# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1038668'
_audit_update_record             
;
2014-12-10 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H40 N2 Ni, 2(C4 H8 O)'
_chemical_formula_sum            'C46 H56 N2 Ni O2'
_chemical_formula_weight         727.63

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'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

_cell_length_a                   9.0713(2)
_cell_length_b                   24.610(2)
_cell_length_c                   16.8975(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3772.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    3057
_cell_measurement_theta_min      2.919
_cell_measurement_theta_max      29.448

_exptl_crystal_description       needle
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.043
_exptl_absorpt_coefficient_mu    0.555
_shelx_estimated_absorpt_T_min   0.803
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;

CrysAlisPro, Agilent Technologies,
 
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
 
(compiled Jul 11 2012,15:38:31)
 
Empirical absorption correction using spherical harmonics,
 
implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_reflns_number            14432
_diffrn_reflns_av_unetI/netI     0.1078
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.925
_diffrn_reflns_theta_max         29.513
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.786
_diffrn_reflns_point_group_measured_fraction_full 0.927
_reflns_number_total             8281
_reflns_number_gt                6023
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_max     0.665
_reflns_Friedel_fraction_full    0.851

_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       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_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)+(0.0791P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8281
_refine_ls_number_parameters     466
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0756
_refine_ls_wR_factor_ref         0.1803
_refine_ls_wR_factor_gt          0.1611
_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
Ni1 Ni 0.95694(7) 0.25601(3) 0.04204(6) 0.0216(2) Uani 1 1 d . . . . .
N1 N 0.9455(5) 0.2813(2) 0.3296(3) 0.0191(11) Uani 1 1 d . . . . .
N2 N 0.9404(5) 0.1956(2) 0.3613(3) 0.0203(11) Uani 1 1 d . . . . .
C1 C 1.1825(6) 0.2276(3) 0.0490(5) 0.0266(14) Uani 1 1 d . . . . .
H1 H 1.2250 0.2104 0.0938 0.032 Uiso 1 1 calc R U . . .
C2 C 1.1081(7) 0.2008(3) -0.0136(4) 0.0289(16) Uani 1 1 d . . . . .
H2 H 1.0895 0.1629 -0.0170 0.035 Uiso 1 1 calc R U . . .
C3 C 1.0665(7) 0.2401(3) -0.0698(4) 0.0294(16) Uani 1 1 d . . . . .
H3 H 1.0192 0.2331 -0.1189 0.035 Uiso 1 1 calc R U . . .
C4 C 1.1070(6) 0.2915(3) -0.0407(4) 0.0253(15) Uani 1 1 d . . . . .
H4 H 1.0878 0.3253 -0.0656 0.030 Uiso 1 1 calc R U . . .
C5 C 1.1832(6) 0.2838(3) 0.0337(4) 0.0265(14) Uani 1 1 d . . . . .
H5 H 1.2254 0.3113 0.0660 0.032 Uiso 1 1 calc R U . . .
C6 C 0.8318(6) 0.2135(3) 0.1058(4) 0.0218(14) Uani 1 1 d . . . . .
C7 C 0.8525(7) 0.1601(3) 0.1321(4) 0.0238(14) Uani 1 1 d . . . . .
H7 H 0.9385 0.1412 0.1156 0.029 Uiso 1 1 calc R U . . .
C8 C 0.7526(7) 0.1334(3) 0.1814(4) 0.0247(15) Uani 1 1 d . . . . .
H8 H 0.7704 0.0970 0.1976 0.030 Uiso 1 1 calc R U . . .
C9 C 0.6253(7) 0.1610(3) 0.2068(4) 0.0287(15) Uani 1 1 d . . . . .
H9 H 0.5576 0.1438 0.2416 0.034 Uiso 1 1 calc R U . . .
C10 C 0.5999(6) 0.2128(3) 0.1810(4) 0.0235(14) Uani 1 1 d . . . . .
H10 H 0.5126 0.2310 0.1972 0.028 Uiso 1 1 calc R U . . .
C11 C 0.6998(7) 0.2400(3) 0.1309(4) 0.0229(14) Uani 1 1 d . . . . .
C12 C 0.6867(6) 0.2948(3) 0.0998(4) 0.0202(13) Uani 1 1 d . . . . .
C13 C 0.5676(7) 0.3294(3) 0.1100(4) 0.0251(15) Uani 1 1 d . . . . .
H13 H 0.4849 0.3176 0.1398 0.030 Uiso 1 1 calc R U . . .
C14 C 0.5674(7) 0.3810(3) 0.0774(4) 0.0278(15) Uani 1 1 d . . . . .
H14 H 0.4851 0.4044 0.0840 0.033 Uiso 1 1 calc R U . . .
C15 C 0.6909(6) 0.3980(3) 0.0344(4) 0.0287(14) Uani 1 1 d . . . . .
H15 H 0.6931 0.4334 0.0119 0.034 Uiso 1 1 calc R U . . .
C16 C 0.8107(6) 0.3632(3) 0.0244(3) 0.0239(14) Uani 1 1 d . . . . .
H16 H 0.8941 0.3758 -0.0043 0.029 Uiso 1 1 calc R U . . .
C17 C 0.8125(6) 0.3108(3) 0.0550(4) 0.0212(13) Uani 1 1 d . . . . .
C18 C 0.9258(6) 0.2322(3) 0.3061(4) 0.0213(14) Uani 1 1 d . . . . .
H18 H 0.9025 0.2233 0.2529 0.026 Uiso 1 1 calc R U . . .
C19 C 0.9782(8) 0.2225(3) 0.4374(4) 0.0301(16) Uani 1 1 d . . . . .
H19A H 1.0763 0.2107 0.4566 0.036 Uiso 1 1 calc R U . . .
H19B H 0.9036 0.2145 0.4785 0.036 Uiso 1 1 calc R U . . .
C20 C 0.9784(7) 0.2831(3) 0.4156(4) 0.0246(14) Uani 1 1 d . . . . .
H20A H 0.9015 0.3033 0.4450 0.029 Uiso 1 1 calc R U . . .
H20B H 1.0756 0.3000 0.4259 0.029 Uiso 1 1 calc R U . . .
C21 C 0.9476(6) 0.1381(3) 0.3488(4) 0.0204(13) Uani 1 1 d . U . . .
C22 C 1.0652(7) 0.1165(3) 0.3033(4) 0.0241(14) Uani 1 1 d . . . . .
C23 C 1.0691(6) 0.0617(3) 0.2903(4) 0.0243(15) Uani 1 1 d . . . . .
H23 H 1.1473 0.0473 0.2593 0.029 Uiso 1 1 calc R U . . .
C24 C 0.9635(6) 0.0260(3) 0.3203(4) 0.0232(14) Uani 1 1 d . . . . .
C25 C 0.8504(7) 0.0487(3) 0.3668(4) 0.0253(14) Uani 1 1 d . . . . .
H25 H 0.7787 0.0253 0.3894 0.030 Uiso 1 1 calc R U . . .
C26 C 0.8400(6) 0.1031(3) 0.3807(4) 0.0238(14) Uani 1 1 d . . . . .
C27 C 1.1834(7) 0.1535(3) 0.2714(4) 0.0288(15) Uani 1 1 d . . . . .
H27A H 1.2662 0.1315 0.2521 0.043 Uiso 1 1 calc R U . . .
H27B H 1.2177 0.1777 0.3135 0.043 Uiso 1 1 calc R U . . .
H27C H 1.1433 0.1751 0.2277 0.043 Uiso 1 1 calc R U . . .
C28 C 0.9677(7) -0.0336(3) 0.3028(4) 0.0272(15) Uani 1 1 d . . . . .
H28A H 0.9204 -0.0536 0.3461 0.041 Uiso 1 1 calc R U . . .
H28B H 1.0704 -0.0455 0.2977 0.041 Uiso 1 1 calc R U . . .
H28C H 0.9150 -0.0408 0.2533 0.041 Uiso 1 1 calc R U . . .
C29 C 0.7153(7) 0.1266(3) 0.4296(5) 0.0339(18) Uani 1 1 d . . . . .
H29A H 0.6357 0.0998 0.4339 0.051 Uiso 1 1 calc R U . . .
H29B H 0.6778 0.1595 0.4041 0.051 Uiso 1 1 calc R U . . .
H29C H 0.7517 0.1355 0.4827 0.051 Uiso 1 1 calc R U . . .
C30 C 0.9462(7) 0.3299(3) 0.2807(4) 0.0220(13) Uani 1 1 d . . . . .
C31 C 0.8155(7) 0.3599(3) 0.2740(4) 0.0239(15) Uani 1 1 d . . . . .
C32 C 0.8213(7) 0.4069(3) 0.2291(4) 0.0273(15) Uani 1 1 d . . . . .
H32 H 0.7336 0.4276 0.2226 0.033 Uiso 1 1 calc R U . . .
C33 C 0.9494(7) 0.4253(3) 0.1932(4) 0.0271(15) Uani 1 1 d . . . . .
C34 C 1.0746(7) 0.3932(3) 0.2014(4) 0.0276(15) Uani 1 1 d . . . . .
H34 H 1.1625 0.4046 0.1757 0.033 Uiso 1 1 calc R U . . .
C35 C 1.0779(7) 0.3456(3) 0.2449(4) 0.0257(15) Uani 1 1 d . . . . .
C36 C 0.6730(7) 0.3414(3) 0.3112(4) 0.0276(16) Uani 1 1 d . . . . .
H36A H 0.6439 0.3064 0.2885 0.041 Uiso 1 1 calc R U . . .
H36B H 0.5958 0.3684 0.3009 0.041 Uiso 1 1 calc R U . . .
H36C H 0.6866 0.3374 0.3685 0.041 Uiso 1 1 calc R U . . .
C37 C 0.9536(8) 0.4764(3) 0.1450(5) 0.0384(18) Uani 1 1 d . . . . .
H37A H 0.9516 0.4671 0.0886 0.058 Uiso 1 1 calc R U . . .
H37B H 1.0441 0.4965 0.1570 0.058 Uiso 1 1 calc R U . . .
H37C H 0.8678 0.4989 0.1579 0.058 Uiso 1 1 calc R U . . .
C38 C 1.2147(6) 0.3110(3) 0.2515(4) 0.0302(16) Uani 1 1 d . . . . .
H38A H 1.2295 0.3004 0.3069 0.045 Uiso 1 1 calc R U . . .
H38B H 1.3002 0.3317 0.2330 0.045 Uiso 1 1 calc R U . . .
H38C H 1.2030 0.2783 0.2190 0.045 Uiso 1 1 calc R U . . .
O1 O 1.2670(5) 0.0288(2) 0.1279(3) 0.0319(11) Uani 1 1 d . . . . .
C39 C 1.2355(7) 0.0717(3) 0.0752(4) 0.0349(17) Uani 1 1 d . . . . .
H39A H 1.1855 0.1018 0.1034 0.042 Uiso 1 1 calc R U . . .
H39B H 1.1705 0.0590 0.0319 0.042 Uiso 1 1 calc R U . . .
C40 C 1.3821(7) 0.0905(3) 0.0424(6) 0.0434(18) Uani 1 1 d . . . . .
H40A H 1.4158 0.1240 0.0694 0.052 Uiso 1 1 calc R U . . .
H40B H 1.3751 0.0977 -0.0151 0.052 Uiso 1 1 calc R U . . .
C41 C 1.4863(8) 0.0435(4) 0.0590(6) 0.053(3) Uani 1 1 d . . . . .
H41A H 1.5339 0.0309 0.0096 0.064 Uiso 1 1 calc R U . . .
H41B H 1.5638 0.0544 0.0971 0.064 Uiso 1 1 calc R U . . .
C42 C 1.3903(7) -0.0003(3) 0.0935(4) 0.0325(16) Uani 1 1 d . . . . .
H42A H 1.3564 -0.0257 0.0519 0.039 Uiso 1 1 calc R U . . .
H42B H 1.4442 -0.0211 0.1345 0.039 Uiso 1 1 calc R U . . .
O2 O 1.1087(6) 0.4334(3) -0.0740(4) 0.0572(18) Uani 1 1 d . . . . .
C43 C 1.2395(9) 0.4342(4) -0.0257(6) 0.052(2) Uani 1 1 d . . . . .
H43A H 1.2610 0.3974 -0.0050 0.062 Uiso 1 1 calc R U . . .
H43B H 1.2269 0.4593 0.0195 0.062 Uiso 1 1 calc R U . . .
C44 C 1.3647(8) 0.4537(4) -0.0797(5) 0.044(2) Uani 1 1 d . . . . .
H44A H 1.4321 0.4786 -0.0513 0.052 Uiso 1 1 calc R U . . .
H44B H 1.4220 0.4227 -0.1008 0.052 Uiso 1 1 calc R U . . .
C45 C 1.2824(7) 0.4830(3) -0.1450(4) 0.0342(17) Uani 1 1 d . . . . .
H45A H 1.2602 0.5210 -0.1300 0.041 Uiso 1 1 calc R U . . .
H45B H 1.3392 0.4828 -0.1951 0.041 Uiso 1 1 calc R U . . .
C46 C 1.1435(8) 0.4497(4) -0.1521(5) 0.043(2) Uani 1 1 d . . . . .
H46A H 1.0626 0.4717 -0.1750 0.052 Uiso 1 1 calc R U . . .
H46B H 1.1601 0.4176 -0.1863 0.052 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C6 1.882(6) . ?
Ni1 C17 1.893(6) . ?
Ni1 C4 2.138(6) . ?
Ni1 C2 2.147(7) . ?
Ni1 C1 2.165(5) . ?
Ni1 C5 2.168(5) . ?
Ni1 C3 2.171(7) . ?
N1 C18 1.285(9) . ?
N1 C30 1.452(8) . ?
N1 C20 1.484(8) . ?
N2 C18 1.302(8) . ?
N2 C21 1.432(8) . ?
N2 C19 1.486(8) . ?
C1 C5 1.406(9) . ?
C1 C2 1.417(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.406(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.405(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.448(9) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.400(9) . ?
C6 C11 1.428(8) . ?
C7 C8 1.396(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.408(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.366(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.408(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.452(9) . ?
C12 C13 1.387(8) . ?
C12 C17 1.426(8) . ?
C13 C14 1.383(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.393(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.390(9) . ?
C16 H16 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.538(11) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C26 1.409(9) . ?
C21 C22 1.417(8) . ?
C22 C23 1.368(10) . ?
C22 C27 1.506(9) . ?
C23 C24 1.396(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.408(9) . ?
C24 C28 1.497(10) . ?
C25 C26 1.361(10) . ?
C25 H25 0.9500 . ?
C26 C29 1.516(9) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C35 1.394(9) . ?
C30 C31 1.402(8) . ?
C31 C32 1.384(10) . ?
C31 C36 1.508(8) . ?
C32 C33 1.387(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.390(9) . ?
C33 C37 1.498(10) . ?
C34 C35 1.384(10) . ?
C34 H34 0.9500 . ?
C35 C38 1.509(9) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O1 C39 1.410(8) . ?
O1 C42 1.450(8) . ?
C39 C40 1.514(9) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.520(10) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.503(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
O2 C46 1.414(10) . ?
O2 C43 1.440(10) . ?
C43 C44 1.533(11) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.515(10) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.509(10) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?

