# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_eb17019
_database_code_depnum_ccdc_archive 'CCDC 1847956'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2021-06-23 deposited with the CCDC.	2021-07-02 downloaded from the CCDC.
;
_audit_creation_date             2021-06-23
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C60 H60 Cl2 Co5 N10 O12 V2, 2(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C62 H68 Cl4 Co5 N10 O22 V2'
_chemical_formula_weight         1843.59
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Co Cl V'
_chemical_oxdiff_usercomment     '@ 120 K 808o'
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'
Co Co 0.3494 0.9721 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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                   15.7439(9)
_cell_length_b                   12.4867(5)
_cell_length_c                   18.9773(12)
_cell_angle_alpha                90
_cell_angle_beta                 106.591(6)
_cell_angle_gamma                90
_cell_volume                     3575.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7290
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.7330
_cell_measurement_theta_min      3.2540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0794 before and 0.0604 after correction. The Ratio of minimum to maximum transmission is 0.8091. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1870
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -1 -2 0.0708
5 1 2 0.0708
5 -1 1 0.0859
-3 5 1 0.1984
1 -5 -2 0.2572
-2 0 5 0.0311
2 0 -5 0.0311
-1 0 1 0.0455
1 0 -1 0.0455

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.062
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.9988 -1.0002 -2.0033 0.1419 -0.2300 0.0439
4.9988 1.0002 2.0033 -0.1419 0.2300 -0.0439
5.0003 -0.9997 1.0028 -0.1098 0.1775 -0.1471
-3.0028 4.9997 0.9990 -0.0147 -0.0122 0.3140
1.0034 -4.9997 -2.0005 0.0584 -0.0834 -0.2766
-2.0056 -0.0010 5.0025 0.1437 0.1158 0.0494
2.0056 0.0010 -5.0025 -0.1437 -0.1158 -0.0494
-1.0013 -0.0003 1.0002 0.0468 0.0050 0.0217
1.0013 0.0003 -1.0002 -0.0468 -0.0050 -0.0217

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34729
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.079
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  33.00   1.00   20.00    --   -7.39 -99.00  60.00   53
  2  ω    -20.00  33.00   1.00   20.00    --   -7.39 -99.00 120.00   53
  3  ω    -28.00  87.00   1.00   20.00    --    8.80  19.00   0.00  115
  4  ω    -19.00  25.00   1.00   20.00    --    8.80  19.00-150.00   44
  5  ω    -60.00  31.00   1.00   20.00    --    8.80 -57.00-180.00   91
  6  ω     24.00  49.00   1.00   20.00    --    8.80 -99.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0301715000
_diffrn_orient_matrix_UB_12      -0.0243918000
_diffrn_orient_matrix_UB_13      0.0166203000
_diffrn_orient_matrix_UB_21      0.0301563000
_diffrn_orient_matrix_UB_22      0.0086393000
_diffrn_orient_matrix_UB_23      0.0352342000
_diffrn_orient_matrix_UB_31      -0.0196977000
_diffrn_orient_matrix_UB_32      0.0505705000
_diffrn_orient_matrix_UB_33      0.0019878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4998
_reflns_number_total             6772
_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 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6772
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0610
_refine_ls_restrained_S_all      1.047
_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)+(0.0586P)²+9.8593P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1475
_refine_special_details          
;
The O-bound H atom was identified from a difference Fourier map and refined with appropriate restraints


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
910_ALERT_3_B Missing # of FCF Reflection(s) Below Theta(Min)          11 Note

Not significant.

#===============================================================================
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00872 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......     16.692 Check
906_ALERT_3_C Large K value in the Analysis of Variance ......      3.374 Check
978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Note

Not significant.


#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          2 Note
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       9.86 Why ?
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co1    --  Cl1_a   ..       11.1 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co3    --  Cl1     ..        5.4 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co3    --  N5      ..        8.0 s.u.
244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl2 Check
860_ALERT_3_G Number of Least-Squares Restraints .............          1 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600       1033 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          1 Note

Not significant.

