# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# 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 
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data_tcd590b
_database_code_depnum_ccdc_archive 'CCDC 1564845'
_audit_update_record             
;
2017-07-26 deposited with the CCDC.
2017-11-28 downloaded from the CCDC.
;
_audit_creation_date             2016-09-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H37 N3 O2, C2 H6 O'
_chemical_formula_sum            'C33 H43 N3 O3'
_chemical_formula_weight         529.70
_chemical_absolute_configuration ad
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_H-M_alt        'P 65'
_space_group_name_Hall           'P 65'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'

_cell_length_a                   8.7435(4)
_cell_length_b                   8.7435(4)
_cell_length_c                   69.045(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4571.2(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    5368
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.28
_cell_measurement_theta_min      3.84
_shelx_estimated_absorpt_T_max   0.977
_shelx_estimated_absorpt_T_min   0.888
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0936 before and 0.0731 after correction.
The Ratio of minimum to maximum transmission is 0.7514.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1716
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'crystallized from EtOH in an NMR tube'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       -82
_diffrn_reflns_number            26441
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.386
_diffrn_reflns_theta_min         3.841
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                4864
_reflns_number_total             5575
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.35A (Buker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2015) '
_computing_data_reduction        'SAINT V8.35A (Buker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 
;
 Flack x determined using 1992 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(17)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5575
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0577
_refine_ls_restrained_S_all      1.035
_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)+(0.0688P)²+0.9525P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1516
_refine_special_details          
'All free iPr groups disordered and modelled with restraints and constraints (DFIX, SADI and EADP) with the following occupancies:C16-C18 23:77%; C19-C21 40:60%; C36-C37 47:53%. The solvent alcohol molecule is disordered also and was modelled with restraints and constraints (SADI and EADP) with 80:20% occupancy.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C16-C16A
 0.3 with sigma of 0.01
 C19-C19A
 0.4 with sigma of 0.01
 C16A-C11 \\sim C16-C11
 with sigma of 0.002
 O37-C38 \\sim O37-C38A
 with sigma of 0.002
 C39A-C38A \\sim C39-C38
 with sigma of 0.002
 C20-C19 \\sim C20A-C19A
 with sigma of 0.01
 C21-C19 \\sim C21A-C19A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C16A) = Uanis(C17A) = Uanis(C18A) = Uanis(C17) = Uanis(C16) = Uanis(C18)
Uanis(C19A) = Uanis(C20A) = Uanis(C21A) = Uanis(C19) = Uanis(C20) = Uanis(C21)
Uanis(C38A) = Uanis(C39A) = Uanis(C38) = Uanis(C39)
4. Others
 Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36A)=Sof(H36A)=
 Sof(H36B)=Sof(H36C)=1-FVAR(1)
 Sof(H34)=Sof(C36)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C35)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=FVAR(1)
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(2)
 Sof(C17)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C16)=Sof(H16)=Sof(C18)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=FVAR(2)
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21A)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(3)
 Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=FVAR(3)
 Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C39A)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=1-FVAR(4)
 Sof(H37)=Sof(C38)=Sof(H38C)=Sof(H38D)=Sof(C39)=Sof(H39D)=Sof(H39E)=Sof(H39F)=
 FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C34(H34A), C34(H34), C16A(H16A), C19A(H19A), C16(H16), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C38A(H38A,H38B), C38(H38C,H38D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C27(H27), C28(H28),
 C29(H29), N9(H9)
5.d Tetrahedral OH refined with riding coordinates:
 O37(H37A), O37(H37)
5.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C17A(H17A,H17B,H17C), C18A(H18A,
 H18B,H18C), C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C), C35A(H35A,H35B,H35C),
 C36A(H36A,H36B,H36C), C39A(H39A,H39B,H39C), C36(H36D,H36E,H36F), C17(H17D,H17E,
 H17F), C18(H18D,H18E,H18F), C20(H20D,H20E,H20F), C21(H21D,H21E,H21F), C35(H35D,
 H35E,H35F), C39(H39D,H39E,H39F)
;
_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
C2 C 0.3481(6) 0.8831(6) 0.49310(6) 0.0428(9) Uani 1 1 d . . . . .
C3 C 0.4920(6) 0.8572(6) 0.49544(6) 0.0497(10) Uani 1 1 d . . . . .
H3 H 0.5789 0.8920 0.4856 0.060 Uiso 1 1 calc R . . . .
C4 C 0.5063(6) 0.7806(7) 0.51224(7) 0.0518(11) Uani 1 1 d . . . . .
H4 H 0.6040 0.7631 0.5142 0.062 Uiso 1 1 calc R . . . .
C5 C 0.3755(6) 0.7293(6) 0.52628(6) 0.0484(10) Uani 1 1 d . . . . .
H5 H 0.3824 0.6775 0.5381 0.058 Uiso 1 1 calc R . . . .
C6 C 0.2349(5) 0.7559(6) 0.52250(5) 0.0399(8) Uani 1 1 d . . . . .
C7 C 0.0916(6) 0.7026(6) 0.53742(6) 0.0438(9) Uani 1 1 d . . . . .
C10 C -0.1898(6) 0.6811(6) 0.54483(6) 0.0468(10) Uani 1 1 d . . . . .
C11 C -0.1785(6) 0.8205(7) 0.55576(7) 0.0543(11) Uani 1 1 d D . . . .
C12 C -0.3183(7) 0.7849(8) 0.56793(7) 0.0607(12) Uani 1 1 d . . . . .
H12 H -0.3145 0.8773 0.5755 0.073 Uiso 1 1 calc R . . . .
C13 C -0.4632(7) 0.6173(8) 0.56919(7) 0.0596(13) Uani 1 1 d . . . . .
H13 H -0.5582 0.5960 0.5775 0.071 Uiso 1 1 calc R . . . .
C14 C -0.4713(6) 0.4813(7) 0.55852(7) 0.0576(12) Uani 1 1 d . . . . .
H14 H -0.5714 0.3664 0.5597 0.069 Uiso 1 1 calc R . . . .
C15 C -0.3349(6) 0.5089(7) 0.54591(7) 0.0546(11) Uani 1 1 d . . . . .
C22 C 0.3316(5) 0.9729(6) 0.47572(6) 0.0428(9) Uani 1 1 d . . . . .
C25 C 0.2340(7) 1.1347(6) 0.45879(7) 0.0498(10) Uani 1 1 d . . . . .
C26 C 0.3357(7) 1.1463(6) 0.44267(6) 0.0526(11) Uani 1 1 d . . . . .
C27 C 0.3556(8) 1.2612(8) 0.42754(8) 0.0700(15) Uani 1 1 d . . . . .
H27 H 0.4231 1.2689 0.4164 0.084 Uiso 1 1 calc R . . . .
C28 C 0.2762(10) 1.3631(8) 0.42890(9) 0.0813(18) Uani 1 1 d . . . . .
H28 H 0.2895 1.4416 0.4187 0.098 Uiso 1 1 calc R . . . .
C29 C 0.1791(10) 1.3521(7) 0.44480(9) 0.0763(17) Uani 1 1 d . . . . .
H29 H 0.1264 1.4243 0.4453 0.092 Uiso 1 1 calc R . . . .
C30 C 0.1534(7) 1.2395(7) 0.46030(7) 0.0578(11) Uani 1 1 d . . . . .
C31 C 0.4138(7) 1.0278(7) 0.44213(6) 0.0536(11) Uani 1 1 d . . . . .
C32 C 0.2873(7) 0.8471(7) 0.43415(7) 0.0575(12) Uani 1 1 d . . . . .
H32A H 0.1772 0.7946 0.4416 0.086 Uiso 1 1 calc GR . . . .
H32B H 0.3404 0.7717 0.4351 0.086 Uiso 1 1 calc GR . . . .
H32C H 0.2623 0.8576 0.4205 0.086 Uiso 1 1 calc GR . . . .
C33 C 0.5915(7) 1.1085(9) 0.43200(7) 0.0678(15) Uani 1 1 d . . . . .
H33A H 0.5752 1.1165 0.4181 0.102 Uiso 1 1 calc GR . . . .
H33B H 0.6444 1.0340 0.4342 0.102 Uiso 1 1 calc GR . . . .
H33C H 0.6697 1.2269 0.4372 0.102 Uiso 1 1 calc GR . . . .
C34 C 0.0571(8) 1.2405(7) 0.47851(8) 0.0599(12) Uani 1 1 d . . . . .
H34A H -0.0008 1.1182 0.4839 0.072 Uiso 0.54(5) 1 calc R . P A 2
H34 H 0.0442 1.1454 0.4875 0.072 Uiso 0.46(5) 1 calc R . P A 1
N1 N 0.2199(4) 0.8326(4) 0.50634(5) 0.0386(7) Uani 1 1 d . . . . .
N9 N -0.0481(4) 0.7155(5) 0.53181(5) 0.0426(8) Uani 1 1 d . . . . .
H9 H -0.0533 0.7460 0.5198 0.051 Uiso 1 1 calc R . . . .
N24 N 0.2173(5) 1.0228(5) 0.47457(5) 0.0434(8) Uani 1 1 d . . . . .
O8 O 0.1066(5) 0.6514(6) 0.55347(5) 0.0611(9) Uani 1 1 d . . . . .
O23 O 0.4559(4) 1.0057(5) 0.46234(5) 0.0508(7) Uani 1 1 d . . . . .
O37 O -0.1383(5) 0.7877(5) 0.49096(5) 0.0585(8) Uani 1 1 d D . . . .
H37A H -0.0381 0.8785 0.4901 0.088 Uiso 0.204(13) 1 calc R . P B 2
H37 H -0.0353 0.8598 0.4873 0.088 Uiso 0.796(13) 1 calc R . P B 1
C16A C -0.0175(14) 1.0025(12) 0.55349(14) 0.0731(14) Uani 0.77(2) 1 d D . P C 2
H16A H 0.0881 0.9867 0.5532 0.088 Uiso 0.77(2) 1 calc R . P C 2
C17A C 0.0095(12) 1.1292(13) 0.57048(18) 0.0731(14) Uani 0.77(2) 1 d . . P C 2
H17A H -0.0959 1.1405 0.5719 0.110 Uiso 0.77(2) 1 calc GR . P C 2
H17B H 0.1121 1.2455 0.5678 0.110 Uiso 0.77(2) 1 calc GR . P C 2
H17C H 0.0295 1.0818 0.5825 0.110 Uiso 0.77(2) 1 calc GR . P C 2
C18A C -0.0166(12) 1.0953(12) 0.53458(18) 0.0731(14) Uani 0.77(2) 1 d . . P C 2
H18A H -0.0212 1.0229 0.5235 0.110 Uiso 0.77(2) 1 calc GR . P C 2
H18B H 0.0916 1.2107 0.5339 0.110 Uiso 0.77(2) 1 calc GR . P C 2
H18C H -0.1196 1.1116 0.5343 0.110 Uiso 0.77(2) 1 calc GR . P C 2
C19A C -0.3320(18) 0.3530(18) 0.53459(19) 0.0760(13) Uani 0.620(12) 1 d D . P D
2
H19A H -0.2074 0.3827 0.5322 0.091 Uiso 0.620(12) 1 calc R . P D 2
C20A C -0.4364(16) 0.1695(15) 0.54454(18) 0.0760(13) Uani 0.620(12) 1 d D . P D
2
H20A H -0.3901 0.1764 0.5576 0.114 Uiso 0.620(12) 1 calc GR . P D 2
H20B H -0.4234 0.0819 0.5370 0.114 Uiso 0.620(12) 1 calc GR . P D 2
H20C H -0.5617 0.1347 0.5453 0.114 Uiso 0.620(12) 1 calc GR . P D 2
C21A C -0.4275(16) 0.3356(14) 0.51511(15) 0.0760(13) Uani 0.620(12) 1 d D . P D
2
H21A H -0.5461 0.3164 0.5177 0.114 Uiso 0.620(12) 1 calc GR . P D 2
H21B H -0.4367 0.2352 0.5078 0.114 Uiso 0.620(12) 1 calc GR . P D 2
H21C H -0.3602 0.4441 0.5076 0.114 Uiso 0.620(12) 1 calc GR . P D 2
C35A C -0.090(4) 1.293(5) 0.4767(4) 0.094(8) Uani 0.54(5) 1 d . . P A 2
H35A H -0.0364 1.4153 0.4723 0.141 Uiso 0.54(5) 1 calc GR . P A 2
H35B H -0.1455 1.2805 0.4893 0.141 Uiso 0.54(5) 1 calc GR . P A 2
H35C H -0.1788 1.2147 0.4673 0.141 Uiso 0.54(5) 1 calc GR . P A 2
C36A C 0.180(2) 1.357(4) 0.4930(3) 0.089(8) Uani 0.54(5) 1 d . . P A 2
H36A H 0.2657 1.3190 0.4960 0.133 Uiso 0.54(5) 1 calc GR . P A 2
H36B H 0.1151 1.3518 0.5048 0.133 Uiso 0.54(5) 1 calc GR . P A 2
H36C H 0.2423 1.4781 0.4881 0.133 Uiso 0.54(5) 1 calc GR . P A 2
C38A C -0.151(5) 0.660(5) 0.4773(4) 0.096(2) Uani 0.204(13) 1 d D . P B 2
H38A H -0.0285 0.7025 0.4729 0.115 Uiso 0.204(13) 1 calc R . P B 2
H38B H -0.1845 0.5520 0.4850 0.115 Uiso 0.204(13) 1 calc R . P B 2
C39A C -0.252(5) 0.599(6) 0.4607(4) 0.096(2) Uani 0.204(13) 1 d D . P B 2
H39A H -0.1920 0.6834 0.4502 0.144 Uiso 0.204(13) 1 calc GR . P B 2
H39B H -0.3674 0.5882 0.4631 0.144 Uiso 0.204(13) 1 calc GR . P B 2
H39C H -0.2671 0.4840 0.4572 0.144 Uiso 0.204(13) 1 calc GR . P B 2
C36 C 0.166(4) 1.429(4) 0.4886(5) 0.111(10) Uani 0.46(5) 1 d . . P A 1
H36D H 0.2761 1.4416 0.4940 0.167 Uiso 0.46(5) 1 calc GR . P A 1
H36E H 0.0959 1.4383 0.4991 0.167 Uiso 0.46(5) 1 calc GR . P A 1
H36F H 0.1948 1.5218 0.4791 0.167 Uiso 0.46(5) 1 calc GR . P A 1
C17 C -0.010(4) 1.075(5) 0.5778(5) 0.0731(14) Uani 0.23(2) 1 d . . P C 1
H17D H -0.1005 1.1096 0.5786 0.110 Uiso 0.23(2) 1 calc GR . P C 1
H17E H 0.1067 1.1791 0.5801 0.110 Uiso 0.23(2) 1 calc GR . P C 1
H17F H -0.0330 0.9854 0.5876 0.110 Uiso 0.23(2) 1 calc GR . P C 1
C16 C -0.013(4) 1.000(3) 0.5575(2) 0.0731(14) Uani 0.23(2) 1 d D . P C 1
H16 H 0.0904 0.9815 0.5566 0.088 Uiso 0.23(2) 1 calc R . P C 1
C18 C 0.002(4) 1.112(5) 0.5429(6) 0.0731(14) Uani 0.23(2) 1 d . . P C 1
H18D H -0.0120 1.0532 0.5304 0.110 Uiso 0.23(2) 1 calc GR . P C 1
H18E H 0.1186 1.2184 0.5435 0.110 Uiso 0.23(2) 1 calc GR . P C 1
H18F H -0.0898 1.1442 0.5444 0.110 Uiso 0.23(2) 1 calc GR . P C 1
C19 C -0.358(3) 0.369(3) 0.5332(3) 0.0760(13) Uani 0.380(12) 1 d D . P D 1
H19 H -0.2478 0.4141 0.5253 0.091 Uiso 0.380(12) 1 calc R . P D 1
C20 C -0.369(3) 0.220(3) 0.5469(3) 0.0760(13) Uani 0.380(12) 1 d D . P D 1
H20D H -0.2603 0.2664 0.5545 0.114 Uiso 0.380(12) 1 calc GR . P D 1
H20E H -0.3841 0.1201 0.5390 0.114 Uiso 0.380(12) 1 calc GR . P D 1
H20F H -0.4702 0.1807 0.5556 0.114 Uiso 0.380(12) 1 calc GR . P D 1
C21 C -0.515(2) 0.296(3) 0.5191(3) 0.0760(13) Uani 0.380(12) 1 d D . P D 1
H21D H -0.6256 0.2490 0.5264 0.114 Uiso 0.380(12) 1 calc GR . P D 1
H21E H -0.5173 0.2007 0.5113 0.114 Uiso 0.380(12) 1 calc GR . P D 1
H21F H -0.5031 0.3903 0.5105 0.114 Uiso 0.380(12) 1 calc GR . P D 1
C35 C -0.108(3) 1.212(4) 0.4731(3) 0.075(7) Uani 0.46(5) 1 d . . P A 1
H35D H -0.0939 1.3142 0.4658 0.112 Uiso 0.46(5) 1 calc GR . P A 1
H35E H -0.1784 1.1965 0.4847 0.112 Uiso 0.46(5) 1 calc GR . P A 1
H35F H -0.1670 1.1060 0.4651 0.112 Uiso 0.46(5) 1 calc GR . P A 1
C38 C -0.2283(15) 0.6602(13) 0.47611(13) 0.096(2) Uani 0.796(13) 1 d D . P B 1
H38C H -0.1673 0.5914 0.4744 0.115 Uiso 0.796(13) 1 calc R . P B 1
H38D H -0.3490 0.5773 0.4808 0.115 Uiso 0.796(13) 1 calc R . P B 1
C39 C -0.2432(14) 0.7195(16) 0.45817(13) 0.096(2) Uani 0.796(13) 1 d D . P B 1
H39D H -0.3174 0.6184 0.4498 0.144 Uiso 0.796(13) 1 calc GR . P B 1
H39E H -0.1257 0.7886 0.4524 0.144 Uiso 0.796(13) 1 calc GR . P B 1
H39F H -0.2971 0.7939 0.4595 0.144 Uiso 0.796(13) 1 calc GR . P B 1


_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
C2 C3 1.395(6) . ?
