .
H1231 H 1.1565 0.4695 0.7061 0.0648 1.0000 Uiso R . . . . .
H1232 H 1.0786 0.4320 0.6929 0.0648 1.0000 Uiso R . . . . .
H1241 H 0.9613 0.4477 0.7570 0.0639 1.0000 Uiso R . . . . .
H1242 H 0.8931 0.4828 0.7071 0.0639 1.0000 Uiso R . . . . .
H1251 H 1.0387 0.4867 0.8038 0.0664 1.0000 Uiso R . . . . .
H1252 H 1.1477 0.5050 0.7610 0.0664 1.0000 Uiso R . . . . .
H1261 H 1.1348 0.5556 0.8108 0.0753 1.0000 Uiso R . . . . .
H1262 H 1.1116 0.5936 0.7538 0.0753 1.0000 Uiso R . . . . .
H1271 H 0.9569 0.6181 0.8047 0.0733 1.0000 Uiso R . . . . .
H1272 H 0.9205 0.5580 0.8332 0.0733 1.0000 Uiso R . . . . .
H1281 H 0.7769 0.6036 0.7745 0.0810 1.0000 Uiso R . . . . .
H1282 H 0.8836 0.6244 0.7311 0.0810 1.0000 Uiso R . . . . .
H1291 H 0.8238 0.5162 0.7816 0.0718 1.0000 Uiso R . . . . .
H1292 H 0.7967 0.5537 0.7248 0.0718 1.0000 Uiso R . . . . .
H1311 H 0.9728 0.7110 0.7343 0.0564 1.0000 Uiso R . . . . .
H1321 H 1.1167 0.7208 0.7864 0.0678 1.0000 Uiso R . . . . .
H1331 H 1.2918 0.7687 0.7465 0.0759 1.0000 Uiso R . . . . .
H1341 H 1.3323 0.8055 0.6579 0.0639 1.0000 Uiso R . . . . .
H1361 H 1.3059 0.8553 0.5701 0.0683 1.0000 Uiso R . . . . .
H1362 H 1.3677 0.7970 0.5816 0.0683 1.0000 Uiso R . . . . .
H1371 H 1.3741 0.8542 0.4924 0.0666 1.0000 Uiso R . . . . .
H1372 H 1.2275 0.8554 0.4957 0.0666 1.0000 Uiso R . . . . .
H1381 H 1.4975 0.7700 0.5013 0.0715 1.0000 Uiso R . . . . .
H1382 H 1.4257 0.7386 0.5540 0.0715 1.0000 Uiso R . . . . .
H1391 H 1.5085 0.6789 0.5185 0.0878 1.0000 Uiso R . . . . .
H1392 H 1.3619 0.6798 0.5236 0.0878 1.0000 Uiso R . . . . .
H1401 H 1.5036 0.7340 0.4311 0.0953 1.0000 Uiso R . . . . .
H1402 H 1.4316 0.6825 0.4432 0.0953 1.0000 Uiso R . . . . .
H1411 H 1.3122 0.7625 0.3938 0.1016 1.0000 Uiso R . . . . .
H1412 H 1.2407 0.7303 0.4464 0.1016 1.0000 Uiso R . . . . .
H1421 H 1.3790 0.8201 0.4261 0.0746 1.0000 Uiso R . . . . .
H1422 H 1.2323 0.8215 0.4318 0.0746 1.0000 Uiso R . . . . .
H1521 H 0.0099 0.6990 0.9225 0.0484 1.0000 Uiso R . . . . .
H1531 H 0.0458 0.6250 0.9015 0.0512 1.0000 Uiso R . . . . .
H1541 H 0.2445 0.6067 0.8652 0.0503 1.0000 Uiso R . . . . .
H1551 H 0.4054 0.6638 0.8531 0.0444 1.0000 Uiso R . . . . .
H1581 H 0.5602 0.7973 0.9186 0.0402 1.0000 Uiso R . . . . .
H1582 H 0.5759 0.8175 0.8591 0.0402 1.0000 Uiso R . . . . .
H1591 H 0.5418 0.8888 0.8909 0.0422 1.0000 Uiso R . . . . .
H1592 H 0.4583 0.8956 0.8469 0.0422 1.0000 Uiso R . . . . .
H1621 H 0.2688 0.9622 0.9932 0.0636 1.0000 Uiso R . . . . .
H1631 H 0.0936 0.9607 1.0472 0.0764 1.0000 Uiso R . . . . .
H1641 H -0.0679 0.9043 1.0558 0.0598 1.0000 Uiso R . . . . .
H1651 H -0.0516 0.8507 1.0108 0.0464 1.0000 Uiso R . . . . .
H1681 H 0.5091 0.7668 0.7812 0.0620 1.0000 Uiso R . . . . .
H1691 H 0.7206 0.7450 0.7512 0.0762 1.0000 Uiso R . . . . .
H1701 H 0.8610 0.6957 0.8126 0.0717 1.0000 Uiso R . . . . .
H1711 H 0.8139 0.6686 0.8998 0.0645 1.0000 Uiso R . . . . .
H1731 H 0.6302 0.6401 1.0153 0.0772 1.0000 Uiso R . . . . .
H1732 H 0.7312 0.6325 0.9751 0.0772 1.0000 Uiso R . . . . .
H1741 H 0.8178 0.6747 1.0142 0.0721 1.0000 Uiso R . . . . .
H1742 H 0.7977 0.7166 0.9581 0.0721 1.0000 Uiso R . . . . .
H1751 H 0.8365 0.7651 1.0203 0.0817 1.0000 Uiso R . . . . .
H1752 H 0.7880 0.7963 0.9655 0.0817 1.0000 Uiso R . . . . .
H1761 H 0.7351 0.8498 1.0122 0.0994 1.0000 Uiso R . . . . .
H1762 H 0.6115 0.8327 1.0004 0.0994 1.0000 Uiso R . . . . .
H1771 H 0.5987 0.8164 1.0879 0.1226 1.0000 Uiso R . . . . .
H1772 H 0.7242 0.7798 1.0955 0.1226 1.0000 Uiso R . . . . .
H1781 H 0.5588 0.7248 1.1207 0.1384 1.0000 Uiso R . . . . .
H1782 H 0.5027 0.7570 1.0674 0.1384 1.0000 Uiso R . . . . .
H1791 H 0.7306 0.6924 1.0816 0.1067 1.0000 Uiso R . . . . .
H1792 H 0.6061 0.6754 1.0704 0.1067 1.0000 Uiso R . . . . .
H1811 H 0.4963 0.9110 1.0016 0.0514 1.0000 Uiso R . . . . .
H1821 H 0.6549 0.9712 0.9866 0.0653 1.0000 Uiso R . . . . .
H1831 H 0.6727 1.0461 0.9075 0.0645 1.0000 Uiso R . . . . .
H1841 H 0.5423 1.0595 0.8419 0.0557 1.0000 Uiso R . . . . .
H1861 H 0.3739 1.0663 0.7902 0.0643 1.0000 Uiso R . . . . .
H1862 H 0.4802 1.0252 0.7835 0.0643 1.0000 Uiso R . . . . .
H1871 H 0.2248 1.0157 0.7764 0.0662 1.0000 Uiso R . . . . .
H1872 H 0.3152 1.0424 0.7279 0.0662 1.0000 Uiso R . . . . .
H1881 H 0.1704 0.9409 0.7656 0.0721 1.0000 Uiso R . . . . .
H1882 H 0.2264 0.9701 0.7094 0.0721 1.0000 Uiso R . . . . .
H1891 H 0.2904 0.8623 0.7742 0.0733 1.0000 Uiso R . . . . .
H1892 H 0.2100 0.8801 0.7268 0.0733 1.0000 Uiso R . . . . .
H1901 H 0.3821 0.9138 0.6721 0.0728 1.0000 Uiso R . . . . .
H1902 H 0.4189 0.8538 0.7087 0.0728 1.0000 Uiso R . . . . .
H1911 H 0.5171 0.8827 0.7597 0.1101 1.0000 Uiso R . . . . .
H1912 H 0.5730 0.9122 0.7034 0.1101 1.0000 Uiso R . . . . .
H1921 H 0.5267 0.9745 0.7413 0.0858 1.0000 Uiso R . . . . .
H1922 H 0.4457 0.9905 0.6944 0.0858 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.831(7)

