# Electronic Supplementary Material (ESI) for Materials Chemistry Frontiers.
# This journal is © the Partner Organisations 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_mandeep202006a_ni_113k2_0m
_database_code_depnum_ccdc_archive 'CCDC 2107801'
loop_
_audit_author_name
_audit_author_address
'Yoshitaka Matsushita'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_mandeep202006a_ni_113k2_0m 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Due to lower crystallinity and weaker peaks in wide angle region
;
_vrf_PLAT414_mandeep202006a_ni_113k2_0m 
;
PROBLEM: Short Intra D-H..H-X       H1       ..H18C     .       1.85 Ang.
RESPONSE: H1 was placed using a riding model and is too close to H18C
;
# Added during the CSD deposition process: Monday 28 November 2022 05:33 AM
# end Validation Reply Form

_audit_creation_date             2022-11-22
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C83 H88 N10 Ni O4, C7 H8'
_chemical_formula_sum            'C90 H96 N10 Ni O4'
_chemical_formula_weight         1440.47
_chemical_melting_point          ?
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      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                   14.6234(10)
_cell_length_b                   20.9545(15)
_cell_length_c                   21.2618(15)
_cell_angle_alpha                116.543(4)
_cell_angle_beta                 98.928(4)
_cell_angle_gamma                99.929(4)
_cell_volume                     5538.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    9440
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      20.12
_shelx_estimated_absorpt_T_max   0.993
_shelx_estimated_absorpt_T_min   0.959
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9774
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_process_details   
;
CrystalClear (Rigaku, 1997--2002)
;
_exptl_crystal_description       Platelet
_exptl_crystal_colour            'Dark purple'
_exptl_crystal_density_diffrn    0.864
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.032
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33208
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        20.176
_diffrn_reflns_theta_max         20.176
_diffrn_reflns_theta_min         1.940
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7140
_reflns_number_total             10418
_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_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         10418
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0701
_refine_ls_restrained_S_all      1.027
_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)+(0.1278P)²+8.0226P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.2189
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 C68, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C68) = Uanis(C69) = Uanis(C73) = Uanis(C75) = Uanis(C74)
Uanis(C69) = Uanis(C1)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C11(H11), C21(H21), C22(H22), C26(H26), C30(H30),
 C40(H40), C51(H51), C55(H55), C66(H66), C67(H67), C71(H71), C75(H75), C88(H88),
  C87(H87), C89(H89), C90(H90), C91(H91)
4.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,
 H59C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C77(H77A,
 H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C),
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3602(4) 0.3294(3) 0.7938(3) 0.0285(6) Uani 1 1 d . . . . .
C2 C 0.3033(4) 0.2645(3) 0.7872(3) 0.0307(16) Uani 1 1 d . . . . .
H2 H 0.257394 0.261969 0.813701 0.037 Uiso 1 1 calc R U . . .
C3 C 0.3256(4) 0.2056(4) 0.7362(3) 0.0350(16) Uani 1 1 d . . . . .
H3 H 0.297221 0.154624 0.719509 0.042 Uiso 1 1 calc R U . . .
C4 C 0.3999(4) 0.2354(4) 0.7126(3) 0.0267(15) Uani 1 1 d . . . . .
C5 C 0.4587(4) 0.1967(3) 0.6728(3) 0.0277(15) Uani 1 1 d . . . . .
C6 C 0.4237(4) 0.1150(3) 0.6324(3) 0.0305(16) Uani 1 1 d . . . . .
C7 C 0.3342(5) 0.0808(4) 0.5834(4) 0.0378(17) Uani 1 1 d . . . . .
H7 H 0.297265 0.111210 0.576172 0.045 Uiso 1 1 calc R U . . .
C8 C 0.2953(5) 0.0055(4) 0.5445(4) 0.0460(19) Uani 1 1 d . . . . .
C9 C 0.3500(5) -0.0383(4) 0.5568(3) 0.0347(17) Uani 1 1 d . . . . .
C10 C 0.4422(4) -0.0074(4) 0.6070(3) 0.0325(16) Uani 1 1 d . . . . .
C11 C 0.4758(4) 0.0689(4) 0.6433(3) 0.0329(16) Uani 1 1 d . . . . .
H11 H 0.537230 0.091343 0.677453 0.039 Uiso 1 1 calc R U . . .
C12 C 0.1926(5) -0.0286(4) 0.4924(5) 0.065(2) Uani 1 1 d . . . . .
C13 C 0.1925(6) -0.0845(4) 0.4159(4) 0.081(3) Uani 1 1 d . . . . .
H13A H 0.127774 -0.101873 0.383352 0.122 Uiso 1 1 calc R U . . .
H13B H 0.211684 -0.126676 0.416805 0.122 Uiso 1 1 calc R U . . .
H13C H 0.238051 -0.060805 0.398223 0.122 Uiso 1 1 calc R U . . .
C14 C 0.1254(6) -0.0647(5) 0.5235(6) 0.099(4) Uani 1 1 d . . . . .
H14A H 0.066517 -0.098133 0.485141 0.149 Uiso 1 1 calc R U . . .
H14B H 0.108879 -0.025978 0.563768 0.149 Uiso 1 1 calc R U . . .
H14C H 0.157905 -0.092865 0.541329 0.149 Uiso 1 1 calc R U . . .
C15 C 0.1519(5) 0.0309(5) 0.4845(6) 0.097(3) Uani 1 1 d . . . . .
H15A H 0.087401 0.007671 0.450780 0.145 Uiso 1 1 calc R U . . .
H15B H 0.194094 0.055336 0.465525 0.145 Uiso 1 1 calc R U . . .
H15C H 0.148082 0.067692 0.532258 0.145 Uiso 1 1 calc R U . . .
C16 C 0.5045(5) -0.0543(4) 0.6202(4) 0.0449(18) Uani 1 1 d . . . . .
C17 C 0.6019(6) -0.0048(4) 0.6787(4) 0.069(2) Uani 1 1 d . . . . .
H17A H 0.639224 -0.036544 0.686309 0.103 Uiso 1 1 calc R U . . .
H17B H 0.589091 0.027740 0.724644 0.103 Uiso 1 1 calc R U . . .
H17C H 0.638421 0.025332 0.661778 0.103 Uiso 1 1 calc R U . . .
C18 C 0.5310(5) -0.1021(4) 0.5499(4) 0.055(2) Uani 1 1 d . . . . .
H18A H 0.573772 -0.129738 0.559522 0.082 Uiso 1 1 calc R U . . .
H18B H 0.563772 -0.070013 0.533274 0.082 Uiso 1 1 calc R U . . .
H18C H 0.472325 -0.136951 0.512145 0.082 Uiso 1 1 calc R U . . .
C19 C 0.4517(7) -0.1015(4) 0.6503(4) 0.076(3) Uani 1 1 d . . . . .
H19A H 0.491683 -0.131758 0.657948 0.114 Uiso 1 1 calc R U . . .
H19B H 0.389998 -0.134031 0.615050 0.114 Uiso 1 1 calc R U . . .
H19C H 0.440214 -0.068514 0.696623 0.114 Uiso 1 1 calc R U . . .
C20 C 0.5473(4) 0.2339(4) 0.6722(3) 0.0283(16) Uani 1 1 d . . . . .
C21 C 0.6226(4) 0.2030(4) 0.6474(3) 0.0344(16) Uani 1 1 d . . . . .
H21 H 0.618609 0.151636 0.621583 0.041 Uiso 1 1 calc R U . . .
C22 C 0.7016(4) 0.2603(4) 0.6675(3) 0.0315(16) Uani 1 1 d . . . . .
H22 H 0.763227 0.256850 0.659825 0.038 Uiso 1 1 calc R U . . .
C23 C 0.6727(4) 0.3258(3) 0.7021(3) 0.0273(15) Uani 1 1 d . . . . .
C24 C 0.7274(4) 0.4007(4) 0.7242(3) 0.0309(16) Uani 1 1 d . . . . .
C25 C 0.8242(4) 0.4311(3) 0.7634(3) 0.0256(15) Uani 1 1 d . . . . .
C26 C 0.8750(4) 0.3899(3) 0.7877(3) 0.0289(15) Uani 1 1 d . . . . .
H26 H 0.840697 0.342035 0.777551 0.035 Uiso 1 1 calc R U . . .
C27 C 0.9691(4) 0.4158(3) 0.8244(3) 0.0301(16) Uani 1 1 d . . . . .
C28 C 1.0225(5) 0.4908(4) 0.8411(3) 0.0342(17) Uani 1 1 d . . . . .
C29 C 0.9695(4) 0.5361(3) 0.8212(3) 0.0309(16) Uani 1 1 d . . . . .
C30 C 0.8744(4) 0.5048(4) 0.7843(3) 0.0323(16) Uani 1 1 d . . . . .
H30 H 0.840003 0.533971 0.771999 0.039 Uiso 1 1 calc R U . . .
C31 C 1.0200(4) 0.3706(4) 0.8505(4) 0.0401(18) Uani 1 1 d . . . . .
C32 C 0.9529(4) 0.2958(4) 0.8300(4) 0.0480(19) Uani 1 1 d . . . . .
H32A H 0.988701 0.268803 0.847353 0.072 Uiso 1 1 calc R U . . .
H32B H 0.927667 0.266836 0.776869 0.072 Uiso 1 1 calc R U . . .
H32C H 0.899392 0.303872 0.852506 0.072 Uiso 1 1 calc R U . . .
C33 C 1.1024(5) 0.3535(4) 0.8127(5) 0.059(2) Uani 1 1 d . . . . .
H33A H 1.133592 0.322726 0.827393 0.089 Uiso 1 1 calc R U . . .
H33B H 1.149868 0.400125 0.827175 0.089 Uiso 1 1 calc R U . . .
H33C H 1.075716 0.327026 0.759683 0.089 Uiso 1 1 calc R U . . .
C34 C 1.0594(5) 0.4130(4) 0.9335(4) 0.064(2) Uani 1 1 d . . . . .
H34A H 1.093234 0.383864 0.949123 0.096 Uiso 1 1 calc R U . . .
H34B H 1.006092 0.421311 0.956210 0.096 Uiso 1 1 calc R U . . .
H34C H 1.104211 0.460791 0.948309 0.096 Uiso 1 1 calc R U . . .
C35 C 1.0215(4) 0.6166(4) 0.8450(3) 0.0380(17) Uani 1 1 d . . . . .
C36 C 1.1091(5) 0.6198(4) 0.8133(4) 0.052(2) Uani 1 1 d . . . . .
H36A H 1.138181 0.671171 0.825758 0.077 Uiso 1 1 calc R U . . .
H36B H 1.088252 0.588665 0.760152 0.077 Uiso 1 1 calc R U . . .
H36C H 1.156586 0.601736 0.833780 0.077 Uiso 1 1 calc R U . . .
C37 C 1.0543(5) 0.6624(4) 0.9281(4) 0.0521(19) Uani 1 1 d . . . . .
H37A H 1.082586 0.714420 0.942556 0.078 Uiso 1 1 calc R U . . .
H37B H 1.102459 0.643566 0.946921 0.078 Uiso 1 1 calc R U . . .
H37C H 0.998878 0.658488 0.948145 0.078 Uiso 1 1 calc R U . . .
C38 C 0.9553(5) 0.6542(4) 0.8185(4) 0.055(2) Uani 1 1 d . . . . .
H38A H 0.992136 0.704105 0.831511 0.083 Uiso 1 1 calc R U . . .
H38B H 0.902063 0.657664 0.841624 0.083 Uiso 1 1 calc R U . . .
H38C H 0.929581 0.624836 0.765436 0.083 Uiso 1 1 calc R U . . .
C39 C 0.6732(4) 0.4418(3) 0.6998(3) 0.0249(15) Uani 1 1 d . . . . .
C40 C 0.6973(4) 0.4804(3) 0.6633(3) 0.0266(15) Uani 1 1 d . . . . .
H40 H 0.756494 0.489012 0.651367 0.032 Uiso 1 1 calc R U . . .
C41 C 0.6177(4) 0.5041(3) 0.6476(3) 0.0288(15) Uani 1 1 d . . . . .
C42 C 0.5452(4) 0.4785(3) 0.6752(3) 0.0244(15) Uani 1 1 d . . . . .
C43 C 0.5975(4) 0.5435(3) 0.6093(3) 0.0282(15) Uani 1 1 d . . . . .
C44 C 0.5116(4) 0.6030(3) 0.5730(3) 0.0294(16) Uani 1 1 d . . . . .
C45 C 0.5984(4) 0.6015(3) 0.5503(3) 0.0269(15) Uani 1 1 d . . . . .
C46 C 0.4746(4) 0.6698(3) 0.5218(3) 0.0292(15) Uani 1 1 d . . . . .
C47 C 0.5594(4) 0.6698(3) 0.4992(3) 0.0315(16) Uani 1 1 d . . . . .
C48 C 0.4084(5) 0.7072(4) 0.5040(3) 0.0340(16) Uani 1 1 d . . . . .
C49 C 0.5870(4) 0.7100(4) 0.4618(4) 0.0342(17) Uani 1 1 d . . . . .
C50 C 0.4434(4) 0.5583(3) 0.6558(3) 0.0279(16) Uani 1 1 d . . . . .
C51 C 0.4648(4) 0.6336(3) 0.7200(3) 0.0282(15) Uani 1 1 d . . . . .
H51 H 0.522716 0.650418 0.756985 0.034 Uiso 1 1 calc R U . . .
C52 C 0.4086(4) 0.6792(4) 0.7294(3) 0.0328(16) Uani 1 1 d . . . . .
C53 C 0.3184(5) 0.6523(4) 0.6684(4) 0.0396(18) Uani 1 1 d . . . . .
C54 C 0.2837(4) 0.5727(4) 0.6128(3) 0.0296(16) Uani 1 1 d . . . . .
C55 C 0.3441(4) 0.5308(4) 0.6072(3) 0.0306(16) Uani 1 1 d . . . . .
H55 H 0.322562 0.480317 0.570131 0.037 Uiso 1 1 calc R U . . .
C56 C 0.4304(5) 0.7548(4) 0.7966(4) 0.0475(19) Uani 1 1 d . . . . .
C57 C 0.5181(5) 0.7673(4) 0.8537(4) 0.0517(19) Uani 1 1 d . . . . .
H57A H 0.531595 0.816662 0.896021 0.078 Uiso 1 1 calc R U . . .
H57B H 0.573693 0.763752 0.833158 0.078 Uiso 1 1 calc R U . . .
H57C H 0.505527 0.729551 0.868915 0.078 Uiso 1 1 calc R U . . .
C58 C 0.4518(6) 0.8167(4) 0.7754(5) 0.068(2) Uani 1 1 d . . . . .
H58A H 0.473135 0.865285 0.819626 0.101 Uiso 1 1 calc R U . . .
H58B H 0.393235 0.813870 0.743624 0.101 Uiso 1 1 calc R U . . .
H58C H 0.502443 0.810142 0.749732 0.101 Uiso 1 1 calc R U . . .
C59 C 0.3456(5) 0.7594(4) 0.8305(4) 0.062(2) Uani 1 1 d . . . . .
H59A H 0.361573 0.807150 0.875253 0.094 Uiso 1 1 calc R U . . .
H59B H 0.331883 0.718999 0.841963 0.094 Uiso 1 1 calc R U . . .
H59C H 0.288916 0.755159 0.795967 0.094 Uiso 1 1 calc R U . . .
C60 C 0.1814(4) 0.5434(4) 0.5622(3) 0.0389(18) Uani 1 1 d . . . . .
C61 C 0.1561(4) 0.4591(4) 0.5162(4) 0.0490(19) Uani 1 1 d . . . . .
H61A H 0.091386 0.440592 0.483359 0.073 Uiso 1 1 calc R U . . .
H61B H 0.158122 0.436968 0.548214 0.073 Uiso 1 1 calc R U . . .
H61C H 0.202761 0.445562 0.487383 0.073 Uiso 1 1 calc R U . . .
C62 C 0.1079(5) 0.5630(4) 0.6082(4) 0.054(2) Uani 1 1 d . . . . .
H62A H 0.042510 0.540497 0.575858 0.081 Uiso 1 1 calc R U . . .
H62B H 0.119768 0.616950 0.635160 0.081 Uiso 1 1 calc R U . . .
H62C H 0.115006 0.543816 0.642585 0.081 Uiso 1 1 calc R U . . .
C63 C 0.1767(5) 0.5774(4) 0.5111(4) 0.055(2) Uani 1 1 d . . . . .
H63A H 0.112440 0.556908 0.477307 0.083 Uiso 1 1 calc R U . . .
H63B H 0.224850 0.565572 0.483490 0.083 Uiso 1 1 calc R U . . .
H63C H 0.189954 0.631371 0.540128 0.083 Uiso 1 1 calc R U . . .
C64 C 0.4621(4) 0.5021(3) 0.6815(3) 0.0279(15) Uani 1 1 d . . . . .
C65 C 0.4019(4) 0.4853(3) 0.7203(3) 0.0251(15) Uani 1 1 d . . . . .
C66 C 0.3281(4) 0.5174(3) 0.7466(3) 0.0269(15) Uani 1 1 d . . . . .
H66 H 0.300428 0.548933 0.733406 0.032 Uiso 1 1 calc R U . . .
C67 C 0.3047(4) 0.4947(3) 0.7937(3) 0.0294(15) Uani 1 1 d . . . . .
H67 H 0.258098 0.507606 0.820287 0.035 Uiso 1 1 calc R U . . .
C68 C 0.3634(4) 0.4476(3) 0.7958(3) 0.0285(6) Uani 1 1 d . U . . .
C69 C 0.3600(4) 0.4064(3) 0.8369(3) 0.0285(6) Uani 1 1 d . U . . .
C70 C 0.3558(4) 0.4380(4) 0.9080(3) 0.0312(16) Uani 1 1 d . . . . .
C71 C 0.3552(4) 0.5143(3) 0.9479(3) 0.0303(16) Uani 1 1 d . . . . .
H71 H 0.363100 0.543617 0.924573 0.036 Uiso 1 1 calc R U . . .
C72 C 0.3442(4) 0.5473(3) 1.0162(3) 0.0306(16) Uani 1 1 d . . . . .
C73 C 0.3391(4) 0.5034(3) 1.0554(3) 0.0285(6) Uani 1 1 d . . . . .
C74 C 0.3413(4) 0.4251(3) 1.0156(3) 0.0285(6) Uani 1 1 d . . . . .
C75 C 0.3522(4) 0.3975(3) 0.9480(3) 0.0285(6) Uani 1 1 d . . . . .
H75 H 0.357844 0.348211 0.924767 0.034 Uiso 1 1 calc R U . . .
C76 C 0.3368(4) 0.6273(3) 1.0525(3) 0.0321(16) Uani 1 1 d . . . . .
C77 C 0.4196(5) 0.6770(4) 1.1209(3) 0.0457(18) Uani 1 1 d . . . . .
H77A H 0.416390 0.728484 1.140806 0.069 Uiso 1 1 calc R U . . .
H77B H 0.481000 0.673500 1.108532 0.069 Uiso 1 1 calc R U . . .
H77C H 0.414498 0.660956 1.157348 0.069 Uiso 1 1 calc R U . . .
C78 C 0.2393(5) 0.6270(4) 1.0733(4) 0.0504(19) Uani 1 1 d . . . . .
H78A H 0.232664 0.677677 1.095869 0.076 Uiso 1 1 calc R U . . .
H78B H 0.237578 0.608063 1.107864 0.076 Uiso 1 1 calc R U . . .
H78C H 0.186162 0.595188 1.029378 0.076 Uiso 1 1 calc R U . . .
C79 C 0.3367(5) 0.6596(4) 1.0009(3) 0.0407(17) Uani 1 1 d . . . . .
H79A H 0.332710 0.710871 1.026197 0.061 Uiso 1 1 calc R U . . .
H79B H 0.281134 0.629945 0.958321 0.061 Uiso 1 1 calc R U . . .
H79C H 0.396104 0.658863 0.985024 0.061 Uiso 1 1 calc R U . . .
C80 C 0.3334(4) 0.3765(3) 1.0529(3) 0.0313(16) Uani 1 1 d . . . . .
C81 C 0.3361(5) 0.2983(4) 1.0038(4) 0.0490(19) Uani 1 1 d . . . . .
H81A H 0.329477 0.269476 1.029372 0.074 Uiso 1 1 calc R U . . .
H81B H 0.397457 0.299528 0.990706 0.074 Uiso 1 1 calc R U . . .
H81C H 0.282990 0.275281 0.959490 0.074 Uiso 1 1 calc R U . . .
C82 C 0.4143(4) 0.4094(4) 1.1224(3) 0.0420(18) Uani 1 1 d . . . . .
H82A H 0.403749 0.380068 1.147126 0.063 Uiso 1 1 calc R U . . .
H82B H 0.415011 0.460700 1.154676 0.063 Uiso 1 1 calc R U . . .
H82C H 0.476033 0.408636 1.110015 0.063 Uiso 1 1 calc R U . . .
C83 C 0.2358(5) 0.3726(4) 1.0731(4) 0.055(2) Uani 1 1 d . . . . .
H83A H 0.232594 0.347099 1.101958 0.083 Uiso 1 1 calc R U . . .
H83B H 0.183003 0.345352 1.028397 0.083 Uiso 1 1 calc R U . . .
H83C H 0.230314 0.422996 1.101549 0.083 Uiso 1 1 calc R U . . .
C85 C 0.1820(5) 0.3085(5) 0.6242(5) 0.094(3) Uani 1 1 d . . . . .
H85A H 0.200438 0.308627 0.670596 0.140 Uiso 1 1 calc R U . . .
H85B H 0.228644 0.348262 0.624404 0.140 Uiso 1 1 calc R U . . .
H85C H 0.180965 0.260593 0.584091 0.140 Uiso 1 1 calc R U . . .
C88 C -0.0213(6) 0.3998(5) 0.6370(5) 0.066(2) Uani 1 1 d . . . . .
H88 H -0.028586 0.448635 0.659317 0.079 Uiso 1 1 calc R U . . .
C87 C 0.0704(6) 0.3876(6) 0.6446(5) 0.074(3) Uani 1 1 d . . . . .
H87 H 0.124925 0.429342 0.672737 0.089 Uiso 1 1 calc R U . . .
C86 C 0.0842(6) 0.3206(5) 0.6143(5) 0.071(2) Uani 1 1 d . . . . .
C89 C -0.0979(6) 0.3411(6) 0.5977(5) 0.064(2) Uani 1 1 d . . . . .
H89 H -0.160423 0.348285 0.591761 0.076 Uiso 1 1 calc R U . . .
C90 C -0.0879(7) 0.2723(6) 0.5664(6) 0.105(4) Uani 1 1 d . . . . .
H90 H -0.142500 0.230967 0.536723 0.126 Uiso 1 1 calc R U . . .
C91 C 0.0006(7) 0.2621(6) 0.5775(7) 0.132(5) Uani 1 1 d . . . . .
H91 H 0.006136 0.212846 0.559419 0.158 Uiso 1 1 calc R U . . .
N1 N 0.5801(3) 0.3107(3) 0.7038(2) 0.0243(12) Uani 1 1 d . . . . .
N2 N 0.4180(3) 0.3118(3) 0.7477(2) 0.0246(12) Uani 1 1 d . . . . .
N3 N 0.4199(3) 0.4397(3) 0.7506(2) 0.0250(12) Uani 1 1 d . . . . .
N4 N 0.5791(3) 0.4366(2) 0.7037(2) 0.0237(12) Uani 1 1 d . . . . .
N5 N 0.5125(3) 0.5643(3) 0.6110(3) 0.0295(13) Uani 1 1 d . . . . .
N6 N 0.6489(3) 0.5642(3) 0.5728(3) 0.0347(13) Uani 1 1 d . . . . .
N7 N 0.4490(3) 0.6362(3) 0.5605(3) 0.0316(13) Uani 1 1 d . . . . .
N8 N 0.6239(3) 0.6338(3) 0.5116(3) 0.0343(13) Uani 1 1 d . . . . .
N9 N 0.3561(4) 0.7370(3) 0.4905(3) 0.0442(15) Uani 1 1 d . . . . .
N10 N 0.6113(4) 0.7446(3) 0.4352(3) 0.0457(15) Uani 1 1 d . . . . .
O1 O 0.3078(3) -0.1136(2) 0.5187(3) 0.0468(12) Uani 1 1 d . . . . .
H1 H 0.349037 -0.135891 0.522793 0.070 Uiso 1 1 calc R U . . .
O2 O 1.1094(3) 0.5155(2) 0.8712(2) 0.0444(12) Uani 1 1 d . . . . .
O3 O 0.2747(3) 0.6969(3) 0.6676(3) 0.0600(14) Uani 1 1 d . . . . .
O4 O 0.3348(3) 0.5322(3) 1.1194(2) 0.0534(13) Uani 1 1 d . . . . .
Ni Ni 0.50204(5) 0.37641(4) 0.72981(4) 0.0298(3) Uani 1 1 d . . . . .


_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
C1 C2 1.403(8) . ?
C1 C69 1.457(8) . ?
C1 N2 1.361(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.363(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.426(8) . ?
C4 C5 1.403(8) . ?
C4 N2 1.383(7) . ?
C5 C6 1.477(8) . ?
C5 C20 1.397(8) . ?
C6 C7 1.379(9) . ?
C6 C11 1.401(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.368(9) . ?
C8 C9 1.399(9) . ?
C8 C12 1.548(10) . ?
C9 C10 1.418(9) . ?
C9 O1 1.376(7) . ?
C10 C11 1.380(8) . ?
C10 C16 1.531(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.521(11) . ?
C12 C14 1.538(11) . ?
C12 C15 1.533(10) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.561(10) . ?
C16 C18 1.537(9) . ?
C16 C19 1.563(10) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.425(8) . ?
C20 N1 1.393(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.368(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.412(8) . ?
C23 C24 1.455(8) . ?
C23 N1 1.346(7) . ?
C24 C25 1.397(8) . ?
C24 C39 1.465(8) . ?
C25 C26 1.437(8) . ?
C25 C30 1.421(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.352(8) . ?
C27 C28 1.483(9) . ?
C27 C31 1.530(8) . ?
C28 C29 1.479(8) . ?
C28 O2 1.232(7) . ?
C29 C30 1.366(8) . ?
C29 C35 1.535(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.528(9) . ?
C31 C33 1.556(9) . ?
C31 C34 1.530(10) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.542(8) . ?
C35 C37 1.529(9) . ?
C35 C38 1.538(9) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.390(8) . ?
C39 N4 1.380(7) . ?
C40 H40 0.9500 . ?
C40 C41 1.391(8) . ?
C41 C42 1.426(8) . ?
C41 C43 1.430(8) . ?
C42 C64 1.392(8) . ?
C42 N4 1.384(7) . ?
C43 N5 1.387(7) . ?
C43 N6 1.314(7) . ?
C44 C45 1.427(8) . ?
C44 N5 1.377(7) . ?
C44 N7 1.305(7) . ?
C45 N6 1.345(7) . ?
C45 N8 1.333(7) . ?
C46 C47 1.398(8) . ?
C46 C48 1.451(9) . ?
C46 N7 1.354(7) . ?
C47 C49 1.445(10) . ?
C47 N8 1.369(7) . ?
C48 N9 1.147(7) . ?
C49 N10 1.144(7) . ?
C50 C51 1.492(8) . ?
C50 C55 1.491(8) . ?
C50 C64 1.548(8) . ?
C50 N5 1.518(7) . ?
C51 H51 0.9500 . ?
C51 C52 1.333(8) . ?
C52 C53 1.517(9) . ?
C52 C56 1.521(9) . ?
C53 C54 1.482(9) . ?
C53 O3 1.223(7) . ?
C54 C55 1.332(8) . ?
C54 C60 1.538(9) . ?
C55 H55 0.9500 . ?
C56 C57 1.519(9) . ?
C56 C58 1.551(9) . ?
C56 C59 1.524(9) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C61 1.528(9) . ?
C60 C62 1.548(9) . ?
C60 C63 1.542(8) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 C65 1.399(8) . ?
C65 C66 1.425(8) . ?
C65 N3 1.409(7) . ?
C66 H66 0.9500 . ?
C66 C67 1.350(8) . ?
C67 H67 0.9500 . ?
C67 C68 1.426(8) . ?
C68 C69 1.477(8) . ?
C68 N3 1.337(7) . ?
C69 C70 1.370(8) . ?
C70 C71 1.441(8) . ?
C70 C75 1.445(8) . ?
C71 H71 0.9500 . ?
C71 C72 1.351(8) . ?
C72 C73 1.492(8) . ?
C72 C76 1.532(8) . ?
C73 C74 1.482(8) . ?
C73 O4 1.236(7) . ?
C74 C75 1.336(8) . ?
C74 C80 1.545(8) . ?
C75 H75 0.9500 . ?
C76 C77 1.527(9) . ?
C76 C78 1.558(8) . ?
C76 C79 1.526(8) . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 C81 1.511(9) . ?
C80 C82 1.524(8) . ?
C80 C83 1.551(8) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C85 C86 1.494(11) . ?
C88 H88 0.9500 . ?
C88 C87 1.406(11) . ?
C88 C89 1.335(11) . ?
C87 H87 0.9500 . ?
C87 C86 1.326(11) . ?
C86 C91 1.392(12) . ?
C89 H89 0.9500 . ?
C89 C90 1.338(11) . ?
C90 H90 0.9500 . ?
C90 C91 1.350(12) . ?
C91 H91 0.9500 . ?
N1 Ni 1.887(5) . ?
N2 Ni 1.876(5) . ?
N3 Ni 1.893(4) . ?
N4 Ni 1.870(4) . ?
O1 H1 0.8400 . ?