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
C6 Ni1 C17 85.0(3) . . ?
C6 Ni1 C4 170.1(3) . . ?
C17 Ni1 C4 103.1(3) . . ?
C6 Ni1 C2 106.5(3) . . ?
C17 Ni1 C2 160.6(3) . . ?
C4 Ni1 C2 64.2(3) . . ?
C6 Ni1 C1 111.1(3) . . ?
C17 Ni1 C1 151.4(3) . . ?
C4 Ni1 C1 64.2(3) . . ?
C2 Ni1 C1 38.4(3) . . ?
C6 Ni1 C5 141.6(3) . . ?
C17 Ni1 C5 116.0(2) . . ?
C4 Ni1 C5 39.3(3) . . ?
C2 Ni1 C5 64.3(3) . . ?
C1 Ni1 C5 37.9(2) . . ?
C6 Ni1 C3 132.4(3) . . ?
C17 Ni1 C3 123.1(3) . . ?
C4 Ni1 C3 38.0(3) . . ?
C2 Ni1 C3 38.0(3) . . ?
C1 Ni1 C3 63.6(3) . . ?
C5 Ni1 C3 64.3(3) . . ?
C18 N1 C30 126.8(6) . . ?
C18 N1 C20 111.0(5) . . ?
C30 N1 C20 122.1(5) . . ?
C18 N2 C21 125.6(5) . . ?
C18 N2 C19 109.6(5) . . ?
C21 N2 C19 123.8(5) . . ?
C5 C1 C2 108.9(6) . . ?
C5 C1 Ni1 71.2(3) . . ?
C2 C1 Ni1 70.1(3) . . ?
C5 C1 H1 125.6 . . ?
C2 C1 H1 125.6 . . ?
Ni1 C1 H1 124.8 . . ?
C3 C2 C1 108.1(6) . . ?
C3 C2 Ni1 71.9(4) . . ?
C1 C2 Ni1 71.5(4) . . ?
C3 C2 H2 125.9 . . ?
C1 C2 H2 125.9 . . ?
Ni1 C2 H2 122.3 . . ?
C4 C3 C2 108.2(6) . . ?
C4 C3 Ni1 69.7(4) . . ?
C2 C3 Ni1 70.1(4) . . ?
C4 C3 H3 125.9 . . ?
C2 C3 H3 125.9 . . ?
Ni1 C3 H3 125.9 . . ?
C3 C4 C5 108.2(6) . . ?
C3 C4 Ni1 72.2(4) . . ?
C5 C4 Ni1 71.5(3) . . ?
C3 C4 H4 125.9 . . ?
C5 C4 H4 125.9 . . ?
Ni1 C4 H4 122.0 . . ?
C1 C5 C4 106.5(6) . . ?
C1 C5 Ni1 71.0(3) . . ?
C4 C5 Ni1 69.2(3) . . ?
C1 C5 H5 126.7 . . ?
C4 C5 H5 126.7 . . ?
Ni1 C5 H5 124.7 . . ?
C7 C6 C11 116.5(6) . . ?
C7 C6 Ni1 128.5(5) . . ?
C11 C6 Ni1 115.0(5) . . ?
C8 C7 C6 123.0(6) . . ?
C8 C7 H7 118.5 . . ?
C6 C7 H7 118.5 . . ?
C7 C8 C9 119.1(6) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 119.5(6) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 121.8(6) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C6 120.1(6) . . ?
C10 C11 C12 127.3(6) . . ?
C6 C11 C12 112.6(6) . . ?
C13 C12 C17 121.2(6) . . ?
C13 C12 C11 126.2(6) . . ?
C17 C12 C11 112.6(5) . . ?
C14 C13 C12 121.1(6) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 118.7(6) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C16 C15 C14 120.2(6) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 122.3(6) . . ?
C17 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C16 C17 C12 116.4(6) . . ?
C16 C17 Ni1 128.8(4) . . ?
C12 C17 Ni1 114.7(5) . . ?
N1 C18 N2 114.6(6) . . ?
N1 C18 H18 122.7 . . ?
N2 C18 H18 122.7 . . ?
N2 C19 C20 103.0(5) . . ?
N2 C19 H19A 111.2 . . ?
C20 C19 H19A 111.2 . . ?
N2 C19 H19B 111.2 . . ?
C20 C19 H19B 111.2 . . ?
H19A C19 H19B 109.1 . . ?
N1 C20 C19 101.9(5) . . ?
N1 C20 H20A 111.4 . . ?
C19 C20 H20A 111.4 . . ?
N1 C20 H20B 111.4 . . ?
C19 C20 H20B 111.4 . . ?
H20A C20 H20B 109.3 . . ?
C26 C21 C22 120.0(6) . . ?
C26 C21 N2 121.1(5) . . ?
C22 C21 N2 119.0(6) . . ?
C23 C22 C21 118.5(6) . . ?
C23 C22 C27 121.2(6) . . ?
C21 C22 C27 120.3(6) . . ?
C22 C23 C24 123.0(6) . . ?
C22 C23 H23 118.5 . . ?
C24 C23 H23 118.5 . . ?
C23 C24 C25 116.9(6) . . ?
C23 C24 C28 121.8(6) . . ?
C25 C24 C28 121.2(6) . . ?
C26 C25 C24 122.5(6) . . ?
C26 C25 H25 118.8 . . ?
C24 C25 H25 118.8 . . ?
C25 C26 C21 119.2(6) . . ?
C25 C26 C29 121.3(6) . . ?
C21 C26 C29 119.5(6) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C35 C30 C31 122.9(6) . . ?
C35 C30 N1 118.6(6) . . ?
C31 C30 N1 118.4(6) . . ?
C32 C31 C30 117.0(6) . . ?
C32 C31 C36 120.9(6) . . ?
C30 C31 C36 122.1(6) . . ?
C31 C32 C33 123.0(6) . . ?
C31 C32 H32 118.5 . . ?
C33 C32 H32 118.5 . . ?
C32 C33 C34 117.1(7) . . ?
C32 C33 C37 122.2(6) . . ?
C34 C33 C37 120.7(6) . . ?
C35 C34 C33 123.5(6) . . ?
C35 C34 H34 118.3 . . ?
C33 C34 H34 118.3 . . ?
C34 C35 C30 116.6(6) . . ?
C34 C35 C38 122.4(6) . . ?
C30 C35 C38 121.0(6) . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C31 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C37 H37A 109.5 . . ?
C33 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C33 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C39 O1 C42 105.9(5) . . ?
O1 C39 C40 106.3(6) . . ?
O1 C39 H39A 110.5 . . ?
C40 C39 H39A 110.5 . . ?
O1 C39 H39B 110.5 . . ?
C40 C39 H39B 110.5 . . ?
H39A C39 H39B 108.7 . . ?
C39 C40 C41 104.2(6) . . ?
C39 C40 H40A 110.9 . . ?
C41 C40 H40A 110.9 . . ?
C39 C40 H40B 110.9 . . ?
C41 C40 H40B 110.9 . . ?
H40A C40 H40B 108.9 . . ?
C42 C41 C40 104.9(6) . . ?
C42 C41 H41A 110.8 . . ?
C40 C41 H41A 110.8 . . ?
C42 C41 H41B 110.8 . . ?
C40 C41 H41B 110.8 . . ?
H41A C41 H41B 108.8 . . ?
O1 C42 C41 104.3(6) . . ?
O1 C42 H42A 110.9 . . ?
C41 C42 H42A 110.9 . . ?
O1 C42 H42B 110.9 . . ?
C41 C42 H42B 110.9 . . ?
H42A C42 H42B 108.9 . . ?
C46 O2 C43 110.0(6) . . ?
O2 C43 C44 106.1(7) . . ?
O2 C43 H43A 110.5 . . ?
C44 C43 H43A 110.5 . . ?
O2 C43 H43B 110.5 . . ?
C44 C43 H43B 110.5 . . ?
H43A C43 H43B 108.7 . . ?
C45 C44 C43 102.5(6) . . ?
C45 C44 H44A 111.3 . . ?
C43 C44 H44A 111.3 . . ?
C45 C44 H44B 111.3 . . ?
C43 C44 H44B 111.3 . . ?
H44A C44 H44B 109.2 . . ?
C46 C45 C44 102.2(6) . . ?
C46 C45 H45A 111.3 . . ?
C44 C45 H45A 111.3 . . ?
C46 C45 H45B 111.3 . . ?
C44 C45 H45B 111.3 . . ?
H45A C45 H45B 109.2 . . ?
O2 C46 C45 105.4(6) . . ?
O2 C46 H46A 110.7 . . ?
C45 C46 H46A 110.7 . . ?
O2 C46 H46B 110.7 . . ?
C45 C46 H46B 110.7 . . ?
H46A C46 H46B 108.8 . . ?

_refine_diff_density_max         1.405
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.088

_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_2
_database_code_depnum_ccdc_archive 'CCDC 1038669'
_audit_update_record             
;
2014-12-10 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H52 N2 Ni O'
_chemical_formula_weight         683.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'

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

_cell_length_a                   17.1430(5)
_cell_length_b                   13.1907(2)
_cell_length_c                   17.5420(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.528(3)
_cell_angle_gamma                90.00
_cell_volume                     3608.8(1)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    14243
_cell_measurement_theta_min      2.9776
_cell_measurement_theta_max      31.2676

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.519
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.076
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_min  0.86588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            41020
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         31.34
_reflns_number_total             10889
_reflns_number_gt                9044
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0352P)²+1.6894P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10889
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0890
_refine_ls_wR_factor_gt          0.0831
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.70304(8) 0.82567(9) 0.21459(8) 0.0119(2) Uani 1 1 d . . .
H1 H 0.7020 0.8153 0.2666 0.014 Uiso 1 1 calc R . .
C2 C 0.70619(9) 0.79164(10) 0.08750(8) 0.0164(2) Uani 1 1 d . . .
H2A H 0.6607 0.7728 0.0341 0.020 Uiso 1 1 calc R . .
H2B H 0.7604 0.7666 0.0901 0.020 Uiso 1 1 calc R . .
C3 C 0.70879(9) 0.90679(9) 0.10120(8) 0.0150(2) Uani 1 1 d . . .
H3A H 0.7570 0.9374 0.0946 0.018 Uiso 1 1 calc R . .
H3B H 0.6562 0.9388 0.0628 0.018 Uiso 1 1 calc R . .
C4 C 0.73091(8) 1.00822(9) 0.23458(8) 0.0122(2) Uani 1 1 d . . .
C5 C 0.66007(8) 1.07137(9) 0.21759(8) 0.0149(2) Uani 1 1 d . . .
C6 C 0.67415(9) 1.16222(10) 0.26249(9) 0.0182(3) Uani 1 1 d . . .
H6 H 0.6283 1.2056 0.2531 0.022 Uiso 1 1 calc R . .
C7 C 0.75509(9) 1.18856(10) 0.32062(9) 0.0198(3) Uani 1 1 d . . .
H7 H 0.7634 1.2500 0.3489 0.024 Uiso 1 1 calc R . .
C8 C 0.82405(9) 1.12376(10) 0.33695(8) 0.0179(3) Uani 1 1 d . . .
H8 H 0.8781 1.1420 0.3766 0.021 Uiso 1 1 calc R . .
C9 C 0.81331(8) 1.03159(9) 0.29457(8) 0.0137(2) Uani 1 1 d . . .
C10 C 0.57079(8) 1.04505(10) 0.15529(9) 0.0201(3) Uani 1 1 d . . .
H10A H 0.5316 1.0518 0.1821 0.024 Uiso 1 1 calc R . .
H10B H 0.5697 0.9748 0.1384 0.024 Uiso 1 1 calc R . .
C11 C 0.53989(10) 1.11243(12) 0.07737(10) 0.0291(3) Uani 1 1 d . . .
H11A H 0.5439 1.1823 0.0939 0.044 Uiso 1 1 calc R . .
H11B H 0.4814 1.0963 0.0418 0.044 Uiso 1 1 calc R . .
H11C H 0.5750 1.1010 0.0475 0.044 Uiso 1 1 calc R . .
C12 C 0.88826(8) 0.96049(10) 0.31557(9) 0.0179(3) Uani 1 1 d . . .
H12A H 0.8699 0.8925 0.3215 0.022 Uiso 1 1 calc R . .
H12B H 0.9328 0.9801 0.3693 0.022 Uiso 1 1 calc R . .
C13 C 0.92624(10) 0.95816(15) 0.25138(10) 0.0328(4) Uani 1 1 d . . .
H13A H 0.8851 0.9303 0.1998 0.049 Uiso 1 1 calc R . .
H13B H 0.9769 0.9169 0.2719 0.049 Uiso 1 1 calc R . .
H13C H 0.9407 1.0258 0.2418 0.049 Uiso 1 1 calc R . .
C14 C 0.68112(9) 0.64687(9) 0.17407(8) 0.0151(2) Uani 1 1 d . . .
C15 C 0.75343(9) 0.59574(10) 0.23129(8) 0.0185(3) Uani 1 1 d . . .
C16 C 0.74264(11) 0.49329(11) 0.24499(10) 0.0262(3) Uani 1 1 d . . .
H16 H 0.7889 0.4565 0.2826 0.031 Uiso 1 1 calc R . .
C17 C 0.66450(12) 0.44593(11) 0.20357(10) 0.0297(4) Uani 1 1 d . . .
H17 H 0.6587 0.3780 0.2143 0.036 Uiso 1 1 calc R . .
C18 C 0.59477(11) 0.49793(11) 0.14628(10) 0.0257(3) Uani 1 1 d . . .
H18 H 0.5429 0.4643 0.1184 0.031 Uiso 1 1 calc R . .
C19 C 0.60141(9) 0.60054(10) 0.12987(9) 0.0189(3) Uani 1 1 d . . .
C20 C 0.83783(9) 0.65035(11) 0.27712(9) 0.0217(3) Uani 1 1 d . . .
H20A H 0.8325 0.6940 0.3192 0.026 Uiso 1 1 calc R . .
H20B H 0.8480 0.6936 0.2374 0.026 Uiso 1 1 calc R . .
C21 C 0.91606(11) 0.58271(14) 0.31992(11) 0.0323(4) Uani 1 1 d . . .
H21A H 0.9108 0.5464 0.3650 0.048 Uiso 1 1 calc R . .
H21B H 0.9669 0.6238 0.3418 0.048 Uiso 1 1 calc R . .
H21C H 0.9198 0.5354 0.2800 0.048 Uiso 1 1 calc R . .
C22 C 0.52419(9) 0.65734(11) 0.06937(9) 0.0233(3) Uani 1 1 d . . .
H22A H 0.4851 0.6095 0.0300 0.028 Uiso 1 1 calc R . .
H22B H 0.5426 0.7047 0.0378 0.028 Uiso 1 1 calc R . .
C23 C 0.47628(10) 0.71568(13) 0.11192(10) 0.0300(3) Uani 1 1 d . . .
H23A H 0.4573 0.6693 0.1429 0.045 Uiso 1 1 calc R . .
H23B H 0.4276 0.7493 0.0702 0.045 Uiso 1 1 calc R . .
H23C H 0.5139 0.7651 0.1495 0.045 Uiso 1 1 calc R . .
C24 C 0.24556(8) 0.28767(9) 0.06812(8) 0.0132(2) Uani 1 1 d . . .
C25 C 0.27414(9) 0.38892(10) 0.08196(8) 0.0165(2) Uani 1 1 d . . .
H25 H 0.2347 0.4408 0.0581 0.020 Uiso 1 1 calc R . .
C26 C 0.35970(9) 0.41397(10) 0.13032(9) 0.0188(3) Uani 1 1 d . . .
H26 H 0.3767 0.4816 0.1368 0.023 Uiso 1 1 calc R . .
C27 C 0.41992(9) 0.33800(10) 0.16893(9) 0.0187(3) Uani 1 1 d . . .
H27 H 0.4765 0.3547 0.2028 0.022 Uiso 1 1 calc R . .
C28 C 0.39427(8) 0.23665(10) 0.15625(8) 0.0159(2) Uani 1 1 d . . .
H28 H 0.4341 0.1857 0.1817 0.019 Uiso 1 1 calc R . .
C29 C 0.30951(8) 0.21132(9) 0.10575(8) 0.0131(2) Uani 1 1 d . . .
C30 C 0.27511(8) 0.10885(9) 0.08097(8) 0.0129(2) Uani 1 1 d . . .
C31 C 0.32214(9) 0.01866(10) 0.10132(8) 0.0158(2) Uani 1 1 d . . .
H31 H 0.3805 0.0201 0.1357 0.019 Uiso 1 1 calc R . .
C32 C 0.28180(9) -0.07323(10) 0.07022(9) 0.0186(3) Uani 1 1 d . . .
H32 H 0.3132 -0.1332 0.0835 0.022 Uiso 1 1 calc R . .
C33 C 0.19415(9) -0.07529(10) 0.01911(9) 0.0193(3) Uani 1 1 d . . .
H33 H 0.1669 -0.1368 -0.0013 0.023 Uiso 1 1 calc R . .
C34 C 0.14718(9) 0.01482(10) -0.00141(8) 0.0172(2) Uani 1 1 d . . .
H34 H 0.0887 0.0122 -0.0354 0.021 Uiso 1 1 calc R . .
C35 C 0.18598(8) 0.10955(9) 0.02799(8) 0.0137(2) Uani 1 1 d . . .
C36 C 0.02288(10) 0.23441(12) -0.11394(9) 0.0265(3) Uani 1 1 d . . .
H36 H 0.0168 0.1932 -0.1591 0.032 Uiso 1 1 calc R . .
C37 C 0.05579(10) 0.33335(12) -0.10003(9) 0.0244(3) Uani 1 1 d . . .
H37 H 0.0749 0.3696 -0.1344 0.029 Uiso 1 1 calc R . .
C38 C 0.05467(9) 0.36819(10) -0.02361(9) 0.0183(3) Uani 1 1 d . . .
H38 H 0.0754 0.4304 0.0017 0.022 Uiso 1 1 calc R . .
C39 C 0.01683(8) 0.29261(10) 0.00755(9) 0.0184(3) Uani 1 1 d . . .
H39 H 0.0050 0.2976 0.0546 0.022 Uiso 1 1 calc R . .
C40 C 0.00040(9) 0.20805(11) -0.04663(10) 0.0228(3) Uani 1 1 d . . .
H40 H -0.0214 0.1459 -0.0396 0.027 Uiso 1 1 calc R . .
C41 C 0.84303(13) 0.25962(15) 0.16324(12) 0.0387(4) Uani 1 1 d . . .
H41A H 0.8522 0.2977 0.2135 0.046 Uiso 1 1 calc R . .
H41B H 0.8583 0.1894 0.1785 0.046 Uiso 1 1 calc R . .
C42 C 0.75050(12) 0.26785(13) 0.10029(12) 0.0336(4) Uani 1 1 d . . .
H42A H 0.7130 0.2814 0.1280 0.040 Uiso 1 1 calc R . .
H42B H 0.7318 0.2061 0.0677 0.040 Uiso 1 1 calc R . .
C43 C 0.75123(11) 0.35804(15) 0.04421(11) 0.0360(4) Uani 1 1 d . . .
H43A H 0.7294 0.3380 -0.0142 0.043 Uiso 1 1 calc R . .
H43B H 0.7172 0.4141 0.0496 0.043 Uiso 1 1 calc R . .
C44 C 0.84537(11) 0.38617(13) 0.07797(12) 0.0329(4) Uani 1 1 d . . .
H44A H 0.8610 0.4029 0.0323 0.039 Uiso 1 1 calc R . .
H44B H 0.8571 0.4444 0.1148 0.039 Uiso 1 1 calc R . .
N1 N 0.71855(7) 0.91415(8) 0.18925(6) 0.01224(19) Uani 1 1 d . . .
N2 N 0.68912(7) 0.75310(8) 0.15878(7) 0.0132(2) Uani 1 1 d . . .
Ni1 Ni 0.134287(10) 0.238256(12) 0.003404(10) 0.01324(5) Uani 1 1 d . . .
O1 O 0.89302(8) 0.30064(9) 0.12290(8) 0.0336(3) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.3147(15) . ?
C1 N2 1.3183(15) . ?
C1 H1 0.9300 . ?
C2 N2 1.4872(15) . ?
C2 C3 1.5356(17) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.4861(16) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.3988(17) . ?
C4 C9 1.4013(17) . ?
C4 N1 1.4412(15) . ?
C5 C6 1.3989(18) . ?
C5 C10 1.5061(18) . ?
C6 C7 1.382(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.3890(19) . ?
C7 H7 0.9300 . ?
C8 C9 1.3967(17) . ?
C8 H8 0.9300 . ?
C9 C12 1.5077(18) . ?
C10 C11 1.529(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.517(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C19 1.4009(19) . ?
C14 C15 1.4021(19) . ?
C14 N2 1.4438(15) . ?
C15 C16 1.3982(19) . ?
C15 C20 1.514(2) . ?
C16 C17 1.380(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.383(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.3981(19) . ?
C18 H18 0.9300 . ?
C19 C22 1.508(2) . ?
C20 C21 1.524(2) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.527(2) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.4084(17) . ?
C24 C29 1.4322(17) . ?
C24 Ni1 1.8853(13) . ?
C25 C26 1.3955(19) . ?
C25 H25 0.9300 . ?
C26 C27 1.396(2) . ?
C26 H26 0.9300 . ?
C27 C28 1.3961(18) . ?
C27 H27 0.9300 . ?
C28 C29 1.3924(18) . ?
C28 H28 0.9300 . ?
C29 C30 1.4666(17) . ?
C30 C31 1.3977(17) . ?
C30 C35 1.4210(18) . ?
C31 C32 1.3898(18) . ?
C31 H31 0.9300 . ?
C32 C33 1.394(2) . ?
C32 H32 0.9300 . ?
C33 C34 1.3965(18) . ?
C33 H33 0.9300 . ?
C34 C35 1.4088(18) . ?
C34 H34 0.9300 . ?
C35 Ni1 1.8806(12) . ?
C36 C37 1.403(2) . ?
C36 C40 1.429(2) . ?
C36 Ni1 2.1503(15) . ?
C36 H36 0.9300 . ?
C37 C38 1.4248(19) . ?
C37 Ni1 2.1562(14) . ?
C37 H37 0.9300 . ?
C38 C39 1.4169(19) . ?
C38 Ni1 2.1184(13) . ?
C38 H38 0.9300 . ?
C39 C40 1.416(2) . ?
C39 Ni1 2.1668(13) . ?
C39 H39 0.9300 . ?
C40 Ni1 2.1272(14) . ?
C40 H40 0.9300 . ?
C41 O1 1.425(2) . ?
C41 C42 1.514(3) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.547(2) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.516(2) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 O1 1.424(2) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 113.16(11) . . ?
N1 C1 H1 123.4 . . ?
N2 C1 H1 123.4 . . ?
N2 C2 C3 102.10(9) . . ?
N2 C2 H2A 111.3 . . ?
C3 C2 H2A 111.3 . . ?
N2 C2 H2B 111.3 . . ?
C3 C2 H2B 111.3 . . ?
H2A C2 H2B 109.2 . . ?
N1 C3 C2 102.16(9) . . ?
N1 C3 H3A 111.3 . . ?
C2 C3 H3A 111.3 . . ?
N1 C3 H3B 111.3 . . ?
C2 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
C5 C4 C9 122.98(11) . . ?
C5 C4 N1 118.64(11) . . ?
C9 C4 N1 118.37(11) . . ?
C6 C5 C4 117.29(12) . . ?
C6 C5 C10 119.47(12) . . ?
C4 C5 C10 123.24(11) . . ?
C7 C6 C5 121.10(12) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C8 120.34(12) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C9 120.86(12) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C4 117.41(12) . . ?
C8 C9 C12 120.04(12) . . ?
C4 C9 C12 122.53(11) . . ?
C5 C10 C11 112.66(11) . . ?
C5 C10 H10A 109.1 . . ?
C11 C10 H10A 109.1 . . ?
C5 C10 H10B 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 C13 114.58(11) . . ?
C9 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
C9 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 123.76(12) . . ?
C19 C14 N2 117.82(12) . . ?
C15 C14 N2 118.42(12) . . ?
C16 C15 C14 116.57(14) . . ?
C16 C15 C20 122.27(13) . . ?
C14 C15 C20 121.14(12) . . ?
C17 C16 C15 121.04(15) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 121.03(13) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C17 C18 C19 120.67(14) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C14 116.90(14) . . ?
C18 C19 C22 120.22(13) . . ?
C14 C19 C22 122.84(12) . . ?
C15 C20 C21 115.76(13) . . ?
C15 C20 H20A 108.3 . . ?
C21 C20 H20A 108.3 . . ?
C15 C20 H20B 108.3 . . ?
C21 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 C23 113.54(12) . . ?
C19 C22 H22A 108.9 . . ?
C23 C22 H22A 108.9 . . ?
C19 C22 H22B 108.9 . . ?
C23 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 116.26(12) . . ?
C25 C24 Ni1 128.63(10) . . ?
C29 C24 Ni1 115.08(9) . . ?
C26 C25 C24 122.14(12) . . ?
C26 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C25 C26 C27 120.26(12) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C28 119.32(12) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C29 C28 C27 120.51(12) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C24 121.43(12) . . ?
C28 C29 C30 126.49(11) . . ?
C24 C29 C30 112.01(11) . . ?
C31 C30 C35 121.47(12) . . ?
C31 C30 C29 126.18(12) . . ?
C35 C30 C29 112.26(11) . . ?
C32 C31 C30 120.12(12) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C33 119.82(12) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C32 C33 C34 120.08(12) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 121.77(12) . . ?
C33 C34 H34 119.1 . . ?
C35 C34 H34 119.1 . . ?
C34 C35 C30 116.73(11) . . ?
C34 C35 Ni1 127.65(10) . . ?
C30 C35 Ni1 115.61(9) . . ?
C37 C36 C40 108.04(13) . . ?
C37 C36 Ni1 71.22(8) . . ?
C40 C36 Ni1 69.61(8) . . ?
C37 C36 H36 126.0 . . ?
C40 C36 H36 126.0 . . ?
Ni1 C36 H36 124.8 . . ?
C36 C37 C38 107.59(13) . . ?
C36 C37 Ni1 70.76(8) . . ?
C38 C37 Ni1 69.10(8) . . ?
C36 C37 H37 126.2 . . ?
C38 C37 H37 126.2 . . ?
Ni1 C37 H37 125.5 . . ?
C39 C38 C37 108.85(13) . . ?
C39 C38 Ni1 72.55(8) . . ?
C37 C38 Ni1 71.97(8) . . ?
C39 C38 H38 125.6 . . ?
C37 C38 H38 125.6 . . ?
Ni1 C38 H38 121.6 . . ?
C40 C39 C38 106.91(13) . . ?
C40 C39 Ni1 69.24(8) . . ?
C38 C39 Ni1 68.86(7) . . ?
C40 C39 H39 126.5 . . ?
C38 C39 H39 126.5 . . ?
Ni1 C39 H39 126.9 . . ?
C39 C40 C36 108.44(13) . . ?
C39 C40 Ni1 72.27(8) . . ?
C36 C40 Ni1 71.36(8) . . ?
C39 C40 H40 125.8 . . ?
C36 C40 H40 125.8 . . ?
Ni1 C40 H40 122.3 . . ?
O1 C41 C42 105.93(14) . . ?
O1 C41 H41A 110.5 . . ?
C42 C41 H41A 110.5 . . ?
O1 C41 H41B 110.5 . . ?
C42 C41 H41B 110.5 . . ?
H41A C41 H41B 108.7 . . ?
C41 C42 C43 103.67(13) . . ?
C41 C42 H42A 111.0 . . ?
C43 C42 H42A 111.0 . . ?
C41 C42 H42B 111.0 . . ?
C43 C42 H42B 111.0 . . ?
H42A C42 H42B 109.0 . . ?
C44 C43 C42 103.18(14) . . ?
C44 C43 H43A 111.1 . . ?
C42 C43 H43A 111.1 . . ?
C44 C43 H43B 111.1 . . ?
C42 C43 H43B 111.1 . . ?
H43A C43 H43B 109.1 . . ?
O1 C44 C43 107.18(13) . . ?
O1 C44 H44A 110.3 . . ?
C43 C44 H44A 110.3 . . ?
O1 C44 H44B 110.3 . . ?
C43 C44 H44B 110.3 . . ?
H44A C44 H44B 108.5 . . ?
C1 N1 C4 125.57(10) . . ?
C1 N1 C3 110.01(10) . . ?
C4 N1 C3 123.85(10) . . ?
C1 N2 C14 124.66(10) . . ?
C1 N2 C2 109.75(10) . . ?
C14 N2 C2 123.71(10) . . ?
C35 Ni1 C24 84.92(5) . . ?
C35 Ni1 C38 168.58(5) . . ?
C24 Ni1 C38 104.59(5) . . ?
C35 Ni1 C40 104.51(5) . . ?
C24 Ni1 C40 164.14(5) . . ?
C38 Ni1 C40 64.82(5) . . ?
C35 Ni1 C36 110.18(6) . . ?
C24 Ni1 C36 149.22(6) . . ?
C38 Ni1 C36 64.61(5) . . ?
C40 Ni1 C36 39.02(6) . . ?
C35 Ni1 C37 142.03(6) . . ?
C24 Ni1 C37 115.31(6) . . ?
C38 Ni1 C37 38.93(5) . . ?
C40 Ni1 C37 64.67(6) . . ?
C36 Ni1 C37 38.01(6) . . ?
C35 Ni1 C39 130.32(5) . . ?
C24 Ni1 C39 125.97(5) . . ?
C38 Ni1 C39 38.59(5) . . ?
C40 Ni1 C39 38.49(5) . . ?
C36 Ni1 C39 64.63(5) . . ?
C37 Ni1 C39 64.64(5) . . ?
C44 O1 C41 104.51(13) . . ?