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O11-H11
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_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
Co1 Co 0.63621(4) 0.68254(5) 0.49444(4) 0.02824(19) Uani 1 1 d . . . . .
Co2 Co 0.500000 0.500000 0.500000 0.0228(2) Uani 1 2 d S . P . .
Co3 Co 0.35621(4) 0.43753(5) 0.35048(4) 0.02749(19) Uani 1 1 d . . . . .
V1 V 0.50357(6) 0.61381(6) 0.34578(5) 0.0296(2) Uani 1 1 d . . . . .
Cl1 Cl 0.35583(9) 0.24981(10) 0.38237(8) 0.0377(3) Uani 1 1 d . . . . .
O1 O 0.6310(2) 0.6108(3) 0.39849(19) 0.0315(8) Uani 1 1 d . . . . .
O2 O 0.4975(2) 0.6559(2) 0.44893(18) 0.0251(7) Uani 1 1 d . . . . .
O3 O 0.3650(2) 0.4709(2) 0.45964(17) 0.0243(7) Uani 1 1 d . . . . .
O4 O 0.4960(2) 0.4552(2) 0.39160(18) 0.0256(7) Uani 1 1 d . . . . .
O5 O 0.3718(2) 0.5889(3) 0.31788(18) 0.0306(8) Uani 1 1 d . . . . .
O6 O 0.4987(3) 0.7219(3) 0.2976(2) 0.0447(10) Uani 1 1 d . . . . .
N1 N 0.7696(3) 0.6940(4) 0.4952(3) 0.0383(11) Uani 1 1 d . . . . .
N2 N 0.5890(3) 0.8365(3) 0.4533(2) 0.0343(11) Uani 1 1 d . . . . .
N3 N 0.2207(3) 0.4638(3) 0.3440(2) 0.0318(10) Uani 1 1 d . . . . .
N4 N 0.5304(3) 0.5086(3) 0.2681(2) 0.0352(10) Uani 1 1 d . . . . .
N5 N 0.3328(3) 0.4133(3) 0.2367(3) 0.0367(11) Uani 1 1 d . . . . .
C1 C 0.8409(4) 0.7239(5) 0.5511(4) 0.0472(15) Uani 1 1 d . . . . .
H1 H 0.831110 0.751149 0.594853 0.057 Uiso 1 1 calc R U . . .
C2 C 0.9258(4) 0.7168(6) 0.5473(4) 0.0587(19) Uani 1 1 d . . . . .
H2 H 0.973913 0.739370 0.587305 0.070 Uiso 1 1 calc R U . . .
C3 C 0.9402(4) 0.6770(7) 0.4857(4) 0.069(2) Uani 1 1 d . . . . .
H3 H 0.998962 0.670772 0.482190 0.083 Uiso 1 1 calc R U . . .
C4 C 0.8692(4) 0.6453(6) 0.4275(4) 0.0572(18) Uani 1 1 d . . . . .
H4 H 0.878402 0.617123 0.383797 0.069 Uiso 1 1 calc R U . . .
C5 C 0.7847(4) 0.6557(5) 0.4346(3) 0.0421(14) Uani 1 1 d . . . . .
C6 C 0.7047(4) 0.6234(5) 0.3722(3) 0.0479(15) Uani 1 1 d . . . . .
H6A H 0.692312 0.679071 0.333475 0.058 Uiso 1 1 calc R U . . .
H6B H 0.717082 0.555297 0.350304 0.058 Uiso 1 1 calc R U . . .
C7 C 0.6373(4) 0.9191(4) 0.4403(3) 0.0392(13) Uani 1 1 d . . . . .
H7 H 0.699488 0.910322 0.450082 0.047 Uiso 1 1 calc R U . . .
C8 C 0.5999(4) 1.0165(4) 0.4131(3) 0.0438(15) Uani 1 1 d . . . . .
H8 H 0.635473 1.073588 0.404377 0.053 Uiso 1 1 calc R U . . .
C9 C 0.5103(4) 1.0279(4) 0.3993(3) 0.0458(15) Uani 1 1 d . . . . .
H9 H 0.483071 1.094313 0.381583 0.055 Uiso 1 1 calc R U . . .
C10 C 0.4597(4) 0.9449(4) 0.4109(3) 0.0373(13) Uani 1 1 d . . . . .
H10 H 0.397302 0.952277 0.400481 0.045 Uiso 1 1 calc R U . . .
C11 C 0.5016(4) 0.8483(4) 0.4383(3) 0.0316(12) Uani 1 1 d . . . . .
C12 C 0.4502(3) 0.7517(4) 0.4531(3) 0.0318(12) Uani 1 1 d . . . . .
H12A H 0.441371 0.758030 0.502532 0.038 Uiso 1 1 calc R U . . .
H12B H 0.391134 0.749295 0.416386 0.038 Uiso 1 1 calc R U . . .
C13 C 0.1472(4) 0.4362(5) 0.2899(3) 0.0440(15) Uani 1 1 d . . . . .
H13 H 0.153820 0.396056 0.249230 0.053 Uiso 1 1 calc R U . . .
C14 C 0.0639(4) 0.4641(6) 0.2917(4) 0.0580(19) Uani 1 1 d . . . . .
H14 H 0.013407 0.444085 0.252909 0.070 Uiso 1 1 calc R U . . .
C15 C 0.0548(4) 0.5214(6) 0.3504(4) 0.066(2) Uani 1 1 d . . . . .
H15 H -0.002317 0.543829 0.351767 0.079 Uiso 1 1 calc R U . . .
C16 C 0.1285(4) 0.5468(5) 0.4077(4) 0.0482(16) Uani 1 1 d . . . . .
H16 H 0.122839 0.584249 0.449751 0.058 Uiso 1 1 calc R U . . .
C17 C 0.2110(3) 0.5160(4) 0.4021(3) 0.0328(12) Uani 1 1 d . . . . .
C18 C 0.2952(3) 0.5424(4) 0.4628(3) 0.0299(11) Uani 1 1 d . . . . .
H18A H 0.313185 0.617105 0.457012 0.036 Uiso 1 1 calc R U . . .
H18B H 0.283688 0.536125 0.511241 0.036 Uiso 1 1 calc R U . . .
C19 C 0.5336(4) 0.5391(6) 0.2011(3) 0.0526(16) Uani 1 1 d . . . . .
H19 H 0.520794 0.611584 0.186738 0.063 Uiso 1 1 calc R U . . .
C20 C 0.5546(6) 0.4703(7) 0.1530(4) 0.076(2) Uani 1 1 d . . . . .
H20 H 0.555434 0.493424 0.105558 0.091 Uiso 1 1 calc R U . . .
C21 C 0.5745(6) 0.3661(7) 0.1755(5) 0.080(2) Uani 1 1 d . . . . .
H21 H 0.589910 0.316713 0.143129 0.096 Uiso 1 1 calc R U . . .
C22 C 0.5724(5) 0.3323(6) 0.2439(4) 0.0554(17) Uani 1 1 d . . . . .
H22 H 0.585281 0.260128 0.258931 0.066 Uiso 1 1 calc R U . . .
C23 C 0.5509(3) 0.4069(4) 0.2905(3) 0.0351(13) Uani 1 1 d . . . . .
C24 C 0.5489(3) 0.3799(4) 0.3666(3) 0.0308(12) Uani 1 1 d . . . . .
H24A H 0.524250 0.307105 0.367182 0.037 Uiso 1 1 calc R U . . .
H24B H 0.609966 0.380477 0.400095 0.037 Uiso 1 1 calc R U . . .
C25 C 0.3307(4) 0.3234(4) 0.1976(3) 0.0401(14) Uani 1 1 d . . . . .
H25 H 0.343786 0.257532 0.223422 0.048 Uiso 1 1 calc R U . . .
C26 C 0.3109(4) 0.3213(5) 0.1227(3) 0.0479(15) Uani 1 1 d . . . . .
H26 H 0.311792 0.255674 0.097681 0.058 Uiso 1 1 calc R U . . .
C27 C 0.2899(4) 0.4143(5) 0.0845(4) 0.0518(16) Uani 1 1 d . . . . .
H27 H 0.275324 0.414417 0.032357 0.062 Uiso 1 1 calc R U . . .
C28 C 0.2901(4) 0.5094(5) 0.1228(3) 0.0472(15) Uani 1 1 d . . . . .
H28 H 0.274586 0.575138 0.097137 0.057 Uiso 1 1 calc R U . . .
C29 C 0.3131(4) 0.5069(4) 0.1980(3) 0.0397(14) Uani 1 1 d . . . . .
C30 C 0.3184(4) 0.6072(4) 0.2451(3) 0.0394(14) Uani 1 1 d . . . . .
H30A H 0.343698 0.666866 0.223255 0.047 Uiso 1 1 calc R U . . .
H30B H 0.258065 0.628153 0.245919 0.047 Uiso 1 1 calc R U . . .
Cl2 Cl 0.80987(10) 0.24567(12) 0.40386(9) 0.0469(4) Uani 1 1 d . . . . .
O7 O 0.7296(3) 0.2313(4) 0.4226(4) 0.0812(17) Uani 1 1 d . . . . .
O8 O 0.8002(5) 0.2169(5) 0.3298(3) 0.099(2) Uani 1 1 d . . . . .
O9 O 0.8357(4) 0.3544(4) 0.4139(3) 0.0866(18) Uani 1 1 d . . . . .
O10 O 0.8749(4) 0.1802(5) 0.4507(4) 0.097(2) Uani 1 1 d . . . . .
O11 O 0.6573(3) 0.0725(4) 0.2500(3) 0.0673(14) Uani 1 1 d D . . . .
H11 H 0.691(4) 0.102(6) 0.289(3) 0.081 Uiso 1 1 d D U . . .
C31 C 0.6890(6) -0.0374(7) 0.2591(6) 0.087(3) Uani 1 1 d . . . . .
H31A H 0.738622 -0.045356 0.237966 0.131 Uiso 1 1 calc R U . . .
H31B H 0.640866 -0.085799 0.233841 0.131 Uiso 1 1 calc R U . . .
H31C H 0.708713 -0.055211 0.311527 0.131 Uiso 1 1 calc R U . . .