C2 C22 1.480(6) . ?
C2 N1 1.339(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.386(6) . ?
C6 C7 1.505(5) . ?
C6 N1 1.341(5) . ?
C7 N9 1.339(5) . ?
C7 O8 1.227(5) . ?
C10 C11 1.394(7) . ?
C10 C15 1.404(7) . ?
C10 N9 1.436(5) . ?
C11 C12 1.385(6) . ?
C11 C16A 1.516(8) . ?
C11 C16 1.515(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.379(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.370(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.397(6) . ?
C15 C19A 1.583(14) . ?
C15 C19 1.43(2) . ?
C22 N24 1.277(5) . ?
C22 O23 1.343(5) . ?
C25 C26 1.397(7) . ?
C25 C30 1.412(7) . ?
C25 N24 1.422(5) . ?
C26 C27 1.398(6) . ?
C26 C31 1.499(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.380(9) . ?
C28 H28 0.9500 . ?
C28 C29 1.362(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.394(7) . ?
C30 C34 1.515(7) . ?
C31 C32 1.508(7) . ?
C31 C33 1.518(7) . ?
C31 O23 1.480(5) . ?
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 1.0000 . ?
C34 H34 1.0000 . ?
C34 C35A 1.57(2) . ?
C34 C36A 1.450(18) . ?
C34 C36 1.59(2) . ?
C34 C35 1.38(3) . ?
N9 H9 0.8800 . ?
O37 H37A 0.8400 . ?
O37 H37 0.8400 . ?
O37 C38A 1.427(9) . ?
O37 C38 1.427(8) . ?
C16A H16A 1.0000 . ?
C16A C17A 1.549(12) . ?
C16A C18A 1.535(14) . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
C19A H19A 1.0000 . ?
C19A C20A 1.554(13) . ?
C19A C21A 1.550(12) . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C35A H35A 0.9800 . ?
C35A H35B 0.9800 . ?
C35A H35C 0.9800 . ?
C36A H36A 0.9800 . ?
C36A H36B 0.9800 . ?
C36A H36C 0.9800 . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C38A C39A 1.374(13) . ?
C39A H39A 0.9800 . ?
C39A H39B 0.9800 . ?
C39A H39C 0.9800 . ?
C36 H36D 0.9800 . ?
C36 H36E 0.9800 . ?
C36 H36F 0.9800 . ?
C17 H17D 0.9800 . ?
C17 H17E 0.9800 . ?
C17 H17F 0.9800 . ?
C17 C16 1.54(4) . ?
C16 H16 1.0000 . ?
C16 C18 1.36(4) . ?
C18 H18D 0.9800 . ?
C18 H18E 0.9800 . ?
C18 H18F 0.9800 . ?
C19 H19 1.0000 . ?
C19 C20 1.572(14) . ?
C19 C21 1.541(14) . ?
C20 H20D 0.9800 . ?
C20 H20E 0.9800 . ?
C20 H20F 0.9800 . ?
C21 H21D 0.9800 . ?
C21 H21E 0.9800 . ?
C21 H21F 0.9800 . ?
C35 H35D 0.9800 . ?
C35 H35E 0.9800 . ?
C35 H35F 0.9800 . ?
C38 H38C 0.9900 . ?
C38 H38D 0.9900 . ?
C38 C39 1.374(13) . ?
C39 H39D 0.9800 . ?
C39 H39E 0.9800 . ?
C39 H39F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C2 C22 121.0(4) . . ?
N1 C2 C3 122.8(4) . . ?
N1 C2 C22 116.2(4) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.1(4) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 118.9(4) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 121.0 . . ?
C6 C5 C4 118.1(4) . . ?
C6 C5 H5 121.0 . . ?
C5 C6 C7 119.4(3) . . ?
N1 C6 C5 123.8(4) . . ?
N1 C6 C7 116.7(3) . . ?
N9 C7 C6 115.4(3) . . ?
O8 C7 C6 120.5(4) . . ?
O8 C7 N9 124.1(4) . . ?
C11 C10 C15 122.7(4) . . ?
C11 C10 N9 118.6(4) . . ?
C15 C10 N9 118.7(4) . . ?
C10 C11 C16A 119.0(7) . . ?
C10 C11 C16 124(2) . . ?
C12 C11 C10 117.6(5) . . ?
C12 C11 C16A 123.4(7) . . ?
C12 C11 C16 117.5(18) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 121.0(5) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.7(4) . . ?
C14 C13 H13 119.7 . . ?
C13 C14 H14 119.5 . . ?
C13 C14 C15 121.0(5) . . ?
C15 C14 H14 119.5 . . ?
C10 C15 C19A 120.2(7) . . ?
C10 C15 C19 123.2(11) . . ?
C14 C15 C10 117.0(5) . . ?
C14 C15 C19A 122.6(7) . . ?
C14 C15 C19 119.3(11) . . ?
N24 C22 C2 122.1(3) . . ?
N24 C22 O23 124.9(4) . . ?
O23 C22 C2 112.8(4) . . ?
C26 C25 C30 121.2(4) . . ?
C26 C25 N24 120.2(4) . . ?
C30 C25 N24 118.5(4) . . ?
C25 C26 C27 119.6(5) . . ?
C25 C26 C31 117.6(4) . . ?
C27 C26 C31 122.8(5) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 C26 119.4(5) . . ?
C28 C27 H27 120.3 . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.4(5) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 H29 118.5 . . ?
C28 C29 C30 122.9(6) . . ?
C30 C29 H29 118.5 . . ?
C25 C30 C34 121.6(4) . . ?
C29 C30 C25 116.4(5) . . ?
C29 C30 C34 121.8(5) . . ?
C26 C31 C32 112.6(4) . . ?
C26 C31 C33 113.8(4) . . ?
C32 C31 C33 111.2(4) . . ?
O23 C31 C26 107.2(3) . . ?
O23 C31 C32 107.9(4) . . ?
O23 C31 C33 103.4(4) . . ?
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 . . ?
C30 C34 H34A 106.9 . . ?
C30 C34 H34 110.1 . . ?
C30 C34 C35A 118.2(10) . . ?
C30 C34 C36 108.8(13) . . ?
C35A C34 H34A 106.9 . . ?
C36A C34 C30 111.0(8) . . ?
C36A C34 H34A 106.9 . . ?
C36A C34 C35A 106.2(12) . . ?
C36 C34 H34 110.1 . . ?
C35 C34 C30 107.9(11) . . ?
C35 C34 H34 110.1 . . ?
C35 C34 C36 109.7(12) . . ?
C2 N1 C6 117.3(3) . . ?
C7 N9 C10 121.9(3) . . ?
C7 N9 H9 119.0 . . ?
C10 N9 H9 119.0 . . ?
C22 N24 C25 117.0(4) . . ?
C22 O23 C31 116.7(3) . . ?
C38A O37 H37A 109.5 . . ?
C38 O37 H37 109.5 . . ?
C11 C16A H16A 107.1 . . ?
C11 C16A C17A 113.7(7) . . ?
C11 C16A C18A 113.6(6) . . ?
C17A C16A H16A 107.1 . . ?
C18A C16A H16A 107.1 . . ?
C18A C16A C17A 107.9(9) . . ?
C16A C17A H17A 109.5 . . ?
C16A C17A H17B 109.5 . . ?
C16A C17A H17C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
C16A C18A H18A 109.5 . . ?
C16A C18A H18B 109.5 . . ?
C16A C18A H18C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C15 C19A H19A 110.1 . . ?
C20A C19A C15 114.6(10) . . ?
C20A C19A H19A 110.1 . . ?
C21A C19A C15 105.9(8) . . ?
C21A C19A H19A 110.1 . . ?
C21A C19A C20A 105.8(11) . . ?
C19A C20A H20A 109.5 . . ?
C19A C20A H20B 109.5 . . ?
C19A C20A H20C 109.5 . . ?
H20A C20A H20B 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C19A C21A H21A 109.5 . . ?
C19A C21A H21B 109.5 . . ?
C19A C21A H21C 109.5 . . ?
H21A C21A H21B 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C34 C35A H35A 109.5 . . ?
C34 C35A H35B 109.5 . . ?
C34 C35A H35C 109.5 . . ?
H35A C35A H35B 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C34 C36A H36A 109.5 . . ?
C34 C36A H36B 109.5 . . ?
C34 C36A H36C 109.5 . . ?
H36A C36A H36B 109.5 . . ?
H36A C36A H36C 109.5 . . ?
H36B C36A H36C 109.5 . . ?
O37 C38A H38A 104.9 . . ?
O37 C38A H38B 104.9 . . ?
H38A C38A H38B 105.8 . . ?
C39A C38A O37 129(3) . . ?
C39A C38A H38A 104.9 . . ?
C39A C38A H38B 104.9 . . ?
C38A C39A H39A 109.5 . . ?
C38A C39A H39B 109.5 . . ?
C38A C39A H39C 109.5 . . ?
H39A C39A H39B 109.5 . . ?
H39A C39A H39C 109.5 . . ?
H39B C39A H39C 109.5 . . ?
C34 C36 H36D 109.5 . . ?
C34 C36 H36E 109.5 . . ?
C34 C36 H36F 109.5 . . ?
H36D C36 H36E 109.5 . . ?
H36D C36 H36F 109.5 . . ?
H36E C36 H36F 109.5 . . ?
H17D C17 H17E 109.5 . . ?
H17D C17 H17F 109.5 . . ?
H17E C17 H17F 109.5 . . ?
C16 C17 H17D 109.5 . . ?
C16 C17 H17E 109.5 . . ?
C16 C17 H17F 109.5 . . ?
C11 C16 C17 109(2) . . ?
C11 C16 H16 107.4 . . ?
C17 C16 H16 107.4 . . ?
C18 C16 C11 112.7(19) . . ?
C18 C16 C17 113(3) . . ?
C18 C16 H16 107.4 . . ?
C16 C18 H18D 109.5 . . ?
C16 C18 H18E 109.5 . . ?
C16 C18 H18F 109.5 . . ?
H18D C18 H18E 109.5 . . ?
H18D C18 H18F 109.5 . . ?
H18E C18 H18F 109.5 . . ?
C15 C19 H19 107.6 . . ?
C15 C19 C20 105.3(15) . . ?
C15 C19 C21 117.3(11) . . ?
C20 C19 H19 107.6 . . ?
C21 C19 H19 107.6 . . ?
C21 C19 C20 111.2(19) . . ?
C19 C20 H20D 109.5 . . ?
C19 C20 H20E 109.5 . . ?
C19 C20 H20F 109.5 . . ?
H20D C20 H20E 109.5 . . ?
H20D C20 H20F 109.5 . . ?
H20E C20 H20F 109.5 . . ?
C19 C21 H21D 109.5 . . ?
C19 C21 H21E 109.5 . . ?
C19 C21 H21F 109.5 . . ?
H21D C21 H21E 109.5 . . ?
H21D C21 H21F 109.5 . . ?