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
N2 C2 C3 N1 15.91(12) . . . . ?
C9 C4 C5 C6 0.99(18) . . . . ?
N1 C4 C5 C6 -179.88(11) . . . . ?
C9 C4 C5 C10 -177.87(12) . . . . ?
N1 C4 C5 C10 1.26(18) . . . . ?
C4 C5 C6 C7 0.62(19) . . . . ?
C10 C5 C6 C7 179.52(12) . . . . ?
C5 C6 C7 C8 -1.4(2) . . . . ?
C6 C7 C8 C9 0.7(2) . . . . ?
C7 C8 C9 C4 0.86(19) . . . . ?
C7 C8 C9 C12 -177.63(12) . . . . ?
C5 C4 C9 C8 -1.71(18) . . . . ?
N1 C4 C9 C8 179.15(11) . . . . ?
C5 C4 C9 C12 176.74(12) . . . . ?
N1 C4 C9 C12 -2.39(17) . . . . ?
C6 C5 C10 C11 70.41(16) . . . . ?
C4 C5 C10 C11 -110.75(15) . . . . ?
C8 C9 C12 C13 -104.86(15) . . . . ?
C4 C9 C12 C13 76.72(16) . . . . ?
C19 C14 C15 C16 -1.51(19) . . . . ?
N2 C14 C15 C16 179.27(11) . . . . ?
C19 C14 C15 C20 -179.97(12) . . . . ?
N2 C14 C15 C20 0.82(18) . . . . ?
C14 C15 C16 C17 0.26(19) . . . . ?
C20 C15 C16 C17 178.70(13) . . . . ?
C15 C16 C17 C18 1.0(2) . . . . ?
C16 C17 C18 C19 -1.0(2) . . . . ?
C17 C18 C19 C14 -0.2(2) . . . . ?
C17 C18 C19 C22 -178.02(13) . . . . ?
C15 C14 C19 C18 1.47(19) . . . . ?
N2 C14 C19 C18 -179.32(11) . . . . ?
C15 C14 C19 C22 179.26(12) . . . . ?
N2 C14 C19 C22 -1.52(18) . . . . ?
C16 C15 C20 C21 16.43(19) . . . . ?
C14 C15 C20 C21 -165.20(12) . . . . ?
C18 C19 C22 C23 95.79(16) . . . . ?
C14 C19 C22 C23 -81.94(17) . . . . ?
C29 C24 C25 C26 -0.67(18) . . . . ?
Ni1 C24 C25 C26 -178.49(10) . . . . ?
C24 C25 C26 C27 -1.8(2) . . . . ?
C25 C26 C27 C28 2.24(19) . . . . ?
C26 C27 C28 C29 -0.09(19) . . . . ?
C27 C28 C29 C24 -2.52(19) . . . . ?
C27 C28 C29 C30 174.30(12) . . . . ?
C25 C24 C29 C28 2.84(17) . . . . ?
Ni1 C24 C29 C28 -179.04(9) . . . . ?
C25 C24 C29 C30 -174.40(11) . . . . ?
Ni1 C24 C29 C30 3.73(13) . . . . ?
C28 C29 C30 C31 -2.5(2) . . . . ?
C24 C29 C30 C31 174.59(12) . . . . ?
C28 C29 C30 C35 -179.15(12) . . . . ?
C24 C29 C30 C35 -2.08(14) . . . . ?
C35 C30 C31 C32 -0.56(18) . . . . ?
C29 C30 C31 C32 -176.95(12) . . . . ?
C30 C31 C32 C33 -0.43(19) . . . . ?
C31 C32 C33 C34 0.6(2) . . . . ?
C32 C33 C34 C35 0.2(2) . . . . ?
C33 C34 C35 C30 -1.15(18) . . . . ?
C33 C34 C35 Ni1 177.25(10) . . . . ?
C31 C30 C35 C34 1.32(18) . . . . ?
C29 C30 C35 C34 178.17(11) . . . . ?
C31 C30 C35 Ni1 -177.28(9) . . . . ?
C29 C30 C35 Ni1 -0.42(13) . . . . ?
C40 C36 C37 C38 0.62(16) . . . . ?
Ni1 C36 C37 C38 -59.54(10) . . . . ?
C40 C36 C37 Ni1 60.16(10) . . . . ?
C36 C37 C38 C39 -3.02(16) . . . . ?
Ni1 C37 C38 C39 -63.61(9) . . . . ?
C36 C37 C38 Ni1 60.59(10) . . . . ?
C37 C38 C39 C40 4.22(15) . . . . ?
Ni1 C38 C39 C40 -59.02(9) . . . . ?
C37 C38 C39 Ni1 63.24(9) . . . . ?
C38 C39 C40 C36 -3.82(15) . . . . ?
Ni1 C39 C40 C36 -62.59(10) . . . . ?
C38 C39 C40 Ni1 58.78(9) . . . . ?
C37 C36 C40 C39 2.00(16) . . . . ?
Ni1 C36 C40 C39 63.18(10) . . . . ?
C37 C36 C40 Ni1 -61.17(10) . . . . ?
O1 C41 C42 C43 -26.28(18) . . . . ?
C41 C42 C43 C44 3.79(18) . . . . ?
C42 C43 C44 O1 19.94(19) . . . . ?
N2 C1 N1 C4 176.05(11) . . . . ?
N2 C1 N1 C3 4.45(15) . . . . ?
C5 C4 N1 C1 -93.39(15) . . . . ?
C9 C4 N1 C1 85.78(15) . . . . ?
C5 C4 N1 C3 77.09(15) . . . . ?
C9 C4 N1 C3 -103.74(14) . . . . ?
C2 C3 N1 C1 -13.27(13) . . . . ?
C2 C3 N1 C4 174.96(11) . . . . ?
N1 C1 N2 C14 171.93(11) . . . . ?
N1 C1 N2 C2 7.09(15) . . . . ?
C19 C14 N2 C1 114.07(14) . . . . ?
C15 C14 N2 C1 -66.66(17) . . . . ?
C19 C14 N2 C2 -83.13(15) . . . . ?
C15 C14 N2 C2 96.13(15) . . . . ?
C3 C2 N2 C1 -14.74(14) . . . . ?
C3 C2 N2 C14 -179.75(11) . . . . ?
C34 C35 Ni1 C24 -176.41(12) . . . . ?
C30 C35 Ni1 C24 2.00(9) . . . . ?
C34 C35 Ni1 C38 36.8(3) . . . . ?
C30 C35 Ni1 C38 -144.8(2) . . . . ?
C34 C35 Ni1 C40 16.55(13) . . . . ?
C30 C35 Ni1 C40 -165.04(9) . . . . ?
C34 C35 Ni1 C36 -24.00(13) . . . . ?
C30 C35 Ni1 C36 154.41(9) . . . . ?
C34 C35 Ni1 C37 -50.71(16) . . . . ?
C30 C35 Ni1 C37 127.70(10) . . . . ?
C34 C35 Ni1 C39 49.33(14) . . . . ?
C30 C35 Ni1 C39 -132.26(9) . . . . ?
C25 C24 Ni1 C35 174.63(12) . . . . ?
C29 C24 Ni1 C35 -3.22(9) . . . . ?
C25 C24 Ni1 C38 -11.81(12) . . . . ?
C29 C24 Ni1 C38 170.35(9) . . . . ?
C25 C24 Ni1 C40 -58.0(3) . . . . ?
C29 C24 Ni1 C40 124.2(2) . . . . ?
C25 C24 Ni1 C36 52.79(17) . . . . ?
C29 C24 Ni1 C36 -125.05(11) . . . . ?
C25 C24 Ni1 C37 28.18(13) . . . . ?
C29 C24 Ni1 C37 -149.66(9) . . . . ?
C25 C24 Ni1 C39 -47.81(14) . . . . ?
C29 C24 Ni1 C39 134.35(9) . . . . ?
C39 C38 Ni1 C35 15.4(3) . . . . ?
C37 C38 Ni1 C35 -101.9(3) . . . . ?
C39 C38 Ni1 C24 -130.31(8) . . . . ?
C37 C38 Ni1 C24 112.39(9) . . . . ?
C39 C38 Ni1 C40 37.10(8) . . . . ?
C37 C38 Ni1 C40 -80.19(10) . . . . ?
C39 C38 Ni1 C36 80.46(9) . . . . ?
C37 C38 Ni1 C36 -36.84(9) . . . . ?
C39 C38 Ni1 C37 117.30(12) . . . . ?
C37 C38 Ni1 C39 -117.30(12) . . . . ?
C39 C40 Ni1 C35 138.45(8) . . . . ?
C36 C40 Ni1 C35 -104.28(9) . . . . ?
C39 C40 Ni1 C24 13.3(2) . . . . ?
C36 C40 Ni1 C24 130.6(2) . . . . ?
C39 C40 Ni1 C38 -37.21(8) . . . . ?
C36 C40 Ni1 C38 80.07(9) . . . . ?
C39 C40 Ni1 C36 -117.28(12) . . . . ?
C39 C40 Ni1 C37 -80.44(9) . . . . ?
C36 C40 Ni1 C37 36.83(8) . . . . ?
C36 C40 Ni1 C39 117.28(12) . . . . ?
C37 C36 Ni1 C35 -153.32(8) . . . . ?
C40 C36 Ni1 C35 88.31(9) . . . . ?
C37 C36 Ni1 C24 -37.68(14) . . . . ?
C40 C36 Ni1 C24 -156.05(10) . . . . ?
C37 C36 Ni1 C38 37.71(8) . . . . ?
C40 C36 Ni1 C38 -80.66(9) . . . . ?
C37 C36 Ni1 C40 118.37(12) . . . . ?
C40 C36 Ni1 C37 -118.37(12) . . . . ?
C37 C36 Ni1 C39 80.63(9) . . . . ?
C40 C36 Ni1 C39 -37.75(8) . . . . ?
C36 C37 Ni1 C35 43.24(13) . . . . ?
C38 C37 Ni1 C35 161.65(9) . . . . ?
C36 C37 Ni1 C24 159.76(8) . . . . ?
C38 C37 Ni1 C24 -81.83(9) . . . . ?
C36 C37 Ni1 C38 -118.42(13) . . . . ?
C36 C37 Ni1 C40 -37.80(9) . . . . ?
C38 C37 Ni1 C40 80.61(9) . . . . ?
C38 C37 Ni1 C36 118.42(13) . . . . ?
C36 C37 Ni1 C39 -80.58(9) . . . . ?
C38 C37 Ni1 C39 37.84(8) . . . . ?
C40 C39 Ni1 C35 -57.37(11) . . . . ?
C38 C39 Ni1 C35 -176.06(8) . . . . ?
C40 C39 Ni1 C24 -175.55(8) . . . . ?
C38 C39 Ni1 C24 65.76(10) . . . . ?
C40 C39 Ni1 C38 118.69(12) . . . . ?
C38 C39 Ni1 C40 -118.69(12) . . . . ?
C40 C39 Ni1 C36 38.27(9) . . . . ?
C38 C39 Ni1 C36 -80.42(9) . . . . ?
C40 C39 Ni1 C37 80.52(10) . . . . ?
C38 C39 Ni1 C37 -38.16(8) . . . . ?
C43 C44 O1 C41 -37.40(18) . . . . ?
C42 C41 O1 C44 39.72(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.919
_diffrn_reflns_theta_full        31.34
_diffrn_measured_fraction_theta_full 0.919
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.057
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1038670'
_audit_update_record             
;
2014-12-10 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            PW34
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H46 N2 Ni O'
_chemical_formula_weight         653.52

