# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_exp_44
_database_code_depnum_ccdc_archive 'CCDC 2271794'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2023-06-23 deposited with the CCDC.	2023-08-16 downloaded from the CCDC.
;
_audit_creation_date             2023-01-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            'compound (5) in manuscript'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H67 N6 Ni O6, H2 O, 0.5[CH2Cl2]'
_chemical_formula_sum            'C48.50 H69 Cl N6 Ni O7'
_chemical_formula_weight         942.25
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H69 N6 Ni O8'
_chemical_oxdiff_usercomment     'Nawal Assadouwi 150 K'
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'
Cl Cl 0.1484 0.1585 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7197(8)
_cell_length_b                   12.5847(8)
_cell_length_c                   16.6523(10)
_cell_angle_alpha                101.829(6)
_cell_angle_beta                 96.030(5)
_cell_angle_gamma                97.639(6)
_cell_volume                     2360.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13180
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.7620
_cell_measurement_theta_min      2.0000
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.776
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1006
_exptl_crystal_recrystallization_method dichloromethane
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55431
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.698
_diffrn_reflns_theta_min         1.859
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -11.00  53.50   0.50   20.00    --   20.00  54.00   0.00  129
  2  ω     83.00 109.00   0.50   20.00    --   20.00  54.00 -30.00   52
  3  ω     77.00 103.00   0.50   20.00    --   20.00  54.00-180.00   52
  4  ω     41.00  67.00   0.50   20.00    --   20.00  54.00-120.00   52
  5  ω     18.00  43.00   0.50   20.00    --   20.00  54.00 -30.00   50
  6  ω     27.00  79.50   0.50   20.00    --   20.00  54.00  30.00  105
  7  ω     55.00  81.00   0.50   20.00    --   20.00  54.00 150.00   52
  8  ω     -3.00  42.50   0.50   20.00    --   20.00  54.00  90.00   91
  9  ω    -23.00  11.00   0.50   20.00    --   20.00  54.00 -60.00   68
 10  ω    -16.00  10.00   0.50   20.00    --   20.00  54.00-180.00   52
 11  ω    -64.00  -3.50   0.50   20.00    --   20.00  54.00  30.00  121
 12  ω    -72.00 -12.50   0.50   20.00    --   20.00  54.00  90.00  119
 13  ω    -70.00   8.50   0.50   20.00    --   20.00  54.00 -30.00  157
 14  ω    -73.00 -20.50   0.50   20.00    --   20.00  54.00-120.00  105
 15  ω    -73.00 -33.50   0.50   20.00    --   20.00  54.00 -60.00   79
 16  ω    -74.00  55.50   0.50   20.00    --   20.00  54.00-150.00  259
 17  ω    -70.00  75.50   0.50   20.00    --   20.00  54.00 120.00  291
 18  ω    -72.00 108.50   0.50   20.00    --   20.00  54.00  60.00  361
 19  ω    -66.00 -33.00   0.50   20.00    --   20.00  54.00 150.00   66
 20  ω    -63.00  65.50   0.50   20.00    --   20.00  54.00 165.66  257
 21  ω    -66.00  55.50   0.50   20.00    --   20.00  54.00 -90.00  243
 22  ω    -68.00 -41.00   0.50   20.00    --   20.00  54.00   0.00   54
 23  ω    -59.00 -32.00   0.50   20.00    --   20.00  54.00-180.00   54
;
_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      0.0073092000
_diffrn_orient_matrix_UB_12      -0.0389433000
_diffrn_orient_matrix_UB_13      0.0247002000
_diffrn_orient_matrix_UB_21      0.0611993000
_diffrn_orient_matrix_UB_22      0.0145372000
_diffrn_orient_matrix_UB_23      0.0035827000
_diffrn_orient_matrix_UB_31      -0.0008436000
_diffrn_orient_matrix_UB_32      0.0409116000
_diffrn_orient_matrix_UB_33      0.0361503000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\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                8992
_reflns_number_total             11983
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         11983
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0437
_refine_ls_restrained_S_all      1.058
_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)+(0.0449P)²+0.5545P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1076
_refine_special_details          
;Olex2 ByPass used to account for the DCM. This was preferable because the DCM 
seemed to be moving about in the void.,SQUEEZE
;
_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. Uiso/Uaniso restraints and constraints
Uanis(C48) = Uanis(C52A)
Uanis(C52) = Uanis(C48A)
Uanis(C49) = Uanis(C51A)
Uanis(C50) = Uanis(C50A)
Uanis(C51) = Uanis(C49A)
3. Others
 Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(C50A)=
 Sof(H50A)=Sof(H50B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=
 Sof(H52B)=1-FVAR(1)
 Sof(C48)=Sof(H48C)=Sof(H48D)=Sof(C49)=Sof(H49C)=Sof(H49D)=Sof(C50)=Sof(H50C)=
 Sof(H50D)=Sof(C51)=Sof(H51C)=Sof(H51D)=Sof(C52)=Sof(H52C)=Sof(H52D)=FVAR(1)
 Fixed X: O1W(0.45516) H1WA(0.47536) H1WB(0.384589)
 Fixed Y: O1W(0.76146) H1WA(0.756129) H1WB(0.77199)
 Fixed Z: O1W(0.7143) H1WA(0.66604) H1WB(0.71272)
4.a Free rotating group:
 N47(C48A,C49A,C50A,C51A,C52A)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C45(H45A,H45B), C46(H46A,H46B), C48A(H48A,H48B), C49A(H49A,H49B), C50A(H50A,
 H50B), C51A(H51A,H51B), C52A(H52A,H52B), C48(H48C,H48D), C49(H49C,H49D),
 C50(H50C,H50D), C51(H51C,H51D), C52(H52C,H52D), C54(H54A,H54B), C55(H55A,H55B),
  C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18),
 C21(H21), C23(H23)
;
_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 0.50984(2) 0.68653(2) 0.46567(2) 0.01680(7) Uani 1 1 d . . . . .
C3 C 0.33875(15) 0.45153(14) 0.41918(11) 0.0176(4) Uani 1 1 d . . . . .
C4 C 0.25792(15) 0.34992(15) 0.39704(11) 0.0197(4) Uani 1 1 d . . . . .
C5 C 0.17194(15) 0.32803(15) 0.44485(12) 0.0225(4) Uani 1 1 d . . . . .
H5 H 0.120271 0.260126 0.430003 0.027 Uiso 1 1 calc R U . . .
C6 C 0.16160(15) 0.40724(15) 0.51573(11) 0.0206(4) Uani 1 1 d . . . . .
C7 C 0.23735(15) 0.50599(14) 0.53990(11) 0.0200(4) Uani 1 1 d . . . . .
H7 H 0.229257 0.557922 0.588311 0.024 Uiso 1 1 calc R U . . .
C8 C 0.32701(15) 0.52924(14) 0.49209(11) 0.0185(4) Uani 1 1 d . . . . .
C9 C 0.42518(15) 0.47154(14) 0.36821(11) 0.0180(4) Uani 1 1 d . . . . .
H9 H 0.431292 0.413780 0.322931 0.022 Uiso 1 1 calc R U . . .
N10 N 0.49809(12) 0.56494(12) 0.37910(9) 0.0178(3) Uani 1 1 d . . . . .
C11 C 0.64108(15) 0.68718(14) 0.33768(11) 0.0181(4) Uani 1 1 d . . . . .
C12 C 0.72021(16) 0.71470(15) 0.28510(12) 0.0238(4) Uani 1 1 d . . . . .
H12 H 0.762889 0.786954 0.295879 0.029 Uiso 1 1 calc R U . . .
C13 C 0.73621(16) 0.63645(16) 0.21732(12) 0.0257(4) Uani 1 1 d . . . . .
H13 H 0.788863 0.655367 0.180965 0.031 Uiso 1 1 calc R U . . .
C14 C 0.67489(16) 0.52959(16) 0.20238(12) 0.0254(4) Uani 1 1 d . . . . .
H14 H 0.687086 0.476132 0.156123 0.031 Uiso 1 1 calc R U . . .
C15 C 0.59623(16) 0.50033(15) 0.25425(12) 0.0225(4) Uani 1 1 d . . . . .
H15 H 0.555684 0.427275 0.243935 0.027 Uiso 1 1 calc R U . . .
C16 C 0.57758(15) 0.57960(14) 0.32164(11) 0.0181(4) Uani 1 1 d . . . . .
N17 N 0.61561(12) 0.75685(12) 0.41010(9) 0.0176(3) Uani 1 1 d . . . . .
