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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# 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 1500227'
_audit_update_record             
;
2016-08-20 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H60 N2 Ni O2'
_chemical_formula_weight         683.63

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.551(2)
_cell_length_b                   16.226(3)
_cell_length_c                   22.289(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.116(2)
_cell_angle_gamma                90
_cell_volume                     4708.4(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9886
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      25.07

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.964
_exptl_crystal_F_000             1480
_exptl_transmission_factor_min   0.2073
_exptl_transmission_factor_max   0.7452
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.441
_shelx_estimated_absorpt_T_min   0.898
_shelx_estimated_absorpt_T_max   0.917
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 'fine-focus sealed tube'
_diffrn_reflns_number            28380
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.564
_diffrn_reflns_theta_max         25.090
_diffrn_reflns_theta_full        25.090
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8320
_reflns_number_gt                6441
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          ?
# SQUEEZE RESULTS (Version =  30715)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.064 0.722 0.370 8 -1 ' '
2 0.064 0.778 0.870 8 -1 ' '
3 0.500 0.698 0.792 1297 213 ' '
4 0.935 0.222 0.130 8 -1 ' '
5 0.936 0.278 0.630 8 -1 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_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)+(0.1000P)²+0.0655P] 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         8320
_refine_ls_number_parameters     440
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1420
_refine_ls_wR_factor_gt          0.1324
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_restrained_S_all      0.968
_refine_ls_shift/su_max          0.003
_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 0.06566(2) 0.02489(2) 0.81915(2) 0.01707(12) Uani 1 1 d . . . . .
O1 O -0.02949(11) 0.09189(10) 0.83743(7) 0.0198(3) Uani 1 1 d . . . . .
O2 O 0.16573(11) 0.09385(10) 0.86292(7) 0.0215(4) Uani 1 1 d . . . . .
N1 N -0.03154(13) -0.05144(12) 0.77605(8) 0.0158(4) Uani 1 1 d . . . . .
N2 N 0.15774(14) -0.05001(12) 0.80011(8) 0.0183(4) Uani 1 1 d . . . . .
C1 C 0.00447(18) -0.11777(14) 0.75597(10) 0.0196(5) Uani 1 1 d . . . . .
C2 C 0.11739(17) -0.11639(14) 0.77034(10) 0.0196(5) Uani 1 1 d . . . . .
C3 C -0.05769(19) -0.18718(15) 0.72219(12) 0.0254(5) Uani 1 1 d . . . . .
H3A H -0.1289 -0.1811 0.7236 0.038 Uiso 1 1 calc R U . . .
H3B H -0.0297 -0.2393 0.7420 0.038 Uiso 1 1 calc R U . . .
H3C H -0.0555 -0.1871 0.6786 0.038 Uiso 1 1 calc R U . . .
C4 C 0.17643(18) -0.18520(15) 0.75254(11) 0.0246(5) Uani 1 1 d . . . . .
H4A H 0.2427 -0.1645 0.7494 0.037 Uiso 1 1 calc R U . . .
H4B H 0.1375 -0.2078 0.7121 0.037 Uiso 1 1 calc R U . . .
H4C H 0.1879 -0.2285 0.7844 0.037 Uiso 1 1 calc R U . . .
C5 C -0.14049(17) -0.04126(15) 0.76449(11) 0.0208(5) Uani 1 1 d . . . . .
C6 C -0.19653(19) -0.01054(17) 0.70584(11) 0.0282(6) Uani 1 1 d . . . . .
C7 C -0.3029(2) -0.0060(2) 0.69447(14) 0.0522(9) Uani 1 1 d . . . . .
H7 H -0.3436 0.0130 0.6550 0.063 Uiso 1 1 calc R U . . .
C8 C -0.3505(2) -0.0287(3) 0.73978(16) 0.0644(12) Uani 1 1 d . . . . .
H8 H -0.4232 -0.0267 0.7309 0.077 Uiso 1 1 calc R U . . .
C9 C -0.2918(2) -0.0542(2) 0.79748(14) 0.0473(8) Uani 1 1 d . . . . .
H9 H -0.3250 -0.0680 0.8285 0.057 Uiso 1 1 calc R U . . .
C10 C -0.18582(19) -0.06027(16) 0.81191(11) 0.0260(5) Uani 1 1 d . . . . .
C11 C -0.1233(2) -0.08897(17) 0.87580(11) 0.0296(6) Uani 1 1 d . . . . .
H11 H -0.0491 -0.0837 0.8773 0.035 Uiso 1 1 calc R U . . .
C12 C -0.1421(3) -0.03399(19) 0.92749(13) 0.0442(8) Uani 1 1 d . . . . .
H12A H -0.1281 0.0236 0.9193 0.066 Uiso 1 1 calc R U . . .
H12B H -0.0965 -0.0510 0.9679 0.066 Uiso 1 1 calc R U . . .
H12C H -0.2138 -0.0394 0.9283 0.066 Uiso 1 1 calc R U . . .
C13 C -0.1427(3) -0.17802(19) 0.88793(15) 0.0555(9) Uani 1 1 d . . . . .
H13A H -0.2167 -0.1871 0.8802 0.083 Uiso 1 1 calc R U . . .
H13B H -0.1074 -0.1917 0.9314 0.083 Uiso 1 1 calc R U . . .
H13C H -0.1166 -0.2132 0.8600 0.083 Uiso 1 1 calc R U . . .
C14 C -0.1433(2) 0.01964(16) 0.65801(12) 0.0288(6) Uani 1 1 d . . . . .
H14 H -0.0752 -0.0087 0.6669 0.035 Uiso 1 1 calc R U . . .
C15 C -0.1232(3) 0.1118(2) 0.66670(16) 0.0620(10) Uani 1 1 d . . . . .
H15A H -0.0794 0.1298 0.6408 0.093 Uiso 1 1 calc R U . . .
H15B H -0.0888 0.1233 0.7107 0.093 Uiso 1 1 calc R U . . .
H15C H -0.1886 0.1416 0.6542 0.093 Uiso 1 1 calc R U . . .
C16 C -0.2022(2) 0.0001(2) 0.59105(13) 0.0423(7) Uani 1 1 d . . . . .
H16A H -0.2709 0.0246 0.5817 0.063 Uiso 1 1 calc R U . . .
H16B H -0.2083 -0.0597 0.5855 0.063 Uiso 1 1 calc R U . . .
H16C H -0.1654 0.0229 0.5627 0.063 Uiso 1 1 calc R U . . .
C17 C 0.26803(17) -0.03803(14) 0.82088(11) 0.0205(5) Uani 1 1 d . . . . .
C18 C 0.32198(18) -0.07243(15) 0.87826(11) 0.0244(5) Uani 1 1 d . . . . .
C19 C 0.42520(19) -0.05281(17) 0.90013(12) 0.0309(6) Uani 1 1 d . . . . .
H19 H 0.4642 -0.0747 0.9390 0.037 Uiso 1 1 calc R U . . .
C20 C 0.47314(19) -0.00187(18) 0.86653(13) 0.0326(6) Uani 1 1 d . . . . .
H20 H 0.5439 0.0112 0.8828 0.039 Uiso 1 1 calc R U . . .
C21 C 0.4181(2) 0.02951(16) 0.80992(13) 0.0298(6) Uani 1 1 d . . . . .
H21 H 0.4514 0.0642 0.7872 0.036 Uiso 1 1 calc R U . . .
C22 C 0.31394(18) 0.01119(16) 0.78512(12) 0.0248(5) Uani 1 1 d . . . . .
C23 C 0.27092(19) -0.12688(16) 0.91666(11) 0.0260(5) Uani 1 1 d . . . . .
H23 H 0.2026 -0.1441 0.8889 0.031 Uiso 1 1 calc R U . . .
C24 C 0.2515(3) -0.07859(19) 0.97064(14) 0.0484(8) Uani 1 1 d . . . . .
H24A H 0.3172 -0.0658 1.0010 0.073 Uiso 1 1 calc R U . . .
H24B H 0.2093 -0.1116 0.9908 0.073 Uiso 1 1 calc R U . . .
H24C H 0.2155 -0.0272 0.9549 0.073 Uiso 1 1 calc R U . . .
C25 C 0.3320(2) -0.20460(19) 0.93953(16) 0.0453(8) Uani 1 1 d . . . . .
H25A H 0.3462 -0.2332 0.9041 0.068 Uiso 1 1 calc R U . . .
H25B H 0.2923 -0.2408 0.9593 0.068 Uiso 1 1 calc R U . . .
H25C H 0.3969 -0.1900 0.9700 0.068 Uiso 1 1 calc R U . . .
C26 C 0.2539(2) 0.04393(17) 0.72114(12) 0.0305(6) Uani 1 1 d . . . . .
H26 H 0.1873 0.0134 0.7079 0.037 Uiso 1 1 calc R U . . .
C27 C 0.3112(3) 0.0289(2) 0.67212(14) 0.0441(8) Uani 1 1 d . . . . .
H27A H 0.3751 0.0608 0.6828 0.066 Uiso 1 1 calc R U . . .
H27B H 0.2681 0.0462 0.6311 0.066 Uiso 1 1 calc R U . . .
H27C H 0.3272 -0.0298 0.6710 0.066 Uiso 1 1 calc R U . . .
C28 C 0.2295(3) 0.1352(2) 0.72405(14) 0.0499(8) Uani 1 1 d . . . . .
H28A H 0.2936 0.1669 0.7355 0.075 Uiso 1 1 calc R U . . .
H28B H 0.1922 0.1441 0.7554 0.075 Uiso 1 1 calc R U . . .
H28C H 0.1871 0.1536 0.6831 0.075 Uiso 1 1 calc R U . . .
C29 C 0.01766(17) 0.15249(13) 0.87629(10) 0.0168(5) Uani 1 1 d . . . . .