H21E C21 H21F 109.5 . . ?
C34 C35 H35D 109.5 . . ?
C34 C35 H35E 109.5 . . ?
C34 C35 H35F 109.5 . . ?
H35D C35 H35E 109.5 . . ?
H35D C35 H35F 109.5 . . ?
H35E C35 H35F 109.5 . . ?
O37 C38 H38C 107.8 . . ?
O37 C38 H38D 107.8 . . ?
H38C C38 H38D 107.1 . . ?
C39 C38 O37 118.2(9) . . ?
C39 C38 H38C 107.8 . . ?
C39 C38 H38D 107.8 . . ?
C38 C39 H39D 109.5 . . ?
C38 C39 H39E 109.5 . . ?
C38 C39 H39F 109.5 . . ?
H39D C39 H39E 109.5 . . ?
H39D C39 H39F 109.5 . . ?
H39E C39 H39F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C33 H33A O8 0.98 2.38 3.337(6) 165 6_664
N9 H9 O37 0.88 2.22 3.077(4) 166 .
O37 H37 N24 0.84 2.13 2.963(5) 173 .

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
C2 C3 C4 C5 0.8(7) . . . . ?
C2 C22 N24 C25 169.1(4) . . . . ?
C2 C22 O23 C31 156.6(4) . . . . ?
C3 C2 C22 N24 -168.8(4) . . . . ?
C3 C2 C22 O23 6.8(6) . . . . ?
C3 C2 N1 C6 0.7(6) . . . . ?
C3 C4 C5 C6 0.9(7) . . . . ?
C4 C5 C6 C7 -179.7(4) . . . . ?
C4 C5 C6 N1 -1.9(7) . . . . ?
C5 C6 C7 N9 -173.2(4) . . . . ?
C5 C6 C7 O8 6.7(7) . . . . ?
C5 C6 N1 C2 1.1(6) . . . . ?
C6 C7 N9 C10 -175.7(4) . . . . ?
C7 C6 N1 C2 178.9(4) . . . . ?
C10 C11 C12 C13 0.1(7) . . . . ?
C10 C11 C16A C17A -161.4(8) . . . . ?
C10 C11 C16A C18A 74.7(12) . . . . ?
C10 C11 C16 C17 -148(2) . . . . ?
C10 C11 C16 C18 86(4) . . . . ?
C10 C15 C19A C20A 148.5(9) . . . . ?
C10 C15 C19A C21A -95.2(9) . . . . ?
C10 C15 C19 C20 121.8(15) . . . . ?
C10 C15 C19 C21 -114.0(18) . . . . ?
C11 C10 C15 C14 0.3(7) . . . . ?
C11 C10 C15 C19A -174.4(6) . . . . ?
C11 C10 C15 C19 172.6(7) . . . . ?
C11 C10 N9 C7 89.6(5) . . . . ?
C11 C12 C13 C14 0.6(8) . . . . ?
C12 C11 C16A C17A 19.9(13) . . . . ?
C12 C11 C16A C18A -104.0(8) . . . . ?
C12 C11 C16 C17 23(3) . . . . ?
C12 C11 C16 C18 -103(3) . . . . ?
C12 C13 C14 C15 -0.9(7) . . . . ?
C13 C14 C15 C10 0.5(7) . . . . ?
C13 C14 C15 C19A 175.1(6) . . . . ?
C13 C14 C15 C19 -172.1(8) . . . . ?
C14 C15 C19A C20A -25.9(12) . . . . ?
C14 C15 C19A C21A 90.3(10) . . . . ?
C14 C15 C19 C20 -66.1(16) . . . . ?
C14 C15 C19 C21 58(2) . . . . ?
C15 C10 C11 C12 -0.6(7) . . . . ?
C15 C10 C11 C16A -179.4(7) . . . . ?
C15 C10 C11 C16 169.7(14) . . . . ?
C15 C10 N9 C7 -91.1(5) . . . . ?
C22 C2 C3 C4 177.0(4) . . . . ?
C22 C2 N1 C6 -178.0(4) . . . . ?
C25 C26 C27 C28 0.9(8) . . . . ?
C25 C26 C31 C32 85.1(5) . . . . ?
C25 C26 C31 C33 -147.1(4) . . . . ?
C25 C26 C31 O23 -33.4(6) . . . . ?
C25 C30 C34 C35A -155(2) . . . . ?
C25 C30 C34 C36A 81.5(18) . . . . ?
C25 C30 C34 C36 111.6(17) . . . . ?
C25 C30 C34 C35 -129.5(17) . . . . ?
C26 C25 C30 C29 0.9(8) . . . . ?
C26 C25 C30 C34 -174.2(5) . . . . ?
C26 C25 N24 C22 17.9(6) . . . . ?
C26 C27 C28 C29 -0.1(10) . . . . ?
C26 C31 O23 C22 45.2(5) . . . . ?
C27 C26 C31 C32 -92.5(6) . . . . ?
C27 C26 C31 C33 35.3(7) . . . . ?
C27 C26 C31 O23 149.0(5) . . . . ?
C27 C28 C29 C30 -0.3(11) . . . . ?
C28 C29 C30 C25 -0.1(9) . . . . ?
C28 C29 C30 C34 175.0(6) . . . . ?
C29 C30 C34 C35A 30(2) . . . . ?
C29 C30 C34 C36A -93.3(18) . . . . ?
C29 C30 C34 C36 -63.2(18) . . . . ?
C29 C30 C34 C35 55.7(18) . . . . ?
C30 C25 C26 C27 -1.3(8) . . . . ?
C30 C25 C26 C31 -179.0(5) . . . . ?
C30 C25 N24 C22 -158.9(4) . . . . ?
C31 C26 C27 C28 178.5(5) . . . . ?
C32 C31 O23 C22 -76.3(5) . . . . ?
C33 C31 O23 C22 165.8(4) . . . . ?
N1 C2 C3 C4 -1.7(7) . . . . ?
N1 C2 C22 N24 9.9(6) . . . . ?
N1 C2 C22 O23 -174.5(4) . . . . ?
N1 C6 C7 N9 8.8(5) . . . . ?
N1 C6 C7 O8 -171.3(4) . . . . ?
N9 C10 C11 C12 178.7(4) . . . . ?
N9 C10 C11 C16A 0.0(8) . . . . ?
N9 C10 C11 C16 -10.9(15) . . . . ?
N9 C10 C15 C14 -179.0(4) . . . . ?
N9 C10 C15 C19A 6.3(7) . . . . ?
N9 C10 C15 C19 -6.8(9) . . . . ?
N24 C22 O23 C31 -27.9(6) . . . . ?
N24 C25 C26 C27 -177.9(5) . . . . ?
N24 C25 C26 C31 4.4(7) . . . . ?
N24 C25 C30 C29 177.6(5) . . . . ?
N24 C25 C30 C34 2.5(7) . . . . ?
O8 C7 N9 C10 4.4(7) . . . . ?
O23 C22 N24 C25 -5.9(6) . . . . ?
C16A C11 C12 C13 178.8(7) . . . . ?
C16 C11 C12 C13 -170.9(16) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MItegen holder'
_olex2_submission_original_sample_id PP499
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tcd21
_database_code_depnum_ccdc_archive 'CCDC 1564847'
_audit_update_record             
;
2017-07-26 deposited with the CCDC.
2017-11-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C33 H40 N4 Ni O2), C4 H10 O'
_chemical_formula_sum            'C70 H90 N8 Ni2 O5'
_chemical_formula_weight         1240.91

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.7514(7)
_cell_length_b                   21.5643(8)
_cell_length_c                   16.1479(6)
_cell_angle_alpha                90
_cell_angle_beta                 110.8990(10)
_cell_angle_gamma                90
_cell_volume                     6750.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9918
_cell_measurement_theta_min      2.322
_cell_measurement_theta_max      27.460

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_F_000             2648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.612
_shelx_estimated_absorpt_T_min   0.898
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7144
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS-2012/1, Bruker 2012'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            72448
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.412
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             15480
_reflns_number_gt                11316
_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       'Bruker APEX2, (Bruker 2012)'
_computing_cell_refinement       'Bruker SAINT, (Bruker 2012)'
_computing_data_reduction        'Bruker SAINT, (Bruker 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL v. 2008/4, (Bruker 2008)'
_computing_publication_material  'Bruker SHELXTL v. 2008/4, (Bruker 2008)'

_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)+(0.0432P)²+4.5024P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15480
_refine_ls_number_parameters     795
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_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
C2 C 0.34018(10) 0.32872(10) 0.29444(13) 0.0194(4) Uani 1 1 d . . . . .
C3 C 0.33452(11) 0.39242(10) 0.28750(14) 0.0248(5) Uani 1 1 d . . . . .
H3 H 0.3693 0.4184 0.3261 0.030 Uiso 1 1 calc R U . . .
C4 C 0.27668(12) 0.41774(10) 0.22256(14) 0.0268(5) Uani 1 1 d . . . . .
H4 H 0.2717 0.4615 0.2165 0.032 Uiso 1 1 calc R U . . .
C5 C 0.22602(11) 0.37906(10) 0.16646(14) 0.0254(5) Uani 1 1 d . . . . .
H5 H 0.1865 0.3960 0.1219 0.030 Uiso 1 1 calc R U . . .
C6 C 0.23449(10) 0.31573(10) 0.17692(13) 0.0191(4) Uani 1 1 d . . . . .
C7 C 0.18795(10) 0.26524(10) 0.12365(13) 0.0208(4) Uani 1 1 d . . . . .
C9 C 0.17822(10) 0.15410(10) 0.11377(14) 0.0217(4) Uani 1 1 d . . . . .
C10 C 0.18074(12) 0.13450(11) 0.03231(15) 0.0296(5) Uani 1 1 d . . . . .
C11 C 0.15031(14) 0.07787(12) -0.00171(18) 0.0421(6) Uani 1 1 d . . . . .
H11 H 0.1503 0.0644 -0.0577 0.051 Uiso 1 1 calc R U . . .
C12 C 0.12025(15) 0.04107(12) 0.04445(19) 0.0447(7) Uani 1 1 d . . . . .
H12 H 0.1006 0.0023 0.0207 0.054 Uiso 1 1 calc R U . . .
C13 C 0.11887(12) 0.06083(11) 0.12528(17) 0.0355(6) Uani 1 1 d . . . . .
H13 H 0.0985 0.0351 0.1569 0.043 Uiso 1 1 calc R U . . .
C14 C 0.14682(11) 0.11774(10) 0.16116(15) 0.0248(4) Uani 1 1 d . . . . .
C15 C 0.14273(11) 0.14130(10) 0.24751(14) 0.0257(5) Uani 1 1 d . . . . .
H15 H 0.1857 0.1656 0.2779 0.031 Uiso 1 1 calc R U . . .
C16 C 0.08179(12) 0.18592(11) 0.22918(16) 0.0320(5) Uani 1 1 d . . . . .
H16A H 0.0873 0.2207 0.1933 0.048 Uiso 1 1 calc R U . . .
H16B H 0.0804 0.2016 0.2855 0.048 Uiso 1 1 calc R U . . .
H16C H 0.0387 0.1640 0.1971 0.048 Uiso 1 1 calc R U . . .
C17 C 0.13966(13) 0.08967(12) 0.31103(17) 0.0375(6) Uani 1 1 d . . . . .
H17A H 0.0963 0.0667 0.2852 0.056 Uiso 1 1 calc R U . . .
H17B H 0.1421 0.1079 0.3677 0.056 Uiso 1 1 calc R U . . .
H17C H 0.1786 0.0613 0.3209 0.056 Uiso 1 1 calc R U . . .
C18 C 0.21907(14) 0.17058(12) -0.01643(16) 0.0363(6) Uani 1 1 d . . . . .
H18 H 0.2342 0.2108 0.0154 0.044 Uiso 1 1 calc R U . . .
C19 C 0.28375(16) 0.13481(14) -0.0126(2) 0.0535(8) Uani 1 1 d . . . . .
H19A H 0.3123 0.1267 0.0494 0.080 Uiso 1 1 calc R U . . .
H19B H 0.3101 0.1595 -0.0405 0.080 Uiso 1 1 calc R U . . .
H19C H 0.2703 0.0954 -0.0443 0.080 Uiso 1 1 calc R U . . .
C20 C 0.1740(2) 0.18527(17) -0.1116(2) 0.0676(10) Uani 1 1 d . . . . .
H20A H 0.1602 0.1466 -0.1451 0.101 Uiso 1 1 calc R U . . .
H20B H 0.1999 0.2110 -0.1388 0.101 Uiso 1 1 calc R U . . .
H20C H 0.1327 0.2077 -0.1122 0.101 Uiso 1 1 calc R U . . .
C21 C 0.39668(10) 0.29046(10) 0.35891(13) 0.0222(4) Uani 1 1 d . . . . .
C23 C 0.42729(10) 0.18453(10) 0.40017(13) 0.0221(4) Uani 1 1 d . . . . .
C24 C 0.47841(12) 0.15612(13) 0.37562(15) 0.0341(6) Uani 1 1 d . . . . .
C25 C 0.51552(13) 0.10763(13) 0.42747(16) 0.0416(7) Uani 1 1 d . . . . .
H25 H 0.5505 0.0880 0.4118 0.050 Uiso 1 1 calc R U . . .
C26 C 0.50285(13) 0.08733(11) 0.50117(16) 0.0387(6) Uani 1 1 d . . . . .
H26 H 0.5285 0.0537 0.5353 0.046 Uiso 1 1 calc R U . . .
C27 C 0.45253(13) 0.11617(11) 0.52523(16) 0.0350(5) Uani 1 1 d . . . . .
H27 H 0.4440 0.1023 0.5762 0.042 Uiso 1 1 calc R U . . .
C28 C 0.41412(11) 0.16542(10) 0.47544(14) 0.0260(5) Uani 1 1 d . . . . .
C29 C 0.35884(12) 0.19675(12) 0.50248(15) 0.0322(5) Uani 1 1 d . . . . .
H29 H 0.3399 0.2320 0.4606 0.039 Uiso 1 1 calc R U . . .
C30 C 0.29930(15) 0.15296(16) 0.4934(2) 0.0565(8) Uani 1 1 d . . . . .
H30A H 0.2828 0.1346 0.4340 0.085 Uiso 1 1 calc R U . . .
H30B H 0.2617 0.1760 0.5026 0.085 Uiso 1 1 calc R U . . .
H30C H 0.3150 0.1200 0.5379 0.085 Uiso 1 1 calc R U . . .
C31 C 0.38846(16) 0.22391(16) 0.59562(18) 0.0521(8) Uani 1 1 d . . . . .