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
C2 C1 C69 130.0(5) . . ?
N2 C1 C2 109.7(5) . . ?
N2 C1 C69 120.1(5) . . ?
C1 C2 H2 126.0 . . ?
C3 C2 C1 107.9(5) . . ?
C3 C2 H2 126.0 . . ?
C2 C3 H3 126.7 . . ?
C2 C3 C4 106.7(5) . . ?
C4 C3 H3 126.7 . . ?
C5 C4 C3 126.0(6) . . ?
N2 C4 C3 108.6(5) . . ?
N2 C4 C5 124.2(5) . . ?
C4 C5 C6 117.2(5) . . ?
C20 C5 C4 121.4(6) . . ?
C20 C5 C6 121.4(5) . . ?
C7 C6 C5 119.8(6) . . ?
C7 C6 C11 116.9(6) . . ?
C11 C6 C5 123.2(6) . . ?
C6 C7 H7 118.1 . . ?
C8 C7 C6 123.9(6) . . ?
C8 C7 H7 118.1 . . ?
C7 C8 C9 117.2(7) . . ?
C7 C8 C12 120.8(6) . . ?
C9 C8 C12 121.9(6) . . ?
C8 C9 C10 122.4(6) . . ?
O1 C9 C8 115.9(6) . . ?
O1 C9 C10 121.6(6) . . ?
C9 C10 C16 123.4(6) . . ?
C11 C10 C9 116.2(6) . . ?
C11 C10 C16 120.3(6) . . ?
C6 C11 H11 118.3 . . ?
C10 C11 C6 123.3(6) . . ?
C10 C11 H11 118.3 . . ?
C13 C12 C8 111.4(6) . . ?
C13 C12 C14 111.1(7) . . ?
C13 C12 C15 105.8(7) . . ?
C14 C12 C8 109.4(7) . . ?
C15 C12 C8 111.2(6) . . ?
C15 C12 C14 107.8(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C16 C17 111.7(6) . . ?
C10 C16 C18 110.0(5) . . ?
C10 C16 C19 110.1(6) . . ?
C17 C16 C19 106.4(6) . . ?
C18 C16 C17 106.0(6) . . ?
C18 C16 C19 112.6(6) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C5 C20 C21 127.5(6) . . ?
N1 C20 C5 123.8(5) . . ?
N1 C20 C21 108.3(5) . . ?
C20 C21 H21 126.1 . . ?
C22 C21 C20 107.8(6) . . ?
C22 C21 H21 126.1 . . ?
C21 C22 H22 127.1 . . ?
C21 C22 C23 105.9(5) . . ?
C23 C22 H22 127.1 . . ?
C22 C23 C24 126.5(5) . . ?
N1 C23 C22 111.7(5) . . ?
N1 C23 C24 121.3(5) . . ?
C23 C24 C39 114.2(5) . . ?
C25 C24 C23 123.7(5) . . ?
C25 C24 C39 122.1(6) . . ?
C24 C25 C26 120.8(6) . . ?
C24 C25 C30 121.6(5) . . ?
C30 C25 C26 117.5(5) . . ?
C25 C26 H26 118.4 . . ?
C27 C26 C25 123.3(6) . . ?
C27 C26 H26 118.4 . . ?
C26 C27 C28 118.5(5) . . ?
C26 C27 C31 121.6(6) . . ?
C28 C27 C31 119.9(5) . . ?
C29 C28 C27 118.9(5) . . ?
O2 C28 C27 120.9(5) . . ?
O2 C28 C29 120.2(6) . . ?
C28 C29 C35 119.4(5) . . ?
C30 C29 C28 118.1(6) . . ?
C30 C29 C35 122.5(5) . . ?
C25 C30 H30 118.3 . . ?
C29 C30 C25 123.5(6) . . ?
C29 C30 H30 118.3 . . ?
C27 C31 C33 108.8(5) . . ?
C32 C31 C27 112.4(5) . . ?
C32 C31 C33 106.6(6) . . ?
C32 C31 C34 107.5(5) . . ?
C34 C31 C27 110.6(6) . . ?
C34 C31 C33 110.8(5) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C29 C35 C36 110.8(5) . . ?
C29 C35 C38 111.8(5) . . ?
C37 C35 C29 110.3(5) . . ?
C37 C35 C36 109.7(5) . . ?
C37 C35 C38 106.9(6) . . ?
C38 C35 C36 107.3(5) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C24 129.6(5) . . ?
N4 C39 C24 119.3(5) . . ?
N4 C39 C40 110.6(5) . . ?
C39 C40 H40 126.7 . . ?
C39 C40 C41 106.6(5) . . ?
C41 C40 H40 126.7 . . ?
C40 C41 C42 107.5(5) . . ?
C40 C41 C43 133.0(5) . . ?
C42 C41 C43 119.4(5) . . ?
C64 C42 C41 124.2(5) . . ?
N4 C42 C41 108.2(5) . . ?
N4 C42 C64 127.0(5) . . ?
N5 C43 C41 116.6(5) . . ?
N6 C43 C41 129.2(5) . . ?
N6 C43 N5 114.2(5) . . ?
N5 C44 C45 104.5(5) . . ?
N7 C44 C45 125.5(5) . . ?
N7 C44 N5 129.9(5) . . ?
N6 C45 C44 111.6(5) . . ?
N8 C45 C44 122.6(5) . . ?
N8 C45 N6 125.8(5) . . ?
C47 C46 C48 120.1(5) . . ?
N7 C46 C47 123.5(5) . . ?
N7 C46 C48 116.4(5) . . ?
C46 C47 C49 121.9(5) . . ?
N8 C47 C46 123.7(5) . . ?
N8 C47 C49 114.4(5) . . ?
N9 C48 C46 179.5(8) . . ?
N10 C49 C47 176.8(7) . . ?
C51 C50 C64 110.0(5) . . ?
C51 C50 N5 106.5(4) . . ?
C55 C50 C51 114.1(5) . . ?
C55 C50 C64 109.9(5) . . ?
C55 C50 N5 107.0(4) . . ?
N5 C50 C64 109.1(4) . . ?
C50 C51 H51 117.6 . . ?
C52 C51 C50 124.8(6) . . ?
C52 C51 H51 117.6 . . ?
C51 C52 C53 116.5(6) . . ?
C51 C52 C56 123.8(6) . . ?
C53 C52 C56 119.6(5) . . ?
C54 C53 C52 119.5(5) . . ?
O3 C53 C52 118.7(7) . . ?
O3 C53 C54 121.8(6) . . ?
C53 C54 C60 118.4(5) . . ?
C55 C54 C53 118.3(6) . . ?
C55 C54 C60 123.2(6) . . ?
C50 C55 H55 118.0 . . ?
C54 C55 C50 123.9(6) . . ?
C54 C55 H55 118.0 . . ?
C52 C56 C58 109.8(6) . . ?
C52 C56 C59 109.8(6) . . ?
C57 C56 C52 110.9(5) . . ?
C57 C56 C58 108.0(6) . . ?
C57 C56 C59 107.6(6) . . ?
C59 C56 C58 110.6(6) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C56 C59 H59A 109.5 . . ?
C56 C59 H59B 109.5 . . ?
C56 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C54 C60 C62 109.9(5) . . ?
C54 C60 C63 109.4(5) . . ?
C61 C60 C54 109.6(5) . . ?
C61 C60 C62 108.3(5) . . ?
C61 C60 C63 108.9(6) . . ?
C63 C60 C62 110.7(5) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C62 H62A 109.5 . . ?
C60 C62 H62B 109.5 . . ?
C60 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C60 C63 H63A 109.5 . . ?
C60 C63 H63B 109.5 . . ?
C60 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C42 C64 C50 119.6(5) . . ?
C42 C64 C65 121.5(5) . . ?
C65 C64 C50 118.2(5) . . ?
C64 C65 C66 129.5(5) . . ?
C64 C65 N3 121.0(5) . . ?
N3 C65 C66 108.7(4) . . ?
C65 C66 H66 126.2 . . ?
C67 C66 C65 107.5(5) . . ?
C67 C66 H66 126.2 . . ?
C66 C67 H67 126.7 . . ?
C66 C67 C68 106.7(5) . . ?
C68 C67 H67 126.7 . . ?
C67 C68 C69 126.6(5) . . ?
N3 C68 C67 111.4(5) . . ?
N3 C68 C69 121.8(5) . . ?
C1 C69 C68 113.2(5) . . ?
C70 C69 C1 124.0(5) . . ?
C70 C69 C68 122.7(6) . . ?
C69 C70 C71 121.7(5) . . ?
C69 C70 C75 122.6(6) . . ?
C71 C70 C75 115.6(5) . . ?
C70 C71 H71 117.6 . . ?
C72 C71 C70 124.7(5) . . ?
C72 C71 H71 117.6 . . ?
C71 C72 C73 118.0(6) . . ?
C71 C72 C76 121.2(5) . . ?
C73 C72 C76 120.8(5) . . ?
C74 C73 C72 117.9(5) . . ?
O4 C73 C72 120.7(6) . . ?
O4 C73 C74 121.4(5) . . ?
C73 C74 C80 120.0(5) . . ?
C75 C74 C73 119.5(5) . . ?
C75 C74 C80 120.5(5) . . ?
C70 C75 H75 118.0 . . ?
C74 C75 C70 124.0(6) . . ?
C74 C75 H75 118.0 . . ?
C72 C76 C78 108.3(5) . . ?
C77 C76 C72 111.0(5) . . ?
C77 C76 C78 109.5(5) . . ?
C79 C76 C72 111.9(5) . . ?
C79 C76 C77 108.9(5) . . ?
C79 C76 C78 107.1(5) . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C76 C78 H78A 109.5 . . ?
C76 C78 H78B 109.5 . . ?
C76 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C76 C79 H79A 109.5 . . ?
C76 C79 H79B 109.5 . . ?
C76 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C74 C80 C83 108.1(5) . . ?
C81 C80 C74 112.4(5) . . ?
C81 C80 C82 107.9(5) . . ?
C81 C80 C83 108.2(5) . . ?
C82 C80 C74 111.5(5) . . ?
C82 C80 C83 108.6(5) . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C80 C82 H82A 109.5 . . ?
C80 C82 H82B 109.5 . . ?
C80 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C80 C83 H83A 109.5 . . ?
C80 C83 H83B 109.5 . . ?
C80 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C86 C85 H85A 109.5 . . ?
C86 C85 H85B 109.5 . . ?
C86 C85 H85C 109.5 . . ?
C87 C88 H88 120.8 . . ?
C89 C88 H88 120.8 . . ?
C89 C88 C87 118.4(9) . . ?
C88 C87 H87 118.5 . . ?
C86 C87 C88 123.0(9) . . ?
C86 C87 H87 118.5 . . ?
C87 C86 C85 122.4(9) . . ?
C87 C86 C91 115.1(8) . . ?
C91 C86 C85 122.3(9) . . ?
C88 C89 H89 119.6 . . ?
C88 C89 C90 120.9(9) . . ?
C90 C89 H89 119.6 . . ?
C89 C90 H90 120.3 . . ?
C89 C90 C91 119.4(9) . . ?
C91 C90 H90 120.3 . . ?
C86 C91 H91 118.6 . . ?
C90 C91 C86 122.9(9) . . ?
C90 C91 H91 118.6 . . ?
C20 N1 Ni 125.1(4) . . ?
C23 N1 C20 106.2(5) . . ?
C23 N1 Ni 128.2(4) . . ?
C1 N2 C4 106.9(5) . . ?
C1 N2 Ni 127.6(4) . . ?
C4 N2 Ni 125.3(4) . . ?
C65 N3 Ni 128.2(4) . . ?
C68 N3 C65 105.6(4) . . ?
C68 N3 Ni 126.2(4) . . ?
C39 N4 C42 106.7(4) . . ?
C39 N4 Ni 128.8(4) . . ?
C42 N4 Ni 124.0(4) . . ?
C43 N5 C50 127.8(5) . . ?
C44 N5 C43 105.3(4) . . ?
C44 N5 C50 126.1(5) . . ?
C43 N6 C45 104.4(5) . . ?
C44 N7 C46 112.3(5) . . ?
C45 N8 C47 112.2(5) . . ?
C9 O1 H1 109.5 . . ?
N1 Ni N3 176.9(2) . . ?
N2 Ni N1 90.8(2) . . ?
N2 Ni N3 89.25(19) . . ?
N4 Ni N1 89.3(2) . . ?
N4 Ni N2 175.0(2) . . ?
N4 Ni N3 90.36(19) . . ?

_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 -0.258 0.000 0.000 2203.6 846.9 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
####################################################################### 
# 
# 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_mandeep202006a_ni_113k1_0m
_database_code_depnum_ccdc_archive 'CCDC 2107802'
loop_
_audit_author_name
_audit_author_address
'Yoshitaka Matsushita'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_mandeep202006a_ni_113k1_0m 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Due to lower crystallinity and weaker peaks in wide angle region
;
_vrf_PLAT234_mandeep202006a_ni_113k1_0m 
;
PROBLEM: Large Hirshfeld Difference C31      --C32      .       0.27 Ang.
RESPONSE: Disordered t-butyl methyl group.
;
_vrf_PLAT341_mandeep202006a_ni_113k1_0m 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01926 Ang.
RESPONSE: Due to poor crystallinity
;
_vrf_PLAT414_mandeep202006a_ni_113k1_0m 
;
PROBLEM: Short Intra D-H..H-X       H2       ..H33B     .       1.89 Ang.
RESPONSE: H2 is placed using riding model and is too close to H33B
;
_vrf_PLAT414_mandeep202006a_ni_113k1_0m_2 
;
PROBLEM: Short Intra D-H..H-X       H2       ..H34C     .       1.83 Ang.
RESPONSE: H2 is placed using riding model and is too close to H34C
;
# Added during the CSD deposition process: Monday 28 November 2022 04:54 AM
# end Validation Reply Form