C30 C 0.12457(17) 0.15448(14) 0.89027(10) 0.0184(5) Uani 1 1 d . . . . .
C31 C 0.18182(17) 0.21486(15) 0.93011(10) 0.0207(5) Uani 1 1 d . . . . .
C32 C 0.12489(18) 0.27200(14) 0.95479(10) 0.0209(5) Uani 1 1 d . . . . .
H32 H 0.1616 0.3139 0.9817 0.025 Uiso 1 1 calc R U . . .
C33 C 0.01868(18) 0.27084(14) 0.94220(10) 0.0192(5) Uani 1 1 d . . . . .
C34 C -0.03551(17) 0.21007(14) 0.90173(10) 0.0190(5) Uani 1 1 d . . . . .
H34 H -0.1083 0.2081 0.8916 0.023 Uiso 1 1 calc R U . . .
C35 C -0.03967(19) 0.33455(15) 0.97013(11) 0.0246(5) Uani 1 1 d . . . . .
C36 C 0.0325(2) 0.38723(16) 1.02120(12) 0.0301(6) Uani 1 1 d . . . . .
H36A H 0.0743 0.3511 1.0537 0.045 Uiso 1 1 calc R U . . .
H36B H -0.0084 0.4241 1.0397 0.045 Uiso 1 1 calc R U . . .
H36C H 0.0774 0.4200 1.0028 0.045 Uiso 1 1 calc R U . . .
C37 C -0.1167(2) 0.29185(19) 0.99923(14) 0.0402(7) Uani 1 1 d . . . . .
H37A H -0.1647 0.2587 0.9674 0.060 Uiso 1 1 calc R U . . .
H37B H -0.1549 0.3336 1.0154 0.060 Uiso 1 1 calc R U . . .
H37C H -0.0796 0.2560 1.0335 0.060 Uiso 1 1 calc R U . . .
C38 C -0.0999(2) 0.39268(17) 0.91779(13) 0.0372(7) Uani 1 1 d . . . . .
H38A H -0.0520 0.4201 0.8985 0.056 Uiso 1 1 calc R U . . .
H38B H -0.1362 0.4342 0.9356 0.056 Uiso 1 1 calc R U . . .
H38C H -0.1497 0.3606 0.8861 0.056 Uiso 1 1 calc R U . . .
C39 C 0.29904(18) 0.21981(16) 0.94566(12) 0.0276(6) Uani 1 1 d . . . . .
C40 C 0.3300(2) 0.23893(19) 0.88640(14) 0.0386(7) Uani 1 1 d . . . . .
H40A H 0.4051 0.2394 0.8959 0.058 Uiso 1 1 calc R U . . .
H40B H 0.3029 0.2930 0.8703 0.058 Uiso 1 1 calc R U . . .
H40C H 0.3019 0.1966 0.8549 0.058 Uiso 1 1 calc R U . . .
C41 C 0.3459(2) 0.13673(18) 0.97112(14) 0.0414(7) Uani 1 1 d . . . . .
H41A H 0.3328 0.1261 1.0115 0.062 Uiso 1 1 calc R U . . .
H41B H 0.4202 0.1380 0.9765 0.062 Uiso 1 1 calc R U . . .
H41C H 0.3147 0.0929 0.9417 0.062 Uiso 1 1 calc R U . . .
C42 C 0.3452(2) 0.2859(2) 0.99462(15) 0.0451(8) Uani 1 1 d . . . . .
H42A H 0.3196 0.2781 1.0312 0.068 Uiso 1 1 calc R U . . .
H42B H 0.3252 0.3407 0.9768 0.068 Uiso 1 1 calc R U . . .
H42C H 0.4202 0.2812 1.0071 0.068 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 O1 1.8171(15) . ?
Ni1 O2 1.8189(16) . ?
Ni1 N1 1.8680(19) . ?
Ni1 N2 1.8730(19) . ?
O1 C29 1.348(3) . ?
O2 C30 1.356(3) . ?
N1 C1 1.311(3) . ?
N1 C5 1.436(3) . ?
N2 C2 1.303(3) . ?
N2 C17 1.450(3) . ?
C1 C2 1.474(3) . ?
C1 C3 1.481(3) . ?
C2 C4 1.490(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C10 1.396(3) . ?
C5 C6 1.408(3) . ?
C6 C7 1.394(4) . ?
C6 C14 1.525(4) . ?
C7 C8 1.391(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.374(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.386(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.514(3) . ?
C11 C13 1.507(4) . ?
C11 C12 1.533(4) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.518(4) . ?
C14 C15 1.523(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C22 1.391(3) . ?
C17 C18 1.401(3) . ?
C18 C19 1.384(4) . ?
C18 C23 1.523(3) . ?
C19 C20 1.391(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.373(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.398(4) . ?
C21 H21 0.9500 . ?
C22 C26 1.528(3) . ?
C23 C25 1.517(4) . ?
C23 C24 1.519(4) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.523(4) . ?
C26 C27 1.525(4) . ?
C26 H26 1.0000 . ?
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 C34 1.393(3) . ?
C29 C30 1.395(3) . ?
C30 C31 1.403(3) . ?
C31 C32 1.412(3) . ?
C31 C39 1.531(3) . ?
C32 C33 1.388(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.399(3) . ?
C33 C35 1.534(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.538(3) . ?
C35 C37 1.538(3) . ?
C35 C38 1.545(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.525(4) . ?
C39 C41 1.531(4) . ?
C39 C42 1.534(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O2 88.94(7) . . ?
O1 Ni1 N1 93.96(7) . . ?
O2 Ni1 N1 176.42(8) . . ?
O1 Ni1 N2 176.21(8) . . ?
O2 Ni1 N2 94.38(8) . . ?
N1 Ni1 N2 82.66(8) . . ?
C29 O1 Ni1 109.95(13) . . ?
C30 O2 Ni1 110.43(13) . . ?
C1 N1 C5 119.66(19) . . ?
C1 N1 Ni1 116.35(15) . . ?
C5 N1 Ni1 123.99(15) . . ?
C2 N2 C17 121.54(19) . . ?
C2 N2 Ni1 116.10(15) . . ?
C17 N2 Ni1 122.22(15) . . ?
N1 C1 C2 112.1(2) . . ?
N1 C1 C3 125.8(2) . . ?
C2 C1 C3 122.1(2) . . ?
N2 C2 C1 112.8(2) . . ?
N2 C2 C4 125.1(2) . . ?
C1 C2 C4 122.2(2) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C10 C5 C6 122.9(2) . . ?
C10 C5 N1 119.0(2) . . ?
C6 C5 N1 118.0(2) . . ?
C7 C6 C5 116.8(2) . . ?
C7 C6 C14 121.4(2) . . ?
C5 C6 C14 121.7(2) . . ?
C8 C7 C6 121.2(3) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C9 C8 C7 119.6(3) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 122.1(3) . . ?
C8 C9 H9 118.9 . . ?
C10 C9 H9 118.9 . . ?
C9 C10 C5 117.0(2) . . ?
C9 C10 C11 120.9(2) . . ?
C5 C10 C11 122.1(2) . . ?
C13 C11 C10 112.6(2) . . ?
C13 C11 C12 110.5(2) . . ?
C10 C11 C12 111.2(2) . . ?
C13 C11 H11 107.5 . . ?
C10 C11 H11 107.5 . . ?
C12 C11 H11 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C16 C14 C15 110.9(2) . . ?
C16 C14 C6 113.5(2) . . ?
C15 C14 C6 109.2(2) . . ?
C16 C14 H14 107.7 . . ?
C15 C14 H14 107.7 . . ?
C6 C14 H14 107.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 123.3(2) . . ?
C22 C17 N2 118.6(2) . . ?
C18 C17 N2 118.0(2) . . ?
C19 C18 C17 116.8(2) . . ?
C19 C18 C23 120.5(2) . . ?
C17 C18 C23 122.7(2) . . ?
C18 C19 C20 121.6(2) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C21 C20 C19 120.0(2) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 121.0(2) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C17 C22 C21 117.3(2) . . ?
C17 C22 C26 121.8(2) . . ?
C21 C22 C26 120.9(2) . . ?
C25 C23 C24 111.2(2) . . ?
C25 C23 C18 112.4(2) . . ?
C24 C23 C18 110.6(2) . . ?
C25 C23 H23 107.5 . . ?
C24 C23 H23 107.5 . . ?
C18 C23 H23 107.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C27 110.2(2) . . ?
C28 C26 C22 111.3(2) . . ?
C27 C26 C22 111.6(2) . . ?
C28 C26 H26 107.8 . . ?
C27 C26 H26 107.8 . . ?
C22 C26 H26 107.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O1 C29 C34 123.0(2) . . ?
O1 C29 C30 116.0(2) . . ?
C34 C29 C30 121.1(2) . . ?
O2 C30 C29 114.45(19) . . ?
O2 C30 C31 124.5(2) . . ?
C29 C30 C31 121.0(2) . . ?
C30 C31 C32 116.1(2) . . ?
C30 C31 C39 122.5(2) . . ?
C32 C31 C39 121.5(2) . . ?
C33 C32 C31 124.1(2) . . ?
C33 C32 H32 118.0 . . ?
C31 C32 H32 118.0 . . ?
C32 C33 C34 118.0(2) . . ?
C32 C33 C35 122.1(2) . . ?
C34 C33 C35 119.9(2) . . ?
C29 C34 C33 119.8(2) . . ?
C29 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C33 C35 C36 112.4(2) . . ?
C33 C35 C37 110.7(2) . . ?
C36 C35 C37 107.7(2) . . ?
C33 C35 C38 109.19(19) . . ?
C36 C35 C38 108.3(2) . . ?
C37 C35 C38 108.4(2) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 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 . . ?
C40 C39 C41 108.4(2) . . ?
C40 C39 C31 109.40(19) . . ?
C41 C39 C31 109.6(2) . . ?
C40 C39 C42 108.6(2) . . ?
C41 C39 C42 107.9(2) . . ?
C31 C39 C42 113.0(2) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