H31A H 0.4063 0.1903 0.6387 0.078 Uiso 1 1 calc R U . . .
H31B H 0.3521 0.2462 0.6089 0.078 Uiso 1 1 calc R U . . .
H31C H 0.4260 0.2526 0.5992 0.078 Uiso 1 1 calc R U . . .
C32 C 0.49360(14) 0.17738(16) 0.29502(17) 0.0519(8) Uani 1 1 d . . . . .
H32 H 0.4570 0.2077 0.2620 0.062 Uiso 1 1 calc R U . . .
C33 C 0.4918(2) 0.1241(2) 0.2322(2) 0.0914(16) Uani 1 1 d . . . . .
H33A H 0.5302 0.0958 0.2608 0.137 Uiso 1 1 calc R U . . .
H33B H 0.4959 0.1406 0.1778 0.137 Uiso 1 1 calc R U . . .
H33C H 0.4481 0.1017 0.2177 0.137 Uiso 1 1 calc R U . . .
C34 C 0.5622(2) 0.21029(16) 0.3213(2) 0.0666(10) Uani 1 1 d . . . . .
H34A H 0.5637 0.2437 0.3630 0.100 Uiso 1 1 calc R U . . .
H34B H 0.5680 0.2278 0.2683 0.100 Uiso 1 1 calc R U . . .
H34C H 0.5995 0.1807 0.3494 0.100 Uiso 1 1 calc R U . . .
C36 C 0.31296(12) 0.07099(11) 0.24784(17) 0.0336(5) Uani 1 1 d . . . . .
C37 C 0.31307(19) 0.00427(13) 0.2385(3) 0.0717(11) Uani 1 1 d . . . . .
H37A H 0.2659 -0.0102 0.2066 0.108 Uiso 1 1 calc R U . . .
H37B H 0.3307 -0.0149 0.2974 0.108 Uiso 1 1 calc R U . . .
H37C H 0.3427 -0.0073 0.2054 0.108 Uiso 1 1 calc R U . . .
C39 C 0.68009(10) 0.23104(10) 0.68713(13) 0.0198(4) Uani 1 1 d . . . . .
C40 C 0.62037(11) 0.22387(10) 0.61382(14) 0.0243(5) Uani 1 1 d . . . . .
H40 H 0.6054 0.1838 0.5902 0.029 Uiso 1 1 calc R U . . .
C41 C 0.58256(11) 0.27651(10) 0.57534(13) 0.0245(5) Uani 1 1 d . . . . .
H41 H 0.5417 0.2726 0.5246 0.029 Uiso 1 1 calc R U . . .
C42 C 0.60472(11) 0.33512(10) 0.61132(13) 0.0227(4) Uani 1 1 d . . . . .
H42 H 0.5794 0.3713 0.5855 0.027 Uiso 1 1 calc R U . . .
C43 C 0.66453(10) 0.33924(9) 0.68551(13) 0.0189(4) Uani 1 1 d . . . . .
C44 C 0.69804(10) 0.39665(9) 0.73627(13) 0.0197(4) Uani 1 1 d . . . . .
C46 C 0.79906(10) 0.42794(9) 0.86037(12) 0.0183(4) Uani 1 1 d . . . . .
C47 C 0.78378(11) 0.44673(9) 0.93463(13) 0.0211(4) Uani 1 1 d . . . . .
C48 C 0.82970(11) 0.48681(10) 0.99537(13) 0.0233(4) Uani 1 1 d . . . . .
H48 H 0.8200 0.5002 1.0458 0.028 Uiso 1 1 calc R U . . .
C49 C 0.88909(11) 0.50746(10) 0.98370(13) 0.0239(4) Uani 1 1 d . . . . .
H49 H 0.9202 0.5339 1.0265 0.029 Uiso 1 1 calc R U . . .
C50 C 0.90291(11) 0.48939(10) 0.90941(14) 0.0226(4) Uani 1 1 d . . . . .
H50 H 0.9433 0.5042 0.9011 0.027 Uiso 1 1 calc R U . . .
C51 C 0.85833(10) 0.44971(9) 0.84664(13) 0.0191(4) Uani 1 1 d . . . . .
C52 C 0.87256(11) 0.43178(10) 0.76364(14) 0.0240(4) Uani 1 1 d . . . . .
H52 H 0.8525 0.3896 0.7455 0.029 Uiso 1 1 calc R U . . .
C53 C 0.94923(13) 0.42813(14) 0.77775(18) 0.0449(7) Uani 1 1 d . . . . .
H53A H 0.9695 0.4697 0.7899 0.067 Uiso 1 1 calc R U . . .
H53B H 0.9549 0.4115 0.7243 0.067 Uiso 1 1 calc R U . . .
H53C H 0.9725 0.4009 0.8281 0.067 Uiso 1 1 calc R U . . .
C54 C 0.83497(15) 0.47625(12) 0.68847(16) 0.0401(6) Uani 1 1 d . . . . .
H54A H 0.7855 0.4756 0.6782 0.060 Uiso 1 1 calc R U . . .
H54B H 0.8424 0.4634 0.6343 0.060 Uiso 1 1 calc R U . . .
H54C H 0.8529 0.5183 0.7046 0.060 Uiso 1 1 calc R U . . .
C55 C 0.72054(12) 0.42255(11) 0.95104(15) 0.0309(5) Uani 1 1 d . . . . .
H55 H 0.6829 0.4161 0.8923 0.037 Uiso 1 1 calc R U . . .
C56 C 0.73691(16) 0.35936(15) 0.99938(19) 0.0522(8) Uani 1 1 d . . . . .
H56A H 0.7531 0.3302 0.9645 0.078 Uiso 1 1 calc R U . . .
H56B H 0.6952 0.3429 1.0065 0.078 Uiso 1 1 calc R U . . .
H56C H 0.7729 0.3649 1.0579 0.078 Uiso 1 1 calc R U . . .
C57 C 0.69397(16) 0.46625(17) 1.0054(2) 0.0633(10) Uani 1 1 d . . . . .
H57A H 0.7300 0.4728 1.0635 0.095 Uiso 1 1 calc R U . . .
H57B H 0.6532 0.4481 1.0131 0.095 Uiso 1 1 calc R U . . .
H57C H 0.6816 0.5061 0.9745 0.095 Uiso 1 1 calc R U . . .
C58 C 0.72979(11) 0.18185(10) 0.73867(13) 0.0210(4) Uani 1 1 d . . . . .
C60 C 0.83609(11) 0.17185(9) 0.86565(14) 0.0245(5) Uani 1 1 d . . . . .
C61 C 0.83403(13) 0.16285(10) 0.95114(14) 0.0313(5) Uani 1 1 d . . . . .
C62 C 0.89147(16) 0.13617(12) 1.01505(16) 0.0440(7) Uani 1 1 d . . . . .
H62 H 0.8914 0.1299 1.0733 0.053 Uiso 1 1 calc R U . . .
C63 C 0.94808(15) 0.11874(13) 0.99576(19) 0.0502(8) Uani 1 1 d . . . . .
H63 H 0.9872 0.1017 1.0409 0.060 Uiso 1 1 calc R U . . .
C64 C 0.94839(13) 0.12587(12) 0.91103(19) 0.0433(7) Uani 1 1 d . . . . .
H64 H 0.9872 0.1123 0.8979 0.052 Uiso 1 1 calc R U . . .
C65 C 0.89238(12) 0.15284(10) 0.84407(16) 0.0303(5) Uani 1 1 d . . . . .
C66 C 0.89467(13) 0.16306(11) 0.75213(17) 0.0346(5) Uani 1 1 d . . . . .
H66 H 0.8475 0.1762 0.7125 0.042 Uiso 1 1 calc R U . . .
C67 C 0.94451(19) 0.21583(16) 0.7538(2) 0.0646(9) Uani 1 1 d . . . . .
H67A H 0.9309 0.2534 0.7776 0.097 Uiso 1 1 calc R U . . .
H67B H 0.9431 0.2239 0.6935 0.097 Uiso 1 1 calc R U . . .
H67C H 0.9914 0.2040 0.7914 0.097 Uiso 1 1 calc R U . . .
C68 C 0.91285(18) 0.10390(15) 0.7131(2) 0.0594(8) Uani 1 1 d . . . . .
H68A H 0.9596 0.0907 0.7495 0.089 Uiso 1 1 calc R U . . .
H68B H 0.9107 0.1120 0.6525 0.089 Uiso 1 1 calc R U . . .
H68C H 0.8800 0.0711 0.7125 0.089 Uiso 1 1 calc R U . . .
C69 C 0.77141(15) 0.18045(13) 0.97233(16) 0.0408(6) Uani 1 1 d . . . . .
H69 H 0.7473 0.2147 0.9312 0.049 Uiso 1 1 calc R U . . .
C70 C 0.7888(2) 0.20409(15) 1.06742(18) 0.0625(9) Uani 1 1 d . . . . .
H70A H 0.8067 0.1698 1.1091 0.094 Uiso 1 1 calc R U . . .
H70B H 0.7470 0.2207 1.0743 0.094 Uiso 1 1 calc R U . . .
H70C H 0.8237 0.2369 1.0796 0.094 Uiso 1 1 calc R U . . .
C71 C 0.72191(18) 0.12574(17) 0.9546(3) 0.0693(10) Uani 1 1 d . . . . .
H71A H 0.7075 0.1139 0.8920 0.104 Uiso 1 1 calc R U . . .
H71B H 0.6813 0.1375 0.9686 0.104 Uiso 1 1 calc R U . . .
H71C H 0.7451 0.0906 0.9918 0.104 Uiso 1 1 calc R U . . .
C73 C 0.91949(12) 0.30729(11) 0.95608(15) 0.0305(5) Uani 1 1 d . . . . .
C74 C 0.98835(14) 0.31079(19) 1.0228(2) 0.0668(10) Uani 1 1 d . . . . .
H74A H 1.0218 0.2945 0.9982 0.100 Uiso 1 1 calc R U . . .
H74B H 0.9902 0.2861 1.0745 0.100 Uiso 1 1 calc R U . . .
H74C H 0.9994 0.3541 1.0406 0.100 Uiso 1 1 calc R U . . .
C75 C 0.5899(2) 0.5116(2) 0.4755(3) 0.0952(15) Uani 1 1 d . . . . .
H75A H 0.6339 0.4894 0.4977 0.143 Uiso 1 1 calc R U . . .
H75B H 0.5734 0.5191 0.5246 0.143 Uiso 1 1 calc R U . . .
H75C H 0.5962 0.5514 0.4501 0.143 Uiso 1 1 calc R U . . .
C76 C 0.5391(2) 0.47439(17) 0.4074(2) 0.0726(11) Uani 1 1 d . . . . .
H76A H 0.5301 0.4353 0.4335 0.087 Uiso 1 1 calc R U . . .
H76B H 0.4951 0.4975 0.3825 0.087 Uiso 1 1 calc R U . . .
C77A C 0.5209(3) 0.4169(3) 0.2842(4) 0.093(2) Uani 0.7 1 d D U P A 1
H77A H 0.4910 0.3983 0.3136 0.112 Uiso 0.7 1 calc R U P A 1
H77B H 0.4906 0.4384 0.2302 0.112 Uiso 0.7 1 calc R U P A 1
C78A C 0.5548(3) 0.3699(2) 0.2592(3) 0.0713(16) Uani 0.7 1 d D . P A 1
H78A H 0.5210 0.3407 0.2211 0.107 Uiso 0.7 1 calc R U P A 1
H78B H 0.5851 0.3482 0.3121 0.107 Uiso 0.7 1 calc R U P A 1
H78C H 0.5824 0.3874 0.2266 0.107 Uiso 0.7 1 calc R U P A 1
C77B C 0.5260(6) 0.4422(6) 0.2578(5) 0.074(3) Uiso 0.3 1 d D . P A 2
H77C H 0.5221 0.3964 0.2580 0.089 Uiso 0.3 1 calc R U P A 2
H77D H 0.5511 0.4531 0.2179 0.089 Uiso 0.3 1 calc R U P A 2
C78B C 0.4554(6) 0.4688(6) 0.2208(8) 0.074(3) Uiso 0.3 1 d D . P A 2
H78D H 0.4220 0.4355 0.1961 0.111 Uiso 0.3 1 calc R U P A 2
H78E H 0.4531 0.4986 0.1740 0.111 Uiso 0.3 1 calc R U P A 2
H78F H 0.4447 0.4900 0.2680 0.111 Uiso 0.3 1 calc R U P A 2
N1 N 0.29048(8) 0.29289(8) 0.24003(10) 0.0171(3) Uani 1 1 d . . . . .
N8 N 0.21417(8) 0.20920(8) 0.15498(11) 0.0190(3) Uani 1 1 d . . . . .
N22 N 0.38331(9) 0.22980(8) 0.34271(11) 0.0197(3) Uani 1 1 d . . . . .
N35 N 0.31174(9) 0.12340(8) 0.25467(11) 0.0226(4) Uani 1 1 d . . . . .
N38 N 0.69971(8) 0.28787(8) 0.72009(10) 0.0177(3) Uani 1 1 d . . . . .
N45 N 0.75764(8) 0.38129(8) 0.80172(10) 0.0186(3) Uani 1 1 d . . . . .
N59 N 0.78258(9) 0.20858(8) 0.80418(10) 0.0201(3) Uani 1 1 d . . . . .
N72 N 0.86610(9) 0.30393(8) 0.90364(11) 0.0230(4) Uani 1 1 d . . . . .
Ni1 Ni 0.30064(2) 0.20918(2) 0.24961(2) 0.01637(6) Uani 1 1 d . . . . .
Ni2 Ni 0.78042(2) 0.29589(2) 0.81300(2) 0.01716(7) Uani 1 1 d . . . . .
O1 O 0.13450(8) 0.27739(7) 0.06087(10) 0.0301(4) Uani 1 1 d . . . . .
O2 O 0.44611(8) 0.31489(8) 0.41723(10) 0.0328(4) Uani 1 1 d . . . . .
O3 O 0.67129(8) 0.44809(7) 0.71669(10) 0.0280(3) Uani 1 1 d . . . . .
O4 O 0.72049(8) 0.12640(7) 0.71965(10) 0.0294(3) Uani 1 1 d . . . . .
O5 O 0.56429(13) 0.46170(15) 0.34229(18) 0.0916(9) Uani 1 1 d 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
C2 N1 1.336(3) . ?
C2 C3 1.380(3) . ?
C2 C21 1.506(3) . ?
C3 C4 1.393(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(3) . ?
C5 H5 0.9500 . ?