_audit_creation_date             2022-11-22
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C83 H88 N10 Ni O4, 1.829(C7 H8)'
_chemical_formula_sum            'C95.81 H102.64 N10 Ni O4'
_chemical_formula_weight         1516.88
_chemical_melting_point          ?
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      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                   14.6443(19)
_cell_length_b                   20.910(3)
_cell_length_c                   21.270(3)
_cell_angle_alpha                116.300(5)
_cell_angle_beta                 98.975(6)
_cell_angle_gamma                99.800(6)
_cell_volume                     5552.8(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8875
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      19.06
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.995
_shelx_estimated_absorpt_T_min   0.964
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.8617
_exptl_absorpt_correction_T_min  0.8251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrystalClear (Rigaku, 1997--2002)
;
_exptl_crystal_colour            'dull violet'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    violet
_exptl_crystal_description       irregular
_exptl_crystal_density_diffrn    0.907
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1615
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.023
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25156
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        19.132
_diffrn_reflns_theta_max         19.132
_diffrn_reflns_theta_min         1.107
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6162
_reflns_number_total             8949
_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       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.689
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.096
_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     708
_refine_ls_number_reflns         8949
_refine_ls_number_restraints     773
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.1238
_refine_ls_restrained_S_all      1.015
_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)+(0.1789P)²+38.1548P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3215
_refine_ls_wR_factor_ref         0.3489
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained planarity
 C100, C101, C102, C103, C104, C105, C106
 with sigma of 0.1
 C200, C201, C202, C203, C204, C205, C206
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C100) = Uanis(C101)
Uanis(C100) = Uanis(C102)
Uanis(C100) = Uanis(C103)
Uanis(C100) = Uanis(C104)
Uanis(C100) = Uanis(C105)
Uanis(C100) = Uanis(C106)
Uanis(C200) = Uanis(C201)
Uanis(C200) = Uanis(C202)
Uanis(C200) = Uanis(C203)
Uanis(C200) = Uanis(C204)
Uanis(C200) = Uanis(C205)
Uanis(C200) = Uanis(C206)
Uanis(C54) = Uanis(C50)
Uanis(C49) = Uanis(C48) = Uanis(C47) = Uanis(C46) = Uanis(C45) = Uanis(C44)
Uanis(C83) = Uanis(C84)
Uanis(N5) = Uanis(N7) = Uanis(N8)
Uanis(C82) = Uanis(C81) = Uanis(C79) = Uanis(C80)
Uanis(C7) = Uanis(C6) = Uanis(C11) = Uanis(C10) = Uanis(C9) = Uanis(C8)
Uanis(C63) = Uanis(C70) = Uanis(C69) = Uanis(C68) = Uanis(C67) = Uanis(C66)
Uanis(C74) = Uanis(C73) = Uanis(C72)
Uanis(C14) = Uanis(C74) = Uanis(C73) = Uanis(C72)
Uanis(C61) = Uanis(C60) = Uanis(C59) = Uanis(C58)
Uanis(C19) = Uanis(C17) = Uanis(C18)
Uanis(C63) = Uanis(C62) = Uanis(C1) = Uanis(C2) = Uanis(C65)
Uanis(C1) = Uanis(C23) = Uanis(C39)
Uanis(N2) = Uanis(N3)
Uanis(C21) = Uanis(C20) = Uanis(C5)
4. Rigid body (RIGU) restrains
 C21, C20, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C101)=Sof(C102)=Sof(H102)=
 Sof(C103)=Sof(H103)=Sof(C104)=Sof(H104)=Sof(C105)=Sof(H105)=Sof(C106)=
 Sof(H106)=FVAR(1)
 Sof(C200)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C201)=Sof(C202)=Sof(H202)=
 Sof(C203)=Sof(H203)=Sof(C204)=Sof(H204)=Sof(C205)=Sof(H205)=Sof(C206)=
 Sof(H206)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C11(H11), C21(H21), C22(H22), C26(H26), C30(H30), C40(H40),
 C41(H41), C45(H45), C49(H49), C59(H59), C60(H60), C66(H66), C70(H70),
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C202(H202),
 C203(H203), C204(H204), C205(H205), C206(H206)
6.b Fitted hexagon refined as free rotating group:
 C101(C102,C103,C104,C105,C106), C201(C202,C203,C204,C205,C206)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C72(H72A,
 H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C),
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C100(H10A,H10B,H10C), C200(H20A,H20B,
 H20C)
6.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4551(8) 0.5227(7) 0.3247(6) 0.0411(10) Uani 1 1 d . U . . .
C2 C 0.3837(8) 0.4991(7) 0.3529(6) 0.0411(10) Uani 1 1 d . U . . .
C3 C 0.3053(7) 0.5231(6) 0.3385(5) 0.033(3) Uani 1 1 d . U . . .
H3 H 0.246797 0.515489 0.351431 0.039 Uiso 1 1 calc R U . . .
C4 C 0.3291(8) 0.5602(6) 0.3014(5) 0.034(3) Uani 1 1 d . U . . .
C5 C 0.2725(8) 0.5999(7) 0.2749(6) 0.0390(18) Uani 1 1 d . U . . .
C6 C 0.1772(8) 0.5714(7) 0.2367(6) 0.0445(14) Uani 1 1 d . U . . .
C7 C 0.1243(8) 0.4958(7) 0.2141(6) 0.0445(14) Uani 1 1 d . U . . .
H7 H 0.159341 0.466034 0.224836 0.053 Uiso 1 1 calc R U . . .
C8 C 0.0318(8) 0.4647(8) 0.1801(6) 0.0445(14) Uani 1 1 d . U . . .
C9 C -0.0211(9) 0.5114(7) 0.1598(6) 0.0445(14) Uani 1 1 d . U . . .
C10 C 0.0317(8) 0.5846(7) 0.1747(6) 0.0445(14) Uani 1 1 d . U . . .
C11 C 0.1264(8) 0.6121(7) 0.2114(6) 0.0445(14) Uani 1 1 d . U . . .
H11 H 0.159848 0.659769 0.220669 0.053 Uiso 1 1 calc R U . . .
C12 C -0.0203(8) 0.3864(8) 0.1575(7) 0.052(3) Uani 1 1 d . U . . .
C13 C -0.0532(10) 0.3395(9) 0.0758(8) 0.079(5) Uani 1 1 d . U . . .
H13A H -0.076511 0.287354 0.062787 0.118 Uiso 1 1 calc R U . . .
H13B H 0.000722 0.345633 0.054965 0.118 Uiso 1 1 calc R U . . .
H13C H -0.105127 0.355261 0.056568 0.118 Uiso 1 1 calc R U . . .
C14 C 0.0463(9) 0.3485(9) 0.1848(8) 0.072(2) Uani 1 1 d . U . . .
H14A H 0.011061 0.297301 0.168544 0.109 Uiso 1 1 calc R U . . .
H14B H 0.067429 0.375639 0.237969 0.109 Uiso 1 1 calc R U . . .
H14C H 0.102369 0.348622 0.164964 0.109 Uiso 1 1 calc R U . . .
C15 C -0.1084(9) 0.3822(9) 0.1884(8) 0.076(4) Uani 1 1 d . U . . .
H15A H -0.132216 0.331885 0.180743 0.114 Uiso 1 1 calc R U . . .
H15B H -0.158938 0.394526 0.163439 0.114 Uiso 1 1 calc R U . . .
H15C H -0.089886 0.417421 0.240501 0.114 Uiso 1 1 calc R U . . .
C16 C -0.0206(9) 0.6295(8) 0.1486(7) 0.059(4) Uani 1 1 d . U . . .
C17 C -0.0578(9) 0.5875(9) 0.0668(8) 0.076(3) Uani 1 1 d . U . . .
H17A H -0.079197 0.620149 0.049499 0.114 Uiso 1 1 calc R U . . .
H17B H -0.111839 0.544804 0.052614 0.114 Uiso 1 1 calc R U . . .
H17C H -0.006417 0.570177 0.045199 0.114 Uiso 1 1 calc R U . . .
C18 C -0.1009(9) 0.6482(9) 0.1856(8) 0.076(3) Uani 1 1 d . U . . .
H18A H -0.128266 0.681796 0.172771 0.114 Uiso 1 1 calc R U . . .
H18B H -0.074898 0.672258 0.238443 0.114 Uiso 1 1 calc R U . . .
H18C H -0.151098 0.602595 0.169487 0.114 Uiso 1 1 calc R U . . .
C19 C 0.0470(9) 0.7040(9) 0.1677(8) 0.076(3) Uani 1 1 d . U . . .
H19A H 0.011299 0.730976 0.149957 0.114 Uiso 1 1 calc R U . . .
H19B H 0.099935 0.695140 0.144742 0.114 Uiso 1 1 calc R U . . .
H19C H 0.072816 0.733429 0.220521 0.114 Uiso 1 1 calc R U . . .
C20 C 0.3256(8) 0.6746(7) 0.2965(6) 0.0390(18) Uani 1 1 d . U . . .
C21 C 0.3027(9) 0.7431(7) 0.3336(6) 0.0390(18) Uani 1 1 d . U . . .
H21 H 0.242883 0.748323 0.344277 0.047 Uiso 1 1 calc R U . . .
C22 C 0.3785(8) 0.7984(7) 0.3509(6) 0.040(3) Uani 1 1 d . U . . .
H22 H 0.382250 0.849783 0.375144 0.048 Uiso 1 1 calc R U . . .
C23 C 0.4535(8) 0.7663(8) 0.3262(6) 0.0411(10) Uani 1 1 d . U . . .
C24 C 0.5430(8) 0.8046(8) 0.3263(6) 0.040(3) Uani 1 1 d . U . . .
C25 C 0.5795(9) 0.8849(7) 0.3667(6) 0.038(3) Uani 1 1 d . U . . .
C26 C 0.5255(8) 0.9331(8) 0.3567(6) 0.045(3) Uani 1 1 d . U . . .
H26 H 0.463550 0.911295 0.323626 0.054 Uiso 1 1 calc R U . . .
C27 C 0.5606(9) 1.0098(8) 0.3934(7) 0.039(3) Uani 1 1 d . U . . .
C28 C 0.6521(9) 1.0384(8) 0.4440(6) 0.040(3) Uani 1 1 d . U . . .
C29 C 0.7061(9) 0.9937(8) 0.4560(7) 0.048(3) Uani 1 1 d . U . . .
C30 C 0.6662(9) 0.9184(8) 0.4159(7) 0.042(3) Uani 1 1 d . U . . .
H30 H 0.702240 0.887469 0.423287 0.051 Uiso 1 1 calc R U . . .
C31 C 0.4974(9) 1.0569(7) 0.3811(7) 0.054(3) Uani 1 1 d . U . . .
C32 C 0.3985(12) 1.0055(9) 0.3235(8) 0.098(6) Uani 1 1 d . U . . .
H32A H 0.359694 0.981599 0.344754 0.147 Uiso 1 1 calc R U . . .
H32B H 0.410629 0.967575 0.280266 0.147 Uiso 1 1 calc R U . . .
H32C H 0.363894 1.035611 0.309907 0.147 Uiso 1 1 calc R U . . .
C33 C 0.4726(10) 1.1047(8) 0.4524(7) 0.065(4) Uani 1 1 d . U . . .
H33A H 0.426136 1.130090 0.442932 0.098 Uiso 1 1 calc R U . . .
H33B H 0.531137 1.141486 0.488307 0.098 Uiso 1 1 calc R U . . .
H33C H 0.444874 1.072900 0.471132 0.098 Uiso 1 1 calc R U . . .
C34 C 0.5507(13) 1.1035(9) 0.3521(8) 0.096(5) Uani 1 1 d . U . . .
H34A H 0.512096 1.134961 0.345185 0.144 Uiso 1 1 calc R U . . .
H34B H 0.561350 1.070528 0.305495 0.144 Uiso 1 1 calc R U . . .
H34C H 0.612713 1.134701 0.387027 0.144 Uiso 1 1 calc R U . . .
C35 C 0.8029(10) 1.0250(9) 0.5069(10) 0.086(5) Uani 1 1 d . U . . .
C36 C 0.8038(11) 1.0824(9) 0.5841(9) 0.106(6) Uani 1 1 d . U . . .
H36A H 0.867358 1.097024 0.617004 0.159 Uiso 1 1 calc R U . . .
H36B H 0.755310 1.060511 0.601082 0.159 Uiso 1 1 calc R U . . .
H36C H 0.789270 1.126034 0.583133 0.159 Uiso 1 1 calc R U . . .
C37 C 0.8735(11) 1.0637(10) 0.4784(11) 0.120(7) Uani 1 1 d . U . . .
H37A H 0.934824 1.090781 0.515510 0.180 Uiso 1 1 calc R U . . .
H37B H 0.845785 1.098438 0.467714 0.180 Uiso 1 1 calc R U . . .
H37C H 0.884089 1.026263 0.434023 0.180 Uiso 1 1 calc R U . . .
C38 C 0.8468(10) 0.9658(9) 0.5144(10) 0.117(7) Uani 1 1 d . U . . .
H38A H 0.805384 0.939655 0.532454 0.176 Uiso 1 1 calc R U . . .
H38B H 0.910699 0.989762 0.548536 0.176 Uiso 1 1 calc R U . . .
H38C H 0.852193 0.930255 0.466780 0.176 Uiso 1 1 calc R U . . .
C39 C 0.6006(8) 0.7636(7) 0.2847(6) 0.0411(10) Uani 1 1 d . U . . .
C40 C 0.6763(10) 0.7966(8) 0.2635(7) 0.062(4) Uani 1 1 d . U . . .
H40 H 0.705662 0.847503 0.280574 0.075 Uiso 1 1 calc R U . . .
C41 C 0.6954(9) 0.7334(8) 0.2105(6) 0.051(3) Uani 1 1 d . U . . .
H41 H 0.739645 0.735313 0.182718 0.062 Uiso 1 1 calc R U . . .
C42 C 0.6430(8) 0.6697(7) 0.2040(6) 0.035(3) Uani 1 1 d . U . . .
C43 C 0.6401(7) 0.5936(7) 0.1612(6) 0.035(3) Uani 1 1 d . U . . .
C44 C 0.6465(7) 0.5612(7) 0.0918(6) 0.0363(13) Uani 1 1 d . U . . .
C45 C 0.6490(7) 0.6040(7) 0.0515(5) 0.0363(13) Uani 1 1 d . U . . .
H45 H 0.642885 0.653189 0.074032 0.044 Uiso 1 1 calc R U . . .
C46 C 0.6597(7) 0.5742(7) -0.0156(5) 0.0363(13) Uani 1 1 d . U . . .
C47 C 0.6611(7) 0.4959(7) -0.0554(6) 0.0363(13) Uani 1 1 d . U . . .
C48 C 0.6565(7) 0.4525(7) -0.0150(5) 0.0363(13) Uani 1 1 d . U . . .
C49 C 0.6453(7) 0.4851(7) 0.0522(5) 0.0363(13) Uani 1 1 d . U . . .
H49 H 0.635853 0.455530 0.075253 0.044 Uiso 1 1 calc R U . . .
C50 C 0.6636(9) 0.3735(7) -0.0513(6) 0.047(2) Uani 1 1 d . U . . .
C51 C 0.6617(9) 0.3392(7) -0.0010(6) 0.053(3) Uani 1 1 d . U . . .
H51A H 0.671089 0.289527 -0.025448 0.079 Uiso 1 1 calc R U . . .
H51B H 0.599549 0.335755 0.010722 0.079 Uiso 1 1 calc R U . . .
H51C H 0.713178 0.370337 0.043789 0.079 Uiso 1 1 calc R U . . .
C52 C 0.5833(10) 0.3243(9) -0.1190(7) 0.076(5) Uani 1 1 d . U . . .
H52A H 0.587519 0.273054 -0.138640 0.115 Uiso 1 1 calc R U . . .
H52B H 0.588645 0.340743 -0.155147 0.115 Uiso 1 1 calc R U . . .
H52C H 0.521529 0.327090 -0.107231 0.115 Uiso 1 1 calc R U . . .
C53 C 0.7627(9) 0.3732(7) -0.0700(7) 0.058(4) Uani 1 1 d . U . . .
H53A H 0.773573 0.324190 -0.084534 0.088 Uiso 1 1 calc R U . . .
H53B H 0.813994 0.410620 -0.027217 0.088 Uiso 1 1 calc R U . . .
H53C H 0.762692 0.384560 -0.110029 0.088 Uiso 1 1 calc R U . . .
C54 C 0.6667(8) 0.6223(7) -0.0542(6) 0.047(2) Uani 1 1 d . U . . .
C55 C 0.5847(9) 0.5900(8) -0.1237(6) 0.064(4) Uani 1 1 d . U . . .
H55A H 0.596739 0.618078 -0.149580 0.095 Uiso 1 1 calc R U . . .
H55B H 0.523722 0.593426 -0.110660 0.095 Uiso 1 1 calc R U . . .
H55C H 0.581381 0.537967 -0.155051 0.095 Uiso 1 1 calc R U . . .
C56 C 0.6616(10) 0.7016(8) -0.0067(8) 0.078(4) Uani 1 1 d . U . . .
H56A H 0.661920 0.728088 -0.034874 0.117 Uiso 1 1 calc R U . . .
H56B H 0.717235 0.727432 0.035849 0.117 Uiso 1 1 calc R U . . .
H56C H 0.602470 0.699962 0.009368 0.117 Uiso 1 1 calc R U . . .
C57 C 0.7654(9) 0.6294(9) -0.0738(8) 0.082(5) Uani 1 1 d . U . . .
H57A H 0.817744 0.649050 -0.029755 0.123 Uiso 1 1 calc R U . . .
H57B H 0.771920 0.663116 -0.094332 0.123 Uiso 1 1 calc R U . . .
H57C H 0.768363 0.580525 -0.109429 0.123 Uiso 1 1 calc R U . . .
C58 C 0.6391(7) 0.5531(6) 0.2040(6) 0.0368(15) Uani 1 1 d . U . . .
C59 C 0.6975(7) 0.5053(6) 0.2066(5) 0.0368(15) Uani 1 1 d . U . . .
H59 H 0.745054 0.492818 0.181126 0.044 Uiso 1 1 calc R U . . .
C60 C 0.6717(7) 0.4822(6) 0.2516(5) 0.0368(15) Uani 1 1 d . U . . .
H60 H 0.697563 0.448802 0.263102 0.044 Uiso 1 1 calc R U . . .
C61 C 0.5990(7) 0.5150(7) 0.2803(5) 0.0368(15) Uani 1 1 d . U . . .
C62 C 0.5405(7) 0.4986(7) 0.3180(6) 0.0411(10) Uani 1 1 d . U . . .
C63 C 0.5585(8) 0.4434(7) 0.3453(6) 0.0411(10) Uani 1 1 d . U . . .
C65 C 0.4045(8) 0.4583(7) 0.3899(6) 0.0411(10) Uani 1 1 d . U . . .
C66 C 0.6582(7) 0.4715(7) 0.3933(6) 0.0411(10) Uani 1 1 d . U . . .
H66 H 0.680807 0.522083 0.429741 0.049 Uiso 1 1 calc R U . . .
C67 C 0.7161(8) 0.4276(7) 0.3864(6) 0.0411(10) Uani 1 1 d . U . . .
C68 C 0.6839(8) 0.3478(7) 0.3327(6) 0.0411(10) Uani 1 1 d . U . . .
C69 C 0.5938(8) 0.3204(7) 0.2699(6) 0.0411(10) Uani 1 1 d . U . . .
C70 C 0.5369(8) 0.3667(7) 0.2808(6) 0.0411(10) Uani 1 1 d . U . . .
H70 H 0.478032 0.349724 0.244883 0.049 Uiso 1 1 calc R U . . .
C71 C 0.8196(7) 0.4576(8) 0.4391(6) 0.048(3) Uani 1 1 d . U . . .
C72 C 0.8233(9) 0.4252(9) 0.4903(7) 0.072(2) Uani 1 1 d . U . . .
H72A H 0.889335 0.440517 0.519887 0.109 Uiso 1 1 calc R U . . .
H72B H 0.801723 0.371009 0.462001 0.109 Uiso 1 1 calc R U . . .
H72C H 0.781225 0.443100 0.522040 0.109 Uiso 1 1 calc R U . . .
C73 C 0.8926(9) 0.4396(9) 0.3960(7) 0.072(2) Uani 1 1 d . U . . .
H73A H 0.957096 0.460115 0.429230 0.109 Uiso 1 1 calc R U . . .
H73B H 0.888641 0.461177 0.363440 0.109 Uiso 1 1 calc R U . . .
H73C H 0.879695 0.385677 0.367211 0.109 Uiso 1 1 calc R U . . .
C74 C 0.8437(9) 0.5418(9) 0.4844(8) 0.072(2) Uani 1 1 d . U . . .
H74A H 0.910874 0.561184 0.512990 0.109 Uiso 1 1 calc R U . . .
H74B H 0.801756 0.555024 0.517092 0.109 Uiso 1 1 calc R U . . .
H74C H 0.834130 0.563301 0.451995 0.109 Uiso 1 1 calc R U . . .
C75 C 0.5723(10) 0.2448(8) 0.2056(7) 0.068(4) Uani 1 1 d . U . . .
C76 C 0.6608(11) 0.2427(8) 0.1727(8) 0.088(5) Uani 1 1 d . U . . .
H76A H 0.644281 0.198335 0.124996 0.131 Uiso 1 1 calc R U . . .
H76B H 0.715028 0.241446 0.205139 0.131 Uiso 1 1 calc R U . . .
H76C H 0.678503 0.286969 0.167233 0.131 Uiso 1 1 calc R U . . .
C77 C 0.5557(14) 0.1820(9) 0.2269(11) 0.115(7) Uani 1 1 d . U . . .
H77A H 0.546833 0.134106 0.184045 0.172 Uiso 1 1 calc R U . . .
H77B H 0.498334 0.181490 0.245133 0.172 Uiso 1 1 calc R U . . .
H77C H 0.611588 0.191140 0.264747 0.172 Uiso 1 1 calc R U . . .
C78 C 0.4852(10) 0.2324(8) 0.1482(8) 0.078(4) Uani 1 1 d . U . . .
H78A H 0.471196 0.182739 0.106662 0.117 Uiso 1 1 calc R U . . .
H78B H 0.498399 0.269539 0.132173 0.117 Uiso 1 1 calc R U . . .
H78C H 0.429820 0.237069 0.168873 0.117 Uiso 1 1 calc R U . . .
C79 C 0.4877(8) 0.3979(6) 0.4276(5) 0.0365(15) Uani 1 1 d . U . . .
C80 C 0.4056(7) 0.3992(6) 0.4492(5) 0.0365(15) Uani 1 1 d . U . . .
C81 C 0.5268(7) 0.3315(6) 0.4785(5) 0.0365(15) Uani 1 1 d . U . . .
C82 C 0.4433(8) 0.3323(6) 0.5027(5) 0.0365(15) Uani 1 1 d . U . . .
C83 C 0.5945(8) 0.2934(7) 0.4964(6) 0.040(2) Uani 1 1 d . U . . .
C84 C 0.4159(8) 0.2929(7) 0.5401(6) 0.040(2) Uani 1 1 d . U . . .
C100 C 0.8183(11) 0.6958(10) 0.3718(8) 0.090(3) Uani 0.916(13) 1 d . U P . .
H10A H 0.767790 0.650414 0.355981 0.135 Uiso 0.916(13) 1 calc R U P . .
H10B H 0.809365 0.712524 0.335521 0.135 Uiso 0.916(13) 1 calc R U P . .
H10C H 0.814891 0.734401 0.418543 0.135 Uiso 0.916(13) 1 calc R U P . .
C101 C 0.9142(6) 0.6805(7) 0.3801(5) 0.090(3) Uani 0.916(13) 1 d G U P . .
C102 C 0.9945(8) 0.7408(5) 0.4200(6) 0.090(3) Uani 0.916(13) 1 d G U P . .
H102 H 0.987360 0.789734 0.440339 0.108 Uiso 0.916(13) 1 calc R U P . .
C103 C 1.0854(6) 0.7297(5) 0.4302(6) 0.090(3) Uani 0.916(13) 1 d G U P . .
H103 H 1.140282 0.770913 0.457510 0.108 Uiso 0.916(13) 1 calc R U P . .
C104 C 1.0958(6) 0.6581(6) 0.4005(6) 0.090(3) Uani 0.916(13) 1 d G U P . .
H104 H 1.157924 0.650456 0.407510 0.108 Uiso 0.916(13) 1 calc R U P . .
C105 C 1.0155(8) 0.5977(5) 0.3606(6) 0.090(3) Uani 0.916(13) 1 d G U P . .
H105 H 1.022643 0.548819 0.340338 0.108 Uiso 0.916(13) 1 calc R U P . .
C106 C 0.9246(6) 0.6089(6) 0.3504(5) 0.090(3) Uani 0.916(13) 1 d G U P . .
H106 H 0.869720 0.567639 0.323166 0.108 Uiso 0.916(13) 1 calc R U P . .
C200 C 0.8725(18) 0.7853(15) 0.5772(15) 0.201(6) Uani 0.914(15) 1 d . U P . .
H20A H 0.843641 0.744902 0.527400 0.302 Uiso 0.914(15) 1 calc R U P . .
H20B H 0.939399 0.786018 0.592778 0.302 Uiso 0.914(15) 1 calc R U P . .
H20C H 0.870239 0.832651 0.578926 0.302 Uiso 0.914(15) 1 calc R U P . .
C201 C 0.8140(12) 0.7730(11) 0.6302(8) 0.201(6) Uani 0.914(15) 1 d G U P . .
C202 C 0.8286(11) 0.7314(11) 0.6648(12) 0.201(6) Uani 0.914(15) 1 d G U P . .
H202 H 0.878191 0.706905 0.658353 0.242 Uiso 0.914(15) 1 calc R U P . .
C203 C 0.7707(15) 0.7255(11) 0.7090(11) 0.201(6) Uani 0.914(15) 1 d G U P . .
H203 H 0.780721 0.697026 0.732719 0.242 Uiso 0.914(15) 1 calc R U P . .
C204 C 0.6982(12) 0.7613(12) 0.7185(9) 0.201(6) Uani 0.914(15) 1 d G U P . .
H204 H 0.658635 0.757267 0.748700 0.242 Uiso 0.914(15) 1 calc R U P . .
C205 C 0.6836(12) 0.8029(11) 0.6838(12) 0.201(6) Uani 0.914(15) 1 d G U P . .
H205 H 0.634018 0.827387 0.690316 0.242 Uiso 0.914(15) 1 calc R U P . .
C206 C 0.7415(15) 0.8088(10) 0.6397(11) 0.201(6) Uani 0.914(15) 1 d G U P . .
H206 H 0.731487 0.837266 0.615950 0.242 Uiso 0.914(15) 1 calc R U P . .
N1 N 0.4218(6) 0.5637(5) 0.2947(4) 0.038(2) Uani 1 1 d . U . . .
N2 N 0.4200(6) 0.6911(5) 0.2947(4) 0.0355(17) Uani 1 1 d . U . . .
N3 N 0.5804(6) 0.6868(5) 0.2501(4) 0.0355(17) Uani 1 1 d . U . . .
N4 N 0.5806(6) 0.5592(5) 0.2478(4) 0.031(2) Uani 1 1 d . U . . .
N5 N 0.4893(6) 0.4352(5) 0.3882(4) 0.0425(15) Uani 1 1 d . U . . .
N6 N 0.3520(6) 0.4368(5) 0.4268(5) 0.044(3) Uani 1 1 d . U . . .
N7 N 0.5530(6) 0.3650(5) 0.4393(5) 0.0425(15) Uani 1 1 d . U . . .
N8 N 0.3782(6) 0.3671(5) 0.4883(5) 0.0425(15) Uani 1 1 d . U . . .
N9 N 0.6460(7) 0.2635(6) 0.5106(6) 0.058(3) Uani 1 1 d . U . . .
N10 N 0.3914(7) 0.2579(6) 0.5667(5) 0.055(3) Uani 1 1 d . U . . .
O1 O -0.1088(5) 0.4857(5) 0.1296(4) 0.065(3) Uani 1 1 d . U . . .
O2 O 0.6927(6) 1.1139(5) 0.4824(5) 0.058(2) Uani 1 1 d . U . . .
H2 H 0.653617 1.135516 0.473008 0.087 Uiso 1 1 calc R U . . .
O3 O 0.6675(7) 0.4697(5) -0.1176(4) 0.079(3) Uani 1 1 d . U . . .
O4 O 0.7287(7) 0.3038(6) 0.3330(5) 0.093(3) Uani 1 1 d . U . . .
Ni Ni 0.49831(10) 0.62422(9) 0.26882(8) 0.0434(6) Uani 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
C1 C2 1.408(14) . ?
C1 C62 1.429(14) . ?
C1 N1 1.381(13) . ?
C2 C3 1.373(14) . ?
C2 C65 1.431(14) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(14) . ?
C4 C5 1.482(14) . ?
C4 N1 1.381(13) . ?
C5 C6 1.377(15) . ?
C5 C20 1.447(16) . ?
C6 C7 1.456(16) . ?
C6 C11 1.437(15) . ?
C7 H7 0.9500 . ?
C7 C8 1.326(15) . ?
C8 C9 1.506(16) . ?
C8 C12 1.502(17) . ?
C9 C10 1.459(16) . ?
C9 O1 1.246(13) . ?
C10 C11 1.362(15) . ?
C10 C16 1.534(16) . ?
C11 H11 0.9500 . ?
C12 C13 1.512(18) . ?
C12 C14 1.552(16) . ?
C12 C15 1.542(16) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.510(18) . ?
C16 C18 1.527(17) . ?
C16 C19 1.536(18) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.426(15) . ?
C20 N2 1.378(13) . ?
C21 H21 0.9500 . ?
C21 C22 1.328(15) . ?
C22 H22 0.9500 . ?
C22 C23 1.433(15) . ?
C23 C24 1.414(16) . ?
C23 N2 1.364(14) . ?
C24 C25 1.455(16) . ?
C24 C39 1.427(15) . ?
C25 C26 1.446(16) . ?
C25 C30 1.353(15) . ?
C26 H26 0.9500 . ?
C26 C27 1.390(15) . ?
C27 C28 1.422(16) . ?
C27 C31 1.535(16) . ?
C28 C29 1.402(16) . ?
C28 O2 1.378(13) . ?
C29 C30 1.374(16) . ?
C29 C35 1.479(19) . ?
C30 H30 0.9500 . ?
C31 C32 1.582(19) . ?
C31 C33 1.542(17) . ?
C31 C34 1.539(19) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.54(2) . ?
C35 C37 1.56(2) . ?
C35 C38 1.54(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.443(16) . ?
C39 N3 1.390(14) . ?
C40 H40 0.9500 . ?
C40 C41 1.414(16) . ?
C41 H41 0.9500 . ?
C41 C42 1.357(15) . ?
C42 C43 1.430(15) . ?
C42 N3 1.418(13) . ?
C43 C44 1.350(14) . ?
C43 C58 1.494(15) . ?
C44 C45 1.488(14) . ?
C44 C49 1.430(15) . ?
C45 H45 0.9500 . ?
C45 C46 1.329(13) . ?
C46 C47 1.479(15) . ?
C46 C54 1.557(15) . ?
C47 C48 1.499(15) . ?
C47 O3 1.215(12) . ?
C48 C49 1.335(13) . ?
C48 C50 1.514(16) . ?
C49 H49 0.9500 . ?
C50 C51 1.528(15) . ?
C50 C52 1.503(17) . ?
C50 C53 1.565(16) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.539(16) . ?
C54 C56 1.536(17) . ?
C54 C57 1.566(16) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C59 1.432(14) . ?
C58 N4 1.340(12) . ?
C59 H59 0.9500 . ?
C59 C60 1.324(13) . ?
C60 H60 0.9500 . ?
C60 C61 1.434(14) . ?
C61 C62 1.362(14) . ?
C61 N4 1.414(13) . ?
C62 C63 1.547(15) . ?
C63 C66 1.494(15) . ?
C63 C70 1.514(15) . ?
C63 N5 1.503(13) . ?
C65 N5 1.407(13) . ?
C65 N6 1.338(13) . ?
C66 H66 0.9500 . ?
C66 C67 1.330(14) . ?
C67 C68 1.478(16) . ?
C67 C71 1.571(16) . ?
C68 C69 1.539(16) . ?
C68 O4 1.220(13) . ?
C69 C70 1.350(14) . ?
C69 C75 1.501(17) . ?
C70 H70 0.9500 . ?
C71 C72 1.514(16) . ?
C71 C73 1.505(16) . ?
C71 C74 1.527(18) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C76 1.563(18) . ?
C75 C77 1.561(19) . ?
C75 C78 1.518(19) . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 C80 1.353(14) . ?
C79 N5 1.374(13) . ?
C79 N7 1.324(13) . ?
C80 N6 1.373(13) . ?
C80 N8 1.347(13) . ?
C81 C82 1.398(14) . ?
C81 C83 1.477(17) . ?
C81 N7 1.364(13) . ?
C82 C84 1.426(16) . ?
C82 N8 1.370(13) . ?
C83 N9 1.143(13) . ?
C84 N10 1.153(13) . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
C100 C101 1.493(16) . ?
C101 C102 1.3900 . ?
C101 C106 1.3900 . ?
C102 H102 0.9500 . ?
C102 C103 1.3900 . ?
C103 H103 0.9500 . ?
C103 C104 1.3900 . ?
C104 H104 0.9500 . ?
C104 C105 1.3900 . ?
C105 H105 0.9500 . ?
C105 C106 1.3900 . ?
C106 H106 0.9500 . ?
C200 H20A 0.9800 . ?
C200 H20B 0.9800 . ?
C200 H20C 0.9800 . ?
C200 C201 1.60(3) . ?
C201 C202 1.3900 . ?
C201 C206 1.3900 . ?
C202 H202 0.9500 . ?
C202 C203 1.3900 . ?
C203 H203 0.9500 . ?
C203 C204 1.3900 . ?
C204 H204 0.9500 . ?
C204 C205 1.3900 . ?
C205 H205 0.9500 . ?
C205 C206 1.3900 . ?
C206 H206 0.9500 . ?
N1 Ni 1.867(9) . ?
N2 Ni 1.907(8) . ?
N3 Ni 1.841(9) . ?
N4 Ni 1.920(8) . ?
O2 H2 0.8400 . ?

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
C2 C1 C62 125.5(10) . . ?
N1 C1 C2 108.3(9) . . ?
N1 C1 C62 125.6(9) . . ?
C1 C2 C65 118.0(9) . . ?
C3 C2 C1 108.7(9) . . ?
C3 C2 C65 133.3(9) . . ?
C2 C3 H3 127.1 . . ?
C4 C3 C2 105.8(9) . . ?
C4 C3 H3 127.1 . . ?
C3 C4 C5 128.8(10) . . ?
C3 C4 N1 111.9(9) . . ?
N1 C4 C5 119.1(9) . . ?
C6 C5 C4 124.5(11) . . ?
C6 C5 C20 122.1(10) . . ?
C20 C5 C4 113.4(10) . . ?
C5 C6 C7 121.9(10) . . ?
C5 C6 C11 122.0(12) . . ?
C11 C6 C7 115.9(10) . . ?
C6 C7 H7 116.9 . . ?
C8 C7 C6 126.2(11) . . ?
C8 C7 H7 116.9 . . ?
C7 C8 C9 116.0(12) . . ?
C7 C8 C12 124.7(11) . . ?
C12 C8 C9 119.2(10) . . ?
C10 C9 C8 119.4(11) . . ?
O1 C9 C8 118.7(12) . . ?
O1 C9 C10 121.9(10) . . ?
C9 C10 C16 119.3(10) . . ?
C11 C10 C9 119.9(11) . . ?
C11 C10 C16 120.9(12) . . ?
C6 C11 H11 118.9 . . ?
C10 C11 C6 122.1(12) . . ?
C10 C11 H11 118.9 . . ?
C8 C12 C13 111.5(10) . . ?
C8 C12 C14 111.1(10) . . ?
C8 C12 C15 112.4(11) . . ?
C13 C12 C14 106.2(11) . . ?
C13 C12 C15 108.5(11) . . ?
C15 C12 C14 106.9(10) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C16 C19 111.8(10) . . ?
C17 C16 C10 109.8(11) . . ?
C17 C16 C18 111.8(10) . . ?
C17 C16 C19 106.6(11) . . ?
C18 C16 C10 110.7(10) . . ?
C18 C16 C19 106.1(11) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C5 130.1(10) . . ?
N2 C20 C5 121.7(10) . . ?
N2 C20 C21 107.3(11) . . ?
C20 C21 H21 125.5 . . ?
C22 C21 C20 108.9(10) . . ?
C22 C21 H21 125.5 . . ?
C21 C22 H22 126.3 . . ?
C21 C22 C23 107.3(11) . . ?
C23 C22 H22 126.3 . . ?
C24 C23 C22 126.1(12) . . ?
N2 C23 C22 108.4(10) . . ?
N2 C23 C24 125.1(10) . . ?
C23 C24 C25 122.9(10) . . ?
C23 C24 C39 119.3(12) . . ?
C39 C24 C25 117.8(10) . . ?
C26 C25 C24 122.1(11) . . ?
C30 C25 C24 121.3(11) . . ?
C30 C25 C26 116.6(12) . . ?
C25 C26 H26 118.6 . . ?
C27 C26 C25 122.8(11) . . ?
C27 C26 H26 118.6 . . ?
C26 C27 C28 115.3(11) . . ?
C26 C27 C31 119.4(11) . . ?
C28 C27 C31 125.1(12) . . ?
C29 C28 C27 123.6(12) . . ?
O2 C28 C27 119.3(11) . . ?
O2 C28 C29 117.1(12) . . ?
C28 C29 C35 122.3(13) . . ?
C30 C29 C28 116.6(12) . . ?
C30 C29 C35 121.1(12) . . ?
C25 C30 C29 125.1(12) . . ?
C25 C30 H30 117.5 . . ?
C29 C30 H30 117.5 . . ?
C27 C31 C32 110.5(11) . . ?
C27 C31 C33 109.8(10) . . ?
C27 C31 C34 108.4(11) . . ?
C33 C31 C32 106.4(11) . . ?
C34 C31 C32 109.0(11) . . ?
C34 C31 C33 112.8(11) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C29 C35 C36 112.5(12) . . ?
C29 C35 C37 109.6(14) . . ?
C29 C35 C38 113.3(13) . . ?
C36 C35 C37 108.2(14) . . ?
C36 C35 C38 107.0(15) . . ?
C38 C35 C37 105.9(13) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C24 C39 C40 122.9(12) . . ?
N3 C39 C24 124.1(10) . . ?
N3 C39 C40 112.2(10) . . ?
C39 C40 H40 129.1 . . ?
C41 C40 C39 101.8(12) . . ?
C41 C40 H40 129.1 . . ?
C40 C41 H41 124.0 . . ?
C42 C41 C40 112.0(11) . . ?
C42 C41 H41 124.0 . . ?
C41 C42 C43 132.7(10) . . ?
C41 C42 N3 109.1(10) . . ?
N3 C42 C43 118.2(10) . . ?
C42 C43 C58 112.3(9) . . ?
C44 C43 C42 125.7(10) . . ?
C44 C43 C58 121.7(10) . . ?
C43 C44 C45 119.9(10) . . ?
C43 C44 C49 123.2(10) . . ?
C49 C44 C45 116.8(9) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 C44 120.7(11) . . ?
C46 C45 H45 119.7 . . ?
C45 C46 C47 121.8(10) . . ?
C45 C46 C54 118.8(10) . . ?
C47 C46 C54 119.3(8) . . ?
C46 C47 C48 117.1(9) . . ?
O3 C47 C46 120.0(10) . . ?
O3 C47 C48 122.8(11) . . ?
C47 C48 C50 119.7(8) . . ?
C49 C48 C47 118.5(10) . . ?
C49 C48 C50 121.8(10) . . ?
C44 C49 H49 117.7 . . ?
C48 C49 C44 124.6(10) . . ?
C48 C49 H49 117.7 . . ?
C48 C50 C51 112.4(9) . . ?
C48 C50 C53 108.8(10) . . ?
C51 C50 C53 105.8(9) . . ?
C52 C50 C48 112.0(10) . . ?
C52 C50 C51 107.7(10) . . ?
C52 C50 C53 110.0(10) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C46 C54 C57 109.7(9) . . ?
C55 C54 C46 112.4(10) . . ?
C55 C54 C57 109.3(9) . . ?
C56 C54 C46 113.2(9) . . ?
C56 C54 C55 105.6(10) . . ?
C56 C54 C57 106.5(11) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C59 C58 C43 127.6(9) . . ?
N4 C58 C43 121.6(9) . . ?
N4 C58 C59 110.8(9) . . ?
C58 C59 H59 126.9 . . ?
C60 C59 C58 106.3(9) . . ?
C60 C59 H59 126.9 . . ?
C59 C60 H60 125.1 . . ?
C59 C60 C61 109.8(9) . . ?
C61 C60 H60 125.1 . . ?
C62 C61 C60 130.6(10) . . ?
C62 C61 N4 121.7(9) . . ?
N4 C61 C60 106.3(8) . . ?
C1 C62 C63 118.3(9) . . ?
C61 C62 C1 122.1(9) . . ?
C61 C62 C63 119.1(9) . . ?
C66 C63 C62 109.1(9) . . ?
C66 C63 C70 114.3(9) . . ?
C66 C63 N5 108.4(8) . . ?
C70 C63 C62 109.4(8) . . ?
N5 C63 C62 111.0(8) . . ?
N5 C63 C70 104.5(9) . . ?
N5 C65 C2 118.9(9) . . ?
N6 C65 C2 128.4(9) . . ?
N6 C65 N5 112.8(9) . . ?
C63 C66 H66 119.2 . . ?
C67 C66 C63 121.7(11) . . ?
C67 C66 H66 119.2 . . ?
C66 C67 C68 121.7(11) . . ?
C66 C67 C71 120.9(11) . . ?
C68 C67 C71 117.2(10) . . ?
C67 C68 C69 118.1(10) . . ?
O4 C68 C67 123.2(11) . . ?
O4 C68 C69 118.4(12) . . ?
C70 C69 C68 115.0(11) . . ?
C70 C69 C75 125.5(11) . . ?
C75 C69 C68 119.4(10) . . ?
C63 C70 H70 117.1 . . ?
C69 C70 C63 125.8(10) . . ?
C69 C70 H70 117.1 . . ?
C72 C71 C67 110.0(9) . . ?
C72 C71 C74 108.4(11) . . ?
C73 C71 C67 110.0(9) . . ?
C73 C71 C72 111.2(10) . . ?
C73 C71 C74 107.7(10) . . ?
C74 C71 C67 109.4(9) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C69 C75 C76 107.1(11) . . ?
C69 C75 C77 112.3(11) . . ?
C69 C75 C78 109.9(11) . . ?
C77 C75 C76 109.2(12) . . ?
C78 C75 C76 108.1(11) . . ?
C78 C75 C77 110.0(13) . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76B 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C77 H77A 109.5 . . ?
C75 C77 H77B 109.5 . . ?
C75 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C75 C78 H78A 109.5 . . ?
C75 C78 H78B 109.5 . . ?
C75 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C80 C79 N5 106.9(9) . . ?
N7 C79 C80 127.2(10) . . ?
N7 C79 N5 125.9(9) . . ?
C79 C80 N6 112.9(9) . . ?
N8 C80 C79 124.2(10) . . ?
N8 C80 N6 122.9(9) . . ?
C82 C81 C83 119.7(9) . . ?
N7 C81 C82 124.7(10) . . ?
N7 C81 C83 115.5(9) . . ?
C81 C82 C84 122.8(10) . . ?
N8 C82 C81 122.5(9) . . ?
N8 C82 C84 114.6(9) . . ?
N9 C83 C81 179.1(12) . . ?
N10 C84 C82 176.3(13) . . ?
H10A C100 H10B 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C101 C100 H10A 109.5 . . ?
C101 C100 H10B 109.5 . . ?
C101 C100 H10C 109.5 . . ?
C102 C101 C100 117.7(10) . . ?
C102 C101 C106 120.0 . . ?
C106 C101 C100 122.3(10) . . ?
C101 C102 H102 120.0 . . ?
C103 C102 C101 120.0 . . ?
C103 C102 H102 120.0 . . ?
C102 C103 H103 120.0 . . ?
C104 C103 C102 120.0 . . ?
C104 C103 H103 120.0 . . ?
C103 C104 H104 120.0 . . ?
C103 C104 C105 120.0 . . ?
C105 C104 H104 120.0 . . ?
C104 C105 H105 120.0 . . ?
C106 C105 C104 120.0 . . ?
C106 C105 H105 120.0 . . ?
C101 C106 H106 120.0 . . ?
C105 C106 C101 120.0 . . ?
C105 C106 H106 120.0 . . ?
H20A C200 H20B 109.5 . . ?
H20A C200 H20C 109.5 . . ?
H20B C200 H20C 109.5 . . ?
C201 C200 H20A 109.5 . . ?
C201 C200 H20B 109.5 . . ?
C201 C200 H20C 109.5 . . ?
C202 C201 C200 127(2) . . ?
C202 C201 C206 120.0 . . ?
C206 C201 C200 113(2) . . ?
C201 C202 H202 120.0 . . ?
C203 C202 C201 120.0 . . ?
C203 C202 H202 120.0 . . ?
C202 C203 H203 120.0 . . ?
C202 C203 C204 120.0 . . ?
C204 C203 H203 120.0 . . ?
C203 C204 H204 120.0 . . ?
C205 C204 C203 120.0 . . ?
C205 C204 H204 120.0 . . ?
C204 C205 H205 120.0 . . ?
C204 C205 C206 120.0 . . ?
C206 C205 H205 120.0 . . ?
C201 C206 H206 120.0 . . ?
C205 C206 C201 120.0 . . ?
C205 C206 H206 120.0 . . ?
C1 N1 Ni 124.7(7) . . ?
C4 N1 C1 105.3(8) . . ?
C4 N1 Ni 129.1(7) . . ?
C20 N2 Ni 126.7(8) . . ?
C23 N2 C20 107.9(9) . . ?
C23 N2 Ni 124.5(7) . . ?
C39 N3 C42 104.8(9) . . ?
C39 N3 Ni 126.1(7) . . ?
C42 N3 Ni 128.9(8) . . ?
C58 N4 C61 106.7(8) . . ?
C58 N4 Ni 125.6(7) . . ?
C61 N4 Ni 127.3(6) . . ?
C65 N5 C63 126.1(8) . . ?
C79 N5 C63 129.0(8) . . ?
C79 N5 C65 104.6(8) . . ?
C65 N6 C80 102.9(8) . . ?
C79 N7 C81 109.9(8) . . ?
C80 N8 C82 111.5(8) . . ?
C28 O2 H2 109.5 . . ?
N1 Ni N2 90.0(4) . . ?
N1 Ni N4 89.6(4) . . ?
N2 Ni N4 177.1(4) . . ?
N3 Ni N1 175.6(4) . . ?
N3 Ni N2 90.7(4) . . ?
N3 Ni N4 89.4(4) . . ?