_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
Co1 Cl1 2.4552(16) 3_666 ?
Co1 O1 2.010(4) . ?
Co1 O2 2.133(3) . ?
Co1 O3 2.108(3) 3_666 ?
Co1 N1 2.101(5) . ?
Co1 N2 2.128(4) . ?
Co2 O2 2.170(3) 3_666 ?
Co2 O2 2.170(3) . ?
Co2 O3 2.075(3) 3_666 ?
Co2 O3 2.075(3) . ?
Co2 O4 2.115(3) 3_666 ?
Co2 O4 2.115(3) . ?
Co3 Cl1 2.4213(14) . ?
Co3 O3 2.079(3) . ?
Co3 O4 2.127(3) . ?
Co3 O5 2.026(3) . ?
Co3 N3 2.127(4) . ?
Co3 N5 2.106(5) . ?
V1 O1 1.969(3) . ?
V1 O2 2.055(3) . ?
V1 O4 2.180(3) . ?
V1 O5 2.014(4) . ?
V1 O6 1.620(4) . ?
V1 N4 2.106(5) . ?
O1 C6 1.397(7) . ?
O2 C12 1.423(6) . ?
O3 C18 1.430(6) . ?
O4 C24 1.423(6) . ?
O5 C30 1.414(6) . ?
N1 C1 1.359(7) . ?
N1 C5 1.327(8) . ?
N2 C7 1.345(7) . ?
N2 C11 1.332(7) . ?
N3 C13 1.354(7) . ?
N3 C17 1.326(7) . ?
N4 C19 1.342(8) . ?
N4 C23 1.348(7) . ?
N5 C25 1.341(7) . ?
N5 C29 1.367(7) . ?
C1 H1 0.9500 . ?
C1 C2 1.361(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.347(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(9) . ?
C5 C6 1.517(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.384(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.367(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.363(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.402(7) . ?
C11 C12 1.522(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13 0.9500 . ?
C13 C14 1.367(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.365(10) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(8) . ?
C17 C18 1.523(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19 0.9500 . ?
C19 C20 1.360(10) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(11) . ?
C21 H21 0.9500 . ?
C21 C22 1.374(11) . ?
C22 H22 0.9500 . ?
C22 C23 1.391(8) . ?
C23 C24 1.492(8) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25 0.9500 . ?
C25 C26 1.364(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.359(9) . ?
C27 H27 0.9500 . ?
C27 C28 1.392(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.369(8) . ?
C29 C30 1.528(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
Cl2 O7 1.419(5) . ?
Cl2 O8 1.416(6) . ?
Cl2 O9 1.414(5) . ?
Cl2 O10 1.410(6) . ?
O11 H11 0.86(2) . ?
O11 C31 1.453(9) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 Cl1 173.64(11) . 3_666 ?
O1 Co1 O2 77.94(13) . . ?
O1 Co1 O3 88.07(13) . 3_666 ?
O1 Co1 N1 79.56(16) . . ?
O1 Co1 N2 98.65(16) . . ?
O2 Co1 Cl1 101.96(10) . 3_666 ?
O3 Co1 Cl1 85.60(9) 3_666 3_666 ?
O3 Co1 O2 84.07(12) 3_666 . ?
O3 Co1 N2 158.46(16) 3_666 . ?
N1 Co1 Cl1 101.02(13) . 3_666 ?
N1 Co1 O2 156.82(16) . . ?
N1 Co1 O3 100.72(15) . 3_666 ?
N1 Co1 N2 100.62(18) . . ?
N2 Co1 Cl1 87.49(13) . 3_666 ?
N2 Co1 O2 77.44(14) . . ?
O2 Co2 O2 180.0 3_666 . ?
O3 Co2 O2 83.91(12) 3_666 . ?
O3 Co2 O2 96.08(12) 3_666 3_666 ?
O3 Co2 O2 83.91(12) . 3_666 ?
O3 Co2 O2 96.09(12) . . ?
O3 Co2 O3 180.0 3_666 . ?
O3 Co2 O4 98.50(12) . 3_666 ?
O3 Co2 O4 81.50(12) 3_666 3_666 ?
O3 Co2 O4 81.50(12) . . ?
O3 Co2 O4 98.50(12) 3_666 . ?
O4 Co2 O2 100.88(12) 3_666 . ?
O4 Co2 O2 79.12(12) . . ?
O4 Co2 O2 79.12(12) 3_666 3_666 ?
O4 Co2 O2 100.88(12) . 3_666 ?
O4 Co2 O4 180.0 3_666 . ?
O3 Co3 Cl1 87.10(9) . . ?
O3 Co3 O4 81.15(12) . . ?
O3 Co3 N3 78.86(14) . . ?
O3 Co3 N5 173.20(15) . . ?
O4 Co3 Cl1 94.87(9) . . ?
O4 Co3 N3 157.11(15) . . ?
O5 Co3 Cl1 171.47(11) . . ?
O5 Co3 O3 97.91(13) . . ?
O5 Co3 O4 79.19(13) . . ?
O5 Co3 N3 92.59(15) . . ?
O5 Co3 N5 79.73(15) . . ?
N3 Co3 Cl1 95.15(12) . . ?
N5 Co3 Cl1 96.04(12) . . ?
N5 Co3 O4 104.53(15) . . ?
N5 Co3 N3 94.81(17) . . ?
O1 V1 O2 80.71(14) . . ?
O1 V1 O4 86.76(13) . . ?
O1 V1 O5 162.56(15) . . ?
O1 V1 N4 88.00(16) . . ?
O2 V1 O4 80.20(12) . . ?
O2 V1 N4 154.11(16) . . ?
O5 V1 O2 88.01(14) . . ?
O5 V1 O4 78.19(13) . . ?
O5 V1 N4 96.72(15) . . ?
O6 V1 O1 100.38(18) . . ?
O6 V1 O2 108.45(17) . . ?
O6 V1 O4 169.46(16) . . ?
O6 V1 O5 95.78(18) . . ?
O6 V1 N4 96.4(2) . . ?
N4 V1 O4 75.93(15) . . ?
Co3 Cl1 Co1 84.36(5) . 3_666 ?
V1 O1 Co1 102.95(16) . . ?
C6 O1 Co1 116.7(3) . . ?
C6 O1 V1 130.2(3) . . ?
Co1 O2 Co2 94.19(12) . . ?
V1 O2 Co1 96.02(14) . . ?
V1 O2 Co2 101.30(12) . . ?
C12 O2 Co1 109.8(3) . . ?
C12 O2 Co2 132.2(3) . . ?
C12 O2 V1 115.8(3) . . ?
Co2 O3 Co1 97.79(12) . 3_666 ?
Co2 O3 Co3 99.93(14) . . ?
Co3 O3 Co1 102.92(13) . 3_666 ?
C18 O3 Co1 116.9(3) . 3_666 ?
C18 O3 Co2 126.4(3) . . ?
C18 O3 Co3 109.5(3) . . ?
Co2 O4 Co3 97.14(14) . . ?
Co2 O4 V1 99.08(12) . . ?
Co3 O4 V1 96.68(12) . . ?
C24 O4 Co2 129.9(3) . . ?
C24 O4 Co3 116.8(3) . . ?
C24 O4 V1 111.3(3) . . ?
V1 O5 Co3 105.62(14) . . ?
C30 O5 Co3 111.0(3) . . ?
C30 O5 V1 120.8(3) . . ?
C1 N1 Co1 128.7(4) . . ?
C5 N1 Co1 113.3(4) . . ?
C5 N1 C1 117.5(5) . . ?
C7 N2 Co1 127.2(4) . . ?
C11 N2 Co1 114.1(3) . . ?
C11 N2 C7 118.7(4) . . ?
C13 N3 Co3 129.0(4) . . ?
C17 N3 Co3 112.3(3) . . ?
C17 N3 C13 118.7(5) . . ?
C19 N4 V1 123.7(4) . . ?
C19 N4 C23 119.7(5) . . ?
C23 N4 V1 116.4(4) . . ?
C25 N5 Co3 131.1(4) . . ?
C25 N5 C29 116.9(5) . . ?
C29 N5 Co3 112.0(3) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.0(6) . . ?
C2 C1 H1 118.5 . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.8(6) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 119.9(6) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.8 . . ?
C5 C4 C3 118.4(6) . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 122.3(5) . . ?
N1 C5 C6 117.2(5) . . ?
C4 C5 C6 120.5(6) . . ?
O1 C6 C5 109.9(5) . . ?
O1 C6 H6A 109.7 . . ?
O1 C6 H6B 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 H7 118.7 . . ?
N2 C7 C8 122.7(6) . . ?
C8 C7 H7 118.7 . . ?
C7 C8 H8 121.0 . . ?
C9 C8 C7 117.9(5) . . ?
C9 C8 H8 121.0 . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.6(5) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 120.7 . . ?
C9 C10 C11 118.7(6) . . ?
C11 C10 H10 120.7 . . ?
N2 C11 C10 121.4(5) . . ?
N2 C11 C12 116.5(4) . . ?
C10 C11 C12 122.1(5) . . ?
O2 C12 C11 109.9(4) . . ?
O2 C12 H12A 109.7 . . ?
O2 C12 H12B 109.7 . . ?
C11 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N3 C13 H13 118.9 . . ?
N3 C13 C14 122.3(6) . . ?
C14 C13 H13 118.9 . . ?
C13 C14 H14 120.7 . . ?
C15 C14 C13 118.6(6) . . ?
C15 C14 H14 120.7 . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.2(6) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 121.0 . . ?
C15 C16 C17 117.9(6) . . ?
C17 C16 H16 121.0 . . ?
N3 C17 C16 122.2(5) . . ?
N3 C17 C18 117.0(4) . . ?
C16 C17 C18 120.8(5) . . ?
O3 C18 C17 110.3(4) . . ?
O3 C18 H18A 109.6 . . ?
O3 C18 H18B 109.6 . . ?
C17 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
N4 C19 H19 118.7 . . ?
N4 C19 C20 122.5(7) . . ?
C20 C19 H19 118.7 . . ?
C19 C20 H20 121.1 . . ?
C19 C20 C21 117.8(7) . . ?
C21 C20 H20 121.1 . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.2(7) . . ?
C22 C21 H21 119.4 . . ?
C21 C22 H22 121.0 . . ?
C21 C22 C23 118.1(7) . . ?
C23 C22 H22 121.0 . . ?
N4 C23 C22 120.6(6) . . ?
N4 C23 C24 116.6(4) . . ?
C22 C23 C24 122.7(5) . . ?
O4 C24 C23 110.5(4) . . ?
O4 C24 H24A 109.6 . . ?
O4 C24 H24B 109.6 . . ?
C23 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
N5 C25 H25 118.2 . . ?
N5 C25 C26 123.7(5) . . ?
C26 C25 H25 118.2 . . ?
C25 C26 H26 120.4 . . ?
C27 C26 C25 119.2(5) . . ?
C27 C26 H26 120.4 . . ?
C26 C27 H27 120.5 . . ?
C26 C27 C28 119.1(6) . . ?
C28 C27 H27 120.5 . . ?
C27 C28 H28 120.5 . . ?
C29 C28 C27 119.0(6) . . ?
C29 C28 H28 120.5 . . ?
N5 C29 C28 122.1(5) . . ?
N5 C29 C30 114.9(5) . . ?
C28 C29 C30 123.0(5) . . ?
O5 C30 C29 110.9(4) . . ?
O5 C30 H30A 109.5 . . ?
O5 C30 H30B 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 108.0 . . ?
O8 Cl2 O7 111.5(4) . . ?
O9 Cl2 O7 109.3(4) . . ?
O9 Cl2 O8 108.8(4) . . ?
O10 Cl2 O7 107.9(4) . . ?
O10 Cl2 O8 109.4(4) . . ?
O10 Cl2 O9 110.0(4) . . ?
C31 O11 H11 101(6) . . ?
O11 C31 H31A 109.5 . . ?
O11 C31 H31B 109.5 . . ?
O11 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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
O11 H11 O8 0.86(2) 2.21(5) 2.943(8) 144(7) . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O1 C6 C5 19.9(6) . . . . ?
Co1 O2 C12 C11 37.5(5) . . . . ?
Co1 O3 C18 C17 -79.7(5) 3_666 . . . ?
Co1 N1 C1 C2 172.5(5) . . . . ?
Co1 N1 C5 C4 -173.0(5) . . . . ?
Co1 N1 C5 C6 7.2(7) . . . . ?
Co1 N2 C7 C8 179.9(4) . . . . ?
Co1 N2 C11 C10 179.9(4) . . . . ?
Co1 N2 C11 C12 0.2(6) . . . . ?
Co2 O2 C12 C11 153.1(3) . . . . ?
Co2 O3 C18 C17 156.0(3) . . . . ?
Co2 O4 C24 C23 -155.5(3) . . . . ?
Co3 O3 C18 C17 36.7(5) . . . . ?
Co3 O4 C24 C23 77.3(4) . . . . ?
Co3 O5 C30 C29 -35.9(6) . . . . ?
Co3 N3 C13 C14 -176.2(5) . . . . ?
Co3 N3 C17 C16 176.5(5) . . . . ?
Co3 N3 C17 C18 -2.7(6) . . . . ?
Co3 N5 C25 C26 177.3(5) . . . . ?
Co3 N5 C29 C28 -175.9(5) . . . . ?
Co3 N5 C29 C30 3.9(6) . . . . ?
V1 O1 C6 C5 159.0(4) . . . . ?
V1 O2 C12 C11 -69.8(4) . . . . ?
V1 O4 C24 C23 -32.4(4) . . . . ?
V1 O5 C30 C29 88.4(5) . . . . ?
V1 N4 C19 C20 177.3(6) . . . . ?
V1 N4 C23 C22 -177.9(4) . . . . ?
V1 N4 C23 C24 2.2(6) . . . . ?
N1 C1 C2 C3 -0.8(11) . . . . ?
N1 C5 C6 O1 -17.6(8) . . . . ?
N2 C7 C8 C9 0.1(9) . . . . ?
N2 C11 C12 O2 -25.7(6) . . . . ?
N3 C13 C14 C15 -0.3(11) . . . . ?
N3 C17 C18 O3 -22.9(7) . . . . ?
N4 C19 C20 C21 -1.1(12) . . . . ?
N4 C23 C24 O4 20.7(6) . . . . ?
N5 C25 C26 C27 -1.6(10) . . . . ?
N5 C29 C30 O5 20.8(7) . . . . ?
C1 N1 C5 C4 0.3(9) . . . . ?
C1 N1 C5 C6 -179.4(5) . . . . ?
C1 C2 C3 C4 0.6(12) . . . . ?
C2 C3 C4 C5 0.0(12) . . . . ?
C3 C4 C5 N1 -0.5(11) . . . . ?
C3 C4 C5 C6 179.3(7) . . . . ?
C4 C5 C6 O1 162.6(6) . . . . ?
C5 N1 C1 C2 0.3(9) . . . . ?
C7 N2 C11 C10 -1.2(8) . . . . ?
C7 N2 C11 C12 179.1(5) . . . . ?
C7 C8 C9 C10 -1.2(9) . . . . ?
C8 C9 C10 C11 1.1(9) . . . . ?
C9 C10 C11 N2 0.1(8) . . . . ?
C9 C10 C11 C12 179.7(5) . . . . ?
C10 C11 C12 O2 154.6(5) . . . . ?
C11 N2 C7 C8 1.1(8) . . . . ?
C13 N3 C17 C16 -2.6(8) . . . . ?
C13 N3 C17 C18 178.1(5) . . . . ?
C13 C14 C15 C16 -2.3(12) . . . . ?
C14 C15 C16 C17 2.4(12) . . . . ?
C15 C16 C17 N3 0.1(10) . . . . ?
C15 C16 C17 C18 179.3(6) . . . . ?
C16 C17 C18 O3 157.8(5) . . . . ?
C17 N3 C13 C14 2.8(9) . . . . ?
C19 N4 C23 C22 -2.3(8) . . . . ?
C19 N4 C23 C24 177.9(5) . . . . ?
C19 C20 C21 C22 0.6(13) . . . . ?
C20 C21 C22 C23 -1.0(12) . . . . ?
C21 C22 C23 N4 1.8(10) . . . . ?
C21 C22 C23 C24 -178.4(6) . . . . ?
C22 C23 C24 O4 -159.1(5) . . . . ?
C23 N4 C19 C20 2.0(9) . . . . ?
C25 N5 C29 C28 1.5(8) . . . . ?
C25 N5 C29 C30 -178.7(5) . . . . ?
C25 C26 C27 C28 0.7(10) . . . . ?
C26 C27 C28 C29 1.2(10) . . . . ?
C27 C28 C29 N5 -2.4(10) . . . . ?
C27 C28 C29 C30 177.9(6) . . . . ?
C28 C29 C30 O5 -159.4(6) . . . . ?
C29 N5 C25 C26 0.5(8) . . . . ?