_refine_diff_density_max         0.515
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.069

####################################################################### 
# 
# 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 1500228'
_audit_update_record             
;
2016-08-20 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H86 N4 Ni2 O2'
_chemical_formula_weight         1012.74

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/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                   13.990(2)
_cell_length_b                   22.730(4)
_cell_length_c                   19.155(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.140(2)
_cell_angle_gamma                90
_cell_volume                     5754.5(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9973
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      24.97

_exptl_crystal_description       block
_exptl_crystal_colour            BLACK
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_F_000             2184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.697
_shelx_estimated_absorpt_T_min   0.818
_shelx_estimated_absorpt_T_max   0.845
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.3247
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 'fine-focus sealed tube'
_diffrn_reflns_number            34992
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.582
_diffrn_reflns_theta_max         24.974
_diffrn_reflns_theta_full        24.974
_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 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10062
_reflns_number_gt                7388
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_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)+(0.1000P)²+0.4078P] 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         10062
_refine_ls_number_parameters     635
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1608
_refine_ls_wR_factor_gt          0.1386
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001

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
Ni2 Ni 0.40857(3) 0.09629(2) 0.20221(2) 0.03195(13) Uani 1 1 d . . . . .
Ni1 Ni 0.60773(3) 0.16352(2) 0.25647(2) 0.03453(14) Uani 1 1 d . . . . .
N3 N 0.37564(18) 0.01863(11) 0.21977(14) 0.0355(6) Uani 1 1 d . . . . .
N1 N 0.70558(18) 0.16272(11) 0.35526(13) 0.0347(6) Uani 1 1 d . . . . .
N2 N 0.64955(18) 0.24452(11) 0.26148(13) 0.0360(6) Uani 1 1 d . . . . .
N4 N 0.31543(19) 0.11702(11) 0.25329(14) 0.0385(6) Uani 1 1 d . . . . .
C1 C 0.7455(2) 0.21442(14) 0.37852(16) 0.0385(7) Uani 1 1 d . . . . .
C5 C 0.7496(2) 0.11117(14) 0.39692(17) 0.0401(7) Uani 1 1 d . . . . .
C2 C 0.7124(2) 0.26143(14) 0.32550(17) 0.0375(7) Uani 1 1 d . . . . .
C17 C 0.6272(3) 0.28281(15) 0.19825(18) 0.0459(8) Uani 1 1 d . . . . .
C10 C 0.7077(3) 0.08728(15) 0.44745(18) 0.0471(8) Uani 1 1 d . . . . .
C11 C 0.8792(3) 0.1101(2) 0.3291(2) 0.0677(12) Uani 1 1 d . . . . .
H11 H 0.8309 0.1403 0.2996 0.081 Uiso 1 1 calc R U . . .
C4 C 0.7543(3) 0.32263(16) 0.3437(2) 0.0564(10) Uani 1 1 d . . . . .
H4A H 0.7331 0.3468 0.2989 0.085 Uiso 1 1 calc R U . . .
H4B H 0.8283 0.3209 0.3631 0.085 Uiso 1 1 calc R U . . .
H4C H 0.7287 0.3400 0.3809 0.085 Uiso 1 1 calc R U . . .
C26 C 0.7523(4) 0.22210(19) 0.1578(2) 0.0684(12) Uani 1 1 d . . . . .
H26 H 0.7445 0.1968 0.1982 0.082 Uiso 1 1 calc R U . . .
C18 C 0.5561(3) 0.32816(18) 0.1868(2) 0.0619(11) Uani 1 1 d . . . . .
C3 C 0.8248(3) 0.22484(18) 0.45302(19) 0.0575(10) Uani 1 1 d . . . . .
H3A H 0.8387 0.1879 0.4809 0.086 Uiso 1 1 calc R U . . .
H3B H 0.8000 0.2542 0.4804 0.086 Uiso 1 1 calc R U . . .
H3C H 0.8870 0.2392 0.4460 0.086 Uiso 1 1 calc R U . . .
C6 C 0.8357(3) 0.08605(17) 0.3860(2) 0.0544(10) Uani 1 1 d . . . . .
C22 C 0.6776(3) 0.27136(18) 0.1474(2) 0.0610(11) Uani 1 1 d . . . . .
C20 C 0.5891(6) 0.3537(3) 0.0748(3) 0.110(2) Uani 1 1 d . . . . .
H20 H 0.5769 0.3786 0.0330 0.132 Uiso 1 1 calc R U . . .
C7 C 0.8798(3) 0.03782(19) 0.4300(3) 0.0710(13) Uani 1 1 d . . . . .
H7 H 0.9382 0.0201 0.4240 0.085 Uiso 1 1 calc R U . . .
C23 C 0.4987(4) 0.3403(2) 0.2396(3) 0.0854(15) Uani 1 1 d . . . . .
H23 H 0.5275 0.3145 0.2839 0.102 Uiso 1 1 calc R U . . .
C8 C 0.8413(3) 0.0156(2) 0.4811(3) 0.0757(13) Uani 1 1 d . . . . .
H8 H 0.8742 -0.0164 0.5113 0.091 Uiso 1 1 calc R U . . .
C9 C 0.7563(3) 0.03893(18) 0.4891(2) 0.0660(11) Uani 1 1 d . . . . .
H9 H 0.7292 0.0220 0.5239 0.079 Uiso 1 1 calc R U . . .
C25 C 0.3874(4) 0.3226(3) 0.2023(5) 0.137(3) Uani 1 1 d . . . . .
H25A H 0.3562 0.3488 0.1603 0.206 Uiso 1 1 calc R U . . .
H25B H 0.3511 0.3259 0.2380 0.206 Uiso 1 1 calc R U . . .
H25C H 0.3841 0.2819 0.1848 0.206 Uiso 1 1 calc R U . . .
C19 C 0.5398(4) 0.3632(2) 0.1242(3) 0.0921(17) Uani 1 1 d . . . . .
H19 H 0.4926 0.3947 0.1158 0.111 Uiso 1 1 calc R U . . .
C21 C 0.6564(5) 0.3083(2) 0.0857(3) 0.0949(17) Uani 1 1 d . . . . .
H21 H 0.6896 0.3015 0.0505 0.114 Uiso 1 1 calc R U . . .
O2 O 0.47416(15) 0.16136(9) 0.17607(12) 0.0400(5) Uani 1 1 d . . . . .
O1 O 0.63230(17) 0.08984(10) 0.21152(13) 0.0480(6) Uani 1 1 d . . . . .
C58 C 0.4751(2) 0.11628(15) 0.12950(17) 0.0409(7) Uani 1 1 d . . . . .
C57 C 0.5601(3) 0.07922(15) 0.15157(18) 0.0427(8) Uani 1 1 d . . . . .
C34 C 0.4894(3) -0.06430(14) 0.22180(19) 0.0450(8) Uani 1 1 d . . . . .
C35 C 0.5088(3) -0.11470(16) 0.1881(2) 0.0585(10) Uani 1 1 d . . . . .
H35 H 0.5690 -0.1362 0.2116 0.070 Uiso 1 1 calc R U . . .
C38 C 0.3319(3) -0.05394(17) 0.1199(2) 0.0531(9) Uani 1 1 d . . . . .
C33 C 0.3992(2) -0.03364(14) 0.18668(18) 0.0411(7) Uani 1 1 d . . . . .
C39 C 0.5650(3) -0.04530(17) 0.2948(2) 0.0548(9) Uani 1 1 d . . . . .
H39 H 0.5493 -0.0035 0.3033 0.066 Uiso 1 1 calc R U . . .
C37 C 0.3570(3) -0.10439(19) 0.0888(2) 0.0694(12) Uani 1 1 d . . . . .
H37 H 0.3120 -0.1182 0.0430 0.083 Uiso 1 1 calc R U . . .
C36 C 0.4439(4) -0.13448(18) 0.1218(3) 0.0717(12) Uani 1 1 d . . . . .
H36 H 0.4596 -0.1688 0.0994 0.086 Uiso 1 1 calc R U . . .
C60 C 0.4102(3) 0.1240(2) 0.0497(2) 0.0697(12) Uani 1 1 d . . . . .
H60A H 0.3442 0.1400 0.0474 0.105 Uiso 1 1 calc R U . . .
H60B H 0.4008 0.0858 0.0246 0.105 Uiso 1 1 calc R U . . .
H60C H 0.4435 0.1512 0.0253 0.105 Uiso 1 1 calc R U . . .
C59 C 0.5713(3) 0.02786(18) 0.1050(2) 0.0637(11) Uani 1 1 d . . . . .
H59A H 0.6343 0.0068 0.1305 0.096 Uiso 1 1 calc R U . . .