C6 N1 1.337(2) . ?
C6 C7 1.505(3) . ?
C7 O1 1.235(2) . ?
C7 N8 1.348(3) . ?
C9 C10 1.400(3) . ?
C9 C14 1.407(3) . ?
C9 N8 1.434(3) . ?
C10 C11 1.394(3) . ?
C10 C18 1.518(3) . ?
C11 C12 1.381(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.515(3) . ?
C15 C17 1.530(3) . ?
C15 C16 1.532(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.520(4) . ?
C18 C19 1.530(4) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 O2 1.236(2) . ?
C21 N22 1.343(3) . ?
C23 C24 1.399(3) . ?
C23 C28 1.400(3) . ?
C23 N22 1.429(3) . ?
C24 C25 1.388(3) . ?
C24 C32 1.515(3) . ?
C25 C26 1.379(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.385(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.397(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.523(3) . ?
C29 C30 1.520(4) . ?
C29 C31 1.524(3) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C34 1.510(5) . ?
C32 C33 1.524(5) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C36 N35 1.137(3) . ?
C36 C37 1.447(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C39 N38 1.340(3) . ?
C39 C40 1.384(3) . ?
C39 C58 1.506(3) . ?
C40 C41 1.394(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.398(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.387(3) . ?
C42 H42 0.9500 . ?
C43 N38 1.335(3) . ?
C43 C44 1.511(3) . ?
C44 O3 1.230(2) . ?
C44 N45 1.350(3) . ?
C46 C47 1.405(3) . ?
C46 C51 1.406(3) . ?
C46 N45 1.438(2) . ?
C47 C48 1.396(3) . ?
C47 C55 1.521(3) . ?
C48 C49 1.385(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.385(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.395(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.522(3) . ?
C52 C54 1.525(3) . ?
C52 C53 1.527(3) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C57 1.519(3) . ?
C55 C56 1.547(4) . ?
C55 H55 1.0000 . ?
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 O4 1.232(2) . ?
C58 N59 1.351(3) . ?
C60 C65 1.394(3) . ?
C60 C61 1.410(3) . ?
C60 N59 1.435(3) . ?
C61 C62 1.393(3) . ?
C61 C69 1.505(4) . ?
C62 C63 1.371(4) . ?
C62 H62 0.9500 . ?
C63 C64 1.379(4) . ?
C63 H63 0.9500 . ?
C64 C65 1.400(3) . ?
C64 H64 0.9500 . ?
C65 C66 1.519(3) . ?
C66 C68 1.528(4) . ?
C66 C67 1.531(4) . ?
C66 H66 1.0000 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 C71 1.523(4) . ?
C69 C70 1.534(4) . ?
C69 H69 1.0000 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C73 N72 1.132(3) . ?
C73 C74 1.452(3) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C76 1.462(5) . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 O5 1.358(4) . ?
C76 H76A 0.9900 . ?
C76 H76B 0.9900 . ?
C77A C78A 1.373(6) . ?
C77A O5 1.422(4) . ?
C77A H77A 0.9900 . ?
C77A H77B 0.9900 . ?
C78A H78A 0.9800 . ?
C78A H78B 0.9800 . ?
C78A H78C 0.9800 . ?
C77B O5 1.378(5) . ?
C77B C78B 1.485(9) . ?
C77B H77C 0.9900 . ?
C77B H77D 0.9900 . ?
C78B H78D 0.9800 . ?
C78B H78E 0.9800 . ?
C78B H78F 0.9800 . ?
N1 Ni1 1.8175(17) . ?
N8 Ni1 1.8970(16) . ?
N22 Ni1 1.8870(17) . ?
N35 Ni1 1.8624(18) . ?
N38 Ni2 1.8148(16) . ?
N45 Ni2 1.8939(17) . ?
N59 Ni2 1.8899(17) . ?
N72 Ni2 1.8646(18) . ?

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
N1 C2 C3 119.92(19) . . ?
N1 C2 C21 111.45(18) . . ?
C3 C2 C21 128.63(19) . . ?
C2 C3 C4 118.5(2) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C3 C4 C5 120.2(2) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C6 C5 C4 118.6(2) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
N1 C6 C5 119.75(19) . . ?
N1 C6 C7 112.04(18) . . ?
C5 C6 C7 128.19(19) . . ?
O1 C7 N8 128.5(2) . . ?
O1 C7 C6 121.41(19) . . ?
N8 C7 C6 110.08(17) . . ?
C10 C9 C14 121.5(2) . . ?
C10 C9 N8 119.90(19) . . ?
C14 C9 N8 118.31(18) . . ?
C11 C10 C9 118.1(2) . . ?
C11 C10 C18 119.5(2) . . ?
C9 C10 C18 122.3(2) . . ?
C12 C11 C10 121.3(2) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 119.9(2) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 121.2(2) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C9 118.0(2) . . ?
C13 C14 C15 121.8(2) . . ?
C9 C14 C15 120.17(19) . . ?
C14 C15 C17 113.7(2) . . ?
C14 C15 C16 110.27(18) . . ?
C17 C15 C16 110.96(19) . . ?
C14 C15 H15 107.2 . . ?
C17 C15 H15 107.2 . . ?
C16 C15 H15 107.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C10 C18 C20 112.5(2) . . ?
C10 C18 C19 109.6(2) . . ?
C20 C18 C19 111.1(2) . . ?
C10 C18 H18 107.8 . . ?
C20 C18 H18 107.8 . . ?
C19 C18 H18 107.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 C21 N22 128.4(2) . . ?
O2 C21 C2 121.5(2) . . ?
N22 C21 C2 110.06(17) . . ?
C24 C23 C28 121.3(2) . . ?
C24 C23 N22 119.23(19) . . ?
C28 C23 N22 119.18(18) . . ?
C25 C24 C23 118.2(2) . . ?
C25 C24 C32 120.4(2) . . ?
C23 C24 C32 121.5(2) . . ?
C26 C25 C24 121.6(2) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C25 C26 C27 119.6(2) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C26 C27 C28 120.8(2) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C27 C28 C23 118.4(2) . . ?
C27 C28 C29 120.4(2) . . ?
C23 C28 C29 121.24(19) . . ?
C30 C29 C28 111.5(2) . . ?
C30 C29 C31 111.2(2) . . ?
C28 C29 C31 111.9(2) . . ?
C30 C29 H29 107.3 . . ?
C28 C29 H29 107.3 . . ?
C31 C29 H29 107.3 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C34 C32 C24 111.4(2) . . ?
C34 C32 C33 109.7(2) . . ?
C24 C32 C33 112.3(3) . . ?
C34 C32 H32 107.7 . . ?
C24 C32 H32 107.7 . . ?
C33 C32 H32 107.7 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N35 C36 C37 178.9(3) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N38 C39 C40 119.63(19) . . ?
N38 C39 C58 111.92(17) . . ?
C40 C39 C58 128.45(19) . . ?
C39 C40 C41 118.71(19) . . ?
C39 C40 H40 120.6 . . ?
C41 C40 H40 120.6 . . ?
C40 C41 C42 120.10(19) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C43 C42 C41 118.50(19) . . ?
C43 C42 H42 120.8 . . ?
C41 C42 H42 120.8 . . ?
N38 C43 C42 119.72(18) . . ?
N38 C43 C44 112.09(17) . . ?
C42 C43 C44 128.19(19) . . ?
O3 C44 N45 128.73(19) . . ?
O3 C44 C43 121.43(18) . . ?
N45 C44 C43 109.84(17) . . ?
C47 C46 C51 120.98(18) . . ?
C47 C46 N45 120.00(18) . . ?
C51 C46 N45 118.75(17) . . ?
C48 C47 C46 118.21(19) . . ?
C48 C47 C55 120.33(18) . . ?
C46 C47 C55 121.42(18) . . ?
C49 C48 C47 121.39(19) . . ?
C49 C48 H48 119.3 . . ?
C47 C48 H48 119.3 . . ?
C48 C49 C50 119.76(19) . . ?
C48 C49 H49 120.1 . . ?
C50 C49 H49 120.1 . . ?
C49 C50 C51 120.89(19) . . ?
C49 C50 H50 119.6 . . ?
C51 C50 H50 119.6 . . ?
C50 C51 C46 118.75(18) . . ?
C50 C51 C52 120.61(18) . . ?
C46 C51 C52 120.62(18) . . ?
C51 C52 C54 109.66(18) . . ?
C51 C52 C53 113.63(18) . . ?
C54 C52 C53 111.2(2) . . ?
C51 C52 H52 107.4 . . ?
C54 C52 H52 107.4 . . ?
C53 C52 H52 107.4 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C57 C55 C47 113.7(2) . . ?
C57 C55 C56 108.3(2) . . ?
C47 C55 C56 110.0(2) . . ?
C57 C55 H55 108.2 . . ?
C47 C55 H55 108.2 . . ?
C56 C55 H55 108.2 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O4 C58 N59 128.3(2) . . ?
O4 C58 C39 122.00(19) . . ?
N59 C58 C39 109.66(17) . . ?
C65 C60 C61 121.7(2) . . ?
C65 C60 N59 119.99(19) . . ?
C61 C60 N59 117.8(2) . . ?
C62 C61 C60 117.7(2) . . ?
C62 C61 C69 121.0(2) . . ?
C60 C61 C69 121.2(2) . . ?
C63 C62 C61 121.4(2) . . ?
C63 C62 H62 119.3 . . ?
C61 C62 H62 119.3 . . ?
C62 C63 C64 120.2(2) . . ?
C62 C63 H63 119.9 . . ?
C64 C63 H63 119.9 . . ?
C63 C64 C65 121.1(3) . . ?
C63 C64 H64 119.5 . . ?
C65 C64 H64 119.5 . . ?
C60 C65 C64 117.9(2) . . ?
C60 C65 C66 121.5(2) . . ?
C64 C65 C66 120.6(2) . . ?
C65 C66 C68 112.3(2) . . ?
C65 C66 C67 110.3(2) . . ?
C68 C66 C67 111.3(2) . . ?
C65 C66 H66 107.6 . . ?
C68 C66 H66 107.6 . . ?
C67 C66 H66 107.6 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C66 C68 H68A 109.5 . . ?
C66 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C66 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C61 C69 C71 109.9(2) . . ?
C61 C69 C70 113.4(3) . . ?
C71 C69 C70 110.3(2) . . ?
C61 C69 H69 107.6 . . ?
C71 C69 H69 107.6 . . ?
C70 C69 H69 107.6 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C69 C71 H71A 109.5 . . ?
C69 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C69 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
N72 C73 C74 179.1(3) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C76 C75 H75A 109.5 . . ?
C76 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C76 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
O5 C76 C75 108.7(3) . . ?
O5 C76 H76A 110.0 . . ?
C75 C76 H76A 110.0 . . ?
O5 C76 H76B 110.0 . . ?
C75 C76 H76B 110.0 . . ?
H76A C76 H76B 108.3 . . ?
C78A C77A O5 115.1(4) . . ?
C78A C77A H77A 108.5 . . ?
O5 C77A H77A 108.5 . . ?
C78A C77A H77B 108.5 . . ?
O5 C77A H77B 108.5 . . ?
H77A C77A H77B 107.5 . . ?
C77A C78A H78A 109.5 . . ?
C77A C78A H78B 109.5 . . ?
H78A C78A H78B 109.5 . . ?
C77A C78A H78C 109.5 . . ?
H78A C78A H78C 109.5 . . ?
H78B C78A H78C 109.5 . . ?
O5 C77B C78B 114.7(9) . . ?
O5 C77B H77C 108.6 . . ?
C78B C77B H77C 108.6 . . ?
O5 C77B H77D 108.6 . . ?
C78B C77B H77D 108.6 . . ?
H77C C77B H77D 107.6 . . ?
C77B C78B H78D 109.5 . . ?
C77B C78B H78E 109.5 . . ?
H78D C78B H78E 109.5 . . ?
C77B C78B H78F 109.5 . . ?
H78D C78B H78F 109.5 . . ?
H78E C78B H78F 109.5 . . ?
C2 N1 C6 123.05(18) . . ?
C2 N1 Ni1 118.64(14) . . ?
C6 N1 Ni1 118.28(14) . . ?
C7 N8 C9 119.69(17) . . ?
C7 N8 Ni1 116.22(13) . . ?
C9 N8 Ni1 124.02(13) . . ?
C21 N22 C23 119.93(17) . . ?
C21 N22 Ni1 116.78(14) . . ?
C23 N22 Ni1 123.01(14) . . ?
C36 N35 Ni1 171.9(2) . . ?
C43 N38 C39 123.33(17) . . ?
C43 N38 Ni2 118.20(14) . . ?
C39 N38 Ni2 118.39(14) . . ?
C44 N45 C46 120.63(17) . . ?
C44 N45 Ni2 116.19(13) . . ?
C46 N45 Ni2 123.15(13) . . ?
C58 N59 C60 121.16(18) . . ?
C58 N59 Ni2 116.72(14) . . ?
C60 N59 Ni2 122.08(13) . . ?
C73 N72 Ni2 176.61(19) . . ?
N1 Ni1 N35 177.44(7) . . ?
N1 Ni1 N22 83.03(7) . . ?
N35 Ni1 N22 97.82(7) . . ?
N1 Ni1 N8 83.32(7) . . ?
N35 Ni1 N8 95.87(7) . . ?
N22 Ni1 N8 166.31(7) . . ?
N38 Ni2 N72 176.55(7) . . ?
N38 Ni2 N59 83.25(7) . . ?
N72 Ni2 N59 96.32(7) . . ?
N38 Ni2 N45 83.57(7) . . ?
N72 Ni2 N45 96.93(7) . . ?
N59 Ni2 N45 166.73(7) . . ?
C76 O5 C77B 125.6(7) . . ?
C76 O5 C77A 108.6(4) . . ?

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 C2 C3 C4 -0.6(3) . . . . ?
C21 C2 C3 C4 -179.37(19) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
C4 C5 C6 N1 0.1(3) . . . . ?
C4 C5 C6 C7 -178.7(2) . . . . ?
N1 C6 C7 O1 -178.14(18) . . . . ?
C5 C6 C7 O1 0.7(3) . . . . ?
N1 C6 C7 N8 1.5(2) . . . . ?
C5 C6 C7 N8 -179.7(2) . . . . ?
C14 C9 C10 C11 0.8(3) . . . . ?
N8 C9 C10 C11 174.4(2) . . . . ?
C14 C9 C10 C18 -175.2(2) . . . . ?
N8 C9 C10 C18 -1.6(3) . . . . ?
C9 C10 C11 C12 -1.9(4) . . . . ?