C18 C 0.65956(15) 0.86252(14) 0.43014(11) 0.0184(4) Uani 1 1 d . . . . .
H18 H 0.706598 0.890007 0.393493 0.022 Uiso 1 1 calc R U . . .
C19 C 0.64247(14) 0.93777(14) 0.50133(11) 0.0168(3) Uani 1 1 d . . . . .
C20 C 0.57723(14) 0.90512(14) 0.56298(11) 0.0175(4) Uani 1 1 d . . . . .
C21 C 0.56620(15) 0.98428(15) 0.63448(11) 0.0203(4) Uani 1 1 d . . . . .
H21 H 0.524737 0.963277 0.676265 0.024 Uiso 1 1 calc R U . . .
C22 C 0.61649(15) 1.09255(14) 0.64278(11) 0.0191(4) Uani 1 1 d . . . . .
C23 C 0.67810(15) 1.12820(15) 0.58168(11) 0.0207(4) Uani 1 1 d . . . . .
H23 H 0.710124 1.203408 0.588419 0.025 Uiso 1 1 calc R U . . .
C24 C 0.69048(15) 1.05219(15) 0.51288(11) 0.0187(4) Uani 1 1 d . . . . .
O25 O 0.74825(11) 1.07714(10) 0.44958(8) 0.0219(3) Uani 1 1 d . . . . .
C26 C 0.78432(16) 1.19246(14) 0.45175(11) 0.0215(4) Uani 1 1 d . . . . .
H26A H 0.833700 1.228030 0.504913 0.026 Uiso 1 1 calc R U . . .
H26B H 0.715080 1.229392 0.447886 0.026 Uiso 1 1 calc R U . . .
C27 C 0.85177(15) 1.20497(15) 0.38036(11) 0.0222(4) Uani 1 1 d . . . . .
H27A H 0.891781 1.281916 0.391174 0.027 Uiso 1 1 calc R U . . .
H27B H 0.912475 1.157220 0.379773 0.027 Uiso 1 1 calc R U . . .
N28 N 0.78317(13) 1.17825(12) 0.29752(10) 0.0221(3) Uani 1 1 d . . . . .
C29 C 0.7631(2) 1.05856(16) 0.26324(13) 0.0348(5) Uani 1 1 d . . . . .
H29A H 0.720173 1.021040 0.300355 0.042 Uiso 1 1 calc R U . . .
H29B H 0.838896 1.032215 0.260956 0.042 Uiso 1 1 calc R U . . .
C30 C 0.6944(2) 1.02866(19) 0.17684(13) 0.0424(6) Uani 1 1 d . . . . .
H30A H 0.616020 1.049316 0.179605 0.051 Uiso 1 1 calc R U . . .
H30B H 0.684965 0.948203 0.155085 0.051 Uiso 1 1 calc R U . . .
C31 C 0.7567(2) 1.08827(18) 0.11822(13) 0.0377(5) Uani 1 1 d . . . . .
H31A H 0.831702 1.062084 0.110590 0.045 Uiso 1 1 calc R U . . .
H31B H 0.708430 1.072505 0.063409 0.045 Uiso 1 1 calc R U . . .
C32 C 0.7779(2) 1.21152(18) 0.15534(13) 0.0342(5) Uani 1 1 d . . . . .
H32A H 0.822416 1.250426 0.119699 0.041 Uiso 1 1 calc R U . . .
H32B H 0.702573 1.238642 0.157908 0.041 Uiso 1 1 calc R U . . .
C33 C 0.84506(19) 1.23553(18) 0.24164(13) 0.0329(5) Uani 1 1 d . . . . .
H33A H 0.922121 1.212125 0.238248 0.039 Uiso 1 1 calc R U . . .
H33B H 0.857757 1.315769 0.265013 0.039 Uiso 1 1 calc R U . . .
O34 O 0.61118(11) 1.17527(10) 0.70900(8) 0.0241(3) Uani 1 1 d . . . . .
C35 C 0.54640(17) 1.14842(15) 0.77279(11) 0.0238(4) Uani 1 1 d . . . . .
H35A H 0.575420 1.087871 0.794318 0.029 Uiso 1 1 calc R U . . .
H35B H 0.462900 1.125466 0.750996 0.029 Uiso 1 1 calc R U . . .
C36 C 0.56440(17) 1.25231(15) 0.84042(12) 0.0242(4) Uani 1 1 d . . . . .
H36A H 0.647603 1.270839 0.863887 0.029 Uiso 1 1 calc R U . . .
H36B H 0.543468 1.313752 0.816097 0.029 Uiso 1 1 calc R U . . .
N37 N 0.49449(14) 1.24071(13) 0.90708(10) 0.0237(3) Uani 1 1 d . . . . .
C38 C 0.53962(19) 1.17169(17) 0.95993(12) 0.0299(4) Uani 1 1 d . . . . .
H38A H 0.618701 1.206391 0.987381 0.036 Uiso 1 1 calc R U . . .
H38B H 0.545240 1.099067 0.925296 0.036 Uiso 1 1 calc R U . . .
C39 C 0.4612(2) 1.15585(18) 1.02576(13) 0.0381(5) Uani 1 1 d . . . . .
H39A H 0.384125 1.115139 0.998460 0.046 Uiso 1 1 calc R U . . .
H39B H 0.495543 1.111585 1.061871 0.046 Uiso 1 1 calc R U . . .
C40 C 0.4465(2) 1.2661(2) 1.07818(14) 0.0437(6) Uani 1 1 d . . . . .
H40A H 0.521170 1.301877 1.112471 0.052 Uiso 1 1 calc R U . . .
H40B H 0.388111 1.254607 1.115725 0.052 Uiso 1 1 calc R U . . .
C41 C 0.4071(2) 1.3395(2) 1.02209(15) 0.0436(6) Uani 1 1 d . . . . .
H41A H 0.327429 1.308551 0.993882 0.052 Uiso 1 1 calc R U . . .
H41B H 0.405139 1.413524 1.055999 0.052 Uiso 1 1 calc R U . . .
C42 C 0.4883(2) 1.34914(16) 0.95771(13) 0.0322(5) Uani 1 1 d . . . . .
H42A H 0.460094 1.396331 0.921597 0.039 Uiso 1 1 calc R U . . .
H42B H 0.566910 1.384340 0.985787 0.039 Uiso 1 1 calc R U . . .
O43 O 0.52578(11) 0.80358(10) 0.55583(8) 0.0206(3) Uani 1 1 d . . . . .
O44 O 0.27232(11) 0.28019(10) 0.32586(8) 0.0246(3) Uani 1 1 d . . . . .
C45 C 0.19429(16) 0.17732(15) 0.30207(12) 0.0254(4) Uani 1 1 d . . . . .
H45A H 0.112657 0.190455 0.297935 0.030 Uiso 1 1 calc R U . . .
H45B H 0.206309 0.132544 0.343750 0.030 Uiso 1 1 calc R U . . .
C46 C 0.22001(17) 0.11809(16) 0.21884(12) 0.0282(4) Uani 1 1 d . . . . .
H46A H 0.225911 0.169868 0.181466 0.034 Uiso 1 1 calc R U . . .
H46B H 0.295609 0.091843 0.226028 0.034 Uiso 1 1 calc R U . . .
N47 N 0.12862(15) 0.02419(13) 0.18122(10) 0.0301(4) Uani 1 1 d G . . . .