H59B H 0.5732 0.0423 0.0572 0.096 Uiso 1 1 calc R U . . .
H59C H 0.5138 0.0011 0.0970 0.096 Uiso 1 1 calc R U . . .
C40 C 0.5533(4) -0.0816(2) 0.3582(3) 0.0901(15) Uani 1 1 d . . . . .
H40A H 0.4842 -0.0774 0.3595 0.135 Uiso 1 1 calc R U . . .
H40B H 0.6014 -0.0676 0.4050 0.135 Uiso 1 1 calc R U . . .
H40C H 0.5668 -0.1230 0.3511 0.135 Uiso 1 1 calc R U . . .
C42 C 0.2324(3) -0.0235(2) 0.0821(2) 0.0748(13) Uani 1 1 d . . . . .
H42 H 0.2308 0.0136 0.1098 0.090 Uiso 1 1 calc R U . . .
C41 C 0.6739(3) -0.0472(2) 0.2973(3) 0.0775(13) Uani 1 1 d . . . . .
H41A H 0.6949 -0.0882 0.2960 0.116 Uiso 1 1 calc R U . . .
H41B H 0.7169 -0.0286 0.3429 0.116 Uiso 1 1 calc R U . . .
H41C H 0.6808 -0.0261 0.2546 0.116 Uiso 1 1 calc R U . . .
C43 C 0.1432(4) -0.0614(4) 0.0831(4) 0.140(3) Uani 1 1 d . . . . .
H43A H 0.1368 -0.0950 0.0498 0.209 Uiso 1 1 calc R U . . .
H43B H 0.0810 -0.0380 0.0668 0.209 Uiso 1 1 calc R U . . .
H43C H 0.1544 -0.0757 0.1335 0.209 Uiso 1 1 calc R U . . .
C44 C 0.2175(4) -0.0071(3) 0.0014(3) 0.1014(17) Uani 1 1 d . . . . .
H44A H 0.2762 0.0154 -0.0009 0.152 Uiso 1 1 calc R U . . .
H44B H 0.1562 0.0169 -0.0182 0.152 Uiso 1 1 calc R U . . .
H44C H 0.2106 -0.0430 -0.0281 0.152 Uiso 1 1 calc R U . . .
C45 C 0.2624(3) 0.17198(15) 0.2496(2) 0.0466(8) Uani 1 1 d . . . . .
C50 C 0.2868(3) 0.21129(16) 0.3090(2) 0.0539(9) Uani 1 1 d . . . . .
C46 C 0.1823(3) 0.18459(17) 0.1845(2) 0.0570(10) Uani 1 1 d . . . . .
C47 C 0.1278(3) 0.2360(2) 0.1806(3) 0.0774(14) Uani 1 1 d . . . . .
H47 H 0.0736 0.2450 0.1369 0.093 Uiso 1 1 calc R U . . .
C54 C 0.3744(3) 0.20052(19) 0.3799(2) 0.0638(11) Uani 1 1 d . . . . .
H54 H 0.3984 0.1593 0.3781 0.077 Uiso 1 1 calc R U . . .
C49 C 0.2283(3) 0.2621(2) 0.3024(3) 0.0782(13) Uani 1 1 d . . . . .
H49 H 0.2430 0.2885 0.3430 0.094 Uiso 1 1 calc R U . . .
C48 C 0.1517(4) 0.2749(2) 0.2402(4) 0.0870(15) Uani 1 1 d . . . . .
H48 H 0.1142 0.3102 0.2370 0.104 Uiso 1 1 calc R U . . .
C56 C 0.4623(4) 0.2417(2) 0.3834(3) 0.0850(14) Uani 1 1 d . . . . .
H56A H 0.4864 0.2334 0.3418 0.127 Uiso 1 1 calc R U . . .
H56B H 0.5175 0.2355 0.4299 0.127 Uiso 1 1 calc R U . . .
H56C H 0.4393 0.2826 0.3806 0.127 Uiso 1 1 calc R U . . .
C29 C 0.3159(2) 0.01527(14) 0.26224(16) 0.0382(7) Uani 1 1 d . . . . .
C30 C 0.2828(2) 0.06950(15) 0.28051(17) 0.0406(7) Uani 1 1 d . . . . .
C31 C 0.2828(3) -0.04222(17) 0.2857(2) 0.0634(11) Uani 1 1 d . . . . .
H31A H 0.2088 -0.0447 0.2670 0.095 Uiso 1 1 calc R U . . .
H31B H 0.3066 -0.0446 0.3398 0.095 Uiso 1 1 calc R U . . .
H31C H 0.3116 -0.0748 0.2656 0.095 Uiso 1 1 calc R U . . .
C32 C 0.2122(3) 0.07345(19) 0.3246(2) 0.0666(11) Uani 1 1 d . . . . .
H32A H 0.2502 0.0672 0.3771 0.100 Uiso 1 1 calc R U . . .
H32B H 0.1597 0.0432 0.3078 0.100 Uiso 1 1 calc R U . . .
H32C H 0.1806 0.1124 0.3180 0.100 Uiso 1 1 calc R U . . .
C51 C 0.1520(3) 0.1415(2) 0.1201(2) 0.0686(12) Uani 1 1 d . . . . .
H51 H 0.2102 0.1140 0.1271 0.082 Uiso 1 1 calc R U . . .
C53 C 0.0621(4) 0.1047(3) 0.1209(4) 0.116(2) Uani 1 1 d . . . . .
H53A H 0.0796 0.0823 0.1671 0.173 Uiso 1 1 calc R U . . .
H53B H 0.0438 0.0775 0.0789 0.173 Uiso 1 1 calc R U . . .
H53C H 0.0046 0.1306 0.1173 0.173 Uiso 1 1 calc R U . . .
C27 C 0.7317(5) 0.1826(3) 0.0898(3) 0.114(2) Uani 1 1 d . . . . .
H27A H 0.6611 0.1694 0.0740 0.171 Uiso 1 1 calc R U . . .
H27B H 0.7767 0.1484 0.1022 0.171 Uiso 1 1 calc R U . . .
H27C H 0.7440 0.2048 0.0497 0.171 Uiso 1 1 calc R U . . .
C28 C 0.8611(4) 0.2435(3) 0.1837(4) 0.118(2) Uani 1 1 d . . . . .
H28A H 0.8734 0.2670 0.1446 0.178 Uiso 1 1 calc R U . . .
H28B H 0.9069 0.2096 0.1952 0.178 Uiso 1 1 calc R U . . .
H28C H 0.8731 0.2678 0.2280 0.178 Uiso 1 1 calc R U . . .
C55 C 0.3433(5) 0.2060(3) 0.4487(3) 0.116(2) Uani 1 1 d . . . . .
H55A H 0.3232 0.2467 0.4536 0.173 Uiso 1 1 calc R U . . .
H55B H 0.4005 0.1953 0.4923 0.173 Uiso 1 1 calc R U . . .
H55C H 0.2862 0.1797 0.4444 0.173 Uiso 1 1 calc R U . . .
C24 C 0.5071(5) 0.4052(3) 0.2670(5) 0.131(3) Uani 1 1 d . . . . .
H24A H 0.5784 0.4154 0.2909 0.197 Uiso 1 1 calc R U . . .
H24B H 0.4707 0.4097 0.3026 0.197 Uiso 1 1 calc R U . . .
H24C H 0.4773 0.4314 0.2248 0.197 Uiso 1 1 calc R U . . .
C52 C 0.1324(6) 0.1718(3) 0.0454(3) 0.124(2) Uani 1 1 d . . . . .
H52A H 0.1269 0.1420 0.0073 0.186 Uiso 1 1 calc R U . . .
H52B H 0.1886 0.1984 0.0482 0.186 Uiso 1 1 calc R U . . .
H52C H 0.0693 0.1943 0.0329 0.186 Uiso 1 1 calc R U . . .
C14 C 0.6143(3) 0.11251(17) 0.45886(19) 0.0515(9) Uani 1 1 d . . . . .
H14 H 0.5852 0.1418 0.4185 0.062 Uiso 1 1 calc R U . . .
C15 C 0.6392(4) 0.1456(2) 0.5319(2) 0.0812(13) Uani 1 1 d . . . . .
H15A H 0.6743 0.1192 0.5727 0.122 Uiso 1 1 calc R U . . .
H15B H 0.5765 0.1596 0.5385 0.122 Uiso 1 1 calc R U . . .
H15C H 0.6829 0.1792 0.5315 0.122 Uiso 1 1 calc R U . . .
C13 C 0.9814(4) 0.1403(2) 0.3635(3) 0.0966(17) Uani 1 1 d . . . . .
H13A H 0.9738 0.1734 0.3940 0.145 Uiso 1 1 calc R U . . .
H13B H 1.0059 0.1547 0.3243 0.145 Uiso 1 1 calc R U . . .
H13C H 1.0301 0.1120 0.3944 0.145 Uiso 1 1 calc R U . . .
C16 C 0.5330(4) 0.0658(2) 0.4519(3) 0.0818(14) Uani 1 1 d . . . . .
H16A H 0.5116 0.0491 0.4020 0.123 Uiso 1 1 calc R U . . .
H16B H 0.4747 0.0838 0.4613 0.123 Uiso 1 1 calc R U . . .
H16C H 0.5606 0.0344 0.4881 0.123 Uiso 1 1 calc R U . . .
C12 C 0.8881(4) 0.0616(3) 0.2750(3) 0.1030(19) Uani 1 1 d . . . . .
H12A H 0.9322 0.0301 0.3026 0.155 Uiso 1 1 calc R U . . .
H12B H 0.9168 0.0784 0.2391 0.155 Uiso 1 1 calc R U . . .
H12C H 0.8208 0.0455 0.2488 0.155 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
Ni2 N3 1.882(3) . ?
Ni2 O2 1.893(2) . ?
Ni2 N4 1.927(2) . ?
Ni2 C58 1.965(3) . ?
Ni1 N2 1.925(3) . ?
Ni1 N1 1.938(2) . ?
Ni1 O1 1.964(2) . ?
Ni1 O2 1.995(2) . ?
N3 C29 1.346(4) . ?
N3 C33 1.435(4) . ?
N1 C1 1.314(4) . ?
N1 C5 1.438(4) . ?
N2 C2 1.311(4) . ?
N2 C17 1.440(4) . ?
N4 C30 1.343(4) . ?
N4 C45 1.443(4) . ?
C1 C2 1.442(4) . ?
C1 C3 1.512(4) . ?
C5 C10 1.396(5) . ?
C5 C6 1.409(5) . ?
C2 C4 1.505(5) . ?
C17 C18 1.399(5) . ?
C17 C22 1.402(5) . ?
C10 C9 1.397(5) . ?
C10 C14 1.508(5) . ?
C11 C6 1.513(6) . ?
C11 C13 1.527(6) . ?
C11 C12 1.546(7) . ?
C11 H11 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C26 C22 1.500(6) . ?
C26 C28 1.518(7) . ?
C26 C27 1.528(6) . ?
C26 H26 1.0000 . ?
C18 C19 1.395(6) . ?
C18 C23 1.510(7) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C6 C7 1.397(6) . ?