C18 C10 C11 C12 174.3(3) . . . . ?
C10 C11 C12 C13 1.2(4) . . . . ?
C11 C12 C13 C14 0.6(4) . . . . ?
C12 C13 C14 C9 -1.6(4) . . . . ?
C12 C13 C14 C15 177.1(2) . . . . ?
C10 C9 C14 C13 0.9(3) . . . . ?
N8 C9 C14 C13 -172.8(2) . . . . ?
C10 C9 C14 C15 -177.8(2) . . . . ?
N8 C9 C14 C15 8.5(3) . . . . ?
C13 C14 C15 C17 28.3(3) . . . . ?
C9 C14 C15 C17 -153.0(2) . . . . ?
C13 C14 C15 C16 -97.1(2) . . . . ?
C9 C14 C15 C16 81.6(2) . . . . ?
C11 C10 C18 C20 57.4(3) . . . . ?
C9 C10 C18 C20 -126.6(3) . . . . ?
C11 C10 C18 C19 -66.8(3) . . . . ?
C9 C10 C18 C19 109.2(3) . . . . ?
N1 C2 C21 O2 -177.04(18) . . . . ?
C3 C2 C21 O2 1.8(3) . . . . ?
N1 C2 C21 N22 2.1(2) . . . . ?
C3 C2 C21 N22 -179.1(2) . . . . ?
C28 C23 C24 C25 0.8(4) . . . . ?
N22 C23 C24 C25 -173.1(2) . . . . ?
C28 C23 C24 C32 -179.0(2) . . . . ?
N22 C23 C24 C32 7.1(4) . . . . ?
C23 C24 C25 C26 0.2(4) . . . . ?
C32 C24 C25 C26 180.0(3) . . . . ?
C24 C25 C26 C27 -0.8(4) . . . . ?
C25 C26 C27 C28 0.4(4) . . . . ?
C26 C27 C28 C23 0.6(4) . . . . ?
C26 C27 C28 C29 179.9(2) . . . . ?
C24 C23 C28 C27 -1.2(3) . . . . ?
N22 C23 C28 C27 172.8(2) . . . . ?
C24 C23 C28 C29 179.5(2) . . . . ?
N22 C23 C28 C29 -6.6(3) . . . . ?
C27 C28 C29 C30 -66.2(3) . . . . ?
C23 C28 C29 C30 113.2(3) . . . . ?
C27 C28 C29 C31 59.1(3) . . . . ?
C23 C28 C29 C31 -121.6(2) . . . . ?
C25 C24 C32 C34 -70.8(4) . . . . ?
C23 C24 C32 C34 109.0(3) . . . . ?
C25 C24 C32 C33 52.9(4) . . . . ?
C23 C24 C32 C33 -127.4(3) . . . . ?
N38 C39 C40 C41 0.9(3) . . . . ?
C58 C39 C40 C41 -178.80(19) . . . . ?
C39 C40 C41 C42 -0.6(3) . . . . ?
C40 C41 C42 C43 -0.1(3) . . . . ?
C41 C42 C43 N38 0.7(3) . . . . ?
C41 C42 C43 C44 -179.35(19) . . . . ?
N38 C43 C44 O3 -176.58(18) . . . . ?
C42 C43 C44 O3 3.5(3) . . . . ?
N38 C43 C44 N45 3.1(2) . . . . ?
C42 C43 C44 N45 -176.81(19) . . . . ?
C51 C46 C47 C48 -1.1(3) . . . . ?
N45 C46 C47 C48 172.83(18) . . . . ?
C51 C46 C47 C55 -178.8(2) . . . . ?
N45 C46 C47 C55 -4.9(3) . . . . ?
C46 C47 C48 C49 -0.4(3) . . . . ?
C55 C47 C48 C49 177.4(2) . . . . ?
C47 C48 C49 C50 1.5(3) . . . . ?
C48 C49 C50 C51 -1.1(3) . . . . ?
C49 C50 C51 C46 -0.4(3) . . . . ?
C49 C50 C51 C52 177.92(19) . . . . ?
C47 C46 C51 C50 1.5(3) . . . . ?
N45 C46 C51 C50 -172.50(18) . . . . ?
C47 C46 C51 C52 -176.81(19) . . . . ?
N45 C46 C51 C52 9.2(3) . . . . ?
C50 C51 C52 C54 -92.8(2) . . . . ?
C46 C51 C52 C54 85.5(2) . . . . ?
C50 C51 C52 C53 32.3(3) . . . . ?
C46 C51 C52 C53 -149.4(2) . . . . ?
C48 C47 C55 C57 28.5(3) . . . . ?
C46 C47 C55 C57 -153.9(2) . . . . ?
C48 C47 C55 C56 -93.2(3) . . . . ?
C46 C47 C55 C56 84.4(3) . . . . ?
N38 C39 C58 O4 179.01(19) . . . . ?
C40 C39 C58 O4 -1.3(3) . . . . ?
N38 C39 C58 N59 -1.4(2) . . . . ?
C40 C39 C58 N59 178.28(19) . . . . ?
C65 C60 C61 C62 2.3(3) . . . . ?
N59 C60 C61 C62 -169.6(2) . . . . ?
C65 C60 C61 C69 -176.7(2) . . . . ?
N59 C60 C61 C69 11.4(3) . . . . ?
C60 C61 C62 C63 -0.4(4) . . . . ?
C69 C61 C62 C63 178.5(2) . . . . ?
C61 C62 C63 C64 -1.8(4) . . . . ?
C62 C63 C64 C65 2.2(4) . . . . ?
C61 C60 C65 C64 -1.8(3) . . . . ?
N59 C60 C65 C64 169.9(2) . . . . ?
C61 C60 C65 C66 -179.5(2) . . . . ?
N59 C60 C65 C66 -7.8(3) . . . . ?
C63 C64 C65 C60 -0.4(4) . . . . ?
C63 C64 C65 C66 177.3(2) . . . . ?
C60 C65 C66 C68 -129.5(2) . . . . ?
C64 C65 C66 C68 52.9(3) . . . . ?
C60 C65 C66 C67 105.7(3) . . . . ?
C64 C65 C66 C67 -71.9(3) . . . . ?
C62 C61 C69 C71 -88.9(3) . . . . ?
C60 C61 C69 C71 90.0(3) . . . . ?
C62 C61 C69 C70 35.1(3) . . . . ?
C60 C61 C69 C70 -145.9(2) . . . . ?
C3 C2 N1 C6 0.8(3) . . . . ?
C21 C2 N1 C6 179.80(17) . . . . ?
C3 C2 N1 Ni1 178.71(15) . . . . ?
C21 C2 N1 Ni1 -2.3(2) . . . . ?
C5 C6 N1 C2 -0.5(3) . . . . ?
C7 C6 N1 C2 178.37(17) . . . . ?
C5 C6 N1 Ni1 -178.45(15) . . . . ?
C7 C6 N1 Ni1 0.5(2) . . . . ?
O1 C7 N8 C9 -0.2(3) . . . . ?
C6 C7 N8 C9 -179.79(17) . . . . ?
O1 C7 N8 Ni1 176.85(18) . . . . ?
C6 C7 N8 Ni1 -2.7(2) . . . . ?
C10 C9 N8 C7 75.9(3) . . . . ?
C14 C9 N8 C7 -110.3(2) . . . . ?
C10 C9 N8 Ni1 -100.9(2) . . . . ?
C14 C9 N8 Ni1 72.9(2) . . . . ?
O2 C21 N22 C23 3.9(3) . . . . ?
C2 C21 N22 C23 -175.16(16) . . . . ?
O2 C21 N22 Ni1 177.97(18) . . . . ?
C2 C21 N22 Ni1 -1.1(2) . . . . ?
C24 C23 N22 C21 -98.6(2) . . . . ?
C28 C23 N22 C21 87.4(2) . . . . ?
C24 C23 N22 Ni1 87.7(2) . . . . ?
C28 C23 N22 Ni1 -86.3(2) . . . . ?
C42 C43 N38 C39 -0.5(3) . . . . ?
C44 C43 N38 C39 179.55(17) . . . . ?
C42 C43 N38 Ni2 176.32(14) . . . . ?
C44 C43 N38 Ni2 -3.6(2) . . . . ?
C40 C39 N38 C43 -0.3(3) . . . . ?
C58 C39 N38 C43 179.42(17) . . . . ?
C40 C39 N38 Ni2 -177.12(14) . . . . ?
C58 C39 N38 Ni2 2.6(2) . . . . ?
O3 C44 N45 C46 0.4(3) . . . . ?
C43 C44 N45 C46 -179.33(16) . . . . ?
O3 C44 N45 Ni2 178.25(18) . . . . ?
C43 C44 N45 Ni2 -1.4(2) . . . . ?
C47 C46 N45 C44 83.8(2) . . . . ?
C51 C46 N45 C44 -102.1(2) . . . . ?
C47 C46 N45 Ni2 -93.9(2) . . . . ?
C51 C46 N45 Ni2 80.2(2) . . . . ?
O4 C58 N59 C60 -2.9(3) . . . . ?
C39 C58 N59 C60 177.57(17) . . . . ?
O4 C58 N59 Ni2 179.28(18) . . . . ?
C39 C58 N59 Ni2 -0.3(2) . . . . ?
C65 C60 N59 C58 85.2(3) . . . . ?
C61 C60 N59 C58 -102.8(2) . . . . ?
C65 C60 N59 Ni2 -97.1(2) . . . . ?
C61 C60 N59 Ni2 74.9(2) . . . . ?
C2 N1 Ni1 N22 1.43(14) . . . . ?
C6 N1 Ni1 N22 179.42(15) . . . . ?
C2 N1 Ni1 N8 -179.56(15) . . . . ?
C6 N1 Ni1 N8 -1.57(14) . . . . ?
C21 N22 Ni1 N1 -0.07(14) . . . . ?
C23 N22 Ni1 N1 173.82(16) . . . . ?
C21 N22 Ni1 N35 177.49(14) . . . . ?
C23 N22 Ni1 N35 -8.62(16) . . . . ?
C21 N22 Ni1 N8 -4.2(4) . . . . ?
C23 N22 Ni1 N8 169.7(3) . . . . ?
C7 N8 Ni1 N1 2.48(14) . . . . ?
C9 N8 Ni1 N1 179.40(16) . . . . ?
C7 N8 Ni1 N35 -175.08(15) . . . . ?
C9 N8 Ni1 N35 1.84(16) . . . . ?
C7 N8 Ni1 N22 6.6(4) . . . . ?
C9 N8 Ni1 N22 -176.5(3) . . . . ?
C43 N38 Ni2 N59 -179.21(15) . . . . ?
C39 N38 Ni2 N59 -2.23(14) . . . . ?
C43 N38 Ni2 N45 2.33(14) . . . . ?
C39 N38 Ni2 N45 179.31(15) . . . . ?
C58 N59 Ni2 N38 1.30(14) . . . . ?
C60 N59 Ni2 N38 -176.50(16) . . . . ?
C58 N59 Ni2 N72 -175.26(15) . . . . ?
C60 N59 Ni2 N72 6.94(17) . . . . ?
C58 N59 Ni2 N45 8.0(4) . . . . ?
C60 N59 Ni2 N45 -169.8(3) . . . . ?
C44 N45 Ni2 N38 -0.30(14) . . . . ?
C46 N45 Ni2 N38 177.53(16) . . . . ?
C44 N45 Ni2 N72 176.26(14) . . . . ?
C46 N45 Ni2 N72 -5.90(16) . . . . ?
C44 N45 Ni2 N59 -7.0(4) . . . . ?
C46 N45 Ni2 N59 170.9(3) . . . . ?
C75 C76 O5 C77B -162.2(8) . . . . ?
C75 C76 O5 C77A 170.0(5) . . . . ?
C78B C77B O5 C76 34.8(16) . . . . ?
C78B C77B O5 C77A 97.4(18) . . . . ?
C78A C77A O5 C76 -136.2(6) . . . . ?
C78A C77A O5 C77B 93.4(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C37 H37C O5 0.98 2.41 3.375(4) 167 2_645
C74 H74A O1 0.98 2.22 2.960(3) 131 1_656

_refine_diff_density_max         0.750
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.057

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_tcd372
_database_code_depnum_ccdc_archive 'CCDC 1564846'
_audit_update_record             
;
2017-07-26 deposited with the CCDC.
2017-11-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C38 H41 Cl N3 Ni O4, C8 H20 N, C2 H3 N'
_chemical_formula_sum            'C48 H64 Cl N5 Ni O4'
_chemical_formula_weight         869.20

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'
Cl Cl 0.1484 0.1585 '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                   11.2143(4)
_cell_length_b                   13.9431(5)
_cell_length_c                   16.1500(6)
_cell_angle_alpha                110.6620(10)
_cell_angle_beta                 91.4110(10)
_cell_angle_gamma                106.7540(10)
_cell_volume                     2239.91(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9846
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      30.63

_exptl_crystal_description       fragment
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_F_000             928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.542
_shelx_estimated_absorpt_T_min   0.872
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6825
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
; 
SADABS-2014/5 (Bruker, 2014/5) was used for absorption correction.
wR2(int) was 0.0494 before and 0.0443 after correction.
The Ratio of minimum to maximum transmission is 0.925.
The λ/2 correction factor is 0.00150.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker PHOTON 50 QUEST ECO'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 5.12
_diffrn_reflns_number            49339
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.298
_diffrn_reflns_theta_max         30.633
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13768
_reflns_number_gt                11396
_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       'APEX2 Ver. 2015.9-0 (Bruker, 2015)'
_computing_cell_refinement       'SAINT+ Ver. 8.35A (Bruker, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.35A (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP (Bruker, 2015)'
_computing_publication_material  'XCIF (Bruker, 2015)'

_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)+(0.0414P)²+1.4301P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13768
_refine_ls_number_parameters     545
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0954
_refine_ls_wR_factor_gt          0.0881
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
N1 N 0.05677(10) 0.08335(9) 0.15203(7) 0.0114(2) Uani 1 1 d . . . . .
C2 C -0.00105(12) 0.14197(10) 0.12695(9) 0.0127(2) Uani 1 1 d . . . . .
C3 C -0.11821(13) 0.09230(11) 0.07469(9) 0.0155(2) Uani 1 1 d . . . . .
H3 H -0.1604 0.1333 0.0566 0.019 Uiso 1 1 calc R U . . .
C4 C -0.17273(13) -0.01930(11) 0.04927(9) 0.0160(2) Uani 1 1 d . . . . .
H4 H -0.2518 -0.0553 0.0121 0.019 Uiso 1 1 calc R U . . .