C48A C 0.1858(13) -0.0314(13) 0.1146(9) 0.0436(7) Uani 0.059(2) 1 d G . P A 2
H48A H 0.271110 -0.014310 0.130515 0.052 Uiso 0.059(2) 1 calc R U P A 2
H48B H 0.166308 -0.004301 0.063847 0.052 Uiso 0.059(2) 1 calc R U P A 2
C49A C 0.147(2) -0.1565(11) 0.0968(17) 0.0493(7) Uani 0.059(2) 1 d G . P A 2
H49A H 0.185651 -0.192988 0.051118 0.059 Uiso 0.059(2) 1 calc R U P A 2
H49B H 0.169730 -0.184330 0.146591 0.059 Uiso 0.059(2) 1 calc R U P A 2
C50A C 0.015(2) -0.1840(13) 0.0727(16) 0.0448(7) Uani 0.059(2) 1 d G . P A 2
H50A H -0.007251 -0.164072 0.019394 0.054 Uiso 0.059(2) 1 calc R U P A 2
H50B H -0.010502 -0.263970 0.065908 0.054 Uiso 0.059(2) 1 calc R U P A 2
C51A C -0.0427(14) -0.1213(15) 0.1391(17) 0.0460(7) Uani 0.059(2) 1 d G . P A 2
H51A H -0.028127 -0.148368 0.190468 0.055 Uiso 0.059(2) 1 calc R U P A 2
H51B H -0.127716 -0.134237 0.121618 0.055 Uiso 0.059(2) 1 calc R U P A 2
C52A C 0.0031(3) 0.0028(13) 0.1568(13) 0.0424(7) Uani 0.059(2) 1 d G . P A 2
H52A H -0.016197 0.031048 0.106618 0.051 Uiso 0.059(2) 1 calc R U P A 2
H52B H -0.035168 0.041926 0.201708 0.051 Uiso 0.059(2) 1 calc R U P A 2
C48 C 0.1216(2) -0.06137(19) 0.22864(15) 0.0424(7) Uani 0.941(2) 1 d . . P A 1
H48C H 0.112350 -0.028824 0.286510 0.051 Uiso 0.941(2) 1 calc R U P A 1
H48D H 0.194661 -0.092856 0.229462 0.051 Uiso 0.941(2) 1 calc R U P A 1
C49 C 0.0187(2) -0.1529(2) 0.19064(16) 0.0460(7) Uani 0.941(2) 1 d . . P A 1
H49C H 0.016065 -0.210564 0.223217 0.055 Uiso 0.941(2) 1 calc R U P A 1
H49D H -0.054800 -0.122385 0.192548 0.055 Uiso 0.941(2) 1 calc R U P A 1
C50 C 0.0308(2) -0.2033(2) 0.10117(17) 0.0448(7) Uani 0.941(2) 1 d . . P A 1
H50C H 0.099565 -0.241216 0.099481 0.054 Uiso 0.941(2) 1 calc R U P A 1
H50D H -0.038898 -0.258001 0.075593 0.054 Uiso 0.941(2) 1 calc R U P A 1
C51 C 0.0442(3) -0.1130(2) 0.05348(16) 0.0493(7) Uani 0.941(2) 1 d . . P A 1
H51C H -0.028757 -0.081569 0.049478 0.059 Uiso 0.941(2) 1 calc R U P A 1
H51D H 0.058524 -0.144395 -0.003424 0.059 Uiso 0.941(2) 1 calc R U P A 1
C52 C 0.1449(2) -0.0216(2) 0.09588(14) 0.0436(7) Uani 0.941(2) 1 d . . P A 1
H52C H 0.218852 -0.051616 0.095705 0.052 Uiso 0.941(2) 1 calc R U P A 1
H52D H 0.149894 0.037423 0.064611 0.052 Uiso 0.941(2) 1 calc R U P A 1
O53 O 0.07103(11) 0.37789(11) 0.55661(8) 0.0283(3) Uani 1 1 d . . . . .
C54 C 0.05182(17) 0.45654(16) 0.62758(12) 0.0260(4) Uani 1 1 d . . . . .
H54A H 0.034989 0.524899 0.611426 0.031 Uiso 1 1 calc R U . . .
H54B H 0.121555 0.474991 0.669902 0.031 Uiso 1 1 calc R U . . .
C55 C -0.05149(17) 0.40380(16) 0.66174(12) 0.0272(4) Uani 1 1 d . . . . .
H55A H -0.118883 0.381201 0.617474 0.033 Uiso 1 1 calc R U . . .
H55B H -0.032249 0.336942 0.679196 0.033 Uiso 1 1 calc R U . . .
N56 N -0.08304(13) 0.47880(13) 0.73221(10) 0.0252(4) Uani 1 1 d . . . . .
C57 C 0.00040(17) 0.49491(18) 0.80738(13) 0.0319(5) Uani 1 1 d . . . . .
H57A H 0.079221 0.520907 0.795833 0.038 Uiso 1 1 calc R U . . .
H57B H 0.001643 0.423910 0.824057 0.038 Uiso 1 1 calc R U . . .
C58 C -0.03191(19) 0.5786(2) 0.87796(15) 0.0435(6) Uani 1 1 d . . . . .
H58A H -0.028264 0.650915 0.862735 0.052 Uiso 1 1 calc R U . . .
H58B H 0.024611 0.587151 0.928280 0.052 Uiso 1 1 calc R U . . .
C59 C -0.1550(2) 0.5415(2) 0.89632(15) 0.0455(6) Uani 1 1 d . . . . .
H59A H -0.156688 0.473946 0.918211 0.055 Uiso 1 1 calc R U . . .
H59B H -0.177685 0.599564 0.938554 0.055 Uiso 1 1 calc R U . . .
C60 C -0.23978(18) 0.51912(19) 0.81634(14) 0.0375(5) Uani 1 1 d . . . . .
H60A H -0.318201 0.489520 0.826554 0.045 Uiso 1 1 calc R U . . .
H60B H -0.244494 0.588779 0.798245 0.045 Uiso 1 1 calc R U . . .
C61 C -0.20044(16) 0.43732(17) 0.74863(13) 0.0282(4) Uani 1 1 d . . . . .
H61A H -0.199610 0.366471 0.765607 0.034 Uiso 1 1 calc R U . . .
H61B H -0.256107 0.424129 0.697278 0.034 Uiso 1 1 calc R U . . .
O62 O 0.39676(10) 0.62363(10) 0.51849(8) 0.0209(3) Uani 1 1 d . . . . .
O1W O 0.455160 0.761460 0.714300 0.0363(4) Uani 1 1 d . . . . .
H1WA H 0.475360 0.756129 0.666040 0.055 Uiso 1 1 d . U . . .
H1WB H 0.384589 0.771990 0.712720 0.055 Uiso 1 1 d . 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
Ni1 N10 1.8538(15) . ?
Ni1 N17 1.8604(14) . ?
Ni1 O43 1.8493(12) . ?
Ni1 O62 1.8461(12) . ?
C3 C4 1.442(2) . ?
C3 C8 1.426(2) . ?
C3 C9 1.418(2) . ?
C4 C5 1.382(2) . ?
C4 O44 1.363(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.408(3) . ?
C6 C7 1.386(2) . ?
C6 O53 1.370(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.419(2) . ?
C8 O62 1.313(2) . ?
C9 H9 0.9500 . ?
C9 N10 1.326(2) . ?
N10 C16 1.425(2) . ?
C11 C12 1.399(2) . ?
C11 C16 1.414(2) . ?
C11 N17 1.423(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.398(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.393(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.398(2) . ?
N17 C18 1.321(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.408(2) . ?
C19 C20 1.436(2) . ?
C19 C24 1.441(2) . ?
C20 C21 1.417(2) . ?
C20 O43 1.315(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.384(2) . ?
C22 C23 1.419(2) . ?
C22 O34 1.366(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.368(2) . ?
C24 O25 1.377(2) . ?
O25 C26 1.449(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.518(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 N28 1.472(2) . ?
N28 C29 1.475(2) . ?
N28 C33 1.480(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.522(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.534(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.524(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.516(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O34 C35 1.438(2) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.515(2) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 N37 1.466(2) . ?
N37 C38 1.465(2) . ?
N37 C42 1.465(2) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.529(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.521(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.522(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.519(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
O44 C45 1.438(2) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.514(3) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 N47 1.468(2) . ?
N47 C48A 1.4605 . ?
N47 C52A 1.4581 . ?
N47 C48 1.459(3) . ?
N47 C52 1.462(3) . ?
C48A H48A 0.9900 . ?
C48A H48B 0.9900 . ?
C48A C49A 1.5379 . ?
C49A H49A 0.9900 . ?
C49A H49B 0.9900 . ?
C49A C50A 1.5291 . ?
C50A H50A 0.9900 . ?
C50A H50B 0.9900 . ?
C50A C51A 1.4983 . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
C51A C52A 1.5396 . ?
C52A H52A 0.9900 . ?
C52A H52B 0.9900 . ?
C48 H48C 0.9900 . ?
C48 H48D 0.9900 . ?
C48 C49 1.534(3) . ?
C49 H49C 0.9900 . ?
C49 H49D 0.9900 . ?
C49 C50 1.524(3) . ?
C50 H50C 0.9900 . ?
C50 H50D 0.9900 . ?
C50 C51 1.515(4) . ?
C51 H51C 0.9900 . ?
C51 H51D 0.9900 . ?
C51 C52 1.531(3) . ?
C52 H52C 0.9900 . ?
C52 H52D 0.9900 . ?
O53 C54 1.436(2) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54 C55 1.522(2) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 N56 1.461(2) . ?