C22 C21 1.399(6) . ?
C20 C19 1.358(9) . ?
C20 C21 1.367(9) . ?
C20 H20 0.9500 . ?
C7 C8 1.360(7) . ?
C7 H7 0.9500 . ?
C23 C25 1.539(7) . ?
C23 C24 1.558(8) . ?
C23 H23 1.0000 . ?
C8 C9 1.356(6) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C19 H19 0.9500 . ?
C21 H21 0.9500 . ?
O2 C58 1.361(4) . ?
O1 C57 1.279(4) . ?
C58 C57 1.404(5) . ?
C58 C60 1.510(5) . ?
C57 C59 1.509(5) . ?
C34 C35 1.385(5) . ?
C34 C33 1.405(5) . ?
C34 C39 1.513(5) . ?
C35 C36 1.373(6) . ?
C35 H35 0.9500 . ?
C38 C37 1.389(5) . ?
C38 C33 1.395(5) . ?
C38 C42 1.511(6) . ?
C39 C41 1.509(6) . ?
C39 C40 1.522(6) . ?
C39 H39 1.0000 . ?
C37 C36 1.357(6) . ?
C37 H37 0.9500 . ?
C36 H36 0.9500 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C42 C43 1.522(7) . ?
C42 C44 1.536(7) . ?
C42 H42 1.0000 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C50 1.398(5) . ?
C45 C46 1.406(5) . ?
C50 C49 1.397(5) . ?
C50 C54 1.521(6) . ?
C46 C47 1.384(6) . ?
C46 C51 1.522(6) . ?
C47 C48 1.395(7) . ?
C47 H47 0.9500 . ?
C54 C55 1.522(6) . ?
C54 C56 1.529(6) . ?
C54 H54 1.0000 . ?
C49 C48 1.346(7) . ?
C49 H49 0.9500 . ?
C48 H48 0.9500 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C29 C30 1.401(5) . ?
C29 C31 1.503(5) . ?
C30 C32 1.498(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C51 C53 1.515(7) . ?
C51 C52 1.530(7) . ?
C51 H51 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C14 C15 1.525(6) . ?
C14 C16 1.530(6) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 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
N3 Ni2 O2 161.53(10) . . ?
N3 Ni2 N4 83.84(11) . . ?
O2 Ni2 N4 114.23(10) . . ?
N3 Ni2 C58 122.96(13) . . ?
O2 Ni2 C58 41.27(12) . . ?
N4 Ni2 C58 149.26(13) . . ?
N2 Ni1 N1 81.63(10) . . ?
N2 Ni1 O1 138.02(10) . . ?
N1 Ni1 O1 104.53(10) . . ?
N2 Ni1 O2 104.74(9) . . ?
N1 Ni1 O2 159.48(10) . . ?
O1 Ni1 O2 83.97(9) . . ?
C29 N3 C33 119.9(3) . . ?
C29 N3 Ni2 113.5(2) . . ?
C33 N3 Ni2 126.3(2) . . ?
C1 N1 C5 118.9(3) . . ?
C1 N1 Ni1 114.1(2) . . ?
C5 N1 Ni1 125.9(2) . . ?
C2 N2 C17 120.3(3) . . ?
C2 N2 Ni1 115.3(2) . . ?
C17 N2 Ni1 123.9(2) . . ?
C30 N4 C45 118.7(3) . . ?
C30 N4 Ni2 111.9(2) . . ?
C45 N4 Ni2 127.6(2) . . ?
N1 C1 C2 114.9(3) . . ?
N1 C1 C3 124.0(3) . . ?
C2 C1 C3 121.0(3) . . ?
C10 C5 C6 121.3(3) . . ?
C10 C5 N1 120.1(3) . . ?
C6 C5 N1 118.7(3) . . ?
N2 C2 C1 113.8(3) . . ?
N2 C2 C4 125.3(3) . . ?
C1 C2 C4 120.8(3) . . ?
C18 C17 C22 121.4(3) . . ?
C18 C17 N2 121.7(3) . . ?
C22 C17 N2 116.9(3) . . ?
C5 C10 C9 117.8(4) . . ?
C5 C10 C14 122.3(3) . . ?
C9 C10 C14 120.0(3) . . ?
C6 C11 C13 113.1(4) . . ?
C6 C11 C12 111.5(4) . . ?
C13 C11 C12 109.9(4) . . ?
C6 C11 H11 107.4 . . ?
C13 C11 H11 107.4 . . ?
C12 C11 H11 107.4 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C22 C26 C28 112.6(4) . . ?
C22 C26 C27 113.4(4) . . ?
C28 C26 C27 110.9(4) . . ?
C22 C26 H26 106.5 . . ?
C28 C26 H26 106.5 . . ?
C27 C26 H26 106.5 . . ?
C19 C18 C17 117.6(4) . . ?
C19 C18 C23 119.9(4) . . ?
C17 C18 C23 122.4(4) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C7 C6 C5 117.3(4) . . ?
C7 C6 C11 121.0(4) . . ?
C5 C6 C11 121.7(3) . . ?
C21 C22 C17 117.4(5) . . ?
C21 C22 C26 120.3(4) . . ?
C17 C22 C26 122.3(3) . . ?
C19 C20 C21 119.7(5) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C8 C7 C6 121.6(4) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C18 C23 C25 108.7(5) . . ?
C18 C23 C24 113.7(4) . . ?
C25 C23 C24 110.9(5) . . ?
C18 C23 H23 107.8 . . ?
C25 C23 H23 107.8 . . ?
C24 C23 H23 107.8 . . ?
C9 C8 C7 120.4(4) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 121.6(4) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C20 C19 C18 122.1(5) . . ?
C20 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
C20 C21 C22 121.8(5) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 H21 119.1 . . ?
C58 O2 Ni2 72.23(16) . . ?
C58 O2 Ni1 108.46(18) . . ?
Ni2 O2 Ni1 103.16(10) . . ?
C57 O1 Ni1 110.7(2) . . ?
O2 C58 C57 116.3(3) . . ?
O2 C58 C60 116.4(3) . . ?
C57 C58 C60 122.9(3) . . ?
O2 C58 Ni2 66.50(15) . . ?
C57 C58 Ni2 101.5(2) . . ?
C60 C58 Ni2 118.5(2) . . ?
O1 C57 C58 119.9(3) . . ?
O1 C57 C59 118.2(3) . . ?
C58 C57 C59 121.9(3) . . ?
C35 C34 C33 118.0(3) . . ?
C35 C34 C39 118.8(3) . . ?
C33 C34 C39 123.2(3) . . ?
C36 C35 C34 122.0(4) . . ?
C36 C35 H35 119.0 . . ?
C34 C35 H35 119.0 . . ?
C37 C38 C33 118.5(4) . . ?
C37 C38 C42 119.7(3) . . ?
C33 C38 C42 121.8(3) . . ?
C38 C33 C34 120.3(3) . . ?
C38 C33 N3 119.7(3) . . ?
C34 C33 N3 120.0(3) . . ?
C41 C39 C34 114.5(3) . . ?
C41 C39 C40 109.3(4) . . ?
C34 C39 C40 110.9(3) . . ?
C41 C39 H39 107.2 . . ?
C34 C39 H39 107.2 . . ?
C40 C39 H39 107.2 . . ?
C36 C37 C38 121.9(4) . . ?
C36 C37 H37 119.0 . . ?
C38 C37 H37 119.0 . . ?
C37 C36 C35 119.1(4) . . ?
C37 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C42 C43 111.4(4) . . ?
C38 C42 C44 113.1(4) . . ?
C43 C42 C44 108.0(4) . . ?
C38 C42 H42 108.0 . . ?
C43 C42 H42 108.0 . . ?
C44 C42 H42 108.0 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C50 C45 C46 120.2(3) . . ?
C50 C45 N4 121.9(3) . . ?
C46 C45 N4 117.8(3) . . ?
C49 C50 C45 118.3(4) . . ?
C49 C50 C54 119.4(4) . . ?
C45 C50 C54 122.3(3) . . ?
C47 C46 C45 119.0(4) . . ?
C47 C46 C51 119.9(4) . . ?
C45 C46 C51 121.1(3) . . ?
C46 C47 C48 120.7(4) . . ?
C46 C47 H47 119.6 . . ?
C48 C47 H47 119.6 . . ?
C50 C54 C55 112.6(4) . . ?
C50 C54 C56 110.0(4) . . ?
C55 C54 C56 111.5(4) . . ?
C50 C54 H54 107.5 . . ?
C55 C54 H54 107.5 . . ?
C56 C54 H54 107.5 . . ?
C48 C49 C50 122.1(5) . . ?
C48 C49 H49 119.0 . . ?
C50 C49 H49 119.0 . . ?
C49 C48 C47 119.7(4) . . ?
C49 C48 H48 120.1 . . ?
C47 C48 H48 120.1 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N3 C29 C30 115.0(3) . . ?
N3 C29 C31 122.9(3) . . ?
C30 C29 C31 122.0(3) . . ?
N4 C30 C29 115.3(3) . . ?
N4 C30 C32 122.8(3) . . ?
C29 C30 C32 121.8(3) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C53 C51 C46 111.0(4) . . ?
C53 C51 C52 111.3(5) . . ?
C46 C51 C52 112.6(4) . . ?
C53 C51 H51 107.2 . . ?
C46 C51 H51 107.2 . . ?
C52 C51 H51 107.2 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C10 C14 C15 111.9(3) . . ?
C10 C14 C16 112.2(3) . . ?
C15 C14 C16 111.2(3) . . ?
C10 C14 H14 107.1 . . ?
C15 C14 H14 107.1 . . ?
C16 C14 H14 107.1 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_refine_diff_density_max         0.811
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.077