_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 -0.769 0.000 0.000 1876.3 676.5 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
####################################################################### 
# 
# 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_mandeep202006a_ni_113k3_0m
_database_code_depnum_ccdc_archive 'CCDC 2107803'
loop_
_audit_author_name
_audit_author_address
'Yoshitaka Matsushita'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_mandeep202006a_ni_113k3_0m 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Due to lower crystallinity and weaker peaks in wide angle region
;
_vrf_PLAT414_mandeep202006a_ni_113k3_0m 
;
PROBLEM: Short Intra D-H..H-X       H1O      ..H39      .       1.64 Ang.
RESPONSE: H10 was placed using a riding model which is close to H39
;
_vrf_PLAT602_mandeep202006a_ni_113k3_0m 
;
PROBLEM: Solvent Accessible VOID(S) in Structure ........          ! Check
RESPONSE: The structure contains substantial voids.
;
_vrf_PLAT934_mandeep202006a_ni_113k3_0m 
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..         20 Check
RESPONSE: Due to poor crystallinity.
;
_vrf_PLAT049_mandeep202006a_ni_113k3_0m 
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.8260 Check
RESPONSE: Low density due to pores in the structure.
;
_vrf_PLAT084_mandeep202006a_ni_113k3_0m 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.36 Report
RESPONSE: Due to poor crystallinity
;
_vrf_PLAT306_mandeep202006a_ni_113k3_0m 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        Ow1 Check
RESPONSE: Disordered water molecules in the structure
;
_vrf_PLAT306_mandeep202006a_ni_113k3_0m_2 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        Ow2 Check
RESPONSE: Disordered water molecules in the structure
;
_vrf_PLAT926_mandeep202006a_ni_113k3_0m 
;
PROBLEM: Reported and Calculated   R1 Differ by .........    -0.0069 Check
RESPONSE: Due to poor crystallinity
;
_vrf_PLAT939_mandeep202006a_ni_113k3_0m 
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .     437.43 Check
RESPONSE: Due to poor crystallinity
;
# Added during the CSD deposition process: Monday 28 November 2022 03:04 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C83 H88 N10 Ni O6'
_chemical_formula_weight         1380.34

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.8586(6)
_cell_length_b                   21.1662(8)
_cell_length_c                   21.3245(8)
_cell_angle_alpha                117.802(2)
_cell_angle_beta                 99.889(2)
_cell_angle_gamma                101.120(2)
_cell_volume                     5550.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    9296
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      21.94

_exptl_crystal_description       Platelet
_exptl_crystal_colour            'Dark purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.826
_exptl_crystal_F_000             1464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.031
_exptl_absorpt_coefficient_mu    0.215
_shelx_estimated_absorpt_T_min   0.976
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7968
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_process_details   
;
CrystalClear (Rigaku, 1997--2002)
;
_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_reflns_number            48976
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.119
_diffrn_reflns_theta_max         21.943
_diffrn_reflns_theta_full        21.943
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             13396
_reflns_number_gt                9125
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13396
_refine_ls_number_parameters     922
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.1034
_refine_ls_wR_factor_ref         0.3556
_refine_ls_wR_factor_gt          0.3211
_refine_ls_goodness_of_fit_ref   1.363
_refine_ls_restrained_S_all      1.363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
C1 C 0.1036(4) 0.0206(4) 0.2841(4) 0.0260(16) Uani 1 1 d . . . . .
C2 C 0.0422(4) 0.0020(4) 0.3185(4) 0.0265(16) Uani 1 1 d . . . . .
C3 C -0.0418(4) 0.0228(4) 0.3220(3) 0.0253(16) Uani 1 1 d . . . . .
C4 C -0.1656(4) 0.0596(4) 0.2972(4) 0.0262(16) Uani 1 1 d . . . . .
C5 C -0.2189(4) 0.0996(4) 0.2726(4) 0.0266(16) Uani 1 1 d . . . . .
C6 C -0.1620(5) 0.1751(4) 0.2967(4) 0.0286(16) Uani 1 1 d . . . . .
C7 C -0.0347(5) 0.2716(4) 0.3315(4) 0.0262(16) Uani 1 1 d . . . . .
C8 C 0.0537(5) 0.3096(4) 0.3337(4) 0.0294(16) Uani 1 1 d . . . . .
C9 C 0.1135(5) 0.2724(4) 0.2963(4) 0.0294(17) Uani 1 1 d . . . . .
C10 C 0.1517(4) 0.1782(4) 0.2155(4) 0.0264(16) Uani 1 1 d . . . . .
C11 C 0.1505(4) 0.1000(4) 0.1708(4) 0.0286(17) Uani 1 1 d . . . . .
C12 C 0.1455(5) 0.0591(4) 0.2103(4) 0.0282(16) Uani 1 1 d . . . . .
C13 C 0.2050(5) 0.0144(4) 0.2146(4) 0.0300(17) Uani 1 1 d . . . . .
H2 H 0.252300 0.002945 0.189965 0.036 Uiso 1 1 calc R U . . .
C14 C 0.1800(5) -0.0080(4) 0.2611(4) 0.0293(16) Uani 1 1 d . . . . .
H1 H 0.207984 -0.037525 0.275891 0.035 Uiso 1 1 calc R U . . .
C15 C 0.1542(4) 0.0672(4) 0.0986(4) 0.0262(16) Uani 1 1 d . . . . .
C16 C 0.1500(4) -0.0109(4) 0.0574(4) 0.0280(16) Uani 1 1 d . . . . .
H22 H 0.143980 -0.038971 0.081355 0.034 Uiso 1 1 calc R U . . .
C17 C 0.1541(4) -0.0462(4) -0.0133(4) 0.0284(16) Uani 1 1 d . . . . .
C18 C 0.1574(5) -0.0032(4) -0.0526(4) 0.0361(18) Uani 1 1 d . . . . .
C19 C 0.1640(4) 0.0768(4) -0.0107(4) 0.0297(17) Uani 1 1 d . . . . .
C20 C 0.1599(4) 0.1074(4) 0.0594(4) 0.0275(16) Uani 1 1 d . . . . .
H3 H 0.160685 0.158322 0.084664 0.033 Uiso 1 1 calc R U . . .
C21 C 0.1721(5) 0.1234(4) -0.0488(4) 0.0332(17) Uani 1 1 d . . . . .
C22 C 0.0818(5) 0.0903(5) -0.1154(4) 0.045(2) Uani 1 1 d . . . . .
H5 H 0.024647 0.090072 -0.098355 0.067 Uiso 1 1 calc R U . . .
H6 H 0.076901 0.038741 -0.151943 0.067 Uiso 1 1 calc R U . . .
H4 H 0.086393 0.121057 -0.138410 0.067 Uiso 1 1 calc R U . . .
C23 C 0.2616(5) 0.1217(5) -0.0757(5) 0.051(2) Uani 1 1 d . . . . .
H8 H 0.264051 0.147832 -0.103331 0.077 Uiso 1 1 calc R U . . .
H7 H 0.258312 0.069366 -0.108092 0.077 Uiso 1 1 calc R U . . .
H9 H 0.319456 0.146749 -0.032689 0.077 Uiso 1 1 calc R U . . .
C24 C 0.1816(6) 0.2052(4) 0.0043(4) 0.051(2) Uani 1 1 d . . . . .
H10 H 0.123144 0.207736 0.019584 0.077 Uiso 1 1 calc R U . . .
H11 H 0.190343 0.233699 -0.020715 0.077 Uiso 1 1 calc R U . . .
H12 H 0.237239 0.226774 0.048294 0.077 Uiso 1 1 calc R U . . .
C25 C 0.1537(5) -0.1271(4) -0.0520(4) 0.0303(17) Uani 1 1 d . . . . .
C26 C 0.0622(5) -0.1787(4) -0.1200(4) 0.044(2) Uani 1 1 d . . . . .
H13 H 0.004812 -0.174054 -0.103705 0.066 Uiso 1 1 calc R U . . .
H15 H 0.062038 -0.231061 -0.142008 0.066 Uiso 1 1 calc R U . . .
H14 H 0.062213 -0.163672 -0.157003 0.066 Uiso 1 1 calc R U . . .
C27 C 0.1572(6) -0.1579(4) -0.0001(4) 0.0396(19) Uani 1 1 d . . . . .
H18 H 0.212730 -0.124890 0.044420 0.059 Uiso 1 1 calc R U . . .
H17 H 0.163058 -0.208522 -0.025662 0.059 Uiso 1 1 calc R U . . .
H16 H 0.098009 -0.160121 0.014330 0.059 Uiso 1 1 calc R U . . .
C28 C 0.2433(6) -0.1327(4) -0.0794(5) 0.047(2) Uani 1 1 d . . . . .
H21 H 0.240251 -0.117974 -0.116818 0.071 Uiso 1 1 calc R U . . .
H19 H 0.244966 -0.184560 -0.101419 0.071 Uiso 1 1 calc R U . . .
H20 H 0.301514 -0.099067 -0.037289 0.071 Uiso 1 1 calc R U . . .
C29 C 0.2109(5) 0.2444(4) 0.2242(4) 0.0295(16) Uani 1 1 d . . . . .
H24 H 0.257534 0.247414 0.199435 0.035 Uiso 1 1 calc R U . . .
C30 C 0.1884(5) 0.3023(4) 0.2744(4) 0.0336(18) Uani 1 1 d . . . . .
H23 H 0.217402 0.354064 0.292206 0.040 Uiso 1 1 calc R U . . .
C31 C 0.0871(5) 0.3931(4) 0.3735(4) 0.0347(18) Uani 1 1 d . . . . .
C32 C 0.0319(5) 0.4339(4) 0.3590(4) 0.0350(18) Uani 1 1 d . . . . .
H44 H -0.029437 0.407167 0.322542 0.042 Uiso 1 1 calc R U . . .
C33 C 0.0628(5) 0.5124(4) 0.3958(4) 0.0366(18) Uani 1 1 d . . . . .
C34 C 0.1544(5) 0.5486(4) 0.4487(4) 0.042(2) Uani 1 1 d D . . . .
C35 C 0.2133(5) 0.5093(4) 0.4646(4) 0.042(2) Uani 1 1 d . . . . .
C36 C 0.3148(6) 0.5505(5) 0.5210(6) 0.066(3) Uani 1 1 d . . . . .
C37 C 0.3792(7) 0.5948(6) 0.4954(9) 0.111(5) Uani 1 1 d . . . . .
H25 H 0.443554 0.620948 0.531523 0.166 Uiso 1 1 calc R U . . .
H26 H 0.350854 0.631581 0.491832 0.166 Uiso 1 1 calc R U . . .
H27 H 0.383755 0.559755 0.446620 0.166 Uiso 1 1 calc R U . . .
C38 C 0.3109(7) 0.6032(6) 0.5990(6) 0.090(4) Uani 1 1 d . . . . .
H28 H 0.267761 0.574648 0.613381 0.134 Uiso 1 1 calc R U . . .
H30 H 0.286989 0.643272 0.599225 0.134 Uiso 1 1 calc R U . . .
H29 H 0.375611 0.625361 0.634473 0.134 Uiso 1 1 calc R U . . .
C39 C 0.3633(7) 0.4951(6) 0.5245(7) 0.090(4) Uani 1 1 d . . . . .
H33 H 0.327211 0.467076 0.542926 0.135 Uiso 1 1 calc R U . . .
H32 H 0.429137 0.522390 0.558216 0.135 Uiso 1 1 calc R U . . .
H31 H 0.364943 0.459998 0.474727 0.135 Uiso 1 1 calc R U . . .
C40 C 0.1791(5) 0.4343(4) 0.4270(4) 0.0400(19) Uani 1 1 d . . . . .
H34 H 0.218270 0.407365 0.436560 0.048 Uiso 1 1 calc R U . . .
C41 C -0.0030(6) 0.5522(4) 0.3780(5) 0.048(2) Uani 1 1 d . . . . .
C42 C 0.0473(9) 0.5994(6) 0.3474(6) 0.081(3) Uani 1 1 d . . . . .
H35 H 0.108694 0.635636 0.384411 0.121 Uiso 1 1 calc R U . . .
H36 H 0.005637 0.626440 0.337484 0.121 Uiso 1 1 calc R U . . .
H37 H 0.059079 0.565630 0.301280 0.121 Uiso 1 1 calc R U . . .
C43 C -0.0303(6) 0.6016(5) 0.4485(5) 0.053(2) Uani 1 1 d . . . . .
H38 H -0.063935 0.569535 0.464213 0.079 Uiso 1 1 calc R U . . .
H40 H -0.072375 0.627646 0.437096 0.079 Uiso 1 1 calc R U . . .
H39 H 0.028269 0.638715 0.488693 0.079 Uiso 1 1 calc R U . . .
C44 C -0.0998(7) 0.4971(5) 0.3174(5) 0.071(3) Uani 1 1 d . . . . .
H43 H -0.087160 0.461441 0.272668 0.106 Uiso 1 1 calc R U . . .
H41 H -0.137184 0.525487 0.305340 0.106 Uiso 1 1 calc R U . . .
H42 H -0.136327 0.469472 0.336032 0.106 Uiso 1 1 calc R U . . .
C45 C -0.1084(5) 0.3016(4) 0.3562(4) 0.0302(17) Uani 1 1 d . . . . .
H46 H -0.103493 0.353344 0.383319 0.036 Uiso 1 1 calc R U . . .
C46 C -0.1886(5) 0.2413(4) 0.3332(4) 0.0307(17) Uani 1 1 d . . . . .
H45 H -0.249434 0.243693 0.340405 0.037 Uiso 1 1 calc R U . . .
C47 C -0.3159(4) 0.0696(4) 0.2338(4) 0.0271(16) Uani 1 1 d . . . . .
C48 C -0.3724(5) -0.0044(4) 0.2124(4) 0.0303(17) Uani 1 1 d . . . . .
H66 H -0.340283 -0.034267 0.223699 0.036 Uiso 1 1 calc R U . . .
C49 C -0.4682(5) -0.0345(4) 0.1774(4) 0.0335(17) Uani 1 1 d . . . . .
C50 C -0.5185(5) 0.0133(4) 0.1614(4) 0.0339(18) Uani 1 1 d . . . . .
C51 C -0.4606(5) 0.0858(4) 0.1746(4) 0.0327(17) Uani 1 1 d . . . . .
C52 C -0.3645(5) 0.1109(4) 0.2096(4) 0.0314(17) Uani 1 1 d . . . . .
H47 H -0.327601 0.157942 0.218744 0.038 Uiso 1 1 calc R U . . .
C53 C -0.5096(5) 0.1302(4) 0.1481(5) 0.044(2) Uani 1 1 d . . . . .
C54 C -0.4369(5) 0.2025(4) 0.1649(5) 0.046(2) Uani 1 1 d . . . . .
H48 H -0.406369 0.235048 0.218692 0.069 Uiso 1 1 calc R U . . .
H50 H -0.470314 0.228954 0.146382 0.069 Uiso 1 1 calc R U . . .
H49 H -0.387675 0.189734 0.140246 0.069 Uiso 1 1 calc R U . . .
C55 C -0.5845(6) 0.1538(5) 0.1888(6) 0.066(3) Uani 1 1 d . . . . .
H51 H -0.633557 0.108777 0.177887 0.099 Uiso 1 1 calc R U . . .
H53 H -0.614940 0.182502 0.171856 0.099 Uiso 1 1 calc R U . . .
H52 H -0.552441 0.185025 0.242521 0.099 Uiso 1 1 calc R U . . .
C56 C -0.5590(7) 0.0814(5) 0.0630(5) 0.065(3) Uani 1 1 d . . . . .
H55 H -0.511783 0.063973 0.037923 0.097 Uiso 1 1 calc R U . . .
H56 H -0.585236 0.111503 0.045651 0.097 Uiso 1 1 calc R U . . .
H54 H -0.611279 0.037968 0.051702 0.097 Uiso 1 1 calc R U . . .
C57 C -0.5256(5) -0.1132(4) 0.1558(5) 0.0409(19) Uani 1 1 d . . . . .
C58 C -0.6037(6) -0.1121(5) 0.1938(6) 0.062(3) Uani 1 1 d . . . . .
H57 H -0.574703 -0.079820 0.247784 0.094 Uiso 1 1 calc R U . . .
H59 H -0.635898 -0.163316 0.181253 0.094 Uiso 1 1 calc R U . . .
H58 H -0.650871 -0.092485 0.176780 0.094 Uiso 1 1 calc R U . . .
C59 C -0.4603(6) -0.1530(5) 0.1780(6) 0.060(3) Uani 1 1 d . . . . .
H62 H -0.409990 -0.156290 0.153341 0.090 Uiso 1 1 calc R U . . .
H61 H -0.499017 -0.203666 0.162703 0.090 Uiso 1 1 calc R U . . .
H60 H -0.430432 -0.124025 0.232040 0.090 Uiso 1 1 calc R U . . .
C60 C -0.5717(6) -0.1613(5) 0.0701(5) 0.059(2) Uani 1 1 d . . . . .
H63 H -0.609599 -0.135540 0.053938 0.089 Uiso 1 1 calc R U . . .
H64 H -0.613654 -0.210486 0.056295 0.089 Uiso 1 1 calc R U . . .
H65 H -0.520870 -0.168133 0.046059 0.089 Uiso 1 1 calc R U . . .
C61 C -0.1923(5) 0.0183(4) 0.3311(4) 0.0283(16) Uani 1 1 d . . . . .
H91 H -0.251688 0.007890 0.340907 0.034 Uiso 1 1 calc R U . . .
C62 C -0.1140(4) -0.0039(4) 0.3471(4) 0.0249(16) Uani 1 1 d . . . . .
C63 C -0.0953(4) -0.0441(4) 0.3829(4) 0.0269(16) Uani 1 1 d . . . . .
C64 C -0.0976(5) -0.1010(4) 0.4418(4) 0.0305(17) Uani 1 1 d . . . . .
C66 C -0.0584(5) -0.1666(4) 0.4950(4) 0.0325(17) Uani 1 1 d . . . . .
C67 C 0.0255(5) -0.1648(4) 0.4749(4) 0.0343(18) Uani 1 1 d . . . . .
C69 C -0.0112(5) -0.1009(4) 0.4217(4) 0.0281(17) Uani 1 1 d . . . . .
C70 C 0.0588(5) -0.0537(4) 0.3435(4) 0.0275(16) Uani 1 1 d . . . . .
C71 C 0.1589(4) -0.0222(4) 0.3966(4) 0.0301(17) Uani 1 1 d . . . . .
H86 H 0.182089 0.029460 0.434538 0.036 Uiso 1 1 calc R U . . .
C72 C 0.2161(5) -0.0649(4) 0.3919(4) 0.0357(18) Uani 1 1 d . . . . .
C73 C 0.1804(6) -0.1461(5) 0.3334(5) 0.045(2) Uani 1 1 d . . . . .
C74 C 0.0914(5) -0.1736(4) 0.2702(4) 0.0375(18) Uani 1 1 d . . . . .
C75 C 0.0376(5) -0.1297(4) 0.2777(4) 0.0312(17) Uani 1 1 d . . . . .
H67 H -0.019333 -0.147891 0.238099 0.037 Uiso 1 1 calc R U . . .
C76 C 0.0672(6) -0.2518(4) 0.2004(5) 0.049(2) Uani 1 1 d . . . . .
C77 C 0.1563(7) -0.2557(6) 0.1697(6) 0.078(3) Uani 1 1 d . . . . .
H68 H 0.142446 -0.305946 0.126413 0.118 Uiso 1 1 calc R U . . .
H69 H 0.212821 -0.245478 0.208507 0.118 Uiso 1 1 calc R U . . .
H70 H 0.169206 -0.218081 0.155095 0.118 Uiso 1 1 calc R U . . .
C78 C -0.0188(7) -0.2673(5) 0.1403(5) 0.073(3) Uani 1 1 d . . . . .
H71 H -0.031792 -0.317243 0.096763 0.109 Uiso 1 1 calc R U . . .
H73 H -0.005782 -0.229202 0.126404 0.109 Uiso 1 1 calc R U . . .
H72 H -0.074973 -0.265738 0.158669 0.109 Uiso 1 1 calc R U . . .
C79 C 0.0449(8) -0.3129(5) 0.2202(6) 0.076(3) Uani 1 1 d . . . . .
H75 H -0.006265 -0.307421 0.243946 0.115 Uiso 1 1 calc R U . . .
H76 H 0.102886 -0.307716 0.254393 0.115 Uiso 1 1 calc R U . . .
H74 H 0.023846 -0.362551 0.174750 0.115 Uiso 1 1 calc R U . . .
C80 C 0.3179(5) -0.0318(5) 0.4472(5) 0.046(2) Uani 1 1 d . . . . .
C81 C 0.3913(6) -0.0498(6) 0.4035(5) 0.062(3) Uani 1 1 d . . . . .
H78 H 0.387204 -0.029064 0.370887 0.093 Uiso 1 1 calc R U . . .
H79 H 0.377004 -0.104474 0.373351 0.093 Uiso 1 1 calc R U . . .
H77 H 0.456388 -0.027412 0.438391 0.093 Uiso 1 1 calc R U . . .
C82 C 0.3198(6) -0.0674(6) 0.4966(5) 0.069(3) Uani 1 1 d . . . . .
H80 H 0.381725 -0.042604 0.535809 0.104 Uiso 1 1 calc R U . . .
H81 H 0.311357 -0.121157 0.465938 0.104 Uiso 1 1 calc R U . . .
H82 H 0.267653 -0.060870 0.519202 0.104 Uiso 1 1 calc R U . . .
C83 C 0.3451(6) 0.0527(5) 0.4962(5) 0.058(2) Uani 1 1 d . . . . .
H85 H 0.412975 0.072976 0.525823 0.087 Uiso 1 1 calc R U . . .
H84 H 0.304964 0.065100 0.529457 0.087 Uiso 1 1 calc R U . . .
H83 H 0.335134 0.074696 0.465112 0.087 Uiso 1 1 calc R U . . .
C84 C 0.0909(5) -0.2007(4) 0.4927(4) 0.0347(18) Uani 1 1 d . . . . .
C86 C -0.0830(5) -0.2059(4) 0.5323(4) 0.0381(19) Uani 1 1 d . . . . .
N1 N 0.0880(4) 0.0663(3) 0.2534(3) 0.0261(13) Uani 1 1 d . . . . .
N2 N -0.0724(4) 0.0648(3) 0.2943(3) 0.0233(13) Uani 1 1 d . . . . .
N3 N -0.0685(4) 0.1931(3) 0.2972(3) 0.0265(13) Uani 1 1 d . . . . .
N4 N 0.0945(4) 0.1950(3) 0.2596(3) 0.0259(13) Uani 1 1 d . . . . .
N5 N -0.1490(4) -0.0659(3) 0.4180(3) 0.0302(14) Uani 1 1 d . . . . .
N6 N -0.0107(4) -0.0617(3) 0.3853(3) 0.0290(14) Uani 1 1 d . . . . .
N7 N -0.1223(4) -0.1349(3) 0.4794(3) 0.0345(15) Uani 1 1 d . . . . .
N8 N 0.0516(4) -0.1320(3) 0.4361(3) 0.0306(14) Uani 1 1 d . . . . .
N9 N 0.1408(5) -0.2296(4) 0.5077(4) 0.0485(17) Uani 1 1 d . . . . .
N10 N -0.1039(5) -0.2388(4) 0.5607(4) 0.0502(18) Uani 1 1 d . . . . .
OW1 O 0.586(2) 0.1484(16) 0.3887(17) 0.362(13) Uiso 1 1 d . . . . .
OW2 O 0.667(2) 0.7800(19) 0.605(2) 0.441(17) Uiso 1 1 d . . . . .
O1 O 0.1920(4) 0.6259(3) 0.4893(3) 0.0514(15) Uani 1 1 d D . . . .
H1O H 0.141(3) 0.6507(17) 0.490(4) 0.077 Uiso 1 1 d D U . . .
O2 O -0.6071(3) -0.0095(3) 0.1344(3) 0.0539(16) Uani 1 1 d . . . . .
O3 O 0.1526(4) -0.0353(3) -0.1190(3) 0.0513(15) Uani 1 1 d . . . . .
O4 O 0.2228(4) -0.1900(3) 0.3352(4) 0.0695(18) Uani 1 1 d . . . . .
Ni Ni 0.00710(6) 0.12786(5) 0.27247(5) 0.0264(4) Uani 1 1 d . . . . .