loop_
_oxford_twin_element_scale_factors
0.7400(14)
0.2600(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . O1 . 1.833(5) yes
Ni1 . O2 . 1.827(5) yes
Ni1 . N1 . 1.860(5) yes
Ni1 . N2 . 1.853(5) yes
Ni2 . O5 . 1.836(4) yes
Ni2 . O6 . 1.842(4) yes
Ni2 . N5 . 1.874(5) yes
Ni2 . N6 . 1.861(5) yes
Ni3 . O9 . 1.828(5) yes
Ni3 . O10 . 1.841(5) yes
Ni3 . N9 . 1.870(5) yes
Ni3 . N10 . 1.859(5) yes
Ni4 . O13 . 1.843(4) yes
Ni4 . O14 . 1.835(4) yes
Ni4 . N13 . 1.858(5) yes
Ni4 . N14 . 1.869(5) yes
O1 . C1 . 1.288(8) yes
O2 . C16 . 1.277(8) yes
O3 . C22 . 1.356(8) yes
O3 . C23 . 1.447(8) yes
O4 . C35 . 1.367(8) yes
O4 . C36 . 1.415(8) yes
O5 . C51 . 1.298(8) yes
O6 . C66 . 1.294(8) yes
O7 . C72 . 1.365(8) yes
O7 . C73 . 1.450(8) yes
O8 . C85 . 1.360(8) yes
O8 . C86 . 1.454(8) yes
O9 . C101 . 1.292(8) yes
O10 . C116 . 1.299(8) yes
O11 . C122 . 1.358(10) yes
O11 . C123 . 1.435(9) yes
O12 . C135 . 1.357(9) yes
O12 . C136 . 1.430(9) yes
O13 . C151 . 1.292(8) yes
O14 . C166 . 1.295(8) yes
O15 . C172 . 1.321(10) yes
O15 . C173 . 1.468(9) yes
O16 . C185 . 1.351(9) yes
O16 . C186 . 1.436(9) yes
N1 . C7 . 1.275(8) yes
N1 . C8 . 1.499(7) yes
N2 . C9 . 1.491(7) yes
N2 . C10 . 1.299(8) yes
N3 . C24 . 1.490(11) yes
N3 . C25 . 1.395(12) yes
N3 . C29 . 1.489(11) yes
N4 . C37 . 1.461(9) yes
N4 . C38 . 1.469(9) yes
N4 . C42 . 1.463(9) yes
N5 . C57 . 1.297(8) yes
N5 . C58 . 1.477(8) yes
N6 . C59 . 1.475(8) yes
N6 . C60 . 1.279(8) yes
N7 . C74 . 1.480(10) yes
N7 . C75 . 1.472(9) yes
N7 . C79 . 1.463(9) yes
N8 . C87 . 1.488(11) yes
N8 . C88 . 1.439(11) yes
N8 . C92 . 1.514(12) yes
N9 . C107 . 1.304(8) yes
N9 . C108 . 1.473(8) yes
N10 . C109 . 1.481(8) yes
N10 . C110 . 1.299(8) yes
N11 . C124 . 1.475(10) yes
N11 . C125 . 1.455(9) yes
N11 . C129 . 1.461(10) yes
N12 . C137 . 1.485(11) yes
N12 . C138 . 1.455(9) yes
N12 . C142 . 1.470(10) yes
N13 . C157 . 1.302(8) yes
N13 . C158 . 1.496(8) yes
N14 . C159 . 1.469(8) yes
N14 . C160 . 1.290(8) yes
N15 . C174 . 1.453(11) yes
N15 . C175 . 1.479(11) yes
N15 . C179 . 1.433(12) yes
N16 . C187 . 1.478(9) yes
N16 . C188 . 1.451(10) yes
N16 . C192 . 1.459(10) yes
C1 . C2 . 1.434(9) yes
C1 . C6 . 1.429(9) yes
C2 . C3 . 1.345(10) yes
C2 . H21 . 0.950 no
C3 . C4 . 1.387(11) yes
C3 . H31 . 0.950 no
C4 . C5 . 1.389(10) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.404(10) yes
C5 . H51 . 0.950 no
C6 . C7 . 1.468(8) yes
C7 . C17 . 1.498(8) yes
C8 . C9 . 1.521(8) yes
C8 . H81 . 0.950 no
C8 . H82 . 0.950 no
C9 . H91 . 0.950 no
C9 . H92 . 0.950 no
C10 . C11 . 1.455(9) yes
C10 . C30 . 1.519(9) yes
C11 . C12 . 1.409(9) yes
C11 . C16 . 1.436(9) yes
C12 . C13 . 1.370(10) yes
C12 . H121 . 0.950 no
C13 . C14 . 1.393(11) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.346(10) yes
C14 . H141 . 0.950 no
C15 . C16 . 1.418(9) yes
C15 . H151 . 0.950 no
C17 . C18 . 1.382(9) yes
C17 . C22 . 1.402(9) yes
C18 . C19 . 1.393(10) yes
C18 . H181 . 0.950 no
C19 . C20 . 1.389(11) yes
C19 . H191 . 0.950 no
C20 . C21 . 1.375(11) yes
C20 . H201 . 0.950 no
C21 . C22 . 1.386(9) yes
C21 . H211 . 0.950 no
C23 . C24 . 1.458(11) yes
C23 . H231 . 0.950 no
C23 . H232 . 0.950 no
C24 . H241 . 0.950 no
C24 . H242 . 0.950 no
C25 . C26 . 1.464(14) yes
C25 . H251 . 0.950 no
C25 . H252 . 0.950 no
C26 . C27 . 1.541(13) yes
C26 . H261 . 0.950 no
C26 . H262 . 0.950 no
C27 . C28 . 1.463(14) yes
C27 . H271 . 0.950 no
C27 . H272 . 0.950 no
C28 . C29 . 1.517(15) yes
C28 . H281 . 0.950 no
C28 . H282 . 0.950 no
C29 . H291 . 0.950 no
C29 . H292 . 0.950 no
C30 . C31 . 1.391(9) yes
C30 . C35 . 1.389(9) yes
C31 . C32 . 1.382(10) yes
C31 . H311 . 0.950 no
C32 . C33 . 1.376(11) yes
C32 . H321 . 0.950 no
C33 . C34 . 1.402(10) yes
C33 . H331 . 0.950 no
C34 . C35 . 1.387(9) yes
C34 . H341 . 0.950 no
C36 . C37 . 1.509(10) yes
C36 . H361 . 0.950 no
C36 . H362 . 0.950 no
C37 . H371 . 0.950 no
C37 . H372 . 0.950 no
C38 . C39 . 1.519(10) yes
C38 . H381 . 0.950 no
C38 . H382 . 0.950 no
C39 . C40 . 1.499(12) yes
C39 . H391 . 0.950 no
C39 . H392 . 0.950 no
C40 . C41 . 1.518(11) yes
C40 . H401 . 0.950 no
C40 . H402 . 0.950 no
C41 . C42 . 1.518(11) yes
C41 . H411 . 0.950 no
C41 . H412 . 0.950 no
C42 . H421 . 0.950 no
C42 . H422 . 0.950 no
C51 . C52 . 1.410(9) yes
C51 . C56 . 1.443(10) yes
C52 . C53 . 1.346(10) yes
C52 . H521 . 0.950 no
C53 . C54 . 1.388(11) yes
C53 . H531 . 0.950 no
C54 . C55 . 1.383(10) yes
C54 . H541 . 0.950 no
C55 . C56 . 1.415(9) yes
C55 . H551 . 0.950 no
C56 . C57 . 1.442(9) yes
C57 . C67 . 1.507(9) yes
C58 . C59 . 1.508(9) yes
C58 . H581 . 0.950 no
C58 . H582 . 0.950 no
C59 . H591 . 0.950 no
C59 . H592 . 0.950 no
C60 . C61 . 1.464(9) yes
C60 . C80 . 1.508(8) yes
C61 . C62 . 1.412(9) yes
C61 . C66 . 1.424(8) yes
C62 . C63 . 1.362(10) yes
C62 . H621 . 0.950 no
C63 . C64 . 1.393(10) yes
C63 . H631 . 0.950 no
C64 . C65 . 1.358(10) yes
C64 . H641 . 0.950 no
C65 . C66 . 1.422(9) yes
C65 . H651 . 0.950 no
C67 . C68 . 1.388(9) yes
C67 . C72 . 1.394(9) yes
C68 . C69 . 1.407(11) yes
C68 . H681 . 0.950 no
C69 . C70 . 1.378(12) yes
C69 . H691 . 0.950 no
C70 . C71 . 1.380(12) yes
C70 . H701 . 0.950 no
C71 . C72 . 1.403(10) yes
C71 . H711 . 0.950 no
C73 . C74 . 1.502(11) yes
C73 . H731 . 0.950 no
C73 . H732 . 0.950 no
C74 . H741 . 0.950 no
C74 . H742 . 0.950 no
C75 . C76 . 1.516(12) yes
C75 . H751 . 0.950 no
C75 . H752 . 0.950 no
C76 . C77 . 1.501(13) yes
C76 . H761 . 0.950 no
C76 . H762 . 0.950 no
C77 . C78 . 1.514(11) yes
C77 . H771 . 0.950 no
C77 . H772 . 0.950 no
C78 . C79 . 1.525(11) yes
C78 . H781 . 0.950 no
C78 . H782 . 0.950 no
C79 . H791 . 0.950 no
C79 . H792 . 0.950 no
C80 . C81 . 1.392(10) yes
C80 . C85 . 1.393(9) yes
C81 . C82 . 1.391(10) yes
C81 . H811 . 0.950 no
C82 . C83 . 1.375(12) yes
C82 . H821 . 0.950 no
C83 . C84 . 1.374(11) yes
C83 . H831 . 0.950 no
C84 . C85 . 1.403(9) yes
C84 . H841 . 0.950 no
C86 . C87 . 1.467(12) yes
C86 . H861 . 0.950 no
C86 . H862 . 0.950 no
C87 . H871 . 0.950 no
C87 . H872 . 0.950 no
C88 . C89 . 1.494(14) yes
C88 . H881 . 0.950 no
C88 . H882 . 0.950 no
C89 . C90 . 1.522(15) yes
C89 . H891 . 0.950 no
C89 . H892 . 0.950 no
C90 . C91 . 1.473(14) yes
C90 . H901 . 0.950 no
C90 . H902 . 0.950 no
C91 . C92 . 1.484(15) yes
C91 . H911 . 0.950 no
C91 . H912 . 0.950 no
C92 . H921 . 0.950 no
C92 . H922 . 0.950 no
C101 . C102 . 1.416(9) yes
C101 . C106 . 1.420(9) yes
C102 . C103 . 1.351(10) yes
C102 . H1021 . 0.950 no
C103 . C104 . 1.389(11) yes
C103 . H1031 . 0.950 no
C104 . C105 . 1.354(10) yes
C104 . H1041 . 0.950 no
C105 . C106 . 1.405(9) yes
C105 . H1051 . 0.950 no
C106 . C107 . 1.443(9) yes
C107 . C117 . 1.512(9) yes
C108 . C109 . 1.473(10) yes
C108 . H1081 . 0.950 no
C108 . H1082 . 0.950 no
C109 . H1091 . 0.950 no
C109 . H1092 . 0.950 no
C110 . C111 . 1.442(9) yes
C110 . C130 . 1.511(9) yes
C111 . C112 . 1.405(9) yes
C111 . C116 . 1.413(9) yes
C112 . C113 . 1.372(10) yes
C112 . H1121 . 0.950 no
C113 . C114 . 1.383(11) yes
C113 . H1131 . 0.950 no
C114 . C115 . 1.356(10) yes
C114 . H1141 . 0.950 no
C115 . C116 . 1.427(9) yes
C115 . H1151 . 0.950 no
C117 . C118 . 1.398(11) yes
C117 . C122 . 1.396(11) yes
C118 . C119 . 1.405(12) yes
C118 . H1181 . 0.950 no
C119 . C120 . 1.387(14) yes
C119 . H1191 . 0.950 no
C120 . C121 . 1.377(14) yes
C120 . H1201 . 0.950 no
C121 . C122 . 1.417(10) yes
C121 . H1211 . 0.950 no
C123 . C124 . 1.511(12) yes
C123 . H1231 . 0.950 no
C123 . H1232 . 0.950 no
C124 . H1241 . 0.950 no
C124 . H1242 . 0.950 no
C125 . C126 . 1.512(11) yes
C125 . H1251 . 0.950 no
C125 . H1252 . 0.950 no
C126 . C127 . 1.526(12) yes
C126 . H1261 . 0.950 no
C126 . H1262 . 0.950 no
C127 . C128 . 1.473(12) yes
C127 . H1271 . 0.950 no
C127 . H1272 . 0.950 no
C128 . C129 . 1.498(13) yes
C128 . H1281 . 0.950 no
C128 . H1282 . 0.950 no
C129 . H1291 . 0.950 no
C129 . H1292 . 0.950 no
C130 . C131 . 1.385(11) yes
C130 . C135 . 1.365(10) yes
C131 . C132 . 1.390(10) yes
C131 . H1311 . 0.950 no
C132 . C133 . 1.357(13) yes
C132 . H1321 . 0.950 no
C133 . C134 . 1.373(13) yes
C133 . H1331 . 0.950 no
C134 . C135 . 1.412(10) yes
C134 . H1341 . 0.950 no
C136 . C137 . 1.517(12) yes
C136 . H1361 . 0.950 no
C136 . H1362 . 0.950 no
C137 . H1371 . 0.950 no
C137 . H1372 . 0.950 no
C138 . C139 . 1.486(13) yes
C138 . H1381 . 0.950 no
C138 . H1382 . 0.950 no
C139 . C140 . 1.519(13) yes
C139 . H1391 . 0.950 no
C139 . H1392 . 0.950 no
C140 . C141 . 1.505(13) yes
C140 . H1401 . 0.950 no
C140 . H1402 . 0.950 no
C141 . C142 . 1.510(14) yes
C141 . H1411 . 0.950 no
C141 . H1412 . 0.950 no
C142 . H1421 . 0.950 no
C142 . H1422 . 0.950 no
C151 . C152 . 1.417(9) yes
C151 . C156 . 1.409(9) yes
C152 . C153 . 1.363(10) yes
C152 . H1521 . 0.950 no
C153 . C154 . 1.394(10) yes
C153 . H1531 . 0.950 no
C154 . C155 . 1.382(9) yes
C154 . H1541 . 0.950 no
C155 . C156 . 1.411(9) yes
C155 . H1551 . 0.950 no
C156 . C157 . 1.448(9) yes
C157 . C167 . 1.529(9) yes
C158 . C159 . 1.498(9) yes
C158 . H1581 . 0.950 no
C158 . H1582 . 0.950 no
C159 . H1591 . 0.950 no
C159 . H1592 . 0.950 no
C160 . C161 . 1.453(9) yes
C160 . C180 . 1.508(9) yes
C161 . C162 . 1.412(10) yes
C161 . C166 . 1.430(9) yes
C162 . C163 . 1.352(11) yes
C162 . H1621 . 0.950 no
C163 . C164 . 1.391(11) yes
C163 . H1631 . 0.950 no
C164 . C165 . 1.348(10) yes
C164 . H1641 . 0.950 no
C165 . C166 . 1.421(9) yes
C165 . H1651 . 0.950 no
C167 . C168 . 1.362(11) yes
C167 . C172 . 1.411(11) yes
C168 . C169 . 1.443(12) yes
C168 . H1681 . 0.950 no
C169 . C170 . 1.356(13) yes
C169 . H1691 . 0.950 no
C170 . C171 . 1.379(13) yes
C170 . H1701 . 0.950 no
C171 . C172 . 1.399(10) yes
C171 . H1711 . 0.950 no
C173 . C174 . 1.457(12) yes
C173 . H1731 . 0.950 no
C173 . H1732 . 0.950 no
C174 . H1741 . 0.950 no
C174 . H1742 . 0.950 no
C175 . C176 . 1.526(14) yes
C175 . H1751 . 0.950 no
C175 . H1752 . 0.950 no
C176 . C177 . 1.534(15) yes
C176 . H1761 . 0.950 no
C176 . H1762 . 0.950 no
C177 . C178 . 1.484(18) yes
C177 . H1771 . 0.950 no
C177 . H1772 . 0.950 no
C178 . C179 . 1.519(16) yes
C178 . H1781 . 0.950 no
C178 . H1782 . 0.950 no
C179 . H1791 . 0.950 no
C179 . H1792 . 0.950 no
C180 . C181 . 1.377(10) yes
C180 . C185 . 1.390(10) yes
C181 . C182 . 1.400(10) yes
C181 . H1811 . 0.950 no
C182 . C183 . 1.380(12) yes
C182 . H1821 . 0.950 no
C183 . C184 . 1.383(12) yes
C183 . H1831 . 0.950 no
C184 . C185 . 1.401(9) yes
C184 . H1841 . 0.950 no
C186 . C187 . 1.515(12) yes
C186 . H1861 . 0.950 no
C186 . H1862 . 0.950 no
C187 . H1871 . 0.950 no
C187 . H1872 . 0.950 no
C188 . C189 . 1.504(12) yes
C188 . H1881 . 0.950 no
C188 . H1882 . 0.950 no
C189 . C190 . 1.496(11) yes
C189 . H1891 . 0.950 no
C189 . H1892 . 0.950 no
C190 . C191 . 1.504(12) yes
C190 . H1901 . 0.950 no
C190 . H1902 . 0.950 no
C191 . C192 . 1.524(14) yes
C191 . H1911 . 0.950 no
C191 . H1912 . 0.950 no
C192 . H1921 . 0.950 no
C192 . H1922 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Ni1 . O2 . 84.3(2) yes
O1 . Ni1 . N1 . 93.3(2) yes
O2 . Ni1 . N1 . 175.1(2) yes
O1 . Ni1 . N2 . 176.4(2) yes
O2 . Ni1 . N2 . 93.9(2) yes
N1 . Ni1 . N2 . 88.7(2) yes
O5 . Ni2 . O6 . 84.26(19) yes
O5 . Ni2 . N5 . 94.2(2) yes
O6 . Ni2 . N5 . 177.5(2) yes
O5 . Ni2 . N6 . 176.1(2) yes
O6 . Ni2 . N6 . 93.5(2) yes
N5 . Ni2 . N6 . 88.1(2) yes
O9 . Ni3 . O10 . 84.9(2) yes
O9 . Ni3 . N9 . 93.3(2) yes
O10 . Ni3 . N9 . 177.3(2) yes
O9 . Ni3 . N10 . 176.2(2) yes
O10 . Ni3 . N10 . 93.5(2) yes
N9 . Ni3 . N10 . 88.3(2) yes
O13 . Ni4 . O14 . 85.0(2) yes
O13 . Ni4 . N13 . 93.4(2) yes
O14 . Ni4 . N13 . 176.1(2) yes
O13 . Ni4 . N14 . 177.3(2) yes
O14 . Ni4 . N14 . 93.7(2) yes
N13 . Ni4 . N14 . 88.1(2) yes
Ni1 . O1 . C1 . 127.8(4) yes
Ni1 . O2 . C16 . 129.3(4) yes
C22 . O3 . C23 . 118.3(6) yes
C35 . O4 . C36 . 117.9(5) yes
Ni2 . O5 . C51 . 128.7(4) yes
Ni2 . O6 . C66 . 127.1(4) yes
C72 . O7 . C73 . 118.2(6) yes
C85 . O8 . C86 . 120.2(6) yes
Ni3 . O9 . C101 . 128.0(4) yes
Ni3 . O10 . C116 . 127.5(4) yes
C122 . O11 . C123 . 119.6(6) yes
C135 . O12 . C136 . 116.0(6) yes
Ni4 . O13 . C151 . 128.4(4) yes
Ni4 . O14 . C166 . 127.2(4) yes
C172 . O15 . C173 . 119.8(6) yes
C185 . O16 . C186 . 118.7(6) yes
Ni1 . N1 . C7 . 131.0(4) yes
Ni1 . N1 . C8 . 110.5(4) yes
C7 . N1 . C8 . 118.3(5) yes
Ni1 . N2 . C9 . 112.1(4) yes
Ni1 . N2 . C10 . 128.7(4) yes
C9 . N2 . C10 . 119.1(5) yes
C24 . N3 . C25 . 112.3(7) yes
C24 . N3 . C29 . 106.4(7) yes
C25 . N3 . C29 . 107.0(7) yes
C37 . N4 . C38 . 111.9(6) yes
C37 . N4 . C42 . 112.6(6) yes
C38 . N4 . C42 . 110.2(6) yes
Ni2 . N5 . C57 . 128.1(5) yes
Ni2 . N5 . C58 . 111.6(4) yes
C57 . N5 . C58 . 120.2(5) yes
Ni2 . N6 . C59 . 110.5(4) yes
Ni2 . N6 . C60 . 129.3(4) yes
C59 . N6 . C60 . 120.1(5) yes
C74 . N7 . C75 . 110.0(6) yes
C74 . N7 . C79 . 112.7(6) yes
C75 . N7 . C79 . 109.7(6) yes
C87 . N8 . C88 . 115.2(7) yes
C87 . N8 . C92 . 105.6(8) yes
C88 . N8 . C92 . 108.3(7) yes
Ni3 . N9 . C107 . 128.7(5) yes
Ni3 . N9 . C108 . 109.6(4) yes
C107 . N9 . C108 . 121.4(6) yes
Ni3 . N10 . C109 . 110.9(4) yes
Ni3 . N10 . C110 . 129.5(4) yes
C109 . N10 . C110 . 119.5(5) yes
C124 . N11 . C125 . 109.5(6) yes
C124 . N11 . C129 . 109.6(6) yes
C125 . N11 . C129 . 109.7(7) yes
C137 . N12 . C138 . 111.7(7) yes
C137 . N12 . C142 . 109.5(6) yes
C138 . N12 . C142 . 109.6(7) yes
Ni4 . N13 . C157 . 129.3(4) yes
Ni4 . N13 . C158 . 111.3(4) yes
C157 . N13 . C158 . 119.0(5) yes
Ni4 . N14 . C159 . 109.9(4) yes
Ni4 . N14 . C160 . 128.9(4) yes
C159 . N14 . C160 . 120.9(5) yes
C174 . N15 . C175 . 109.2(7) yes
C174 . N15 . C179 . 110.1(8) yes
C175 . N15 . C179 . 108.6(9) yes
C187 . N16 . C188 . 110.5(6) yes
C187 . N16 . C192 . 109.6(7) yes
C188 . N16 . C192 . 109.8(7) yes
O1 . C1 . C2 . 117.3(6) yes
O1 . C1 . C6 . 125.4(6) yes
C2 . C1 . C6 . 117.2(6) yes
C1 . C2 . C3 . 122.0(7) yes
C1 . C2 . H21 . 119.0 no
C3 . C2 . H21 . 119.0 no
C2 . C3 . C4 . 121.2(7) yes
C2 . C3 . H31 . 119.4 no
C4 . C3 . H31 . 119.4 no
C3 . C4 . C5 . 119.1(7) yes
C3 . C4 . H41 . 120.4 no
C5 . C4 . H41 . 120.5 no
C4 . C5 . C6 . 121.7(7) yes
C4 . C5 . H51 . 119.1 no
C6 . C5 . H51 . 119.1 no
C1 . C6 . C5 . 118.7(6) yes
C1 . C6 . C7 . 120.7(6) yes
C5 . C6 . C7 . 120.4(6) yes
C6 . C7 . N1 . 121.0(6) yes
C6 . C7 . C17 . 115.9(5) yes
N1 . C7 . C17 . 123.1(6) yes
N1 . C8 . C9 . 107.1(5) yes
N1 . C8 . H81 . 110.1 no
C9 . C8 . H81 . 110.1 no
N1 . C8 . H82 . 110.1 no
C9 . C8 . H82 . 110.1 no
H81 . C8 . H82 . 109.5 no
C8 . C9 . N2 . 107.4(5) yes
C8 . C9 . H91 . 110.0 no
N2 . C9 . H91 . 110.0 no
C8 . C9 . H92 . 110.0 no
N2 . C9 . H92 . 110.0 no
H91 . C9 . H92 . 109.5 no
N2 . C10 . C11 . 123.1(6) yes
N2 . C10 . C30 . 119.8(5) yes
C11 . C10 . C30 . 117.1(6) yes
C10 . C11 . C12 . 120.7(6) yes
C10 . C11 . C16 . 120.3(6) yes
C12 . C11 . C16 . 118.9(6) yes
C11 . C12 . C13 . 122.0(7) yes
C11 . C12 . H121 . 119.0 no
C13 . C12 . H121 . 119.0 no
C12 . C13 . C14 . 119.4(7) yes
C12 . C13 . H131 . 120.3 no
C14 . C13 . H131 . 120.3 no
C13 . C14 . C15 . 119.9(7) yes
C13 . C14 . H141 . 120.1 no
C15 . C14 . H141 . 120.1 no
C14 . C15 . C16 . 123.9(7) yes
C14 . C15 . H151 . 118.0 no
C16 . C15 . H151 . 118.0 no
C11 . C16 . C15 . 115.8(6) yes
C11 . C16 . O2 . 124.6(6) yes
C15 . C16 . O2 . 119.6(6) yes
C7 . C17 . C18 . 120.5(6) yes
C7 . C17 . C22 . 119.7(6) yes
C18 . C17 . C22 . 119.7(6) yes
C17 . C18 . C19 . 120.6(7) yes
C17 . C18 . H181 . 119.7 no
C19 . C18 . H181 . 119.7 no
C18 . C19 . C20 . 119.0(7) yes
C18 . C19 . H191 . 120.5 no
C20 . C19 . H191 . 120.5 no
C19 . C20 . C21 . 120.8(7) yes
C19 . C20 . H201 . 119.6 no
C21 . C20 . H201 . 119.6 no
C20 . C21 . C22 . 120.4(7) yes
C20 . C21 . H211 . 119.8 no
C22 . C21 . H211 . 119.8 no
C17 . C22 . C21 . 119.4(6) yes
C17 . C22 . O3 . 114.7(6) yes
C21 . C22 . O3 . 125.9(6) yes
O3 . C23 . C24 . 108.9(7) yes
O3 . C23 . H231 . 109.6 no
C24 . C23 . H231 . 109.6 no
O3 . C23 . H232 . 109.7 no
C24 . C23 . H232 . 109.6 no
H231 . C23 . H232 . 109.5 no
N3 . C24 . C23 . 112.8(8) yes
N3 . C24 . H241 . 108.6 no
C23 . C24 . H241 . 108.6 no
N3 . C24 . H242 . 108.7 no
C23 . C24 . H242 . 108.6 no
H241 . C24 . H242 . 109.5 no
N3 . C25 . C26 . 110.5(9) yes
N3 . C25 . H251 . 109.2 no
C26 . C25 . H251 . 109.2 no
N3 . C25 . H252 . 109.2 no
C26 . C25 . H252 . 109.2 no
H251 . C25 . H252 . 109.5 no
C25 . C26 . C27 . 110.6(9) yes
C25 . C26 . H261 . 109.2 no
C27 . C26 . H261 . 109.2 no
C25 . C26 . H262 . 109.2 no
C27 . C26 . H262 . 109.1 no
H261 . C26 . H262 . 109.5 no
C26 . C27 . C28 . 108.9(8) yes
C26 . C27 . H271 . 109.7 no
C28 . C27 . H271 . 109.6 no
C26 . C27 . H272 . 109.6 no
C28 . C27 . H272 . 109.6 no
H271 . C27 . H272 . 109.5 no
C27 . C28 . C29 . 112.3(9) yes
C27 . C28 . H281 . 108.7 no
C29 . C28 . H281 . 108.8 no
C27 . C28 . H282 . 108.8 no
C29 . C28 . H282 . 108.8 no
H281 . C28 . H282 . 109.5 no
C28 . C29 . N3 . 108.8(8) yes
C28 . C29 . H291 . 109.6 no
N3 . C29 . H291 . 109.6 no
C28 . C29 . H292 . 109.7 no
N3 . C29 . H292 . 109.7 no
H291 . C29 . H292 . 109.5 no
C10 . C30 . C31 . 119.5(6) yes
C10 . C30 . C35 . 120.9(6) yes
C31 . C30 . C35 . 119.6(6) yes
C30 . C31 . C32 . 120.3(7) yes
C30 . C31 . H311 . 119.8 no
C32 . C31 . H311 . 119.8 no
C31 . C32 . C33 . 119.8(7) yes
C31 . C32 . H321 . 120.1 no
C33 . C32 . H321 . 120.1 no
C32 . C33 . C34 . 121.0(7) yes
C32 . C33 . H331 . 119.5 no
C34 . C33 . H331 . 119.5 no
C33 . C34 . C35 . 118.7(7) yes
C33 . C34 . H341 . 120.7 no
C35 . C34 . H341 . 120.7 no
C30 . C35 . C34 . 120.6(7) yes
C30 . C35 . O4 . 115.6(6) yes
C34 . C35 . O4 . 123.8(6) yes
O4 . C36 . C37 . 109.4(6) yes
O4 . C36 . H361 . 109.5 no
C37 . C36 . H361 . 109.5 no
O4 . C36 . H362 . 109.5 no
C37 . C36 . H362 . 109.5 no
H361 . C36 . H362 . 109.5 no
C36 . C37 . N4 . 113.0(6) yes
C36 . C37 . H371 . 108.5 no
N4 . C37 . H371 . 108.6 no
C36 . C37 . H372 . 108.6 no
N4 . C37 . H372 . 108.6 no
H371 . C37 . H372 . 109.5 no
N4 . C38 . C39 . 110.6(6) yes
N4 . C38 . H381 . 109.2 no
C39 . C38 . H381 . 109.2 no
N4 . C38 . H382 . 109.2 no
C39 . C38 . H382 . 109.2 no
H381 . C38 . H382 . 109.5 no
C38 . C39 . C40 . 112.1(7) yes
C38 . C39 . H391 . 108.8 no
C40 . C39 . H391 . 108.8 no
C38 . C39 . H392 . 108.8 no
C40 . C39 . H392 . 108.8 no
H391 . C39 . H392 . 109.5 no
C39 . C40 . C41 . 110.9(7) yes
C39 . C40 . H401 . 109.1 no
C41 . C40 . H401 . 109.1 no
C39 . C40 . H402 . 109.1 no
C41 . C40 . H402 . 109.1 no
H401 . C40 . H402 . 109.5 no
C40 . C41 . C42 . 110.7(6) yes
C40 . C41 . H411 . 109.1 no
C42 . C41 . H411 . 109.1 no
C40 . C41 . H412 . 109.2 no
C42 . C41 . H412 . 109.2 no
H411 . C41 . H412 . 109.5 no
C41 . C42 . N4 . 110.4(6) yes
C41 . C42 . H421 . 109.2 no
N4 . C42 . H421 . 109.3 no
C41 . C42 . H422 . 109.3 no
N4 . C42 . H422 . 109.2 no
H421 . C42 . H422 . 109.5 no
O5 . C51 . C52 . 118.8(6) yes
O5 . C51 . C56 . 123.8(6) yes
C52 . C51 . C56 . 117.4(6) yes
C51 . C52 . C53 . 122.6(7) yes
C51 . C52 . H521 . 118.7 no
C53 . C52 . H521 . 118.7 no
C52 . C53 . C54 . 120.9(7) yes
C52 . C53 . H531 . 119.6 no
C54 . C53 . H531 . 119.5 no
C53 . C54 . C55 . 119.4(7) yes
C53 . C54 . H541 . 120.3 no
C55 . C54 . H541 . 120.3 no
C54 . C55 . C56 . 121.5(7) yes
C54 . C55 . H551 . 119.2 no
C56 . C55 . H551 . 119.3 no
C51 . C56 . C55 . 118.1(6) yes
C51 . C56 . C57 . 121.6(6) yes
C55 . C56 . C57 . 120.2(6) yes
C56 . C57 . N5 . 123.4(6) yes
C56 . C57 . C67 . 117.0(6) yes
N5 . C57 . C67 . 119.6(6) yes
N5 . C58 . C59 . 107.7(5) yes
N5 . C58 . H581 . 109.9 no
C59 . C58 . H581 . 109.9 no
N5 . C58 . H582 . 109.9 no
C59 . C58 . H582 . 109.9 no
H581 . C58 . H582 . 109.5 no
C58 . C59 . N6 . 108.0(5) yes
C58 . C59 . H591 . 109.8 no
N6 . C59 . H591 . 109.8 no
C58 . C59 . H592 . 109.8 no
N6 . C59 . H592 . 109.8 no
H591 . C59 . H592 . 109.5 no
N6 . C60 . C61 . 123.2(5) yes
N6 . C60 . C80 . 120.9(6) yes
C61 . C60 . C80 . 115.9(5) yes
C60 . C61 . C62 . 121.5(6) yes
C60 . C61 . C66 . 119.3(6) yes
C62 . C61 . C66 . 119.1(6) yes
C61 . C62 . C63 . 122.3(6) yes
C61 . C62 . H621 . 118.8 no
C63 . C62 . H621 . 118.8 no
C62 . C63 . C64 . 119.0(7) yes
C62 . C63 . H631 . 120.5 no
C64 . C63 . H631 . 120.5 no
C63 . C64 . C65 . 120.4(7) yes
C63 . C64 . H641 . 119.8 no
C65 . C64 . H641 . 119.8 no
C64 . C65 . C66 . 122.9(7) yes
C64 . C65 . H651 . 118.5 no
C66 . C65 . H651 . 118.5 no
C61 . C66 . C65 . 116.2(6) yes
C61 . C66 . O6 . 126.5(6) yes
C65 . C66 . O6 . 117.3(6) yes
C57 . C67 . C68 . 119.0(6) yes
C57 . C67 . C72 . 120.8(6) yes
C68 . C67 . C72 . 120.2(6) yes
C67 . C68 . C69 . 119.8(7) yes
C67 . C68 . H681 . 120.1 no
C69 . C68 . H681 . 120.1 no
C68 . C69 . C70 . 119.5(8) yes
C68 . C69 . H691 . 120.3 no
C70 . C69 . H691 . 120.2 no
C69 . C70 . C71 . 121.1(7) yes
C69 . C70 . H701 . 119.5 no
C71 . C70 . H701 . 119.4 no
C70 . C71 . C72 . 119.8(7) yes
C70 . C71 . H711 . 120.1 no
C72 . C71 . H711 . 120.1 no
C71 . C72 . C67 . 119.6(7) yes
C71 . C72 . O7 . 124.6(7) yes
C67 . C72 . O7 . 115.8(6) yes
O7 . C73 . C74 . 109.4(6) yes
O7 . C73 . H731 . 109.5 no
C74 . C73 . H731 . 109.5 no
O7 . C73 . H732 . 109.5 no
C74 . C73 . H732 . 109.5 no
H731 . C73 . H732 . 109.5 no
C73 . C74 . N7 . 115.0(6) yes
C73 . C74 . H741 . 108.1 no
N7 . C74 . H741 . 108.1 no
C73 . C74 . H742 . 108.1 no
N7 . C74 . H742 . 108.1 no
H741 . C74 . H742 . 109.5 no
N7 . C75 . C76 . 110.7(7) yes
N7 . C75 . H751 . 109.2 no
C76 . C75 . H751 . 109.2 no
N7 . C75 . H752 . 109.2 no
C76 . C75 . H752 . 109.1 no
H751 . C75 . H752 . 109.5 no
C75 . C76 . C77 . 111.1(7) yes
C75 . C76 . H761 . 109.1 no
C77 . C76 . H761 . 109.1 no
C75 . C76 . H762 . 109.0 no
C77 . C76 . H762 . 109.1 no
H761 . C76 . H762 . 109.5 no
C76 . C77 . C78 . 111.3(7) yes
C76 . C77 . H771 . 109.0 no
C78 . C77 . H771 . 109.0 no
C76 . C77 . H772 . 109.0 no
C78 . C77 . H772 . 109.0 no
H771 . C77 . H772 . 109.5 no
C77 . C78 . C79 . 110.4(7) yes
C77 . C78 . H781 . 109.2 no
C79 . C78 . H781 . 109.2 no
C77 . C78 . H782 . 109.3 no
C79 . C78 . H782 . 109.3 no
H781 . C78 . H782 . 109.5 no
C78 . C79 . N7 . 110.4(6) yes
C78 . C79 . H791 . 109.2 no
N7 . C79 . H791 . 109.2 no
C78 . C79 . H792 . 109.3 no
N7 . C79 . H792 . 109.3 no
H791 . C79 . H792 . 109.5 no
C60 . C80 . C81 . 120.1(6) yes
C60 . C80 . C85 . 119.3(6) yes
C81 . C80 . C85 . 120.6(6) yes
C80 . C81 . C82 . 119.8(7) yes
C80 . C81 . H811 . 120.1 no
C82 . C81 . H811 . 120.1 no
C81 . C82 . C83 . 119.2(8) yes
C81 . C82 . H821 . 120.4 no
C83 . C82 . H821 . 120.4 no
C82 . C83 . C84 . 122.0(7) yes
C82 . C83 . H831 . 119.0 no
C84 . C83 . H831 . 119.0 no
C83 . C84 . C85 . 119.4(7) yes
C83 . C84 . H841 . 120.3 no
C85 . C84 . H841 . 120.3 no
C84 . C85 . C80 . 119.1(7) yes
C84 . C85 . O8 . 125.4(6) yes
C80 . C85 . O8 . 115.5(6) yes
O8 . C86 . C87 . 112.3(7) yes
O8 . C86 . H861 . 108.8 no
C87 . C86 . H861 . 108.8 no
O8 . C86 . H862 . 108.7 no
C87 . C86 . H862 . 108.7 no
H861 . C86 . H862 . 109.5 no
N8 . C87 . C86 . 114.2(8) yes
N8 . C87 . H871 . 108.3 no
C86 . C87 . H871 . 108.3 no
N8 . C87 . H872 . 108.3 no
C86 . C87 . H872 . 108.3 no
H871 . C87 . H872 . 109.5 no
N8 . C88 . C89 . 112.1(8) yes
N8 . C88 . H881 . 108.8 no
C89 . C88 . H881 . 108.8 no
N8 . C88 . H882 . 108.8 no
C89 . C88 . H882 . 108.8 no
H881 . C88 . H882 . 109.5 no
C88 . C89 . C90 . 109.6(8) yes
C88 . C89 . H891 . 109.5 no
C90 . C89 . H891 . 109.4 no
C88 . C89 . H892 . 109.5 no
C90 . C89 . H892 . 109.4 no
H891 . C89 . H892 . 109.5 no
C89 . C90 . C91 . 109.6(8) yes
C89 . C90 . H901 . 109.4 no
C91 . C90 . H901 . 109.4 no
C89 . C90 . H902 . 109.4 no
C91 . C90 . H902 . 109.4 no
H901 . C90 . H902 . 109.5 no
C90 . C91 . C92 . 111.1(10) yes
C90 . C91 . H911 . 109.0 no
C92 . C91 . H911 . 109.1 no
C90 . C91 . H912 . 109.1 no
C92 . C91 . H912 . 109.1 no
H911 . C91 . H912 . 109.5 no
N8 . C92 . C91 . 111.4(8) yes
N8 . C92 . H921 . 109.0 no
C91 . C92 . H921 . 109.0 no
N8 . C92 . H922 . 108.9 no
C91 . C92 . H922 . 108.9 no
H921 . C92 . H922 . 109.5 no
O9 . C101 . C102 . 118.5(6) yes
O9 . C101 . C106 . 125.0(6) yes
C102 . C101 . C106 . 116.4(6) yes
C101 . C102 . C103 . 123.0(7) yes
C101 . C102 . H1021 . 118.5 no
C103 . C102 . H1021 . 118.5 no
C102 . C103 . C104 . 120.1(7) yes
C102 . C103 . H1031 . 119.9 no
C104 . C103 . H1031 . 119.9 no
C103 . C104 . C105 . 119.0(7) yes
C103 . C104 . H1041 . 120.5 no
C105 . C104 . H1041 . 120.5 no
C104 . C105 . C106 . 122.7(7) yes
C104 . C105 . H1051 . 118.6 no
C106 . C105 . H1051 . 118.7 no
C101 . C106 . C105 . 118.6(6) yes
C101 . C106 . C107 . 121.1(6) yes
C105 . C106 . C107 . 120.2(6) yes
C106 . C107 . N9 . 122.4(6) yes
C106 . C107 . C117 . 119.3(6) yes
N9 . C107 . C117 . 118.4(6) yes
N9 . C108 . C109 . 108.3(6) yes
N9 . C108 . H1081 . 109.8 no
C109 . C108 . H1081 . 109.8 no
N9 . C108 . H1082 . 109.8 no
C109 . C108 . H1082 . 109.8 no
H1081 . C108 . H1082 . 109.5 no
N10 . C109 . C108 . 108.8(6) yes
N10 . C109 . H1091 . 109.7 no
C108 . C109 . H1091 . 109.7 no
N10 . C109 . H1092 . 109.6 no
C108 . C109 . H1092 . 109.6 no
H1091 . C109 . H1092 . 109.5 no
N10 . C110 . C111 . 122.5(6) yes
N10 . C110 . C130 . 119.4(6) yes
C111 . C110 . C130 . 118.0(6) yes
C110 . C111 . C112 . 119.4(6) yes
C110 . C111 . C116 . 120.9(6) yes
C112 . C111 . C116 . 119.6(6) yes
C111 . C112 . C113 . 121.2(7) yes
C111 . C112 . H1121 . 119.4 no
C113 . C112 . H1121 . 119.4 no
C112 . C113 . C114 . 119.3(7) yes
C112 . C113 . H1131 . 120.4 no
C114 . C113 . H1131 . 120.4 no
C113 . C114 . C115 . 121.5(7) yes
C113 . C114 . H1141 . 119.2 no
C115 . C114 . H1141 . 119.2 no
C114 . C115 . C116 . 121.0(7) yes
C114 . C115 . H1151 . 119.5 no
C116 . C115 . H1151 . 119.5 no
C115 . C116 . C111 . 117.3(6) yes
C115 . C116 . O10 . 116.7(6) yes
C111 . C116 . O10 . 125.9(6) yes
C107 . C117 . C118 . 120.5(8) yes
C107 . C117 . C122 . 117.9(7) yes
C118 . C117 . C122 . 121.5(7) yes
C117 . C118 . C119 . 118.6(9) yes
C117 . C118 . H1181 . 120.7 no
C119 . C118 . H1181 . 120.7 no
C118 . C119 . C120 . 119.4(9) yes
C118 . C119 . H1191 . 120.3 no
C120 . C119 . H1191 . 120.3 no
C119 . C120 . C121 . 122.8(8) yes
C119 . C120 . H1201 . 118.6 no
C121 . C120 . H1201 . 118.6 no
C120 . C121 . C122 . 118.3(9) yes
C120 . C121 . H1211 . 120.9 no
C122 . C121 . H1211 . 120.8 no
C121 . C122 . C117 . 119.4(8) yes
C121 . C122 . O11 . 124.3(8) yes
C117 . C122 . O11 . 116.3(6) yes
O11 . C123 . C124 . 106.9(6) yes
O11 . C123 . H1231 . 110.1 no
C124 . C123 . H1231 . 110.1 no
O11 . C123 . H1232 . 110.1 no
C124 . C123 . H1232 . 110.1 no
H1231 . C123 . H1232 . 109.5 no
C123 . C124 . N11 . 112.2(7) yes
C123 . C124 . H1241 . 108.8 no
N11 . C124 . H1241 . 108.8 no
C123 . C124 . H1242 . 108.8 no
N11 . C124 . H1242 . 108.8 no
H1241 . C124 . H1242 . 109.5 no
N11 . C125 . C126 . 111.2(7) yes
N11 . C125 . H1251 . 109.0 no
C126 . C125 . H1251 . 109.0 no
N11 . C125 . H1252 . 109.0 no
C126 . C125 . H1252 . 109.0 no
H1251 . C125 . H1252 . 109.5 no
C125 . C126 . C127 . 110.3(8) yes
C125 . C126 . H1261 . 109.3 no
C127 . C126 . H1261 . 109.3 no
C125 . C126 . H1262 . 109.3 no
C127 . C126 . H1262 . 109.2 no
H1261 . C126 . H1262 . 109.5 no
C126 . C127 . C128 . 109.7(8) yes
C126 . C127 . H1271 . 109.4 no
C128 . C127 . H1271 . 109.4 no
C126 . C127 . H1272 . 109.4 no
C128 . C127 . H1272 . 109.4 no
H1271 . C127 . H1272 . 109.5 no
C127 . C128 . C129 . 111.5(8) yes
C127 . C128 . H1281 . 109.0 no
C129 . C128 . H1281 . 109.0 no
C127 . C128 . H1282 . 108.9 no
C129 . C128 . H1282 . 109.0 no
H1281 . C128 . H1282 . 109.5 no
C128 . C129 . N11 . 112.1(7) yes
C128 . C129 . H1291 . 108.9 no
N11 . C129 . H1291 . 108.8 no
C128 . C129 . H1292 . 108.8 no
N11 . C129 . H1292 . 108.8 no
H1291 . C129 . H1292 . 109.5 no
C110 . C130 . C131 . 119.4(7) yes
C110 . C130 . C135 . 121.4(7) yes
C131 . C130 . C135 . 119.2(7) yes
C130 . C131 . C132 . 122.2(8) yes
C130 . C131 . H1311 . 118.9 no
C132 . C131 . H1311 . 118.9 no
C131 . C132 . C133 . 116.7(9) yes
C131 . C132 . H1321 . 121.6 no
C133 . C132 . H1321 . 121.6 no
C132 . C133 . C134 . 124.0(8) yes
C132 . C133 . H1331 . 118.0 no
C134 . C133 . H1331 . 118.0 no
C133 . C134 . C135 . 117.7(8) yes
C133 . C134 . H1341 . 121.2 no
C135 . C134 . H1341 . 121.2 no
C134 . C135 . C130 . 120.3(8) yes
C134 . C135 . O12 . 124.7(7) yes
C130 . C135 . O12 . 115.1(6) yes
O12 . C136 . C137 . 108.5(7) yes
O12 . C136 . H1361 . 109.7 no
C137 . C136 . H1361 . 109.7 no
O12 . C136 . H1362 . 109.7 no
C137 . C136 . H1362 . 109.7 no
H1361 . C136 . H1362 . 109.5 no
C136 . C137 . N12 . 113.6(7) yes
C136 . C137 . H1371 . 108.4 no
N12 . C137 . H1371 . 108.4 no
C136 . C137 . H1372 . 108.4 no
N12 . C137 . H1372 . 108.4 no
H1371 . C137 . H1372 . 109.5 no
N12 . C138 . C139 . 110.4(8) yes
N12 . C138 . H1381 . 109.2 no
C139 . C138 . H1381 . 109.3 no
N12 . C138 . H1382 . 109.2 no
C139 . C138 . H1382 . 109.2 no
H1381 . C138 . H1382 . 109.5 no
C138 . C139 . C140 . 112.4(9) yes
C138 . C139 . H1391 . 108.7 no
C140 . C139 . H1391 . 108.7 no
C138 . C139 . H1392 . 108.7 no
C140 . C139 . H1392 . 108.8 no
H1391 . C139 . H1392 . 109.5 no
C139 . C140 . C141 . 107.6(9) yes
C139 . C140 . H1401 . 110.0 no
C141 . C140 . H1401 . 110.0 no
C139 . C140 . H1402 . 109.9 no
C141 . C140 . H1402 . 109.9 no
H1401 . C140 . H1402 . 109.5 no
C140 . C141 . C142 . 109.4(9) yes
C140 . C141 . H1411 . 109.5 no
C142 . C141 . H1411 . 109.5 no
C140 . C141 . H1412 . 109.5 no
C142 . C141 . H1412 . 109.5 no
H1411 . C141 . H1412 . 109.5 no
C141 . C142 . N12 . 112.4(7) yes
C141 . C142 . H1421 . 108.8 no
N12 . C142 . H1421 . 108.7 no
C141 . C142 . H1422 . 108.7 no
N12 . C142 . H1422 . 108.7 no
H1421 . C142 . H1422 . 109.5 no
O13 . C151 . C152 . 117.5(6) yes
O13 . C151 . C156 . 125.0(6) yes
C152 . C151 . C156 . 117.4(6) yes
C151 . C152 . C153 . 122.4(7) yes
C151 . C152 . H1521 . 118.8 no
C153 . C152 . H1521 . 118.8 no
C152 . C153 . C154 . 120.7(7) yes
C152 . C153 . H1531 . 119.7 no
C154 . C153 . H1531 . 119.6 no
C153 . C154 . C155 . 118.0(7) yes
C153 . C154 . H1541 . 121.0 no
C155 . C154 . H1541 . 121.0 no
C154 . C155 . C156 . 122.7(7) yes
C154 . C155 . H1551 . 118.7 no
C156 . C155 . H1551 . 118.7 no
C155 . C156 . C151 . 118.7(6) yes
C155 . C156 . C157 . 119.6(6) yes
C151 . C156 . C157 . 121.6(6) yes
C156 . C157 . N13 . 122.3(6) yes
C156 . C157 . C167 . 119.0(6) yes
N13 . C157 . C167 . 118.6(6) yes
N13 . C158 . C159 . 106.5(5) yes
N13 . C158 . H1581 . 110.2 no
C159 . C158 . H1581 . 110.2 no
N13 . C158 . H1582 . 110.2 no
C159 . C158 . H1582 . 110.2 no
H1581 . C158 . H1582 . 109.5 no
C158 . C159 . N14 . 107.9(5) yes
C158 . C159 . H1591 . 109.9 no
N14 . C159 . H1591 . 109.9 no
C158 . C159 . H1592 . 109.8 no
N14 . C159 . H1592 . 109.9 no
H1591 . C159 . H1592 . 109.5 no
N14 . C160 . C161 . 122.0(6) yes
N14 . C160 . C180 . 119.9(6) yes
C161 . C160 . C180 . 118.0(6) yes
C160 . C161 . C162 . 121.2(6) yes
C160 . C161 . C166 . 121.3(6) yes
C162 . C161 . C166 . 117.4(6) yes
C161 . C162 . C163 . 123.0(7) yes
C161 . C162 . H1621 . 118.5 no
C163 . C162 . H1621 . 118.5 no
C162 . C163 . C164 . 119.3(7) yes
C162 . C163 . H1631 . 120.3 no
C164 . C163 . H1631 . 120.3 no
C163 . C164 . C165 . 120.5(7) yes
C163 . C164 . H1641 . 119.8 no
C165 . C164 . H1641 . 119.8 no
C164 . C165 . C166 . 122.2(7) yes
C164 . C165 . H1651 . 118.9 no
C166 . C165 . H1651 . 118.9 no
C161 . C166 . C165 . 117.4(6) yes
C161 . C166 . O14 . 124.3(6) yes
C165 . C166 . O14 . 118.2(6) yes
C157 . C167 . C168 . 118.8(7) yes
C157 . C167 . C172 . 118.1(7) yes
C168 . C167 . C172 . 123.1(7) yes
C167 . C168 . C169 . 119.5(9) yes
C167 . C168 . H1681 . 120.3 no
C169 . C168 . H1681 . 120.2 no
C168 . C169 . C170 . 116.0(9) yes
C168 . C169 . H1691 . 122.0 no
C170 . C169 . H1691 . 122.0 no
C169 . C170 . C171 . 125.4(9) yes
C169 . C170 . H1701 . 117.3 no
C171 . C170 . H1701 . 117.3 no
C170 . C171 . C172 . 118.9(9) yes
C170 . C171 . H1711 . 120.5 no
C172 . C171 . H1711 . 120.5 no
C167 . C172 . C171 . 117.0(8) yes
C167 . C172 . O15 . 117.2(6) yes
C171 . C172 . O15 . 125.8(8) yes
O15 . C173 . C174 . 113.5(7) yes
O15 . C173 . H1731 . 108.5 no
C174 . C173 . H1731 . 108.5 no
O15 . C173 . H1732 . 108.4 no
C174 . C173 . H1732 . 108.5 no
H1731 . C173 . H1732 . 109.5 no
C173 . C174 . N15 . 113.3(8) yes
C173 . C174 . H1741 . 108.5 no
N15 . C174 . H1741 . 108.5 no
C173 . C174 . H1742 . 108.5 no
N15 . C174 . H1742 . 108.5 no
H1741 . C174 . H1742 . 109.5 no
N15 . C175 . C176 . 109.3(7) yes
N15 . C175 . H1751 . 109.5 no
C176 . C175 . H1751 . 109.5 no
N15 . C175 . H1752 . 109.5 no
C176 . C175 . H1752 . 109.5 no
H1751 . C175 . H1752 . 109.5 no
C175 . C176 . C177 . 109.2(9) yes
C175 . C176 . H1761 . 109.5 no
C177 . C176 . H1761 . 109.6 no
C175 . C176 . H1762 . 109.5 no
C177 . C176 . H1762 . 109.6 no
H1761 . C176 . H1762 . 109.5 no
C176 . C177 . C178 . 107.0(12) yes
C176 . C177 . H1771 . 110.1 no
C178 . C177 . H1771 . 110.1 no
C176 . C177 . H1772 . 110.1 no
C178 . C177 . H1772 . 110.1 no
H1771 . C177 . H1772 . 109.5 no
C177 . C178 . C179 . 111.9(11) yes
C177 . C178 . H1781 . 108.9 no
C179 . C178 . H1781 . 108.8 no
C177 . C178 . H1782 . 108.9 no
C179 . C178 . H1782 . 108.9 no
H1781 . C178 . H1782 . 109.5 no
C178 . C179 . N15 . 110.4(10) yes
C178 . C179 . H1791 . 109.2 no
N15 . C179 . H1791 . 109.2 no
C178 . C179 . H1792 . 109.3 no
N15 . C179 . H1792 . 109.3 no
H1791 . C179 . H1792 . 109.5 no
C160 . C180 . C181 . 121.4(6) yes
C160 . C180 . C185 . 119.6(6) yes
C181 . C180 . C185 . 119.0(6) yes
C180 . C181 . C182 . 121.1(8) yes
C180 . C181 . H1811 . 119.5 no
C182 . C181 . H1811 . 119.5 no
C181 . C182 . C183 . 118.9(8) yes
C181 . C182 . H1821 . 120.5 no
C183 . C182 . H1821 . 120.6 no
C182 . C183 . C184 . 121.4(7) yes
C182 . C183 . H1831 . 119.3 no
C184 . C183 . H1831 . 119.3 no
C183 . C184 . C185 . 118.7(8) yes
C183 . C184 . H1841 . 120.7 no
C185 . C184 . H1841 . 120.6 no
C184 . C185 . C180 . 120.9(7) yes
C184 . C185 . O16 . 124.3(7) yes
C180 . C185 . O16 . 114.8(6) yes
O16 . C186 . C187 . 106.7(6) yes
O16 . C186 . H1861 . 110.2 no
C187 . C186 . H1861 . 110.1 no
O16 . C186 . H1862 . 110.2 no
C187 . C186 . H1862 . 110.2 no
H1861 . C186 . H1862 . 109.5 no
C186 . C187 . N16 . 113.2(7) yes
C186 . C187 . H1871 . 108.6 no
N16 . C187 . H1871 . 108.5 no
C186 . C187 . H1872 . 108.5 no
N16 . C187 . H1872 . 108.5 no
H1871 . C187 . H1872 . 109.5 no
N16 . C188 . C189 . 112.0(7) yes
N16 . C188 . H1881 . 108.9 no
C189 . C188 . H1881 . 108.8 no
N16 . C188 . H1882 . 108.8 no
C189 . C188 . H1882 . 108.8 no
H1881 . C188 . H1882 . 109.5 no
C188 . C189 . C190 . 112.1(8) yes
C188 . C189 . H1891 . 108.8 no
C190 . C189 . H1891 . 108.8 no
C188 . C189 . H1892 . 108.8 no
C190 . C189 . H1892 . 108.8 no
H1891 . C189 . H1892 . 109.5 no
C189 . C190 . C191 . 108.1(7) yes
C189 . C190 . H1901 . 109.8 no
C191 . C190 . H1901 . 109.8 no
C189 . C190 . H1902 . 109.8 no
C191 . C190 . H1902 . 109.8 no
H1901 . C190 . H1902 . 109.5 no
C190 . C191 . C192 . 111.3(9) yes
C190 . C191 . H1911 . 109.0 no
C192 . C191 . H1911 . 109.0 no
C190 . C191 . H1912 . 109.0 no
C192 . C191 . H1912 . 109.0 no
H1911 . C191 . H1912 . 109.5 no
C191 . C192 . N16 . 111.0(8) yes
C191 . C192 . H1921 . 109.1 no
N16 . C192 . H1921 . 109.1 no
C191 . C192 . H1922 . 109.1 no
N16 . C192 . H1922 . 109.1 no
H1921 . C192 . H1922 . 109.5 no


loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C1 176.8(6) . . . . no
N1 Ni1 O1 C1 -7.5(6) . . . . no
O1 Ni1 O2 C16 -178.8(7) . . . . no
N2 Ni1 O2 C16 -2.0(7) . . . . no
O1 Ni1 N1 C7 7.5(6) . . . . no
O1 Ni1 N1 C8 -167.2(4) . . . . no
N2 Ni1 N1 C7 -169.5(6) . . . . no
N2 Ni1 N1 C8 15.8(4) . . . . no
O2 Ni1 N2 C9 -176.5(4) . . . . no
O2 Ni1 N2 C10 -1.3(6) . . . . no
N1 Ni1 N2 C9 7.7(4) . . . . no
N1 Ni1 N2 C10 -177.2(6) . . . . no
O5 Ni2 N5 C57 1.7(6) . . . . no
O5 Ni2 N5 C58 -175.9(5) . . . . no
N6 Ni2 N5 C57 -175.3(6) . . . . no
N6 Ni2 N5 C58 7.1(5) . . . . no
O6 Ni2 N6 C59 -165.8(5) . . . . no
O6 Ni2 N6 C60 10.9(6) . . . . no
N5 Ni2 N6 C59 16.2(5) . . . . no
N5 Ni2 N6 C60 -167.2(6) . . . . no
O6 Ni2 O5 C51 178.3(7) . . . . no
N5 Ni2 O5 C51 -3.7(7) . . . . no
O5 Ni2 O6 C66 173.2(6) . . . . no
N6 Ni2 O6 C66 -10.0(6) . . . . no
O10 Ni3 N10 C109 -176.0(5) . . . . no
O10 Ni3 N10 C110 0.5(7) . . . . no
N10 Ni3 N9 C108 16.7(5) . . . . no
N9 Ni3 N10 C110 -177.4(6) . . . . no
O10 Ni3 O9 C101 169.1(6) . . . . no
N9 Ni3 O9 C101 -13.1(6) . . . . no
O9 Ni3 O10 C116 -172.7(6) . . . . no
N10 Ni3 O10 C116 3.9(6) . . . . no
O9 Ni3 N9 C107 7.1(6) . . . . no
O9 Ni3 N9 C108 -166.7(4) . . . . no
N10 Ni3 N9 C107 -169.5(6) . . . . no
N9 Ni3 N10 C109 6.0(5) . . . . no
N14 Ni4 O14 C166 -17.0(5) . . . . no
O13 Ni4 N13 C157 -1.1(6) . . . . no
O13 Ni4 O14 C166 165.3(5) . . . . no
N14 Ni4 N13 C157 -178.8(6) . . . . no
N14 Ni4 N13 C158 8.8(5) . . . . no
O13 Ni4 N13 C158 -173.5(4) . . . . no
N13 Ni4 N14 C159 16.2(4) . . . . no
N13 Ni4 O13 C151 1.0(6) . . . . no
O14 Ni4 N14 C160 7.3(6) . . . . no
N13 Ni4 N14 C160 -169.2(6) . . . . no
O14 Ni4 N14 C159 -167.2(4) . . . . no
O14 Ni4 O13 C151 -175.5(6) . . . . no
Ni1 O1 C1 C2 -176.5(5) . . . . no
Ni1 O1 C1 C6 2.2(10) . . . . no
Ni1 O2 C16 C11 4.8(11) . . . . no
Ni1 O2 C16 C15 -177.3(5) . . . . no
C23 O3 C22 C21 11.8(10) . . . . no
C23 O3 C22 C17 -169.0(6) . . . . no
C22 O3 C23 C24 153.0(7) . . . . no
C36 O4 C35 C34 -0.1(11) . . . . no
C35 O4 C36 C37 177.5(6) . . . . no
C36 O4 C35 C30 -179.6(7) . . . . no
Ni2 O5 C51 C56 4.7(11) . . . . no
Ni2 O5 C51 C52 -177.7(5) . . . . no
Ni2 O6 C66 C65 -175.6(5) . . . . no
Ni2 O6 C66 C61 4.3(11) . . . . no
C73 O7 C72 C67 -175.8(6) . . . . no
C72 O7 C73 C74 179.0(6) . . . . no
C73 O7 C72 C71 3.1(11) . . . . no
C86 O8 C85 C84 11.1(11) . . . . no
C85 O8 C86 C87 77.0(10) . . . . no
C86 O8 C85 C80 -168.6(7) . . . . no
Ni3 O9 C101 C102 -168.4(5) . . . . no
Ni3 O9 C101 C106 11.2(11) . . . . no
Ni3 O10 C116 C115 170.7(5) . . . . no
Ni3 O10 C116 C111 -5.9(11) . . . . no
C123 O11 C122 C121 10.6(12) . . . . no
C123 O11 C122 C117 -169.7(7) . . . . no
C122 O11 C123 C124 166.6(7) . . . . no
C135 O12 C136 C137 171.3(7) . . . . no
C136 O12 C135 C130 -171.3(8) . . . . no
C136 O12 C135 C134 8.1(12) . . . . no
Ni4 O13 C151 C152 175.2(5) . . . . no
Ni4 O13 C151 C156 -1.1(11) . . . . no
Ni4 O14 C166 C165 -164.1(5) . . . . no
Ni4 O14 C166 C161 16.3(9) . . . . no
C172 O15 C173 C174 78.8(10) . . . . no
C173 O15 C172 C171 6.0(13) . . . . no
C173 O15 C172 C167 -174.3(8) . . . . no
C186 O16 C185 C184 13.8(11) . . . . no
C186 O16 C185 C180 -167.3(7) . . . . no
C185 O16 C186 C187 168.8(7) . . . . no
Ni1 N1 C7 C17 -179.2(4) . . . . no
C8 N1 C7 C6 172.5(6) . . . . no
C8 N1 C7 C17 -4.8(9) . . . . no
Ni1 N1 C7 C6 -1.9(9) . . . . no
Ni1 N1 C8 C9 -34.6(7) . . . . no
C7 N1 C8 C9 149.9(6) . . . . no
C9 N2 C10 C11 176.6(6) . . . . no
Ni1 N2 C10 C11 1.8(9) . . . . no
Ni1 N2 C10 C30 -178.6(5) . . . . no
C10 N2 C9 C8 155.8(6) . . . . no
Ni1 N2 C9 C8 -28.6(7) . . . . no
C9 N2 C10 C30 -3.8(9) . . . . no
C29 N3 C25 C26 -67.8(12) . . . . no
C24 N3 C29 C28 -175.9(9) . . . . no
C24 N3 C25 C26 175.8(10) . . . . no
C25 N3 C24 C23 -78.1(11) . . . . no
C29 N3 C24 C23 165.2(8) . . . . no
C25 N3 C29 C28 63.9(11) . . . . no
C38 N4 C37 C36 -133.9(7) . . . . no
C42 N4 C37 C36 101.3(8) . . . . no
C42 N4 C38 C39 -59.9(8) . . . . no
C38 N4 C42 C41 61.6(8) . . . . no
C37 N4 C42 C41 -172.6(7) . . . . no
C37 N4 C38 C39 173.9(6) . . . . no
Ni2 N5 C57 C67 177.5(5) . . . . no
C58 N5 C57 C67 -5.1(10) . . . . no
Ni2 N5 C58 C59 -28.0(7) . . . . no
C58 N5 C57 C56 176.8(7) . . . . no
C57 N5 C58 C59 154.2(7) . . . . no
Ni2 N5 C57 C56 -0.6(10) . . . . no
Ni2 N6 C60 C80 177.5(5) . . . . no
C60 N6 C59 C58 147.8(6) . . . . no
C59 N6 C60 C61 170.7(6) . . . . no
Ni2 N6 C60 C61 -5.7(9) . . . . no
C59 N6 C60 C80 -6.2(9) . . . . no
Ni2 N6 C59 C58 -35.2(7) . . . . no
C74 N7 C79 C78 -175.3(6) . . . . no
C75 N7 C79 C78 61.8(8) . . . . no
C79 N7 C75 C76 -61.2(8) . . . . no
C79 N7 C74 C73 96.2(8) . . . . no
C75 N7 C74 C73 -141.2(7) . . . . no
C74 N7 C75 C76 174.3(7) . . . . no
C92 N8 C87 C86 -158.7(9) . . . . no
C88 N8 C92 C91 -57.9(12) . . . . no
C92 N8 C88 C89 59.4(11) . . . . no
C88 N8 C87 C86 82.0(11) . . . . no
C87 N8 C92 C91 178.2(9) . . . . no
C87 N8 C88 C89 177.3(8) . . . . no
Ni3 N9 C107 C106 0.9(11) . . . . no
Ni3 N9 C108 C109 -35.5(6) . . . . no
C108 N9 C107 C106 174.1(7) . . . . no
C108 N9 C107 C117 -5.2(10) . . . . no
C107 N9 C108 C109 150.1(7) . . . . no
Ni3 N9 C107 C117 -178.5(5) . . . . no
Ni3 N10 C109 C108 -27.3(7) . . . . no
C109 N10 C110 C111 173.3(7) . . . . no
Ni3 N10 C110 C130 173.9(5) . . . . no
Ni3 N10 C110 C111 -3.0(11) . . . . no
C110 N10 C109 C108 155.8(7) . . . . no
C109 N10 C110 C130 -9.9(10) . . . . no
C125 N11 C129 C128 58.4(11) . . . . no
C129 N11 C124 C123 163.4(7) . . . . no
C129 N11 C125 C126 -58.7(10) . . . . no
C124 N11 C129 C128 178.6(7) . . . . no
C125 N11 C124 C123 -76.1(8) . . . . no
C124 N11 C125 C126 -179.0(7) . . . . no
C142 N12 C138 C139 -57.7(10) . . . . no
C138 N12 C137 C136 -60.9(9) . . . . no
C137 N12 C138 C139 -179.2(7) . . . . no
C138 N12 C142 C141 58.8(10) . . . . no
C137 N12 C142 C141 -178.3(8) . . . . no
C142 N12 C137 C136 177.5(7) . . . . no
Ni4 N13 C158 C159 -30.8(7) . . . . no
C157 N13 C158 C159 155.9(7) . . . . no
C158 N13 C157 C156 173.1(7) . . . . no
Ni4 N13 C157 C156 1.2(11) . . . . no
C158 N13 C157 C167 -2.5(10) . . . . no
Ni4 N13 C157 C167 -174.4(5) . . . . no
C159 N14 C160 C161 177.3(6) . . . . no
Ni4 N14 C160 C161 3.3(9) . . . . no
C159 N14 C160 C180 -4.0(9) . . . . no
Ni4 N14 C159 C158 -37.1(6) . . . . no
C160 N14 C159 C158 147.8(6) . . . . no
Ni4 N14 C160 C180 -178.0(5) . . . . no
C175 N15 C174 C173 -163.4(8) . . . . no
C174 N15 C175 C176 176.7(8) . . . . no
C175 N15 C179 C178 61.1(12) . . . . no
C179 N15 C174 C173 77.3(11) . . . . no
C179 N15 C175 C176 -63.1(11) . . . . no
C174 N15 C179 C178 -179.3(9) . . . . no
C187 N16 C188 C189 178.6(7) . . . . no
C188 N16 C192 C191 -58.0(10) . . . . no
C192 N16 C188 C189 57.6(10) . . . . no
C192 N16 C187 C186 -74.4(8) . . . . no
C188 N16 C187 C186 164.6(7) . . . . no
C187 N16 C192 C191 -179.4(7) . . . . no
C2 C1 C6 C5 0.6(11) . . . . no
C6 C1 C2 C3 -1.6(11) . . . . no
O1 C1 C6 C7 6.3(11) . . . . no
O1 C1 C2 C3 177.2(7) . . . . no
C2 C1 C6 C7 -175.1(6) . . . . no
O1 C1 C6 C5 -178.1(7) . . . . no
C1 C2 C3 C4 0.5(13) . . . . no
C2 C3 C4 C5 1.7(12) . . . . no
C3 C4 C5 C6 -2.7(12) . . . . no
C4 C5 C6 C1 1.5(12) . . . . no
C4 C5 C6 C7 177.2(7) . . . . no
C5 C6 C7 N1 178.1(7) . . . . no
C1 C6 C7 C17 171.1(6) . . . . no
C5 C6 C7 C17 -4.5(10) . . . . no
C1 C6 C7 N1 -6.3(10) . . . . no
C6 C7 C17 C22 -100.6(7) . . . . no
N1 C7 C17 C18 -104.5(8) . . . . no
N1 C7 C17 C22 76.8(8) . . . . no
C6 C7 C17 C18 78.1(8) . . . . no
N1 C8 C9 N2 39.7(7) . . . . no
C30 C10 C11 C16 -178.7(7) . . . . no
C30 C10 C11 C12 1.2(10) . . . . no
C11 C10 C30 C31 74.7(9) . . . . no
N2 C10 C30 C31 -104.9(8) . . . . no
N2 C10 C30 C35 75.3(9) . . . . no
N2 C10 C11 C12 -179.2(7) . . . . no
N2 C10 C11 C16 0.9(10) . . . . no
C11 C10 C30 C35 -105.1(8) . . . . no
C10 C11 C16 C15 177.8(7) . . . . no
C12 C11 C16 C15 -2.1(11) . . . . no
C16 C11 C12 C13 1.5(12) . . . . no
C10 C11 C16 O2 -4.3(12) . . . . no
C10 C11 C12 C13 -178.4(7) . . . . no
C12 C11 C16 O2 175.8(7) . . . . no
C11 C12 C13 C14 1.0(12) . . . . no
C12 C13 C14 C15 -2.7(12) . . . . no
C13 C14 C15 C16 2.0(13) . . . . no
C14 C15 C16 O2 -177.6(8) . . . . no
C14 C15 C16 C11 0.5(12) . . . . no
C22 C17 C18 C19 1.8(11) . . . . no
C7 C17 C22 C21 176.0(6) . . . . no
C7 C17 C18 C19 -176.9(7) . . . . no
C7 C17 C22 O3 -3.2(8) . . . . no
C18 C17 C22 C21 -2.6(10) . . . . no
C18 C17 C22 O3 178.2(6) . . . . no
C17 C18 C19 C20 -1.1(12) . . . . no
C18 C19 C20 C21 1.3(12) . . . . no
C19 C20 C21 C22 -2.2(12) . . . . no
C20 C21 C22 O3 -178.1(7) . . . . no
C20 C21 C22 C17 2.8(11) . . . . no
O3 C23 C24 N3 -67.3(10) . . . . no
N3 C25 C26 C27 62.5(13) . . . . no
C25 C26 C27 C28 -52.0(13) . . . . no
C26 C27 C28 C29 50.5(14) . . . . no
C27 C28 C29 N3 -57.4(13) . . . . no
C35 C30 C31 C32 -1.1(12) . . . . no
C10 C30 C35 O4 0.1(11) . . . . no
C10 C30 C31 C32 179.1(7) . . . . no
C10 C30 C35 C34 -179.4(7) . . . . no
C31 C30 C35 C34 0.7(12) . . . . no
C31 C30 C35 O4 -179.8(7) . . . . no
C30 C31 C32 C33 0.2(13) . . . . no
C31 C32 C33 C34 1.1(13) . . . . no
C32 C33 C34 C35 -1.5(12) . . . . no
C33 C34 C35 O4 -178.9(7) . . . . no
C33 C34 C35 C30 0.6(12) . . . . no
O4 C36 C37 N4 -71.7(8) . . . . no
N4 C38 C39 C40 55.2(9) . . . . no
C38 C39 C40 C41 -51.3(9) . . . . no
C39 C40 C41 C42 52.4(9) . . . . no
C40 C41 C42 N4 -57.7(9) . . . . no
C52 C51 C56 C57 179.7(7) . . . . no
O5 C51 C52 C53 -176.5(8) . . . . no
O5 C51 C56 C57 -2.7(12) . . . . no
C56 C51 C52 C53 1.3(12) . . . . no
O5 C51 C56 C55 175.7(7) . . . . no
C52 C51 C56 C55 -1.9(11) . . . . no
C51 C52 C53 C54 0.4(13) . . . . no
C52 C53 C54 C55 -1.4(13) . . . . no
C53 C54 C55 C56 0.6(13) . . . . no
C54 C55 C56 C51 1.1(12) . . . . no
C54 C55 C56 C57 179.5(8) . . . . no
C55 C56 C57 N5 -177.8(7) . . . . no
C55 C56 C57 C67 4.1(11) . . . . no
C51 C56 C57 C67 -177.5(7) . . . . no
C51 C56 C57 N5 0.6(12) . . . . no
N5 C57 C67 C72 76.2(9) . . . . no
C56 C57 C67 C72 -105.6(8) . . . . no
N5 C57 C67 C68 -105.7(8) . . . . no
C56 C57 C67 C68 72.5(9) . . . . no
N5 C58 C59 N6 40.1(8) . . . . no
N6 C60 C80 C85 76.6(9) . . . . no
N6 C60 C80 C81 -105.3(8) . . . . no
N6 C60 C61 C66 -3.9(9) . . . . no
C80 C60 C61 C62 -4.4(9) . . . . no
C80 C60 C61 C66 173.1(6) . . . . no
C61 C60 C80 C81 77.6(8) . . . . no
C61 C60 C80 C85 -100.4(8) . . . . no
N6 C60 C61 C62 178.6(6) . . . . no
C66 C61 C62 C63 -0.5(11) . . . . no
C60 C61 C66 O6 4.6(11) . . . . no
C60 C61 C66 C65 -175.5(6) . . . . no
C60 C61 C62 C63 177.1(7) . . . . no
C62 C61 C66 C65 2.1(10) . . . . no
C62 C61 C66 O6 -177.8(7) . . . . no
C61 C62 C63 C64 -1.2(12) . . . . no
C62 C63 C64 C65 1.1(12) . . . . no
C63 C64 C65 C66 0.7(13) . . . . no
C64 C65 C66 C61 -2.3(12) . . . . no
C64 C65 C66 O6 177.7(7) . . . . no
C57 C67 C68 C69 -179.2(7) . . . . no
C68 C67 C72 C71 0.8(11) . . . . no
C68 C67 C72 O7 179.7(6) . . . . no
C57 C67 C72 O7 -2.3(10) . . . . no
C72 C67 C68 C69 -1.1(11) . . . . no
C57 C67 C72 C71 178.8(7) . . . . no
C67 C68 C69 C70 0.9(13) . . . . no
C68 C69 C70 C71 -0.4(14) . . . . no
C69 C70 C71 C72 0.1(14) . . . . no
C70 C71 C72 O7 -179.1(8) . . . . no
C70 C71 C72 C67 -0.3(12) . . . . no
O7 C73 C74 N7 -67.1(9) . . . . no
N7 C75 C76 C77 56.4(10) . . . . no
C75 C76 C77 C78 -52.1(11) . . . . no
C76 C77 C78 C79 52.5(10) . . . . no
C77 C78 C79 N7 -57.6(9) . . . . no
C60 C80 C85 C84 176.7(6) . . . . no
C60 C80 C85 O8 -3.6(10) . . . . no
C81 C80 C85 C84 -1.3(11) . . . . no
C85 C80 C81 C82 0.4(12) . . . . no
C81 C80 C85 O8 178.4(7) . . . . no
C60 C80 C81 C82 -177.7(7) . . . . no
C80 C81 C82 C83 1.0(12) . . . . no
C81 C82 C83 C84 -1.5(13) . . . . no
C82 C83 C84 C85 0.5(12) . . . . no
C83 C84 C85 O8 -178.8(7) . . . . no
C83 C84 C85 C80 0.9(11) . . . . no
O8 C86 C87 N8 68.0(11) . . . . no
N8 C88 C89 C90 -59.7(12) . . . . no
C88 C89 C90 C91 56.1(13) . . . . no
C89 C90 C91 C92 -56.0(13) . . . . no
C90 C91 C92 N8 57.5(13) . . . . no
O9 C101 C102 C103 -178.0(7) . . . . no
C106 C101 C102 C103 2.4(12) . . . . no
O9 C101 C106 C105 177.7(7) . . . . no
O9 C101 C106 C107 0.8(12) . . . . no
C102 C101 C106 C105 -2.8(11) . . . . no
C102 C101 C106 C107 -179.7(7) . . . . no
C101 C102 C103 C104 -0.3(13) . . . . no
C102 C103 C104 C105 -1.5(12) . . . . no
C103 C104 C105 C106 1.0(13) . . . . no
C104 C105 C106 C101 1.2(12) . . . . no
C104 C105 C106 C107 178.1(8) . . . . no
C105 C106 C107 N9 176.4(7) . . . . no
C105 C106 C107 C117 -4.2(11) . . . . no
C101 C106 C107 N9 -6.8(12) . . . . no
C101 C106 C107 C117 172.6(7) . . . . no
N9 C107 C117 C122 72.8(10) . . . . no
C106 C107 C117 C118 76.1(11) . . . . no
N9 C107 C117 C118 -104.6(9) . . . . no
C106 C107 C117 C122 -106.6(9) . . . . no
N9 C108 C109 N10 40.2(8) . . . . no
C130 C110 C111 C116 -175.2(7) . . . . no
C130 C110 C111 C112 8.3(11) . . . . no
N10 C110 C111 C112 -174.8(7) . . . . no
N10 C110 C111 C116 1.8(12) . . . . no
C111 C110 C130 C131 75.4(10) . . . . no
N10 C110 C130 C131 -101.6(9) . . . . no
N10 C110 C130 C135 77.1(11) . . . . no
C111 C110 C130 C135 -105.8(9) . . . . no
C110 C111 C116 O10 2.8(12) . . . . no
C110 C111 C112 C113 174.7(8) . . . . no
C116 C111 C112 C113 -1.9(12) . . . . no
C112 C111 C116 C115 2.8(11) . . . . no
C110 C111 C116 C115 -173.7(7) . . . . no
C112 C111 C116 O10 179.4(7) . . . . no
C111 C112 C113 C114 0.9(13) . . . . no
C112 C113 C114 C115 -0.9(15) . . . . no
C113 C114 C115 C116 1.9(14) . . . . no
C114 C115 C116 C111 -2.8(12) . . . . no
C114 C115 C116 O10 -179.7(8) . . . . no
C118 C117 C122 C121 -0.5(13) . . . . no
C107 C117 C122 O11 2.5(11) . . . . no
C107 C117 C118 C119 177.7(9) . . . . no
C122 C117 C118 C119 0.4(14) . . . . no
C107 C117 C122 C121 -177.8(8) . . . . no
C118 C117 C122 O11 179.9(8) . . . . no
C117 C118 C119 C120 -0.7(15) . . . . no
C118 C119 C120 C121 1.1(17) . . . . no
C119 C120 C121 C122 -1.1(16) . . . . no
C120 C121 C122 O11 -179.6(9) . . . . no
C120 C121 C122 C117 0.8(14) . . . . no
O11 C123 C124 N11 -71.2(8) . . . . no
N11 C125 C126 C127 57.2(10) . . . . no
C125 C126 C127 C128 -54.3(12) . . . . no
C126 C127 C128 C129 54.2(11) . . . . no
C127 C128 C129 N11 -57.2(11) . . . . no
C110 C130 C131 C132 178.6(9) . . . . no
C135 C130 C131 C132 -0.2(14) . . . . no
C110 C130 C135 O12 1.1(12) . . . . no
C110 C130 C135 C134 -178.3(8) . . . . no
C131 C130 C135 O12 179.9(8) . . . . no
C131 C130 C135 C134 0.4(13) . . . . no
C130 C131 C132 C133 0.1(15) . . . . no
C131 C132 C133 C134 -0.2(17) . . . . no
C132 C133 C134 C135 0.5(16) . . . . no
C133 C134 C135 O12 -180.0(9) . . . . no
C133 C134 C135 C130 -0.6(13) . . . . no
O12 C136 C137 N12 -68.3(9) . . . . no
N12 C138 C139 C140 59.1(11) . . . . no
C138 C139 C140 C141 -57.5(12) . . . . no
C139 C140 C141 C142 55.8(12) . . . . no
C140 C141 C142 N12 -58.8(11) . . . . no
O13 C151 C152 C153 -176.9(7) . . . . no
C156 C151 C152 C153 -0.3(12) . . . . no
O13 C151 C156 C155 177.1(7) . . . . no
O13 C151 C156 C157 0.9(12) . . . . no
C152 C151 C156 C155 0.8(11) . . . . no
C152 C151 C156 C157 -175.4(7) . . . . no
C151 C152 C153 C154 -0.5(12) . . . . no
C152 C153 C154 C155 0.8(12) . . . . no
C153 C154 C155 C156 -0.3(12) . . . . no
C154 C155 C156 C151 -0.5(12) . . . . no
C154 C155 C156 C157 175.8(7) . . . . no
C151 C156 C157 N13 -0.9(12) . . . . no
C151 C156 C157 C167 174.7(7) . . . . no
C155 C156 C157 N13 -177.1(7) . . . . no
C155 C156 C157 C167 -1.5(11) . . . . no
N13 C157 C167 C168 -100.8(9) . . . . no
N13 C157 C167 C172 77.2(10) . . . . no
C156 C157 C167 C168 83.5(10) . . . . no
C156 C157 C167 C172 -98.6(9) . . . . no
N13 C158 C159 N14 43.1(7) . . . . no
N14 C160 C161 C162 173.5(7) . . . . no
N14 C160 C161 C166 -8.8(10) . . . . no
C180 C160 C161 C162 -5.2(10) . . . . no
C180 C160 C161 C166 172.5(6) . . . . no
N14 C160 C180 C181 -105.2(8) . . . . no
N14 C160 C180 C185 72.7(9) . . . . no
C161 C160 C180 C181 73.6(10) . . . . no
C161 C160 C180 C185 -108.6(8) . . . . no
C160 C161 C162 C163 -178.3(8) . . . . no
C166 C161 C162 C163 3.9(13) . . . . no
C160 C161 C166 O14 -1.2(11) . . . . no
C160 C161 C166 C165 179.2(7) . . . . no
C162 C161 C166 O14 176.6(7) . . . . no
C162 C161 C166 C165 -3.0(10) . . . . no
C161 C162 C163 C164 -2.4(15) . . . . no
C162 C163 C164 C165 0.0(14) . . . . no
C163 C164 C165 C166 0.7(13) . . . . no
C164 C165 C166 O14 -178.8(7) . . . . no
C164 C165 C166 C161 0.8(11) . . . . no
C157 C167 C168 C169 175.9(8) . . . . no
C172 C167 C168 C169 -1.9(14) . . . . no
C157 C167 C172 O15 4.6(11) . . . . no
C157 C167 C172 C171 -175.7(8) . . . . no
C168 C167 C172 O15 -177.6(8) . . . . no
C168 C167 C172 C171 2.2(13) . . . . no
C167 C168 C169 C170 1.1(14) . . . . no
C168 C169 C170 C171 -0.7(17) . . . . no
C169 C170 C171 C172 1.0(17) . . . . no
C170 C171 C172 O15 178.1(9) . . . . no
C170 C171 C172 C167 -1.6(13) . . . . no
O15 C173 C174 N15 66.7(11) . . . . no
N15 C175 C176 C177 61.8(11) . . . . no
C175 C176 C177 C178 -57.8(13) . . . . no
C176 C177 C178 C179 56.9(15) . . . . no
C177 C178 C179 N15 -60.3(14) . . . . no
C160 C180 C181 C182 175.7(8) . . . . no
C185 C180 C181 C182 -2.1(13) . . . . no
C160 C180 C185 O16 2.3(11) . . . . no
C160 C180 C185 C184 -178.7(7) . . . . no
C181 C180 C185 O16 -179.8(7) . . . . no
C181 C180 C185 C184 -0.8(12) . . . . no
C180 C181 C182 C183 3.2(14) . . . . no
C181 C182 C183 C184 -1.3(15) . . . . no
C182 C183 C184 C185 -1.5(14) . . . . no
C183 C184 C185 O16 -178.5(8) . . . . no
C183 C184 C185 C180 2.6(13) . . . . no
O16 C186 C187 N16 -67.5(8) . . . . no
N16 C188 C189 C190 -57.4(11) . . . . no
C188 C189 C190 C191 54.6(12) . . . . no
C189 C190 C191 C192 -55.0(12) . . . . no
C190 C191 C192 N16 58.2(12) . . . . no

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Ni1 C142 3.649(9) . 1_455 no
Ni2 C178 3.891(17) . 1_554 no
Ni2 C179 3.552(11) . 1_554 no
Ni3 C24 3.503(11) . 1_655 no
Ni4 C88 3.777(10) . 1_556 no
O1 O2 2.456(7) . . no
O1 N1 2.685(7) . . no
O1 C142 3.333(11) . 1_455 no
O1 C7 2.937(8) . . no
O2 C10 2.904(8) . . no
O2 O1 2.456(7) . . no
O2 N2 2.689(7) . . no
O3 N3 2.930(10) . . no
O3 C8 3.110(7) . . no
O3 N1 3.111(7) . . no
O4 N2 3.144(7) . . no
O4 C42 3.299(10) . . no
O4 N4 2.994(8) . . no
O4 C9 3.133(7) . . no
O5 N5 2.720(7) . . no
O5 O6 2.468(7) . . no
O5 C57 2.926(8) . . no
O6 C179 3.247(13) . 1_554 no
O6 C60 2.921(8) . . no
O6 N6 2.697(6) . . no
O6 C125 3.262(12) . 2_766 no
O7 N7 3.008(8) . . no
O7 C58 3.120(9) . . no
O7 C79 3.235(10) . . no
O7 N5 3.136(7) . . no
O8 C59 3.069(9) . . no
O8 C173 3.348(11) . 1_554 no
O8 N8 3.032(10) . . no
O8 N6 3.086(7) . . no
O9 N9 2.690(7) . . no
O9 C107 2.911(9) . . no
O9 O10 2.479(8) . . no
O10 C110 2.919(8) . . no
O10 C75 3.400(10) . 2_666 no
O10 N10 2.695(7) . . no
O10 C24 3.378(12) . 1_655 no
O11 C108 3.047(10) . . no
O11 N11 2.953(8) . . no
O11 N9 3.046(8) . . no
O12 C109 3.096(10) . . no
O12 N10 3.149(8) . . no
O12 N12 2.985(9) . . no
O13 O14 2.483(8) . . no
O13 N13 2.694(7) . . no
O13 C157 2.914(8) . . no
O14 C88 3.352(12) . 1_556 no
O14 C160 2.921(8) . . no
O14 N14 2.702(7) . . no
O15 N13 3.167(8) . . no
O15 C158 3.243(10) . . no
O15 N15 3.003(10) . . no
O15 C86 3.360(10) . 1_556 no
O16 N14 3.057(8) . . no
O16 C34 3.321(10) . 2_576 no
O16 N16 2.932(8) . . no
O16 C159 3.068(10) . . no
N1 C1 2.860(8) . . no
N1 N2 2.596(7) . . no
N1 C9 2.429(8) . . no
N2 C8 2.428(9) . . no
N2 C16 2.892(9) . . no
N5 C59 2.409(10) . . no
N5 N6 2.598(8) . . no
N5 C51 2.917(9) . . no
N6 C66 2.867(8) . . no
N6 C58 2.413(9) . . no
N8 C59 3.426(11) . . no
N9 C109 2.388(10) . . no
N9 N10 2.597(8) . . no
N9 C101 2.879(9) . . no
N10 C108 2.402(10) . . no
N10 C116 2.869(9) . . no
N13 C159 2.400(10) . . no
N13 C151 2.884(9) . . no
N13 N14 2.591(8) . . no
N14 C166 2.890(8) . . no
N14 C158 2.398(10) . . no
C1 C192 3.436(12) . 2_676 no
C2 C192 3.547(13) . 2_676 no
C5 C18 3.232(11) . . no
C8 C22 3.212(9) . . no
C9 C35 3.162(10) . . no
C12 C31 3.257(11) . . no
C23 C116 3.586(11) . 1_455 no
C24 C116 3.553(13) . 1_455 no
C33 C186 3.578(12) . 2_576 no
C36 C166 3.421(10) . 2_576 no
C52 C123 3.599(12) . 2_766 no
C55 C68 3.206(11) . . no
C58 C72 3.181(11) . . no
C59 C85 3.175(11) . . no
C62 C81 3.252(10) . . no
C65 C125 3.530(13) . 2_766 no
C66 C125 3.408(13) . 2_766 no
C84 C87 3.391(14) . . no
C86 C151 3.445(11) . 1_554 no
C86 C156 3.558(11) . 1_554 no
C88 C166 3.480(13) . 1_554 no
C103 C120 3.559(14) . 2_766 no
C104 C105 3.590(12) . 2_766 no
C105 C118 3.288(12) . . no
C105 C105 3.573(12) . 2_766 no
C108 C122 3.090(12) . . no
C109 C135 3.138(12) . . no
C112 C131 3.304(11) . . no
C125 Ni2 4.104(10) . 2_766 no
C155 C168 3.378(11) . . no
C158 C168 3.531(12) . . no
C158 C172 3.153(12) . . no
C159 C185 3.131(12) . . no
C162 C181 3.239(11) . . no
C171 C174 3.355(14) . . no
C176 C181 3.401(15) . . no
C182 C182 3.472(15) . 2_677 no




_iucr_refine_instruction_details_constraints 
;
#
# Punched on 07/06/16 at 13:52:48
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H(252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) H   ( 592,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) H   ( 742,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) H   ( 752,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) H   ( 772,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) H   ( 782,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) H   ( 792,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  86,X'S) H   ( 861,X'S) H   ( 862,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) H   ( 872,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) H   ( 882,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) H   ( 892,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) H   ( 902,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) H   ( 912,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) H   ( 922,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) H   (1082,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) H   (1092,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 119,X'S) H   (1191,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) 
RIDE C   ( 121,X'S) H   (1211,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) H   (1232,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) H   (1242,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) H   (1252,X'S) 
RIDE C   ( 126,X'S) H   (1261,X'S) H   (1262,X'S) 
RIDE C   ( 127,X'S) H   (1271,X'S) H   (1272,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) H   (1282,X'S) 
RIDE C   ( 129,X'S) H   (1291,X'S) H   (1292,X'S) 
RIDE C   ( 131,X'S) H   (1311,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) H   (1362,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) H   (1372,X'S) 
RIDE C   ( 138,X'S) H   (1381,X'S) H   (1382,X'S) 
RIDE C   ( 139,X'S) H   (1391,X'S) H   (1392,X'S) 
RIDE C   ( 140,X'S) H   (1401,X'S) H   (1402,X'S) 
RIDE C   ( 141,X'S) H   (1411,X'S) H   (1412,X'S) 
RIDE C   ( 142,X'S) H   (1421,X'S) H   (1422,X'S) 
RIDE C   ( 152,X'S) H   (1521,X'S) 
RIDE C   ( 153,X'S) H   (1531,X'S) 
RIDE C   ( 154,X'S) H   (1541,X'S) 
RIDE C   ( 155,X'S) H   (1551,X'S) 
RIDE C   ( 158,X'S) H   (1581,X'S) H   (1582,X'S) 
RIDE C   ( 159,X'S) H   (1591,X'S) H   (1592,X'S) 
RIDE C   ( 162,X'S) H   (1621,X'S) 
RIDE C   ( 163,X'S) H   (1631,X'S) 
RIDE C   ( 164,X'S) H   (1641,X'S) 
RIDE C   ( 165,X'S) H   (1651,X'S) 
RIDE C   ( 168,X'S) H   (1681,X'S) 
RIDE C   ( 169,X'S) H   (1691,X'S) 
RIDE C   ( 170,X'S) H   (1701,X'S) 
RIDE C   ( 171,X'S) H   (1711,X'S) 
RIDE C   ( 173,X'S) H   (1731,X'S) H   (1732,X'S) 
RIDE C   ( 174,X'S) H   (1741,X'S) H   (1742,X'S) 
RIDE C   ( 175,X'S) H   (1751,X'S) H   (1752,X'S) 
RIDE C   ( 176,X'S) H   (1761,X'S) H   (1762,X'S) 
RIDE C   ( 177,X'S) H   (1771,X'S) H   (1772,X'S) 
RIDE C   ( 178,X'S) H   (1781,X'S) H   (1782,X'S) 
RIDE C   ( 179,X'S) H   (1791,X'S) H   (1792,X'S) 
RIDE C   ( 181,X'S) H   (1811,X'S) 
RIDE C   ( 182,X'S) H   (1821,X'S) 
RIDE C   ( 183,X'S) H   (1831,X'S) 
RIDE C   ( 184,X'S) H   (1841,X'S) 
RIDE C   ( 186,X'S) H   (1861,X'S) H   (1862,X'S) 
RIDE C   ( 187,X'S) H   (1871,X'S) H   (1872,X'S) 
RIDE C   ( 188,X'S) H   (1881,X'S) H   (1882,X'S) 
RIDE C   ( 189,X'S) H   (1891,X'S) H   (1892,X'S) 
RIDE C   ( 190,X'S) H   (1901,X'S) H   (1902,X'S) 
RIDE C   ( 191,X'S) H   (1911,X'S) H   (1912,X'S) 
RIDE C   ( 192,X'S) H   (1921,X'S) H   (1922,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 07/06/16 at 13:52:48
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
5 8 6 x .
5 8 7 x .