####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1500229'
_audit_update_record             
;
2016-08-20 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H60 N2 Na Ni O3'
_chemical_formula_weight         770.66

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'
Na Na 0.0362 0.0249 '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'

_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                   11.400(2)
_cell_length_b                   28.893(5)
_cell_length_c                   13.698(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.651(3)
_cell_angle_gamma                90
_cell_volume                     4507.1(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8949
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      24.98

_exptl_crystal_description       Block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   0.4660
_exptl_transmission_factor_max   0.7452
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.478
_shelx_estimated_absorpt_T_min   0.890
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 'fine-focus sealed tube'
_diffrn_reflns_number            27877
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.410
_diffrn_reflns_theta_max         25.053
_diffrn_reflns_theta_full        25.053
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7944
_reflns_number_gt                5283
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_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)+(0.0800P)²+3.0000P] 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         7944
_refine_ls_number_parameters     490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1686
_refine_ls_wR_factor_gt          0.1478
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.010
_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 0.24045(4) 0.86997(2) 0.14955(3) 0.04648(16) Uani 1 1 d . . . . .
Na1 Na 0.25017(16) 0.99647(5) 0.23280(10) 0.0694(4) Uani 1 1 d . . . . .
O1 O 0.2387(2) 0.93435(7) 0.13500(14) 0.0515(6) Uani 1 1 d . . . . .
O2 O 0.2441(3) 0.86629(8) 0.01680(16) 0.0645(7) Uani 1 1 d . . . . .
O3 O 0.2762(5) 1.07426(13) 0.2623(3) 0.1254(15) Uani 1 1 d . . . . .
N1 N 0.2350(2) 0.86855(8) 0.28547(17) 0.0410(6) Uani 1 1 d . . . . .
N2 N 0.2393(3) 0.80596(9) 0.1639(2) 0.0492(7) Uani 1 1 d . . . . .
C1 C 0.2277(3) 0.82609(11) 0.3253(2) 0.0475(8) Uani 1 1 d . . . . .
C2 C 0.2305(3) 0.79050(11) 0.2550(3) 0.0530(8) Uani 1 1 d . . . . .
C3 C 0.2170(4) 0.81845(14) 0.4305(3) 0.0732(12) Uani 1 1 d . . . . .
H3A H 0.2873 0.8302 0.4661 0.110 Uiso 1 1 calc R U . . .
H3B H 0.2090 0.7852 0.4432 0.110 Uiso 1 1 calc R U . . .
H3C H 0.1476 0.8348 0.4524 0.110 Uiso 1 1 calc R U . . .
C4 C 0.2239(4) 0.73954(13) 0.2780(3) 0.0769(12) Uani 1 1 d . . . . .
H4A H 0.2539 0.7217 0.2237 0.115 Uiso 1 1 calc R U . . .
H4B H 0.1421 0.7309 0.2874 0.115 Uiso 1 1 calc R U . . .
H4C H 0.2715 0.7330 0.3379 0.115 Uiso 1 1 calc R U . . .
C5 C 0.2487(4) 0.77470(11) 0.0836(3) 0.0592(10) Uani 1 1 d . . . . .
C6 C 0.1507(5) 0.76184(14) 0.0291(4) 0.0859(14) Uani 1 1 d . . . . .
C7 C 0.1653(6) 0.73205(17) -0.0519(4) 0.117(2) Uani 1 1 d . . . . .
H7 H 0.0988 0.7223 -0.0911 0.140 Uiso 1 1 calc R U . . .
C8 C 0.2739(7) 0.7176(2) -0.0732(4) 0.124(2) Uani 1 1 d . . . . .
H8 H 0.2823 0.6974 -0.1271 0.149 Uiso 1 1 calc R U . . .
C9 C 0.3712(6) 0.73106(19) -0.0203(4) 0.117(2) Uani 1 1 d . . . . .
H9 H 0.4463 0.7205 -0.0378 0.140 Uiso 1 1 calc R U . . .
C10 C 0.3614(5) 0.76049(14) 0.0602(3) 0.0821(13) Uani 1 1 d . . . . .
C11 C 0.4713(5) 0.7762(2) 0.1195(5) 0.121(2) Uani 1 1 d . . . . .
H11 H 0.4451 0.7933 0.1780 0.145 Uiso 1 1 calc R U . . .
C12 C 0.5499(6) 0.7368(3) 0.1557(5) 0.147(3) Uani 1 1 d . . . . .
H12A H 0.5035 0.7143 0.1910 0.220 Uiso 1 1 calc R U . . .
H12B H 0.6128 0.7491 0.1995 0.220 Uiso 1 1 calc R U . . .
H12C H 0.5844 0.7216 0.0998 0.220 Uiso 1 1 calc R U . . .
C13 C 0.5388(7) 0.8095(3) 0.0588(8) 0.200(4) Uani 1 1 d . . . . .
H13A H 0.6159 0.8154 0.0910 0.301 Uiso 1 1 calc R U . . .
H13B H 0.4953 0.8386 0.0518 0.301 Uiso 1 1 calc R U . . .
H13C H 0.5492 0.7961 -0.0060 0.301 Uiso 1 1 calc R U . . .
C14 C 0.0321(6) 0.7796(2) 0.0499(6) 0.134(3) Uani 1 1 d . . . . .
H14 H 0.0444 0.8044 0.1004 0.161 Uiso 1 1 calc R U . . .
C15 C -0.0468(7) 0.7436(3) 0.0944(7) 0.200(4) Uani 1 1 d . . . . .
H15A H -0.0527 0.7164 0.0516 0.300 Uiso 1 1 calc R U . . .
H15B H -0.1252 0.7567 0.1017 0.300 Uiso 1 1 calc R U . . .
H15C H -0.0133 0.7344 0.1587 0.300 Uiso 1 1 calc R U . . .
C16 C -0.0283(7) 0.8029(3) -0.0383(8) 0.200(4) Uani 1 1 d . . . . .
H16A H 0.0214 0.8279 -0.0612 0.299 Uiso 1 1 calc R U . . .
H16B H -0.1039 0.8156 -0.0200 0.299 Uiso 1 1 calc R U . . .
H16C H -0.0414 0.7801 -0.0907 0.299 Uiso 1 1 calc R U . . .
C17 C 0.2365(3) 0.90856(11) 0.3455(2) 0.0435(8) Uani 1 1 d . . . . .
C18 C 0.3450(3) 0.92612(13) 0.3816(3) 0.0591(9) Uani 1 1 d . . . . .
C19 C 0.3447(4) 0.96802(15) 0.4336(3) 0.0761(12) Uani 1 1 d . . . . .
H19 H 0.4209 0.9813 0.4596 0.091 Uiso 1 1 calc R U . . .
C20 C 0.2431(5) 0.99085(14) 0.4501(3) 0.0729(12) Uani 1 1 d . . . . .
H20 H 0.2453 1.0199 0.4900 0.087 Uiso 1 1 calc R U . . .
C21 C 0.1371(4) 0.97278(13) 0.4171(3) 0.0642(10) Uani 1 1 d . . . . .