_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
C1 C2 1.374(9) . ?
C1 N1 1.428(8) . ?
C1 C14 1.440(9) . ?
C2 C3 1.402(9) . ?
C2 C70 1.545(9) . ?
C3 N2 1.379(8) . ?
C3 C62 1.415(9) . ?
C4 N2 1.382(8) . ?
C4 C61 1.415(9) . ?
C4 C5 1.465(9) . ?
C5 C47 1.384(9) . ?
C5 C6 1.449(9) . ?
C6 N3 1.364(8) . ?
C6 C46 1.423(9) . ?
C7 C8 1.381(9) . ?
C7 N3 1.403(8) . ?
C7 C45 1.427(9) . ?
C8 C9 1.405(10) . ?
C8 C31 1.485(10) . ?
C9 N4 1.389(8) . ?
C9 C30 1.428(9) . ?
C10 N4 1.345(8) . ?
C10 C29 1.412(9) . ?
C10 C11 1.470(9) . ?
C11 C15 1.380(9) . ?
C11 C12 1.464(9) . ?
C12 N1 1.337(8) . ?
C12 C13 1.435(9) . ?
C13 C14 1.359(9) . ?
C13 H2 0.9500 . ?
C14 H1 0.9500 . ?
C15 C20 1.446(9) . ?
C15 C16 1.446(9) . ?
C16 C17 1.353(9) . ?
C16 H22 0.9500 . ?
C17 C18 1.496(10) . ?
C17 C25 1.512(10) . ?
C18 O3 1.235(9) . ?
C18 C19 1.473(10) . ?
C19 C20 1.342(9) . ?
C19 C21 1.544(9) . ?
C20 H3 0.9500 . ?
C21 C24 1.524(10) . ?
C21 C23 1.536(10) . ?
C21 C22 1.538(10) . ?
C22 H5 0.9800 . ?
C22 H6 0.9800 . ?
C22 H4 0.9800 . ?
C23 H8 0.9800 . ?
C23 H7 0.9800 . ?
C23 H9 0.9800 . ?
C24 H10 0.9800 . ?
C24 H11 0.9800 . ?
C24 H12 0.9800 . ?
C25 C27 1.524(9) . ?
C25 C28 1.546(10) . ?
C25 C26 1.553(10) . ?
C26 H13 0.9800 . ?
C26 H15 0.9800 . ?
C26 H14 0.9800 . ?
C27 H18 0.9800 . ?
C27 H17 0.9800 . ?
C27 H16 0.9800 . ?
C28 H21 0.9800 . ?
C28 H19 0.9800 . ?
C28 H20 0.9800 . ?
C29 C30 1.350(10) . ?
C29 H24 0.9500 . ?
C30 H23 0.9500 . ?
C31 C32 1.398(10) . ?
C31 C40 1.416(10) . ?
C32 C33 1.396(10) . ?
C32 H44 0.9500 . ?
C33 C34 1.406(10) . ?
C33 C41 1.517(10) . ?
C34 O1 1.378(9) . ?
C34 C35 1.419(10) . ?
C35 C40 1.334(10) . ?
C35 C36 1.540(11) . ?
C36 C39 1.513(12) . ?
C36 C38 1.531(14) . ?
C36 C37 1.549(15) . ?
C37 H25 0.9800 . ?
C37 H26 0.9800 . ?
C37 H27 0.9800 . ?
C38 H28 0.9800 . ?
C38 H30 0.9800 . ?
C38 H29 0.9800 . ?
C39 H33 0.9800 . ?
C39 H32 0.9800 . ?
C39 H31 0.9800 . ?
C40 H34 0.9500 . ?
C41 C44 1.552(12) . ?
C41 C43 1.558(12) . ?
C41 C42 1.572(11) . ?
C42 H35 0.9800 . ?
C42 H36 0.9800 . ?
C42 H37 0.9800 . ?
C43 H38 0.9800 . ?
C43 H40 0.9800 . ?
C43 H39 0.9800 . ?
C44 H43 0.9800 . ?
C44 H41 0.9800 . ?
C44 H42 0.9800 . ?
C45 C46 1.384(9) . ?
C45 H46 0.9500 . ?
C46 H45 0.9500 . ?
C47 C48 1.436(9) . ?
C47 C52 1.444(9) . ?
C48 C49 1.353(9) . ?
C48 H66 0.9500 . ?
C49 C50 1.492(9) . ?
C49 C57 1.522(10) . ?
C50 O2 1.239(8) . ?
C50 C51 1.476(10) . ?
C51 C52 1.359(9) . ?
C51 C53 1.533(10) . ?
C52 H47 0.9500 . ?
C53 C54 1.535(10) . ?
C53 C55 1.543(11) . ?
C53 C56 1.550(12) . ?
C54 H48 0.9800 . ?
C54 H50 0.9800 . ?
C54 H49 0.9800 . ?
C55 H51 0.9800 . ?
C55 H53 0.9800 . ?
C55 H52 0.9800 . ?
C56 H55 0.9800 . ?
C56 H56 0.9800 . ?
C56 H54 0.9800 . ?
C57 C58 1.523(11) . ?
C57 C59 1.550(10) . ?
C57 C60 1.553(12) . ?
C58 H57 0.9800 . ?
C58 H59 0.9800 . ?
C58 H58 0.9800 . ?
C59 H62 0.9800 . ?
C59 H61 0.9800 . ?
C59 H60 0.9800 . ?
C60 H63 0.9800 . ?
C60 H64 0.9800 . ?
C60 H65 0.9800 . ?
C61 C62 1.384(9) . ?
C61 H91 0.9500 . ?
C62 C63 1.418(9) . ?
C63 N5 1.339(8) . ?
C63 N6 1.378(8) . ?
C64 N7 1.352(8) . ?
C64 N5 1.354(8) . ?
C64 C69 1.421(9) . ?
C66 N7 1.345(9) . ?
C66 C67 1.385(10) . ?
C66 C86 1.435(11) . ?
C67 N8 1.364(9) . ?
C67 C84 1.446(10) . ?
C69 N8 1.312(8) . ?
C69 N6 1.375(8) . ?
C70 C75 1.483(10) . ?
C70 C71 1.509(9) . ?
C70 N6 1.510(8) . ?
C71 C72 1.338(9) . ?
C71 H86 0.9500 . ?
C72 C73 1.488(11) . ?
C72 C80 1.542(10) . ?
C73 O4 1.228(9) . ?
C73 C74 1.505(11) . ?
C74 C75 1.313(9) . ?
C74 C76 1.539(11) . ?
C75 H67 0.9500 . ?
C76 C78 1.505(12) . ?
C76 C79 1.533(11) . ?
C76 C77 1.575(12) . ?
C77 H68 0.9800 . ?
C77 H69 0.9800 . ?
C77 H70 0.9800 . ?
C78 H71 0.9800 . ?
C78 H73 0.9800 . ?
C78 H72 0.9800 . ?
C79 H75 0.9800 . ?
C79 H76 0.9800 . ?
C79 H74 0.9800 . ?
C80 C83 1.512(12) . ?
C80 C81 1.543(11) . ?
C80 C82 1.554(11) . ?
C81 H78 0.9800 . ?
C81 H79 0.9800 . ?
C81 H77 0.9800 . ?
C82 H80 0.9800 . ?
C82 H81 0.9800 . ?
C82 H82 0.9800 . ?
C83 H85 0.9800 . ?
C83 H84 0.9800 . ?
C83 H83 0.9800 . ?
C84 N9 1.141(9) . ?
C86 N10 1.150(9) . ?
N1 Ni 1.894(5) . ?
N2 Ni 1.885(5) . ?
N3 Ni 1.890(5) . ?
N4 Ni 1.886(5) . ?
O1 H1O 1.00(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 121.3(5) . . ?
C2 C1 C14 130.3(6) . . ?
N1 C1 C14 107.6(5) . . ?
C1 C2 C3 122.5(6) . . ?
C1 C2 C70 117.9(6) . . ?
C3 C2 C70 118.9(5) . . ?
N2 C3 C2 126.0(5) . . ?
N2 C3 C62 109.2(5) . . ?
C2 C3 C62 124.4(6) . . ?
N2 C4 C61 110.5(5) . . ?
N2 C4 C5 120.0(5) . . ?
C61 C4 C5 129.2(6) . . ?
C47 C5 C6 123.0(6) . . ?
C47 C5 C4 123.1(6) . . ?
C6 C5 C4 113.8(5) . . ?
N3 C6 C46 110.6(6) . . ?
N3 C6 C5 122.9(6) . . ?
C46 C6 C5 125.8(6) . . ?
C8 C7 N3 123.0(6) . . ?
C8 C7 C45 128.1(6) . . ?
N3 C7 C45 108.8(5) . . ?
C7 C8 C9 122.6(6) . . ?
C7 C8 C31 120.3(6) . . ?
C9 C8 C31 117.0(6) . . ?
N4 C9 C8 123.8(6) . . ?
N4 C9 C30 107.6(6) . . ?
C8 C9 C30 127.1(6) . . ?
N4 C10 C29 110.6(6) . . ?
N4 C10 C11 120.1(6) . . ?
C29 C10 C11 129.3(6) . . ?
C15 C11 C12 122.2(6) . . ?
C15 C11 C10 124.2(6) . . ?
C12 C11 C10 113.6(6) . . ?
N1 C12 C13 112.1(5) . . ?
N1 C12 C11 121.2(6) . . ?
C13 C12 C11 126.4(6) . . ?
C14 C13 C12 106.0(6) . . ?
C14 C13 H2 127.0 . . ?
C12 C13 H2 127.0 . . ?
C13 C14 C1 108.3(6) . . ?
C13 C14 H1 125.9 . . ?
C1 C14 H1 125.9 . . ?
C11 C15 C20 122.5(6) . . ?
C11 C15 C16 121.0(6) . . ?
C20 C15 C16 116.5(6) . . ?
C17 C16 C15 123.9(6) . . ?
C17 C16 H22 118.1 . . ?
C15 C16 H22 118.1 . . ?
C16 C17 C18 118.0(6) . . ?
C16 C17 C25 121.2(6) . . ?
C18 C17 C25 120.8(6) . . ?
O3 C18 C19 121.5(6) . . ?
O3 C18 C17 120.0(7) . . ?
C19 C18 C17 118.5(6) . . ?
C20 C19 C18 119.3(6) . . ?
C20 C19 C21 121.0(6) . . ?
C18 C19 C21 119.7(6) . . ?
C19 C20 C15 123.6(6) . . ?
C19 C20 H3 118.2 . . ?
C15 C20 H3 118.2 . . ?
C24 C21 C23 108.2(6) . . ?
C24 C21 C22 108.2(6) . . ?
C23 C21 C22 109.6(6) . . ?
C24 C21 C19 111.7(6) . . ?
C23 C21 C19 109.3(5) . . ?
C22 C21 C19 109.8(6) . . ?
C21 C22 H5 109.5 . . ?
C21 C22 H6 109.5 . . ?
H5 C22 H6 109.5 . . ?
C21 C22 H4 109.5 . . ?
H5 C22 H4 109.5 . . ?
H6 C22 H4 109.5 . . ?
C21 C23 H8 109.5 . . ?
C21 C23 H7 109.5 . . ?
H8 C23 H7 109.5 . . ?
C21 C23 H9 109.5 . . ?
H8 C23 H9 109.5 . . ?
H7 C23 H9 109.5 . . ?
C21 C24 H10 109.5 . . ?
C21 C24 H11 109.5 . . ?
H10 C24 H11 109.5 . . ?
C21 C24 H12 109.5 . . ?
H10 C24 H12 109.5 . . ?
H11 C24 H12 109.5 . . ?
C17 C25 C27 111.9(6) . . ?
C17 C25 C28 109.8(6) . . ?
C27 C25 C28 107.1(6) . . ?
C17 C25 C26 111.4(5) . . ?
C27 C25 C26 107.8(6) . . ?
C28 C25 C26 108.6(6) . . ?
C25 C26 H13 109.5 . . ?
C25 C26 H15 109.5 . . ?
H13 C26 H15 109.5 . . ?
C25 C26 H14 109.5 . . ?
H13 C26 H14 109.5 . . ?
H15 C26 H14 109.5 . . ?
C25 C27 H18 109.5 . . ?
C25 C27 H17 109.5 . . ?
H18 C27 H17 109.5 . . ?
C25 C27 H16 109.5 . . ?
H18 C27 H16 109.5 . . ?
H17 C27 H16 109.5 . . ?
C25 C28 H21 109.5 . . ?
C25 C28 H19 109.5 . . ?
H21 C28 H19 109.5 . . ?
C25 C28 H20 109.5 . . ?
H21 C28 H20 109.5 . . ?
H19 C28 H20 109.5 . . ?
C30 C29 C10 106.7(6) . . ?
C30 C29 H24 126.7 . . ?
C10 C29 H24 126.7 . . ?
C29 C30 C9 108.1(6) . . ?
C29 C30 H23 126.0 . . ?
C9 C30 H23 126.0 . . ?
C32 C31 C40 117.4(7) . . ?
C32 C31 C8 122.4(6) . . ?
C40 C31 C8 120.2(6) . . ?
C33 C32 C31 122.9(7) . . ?
C33 C32 H44 118.6 . . ?
C31 C32 H44 118.6 . . ?
C32 C33 C34 115.8(6) . . ?
C32 C33 C41 119.3(7) . . ?
C34 C33 C41 124.9(6) . . ?
O1 C34 C33 121.0(7) . . ?
O1 C34 C35 115.8(6) . . ?
C33 C34 C35 123.2(6) . . ?
C40 C35 C34 117.7(7) . . ?
C40 C35 C36 120.4(7) . . ?
C34 C35 C36 121.9(7) . . ?
C39 C36 C38 108.2(9) . . ?
C39 C36 C35 110.9(7) . . ?
C38 C36 C35 111.2(7) . . ?
C39 C36 C37 105.9(8) . . ?
C38 C36 C37 110.6(9) . . ?
C35 C36 C37 109.8(9) . . ?
C36 C37 H25 109.5 . . ?
C36 C37 H26 109.5 . . ?
H25 C37 H26 109.5 . . ?
C36 C37 H27 109.5 . . ?
H25 C37 H27 109.5 . . ?
H26 C37 H27 109.5 . . ?
C36 C38 H28 109.5 . . ?
C36 C38 H30 109.5 . . ?
H28 C38 H30 109.5 . . ?
C36 C38 H29 109.5 . . ?
H28 C38 H29 109.5 . . ?
H30 C38 H29 109.5 . . ?
C36 C39 H33 109.5 . . ?
C36 C39 H32 109.5 . . ?
H33 C39 H32 109.5 . . ?
C36 C39 H31 109.5 . . ?
H33 C39 H31 109.5 . . ?
H32 C39 H31 109.5 . . ?
C35 C40 C31 123.1(7) . . ?
C35 C40 H34 118.4 . . ?
C31 C40 H34 118.4 . . ?
C33 C41 C44 113.0(6) . . ?
C33 C41 C43 109.5(6) . . ?
C44 C41 C43 105.6(7) . . ?
C33 C41 C42 109.6(7) . . ?
C44 C41 C42 106.7(7) . . ?
C43 C41 C42 112.4(7) . . ?
C41 C42 H35 109.5 . . ?
C41 C42 H36 109.5 . . ?
H35 C42 H36 109.5 . . ?
C41 C42 H37 109.5 . . ?
H35 C42 H37 109.5 . . ?
H36 C42 H37 109.5 . . ?
C41 C43 H38 109.5 . . ?
C41 C43 H40 109.5 . . ?
H38 C43 H40 109.5 . . ?
C41 C43 H39 109.5 . . ?
H38 C43 H39 109.5 . . ?
H40 C43 H39 109.5 . . ?
C41 C44 H43 109.5 . . ?
C41 C44 H41 109.5 . . ?
H43 C44 H41 109.5 . . ?
C41 C44 H42 109.5 . . ?
H43 C44 H42 109.5 . . ?
H41 C44 H42 109.5 . . ?
C46 C45 C7 107.3(6) . . ?
C46 C45 H46 126.4 . . ?
C7 C45 H46 126.4 . . ?
C45 C46 C6 106.7(6) . . ?
C45 C46 H45 126.7 . . ?
C6 C46 H45 126.7 . . ?
C5 C47 C48 122.6(6) . . ?
C5 C47 C52 120.8(6) . . ?
C48 C47 C52 116.6(6) . . ?
C49 C48 C47 124.4(6) . . ?
C49 C48 H66 117.8 . . ?
C47 C48 H66 117.8 . . ?
C48 C49 C50 117.5(6) . . ?
C48 C49 C57 122.9(6) . . ?
C50 C49 C57 119.6(6) . . ?
O2 C50 C51 121.0(6) . . ?
O2 C50 C49 120.1(6) . . ?
C51 C50 C49 118.9(6) . . ?
C52 C51 C50 118.6(6) . . ?
C52 C51 C53 121.9(6) . . ?
C50 C51 C53 119.5(6) . . ?
C51 C52 C47 123.2(6) . . ?
C51 C52 H47 118.4 . . ?
C47 C52 H47 118.4 . . ?
C51 C53 C54 111.6(6) . . ?
C51 C53 C55 110.1(6) . . ?
C54 C53 C55 107.2(7) . . ?
C51 C53 C56 109.7(6) . . ?
C54 C53 C56 108.1(7) . . ?
C55 C53 C56 110.1(7) . . ?
C53 C54 H48 109.5 . . ?
C53 C54 H50 109.5 . . ?
H48 C54 H50 109.5 . . ?
C53 C54 H49 109.5 . . ?
H48 C54 H49 109.5 . . ?
H50 C54 H49 109.5 . . ?
C53 C55 H51 109.5 . . ?
C53 C55 H53 109.5 . . ?
H51 C55 H53 109.5 . . ?
C53 C55 H52 109.5 . . ?
H51 C55 H52 109.5 . . ?
H53 C55 H52 109.5 . . ?
C53 C56 H55 109.5 . . ?
C53 C56 H56 109.5 . . ?
H55 C56 H56 109.5 . . ?
C53 C56 H54 109.5 . . ?
H55 C56 H54 109.5 . . ?
H56 C56 H54 109.5 . . ?
C49 C57 C58 112.1(7) . . ?
C49 C57 C59 111.4(6) . . ?
C58 C57 C59 106.9(7) . . ?
C49 C57 C60 109.0(6) . . ?
C58 C57 C60 109.7(7) . . ?
C59 C57 C60 107.6(7) . . ?
C57 C58 H57 109.5 . . ?
C57 C58 H59 109.5 . . ?
H57 C58 H59 109.5 . . ?
C57 C58 H58 109.5 . . ?
H57 C58 H58 109.5 . . ?
H59 C58 H58 109.5 . . ?
C57 C59 H62 109.5 . . ?
C57 C59 H61 109.5 . . ?
H62 C59 H61 109.5 . . ?
C57 C59 H60 109.5 . . ?
H62 C59 H60 109.5 . . ?
H61 C59 H60 109.5 . . ?
C57 C60 H63 109.5 . . ?
C57 C60 H64 109.5 . . ?
H63 C60 H64 109.5 . . ?
C57 C60 H65 109.5 . . ?
H63 C60 H65 109.5 . . ?
H64 C60 H65 109.5 . . ?
C62 C61 C4 105.8(5) . . ?
C62 C61 H91 127.1 . . ?
C4 C61 H91 127.1 . . ?
C61 C62 C3 108.1(5) . . ?
C61 C62 C63 132.8(6) . . ?
C3 C62 C63 119.1(6) . . ?
N5 C63 N6 114.1(5) . . ?
N5 C63 C62 127.9(6) . . ?
N6 C63 C62 118.0(5) . . ?
N7 C64 N5 126.4(6) . . ?
N7 C64 C69 120.9(6) . . ?
N5 C64 C69 112.6(6) . . ?
N7 C66 C67 123.5(6) . . ?
N7 C66 C86 116.1(6) . . ?
C67 C66 C86 120.3(6) . . ?
N8 C67 C66 123.9(6) . . ?
N8 C67 C84 115.2(6) . . ?
C66 C67 C84 120.9(6) . . ?
N8 C69 N6 129.9(6) . . ?
N8 C69 C64 126.0(6) . . ?
N6 C69 C64 104.1(5) . . ?
C75 C70 C71 114.4(6) . . ?
C75 C70 N6 106.2(5) . . ?
C71 C70 N6 107.1(5) . . ?
C75 C70 C2 110.2(5) . . ?
C71 C70 C2 109.2(5) . . ?
N6 C70 C2 109.6(5) . . ?
C72 C71 C70 121.9(7) . . ?
C72 C71 H86 119.0 . . ?
C70 C71 H86 119.0 . . ?
C71 C72 C73 119.6(6) . . ?
C71 C72 C80 121.1(7) . . ?
C73 C72 C80 119.2(6) . . ?
O4 C73 C72 121.5(7) . . ?
O4 C73 C74 120.1(8) . . ?
C72 C73 C74 118.3(6) . . ?
C75 C74 C73 118.0(7) . . ?
C75 C74 C76 123.2(7) . . ?
C73 C74 C76 118.8(6) . . ?
C74 C75 C70 125.0(6) . . ?
C74 C75 H67 117.5 . . ?
C70 C75 H67 117.5 . . ?
C78 C76 C79 108.1(8) . . ?
C78 C76 C74 111.7(6) . . ?
C79 C76 C74 110.0(7) . . ?
C78 C76 C77 108.8(8) . . ?
C79 C76 C77 109.2(7) . . ?
C74 C76 C77 109.0(7) . . ?
C76 C77 H68 109.5 . . ?
C76 C77 H69 109.5 . . ?
H68 C77 H69 109.5 . . ?
C76 C77 H70 109.5 . . ?
H68 C77 H70 109.5 . . ?
H69 C77 H70 109.5 . . ?
C76 C78 H71 109.5 . . ?
C76 C78 H73 109.5 . . ?
H71 C78 H73 109.5 . . ?
C76 C78 H72 109.5 . . ?
H71 C78 H72 109.5 . . ?
H73 C78 H72 109.5 . . ?
C76 C79 H75 109.5 . . ?
C76 C79 H76 109.5 . . ?
H75 C79 H76 109.5 . . ?
C76 C79 H74 109.5 . . ?
H75 C79 H74 109.5 . . ?
H76 C79 H74 109.5 . . ?
C83 C80 C72 111.2(6) . . ?
C83 C80 C81 108.2(7) . . ?
C72 C80 C81 109.2(6) . . ?
C83 C80 C82 109.2(7) . . ?
C72 C80 C82 108.5(6) . . ?
C81 C80 C82 110.4(7) . . ?
C80 C81 H78 109.5 . . ?
C80 C81 H79 109.5 . . ?
H78 C81 H79 109.5 . . ?
C80 C81 H77 109.5 . . ?
H78 C81 H77 109.5 . . ?
H79 C81 H77 109.5 . . ?
C80 C82 H80 109.5 . . ?
C80 C82 H81 109.5 . . ?
H80 C82 H81 109.5 . . ?
C80 C82 H82 109.5 . . ?
H80 C82 H82 109.5 . . ?
H81 C82 H82 109.5 . . ?
C80 C83 H85 109.5 . . ?
C80 C83 H84 109.5 . . ?
H85 C83 H84 109.5 . . ?
C80 C83 H83 109.5 . . ?
H85 C83 H83 109.5 . . ?
H84 C83 H83 109.5 . . ?
N9 C84 C67 178.0(8) . . ?
N10 C86 C66 178.5(9) . . ?
C12 N1 C1 105.8(5) . . ?
C12 N1 Ni 126.6(4) . . ?
C1 N1 Ni 127.6(4) . . ?
C3 N2 C4 106.2(5) . . ?
C3 N2 Ni 124.8(4) . . ?
C4 N2 Ni 128.3(4) . . ?
C6 N3 C7 106.5(5) . . ?
C6 N3 Ni 126.8(4) . . ?
C7 N3 Ni 126.0(4) . . ?
C10 N4 C9 107.0(5) . . ?
C10 N4 Ni 127.4(5) . . ?
C9 N4 Ni 125.5(4) . . ?
C63 N5 C64 103.0(5) . . ?
C69 N6 C63 106.2(5) . . ?
C69 N6 C70 126.0(5) . . ?
C63 N6 C70 126.8(5) . . ?
C66 N7 C64 113.8(6) . . ?
C69 N8 C67 111.9(6) . . ?
C34 O1 H1O 112(2) . . ?
N2 Ni N4 174.7(2) . . ?
N2 Ni N3 90.3(2) . . ?
N4 Ni N3 90.4(2) . . ?
N2 Ni N1 90.1(2) . . ?
N4 Ni N1 88.9(2) . . ?
N3 Ni N1 176.6(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
N1 C1 C2 C3 3.7(10) . . . . ?
C14 C1 C2 C3 -165.2(7) . . . . ?
N1 C1 C2 C70 174.3(6) . . . . ?
C14 C1 C2 C70 5.4(11) . . . . ?
C1 C2 C3 N2 -1.8(11) . . . . ?
C70 C2 C3 N2 -172.3(6) . . . . ?
C1 C2 C3 C62 170.5(6) . . . . ?
C70 C2 C3 C62 -0.1(10) . . . . ?
N2 C4 C5 C47 141.7(7) . . . . ?
C61 C4 C5 C47 -44.2(11) . . . . ?
N2 C4 C5 C6 -42.0(9) . . . . ?
C61 C4 C5 C6 132.2(7) . . . . ?
C47 C5 C6 N3 -143.6(7) . . . . ?
C4 C5 C6 N3 40.0(9) . . . . ?
C47 C5 C6 C46 47.0(10) . . . . ?
C4 C5 C6 C46 -129.4(7) . . . . ?
N3 C7 C8 C9 5.7(10) . . . . ?
C45 C7 C8 C9 -168.7(6) . . . . ?
N3 C7 C8 C31 -177.4(6) . . . . ?
C45 C7 C8 C31 8.1(10) . . . . ?
C7 C8 C9 N4 -6.2(10) . . . . ?
C31 C8 C9 N4 176.8(6) . . . . ?
C7 C8 C9 C30 158.3(7) . . . . ?
C31 C8 C9 C30 -18.7(10) . . . . ?
N4 C10 C11 C15 139.5(6) . . . . ?
C29 C10 C11 C15 -45.0(10) . . . . ?
N4 C10 C11 C12 -40.8(8) . . . . ?
C29 C10 C11 C12 134.6(7) . . . . ?
C15 C11 C12 N1 -138.7(7) . . . . ?
C10 C11 C12 N1 41.6(8) . . . . ?
C15 C11 C12 C13 48.0(10) . . . . ?
C10 C11 C12 C13 -131.7(7) . . . . ?
N1 C12 C13 C14 1.8(8) . . . . ?
C11 C12 C13 C14 175.6(7) . . . . ?
C12 C13 C14 C1 1.5(8) . . . . ?
C2 C1 C14 C13 166.0(7) . . . . ?
N1 C1 C14 C13 -4.1(7) . . . . ?
C12 C11 C15 C20 -179.6(6) . . . . ?
C10 C11 C15 C20 0.1(10) . . . . ?
C12 C11 C15 C16 2.1(9) . . . . ?
C10 C11 C15 C16 -178.2(6) . . . . ?
C11 C15 C16 C17 -179.4(6) . . . . ?
C20 C15 C16 C17 2.2(9) . . . . ?
C15 C16 C17 C18 -3.8(9) . . . . ?
C15 C16 C17 C25 177.3(6) . . . . ?
C16 C17 C18 O3 -173.6(6) . . . . ?
C25 C17 C18 O3 5.3(10) . . . . ?
C16 C17 C18 C19 5.0(9) . . . . ?
C25 C17 C18 C19 -176.1(6) . . . . ?
O3 C18 C19 C20 173.7(7) . . . . ?
C17 C18 C19 C20 -4.9(9) . . . . ?
O3 C18 C19 C21 -4.2(10) . . . . ?
C17 C18 C19 C21 177.3(6) . . . . ?
C18 C19 C20 C15 3.4(10) . . . . ?
C21 C19 C20 C15 -178.7(6) . . . . ?
C11 C15 C20 C19 179.7(6) . . . . ?
C16 C15 C20 C19 -1.9(9) . . . . ?
C20 C19 C21 C24 4.0(9) . . . . ?
C18 C19 C21 C24 -178.1(6) . . . . ?
C20 C19 C21 C23 123.8(7) . . . . ?
C18 C19 C21 C23 -58.4(8) . . . . ?
C20 C19 C21 C22 -116.0(7) . . . . ?
C18 C19 C21 C22 61.9(8) . . . . ?
C16 C17 C25 C27 -5.0(9) . . . . ?
C18 C17 C25 C27 176.1(6) . . . . ?
C16 C17 C25 C28 -123.9(7) . . . . ?
C18 C17 C25 C28 57.2(8) . . . . ?
C16 C17 C25 C26 115.7(7) . . . . ?
C18 C17 C25 C26 -63.2(8) . . . . ?
N4 C10 C29 C30 -0.4(8) . . . . ?
C11 C10 C29 C30 -176.2(6) . . . . ?
C10 C29 C30 C9 -1.1(7) . . . . ?
N4 C9 C30 C29 2.2(7) . . . . ?
C8 C9 C30 C29 -164.3(7) . . . . ?
C7 C8 C31 C32 -53.5(10) . . . . ?
C9 C8 C31 C32 123.6(7) . . . . ?
C7 C8 C31 C40 128.3(7) . . . . ?
C9 C8 C31 C40 -54.7(9) . . . . ?
C40 C31 C32 C33 -1.4(10) . . . . ?
C8 C31 C32 C33 -179.6(6) . . . . ?
C31 C32 C33 C34 0.4(10) . . . . ?
C31 C32 C33 C41 -178.4(7) . . . . ?
C32 C33 C34 O1 -179.1(6) . . . . ?
C41 C33 C34 O1 -0.3(11) . . . . ?
C32 C33 C34 C35 0.3(11) . . . . ?
C41 C33 C34 C35 179.0(7) . . . . ?
O1 C34 C35 C40 179.4(7) . . . . ?
C33 C34 C35 C40 0.0(11) . . . . ?
O1 C34 C35 C36 -2.8(11) . . . . ?
C33 C34 C35 C36 177.8(7) . . . . ?
C40 C35 C36 C39 0.4(12) . . . . ?
C34 C35 C36 C39 -177.4(9) . . . . ?
C40 C35 C36 C38 -120.1(9) . . . . ?
C34 C35 C36 C38 62.1(11) . . . . ?
C40 C35 C36 C37 117.1(9) . . . . ?
C34 C35 C36 C37 -60.7(10) . . . . ?
C34 C35 C40 C31 -1.0(11) . . . . ?
C36 C35 C40 C31 -178.9(7) . . . . ?
C32 C31 C40 C35 1.6(11) . . . . ?
C8 C31 C40 C35 179.9(7) . . . . ?
C32 C33 C41 C44 -0.9(10) . . . . ?
C34 C33 C41 C44 -179.6(7) . . . . ?
C32 C33 C41 C43 116.6(8) . . . . ?
C34 C33 C41 C43 -62.1(9) . . . . ?
C32 C33 C41 C42 -119.7(8) . . . . ?
C34 C33 C41 C42 61.6(10) . . . . ?
C8 C7 C45 C46 171.7(7) . . . . ?
N3 C7 C45 C46 -3.4(7) . . . . ?
C7 C45 C46 C6 1.8(7) . . . . ?
N3 C6 C46 C45 0.5(7) . . . . ?
C5 C6 C46 C45 171.1(6) . . . . ?
C6 C5 C47 C48 -177.7(6) . . . . ?
C4 C5 C47 C48 -1.7(10) . . . . ?
C6 C5 C47 C52 5.1(10) . . . . ?
C4 C5 C47 C52 -178.8(6) . . . . ?
C5 C47 C48 C49 177.0(7) . . . . ?
C52 C47 C48 C49 -5.8(10) . . . . ?
C47 C48 C49 C50 -1.3(10) . . . . ?
C47 C48 C49 C57 -179.8(7) . . . . ?
C48 C49 C50 O2 -174.7(7) . . . . ?
C57 C49 C50 O2 3.8(11) . . . . ?
C48 C49 C50 C51 8.5(10) . . . . ?
C57 C49 C50 C51 -173.0(6) . . . . ?
O2 C50 C51 C52 174.9(7) . . . . ?
C49 C50 C51 C52 -8.3(10) . . . . ?
O2 C50 C51 C53 -5.5(11) . . . . ?
C49 C50 C51 C53 171.3(6) . . . . ?
C50 C51 C52 C47 0.9(10) . . . . ?
C53 C51 C52 C47 -178.6(6) . . . . ?
C5 C47 C52 C51 -176.7(6) . . . . ?
C48 C47 C52 C51 6.0(10) . . . . ?
C52 C51 C53 C54 1.3(10) . . . . ?
C50 C51 C53 C54 -178.2(7) . . . . ?
C52 C51 C53 C55 -117.6(8) . . . . ?
C50 C51 C53 C55 62.9(9) . . . . ?
C52 C51 C53 C56 121.1(8) . . . . ?
C50 C51 C53 C56 -58.4(9) . . . . ?
C48 C49 C57 C58 118.8(8) . . . . ?
C50 C49 C57 C58 -59.6(9) . . . . ?
C48 C49 C57 C59 -0.9(11) . . . . ?
C50 C49 C57 C59 -179.3(7) . . . . ?
C48 C49 C57 C60 -119.5(7) . . . . ?
C50 C49 C57 C60 62.1(9) . . . . ?
N2 C4 C61 C62 -1.8(8) . . . . ?
C5 C4 C61 C62 -176.4(7) . . . . ?
C4 C61 C62 C3 -0.9(7) . . . . ?
C4 C61 C62 C63 177.5(7) . . . . ?
N2 C3 C62 C61 3.3(7) . . . . ?
C2 C3 C62 C61 -170.1(6) . . . . ?
N2 C3 C62 C63 -175.4(5) . . . . ?
C2 C3 C62 C63 11.2(10) . . . . ?
C61 C62 C63 N5 -6.9(12) . . . . ?
C3 C62 C63 N5 171.3(6) . . . . ?
C61 C62 C63 N6 175.5(7) . . . . ?
C3 C62 C63 N6 -6.2(9) . . . . ?
N7 C66 C67 N8 -1.2(11) . . . . ?
C86 C66 C67 N8 176.6(7) . . . . ?
N7 C66 C67 C84 -179.4(7) . . . . ?
C86 C66 C67 C84 -1.6(11) . . . . ?
N7 C64 C69 N8 0.2(11) . . . . ?
N5 C64 C69 N8 -178.7(6) . . . . ?
N7 C64 C69 N6 -179.8(6) . . . . ?
N5 C64 C69 N6 1.4(8) . . . . ?
C1 C2 C70 C75 -68.0(7) . . . . ?
C3 C2 C70 C75 102.9(7) . . . . ?
C1 C2 C70 C71 58.4(8) . . . . ?
C3 C2 C70 C71 -130.7(6) . . . . ?
C1 C2 C70 N6 175.4(6) . . . . ?
C3 C2 C70 N6 -13.6(8) . . . . ?
C75 C70 C71 C72 -12.2(8) . . . . ?
N6 C70 C71 C72 105.2(7) . . . . ?
C2 C70 C71 C72 -136.2(6) . . . . ?
C70 C71 C72 C73 -0.7(9) . . . . ?
C70 C71 C72 C80 -179.5(6) . . . . ?
C71 C72 C73 O4 -166.7(7) . . . . ?
C80 C72 C73 O4 12.1(10) . . . . ?
C71 C72 C73 C74 14.7(10) . . . . ?
C80 C72 C73 C74 -166.5(6) . . . . ?
O4 C73 C74 C75 166.3(7) . . . . ?
C72 C73 C74 C75 -15.1(10) . . . . ?
O4 C73 C74 C76 -13.1(10) . . . . ?
C72 C73 C74 C76 165.5(6) . . . . ?
C73 C74 C75 C70 1.4(10) . . . . ?
C76 C74 C75 C70 -179.2(6) . . . . ?
C71 C70 C75 C74 11.9(9) . . . . ?
N6 C70 C75 C74 -106.0(7) . . . . ?
C2 C70 C75 C74 135.3(7) . . . . ?
C75 C74 C76 C78 5.7(11) . . . . ?
C73 C74 C76 C78 -174.9(7) . . . . ?
C75 C74 C76 C79 -114.4(8) . . . . ?
C73 C74 C76 C79 65.0(9) . . . . ?
C75 C74 C76 C77 126.0(8) . . . . ?
C73 C74 C76 C77 -54.6(9) . . . . ?
C71 C72 C80 C83 -7.8(9) . . . . ?
C73 C72 C80 C83 173.3(6) . . . . ?
C71 C72 C80 C81 -127.2(8) . . . . ?
C73 C72 C80 C81 54.0(9) . . . . ?
C71 C72 C80 C82 112.3(8) . . . . ?
C73 C72 C80 C82 -66.5(9) . . . . ?
C13 C12 N1 C1 -4.2(7) . . . . ?
C11 C12 N1 C1 -178.4(6) . . . . ?
C13 C12 N1 Ni 173.4(4) . . . . ?
C11 C12 N1 Ni -0.8(9) . . . . ?
C2 C1 N1 C12 -166.1(6) . . . . ?
C14 C1 N1 C12 5.0(7) . . . . ?
C2 C1 N1 Ni 16.3(9) . . . . ?
C14 C1 N1 Ni -172.6(4) . . . . ?
C2 C3 N2 C4 169.0(6) . . . . ?
C62 C3 N2 C4 -4.3(7) . . . . ?
C2 C3 N2 Ni -19.7(9) . . . . ?
C62 C3 N2 Ni 167.0(4) . . . . ?
C61 C4 N2 C3 3.8(7) . . . . ?
C5 C4 N2 C3 178.9(6) . . . . ?
C61 C4 N2 Ni -167.1(4) . . . . ?
C5 C4 N2 Ni 8.0(9) . . . . ?
C46 C6 N3 C7 -2.6(7) . . . . ?
C5 C6 N3 C7 -173.5(6) . . . . ?
C46 C6 N3 Ni 167.7(4) . . . . ?
C5 C6 N3 Ni -3.1(9) . . . . ?
C8 C7 N3 C6 -171.7(6) . . . . ?
C45 C7 N3 C6 3.7(7) . . . . ?
C8 C7 N3 Ni 17.9(9) . . . . ?
C45 C7 N3 Ni -166.8(4) . . . . ?
C29 C10 N4 C9 1.8(7) . . . . ?
C11 C10 N4 C9 178.0(6) . . . . ?
C29 C10 N4 Ni -176.6(4) . . . . ?
C11 C10 N4 Ni -0.4(8) . . . . ?
C8 C9 N4 C10 164.7(6) . . . . ?
C30 C9 N4 C10 -2.4(7) . . . . ?
C8 C9 N4 Ni -16.9(9) . . . . ?
C30 C9 N4 Ni 176.0(4) . . . . ?
N6 C63 N5 C64 -1.9(7) . . . . ?
C62 C63 N5 C64 -179.6(7) . . . . ?
N7 C64 N5 C63 -178.5(7) . . . . ?
C69 C64 N5 C63 0.3(7) . . . . ?
N8 C69 N6 C63 177.7(7) . . . . ?
C64 C69 N6 C63 -2.4(7) . . . . ?
N8 C69 N6 C70 8.6(11) . . . . ?
C64 C69 N6 C70 -171.4(6) . . . . ?
N5 C63 N6 C69 2.9(8) . . . . ?
C62 C63 N6 C69 -179.2(6) . . . . ?
N5 C63 N6 C70 171.8(6) . . . . ?
C62 C63 N6 C70 -10.3(10) . . . . ?
C75 C70 N6 C69 67.4(7) . . . . ?
C71 C70 N6 C69 -55.2(8) . . . . ?
C2 C70 N6 C69 -173.5(6) . . . . ?
C75 C70 N6 C63 -99.4(7) . . . . ?
C71 C70 N6 C63 138.0(6) . . . . ?
C2 C70 N6 C63 19.7(9) . . . . ?
C67 C66 N7 C64 0.3(10) . . . . ?
C86 C66 N7 C64 -177.6(6) . . . . ?
N5 C64 N7 C66 178.9(7) . . . . ?
C69 C64 N7 C66 0.2(9) . . . . ?
N6 C69 N8 C67 179.0(7) . . . . ?
C64 C69 N8 C67 -1.0(10) . . . . ?
C66 C67 N8 C69 1.4(10) . . . . ?
C84 C67 N8 C69 179.8(6) . . . . ?
C3 N2 Ni N3 -148.4(5) . . . . ?
C4 N2 Ni N3 20.9(6) . . . . ?
C3 N2 Ni N1 28.2(5) . . . . ?
C4 N2 Ni N1 -162.5(6) . . . . ?
C10 N4 Ni N3 -152.9(5) . . . . ?
C9 N4 Ni N3 29.0(5) . . . . ?
C10 N4 Ni N1 30.4(5) . . . . ?
C9 N4 Ni N1 -147.7(5) . . . . ?
C6 N3 Ni N2 -23.5(5) . . . . ?
C7 N3 Ni N2 145.1(5) . . . . ?
C6 N3 Ni N4 161.8(5) . . . . ?
C7 N3 Ni N4 -29.6(5) . . . . ?
C12 N1 Ni N2 155.5(5) . . . . ?
C1 N1 Ni N2 -27.4(5) . . . . ?
C12 N1 Ni N4 -29.7(5) . . . . ?
C1 N1 Ni N4 147.4(5) . . . . ?