#===END


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

data_ral1707SNQ
_database_code_depnum_ccdc_archive 'CCDC 1988292'
loop_
_audit_author_name
_audit_author_address
'Anthony Willis'
;Australian National University
Australia
;
_audit_update_record             
;
2020-03-05 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_audit_creation_date             17-02-06
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1707SNQ\Tony_ral1707SNQ_da At 14: 8 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   7.9887(1)
_cell_length_b                   20.7141(2)
_cell_length_c                   12.4586(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.9200(10)
_cell_angle_gamma                90
_cell_volume                     2036.70(5)

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

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni -3.0029 0.5091 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C22 H22 N2 Ni1 O6 
# Dc =      1.53 Fooo =    976.00 Mu =     17.52 M =    469.14
# Found Formula = C22 H22 N2 Ni1 O6 
# Dc =      1.53 FOOO =    976.00 Mu =     17.52 M =    469.14

_chemical_formula_sum            'C22 H22 N2 Ni O6'
_chemical_formula_moiety         'C22 H18 N2 Ni O4, 2(H2 O)'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         469.14


_cell_measurement_reflns_used    13177
_cell_measurement_theta_min      4
_cell_measurement_theta_max      74
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.029
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_max          0.132

_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    1.752

# Sheldrick geometric approximatio 0.86 0.95 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro version 1.171.38.43 (Rigaku Oxford Diffraction, 2016)
(Release 29 April 2016; compiled 27 May 2016,16:53)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_T_max  0.95
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
#_diffrn_ambient_temperature 150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_measurement_method       'ω scans'


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

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

_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            31987
_reflns_number_total             4095
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0424

# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 4095 
# Theoretical number of reflections is about 8233 


_diffrn_reflns_theta_min         4.178
_diffrn_reflns_theta_max         73.709
_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        73.709
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -9
_reflns_limit_h_max              9
_reflns_limit_k_min              0
_reflns_limit_k_max              25
_reflns_limit_l_min              0
_reflns_limit_l_max              15

_oxford_diffrn_Wilson_B_factor   2.18
_oxford_diffrn_Wilson_scale      0.25

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

_refine_diff_density_min         -0.50
_refine_diff_density_max         0.88


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         4095
_refine_ls_number_restraints     0
_refine_ls_number_parameters     298
_oxford_refine_ls_R_factor_ref   0.0412
_refine_ls_wR_factor_ref         0.0975
_refine_ls_goodness_of_fit_ref   1.0306
_refine_ls_shift/su_max          0.0004556
_refine_ls_shift/su_mean         0.0000486


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4095
_refine_ls_R_factor_all          0.0412
_refine_ls_wR_factor_all         0.0975

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3802
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_gt          0.0954

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 2.28P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               

The H atoms were all located in a difference map, but 
those bonded to C
 were repositioned geometrically. 
The H atoms were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98Å, O---H = 0.83Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints
and the displacement parameters were held fixed. 
Finally the positions of the H atoms bonded to O were allowed 
to refine freely.

 

The largest feature in the
final difference electron density map is located 
near C3 and C4 but appears to have no chemical significance.
The next largest features are near O2, C3 and the Ni atom.
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.19982(4) 0.214639(16) 0.40469(3) 0.0228 1.0000 Uani . . . . . .
O1 O 0.07276(17) 0.13995(7) 0.37670(12) 0.0262 1.0000 Uani . . . . . .
O2 O 0.35850(17) 0.16069(7) 0.47926(12) 0.0278 1.0000 Uani . . . . . .
O3 O -0.42551(18) 0.01270(8) 0.29309(14) 0.0320 1.0000 Uani . . . . . .
O4 O 0.90024(18) 0.07844(8) 0.61312(14) 0.0324 1.0000 Uani . . . . . .
O5 O 0.2483(2) 0.09128(8) 0.64224(14) 0.0321 1.0000 Uani . . . . . .
O6 O 0.2657(2) 0.02736(8) 0.38285(18) 0.0419 1.0000 Uani . . . . . .
N1 N 0.0405(2) 0.26716(8) 0.32566(15) 0.0272 1.0000 Uani . . . . . .
N2 N 0.3305(2) 0.28849(8) 0.43685(15) 0.0264 1.0000 Uani . . . . . .
C1 C -0.0875(2) 0.13505(10) 0.33109(16) 0.0240 1.0000 Uani . . . . . .
C2 C -0.1687(2) 0.07525(10) 0.33185(16) 0.0245 1.0000 Uani . . . . . .
C3 C -0.3382(3) 0.06848(10) 0.28716(18) 0.0287 1.0000 Uani . . . . . .
C4 C -0.4303(3) 0.12049(12) 0.2370(2) 0.0372 1.0000 Uani . . . . . .
C5 C -0.3518(3) 0.17863(11) 0.2341(2) 0.0378 1.0000 Uani . . . . . .
C6 C -0.1802(3) 0.18810(10) 0.28051(17) 0.0283 1.0000 Uani . . . . . .
C7 C -0.1088(3) 0.25101(11) 0.27760(18) 0.0298 1.0000 Uani . . . . . .
C8 C 0.1021(3) 0.33297(11) 0.3124(2) 0.0363 1.0000 Uani . . . . . .
C9 C 0.2273(3) 0.34750(10) 0.4122(2) 0.0359 1.0000 Uani . . . . . .
C10 C 0.4911(3) 0.29231(10) 0.47784(16) 0.0250 1.0000 Uani . . . . . .
C11 C 0.5924(2) 0.23586(10) 0.51098(16) 0.0240 1.0000 Uani . . . . . .
C12 C 0.7688(3) 0.24190(10) 0.54768(17) 0.0268 1.0000 Uani . . . . . .
C13 C 0.8693(3) 0.19029(10) 0.58036(18) 0.0280 1.0000 Uani . . . . . .
C14 C 0.7966(2) 0.12839(10) 0.57854(16) 0.0249 1.0000 Uani . . . . . .
C15 C 0.6257(2) 0.12006(9) 0.54381(16) 0.0244 1.0000 Uani . . . . . .
C16 C 0.5207(2) 0.17290(9) 0.50964(16) 0.0230 1.0000 Uani . . . . . .
C17 C 0.5765(3) 0.35708(10) 0.48979(17) 0.0256 1.0000 Uani . . . . . .
C18 C 0.6528(4) 0.38127(12) 0.4063(2) 0.0430 1.0000 Uani . . . . . .
C19 C 0.7385(4) 0.43977(13) 0.4186(3) 0.0517 1.0000 Uani . . . . . .
C20 C 0.7459(3) 0.47405(11) 0.5129(2) 0.0438 1.0000 Uani . . . . . .
C21 C 0.6675(3) 0.45119(11) 0.5955(2) 0.0393 1.0000 Uani . . . . . .
C22 C 0.5836(3) 0.39230(11) 0.58496(18) 0.0330 1.0000 Uani . . . . . .
H1 H -0.370(4) -0.0140(15) 0.316(3) 0.0479 1.0000 Uiso . . . . . .
H2 H 0.856(4) 0.0468(16) 0.617(3) 0.0482 1.0000 Uiso . . . . . .
H3 H 0.277(4) 0.1089(15) 0.583(3) 0.0478 1.0000 Uiso . . . . . .
H4 H 0.159(4) 0.0881(15) 0.634(3) 0.0481 1.0000 Uiso . . . . . .
H5 H 0.229(4) 0.0654(18) 0.387(3) 0.0630 1.0000 Uiso . . . . . .
H6 H 0.353(5) 0.0313(17) 0.359(3) 0.0628 1.0000 Uiso . . . . . .
H21 H -0.1104 0.0412 0.3651 0.0294 1.0000 Uiso R . . . . .
H41 H -0.5433 0.1154 0.2082 0.0454 1.0000 Uiso R . . . . .
H51 H -0.4120 0.2139 0.2011 0.0462 1.0000 Uiso R . . . . .
H71 H -0.1727 0.2830 0.2380 0.0355 1.0000 Uiso R . . . . .
H81 H 0.1625 0.3347 0.2494 0.0443 1.0000 Uiso R . . . . .
H82 H 0.0095 0.3643 0.3042 0.0443 1.0000 Uiso R . . . . .
H91 H 0.1668 0.3567 0.4745 0.0425 1.0000 Uiso R . . . . .
H92 H 0.2987 0.3835 0.3982 0.0422 1.0000 Uiso R . . . . .
H121 H 0.8170 0.2828 0.5493 0.0322 1.0000 Uiso R . . . . .
H131 H 0.9843 0.1950 0.6018 0.0343 1.0000 Uiso R . . . . .
H151 H 0.5767 0.0794 0.5415 0.0284 1.0000 Uiso R . . . . .
H181 H 0.6461 0.3588 0.3411 0.0520 1.0000 Uiso R . . . . .
H191 H 0.7901 0.4552 0.3623 0.0627 1.0000 Uiso R . . . . .
H201 H 0.8064 0.5126 0.5197 0.0533 1.0000 Uiso R . . . . .
H211 H 0.6711 0.4746 0.6601 0.0473 1.0000 Uiso R . . . . .
H221 H 0.5313 0.3763 0.6406 0.0399 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.226(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . O1 . 1.8536(14) yes
Ni1 . O2 . 1.8313(14) yes
Ni1 . N1 . 1.8396(17) yes
Ni1 . N2 . 1.8602(17) yes
O1 . C1 . 1.321(2) yes
O2 . C16 . 1.317(2) yes
O3 . C3 . 1.358(3) yes
O3 . H1 . 0.74(3) no
O4 . C14 . 1.353(2) yes
O4 . H2 . 0.75(3) no
O5 . H3 . 0.88(3) no
O5 . H4 . 0.71(3) no
O6 . H5 . 0.84(4) no
O6 . H6 . 0.80(4) no
N1 . C7 . 1.293(3) yes
N1 . C8 . 1.467(3) yes
N2 . C9 . 1.479(3) yes
N2 . C10 . 1.308(3) yes
C1 . C2 . 1.399(3) yes
C1 . C6 . 1.417(3) yes
C2 . C3 . 1.389(3) yes
C2 . H21 . 0.909 no
C3 . C4 . 1.396(3) yes
C4 . C5 . 1.361(3) yes
C4 . H41 . 0.924 no
C5 . C6 . 1.417(3) yes
C5 . H51 . 0.933 no
C6 . C7 . 1.425(3) yes
C7 . H71 . 0.930 no
C8 . C9 . 1.500(3) yes
C8 . H81 . 0.984 no
C8 . H82 . 0.977 no
C9 . H91 . 0.994 no
C9 . H92 . 0.970 no
C10 . C11 . 1.445(3) yes
C10 . C17 . 1.502(3) yes
C11 . C12 . 1.418(3) yes
C11 . C16 . 1.424(3) yes
C12 . C13 . 1.361(3) yes
C12 . H121 . 0.930 no
C13 . C14 . 1.406(3) yes
C13 . H131 . 0.921 no
C14 . C15 . 1.378(3) yes
C15 . C16 . 1.404(3) yes
C15 . H151 . 0.927 no
C17 . C18 . 1.379(3) yes
C17 . C22 . 1.386(3) yes
C18 . C19 . 1.389(3) yes
C18 . H181 . 0.930 no
C19 . C20 . 1.367(4) yes
C19 . H191 . 0.923 no
C20 . C21 . 1.370(4) yes
C20 . H201 . 0.931 no
C21 . C22 . 1.388(3) yes
C21 . H211 . 0.935 no
C22 . H221 . 0.924 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Ni1 . O2 . 84.37(6) yes
O1 . Ni1 . N1 . 94.57(7) yes
O2 . Ni1 . N1 . 178.07(8) yes
O1 . Ni1 . N2 . 178.22(7) yes
O2 . Ni1 . N2 . 94.10(7) yes
N1 . Ni1 . N2 . 86.99(8) yes
Ni1 . O1 . C1 . 127.64(13) yes
Ni1 . O2 . C16 . 126.98(13) yes
C3 . O3 . H1 . 112(2) no
C14 . O4 . H2 . 115(2) no
H3 . O5 . H4 . 108(3) no
H5 . O6 . H6 . 105(3) no
Ni1 . N1 . C7 . 127.37(15) yes
Ni1 . N1 . C8 . 113.15(14) yes
C7 . N1 . C8 . 119.33(18) yes
Ni1 . N2 . C9 . 111.04(13) yes
Ni1 . N2 . C10 . 128.15(14) yes
C9 . N2 . C10 . 120.80(17) yes
O1 . C1 . C2 . 118.97(17) yes
O1 . C1 . C6 . 122.43(19) yes
C2 . C1 . C6 . 118.59(18) yes
C1 . C2 . C3 . 120.72(18) yes
C1 . C2 . H21 . 119.0 no
C3 . C2 . H21 . 120.2 no
C2 . C3 . O3 . 122.76(19) yes
C2 . C3 . C4 . 121.0(2) yes
O3 . C3 . C4 . 116.19(18) yes
C3 . C4 . C5 . 118.8(2) yes
C3 . C4 . H41 . 120.0 no
C5 . C4 . H41 . 121.2 no
C4 . C5 . C6 . 122.2(2) yes
C4 . C5 . H51 . 119.7 no
C6 . C5 . H51 . 118.1 no
C1 . C6 . C5 . 118.7(2) yes
C1 . C6 . C7 . 122.46(18) yes
C5 . C6 . C7 . 118.82(19) yes
C6 . C7 . N1 . 124.66(19) yes
C6 . C7 . H71 . 118.5 no
N1 . C7 . H71 . 116.9 no
N1 . C8 . C9 . 106.59(18) yes
N1 . C8 . H81 . 109.7 no
C9 . C8 . H81 . 107.9 no
N1 . C8 . H82 . 111.5 no
C9 . C8 . H82 . 110.5 no
H81 . C8 . H82 . 110.4 no
C8 . C9 . N2 . 106.53(18) yes
C8 . C9 . H91 . 110.0 no
N2 . C9 . H91 . 108.6 no
C8 . C9 . H92 . 109.8 no
N2 . C9 . H92 . 110.4 no
H91 . C9 . H92 . 111.4 no
N2 . C10 . C11 . 122.31(18) yes
N2 . C10 . C17 . 119.72(18) yes
C11 . C10 . C17 . 117.96(17) yes
C10 . C11 . C12 . 120.34(18) yes
C10 . C11 . C16 . 122.10(17) yes
C12 . C11 . C16 . 117.55(18) yes
C11 . C12 . C13 . 122.55(19) yes
C11 . C12 . H121 . 118.4 no
C13 . C12 . H121 . 119.1 no
C12 . C13 . C14 . 119.23(18) yes
C12 . C13 . H131 . 121.3 no
C14 . C13 . H131 . 119.5 no
C13 . C14 . O4 . 117.48(17) yes
C13 . C14 . C15 . 120.39(18) yes
O4 . C14 . C15 . 122.12(18) yes
C14 . C15 . C16 . 120.91(18) yes
C14 . C15 . H151 . 121.1 no
C16 . C15 . H151 . 118.0 no
C11 . C16 . C15 . 119.36(17) yes
C11 . C16 . O2 . 123.75(17) yes
C15 . C16 . O2 . 116.88(17) yes
C10 . C17 . C18 . 119.78(19) yes
C10 . C17 . C22 . 120.85(19) yes
C18 . C17 . C22 . 119.3(2) yes
C17 . C18 . C19 . 120.1(2) yes
C17 . C18 . H181 . 120.3 no
C19 . C18 . H181 . 119.6 no
C18 . C19 . C20 . 120.2(3) yes
C18 . C19 . H191 . 119.2 no
C20 . C19 . H191 . 120.6 no
C19 . C20 . C21 . 120.2(2) yes
C19 . C20 . H201 . 118.4 no
C21 . C20 . H201 . 121.4 no
C20 . C21 . C22 . 120.2(2) yes
C20 . C21 . H211 . 120.7 no
C22 . C21 . H211 . 119.1 no
C21 . C22 . C17 . 119.9(2) yes
C21 . C22 . H221 . 120.7 no
C17 . C22 . H221 . 119.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O3 . H1 . O5 2_556 171(3) 0.74(3) 1.90(3) 2.634(3) yes
O4 . H2 . O6 2_656 175(3) 0.75(3) 1.82(3) 2.566(3) yes
O5 . H3 . O2 . 167(3) 0.88(3) 1.88(3) 2.742(3) yes
O5 . H4 . O4 1_455 179(4) 0.71(3) 2.05(3) 2.761(3) yes
O6 . H5 . O1 . 161(3) 0.85(4) 1.98(4) 2.790(3) yes
O6 . H6 . O3 1_655 163(3) 0.80(4) 2.10(4) 2.878(3) yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C1 171.50(16) . . . . no
N1 Ni1 O1 C1 -10.13(17) . . . . no
O1 Ni1 O2 C16 162.71(16) . . . . no
N2 Ni1 O2 C16 -18.19(17) . . . . no
O1 Ni1 N1 C7 4.0(2) . . . . no
O1 Ni1 N1 C8 -171.49(15) . . . . no
N2 Ni1 N1 C7 -175.2(2) . . . . no
N2 Ni1 N1 C8 9.36(15) . . . . no
O2 Ni1 N2 C9 -165.97(15) . . . . no
O2 Ni1 N2 C10 12.66(19) . . . . no
N1 Ni1 N2 C9 15.63(15) . . . . no
N1 Ni1 N2 C10 -165.74(19) . . . . no
Ni1 O1 C1 C2 -170.33(14) . . . . no
Ni1 O1 C1 C6 10.2(3) . . . . no
Ni1 O2 C16 C11 15.0(3) . . . . no
Ni1 O2 C16 C15 -165.99(14) . . . . no
Ni1 N1 C7 C6 2.2(3) . . . . no
C8 N1 C7 C6 177.4(2) . . . . no
Ni1 N1 C8 C9 -31.2(2) . . . . no
C7 N1 C8 C9 153.0(2) . . . . no
Ni1 N2 C9 C8 -35.9(2) . . . . no
C10 N2 C9 C8 145.4(2) . . . . no
Ni1 N2 C10 C11 -3.6(3) . . . . no
Ni1 N2 C10 C17 175.33(15) . . . . no
C9 N2 C10 C11 174.94(19) . . . . no
C9 N2 C10 C17 -6.2(3) . . . . no
O1 C1 C2 C3 178.40(19) . . . . no
C6 C1 C2 C3 -2.1(3) . . . . no
O1 C1 C6 C5 -179.68(19) . . . . no
O1 C1 C6 C7 -1.7(3) . . . . no
C2 C1 C6 C5 0.8(3) . . . . no
C2 C1 C6 C7 178.8(2) . . . . no
C1 C2 C3 O3 -175.04(19) . . . . no
C1 C2 C3 C4 2.3(3) . . . . no
O3 C3 C4 C5 176.4(2) . . . . no
C2 C3 C4 C5 -1.1(4) . . . . no
C3 C4 C5 C6 -0.2(4) . . . . no
C4 C5 C6 C1 0.3(3) . . . . no
C4 C5 C6 C7 -177.8(2) . . . . no
C1 C6 C7 N1 -4.7(4) . . . . no
C5 C6 C7 N1 173.3(2) . . . . no
N1 C8 C9 N2 41.7(2) . . . . no
N2 C10 C11 C12 175.4(2) . . . . no
N2 C10 C11 C16 -5.4(3) . . . . no
C17 C10 C11 C12 -3.5(3) . . . . no
C17 C10 C11 C16 175.70(18) . . . . no
N2 C10 C17 C18 -90.2(3) . . . . no
N2 C10 C17 C22 91.5(3) . . . . no
C11 C10 C17 C18 88.7(3) . . . . no
C11 C10 C17 C22 -89.6(3) . . . . no
C10 C11 C12 C13 179.6(2) . . . . no
C16 C11 C12 C13 0.4(3) . . . . no
C10 C11 C16 O2 -0.4(3) . . . . no
C10 C11 C16 C15 -179.41(18) . . . . no
C12 C11 C16 O2 178.81(18) . . . . no
C12 C11 C16 C15 -0.2(3) . . . . no
C11 C12 C13 C14 -0.3(3) . . . . no
C12 C13 C14 O4 -179.07(19) . . . . no
C12 C13 C14 C15 0.2(3) . . . . no
O4 C14 C15 C16 179.19(18) . . . . no
C13 C14 C15 C16 0.0(3) . . . . no
C14 C15 C16 O2 -179.03(18) . . . . no
C14 C15 C16 C11 0.0(3) . . . . no
C10 C17 C18 C19 -177.1(3) . . . . no
C22 C17 C18 C19 1.2(4) . . . . no
C10 C17 C22 C21 178.1(2) . . . . no
C18 C17 C22 C21 -0.2(4) . . . . no
C17 C18 C19 C20 -0.8(4) . . . . no
C18 C19 C20 C21 -0.6(4) . . . . no
C19 C20 C21 C22 1.6(4) . . . . no
C20 C21 C22 C17 -1.2(4) . . . . no

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Ni1 O5 3.8837(17) . . no
Ni1 O6 3.9300(17) . . no
Ni1 C13 3.716(2) . 1_455 no
O1 O2 2.475(2) . . no
O1 O6 2.790(2) . . no
O1 N1 2.714(2) . . no
O1 C7 2.892(3) . . no
O1 C13 3.383(3) . 1_455 no
O2 O5 2.742(2) . . no
O2 O6 3.057(2) . . no
O2 C10 2.926(3) . . no
O2 N2 2.702(2) . . no
O3 O6 2.878(2) . 1_455 no
O3 O5 2.634(2) . 2_556 no
O4 O5 2.761(2) . 1_655 no
O4 O6 2.566(2) . 2_656 no
O5 C16 3.382(2) . . no
N1 N2 2.547(2) . . no
N1 C1 2.926(3) . . no
N1 C9 2.379(3) . . no
N2 C8 2.389(3) . . no
N2 C16 2.905(2) . . no
C1 C13 3.377(3) . 1_455 no
C1 C22 3.591(3) . 4_454 no
C1 C14 3.356(3) . 1_455 no
C2 C14 3.316(3) . 1_455 no
C2 C15 3.446(3) . 1_455 no
C3 C15 3.426(3) . 1_455 no
C6 C12 3.593(3) . 1_455 no
C8 C15 3.518(3) . 4_454 no
C8 C14 3.598(3) . 4_454 no
C9 C18 3.482(4) . . no
C9 C22 3.420(3) . . no
C12 C22 3.511(3) . . no
C12 C18 3.434(3) . . no

_iucr_refine_instruction_details_constraints 
;
#
# Punched on 06/02/17 at 14:38:27
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S H(1,X'S) UNTIL H(6) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 06/02/17 at 14:38:27
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


#===END


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

data_ral1706SNQ
_database_code_depnum_ccdc_archive 'CCDC 1988290'
loop_
_audit_author_name
_audit_author_address
'Anthony Willis'
;Australian National University
Australia
;
_audit_update_record             
;
2020-03-05 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_audit_creation_date             17-01-31
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title 'Z:\ral1706SNQ\Tony_ral1706SNQ_da At 15:25 on'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   13.1465(1)
_cell_length_b                   14.9679(1)
_cell_length_c                   16.4141(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.3576(11)
_cell_angle_gamma                90
_cell_volume                     3082.81(5)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni -3.0029 0.5091 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C32 H34 N2 Ni1 O6 S2 
# Dc =      1.43 Fooo =   1392.00 Mu =     25.65 M =    665.47
# Found Formula = C32 H34 N2 Ni1 O6 S2 
# Dc =      1.43 FOOO =   1392.00 Mu =     25.65 M =    665.47

_chemical_formula_sum            'C32 H34 N2 Ni1 O6 S2'
_chemical_formula_moiety         'C28 H22 N2 Ni O4, 2(C2 H6 O S)'
_chemical_compound_source        ' from U of Wollongong'
_chemical_formula_weight         665.47


_cell_measurement_reflns_used    20116
_cell_measurement_theta_min      4
_cell_measurement_theta_max      74
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_min          0.036
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_max          0.369

_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    2.565

# Sheldrick geometric approximatio 0.57 0.91 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro version 1.171.38.43 (Rigaku Oxford Diffraction, 2016)
(Release 29 April 2016; compiled 27 May 2016,16:53)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  0.91
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
#_diffrn_ambient_temperature 150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_measurement_method       'ω scans'


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

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

_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            35398
_reflns_number_total             6213
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.0429

# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 6213 
# Theoretical number of reflections is about 12520 


_diffrn_reflns_theta_min         3.522
_diffrn_reflns_theta_max         74.016
_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        72.813
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -16
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              20

_oxford_diffrn_Wilson_B_factor   1.80
_oxford_diffrn_Wilson_scale      0.14

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

_refine_diff_density_min         -0.54
_refine_diff_density_max         1.21


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         6213
_refine_ls_number_restraints     0
_refine_ls_number_parameters     394
_oxford_refine_ls_R_factor_ref   0.0381
_refine_ls_wR_factor_ref         0.0993
_refine_ls_goodness_of_fit_ref   0.9963
_refine_ls_shift/su_max          0.0015379
_refine_ls_shift/su_mean         0.0000795


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6213
_refine_ls_R_factor_all          0.0381
_refine_ls_wR_factor_all         0.0993

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5834
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_gt          0.0974

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.06P)² + 2.61P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_special_details          
# see also _refine_ls_hydrogen for refinement keywords.                         
;                                                                               

The H atoms were all located in a difference map, but 
those bonded to C
 were repositioned geometrically. 
The H atoms were initially refined with soft restraints on the 
bond lengths and angles to regularise their geometry 
(C---H in the range 0.93--0.98Å, O---H = 0.83Å) and with
Uiso(H) in the range 1.2-1.5 times Ueq of the parent atom, 
after which the positions were refined with riding constraints
and the displacement parameters were held fixed. 
Finally the positions of the H atoms bonded to O were also allowed 
to refine freely.