_olex2_date_sample_data_collection 2017-01-20
_olex2_date_sample_submission    2017-01-16
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 808o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.449
_oxdiff_exptl_absorpt_empirical_full_min 0.722
_vrf_PLAT910_eb17019             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: Not significant
;
####################################################################### 
# 
# 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_eb17037
_database_code_depnum_ccdc_archive 'CCDC 1847957'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2021-06-23 deposited with the CCDC.	2021-07-02 downloaded from the CCDC.
;
_audit_creation_date             2021-06-23
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2016/6
loop_
_audit_author_email
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C60 H60 Cl2 N10 Ni5 O12 V2, 2(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C62 H68 Cl4 N10 Ni5 O22 V2'
_chemical_formula_weight         1842.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C62H68Cl4Ni5N10O22V2 '
_chemical_oxdiff_usercomment     '@ 120 K 845o (ii)'
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'
V V 0.3005 0.5294 '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                   15.7800(3)
_cell_length_b                   12.4392(2)
_cell_length_c                   19.0165(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.745(2)
_cell_angle_gamma                90
_cell_volume                     3555.16(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    28878
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      32.6410
_cell_measurement_theta_min      3.4520
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 5 -25 0.1544
-20 1 19 0.0877
-17 -1 23 0.0856
17 -6 8 0.2121
19 0 -21 0.0712
-4 -15 -12 0.1199
14 -12 5 0.1525
-1 16 10 0.1629
-12 14 -2 0.1403
-7 17 4 0.1242
-1 -16 -11 0.1049
22 -3 -11 0.1206
3 10 -22 0.1262
19 6 -16 0.0950
10 15 -11 0.1011
-1 15 -14 0.1140
6 -13 14 0.1673
16 -9 -18 0.0844
-14 8 21 0.0994
-13 -14 3 0.1250