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'
Ni Ni 0.3393 1.1124 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   13.0464(6)
_cell_length_b                   17.1568(8)
_cell_length_c                   15.5211(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.257(2)
_cell_angle_gamma                90.00
_cell_volume                     3407.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7165
_cell_measurement_theta_min      2.546
_cell_measurement_theta_max      27.485

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaApexII
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean 8.3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22387
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_av_sigmaI/netI    0.1326
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         23.25
_reflns_number_total             4859
_reflns_number_gt                3240
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
'Collect data collection software (Nonius B.V., 1998)'
_computing_cell_refinement       'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    
'SIR97 (Altomare A., Burla M.C., Camalli M., Cascarano, Giacovazzo, Guagliardi , Moliterni, Polidori, Spagna,1999))'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+7.1176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4859
_refine_ls_number_parameters     421
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.122
_refine_ls_R_factor_gt           0.073
_refine_ls_wR_factor_ref         0.140
_refine_ls_wR_factor_gt          0.124
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_restrained_S_all      1.08
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7139(4) 0.0529(3) 0.3081(3) 0.0196(14) Uani 1 1 d . . .
H1 H 0.7202 0.1080 0.3050 0.024 Uiso 1 1 calc R . .
C2 C 0.7106(4) -0.0726(3) 0.2742(4) 0.0240(15) Uani 1 1 d . . .
H2 H 0.7144 -0.1192 0.2419 0.029 Uiso 1 1 calc R . .
C3 C 0.6926(4) -0.0670(3) 0.3574(3) 0.0223(14) Uani 1 1 d . . .
H3 H 0.6810 -0.1087 0.3946 0.027 Uiso 1 1 calc R . .
C4 C 0.6771(4) 0.0432(3) 0.4594(3) 0.0187(13) Uani 1 1 d . . .
C5 C 0.5811(4) 0.0785(3) 0.4609(3) 0.0215(14) Uani 1 1 d . . .
C6 C 0.5662(4) 0.1090(3) 0.5406(3) 0.0233(14) Uani 1 1 d . . .
H6 H 0.5014 0.1332 0.5432 0.028 Uiso 1 1 calc R . .
C7 C 0.6423(5) 0.1054(3) 0.6162(3) 0.0246(15) Uani 1 1 d . . .
C8 C 0.7369(4) 0.0698(3) 0.6115(4) 0.0242(15) Uani 1 1 d . . .
H8 H 0.7897 0.0669 0.6630 0.029 Uiso 1 1 calc R . .
C9 C 0.7565(4) 0.0383(3) 0.5341(3) 0.0198(14) Uani 1 1 d . . .
C10 C 0.4957(4) 0.0815(3) 0.3798(4) 0.0306(16) Uani 1 1 d . . .
H10A H 0.4287 0.0923 0.3969 0.046 Uiso 1 1 calc R . .
H10B H 0.4919 0.0313 0.3493 0.046 Uiso 1 1 calc R . .
H10C H 0.5113 0.1228 0.3407 0.046 Uiso 1 1 calc R . .
C11 C 0.6218(5) 0.1380(4) 0.7017(3) 0.0374(17) Uani 1 1 d . . .
H11A H 0.6734 0.1785 0.7232 0.056 Uiso 1 1 calc R . .
H11B H 0.6273 0.0961 0.7453 0.056 Uiso 1 1 calc R . .
H11C H 0.5515 0.1605 0.6921 0.056 Uiso 1 1 calc R . .
C12 C 0.8594(4) -0.0023(3) 0.5331(4) 0.0305(16) Uani 1 1 d . . .
H12A H 0.9158 0.0248 0.5727 0.046 Uiso 1 1 calc R . .
H12B H 0.8733 -0.0017 0.4733 0.046 Uiso 1 1 calc R . .
H12C H 0.8555 -0.0564 0.5526 0.046 Uiso 1 1 calc R . .
C13 C 0.7486(4) 0.0218(3) 0.1613(3) 0.0152(13) Uani 1 1 d . . .
C14 C 0.8515(4) 0.0130(3) 0.1524(3) 0.0208(14) Uani 1 1 d . . .
C15 C 0.8748(5) 0.0291(3) 0.0701(4) 0.0245(15) Uani 1 1 d . . .
H15 H 0.9444 0.0224 0.0617 0.029 Uiso 1 1 calc R . .
C16 C 0.7987(5) 0.0549(3) 0.0001(3) 0.0219(14) Uani 1 1 d . . .
C17 C 0.6982(5) 0.0628(3) 0.0134(4) 0.0258(15) Uani 1 1 d . . .
H17 H 0.6459 0.0797 -0.0343 0.031 Uiso 1 1 calc R . .
C18 C 0.6691(4) 0.0472(3) 0.0940(4) 0.0228(14) Uani 1 1 d . . .
C19 C 0.5588(4) 0.0595(3) 0.1087(4) 0.0310(16) Uani 1 1 d . . .
H19A H 0.5356 0.0128 0.1357 0.046 Uiso 1 1 calc R . .
H19B H 0.5121 0.0693 0.0522 0.046 Uiso 1 1 calc R . .
H19C H 0.5575 0.1043 0.1476 0.046 Uiso 1 1 calc R . .
C20 C 0.9369(4) -0.0128(3) 0.2273(4) 0.0331(16) Uani 1 1 d . . .
H20A H 0.9366 0.0206 0.2785 0.050 Uiso 1 1 calc R . .
H20B H 1.0048 -0.0088 0.2096 0.050 Uiso 1 1 calc R . .
H20C H 0.9247 -0.0670 0.2425 0.050 Uiso 1 1 calc R . .
C21 C 0.8269(5) 0.0736(3) -0.0874(3) 0.0349(17) Uani 1 1 d . . .
H21A H 0.8203 0.0265 -0.1238 0.052 Uiso 1 1 calc R . .
H21B H 0.8990 0.0926 -0.0781 0.052 Uiso 1 1 calc R . .
H21C H 0.7796 0.1139 -0.1172 0.052 Uiso 1 1 calc R . .
C22 C 0.7979(4) 0.2393(3) 0.1831(3) 0.0167(13) Uani 1 1 d . . .
C23 C 0.8697(4) 0.2331(3) 0.1280(3) 0.0214(14) Uani 1 1 d . . .
H23 H 0.9399 0.2195 0.1525 0.026 Uiso 1 1 calc R . .
C24 C 0.8415(4) 0.2464(3) 0.0373(3) 0.0226(14) Uani 1 1 d . . .
H24 H 0.8924 0.2430 0.0012 0.027 Uiso 1 1 calc R . .
C25 C 0.7383(5) 0.2645(3) 0.0005(3) 0.0237(14) Uani 1 1 d . . .
H25 H 0.7186 0.2734 -0.0609 0.028 Uiso 1 1 calc R . .
C26 C 0.6644(5) 0.2695(3) 0.0528(3) 0.0227(14) Uani 1 1 d . . .
H26 H 0.5939 0.2816 0.0275 0.027 Uiso 1 1 calc R . .
C27 C 0.6936(4) 0.2567(3) 0.1431(3) 0.0174(13) Uani 1 1 d . . .
C28 C 0.6254(4) 0.2645(3) 0.2069(3) 0.0183(13) Uani 1 1 d . . .
C29 C 0.5185(4) 0.2801(3) 0.1893(4) 0.0210(14) Uani 1 1 d . . .
H29 H 0.4824 0.2846 0.1301 0.025 Uiso 1 1 calc R . .
C30 C 0.4639(5) 0.2890(3) 0.2570(4) 0.0296(15) Uani 1 1 d . . .
H30 H 0.3911 0.2997 0.2444 0.036 Uiso 1 1 calc R . .
C31 C 0.5168(5) 0.2822(3) 0.3431(4) 0.0312(16) Uani 1 1 d . . .
H31 H 0.4804 0.2886 0.3900 0.037 Uiso 1 1 calc R . .
C32 C 0.6240(5) 0.2658(3) 0.3611(4) 0.0239(14) Uani 1 1 d . . .
H32 H 0.6592 0.2613 0.4205 0.029 Uiso 1 1 calc R . .
C33 C 0.6807(4) 0.2560(3) 0.2948(3) 0.0182(13) Uani 1 1 d . . .
C34 C 0.9883(4) 0.2098(3) 0.3442(4) 0.0257(15) Uani 1 1 d . . .
H34 H 1.0278 0.1918 0.3029 0.031 Uiso 1 1 calc R . .
C35 C 0.9342(5) 0.1627(3) 0.3942(4) 0.0311(16) Uani 1 1 d . . .
H35 H 0.9345 0.1073 0.3951 0.037 Uiso 1 1 calc R . .
C36 C 0.8791(4) 0.2113(3) 0.4432(4) 0.0271(15) Uani 1 1 d . . .
H36 H 0.8330 0.1949 0.4800 0.033 Uiso 1 1 calc R . .
C37 C 0.9061(4) 0.2898(3) 0.4264(3) 0.0251(15) Uani 1 1 d . . .
H37 H 0.8824 0.3350 0.4519 0.030 Uiso 1 1 calc R . .
C38 C 0.9740(4) 0.2890(3) 0.3657(4) 0.0264(15) Uani 1 1 d . . .
H38 H 1.0043 0.3332 0.3435 0.032 Uiso 1 1 calc R . .
C39 C 0.7313(5) 0.3717(4) 0.7401(4) 0.0402(18) Uani 1 1 d . . .
H39A H 0.7450 0.3211 0.7709 0.048 Uiso 1 1 calc R . .
H39B H 0.7375 0.4137 0.7846 0.048 Uiso 1 1 calc R . .
C40 C 0.8080(5) 0.3847(3) 0.6801(4) 0.0390(18) Uani 1 1 d . . .
H40A H 0.8762 0.3598 0.7035 0.047 Uiso 1 1 calc R . .
H40B H 0.8190 0.4410 0.6709 0.047 Uiso 1 1 calc R . .
C41 C 0.7533(5) 0.3457(4) 0.5960(4) 0.0473(19) Uani 1 1 d . . .
H41A H 0.7657 0.3747 0.5439 0.057 Uiso 1 1 calc R . .
H41B H 0.7780 0.2914 0.5928 0.057 Uiso 1 1 calc R . .
C42 C 0.6396(5) 0.3474(4) 0.6015(4) 0.0377(17) Uani 1 1 d . . .
H42A H 0.6014 0.3838 0.5570 0.045 Uiso 1 1 calc R . .
H42B H 0.6087 0.2949 0.5897 0.045 Uiso 1 1 calc R . .
Ni1 Ni 0.82561(5) 0.23650(4) 0.30740(4) 0.0180(2) Uani 1 1 d . . .
N2 N 0.7225(3) 0.0025(2) 0.2458(3) 0.0197(11) Uani 1 1 d . . .
N4 N 0.6945(3) 0.0117(2) 0.3769(3) 0.0194(11) Uani 1 1 d . . .
O1 O 0.6311(3) 0.3721(3) 0.6867(3) 0.0538(14) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.318(6) . ?
C1 N4 1.346(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.360(7) . ?
C2 N2 1.381(6) . ?
C2 H2 0.9500 . ?
C3 N4 1.382(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(7) . ?
C4 C9 1.399(7) . ?
C4 N4 1.448(6) . ?
C5 C6 1.391(7) . ?
C5 C10 1.510(7) . ?
C6 C7 1.382(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.392(8) . ?
C7 C11 1.512(7) . ?
C8 C9 1.385(7) . ?
C8 H8 0.9500 . ?
C9 C12 1.515(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.385(7) . ?
C13 C18 1.391(7) . ?
C13 N2 1.456(6) . ?
C14 C15 1.396(7) . ?
C14 C20 1.512(7) . ?
C15 C16 1.393(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.373(7) . ?
C16 C21 1.509(7) . ?
C17 C18 1.402(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.514(7) . ?
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 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.390(7) . ?
C22 C27 1.413(7) . ?
C22 Ni1 1.893(5) . ?
C23 C24 1.403(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.379(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.396(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.461(7) . ?
C28 C29 1.395(7) . ?
C28 C33 1.421(7) . ?
C29 C30 1.388(7) . ?
C29 H29 0.9500 . ?
C30 C31 1.384(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.400(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(7) . ?
C32 H32 0.9500 . ?
C33 Ni1 1.892(5) . ?
C34 C35 1.403(8) . ?
C34 C38 1.421(7) . ?
C34 Ni1 2.137(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.415(8) . ?
C35 Ni1 2.164(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.429(7) . ?
C36 Ni1 2.131(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.413(8) . ?
C37 Ni1 2.144(5) . ?
C37 H37 0.9500 . ?
C38 Ni1 2.167(5) . ?
C38 H38 0.9500 . ?
C39 O1 1.405(7) . ?
C39 C40 1.512(8) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.515(8) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.502(8) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 O1 1.414(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?