 

The largest features in the
final difference electron density map are located 
near S2 and then midway between bonded C atoms.
The former might suggest a very small degree
of disorder in the packing of this solvate molecule.
;

# 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 0.49841(2) 0.109413(18) 0.608626(16) 0.0141 1.0000 Uani . . . . . .
S1 S 0.44915(4) 0.45365(3) 0.63060(3) 0.0283 1.0000 Uani . . . . . .
S2 S 0.11779(5) 0.55984(3) 0.45005(3) 0.0348 1.0000 Uani . . . . . .
O1 O 0.46052(9) 0.09828(8) 0.70708(7) 0.0191 1.0000 Uani . . . . . .
O2 O 0.63238(9) 0.07784(8) 0.67513(7) 0.0193 1.0000 Uani . . . . . .
O3 O 0.19248(11) 0.32078(9) 0.50553(9) 0.0268 1.0000 Uani . . . . . .
O4 O 0.63100(11) 0.31240(9) 0.45583(8) 0.0264 1.0000 Uani . . . . . .
O5 O 0.36930(14) 0.51506(10) 0.57163(10) 0.0439 1.0000 Uani . . . . . .
O6 O 0.08515(13) 0.46293(11) 0.43658(12) 0.0480 1.0000 Uani . . . . . .
N1 N 0.36004(11) 0.13182(9) 0.54114(8) 0.0154 1.0000 Uani . . . . . .
N2 N 0.54114(11) 0.12921(9) 0.51221(8) 0.0155 1.0000 Uani . . . . . .
C1 C 0.37479(13) 0.13217(11) 0.71989(10) 0.0172 1.0000 Uani . . . . . .
C2 C 0.37087(14) 0.13688(12) 0.80532(11) 0.0222 1.0000 Uani . . . . . .
C3 C 0.28410(15) 0.17140(13) 0.82472(11) 0.0249 1.0000 Uani . . . . . .
C4 C 0.19647(15) 0.20446(14) 0.76058(12) 0.0271 1.0000 Uani . . . . . .
C5 C 0.19772(14) 0.19954(13) 0.67749(11) 0.0234 1.0000 Uani . . . . . .
C6 C 0.28436(13) 0.16302(11) 0.65459(10) 0.0171 1.0000 Uani . . . . . .
C7 C 0.27708(13) 0.15381(11) 0.56494(10) 0.0162 1.0000 Uani . . . . . .
C8 C 0.35007(13) 0.11563(11) 0.45046(10) 0.0182 1.0000 Uani . . . . . .
C9 C 0.45130(13) 0.14896(12) 0.43532(10) 0.0199 1.0000 Uani . . . . . .
C10 C 0.63805(13) 0.13776(10) 0.50756(10) 0.0160 1.0000 Uani . . . . . .
C11 C 0.73157(13) 0.12390(11) 0.58024(10) 0.0171 1.0000 Uani . . . . . .
C12 C 0.83395(14) 0.13950(12) 0.57149(12) 0.0230 1.0000 Uani . . . . . .
C13 C 0.92508(15) 0.12474(13) 0.63796(13) 0.0277 1.0000 Uani . . . . . .
C14 C 0.91662(14) 0.09306(13) 0.71559(12) 0.0266 1.0000 Uani . . . . . .
C15 C 0.81863(14) 0.07721(13) 0.72663(11) 0.0238 1.0000 Uani . . . . . .
C16 C 0.72305(13) 0.09290(11) 0.65956(10) 0.0177 1.0000 Uani . . . . . .
C17 C 0.16960(13) 0.16505(12) 0.50035(10) 0.0184 1.0000 Uani . . . . . .
C18 C 0.12958(13) 0.24965(12) 0.47342(11) 0.0198 1.0000 Uani . . . . . .
C19 C 0.02729(14) 0.25876(14) 0.41580(12) 0.0269 1.0000 Uani . . . . . .
C20 C -0.03327(15) 0.18319(16) 0.38604(13) 0.0346 1.0000 Uani . . . . . .
C21 C 0.00597(16) 0.09915(15) 0.41194(14) 0.0343 1.0000 Uani . . . . . .
C22 C 0.10753(15) 0.08995(13) 0.46945(13) 0.0273 1.0000 Uani . . . . . .
C23 C 0.65397(13) 0.16255(11) 0.42383(10) 0.0173 1.0000 Uani . . . . . .
C24 C 0.64806(13) 0.25236(12) 0.39962(11) 0.0194 1.0000 Uani . . . . . .
C25 C 0.65905(14) 0.27618(13) 0.32061(11) 0.0233 1.0000 Uani . . . . . .
C26 C 0.67574(14) 0.21046(13) 0.26668(11) 0.0246 1.0000 Uani . . . . . .
C27 C 0.68224(14) 0.12103(13) 0.29031(11) 0.0241 1.0000 Uani . . . . . .
C28 C 0.67164(14) 0.09738(12) 0.36891(11) 0.0209 1.0000 Uani . . . . . .
C29 C 0.45647(17) 0.35921(15) 0.56675(13) 0.0338 1.0000 Uani . . . . . .
C30 C 0.3808(2) 0.40245(15) 0.69652(13) 0.0375 1.0000 Uani . . . . . .
C31 C 0.2026(2) 0.5773(2) 0.38594(16) 0.0481 1.0000 Uani . . . . . .
C32 C 0.0046(2) 0.61873(17) 0.38560(19) 0.0493 1.0000 Uani . . . . . .
H3 H 0.160(2) 0.3704(19) 0.4883(17) 0.0414 1.0000 Uiso . . . . . .
H4 H 0.630(2) 0.3618(19) 0.4398(17) 0.0408 1.0000 Uiso . . . . . .
H21 H 0.4292 0.1155 0.8471 0.0273 1.0000 Uiso R . . . . .
H31 H 0.2839 0.1727 0.8821 0.0295 1.0000 Uiso R . . . . .
H41 H 0.1383 0.2298 0.7745 0.0323 1.0000 Uiso R . . . . .
H51 H 0.1395 0.2206 0.6350 0.0280 1.0000 Uiso R . . . . .
H81 H 0.3414 0.0523 0.4400 0.0214 1.0000 Uiso R . . . . .
H82 H 0.2884 0.1460 0.4131 0.0212 1.0000 Uiso R . . . . .
H91 H 0.4483 0.2131 0.4261 0.0242 1.0000 Uiso R . . . . .
H92 H 0.4619 0.1208 0.3862 0.0243 1.0000 Uiso R . . . . .
H121 H 0.8399 0.1616 0.5202 0.0273 1.0000 Uiso R . . . . .
H131 H 0.9918 0.1359 0.6315 0.0339 1.0000 Uiso R . . . . .
H141 H 0.9770 0.0822 0.7599 0.0314 1.0000 Uiso R . . . . .
H151 H 0.8131 0.0556 0.7790 0.0278 1.0000 Uiso R . . . . .
H191 H 0.0008 0.3157 0.3973 0.0324 1.0000 Uiso R . . . . .
H201 H -0.1016 0.1900 0.3488 0.0421 1.0000 Uiso R . . . . .
H211 H -0.0339 0.0482 0.3918 0.0410 1.0000 Uiso R . . . . .
H221 H 0.1368 0.0310 0.4909 0.0295 1.0000 Uiso R . . . . .
H251 H 0.6551 0.3355 0.3056 0.0280 1.0000 Uiso R . . . . .
H261 H 0.6815 0.2269 0.2136 0.0304 1.0000 Uiso R . . . . .
H271 H 0.6943 0.0778 0.2543 0.0296 1.0000 Uiso R . . . . .
H281 H 0.6746 0.0364 0.3858 0.0230 1.0000 Uiso R . . . . .
H291 H 0.4924 0.3777 0.5269 0.0513 1.0000 Uiso R . . . . .
H292 H 0.4982 0.3155 0.6034 0.0515 1.0000 Uiso R . . . . .
H293 H 0.3856 0.3371 0.5394 0.0502 1.0000 Uiso R . . . . .
H301 H 0.3683 0.4464 0.7345 0.0563 1.0000 Uiso R . . . . .
H302 H 0.4239 0.3542 0.7276 0.0565 1.0000 Uiso R . . . . .
H303 H 0.3139 0.3798 0.6609 0.0551 1.0000 Uiso R . . . . .
H311 H 0.2656 0.5425 0.4076 0.0715 1.0000 Uiso R . . . . .
H312 H 0.2216 0.6404 0.3877 0.0720 1.0000 Uiso R . . . . .
H313 H 0.1642 0.5595 0.3296 0.0719 1.0000 Uiso R . . . . .
H321 H -0.0550 0.6108 0.4089 0.0737 1.0000 Uiso R . . . . .
H322 H 0.0219 0.6823 0.3856 0.0738 1.0000 Uiso R . . . . .
H323 H -0.0136 0.5954 0.3263 0.0737 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.82(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . O1 . 1.8352(12) yes
Ni1 . O2 . 1.8357(12) yes
Ni1 . N1 . 1.8564(14) yes
Ni1 . N2 . 1.8543(14) yes
S1 . O5 . 1.5091(15) yes
S1 . C29 . 1.779(2) yes
S1 . C30 . 1.773(2) yes
S2 . O6 . 1.5102(17) yes
S2 . C31 . 1.766(3) yes
S2 . C32 . 1.781(2) yes
O1 . C1 . 1.309(2) yes
O2 . C16 . 1.311(2) yes
O3 . C18 . 1.355(2) yes
O3 . H3 . 0.86(3) no
O4 . C24 . 1.354(2) yes
O4 . H4 . 0.78(3) no
N1 . C7 . 1.306(2) yes
N1 . C8 . 1.475(2) yes
N2 . C9 . 1.4784(19) yes
N2 . C10 . 1.305(2) yes
C1 . C2 . 1.420(2) yes
C1 . C6 . 1.420(2) yes
C2 . C3 . 1.373(3) yes
C2 . H21 . 0.920 no
C3 . C4 . 1.399(3) yes
C3 . H31 . 0.943 no
C4 . C5 . 1.371(3) yes
C4 . H41 . 0.940 no
C5 . C6 . 1.412(2) yes
C5 . H51 . 0.924 no
C6 . C7 . 1.452(2) yes
C7 . C17 . 1.502(2) yes
C8 . C9 . 1.510(2) yes
C8 . H81 . 0.964 no
C8 . H82 . 0.972 no
C9 . H91 . 0.971 no
C9 . H92 . 0.956 no
C10 . C11 . 1.450(2) yes
C10 . C23 . 1.497(2) yes
C11 . C12 . 1.415(2) yes
C11 . C16 . 1.418(2) yes
C12 . C13 . 1.376(3) yes
C12 . H121 . 0.929 no
C13 . C14 . 1.395(3) yes
C13 . H131 . 0.930 no
C14 . C15 . 1.374(3) yes
C14 . H141 . 0.917 no
C15 . C16 . 1.422(2) yes
C15 . H151 . 0.942 no
C17 . C18 . 1.392(2) yes
C17 . C22 . 1.393(2) yes
C18 . C19 . 1.401(2) yes
C19 . C20 . 1.386(3) yes
C19 . H191 . 0.937 no
C20 . C21 . 1.378(3) yes
C20 . H201 . 0.930 no
C21 . C22 . 1.393(3) yes
C21 . H211 . 0.929 no
C22 . H221 . 0.985 no
C23 . C24 . 1.397(2) yes
C23 . C28 . 1.394(2) yes
C24 . C25 . 1.394(2) yes
C25 . C26 . 1.384(3) yes
C25 . H251 . 0.919 no
C26 . C27 . 1.389(3) yes
C26 . H261 . 0.930 no
C27 . C28 . 1.384(3) yes
C27 . H271 . 0.921 no
C28 . H281 . 0.952 no
C29 . H291 . 0.955 no
C29 . H292 . 0.946 no
C29 . H293 . 0.964 no
C30 . H301 . 0.955 no
C30 . H302 . 0.964 no
C30 . H303 . 0.961 no
C31 . H311 . 0.953 no
C31 . H312 . 0.975 no
C31 . H313 . 0.951 no
C32 . H321 . 0.976 no
C32 . H322 . 0.979 no
C32 . H323 . 0.994 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . Ni1 . O2 . 85.25(5) yes
O1 . Ni1 . N1 . 93.83(6) yes
O2 . Ni1 . N1 . 175.46(6) yes
O1 . Ni1 . N2 . 175.57(6) yes
O2 . Ni1 . N2 . 93.87(6) yes
N1 . Ni1 . N2 . 87.38(6) yes
O5 . S1 . C29 . 104.81(10) yes
O5 . S1 . C30 . 105.82(11) yes
C29 . S1 . C30 . 98.18(11) yes
O6 . S2 . C31 . 104.92(12) yes
O6 . S2 . C32 . 103.76(11) yes
C31 . S2 . C32 . 97.87(13) yes
Ni1 . O1 . C1 . 125.40(11) yes
Ni1 . O2 . C16 . 127.34(11) yes
C18 . O3 . H3 . 111.3(18) no
C24 . O4 . H4 . 113(2) no
Ni1 . N1 . C7 . 128.63(11) yes
Ni1 . N1 . C8 . 110.41(10) yes
C7 . N1 . C8 . 120.85(14) yes
Ni1 . N2 . C9 . 113.10(10) yes
Ni1 . N2 . C10 . 127.97(11) yes
C9 . N2 . C10 . 118.39(13) yes
O1 . C1 . C2 . 117.67(15) yes
O1 . C1 . C6 . 124.89(15) yes
C2 . C1 . C6 . 117.42(15) yes
C1 . C2 . C3 . 121.66(16) yes
C1 . C2 . H21 . 116.8 no
C3 . C2 . H21 . 121.6 no
C2 . C3 . C4 . 120.87(16) yes
C2 . C3 . H31 . 119.3 no
C4 . C3 . H31 . 119.9 no
C3 . C4 . C5 . 118.56(17) yes
C3 . C4 . H41 . 120.5 no
C5 . C4 . H41 . 121.0 no
C4 . C5 . C6 . 122.40(16) yes
C4 . C5 . H51 . 118.6 no
C6 . C5 . H51 . 119.0 no
C1 . C6 . C5 . 119.03(15) yes
C1 . C6 . C7 . 121.43(15) yes
C5 . C6 . C7 . 119.47(15) yes
C6 . C7 . N1 . 121.25(14) yes
C6 . C7 . C17 . 117.93(14) yes
N1 . C7 . C17 . 120.73(14) yes
N1 . C8 . C9 . 107.13(13) yes
N1 . C8 . H81 . 108.2 no
C9 . C8 . H81 . 111.0 no
N1 . C8 . H82 . 111.5 no
C9 . C8 . H82 . 110.6 no
H81 . C8 . H82 . 108.3 no
C8 . C9 . N2 . 108.20(13) yes
C8 . C9 . H91 . 110.8 no
N2 . C9 . H91 . 108.4 no
C8 . C9 . H92 . 110.5 no
N2 . C9 . H92 . 110.6 no
H91 . C9 . H92 . 108.3 no
N2 . C10 . C11 . 122.73(15) yes
N2 . C10 . C23 . 118.96(14) yes
C11 . C10 . C23 . 118.31(14) yes
C10 . C11 . C12 . 119.45(15) yes
C10 . C11 . C16 . 121.50(15) yes
C12 . C11 . C16 . 119.04(15) yes
C11 . C12 . C13 . 121.50(17) yes
C11 . C12 . H121 . 119.4 no
C13 . C12 . H121 . 119.1 no
C12 . C13 . C14 . 119.40(17) yes
C12 . C13 . H131 . 120.5 no
C14 . C13 . H131 . 120.1 no
C13 . C14 . C15 . 120.84(16) yes
C13 . C14 . H141 . 119.9 no
C15 . C14 . H141 . 119.2 no
C14 . C15 . C16 . 121.08(17) yes
C14 . C15 . H151 . 120.7 no
C16 . C15 . H151 . 118.2 no
C15 . C16 . C11 . 118.13(16) yes
C15 . C16 . O2 . 117.75(15) yes
C11 . C16 . O2 . 124.12(15) yes
C7 . C17 . C18 . 120.87(15) yes
C7 . C17 . C22 . 119.49(16) yes
C18 . C17 . C22 . 119.59(16) yes
C17 . C18 . O3 . 117.55(15) yes
C17 . C18 . C19 . 119.92(16) yes
O3 . C18 . C19 . 122.53(16) yes
C18 . C19 . C20 . 119.57(18) yes
C18 . C19 . H191 . 119.7 no
C20 . C19 . H191 . 120.7 no
C19 . C20 . C21 . 120.91(18) yes
C19 . C20 . H201 . 118.9 no
C21 . C20 . H201 . 120.2 no
C20 . C21 . C22 . 119.62(19) yes
C20 . C21 . H211 . 121.4 no
C22 . C21 . H211 . 119.0 no
C21 . C22 . C17 . 120.40(18) yes
C21 . C22 . H221 . 121.6 no
C17 . C22 . H221 . 118.0 no
C10 . C23 . C24 . 119.23(15) yes
C10 . C23 . C28 . 121.06(15) yes
C24 . C23 . C28 . 119.69(16) yes
C23 . C24 . O4 . 116.83(15) yes
C23 . C24 . C25 . 119.89(16) yes
O4 . C24 . C25 . 123.28(16) yes
C24 . C25 . C26 . 119.58(17) yes
C24 . C25 . H251 . 118.9 no
C26 . C25 . H251 . 121.5 no
C25 . C26 . C27 . 120.98(16) yes
C25 . C26 . H261 . 119.0 no
C27 . C26 . H261 . 120.1 no
C26 . C27 . C28 . 119.45(17) yes
C26 . C27 . H271 . 120.4 no
C28 . C27 . H271 . 120.2 no
C23 . C28 . C27 . 120.42(17) yes
C23 . C28 . H281 . 118.9 no
C27 . C28 . H281 . 120.6 no
S1 . C29 . H291 . 107.3 no
S1 . C29 . H292 . 107.4 no
H291 . C29 . H292 . 108.9 no
S1 . C29 . H293 . 109.4 no
H291 . C29 . H293 . 112.8 no
H292 . C29 . H293 . 110.8 no
S1 . C30 . H301 . 108.6 no
S1 . C30 . H302 . 108.8 no
H301 . C30 . H302 . 111.1 no
S1 . C30 . H303 . 108.6 no
H301 . C30 . H303 . 109.6 no
H302 . C30 . H303 . 110.2 no
S2 . C31 . H311 . 109.2 no
S2 . C31 . H312 . 109.2 no
H311 . C31 . H312 . 109.4 no
S2 . C31 . H313 . 106.9 no
H311 . C31 . H313 . 111.1 no
H312 . C31 . H313 . 111.0 no
S2 . C32 . H321 . 109.5 no
S2 . C32 . H322 . 109.1 no
H321 . C32 . H322 . 109.4 no
S2 . C32 . H323 . 108.8 no
H321 . C32 . H323 . 110.8 no
H322 . C32 . H323 . 109.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O3 . H3 . O6 . 170(3) 0.86(3) 1.76(3) 2.616(3) yes
O4 . H4 . O5 2_666 166(3) 0.78(3) 1.85(3) 2.622(3) yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C1 161.75(13) . . . . no
N1 Ni1 O1 C1 -22.71(14) . . . . no
O1 Ni1 O2 C16 -158.85(14) . . . . no
N2 Ni1 O2 C16 16.79(14) . . . . no
O1 Ni1 N1 C7 15.05(15) . . . . no
O1 Ni1 N1 C8 -161.12(10) . . . . no
N2 Ni1 N1 C7 -160.68(15) . . . . no
N2 Ni1 N1 C8 23.15(11) . . . . no
O2 Ni1 N2 C9 174.19(11) . . . . no
O2 Ni1 N2 C10 -14.49(14) . . . . no
N1 Ni1 N2 C9 -1.43(11) . . . . no
N1 Ni1 N2 C10 169.89(14) . . . . no
Ni1 O1 C1 C2 -164.38(12) . . . . no
Ni1 O1 C1 C6 16.9(2) . . . . no
Ni1 O2 C16 C11 -11.1(2) . . . . no
Ni1 O2 C16 C15 168.83(12) . . . . no
Ni1 N1 C7 C6 -0.7(2) . . . . no
Ni1 N1 C7 C17 -177.08(12) . . . . no
C8 N1 C7 C6 175.10(15) . . . . no
C8 N1 C7 C17 -1.3(2) . . . . no
Ni1 N1 C8 C9 -38.62(15) . . . . no
C7 N1 C8 C9 144.87(15) . . . . no
Ni1 N2 C9 C8 -19.79(16) . . . . no
C10 N2 C9 C8 167.98(14) . . . . no
Ni1 N2 C10 C11 6.3(2) . . . . no
Ni1 N2 C10 C23 -173.98(11) . . . . no
C9 N2 C10 C11 177.19(14) . . . . no
C9 N2 C10 C23 -3.1(2) . . . . no
O1 C1 C2 C3 -180.00(18) . . . . no
C6 C1 C2 C3 -1.2(3) . . . . no
O1 C1 C6 C5 -178.95(16) . . . . no
O1 C1 C6 C7 4.1(3) . . . . no
C2 C1 C6 C5 2.4(2) . . . . no
C2 C1 C6 C7 -174.61(16) . . . . no
C1 C2 C3 C4 -0.9(3) . . . . no
C2 C3 C4 C5 1.7(3) . . . . no
C3 C4 C5 C6 -0.5(3) . . . . no
C4 C5 C6 C1 -1.6(3) . . . . no
C4 C5 C6 C7 175.45(18) . . . . no
C1 C6 C7 N1 -12.4(3) . . . . no
C1 C6 C7 C17 164.07(16) . . . . no
C5 C6 C7 N1 170.65(16) . . . . no
C5 C6 C7 C17 -12.9(2) . . . . no
N1 C7 C17 C18 -101.1(2) . . . . no
N1 C7 C17 C22 81.3(2) . . . . no
C6 C7 C17 C18 82.4(2) . . . . no
C6 C7 C17 C22 -95.2(2) . . . . no
N1 C8 C9 N2 36.63(17) . . . . no
N2 C10 C11 C12 -176.32(15) . . . . no
N2 C10 C11 C16 5.3(2) . . . . no
C23 C10 C11 C12 3.9(2) . . . . no
C23 C10 C11 C16 -174.51(15) . . . . no
N2 C10 C23 C24 82.6(2) . . . . no
N2 C10 C23 C28 -95.6(2) . . . . no
C11 C10 C23 C24 -97.60(19) . . . . no
C11 C10 C23 C28 84.2(2) . . . . no
C10 C11 C12 C13 -178.07(17) . . . . no
C16 C11 C12 C13 0.4(3) . . . . no
C10 C11 C16 O2 -2.8(3) . . . . no
C10 C11 C16 C15 177.27(16) . . . . no
C12 C11 C16 O2 178.72(16) . . . . no
C12 C11 C16 C15 -1.2(2) . . . . no
C11 C12 C13 C14 0.5(3) . . . . no
C12 C13 C14 C15 -0.6(3) . . . . no
C13 C14 C15 C16 -0.3(3) . . . . no
C14 C15 C16 O2 -178.79(17) . . . . no
C14 C15 C16 C11 1.1(3) . . . . no
C7 C17 C18 O3 2.1(2) . . . . no
C7 C17 C18 C19 -177.34(16) . . . . no
C22 C17 C18 O3 179.61(17) . . . . no
C22 C17 C18 C19 0.2(3) . . . . no
C7 C17 C22 C21 177.58(18) . . . . no
C18 C17 C22 C21 0.0(3) . . . . no
O3 C18 C19 C20 -179.39(18) . . . . no
C17 C18 C19 C20 0.0(3) . . . . no
C18 C19 C20 C21 -0.4(3) . . . . no
C19 C20 C21 C22 0.6(3) . . . . no
C20 C21 C22 C17 -0.4(3) . . . . no
C10 C23 C24 O4 1.9(2) . . . . no
C10 C23 C24 C25 -177.80(16) . . . . no
C28 C23 C24 O4 -179.86(16) . . . . no
C28 C23 C24 C25 0.5(3) . . . . no
C10 C23 C28 C27 177.57(17) . . . . no
C24 C23 C28 C27 -0.7(3) . . . . no
O4 C24 C25 C26 -179.63(17) . . . . no
C23 C24 C25 C26 0.0(3) . . . . no
C24 C25 C26 C27 -0.3(3) . . . . no
C25 C26 C27 C28 0.1(3) . . . . no
C26 C27 C28 C23 0.4(3) . . . . no

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Ni1 C29 3.812(2) . . no
Ni1 C25 3.8878(18) . 4_555 no
Ni1 C26 3.9782(19) . 4_555 no
Ni1 C28 3.8995(19) . 2_656 no
S1 O1 3.3627(12) . 3_656 no
S1 C2 3.5695(19) . 3_656 no
S1 C27 3.5663(19) . 4_555 no
S2 O5 3.3805(19) . . no
O1 C7 2.931(2) . . no
O1 O2 2.4860(17) . . no
O1 C25 3.304(2) . 4_555 no
O1 N1 2.6961(17) . . no
O2 N2 2.6958(17) . . no
O2 C25 3.178(2) . 4_555 no
O2 C10 2.9151(19) . . no
O2 C30 3.403(2) . 3_646 no
O3 O6 2.617(2) . . no
O3 C5 3.339(2) . . no
O3 C29 3.362(3) . . no
O3 C6 3.355(2) . . no
O4 N2 3.2284(19) . . no
O4 O5 2.621(2) . 2_666 no
O4 C31 3.297(3) . 2_666 no
O4 C29 3.400(3) . . no
O4 C9 3.347(2) . . no
O5 O4 2.621(2) . 2_666 no
O5 C31 3.313(3) . . no
O6 C19 3.143(3) . . no
O6 C18 3.269(2) . . no
N1 N2 2.563(2) . . no
N1 C1 2.882(2) . . no
N1 C9 2.401(2) . . no
N2 C8 2.421(2) . . no
N2 C16 2.901(2) . . no
C5 C18 3.286(2) . . no
C8 C22 3.317(3) . . no
C8 C16 3.591(2) . 2_656 no
C9 C28 3.473(3) . . no
C9 C24 3.215(3) . . no
C12 C28 3.431(3) . . no
C12 C24 3.560(3) . . no
C16 C25 3.587(2) . 4_555 no
C16 C26 3.577(3) . 4_555 no



_iucr_refine_instruction_details_constraints 
;
#
# Punched on 31/01/17 at 12:27:01
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S H(3,X'S) H(4,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) H   ( 292,X'S) H   ( 293,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) H   ( 303,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 31/01/17 at 12:27:01
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


#===END

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

data_cmpd15_exp_132_tsb
_database_code_depnum_ccdc_archive 'CCDC 1984625'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_audit_creation_date             2020-02-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
N-(4-(hydroxybenzophenylidene))-N'-(naphthalidine)ethylenediaminenickel(II)
_chemical_formula_moiety         'C26 H20 N2 Ni O3, H2 O'
_chemical_formula_sum            'C26 H22 N2 Ni O4'
_chemical_formula_weight         485.16
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C26H22N2Ni1O4
_chemical_oxdiff_usercomment     'TSB 27_P from DMSO/water'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   13.4737(3)
_cell_length_b                   18.9348(3)
_cell_length_c                   8.4020(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.792(2)
_cell_angle_gamma                90
_cell_volume                     2098.30(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13822
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.6740
_cell_measurement_theta_min      1.9060
_shelx_estimated_absorpt_T_max   0.953
_shelx_estimated_absorpt_T_min   0.660
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.48a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_recrystallization_method 'crystallised from DMSO/water'
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            21869
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.770
_diffrn_reflns_theta_min         2.848
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_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    -74.00 110.00   0.50   20.00    --   20.00  54.00-150.00  368
  2  ω    -74.00 109.50   0.50   20.00    --   20.00  54.00  90.00  367
  3  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00  30.00  368
  4  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00  30.00  368
  5  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00 120.00  368
  6  ω     11.00  82.00   0.50   20.00    --   20.00  54.00 120.00  142
  7  ω     -5.00 106.50   0.50   20.00    --   20.00  54.00 -30.00  223
  8  ω    -72.00 -47.00   0.50   20.00    --   20.00  54.00 150.00   50
  9  ω    -73.00  39.00   0.50   20.00    --   20.00  54.00  60.00  224
 10  ω    -41.00  11.50   0.50   20.00    --   20.00  54.00-150.00  105
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0057104000
_diffrn_orient_matrix_UB_12      -0.0371719000
_diffrn_orient_matrix_UB_13      -0.0019447000
_diffrn_orient_matrix_UB_21      0.0058510000
_diffrn_orient_matrix_UB_22      0.0021029000
_diffrn_orient_matrix_UB_23      -0.0817222000
_diffrn_orient_matrix_UB_31      0.0530393000
_diffrn_orient_matrix_UB_32      0.0037366000
_diffrn_orient_matrix_UB_33      0.0270872000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.868
_reflns_Friedel_fraction_max     0.823
_reflns_number_gt                4792
_reflns_number_total             4964
_reflns_odcompleteness_completeness 99.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_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         0.311
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 
;
 Flack x determined using 2094 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4964
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0256
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0465P)²+0.2590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0680
_refine_special_details          
;
The [E2-1] statistic was ca. 0.85 and solution was tried in Cc and C2/c using 
SHELXT. The best solution in SHELXT was Cc. SHELXS did not find a good 
solution in C2/c. The refinement in Cc went well and the data looked acentric 
from a Wilson plots and a plot of cumulative intensity in OLEX2. The data was 
taken into PLATON to look for missed symmetry and no change in space group 
was suggested.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1W(H1WA,H1WB)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.48601(3) 0.70576(2) 0.58912(3) 0.01915(8) Uani 1 1 d . . . . .
O2 O 0.41324(15) 0.64583(9) 0.6936(2) 0.0244(4) Uani 1 1 d . . . . .
O4 O 0.25533(15) 0.55326(9) 1.1031(2) 0.0272(4) Uani 1 1 d . . . . .
H4 H 0.258775 0.516943 1.051384 0.041 Uiso 1 1 calc GR . . . .
O18 O 0.48850(15) 0.63077(9) 0.4493(2) 0.0236(4) Uani 1 1 d . . . . .
N1 N 0.48611(17) 0.78078(10) 0.7341(3) 0.0211(4) Uani 1 1 d . . . . .
N2 N 0.54733(16) 0.76579(11) 0.4675(3) 0.0219(4) Uani 1 1 d . . . . .
C1 C 0.39204(18) 0.72330(14) 0.9131(3) 0.0193(4) Uani 1 1 d . . . . .
C2 C 0.38045(18) 0.65771(12) 0.8279(3) 0.0197(4) Uani 1 1 d . . . . .
C3 C 0.33071(18) 0.60147(12) 0.8889(3) 0.0212(4) Uani 1 1 d . . . . .
H3 H 0.319638 0.559467 0.830633 0.025 Uiso 1 1 calc R . . . .
C4 C 0.29808(18) 0.60773(12) 1.0341(3) 0.0203(4) Uani 1 1 d . . . . .
C5 C 0.30898(19) 0.67200(13) 1.1190(3) 0.0227(5) Uani 1 1 d . . . . .
H5 H 0.285121 0.676761 1.214776 0.027 Uiso 1 1 calc R . . . .
C6 C 0.35521(19) 0.72774(13) 1.0592(3) 0.0213(4) Uani 1 1 d . . . . .
H6 H 0.362667 0.770035 1.116703 0.026 Uiso 1 1 calc R . . . .
C7 C 0.44293(18) 0.78386(12) 0.8593(3) 0.0194(4) Uani 1 1 d . . . . .
C8 C 0.44237(19) 0.85188(12) 0.9531(3) 0.0213(4) Uani 1 1 d . . . . .
C9 C 0.3496(2) 0.88470(13) 0.9528(4) 0.0279(5) Uani 1 1 d . . . . .
H9 H 0.290188 0.866146 0.890852 0.033 Uiso 1 1 calc R . . . .
C10 C 0.3461(2) 0.94524(15) 1.0455(4) 0.0375(7) Uani 1 1 d . . . . .
H10 H 0.284168 0.966939 1.045603 0.045 Uiso 1 1 calc R . . . .
C11 C 0.4339(3) 0.97319(16) 1.1370(4) 0.0451(8) Uani 1 1 d . . . . .
H11 H 0.430858 1.012812 1.201285 0.054 Uiso 1 1 calc R . . . .
C12 C 0.5261(3) 0.94248(16) 1.1334(4) 0.0403(7) Uani 1 1 d . . . . .
H12 H 0.585438 0.962258 1.192766 0.048 Uiso 1 1 calc R . . . .
C13 C 0.5309(2) 0.88192(14) 1.0411(3) 0.0285(5) Uani 1 1 d . . . . .
H13 H 0.593300 0.861566 1.038418 0.034 Uiso 1 1 calc R . . . .
C14 C 0.5449(2) 0.84176(13) 0.6925(3) 0.0273(5) Uani 1 1 d . . . . .
H14A H 0.615145 0.838172 0.748639 0.033 Uiso 1 1 calc R . . . .
H14B H 0.517171 0.885561 0.724539 0.033 Uiso 1 1 calc R . . . .
C15 C 0.5376(2) 0.84043(13) 0.5115(3) 0.0274(5) Uani 1 1 d . . . . .
H15A H 0.472981 0.859368 0.455618 0.033 Uiso 1 1 calc R . . . .
H15B H 0.591524 0.868369 0.482254 0.033 Uiso 1 1 calc R . . . .
C16 C 0.59058(19) 0.75043(13) 0.3470(3) 0.0229(5) Uani 1 1 d . . . . .
H16 H 0.623189 0.786768 0.303593 0.027 Uiso 1 1 calc R . . . .
C17 C 0.59176(18) 0.68201(14) 0.2764(3) 0.0203(4) Uani 1 1 d . . . . .
C18 C 0.53496(18) 0.62676(12) 0.3275(3) 0.0203(4) Uani 1 1 d . . . . .
C19 C 0.52669(19) 0.56126(13) 0.2405(3) 0.0243(5) Uani 1 1 d . . . . .
H19 H 0.490836 0.524155 0.274494 0.029 Uiso 1 1 calc R . . . .
C20 C 0.5701(2) 0.55207(13) 0.1093(3) 0.0260(5) Uani 1 1 d . . . . .
H20 H 0.562056 0.509149 0.054308 0.031 Uiso 1 1 calc R . . . .
C21 C 0.62770(19) 0.60679(14) 0.0540(3) 0.0240(5) Uani 1 1 d . . . . .
C22 C 0.64047(17) 0.67196(13) 0.1389(3) 0.0213(5) Uani 1 1 d . . . . .
C23 C 0.70262(19) 0.72349(14) 0.0861(3) 0.0246(5) Uani 1 1 d . . . . .
H23 H 0.714546 0.766011 0.142145 0.030 Uiso 1 1 calc R . . . .
C24 C 0.7457(2) 0.71194(14) -0.0465(4) 0.0289(6) Uani 1 1 d . . . . .
H24 H 0.786432 0.746706 -0.078262 0.035 Uiso 1 1 calc R . . . .
C25 C 0.7295(2) 0.64909(16) -0.1341(4) 0.0335(6) Uani 1 1 d . . . . .
H25 H 0.757422 0.642506 -0.225558 0.040 Uiso 1 1 calc R . . . .
C26 C 0.6718(2) 0.59678(16) -0.0840(3) 0.0315(6) Uani 1 1 d . . . . .
H26 H 0.661683 0.554451 -0.141134 0.038 Uiso 1 1 calc R . . . .
O1W O 0.27286(15) 0.43018(9) 0.9621(2) 0.0277(4) Uani 1 1 d . . . . .
H1WA H 0.274089 0.433339 0.861668 0.042 Uiso 1 1 d G . . . .
H1WB H 0.328261 0.412306 1.012886 0.042 Uiso 1 1 d G . . . .


_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 O2 1.8361(17) . ?
Ni1 O18 1.8478(17) . ?
Ni1 N1 1.871(2) . ?
Ni1 N2 1.834(2) . ?
O2 C2 1.313(3) . ?
O4 H4 0.8200 . ?
O4 C4 1.367(3) . ?
O18 C18 1.306(3) . ?
N1 C7 1.304(3) . ?
N1 C14 1.482(3) . ?
N2 C15 1.473(3) . ?
N2 C16 1.300(3) . ?
C1 C2 1.426(3) . ?
C1 C6 1.417(3) . ?
C1 C7 1.455(3) . ?
C2 C3 1.409(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.384(3) . ?
C4 C5 1.403(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.372(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.510(3) . ?
C8 C9 1.396(4) . ?
C8 C13 1.390(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.392(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.378(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.378(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.393(4) . ?
C13 H13 0.9300 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.503(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16 0.9300 . ?
C16 C17 1.426(4) . ?
C17 C18 1.414(3) . ?
C17 C22 1.453(3) . ?
C18 C19 1.432(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.361(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.428(4) . ?
C21 C22 1.418(4) . ?
C21 C26 1.419(4) . ?
C22 C23 1.415(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.375(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.393(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.377(4) . ?
C26 H26 0.9300 . ?
O1W H1WA 0.8498 . ?
O1W H1WB 0.8505 . ?