H21 H 0.0627 0.9887 0.4336 0.077 Uiso 1 1 calc R U . . .
C22 C 0.1315(3) 0.93144(11) 0.3639(2) 0.0514(8) Uani 1 1 d . . . . .
C23 C -0.0707(5) 0.9070(2) 0.4107(5) 0.127(2) Uani 1 1 d . . . . .
H23A H -0.0322 0.8907 0.4662 0.191 Uiso 1 1 calc R U . . .
H23B H -0.1402 0.8896 0.3873 0.191 Uiso 1 1 calc R U . . .
H23C H -0.0945 0.9379 0.4315 0.191 Uiso 1 1 calc R U . . .
C24 C 0.0151(4) 0.91135(16) 0.3280(3) 0.0774(12) Uani 1 1 d . . . . .
H24 H 0.0303 0.8795 0.3031 0.093 Uiso 1 1 calc R U . . .
C25 C -0.0380(5) 0.9393(3) 0.2439(5) 0.143(3) Uani 1 1 d . . . . .
H25A H -0.0589 0.9702 0.2672 0.214 Uiso 1 1 calc R U . . .
H25B H -0.1087 0.9237 0.2171 0.214 Uiso 1 1 calc R U . . .
H25C H 0.0190 0.9422 0.1928 0.214 Uiso 1 1 calc R U . . .
C26 C 0.4579(4) 0.90053(18) 0.3669(4) 0.0924(16) Uani 1 1 d . . . . .
H26 H 0.4369 0.8686 0.3441 0.111 Uiso 1 1 calc R U . . .
C27 C 0.5341(5) 0.8958(2) 0.4604(5) 0.131(2) Uani 1 1 d . . . . .
H27A H 0.5713 0.9256 0.4762 0.196 Uiso 1 1 calc R U . . .
H27B H 0.5948 0.8724 0.4513 0.196 Uiso 1 1 calc R U . . .
H27C H 0.4852 0.8864 0.5140 0.196 Uiso 1 1 calc R U . . .
C28 C 0.5263(6) 0.9234(3) 0.2873(5) 0.177(4) Uani 1 1 d . . . . .
H28A H 0.4733 0.9298 0.2305 0.266 Uiso 1 1 calc R U . . .
H28B H 0.5893 0.9027 0.2681 0.266 Uiso 1 1 calc R U . . .
H28C H 0.5603 0.9525 0.3121 0.266 Uiso 1 1 calc R U . . .
C29 C 0.2386(3) 0.94454(11) 0.0375(2) 0.0492(8) Uani 1 1 d . . . . .
C30 C 0.2399(3) 0.90827(12) -0.0254(2) 0.0560(9) Uani 1 1 d . . . . .
C31 C 0.2359(4) 0.90795(14) -0.1329(3) 0.0646(11) Uani 1 1 d . . . . .
C32 C 0.2594(4) 0.86690(14) -0.1809(3) 0.0773(13) Uani 1 1 d . . . . .
H32 H 0.2765 0.8397 -0.1439 0.093 Uiso 1 1 calc R U . . .
C33 C 0.2584(5) 0.86503(18) -0.2821(3) 0.0985(17) Uani 1 1 d . . . . .
H33 H 0.2755 0.8365 -0.3129 0.118 Uiso 1 1 calc R U . . .
C34 C 0.2337(6) 0.9029(2) -0.3387(3) 0.110(2) Uani 1 1 d . . . . .
H34 H 0.2333 0.9013 -0.4080 0.132 Uiso 1 1 calc R U . . .
C35 C 0.2099(7) 0.9428(2) -0.2923(3) 0.127(2) Uani 1 1 d . . . . .
H35 H 0.1933 0.9698 -0.3301 0.152 Uiso 1 1 calc R U . . .
C36 C 0.2089(5) 0.94556(17) -0.1916(3) 0.1014(18) Uani 1 1 d . . . . .
H36 H 0.1891 0.9741 -0.1622 0.122 Uiso 1 1 calc R U . . .
C37 C 0.2384(4) 0.99497(12) 0.0153(2) 0.0577(10) Uani 1 1 d . . . . .
C38 C 0.1433(4) 1.02212(14) 0.0386(3) 0.0757(12) Uani 1 1 d . . . . .
H38 H 0.0774 1.0083 0.0671 0.091 Uiso 1 1 calc R U . . .
C39 C 0.1441(6) 1.06950(18) 0.0204(4) 0.111(2) Uani 1 1 d . . . . .
H39 H 0.0784 1.0879 0.0361 0.134 Uiso 1 1 calc R U . . .
C40 C 0.2368(8) 1.08938(19) -0.0191(4) 0.129(3) Uani 1 1 d . . . . .
H40 H 0.2360 1.1217 -0.0315 0.155 Uiso 1 1 calc R U . . .
C41 C 0.3311(7) 1.0641(2) -0.0416(5) 0.139(3) Uani 1 1 d . . . . .
H41 H 0.3966 1.0787 -0.0690 0.166 Uiso 1 1 calc R U . . .
C42 C 0.3326(5) 1.01601(16) -0.0243(4) 0.0970(16) Uani 1 1 d . . . . .
H42 H 0.3992 0.9982 -0.0401 0.116 Uiso 1 1 calc R U . . .
C43 C 0.4655(10) 1.0583(4) 0.2289(8) 0.224(6) Uani 1 1 d . . . . .
H43A H 0.4785 1.0399 0.2885 0.337 Uiso 1 1 calc R U . . .
H43B H 0.5404 1.0712 0.2094 0.337 Uiso 1 1 calc R U . . .
H43C H 0.4323 1.0385 0.1764 0.337 Uiso 1 1 calc R U . . .
C44 C 0.3847(10) 1.0956(3) 0.2472(7) 0.180(5) Uani 1 1 d . . . . .
H44A H 0.4116 1.1135 0.3057 0.216 Uiso 1 1 calc R U . . .
H44B H 0.3781 1.1169 0.1905 0.216 Uiso 1 1 calc R U . . .
C45 C 0.2004(13) 1.1121(3) 0.2830(10) 0.219(6) Uani 1 1 d . . . . .
H45A H 0.2231 1.1266 0.3466 0.263 Uiso 1 1 calc R U . . .
H45B H 0.2013 1.1359 0.2311 0.263 Uiso 1 1 calc R U . . .
C46 C 0.0953(12) 1.0918(4) 0.2854(9) 0.226(6) Uani 1 1 d . . . . .
H46A H 0.1045 1.0582 0.2783 0.339 Uiso 1 1 calc R U . . .
H46B H 0.0440 1.1036 0.2317 0.339 Uiso 1 1 calc R U . . .
H46C H 0.0605 1.0985 0.3479 0.339 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 O2 1.824(2) . ?
Ni1 N2 1.860(3) . ?
Ni1 N1 1.866(2) . ?
Ni1 O1 1.871(2) . ?
Na1 O1 2.240(2) . ?
Na1 O3 2.300(4) . ?
Na1 C21 2.967(4) . ?
Na1 C22 2.968(4) . ?
Na1 C37 2.977(4) . ?
Na1 C17 2.980(3) . ?
Na1 C20 2.986(4) . ?
Na1 C19 3.022(5) . ?
Na1 C18 3.041(4) . ?
Na1 C29 3.065(3) . ?
O1 C29 1.368(4) . ?
O2 C30 1.344(4) . ?
O3 C44 1.406(9) . ?
O3 C45 1.431(12) . ?
N1 C1 1.347(4) . ?
N1 C17 1.419(4) . ?
N2 C2 1.334(4) . ?
N2 C5 1.430(4) . ?
C1 C2 1.410(5) . ?
C1 C3 1.468(5) . ?
C2 C4 1.508(5) . ?
C5 C6 1.366(6) . ?
C5 C10 1.400(6) . ?
C6 C7 1.421(7) . ?
C6 C14 1.487(8) . ?
C7 C8 1.352(9) . ?
C8 C9 1.354(9) . ?
C9 C10 1.401(6) . ?
C10 C11 1.530(8) . ?
C11 C13 1.507(9) . ?
C11 C12 1.516(9) . ?
C14 C16 1.519(10) . ?
C14 C15 1.522(10) . ?
C17 C22 1.400(5) . ?
C17 C18 1.405(5) . ?
C18 C19 1.405(5) . ?
C18 C26 1.506(6) . ?
C19 C20 1.361(6) . ?
C20 C21 1.374(6) . ?
C21 C22 1.399(5) . ?
C22 C24 1.509(6) . ?
C23 C24 1.537(7) . ?
C24 C25 1.512(7) . ?
C26 C27 1.519(7) . ?
C26 C28 1.521(9) . ?
C29 C30 1.357(4) . ?
C29 C37 1.488(5) . ?
C30 C31 1.471(5) . ?
C31 C36 1.378(6) . ?
C31 C32 1.388(5) . ?
C32 C33 1.387(6) . ?
C33 C34 1.362(7) . ?
C34 C35 1.350(7) . ?
C35 C36 1.382(6) . ?
C37 C42 1.368(6) . ?
C37 C38 1.387(5) . ?
C38 C39 1.392(6) . ?
C39 C40 1.339(9) . ?
C40 C41 1.347(9) . ?
C41 C42 1.410(7) . ?
C43 C44 1.448(13) . ?
C45 C46 1.337(14) . ?