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
N2 C1 N4 107.1(5) . . ?
N2 C1 H1 126.5 . . ?
N4 C1 H1 126.5 . . ?
C3 C2 N2 106.7(5) . . ?
C3 C2 H2 126.6 . . ?
N2 C2 H2 126.6 . . ?
C2 C3 N4 106.2(5) . . ?
C2 C3 H3 126.9 . . ?
N4 C3 H3 126.9 . . ?
C5 C4 C9 122.3(5) . . ?
C5 C4 N4 118.2(5) . . ?
C9 C4 N4 119.5(5) . . ?
C6 C5 C4 117.4(5) . . ?
C6 C5 C10 121.4(5) . . ?
C4 C5 C10 121.3(5) . . ?
C7 C6 C5 122.4(5) . . ?
C7 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C6 C7 C8 118.2(5) . . ?
C6 C7 C11 120.5(5) . . ?
C8 C7 C11 121.3(5) . . ?
C9 C8 C7 122.2(5) . . ?
C9 C8 H8 118.9 . . ?
C7 C8 H8 118.9 . . ?
C8 C9 C4 117.6(5) . . ?
C8 C9 C12 120.2(5) . . ?
C4 C9 C12 122.2(5) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 123.6(5) . . ?
C14 C13 N2 117.8(5) . . ?
C18 C13 N2 118.5(5) . . ?
C13 C14 C15 117.3(5) . . ?
C13 C14 C20 122.6(5) . . ?
C15 C14 C20 120.2(5) . . ?
C16 C15 C14 121.8(6) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C17 C16 C15 118.0(5) . . ?
C17 C16 C21 121.5(5) . . ?
C15 C16 C21 120.5(6) . . ?
C16 C17 C18 123.3(5) . . ?
C16 C17 H17 118.4 . . ?
C18 C17 H17 118.4 . . ?
C13 C18 C17 116.0(5) . . ?
C13 C18 C19 121.4(5) . . ?
C17 C18 C19 122.6(5) . . ?
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 . . ?
C14 C20 H20A 109.5 . . ?
C14 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C14 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C27 116.9(5) . . ?
C23 C22 Ni1 127.4(4) . . ?
C27 C22 Ni1 115.4(4) . . ?
C22 C23 C24 121.9(5) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 H23 119.1 . . ?
C25 C24 C23 119.4(5) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C26 C25 C24 120.3(5) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 119.7(5) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C26 C27 C22 121.7(5) . . ?
C26 C27 C28 125.7(5) . . ?
C22 C27 C28 112.5(4) . . ?
C29 C28 C33 120.6(5) . . ?
C29 C28 C27 127.1(5) . . ?
C33 C28 C27 112.3(5) . . ?
C30 C29 C28 120.9(5) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C31 C30 C29 119.3(6) . . ?
C31 C30 H30 120.4 . . ?
C29 C30 H30 120.4 . . ?
C30 C31 C32 120.0(6) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C33 C32 C31 122.1(5) . . ?
C33 C32 H32 118.9 . . ?
C31 C32 H32 118.9 . . ?
C32 C33 C28 117.1(5) . . ?
C32 C33 Ni1 127.6(4) . . ?
C28 C33 Ni1 115.3(4) . . ?
C35 C34 C38 108.5(5) . . ?
C35 C34 Ni1 72.0(3) . . ?
C38 C34 Ni1 71.8(3) . . ?
C35 C34 H34 125.8 . . ?
C38 C34 H34 125.8 . . ?
Ni1 C34 H34 122.1 . . ?
C34 C35 C36 108.7(5) . . ?
C34 C35 Ni1 69.9(3) . . ?
C36 C35 Ni1 69.5(3) . . ?
C34 C35 H35 125.6 . . ?
C36 C35 H35 125.6 . . ?
Ni1 C35 H35 126.5 . . ?
C35 C36 C37 106.8(6) . . ?
C35 C36 Ni1 72.0(3) . . ?
C37 C36 Ni1 71.0(3) . . ?
C35 C36 H36 126.6 . . ?
C37 C36 H36 126.6 . . ?
Ni1 C36 H36 122.2 . . ?
C38 C37 C36 108.7(5) . . ?
C38 C37 Ni1 71.7(3) . . ?
C36 C37 Ni1 70.0(3) . . ?
C38 C37 H37 125.6 . . ?
C36 C37 H37 125.6 . . ?
Ni1 C37 H37 124.2 . . ?
C37 C38 C34 107.1(5) . . ?
C37 C38 Ni1 70.0(3) . . ?
C34 C38 Ni1 69.6(3) . . ?
C37 C38 H38 126.4 . . ?
C34 C38 H38 126.4 . . ?
Ni1 C38 H38 125.5 . . ?
O1 C39 C40 106.7(5) . . ?
O1 C39 H39A 110.4 . . ?
C40 C39 H39A 110.4 . . ?
O1 C39 H39B 110.4 . . ?
C40 C39 H39B 110.4 . . ?
H39A C39 H39B 108.6 . . ?
C39 C40 C41 102.0(5) . . ?
C39 C40 H40A 111.4 . . ?
C41 C40 H40A 111.4 . . ?
C39 C40 H40B 111.4 . . ?
C41 C40 H40B 111.4 . . ?
H40A C40 H40B 109.2 . . ?
C42 C41 C40 104.3(5) . . ?
C42 C41 H41A 110.9 . . ?
C40 C41 H41A 110.9 . . ?
C42 C41 H41B 110.9 . . ?
C40 C41 H41B 110.9 . . ?
H41A C41 H41B 108.9 . . ?
O1 C42 C41 108.5(5) . . ?
O1 C42 H42A 110.0 . . ?
C41 C42 H42A 110.0 . . ?
O1 C42 H42B 110.0 . . ?
C41 C42 H42B 110.0 . . ?
H42A C42 H42B 108.4 . . ?
C33 Ni1 C22 84.4(2) . . ?
C33 Ni1 C36 105.4(2) . . ?
C22 Ni1 C36 166.8(2) . . ?
C33 Ni1 C34 170.3(2) . . ?
C22 Ni1 C34 105.1(2) . . ?
C36 Ni1 C34 64.9(2) . . ?
C33 Ni1 C37 109.0(2) . . ?
C22 Ni1 C37 146.2(2) . . ?
C36 Ni1 C37 39.06(19) . . ?
C34 Ni1 C37 64.4(2) . . ?
C33 Ni1 C35 133.4(2) . . ?
C22 Ni1 C35 128.4(2) . . ?
C36 Ni1 C35 38.5(2) . . ?
C34 Ni1 C35 38.1(2) . . ?
C37 Ni1 C35 64.0(2) . . ?
C33 Ni1 C38 139.7(2) . . ?
C22 Ni1 C38 113.1(2) . . ?
C36 Ni1 C38 65.0(2) . . ?
C34 Ni1 C38 38.6(2) . . ?
C37 Ni1 C38 38.3(2) . . ?
C35 Ni1 C38 63.9(2) . . ?
C1 N2 C2 110.3(5) . . ?
C1 N2 C13 125.5(4) . . ?
C2 N2 C13 124.1(4) . . ?
C1 N4 C3 109.7(4) . . ?
C1 N4 C4 126.3(4) . . ?
C3 N4 C4 124.0(4) . . ?
C39 O1 C42 108.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        23.25
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.089
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1038671'
_audit_update_record             
;
2014-12-10 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H36 N2 Ni'
_chemical_formula_weight         519.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_cell_setting           monoclinic

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

_cell_length_a                   10.6985(1)
_cell_length_b                   15.4023(1)
_cell_length_c                   16.7954(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.035(1)
_cell_angle_gamma                90.00
_cell_volume                     2752.23(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21236
_cell_measurement_theta_min      3.2160
_cell_measurement_theta_max      34.8674