N56 C57 1.466(3) . ?
N56 C61 1.479(2) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.525(3) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.537(3) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.528(3) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.518(3) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
O1W H1WA 0.85350(5) . ?
O1W H1WB 0.85340(6) . ?

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
N10 Ni1 N17 86.29(6) . . ?
O43 Ni1 N10 176.79(6) . . ?
O43 Ni1 N17 94.82(6) . . ?
O62 Ni1 N10 95.10(6) . . ?
O62 Ni1 N17 175.52(6) . . ?
O62 Ni1 O43 84.02(5) . . ?
C8 C3 C4 117.84(15) . . ?
C9 C3 C4 119.71(16) . . ?
C9 C3 C8 122.45(16) . . ?
C5 C4 C3 121.30(16) . . ?
O44 C4 C3 114.94(15) . . ?
O44 C4 C5 123.75(16) . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.41(16) . . ?
C6 C5 H5 120.3 . . ?
C7 C6 C5 121.55(16) . . ?
O53 C6 C5 114.16(15) . . ?
O53 C6 C7 124.29(16) . . ?
C6 C7 H7 120.1 . . ?
C6 C7 C8 119.77(16) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C3 120.11(16) . . ?
O62 C8 C3 122.88(16) . . ?
O62 C8 C7 117.01(16) . . ?
C3 C9 H9 117.6 . . ?
N10 C9 C3 124.80(16) . . ?
N10 C9 H9 117.6 . . ?
C9 N10 Ni1 126.04(12) . . ?
C9 N10 C16 120.70(15) . . ?
C16 N10 Ni1 113.26(11) . . ?
C12 C11 C16 120.05(16) . . ?
C12 C11 N17 126.97(16) . . ?
C16 C11 N17 112.98(15) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.87(17) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.01(17) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 121.01(17) . . ?
C15 C14 H14 119.5 . . ?
C14 C15 H15 120.4 . . ?
C14 C15 C16 119.28(17) . . ?
C16 C15 H15 120.4 . . ?
C11 C16 N10 113.56(15) . . ?
C15 C16 N10 126.69(16) . . ?
C15 C16 C11 119.75(16) . . ?
C11 N17 Ni1 113.56(11) . . ?
C18 N17 Ni1 125.44(12) . . ?
C18 N17 C11 120.86(15) . . ?
N17 C18 H18 117.3 . . ?
N17 C18 C19 125.40(16) . . ?
C19 C18 H18 117.3 . . ?
C18 C19 C20 122.42(15) . . ?
C18 C19 C24 119.32(15) . . ?
C20 C19 C24 118.26(15) . . ?
C21 C20 C19 119.65(15) . . ?
O43 C20 C19 122.54(15) . . ?
O43 C20 C21 117.81(15) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 C20 119.27(16) . . ?
C22 C21 H21 120.4 . . ?
C21 C22 C23 122.48(16) . . ?
O34 C22 C21 124.08(16) . . ?
O34 C22 C23 113.44(15) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 C22 118.73(16) . . ?
C24 C23 H23 120.6 . . ?
C23 C24 C19 121.56(16) . . ?
C23 C24 O25 123.88(16) . . ?
O25 C24 C19 114.56(15) . . ?
C24 O25 C26 117.17(13) . . ?
O25 C26 H26A 109.6 . . ?
O25 C26 H26B 109.6 . . ?
O25 C26 C27 110.24(14) . . ?
H26A C26 H26B 108.1 . . ?
C27 C26 H26A 109.6 . . ?
C27 C26 H26B 109.6 . . ?
C26 C27 H27A 108.3 . . ?
C26 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
N28 C27 C26 116.02(15) . . ?
N28 C27 H27A 108.3 . . ?
N28 C27 H27B 108.3 . . ?
C27 N28 C29 110.60(15) . . ?
C27 N28 C33 109.69(14) . . ?
C29 N28 C33 109.81(16) . . ?
N28 C29 H29A 109.3 . . ?
N28 C29 H29B 109.3 . . ?
N28 C29 C30 111.77(18) . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 H29A 109.3 . . ?
C30 C29 H29B 109.3 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 C31 110.67(18) . . ?
H30A C30 H30B 108.1 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C30 C31 H31A 109.9 . . ?
C30 C31 H31B 109.9 . . ?
H31A C31 H31B 108.3 . . ?
C32 C31 C30 108.96(18) . . ?
C32 C31 H31A 109.9 . . ?
C32 C31 H31B 109.9 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 C31 110.17(18) . . ?
C33 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
N28 C33 C32 112.01(16) . . ?
N28 C33 H33A 109.2 . . ?
N28 C33 H33B 109.2 . . ?
C32 C33 H33A 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C22 O34 C35 117.73(14) . . ?
O34 C35 H35A 110.6 . . ?
O34 C35 H35B 110.6 . . ?
O34 C35 C36 105.86(14) . . ?
H35A C35 H35B 108.7 . . ?
C36 C35 H35A 110.6 . . ?
C36 C35 H35B 110.6 . . ?
C35 C36 H36A 109.2 . . ?
C35 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
N37 C36 C35 112.26(15) . . ?
N37 C36 H36A 109.2 . . ?
N37 C36 H36B 109.2 . . ?
C38 N37 C36 112.56(15) . . ?
C42 N37 C36 110.13(15) . . ?
C42 N37 C38 109.66(15) . . ?
N37 C38 H38A 109.4 . . ?
N37 C38 H38B 109.4 . . ?
N37 C38 C39 111.32(17) . . ?
H38A C38 H38B 108.0 . . ?
C39 C38 H38A 109.4 . . ?
C39 C38 H38B 109.4 . . ?
C38 C39 H39A 109.4 . . ?
C38 C39 H39B 109.4 . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 C38 110.96(17) . . ?
C40 C39 H39A 109.4 . . ?
C40 C39 H39B 109.4 . . ?
C39 C40 H40A 109.7 . . ?
C39 C40 H40B 109.7 . . ?
C39 C40 C41 109.63(19) . . ?
H40A C40 H40B 108.2 . . ?
C41 C40 H40A 109.7 . . ?
C41 C40 H40B 109.7 . . ?
C40 C41 H41A 109.4 . . ?
C40 C41 H41B 109.4 . . ?
H41A C41 H41B 108.0 . . ?
C42 C41 C40 111.12(19) . . ?
C42 C41 H41A 109.4 . . ?
C42 C41 H41B 109.4 . . ?
N37 C42 C41 110.86(17) . . ?
N37 C42 H42A 109.5 . . ?
N37 C42 H42B 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 108.1 . . ?
C20 O43 Ni1 128.01(11) . . ?
C4 O44 C45 116.71(14) . . ?
O44 C45 H45A 110.2 . . ?
O44 C45 H45B 110.2 . . ?
O44 C45 C46 107.39(15) . . ?
H45A C45 H45B 108.5 . . ?
C46 C45 H45A 110.2 . . ?
C46 C45 H45B 110.2 . . ?
C45 C46 H46A 109.4 . . ?
C45 C46 H46B 109.4 . . ?
H46A C46 H46B 108.0 . . ?
N47 C46 C45 111.10(16) . . ?
N47 C46 H46A 109.4 . . ?
N47 C46 H46B 109.4 . . ?
C48A N47 C46 100.0(6) . . ?
C52A N47 C46 138.5(6) . . ?
C52A N47 C48A 109.8 . . ?
C48 N47 C46 112.97(17) . . ?
C48 N47 C52 110.43(19) . . ?
C52 N47 C46 110.42(17) . . ?
N47 C48A H48A 109.5 . . ?
N47 C48A H48B 109.5 . . ?
N47 C48A C49A 110.6 . . ?
H48A C48A H48B 108.1 . . ?
C49A C48A H48A 109.5 . . ?
C49A C48A H48B 109.5 . . ?
C48A C49A H49A 109.6 . . ?
C48A C49A H49B 109.6 . . ?
H49A C49A H49B 108.2 . . ?
C50A C49A C48A 110.1 . . ?
C50A C49A H49A 109.6 . . ?
C50A C49A H49B 109.6 . . ?
C49A C50A H50A 109.8 . . ?
C49A C50A H50B 109.8 . . ?
H50A C50A H50B 108.3 . . ?
C51A C50A C49A 109.2 . . ?
C51A C50A H50A 109.8 . . ?
C51A C50A H50B 109.8 . . ?
C50A C51A H51A 109.4 . . ?
C50A C51A H51B 109.4 . . ?
C50A C51A C52A 111.3 . . ?