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
O2 Ni1 O18 84.84(8) . . ?
O2 Ni1 N1 95.01(8) . . ?
O18 Ni1 N1 178.66(10) . . ?
N2 Ni1 O2 174.12(10) . . ?
N2 Ni1 O18 93.05(9) . . ?
N2 Ni1 N1 87.23(9) . . ?
C2 O2 Ni1 127.71(15) . . ?
C4 O4 H4 109.5 . . ?
C18 O18 Ni1 128.08(15) . . ?
C7 N1 Ni1 128.20(17) . . ?
C7 N1 C14 120.2(2) . . ?
C14 N1 Ni1 111.55(16) . . ?
C15 N2 Ni1 112.42(16) . . ?
C16 N2 Ni1 128.30(18) . . ?
C16 N2 C15 119.1(2) . . ?
C2 C1 C7 122.7(2) . . ?
C6 C1 C2 117.7(2) . . ?
C6 C1 C7 119.5(2) . . ?
O2 C2 C1 124.0(2) . . ?
O2 C2 C3 116.9(2) . . ?
C3 C2 C1 119.1(2) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.1(2) . . ?
C4 C3 H3 119.5 . . ?
O4 C4 C3 123.1(2) . . ?
O4 C4 C5 116.6(2) . . ?
C3 C4 C5 120.2(2) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 C4 119.3(2) . . ?
C6 C5 H5 120.3 . . ?
C1 C6 H6 118.8 . . ?
C5 C6 C1 122.5(2) . . ?
C5 C6 H6 118.8 . . ?
N1 C7 C1 122.1(2) . . ?
N1 C7 C8 120.6(2) . . ?
C1 C7 C8 117.2(2) . . ?
C9 C8 C7 118.6(2) . . ?
C13 C8 C7 122.1(2) . . ?
C13 C8 C9 119.3(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 119.9(3) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0(3) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.2(3) . . ?
C13 C12 H12 119.9 . . ?
C8 C13 C12 120.1(3) . . ?
C8 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
N1 C14 H14A 110.2 . . ?
N1 C14 H14B 110.2 . . ?
N1 C14 C15 107.3(2) . . ?
H14A C14 H14B 108.5 . . ?
C15 C14 H14A 110.2 . . ?
C15 C14 H14B 110.2 . . ?
N2 C15 C14 106.2(2) . . ?
N2 C15 H15A 110.5 . . ?
N2 C15 H15B 110.5 . . ?
C14 C15 H15A 110.5 . . ?
C14 C15 H15B 110.5 . . ?
H15A C15 H15B 108.7 . . ?
N2 C16 H16 117.6 . . ?
N2 C16 C17 124.9(2) . . ?
C17 C16 H16 117.6 . . ?
C16 C17 C22 119.7(2) . . ?
C18 C17 C16 119.5(2) . . ?
C18 C17 C22 120.3(2) . . ?
O18 C18 C17 124.8(2) . . ?
O18 C18 C19 116.8(2) . . ?
C17 C18 C19 118.4(2) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 C18 121.5(2) . . ?
C20 C19 H19 119.2 . . ?
C19 C20 H20 119.2 . . ?
C19 C20 C21 121.5(2) . . ?
C21 C20 H20 119.2 . . ?
C22 C21 C20 119.1(2) . . ?
C22 C21 C26 119.9(2) . . ?
C26 C21 C20 121.0(2) . . ?
C21 C22 C17 119.1(2) . . ?
C23 C22 C17 123.5(2) . . ?
C23 C22 C21 117.4(2) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 C22 121.3(3) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 H24 119.4 . . ?
C23 C24 C25 121.2(3) . . ?
C25 C24 H24 119.4 . . ?
C24 C25 H25 120.3 . . ?
C26 C25 C24 119.4(3) . . ?
C26 C25 H25 120.3 . . ?
C21 C26 H26 119.6 . . ?
C25 C26 C21 120.7(3) . . ?
C25 C26 H26 119.6 . . ?
H1WA O1W H1WB 109.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O4 H4 O1W 0.82 1.83 2.647(2) 172.3 . yes
O1W H1WB O2 0.85 2.03 2.816(3) 153.4 2_565 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O2 C2 C1 3.6(4) . . . . ?
Ni1 O2 C2 C3 -176.61(17) . . . . ?
Ni1 O18 C18 C17 -1.8(4) . . . . ?
Ni1 O18 C18 C19 178.38(17) . . . . ?
Ni1 N1 C7 C1 5.0(4) . . . . ?
Ni1 N1 C7 C8 -173.81(18) . . . . ?
Ni1 N1 C14 C15 29.6(3) . . . . ?
Ni1 N2 C15 C14 36.3(3) . . . . ?
Ni1 N2 C16 C17 5.1(4) . . . . ?
O2 Ni1 O18 C18 -176.2(2) . . . . ?
O2 Ni1 N1 C7 -2.2(2) . . . . ?
O2 Ni1 N1 C14 177.44(18) . . . . ?
O2 C2 C3 C4 176.7(2) . . . . ?
O4 C4 C5 C6 177.3(2) . . . . ?
O18 Ni1 O2 C2 176.4(2) . . . . ?
O18 Ni1 N2 C15 164.73(18) . . . . ?
O18 Ni1 N2 C16 -10.9(2) . . . . ?
O18 C18 C19 C20 178.4(2) . . . . ?
N1 Ni1 O2 C2 -2.2(2) . . . . ?
N1 Ni1 N2 C15 -16.59(18) . . . . ?
N1 Ni1 N2 C16 167.7(3) . . . . ?
N1 C7 C8 C9 115.2(3) . . . . ?
N1 C7 C8 C13 -65.8(3) . . . . ?
N1 C14 C15 N2 -41.0(3) . . . . ?
N2 Ni1 O18 C18 9.3(2) . . . . ?
N2 Ni1 N1 C7 172.4(2) . . . . ?
N2 Ni1 N1 C14 -8.01(19) . . . . ?
N2 C16 C17 C18 6.1(4) . . . . ?
N2 C16 C17 C22 178.4(2) . . . . ?
C1 C2 C3 C4 -3.5(4) . . . . ?
C1 C7 C8 C9 -63.7(3) . . . . ?
C1 C7 C8 C13 115.3(3) . . . . ?
C2 C1 C6 C5 -0.5(4) . . . . ?
C2 C1 C7 N1 -3.8(4) . . . . ?
C2 C1 C7 C8 175.1(2) . . . . ?
C2 C3 C4 O4 -175.7(2) . . . . ?
C2 C3 C4 C5 3.6(4) . . . . ?
C3 C4 C5 C6 -2.1(4) . . . . ?
C4 C5 C6 C1 0.5(4) . . . . ?
C6 C1 C2 O2 -178.3(2) . . . . ?
C6 C1 C2 C3 1.9(3) . . . . ?
C6 C1 C7 N1 173.8(2) . . . . ?
C6 C1 C7 C8 -7.3(3) . . . . ?
C7 N1 C14 C15 -150.7(2) . . . . ?
C7 C1 C2 O2 -0.7(4) . . . . ?
C7 C1 C2 C3 179.6(2) . . . . ?
C7 C1 C6 C5 -178.2(2) . . . . ?
C7 C8 C9 C10 176.4(3) . . . . ?
C7 C8 C13 C12 -176.3(2) . . . . ?
C8 C9 C10 C11 0.3(5) . . . . ?
C9 C8 C13 C12 2.7(4) . . . . ?
C9 C10 C11 C12 2.0(5) . . . . ?
C10 C11 C12 C13 -1.9(5) . . . . ?
C11 C12 C13 C8 -0.4(5) . . . . ?
C13 C8 C9 C10 -2.6(4) . . . . ?
C14 N1 C7 C1 -174.5(2) . . . . ?
C14 N1 C7 C8 6.6(4) . . . . ?
C15 N2 C16 C17 -170.3(2) . . . . ?
C16 N2 C15 C14 -147.6(2) . . . . ?
C16 C17 C18 O18 -7.8(4) . . . . ?
C16 C17 C18 C19 172.0(2) . . . . ?
C16 C17 C22 C21 -170.3(2) . . . . ?
C16 C17 C22 C23 11.2(4) . . . . ?
C17 C18 C19 C20 -1.5(4) . . . . ?
C17 C22 C23 C24 -178.9(2) . . . . ?
C18 C17 C22 C21 1.9(3) . . . . ?
C18 C17 C22 C23 -176.7(2) . . . . ?
C18 C19 C20 C21 1.3(4) . . . . ?
C19 C20 C21 C22 0.5(4) . . . . ?
C19 C20 C21 C26 -179.4(3) . . . . ?
C20 C21 C22 C17 -2.0(4) . . . . ?
C20 C21 C22 C23 176.6(2) . . . . ?
C20 C21 C26 C25 -178.3(3) . . . . ?
C21 C22 C23 C24 2.5(4) . . . . ?
C22 C17 C18 O18 -179.9(2) . . . . ?
C22 C17 C18 C19 -0.1(3) . . . . ?
C22 C21 C26 C25 1.8(4) . . . . ?
C22 C23 C24 C25 0.2(4) . . . . ?
C23 C24 C25 C26 -2.0(5) . . . . ?
C24 C25 C26 C21 1.0(5) . . . . ?
C26 C21 C22 C17 177.9(2) . . . . ?
C26 C21 C22 C23 -3.5(4) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.167
_oxdiff_exptl_absorpt_empirical_full_min 0.889
####################################################################### 
# 
# 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_cmpd16_exp_134_tsb
_database_code_depnum_ccdc_archive 'CCDC 1984626'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_audit_creation_date             2020-02-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
N-(4-((1-(2-ethyl)piperidine)oxy)benzophenylidene)-N'-(naphthalidine)ethylenediaminenickel(II)
_chemical_formula_moiety         'C33 H33 N3 Ni O3'
_chemical_formula_sum            'C33 H33 N3 Ni O3'
_chemical_formula_weight         578.33
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C33H33N3Ni1O3
_chemical_oxdiff_usercomment     'TSB 27 from DCM/MeOH'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   18.9200(4)
_cell_length_b                   7.61382(12)
_cell_length_c                   19.7486(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.5135(16)
_cell_angle_gamma                90
_cell_volume                     2805.73(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    29870
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.5700
_cell_measurement_theta_min      1.7240
_shelx_estimated_absorpt_T_max   0.911
_shelx_estimated_absorpt_T_min   0.759
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.48a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method 'from DCM/MeOH'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73796
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.697
_diffrn_reflns_theta_min         2.091
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 110.00   0.50    8.50    --   20.00  54.00 -97.68  368
  2  ω    -74.00 110.00   0.50    8.50    --   20.00  54.00 -62.93  368
  3  ω    -74.00 110.00   0.50    8.50    --   20.00  54.00 -55.68  368
  4  ω    -74.00 110.00   0.50    8.50    --   20.00  54.00 -55.68  368
  5  ω    -74.00 109.50   0.50    8.50    --   20.00  54.00-133.48  367
  6  ω    -74.00 109.50   0.50    8.50    --   20.00  54.00 164.70  367
  7  ω    -74.00 110.00   0.50    8.50    --   20.00  54.00-120.00  368
  8  ω     60.00 110.00   0.50    8.50    --   20.00  54.00-120.00  100
  9  ω    -69.00  48.00   0.50    8.50    --   20.00  54.00 -80.48  234
 10  ω     85.00 110.00   0.50    8.50    --   20.00  54.00 -80.48   50
 11  ω    -63.00  45.00   0.50    8.50    --   20.00  54.00  30.00  216
 12  ω     51.00  77.00   0.50    8.50    --   20.00  54.00  30.00   52
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0363243000
_diffrn_orient_matrix_UB_12      -0.0194346000
_diffrn_orient_matrix_UB_13      -0.0017386000
_diffrn_orient_matrix_UB_21      -0.0072291000
_diffrn_orient_matrix_UB_22      0.0097036000
_diffrn_orient_matrix_UB_23      -0.0361806000
_diffrn_orient_matrix_UB_31      0.0085794000
_diffrn_orient_matrix_UB_32      0.0906426000
_diffrn_orient_matrix_UB_33      0.0035141000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                13184
_reflns_number_total             14383
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.48a (Rigaku OD, 2019)'
_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         0.536
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 
;
 Flack x determined using 5621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         14383
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0307
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0455P)²+0.7377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0810
_refine_special_details          
;
This data was treated in the same way as above. The [E2-1] statistic was ca. 
0.85 and solution was tried in P2(1) and P2(1)/m using SHELXT. The best 
solution in SHELXT was P2(1) where both molecules 'dropped out' and the 
refinement went well and this is the solution provided. SHELXS found a 
reasonable looking solution in P2(1) but refinement did not go well and 
led to a chemically unreasonable (polymeric) structure. The data seemed 
neither strongly centric or acentric in plots (Wilson or Cumulative 
intensity in OLEX2). The data was taken into PLATON to look for missed 
symmetry and no change in space group was suggested.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C1A(H1AA,H1AB),
  C26A(H26C,H26D), C27A(H27C,H27D), C28A(H28C,H28D), C29A(H29C,H29D), C30A(H30C,
 H30D), C31A(H31C,H31D), C32A(H32C,H32D), C33A(H33C,H33D)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14),
 C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C2A(H2A),
  C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A), C14A(H14A),
 C16A(H16A), C17A(H17A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A),
 C25A(H25A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.25443(2) 1.44663(4) 0.56421(2) 0.01956(7) Uani 1 1 d . . . . .
O1 O 0.32883(9) 1.4975(2) 0.51679(9) 0.0233(4) Uani 1 1 d . . . . .
O2 O 0.32446(9) 1.3546(2) 0.63029(9) 0.0248(4) Uani 1 1 d . . . . .
O3 O 0.43617(11) 1.1639(3) 0.85228(10) 0.0347(5) Uani 1 1 d . . . . .
N1 N 0.18682(11) 1.5559(3) 0.49971(11) 0.0216(4) Uani 1 1 d . . . . .
N2 N 0.17885(11) 1.3755(3) 0.60764(11) 0.0222(4) Uani 1 1 d . . . . .
N3 N 0.58816(14) 1.0206(4) 0.90603(13) 0.0410(6) Uani 1 1 d . . . . .
C1 C 0.11754(14) 1.5777(4) 0.52401(14) 0.0256(5) Uani 1 1 d . . . . .
H1A H 0.078744 1.589469 0.485483 0.031 Uiso 1 1 calc R . . . .
H1B H 0.118351 1.681180 0.552798 0.031 Uiso 1 1 calc R . . . .
C2 C 0.19451(14) 1.6219(3) 0.44102(13) 0.0238(5) Uani 1 1 d . . . . .
H2 H 0.154828 1.675474 0.415112 0.029 Uiso 1 1 calc R . . . .
C3 C 0.25988(13) 1.6185(3) 0.41287(13) 0.0212(5) Uani 1 1 d . . . . .
C4 C 0.26072(14) 1.6786(3) 0.34337(12) 0.0222(5) Uani 1 1 d . . . . .
C5 C 0.20033(15) 1.7550(3) 0.30148(14) 0.0271(5) Uani 1 1 d . . . . .
H5 H 0.158408 1.772002 0.319439 0.033 Uiso 1 1 calc R . . . .
C6 C 0.20261(16) 1.8047(4) 0.23433(14) 0.0316(6) Uani 1 1 d . . . . .
H6 H 0.162415 1.854846 0.207935 0.038 Uiso 1 1 calc R . . . .
C7 C 0.26530(17) 1.7797(4) 0.20581(15) 0.0369(7) Uani 1 1 d . . . . .
H7 H 0.266335 1.811351 0.160500 0.044 Uiso 1 1 calc R . . . .
C8 C 0.32459(16) 1.7088(4) 0.24510(14) 0.0337(6) Uani 1 1 d . . . . .
H8 H 0.365922 1.692642 0.226070 0.040 Uiso 1 1 calc R . . . .
C9 C 0.32451(14) 1.6592(3) 0.31421(13) 0.0260(5) Uani 1 1 d . . . . .
C10 C 0.38724(15) 1.5908(4) 0.35633(14) 0.0297(6) Uani 1 1 d . . . . .
H10 H 0.429178 1.579002 0.337926 0.036 Uiso 1 1 calc R . . . .
C11 C 0.38710(14) 1.5426(4) 0.42275(14) 0.0276(5) Uani 1 1 d . . . . .
H11 H 0.429335 1.502236 0.449012 0.033 Uiso 1 1 calc R . . . .
C12 C 0.32349(13) 1.5524(3) 0.45312(13) 0.0222(5) Uani 1 1 d . . . . .
C13 C 0.31663(14) 1.2918(3) 0.69066(13) 0.0222(5) Uani 1 1 d . . . . .
C14 C 0.38013(14) 1.2612(3) 0.73845(13) 0.0251(5) Uani 1 1 d . . . . .
H14 H 0.424378 1.288541 0.726515 0.030 Uiso 1 1 calc R . . . .
C15 C 0.37711(14) 1.1912(4) 0.80253(13) 0.0261(5) Uani 1 1 d . . . . .
C16 C 0.31095(15) 1.1415(4) 0.82085(13) 0.0271(5) Uani 1 1 d . . . . .
H16 H 0.309290 1.089158 0.863117 0.032 Uiso 1 1 calc R . . . .
C17 C 0.24923(15) 1.1715(3) 0.77539(13) 0.0264(5) Uani 1 1 d . . . . .
H17 H 0.205731 1.138178 0.787566 0.032 Uiso 1 1 calc R . . . .
C18 C 0.24905(14) 1.2515(3) 0.71028(13) 0.0226(5) Uani 1 1 d . . . . .
C19 C 0.18205(13) 1.2898(3) 0.66566(13) 0.0221(5) Uani 1 1 d . . . . .
C20 C 0.11299(14) 1.2281(3) 0.68650(14) 0.0268(5) Uani 1 1 d . . . . .
C21 C 0.08532(16) 1.3108(4) 0.73962(15) 0.0348(6) Uani 1 1 d . . . . .
H21 H 0.109884 1.404163 0.763119 0.042 Uiso 1 1 calc R . . . .
C22 C 0.02095(19) 1.2534(5) 0.75734(19) 0.0469(9) Uani 1 1 d . . . . .
H22 H 0.002573 1.308247 0.792764 0.056 Uiso 1 1 calc R . . . .
C23 C -0.01571(18) 1.1150(5) 0.7223(2) 0.0502(10) Uani 1 1 d . . . . .
H23 H -0.058525 1.076429 0.734524 0.060 Uiso 1 1 calc R . . . .
C24 C 0.01114(17) 1.0330(4) 0.6689(2) 0.0462(9) Uani 1 1 d . . . . .
H24 H -0.014041 0.940758 0.645267 0.055 Uiso 1 1 calc R . . . .
C25 C 0.07570(15) 1.0887(4) 0.65080(16) 0.0334(6) Uani 1 1 d . . . . .
H25 H 0.093812 1.033695 0.615274 0.040 Uiso 1 1 calc R . . . .
C26 C 0.10812(13) 1.4127(3) 0.56483(13) 0.0261(5) Uani 1 1 d . . . . .
H26A H 0.071982 1.431000 0.593704 0.031 Uiso 1 1 calc R . . . .
H26B H 0.093359 1.315121 0.534148 0.031 Uiso 1 1 calc R . . . .
C27 C 0.50240(16) 1.2384(4) 0.84059(15) 0.0357(7) Uani 1 1 d . . . . .
H27A H 0.496962 1.364156 0.833914 0.043 Uiso 1 1 calc R . . . .
H27B H 0.515870 1.188072 0.799423 0.043 Uiso 1 1 calc R . . . .
C28 C 0.56065(17) 1.2013(5) 0.90193(15) 0.0397(7) Uani 1 1 d . . . . .
H28A H 0.600323 1.280896 0.900177 0.048 Uiso 1 1 calc R . . . .
H28B H 0.541738 1.226798 0.943623 0.048 Uiso 1 1 calc R . . . .
C29 C 0.5405(2) 0.8996(6) 0.9345(2) 0.0628(12) Uani 1 1 d . . . . .
H29A H 0.493119 0.904030 0.906871 0.075 Uiso 1 1 calc R . . . .
H29B H 0.536350 0.936117 0.980768 0.075 Uiso 1 1 calc R . . . .
C30 C 0.5691(3) 0.7100(7) 0.9361(3) 0.0743(14) Uani 1 1 d . . . . .
H30A H 0.537515 0.633307 0.956556 0.089 Uiso 1 1 calc R . . . .
H30B H 0.569713 0.670043 0.889558 0.089 Uiso 1 1 calc R . . . .
C31 C 0.6445(3) 0.7004(9) 0.9774(2) 0.097(2) Uani 1 1 d . . . . .
H31A H 0.663608 0.582886 0.974684 0.116 Uiso 1 1 calc R . . . .
H31B H 0.643219 0.726714 1.025226 0.116 Uiso 1 1 calc R . . . .
C32 C 0.6925(3) 0.8330(8) 0.9485(3) 0.0881(18) Uani 1 1 d . . . . .
H32A H 0.739652 0.833296 0.976589 0.106 Uiso 1 1 calc R . . . .
H32B H 0.697750 0.799031 0.902262 0.106 Uiso 1 1 calc R . . . .
C33 C 0.6602(2) 1.0167(7) 0.9474(2) 0.0675(13) Uani 1 1 d . . . . .
H33A H 0.657550 1.053215 0.993968 0.081 Uiso 1 1 calc R . . . .
H33B H 0.690937 1.098832 0.928444 0.081 Uiso 1 1 calc R . . . .
Ni1A Ni 0.26236(2) 0.95350(4) 0.55999(2) 0.02083(7) Uani 1 1 d . . . . .
O1A O 0.17156(10) 1.0016(2) 0.51254(9) 0.0258(4) Uani 1 1 d . . . . .
O2A O 0.21486(10) 0.8565(3) 0.62473(9) 0.0268(4) Uani 1 1 d . . . . .
O3A O 0.16668(13) 0.6506(3) 0.83397(11) 0.0403(5) Uani 1 1 d . . . . .
N1A N 0.30724(11) 1.0636(3) 0.49521(11) 0.0232(4) Uani 1 1 d . . . . .
N2A N 0.35304(11) 0.8848(3) 0.60409(11) 0.0232(4) Uani 1 1 d . . . . .
N3A N 0.09840(19) 0.7542(4) 0.96246(14) 0.0491(7) Uani 1 1 d . . . . .
C1A C 0.38474(14) 1.0857(4) 0.51980(14) 0.0263(5) Uani 1 1 d . . . . .
H1AA H 0.393554 1.189775 0.548254 0.032 Uiso 1 1 calc R . . . .
H1AB H 0.410330 1.097141 0.481323 0.032 Uiso 1 1 calc R . . . .
C2A C 0.27896(14) 1.1270(3) 0.43590(13) 0.0240(5) Uani 1 1 d . . . . .
H2A H 0.309448 1.179684 0.409505 0.029 Uiso 1 1 calc R . . . .
C3A C 0.20370(14) 1.1215(3) 0.40811(13) 0.0225(5) Uani 1 1 d . . . . .
C4A C 0.17820(14) 1.1793(3) 0.33843(13) 0.0251(5) Uani 1 1 d . . . . .
C5A C 0.22274(17) 1.2556(4) 0.29534(14) 0.0306(6) Uani 1 1 d . . . . .
H5A H 0.271035 1.273196 0.312416 0.037 Uiso 1 1 calc R . . . .
C6A C 0.19621(19) 1.3044(4) 0.22861(15) 0.0365(7) Uani 1 1 d . . . . .
H6A H 0.226684 1.355455 0.201794 0.044 Uiso 1 1 calc R . . . .
C7A C 0.12364(19) 1.2779(4) 0.20074(15) 0.0389(7) Uani 1 1 d . . . . .
H7A H 0.106357 1.308290 0.155412 0.047 Uiso 1 1 calc R . . . .
C8A C 0.07864(17) 1.2067(4) 0.24124(14) 0.0352(6) Uani 1 1 d . . . . .
H8A H 0.030566 1.189787 0.223066 0.042 Uiso 1 1 calc R . . . .
C9A C 0.10414(16) 1.1585(3) 0.31029(14) 0.0289(6) Uani 1 1 d . . . . .
C10A C 0.05658(15) 1.0904(4) 0.35301(15) 0.0317(6) Uani 1 1 d . . . . .
H10A H 0.008235 1.077727 0.335012 0.038 Uiso 1 1 calc R . . . .
C11A C 0.08028(15) 1.0438(4) 0.41942(15) 0.0296(6) Uani 1 1 d . . . . .
H11A H 0.047616 1.003328 0.446220 0.036 Uiso 1 1 calc R . . . .
C12A C 0.15495(14) 1.0559(3) 0.44895(13) 0.0232(5) Uani 1 1 d . . . . .
C13A C 0.24274(15) 0.7924(3) 0.68461(13) 0.0249(5) Uani 1 1 d . . . . .
C14A C 0.19506(16) 0.7505(3) 0.73028(14) 0.0290(6) Uani 1 1 d . . . . .
H14A H 0.146239 0.769985 0.716771 0.035 Uiso 1 1 calc R . . . .
C15A C 0.21958(16) 0.6811(4) 0.79482(14) 0.0311(6) Uani 1 1 d . . . . .
C16A C 0.29248(17) 0.6458(4) 0.81631(14) 0.0329(6) Uani 1 1 d . . . . .
H16A H 0.308765 0.598133 0.859424 0.039 Uiso 1 1 calc R . . . .
C17A C 0.33951(16) 0.6837(4) 0.77190(14) 0.0303(6) Uani 1 1 d . . . . .
H17A H 0.387816 0.658248 0.785749 0.036 Uiso 1 1 calc R . . . .
C18A C 0.31776(15) 0.7597(3) 0.70595(13) 0.0251(5) Uani 1 1 d . . . . .
C19A C 0.36969(14) 0.7985(3) 0.66192(13) 0.0236(5) Uani 1 1 d . . . . .
C20A C 0.44573(14) 0.7345(3) 0.68226(14) 0.0266(5) Uani 1 1 d . . . . .
C21A C 0.49253(17) 0.8169(4) 0.73438(15) 0.0355(6) Uani 1 1 d . . . . .
H21A H 0.476551 0.909994 0.758328 0.043 Uiso 1 1 calc R . . . .
C22A C 0.56349(18) 0.7599(5) 0.75079(18) 0.0442(8) Uani 1 1 d . . . . .
H22A H 0.594960 0.816453 0.785069 0.053 Uiso 1 1 calc R . . . .
C23A C 0.58700(17) 0.6188(5) 0.71589(19) 0.0459(8) Uani 1 1 d . . . . .
H23A H 0.634146 0.580399 0.727057 0.055 Uiso 1 1 calc R . . . .
C24A C 0.54013(17) 0.5347(4) 0.66423(18) 0.0398(7) Uani 1 1 d . . . . .
H24A H 0.556098 0.440228 0.641026 0.048 Uiso 1 1 calc R . . . .
C25A C 0.46921(15) 0.5917(4) 0.64706(15) 0.0306(6) Uani 1 1 d . . . . .
H25A H 0.437889 0.535342 0.612600 0.037 Uiso 1 1 calc R . . . .
C26A C 0.40901(13) 0.9224(4) 0.56117(13) 0.0263(5) Uani 1 1 d . . . . .
H26C H 0.413691 0.824335 0.530869 0.032 Uiso 1 1 calc R . . . .
H26D H 0.454981 0.942543 0.590014 0.032 Uiso 1 1 calc R . . . .
C27A C 0.1861(2) 0.5821(5) 0.90182(16) 0.0460(8) Uani 1 1 d . . . . .
H27C H 0.223691 0.653095 0.927744 0.055 Uiso 1 1 calc R . . . .
H27D H 0.203549 0.462724 0.900018 0.055 Uiso 1 1 calc R . . . .
C28A C 0.1200(2) 0.5855(5) 0.93590(19) 0.0537(10) Uani 1 1 d . . . . .
H28C H 0.080021 0.542066 0.902970 0.064 Uiso 1 1 calc R . . . .
H28D H 0.127476 0.502826 0.973785 0.064 Uiso 1 1 calc R . . . .
C29A C 0.1455(3) 0.8135(6) 1.0216(2) 0.0702(14) Uani 1 1 d . . . . .
H29C H 0.190590 0.849263 1.008560 0.084 Uiso 1 1 calc R . . . .
H29D H 0.155206 0.717765 1.054201 0.084 Uiso 1 1 calc R . . . .
C30A C 0.1133(3) 0.9690(6) 1.05590(19) 0.0746(14) Uani 1 1 d . . . . .
H30C H 0.071314 0.929856 1.074055 0.089 Uiso 1 1 calc R . . . .
H30D H 0.148028 1.012352 1.093859 0.089 Uiso 1 1 calc R . . . .
C31A C 0.0925(3) 1.1150(5) 1.0047(2) 0.0640(12) Uani 1 1 d . . . . .
H31C H 0.135263 1.165806 0.991688 0.077 Uiso 1 1 calc R . . . .
H31D H 0.067650 1.206520 1.025667 0.077 Uiso 1 1 calc R . . . .
C32A C 0.0444(3) 1.0457(6) 0.9416(2) 0.0692(13) Uani 1 1 d . . . . .
H32C H 0.034544 1.138470 0.907711 0.083 Uiso 1 1 calc R . . . .
H32D H -0.000764 1.007373 0.953717 0.083 Uiso 1 1 calc R . . . .
C33A C 0.0811(2) 0.8904(5) 0.91118(18) 0.0551(10) Uani 1 1 d . . . . .
H33C H 0.049361 0.843557 0.871704 0.066 Uiso 1 1 calc R . . . .
H33D H 0.124556 0.930673 0.896029 0.066 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 O1 1.8560(18) . ?
Ni1 O2 1.8381(18) . ?
Ni1 N1 1.847(2) . ?
Ni1 N2 1.865(2) . ?
O1 C12 1.313(3) . ?
O2 C13 1.315(3) . ?
O3 C15 1.376(3) . ?
O3 C27 1.429(4) . ?
N1 C1 1.478(3) . ?
N1 C2 1.293(3) . ?
N2 C19 1.311(3) . ?
N2 C26 1.487(3) . ?
N3 C28 1.468(5) . ?
N3 C29 1.465(5) . ?
N3 C33 1.469(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C26 1.519(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.438(4) . ?
C3 C4 1.450(3) . ?
C3 C12 1.420(4) . ?
C4 C5 1.420(4) . ?
C4 C9 1.428(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.387(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.407(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.366(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.416(4) . ?
C9 C10 1.430(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.363(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.433(4) . ?
C13 C14 1.419(4) . ?
C13 C18 1.429(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.383(4) . ?
C15 C16 1.411(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.369(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.423(4) . ?
C18 C19 1.449(4) . ?
C19 C20 1.508(3) . ?
C20 C21 1.398(4) . ?
C20 C25 1.399(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.392(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.383(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.392(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.395(4) . ?
C25 H25 0.9300 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.523(4) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.540(6) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.524(7) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.529(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.525(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
Ni1A O1A 1.8523(19) . ?
Ni1A O2A 1.8352(18) . ?
Ni1A N1A 1.849(2) . ?
Ni1A N2A 1.866(2) . ?
O1A C12A 1.310(3) . ?
O2A C13A 1.307(3) . ?
O3A C15A 1.382(3) . ?
O3A C27A 1.428(4) . ?
N1A C1A 1.476(3) . ?
N1A C2A 1.298(3) . ?
N2A C19A 1.310(3) . ?
N2A C26A 1.490(3) . ?
N3A C28A 1.470(4) . ?
N3A C29A 1.420(5) . ?
N3A C33A 1.449(5) . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C1A C26A 1.517(4) . ?
C2A H2A 0.9300 . ?
C2A C3A 1.439(4) . ?
C3A C4A 1.449(3) . ?
C3A C12A 1.413(4) . ?
C4A C5A 1.417(4) . ?
C4A C9A 1.428(4) . ?
C5A H5A 0.9300 . ?
C5A C6A 1.381(4) . ?
C6A H6A 0.9300 . ?
C6A C7A 1.407(5) . ?
C7A H7A 0.9300 . ?
C7A C8A 1.372(5) . ?
C8A H8A 0.9300 . ?
C8A C9A 1.418(4) . ?
C9A C10A 1.429(4) . ?
C10A H10A 0.9300 . ?
C10A C11A 1.361(4) . ?
C11A H11A 0.9300 . ?
C11A C12A 1.440(4) . ?
C13A C14A 1.413(4) . ?
C13A C18A 1.434(4) . ?
C14A H14A 0.9300 . ?
C14A C15A 1.387(4) . ?
C15A C16A 1.400(4) . ?
C16A H16A 0.9300 . ?
C16A C17A 1.379(4) . ?
C17A H17A 0.9300 . ?
C17A C18A 1.422(4) . ?
C18A C19A 1.446(4) . ?
C19A C20A 1.509(4) . ?
C20A C21A 1.391(4) . ?
C20A C25A 1.402(4) . ?
C21A H21A 0.9300 . ?
C21A C22A 1.397(5) . ?
C22A H22A 0.9300 . ?
C22A C23A 1.389(5) . ?
C23A H23A 0.9300 . ?
C23A C24A 1.392(5) . ?
C24A H24A 0.9300 . ?
C24A C25A 1.397(4) . ?
C25A H25A 0.9300 . ?
C26A H26C 0.9700 . ?
C26A H26D 0.9700 . ?
C27A H27C 0.9700 . ?
C27A H27D 0.9700 . ?
C27A C28A 1.515(5) . ?
C28A H28C 0.9700 . ?
C28A H28D 0.9700 . ?
C29A H29C 0.9700 . ?
C29A H29D 0.9700 . ?
C29A C30A 1.539(6) . ?
C30A H30C 0.9700 . ?
C30A H30D 0.9700 . ?
C30A C31A 1.510(6) . ?
C31A H31C 0.9700 . ?
C31A H31D 0.9700 . ?
C31A C32A 1.511(6) . ?
C32A H32C 0.9700 . ?
C32A H32D 0.9700 . ?
C32A C33A 1.542(6) . ?
C33A H33C 0.9700 . ?
C33A H33D 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N2 174.68(9) . . ?
O2 Ni1 O1 85.41(8) . . ?
O2 Ni1 N1 175.63(10) . . ?
O2 Ni1 N2 94.61(9) . . ?
N1 Ni1 O1 93.13(9) . . ?
N1 Ni1 N2 87.23(9) . . ?
C12 O1 Ni1 127.23(16) . . ?
C13 O2 Ni1 127.31(17) . . ?
C15 O3 C27 117.1(2) . . ?
C1 N1 Ni1 112.15(16) . . ?
C2 N1 Ni1 128.70(18) . . ?
C2 N1 C1 119.0(2) . . ?
C19 N2 Ni1 128.17(18) . . ?
C19 N2 C26 119.9(2) . . ?
C26 N2 Ni1 111.70(16) . . ?
C28 N3 C33 109.7(3) . . ?
C29 N3 C28 112.0(3) . . ?
C29 N3 C33 110.3(3) . . ?
N1 C1 H1A 110.6 . . ?
N1 C1 H1B 110.6 . . ?
N1 C1 C26 105.5(2) . . ?
H1A C1 H1B 108.8 . . ?
C26 C1 H1A 110.6 . . ?
C26 C1 H1B 110.6 . . ?
N1 C2 H2 117.6 . . ?
N1 C2 C3 124.8(2) . . ?
C3 C2 H2 117.6 . . ?
C2 C3 C4 120.3(2) . . ?
C12 C3 C2 119.6(2) . . ?
C12 C3 C4 120.1(2) . . ?
C5 C4 C3 123.2(2) . . ?
C5 C4 C9 117.4(2) . . ?
C9 C4 C3 119.4(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.3(3) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.5(3) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.2 . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 119.3 . . ?
C7 C8 C9 121.4(3) . . ?
C9 C8 H8 119.3 . . ?
C4 C9 C10 118.6(2) . . ?
C8 C9 C4 119.8(2) . . ?
C8 C9 C10 121.6(2) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 C9 121.6(2) . . ?
C11 C10 H10 119.2 . . ?
C10 C11 H11 119.2 . . ?
C10 C11 C12 121.6(3) . . ?
C12 C11 H11 119.2 . . ?
O1 C12 C3 124.9(2) . . ?
O1 C12 C11 116.6(2) . . ?
C3 C12 C11 118.5(2) . . ?
O2 C13 C14 116.9(2) . . ?
O2 C13 C18 124.3(2) . . ?
C14 C13 C18 118.8(2) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.9(2) . . ?
C15 C14 H14 119.6 . . ?
O3 C15 C14 124.1(2) . . ?
O3 C15 C16 115.2(2) . . ?
C14 C15 C16 120.7(2) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 C15 118.9(2) . . ?
C17 C16 H16 120.5 . . ?
C16 C17 H17 118.7 . . ?
C16 C17 C18 122.6(2) . . ?
C18 C17 H17 118.7 . . ?
C13 C18 C19 121.6(2) . . ?
C17 C18 C13 117.9(2) . . ?
C17 C18 C19 120.5(2) . . ?
N2 C19 C18 122.8(2) . . ?
N2 C19 C20 118.5(2) . . ?
C18 C19 C20 118.8(2) . . ?
C21 C20 C19 120.9(2) . . ?
C21 C20 C25 120.0(3) . . ?
C25 C20 C19 119.1(2) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 119.9(3) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.1(3) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.3(3) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.2(3) . . ?
C25 C24 H24 119.9 . . ?
C20 C25 H25 120.3 . . ?
C24 C25 C20 119.5(3) . . ?
C24 C25 H25 120.3 . . ?
N2 C26 C1 106.6(2) . . ?
N2 C26 H26A 110.4 . . ?
N2 C26 H26B 110.4 . . ?
C1 C26 H26A 110.4 . . ?
C1 C26 H26B 110.4 . . ?
H26A C26 H26B 108.6 . . ?
O3 C27 H27A 109.7 . . ?
O3 C27 H27B 109.7 . . ?
O3 C27 C28 109.7(2) . . ?
H27A C27 H27B 108.2 . . ?
C28 C27 H27A 109.7 . . ?
C28 C27 H27B 109.7 . . ?
N3 C28 C27 114.9(3) . . ?
N3 C28 H28A 108.5 . . ?
N3 C28 H28B 108.5 . . ?
C27 C28 H28A 108.5 . . ?
C27 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
N3 C29 H29A 109.4 . . ?
N3 C29 H29B 109.4 . . ?
N3 C29 C30 111.1(3) . . ?
H29A C29 H29B 108.0 . . ?
C30 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C31 C30 C29 110.5(5) . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C30 C31 H31A 109.8 . . ?
C30 C31 H31B 109.8 . . ?
C30 C31 C32 109.2(4) . . ?
H31A C31 H31B 108.3 . . ?
C32 C31 H31A 109.8 . . ?
C32 C31 H31B 109.8 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 C31 110.5(4) . . ?
C33 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
N3 C33 C32 111.0(4) . . ?
N3 C33 H33A 109.4 . . ?
N3 C33 H33B 109.4 . . ?
C32 C33 H33A 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
O1A Ni1A N2A 174.76(9) . . ?
O2A Ni1A O1A 84.95(8) . . ?
O2A Ni1A N1A 176.56(10) . . ?
O2A Ni1A N2A 94.60(9) . . ?
N1A Ni1A O1A 93.09(9) . . ?
N1A Ni1A N2A 87.60(10) . . ?
C12A O1A Ni1A 127.08(17) . . ?
C13A O2A Ni1A 127.56(18) . . ?
C15A O3A C27A 119.3(3) . . ?
C1A N1A Ni1A 111.64(16) . . ?
C2A N1A Ni1A 128.69(19) . . ?
C2A N1A C1A 119.6(2) . . ?
C19A N2A Ni1A 128.15(18) . . ?
C19A N2A C26A 120.1(2) . . ?
C26A N2A Ni1A 111.45(16) . . ?
C29A N3A C28A 113.4(3) . . ?
C29A N3A C33A 112.7(3) . . ?
C33A N3A C28A 114.8(3) . . ?
N1A C1A H1AA 110.5 . . ?
N1A C1A H1AB 110.5 . . ?
N1A C1A C26A 106.2(2) . . ?
H1AA C1A H1AB 108.7 . . ?
C26A C1A H1AA 110.5 . . ?
C26A C1A H1AB 110.5 . . ?
N1A C2A H2A 117.7 . . ?
N1A C2A C3A 124.6(2) . . ?
C3A C2A H2A 117.7 . . ?
C2A C3A C4A 120.4(2) . . ?
C12A C3A C2A 119.4(2) . . ?
C12A C3A C4A 120.2(2) . . ?
C5A C4A C3A 123.8(2) . . ?
C5A C4A C9A 117.0(2) . . ?
C9A C4A C3A 119.1(2) . . ?
C4A C5A H5A 119.2 . . ?
C6A C5A C4A 121.7(3) . . ?
C6A C5A H5A 119.2 . . ?
C5A C6A H6A 119.6 . . ?
C5A C6A C7A 120.8(3) . . ?
C7A C6A H6A 119.6 . . ?
C6A C7A H7A 120.4 . . ?
C8A C7A C6A 119.2(3) . . ?
C8A C7A H7A 120.4 . . ?
C7A C8A H8A 119.4 . . ?
C7A C8A C9A 121.2(3) . . ?
C9A C8A H8A 119.4 . . ?
C4A C9A C10A 118.9(2) . . ?
C8A C9A C4A 120.1(3) . . ?
C8A C9A C10A 121.0(3) . . ?
C9A C10A H10A 119.2 . . ?
C11A C10A C9A 121.6(3) . . ?
C11A C10A H10A 119.2 . . ?
C10A C11A H11A 119.4 . . ?
C10A C11A C12A 121.2(3) . . ?
C12A C11A H11A 119.4 . . ?
O1A C12A C3A 125.7(2) . . ?
O1A C12A C11A 115.6(2) . . ?
C3A C12A C11A 118.7(2) . . ?
O2A C13A C14A 117.2(2) . . ?
O2A C13A C18A 124.2(2) . . ?
C14A C13A C18A 118.6(2) . . ?
C13A C14A H14A 119.3 . . ?
C15A C14A C13A 121.4(3) . . ?
C15A C14A H14A 119.3 . . ?
O3A C15A C14A 114.5(3) . . ?
O3A C15A C16A 124.5(3) . . ?
C14A C15A C16A 121.0(3) . . ?
C15A C16A H16A 120.9 . . ?
C17A C16A C15A 118.3(3) . . ?
C17A C16A H16A 120.9 . . ?
C16A C17A H17A 118.4 . . ?
C16A C17A C18A 123.2(3) . . ?
C18A C17A H17A 118.4 . . ?
C13A C18A C19A 121.7(2) . . ?
C17A C18A C13A 117.5(2) . . ?
C17A C18A C19A 120.7(2) . . ?
N2A C19A C18A 122.5(2) . . ?
N2A C19A C20A 118.4(2) . . ?
C18A C19A C20A 119.1(2) . . ?
C21A C20A C19A 120.9(2) . . ?
C21A C20A C25A 120.1(3) . . ?
C25A C20A C19A 119.0(2) . . ?
C20A C21A H21A 120.0 . . ?
C20A C21A C22A 120.1(3) . . ?
C22A C21A H21A 120.0 . . ?
C21A C22A H22A 120.0 . . ?
C23A C22A C21A 120.0(3) . . ?
C23A C22A H22A 120.0 . . ?
C22A C23A H23A 119.9 . . ?
C22A C23A C24A 120.1(3) . . ?
C24A C23A H23A 119.9 . . ?
C23A C24A H24A 119.8 . . ?
C23A C24A C25A 120.3(3) . . ?
C25A C24A H24A 119.8 . . ?
C20A C25A H25A 120.3 . . ?
C24A C25A C20A 119.4(3) . . ?
C24A C25A H25A 120.3 . . ?
N2A C26A C1A 106.5(2) . . ?
N2A C26A H26C 110.4 . . ?
N2A C26A H26D 110.4 . . ?
C1A C26A H26C 110.4 . . ?
C1A C26A H26D 110.4 . . ?
H26C C26A H26D 108.6 . . ?
O3A C27A H27C 110.1 . . ?
O3A C27A H27D 110.1 . . ?
O3A C27A C28A 107.9(3) . . ?
H27C C27A H27D 108.4 . . ?
C28A C27A H27C 110.1 . . ?
C28A C27A H27D 110.1 . . ?
N3A C28A C27A 118.1(3) . . ?
N3A C28A H28C 107.8 . . ?
N3A C28A H28D 107.8 . . ?
C27A C28A H28C 107.8 . . ?
C27A C28A H28D 107.8 . . ?
H28C C28A H28D 107.1 . . ?
N3A C29A H29C 109.3 . . ?
N3A C29A H29D 109.3 . . ?
N3A C29A C30A 111.5(4) . . ?
H29C C29A H29D 108.0 . . ?
C30A C29A H29C 109.3 . . ?
C30A C29A H29D 109.3 . . ?
C29A C30A H30C 109.6 . . ?
C29A C30A H30D 109.6 . . ?
H30C C30A H30D 108.1 . . ?
C31A C30A C29A 110.5(3) . . ?
C31A C30A H30C 109.6 . . ?
C31A C30A H30D 109.6 . . ?
C30A C31A H31C 109.6 . . ?
C30A C31A H31D 109.6 . . ?
C30A C31A C32A 110.5(4) . . ?
H31C C31A H31D 108.1 . . ?
C32A C31A H31C 109.6 . . ?
C32A C31A H31D 109.6 . . ?
C31A C32A H32C 109.7 . . ?
C31A C32A H32D 109.7 . . ?
C31A C32A C33A 110.0(4) . . ?
H32C C32A H32D 108.2 . . ?
C33A C32A H32C 109.7 . . ?
C33A C32A H32D 109.7 . . ?
N3A C33A C32A 109.9(3) . . ?
N3A C33A H33C 109.7 . . ?
N3A C33A H33D 109.7 . . ?
C32A C33A H33C 109.7 . . ?
C32A C33A H33D 109.7 . . ?
H33C C33A H33D 108.2 . . ?