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.524
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.159
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9857 4.9901 -24.9768 -0.7521 0.0911 0.6623
-19.9835 1.0110 19.0069 0.9325 -0.1039 0.3725
-16.9825 -0.9877 22.9995 0.9929 -0.1348 0.1148
16.9994 -5.9998 7.9705 -0.0844 -0.0021 -1.0019
18.9830 -0.0118 -21.0039 -0.9719 0.1270 -0.2640
-4.0247 -14.9912 -11.9698 -0.3099 -0.9573 0.1670
13.9909 -11.9954 4.9826 -0.1292 -0.3925 -0.9218
-0.9756 15.9918 9.9786 0.3439 0.9196 0.1044
-11.9866 13.9940 -1.9903 0.1853 0.5531 0.8057
-6.9790 16.9917 3.9934 0.2773 0.8360 0.5138
-1.0251 -15.9913 -10.9746 -0.3369 -0.9576 0.0014
21.9875 -3.0083 -11.0175 -0.7351 0.0885 -0.6866
2.9932 9.9866 -21.9867 -0.6907 0.4126 0.6038
18.9931 5.9853 -16.0139 -0.8126 0.4871 -0.2705
10.0066 14.9834 -11.0129 -0.4833 0.8715 0.1472
-0.9953 14.9866 -13.9935 -0.3709 0.6815 0.6682
5.9972 -12.9897 13.9848 0.2829 -0.4983 -0.8336
15.9761 -9.0038 -17.9965 -0.8438 -0.3781 -0.3871
-13.9749 8.0045 20.9909 0.8945 0.3779 0.2136
-13.0117 -13.9850 3.0256 0.3023 -0.9249 0.1885

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            90810
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.985
_diffrn_reflns_theta_min         3.072
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00 -57.00   1.00   10.00    --  -17.68-178.00-150.00   47
  2  ω    -92.00  14.00   1.00   10.00    --  -17.68 -77.00 120.00  106
  3  ω    -49.00  56.00   1.00   10.00    --  -17.68  77.00 -30.00  105
  4  ω   -103.00 -55.00   1.00   10.00    --  -17.68 178.00  60.00   48
  5  ω    -12.00  93.00   1.00   10.00    --   19.09  77.00-150.00  105
  6  ω    -12.00  93.00   1.00   10.00    --   19.09  77.00 -60.00  105
  7  ω    -51.00  37.00   1.00   10.00    --   19.09 -38.00 -60.00   88
  8  ω     12.00  91.00   1.00   10.00    --   19.09  38.00 150.00   79
  9  ω     38.00  64.00   1.00   10.00    --   19.09 178.00 -30.00   26
 10  ω    -18.00   9.00   1.00   10.00    --   19.09 -38.00  60.00   27
 11  ω    -19.00  58.00   1.00   10.00    --   19.09 -99.00  60.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0182721000
_diffrn_orient_matrix_UB_12      0.0018205000
_diffrn_orient_matrix_UB_13      0.0297550000
_diffrn_orient_matrix_UB_21      0.0152109000
_diffrn_orient_matrix_UB_22      0.0536453000
_diffrn_orient_matrix_UB_23      0.0076722000
_diffrn_orient_matrix_UB_31      -0.0407720000
_diffrn_orient_matrix_UB_32      0.0191996000
_diffrn_orient_matrix_UB_33      -0.0242909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10678
_reflns_number_total             12777
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         12777
_refine_ls_number_restraints     155
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0341
_refine_ls_restrained_S_all      1.042
_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)+(0.0287P)²+2.6346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0770
_refine_special_details          
;
The O-bound H atom was identified from a difference Fourier map and refined with appropriate restraints

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
910_ALERT_3_B Missing # of FCF Reflection(s) Below Theta(Min)          11 Note

Not significant

#===============================================================================
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        Cl2 Check
480_ALERT_4_C Long H...A H-Bond Reported H11    ..  O7A     ..       2.89 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      2.742 Check

Not significant


#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         11 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          9 Report
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
176_ALERT_4_G The CIF-Embedded .res File Contains SADI Records          2 Report
187_ALERT_4_G The CIF-Embedded .res File Contains RIGU Records          2 Report
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ni1    --  N1      ..        6.7 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ni1    --  N2      ..        6.2 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ni1    --  Cl1_a   ..        9.3 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ni3    --  Cl1     ..        7.1 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ni3    --  N5      ..        7.7 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  V1     --  O6      ..        5.7 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  V1     --  N4      ..        5.7 s.u.
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2)..         80 % Note
860_ALERT_3_G Number of Least-Squares Restraints .............        155 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        568 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          1 Note
978_ALERT_2_G Number C-C Bonds with Positive Residual Density.         15 Note