H51A C51A H51B 108.0 . . ?
C52A C51A H51A 109.4 . . ?
C52A C51A H51B 109.4 . . ?
N47 C52A C51A 110.6 . . ?
N47 C52A H52A 109.5 . . ?
N47 C52A H52B 109.5 . . ?
C51A C52A H52A 109.5 . . ?
C51A C52A H52B 109.5 . . ?
H52A C52A H52B 108.1 . . ?
N47 C48 H48C 109.5 . . ?
N47 C48 H48D 109.5 . . ?
N47 C48 C49 110.8(2) . . ?
H48C C48 H48D 108.1 . . ?
C49 C48 H48C 109.5 . . ?
C49 C48 H48D 109.5 . . ?
C48 C49 H49C 109.6 . . ?
C48 C49 H49D 109.6 . . ?
H49C C49 H49D 108.1 . . ?
C50 C49 C48 110.2(2) . . ?
C50 C49 H49C 109.6 . . ?
C50 C49 H49D 109.6 . . ?
C49 C50 H50C 109.8 . . ?
C49 C50 H50D 109.8 . . ?
H50C C50 H50D 108.3 . . ?
C51 C50 C49 109.2(2) . . ?
C51 C50 H50C 109.8 . . ?
C51 C50 H50D 109.8 . . ?
C50 C51 H51C 109.4 . . ?
C50 C51 H51D 109.4 . . ?
C50 C51 C52 111.2(2) . . ?
H51C C51 H51D 108.0 . . ?
C52 C51 H51C 109.4 . . ?
C52 C51 H51D 109.4 . . ?
N47 C52 C51 110.9(2) . . ?
N47 C52 H52C 109.5 . . ?
N47 C52 H52D 109.5 . . ?
C51 C52 H52C 109.5 . . ?
C51 C52 H52D 109.5 . . ?
H52C C52 H52D 108.0 . . ?
C6 O53 C54 117.41(14) . . ?
O53 C54 H54A 110.3 . . ?
O53 C54 H54B 110.3 . . ?
O53 C54 C55 106.93(14) . . ?
H54A C54 H54B 108.6 . . ?
C55 C54 H54A 110.3 . . ?
C55 C54 H54B 110.3 . . ?
C54 C55 H55A 109.2 . . ?
C54 C55 H55B 109.2 . . ?
H55A C55 H55B 107.9 . . ?
N56 C55 C54 111.89(15) . . ?
N56 C55 H55A 109.2 . . ?
N56 C55 H55B 109.2 . . ?
C55 N56 C57 112.60(16) . . ?
C55 N56 C61 109.93(15) . . ?
C57 N56 C61 109.63(15) . . ?
N56 C57 H57A 109.5 . . ?
N56 C57 H57B 109.5 . . ?
N56 C57 C58 110.89(18) . . ?
H57A C57 H57B 108.0 . . ?
C58 C57 H57A 109.5 . . ?
C58 C57 H57B 109.5 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 C59 110.68(19) . . ?
H58A C58 H58B 108.1 . . ?
C59 C58 H58A 109.5 . . ?
C59 C58 H58B 109.5 . . ?
C58 C59 H59A 109.9 . . ?
C58 C59 H59B 109.9 . . ?
H59A C59 H59B 108.3 . . ?
C60 C59 C58 108.95(19) . . ?
C60 C59 H59A 109.9 . . ?
C60 C59 H59B 109.9 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 108.1 . . ?
C61 C60 C59 110.58(18) . . ?
C61 C60 H60A 109.5 . . ?
C61 C60 H60B 109.5 . . ?
N56 C61 C60 110.90(16) . . ?
N56 C61 H61A 109.5 . . ?
N56 C61 H61B 109.5 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 108.0 . . ?
C8 O62 Ni1 128.19(11) . . ?
H1WA O1W H1WB 109.471(5) . . ?

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 N10 C16 C11 -5.87(19) . . . . ?
Ni1 N10 C16 C15 174.37(15) . . . . ?
Ni1 N17 C18 C19 6.4(3) . . . . ?
C3 C4 C5 C6 1.2(3) . . . . ?
C3 C4 O44 C45 179.30(16) . . . . ?
C3 C8 O62 Ni1 8.2(3) . . . . ?
C3 C9 N10 Ni1 3.8(3) . . . . ?
C3 C9 N10 C16 -176.24(16) . . . . ?
C4 C3 C8 C7 -0.6(3) . . . . ?
C4 C3 C8 O62 179.11(16) . . . . ?
C4 C3 C9 N10 174.71(17) . . . . ?
C4 C5 C6 C7 -1.4(3) . . . . ?
C4 C5 C6 O53 177.99(16) . . . . ?
C4 O44 C45 C46 175.66(15) . . . . ?
C5 C4 O44 C45 -1.8(3) . . . . ?
C5 C6 C7 C8 0.7(3) . . . . ?
C5 C6 O53 C54 -177.39(16) . . . . ?
C6 C7 C8 C3 0.3(3) . . . . ?
C6 C7 C8 O62 -179.37(17) . . . . ?
C6 O53 C54 C55 -179.31(16) . . . . ?
C7 C6 O53 C54 2.0(3) . . . . ?
C7 C8 O62 Ni1 -172.10(12) . . . . ?
C8 C3 C4 C5 -0.2(3) . . . . ?
C8 C3 C4 O44 178.73(15) . . . . ?
C8 C3 C9 N10 -4.5(3) . . . . ?
C9 C3 C4 C5 -179.43(17) . . . . ?
C9 C3 C4 O44 -0.5(2) . . . . ?
C9 C3 C8 C7 178.64(16) . . . . ?
C9 C3 C8 O62 -1.7(3) . . . . ?
C9 N10 C16 C11 174.15(16) . . . . ?
C9 N10 C16 C15 -5.6(3) . . . . ?
N10 Ni1 N17 C11 -4.19(12) . . . . ?
N10 Ni1 N17 C18 171.54(15) . . . . ?
N10 Ni1 O62 C8 -7.27(15) . . . . ?
C11 C12 C13 C14 -1.2(3) . . . . ?
C11 N17 C18 C19 -178.19(16) . . . . ?
C12 C11 C16 N10 -178.28(16) . . . . ?
C12 C11 C16 C15 1.5(3) . . . . ?
C12 C11 N17 Ni1 -177.22(15) . . . . ?
C12 C11 N17 C18 6.8(3) . . . . ?
C12 C13 C14 C15 0.8(3) . . . . ?
C13 C14 C15 C16 0.8(3) . . . . ?
C14 C15 C16 N10 177.88(17) . . . . ?
C14 C15 C16 C11 -1.9(3) . . . . ?
C16 C11 C12 C13 0.0(3) . . . . ?
C16 C11 N17 Ni1 1.90(19) . . . . ?
C16 C11 N17 C18 -174.05(16) . . . . ?
N17 Ni1 N10 C9 -174.44(15) . . . . ?
N17 Ni1 N10 C16 5.58(12) . . . . ?
N17 Ni1 O43 C20 12.16(15) . . . . ?
N17 C11 C12 C13 179.09(17) . . . . ?
N17 C11 C16 N10 2.5(2) . . . . ?
N17 C11 C16 C15 -177.68(15) . . . . ?
N17 C18 C19 C20 2.7(3) . . . . ?
N17 C18 C19 C24 -176.49(17) . . . . ?
C18 C19 C20 C21 178.08(16) . . . . ?
C18 C19 C20 O43 -2.3(3) . . . . ?
C18 C19 C24 C23 -178.80(17) . . . . ?
C18 C19 C24 O25 1.4(2) . . . . ?
C19 C20 C21 C22 1.4(3) . . . . ?
C19 C20 O43 Ni1 -7.2(2) . . . . ?
C19 C24 O25 C26 171.60(15) . . . . ?
C20 C19 C24 C23 2.0(3) . . . . ?
C20 C19 C24 O25 -177.83(15) . . . . ?
C20 C21 C22 C23 0.7(3) . . . . ?
C20 C21 C22 O34 180.00(16) . . . . ?
C21 C20 O43 Ni1 172.37(12) . . . . ?
C21 C22 C23 C24 -1.5(3) . . . . ?
C21 C22 O34 C35 -1.8(3) . . . . ?
C22 C23 C24 C19 0.1(3) . . . . ?
C22 C23 C24 O25 179.92(16) . . . . ?
C22 O34 C35 C36 175.26(15) . . . . ?
C23 C22 O34 C35 177.47(16) . . . . ?