_refine_diff_density_max         1.221
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.183


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
####################################################################### 
# 
# 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_ox3_200k1_0m
_database_code_depnum_ccdc_archive 'CCDC 2107804'
loop_
_audit_author_name
_audit_author_address
'Yoshitaka Matsushita'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_ox3_200k1_0m        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Due to lower crystallinity and weaker peaks in wide angle region
;
_vrf_PLAT414_ox3_200k1_0m        
;
PROBLEM: Short Intra D-H..H-X       H1       ..H14B     .       1.80 Ang.
RESPONSE: H1 was placed using a riding model which is close to H14B
;
_vrf_PLAT910_ox3_200k1_0m        
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note
RESPONSE: Due to poor crystallinity 
;
# Added during the CSD deposition process: Monday 28 November 2022 05:29 AM
# end Validation Reply Form

_audit_creation_date             2022-11-04
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C83 H88 N10 Ni O4'
_chemical_formula_sum            'C83 H88 N10 Ni O4'
_chemical_formula_weight         1348.34
_chemical_melting_point          ?
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      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                   14.8148(10)
_cell_length_b                   21.1091(16)
_cell_length_c                   21.3832(15)
_cell_angle_alpha                117.161(3)
_cell_angle_beta                 99.568(3)
_cell_angle_gamma                100.567(3)
_cell_volume                     5604.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9863
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      21.36

_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.947
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8251
_exptl_absorpt_correction_T_max  0.8617
_exptl_absorpt_process_details   
;
CrystalClear (Rigaku, 1997--2002)
;
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.799
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.077
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42479
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        21.507
_diffrn_reflns_theta_max         21.507
_diffrn_reflns_theta_min         2.234
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9160
_reflns_number_total             12634
_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_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         12634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0698
_refine_ls_restrained_S_all      1.024
_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)+(0.1167P)²+8.3430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2164
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C11(H11), C21(H21), C22(H22), C26(H26), C30(H30),
 C40(H40), C52(H52), C56(H56), C66(H66), C67(H67), C71(H71), C75(H75)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C77(H77A,
 H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C),
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6475(3) 0.6735(3) 0.2118(2) 0.0381(11) Uani 1 1 d . . . . .
C2 C 0.7062(3) 0.7382(3) 0.2196(3) 0.0496(13) Uani 1 1 d . . . . .
H2 H 0.752768 0.740438 0.194395 0.059 Uiso 1 1 calc R U . . .
C3 C 0.6840(3) 0.7980(3) 0.2705(3) 0.0534(14) Uani 1 1 d . . . . .
H3 H 0.712573 0.849203 0.287474 0.064 Uiso 1 1 calc R U . . .
C4 C 0.6104(3) 0.7680(3) 0.2923(3) 0.0420(12) Uani 1 1 d . . . . .
C5 C 0.5500(3) 0.8057(3) 0.3306(2) 0.0438(12) Uani 1 1 d . . . . .
C6 C 0.5838(3) 0.8871(3) 0.3699(3) 0.0469(13) Uani 1 1 d . . . . .
C7 C 0.5307(4) 0.9306(3) 0.3572(3) 0.0511(13) Uani 1 1 d . . . . .
H7 H 0.469968 0.906283 0.321300 0.061 Uiso 1 1 calc R U . . .
C8 C 0.5631(4) 1.0077(3) 0.3948(3) 0.0517(13) Uani 1 1 d . . . . .
C9 C 0.6533(4) 1.0419(3) 0.4470(3) 0.0561(14) Uani 1 1 d . . . . .
C10 C 0.7107(3) 1.0008(3) 0.4625(3) 0.0594(15) Uani 1 1 d . . . . .
C11 C 0.6722(4) 0.9234(3) 0.4217(3) 0.0537(14) Uani 1 1 d . . . . .
H11 H 0.708915 0.894059 0.430093 0.064 Uiso 1 1 calc R U . . .
C12 C 0.4999(4) 1.0520(3) 0.3787(3) 0.0654(16) Uani 1 1 d . . . . .
C13 C 0.4048(5) 0.9990(4) 0.3180(4) 0.097(2) Uani 1 1 d . . . . .
H13A H 0.367919 1.028434 0.306724 0.145 Uiso 1 1 calc R U . . .
H13B H 0.367329 0.970249 0.335221 0.145 Uiso 1 1 calc R U . . .
H13C H 0.419091 0.964840 0.273715 0.145 Uiso 1 1 calc R U . . .
C14 C 0.4717(4) 1.1002(4) 0.4478(4) 0.0762(18) Uani 1 1 d . . . . .
H14A H 0.431802 1.128280 0.437145 0.114 Uiso 1 1 calc R U . . .
H14B H 0.529748 1.135011 0.487821 0.114 Uiso 1 1 calc R U . . .
H14C H 0.435753 1.067954 0.462395 0.114 Uiso 1 1 calc R U . . .
C15 C 0.5506(6) 1.0991(4) 0.3500(4) 0.100(2) Uani 1 1 d . . . . .
H15A H 0.508461 1.125547 0.338814 0.150 Uiso 1 1 calc R U . . .
H15B H 0.565654 1.066411 0.305443 0.150 Uiso 1 1 calc R U . . .
H15C H 0.609993 1.135231 0.387519 0.150 Uiso 1 1 calc R U . . .
C16 C 0.8098(4) 1.0378(4) 0.5171(4) 0.087(2) Uani 1 1 d . . . . .
C17 C 0.8050(5) 1.0915(4) 0.5934(4) 0.113(3) Uani 1 1 d . . . . .
H17A H 0.867402 1.108667 0.629173 0.170 Uiso 1 1 calc R U . . .
H17B H 0.756015 1.065938 0.606552 0.170 Uiso 1 1 calc R U . . .
H17C H 0.788531 1.134384 0.593364 0.170 Uiso 1 1 calc R U . . .
C18 C 0.8765(5) 1.0798(6) 0.4906(7) 0.158(4) Uani 1 1 d . . . . .
H18A H 0.935624 1.112459 0.530276 0.236 Uiso 1 1 calc R U . . .
H18B H 0.843909 1.109756 0.476575 0.236 Uiso 1 1 calc R U . . .
H18C H 0.892041 1.043626 0.448158 0.236 Uiso 1 1 calc R U . . .
C19 C 0.8557(5) 0.9809(5) 0.5244(5) 0.137(4) Uani 1 1 d . . . . .
H19A H 0.919599 1.007109 0.559691 0.205 Uiso 1 1 calc R U . . .
H19B H 0.861256 0.945829 0.476537 0.205 Uiso 1 1 calc R U . . .
H19C H 0.815654 0.953608 0.541560 0.205 Uiso 1 1 calc R U . . .
C20 C 0.4611(3) 0.7678(3) 0.3290(2) 0.0400(12) Uani 1 1 d . . . . .
C21 C 0.3867(3) 0.7984(3) 0.3534(3) 0.0451(12) Uani 1 1 d . . . . .
H21 H 0.390835 0.849769 0.379313 0.054 Uiso 1 1 calc R U . . .
C22 C 0.3101(3) 0.7409(3) 0.3329(3) 0.0428(12) Uani 1 1 d . . . . .
H22 H 0.249448 0.743876 0.340805 0.051 Uiso 1 1 calc R U . . .
C23 C 0.3361(3) 0.6753(3) 0.2976(2) 0.0378(11) Uani 1 1 d . . . . .
C24 C 0.2791(3) 0.5996(3) 0.2740(2) 0.0386(12) Uani 1 1 d . . . . .
C25 C 0.1837(3) 0.5698(3) 0.2356(2) 0.0381(12) Uani 1 1 d . . . . .
C26 C 0.1291(3) 0.4963(3) 0.2149(2) 0.0397(12) Uani 1 1 d . . . . .
H26 H 0.161845 0.466826 0.226847 0.048 Uiso 1 1 calc R U . . .
C27 C 0.0344(3) 0.4659(3) 0.1796(3) 0.0451(13) Uani 1 1 d . . . . .
C28 C -0.0174(3) 0.5119(3) 0.1607(3) 0.0521(14) Uani 1 1 d . . . . .
C29 C 0.0393(3) 0.5856(3) 0.1758(3) 0.0436(12) Uani 1 1 d . . . . .
C30 C 0.1330(3) 0.6106(3) 0.2102(3) 0.0430(12) Uani 1 1 d . . . . .
H30 H 0.168495 0.657461 0.218617 0.052 Uiso 1 1 calc R U . . .
C31 C -0.0212(3) 0.3871(3) 0.1579(3) 0.0602(15) Uani 1 1 d . . . . .
C32 C 0.0437(4) 0.3493(4) 0.1821(4) 0.085(2) Uani 1 1 d . . . . .
H32A H 0.009315 0.296421 0.160615 0.128 Uiso 1 1 calc R U . . .
H32B H 0.062315 0.373198 0.235751 0.128 Uiso 1 1 calc R U . . .
H32C H 0.101213 0.353827 0.165636 0.128 Uiso 1 1 calc R U . . .
C33 C -0.0619(5) 0.3398(4) 0.0732(4) 0.088(2) Uani 1 1 d . . . . .
H33A H -0.099806 0.289680 0.059240 0.132 Uiso 1 1 calc R U . . .
H33B H -0.008876 0.336185 0.051005 0.132 Uiso 1 1 calc R U . . .
H33C H -0.102697 0.363464 0.055801 0.132 Uiso 1 1 calc R U . . .
C34 C -0.1036(4) 0.3889(4) 0.1943(4) 0.090(2) Uani 1 1 d . . . . .
H34A H -0.135145 0.338347 0.183158 0.135 Uiso 1 1 calc R U . . .
H34B H -0.150229 0.407771 0.175216 0.135 Uiso 1 1 calc R U . . .
H34C H -0.077369 0.421529 0.247538 0.135 Uiso 1 1 calc R U . . .
C35 C -0.0111(3) 0.6298(3) 0.1493(3) 0.0582(15) Uani 1 1 d . . . . .
C36 C -0.0535(5) 0.5850(4) 0.0656(4) 0.092(2) Uani 1 1 d . . . . .
H36A H -0.085928 0.613687 0.049416 0.139 Uiso 1 1 calc R U . . .
H36B H -0.099642 0.537690 0.051369 0.139 Uiso 1 1 calc R U . . .
H36C H -0.001923 0.575006 0.042518 0.139 Uiso 1 1 calc R U . . .
C37 C -0.0887(4) 0.6498(4) 0.1866(4) 0.096(2) Uani 1 1 d . . . . .
H37A H -0.120023 0.678236 0.169237 0.144 Uiso 1 1 calc R U . . .
H37B H -0.059933 0.680075 0.239854 0.144 Uiso 1 1 calc R U . . .
H37C H -0.136313 0.604122 0.174803 0.144 Uiso 1 1 calc R U . . .
C38 C 0.0585(4) 0.7025(4) 0.1666(4) 0.082(2) Uani 1 1 d . . . . .
H38A H 0.023735 0.729349 0.149289 0.123 Uiso 1 1 calc R U . . .
H38B H 0.108402 0.691346 0.141849 0.123 Uiso 1 1 calc R U . . .
H38C H 0.088198 0.733349 0.219677 0.123 Uiso 1 1 calc R U . . .
C39 C 0.3339(3) 0.5599(3) 0.2995(2) 0.0337(11) Uani 1 1 d . . . . .
C40 C 0.3075(3) 0.5196(3) 0.3332(2) 0.0363(11) Uani 1 1 d . . . . .
H40 H 0.248054 0.509979 0.343359 0.044 Uiso 1 1 calc R U . . .
C41 C 0.3862(3) 0.4959(3) 0.3493(2) 0.0358(11) Uani 1 1 d . . . . .
C42 C 0.4574(3) 0.5220(3) 0.3229(2) 0.0342(11) Uani 1 1 d . . . . .
C43 C 0.5415(3) 0.4997(3) 0.3180(2) 0.0366(11) Uani 1 1 d . . . . .
C44 C 0.5585(3) 0.4445(3) 0.3436(2) 0.0349(11) Uani 1 1 d . . . . .
C45 C 0.4064(3) 0.4573(3) 0.3864(2) 0.0385(11) Uani 1 1 d . . . . .
C46 C 0.4891(3) 0.3990(3) 0.4239(2) 0.0386(11) Uani 1 1 d . . . . .
C47 C 0.4037(3) 0.3993(3) 0.4452(2) 0.0404(12) Uani 1 1 d . . . . .
C48 C 0.5252(3) 0.3329(3) 0.4750(2) 0.0414(12) Uani 1 1 d . . . . .
C49 C 0.4417(3) 0.3327(3) 0.4967(2) 0.0435(12) Uani 1 1 d . . . . .
C50 C 0.5910(4) 0.2967(3) 0.4937(3) 0.0501(13) Uani 1 1 d . . . . .
C51 C 0.4154(4) 0.2930(3) 0.5338(3) 0.0530(14) Uani 1 1 d . . . . .
C52 C 0.5376(3) 0.3688(3) 0.2789(3) 0.0414(12) Uani 1 1 d . . . . .
H52 H 0.480394 0.350939 0.240509 0.050 Uiso 1 1 calc R U . . .
C53 C 0.5938(3) 0.3243(3) 0.2709(3) 0.0477(13) Uani 1 1 d . . . . .
C54 C 0.6825(4) 0.3521(4) 0.3332(3) 0.0603(16) Uani 1 1 d . . . . .
C55 C 0.7168(3) 0.4325(3) 0.3901(3) 0.0460(13) Uani 1 1 d . . . . .
C56 C 0.6583(3) 0.4740(3) 0.3945(3) 0.0413(12) Uani 1 1 d . . . . .
H56 H 0.680508 0.524962 0.431847 0.050 Uiso 1 1 calc R U . . .
C57 C 0.5711(4) 0.2476(3) 0.2029(3) 0.0713(17) Uani 1 1 d . . . . .
C58 C 0.4825(5) 0.2333(4) 0.1440(4) 0.091(2) Uani 1 1 d . . . . .
H58A H 0.466929 0.182802 0.102257 0.136 Uiso 1 1 calc R U . . .
H58B H 0.495947 0.269587 0.127652 0.136 Uiso 1 1 calc R U . . .
H58C H 0.428189 0.238482 0.164648 0.136 Uiso 1 1 calc R U . . .
C59 C 0.6576(5) 0.2443(4) 0.1715(4) 0.104(2) Uani 1 1 d . . . . .
H59A H 0.640229 0.198460 0.123929 0.156 Uiso 1 1 calc R U . . .
H59B H 0.711473 0.244836 0.205422 0.156 Uiso 1 1 calc R U . . .
H59C H 0.676153 0.287561 0.165151 0.156 Uiso 1 1 calc R U . . .
C60 C 0.5499(5) 0.1857(4) 0.2220(5) 0.103(2) Uani 1 1 d . . . . .
H60A H 0.534640 0.137042 0.177565 0.155 Uiso 1 1 calc R U . . .
H60B H 0.495258 0.188134 0.242421 0.155 Uiso 1 1 calc R U . . .
H60C H 0.606231 0.192229 0.258225 0.155 Uiso 1 1 calc R U . . .
C61 C 0.8178(3) 0.4628(4) 0.4433(3) 0.0577(15) Uani 1 1 d . . . . .
C62 C 0.8897(4) 0.4454(4) 0.3994(3) 0.083(2) Uani 1 1 d . . . . .
H62A H 0.953754 0.461956 0.432880 0.124 Uiso 1 1 calc R U . . .
H62B H 0.889857 0.471480 0.371421 0.124 Uiso 1 1 calc R U . . .
H62C H 0.871750 0.391570 0.365497 0.124 Uiso 1 1 calc R U . . .
C63 C 0.8202(4) 0.4278(4) 0.4928(4) 0.085(2) Uani 1 1 d . . . . .
H63A H 0.883332 0.449620 0.528938 0.127 Uiso 1 1 calc R U . . .
H63B H 0.808083 0.373849 0.462649 0.127 Uiso 1 1 calc R U . . .
H63C H 0.770808 0.437648 0.518238 0.127 Uiso 1 1 calc R U . . .
C64 C 0.8444(4) 0.5474(4) 0.4921(3) 0.0787(19) Uani 1 1 d . . . . .
H64A H 0.910823 0.566432 0.522795 0.118 Uiso 1 1 calc R U . . .
H64B H 0.801687 0.559655 0.523568 0.118 Uiso 1 1 calc R U . . .
H64C H 0.837580 0.570238 0.461420 0.118 Uiso 1 1 calc R U . . .
C65 C 0.6015(3) 0.5173(3) 0.2817(2) 0.0358(11) Uani 1 1 d . . . . .
C66 C 0.6768(3) 0.4870(3) 0.2574(2) 0.0387(12) Uani 1 1 d . . . . .
H66 H 0.704371 0.456458 0.271263 0.046 Uiso 1 1 calc R U . . .
C67 C 0.7009(3) 0.5096(3) 0.2116(2) 0.0364(11) Uani 1 1 d . . . . .
H67 H 0.748033 0.497528 0.186654 0.044 Uiso 1 1 calc R U . . .
C68 C 0.6428(3) 0.5553(3) 0.2073(2) 0.0385(12) Uani 1 1 d . . . . .
C69 C 0.6462(3) 0.5970(3) 0.1681(2) 0.0383(12) Uani 1 1 d . . . . .
C70 C 0.6518(3) 0.5641(3) 0.0965(3) 0.0405(12) Uani 1 1 d . . . . .
C71 C 0.6562(3) 0.6055(3) 0.0578(2) 0.0390(12) Uani 1 1 d . . . . .
H71 H 0.655255 0.655788 0.082567 0.047 Uiso 1 1 calc R U . . .
C72 C 0.6617(3) 0.5758(3) -0.0113(2) 0.0385(12) Uani 1 1 d . . . . .
C73 C 0.6585(4) 0.4969(3) -0.0517(3) 0.0501(13) Uani 1 1 d . . . . .
C74 C 0.6546(3) 0.4537(3) -0.0128(3) 0.0395(12) Uani 1 1 d . . . . .
C75 C 0.6488(3) 0.4875(3) 0.0561(2) 0.0367(11) Uani 1 1 d . . . . .
H75 H 0.642290 0.458817 0.079672 0.044 Uiso 1 1 calc R U . . .
C76 C 0.6705(3) 0.6229(3) -0.0491(3) 0.0464(13) Uani 1 1 d . . . . .
C77 C 0.6775(5) 0.7031(3) 0.0021(3) 0.0730(17) Uani 1 1 d . . . . .
H77A H 0.684448 0.731362 -0.023480 0.110 Uiso 1 1 calc R U . . .
H77B H 0.733214 0.724734 0.045048 0.110 Uiso 1 1 calc R U . . .
H77C H 0.619179 0.705272 0.018004 0.110 Uiso 1 1 calc R U . . .
C78 C 0.5841(4) 0.5916(3) -0.1153(3) 0.0659(16) Uani 1 1 d . . . . .
H78A H 0.591662 0.621453 -0.139212 0.099 Uiso 1 1 calc R U . . .
H78B H 0.525874 0.593228 -0.099300 0.099 Uiso 1 1 calc R U . . .
H78C H 0.579093 0.539845 -0.149988 0.099 Uiso 1 1 calc R U . . .
C79 C 0.7627(4) 0.6225(4) -0.0742(4) 0.085(2) Uani 1 1 d . . . . .
H79A H 0.769262 0.653361 -0.097164 0.128 Uiso 1 1 calc R U . . .
H79B H 0.758783 0.571298 -0.109669 0.128 Uiso 1 1 calc R U . . .
H79C H 0.818512 0.642587 -0.031608 0.128 Uiso 1 1 calc R U . . .
C80 C 0.6565(3) 0.3732(3) -0.0523(3) 0.0477(13) Uani 1 1 d . . . . .
C81 C 0.7466(4) 0.3681(4) -0.0783(3) 0.0739(18) Uani 1 1 d . . . . .
H81A H 0.745250 0.315754 -0.105249 0.111 Uiso 1 1 calc R U . . .
H81B H 0.803557 0.395946 -0.035721 0.111 Uiso 1 1 calc R U . . .
H81C H 0.748530 0.389353 -0.110473 0.111 Uiso 1 1 calc R U . . .
C82 C 0.6587(4) 0.3398(3) -0.0007(3) 0.0628(15) Uani 1 1 d . . . . .
H82A H 0.664334 0.289250 -0.026652 0.094 Uiso 1 1 calc R U . . .
H82B H 0.599494 0.338051 0.013937 0.094 Uiso 1 1 calc R U . . .
H82C H 0.713793 0.371051 0.042964 0.094 Uiso 1 1 calc R U . . .
C83 C 0.5674(4) 0.3238(3) -0.1179(3) 0.0736(17) Uani 1 1 d . . . . .
H83A H 0.570644 0.272455 -0.142294 0.110 Uiso 1 1 calc R U . . .
H83B H 0.564678 0.342231 -0.152536 0.110 Uiso 1 1 calc R U . . .
H83C H 0.509956 0.325133 -0.100895 0.110 Uiso 1 1 calc R U . . .
N1 N 0.5908(2) 0.6911(2) 0.25641(19) 0.0379(9) Uani 1 1 d . . . . .
N2 N 0.4276(2) 0.6902(2) 0.2954(2) 0.0375(9) Uani 1 1 d . . . . .
N3 N 0.4260(2) 0.5631(2) 0.29407(19) 0.0354(9) Uani 1 1 d . . . . .
N4 N 0.5857(2) 0.5626(2) 0.25111(18) 0.0353(9) Uani 1 1 d . . . . .
N5 N 0.4900(2) 0.4372(2) 0.38634(19) 0.0383(9) Uani 1 1 d . . . . .
N6 N 0.3533(3) 0.4366(2) 0.4221(2) 0.0470(11) Uani 1 1 d . . . . .
N7 N 0.5510(3) 0.3661(2) 0.4369(2) 0.0421(10) Uani 1 1 d . . . . .
N8 N 0.3786(3) 0.3664(2) 0.4826(2) 0.0459(10) Uani 1 1 d . . . . .
N9 N 0.6415(3) 0.2676(3) 0.5082(3) 0.0686(14) Uani 1 1 d . . . . .
N10 N 0.3925(3) 0.2597(3) 0.5607(3) 0.0699(14) Uani 1 1 d . . . . .
O1 O 0.6918(3) 1.1173(2) 0.4871(2) 0.0749(11) Uani 1 1 d . . . . .
H1 H 0.650035 1.137660 0.481038 0.112 Uiso 1 1 calc R U . . .
O2 O -0.1052(2) 0.4891(2) 0.1335(2) 0.0754(12) Uani 1 1 d . . . . .
O3 O 0.6543(4) 0.4661(2) -0.1175(2) 0.0885(14) Uani 1 1 d . . . . .
O4 O 0.7249(3) 0.3081(3) 0.3347(3) 0.0994(15) Uani 1 1 d . . . . .
Ni Ni 0.50440(4) 0.62507(4) 0.27094(3) 0.0413(2) Uani 1 1 d . . . . .