_exptl_crystal_description       block
_exptl_crystal_colour            'deep red'
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_min  0.69742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_reflns_number            43738
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         34.95
_reflns_number_total             11418
_reflns_number_gt                9716
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0415P)²+0.6918P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11418
_refine_ls_number_parameters     329
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0877
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.73784(11) 0.51926(7) 0.16552(7) 0.0277(2) Uani 1 1 d . . .
H1 H 0.6856 0.5202 0.2079 0.033 Uiso 1 1 calc R . .
C2 C 0.86902(11) 0.50960(7) 0.17361(7) 0.0298(2) Uani 1 1 d . . .
H2 H 0.9216 0.5027 0.2224 0.036 Uiso 1 1 calc R . .
C3 C 0.90920(13) 0.51200(7) 0.09510(8) 0.0354(3) Uani 1 1 d . . .
H3 H 0.9932 0.5051 0.0826 0.042 Uiso 1 1 calc R . .
C4 C 0.80367(15) 0.52624(7) 0.03949(7) 0.0379(3) Uani 1 1 d . . .
H4 H 0.8039 0.5338 -0.0166 0.046 Uiso 1 1 calc R . .
C5 C 0.69737(13) 0.52731(7) 0.08250(8) 0.0337(2) Uani 1 1 d . . .
H5 H 0.6126 0.5326 0.0597 0.040 Uiso 1 1 calc R . .
C6 C 0.89671(9) 0.30758(6) 0.10712(5) 0.01810(15) Uani 1 1 d . . .
C7 C 1.02894(9) 0.30677(7) 0.11539(6) 0.02338(18) Uani 1 1 d . . .
H7 H 1.0731 0.3603 0.1202 0.028 Uiso 1 1 calc R . .
C8 C 1.09694(10) 0.22931(8) 0.11670(6) 0.0271(2) Uani 1 1 d . . .
H8 H 1.1862 0.2309 0.1218 0.033 Uiso 1 1 calc R . .
C9 C 1.03500(10) 0.14980(7) 0.11057(6) 0.0269(2) Uani 1 1 d . . .
H9 H 1.0816 0.0972 0.1126 0.032 Uiso 1 1 calc R . .
C10 C 0.90423(10) 0.14793(6) 0.10143(6) 0.02277(17) Uani 1 1 d . . .
H10 H 0.8613 0.0939 0.0967 0.027 Uiso 1 1 calc R . .
C11 C 0.83588(9) 0.22546(6) 0.09926(5) 0.01752(15) Uani 1 1 d . . .
C12 C 0.69915(9) 0.23338(6) 0.08560(5) 0.01803(15) Uani 1 1 d . . .
C13 C 0.61481(10) 0.16524(7) 0.06614(6) 0.02441(18) Uani 1 1 d . . .
H13 H 0.6440 0.1070 0.0675 0.029 Uiso 1 1 calc R . .
C14 C 0.48812(10) 0.18298(8) 0.04475(7) 0.0312(2) Uani 1 1 d . . .
H14 H 0.4311 0.1371 0.0298 0.037 Uiso 1 1 calc R . .
C15 C 0.44540(10) 0.26842(8) 0.04538(7) 0.0317(2) Uani 1 1 d . . .
H15 H 0.3590 0.2807 0.0309 0.038 Uiso 1 1 calc R . .
C16 C 0.52896(9) 0.33624(7) 0.06726(6) 0.02522(19) Uani 1 1 d . . .
H16 H 0.4975 0.3938 0.0694 0.030 Uiso 1 1 calc R . .
C17 C 0.65864(9) 0.32128(6) 0.08617(5) 0.01860(15) Uani 1 1 d . . .
C18 C 0.42809(9) 0.93302(6) 0.17103(6) 0.01917(15) Uani 1 1 d . . .
C19 C 0.52860(9) 0.98784(6) 0.19480(6) 0.02101(16) Uani 1 1 d . . .
H19 H 0.5216 1.0479 0.1825 0.025 Uiso 1 1 calc R . .
C20 C 0.63933(9) 0.95677(6) 0.23629(6) 0.02086(16) Uani 1 1 d . . .
C21 C 0.65041(9) 0.86808(6) 0.25205(6) 0.02116(16) Uani 1 1 d . . .
H21 H 0.7266 0.8463 0.2789 0.025 Uiso 1 1 calc R . .
C22 C 0.55245(9) 0.81058(6) 0.22944(5) 0.01844(15) Uani 1 1 d . . .
C23 C 0.44207(8) 0.84530(6) 0.19069(5) 0.01620(14) Uani 1 1 d . . .
N1 N 0.33675(7) 0.78844(5) 0.16948(4) 0.01722(13) Uani 1 1 d . . .
C25 C 0.23339(9) 0.78461(6) 0.20788(5) 0.01793(15) Uani 1 1 d . . .
H25 H 0.2205 0.8145 0.2558 0.022 Uiso 1 1 calc R . .
N2 N 0.15170(8) 0.73153(5) 0.16700(5) 0.01966(14) Uani 1 1 d . . .
C27 C 0.20435(10) 0.70035(6) 0.10088(6) 0.02287(18) Uani 1 1 d . . .
H27 H 0.1660 0.6616 0.0616 0.027 Uiso 1 1 calc R . .
C28 C 0.32057(10) 0.73537(6) 0.10245(5) 0.02138(17) Uani 1 1 d . . .
H28 H 0.3796 0.7255 0.0649 0.026 Uiso 1 1 calc R . .
C29 C 0.02524(10) 0.71134(7) 0.18884(6) 0.02560(19) Uani 1 1 d . . .
H29A H 0.0163 0.7350 0.2428 0.031 Uiso 1 1 calc R . .
H29B H 0.0148 0.6476 0.1911 0.031 Uiso 1 1 calc R . .
C30 C -0.07726(10) 0.74936(7) 0.12899(6) 0.02575(19) Uani 1 1 d . . .
H30A H -0.0676 0.7257 0.0752 0.031 Uiso 1 1 calc R . .
H30B H -0.1602 0.7305 0.1438 0.031 Uiso 1 1 calc R . .
C31 C -0.07492(11) 0.84790(7) 0.12493(8) 0.0322(2) Uani 1 1 d . . .
H31A H 0.0033 0.8669 0.1033 0.039 Uiso 1 1 calc R . .
H31B H -0.0745 0.8719 0.1796 0.039 Uiso 1 1 calc R . .
C32 C -0.18804(12) 0.88379(9) 0.07221(8) 0.0350(2) Uani 1 1 d . . .
H32A H -0.1899 0.8591 0.0183 0.053 Uiso 1 1 calc R . .
H32B H -0.1815 0.9471 0.0692 0.053 Uiso 1 1 calc R . .
H32C H -0.2654 0.8681 0.0952 0.053 Uiso 1 1 calc R . .
C33 C 0.30884(10) 0.96724(7) 0.12573(7) 0.0278(2) Uani 1 1 d . . .
H33A H 0.2398 0.9630 0.1595 0.042 Uiso 1 1 calc R . .
H33B H 0.2886 0.9329 0.0770 0.042 Uiso 1 1 calc R . .
H33C H 0.3208 1.0281 0.1113 0.042 Uiso 1 1 calc R . .
C34 C 0.74525(11) 1.01813(7) 0.26338(8) 0.0309(2) Uani 1 1 d . . .
H34A H 0.7385 1.0704 0.2299 0.046 Uiso 1 1 calc R . .
H34B H 0.8259 0.9896 0.2585 0.046 Uiso 1 1 calc R . .
H34C H 0.7402 1.0343 0.3194 0.046 Uiso 1 1 calc R . .
C35 C 0.56442(11) 0.71501(6) 0.24667(7) 0.0280(2) Uani 1 1 d . . .
H35A H 0.5015 0.6977 0.2820 0.042 Uiso 1 1 calc R . .
H35B H 0.6487 0.7026 0.2729 0.042 Uiso 1 1 calc R . .
H35C H 0.5508 0.6824 0.1964 0.042 Uiso 1 1 calc R . .
Ni1 Ni 0.788236(12) 0.404334(8) 0.103857(7) 0.01806(4) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.4036(17) . ?
C1 C5 1.4214(17) . ?
C1 Ni1 2.1481(10) . ?
C1 H1 0.9500 . ?
C2 C3 1.4297(17) . ?
C2 Ni1 2.1296(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.405(2) . ?
C3 Ni1 2.1181(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.410(2) . ?
C4 Ni1 2.1815(11) . ?
C4 H4 0.9500 . ?
C5 Ni1 2.1420(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.4069(13) . ?
C6 C11 1.4223(13) . ?
C6 Ni1 1.8860(9) . ?
C7 C8 1.3964(15) . ?
C7 H7 0.9500 . ?
C8 C9 1.3910(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.3916(15) . ?
C9 H9 0.9500 . ?
C10 C11 1.3987(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.4618(13) . ?
C12 C13 1.4002(13) . ?
C12 C17 1.4218(13) . ?
C13 C14 1.3923(15) . ?
C13 H13 0.9500 . ?
C14 C15 1.3935(18) . ?
C14 H14 0.9500 . ?
C15 C16 1.3986(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.4093(13) . ?
C16 H16 0.9500 . ?
C17 Ni1 1.8869(9) . ?
C18 C19 1.3922(13) . ?
C18 C23 1.3951(12) . ?
C18 C33 1.5101(14) . ?
C19 C20 1.3944(14) . ?
C19 H19 0.9500 . ?
C20 C21 1.3940(13) . ?
C20 C34 1.5086(14) . ?
C21 C22 1.3940(13) . ?
C21 H21 0.9500 . ?
C22 C23 1.3937(13) . ?
C22 C35 1.5030(13) . ?
C23 N1 1.4419(11) . ?
N1 C25 1.3387(12) . ?
N1 C28 1.3873(12) . ?
C25 N2 1.3333(11) . ?
C25 H25 0.9500 . ?
N2 C27 1.3830(13) . ?
N2 C29 1.4718(13) . ?
C27 C28 1.3531(15) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.5246(15) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.5195(16) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.5261(17) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 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 C1 C5 107.61(10) . . ?
C2 C1 Ni1 70.13(6) . . ?
C5 C1 Ni1 70.42(6) . . ?
C2 C1 H1 126.2 . . ?
C5 C1 H1 126.2 . . ?
Ni1 C1 H1 124.9 . . ?
C1 C2 C3 107.61(11) . . ?
C1 C2 Ni1 71.56(6) . . ?
C3 C2 Ni1 69.90(6) . . ?
C1 C2 H2 126.2 . . ?
C3 C2 H2 126.2 . . ?
Ni1 C2 H2 124.0 . . ?
C4 C3 C2 108.59(11) . . ?
C4 C3 Ni1 73.40(7) . . ?
C2 C3 Ni1 70.77(6) . . ?
C4 C3 H3 125.7 . . ?
C2 C3 H3 125.7 . . ?
Ni1 C3 H3 121.8 . . ?
C3 C4 C5 107.24(11) . . ?
C3 C4 Ni1 68.50(6) . . ?
C5 C4 Ni1 69.45(6) . . ?
C3 C4 H4 126.4 . . ?
C5 C4 H4 126.4 . . ?
Ni1 C4 H4 127.2 . . ?
C4 C5 C1 108.82(12) . . ?
C4 C5 Ni1 72.49(7) . . ?
C1 C5 Ni1 70.88(6) . . ?
C4 C5 H5 125.6 . . ?
C1 C5 H5 125.6 . . ?
Ni1 C5 H5 122.7 . . ?
C7 C6 C11 116.54(9) . . ?
C7 C6 Ni1 128.25(7) . . ?
C11 C6 Ni1 115.21(7) . . ?
C8 C7 C6 121.73(9) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C9 C8 C7 120.51(10) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 119.47(9) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C11 120.13(9) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C6 121.60(9) . . ?
C10 C11 C12 125.96(8) . . ?
C6 C11 C12 112.38(8) . . ?
C13 C12 C17 121.73(9) . . ?
C13 C12 C11 125.71(9) . . ?
C17 C12 C11 112.28(8) . . ?
C14 C13 C12 119.94(10) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 119.64(10) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C14 C15 C16 120.41(10) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C17 121.60(10) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C16 C17 C12 116.59(9) . . ?
C16 C17 Ni1 127.90(8) . . ?
C12 C17 Ni1 115.29(7) . . ?
C19 C18 C23 117.33(8) . . ?
C19 C18 C33 121.26(9) . . ?
C23 C18 C33 121.41(9) . . ?
C18 C19 C20 121.68(9) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C21 C20 C19 118.82(9) . . ?
C21 C20 C34 120.70(9) . . ?
C19 C20 C34 120.49(9) . . ?
C22 C21 C20 121.63(9) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
C23 C22 C21 117.34(8) . . ?
C23 C22 C35 121.10(8) . . ?
C21 C22 C35 121.56(9) . . ?
C22 C23 C18 123.14(8) . . ?
C22 C23 N1 118.95(8) . . ?
C18 C23 N1 117.92(8) . . ?
C25 N1 C28 109.03(8) . . ?
C25 N1 C23 124.84(7) . . ?
C28 N1 C23 125.87(8) . . ?
N2 C25 N1 107.99(8) . . ?
N2 C25 H25 126.0 . . ?
N1 C25 H25 126.0 . . ?
C25 N2 C27 109.04(8) . . ?
C25 N2 C29 124.83(8) . . ?
C27 N2 C29 126.12(8) . . ?
C28 C27 N2 107.27(8) . . ?
C28 C27 H27 126.4 . . ?
N2 C27 H27 126.4 . . ?
C27 C28 N1 106.66(9) . . ?
C27 C28 H28 126.7 . . ?
N1 C28 H28 126.7 . . ?
N2 C29 C30 111.76(8) . . ?
N2 C29 H29A 109.3 . . ?
C30 C29 H29A 109.3 . . ?
N2 C29 H29B 109.3 . . ?
C30 C29 H29B 109.3 . . ?
H29A C29 H29B 107.9 . . ?
C31 C30 C29 113.52(9) . . ?
C31 C30 H30A 108.9 . . ?
C29 C30 H30A 108.9 . . ?
C31 C30 H30B 108.9 . . ?
C29 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C30 C31 C32 111.84(10) . . ?
C30 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
C30 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
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 . . ?
C18 C33 H33A 109.5 . . ?
C18 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C18 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C20 C34 H34A 109.5 . . ?
C20 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C20 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C22 C35 H35A 109.5 . . ?
C22 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C22 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C6 Ni1 C17 84.76(4) . . ?
C6 Ni1 C3 104.01(5) . . ?
C17 Ni1 C3 164.59(5) . . ?
C6 Ni1 C2 111.88(4) . . ?
C17 Ni1 C2 148.40(4) . . ?
C3 Ni1 C2 39.34(5) . . ?
C6 Ni1 C5 166.07(5) . . ?
C17 Ni1 C5 105.08(5) . . ?
C3 Ni1 C5 64.27(5) . . ?
C2 Ni1 C5 64.51(5) . . ?
C6 Ni1 C1 145.28(4) . . ?
C17 Ni1 C1 114.65(4) . . ?
C3 Ni1 C1 64.82(5) . . ?
C2 Ni1 C1 38.31(5) . . ?
C5 Ni1 C1 38.70(5) . . ?
C6 Ni1 C4 128.03(5) . . ?
C17 Ni1 C4 126.74(5) . . ?
C3 Ni1 C4 38.10(6) . . ?
C2 Ni1 C4 64.52(5) . . ?
C5 Ni1 C4 38.05(5) . . ?
C1 Ni1 C4 64.25(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
C5 C1 C2 C3 0.17(12) . . . . ?
Ni1 C1 C2 C3 60.93(7) . . . . ?
C5 C1 C2 Ni1 -60.76(8) . . . . ?
C1 C2 C3 C4 2.12(13) . . . . ?
Ni1 C2 C3 C4 64.11(8) . . . . ?
C1 C2 C3 Ni1 -61.99(8) . . . . ?
C2 C3 C4 C5 -3.56(13) . . . . ?
Ni1 C3 C4 C5 58.86(8) . . . . ?
C2 C3 C4 Ni1 -62.42(8) . . . . ?
C3 C4 C5 C1 3.68(13) . . . . ?
Ni1 C4 C5 C1 61.94(8) . . . . ?
C3 C4 C5 Ni1 -58.26(8) . . . . ?
C2 C1 C5 C4 -2.39(13) . . . . ?
Ni1 C1 C5 C4 -62.96(8) . . . . ?
C2 C1 C5 Ni1 60.57(8) . . . . ?
C11 C6 C7 C8 -0.68(14) . . . . ?
Ni1 C6 C7 C8 -179.90(8) . . . . ?
C6 C7 C8 C9 -0.64(16) . . . . ?
C7 C8 C9 C10 1.31(16) . . . . ?
C8 C9 C10 C11 -0.64(15) . . . . ?
C9 C10 C11 C6 -0.73(14) . . . . ?
C9 C10 C11 C12 176.40(9) . . . . ?
C7 C6 C11 C10 1.36(13) . . . . ?
Ni1 C6 C11 C10 -179.32(7) . . . . ?
C7 C6 C11 C12 -176.13(8) . . . . ?
Ni1 C6 C11 C12 3.20(10) . . . . ?
C10 C11 C12 C13 -5.42(15) . . . . ?
C6 C11 C12 C13 171.93(9) . . . . ?
C10 C11 C12 C17 -179.42(9) . . . . ?
C6 C11 C12 C17 -2.07(11) . . . . ?
C17 C12 C13 C14 1.59(15) . . . . ?
C11 C12 C13 C14 -171.88(9) . . . . ?
C12 C13 C14 C15 -2.07(16) . . . . ?
C13 C14 C15 C16 0.07(17) . . . . ?
C14 C15 C16 C17 2.52(17) . . . . ?
C15 C16 C17 C12 -2.93(14) . . . . ?
C15 C16 C17 Ni1 171.43(8) . . . . ?
C13 C12 C17 C16 0.89(13) . . . . ?
C11 C12 C17 C16 175.16(8) . . . . ?
C13 C12 C17 Ni1 -174.19(7) . . . . ?
C11 C12 C17 Ni1 0.08(10) . . . . ?
C23 C18 C19 C20 0.29(14) . . . . ?
C33 C18 C19 C20 -179.66(9) . . . . ?
C18 C19 C20 C21 1.94(14) . . . . ?
C18 C19 C20 C34 -178.22(9) . . . . ?
C19 C20 C21 C22 -1.89(14) . . . . ?
C34 C20 C21 C22 178.26(10) . . . . ?
C20 C21 C22 C23 -0.38(14) . . . . ?
C20 C21 C22 C35 -179.84(10) . . . . ?
C21 C22 C23 C18 2.77(13) . . . . ?
C35 C22 C23 C18 -177.76(9) . . . . ?
C21 C22 C23 N1 -177.35(8) . . . . ?
C35 C22 C23 N1 2.12(13) . . . . ?
C19 C18 C23 C22 -2.73(13) . . . . ?
C33 C18 C23 C22 177.22(9) . . . . ?
C19 C18 C23 N1 177.39(8) . . . . ?
C33 C18 C23 N1 -2.66(13) . . . . ?
C22 C23 N1 C25 104.83(11) . . . . ?
C18 C23 N1 C25 -75.28(11) . . . . ?
C22 C23 N1 C28 -81.61(11) . . . . ?
C18 C23 N1 C28 98.28(11) . . . . ?
C28 N1 C25 N2 -0.60(10) . . . . ?
C23 N1 C25 N2 173.88(8) . . . . ?
N1 C25 N2 C27 0.22(10) . . . . ?
N1 C25 N2 C29 -178.78(8) . . . . ?
C25 N2 C27 C28 0.25(11) . . . . ?
C29 N2 C27 C28 179.24(9) . . . . ?
N2 C27 C28 N1 -0.60(11) . . . . ?
C25 N1 C28 C27 0.76(11) . . . . ?
C23 N1 C28 C27 -173.66(8) . . . . ?
C25 N2 C29 C30 111.50(10) . . . . ?
C27 N2 C29 C30 -67.33(13) . . . . ?
N2 C29 C30 C31 -62.73(12) . . . . ?
C29 C30 C31 C32 -173.04(10) . . . . ?
C7 C6 Ni1 C17 176.67(9) . . . . ?
C11 C6 Ni1 C17 -2.56(7) . . . . ?
C7 C6 Ni1 C3 9.55(10) . . . . ?
C11 C6 Ni1 C3 -169.69(7) . . . . ?
C7 C6 Ni1 C2 -31.09(10) . . . . ?
C11 C6 Ni1 C2 149.67(7) . . . . ?
C7 C6 Ni1 C5 41.0(2) . . . . ?
C11 C6 Ni1 C5 -138.21(17) . . . . ?
C7 C6 Ni1 C1 -56.25(12) . . . . ?
C11 C6 Ni1 C1 124.52(8) . . . . ?
C7 C6 Ni1 C4 42.98(11) . . . . ?
C11 C6 Ni1 C4 -136.25(7) . . . . ?
C16 C17 Ni1 C6 -173.07(9) . . . . ?
C12 C17 Ni1 C6 1.35(7) . . . . ?
C16 C17 Ni1 C3 -47.5(2) . . . . ?
C12 C17 Ni1 C3 126.92(15) . . . . ?
C16 C17 Ni1 C2 62.52(12) . . . . ?
C12 C17 Ni1 C2 -123.05(9) . . . . ?
C16 C17 Ni1 C5 -3.11(10) . . . . ?
C12 C17 Ni1 C5 171.31(7) . . . . ?
C16 C17 Ni1 C1 36.92(10) . . . . ?
C12 C17 Ni1 C1 -148.65(7) . . . . ?
C16 C17 Ni1 C4 -38.37(11) . . . . ?
C12 C17 Ni1 C4 136.06(7) . . . . ?
C4 C3 Ni1 C6 135.30(7) . . . . ?
C2 C3 Ni1 C6 -107.55(7) . . . . ?
C4 C3 Ni1 C17 11.9(2) . . . . ?
C2 C3 Ni1 C17 129.05(16) . . . . ?
C4 C3 Ni1 C2 -117.15(10) . . . . ?
C4 C3 Ni1 C5 -36.68(7) . . . . ?
C2 C3 Ni1 C5 80.47(8) . . . . ?
C4 C3 Ni1 C1 -79.73(8) . . . . ?
C2 C3 Ni1 C1 37.42(7) . . . . ?
C2 C3 Ni1 C4 117.15(10) . . . . ?
C1 C2 Ni1 C6 -157.01(6) . . . . ?
C3 C2 Ni1 C6 85.50(8) . . . . ?
C1 C2 Ni1 C17 -39.31(11) . . . . ?
C3 C2 Ni1 C17 -156.80(8) . . . . ?
C1 C2 Ni1 C3 117.49(10) . . . . ?
C1 C2 Ni1 C5 37.69(7) . . . . ?
C3 C2 Ni1 C5 -79.80(8) . . . . ?
C3 C2 Ni1 C1 -117.49(10) . . . . ?
C1 C2 Ni1 C4 80.03(8) . . . . ?
C3 C2 Ni1 C4 -37.46(8) . . . . ?
C4 C5 Ni1 C6 2.5(2) . . . . ?
C1 C5 Ni1 C6 -115.37(18) . . . . ?
C4 C5 Ni1 C17 -131.37(8) . . . . ?
C1 C5 Ni1 C17 110.77(7) . . . . ?
C4 C5 Ni1 C3 36.72(8) . . . . ?
C1 C5 Ni1 C3 -81.14(8) . . . . ?
C4 C5 Ni1 C2 80.55(9) . . . . ?
C1 C5 Ni1 C2 -37.31(7) . . . . ?
C4 C5 Ni1 C1 117.86(11) . . . . ?
C1 C5 Ni1 C4 -117.86(11) . . . . ?
C2 C1 Ni1 C6 39.52(10) . . . . ?
C5 C1 Ni1 C6 157.55(8) . . . . ?
C2 C1 Ni1 C17 158.58(7) . . . . ?
C5 C1 Ni1 C17 -83.39(8) . . . . ?
C2 C1 Ni1 C3 -38.42(7) . . . . ?
C5 C1 Ni1 C3 79.61(8) . . . . ?
C5 C1 Ni1 C2 118.03(10) . . . . ?
C2 C1 Ni1 C5 -118.03(10) . . . . ?
C2 C1 Ni1 C4 -80.80(8) . . . . ?
C5 C1 Ni1 C4 37.23(8) . . . . ?
C3 C4 Ni1 C6 -60.04(9) . . . . ?
C5 C4 Ni1 C6 -179.24(7) . . . . ?
C3 C4 Ni1 C17 -176.08(7) . . . . ?
C5 C4 Ni1 C17 64.73(9) . . . . ?
C5 C4 Ni1 C3 -119.19(11) . . . . ?
C3 C4 Ni1 C2 38.67(7) . . . . ?
C5 C4 Ni1 C2 -80.53(8) . . . . ?
C3 C4 Ni1 C5 119.19(11) . . . . ?
C3 C4 Ni1 C1 81.34(8) . . . . ?
C5 C4 Ni1 C1 -37.85(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        34.95
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.055
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1038672'
_audit_update_record             
;
2014-12-10 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H40 N2 Ni'
_chemical_formula_weight         583.43

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'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   13.4758(2)
_cell_length_b                   13.6096(2)
_cell_length_c                   17.1452(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.054(2)
_cell_angle_gamma                90
_cell_volume                     3036.52(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    12549
_cell_measurement_theta_min      3.2302
_cell_measurement_theta_max      33.3561

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.630
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.290
_exptl_absorpt_coefficient_mu    0.668
_shelx_estimated_absorpt_T_min   0.678
_shelx_estimated_absorpt_T_max   0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_reflns_number            24629
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.237
_diffrn_reflns_theta_max         33.432
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10953
_reflns_number_gt                9418
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?