C23 C24 O25 C26 -8.2(2) . . . . ?
C24 C19 C20 C21 -2.8(2) . . . . ?
C24 C19 C20 O43 176.82(16) . . . . ?
C24 O25 C26 C27 177.08(15) . . . . ?
O25 C26 C27 N28 72.2(2) . . . . ?
C26 C27 N28 C29 -82.2(2) . . . . ?
C26 C27 N28 C33 156.58(16) . . . . ?
C27 N28 C29 C30 -178.89(17) . . . . ?
C27 N28 C33 C32 -179.65(17) . . . . ?
N28 C29 C30 C31 57.2(3) . . . . ?
C29 N28 C33 C32 58.6(2) . . . . ?
C29 C30 C31 C32 -55.4(3) . . . . ?
C30 C31 C32 C33 55.8(2) . . . . ?
C31 C32 C33 N28 -58.6(2) . . . . ?
C33 N28 C29 C30 -57.7(2) . . . . ?
O34 C22 C23 C24 179.14(16) . . . . ?
O34 C35 C36 N37 174.77(15) . . . . ?
C35 C36 N37 C38 73.5(2) . . . . ?
C35 C36 N37 C42 -163.84(17) . . . . ?
C36 N37 C38 C39 -176.80(16) . . . . ?
C36 N37 C42 C41 174.72(18) . . . . ?
N37 C38 C39 C40 -56.8(2) . . . . ?
C38 N37 C42 C41 -60.9(2) . . . . ?
C38 C39 C40 C41 52.5(3) . . . . ?
C39 C40 C41 C42 -53.5(3) . . . . ?
C40 C41 C42 N37 58.3(3) . . . . ?
C42 N37 C38 C39 60.2(2) . . . . ?
O43 Ni1 N17 C11 172.78(12) . . . . ?
O43 Ni1 N17 C18 -11.48(15) . . . . ?
O43 Ni1 O62 C8 175.83(15) . . . . ?
O43 C20 C21 C22 -178.16(16) . . . . ?
O44 C4 C5 C6 -177.64(17) . . . . ?
O44 C45 C46 N47 -167.55(16) . . . . ?
C45 C46 N47 C48A -167.5(9) . . . . ?
C45 C46 N47 C52A 56.7(14) . . . . ?
C45 C46 N47 C48 -64.6(2) . . . . ?
C45 C46 N47 C52 171.19(19) . . . . ?
C46 N47 C48A C49A 148.0(7) . . . . ?
C46 N47 C52A C51A -166.4(10) . . . . ?
C46 N47 C48 C49 175.39(19) . . . . ?
C46 N47 C52 C51 -174.9(2) . . . . ?
N47 C48A C49A C50A 58.7 . . . . ?
N47 C48 C49 C50 58.5(3) . . . . ?
C48A N47 C52A C51A 60.4 . . . . ?
C48A C49A C50A C51A -54.7 . . . . ?
C49A C50A C51A C52A 54.4 . . . . ?
C50A C51A C52A N47 -57.9 . . . . ?
C52A N47 C48A C49A -61.4 . . . . ?
C48 N47 C52 C51 59.4(3) . . . . ?
C48 C49 C50 C51 -54.9(3) . . . . ?
C49 C50 C51 C52 54.5(3) . . . . ?
C50 C51 C52 N47 -57.1(3) . . . . ?
C52 N47 C48 C49 -60.4(3) . . . . ?
O53 C6 C7 C8 -178.70(17) . . . . ?
O53 C54 C55 N56 -177.16(16) . . . . ?
C54 C55 N56 C57 -73.0(2) . . . . ?
C54 C55 N56 C61 164.47(17) . . . . ?
C55 N56 C57 C58 176.75(17) . . . . ?
C55 N56 C61 C60 -174.69(17) . . . . ?
N56 C57 C58 C59 58.1(3) . . . . ?
C57 N56 C61 C60 61.0(2) . . . . ?
C57 C58 C59 C60 -54.3(3) . . . . ?
C58 C59 C60 C61 54.7(3) . . . . ?
C59 C60 C61 N56 -58.8(2) . . . . ?
C61 N56 C57 C58 -60.5(2) . . . . ?
O62 Ni1 N10 C9 1.29(15) . . . . ?
O62 Ni1 N10 C16 -178.69(12) . . . . ?
O62 Ni1 O43 C20 -163.50(15) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 41 electrons were 
found in a volume of 156Å³ in 2 voids per unit cell. 
This is consistent with the presence of 0.5[CH2Cl2] per Asymmetric Unit 
which account for 42 electrons per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 109.5 40.7 '1 dichloromethane'
2 0.217 0.596 0.972 22.7 0.0 ?
3 0.783 0.404 0.028 22.7 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'MiTeGen mount + Paratone-N'
_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 1.235
_oxdiff_exptl_absorpt_empirical_full_min 0.879
####################################################################### 
# 
# 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_exp_218_na
_database_code_depnum_ccdc_archive 'CCDC 2271795'
loop_
_audit_author_name
_audit_author_address
'Christopher Richardson'
;University of Wollongong
Australia
;
_audit_update_record             
;
2023-08-04 deposited with the CCDC.	2023-08-16 downloaded from the CCDC.
;
_audit_creation_date             2023-08-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            'compound (9) in manuscript'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H58 N6 Ni O10, 1.6(H2 O)'
_chemical_formula_sum            'C44 H61.20 N6 Ni O11.60'
_chemical_formula_weight         918.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         C44H48N6Ni1O10
_chemical_oxdiff_usercomment     Ni34
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           15
_space_group_name_H-M_alt        'C 1 2/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'
'-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                   30.6127(5)
_cell_length_b                   15.8401(3)
_cell_length_c                   9.8494(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.209(2)
_cell_angle_gamma                90
_cell_volume                     4748.04(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21460
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.3850
_cell_measurement_theta_min      2.3730
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.856
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_recrystallization_method 'Chloroform / Pet. spirit'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            64511
_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         29.575
_diffrn_reflns_theta_min         2.384
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'HyPix Bantam HPC'
_diffrn_detector_area_resol_mean 10
_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   20.00    --   20.00  54.00 120.00  368
  2  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00-120.00  368
  3  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00 -60.00  368
  4  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00-180.00  368
  5  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00  30.00  368
  6  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00  90.00  368
  7  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00-150.00  368
  8  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00 -30.00  368
  9  ω    -74.00 110.00   0.50   20.00    --   20.00  54.00  60.00  368
 10  ω    -74.00 -41.50   0.50   20.00    --   20.00  54.00 -90.00   65
;
_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      -0.0230724000
_diffrn_orient_matrix_UB_12      0.0061373000
_diffrn_orient_matrix_UB_13      -0.0093862000
_diffrn_orient_matrix_UB_21      -0.0014339000
_diffrn_orient_matrix_UB_22      -0.0128468000
_diffrn_orient_matrix_UB_23      0.0683758000
_diffrn_orient_matrix_UB_31      0.0028975000
_diffrn_orient_matrix_UB_32      0.0424664000
_diffrn_orient_matrix_UB_33      0.0220346000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\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                5665
_reflns_number_total             6653
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         6653
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0308
_refine_ls_restrained_S_all      1.035
_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)+(0.0387P)²+3.0887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0821
_refine_special_details          SQUEEZE
_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. Others
 Fixed Sof: O1W(0.8) H1WA(0.8) H1WB(0.8)
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C9(H9)
;
_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 0.500000 0.53716(2) 0.250000 0.01640(6) Uani 1 2 d S T P . .
O1 O 0.52590(3) 0.62390(5) 0.16368(8) 0.02093(17) Uani 1 1 d . . . . .
O2 O 0.61585(3) 0.46760(5) -0.11097(9) 0.02228(17) Uani 1 1 d . . . . .
O3 O 0.69667(4) 0.18680(6) 0.08063(10) 0.0394(3) Uani 1 1 d . . . . .
O4 O 0.62413(3) 0.76591(5) -0.09888(9) 0.02636(19) Uani 1 1 d . . . . .
O5 O 0.75462(3) 0.91201(6) 0.15923(10) 0.0332(2) Uani 1 1 d . . . . .
N1 N 0.52732(3) 0.45221(6) 0.16156(10) 0.01711(18) Uani 1 1 d . . . . .
N2 N 0.66234(3) 0.31507(6) -0.10541(10) 0.0237(2) Uani 1 1 d . . . . .
N3 N 0.68055(3) 0.92997(6) -0.03880(10) 0.0227(2) Uani 1 1 d . . . . .