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 O1 C12 C3 14.0(3) . . . . ?
Ni1 O1 C12 C11 -165.50(18) . . . . ?
Ni1 O2 C13 C14 -167.42(18) . . . . ?
Ni1 O2 C13 C18 13.3(4) . . . . ?
Ni1 N1 C1 C26 -37.2(2) . . . . ?
Ni1 N1 C2 C3 1.7(4) . . . . ?
Ni1 N2 C19 C18 6.8(4) . . . . ?
Ni1 N2 C19 C20 -172.95(18) . . . . ?
Ni1 N2 C26 C1 -31.9(2) . . . . ?
O1 Ni1 O2 C13 175.3(2) . . . . ?
O1 Ni1 N1 C1 -168.82(17) . . . . ?
O1 Ni1 N1 C2 6.4(2) . . . . ?
O2 Ni1 O1 C12 170.2(2) . . . . ?
O2 Ni1 N2 C19 0.1(2) . . . . ?
O2 Ni1 N2 C26 -174.43(16) . . . . ?
O2 C13 C14 C15 -178.4(2) . . . . ?
O2 C13 C18 C17 175.1(2) . . . . ?
O2 C13 C18 C19 -4.7(4) . . . . ?
O3 C15 C16 C17 177.2(2) . . . . ?
O3 C27 C28 N3 75.8(3) . . . . ?
N1 Ni1 O1 C12 -13.9(2) . . . . ?
N1 Ni1 N2 C19 -176.0(2) . . . . ?
N1 Ni1 N2 C26 9.54(17) . . . . ?
N1 C1 C26 N2 42.9(3) . . . . ?
N1 C2 C3 C4 173.1(2) . . . . ?
N1 C2 C3 C12 -5.7(4) . . . . ?
N2 Ni1 O2 C13 -10.0(2) . . . . ?
N2 Ni1 N1 C1 16.49(18) . . . . ?
N2 Ni1 N1 C2 -168.3(2) . . . . ?
N2 C19 C20 C21 -106.8(3) . . . . ?
N2 C19 C20 C25 71.7(3) . . . . ?
N3 C29 C30 C31 57.3(5) . . . . ?
C1 N1 C2 C3 176.6(2) . . . . ?
C2 N1 C1 C26 147.1(2) . . . . ?
C2 C3 C4 C5 4.8(4) . . . . ?
C2 C3 C4 C9 -174.3(2) . . . . ?
C2 C3 C12 O1 -2.4(4) . . . . ?
C2 C3 C12 C11 177.0(2) . . . . ?
C3 C4 C5 C6 -177.5(3) . . . . ?
C3 C4 C9 C8 176.6(2) . . . . ?
C3 C4 C9 C10 -3.9(4) . . . . ?
C4 C3 C12 O1 178.8(2) . . . . ?
C4 C3 C12 C11 -1.7(4) . . . . ?
C4 C5 C6 C7 0.2(4) . . . . ?
C4 C9 C10 C11 0.7(4) . . . . ?
C5 C4 C9 C8 -2.6(4) . . . . ?
C5 C4 C9 C10 176.9(2) . . . . ?
C5 C6 C7 C8 -1.1(5) . . . . ?
C6 C7 C8 C9 0.1(5) . . . . ?
C7 C8 C9 C4 1.8(4) . . . . ?
C7 C8 C9 C10 -177.7(3) . . . . ?
C8 C9 C10 C11 -179.8(3) . . . . ?
C9 C4 C5 C6 1.6(4) . . . . ?
C9 C10 C11 C12 2.1(4) . . . . ?
C10 C11 C12 O1 177.9(2) . . . . ?
C10 C11 C12 C3 -1.6(4) . . . . ?
C12 C3 C4 C5 -176.5(2) . . . . ?
C12 C3 C4 C9 4.5(4) . . . . ?
C13 C14 C15 O3 -177.6(2) . . . . ?
C13 C14 C15 C16 2.8(4) . . . . ?
C13 C18 C19 N2 -5.6(4) . . . . ?
C13 C18 C19 C20 174.1(2) . . . . ?
C14 C13 C18 C17 -4.1(3) . . . . ?
C14 C13 C18 C19 176.1(2) . . . . ?
C14 C15 C16 C17 -3.2(4) . . . . ?
C15 O3 C27 C28 177.7(3) . . . . ?
C15 C16 C17 C18 -0.2(4) . . . . ?
C16 C17 C18 C13 3.8(4) . . . . ?
C16 C17 C18 C19 -176.4(2) . . . . ?
C17 C18 C19 N2 174.6(2) . . . . ?
C17 C18 C19 C20 -5.7(3) . . . . ?
C18 C13 C14 C15 1.0(4) . . . . ?
C18 C19 C20 C21 73.4(3) . . . . ?
C18 C19 C20 C25 -108.1(3) . . . . ?
C19 N2 C26 C1 153.0(2) . . . . ?
C19 C20 C21 C22 179.0(3) . . . . ?
C19 C20 C25 C24 -178.8(3) . . . . ?
C20 C21 C22 C23 -0.2(5) . . . . ?
C21 C20 C25 C24 -0.3(4) . . . . ?
C21 C22 C23 C24 -0.5(5) . . . . ?
C22 C23 C24 C25 0.7(5) . . . . ?
C23 C24 C25 C20 -0.3(5) . . . . ?
C25 C20 C21 C22 0.5(4) . . . . ?
C26 N2 C19 C18 -179.1(2) . . . . ?
C26 N2 C19 C20 1.2(3) . . . . ?
C27 O3 C15 C14 10.4(4) . . . . ?
C27 O3 C15 C16 -169.9(3) . . . . ?
C28 N3 C29 C30 178.1(4) . . . . ?
C28 N3 C33 C32 -176.0(4) . . . . ?
C29 N3 C28 C27 -80.0(4) . . . . ?
C29 N3 C33 C32 60.1(5) . . . . ?
C29 C30 C31 C32 -54.5(5) . . . . ?
C30 C31 C32 C33 55.2(6) . . . . ?
C31 C32 C33 N3 -58.4(6) . . . . ?
C33 N3 C28 C27 157.1(3) . . . . ?
C33 N3 C29 C30 -59.4(5) . . . . ?
Ni1A O1A C12A C3A -13.2(4) . . . . ?
Ni1A O1A C12A C11A 165.89(18) . . . . ?
Ni1A O2A C13A C14A 170.07(18) . . . . ?
Ni1A O2A C13A C18A -11.0(4) . . . . ?
Ni1A N1A C1A C26A 36.8(2) . . . . ?
Ni1A N1A C2A C3A -0.6(4) . . . . ?
Ni1A N2A C19A C18A -7.6(4) . . . . ?
Ni1A N2A C19A C20A 171.16(18) . . . . ?
Ni1A N2A C26A C1A 31.8(2) . . . . ?
O1A Ni1A O2A C13A -175.3(2) . . . . ?
O1A Ni1A N1A C1A 169.24(17) . . . . ?
O1A Ni1A N1A C2A -7.1(2) . . . . ?
O2A Ni1A O1A C12A -169.1(2) . . . . ?
O2A Ni1A N2A C19A -0.6(2) . . . . ?
O2A Ni1A N2A C26A 172.90(16) . . . . ?
O2A C13A C14A C15A 179.7(2) . . . . ?
O2A C13A C18A C17A -177.8(2) . . . . ?
O2A C13A C18A C19A 0.9(4) . . . . ?
O3A C15A C16A C17A -179.7(3) . . . . ?
O3A C27A C28A N3A -78.1(4) . . . . ?
N1A Ni1A O1A C12A 13.7(2) . . . . ?
N1A Ni1A N2A C19A 176.8(2) . . . . ?
N1A Ni1A N2A C26A -9.73(17) . . . . ?
N1A C1A C26A N2A -42.8(3) . . . . ?
N1A C2A C3A C4A -173.5(2) . . . . ?
N1A C2A C3A C12A 5.2(4) . . . . ?
N2A Ni1A O2A C13A 9.9(2) . . . . ?
N2A Ni1A N1A C1A -15.95(17) . . . . ?
N2A Ni1A N1A C2A 167.7(2) . . . . ?
N2A C19A C20A C21A 105.9(3) . . . . ?
N2A C19A C20A C25A -73.1(3) . . . . ?
N3A C29A C30A C31A -54.8(6) . . . . ?
C1A N1A C2A C3A -176.7(2) . . . . ?
C2A N1A C1A C26A -146.5(2) . . . . ?
C2A C3A C4A C5A -4.8(4) . . . . ?
C2A C3A C4A C9A 174.7(2) . . . . ?
C2A C3A C12A O1A 1.9(4) . . . . ?
C2A C3A C12A C11A -177.2(2) . . . . ?
C3A C4A C5A C6A 178.3(3) . . . . ?
C3A C4A C9A C8A -177.1(2) . . . . ?
C3A C4A C9A C10A 3.6(4) . . . . ?
C4A C3A C12A O1A -179.3(2) . . . . ?
C4A C3A C12A C11A 1.5(4) . . . . ?
C4A C5A C6A C7A -0.8(4) . . . . ?
C4A C9A C10A C11A -0.6(4) . . . . ?
C5A C4A C9A C8A 2.4(4) . . . . ?
C5A C4A C9A C10A -176.8(2) . . . . ?
C5A C6A C7A C8A 1.7(5) . . . . ?
C6A C7A C8A C9A -0.5(5) . . . . ?
C7A C8A C9A C4A -1.6(4) . . . . ?
C7A C8A C9A C10A 177.7(3) . . . . ?
C8A C9A C10A C11A -179.9(3) . . . . ?
C9A C4A C5A C6A -1.3(4) . . . . ?
C9A C10A C11A C12A -2.0(4) . . . . ?
C10A C11A C12A O1A -177.7(3) . . . . ?
C10A C11A C12A C3A 1.5(4) . . . . ?
C12A C3A C4A C5A 176.4(2) . . . . ?
C12A C3A C4A C9A -4.0(4) . . . . ?
C13A C14A C15A O3A 178.7(2) . . . . ?
C13A C14A C15A C16A -1.6(4) . . . . ?
C13A C18A C19A N2A 8.6(4) . . . . ?
C13A C18A C19A C20A -170.2(2) . . . . ?
C14A C13A C18A C17A 1.0(4) . . . . ?
C14A C13A C18A C19A 179.8(2) . . . . ?
C14A C15A C16A C17A 0.7(4) . . . . ?
C15A O3A C27A C28A 172.3(3) . . . . ?
C15A C16A C17A C18A 1.2(4) . . . . ?
C16A C17A C18A C13A -2.1(4) . . . . ?
C16A C17A C18A C19A 179.2(3) . . . . ?
C17A C18A C19A N2A -172.7(2) . . . . ?
C17A C18A C19A C20A 8.5(4) . . . . ?
C18A C13A C14A C15A 0.7(4) . . . . ?
C18A C19A C20A C21A -75.3(3) . . . . ?
C18A C19A C20A C25A 105.7(3) . . . . ?
C19A N2A C26A C1A -154.1(2) . . . . ?
C19A C20A C21A C22A -177.6(3) . . . . ?
C19A C20A C25A C24A 178.2(3) . . . . ?
C20A C21A C22A C23A -1.2(5) . . . . ?
C21A C20A C25A C24A -0.8(4) . . . . ?
C21A C22A C23A C24A 0.5(5) . . . . ?
C22A C23A C24A C25A 0.1(5) . . . . ?
C23A C24A C25A C20A 0.1(4) . . . . ?
C25A C20A C21A C22A 1.4(4) . . . . ?
C26A N2A C19A C18A 179.4(2) . . . . ?
C26A N2A C19A C20A -1.8(3) . . . . ?
C27A O3A C15A C14A -178.9(3) . . . . ?
C27A O3A C15A C16A 1.5(4) . . . . ?
C28A N3A C29A C30A -168.5(4) . . . . ?
C28A N3A C33A C32A 168.1(4) . . . . ?
C29A N3A C28A C27A -70.6(5) . . . . ?
C29A N3A C33A C32A -60.0(5) . . . . ?
C29A C30A C31A C32A 53.2(6) . . . . ?
C30A C31A C32A C33A -54.8(5) . . . . ?
C31A C32A C33A N3A 57.2(5) . . . . ?
C33A N3A C28A C27A 60.9(5) . . . . ?
C33A N3A C29A C30A 58.9(5) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.097
_oxdiff_exptl_absorpt_empirical_full_min 0.943