_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
C1 C2 1.399(6) . ?
C1 C69 1.446(6) . ?
C1 N1 1.345(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.380(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.412(6) . ?
C4 C5 1.421(6) . ?
C4 N1 1.386(6) . ?
C5 C6 1.462(7) . ?
C5 C20 1.395(6) . ?
C6 C7 1.400(7) . ?
C6 C11 1.381(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.385(7) . ?
C8 C9 1.402(7) . ?
C8 C12 1.541(7) . ?
C9 C10 1.424(7) . ?
C9 O1 1.361(6) . ?
C10 C11 1.396(7) . ?
C10 C16 1.518(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.552(9) . ?
C12 C14 1.544(8) . ?
C12 C15 1.537(8) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.526(10) . ?
C16 C18 1.552(10) . ?
C16 C19 1.537(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.431(6) . ?
C20 N2 1.398(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.341(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.403(6) . ?
C23 C24 1.466(6) . ?
C23 N2 1.347(5) . ?
C24 C25 1.373(6) . ?
C24 C39 1.478(6) . ?
C25 C26 1.432(6) . ?
C25 C30 1.459(6) . ?
C26 H26 0.9500 . ?
C26 C27 1.350(6) . ?
C27 C28 1.493(7) . ?
C27 C31 1.524(7) . ?
C28 C29 1.483(7) . ?
C28 O2 1.235(5) . ?
C29 C30 1.336(6) . ?
C29 C35 1.531(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.525(7) . ?
C31 C33 1.551(8) . ?
C31 C34 1.550(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.536(9) . ?
C35 C37 1.521(8) . ?
C35 C38 1.527(8) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.388(6) . ?
C39 N3 1.380(5) . ?
C40 H40 0.9500 . ?
C40 C41 1.401(6) . ?
C41 C42 1.416(6) . ?
C41 C45 1.408(6) . ?
C42 C43 1.413(6) . ?
C42 N3 1.374(5) . ?
C43 C44 1.539(6) . ?
C43 C65 1.379(6) . ?
C44 C52 1.491(6) . ?
C44 C56 1.506(6) . ?
C44 N5 1.505(5) . ?
C45 N5 1.379(5) . ?
C45 N6 1.332(5) . ?
C46 C47 1.415(6) . ?
C46 N5 1.375(5) . ?
C46 N7 1.313(5) . ?
C47 N6 1.367(6) . ?
C47 N8 1.331(5) . ?
C48 C49 1.391(6) . ?
C48 C50 1.456(7) . ?
C48 N7 1.352(6) . ?
C49 C51 1.443(7) . ?
C49 N8 1.346(6) . ?
C50 N9 1.139(6) . ?
C51 N10 1.133(6) . ?
C52 H52 0.9500 . ?
C52 C53 1.339(6) . ?
C53 C54 1.505(7) . ?
C53 C57 1.529(8) . ?
C54 C55 1.487(8) . ?
C54 O4 1.222(6) . ?
C55 C56 1.325(6) . ?
C55 C61 1.536(7) . ?
C56 H56 0.9500 . ?
C57 C58 1.534(9) . ?
C57 C59 1.541(8) . ?
C57 C60 1.535(8) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.520(7) . ?
C61 C63 1.543(7) . ?
C61 C64 1.529(8) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 C66 1.440(6) . ?
C65 N4 1.414(5) . ?
C66 H66 0.9500 . ?
C66 C67 1.339(6) . ?
C67 H67 0.9500 . ?
C67 C68 1.428(6) . ?
C68 C69 1.466(6) . ?
C68 N4 1.340(5) . ?
C69 C70 1.387(6) . ?
C70 C71 1.454(6) . ?
C70 C75 1.431(6) . ?
C71 H71 0.9500 . ?
C71 C72 1.341(6) . ?
C72 C73 1.473(7) . ?
C72 C76 1.540(6) . ?
C73 C74 1.489(6) . ?
C73 O3 1.235(6) . ?
C74 C75 1.339(6) . ?
C74 C80 1.522(7) . ?
C75 H75 0.9500 . ?
C76 C77 1.512(7) . ?
C76 C78 1.521(7) . ?
C76 C79 1.549(7) . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 C81 1.532(7) . ?
C80 C82 1.554(7) . ?
C80 C83 1.530(7) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
N1 Ni 1.884(4) . ?
N2 Ni 1.891(3) . ?
N3 Ni 1.879(3) . ?
N4 Ni 1.901(3) . ?
O1 H1 0.8400 . ?

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
C2 C1 C69 129.0(4) . . ?
N1 C1 C2 110.3(4) . . ?
N1 C1 C69 120.6(4) . . ?
C1 C2 H2 126.3 . . ?
C3 C2 C1 107.4(4) . . ?
C3 C2 H2 126.3 . . ?
C2 C3 H3 126.8 . . ?
C2 C3 C4 106.4(5) . . ?
C4 C3 H3 126.8 . . ?
C3 C4 C5 126.6(5) . . ?
N1 C4 C3 108.9(4) . . ?
N1 C4 C5 123.0(4) . . ?
C4 C5 C6 116.4(4) . . ?
C20 C5 C4 122.4(5) . . ?
C20 C5 C6 121.1(4) . . ?
C7 C6 C5 123.0(5) . . ?
C11 C6 C5 119.1(4) . . ?
C11 C6 C7 117.9(5) . . ?
C6 C7 H7 118.7 . . ?
C8 C7 C6 122.6(5) . . ?
C8 C7 H7 118.7 . . ?
C7 C8 C9 117.3(5) . . ?
C7 C8 C12 119.7(5) . . ?
C9 C8 C12 123.1(5) . . ?
C8 C9 C10 122.8(5) . . ?
O1 C9 C8 122.0(5) . . ?
O1 C9 C10 115.1(5) . . ?
C9 C10 C16 122.8(5) . . ?
C11 C10 C9 115.8(5) . . ?
C11 C10 C16 121.4(5) . . ?
C6 C11 C10 123.6(5) . . ?
C6 C11 H11 118.2 . . ?
C10 C11 H11 118.2 . . ?
C8 C12 C13 111.3(5) . . ?
C8 C12 C14 110.0(4) . . ?
C14 C12 C13 106.4(5) . . ?
C15 C12 C8 110.9(5) . . ?
C15 C12 C13 106.3(5) . . ?
C15 C12 C14 111.9(5) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C16 C17 110.7(5) . . ?
C10 C16 C18 109.2(6) . . ?
C10 C16 C19 112.3(6) . . ?
C17 C16 C18 110.4(7) . . ?
C17 C16 C19 106.9(7) . . ?
C19 C16 C18 107.3(6) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C5 C20 C21 127.7(5) . . ?
C5 C20 N2 123.3(4) . . ?
N2 C20 C21 108.8(4) . . ?
C20 C21 H21 126.5 . . ?
C22 C21 C20 107.1(4) . . ?
C22 C21 H21 126.5 . . ?
C21 C22 H22 126.3 . . ?
C21 C22 C23 107.4(4) . . ?
C23 C22 H22 126.3 . . ?
C22 C23 C24 126.4(4) . . ?
N2 C23 C22 111.6(4) . . ?
N2 C23 C24 121.5(4) . . ?
C23 C24 C39 112.8(4) . . ?
C25 C24 C23 124.0(4) . . ?
C25 C24 C39 123.2(4) . . ?
C24 C25 C26 122.8(4) . . ?
C24 C25 C30 121.2(4) . . ?
C26 C25 C30 115.9(4) . . ?
C25 C26 H26 117.6 . . ?
C27 C26 C25 124.8(4) . . ?
C27 C26 H26 117.6 . . ?
C26 C27 C28 117.9(5) . . ?
C26 C27 C31 123.3(4) . . ?
C28 C27 C31 118.8(4) . . ?
C29 C28 C27 118.2(4) . . ?
O2 C28 C27 120.5(5) . . ?
O2 C28 C29 121.2(4) . . ?
C28 C29 C35 118.8(4) . . ?
C30 C29 C28 119.3(4) . . ?
C30 C29 C35 121.8(5) . . ?
C25 C30 H30 118.3 . . ?
C29 C30 C25 123.5(5) . . ?
C29 C30 H30 118.3 . . ?
C27 C31 C32 111.1(4) . . ?
C27 C31 C33 109.4(4) . . ?
C27 C31 C34 110.5(5) . . ?
C32 C31 C33 107.6(5) . . ?
C32 C31 C34 107.9(5) . . ?
C34 C31 C33 110.3(5) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C29 C35 C36 110.3(5) . . ?
C37 C35 C29 110.5(4) . . ?
C37 C35 C36 110.7(5) . . ?
C37 C35 C38 107.4(5) . . ?
C38 C35 C29 111.8(4) . . ?
C38 C35 C36 106.0(5) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C24 128.7(4) . . ?
N3 C39 C24 119.9(4) . . ?
N3 C39 C40 111.3(3) . . ?
C39 C40 H40 126.9 . . ?
C39 C40 C41 106.2(3) . . ?
C41 C40 H40 126.9 . . ?
C40 C41 C42 106.7(4) . . ?
C40 C41 C45 134.0(4) . . ?
C45 C41 C42 119.2(4) . . ?
C43 C42 C41 124.0(4) . . ?
N3 C42 C41 109.8(3) . . ?
N3 C42 C43 125.6(4) . . ?
C42 C43 C44 118.7(3) . . ?
C65 C43 C42 122.0(4) . . ?
C65 C43 C44 118.6(4) . . ?
C52 C44 C43 109.9(3) . . ?
C52 C44 C56 113.8(4) . . ?
C52 C44 N5 106.3(4) . . ?
C56 C44 C43 109.5(4) . . ?
N5 C44 C43 110.0(3) . . ?
N5 C44 C56 107.2(3) . . ?
N5 C45 C41 118.0(3) . . ?
N6 C45 C41 127.4(4) . . ?
N6 C45 N5 114.5(4) . . ?
N5 C46 C47 105.6(4) . . ?
N7 C46 C47 125.2(4) . . ?
N7 C46 N5 129.1(4) . . ?
N6 C47 C46 111.2(4) . . ?
N8 C47 C46 122.3(4) . . ?
N8 C47 N6 126.5(4) . . ?
C49 C48 C50 120.3(4) . . ?
N7 C48 C49 123.6(4) . . ?
N7 C48 C50 116.1(4) . . ?
C48 C49 C51 121.1(4) . . ?
N8 C49 C48 123.5(4) . . ?
N8 C49 C51 115.4(4) . . ?
N9 C50 C48 179.1(5) . . ?
N10 C51 C49 177.5(6) . . ?
C44 C52 H52 117.7 . . ?
C53 C52 C44 124.7(4) . . ?
C53 C52 H52 117.7 . . ?
C52 C53 C54 117.2(5) . . ?
C52 C53 C57 123.2(5) . . ?
C54 C53 C57 119.6(4) . . ?
C55 C54 C53 119.0(4) . . ?
O4 C54 C53 119.0(6) . . ?
O4 C54 C55 122.1(5) . . ?
C54 C55 C61 117.9(4) . . ?
C56 C55 C54 119.0(5) . . ?
C56 C55 C61 123.0(5) . . ?
C44 C56 H56 118.3 . . ?
C55 C56 C44 123.5(5) . . ?
C55 C56 H56 118.3 . . ?
C53 C57 C58 110.8(5) . . ?
C53 C57 C59 108.9(5) . . ?
C53 C57 C60 110.9(5) . . ?
C58 C57 C59 109.1(6) . . ?
C58 C57 C60 107.6(6) . . ?
C60 C57 C59 109.6(5) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C55 C61 C63 109.4(4) . . ?
C62 C61 C55 109.1(4) . . ?
C62 C61 C63 111.5(5) . . ?
C62 C61 C64 108.1(5) . . ?
C64 C61 C55 110.4(4) . . ?
C64 C61 C63 108.4(5) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C43 C65 C66 129.7(4) . . ?
C43 C65 N4 121.9(3) . . ?
N4 C65 C66 107.7(3) . . ?
C65 C66 H66 126.2 . . ?
C67 C66 C65 107.7(4) . . ?
C67 C66 H66 126.2 . . ?
C66 C67 H67 126.3 . . ?
C66 C67 C68 107.4(4) . . ?
C68 C67 H67 126.3 . . ?
C67 C68 C69 128.3(4) . . ?
N4 C68 C67 110.8(4) . . ?
N4 C68 C69 120.6(4) . . ?
C1 C69 C68 113.9(4) . . ?
C70 C69 C1 125.2(4) . . ?
C70 C69 C68 120.8(4) . . ?
C69 C70 C71 121.0(4) . . ?
C69 C70 C75 122.2(4) . . ?
C75 C70 C71 116.8(4) . . ?
C70 C71 H71 118.6 . . ?
C72 C71 C70 122.9(5) . . ?
C72 C71 H71 118.6 . . ?
C71 C72 C73 119.2(4) . . ?
C71 C72 C76 121.0(4) . . ?
C73 C72 C76 119.8(4) . . ?
C72 C73 C74 118.7(4) . . ?
O3 C73 C72 120.8(4) . . ?
O3 C73 C74 120.5(5) . . ?
C73 C74 C80 119.5(4) . . ?
C75 C74 C73 118.2(4) . . ?
C75 C74 C80 122.3(4) . . ?
C70 C75 H75 117.9 . . ?
C74 C75 C70 124.2(4) . . ?
C74 C75 H75 117.9 . . ?
C72 C76 C79 109.4(4) . . ?
C77 C76 C72 111.9(4) . . ?
C77 C76 C78 107.9(4) . . ?
C77 C76 C79 107.5(5) . . ?
C78 C76 C72 110.6(4) . . ?
C78 C76 C79 109.3(4) . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C76 C78 H78A 109.5 . . ?
C76 C78 H78B 109.5 . . ?
C76 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C76 C79 H79A 109.5 . . ?
C76 C79 H79B 109.5 . . ?
C76 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C74 C80 C81 110.6(4) . . ?
C74 C80 C82 111.5(4) . . ?
C74 C80 C83 111.2(4) . . ?
C81 C80 C82 106.7(4) . . ?
C83 C80 C81 109.5(4) . . ?
C83 C80 C82 107.1(4) . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C80 C82 H82A 109.5 . . ?
C80 C82 H82B 109.5 . . ?
C80 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C80 C83 H83A 109.5 . . ?
C80 C83 H83B 109.5 . . ?
C80 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C1 N1 C4 107.0(4) . . ?
C1 N1 Ni 127.0(3) . . ?
C4 N1 Ni 125.9(3) . . ?
C20 N2 Ni 125.4(3) . . ?
C23 N2 C20 105.2(4) . . ?
C23 N2 Ni 128.4(3) . . ?
C39 N3 Ni 128.3(3) . . ?
C42 N3 C39 105.9(3) . . ?
C42 N3 Ni 124.8(3) . . ?
C65 N4 Ni 127.3(3) . . ?
C68 N4 C65 106.3(3) . . ?
C68 N4 Ni 126.4(3) . . ?
C45 N5 C44 126.9(3) . . ?
C46 N5 C44 127.2(3) . . ?
C46 N5 C45 105.2(3) . . ?
C45 N6 C47 103.4(3) . . ?
C46 N7 C48 112.2(4) . . ?
C47 N8 C49 113.3(4) . . ?
C9 O1 H1 109.5 . . ?
N1 Ni N2 90.69(15) . . ?
N1 Ni N4 88.83(15) . . ?
N2 Ni N4 177.18(16) . . ?
N3 Ni N1 174.73(15) . . ?
N3 Ni N2 90.06(15) . . ?
N3 Ni N4 90.17(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 -0.498 -0.409 0.758 2585.8 904.7 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
####################################################################### 
# 
# 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_hill202002a@113k1_0m
_database_code_depnum_ccdc_archive 'CCDC 2209423'
loop_
_audit_author_name
_audit_author_address
'Yoshitaka Matsushita'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2022-11-28 deposited with the CCDC.	2022-12-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_hill202002a@113k1_0m 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Due to lower crystallinity and weaker peaks in wide angle region
;
_vrf_PLAT414_hill202002a@113k1_0m 
;
PROBLEM: Short Intra D-H..H-X       H3       ..H65B     .       1.78 Ang.
RESPONSE: H3 was placed using a riding model which is close to H65B
;
_vrf_PLAT230_hill202002a@113k1_0m 
;
PROBLEM: Hirshfeld Test Diff for    C17      --C19      .       16.7 s.u.
RESPONSE: Due to poor crystallinity
;
_vrf_PLAT230_hill202002a@113k1_0m_2 
;
PROBLEM: Hirshfeld Test Diff for    C17      --C20      .       13.5 s.u.
RESPONSE: Due to poor crystallinity.
;
_vrf_PLAT230_hill202002a@113k1_0m_3 
;
PROBLEM: Hirshfeld Test Diff for    C30      --C90      .       12.2 s.u.
RESPONSE: Due to poor crystallinity
;
_vrf_PLAT230_hill202002a@113k1_0m_4 
;
PROBLEM: Hirshfeld Test Diff for    C35      --C36      .       10.5 s.u.
RESPONSE: Due to poor crystallinity
;
_vrf_PLAT230_hill202002a@113k1_0m_5 
;
PROBLEM: Hirshfeld Test Diff for    C67      --C78      .       11.8 s.u.
RESPONSE: Due to poor crystallinity
;
_vrf_PLAT230_hill202002a@113k1_0m_6 
;
PROBLEM: Hirshfeld Test Diff for    C78      --C85      .       11.7 s.u.
RESPONSE: Due to poor crystallinity
;
_vrf_PLAT414_hill202002a@113k1_0m_2 
;
PROBLEM: Short Intra D-H..H-X       H1       ..H67A     .       1.87 Ang.
RESPONSE: H1 was placed using a riding model which is close to H67A
;
_vrf_PLAT420_hill202002a@113k1_0m 
;
PROBLEM: D-H Bond Without Acceptor  O3       --H3       .     Please Check
RESPONSE: Not accessible for H-bonding
;
# Added during the CSD deposition process: Monday 28 November 2022 02:24 AM
# end Validation Reply Form

_audit_creation_date             2022-11-04
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C83 H89 N10 Ni O5, [+ solvents]'
_chemical_formula_sum            'C83 H90 N10 Ni O5'
_chemical_formula_weight         1366.35
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   16.7677(7)
_cell_length_b                   27.5318(10)
_cell_length_c                   21.8285(9)
_cell_angle_alpha                90
_cell_angle_beta                 106.193(2)
_cell_angle_gamma                90
_cell_volume                     9677.2(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      20.92
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.995
_shelx_estimated_absorpt_T_min   0.975
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrystalClear (Rigaku, 1997--2002)
;