C1 C 0.51476(4) 0.21854(8) 0.20109(13) 0.0253(2) Uani 1 1 d . . . . .
H1 H 0.524668 0.166459 0.167672 0.030 Uiso 1 1 calc R U . . .
C2 C 0.52982(4) 0.29370(8) 0.15203(12) 0.0224(2) Uani 1 1 d . . . . .
H2 H 0.550077 0.293417 0.085460 0.027 Uiso 1 1 calc R U . . .
C3 C 0.51501(3) 0.36999(7) 0.20115(11) 0.0178(2) Uani 1 1 d . . . . .
C4 C 0.55561(4) 0.46248(7) 0.07199(11) 0.0180(2) Uani 1 1 d . . . . .
H4 H 0.566769 0.413159 0.033051 0.022 Uiso 1 1 calc R U . . .
C5 C 0.57076(3) 0.54138(7) 0.02897(11) 0.0177(2) Uani 1 1 d . . . . .
C6 C 0.60354(4) 0.54432(7) -0.06478(11) 0.0185(2) Uani 1 1 d . . . . .
C7 C 0.62077(4) 0.61926(7) -0.10346(12) 0.0213(2) Uani 1 1 d . . . . .
H7 H 0.643239 0.619948 -0.162853 0.026 Uiso 1 1 calc R U . . .
C8 C 0.60461(4) 0.69553(7) -0.05371(12) 0.0208(2) Uani 1 1 d . . . . .
C9 C 0.57248(4) 0.69637(7) 0.03332(12) 0.0206(2) Uani 1 1 d . . . . .
H9 H 0.561783 0.748544 0.063926 0.025 Uiso 1 1 calc R U . . .
C10 C 0.55535(4) 0.61944(7) 0.07723(11) 0.0182(2) Uani 1 1 d . . . . .
C11 C 0.65524(4) 0.46597(8) -0.17721(12) 0.0225(2) Uani 1 1 d . . . . .
H11A H 0.680020 0.488931 -0.115231 0.027 Uiso 1 1 calc R U . . .
H11B H 0.651515 0.501494 -0.260360 0.027 Uiso 1 1 calc R U . . .
C12 C 0.66506(4) 0.37612(8) -0.21516(12) 0.0240(2) Uani 1 1 d . . . . .
H12A H 0.644150 0.359250 -0.294253 0.029 Uiso 1 1 calc R U . . .
H12B H 0.694993 0.373918 -0.244287 0.029 Uiso 1 1 calc R U . . .
C13 C 0.69052(5) 0.33565(9) 0.02005(13) 0.0296(3) Uani 1 1 d . . . . .
H13A H 0.682250 0.391489 0.054494 0.035 Uiso 1 1 calc R U . . .
H13B H 0.721574 0.338363 0.000861 0.035 Uiso 1 1 calc R U . . .
C14 C 0.68529(6) 0.26867(9) 0.12657(14) 0.0372(3) Uani 1 1 d . . . . .
H14A H 0.704288 0.282752 0.211338 0.045 Uiso 1 1 calc R U . . .
H14B H 0.654444 0.268088 0.148129 0.045 Uiso 1 1 calc R U . . .
C15 C 0.67002(6) 0.16630(9) -0.04232(16) 0.0417(4) Uani 1 1 d . . . . .
H15A H 0.638897 0.163076 -0.023985 0.050 Uiso 1 1 calc R U . . .
H15B H 0.678661 0.110212 -0.074797 0.050 Uiso 1 1 calc R U . . .
C16 C 0.67458(5) 0.23129(9) -0.15224(14) 0.0349(3) Uani 1 1 d . . . . .
H16A H 0.705325 0.232386 -0.174719 0.042 Uiso 1 1 calc R U . . .
H16B H 0.655374 0.215877 -0.235934 0.042 Uiso 1 1 calc R U . . .
C17 C 0.60873(4) 0.84618(8) -0.05671(14) 0.0262(2) Uani 1 1 d . . . . .
H17A H 0.610927 0.849069 0.044202 0.031 Uiso 1 1 calc R U . . .
H17B H 0.577577 0.854202 -0.093109 0.031 Uiso 1 1 calc R U . . .
C18 C 0.63711(4) 0.91477(8) -0.11161(13) 0.0271(3) Uani 1 1 d . . . . .
H18A H 0.641064 0.900401 -0.207330 0.033 Uiso 1 1 calc R U . . .
H18B H 0.620475 0.968437 -0.113490 0.033 Uiso 1 1 calc R U . . .
C19 C 0.71102(4) 0.85925(8) -0.04320(14) 0.0287(3) Uani 1 1 d . . . . .
H19A H 0.712615 0.841832 -0.139073 0.034 Uiso 1 1 calc R U . . .
H19B H 0.700507 0.810538 0.007221 0.034 Uiso 1 1 calc R U . . .
C20 C 0.75598(4) 0.88595(9) 0.02085(15) 0.0322(3) Uani 1 1 d . . . . .
H20A H 0.776722 0.838185 0.018027 0.039 Uiso 1 1 calc R U . . .
H20B H 0.766812 0.933120 -0.032321 0.039 Uiso 1 1 calc R U . . .
C21 C 0.72509(5) 0.98108(9) 0.16405(14) 0.0309(3) Uani 1 1 d . . . . .
H21A H 0.735898 1.029536 0.113699 0.037 Uiso 1 1 calc R U . . .
H21B H 0.724119 0.998529 0.260191 0.037 Uiso 1 1 calc R U . . .
C22 C 0.67924(4) 0.95784(8) 0.10198(13) 0.0275(3) Uani 1 1 d . . . . .
H22A H 0.667431 0.912080 0.155932 0.033 Uiso 1 1 calc R U . . .
H22B H 0.659608 1.007397 0.103951 0.033 Uiso 1 1 calc R U . . .
O1W O 0.57080(4) 0.73372(8) 0.37043(14) 0.0366(3) Uani 0.8 1 d G . P . .
H1WA H 0.596031 0.710790 0.382401 0.055 Uiso 0.8 1 d G U P . .
H1WB H 0.555399 0.699848 0.318215 0.055 Uiso 0.8 1 d G U 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 O1 1.8399(8) . ?
Ni1 O1 1.8400(8) 2_655 ?
Ni1 N1 1.8511(9) 2_655 ?
Ni1 N1 1.8511(9) . ?
O1 C10 1.3073(13) . ?
O2 C6 1.3649(14) . ?
O2 C11 1.4321(13) . ?
O3 C14 1.4290(17) . ?
O3 C15 1.4226(19) . ?
O4 C8 1.3620(14) . ?
O4 C17 1.4331(15) . ?
O5 C20 1.4290(17) . ?
O5 C21 1.4232(17) . ?
N1 C3 1.4220(14) . ?
N1 C4 1.3114(14) . ?
N2 C12 1.4595(16) . ?
N2 C13 1.4653(16) . ?
N2 C16 1.4669(16) . ?
N3 C18 1.4610(16) . ?
N3 C19 1.4614(16) . ?
N3 C22 1.4599(16) . ?
C1 C1 1.391(3) 2_655 ?
C1 H1 0.9500 . ?
C1 C2 1.3826(17) . ?
C2 H2 0.9500 . ?
C2 C3 1.3954(15) . ?
C3 C3 1.401(2) 2_655 ?
C4 H4 0.9500 . ?
C4 C5 1.4139(15) . ?
C5 C6 1.4362(15) . ?
C5 C10 1.4233(15) . ?
C6 C7 1.3695(16) . ?
C7 H7 0.9500 . ?
C7 C8 1.4131(16) . ?
C8 C9 1.3731(16) . ?
C9 H9 0.9500 . ?
C9 C10 1.4127(15) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.5100(17) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.5127(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.511(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.5262(17) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.5111(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.5146(19) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8499 . ?

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 O1 83.37(5) . 2_655 ?
O1 Ni1 N1 94.94(4) . . ?
O1 Ni1 N1 178.24(4) 2_655 . ?
O1 Ni1 N1 178.24(4) . 2_655 ?
O1 Ni1 N1 94.95(4) 2_655 2_655 ?
N1 Ni1 N1 86.74(6) 2_655 . ?
C10 O1 Ni1 128.51(7) . . ?
C6 O2 C11 116.38(9) . . ?
C15 O3 C14 109.85(11) . . ?
C8 O4 C17 117.50(9) . . ?
C21 O5 C20 109.76(10) . . ?
C3 N1 Ni1 112.96(7) . . ?
C4 N1 Ni1 126.24(8) . . ?