C5 C -0.11098(13) -0.07787(11) 0.07848(9) 0.0152(2) Uani 1 1 d . . . . .
H5 H -0.1481 -0.1535 0.0630 0.018 Uiso 1 1 calc R U . . .
C6 C 0.00573(12) -0.02323(10) 0.13063(9) 0.0126(2) Uani 1 1 d . . . . .
C7 C 0.08933(12) -0.06825(10) 0.16954(9) 0.0131(2) Uani 1 1 d . . . . .
O8 O 0.05293(10) -0.16374(8) 0.16297(7) 0.0191(2) Uani 1 1 d . . . . .
N9 N 0.19926(10) 0.00891(9) 0.21097(7) 0.0121(2) Uani 1 1 d . . . . .
C10 C 0.28799(12) -0.02072(10) 0.25361(9) 0.0125(2) Uani 1 1 d . . . . .
C11 C 0.36326(12) -0.07741(10) 0.20280(9) 0.0132(2) Uani 1 1 d . . . . .
C12 C 0.44066(13) -0.11328(11) 0.24586(9) 0.0172(3) Uani 1 1 d . . . . .
H12 H 0.4886 -0.1553 0.2118 0.021 Uiso 1 1 calc R U . . .
C13 C 0.44888(14) -0.08888(12) 0.33695(10) 0.0191(3) Uani 1 1 d . . . . .
H13 H 0.5003 -0.1156 0.3648 0.023 Uiso 1 1 calc R U . . .
C14 C 0.38188(14) -0.02531(11) 0.38745(9) 0.0176(3) Uani 1 1 d . . . . .
H14 H 0.3915 -0.0052 0.4505 0.021 Uiso 1 1 calc R U . . .
C15 C 0.30057(13) 0.00965(11) 0.34725(9) 0.0144(2) Uani 1 1 d . . . . .
C16 C 0.22707(14) 0.07913(11) 0.40251(9) 0.0172(3) Uani 1 1 d . . . . .
H16 H 0.2242 0.1331 0.3756 0.021 Uiso 1 1 calc R U . . .
C17 C 0.28777(16) 0.14200(13) 0.50049(10) 0.0242(3) Uani 1 1 d . . . . .
H17A H 0.2833 0.0912 0.5304 0.036 Uiso 1 1 calc R U . . .
H17B H 0.2427 0.1923 0.5307 0.036 Uiso 1 1 calc R U . . .
H17C H 0.3760 0.1826 0.5029 0.036 Uiso 1 1 calc R U . . .
C18 C 0.09146(16) 0.01111(14) 0.39883(12) 0.0293(4) Uani 1 1 d . . . . .
H18A H 0.0544 -0.0324 0.3364 0.044 Uiso 1 1 calc R U . . .
H18B H 0.0424 0.0589 0.4266 0.044 Uiso 1 1 calc R U . . .
H18C H 0.0907 -0.0367 0.4312 0.044 Uiso 1 1 calc R U . . .
C19 C 0.36379(13) -0.10040(11) 0.10358(9) 0.0156(2) Uani 1 1 d . . . . .
H19 H 0.3207 -0.0543 0.0879 0.019 Uiso 1 1 calc R U . . .
C20 C 0.49815(14) -0.07118(12) 0.08065(10) 0.0201(3) Uani 1 1 d . . . . .
H20A H 0.5425 0.0055 0.1150 0.030 Uiso 1 1 calc R U . . .
H20B H 0.4951 -0.0852 0.0166 0.030 Uiso 1 1 calc R U . . .
H20C H 0.5427 -0.1152 0.0956 0.030 Uiso 1 1 calc R U . . .
C21 C 0.29072(15) -0.21863(12) 0.04732(10) 0.0207(3) Uani 1 1 d . . . . .
H21A H 0.3284 -0.2658 0.0639 0.031 Uiso 1 1 calc R U . . .
H21B H 0.2941 -0.2316 -0.0162 0.031 Uiso 1 1 calc R U . . .
H21C H 0.2029 -0.2342 0.0582 0.031 Uiso 1 1 calc R U . . .
C22 C 0.07701(13) 0.25937(10) 0.16082(9) 0.0134(2) Uani 1 1 d . . . . .
O23 O 0.03276(10) 0.32731(8) 0.15114(7) 0.0193(2) Uani 1 1 d . . . . .
N24 N 0.19071(11) 0.27399(9) 0.20082(8) 0.0130(2) Uani 1 1 d . . . . .
C25 C 0.28000(12) 0.38055(10) 0.23547(9) 0.0134(2) Uani 1 1 d . . . . .
C26 C 0.35045(13) 0.42180(11) 0.17768(9) 0.0145(2) Uani 1 1 d . . . . .
C27 C 0.43607(13) 0.52609(11) 0.21350(10) 0.0179(3) Uani 1 1 d . . . . .
H27 H 0.4827 0.5556 0.1750 0.021 Uiso 1 1 calc R U . . .
C28 C 0.45441(14) 0.58754(11) 0.30420(10) 0.0198(3) Uani 1 1 d . . . . .
H28 H 0.5125 0.6587 0.3274 0.024 Uiso 1 1 calc R U . . .
C29 C 0.38747(15) 0.54463(12) 0.36089(10) 0.0201(3) Uani 1 1 d . . . . .
H29 H 0.4013 0.5865 0.4232 0.024 Uiso 1 1 calc R U . . .
C30 C 0.30012(14) 0.44105(11) 0.32798(9) 0.0167(3) Uani 1 1 d . . . . .
C31 C 0.22988(15) 0.39720(11) 0.39275(9) 0.0194(3) Uani 1 1 d . . . . .
H31 H 0.1799 0.3198 0.3586 0.023 Uiso 1 1 calc R U . . .
C32 C 0.32103(17) 0.40109(15) 0.46680(12) 0.0296(4) Uani 1 1 d . . . . .
H32A H 0.3806 0.3637 0.4400 0.044 Uiso 1 1 calc R U . . .
H32B H 0.2737 0.3655 0.5039 0.044 Uiso 1 1 calc R U . . .
H32C H 0.3672 0.4766 0.5039 0.044 Uiso 1 1 calc R U . . .
C33 C 0.13795(16) 0.45771(14) 0.43233(12) 0.0273(3) Uani 1 1 d . . . . .
H33A H 0.1844 0.5346 0.4644 0.041 Uiso 1 1 calc R U . . .
H33B H 0.0941 0.4279 0.4739 0.041 Uiso 1 1 calc R U . . .
H33C H 0.0764 0.4495 0.3841 0.041 Uiso 1 1 calc R U . . .
C34 C 0.33487(14) 0.35646(11) 0.07819(9) 0.0174(3) Uani 1 1 d . . . . .
H34 H 0.2864 0.2798 0.0678 0.021 Uiso 1 1 calc R U . . .
C35 C 0.46079(16) 0.35752(13) 0.04339(11) 0.0243(3) Uani 1 1 d . . . . .
H35A H 0.5099 0.4317 0.0518 0.036 Uiso 1 1 calc R U . . .
H35B H 0.4455 0.3119 -0.0204 0.036 Uiso 1 1 calc R U . . .
H35C H 0.5076 0.3297 0.0764 0.036 Uiso 1 1 calc R U . . .
C36 C 0.25831(16) 0.39623(14) 0.02540(11) 0.0254(3) Uani 1 1 d . . . . .
H36A H 0.1760 0.3910 0.0459 0.038 Uiso 1 1 calc R U . . .
H36B H 0.2467 0.3515 -0.0384 0.038 Uiso 1 1 calc R U . . .
H36C H 0.3032 0.4717 0.0349 0.038 Uiso 1 1 calc R U . . .
O37 O 0.37693(9) 0.21137(8) 0.27334(6) 0.01433(18) Uani 1 1 d . . . . .
C38 C 0.46709(13) 0.20380(10) 0.22612(9) 0.0147(2) Uani 1 1 d . . . . .
O39 O 0.46046(11) 0.18149(9) 0.14508(7) 0.0223(2) Uani 1 1 d . . . . .
C40 C 0.58952(13) 0.22249(11) 0.27973(9) 0.0143(2) Uani 1 1 d . . . . .
C41 C 0.58810(13) 0.21669(11) 0.36400(9) 0.0155(2) Uani 1 1 d . . . . .
H41 H 0.5117 0.2048 0.3887 0.019 Uiso 1 1 calc R U . . .
C42 C 0.69919(14) 0.22847(11) 0.41128(9) 0.0176(3) Uani 1 1 d . . . . .
C43 C 0.81284(14) 0.25019(12) 0.37867(11) 0.0215(3) Uani 1 1 d . . . . .
H43 H 0.8888 0.2606 0.4130 0.026 Uiso 1 1 calc R U . . .
C44 C 0.81356(14) 0.25642(13) 0.29464(11) 0.0218(3) Uani 1 1 d . . . . .
H44 H 0.8907 0.2715 0.2713 0.026 Uiso 1 1 calc R U . . .
C45 C 0.70220(14) 0.24073(12) 0.24468(10) 0.0186(3) Uani 1 1 d . . . . .
H45 H 0.7030 0.2424 0.1864 0.022 Uiso 1 1 calc R U . . .
N46 N 0.95358(11) 0.59723(9) 0.24675(8) 0.0161(2) Uani 1 1 d . . . . .
C47 C 0.86660(14) 0.50945(12) 0.27193(12) 0.0233(3) Uani 1 1 d . . . . .
H47A H 0.8701 0.4385 0.2309 0.028 Uiso 1 1 calc R U . . .
H47B H 0.8982 0.5193 0.3331 0.028 Uiso 1 1 calc R U . . .
C48 C 0.73063(16) 0.50703(15) 0.26890(15) 0.0357(4) Uani 1 1 d . . . . .
H48A H 0.7261 0.5779 0.3072 0.054 Uiso 1 1 calc R U . . .
H48B H 0.6823 0.4518 0.2902 0.054 Uiso 1 1 calc R U . . .
H48C H 0.6955 0.4898 0.2073 0.054 Uiso 1 1 calc R U . . .
C49 C 1.08437(13) 0.58710(11) 0.25527(10) 0.0179(3) Uani 1 1 d . . . . .
H49A H 1.1107 0.6012 0.3185 0.022 Uiso 1 1 calc R U . . .
H49B H 1.0797 0.5117 0.2195 0.022 Uiso 1 1 calc R U . . .
C50 C 1.18415(16) 0.66213(15) 0.22561(14) 0.0318(4) Uani 1 1 d . . . . .
H50A H 1.1647 0.6432 0.1612 0.048 Uiso 1 1 calc R U . . .
H50B H 1.2663 0.6550 0.2385 0.048 Uiso 1 1 calc R U . . .
H50C H 1.1862 0.7369 0.2578 0.048 Uiso 1 1 calc R U . . .
C51 C 0.95209(15) 0.70830(11) 0.30730(10) 0.0206(3) Uani 1 1 d . . . . .
H51A H 1.0163 0.7636 0.2930 0.025 Uiso 1 1 calc R U . . .
H51B H 0.8690 0.7153 0.2943 0.025 Uiso 1 1 calc R U . . .
C52 C 0.97714(17) 0.73138(15) 0.40609(11) 0.0297(4) Uani 1 1 d . . . . .
H52A H 0.9104 0.6805 0.4219 0.045 Uiso 1 1 calc R U . . .
H52B H 0.9789 0.8055 0.4407 0.045 Uiso 1 1 calc R U . . .
H52C H 1.0584 0.7231 0.4196 0.045 Uiso 1 1 calc R U . . .
C53 C 0.91114(16) 0.58519(12) 0.15302(10) 0.0237(3) Uani 1 1 d . . . . .
H53A H 0.8289 0.5980 0.1517 0.028 Uiso 1 1 calc R U . . .
H53B H 0.9723 0.6415 0.1379 0.028 Uiso 1 1 calc R U . . .
C54 C 0.8986(2) 0.47575(15) 0.08255(12) 0.0397(5) Uani 1 1 d . . . . .
H54A H 0.9779 0.4601 0.0860 0.060 Uiso 1 1 calc R U . . .
H54B H 0.8786 0.4760 0.0232 0.060 Uiso 1 1 calc R U . . .
H54C H 0.8310 0.4202 0.0928 0.060 Uiso 1 1 calc R U . . .
N55 N 0.70909(16) 0.77421(14) 0.23161(13) 0.0399(4) Uani 1 1 d . . . . .
C56 C 0.73646(16) 0.86583(15) 0.25571(12) 0.0289(3) Uani 1 1 d . . . . .
C57 C 0.76885(17) 0.98338(15) 0.28710(13) 0.0320(4) Uani 1 1 d . . . . .
H57A H 0.7189 1.0024 0.2484 0.048 Uiso 1 1 calc R U . . .
H57B H 0.8585 1.0150 0.2854 0.048 Uiso 1 1 calc R U . . .
H57C H 0.7509 1.0116 0.3486 0.048 Uiso 1 1 calc R U . . .
Cl1 Cl 0.69304(4) 0.21267(3) 0.51369(3) 0.02721(9) Uani 1 1 d . . . . .
Ni1 Ni 0.21552(2) 0.14894(2) 0.21116(2) 0.01101(5) 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
N1 C2 1.3338(16) . ?
N1 C6 1.3390(16) . ?
N1 Ni1 1.8108(11) . ?
C2 C3 1.3880(18) . ?
C2 C22 1.5045(18) . ?
C3 C4 1.3971(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.3967(19) . ?
C4 H4 0.9500 . ?
C5 C6 1.3859(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.5021(18) . ?
C7 O8 1.2391(16) . ?
C7 N9 1.3460(17) . ?
N9 C10 1.4280(16) . ?
N9 Ni1 1.9068(11) . ?
C10 C11 1.4042(18) . ?
C10 C15 1.4103(18) . ?
C11 C12 1.3975(18) . ?
C11 C19 1.5197(18) . ?
C12 C13 1.382(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.3932(19) . ?
C14 H14 0.9500 . ?
C15 C16 1.5169(19) . ?
C16 C18 1.530(2) . ?
C16 C17 1.536(2) . ?
C16 H16 1.0000 . ?
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 C21 1.530(2) . ?
C19 C20 1.534(2) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 O23 1.2408(16) . ?
C22 N24 1.3421(17) . ?
N24 C25 1.4323(16) . ?
N24 Ni1 1.9048(11) . ?
C25 C30 1.4067(19) . ?
C25 C26 1.4068(19) . ?
C26 C27 1.3947(19) . ?
C26 C34 1.5178(19) . ?
C27 C28 1.386(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.386(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.3946(19) . ?