Not significant


#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O11-H11
 0.84 with sigma of 0.02
 O7-O8 \\sim O7-O9 \\sim O7-O10 \\sim O8-O9 \\sim O8-O10 \\sim O9-O10 \\sim
O9A-O10A \\sim O9A-O7A \\sim O9A-
 O8A \\sim O10A-O7A \\sim O10A-O8A \\sim O7A-O8A
 with sigma of 0.04
 Cl2-O7 \\sim Cl2-O8 \\sim Cl2-O9 \\sim Cl2-O10 \\sim Cl2-O9A \\sim Cl2-O10A
\\sim Cl2-O7A \\sim Cl2-O8A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O7, O8, O9, O10, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9A, O10A, O7A, O8A, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O9A)=Sof(O10A)=Sof(O7A)=Sof(O8A)=1-FVAR(1)
 Sof(O7)=Sof(O8)=Sof(O9)=Sof(O10)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_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 0.63468(2) 0.68157(2) 0.49373(2) 0.01304(4) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 0.500000 0.01128(5) Uani 1 2 d S T P . .
Ni3 Ni 0.35329(2) 0.43732(2) 0.35250(2) 0.01263(4) Uani 1 1 d . . . . .
V1 V 0.49791(2) 0.61367(2) 0.34674(2) 0.01352(5) Uani 1 1 d . . . . .
Cl1 Cl 0.35452(2) 0.25033(3) 0.38504(2) 0.01604(7) Uani 1 1 d . . . . .
O1 O 0.62658(7) 0.60844(9) 0.39851(6) 0.0159(2) Uani 1 1 d . . . . .
O2 O 0.49756(7) 0.65407(8) 0.45156(6) 0.0136(2) Uani 1 1 d . . . . .
O3 O 0.36582(7) 0.47023(8) 0.46035(6) 0.01267(19) Uani 1 1 d . . . . .
O4 O 0.49149(7) 0.45428(8) 0.39211(6) 0.0130(2) Uani 1 1 d . . . . .
O5 O 0.36562(7) 0.59109(9) 0.32148(6) 0.0146(2) Uani 1 1 d . . . . .
O6 O 0.49159(8) 0.72141(10) 0.29853(7) 0.0227(2) Uani 1 1 d . . . . .
N1 N 0.76591(9) 0.69320(11) 0.49645(8) 0.0174(3) Uani 1 1 d . . . . .
N2 N 0.58988(9) 0.83178(11) 0.45159(8) 0.0172(3) Uani 1 1 d . . . . .
N3 N 0.22070(8) 0.46038(11) 0.34463(7) 0.0159(2) Uani 1 1 d . . . . .
N4 N 0.52360(9) 0.50875(12) 0.26878(8) 0.0183(3) Uani 1 1 d . . . . .
N5 N 0.33137(9) 0.41392(11) 0.24078(8) 0.0160(2) Uani 1 1 d . . . . .
C1 C 0.83675(11) 0.72378(14) 0.55321(10) 0.0203(3) Uani 1 1 d . . . . .
H1 H 0.827153 0.748252 0.597489 0.024 Uiso 1 1 calc R . . . .
C2 C 0.92263(11) 0.72077(16) 0.54921(11) 0.0274(4) Uani 1 1 d . . . . .
H2 H 0.971085 0.744471 0.589552 0.033 Uiso 1 1 calc R . . . .
C3 C 0.93685(12) 0.68265(17) 0.48543(12) 0.0307(4) Uani 1 1 d . . . . .
H3 H 0.995461 0.678459 0.481745 0.037 Uiso 1 1 calc R . . . .
C4 C 0.86474(11) 0.65064(17) 0.42700(11) 0.0274(4) Uani 1 1 d . . . . .
H4 H 0.873180 0.624148 0.382759 0.033 Uiso 1 1 calc R . . . .
C5 C 0.77972(11) 0.65789(14) 0.43407(10) 0.0204(3) Uani 1 1 d . . . . .
C6 C 0.69792(11) 0.62810(17) 0.37124(10) 0.0255(4) Uani 1 1 d . . . . .
H6A H 0.682600 0.687443 0.334862 0.031 Uiso 1 1 calc R . . . .
H6B H 0.710241 0.563076 0.345957 0.031 Uiso 1 1 calc R . . . .
C7 C 0.63803(11) 0.91387(14) 0.43772(10) 0.0207(3) Uani 1 1 d . . . . .
H7 H 0.700070 0.903780 0.446497 0.025 Uiso 1 1 calc R . . . .
C8 C 0.60106(13) 1.01237(14) 0.41121(10) 0.0242(3) Uani 1 1 d . . . . .
H8 H 0.636842 1.068539 0.401661 0.029 Uiso 1 1 calc R . . . .
C9 C 0.51072(13) 1.02714(14) 0.39894(10) 0.0250(4) Uani 1 1 d . . . . .
H9 H 0.483618 1.094084 0.381155 0.030 Uiso 1 1 calc R . . . .
C10 C 0.46023(12) 0.94328(13) 0.41287(10) 0.0209(3) Uani 1 1 d . . . . .
H10 H 0.398095 0.951787 0.404459 0.025 Uiso 1 1 calc R . . . .
C11 C 0.50205(10) 0.84625(13) 0.43940(9) 0.0168(3) Uani 1 1 d . . . . .
C12 C 0.45123(10) 0.75084(12) 0.45575(9) 0.0164(3) Uani 1 1 d . . . . .
H12A H 0.444890 0.758343 0.505731 0.020 Uiso 1 1 calc R . . . .
H12B H 0.390923 0.748469 0.419606 0.020 Uiso 1 1 calc R . . . .
C13 C 0.14734(11) 0.43181(14) 0.28986(9) 0.0209(3) Uani 1 1 d . . . . .
H13 H 0.154065 0.391559 0.249442 0.025 Uiso 1 1 calc R . . . .
C14 C 0.06251(11) 0.45912(16) 0.29049(11) 0.0267(4) Uani 1 1 d . . . . .
H14 H 0.011770 0.438277 0.251169 0.032 Uiso 1 1 calc R . . . .
C15 C 0.05330(11) 0.51764(17) 0.34989(11) 0.0289(4) Uani 1 1 d . . . . .
H15 H -0.004002 0.539049 0.351150 0.035 Uiso 1 1 calc R . . . .
C16 C 0.12841(11) 0.54458(14) 0.40733(10) 0.0217(3) Uani 1 1 d . . . . .
H16 H 0.123244 0.582856 0.449063 0.026 Uiso 1 1 calc R . . . .
C17 C 0.21156(10) 0.51452(12) 0.40275(9) 0.0156(3) Uani 1 1 d . . . . .
C18 C 0.29668(9) 0.54144(12) 0.46332(9) 0.0147(3) Uani 1 1 d . . . . .
H18A H 0.314369 0.616400 0.457286 0.018 Uiso 1 1 calc R . . . .
H18B H 0.286529 0.535441 0.512045 0.018 Uiso 1 1 calc R . . . .
C19 C 0.52722(13) 0.54042(17) 0.20195(10) 0.0277(4) Uani 1 1 d . . . . .
H19 H 0.511984 0.612488 0.186768 0.033 Uiso 1 1 calc R . . . .
C20 C 0.55225(16) 0.4719(2) 0.15492(12) 0.0401(5) Uani 1 1 d . . . . .
H20 H 0.553889 0.495739 0.107888 0.048 Uiso 1 1 calc R . . . .
C21 C 0.57495(17) 0.3674(2) 0.17808(13) 0.0418(5) Uani 1 1 d . . . . .
H21 H 0.592452 0.318480 0.146736 0.050 Uiso 1 1 calc R . . . .
C22 C 0.57221(13) 0.33413(16) 0.24667(11) 0.0302(4) Uani 1 1 d . . . . .
H22 H 0.587655 0.262522 0.262924 0.036 Uiso 1 1 calc R . . . .
C23 C 0.54640(10) 0.40745(14) 0.29147(9) 0.0186(3) Uani 1 1 d . . . . .
C24 C 0.54421(10) 0.37950(13) 0.36783(9) 0.0164(3) Uani 1 1 d . . . . .
H24A H 0.519421 0.306355 0.367637 0.020 Uiso 1 1 calc R . . . .
H24B H 0.605526 0.379751 0.402359 0.020 Uiso 1 1 calc R . . . .
C25 C 0.33335(11) 0.32220(13) 0.20382(9) 0.0192(3) Uani 1 1 d . . . . .
H25 H 0.349682 0.257337 0.230947 0.023 Uiso 1 1 calc R . . . .
C26 C 0.31251(12) 0.31901(14) 0.12795(10) 0.0241(3) Uani 1 1 d . . . . .
H26 H 0.315134 0.253183 0.103362 0.029 Uiso 1 1 calc R . . . .
C27 C 0.28773(13) 0.41313(15) 0.08814(10) 0.0255(4) Uani 1 1 d . . . . .
H27 H 0.272800 0.412842 0.035826 0.031 Uiso 1 1 calc R . . . .
C28 C 0.28505(11) 0.50757(14) 0.12575(9) 0.0210(3) Uani 1 1 d . . . . .
H28 H 0.267398 0.572912 0.099503 0.025 Uiso 1 1 calc R . . . .
C29 C 0.30842(10) 0.50588(13) 0.20221(9) 0.0159(3) Uani 1 1 d . . . . .
C30 C 0.31076(11) 0.60563(13) 0.24832(9) 0.0177(3) Uani 1 1 d . . . . .
H30A H 0.333214 0.666926 0.225931 0.021 Uiso 1 1 calc R . . . .
H30B H 0.249637 0.623173 0.248507 0.021 Uiso 1 1 calc R . . . .
Cl2 Cl 0.81087(3) 0.24339(4) 0.40537(3) 0.02934(10) Uani 1 1 d D U . . .
O7 O 0.7284(3) 0.2312(4) 0.4217(2) 0.0349(12) Uani 0.68(2) 1 d D U . A 1