C4 N1 C3 120.80(9) . . ?
C12 N2 C13 113.68(10) . . ?
C12 N2 C16 109.24(10) . . ?
C13 N2 C16 108.62(10) . . ?
C18 N3 C19 114.15(10) . . ?
C22 N3 C18 113.52(10) . . ?
C22 N3 C19 110.07(10) . . ?
C1 C1 H1 119.7 2_655 . ?
C2 C1 C1 120.56(7) . 2_655 ?
C2 C1 H1 119.7 . . ?
C1 C2 H2 120.3 . . ?
C1 C2 C3 119.43(11) . . ?
C3 C2 H2 120.3 . . ?
C2 C3 N1 126.32(10) . . ?
C2 C3 C3 120.01(7) . 2_655 ?
C3 C3 N1 113.67(6) 2_655 . ?
N1 C4 H4 117.5 . . ?
N1 C4 C5 124.97(10) . . ?
C5 C4 H4 117.5 . . ?
C4 C5 C6 119.74(10) . . ?
C4 C5 C10 122.45(10) . . ?
C10 C5 C6 117.80(10) . . ?
O2 C6 C5 115.01(10) . . ?
O2 C6 C7 123.40(10) . . ?
C7 C6 C5 121.59(10) . . ?
C6 C7 H7 120.5 . . ?
C6 C7 C8 119.00(10) . . ?
C8 C7 H7 120.5 . . ?
O4 C8 C7 113.84(10) . . ?
O4 C8 C9 124.42(11) . . ?
C9 C8 C7 121.74(11) . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.84(11) . . ?
C10 C9 H9 120.1 . . ?
O1 C10 C5 122.77(10) . . ?
O1 C10 C9 117.24(10) . . ?
C9 C10 C5 119.98(10) . . ?
O2 C11 H11A 109.8 . . ?
O2 C11 H11B 109.8 . . ?
O2 C11 C12 109.25(10) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.8 . . ?
C12 C11 H11B 109.8 . . ?
N2 C12 C11 114.35(10) . . ?
N2 C12 H12A 108.7 . . ?
N2 C12 H12B 108.7 . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
N2 C13 H13A 109.8 . . ?
N2 C13 H13B 109.8 . . ?
N2 C13 C14 109.39(12) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
O3 C14 C13 111.66(11) . . ?
O3 C14 H14A 109.3 . . ?
O3 C14 H14B 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
O3 C15 H15A 109.3 . . ?
O3 C15 H15B 109.3 . . ?
O3 C15 C16 111.43(13) . . ?
H15A C15 H15B 108.0 . . ?
C16 C15 H15A 109.3 . . ?
C16 C15 H15B 109.3 . . ?
N2 C16 C15 110.14(11) . . ?
N2 C16 H16A 109.6 . . ?
N2 C16 H16B 109.6 . . ?
C15 C16 H16A 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
O4 C17 H17A 110.1 . . ?
O4 C17 H17B 110.1 . . ?
O4 C17 C18 108.13(10) . . ?
H17A C17 H17B 108.4 . . ?
C18 C17 H17A 110.1 . . ?
C18 C17 H17B 110.1 . . ?
N3 C18 C17 117.79(10) . . ?
N3 C18 H18A 107.9 . . ?
N3 C18 H18B 107.9 . . ?
C17 C18 H18A 107.9 . . ?
C17 C18 H18B 107.9 . . ?
H18A C18 H18B 107.2 . . ?
N3 C19 H19A 109.8 . . ?
N3 C19 H19B 109.8 . . ?
N3 C19 C20 109.18(10) . . ?
H19A C19 H19B 108.3 . . ?
C20 C19 H19A 109.8 . . ?
C20 C19 H19B 109.8 . . ?
O5 C20 C19 111.08(11) . . ?
O5 C20 H20A 109.4 . . ?
O5 C20 H20B 109.4 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
O5 C21 H21A 109.4 . . ?
O5 C21 H21B 109.4 . . ?
O5 C21 C22 111.34(11) . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
N3 C22 C21 109.72(10) . . ?
N3 C22 H22A 109.7 . . ?
N3 C22 H22B 109.7 . . ?
C21 C22 H22A 109.7 . . ?
C21 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
H1WA O1W H1WB 104.5 . . ?

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 C10 C5 3.77(16) . . . . ?
Ni1 O1 C10 C9 -175.27(8) . . . . ?
Ni1 N1 C3 C2 179.63(9) . . . . ?
Ni1 N1 C3 C3 -0.22(15) . . . 2_655 ?
Ni1 N1 C4 C5 1.12(17) . . . . ?
O1 Ni1 O1 C10 175.83(12) 2_655 . . . ?
O1 Ni1 N1 C3 -179.42(7) . . . . ?
O1 Ni1 N1 C4 1.19(10) . . . . ?
O2 C6 C7 C8 177.65(10) . . . . ?
O2 C11 C12 N2 -47.61(14) . . . . ?
O3 C15 C16 N2 -58.44(17) . . . . ?
O4 C8 C9 C10 -178.05(11) . . . . ?
O4 C17 C18 N3 -78.53(14) . . . . ?
O5 C21 C22 N3 -57.60(14) . . . . ?
N1 Ni1 O1 C10 -3.65(10) . . . . ?
N1 Ni1 N1 C3 0.08(5) 2_655 . . . ?
N1 Ni1 N1 C4 -179.31(12) 2_655 . . . ?
N1 C4 C5 C6 176.81(10) . . . . ?
N1 C4 C5 C10 -1.90(18) . . . . ?
N2 C13 C14 O3 59.12(16) . . . . ?
N3 C19 C20 O5 59.10(15) . . . . ?
C1 C1 C2 C3 -0.2(2) 2_655 . . . ?
C1 C2 C3 N1 179.87(11) . . . . ?
C1 C2 C3 C3 -0.3(2) . . . 2_655 ?
C3 N1 C4 C5 -178.23(10) . . . . ?
C4 N1 C3 C2 -0.94(17) . . . . ?
C4 N1 C3 C3 179.21(12) . . . 2_655 ?
C4 C5 C6 O2 3.40(15) . . . . ?
C4 C5 C6 C7 -176.54(10) . . . . ?
C4 C5 C10 O1 -0.60(17) . . . . ?
C4 C5 C10 C9 178.41(10) . . . . ?
C5 C6 C7 C8 -2.41(17) . . . . ?
C6 O2 C11 C12 177.22(9) . . . . ?
C6 C5 C10 O1 -179.34(10) . . . . ?
C6 C5 C10 C9 -0.33(16) . . . . ?
C6 C7 C8 O4 180.00(10) . . . . ?
C6 C7 C8 C9 0.67(18) . . . . ?
C7 C8 C9 C10 1.20(17) . . . . ?
C8 O4 C17 C18 176.44(10) . . . . ?
C8 C9 C10 O1 177.73(10) . . . . ?
C8 C9 C10 C5 -1.33(17) . . . . ?
C10 C5 C6 O2 -177.82(9) . . . . ?
C10 C5 C6 C7 2.24(16) . . . . ?
C11 O2 C6 C5 -165.49(10) . . . . ?
C11 O2 C6 C7 14.45(16) . . . . ?
C12 N2 C13 C14 -179.92(11) . . . . ?
C12 N2 C16 C15 -177.46(12) . . . . ?
C13 N2 C12 C11 -55.78(14) . . . . ?
C13 N2 C16 C15 58.04(16) . . . . ?
C14 O3 C15 C16 57.47(17) . . . . ?
C15 O3 C14 C13 -58.12(17) . . . . ?
C16 N2 C12 C11 -177.26(11) . . . . ?
C16 N2 C13 C14 -58.09(14) . . . . ?
C17 O4 C8 C7 178.10(10) . . . . ?
C17 O4 C8 C9 -2.60(17) . . . . ?
C18 N3 C19 C20 173.49(11) . . . . ?
C18 N3 C22 C21 -173.86(10) . . . . ?
C19 N3 C18 C17 65.37(15) . . . . ?
C19 N3 C22 C21 56.79(13) . . . . ?
C20 O5 C21 C22 58.59(14) . . . . ?
C21 O5 C20 C19 -59.50(14) . . . . ?
C22 N3 C18 C17 -61.88(15) . . . . ?
C22 N3 C19 C20 -57.50(14) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 -0.633 343.3 106.9 '2 chloroform'
2 0.500 0.000 -0.972 343.3 106.9 '2 chloroform'

_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 1.105
_oxdiff_exptl_absorpt_empirical_full_min 0.927