# start Validation Reply Form
_vrf_PLAT260_cmpd3_exp_140_tsb19_p 
;
PROBLEM: Large Average Ueq of Residue Including O3AA 0.130 Check
RESPONSE: This atom is not well-behaved but was left as is because it is the 
minor component of a disoredered solvate molecule and not central to the 
structure or model interpretation.
;
_vrf_PLAT041_cmpd4_exp_104_sp    
;
PROBLEM: Calc. and Reported SumFormula Strings Differ Please Check
RESPONSE: The difference is 0.01. Probably rounding.
;
_vrf_PLAT077_cmpd4_exp_104_sp    
;
PROBLEM: Unitcell Contains Non-integer Number of Atoms .. Please Check
RESPONSE: Includes the refinement of a partial occupancy water molecule (0.15).
;
_vrf_PLAT161_cmpd4_exp_104_sp    
;
PROBLEM: Missing or Zero s.u. (esd) on x-coordinate for O1W Check
RESPONSE: A partial occupancy water molecule (0.15) that makes a sensible 
D-A contact with a piperidinyl nitrogen atom. Free refinement of the 
occupancy of the water came close to 0.15 and it was fixed at that. 
The position of this water did not refine well with the low occupancy 
(FMLS did not converge), so its position was fixed therefore the distance 
and relationship of this interaction was not taken further.
;
_vrf_PLAT162_cmpd4_exp_104_sp    
;
PROBLEM: Missing or Zero s.u. (esd) on y-coordinate for O1W Check
RESPONSE: See response to _vrf_PLAT161_cmpd4_exp_104_sp.
;
_vrf_PLAT163_cmpd4_exp_104_sp    
;
PROBLEM: Missing or Zero s.u. (esd) on z-coordinate for O1W Check
RESPONSE: See response to _vrf_PLAT161_cmpd4_exp_104_sp.
;
_vrf_PLAT915_cmpd15_exp_132_tsb  
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage 82 %
RESPONSE: The coverage is a little low but the _refine_ls_abs_structure_Flack
gives a good result -0.012(6). More discussion about the data treatment
is given in _refine_special_details.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cmpd4_exp_104_sp
_database_code_depnum_ccdc_archive 'CCDC 1984623'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2020-02-18 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_audit_creation_date             2020-02-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
N,N'-Bis-(4'-((1-(2-ethyl)piperidine)oxy)benzophenylidene)ethylenediaminenickel(II)
_chemical_formula_moiety         'C42 H47.67 N4 Ni O4, C H Cl3, 0.15(H2 O)'
_chemical_formula_sum            'C43 H48.96 Cl3 N4 Ni O4.15'
_chemical_formula_weight         853.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C43 H49 Cl3 N4 Ni O4.15'
_chemical_oxdiff_usercomment     'TSB 19'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.9317(3)
_cell_length_b                   14.6642(6)
_cell_length_c                   14.9018(5)
_cell_angle_alpha                84.318(3)
_cell_angle_beta                 76.970(3)
_cell_angle_gamma                73.292(3)
_cell_volume                     2023.80(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12865
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.5970
_cell_measurement_theta_min      1.9750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'translucent red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             894
_exptl_crystal_recrystallization_method 'from chloroform'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38950
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         1.981
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 109.00   0.50   20.00    --   20.00  54.00  30.00  366
  2  ω    -56.00 -29.00   0.50   20.00    --   20.00  54.00 120.00   54
  3  ω     18.00  72.00   0.50   20.00    --   20.00  54.00 120.00  108
  4  ω    -71.00 110.00   0.50   20.00    --   20.00  54.00 -90.00  362
  5  ω    -41.00 -16.00   0.50   20.00    --   20.00  54.00-150.00   50
  6  ω      4.00  30.00   0.50   20.00    --   20.00  54.00-150.00   52
  7  ω     36.00  61.00   0.50   20.00    --   20.00  54.00-150.00   50
  8  ω    -73.00  32.00   0.50   20.00    --   20.00  54.00 150.00  210
  9  ω     39.00  64.00   0.50   20.00    --   20.00  54.00 150.00   50
 10  ω     85.00 110.00   0.50   20.00    --   20.00  54.00 150.00   50
 11  ω    -65.00   2.00   0.50   20.00    --   20.00  54.00  60.00  134
 12  ω      7.00  33.00   0.50   20.00    --   20.00  54.00  60.00   52
 13  ω    -73.00 -26.00   0.50   20.00    --   20.00  54.00-120.00   94
 14  ω    -61.00 -35.00   0.50   20.00    --   20.00  54.00-180.00   52
 15  ω     -8.00  17.00   0.50   20.00    --   20.00  54.00-180.00   50
 16  ω    -69.00 -42.00   0.50   20.00    --   20.00  54.00 -60.00   54
 17  ω    -63.00  67.00   0.50   20.00    --   20.00  54.00  90.00  260
 18  ω    -70.00  72.00   0.50   20.00    --   20.00  54.00 -13.07  284
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0446175000
_diffrn_orient_matrix_UB_12      -0.0166580000
_diffrn_orient_matrix_UB_13      -0.0427475000
_diffrn_orient_matrix_UB_21      -0.0562303000
_diffrn_orient_matrix_UB_22      0.0242317000
_diffrn_orient_matrix_UB_23      -0.0229533000
_diffrn_orient_matrix_UB_31      0.0256055000
_diffrn_orient_matrix_UB_32      0.0410992000
_diffrn_orient_matrix_UB_33      -0.0059955000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8551
_reflns_number_total             10295
_reflns_odcompleteness_completeness 98.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         10295
_refine_ls_number_restraints     146
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0346
_refine_ls_restrained_S_all      1.050
_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)+(0.0386P)²+0.7952P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0890
_refine_special_details          
; O1W is a partially occupancy water molecule (0.15) that makes a 
sensible D-A contact with a piperidinyl nitrogen atom. Free 
refinement of the occupancy of the water came close to 0.15 and it 
was fixed at that. The position of this water did not refine well 
with the low occupancy (FMLS did not converge), so its position 
was fixed therefore the distance and relationship of this interaction 
was not taken further.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C4DA-Cl1A = C4DA-Cl1B
 1.76 with sigma of 0.005
 N2-C1 \\sim N2-C1A
 with sigma of 0.02
 N2P-C1P \\sim N2P-C1AP
 with sigma of 0.02
 C1-C1P \\sim C1A-C1AP
 with sigma of 0.02
 C19P-N20P \\sim C19-N20
 with sigma of 0.02
 C19P-N20P \\sim C19-N20A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C22A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C1) = Uanis(C1A)
Uanis(C21) = Uanis(C25A)
Uanis(C23) = Uanis(C23A)
4. Rigid body (RIGU) restrains
 C19, N20, C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, N20A, C21A, C22A, C23A, C24A, C25A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N20P, C21P, C22P, C23P, C24P, C25P} sigma for 1-2: 0.01, 1-3: 0.02
as
{N20, C21, C22, C23, C24, C25}
{N20P, C21P, C22P, C23P, C24P, C25P} sigma for 1-2: 0.01, 1-3: 0.02
as
{N20A, C21A, C22A, C23A, C24A, C25A}
6. Others
 Sof(H4DB)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=1-FVAR(1)
 Sof(H4DA)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1AP)=Sof(H1AC)=Sof(H1AD)=1-FVAR(2)
 Sof(C1P)=Sof(H1PA)=Sof(H1PB)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(2)
 Sof(N20A)=Sof(C21A)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22E)=Sof(H22F)=
 Sof(C23A)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24E)=Sof(H24F)=Sof(C25A)=
 Sof(H25E)=Sof(H25F)=1-FVAR(3)
 Sof(H19C)=Sof(H19D)=Sof(N20)=Sof(C21)=Sof(H21C)=Sof(H21D)=Sof(C22)=Sof(H22C)=
 Sof(H22D)=Sof(C23)=Sof(H23C)=Sof(H23D)=Sof(C24)=Sof(H24C)=Sof(H24D)=Sof(C25)=
 Sof(H25C)=Sof(H25D)=FVAR(3)
 Fixed Sof: O1W(0.15) H1WA(0.15) H1WB(0.15)
 Fixed X: O1W(-0.14243)
 Fixed Y: O1W(0.89371)
 Fixed Z: O1W(0.88236)
7.a Free rotating group:
 O1W(H1WA,H1WB)
7.b Ternary CH refined with riding coordinates:
 C4DA(H4DA), C4DA(H4DB)
7.c Secondary CH2 refined with riding coordinates:
 C1P(H1PA,H1PB), C18P(H18A,H18B), C19P(H19A,H19B), C21P(H21A,H21B), C22P(H22A,
 H22B), C23P(H23A,H23B), C24P(H24A,H24B), C25P(H25A,H25B), C1(H1A,H1B),
 C18(H18C,H18D), C19(H19C,H19D), C21(H21C,H21D), C22(H22C,H22D), C23(H23C,H23D),
  C24(H24C,H24D), C25(H25C,H25D), C21A(H21E,H21F), C22A(H22E,H22F), C23A(H23E,
 H23F), C24A(H24E,H24F), C25A(H25E,H25F), C1A(H1AA,H1AB), C1AP(H1AC,H1AD)
7.d Aromatic/amide H refined with riding coordinates:
 C5P(H5P), C6P(H6P), C8P(H8P), C9P(H9P), C11P(H11P), C12P(H12P), C13P(H13P),
 C14P(H14P), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.77588(2) 0.42803(2) 0.53935(2) 0.02082(6) Uani 1 1 d . . . . .
C1P C 0.5275(2) 0.55812(15) 0.6198(2) 0.0247(5) Uani 0.897(7) 1 d D . P A 1
H1PA H 0.472243 0.584619 0.678339 0.030 Uiso 0.897(7) 1 calc R . P A 1
H1PB H 0.461459 0.558856 0.580578 0.030 Uiso 0.897(7) 1 calc R . P A 1
N2P N 0.61474(13) 0.45931(9) 0.63442(8) 0.0223(2) Uani 1 1 d D . . . .
C3P C 0.57473(15) 0.40690(10) 0.70616(10) 0.0214(3) Uani 1 1 d . . . . .
C4P C 0.44747(15) 0.45063(10) 0.77917(10) 0.0228(3) Uani 1 1 d . . . . .
C5P C 0.31017(16) 0.48298(11) 0.76134(10) 0.0241(3) Uani 1 1 d . . . . .
H5P H 0.295819 0.473797 0.703714 0.029 Uiso 1 1 calc R . . . .
C6P C 0.19357(16) 0.52871(11) 0.82724(10) 0.0244(3) Uani 1 1 d . . . . .
H6P H 0.102409 0.550243 0.813749 0.029 Uiso 1 1 calc R . . . .
C7P C 0.21450(16) 0.54194(10) 0.91345(10) 0.0244(3) Uani 1 1 d . . . . .
C8P C 0.35113(17) 0.50735(12) 0.93328(11) 0.0314(4) Uani 1 1 d . . . . .
H8P H 0.364913 0.514646 0.991565 0.038 Uiso 1 1 calc R . . . .
C9P C 0.46624(17) 0.46227(12) 0.86686(11) 0.0302(3) Uani 1 1 d . . . . .
H9P H 0.557032 0.439499 0.880762 0.036 Uiso 1 1 calc R . . . .
C10P C 0.64894(15) 0.30723(11) 0.71742(10) 0.0228(3) Uani 1 1 d . . . . .
C11P C 0.59754(18) 0.25231(12) 0.79418(11) 0.0304(3) Uani 1 1 d . . . . .
H11P H 0.517549 0.281894 0.837683 0.036 Uiso 1 1 calc R . . . .
C12P C 0.66144(19) 0.15736(12) 0.80652(12) 0.0348(4) Uani 1 1 d . . . . .
H12P H 0.625646 0.123280 0.857847 0.042 Uiso 1 1 calc R . . . .
C13P C 0.78124(18) 0.11196(12) 0.74115(11) 0.0314(3) Uani 1 1 d . . . . .
H13P H 0.826482 0.047683 0.749635 0.038 Uiso 1 1 calc R . . . .
C14P C 0.83211(17) 0.16185(11) 0.66473(11) 0.0288(3) Uani 1 1 d . . . . .
H14P H 0.910677 0.130290 0.621363 0.035 Uiso 1 1 calc R . . . .
C15P C 0.76819(16) 0.26034(10) 0.64996(10) 0.0234(3) Uani 1 1 d . . . . .
O16P O 0.82266(11) 0.30145(7) 0.57432(7) 0.0265(2) Uani 1 1 d . . . . .
O17P O 0.10945(12) 0.58720(8) 0.98301(7) 0.0295(2) Uani 1 1 d . . . . .
C18P C -0.03103(17) 0.63091(12) 0.96338(11) 0.0297(3) Uani 1 1 d . . . . .
H18A H -0.070452 0.582697 0.947697 0.036 Uiso 1 1 calc R . . . .
H18B H -0.024545 0.676047 0.911484 0.036 Uiso 1 1 calc R . . . .
C19P C -0.12720(17) 0.68158(12) 1.04792(12) 0.0323(4) Uani 1 1 d D . . . .
H19A H -0.225549 0.682572 1.048724 0.039 Uiso 1 1 calc R . . . .
H19B H -0.100441 0.645305 1.102303 0.039 Uiso 1 1 calc R . . . .
N20P N -0.12134(15) 0.77896(10) 1.05340(9) 0.0331(3) Uani 1 1 d D . . . .
C21P C 0.01804(19) 0.78322(12) 1.06772(13) 0.0383(4) Uani 1 1 d D . . . .
H21A H 0.093748 0.750722 1.018721 0.046 Uiso 1 1 calc R . . . .
H21B H 0.034917 0.750662 1.125728 0.046 Uiso 1 1 calc R . . . .
C22P C 0.0228(3) 0.88546(14) 1.06896(16) 0.0527(5) Uani 1 1 d D . . . .
H22A H 0.012319 0.916978 1.009558 0.063 Uiso 1 1 calc R . . . .
H22B H 0.114988 0.886443 1.079939 0.063 Uiso 1 1 calc R . . . .
C23P C -0.0976(3) 0.93874(15) 1.14438(15) 0.0561(6) Uani 1 1 d D . . . .
H23A H -0.080559 0.912423 1.204448 0.067 Uiso 1 1 calc R . . . .
H23B H -0.099296 1.005460 1.140900 0.067 Uiso 1 1 calc R . . . .
C24P C -0.2396(3) 0.92952(14) 1.13227(15) 0.0560(6) Uani 1 1 d D . . . .
H24A H -0.261873 0.963067 1.075701 0.067 Uiso 1 1 calc R . . . .
H24B H -0.314823 0.958669 1.183161 0.067 Uiso 1 1 calc R . . . .
C25P C -0.2357(2) 0.82598(14) 1.12865(13) 0.0427(5) Uani 1 1 d D . . . .
H25A H -0.219711 0.793374 1.186792 0.051 Uiso 1 1 calc R . . . .
H25B H -0.327610 0.821993 1.119733 0.051 Uiso 1 1 calc R . . . .
C1 C 0.6294(3) 0.61546(13) 0.57497(16) 0.0254(5) Uani 0.897(7) 1 d D . P A 1
H1A H 0.578324 0.674033 0.547148 0.030 Uiso 0.897(7) 1 calc R . P A 1
H1B H 0.674414 0.631606 0.620301 0.030 Uiso 0.897(7) 1 calc R . P A 1
N2 N 0.73928(13) 0.55638(9) 0.50363(8) 0.0227(3) Uani 1 1 d D . . . .
C3 C 0.80654(15) 0.59830(10) 0.43354(10) 0.0211(3) Uani 1 1 d . . . . .
C4 C 0.74951(15) 0.70308(10) 0.41618(10) 0.0222(3) Uani 1 1 d . . . . .
C5 C 0.61909(16) 0.73573(11) 0.38816(11) 0.0252(3) Uani 1 1 d . . . . .
H5 H 0.572676 0.691855 0.378622 0.030 Uiso 1 1 calc R . . . .
C6 C 0.55631(16) 0.83206(11) 0.37405(11) 0.0254(3) Uani 1 1 d . . . . .
H6 H 0.468081 0.852674 0.356357 0.031 Uiso 1 1 calc R . . . .
C7 C 0.62695(16) 0.89712(10) 0.38670(10) 0.0241(3) Uani 1 1 d . . . . .
C8 C 0.75893(16) 0.86529(11) 0.41351(11) 0.0270(3) Uani 1 1 d . . . . .
H8 H 0.806587 0.909110 0.421302 0.032 Uiso 1 1 calc R . . . .
C9 C 0.81975(16) 0.76889(11) 0.42867(11) 0.0256(3) Uani 1 1 d . . . . .
H9 H 0.907371 0.748271 0.447156 0.031 Uiso 1 1 calc R . . . .
C10 C 0.93011(15) 0.54512(10) 0.36864(10) 0.0212(3) Uani 1 1 d . . . . .
C11 C 0.99811(16) 0.59391(11) 0.29341(10) 0.0254(3) Uani 1 1 d . . . . .
H11 H 0.964345 0.659855 0.287737 0.030 Uiso 1 1 calc R . . . .
C12 C 1.11227(17) 0.54697(12) 0.22859(11) 0.0290(3) Uani 1 1 d . . . . .
H12 H 1.155861 0.580777 0.180206 0.035 Uiso 1 1 calc R . . . .
C13 C 1.16224(16) 0.44793(11) 0.23608(11) 0.0275(3) Uani 1 1 d . . . . .
H13 H 1.238878 0.415507 0.192021 0.033 Uiso 1 1 calc R . . . .
C14 C 1.09884(16) 0.39783(11) 0.30830(11) 0.0267(3) Uani 1 1 d . . . . .
H14 H 1.133238 0.331803 0.311932 0.032 Uiso 1 1 calc R . . . .
C15 C 0.98239(15) 0.44458(10) 0.37718(10) 0.0222(3) Uani 1 1 d . . . . .
O16 O 0.93026(12) 0.39115(7) 0.44385(7) 0.0277(2) Uani 1 1 d . . . . .
O17 O 0.57687(12) 0.99330(7) 0.37359(8) 0.0300(2) Uani 1 1 d . . . . .
C18 C 0.43416(17) 1.02986(11) 0.35724(13) 0.0335(4) Uani 1 1 d . . . . .
H18C H 0.364496 1.020074 0.411819 0.040 Uiso 1 1 calc R . . . .
H18D H 0.422910 0.997702 0.306692 0.040 Uiso 1 1 calc R . . . .
C19 C 0.4120(2) 1.13475(12) 0.33367(13) 0.0374(4) Uani 1 1 d D U . . .
H19C H 0.310053 1.166557 0.341998 0.045 Uiso 0.834(5) 1 calc R . P B 1
H19D H 0.451880 1.162697 0.374233 0.045 Uiso 0.834(5) 1 calc R . P B 1
N20 N 0.4842(2) 1.14766(15) 0.23613(13) 0.0314(5) Uani 0.834(5) 1 d D U P B 1
C21 C 0.3874(6) 1.1529(5) 0.1749(3) 0.0555(6) Uani 0.834(5) 1 d D U P B 1
H21C H 0.305558 1.208372 0.188344 0.067 Uiso 0.834(5) 1 calc R . P B 1
H21D H 0.352201 1.096741 0.184979 0.067 Uiso 0.834(5) 1 calc R . P B 1
C22 C 0.4643(4) 1.1595(2) 0.07467(19) 0.0781(12) Uani 0.834(5) 1 d D U P B 1
H22C H 0.540579 1.101405 0.059702 0.094 Uiso 0.834(5) 1 calc R . P B 1
H22D H 0.396976 1.166196 0.034739 0.094 Uiso 0.834(5) 1 calc R . P B 1
C23 C 0.5274(5) 1.2443(2) 0.0579(2) 0.0822(12) Uani 0.834(5) 1 d D U P B 1
H23C H 0.584429 1.243645 -0.004281 0.099 Uiso 0.834(5) 1 calc R . P B 1
H23D H 0.450464 1.303127 0.064197 0.099 Uiso 0.834(5) 1 calc R . P B 1
C24 C 0.6209(4) 1.2398(3) 0.1267(2) 0.0631(11) Uani 0.834(5) 1 d D U P B 1
H24C H 0.704742 1.185434 0.114867 0.076 Uiso 0.834(5) 1 calc R . P B 1
H24D H 0.653591 1.296947 0.119504 0.076 Uiso 0.834(5) 1 calc R . P B 1
C25 C 0.5385(3) 1.23134(18) 0.22379(15) 0.0390(6) Uani 0.834(5) 1 d D U P B 1
H25C H 0.600727 1.226709 0.266680 0.047 Uiso 0.834(5) 1 calc R . P B 1
H25D H 0.458675 1.287989 0.237115 0.047 Uiso 0.834(5) 1 calc R . P B 1
N20A N 0.4347(11) 1.1883(8) 0.2523(6) 0.041(2) Uani 0.166(5) 1 d D U P B 2
C21A C 0.5900(12) 1.1733(10) 0.2318(7) 0.045(3) Uani 0.166(5) 1 d D U P B 2
H21E H 0.637474 1.106257 0.222188 0.054 Uiso 0.166(5) 1 calc R . P B 2
H21F H 0.618773 1.191693 0.283825 0.054 Uiso 0.166(5) 1 calc R . P B 2
C22A C 0.636(2) 1.231(2) 0.1467(12) 0.095(7) Uani 0.166(5) 1 d D U P B 2
H22E H 0.606125 1.297982 0.161164 0.114 Uiso 0.166(5) 1 calc R . P B 2
H22F H 0.740293 1.212149 0.128917 0.114 Uiso 0.166(5) 1 calc R . P B 2
C23A C 0.5745(19) 1.2189(14) 0.0666(9) 0.0822(12) Uani 0.166(5) 1 d D U P B 2
H23E H 0.586861 1.268864 0.020373 0.099 Uiso 0.166(5) 1 calc R . P B 2
H23F H 0.628729 1.158420 0.039260 0.099 Uiso 0.166(5) 1 calc R . P B 2
C24A C 0.4186(18) 1.2216(14) 0.0912(9) 0.083(4) Uani 0.166(5) 1 d D U P B 2
H24E H 0.392113 1.199724 0.039989 0.099 Uiso 0.166(5) 1 calc R . P B 2
H24F H 0.360845 1.286602 0.102531 0.099 Uiso 0.166(5) 1 calc R . P B 2
C25A C 0.388(3) 1.159(2) 0.1762(11) 0.0555(6) Uani 0.166(5) 1 d D U P B 2
H25E H 0.285995 1.164372 0.193138 0.067 Uiso 0.166(5) 1 calc R . P B 2
H25F H 0.438700 1.092991 0.163211 0.067 Uiso 0.166(5) 1 calc R . P B 2
C1A C 0.5893(19) 0.6098(13) 0.5545(12) 0.0254(5) Uani 0.103(7) 1 d D . P A 2
H1AA H 0.585300 0.675831 0.560440 0.030 Uiso 0.103(7) 1 calc R . P A 2
H1AB H 0.518232 0.608241 0.519866 0.030 Uiso 0.103(7) 1 calc R . P A 2
C1AP C 0.557(3) 0.5638(11) 0.6477(14) 0.038(6) Uani 0.103(7) 1 d D . P A 2
H1AC H 0.603571 0.583952 0.689896 0.046 Uiso 0.103(7) 1 calc R . P A 2
H1AD H 0.454433 0.580492 0.672301 0.046 Uiso 0.103(7) 1 calc R . P A 2
C4DA C 0.10815(18) 0.80891(12) 0.60629(13) 0.0360(4) Uani 1 1 d D . . . .
H4DA H 0.101868 0.752564 0.578941 0.043 Uiso 0.428(18) 1 calc R . P C 1
H4DB H 0.110344 0.758870 0.566558 0.043 Uiso 0.572(18) 1 calc R . P C 2
Cl1A Cl -0.0390(4) 0.9070(2) 0.5881(3) 0.0418(10) Uani 0.428(18) 1 d D . P C 1
Cl2A Cl 0.0814(6) 0.7898(4) 0.7282(4) 0.0581(9) Uani 0.428(18) 1 d . . P C 1
Cl3A Cl 0.2738(5) 0.8278(5) 0.5603(3) 0.0520(10) Uani 0.428(18) 1 d . . P C 1
Cl1B Cl -0.0379(4) 0.9039(3) 0.5972(4) 0.0881(14) Uani 0.572(18) 1 d D . P C 2
Cl2B Cl 0.1111(9) 0.7607(7) 0.7169(5) 0.0819(15) Uani 0.572(18) 1 d . . P C 2
Cl3B Cl 0.2610(6) 0.8504(6) 0.5638(3) 0.0770(11) Uani 0.572(18) 1 d . . P C 2
O1W O -0.142430 0.893710 0.882360 0.104(5) Uani 0.15 1 d . U P . .
H1WA H -0.232398 0.914229 0.885528 0.155 Uiso 0.15 1 d G . P . .
H1WB H -0.134322 0.863544 0.933423 0.155 Uiso 0.15 1 d G . P . .


_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 N2P 1.8609(12) . ?
Ni1 O16P 1.8315(10) . ?
Ni1 N2 1.8583(12) . ?
Ni1 O16 1.8332(10) . ?
C1P H1PA 0.9700 . ?
C1P H1PB 0.9700 . ?
C1P N2P 1.483(2) . ?
C1P C1 1.500(3) . ?
N2P C3P 1.3088(19) . ?
N2P C1AP 1.490(16) . ?
C3P C4P 1.4981(19) . ?
C3P C10P 1.447(2) . ?
C4P C5P 1.386(2) . ?
C4P C9P 1.394(2) . ?
C5P H5P 0.9300 . ?
C5P C6P 1.388(2) . ?
C6P H6P 0.9300 . ?
C6P C7P 1.387(2) . ?
C7P C8P 1.393(2) . ?
C7P O17P 1.3616(17) . ?
C8P H8P 0.9300 . ?
C8P C9P 1.381(2) . ?
C9P H9P 0.9300 . ?
C10P C11P 1.417(2) . ?
C10P C15P 1.421(2) . ?
C11P H11P 0.9300 . ?
C11P C12P 1.367(2) . ?
C12P H12P 0.9300 . ?
C12P C13P 1.399(2) . ?
C13P H13P 0.9300 . ?
C13P C14P 1.370(2) . ?
C14P H14P 0.9300 . ?
C14P C15P 1.418(2) . ?
C15P O16P 1.3056(18) . ?
O17P C18P 1.4407(19) . ?
C18P H18A 0.9700 . ?
C18P H18B 0.9700 . ?
C18P C19P 1.512(2) . ?
C19P H19A 0.9700 . ?
C19P H19B 0.9700 . ?
C19P N20P 1.457(2) . ?
N20P C21P 1.467(2) . ?
N20P C25P 1.467(2) . ?
C21P H21A 0.9700 . ?
C21P H21B 0.9700 . ?
C21P C22P 1.516(2) . ?
C22P H22A 0.9700 . ?
C22P H22B 0.9700 . ?
C22P C23P 1.528(3) . ?
C23P H23A 0.9700 . ?
C23P H23B 0.9700 . ?
C23P C24P 1.507(3) . ?
C24P H24A 0.9700 . ?
C24P H24B 0.9700 . ?
C24P C25P 1.514(3) . ?
C25P H25A 0.9700 . ?
C25P H25B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 N2 1.479(2) . ?
N2 C3 1.3075(19) . ?
N2 C1A 1.531(14) . ?
C3 C4 1.4952(19) . ?
C3 C10 1.4537(19) . ?
C4 C5 1.389(2) . ?
C4 C9 1.391(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.386(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.385(2) . ?
C7 C8 1.394(2) . ?
C7 O17 1.3641(17) . ?
C8 H8 0.9300 . ?
C8 C9 1.386(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.415(2) . ?
C10 C15 1.418(2) . ?
C11 H11 0.9300 . ?
C11 C12 1.372(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.395(2) . ?
C13 H13 0.9300 . ?
C13 C14 1.378(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.418(2) . ?
C15 O16 1.3100(18) . ?
O17 C18 1.4313(19) . ?
C18 H18C 0.9700 . ?
C18 H18D 0.9700 . ?
C18 C19 1.507(2) . ?
C19 H19C 0.9700 . ?
C19 H19D 0.9700 . ?
C19 N20 1.489(3) . ?
C19 N20A 1.389(8) . ?
N20 C21 1.450(4) . ?
N20 C25 1.456(3) . ?
C21 H21C 0.9700 . ?
C21 H21D 0.9700 . ?
C21 C22 1.524(5) . ?
C22 H22C 0.9700 . ?
C22 H22D 0.9700 . ?
C22 C23 1.523(5) . ?
C23 H23C 0.9700 . ?
C23 H23D 0.9700 . ?
C23 C24 1.516(5) . ?
C24 H24C 0.9700 . ?
C24 H24D 0.9700 . ?
C24 C25 1.505(4) . ?
C25 H25C 0.9700 . ?
C25 H25D 0.9700 . ?
N20A C21A 1.458(8) . ?
N20A C25A 1.460(9) . ?
C21A H21E 0.9700 . ?
C21A H21F 0.9700 . ?
C21A C22A 1.513(9) . ?
C22A H22E 0.9700 . ?
C22A H22F 0.9700 . ?
C22A C23A 1.506(9) . ?
C23A H23E 0.9700 . ?
C23A H23F 0.9700 . ?
C23A C24A 1.498(9) . ?
C24A H24E 0.9700 . ?
C24A H24F 0.9700 . ?
C24A C25A 1.515(9) . ?
C25A H25E 0.9700 . ?
C25A H25F 0.9700 . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
C1A C1AP 1.491(17) . ?
C1AP H1AC 0.9700 . ?
C1AP H1AD 0.9700 . ?
C4DA H4DA 0.9800 . ?
C4DA H4DB 0.9800 . ?
C4DA Cl1A 1.780(3) . ?
C4DA Cl2A 1.782(6) . ?
C4DA Cl3A 1.724(5) . ?
C4DA Cl1B 1.718(3) . ?
C4DA Cl2B 1.731(5) . ?
C4DA Cl3B 1.760(5) . ?
O1W H1WA 0.8487 . ?
O1W H1WB 0.8495 . ?

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
O16P Ni1 N2P 93.66(5) . . ?
O16P Ni1 N2 176.71(5) . . ?
O16P Ni1 O16 84.04(5) . . ?
N2 Ni1 N2P 88.46(5) . . ?
O16 Ni1 N2P 176.33(5) . . ?
O16 Ni1 N2 93.97(5) . . ?
H1PA C1P H1PB 108.5 . . ?
N2P C1P H1PA 110.2 . . ?
N2P C1P H1PB 110.2 . . ?
N2P C1P C1 107.43(17) . . ?
C1 C1P H1PA 110.2 . . ?
C1 C1P H1PB 110.2 . . ?
C1P N2P Ni1 110.30(13) . . ?
C3P N2P Ni1 128.84(10) . . ?
C3P N2P C1P 120.86(15) . . ?
C3P N2P C1AP 114.1(8) . . ?
C1AP N2P Ni1 113.1(10) . . ?
N2P C3P C4P 119.37(13) . . ?
N2P C3P C10P 122.18(13) . . ?
C10P C3P C4P 118.45(13) . . ?
C5P C4P C3P 121.67(13) . . ?
C5P C4P C9P 118.36(13) . . ?
C9P C4P C3P 119.95(13) . . ?
C4P C5P H5P 119.1 . . ?
C4P C5P C6P 121.72(14) . . ?
C6P C5P H5P 119.1 . . ?
C5P C6P H6P 120.4 . . ?
C7P C6P C5P 119.26(14) . . ?
C7P C6P H6P 120.4 . . ?
C6P C7P C8P 119.67(13) . . ?
O17P C7P C6P 124.72(14) . . ?
O17P C7P C8P 115.61(13) . . ?
C7P C8P H8P 119.8 . . ?
C9P C8P C7P 120.37(15) . . ?
C9P C8P H8P 119.8 . . ?
C4P C9P H9P 119.7 . . ?
C8P C9P C4P 120.57(14) . . ?
C8P C9P H9P 119.7 . . ?
C11P C10P C3P 120.09(13) . . ?
C11P C10P C15P 118.17(13) . . ?
C15P C10P C3P 121.61(13) . . ?
C10P C11P H11P 118.8 . . ?
C12P C11P C10P 122.30(15) . . ?
C12P C11P H11P 118.8 . . ?
C11P C12P H12P 120.3 . . ?
C11P C12P C13P 119.33(15) . . ?
C13P C12P H12P 120.3 . . ?
C12P C13P H13P 119.9 . . ?
C14P C13P C12P 120.24(15) . . ?
C14P C13P H13P 119.9 . . ?
C13P C14P H14P 119.1 . . ?
C13P C14P C15P 121.76(14) . . ?
C15P C14P H14P 119.1 . . ?
C14P C15P C10P 118.15(14) . . ?
O16P C15P C10P 124.51(13) . . ?
O16P C15P C14P 117.34(13) . . ?
C15P O16P Ni1 128.22(9) . . ?
C7P O17P C18P 117.59(12) . . ?
O17P C18P H18A 110.0 . . ?
O17P C18P H18B 110.0 . . ?
O17P C18P C19P 108.51(13) . . ?
H18A C18P H18B 108.4 . . ?
C19P C18P H18A 110.0 . . ?
C19P C18P H18B 110.0 . . ?
C18P C19P H19A 108.6 . . ?
C18P C19P H19B 108.6 . . ?
H19A C19P H19B 107.6 . . ?
N20P C19P C18P 114.45(13) . . ?
N20P C19P H19A 108.6 . . ?
N20P C19P H19B 108.6 . . ?
C19P N20P C21P 112.44(13) . . ?
C19P N20P C25P 109.49(14) . . ?
C21P N20P C25P 109.54(15) . . ?
N20P C21P H21A 109.4 . . ?
N20P C21P H21B 109.4 . . ?
N20P C21P C22P 111.10(16) . . ?
H21A C21P H21B 108.0 . . ?
C22P C21P H21A 109.4 . . ?
C22P C21P H21B 109.4 . . ?
C21P C22P H22A 109.6 . . ?
C21P C22P H22B 109.6 . . ?
C21P C22P C23P 110.38(17) . . ?
H22A C22P H22B 108.1 . . ?
C23P C22P H22A 109.6 . . ?
C23P C22P H22B 109.6 . . ?
C22P C23P H23A 109.8 . . ?
C22P C23P H23B 109.8 . . ?
H23A C23P H23B 108.2 . . ?
C24P C23P C22P 109.54(19) . . ?
C24P C23P H23A 109.8 . . ?
C24P C23P H23B 109.8 . . ?
C23P C24P H24A 109.4 . . ?
C23P C24P H24B 109.4 . . ?
C23P C24P C25P 111.02(17) . . ?
H24A C24P H24B 108.0 . . ?
C25P C24P H24A 109.4 . . ?
C25P C24P H24B 109.4 . . ?
N20P C25P C24P 111.02(16) . . ?
N20P C25P H25A 109.4 . . ?
N20P C25P H25B 109.4 . . ?
C24P C25P H25A 109.4 . . ?
C24P C25P H25B 109.4 . . ?
H25A C25P H25B 108.0 . . ?
C1P C1 H1A 110.3 . . ?
C1P C1 H1B 110.3 . . ?
H1A C1 H1B 108.5 . . ?
N2 C1 C1P 107.31(19) . . ?
N2 C1 H1A 110.3 . . ?
N2 C1 H1B 110.3 . . ?
C1 N2 Ni1 110.82(10) . . ?
C3 N2 Ni1 129.51(10) . . ?
C3 N2 C1 119.12(13) . . ?
C3 N2 C1A 119.6(7) . . ?
C1A N2 Ni1 109.3(7) . . ?
N2 C3 C4 119.11(12) . . ?
N2 C3 C10 121.91(13) . . ?
C10 C3 C4 118.87(13) . . ?
C5 C4 C3 118.17(13) . . ?
C5 C4 C9 118.90(13) . . ?
C9 C4 C3 122.91(13) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.70(14) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 H6 120.5 . . ?
C7 C6 C5 119.01(14) . . ?
C7 C6 H6 120.5 . . ?
C6 C7 C8 119.92(14) . . ?
O17 C7 C6 124.27(14) . . ?
O17 C7 C8 115.81(14) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.58(14) . . ?
C9 C8 H8 119.7 . . ?
C4 C9 H9 120.1 . . ?
C8 C9 C4 119.88(14) . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C3 119.62(13) . . ?
C11 C10 C15 118.75(13) . . ?
C15 C10 C3 121.61(13) . . ?
C10 C11 H11 119.0 . . ?
C12 C11 C10 122.05(14) . . ?
C12 C11 H11 119.0 . . ?
C11 C12 H12 120.4 . . ?
C11 C12 C13 119.24(15) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.46(14) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.2 . . ?
C13 C14 C15 121.53(14) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 C10 117.95(14) . . ?
O16 C15 C10 124.85(13) . . ?
O16 C15 C14 117.20(13) . . ?
C15 O16 Ni1 128.11(9) . . ?
C7 O17 C18 117.54(12) . . ?
O17 C18 H18C 110.3 . . ?
O17 C18 H18D 110.3 . . ?
O17 C18 C19 106.99(14) . . ?
H18C C18 H18D 108.6 . . ?
C19 C18 H18C 110.3 . . ?
C19 C18 H18D 110.3 . . ?
C18 C19 H19C 109.8 . . ?
C18 C19 H19D 109.8 . . ?
H19C C19 H19D 108.3 . . ?
N20 C19 C18 109.16(16) . . ?
N20 C19 H19C 109.8 . . ?
N20 C19 H19D 109.8 . . ?
N20A C19 C18 134.4(5) . . ?
C21 N20 C19 110.4(2) . . ?
C21 N20 C25 111.3(3) . . ?
C25 N20 C19 111.16(18) . . ?
N20 C21 H21C 109.6 . . ?
N20 C21 H21D 109.6 . . ?
N20 C21 C22 110.5(3) . . ?
H21C C21 H21D 108.1 . . ?
C22 C21 H21C 109.6 . . ?
C22 C21 H21D 109.6 . . ?
C21 C22 H22C 109.5 . . ?
C21 C22 H22D 109.5 . . ?
H22C C22 H22D 108.1 . . ?
C23 C22 C21 110.8(3) . . ?
C23 C22 H22C 109.5 . . ?
C23 C22 H22D 109.5 . . ?
C22 C23 H23C 109.7 . . ?
C22 C23 H23D 109.7 . . ?
H23C C23 H23D 108.2 . . ?
C24 C23 C22 109.9(3) . . ?
C24 C23 H23C 109.7 . . ?
C24 C23 H23D 109.7 . . ?
C23 C24 H24C 109.5 . . ?
C23 C24 H24D 109.5 . . ?
H24C C24 H24D 108.1 . . ?
C25 C24 C23 110.7(3) . . ?
C25 C24 H24C 109.5 . . ?
C25 C24 H24D 109.5 . . ?
N20 C25 C24 110.9(2) . . ?
N20 C25 H25C 109.5 . . ?
N20 C25 H25D 109.5 . . ?
C24 C25 H25C 109.5 . . ?
C24 C25 H25D 109.5 . . ?
H25C C25 H25D 108.1 . . ?
C19 N20A C21A 102.7(8) . . ?
C19 N20A C25A 114.3(9) . . ?
C21A N20A C25A 110.9(11) . . ?
N20A C21A H21E 109.5 . . ?
N20A C21A H21F 109.5 . . ?
N20A C21A C22A 110.9(10) . . ?
H21E C21A H21F 108.1 . . ?
C22A C21A H21E 109.5 . . ?
C22A C21A H21F 109.5 . . ?
C21A C22A H22E 109.0 . . ?
C21A C22A H22F 109.0 . . ?
H22E C22A H22F 107.8 . . ?
C23A C22A C21A 112.7(10) . . ?
C23A C22A H22E 109.0 . . ?
C23A C22A H22F 109.0 . . ?
C22A C23A H23E 108.6 . . ?
C22A C23A H23F 108.6 . . ?
H23E C23A H23F 107.6 . . ?
C24A C23A C22A 114.5(10) . . ?
C24A C23A H23E 108.6 . . ?
C24A C23A H23F 108.6 . . ?
C23A C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
C23A C24A C25A 110.8(10) . . ?
H24E C24A H24F 108.1 . . ?
C25A C24A H24E 109.5 . . ?
C25A C24A H24F 109.5 . . ?
N20A C25A C24A 109.8(11) . . ?
N20A C25A H25E 109.7 . . ?
N20A C25A H25F 109.7 . . ?
C24A C25A H25E 109.7 . . ?
C24A C25A H25F 109.7 . . ?
H25E C25A H25F 108.2 . . ?
N2 C1A H1AA 109.8 . . ?
N2 C1A H1AB 109.8 . . ?
H1AA C1A H1AB 108.3 . . ?
C1AP C1A N2 109.3(16) . . ?
C1AP C1A H1AA 109.8 . . ?
C1AP C1A H1AB 109.8 . . ?
N2P C1AP C1A 105.7(14) . . ?
N2P C1AP H1AC 110.6 . . ?
N2P C1AP H1AD 110.6 . . ?
C1A C1AP H1AC 110.6 . . ?
C1A C1AP H1AD 110.6 . . ?
H1AC C1AP H1AD 108.7 . . ?
Cl1A C4DA H4DA 108.8 . . ?
Cl1A C4DA Cl2A 104.9(2) . . ?
Cl2A C4DA H4DA 108.8 . . ?
Cl3A C4DA H4DA 108.8 . . ?
Cl3A C4DA Cl1A 113.8(3) . . ?
Cl3A C4DA Cl2A 111.6(3) . . ?
Cl1B C4DA H4DB 108.6 . . ?
Cl1B C4DA Cl2B 114.8(3) . . ?
Cl1B C4DA Cl3B 106.3(3) . . ?
Cl2B C4DA H4DB 108.6 . . ?
Cl2B C4DA Cl3B 109.7(2) . . ?
Cl3B C4DA H4DB 108.6 . . ?
H1WA O1W H1WB 104.5 . . ?

_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.124
_oxdiff_exptl_absorpt_empirical_full_min 0.895