O8 O 0.7980(4) 0.2169(4) 0.3288(2) 0.0457(13) Uani 0.68(2) 1 d D U . A 1
O9 O 0.8442(4) 0.3505(5) 0.4187(5) 0.0468(13) Uani 0.68(2) 1 d D U . A 1
O10 O 0.8743(4) 0.1696(6) 0.4503(4) 0.0554(15) Uani 0.68(2) 1 d D U . A 1
O11 O 0.65950(11) 0.07288(14) 0.24934(9) 0.0393(4) Uani 1 1 d D . . . .
H11 H 0.7012(15) 0.113(2) 0.2739(14) 0.047 Uiso 1 1 d DR . . . .
C31 C 0.69079(17) -0.0345(2) 0.25668(15) 0.0463(6) Uani 1 1 d . . . . .
H31A H 0.742154 -0.040127 0.238130 0.069 Uiso 1 1 calc GR . . . .
H31B H 0.643369 -0.082323 0.228146 0.069 Uiso 1 1 calc GR . . . .
H31C H 0.708498 -0.055429 0.308829 0.069 Uiso 1 1 calc GR . . . .
O9A O 0.8242(18) 0.3592(9) 0.4127(10) 0.076(5) Uani 0.32(2) 1 d D U . A 2
O10A O 0.8748(8) 0.1903(18) 0.4631(11) 0.080(5) Uani 0.32(2) 1 d D U . A 2
O7A O 0.7250(8) 0.2270(15) 0.4108(14) 0.110(7) Uani 0.32(2) 1 d D U . A 2
O8A O 0.8153(18) 0.2111(13) 0.3364(8) 0.111(7) Uani 0.32(2) 1 d D U . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 Cl1 2.4130(4) 3_666 ?
Ni1 O1 1.9953(11) . ?
Ni1 O2 2.0939(11) . ?
Ni1 O3 2.0814(11) 3_666 ?
Ni1 N1 2.0607(13) . ?
Ni1 N2 2.0707(14) . ?
Ni2 O2 2.1217(11) 3_666 ?
Ni2 O2 2.1217(11) . ?
Ni2 O3 2.0533(10) . ?
Ni2 O3 2.0532(10) 3_666 ?
Ni2 O4 2.0936(11) . ?
Ni2 O4 2.0936(11) 3_666 ?
Ni3 Cl1 2.4055(4) . ?
Ni3 O3 2.0410(11) . ?
Ni3 O4 2.0896(10) . ?
Ni3 O5 2.0283(11) . ?
Ni3 N3 2.0716(13) . ?
Ni3 N5 2.0664(14) . ?
V1 O1 1.9692(11) . ?
V1 O2 2.0573(11) . ?
V1 O4 2.1769(11) . ?
V1 O5 2.0140(11) . ?
V1 O6 1.6096(12) . ?
V1 N4 2.1051(14) . ?
O1 C6 1.3971(19) . ?
O2 C12 1.4232(18) . ?
O3 C18 1.4198(17) . ?
O4 C24 1.4158(18) . ?
O5 C30 1.4083(19) . ?
N1 C1 1.351(2) . ?
N1 C5 1.344(2) . ?
N2 C7 1.346(2) . ?
N2 C11 1.346(2) . ?
N3 C13 1.348(2) . ?
N3 C17 1.339(2) . ?
N4 C19 1.348(2) . ?
N4 C23 1.345(2) . ?
N5 C25 1.345(2) . ?
N5 C29 1.347(2) . ?
C1 H1 0.9500 . ?
C1 C2 1.381(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.383(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.385(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(2) . ?
C5 C6 1.514(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.384(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.385(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.394(2) . ?
C11 C12 1.517(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13 0.9500 . ?
C13 C14 1.385(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.388(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.386(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.392(2) . ?
C17 C18 1.517(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19 0.9500 . ?
C19 C20 1.377(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.382(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.391(2) . ?
C23 C24 1.504(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25 0.9500 . ?
C25 C26 1.379(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.384(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.383(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.387(2) . ?
C29 C30 1.513(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
Cl2 O7 1.435(4) . ?
Cl2 O8 1.446(4) . ?
Cl2 O9 1.426(5) . ?
Cl2 O10 1.433(4) . ?
Cl2 O9A 1.456(10) . ?
Cl2 O10A 1.409(10) . ?
Cl2 O7A 1.405(10) . ?
Cl2 O8A 1.394(10) . ?
O11 H11 0.846(17) . ?
O11 C31 1.416(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 Cl1 173.43(4) . 3_666 ?
O1 Ni1 O2 78.76(4) . . ?
O1 Ni1 O3 87.70(4) . 3_666 ?
O1 Ni1 N1 80.84(5) . . ?
O1 Ni1 N2 98.06(5) . . ?
O2 Ni1 Cl1 100.78(3) . 3_666 ?
O3 Ni1 Cl1 85.75(3) 3_666 3_666 ?
O3 Ni1 O2 82.93(4) 3_666 . ?
N1 Ni1 Cl1 99.99(4) . 3_666 ?
N1 Ni1 O2 159.12(5) . . ?
N1 Ni1 O3 100.69(5) . 3_666 ?
N1 Ni1 N2 99.69(5) . . ?
N2 Ni1 Cl1 88.24(4) . 3_666 ?
N2 Ni1 O2 78.94(5) . . ?
N2 Ni1 O3 159.47(5) . 3_666 ?
O2 Ni2 O2 180.0 3_666 . ?
O3 Ni2 O2 97.08(4) 3_666 3_666 ?
O3 Ni2 O2 82.92(4) . 3_666 ?
O3 Ni2 O2 82.92(4) 3_666 . ?
O3 Ni2 O2 97.08(4) . . ?
O3 Ni2 O3 180.0 3_666 . ?
O3 Ni2 O4 99.20(4) 3_666 . ?
O3 Ni2 O4 80.80(4) . . ?
O3 Ni2 O4 80.80(4) 3_666 3_666 ?
O3 Ni2 O4 99.20(4) . 3_666 ?
O4 Ni2 O2 99.64(4) . 3_666 ?
O4 Ni2 O2 80.36(4) . . ?
O4 Ni2 O2 99.64(4) 3_666 . ?
O4 Ni2 O2 80.36(4) 3_666 3_666 ?
O4 Ni2 O4 180.0 3_666 . ?
O3 Ni3 Cl1 86.83(3) . . ?
O3 Ni3 O4 81.18(4) . . ?
O3 Ni3 N3 80.28(5) . . ?
O3 Ni3 N5 174.85(5) . . ?
O4 Ni3 Cl1 94.54(3) . . ?
O5 Ni3 Cl1 173.06(3) . . ?
O5 Ni3 O3 96.58(4) . . ?
O5 Ni3 O4 80.07(4) . . ?
O5 Ni3 N3 91.88(5) . . ?
O5 Ni3 N5 80.48(5) . . ?
N3 Ni3 Cl1 94.66(4) . . ?
N3 Ni3 O4 158.78(5) . . ?
N5 Ni3 Cl1 96.54(4) . . ?
N5 Ni3 O4 102.36(5) . . ?
N5 Ni3 N3 95.53(5) . . ?
O1 V1 O2 80.24(4) . . ?
O1 V1 O4 86.40(4) . . ?
O1 V1 O5 161.90(5) . . ?
O1 V1 N4 86.62(5) . . ?
O2 V1 O4 79.88(4) . . ?
O2 V1 N4 153.09(5) . . ?
O5 V1 O2 87.51(4) . . ?
O5 V1 O4 78.31(4) . . ?
O5 V1 N4 98.84(5) . . ?
O6 V1 O1 100.82(6) . . ?
O6 V1 O2 109.29(6) . . ?
O6 V1 O4 169.05(6) . . ?
O6 V1 O5 95.77(6) . . ?
O6 V1 N4 96.14(6) . . ?
N4 V1 O4 75.92(5) . . ?
Ni3 Cl1 Ni1 84.202(13) . 3_666 ?
V1 O1 Ni1 102.11(5) . . ?
C6 O1 Ni1 114.90(10) . . ?
C6 O1 V1 129.30(10) . . ?
Ni1 O2 Ni2 95.82(4) . . ?
V1 O2 Ni1 95.93(4) . . ?
V1 O2 Ni2 101.24(5) . . ?
C12 O2 Ni1 109.21(9) . . ?
C12 O2 Ni2 132.95(9) . . ?
C12 O2 V1 114.46(9) . . ?
Ni2 O3 Ni1 98.33(4) . 3_666 ?
Ni3 O3 Ni1 103.19(5) . 3_666 ?
Ni3 O3 Ni2 100.28(4) . . ?
C18 O3 Ni1 116.62(9) . 3_666 ?
C18 O3 Ni2 126.28(9) . . ?
C18 O3 Ni3 108.96(9) . . ?
Ni2 O4 V1 98.29(4) . . ?
Ni3 O4 Ni2 97.40(4) . . ?
Ni3 O4 V1 96.81(4) . . ?
C24 O4 Ni2 129.01(9) . . ?
C24 O4 Ni3 117.94(9) . . ?
C24 O4 V1 111.48(9) . . ?
V1 O5 Ni3 104.27(5) . . ?
C30 O5 Ni3 108.90(9) . . ?
C30 O5 V1 119.87(10) . . ?
C1 N1 Ni1 128.36(12) . . ?
C5 N1 Ni1 112.77(11) . . ?
C5 N1 C1 118.70(14) . . ?
C7 N2 Ni1 127.88(11) . . ?
C11 N2 Ni1 113.55(11) . . ?
C11 N2 C7 118.55(14) . . ?
C13 N3 Ni3 129.05(12) . . ?
C17 N3 Ni3 111.75(10) . . ?
C17 N3 C13 119.17(14) . . ?
C19 N4 V1 123.73(13) . . ?
C23 N4 V1 116.42(11) . . ?
C23 N4 C19 119.48(15) . . ?
C25 N5 Ni3 129.29(11) . . ?
C25 N5 C29 118.74(14) . . ?
C29 N5 Ni3 111.91(10) . . ?
N1 C1 H1 118.8 . . ?
N1 C1 C2 122.39(17) . . ?