_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0406P)²+1.2950P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10953
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_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
Ni1 Ni 0.85600(2) 0.78039(2) 0.77955(2) 0.01110(4) Uani 1 1 d . . . . .
N1 N 0.95398(7) 0.71895(7) 0.94390(6) 0.01410(17) Uani 1 1 d . . . . .
N2 N 0.79300(7) 0.75297(8) 0.92752(6) 0.01392(17) Uani 1 1 d . . . . .
C1 C 0.86830(8) 0.74826(8) 0.88842(6) 0.01166(17) Uani 1 1 d . . . . .
C2 C 0.93630(9) 0.69404(10) 1.02285(7) 0.0179(2) Uani 1 1 d . . . . .
H2A H 0.9860 0.7281 1.0674 0.022 Uiso 1 1 calc R U . . .
H2B H 0.9413 0.6223 1.0326 0.022 Uiso 1 1 calc R U . . .
C3 C 0.82781(9) 0.73065(10) 1.01431(7) 0.0196(2) Uani 1 1 d . . . . .
H3A H 0.7845 0.6794 1.0299 0.024 Uiso 1 1 calc R U . . .
H3B H 0.8273 0.7901 1.0474 0.024 Uiso 1 1 calc R U . . .
C4 C 1.04866(8) 0.68402(9) 0.93117(6) 0.01395(19) Uani 1 1 d . . . . .
C5 C 1.05261(9) 0.58877(9) 0.90113(7) 0.0160(2) Uani 1 1 d . . . . .
C6 C 1.14799(9) 0.55031(9) 0.90020(7) 0.0188(2) Uani 1 1 d . . . . .
H6 H 1.1518 0.4856 0.8804 0.023 Uiso 1 1 calc R U . . .
C7 C 1.23816(9) 0.60460(10) 0.92771(7) 0.0188(2) Uani 1 1 d . . . . .
C8 C 1.23121(9) 0.69902(10) 0.95555(7) 0.0179(2) Uani 1 1 d . . . . .
H8 H 1.2920 0.7371 0.9729 0.021 Uiso 1 1 calc R U . . .
C9 C 1.13740(8) 0.74012(9) 0.95901(7) 0.01494(19) Uani 1 1 d . . . . .
C10 C 0.95636(9) 0.52983(9) 0.86893(8) 0.0220(2) Uani 1 1 d . . . . .
H10A H 0.9734 0.4684 0.8455 0.033 Uiso 1 1 calc R U . . .
H10B H 0.9080 0.5678 0.8272 0.033 Uiso 1 1 calc R U . . .
H10C H 0.9248 0.5148 0.9130 0.033 Uiso 1 1 calc R U . . .
C11 C 1.34032(10) 0.56155(12) 0.92564(9) 0.0285(3) Uani 1 1 d . . . . .
H11A H 1.3462 0.5608 0.8699 0.043 Uiso 1 1 calc R U . . .
H11B H 1.3455 0.4943 0.9467 0.043 Uiso 1 1 calc R U . . .
H11C H 1.3958 0.6016 0.9590 0.043 Uiso 1 1 calc R U . . .
C12 C 1.13521(9) 0.84124(9) 0.99279(7) 0.0195(2) Uani 1 1 d . . . . .
H12A H 1.0638 0.8616 0.9862 0.029 Uiso 1 1 calc R U . . .
H12B H 1.1691 0.8872 0.9640 0.029 Uiso 1 1 calc R U . . .
H12C H 1.1713 0.8411 1.0503 0.029 Uiso 1 1 calc R U . . .
C13 C 0.68558(8) 0.76815(8) 0.89300(7) 0.01357(19) Uani 1 1 d . . . . .
C14 C 0.64412(9) 0.86229(9) 0.88976(7) 0.0170(2) Uani 1 1 d . . . . .
C15 C 0.53865(9) 0.87380(10) 0.85618(9) 0.0235(2) Uani 1 1 d . . . . .
H15 H 0.5096 0.9377 0.8529 0.028 Uiso 1 1 calc R U . . .
C16 C 0.47515(9) 0.79423(11) 0.82740(9) 0.0248(3) Uani 1 1 d . . . . .
C17 C 0.51832(9) 0.70115(10) 0.83424(8) 0.0215(2) Uani 1 1 d . . . . .
H17 H 0.4753 0.6461 0.8156 0.026 Uiso 1 1 calc R U . . .
C18 C 0.62290(9) 0.68591(9) 0.86759(7) 0.0166(2) Uani 1 1 d . . . . .
C19 C 0.70922(10) 0.95050(10) 0.92018(9) 0.0241(3) Uani 1 1 d . . . . .
H19A H 0.7690 0.9306 0.9634 0.036 Uiso 1 1 calc R U . . .
H19B H 0.6688 0.9987 0.9413 0.036 Uiso 1 1 calc R U . . .
H19C H 0.7325 0.9799 0.8758 0.036 Uiso 1 1 calc R U . . .
C20 C 0.36158(10) 0.80846(16) 0.79019(12) 0.0401(4) Uani 1 1 d . . . . .
H20A H 0.3233 0.7889 0.8290 0.060 Uiso 1 1 calc R U . . .
H20B H 0.3399 0.7680 0.7415 0.060 Uiso 1 1 calc R U . . .
H20C H 0.3479 0.8778 0.7759 0.060 Uiso 1 1 calc R U . . .
C21 C 0.66518(11) 0.58337(9) 0.87366(8) 0.0234(2) Uani 1 1 d . . . . .
H21A H 0.6692 0.5570 0.9276 0.035 Uiso 1 1 calc R U . . .
H21B H 0.7340 0.5844 0.8645 0.035 Uiso 1 1 calc R U . . .
H21C H 0.6199 0.5417 0.8329 0.035 Uiso 1 1 calc R U . . .
C22 C 0.75392(10) 0.67463(10) 0.70770(8) 0.0227(2) Uani 1 1 d . . . . .
H22 H 0.7435 0.6119 0.7285 0.027 Uiso 1 1 calc R U . . .
C23 C 0.69227(9) 0.76026(11) 0.70843(7) 0.0209(2) Uani 1 1 d . . . . .
H23 H 0.6324 0.7633 0.7279 0.025 Uiso 1 1 calc R U . . .
C24 C 0.73463(9) 0.83741(10) 0.67612(7) 0.0202(2) Uani 1 1 d . . . . .
H24 H 0.7088 0.9026 0.6687 0.024 Uiso 1 1 calc R U . . .
C25 C 0.82420(9) 0.80169(10) 0.65580(7) 0.0194(2) Uani 1 1 d . . . . .
H25 H 0.8706 0.8403 0.6355 0.023 Uiso 1 1 calc R U . . .
C26 C 0.83267(9) 0.69952(10) 0.67077(7) 0.0213(2) Uani 1 1 d . . . . .
H26 H 0.8817 0.6562 0.6584 0.026 Uiso 1 1 calc R U . . .
C27 C 0.96376(8) 0.87687(8) 0.80085(6) 0.01282(18) Uani 1 1 d . . . . .
C28 C 0.95372(9) 0.95816(9) 0.84839(7) 0.0165(2) Uani 1 1 d . . . . .
H28 H 0.8981 0.9590 0.8729 0.020 Uiso 1 1 calc R U . . .
C29 C 1.02089(10) 1.03782(9) 0.86157(8) 0.0202(2) Uani 1 1 d . . . . .
H29 H 1.0101 1.0916 0.8937 0.024 Uiso 1 1 calc R U . . .
C30 C 1.10368(9) 1.03818(9) 0.82751(8) 0.0200(2) Uani 1 1 d . . . . .
H30 H 1.1511 1.0913 0.8368 0.024 Uiso 1 1 calc R U . . .
C31 C 1.11566(9) 0.95947(9) 0.77969(7) 0.0171(2) Uani 1 1 d . . . . .
H31 H 1.1720 0.9594 0.7560 0.020 Uiso 1 1 calc R U . . .
C32 C 1.04749(8) 0.87985(8) 0.76505(6) 0.01343(18) Uani 1 1 d . . . . .
C33 C 1.06794(8) 0.80243(9) 0.70983(7) 0.01402(19) Uani 1 1 d . . . . .
C34 C 1.06060(9) 0.82352(10) 0.62874(7) 0.0202(2) Uani 1 1 d . . . . .
H34 H 1.0420 0.8879 0.6088 0.024 Uiso 1 1 calc R U . . .
C35 C 1.08002(11) 0.75210(12) 0.57664(8) 0.0263(3) Uani 1 1 d . . . . .
H35 H 1.0730 0.7674 0.5214 0.032 Uiso 1 1 calc R U . . .
C36 C 1.10958(10) 0.65853(11) 0.60540(8) 0.0260(3) Uani 1 1 d . . . . .
H36 H 1.1232 0.6095 0.5701 0.031 Uiso 1 1 calc R U . . .
C37 C 1.11920(10) 0.63692(10) 0.68599(8) 0.0222(2) Uani 1 1 d . . . . .
H37 H 1.1405 0.5732 0.7062 0.027 Uiso 1 1 calc R U . . .
C38 C 1.09788(9) 0.70809(9) 0.73737(7) 0.0174(2) Uani 1 1 d . . . . .
H38 H 1.1038 0.6921 0.7923 0.021 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.8821(11) . ?
Ni1 C27 1.9211(11) . ?
Ni1 C25 2.0729(11) . ?
Ni1 C26 2.1175(12) . ?
Ni1 C22 2.1450(12) . ?
Ni1 C24 2.2171(11) . ?
Ni1 C23 2.2434(11) . ?
N1 C1 1.3514(13) . ?
N1 C4 1.4305(14) . ?
N1 C2 1.4737(14) . ?
N2 C1 1.3553(14) . ?
N2 C13 1.4294(14) . ?
N2 C3 1.4710(15) . ?
C2 C3 1.5152(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.3944(15) . ?
C4 C5 1.4010(16) . ?
C5 C6 1.3917(16) . ?
C5 C10 1.5029(16) . ?
C6 C7 1.3954(18) . ?
C6 H6 0.9500 . ?
C7 C8 1.3824(18) . ?
C7 C11 1.5050(17) . ?
C8 C9 1.3977(16) . ?
C8 H8 0.9500 . ?
C9 C12 1.4963(17) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.3931(16) . ?
C13 C18 1.4018(16) . ?
C14 C15 1.3968(16) . ?
C14 C19 1.4983(17) . ?
C15 C16 1.389(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(2) . ?
C16 C20 1.5099(18) . ?
C17 C18 1.3919(17) . ?
C17 H17 0.9500 . ?
C18 C21 1.5007(18) . ?
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 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C26 1.4110(19) . ?
C22 C23 1.433(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3783(18) . ?
C23 H23 0.9500 . ?
C24 C25 1.4259(17) . ?
C24 H24 0.9500 . ?
C25 C26 1.4132(19) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.4014(16) . ?
C27 C32 1.4183(15) . ?
C28 C29 1.3927(16) . ?
C28 H28 0.9500 . ?
C29 C30 1.3871(17) . ?
C29 H29 0.9500 . ?
C30 C31 1.3837(17) . ?
C30 H30 0.9500 . ?
C31 C32 1.4005(16) . ?
C31 H31 0.9500 . ?
C32 C33 1.4894(16) . ?
C33 C38 1.3911(16) . ?
C33 C34 1.3977(16) . ?
C34 C35 1.3902(19) . ?
C34 H34 0.9500 . ?
C35 C36 1.386(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.3855(19) . ?
C36 H36 0.9500 . ?
C37 C38 1.3886(17) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?

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
C1 Ni1 C27 95.89(5) . . ?
C1 Ni1 C25 171.55(5) . . ?
C27 Ni1 C25 92.53(5) . . ?
C1 Ni1 C26 135.03(5) . . ?
C27 Ni1 C26 117.05(5) . . ?
C25 Ni1 C26 39.40(5) . . ?
C1 Ni1 C22 106.96(5) . . ?
C27 Ni1 C22 155.25(5) . . ?
C25 Ni1 C22 64.84(5) . . ?
C26 Ni1 C22 38.65(5) . . ?
C1 Ni1 C24 136.99(5) . . ?
C27 Ni1 C24 106.08(5) . . ?
C25 Ni1 C24 38.64(5) . . ?
C26 Ni1 C24 64.38(5) . . ?
C22 Ni1 C24 62.98(5) . . ?
C1 Ni1 C23 109.36(4) . . ?
C27 Ni1 C23 140.80(5) . . ?
C25 Ni1 C23 63.13(4) . . ?
C26 Ni1 C23 63.75(5) . . ?
C22 Ni1 C23 38.04(5) . . ?
C24 Ni1 C23 35.99(5) . . ?
C1 N1 C4 128.58(9) . . ?
C1 N1 C2 113.70(9) . . ?
C4 N1 C2 115.28(9) . . ?
C1 N2 C13 127.58(9) . . ?
C1 N2 C3 114.05(9) . . ?
C13 N2 C3 118.12(9) . . ?
N1 C1 N2 106.16(9) . . ?
N1 C1 Ni1 127.28(8) . . ?
N2 C1 Ni1 126.53(8) . . ?
N1 C2 C3 102.58(9) . . ?
N1 C2 H2A 111.3 . . ?
C3 C2 H2A 111.3 . . ?
N1 C2 H2B 111.3 . . ?
C3 C2 H2B 111.3 . . ?
H2A C2 H2B 109.2 . . ?
N2 C3 C2 102.23(9) . . ?
N2 C3 H3A 111.3 . . ?
C2 C3 H3A 111.3 . . ?
N2 C3 H3B 111.3 . . ?
C2 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
C9 C4 C5 121.43(10) . . ?
C9 C4 N1 119.04(10) . . ?
C5 C4 N1 118.96(10) . . ?
C6 C5 C4 118.40(11) . . ?
C6 C5 C10 120.44(11) . . ?
C4 C5 C10 121.15(10) . . ?
C5 C6 C7 121.51(12) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C6 118.54(11) . . ?
C8 C7 C11 120.96(12) . . ?
C6 C7 C11 120.49(12) . . ?
C7 C8 C9 121.99(11) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 H8 119.0 . . ?
C4 C9 C8 118.10(11) . . ?
C4 C9 C12 122.32(10) . . ?
C8 C9 C12 119.57(10) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 121.26(10) . . ?
C14 C13 N2 120.13(10) . . ?
C18 C13 N2 118.49(10) . . ?
C13 C14 C15 118.30(11) . . ?
C13 C14 C19 122.04(10) . . ?
C15 C14 C19 119.65(11) . . ?
C16 C15 C14 121.74(12) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C17 C16 C15 118.44(11) . . ?
C17 C16 C20 120.67(14) . . ?
C15 C16 C20 120.90(14) . . ?
C16 C17 C18 121.92(12) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C17 C18 C13 118.21(11) . . ?
C17 C18 C21 119.52(11) . . ?
C13 C18 C21 122.26(11) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C26 C22 C23 108.30(12) . . ?
C26 C22 Ni1 69.62(7) . . ?
C23 C22 Ni1 74.70(7) . . ?
C26 C22 H22 125.9 . . ?
C23 C22 H22 125.9 . . ?
Ni1 C22 H22 121.5 . . ?
C24 C23 C22 108.32(11) . . ?
C24 C23 Ni1 70.96(7) . . ?
C22 C23 Ni1 67.26(7) . . ?
C24 C23 H23 125.8 . . ?
C22 C23 H23 125.8 . . ?
Ni1 C23 H23 127.5 . . ?
C23 C24 C25 107.68(12) . . ?
C23 C24 Ni1 73.04(7) . . ?
C25 C24 Ni1 65.20(6) . . ?
C23 C24 H24 126.2 . . ?
C25 C24 H24 126.2 . . ?
Ni1 C24 H24 127.1 . . ?
C26 C25 C24 108.94(11) . . ?
C26 C25 Ni1 72.00(7) . . ?
C24 C25 Ni1 76.15(7) . . ?
C26 C25 H25 125.5 . . ?
C24 C25 H25 125.5 . . ?
Ni1 C25 H25 118.2 . . ?
C22 C26 C25 106.44(11) . . ?
C22 C26 Ni1 71.73(7) . . ?
C25 C26 Ni1 68.60(7) . . ?
C22 C26 H26 126.8 . . ?
C25 C26 H26 126.8 . . ?
Ni1 C26 H26 124.5 . . ?
C28 C27 C32 115.92(10) . . ?
C28 C27 Ni1 117.89(8) . . ?
C32 C27 Ni1 125.75(8) . . ?
C29 C28 C27 123.50(11) . . ?
C29 C28 H28 118.2 . . ?
C27 C28 H28 118.2 . . ?
C30 C29 C28 119.63(11) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C31 C30 C29 118.50(11) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
C30 C31 C32 122.22(11) . . ?
C30 C31 H31 118.9 . . ?
C32 C31 H31 118.9 . . ?
C31 C32 C27 120.20(10) . . ?
C31 C32 C33 116.12(10) . . ?
C27 C32 C33 123.66(10) . . ?
C38 C33 C34 117.81(11) . . ?
C38 C33 C32 121.49(10) . . ?
C34 C33 C32 120.66(11) . . ?
C35 C34 C33 121.26(12) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C36 C35 C34 119.90(12) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C37 C36 C35 119.57(12) . . ?
C37 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
C36 C37 C38 120.22(13) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C37 C38 C33 121.20(11) . . ?
C37 C38 H38 119.4 . . ?
C33 C38 H38 119.4 . . ?