C29 H29 0.9500 . ?
C30 C31 1.518(2) . ?
C31 C33 1.529(2) . ?
C31 C32 1.530(2) . ?
C31 H31 1.0000 . ?
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 C35 1.531(2) . ?
C34 C36 1.531(2) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O37 C38 1.2874(17) . ?
O37 Ni1 1.8514(10) . ?
C38 O39 1.2288(17) . ?
C38 C40 1.5095(19) . ?
C40 C45 1.3906(19) . ?
C40 C41 1.3917(19) . ?
C41 C42 1.3816(19) . ?
C41 H41 0.9500 . ?
C42 C43 1.384(2) . ?
C42 Cl1 1.7444(15) . ?
C43 C44 1.390(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.388(2) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
N46 C53 1.5117(18) . ?
N46 C47 1.5156(19) . ?
N46 C51 1.5171(18) . ?
N46 C49 1.5211(18) . ?
C47 C48 1.515(2) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.510(2) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.514(2) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.512(2) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
N55 C56 1.138(2) . ?
C56 C57 1.462(3) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 N1 C6 122.91(12) . . ?
C2 N1 Ni1 118.54(9) . . ?
C6 N1 Ni1 118.42(9) . . ?
N1 C2 C3 120.00(12) . . ?
N1 C2 C22 111.71(11) . . ?
C3 C2 C22 128.28(12) . . ?
C2 C3 C4 118.54(12) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 119.98(12) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 118.51(12) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
N1 C6 C5 120.02(12) . . ?
N1 C6 C7 111.79(11) . . ?
C5 C6 C7 128.19(12) . . ?
O8 C7 N9 128.68(12) . . ?
O8 C7 C6 120.79(12) . . ?
N9 C7 C6 110.51(11) . . ?
C7 N9 C10 117.25(11) . . ?
C7 N9 Ni1 115.67(9) . . ?
C10 N9 Ni1 126.99(9) . . ?
C11 C10 C15 120.72(12) . . ?
C11 C10 N9 120.14(11) . . ?
C15 C10 N9 119.13(12) . . ?
C12 C11 C10 118.26(12) . . ?
C12 C11 C19 119.24(12) . . ?
C10 C11 C19 122.50(11) . . ?
C13 C12 C11 121.32(13) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 119.73(13) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C15 121.04(13) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C14 C15 C10 118.57(12) . . ?
C14 C15 C16 121.05(12) . . ?
C10 C15 C16 120.38(12) . . ?
C15 C16 C18 111.02(12) . . ?
C15 C16 C17 113.22(12) . . ?
C18 C16 C17 109.43(13) . . ?
C15 C16 H16 107.6 . . ?
C18 C16 H16 107.6 . . ?
C17 C16 H16 107.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C19 C21 111.16(11) . . ?
C11 C19 C20 111.60(11) . . ?
C21 C19 C20 110.35(12) . . ?
C11 C19 H19 107.9 . . ?
C21 C19 H19 107.9 . . ?
C20 C19 H19 107.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O23 C22 N24 129.16(13) . . ?
O23 C22 C2 120.35(12) . . ?
N24 C22 C2 110.48(11) . . ?
C22 N24 C25 118.71(11) . . ?
C22 N24 Ni1 115.68(9) . . ?
C25 N24 Ni1 125.54(9) . . ?
C30 C25 C26 120.68(12) . . ?
C30 C25 N24 119.27(12) . . ?
C26 C25 N24 119.98(12) . . ?
C27 C26 C25 118.52(13) . . ?
C27 C26 C34 119.61(12) . . ?
C25 C26 C34 121.87(12) . . ?
C28 C27 C26 121.28(13) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C27 C28 C29 119.64(13) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C28 C29 C30 121.09(13) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C29 C30 C25 118.72(13) . . ?
C29 C30 C31 119.17(13) . . ?
C25 C30 C31 122.12(12) . . ?
C30 C31 C33 111.23(12) . . ?
C30 C31 C32 111.21(13) . . ?
C33 C31 C32 110.79(13) . . ?
C30 C31 H31 107.8 . . ?
C33 C31 H31 107.8 . . ?
C32 C31 H31 107.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C34 C35 112.68(12) . . ?
C26 C34 C36 110.65(12) . . ?
C35 C34 C36 110.35(12) . . ?
C26 C34 H34 107.6 . . ?
C35 C34 H34 107.6 . . ?
C36 C34 H34 107.6 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 O37 Ni1 116.25(9) . . ?
O39 C38 O37 126.59(13) . . ?
O39 C38 C40 119.96(13) . . ?
O37 C38 C40 113.43(11) . . ?
C45 C40 C41 119.79(13) . . ?
C45 C40 C38 121.03(12) . . ?
C41 C40 C38 119.12(12) . . ?
C42 C41 C40 119.17(13) . . ?
C42 C41 H41 120.4 . . ?
C40 C41 H41 120.4 . . ?
C41 C42 C43 121.79(13) . . ?
C41 C42 Cl1 118.15(11) . . ?
C43 C42 Cl1 120.05(11) . . ?
C42 C43 C44 118.64(13) . . ?
C42 C43 H43 120.7 . . ?
C44 C43 H43 120.7 . . ?
C45 C44 C43 120.39(14) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C40 120.14(13) . . ?
C44 C45 H45 119.9 . . ?
C40 C45 H45 119.9 . . ?
C53 N46 C47 111.03(12) . . ?
C53 N46 C51 105.81(11) . . ?
C47 N46 C51 111.11(12) . . ?
C53 N46 C49 111.48(12) . . ?
C47 N46 C49 106.52(10) . . ?
C51 N46 C49 110.97(11) . . ?
C48 C47 N46 114.69(13) . . ?
C48 C47 H47A 108.6 . . ?
N46 C47 H47A 108.6 . . ?
C48 C47 H47B 108.6 . . ?
N46 C47 H47B 108.6 . . ?
H47A C47 H47B 107.6 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 N46 114.96(12) . . ?
C50 C49 H49A 108.5 . . ?
N46 C49 H49A 108.5 . . ?
C50 C49 H49B 108.5 . . ?
N46 C49 H49B 108.5 . . ?
H49A C49 H49B 107.5 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 N46 114.19(12) . . ?
C52 C51 H51A 108.7 . . ?
N46 C51 H51A 108.7 . . ?
C52 C51 H51B 108.7 . . ?
N46 C51 H51B 108.7 . . ?
H51A C51 H51B 107.6 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 N46 113.98(12) . . ?
C54 C53 H53A 108.8 . . ?
N46 C53 H53A 108.8 . . ?
C54 C53 H53B 108.8 . . ?
N46 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N55 C56 C57 178.8(2) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N1 Ni1 O37 177.61(5) . . ?
N1 Ni1 N24 83.32(5) . . ?
O37 Ni1 N24 98.91(5) . . ?
N1 Ni1 N9 83.35(5) . . ?
O37 Ni1 N9 94.40(4) . . ?
N24 Ni1 N9 166.51(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N1 C2 C3 -1.5(2) . . . . ?
Ni1 N1 C2 C3 174.27(10) . . . . ?
C6 N1 C2 C22 179.49(12) . . . . ?
Ni1 N1 C2 C22 -4.79(15) . . . . ?
N1 C2 C3 C4 -0.2(2) . . . . ?
C22 C2 C3 C4 178.67(13) . . . . ?
C2 C3 C4 C5 1.8(2) . . . . ?
C3 C4 C5 C6 -1.7(2) . . . . ?
C2 N1 C6 C5 1.5(2) . . . . ?
Ni1 N1 C6 C5 -174.20(10) . . . . ?
C2 N1 C6 C7 -178.40(12) . . . . ?
Ni1 N1 C6 C7 5.87(15) . . . . ?
C4 C5 C6 N1 0.1(2) . . . . ?
C4 C5 C6 C7 180.00(13) . . . . ?
N1 C6 C7 O8 173.95(12) . . . . ?
C5 C6 C7 O8 -6.0(2) . . . . ?
N1 C6 C7 N9 -4.50(16) . . . . ?
C5 C6 C7 N9 175.58(13) . . . . ?
O8 C7 N9 C10 0.1(2) . . . . ?
C6 C7 N9 C10 178.39(11) . . . . ?
O8 C7 N9 Ni1 -176.83(12) . . . . ?
C6 C7 N9 Ni1 1.47(14) . . . . ?
C7 N9 C10 C11 79.49(16) . . . . ?
Ni1 N9 C10 C11 -103.98(13) . . . . ?
C7 N9 C10 C15 -101.81(14) . . . . ?
Ni1 N9 C10 C15 74.72(15) . . . . ?
C15 C10 C11 C12 6.96(19) . . . . ?
N9 C10 C11 C12 -174.36(12) . . . . ?
C15 C10 C11 C19 -172.75(12) . . . . ?
N9 C10 C11 C19 5.93(19) . . . . ?
C10 C11 C12 C13 -3.5(2) . . . . ?
C19 C11 C12 C13 176.19(13) . . . . ?
C11 C12 C13 C14 -1.7(2) . . . . ?
C12 C13 C14 C15 3.6(2) . . . . ?
C13 C14 C15 C10 -0.2(2) . . . . ?
C13 C14 C15 C16 179.92(13) . . . . ?
C11 C10 C15 C14 -5.1(2) . . . . ?
N9 C10 C15 C14 176.17(12) . . . . ?
C11 C10 C15 C16 174.71(12) . . . . ?
N9 C10 C15 C16 -3.98(19) . . . . ?
C14 C15 C16 C18 -100.15(16) . . . . ?
C10 C15 C16 C18 80.01(16) . . . . ?
C14 C15 C16 C17 23.40(19) . . . . ?
C10 C15 C16 C17 -156.44(13) . . . . ?
C12 C11 C19 C21 75.69(16) . . . . ?
C10 C11 C19 C21 -104.60(14) . . . . ?
C12 C11 C19 C20 -47.98(17) . . . . ?
C10 C11 C19 C20 131.74(13) . . . . ?
N1 C2 C22 O23 -173.04(12) . . . . ?
C3 C2 C22 O23 8.0(2) . . . . ?
N1 C2 C22 N24 5.80(16) . . . . ?
C3 C2 C22 N24 -173.16(13) . . . . ?
O23 C22 N24 C25 -2.9(2) . . . . ?
C2 C22 N24 C25 178.39(11) . . . . ?
O23 C22 N24 Ni1 174.24(12) . . . . ?
C2 C22 N24 Ni1 -4.47(14) . . . . ?
C22 N24 C25 C30 102.30(15) . . . . ?
Ni1 N24 C25 C30 -74.53(15) . . . . ?
C22 N24 C25 C26 -80.49(16) . . . . ?
Ni1 N24 C25 C26 102.67(13) . . . . ?
C30 C25 C26 C27 -3.20(19) . . . . ?
N24 C25 C26 C27 179.64(12) . . . . ?
C30 C25 C26 C34 177.28(12) . . . . ?
N24 C25 C26 C34 0.11(19) . . . . ?
C25 C26 C27 C28 1.5(2) . . . . ?
C34 C26 C27 C28 -178.92(13) . . . . ?
C26 C27 C28 C29 0.6(2) . . . . ?
C27 C28 C29 C30 -1.1(2) . . . . ?
C28 C29 C30 C25 -0.5(2) . . . . ?
C28 C29 C30 C31 179.51(14) . . . . ?
C26 C25 C30 C29 2.7(2) . . . . ?
N24 C25 C30 C29 179.89(13) . . . . ?
C26 C25 C30 C31 -177.33(13) . . . . ?
N24 C25 C30 C31 -0.1(2) . . . . ?
C29 C30 C31 C33 68.72(18) . . . . ?
C25 C30 C31 C33 -111.25(15) . . . . ?
C29 C30 C31 C32 -55.29(18) . . . . ?
C25 C30 C31 C32 124.74(15) . . . . ?
C27 C26 C34 C35 48.20(17) . . . . ?
C25 C26 C34 C35 -132.28(14) . . . . ?
C27 C26 C34 C36 -75.88(17) . . . . ?
C25 C26 C34 C36 103.65(15) . . . . ?
Ni1 O37 C38 O39 17.06(18) . . . . ?
Ni1 O37 C38 C40 -161.32(8) . . . . ?
O39 C38 C40 C45 15.6(2) . . . . ?
O37 C38 C40 C45 -165.88(12) . . . . ?
O39 C38 C40 C41 -161.64(13) . . . . ?
O37 C38 C40 C41 16.87(17) . . . . ?
C45 C40 C41 C42 -0.5(2) . . . . ?
C38 C40 C41 C42 176.82(12) . . . . ?
C40 C41 C42 C43 2.6(2) . . . . ?
C40 C41 C42 Cl1 -176.17(10) . . . . ?
C41 C42 C43 C44 -2.3(2) . . . . ?
Cl1 C42 C43 C44 176.50(12) . . . . ?
C42 C43 C44 C45 -0.2(2) . . . . ?
C43 C44 C45 C40 2.3(2) . . . . ?
C41 C40 C45 C44 -2.0(2) . . . . ?
C38 C40 C45 C44 -179.21(13) . . . . ?
C53 N46 C47 C48 -59.28(18) . . . . ?
C51 N46 C47 C48 58.19(18) . . . . ?
C49 N46 C47 C48 179.16(14) . . . . ?
C53 N46 C49 C50 53.92(17) . . . . ?
C47 N46 C49 C50 175.19(14) . . . . ?
C51 N46 C49 C50 -63.74(17) . . . . ?
C53 N46 C51 C52 173.15(14) . . . . ?
C47 N46 C51 C52 52.54(17) . . . . ?
C49 N46 C51 C52 -65.78(16) . . . . ?
C47 N46 C53 C54 -55.76(19) . . . . ?
C51 N46 C53 C54 -176.42(16) . . . . ?
C49 N46 C53 C54 62.84(19) . . . . ?
C2 N1 Ni1 N24 1.97(10) . . . . ?
C6 N1 Ni1 N24 177.89(11) . . . . ?
C2 N1 Ni1 N9 179.94(10) . . . . ?
C6 N1 Ni1 N9 -4.14(10) . . . . ?
C38 O37 Ni1 N24 -95.94(10) . . . . ?
C38 O37 Ni1 N9 86.29(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C49 H49B O23 0.99 2.30 3.2754(17) 168 1_655
C51 H51B N55 0.99 2.50 3.441(2) 158 .
C52 H52C Cl1 0.98 2.73 3.6544(19) 157 2_766
C53 H53B O8 0.99 2.48 3.3452(18) 146 1_665

_refine_diff_density_max         0.551
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.063