C2 C1 H1 118.8 . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C3 118.81(17) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.28(17) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 118.99(18) . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 121.81(16) . . ?
N1 C5 C6 116.63(14) . . ?
C4 C5 C6 121.55(16) . . ?
O1 C6 C5 109.86(14) . . ?
O1 C6 H6A 109.7 . . ?
O1 C6 H6B 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 H7 118.6 . . ?
N2 C7 C8 122.85(16) . . ?
C8 C7 H7 118.6 . . ?
C7 C8 H8 120.8 . . ?
C7 C8 C9 118.47(16) . . ?
C9 C8 H8 120.8 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.34(16) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 120.5 . . ?
C9 C10 C11 118.97(16) . . ?
C11 C10 H10 120.5 . . ?
N2 C11 C10 121.82(15) . . ?
N2 C11 C12 116.18(13) . . ?
C10 C11 C12 122.00(14) . . ?
O2 C12 C11 109.73(12) . . ?
O2 C12 H12A 109.7 . . ?
O2 C12 H12B 109.7 . . ?
C11 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N3 C13 H13 118.9 . . ?
N3 C13 C14 122.25(16) . . ?
C14 C13 H13 118.9 . . ?
C13 C14 H14 120.8 . . ?
C13 C14 C15 118.48(16) . . ?
C15 C14 H14 120.8 . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.46(16) . . ?
C16 C15 H15 120.3 . . ?
C15 C16 H16 120.6 . . ?
C15 C16 C17 118.78(16) . . ?
C17 C16 H16 120.6 . . ?
N3 C17 C16 121.82(15) . . ?
N3 C17 C18 116.40(13) . . ?
C16 C17 C18 121.77(15) . . ?
O3 C18 C17 110.21(12) . . ?
O3 C18 H18A 109.6 . . ?
O3 C18 H18B 109.6 . . ?
C17 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
N4 C19 H19 118.9 . . ?
N4 C19 C20 122.3(2) . . ?
C20 C19 H19 118.9 . . ?
C19 C20 H20 120.9 . . ?
C19 C20 C21 118.2(2) . . ?
C21 C20 H20 120.9 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.15(19) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.6 . . ?
C21 C22 C23 118.75(19) . . ?
C23 C22 H22 120.6 . . ?
N4 C23 C22 121.16(17) . . ?
N4 C23 C24 116.35(14) . . ?
C22 C23 C24 122.49(16) . . ?
O4 C24 C23 110.59(13) . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
N5 C25 H25 118.8 . . ?
N5 C25 C26 122.33(16) . . ?
C26 C25 H25 118.8 . . ?
C25 C26 H26 120.5 . . ?
C25 C26 C27 119.02(16) . . ?
C27 C26 H26 120.5 . . ?
C26 C27 H27 120.5 . . ?
C28 C27 C26 118.94(16) . . ?
C28 C27 H27 120.5 . . ?
C27 C28 H28 120.4 . . ?
C27 C28 C29 119.27(16) . . ?
C29 C28 H28 120.4 . . ?
N5 C29 C28 121.67(15) . . ?
N5 C29 C30 115.19(14) . . ?
C28 C29 C30 123.14(14) . . ?
O5 C30 C29 111.48(12) . . ?
O5 C30 H30A 109.3 . . ?
O5 C30 H30B 109.3 . . ?
C29 C30 H30A 109.3 . . ?
C29 C30 H30B 109.3 . . ?
H30A C30 H30B 108.0 . . ?
O7 Cl2 O8 109.6(3) . . ?
O9 Cl2 O7 111.7(4) . . ?
O9 Cl2 O8 108.8(4) . . ?
O9 Cl2 O10 109.8(4) . . ?
O10 Cl2 O7 108.6(3) . . ?
O10 Cl2 O8 108.3(4) . . ?
O10A Cl2 O9A 109.9(9) . . ?
O7A Cl2 O9A 104.5(10) . . ?
O7A Cl2 O10A 110.6(9) . . ?
O8A Cl2 O9A 109.2(9) . . ?
O8A Cl2 O10A 111.7(10) . . ?
O8A Cl2 O7A 110.7(10) . . ?
C31 O11 H11 108.4(19) . . ?
O11 C31 H31A 109.5 . . ?
O11 C31 H31B 109.5 . . ?
O11 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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
O11 H11 O8 0.846(17) 2.029(18) 2.874(4) 177(3) .
O11 H11 O7A 0.846(17) 2.89(3) 3.50(3) 131(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 C6 C5 24.82(19) . . . . ?
Ni1 O2 C12 C11 37.03(14) . . . . ?
Ni1 O3 C18 C17 -79.55(13) 3_666 . . . ?
Ni1 N1 C1 C2 175.30(14) . . . . ?
Ni1 N1 C5 C4 -174.65(15) . . . . ?
Ni1 N1 C5 C6 6.37(19) . . . . ?
Ni1 N2 C7 C8 -178.19(13) . . . . ?
Ni1 N2 C11 C10 178.36(13) . . . . ?
Ni1 N2 C11 C12 -1.99(17) . . . . ?
Ni2 O2 C12 C11 155.12(10) . . . . ?
Ni2 O3 C18 C17 155.77(10) . . . . ?
Ni2 O4 C24 C23 -153.10(10) . . . . ?
Ni3 O3 C18 C17 36.68(14) . . . . ?
Ni3 O4 C24 C23 78.78(14) . . . . ?
Ni3 O5 C30 C29 -36.16(15) . . . . ?
Ni3 N3 C13 C14 -175.75(14) . . . . ?
Ni3 N3 C17 C16 176.32(13) . . . . ?
Ni3 N3 C17 C18 -3.63(17) . . . . ?
Ni3 N5 C25 C26 176.53(13) . . . . ?
Ni3 N5 C29 C28 -175.79(12) . . . . ?
Ni3 N5 C29 C30 4.60(16) . . . . ?
V1 O1 C6 C5 157.57(11) . . . . ?
V1 O2 C12 C11 -69.15(13) . . . . ?
V1 O4 C24 C23 -31.88(14) . . . . ?
V1 O5 C30 C29 83.64(14) . . . . ?
V1 N4 C19 C20 173.85(16) . . . . ?
V1 N4 C23 C22 -174.41(13) . . . . ?
V1 N4 C23 C24 4.32(18) . . . . ?
N1 C1 C2 C3 -1.6(3) . . . . ?
N1 C5 C6 O1 -20.3(2) . . . . ?
N2 C7 C8 C9 0.4(3) . . . . ?
N2 C11 C12 O2 -23.93(19) . . . . ?
N3 C13 C14 C15 -0.2(3) . . . . ?
N3 C17 C18 O3 -22.31(19) . . . . ?
N4 C19 C20 C21 -0.5(3) . . . . ?
N4 C23 C24 O4 18.96(19) . . . . ?
N5 C25 C26 C27 -0.7(3) . . . . ?
N5 C29 C30 O5 21.23(19) . . . . ?
C1 N1 C5 C4 0.9(3) . . . . ?
C1 N1 C5 C6 -178.03(16) . . . . ?
C1 C2 C3 C4 1.3(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 N1 -1.2(3) . . . . ?
C3 C4 C5 C6 177.70(19) . . . . ?
C4 C5 C6 O1 160.72(17) . . . . ?
C5 N1 C1 C2 0.5(3) . . . . ?
C7 N2 C11 C10 0.1(2) . . . . ?
C7 N2 C11 C12 179.78(14) . . . . ?
C7 C8 C9 C10 -0.5(3) . . . . ?
C8 C9 C10 C11 0.4(3) . . . . ?
C9 C10 C11 N2 -0.2(3) . . . . ?
C9 C10 C11 C12 -179.86(16) . . . . ?
C10 C11 C12 O2 155.72(15) . . . . ?
C11 N2 C7 C8 -0.2(3) . . . . ?
C13 N3 C17 C16 -1.7(2) . . . . ?
C13 N3 C17 C18 178.38(14) . . . . ?
C13 C14 C15 C16 -1.6(3) . . . . ?
C14 C15 C16 C17 1.8(3) . . . . ?
C15 C16 C17 N3 -0.1(3) . . . . ?
C15 C16 C17 C18 179.82(17) . . . . ?
C16 C17 C18 O3 157.75(15) . . . . ?
C17 N3 C13 C14 1.9(3) . . . . ?
C19 N4 C23 C22 -1.1(2) . . . . ?
C19 N4 C23 C24 177.61(15) . . . . ?
C19 C20 C21 C22 0.0(4) . . . . ?
C20 C21 C22 C23 0.0(3) . . . . ?
C21 C22 C23 N4 0.6(3) . . . . ?
C21 C22 C23 C24 -178.04(18) . . . . ?
C22 C23 C24 O4 -162.32(15) . . . . ?
C23 N4 C19 C20 1.1(3) . . . . ?
C25 N5 C29 C28 1.5(2) . . . . ?
C25 N5 C29 C30 -178.14(14) . . . . ?
C25 C26 C27 C28 0.3(3) . . . . ?
C26 C27 C28 C29 0.9(3) . . . . ?
C27 C28 C29 N5 -1.8(3) . . . . ?
C27 C28 C29 C30 177.73(16) . . . . ?
C28 C29 C30 O5 -158.37(15) . . . . ?
C29 N5 C25 C26 -0.2(2) . . . . ?

_olex2_date_sample_data_collection 2017-03-17
_olex2_date_sample_submission    2017-03-16
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 845o(ii)
_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 1.279
_oxdiff_exptl_absorpt_empirical_full_min 0.804
_vrf_PLAT910_eb17037             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: Not significant
;