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
C4 N1 C1 N2 166.38(11) . . . . ?
C2 N1 C1 N2 5.14(13) . . . . ?
C4 N1 C1 Ni1 -15.49(17) . . . . ?
C2 N1 C1 Ni1 -176.72(8) . . . . ?
C13 N2 C1 N1 -171.31(11) . . . . ?
C3 N2 C1 N1 2.77(13) . . . . ?
C13 N2 C1 Ni1 10.53(17) . . . . ?
C3 N2 C1 Ni1 -175.39(9) . . . . ?
C27 Ni1 C1 N1 -54.50(11) . . . . ?
C26 Ni1 C1 N1 84.11(11) . . . . ?
C22 Ni1 C1 N1 115.91(10) . . . . ?
C24 Ni1 C1 N1 -175.76(9) . . . . ?
C23 Ni1 C1 N1 155.96(10) . . . . ?
C27 Ni1 C1 N2 123.28(10) . . . . ?
C26 Ni1 C1 N2 -98.12(11) . . . . ?
C22 Ni1 C1 N2 -66.31(11) . . . . ?
C24 Ni1 C1 N2 2.02(14) . . . . ?
C23 Ni1 C1 N2 -26.27(11) . . . . ?
C1 N1 C2 C3 -10.37(14) . . . . ?
C4 N1 C2 C3 -174.22(10) . . . . ?
C1 N2 C3 C2 -8.89(14) . . . . ?
C13 N2 C3 C2 165.79(10) . . . . ?
N1 C2 C3 N2 10.58(12) . . . . ?
C1 N1 C4 C9 113.86(13) . . . . ?
C2 N1 C4 C9 -85.14(13) . . . . ?
C1 N1 C4 C5 -74.70(15) . . . . ?
C2 N1 C4 C5 86.29(13) . . . . ?
C9 C4 C5 C6 0.56(16) . . . . ?
N1 C4 C5 C6 -170.66(10) . . . . ?
C9 C4 C5 C10 -178.16(11) . . . . ?
N1 C4 C5 C10 10.62(16) . . . . ?
C4 C5 C6 C7 -0.51(17) . . . . ?
C10 C5 C6 C7 178.23(11) . . . . ?
C5 C6 C7 C8 -0.68(17) . . . . ?
C5 C6 C7 C11 -179.65(11) . . . . ?
C6 C7 C8 C9 1.87(17) . . . . ?
C11 C7 C8 C9 -179.17(11) . . . . ?
C5 C4 C9 C8 0.56(16) . . . . ?
N1 C4 C9 C8 171.77(10) . . . . ?
C5 C4 C9 C12 -178.81(10) . . . . ?
N1 C4 C9 C12 -7.60(16) . . . . ?
C7 C8 C9 C4 -1.81(17) . . . . ?
C7 C8 C9 C12 177.58(11) . . . . ?
C1 N2 C13 C14 -95.17(14) . . . . ?
C3 N2 C13 C14 90.96(14) . . . . ?
C1 N2 C13 C18 88.83(14) . . . . ?
C3 N2 C13 C18 -85.03(13) . . . . ?
C18 C13 C14 C15 -3.57(17) . . . . ?
N2 C13 C14 C15 -179.45(11) . . . . ?
C18 C13 C14 C19 177.12(11) . . . . ?
N2 C13 C14 C19 1.23(17) . . . . ?
C13 C14 C15 C16 0.85(19) . . . . ?
C19 C14 C15 C16 -179.81(13) . . . . ?
C14 C15 C16 C17 1.5(2) . . . . ?
C14 C15 C16 C20 -179.09(14) . . . . ?
C15 C16 C17 C18 -1.1(2) . . . . ?
C20 C16 C17 C18 179.40(13) . . . . ?
C16 C17 C18 C13 -1.45(18) . . . . ?
C16 C17 C18 C21 179.79(12) . . . . ?
C14 C13 C18 C17 3.86(17) . . . . ?
N2 C13 C18 C17 179.81(10) . . . . ?
C14 C13 C18 C21 -177.42(11) . . . . ?
N2 C13 C18 C21 -1.47(16) . . . . ?
C26 C22 C23 C24 -2.67(14) . . . . ?
Ni1 C22 C23 C24 59.25(9) . . . . ?
C26 C22 C23 Ni1 -61.91(8) . . . . ?
C22 C23 C24 C25 -0.85(13) . . . . ?
Ni1 C23 C24 C25 56.12(8) . . . . ?
C22 C23 C24 Ni1 -56.98(8) . . . . ?
C23 C24 C25 C26 4.08(13) . . . . ?
Ni1 C24 C25 C26 65.10(8) . . . . ?
C23 C24 C25 Ni1 -61.02(9) . . . . ?
C23 C22 C26 C25 5.08(13) . . . . ?
Ni1 C22 C26 C25 -60.12(8) . . . . ?
C23 C22 C26 Ni1 65.20(8) . . . . ?
C24 C25 C26 C22 -5.64(13) . . . . ?
Ni1 C25 C26 C22 62.17(8) . . . . ?
C24 C25 C26 Ni1 -67.82(8) . . . . ?
C32 C27 C28 C29 -0.55(17) . . . . ?
Ni1 C27 C28 C29 -173.36(9) . . . . ?
C27 C28 C29 C30 -0.92(19) . . . . ?
C28 C29 C30 C31 1.33(18) . . . . ?
C29 C30 C31 C32 -0.28(18) . . . . ?
C30 C31 C32 C27 -1.23(17) . . . . ?
C30 C31 C32 C33 177.72(11) . . . . ?
C28 C27 C32 C31 1.59(15) . . . . ?
Ni1 C27 C32 C31 173.76(8) . . . . ?
C28 C27 C32 C33 -177.27(10) . . . . ?
Ni1 C27 C32 C33 -5.11(15) . . . . ?
C31 C32 C33 C38 113.43(12) . . . . ?
C27 C32 C33 C38 -67.67(15) . . . . ?
C31 C32 C33 C34 -64.58(14) . . . . ?
C27 C32 C33 C34 114.33(13) . . . . ?
C38 C33 C34 C35 1.57(18) . . . . ?
C32 C33 C34 C35 179.65(11) . . . . ?
C33 C34 C35 C36 -1.5(2) . . . . ?
C34 C35 C36 C37 0.2(2) . . . . ?
C35 C36 C37 C38 1.0(2) . . . . ?
C36 C37 C38 C33 -0.88(19) . . . . ?
C34 C33 C38 C37 -0.38(17) . . . . ?
C32 C33 C38 C37 -178.44(11) . . . . ?

_refine_diff_density_max         0.468
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.060

_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_7
_database_code_depnum_ccdc_archive 'CCDC 1038673'
_audit_update_record             
;
2014-12-10 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C21 H27 N2)1+ 3, NiCl4 2-, Cl1-, 6(C H2  Cl2)'
_chemical_formula_sum            'C69 H93 Cl17 N6 Ni'
_chemical_formula_weight         1667.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c :H'
_space_group_name_Hall           'R 3 -2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-y+2/3, -x+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-y+1/3, -x+2/3, z+7/6'

_cell_length_a                   15.3884(4)
_cell_length_b                   15.3884(4)
_cell_length_c                   61.781(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     12669.9(8)
_cell_formula_units_Z            6
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    24781
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      26.73

_exptl_crystal_description       plate
_exptl_crystal_colour            willow-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_F_000             5196
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.808
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.60318
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
;
 Data collection Nonius Kappa CCD diffractometer Absorption 
correction: multi-scan (DENZO and SCALEPACK; (2011) 
by Seyma Goren Keskin , Julie M. Stanley , Michelle L. Mejia ,
 Bradley J. Holliday , T Min , T Max
;

_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaApexII
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            51307
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_theta_min         2.826
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5990
_reflns_number_gt                5395
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.996

_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       'COLLECT (Nonius B.V., 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0900P)²+32.5710P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5990
_refine_ls_number_parameters     297
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1693
_refine_ls_wR_factor_gt          0.1636
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_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
N11 N 0.5419(4) 0.5056(4) 0.63066(8) 0.0419(10) Uani 1 1 d . . . . .
N21 N 0.5587(4) 0.5163(4) 0.59535(8) 0.0415(11) Uani 1 1 d . . . . .
C1 C 0.5552(4) 0.4667(4) 0.61290(10) 0.0417(12) Uani 1 1 d . . . . .
H1 H 0.5616 0.4084 0.6128 0.050 Uiso 1 1 calc R U . . .
C2 C 0.5398(5) 0.5990(4) 0.62564(10) 0.0435(12) Uani 1 1 d . . . . .
H2A H 0.5969 0.6583 0.6325 0.052 Uiso 1 1 calc R U . . .
H2B H 0.4763 0.5942 0.6305 0.052 Uiso 1 1 calc R U . . .
C3 C 0.5486(4) 0.6041(4) 0.60071(10) 0.0414(12) Uani 1 1 d . . . . .
H3A H 0.4878 0.5990 0.5940 0.050 Uiso 1 1 calc R U . . .
H3B H 0.6082 0.6672 0.5959 0.050 Uiso 1 1 calc R U . . .
C11 C 0.5372(5) 0.4706(5) 0.65238(10) 0.0464(13) Uani 1 1 d . . . . .
C12 C 0.4454(5) 0.4222(5) 0.66287(12) 0.0577(16) Uani 1 1 d . . . . .
C13 C 0.4435(6) 0.3913(5) 0.68410(13) 0.0640(19) Uani 1 1 d . . . . .
H13 H 0.3813 0.3571 0.6916 0.077 Uiso 1 1 calc R U . . .
C14 C 0.5304(6) 0.4094(5) 0.69449(11) 0.0584(18) Uani 1 1 d . . . . .
C15 C 0.6214(6) 0.4579(5) 0.68365(11) 0.0548(16) Uani 1 1 d . . . . .
H15 H 0.6807 0.4690 0.6908 0.066 Uiso 1 1 calc R U . . .
C16 C 0.6274(5) 0.4910(4) 0.66223(9) 0.0435(12) Uani 1 1 d . . . . .
C17 C 0.3496(6) 0.4015(8) 0.65133(19) 0.091(3) Uani 1 1 d . . . . .
H17A H 0.3510 0.4650 0.6487 0.137 Uiso 1 1 calc R U . . .
H17B H 0.2915 0.3581 0.6604 0.137 Uiso 1 1 calc R U . . .
H17C H 0.3445 0.3681 0.6375 0.137 Uiso 1 1 calc R U . . .
C18 C 0.5252(8) 0.3746(6) 0.71775(12) 0.078(3) Uani 1 1 d . . . . .
H18A H 0.5162 0.4197 0.7275 0.117 Uiso 1 1 calc R U . . .
H18B H 0.5876 0.3756 0.7214 0.117 Uiso 1 1 calc R U . . .
H18C H 0.4685 0.3062 0.7193 0.117 Uiso 1 1 calc R U . . .
C19 C 0.7260(5) 0.5448(6) 0.65078(11) 0.0531(15) Uani 1 1 d . . . . .
H19A H 0.7272 0.5027 0.6390 0.080 Uiso 1 1 calc R U . . .
H19B H 0.7802 0.5593 0.6610 0.080 Uiso 1 1 calc R U . . .
H19C H 0.7353 0.6079 0.6448 0.080 Uiso 1 1 calc R U . . .
C21 C 0.5752(5) 0.4959(5) 0.57368(10) 0.0444(13) Uani 1 1 d . . . . .
C22 C 0.6741(5) 0.5320(5) 0.56685(12) 0.0526(16) Uani 1 1 d . . . . .
C23 C 0.6873(6) 0.5177(6) 0.54472(13) 0.0610(19) Uani 1 1 d . . . . .
H23 H 0.7532 0.5397 0.5395 0.073 Uiso 1 1 calc R U . . .
C24 C 0.6083(7) 0.4731(6) 0.53048(13) 0.066(2) Uani 1 1 d . . . . .
C25 C 0.5120(7) 0.4366(6) 0.53816(12) 0.0601(18) Uani 1 1 d . . . . .
H25 H 0.4572 0.4032 0.5284 0.072 Uiso 1 1 calc R U . . .
C26 C 0.4925(5) 0.4472(5) 0.55960(11) 0.0485(14) Uani 1 1 d . . . . .
C27 C 0.7602(6) 0.5822(7) 0.58172(15) 0.071(2) Uani 1 1 d . . . . .
H27A H 0.8227 0.6143 0.5734 0.106 Uiso 1 1 calc R U . . .
H27B H 0.7606 0.5326 0.5916 0.106 Uiso 1 1 calc R U . . .
H27C H 0.7545 0.6332 0.5901 0.106 Uiso 1 1 calc R U . . .
C28 C 0.6255(10) 0.4599(8) 0.50649(15) 0.092(3) Uani 1 1 d . . . . .
H28A H 0.6041 0.3893 0.5037 0.138 Uiso 1 1 calc R U . . .
H28B H 0.6969 0.5017 0.5030 0.138 Uiso 1 1 calc R U . . .
H28C H 0.5864 0.4802 0.4974 0.138 Uiso 1 1 calc R U . . .
C29 C 0.3875(5) 0.4082(5) 0.56729(11) 0.0509(15) Uani 1 1 d . . . . .
H29A H 0.3767 0.4646 0.5702 0.076 Uiso 1 1 calc R U . . .
H29B H 0.3766 0.3692 0.5806 0.076 Uiso 1 1 calc R U . . .
H29C H 0.3405 0.3652 0.5561 0.076 Uiso 1 1 calc R U . . .
Ni Ni 0.3333 0.6667 0.61769(2) 0.0399(3) Uani 1 3 d S T P . .
Cl1 Cl 0.28690(11) 0.50896(13) 0.60696(3) 0.0531(4) Uani 1 1 d . . . . .
Cl2 Cl 0.3333 0.6667 0.65407(4) 0.0571(7) Uani 1 3 d S T P . .
Cl3 Cl 0.6667 0.3333 0.61118(5) 0.0483(6) Uani 1 3 d S T P . .
C4 C 0.5238(11) 0.6696(10) 0.6889(2) 0.127(6) Uani 1 1 d . . . . .
H4A1 H 0.5212 0.6103 0.6958 0.152 Uiso 1 1 calc R U . . .
H4A2 H 0.4671 0.6462 0.6786 0.152 Uiso 1 1 calc R U . . .
Cl4 Cl 0.5158(4) 0.7500(5) 0.70925(9) 0.182(2) Uani 1 1 d . . . . .
Cl5 Cl 0.6345(4) 0.7385(3) 0.67575(7) 0.151(2) Uani 1 1 d . . . . .
C5 C 0.7584(11) 0.9011(11) 0.6045(4) 0.160(8) Uani 1 1 d . . . . .
H5A H 0.6862 0.8768 0.6069 0.192 Uiso 0.723(14) 1 calc R U P A 1
H5B H 0.7961 0.9750 0.6062 0.192 Uiso 0.723(14) 1 calc R U P A 1
H5C H 0.7775 0.8940 0.5896 0.192 Uiso 0.277(14) 1 calc R U P A 2
H5D H 0.6843 0.8677 0.6052 0.192 Uiso 0.277(14) 1 calc R U P A 2
Cl6 Cl 0.8043(5) 0.8418(6) 0.62382(10) 0.203(3) Uani 1 1 d . . . . .
Cl7A Cl 0.7766(5) 0.8692(8) 0.58039(15) 0.211(6) Uani 0.723(14) 1 d . . P A 1
Cl7B Cl 0.8097(14) 1.0248(13) 0.6108(4) 0.195(13) Uani 0.277(14) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N11 C1 1.314(8) . ?
N11 C11 1.434(8) . ?
N11 C2 1.487(7) . ?
N21 C1 1.312(8) . ?
N21 C21 1.426(8) . ?
N21 C3 1.473(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.544(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C11 C12 1.385(10) . ?
C11 C16 1.400(9) . ?
C12 C13 1.390(11) . ?
C12 C17 1.521(12) . ?
C13 C14 1.380(12) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(12) . ?
C14 C18 1.522(10) . ?
C15 C16 1.404(9) . ?
C15 H15 0.9500 . ?
C16 C19 1.494(10) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 C22 1.399(8) . ?
C21 C26 1.409(10) . ?
C22 C23 1.415(11) . ?
C22 C27 1.474(12) . ?
C23 C24 1.374(13) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(12) . ?
C24 C28 1.537(11) . ?
C25 C26 1.386(10) . ?
C25 H25 0.9500 . ?
C26 C29 1.492(9) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
Ni Cl2 2.247(3) . ?
Ni Cl1 2.2595(16) 2_665 ?
Ni Cl1 2.2596(16) . ?
Ni Cl1 2.2597(16) 3_565 ?
C4 Cl5 1.697(17) . ?
C4 Cl4 1.810(18) . ?
C4 H4A1 0.9900 . ?
C4 H4A2 0.9900 . ?
C5 Cl7A 1.64(2) . ?
C5 Cl7B 1.70(3) . ?
C5 Cl6 1.84(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 H5C 0.9900 . ?
C5 H5D 0.9900 . ?

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
C1 N11 C11 126.9(5) . . ?
C1 N11 C2 110.5(5) . . ?
C11 N11 C2 122.5(5) . . ?
C1 N21 C21 127.4(5) . . ?
C1 N21 C3 110.8(5) . . ?
C21 N21 C3 121.7(4) . . ?
N21 C1 N11 113.3(5) . . ?
N21 C1 H1 123.3 . . ?
N11 C1 H1 123.3 . . ?
N11 C2 C3 102.3(5) . . ?
N11 C2 H2A 111.3 . . ?
C3 C2 H2A 111.3 . . ?
N11 C2 H2B 111.3 . . ?
C3 C2 H2B 111.3 . . ?
H2A C2 H2B 109.2 . . ?
N21 C3 C2 103.0(4) . . ?
N21 C3 H3A 111.2 . . ?
C2 C3 H3A 111.2 . . ?
N21 C3 H3B 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C12 C11 C16 123.2(6) . . ?
C12 C11 N11 119.1(6) . . ?
C16 C11 N11 117.7(6) . . ?
C11 C12 C13 117.8(7) . . ?
C11 C12 C17 120.9(7) . . ?
C13 C12 C17 121.2(7) . . ?
C14 C13 C12 121.1(7) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 120.0(6) . . ?
C13 C14 C18 119.5(7) . . ?
C15 C14 C18 120.5(8) . . ?
C14 C15 C16 121.0(7) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 116.8(6) . . ?
C11 C16 C19 122.4(6) . . ?
C15 C16 C19 120.8(6) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C21 C26 122.6(6) . . ?
C22 C21 N21 118.3(6) . . ?
C26 C21 N21 118.9(5) . . ?
C21 C22 C23 116.2(7) . . ?
C21 C22 C27 122.2(6) . . ?
C23 C22 C27 121.6(6) . . ?
C24 C23 C22 122.4(7) . . ?
C24 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C23 C24 C25 119.0(7) . . ?
C23 C24 C28 121.0(8) . . ?
C25 C24 C28 119.9(9) . . ?
C24 C25 C26 122.1(8) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
C25 C26 C21 117.5(6) . . ?
C25 C26 C29 120.8(7) . . ?
C21 C26 C29 121.7(6) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Cl2 Ni Cl1 107.06(6) . 2_665 ?
Cl2 Ni Cl1 107.06(6) . . ?
Cl1 Ni Cl1 111.77(5) 2_665 . ?
Cl2 Ni Cl1 107.06(6) . 3_565 ?
Cl1 Ni Cl1 111.77(5) 2_665 3_565 ?
Cl1 Ni Cl1 111.76(5) . 3_565 ?
Cl5 C4 Cl4 107.2(7) . . ?
Cl5 C4 H4A1 110.3 . . ?
Cl4 C4 H4A1 110.3 . . ?
Cl5 C4 H4A2 110.3 . . ?
Cl4 C4 H4A2 110.3 . . ?
H4A1 C4 H4A2 108.5 . . ?
Cl7A C5 Cl6 106.0(9) . . ?
Cl7B C5 Cl6 109.1(14) . . ?
Cl7A C5 H5A 110.5 . . ?
Cl6 C5 H5A 110.5 . . ?
Cl7A C5 H5B 110.5 . . ?
Cl6 C5 H5B 110.5 . . ?
H5A C5 H5B 108.7 . . ?
Cl7B C5 H5C 109.9 . . ?
Cl6 C5 H5C 109.9 . . ?
Cl7B C5 H5D 109.9 . . ?
Cl6 C5 H5D 109.9 . . ?
H5C C5 H5D 108.3 . . ?

_refine_diff_density_max         0.653
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.066

_shelxl_version_number           2013-4