_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.938
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73667
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        20.956
_diffrn_reflns_theta_max         20.956
_diffrn_reflns_theta_min         1.943
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7995
_reflns_number_total             10225
_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       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         10225
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.1123
_refine_ls_restrained_S_all      1.031
_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)+(0.1869P)²+39.8460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3019
_refine_ls_wR_factor_ref         0.3231
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O2-H2
 1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C74) = Uanis(C79) = Uanis(C36) = Uanis(C61)
Uanis(C78) = Uanis(C35)
Uanis(C67) = Uanis(C32) = Uanis(C90) = Uanis(C31)
Uanis(C78) = Uanis(C30)
Uanis(C20) = Uanis(C82) = Uanis(C67) = Uanis(C74)
Uanis(C19) = Uanis(C31) = Uanis(C90) = Uanis(C32)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C21(H21), C23(H23), C24(H24), C28(H28), C42(H42), C44(H44), C47(H47),
 C48(H48), C49(H49), C68(H68), C69(H69), C81(H81), C87(H87), C88(H88)
4.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C),
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C61(H61A,H61B,H61C), C65(H65A,H65B,H65C), C67(H67A,
 H67B,H67C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C79(H79A,H79B,H79C),
 C82(H82A,H82B,H82C), C90(H90A,H90B,H90C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3)
;
_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
C1 C 0.6084(4) 0.6363(3) 0.3389(4) 0.0484(19) Uani 1 1 d . . . . .
C3 C 0.5555(4) 0.5950(3) 0.3178(4) 0.050(2) Uani 1 1 d . . . . .
C5 C 0.5115(4) 0.5185(3) 0.3073(4) 0.057(2) Uani 1 1 d . . . . .
H5 H 0.506145 0.484603 0.313356 0.069 Uiso 1 1 calc R U . . .
C6 C 0.4616(5) 0.5465(3) 0.2570(4) 0.054(2) Uani 1 1 d . . . . .
C7 C 0.3862(5) 0.5330(3) 0.2130(4) 0.052(2) Uani 1 1 d . . . . .
C8 C 0.3678(5) 0.4796(2) 0.2065(4) 0.053(2) Uani 1 1 d . . . . .
C9 C 0.8225(7) 0.7859(8) 0.0746(9) 0.211(11) Uani 1 1 d . . . . .
H9A H 0.825873 0.816982 0.053448 0.316 Uiso 1 1 calc R U . . .
H9B H 0.867886 0.764735 0.070930 0.316 Uiso 1 1 calc R U . . .
H9C H 0.827043 0.791707 0.119713 0.316 Uiso 1 1 calc R U . . .
C10 C 0.6380(9) 0.5134(6) 0.1957(7) 0.171(8) Uani 1 1 d . . . . .
H10A H 0.603655 0.532456 0.216548 0.256 Uiso 1 1 calc R U . . .
H10B H 0.645458 0.480559 0.213697 0.256 Uiso 1 1 calc R U . . .
H10C H 0.610595 0.511573 0.149807 0.256 Uiso 1 1 calc R U . . .
C11 C 0.4735(5) 0.3635(3) 0.1723(5) 0.073(3) Uani 1 1 d . . . . .
C12 C 0.5530(6) 0.3900(3) 0.1699(6) 0.091(3) Uani 1 1 d . . . . .
H12A H 0.543778 0.406226 0.128603 0.136 Uiso 1 1 calc R U . . .
H12B H 0.598316 0.366465 0.175519 0.136 Uiso 1 1 calc R U . . .
H12C H 0.567626 0.414177 0.204174 0.136 Uiso 1 1 calc R U . . .
C13 C 0.5000(6) 0.3238(3) 0.2239(6) 0.091(3) Uani 1 1 d . . . . .
H13A H 0.450971 0.305527 0.226665 0.136 Uiso 1 1 calc R U . . .
H13B H 0.526392 0.338977 0.265170 0.136 Uiso 1 1 calc R U . . .
H13C H 0.539437 0.301682 0.212561 0.136 Uiso 1 1 calc R U . . .
C14 C 0.4381(7) 0.3406(4) 0.1068(6) 0.104(4) Uani 1 1 d . . . . .
H14A H 0.391398 0.319441 0.107607 0.156 Uiso 1 1 calc R U . . .
H14B H 0.481271 0.321447 0.095664 0.156 Uiso 1 1 calc R U . . .
H14C H 0.418727 0.366245 0.074945 0.156 Uiso 1 1 calc R U . . .
C15 C 0.3338(5) 0.3811(2) 0.1943(4) 0.059(2) Uani 1 1 d . . . . .
C16 C 0.2738(4) 0.4116(2) 0.2092(4) 0.055(2) Uani 1 1 d . . . . .
C17 C 0.1947(4) 0.3934(3) 0.2216(5) 0.063(2) Uani 1 1 d . . . . .
C18 C 0.2091(6) 0.3526(3) 0.2703(5) 0.081(3) Uani 1 1 d . . . . .
H18A H 0.155724 0.341791 0.275481 0.122 Uiso 1 1 calc R U . . .
H18B H 0.244477 0.364311 0.311274 0.122 Uiso 1 1 calc R U . . .
H18C H 0.236516 0.325380 0.255446 0.122 Uiso 1 1 calc R U . . .
C19 C 0.1354(9) 0.3765(5) 0.1574(8) 0.1353(16) Uani 1 1 d . . . . .
H19A H 0.090612 0.356865 0.165448 0.203 Uiso 1 1 calc R U . . .
H19B H 0.166419 0.356878 0.134277 0.203 Uiso 1 1 calc R U . . .
H19C H 0.111698 0.404862 0.131647 0.203 Uiso 1 1 calc R U . . .
C20 C 0.1483(9) 0.4339(5) 0.2452(8) 0.1353(16) Uani 1 1 d . . . . .
H20A H 0.096712 0.420883 0.251413 0.203 Uiso 1 1 calc R U . . .
H20B H 0.135196 0.460015 0.213473 0.203 Uiso 1 1 calc R U . . .
H20C H 0.183219 0.446633 0.285689 0.203 Uiso 1 1 calc R U . . .
C21 C 0.2945(4) 0.4616(3) 0.2156(4) 0.056(2) Uani 1 1 d . . . . .
H21 H 0.256917 0.483542 0.226416 0.068 Uiso 1 1 calc R U . . .
C22 C 0.3294(5) 0.5665(3) 0.1793(4) 0.056(2) Uani 1 1 d . . . . .
C23 C 0.2460(5) 0.5587(3) 0.1418(4) 0.061(2) Uani 1 1 d . . . . .
H23 H 0.223137 0.528281 0.125096 0.073 Uiso 1 1 calc R U . . .
C24 C 0.2057(5) 0.6004(3) 0.1341(4) 0.067(2) Uani 1 1 d . . . . .
H24 H 0.148857 0.605418 0.112053 0.080 Uiso 1 1 calc R U . . .
C25 C 0.2643(5) 0.6366(2) 0.1656(4) 0.051(2) Uani 1 1 d . . . . .
C26 C 0.2527(4) 0.6882(3) 0.1680(4) 0.057(2) Uani 1 1 d . . . . .
C27 C 0.1891(5) 0.7082(3) 0.1891(5) 0.069(3) Uani 1 1 d . . . . .
C28 C 0.1278(5) 0.6793(4) 0.2069(5) 0.075(3) Uani 1 1 d . . . . .
H28 H 0.131572 0.645168 0.201777 0.090 Uiso 1 1 calc R U . . .
C29 C 0.0675(6) 0.6942(5) 0.2292(6) 0.104(4) Uani 1 1 d . . . . .
C30 C 0.0058(8) 0.6618(5) 0.2455(7) 0.110(2) Uani 1 1 d . . . . .
C31 C 0.0131(9) 0.6119(5) 0.2269(8) 0.1353(16) Uani 1 1 d . . . . .
H31A H -0.029688 0.592149 0.237780 0.203 Uiso 1 1 calc R U . . .
H31B H 0.068127 0.599390 0.249512 0.203 Uiso 1 1 calc R U . . .
H31C H 0.005681 0.610335 0.180796 0.203 Uiso 1 1 calc R U . . .
C32 C -0.0806(9) 0.6829(5) 0.2229(8) 0.1353(16) Uani 1 1 d . . . . .
H32A H -0.099419 0.682128 0.176162 0.203 Uiso 1 1 calc R U . . .
H32B H -0.079878 0.716540 0.237648 0.203 Uiso 1 1 calc R U . . .
H32C H -0.118583 0.663688 0.240131 0.203 Uiso 1 1 calc R U . . .
C33 C 0.0594(9) 0.7488(6) 0.2327(9) 0.158(7) Uani 1 1 d . . . . .
C34 C 0.1254(8) 0.7798(4) 0.2237(9) 0.150(7) Uani 1 1 d . . . . .
C35 C 0.1182(8) 0.8353(5) 0.2243(6) 0.110(2) Uani 1 1 d . . . . .
C36 C 0.1031(9) 0.8469(5) 0.2823(8) 0.1353(16) Uani 1 1 d . . . . .
H36A H 0.059134 0.825877 0.288941 0.203 Uiso 1 1 calc R U . . .
H36B H 0.085665 0.880932 0.281587 0.203 Uiso 1 1 calc R U . . .
H36C H 0.153987 0.842087 0.317064 0.203 Uiso 1 1 calc R U . . .
C37 C 1.0668(8) 0.7798(4) 0.4914(7) 0.138(6) Uani 1 1 d . . . . .
C39 C 0.7131(9) 0.5800(6) 0.1619(6) 0.136(6) Uani 1 1 d . . . . .
H39A H 0.765862 0.597451 0.168847 0.204 Uiso 1 1 calc R U . . .
H39B H 0.670944 0.602115 0.169433 0.204 Uiso 1 1 calc R U . . .
H39C H 0.695125 0.568076 0.117925 0.204 Uiso 1 1 calc R U . . .
C40 C 0.7539(8) 0.7040(4) 0.0589(7) 0.125(5) Uani 1 1 d . . . . .
H40A H 0.803873 0.692065 0.048743 0.187 Uiso 1 1 calc R U . . .
H40B H 0.705091 0.686948 0.032415 0.187 Uiso 1 1 calc R U . . .
H40C H 0.758831 0.697909 0.104029 0.187 Uiso 1 1 calc R U . . .
C41 C 0.7869(10) 0.5040(6) 0.1858(10) 0.182(8) Uani 1 1 d . . . . .
H41A H 0.760390 0.490996 0.143209 0.273 Uiso 1 1 calc R U . . .
H41B H 0.802883 0.477126 0.216236 0.273 Uiso 1 1 calc R U . . .
H41C H 0.836483 0.522505 0.184902 0.273 Uiso 1 1 calc R U . . .
C42 C 0.3730(5) 0.7670(3) 0.0952(5) 0.068(3) Uani 1 1 d . . . . .
H42 H 0.381917 0.790129 0.065522 0.082 Uiso 1 1 calc R U . . .
C43 C 0.8829(4) 0.6897(3) 0.4018(4) 0.053(2) Uani 1 1 d . . . . .
C44 C 0.4249(5) 0.4472(3) 0.1946(4) 0.058(2) Uani 1 1 d . . . . .
H44 H 0.476290 0.459516 0.190955 0.070 Uiso 1 1 calc R U . . .
C45 C 0.7570(6) 0.5536(4) 0.2764(6) 0.082(3) Uani 1 1 d . . . . .
C46 C 0.3148(4) 0.7174(3) 0.1509(4) 0.052(2) Uani 1 1 d . . . . .
C47 C 0.6555(4) 0.7291(2) 0.2341(4) 0.0442(19) Uani 1 1 d . . . . .
H47 H 0.688001 0.752131 0.219271 0.053 Uiso 1 1 calc R U . . .
C48 C 0.3008(5) 0.7562(3) 0.1060(5) 0.067(2) Uani 1 1 d . . . . .
H48 H 0.249134 0.771632 0.087063 0.080 Uiso 1 1 calc R U . . .
C49 C 0.5685(5) 0.5482(3) 0.3456(4) 0.056(2) Uani 1 1 d . . . . .
H49 H 0.609310 0.539381 0.383724 0.067 Uiso 1 1 calc R U . . .
C51 C 0.6131(4) 0.6721(2) 0.2897(4) 0.0474(19) Uani 1 1 d . . . . .
C52 C 0.7425(7) 0.4714(5) 0.4521(9) 0.167(8) Uani 1 1 d . . . . .
H52A H 0.702841 0.493209 0.463704 0.250 Uiso 1 1 calc R U . . .
H52B H 0.758887 0.445690 0.484279 0.250 Uiso 1 1 calc R U . . .
H52C H 0.716429 0.456766 0.410386 0.250 Uiso 1 1 calc R U . . .
C53 C 0.7259(8) 0.7584(4) -0.0258(6) 0.108(4) Uani 1 1 d . . . . .
H53A H 0.675751 0.738767 -0.042257 0.161 Uiso 1 1 calc R U . . .
H53B H 0.772846 0.742775 -0.036262 0.161 Uiso 1 1 calc R U . . .
H53C H 0.717038 0.790811 -0.045175 0.161 Uiso 1 1 calc R U . . .
C54 C 0.7725(7) 0.5228(3) 0.3285(8) 0.099(4) Uani 1 1 d . . . . .
C55 C 0.4351(4) 0.7369(3) 0.1369(4) 0.056(2) Uani 1 1 d . . . . .
C56 C 0.7627(4) 0.7071(3) 0.3340(4) 0.0476(19) Uani 1 1 d . . . . .
C58 C 0.5197(4) 0.7409(2) 0.1500(4) 0.0485(19) Uani 1 1 d . . . . .
C59 C 0.6708(5) 0.7857(3) 0.0641(4) 0.059(2) Uani 1 1 d . . . . .
C61 C 0.0352(9) 0.8530(5) 0.1764(8) 0.1353(16) Uani 1 1 d . . . . .
H61A H 0.029363 0.838258 0.134539 0.203 Uiso 1 1 calc R U . . .
H61B H 0.036222 0.888456 0.172624 0.203 Uiso 1 1 calc R U . . .
H61C H -0.011768 0.843376 0.192155 0.203 Uiso 1 1 calc R U . . .
C62 C 0.9985(6) 0.7494(3) 0.4616(5) 0.092(3) Uani 1 1 d . . . . .
C63 C 0.6810(4) 0.7024(2) 0.2893(4) 0.0418(18) Uani 1 1 d . . . . .
C64 C 0.8214(7) 0.5009(4) 0.4489(9) 0.126(5) Uani 1 1 d . . . . .
C65 C 0.8894(8) 0.4672(4) 0.4475(10) 0.177(8) Uani 1 1 d . . . . .
H65A H 0.941547 0.485374 0.455147 0.266 Uiso 1 1 calc R U . . .
H65B H 0.876964 0.451454 0.405607 0.266 Uiso 1 1 calc R U . . .
H65C H 0.894841 0.442486 0.480662 0.266 Uiso 1 1 calc R U . . .
C66 C 0.5611(4) 0.7743(2) 0.1147(4) 0.0456(19) Uani 1 1 d . . . . .
C67 C 0.5330(9) 0.9196(5) -0.0089(8) 0.1353(16) Uani 1 1 d . . . . .
H67A H 0.579504 0.909275 -0.024802 0.203 Uiso 1 1 calc R U . . .
H67B H 0.525091 0.954719 -0.014583 0.203 Uiso 1 1 calc R U . . .
H67C H 0.482295 0.902748 -0.032782 0.203 Uiso 1 1 calc R U . . .
C68 C 0.7734(5) 0.6027(3) 0.2912(5) 0.067(2) Uani 1 1 d . . . . .
H68 H 0.767554 0.625641 0.257758 0.081 Uiso 1 1 calc R U . . .
C69 C 0.8140(5) 0.5863(3) 0.4037(6) 0.077(3) Uani 1 1 d . . . . .
H69 H 0.834725 0.598213 0.445969 0.092 Uiso 1 1 calc R U . . .
C70 C 0.7243(9) 0.5382(5) 0.2069(8) 0.126(5) Uani 1 1 d . . . . .
C71 C 1.0810(8) 0.6793(4) 0.5101(8) 0.152(7) Uani 1 1 d . . . . .
C72 C 0.8747(5) 0.7394(3) 0.3914(4) 0.054(2) Uani 1 1 d . . . . .
C73 C 0.8489(8) 0.5292(5) 0.5158(8) 0.141(6) Uani 1 1 d . . . . .
H73A H 0.802185 0.548525 0.521022 0.211 Uiso 1 1 calc R U . . .
H73B H 0.895727 0.550695 0.516448 0.211 Uiso 1 1 calc R U . . .
H73C H 0.865646 0.505638 0.550661 0.211 Uiso 1 1 calc R U . . .
C74 C 0.6167(9) 0.9414(5) 0.0994(8) 0.1353(16) Uani 1 1 d . . . . .
H74A H 0.599303 0.974776 0.086590 0.203 Uiso 1 1 calc R U . . .
H74B H 0.669500 0.934651 0.090128 0.203 Uiso 1 1 calc R U . . .
H74C H 0.623719 0.937653 0.145283 0.203 Uiso 1 1 calc R U . . .
C75 C 0.7979(5) 0.6181(3) 0.3538(5) 0.057(2) Uani 1 1 d . . . . .
C77 C 0.8006(6) 0.5366(3) 0.3938(7) 0.084(3) Uani 1 1 d . . . . .
C78 C 0.5520(8) 0.9067(5) 0.0633(6) 0.110(2) Uani 1 1 d . . . . .
C79 C 0.1930(9) 0.8600(5) 0.2206(8) 0.1353(16) Uani 1 1 d . . . . .
H79A H 0.189980 0.894320 0.231501 0.203 Uiso 1 1 calc R U . . .
H79B H 0.198382 0.857287 0.177133 0.203 Uiso 1 1 calc R U . . .
H79C H 0.241378 0.844985 0.250594 0.203 Uiso 1 1 calc R U . . .
C80 C 0.4108(5) 0.3978(3) 0.1879(4) 0.057(2) Uani 1 1 d . . . . .
C81 C 0.5383(4) 0.8235(2) 0.1044(4) 0.0484(19) Uani 1 1 d . . . . .
H81 H 0.494759 0.835988 0.119857 0.058 Uiso 1 1 calc R U . . .
C82 C 0.4735(8) 0.9174(5) 0.0832(8) 0.1353(16) Uani 1 1 d . . . . .
H82A H 0.480014 0.904993 0.126401 0.203 Uiso 1 1 calc R U . . .
H82B H 0.425954 0.901409 0.053467 0.203 Uiso 1 1 calc R U . . .
H82C H 0.464004 0.952509 0.082429 0.203 Uiso 1 1 calc R U . . .
C83 C 0.7439(6) 0.7630(4) 0.0445(5) 0.086(3) Uani 1 1 d . . . . .
C84 C 1.0071(6) 0.6997(3) 0.4705(6) 0.099(4) Uani 1 1 d . . . . .
C85 C 0.5779(5) 0.8536(2) 0.0722(4) 0.052(2) Uani 1 1 d . . . . .
C86 C 0.6448(5) 0.8333(4) 0.0525(4) 0.065(2) Uani 1 1 d . . . . .
C87 C 0.6256(5) 0.7570(3) 0.0940(4) 0.052(2) Uani 1 1 d . . . . .
H87 H 0.639840 0.723591 0.100493 0.063 Uiso 1 1 calc R U . . .
C88 C 0.1837(6) 0.7600(3) 0.1996(7) 0.103(4) Uani 1 1 d . . . . .
H88 H 0.222915 0.780872 0.188907 0.123 Uiso 1 1 calc R U . . .
C89 C 0.5741(4) 0.7164(2) 0.2038(4) 0.0430(18) Uani 1 1 d . . . . .
C90 C 0.0180(9) 0.6621(5) 0.3139(8) 0.1353(16) Uani 1 1 d . . . . .
H90A H 0.058255 0.687459 0.333349 0.203 Uiso 1 1 calc R U . . .
H90B H 0.039141 0.630450 0.331700 0.203 Uiso 1 1 calc R U . . .
H90C H -0.034943 0.668774 0.323024 0.203 Uiso 1 1 calc R U . . .
H2 H 0.261(4) 0.319(6) 0.176(8) 0.203 Uiso 1 1 d D U . . .
N1 N 0.3395(3) 0.61618(19) 0.1901(3) 0.0472(16) Uani 1 1 d . . . . .
N2 N 0.4905(4) 0.5948(2) 0.2638(3) 0.0511(16) Uani 1 1 d . . . . .
N3 N 0.3943(3) 0.7044(2) 0.1679(3) 0.0491(16) Uani 1 1 d . . . . .
N4 N 0.5473(3) 0.68051(18) 0.2375(3) 0.0440(15) Uani 1 1 d . . . . .
N5 N 1.1193(7) 0.8053(4) 0.5211(7) 0.160(6) Uani 1 1 d . . . . .
N6 N 1.1408(8) 0.6625(4) 0.5429(9) 0.202(9) Uani 1 1 d . . . . .
N7 N 0.9466(4) 0.6672(2) 0.4408(4) 0.071(2) Uani 1 1 d . . . . .
N8 N 0.9323(4) 0.7704(2) 0.4211(4) 0.073(2) Uani 1 1 d . . . . .
N9 N 0.8107(3) 0.6693(2) 0.3650(3) 0.0453(15) Uani 1 1 d . . . . .
N10 N 0.8002(3) 0.7498(2) 0.3482(3) 0.0497(16) Uani 1 1 d . . . . .
O1 O 0.6896(4) 0.8643(3) 0.0237(3) 0.087(2) Uani 1 1 d . . . . .
H1 H 0.666921 0.865229 -0.015767 0.130 Uiso 1 1 calc R U . . .
O2 O 0.3190(3) 0.33237(18) 0.1836(3) 0.0731(17) Uani 1 1 d D . . . .
O3 O 0.7581(7) 0.4728(2) 0.3136(6) 0.161(4) Uani 1 1 d . . . . .
H3 H 0.779572 0.456037 0.346213 0.241 Uiso 1 1 calc R U . . .
O4 O -0.0003(9) 0.7671(5) 0.2445(10) 0.238(8) Uani 1 1 d . . . . .
O5 O 0.6544(3) 0.64033(19) 0.3936(3) 0.0577(14) Uani 1 1 d . . . . .
Ni Ni 0.44302(5) 0.64941(3) 0.21653(5) 0.0459(4) Uani 1 1 d . . . . .


_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
C1 C3 1.437(10) . ?
C1 C51 1.476(11) . ?
C1 O5 1.234(9) . ?
C3 C49 1.413(10) . ?
C3 N2 1.364(9) . ?
C5 C6 1.409(11) . ?
C5 C49 1.355(11) . ?
C6 C7 1.409(11) . ?
C6 N2 1.410(9) . ?
C7 C8 1.498(10) . ?
C7 C22 1.383(11) . ?
C8 C21 1.390(10) . ?
C8 C44 1.386(11) . ?
C9 C83 1.444(17) . ?
C10 C70 1.557(16) . ?
C11 C12 1.532(11) . ?
C11 C13 1.543(13) . ?
C11 C14 1.524(15) . ?
C11 C80 1.521(11) . ?
C15 C16 1.416(11) . ?
C15 C80 1.413(11) . ?
C15 O2 1.373(9) . ?
C16 C17 1.512(11) . ?
C16 C21 1.416(10) . ?
C17 C18 1.518(13) . ?
C17 C19 1.548(17) . ?
C17 C20 1.527(15) . ?
C22 C23 1.426(11) . ?
C22 N1 1.390(9) . ?
C23 C24 1.319(11) . ?
C24 C25 1.435(11) . ?
C25 C26 1.436(11) . ?
C25 N1 1.348(9) . ?
C26 C27 1.388(11) . ?
C26 C46 1.444(10) . ?
C27 C28 1.437(12) . ?
C27 C88 1.451(13) . ?
C28 C29 1.305(14) . ?
C29 C30 1.484(15) . ?
C29 C33 1.512(18) . ?
C30 C31 1.447(17) . ?
C30 C32 1.510(18) . ?
C30 C90 1.450(19) . ?
C33 C34 1.453(17) . ?
C33 O4 1.211(15) . ?
C34 C35 1.535(16) . ?
C34 C88 1.347(14) . ?
C35 C36 1.395(17) . ?
C35 C61 1.566(18) . ?
C35 C79 1.449(16) . ?
C37 C62 1.421(14) . ?
C37 N5 1.170(13) . ?
C39 C70 1.49(2) . ?
C40 C83 1.655(15) . ?
C41 C70 1.572(18) . ?
C42 C48 1.329(11) . ?
C42 C55 1.439(11) . ?
C43 C72 1.389(11) . ?
C43 N7 1.320(10) . ?
C43 N9 1.372(9) . ?
C44 C80 1.381(10) . ?
C45 C54 1.385(16) . ?
C45 C68 1.400(12) . ?
C45 C70 1.522(17) . ?
C46 C48 1.425(11) . ?
C46 N3 1.329(9) . ?
C47 C63 1.375(10) . ?
C47 C89 1.385(9) . ?
C51 C63 1.412(10) . ?
C51 N4 1.366(9) . ?
C52 C64 1.571(15) . ?
C53 C83 1.483(15) . ?
C54 C77 1.422(17) . ?
C54 O3 1.418(12) . ?
C55 C58 1.371(10) . ?
C55 N3 1.408(9) . ?
C56 C63 1.449(10) . ?
C56 N9 1.374(9) . ?
C56 N10 1.330(9) . ?
C58 C66 1.489(10) . ?
C58 C89 1.437(10) . ?
C59 C83 1.539(12) . ?
C59 C86 1.382(12) . ?
C59 C87 1.379(11) . ?
C62 C84 1.384(13) . ?
C62 N8 1.341(11) . ?
C64 C65 1.478(17) . ?
C64 C73 1.60(2) . ?
C64 C77 1.516(17) . ?
C66 C81 1.408(10) . ?
C66 C87 1.369(10) . ?
C67 C78 1.560(18) . ?
C68 C75 1.379(12) . ?
C69 C75 1.366(12) . ?
C69 C77 1.393(13) . ?
C71 C84 1.414(15) . ?
C71 N6 1.156(13) . ?
C72 N8 1.315(10) . ?
C72 N10 1.368(9) . ?
C74 C78 1.494(17) . ?
C75 N9 1.436(10) . ?
C78 C82 1.525(17) . ?
C78 C85 1.524(14) . ?
C81 C85 1.372(10) . ?
C84 N7 1.372(11) . ?
C85 C86 1.422(12) . ?
C86 O1 1.397(10) . ?
C89 N4 1.381(9) . ?
N1 Ni 1.903(5) . ?
N2 Ni 1.871(6) . ?
N3 Ni 1.899(6) . ?
N4 Ni 1.885(5) . ?

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
C3 C1 C51 116.8(7) . . ?
O5 C1 C3 123.0(7) . . ?
O5 C1 C51 119.9(7) . . ?
C49 C3 C1 125.2(7) . . ?
N2 C3 C1 123.5(6) . . ?
N2 C3 C49 111.0(6) . . ?
C49 C5 C6 108.2(6) . . ?
C5 C6 N2 108.8(6) . . ?
C7 C6 C5 127.7(7) . . ?
C7 C6 N2 122.5(7) . . ?
C6 C7 C8 116.4(7) . . ?
C22 C7 C6 122.7(7) . . ?
C22 C7 C8 120.8(7) . . ?
C21 C8 C7 120.2(7) . . ?
C44 C8 C7 121.0(7) . . ?
C44 C8 C21 118.7(7) . . ?
C12 C11 C13 106.6(8) . . ?
C14 C11 C12 106.3(9) . . ?
C14 C11 C13 110.5(8) . . ?
C80 C11 C12 112.0(7) . . ?
C80 C11 C13 110.6(8) . . ?
C80 C11 C14 110.7(8) . . ?
C80 C15 C16 123.8(6) . . ?
O2 C15 C16 120.8(6) . . ?
O2 C15 C80 115.3(7) . . ?
C15 C16 C17 124.0(6) . . ?
C21 C16 C15 115.4(6) . . ?
C21 C16 C17 120.5(7) . . ?
C16 C17 C18 113.2(7) . . ?
C16 C17 C19 108.1(8) . . ?
C16 C17 C20 111.9(7) . . ?
C18 C17 C19 110.3(8) . . ?
C18 C17 C20 107.5(9) . . ?
C20 C17 C19 105.5(9) . . ?
C8 C21 C16 122.4(7) . . ?
C7 C22 C23 128.5(7) . . ?
C7 C22 N1 122.3(7) . . ?
N1 C22 C23 107.5(6) . . ?
C24 C23 C22 109.1(7) . . ?
C23 C24 C25 106.6(7) . . ?
C24 C25 C26 128.5(7) . . ?
N1 C25 C24 109.9(6) . . ?
N1 C25 C26 121.4(6) . . ?
C25 C26 C46 115.1(7) . . ?
C27 C26 C25 122.0(7) . . ?
C27 C26 C46 122.8(7) . . ?
C26 C27 C28 122.9(8) . . ?
C26 C27 C88 122.0(7) . . ?
C28 C27 C88 115.0(8) . . ?
C29 C28 C27 127.8(10) . . ?
C28 C29 C30 124.4(12) . . ?
C28 C29 C33 114.9(9) . . ?
C30 C29 C33 120.5(10) . . ?
C29 C30 C32 111.1(11) . . ?
C31 C30 C29 112.6(11) . . ?
C31 C30 C32 115.0(12) . . ?
C31 C30 C90 107.3(12) . . ?
C90 C30 C29 109.5(11) . . ?
C90 C30 C32 100.5(11) . . ?
C34 C33 C29 119.6(10) . . ?
O4 C33 C29 121.0(12) . . ?
O4 C33 C34 119.4(14) . . ?
C33 C34 C35 121.2(10) . . ?
C88 C34 C33 118.6(11) . . ?
C88 C34 C35 118.3(11) . . ?
C34 C35 C61 111.2(12) . . ?
C36 C35 C34 105.7(12) . . ?
C36 C35 C61 100.5(12) . . ?
C36 C35 C79 108.8(12) . . ?
C79 C35 C34 113.2(11) . . ?
C79 C35 C61 116.0(11) . . ?
N5 C37 C62 172.9(19) . . ?
C48 C42 C55 107.1(8) . . ?
N7 C43 C72 126.4(7) . . ?
N7 C43 N9 127.6(7) . . ?
N9 C43 C72 106.0(7) . . ?
C80 C44 C8 123.2(7) . . ?
C54 C45 C68 114.9(10) . . ?
C54 C45 C70 125.7(11) . . ?
C68 C45 C70 119.4(12) . . ?
C48 C46 C26 127.1(7) . . ?
N3 C46 C26 121.2(6) . . ?
N3 C46 C48 110.6(6) . . ?
C63 C47 C89 108.0(6) . . ?
C42 C48 C46 107.8(7) . . ?
C5 C49 C3 106.7(7) . . ?
C63 C51 C1 127.2(7) . . ?
N4 C51 C1 121.6(6) . . ?
N4 C51 C63 111.1(6) . . ?
C45 C54 C77 126.4(9) . . ?
C45 C54 O3 115.1(13) . . ?
O3 C54 C77 118.5(13) . . ?
C58 C55 C42 127.6(7) . . ?
C58 C55 N3 124.3(7) . . ?
N3 C55 C42 107.8(6) . . ?
N9 C56 C63 125.3(6) . . ?
N10 C56 C63 122.2(7) . . ?
N10 C56 N9 112.4(6) . . ?
C55 C58 C66 123.1(7) . . ?
C55 C58 C89 121.1(7) . . ?
C89 C58 C66 115.5(6) . . ?
C86 C59 C83 124.7(8) . . ?
C87 C59 C83 119.0(8) . . ?
C87 C59 C86 116.3(7) . . ?
C84 C62 C37 118.6(9) . . ?
N8 C62 C37 117.5(8) . . ?
N8 C62 C84 123.5(8) . . ?
C47 C63 C51 105.5(6) . . ?
C47 C63 C56 123.1(6) . . ?
C51 C63 C56 131.4(7) . . ?
C52 C64 C73 104.1(14) . . ?
C65 C64 C52 109.9(10) . . ?
C65 C64 C73 107.2(12) . . ?
C65 C64 C77 113.4(14) . . ?
C77 C64 C52 111.2(10) . . ?
C77 C64 C73 110.6(10) . . ?
C81 C66 C58 122.1(7) . . ?
C87 C66 C58 118.7(6) . . ?
C87 C66 C81 119.1(7) . . ?
C75 C68 C45 120.8(10) . . ?
C75 C69 C77 121.3(11) . . ?
C10 C70 C41 111.0(10) . . ?
C39 C70 C10 107.1(14) . . ?
C39 C70 C41 104.1(12) . . ?
C39 C70 C45 112.7(9) . . ?
C45 C70 C10 109.8(10) . . ?
C45 C70 C41 112.0(13) . . ?
N6 C71 C84 179(2) . . ?
N8 C72 C43 122.1(7) . . ?
N8 C72 N10 127.4(7) . . ?
N10 C72 C43 110.5(6) . . ?
C68 C75 N9 117.5(8) . . ?
C69 C75 C68 122.0(8) . . ?
C69 C75 N9 120.4(8) . . ?
C54 C77 C64 124.1(11) . . ?
C69 C77 C54 114.3(10) . . ?
C69 C77 C64 121.4(13) . . ?
C74 C78 C67 107.6(10) . . ?
C74 C78 C82 106.5(11) . . ?
C74 C78 C85 114.1(10) . . ?
C82 C78 C67 107.1(11) . . ?
C85 C78 C67 108.5(10) . . ?
C85 C78 C82 112.7(9) . . ?
C15 C80 C11 121.9(6) . . ?
C44 C80 C11 121.8(7) . . ?
C44 C80 C15 116.4(7) . . ?
C85 C81 C66 120.9(7) . . ?
C9 C83 C40 108.2(12) . . ?
C9 C83 C53 113.8(11) . . ?
C9 C83 C59 113.1(10) . . ?
C53 C83 C40 95.4(10) . . ?
C53 C83 C59 111.9(8) . . ?
C59 C83 C40 113.1(8) . . ?
C62 C84 C71 121.2(8) . . ?
N7 C84 C62 123.0(8) . . ?
N7 C84 C71 115.8(8) . . ?
C81 C85 C78 118.9(8) . . ?
C81 C85 C86 116.9(7) . . ?
C86 C85 C78 124.0(8) . . ?
C59 C86 C85 123.5(7) . . ?
C59 C86 O1 118.7(8) . . ?
O1 C86 C85 117.6(8) . . ?
C66 C87 C59 123.1(7) . . ?
C34 C88 C27 122.8(9) . . ?
C47 C89 C58 126.1(6) . . ?
N4 C89 C47 110.4(6) . . ?
N4 C89 C58 123.0(6) . . ?
C22 N1 Ni 125.6(5) . . ?
C25 N1 C22 106.7(6) . . ?
C25 N1 Ni 126.3(4) . . ?
C3 N2 C6 105.2(6) . . ?
C3 N2 Ni 126.0(5) . . ?
C6 N2 Ni 128.3(5) . . ?
C46 N3 C55 106.2(6) . . ?
C46 N3 Ni 127.7(5) . . ?
C55 N3 Ni 125.7(4) . . ?
C51 N4 C89 105.0(5) . . ?
C51 N4 Ni 127.2(5) . . ?
C89 N4 Ni 127.8(5) . . ?
C43 N7 C84 111.0(7) . . ?
C72 N8 C62 113.9(7) . . ?
C43 N9 C56 106.2(6) . . ?
C43 N9 C75 124.5(6) . . ?
C56 N9 C75 128.3(6) . . ?
C56 N10 C72 104.9(6) . . ?
N2 Ni N1 89.6(2) . . ?
N2 Ni N3 179.5(3) . . ?
N2 Ni N4 90.4(2) . . ?
N3 Ni N1 90.0(2) . . ?
N4 Ni N1 175.9(3) . . ?
N4 Ni N3 89.9(2) . . ?

_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 -0.831 -0.830 -0.432 3474.6 1088.1 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_colour            'Dark violet'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform methanol'