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
O2 Ni1 N2 92.74(11) . . ?
O2 Ni1 N1 175.37(10) . . ?
N2 Ni1 N1 82.67(11) . . ?
O2 Ni1 O1 87.27(9) . . ?
N2 Ni1 O1 179.00(12) . . ?
N1 Ni1 O1 97.32(10) . . ?
O1 Na1 O3 153.05(13) . . ?
O1 Na1 C21 107.96(11) . . ?
O3 Na1 C21 97.68(13) . . ?
O1 Na1 C22 80.73(9) . . ?
O3 Na1 C22 124.82(13) . . ?
C21 Na1 C22 27.27(9) . . ?
O1 Na1 C37 52.49(9) . . ?
O3 Na1 C37 100.91(13) . . ?
C21 Na1 C37 147.88(14) . . ?
C22 Na1 C37 126.56(11) . . ?
O1 Na1 C17 67.92(9) . . ?
O3 Na1 C17 138.69(13) . . ?
C21 Na1 C17 47.72(9) . . ?
C22 Na1 C17 27.22(9) . . ?
C37 Na1 C17 120.35(10) . . ?
O1 Na1 C20 123.31(11) . . ?
O3 Na1 C20 83.54(13) . . ?
C21 Na1 C20 26.68(11) . . ?
C22 Na1 C20 47.81(11) . . ?
C37 Na1 C20 174.29(13) . . ?
C17 Na1 C20 55.43(10) . . ?
O1 Na1 C19 109.57(11) . . ?
O3 Na1 C19 93.92(14) . . ?
C21 Na1 C19 46.63(13) . . ?
C22 Na1 C19 55.26(11) . . ?
C37 Na1 C19 154.83(13) . . ?
C17 Na1 C19 47.26(10) . . ?
C20 Na1 C19 26.17(12) . . ?
O1 Na1 C18 82.77(9) . . ?
O3 Na1 C18 119.77(14) . . ?
C21 Na1 C18 55.29(11) . . ?
C22 Na1 C18 47.88(11) . . ?
C37 Na1 C18 131.24(11) . . ?
C17 Na1 C18 26.96(9) . . ?
C20 Na1 C18 47.22(11) . . ?
C19 Na1 C18 26.80(10) . . ?
O1 Na1 C29 24.04(8) . . ?
O3 Na1 C29 129.16(13) . . ?
C21 Na1 C29 128.82(11) . . ?
C22 Na1 C29 102.47(10) . . ?
C37 Na1 C29 28.48(9) . . ?
C17 Na1 C29 91.95(9) . . ?
C20 Na1 C29 147.31(11) . . ?
C19 Na1 C29 131.35(12) . . ?
C18 Na1 C29 104.91(10) . . ?
C29 O1 Ni1 108.52(18) . . ?
C29 O1 Na1 114.14(19) . . ?
Ni1 O1 Na1 137.14(11) . . ?
C30 O2 Ni1 112.00(19) . . ?
C44 O3 C45 103.7(7) . . ?
C44 O3 Na1 120.7(6) . . ?
C45 O3 Na1 135.1(6) . . ?
C1 N1 C17 120.4(3) . . ?
C1 N1 Ni1 115.5(2) . . ?
C17 N1 Ni1 124.11(19) . . ?
C2 N2 C5 121.3(3) . . ?
C2 N2 Ni1 115.6(2) . . ?
C5 N2 Ni1 123.1(2) . . ?
N1 C1 C2 112.6(3) . . ?
N1 C1 C3 123.0(3) . . ?
C2 C1 C3 124.5(3) . . ?
N2 C2 C1 113.6(3) . . ?
N2 C2 C4 121.9(3) . . ?
C1 C2 C4 124.5(3) . . ?
C6 C5 C10 122.1(4) . . ?
C6 C5 N2 120.2(4) . . ?
C10 C5 N2 117.6(3) . . ?
C5 C6 C7 118.0(5) . . ?
C5 C6 C14 122.0(4) . . ?
C7 C6 C14 119.9(5) . . ?
C8 C7 C6 119.8(5) . . ?
C7 C8 C9 122.1(5) . . ?
C8 C9 C10 120.2(6) . . ?
C5 C10 C9 117.7(5) . . ?
C5 C10 C11 122.0(4) . . ?
C9 C10 C11 120.3(5) . . ?
C13 C11 C12 110.4(6) . . ?
C13 C11 C10 108.8(7) . . ?
C12 C11 C10 114.1(5) . . ?
C6 C14 C16 112.5(7) . . ?
C6 C14 C15 113.6(6) . . ?
C16 C14 C15 111.5(6) . . ?
C22 C17 C18 120.8(3) . . ?
C22 C17 N1 120.1(3) . . ?
C18 C17 N1 119.0(3) . . ?
C22 C17 Na1 75.90(19) . . ?
C18 C17 Na1 78.9(2) . . ?
N1 C17 Na1 113.17(18) . . ?
C17 C18 C19 117.8(4) . . ?
C17 C18 C26 121.3(3) . . ?
C19 C18 C26 120.8(4) . . ?
C17 C18 Na1 74.1(2) . . ?
C19 C18 Na1 75.8(2) . . ?
C26 C18 Na1 121.2(3) . . ?
C20 C19 C18 121.6(4) . . ?
C20 C19 Na1 75.5(3) . . ?
C18 C19 Na1 77.4(2) . . ?
C19 C20 C21 120.2(4) . . ?
C19 C20 Na1 78.4(2) . . ?
C21 C20 Na1 75.9(2) . . ?
C20 C21 C22 121.0(4) . . ?
C20 C21 Na1 77.5(2) . . ?
C22 C21 Na1 76.4(2) . . ?
C21 C22 C17 118.5(3) . . ?
C21 C22 C24 121.1(3) . . ?
C17 C22 C24 120.4(3) . . ?
C21 C22 Na1 76.3(2) . . ?
C17 C22 Na1 76.88(19) . . ?
C24 C22 Na1 117.7(3) . . ?
C22 C24 C25 111.0(4) . . ?
C22 C24 C23 111.8(4) . . ?
C25 C24 C23 111.1(5) . . ?
C18 C26 C27 113.0(4) . . ?
C18 C26 C28 110.5(5) . . ?
C27 C26 C28 110.6(5) . . ?
C30 C29 O1 117.0(3) . . ?
C30 C29 C37 128.8(3) . . ?
O1 C29 C37 114.2(3) . . ?
C30 C29 Na1 158.6(2) . . ?
O1 C29 Na1 41.82(13) . . ?
C37 C29 Na1 72.46(17) . . ?
O2 C30 C29 115.2(3) . . ?
O2 C30 C31 115.1(3) . . ?
C29 C30 C31 129.8(3) . . ?
C36 C31 C32 116.1(4) . . ?
C36 C31 C30 125.1(4) . . ?
C32 C31 C30 118.8(4) . . ?
C33 C32 C31 120.9(4) . . ?
C34 C33 C32 122.0(4) . . ?
C35 C34 C33 117.3(4) . . ?
C34 C35 C36 122.0(5) . . ?
C31 C36 C35 121.6(5) . . ?
C42 C37 C38 118.5(4) . . ?
C42 C37 C29 121.5(4) . . ?
C38 C37 C29 120.0(4) . . ?
C42 C37 Na1 113.0(3) . . ?
C38 C37 Na1 76.2(2) . . ?
C29 C37 Na1 79.07(17) . . ?
C37 C38 C39 120.2(5) . . ?
C40 C39 C38 120.4(6) . . ?
C39 C40 C41 120.9(5) . . ?
C40 C41 C42 120.0(6) . . ?
C37 C42 C41 120.0(5) . . ?
O3 C44 C43 105.6(8) . . ?
C46 C45 O3 102.6(9) . . ?

_refine_diff_density_max         0.485
_refine_diff_density_min         -0.269
_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_3
_database_code_depnum_ccdc_archive 'CCDC 1500226'
_audit_update_record             
;
2016-08-20 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H48 N2 Ni O2'
_chemical_formula_weight         611.48

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

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.730(3)
_cell_length_b                   15.912(3)
_cell_length_c                   15.083(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.038(3)
_cell_angle_gamma                90
_cell_volume                     3533.0(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8189
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      24.95

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   0.2714
_exptl_transmission_factor_max   0.7452
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.581
_shelx_estimated_absorpt_T_min   0.868
_shelx_estimated_absorpt_T_max   0.893
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 'fine-focus sealed tube'
_diffrn_reflns_number            21798
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.383
_diffrn_reflns_theta_max         25.136
_diffrn_reflns_theta_full        25.136
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             6256
_reflns_number_gt                4741
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_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)+(0.0962P)²+0.6959P] 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         6256
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1618
_refine_ls_wR_factor_gt          0.1450
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001

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 0.74061(2) 0.86168(2) 0.24153(2) 0.03707(16) Uani 1 1 d . . . . .
O1 O 0.77098(13) 0.95045(13) 0.30988(13) 0.0445(5) Uani 1 1 d . . . . .
O2 O 0.64034(14) 0.85282(12) 0.30733(14) 0.0435(5) Uani 1 1 d . . . . .
N1 N 0.84124(15) 0.87217(14) 0.17231(17) 0.0381(6) Uani 1 1 d . . . . .
N2 N 0.71383(15) 0.77256(14) 0.16628(15) 0.0356(5) Uani 1 1 d . . . . .
C1 C 0.8487(2) 0.81564(18) 0.1096(2) 0.0429(7) Uani 1 1 d . . . . .
C2 C 0.77442(19) 0.75701(17) 0.10632(19) 0.0392(6) Uani 1 1 d . . . . .
C3 C 0.9250(2) 0.8138(2) 0.0468(3) 0.0630(10) Uani 1 1 d . . . . .
H3A H 0.9549 0.8688 0.0466 0.094 Uiso 1 1 calc R U . . .
H3B H 0.9010 0.8008 -0.0131 0.094 Uiso 1 1 calc R U . . .
H3C H 0.9690 0.7707 0.0657 0.094 Uiso 1 1 calc R U . . .
C4 C 0.7667(3) 0.6869(2) 0.0404(2) 0.0566(9) Uani 1 1 d . . . . .
H4A H 0.7100 0.6561 0.0486 0.085 Uiso 1 1 calc R U . . .
H4B H 0.8184 0.6486 0.0493 0.085 Uiso 1 1 calc R U . . .
H4C H 0.7668 0.7100 -0.0198 0.085 Uiso 1 1 calc R U . . .
C5 C 0.90192(19) 0.94353(18) 0.1820(2) 0.0416(7) Uani 1 1 d . . . . .
C6 C 0.9709(2) 0.9415(2) 0.2467(3) 0.0629(10) Uani 1 1 d . . . . .
C7 C 1.0235(2) 1.0137(3) 0.2594(3) 0.0734(11) Uani 1 1 d . . . . .
H7 H 1.0712 1.0139 0.3035 0.088 Uiso 1 1 calc R U . . .
C8 C 1.0077(3) 1.0837(2) 0.2098(3) 0.0671(10) Uani 1 1 d . . . . .
H8 H 1.0441 1.1324 0.2197 0.081 Uiso 1 1 calc R U . . .
C9 C 0.9394(2) 1.0846(2) 0.1454(3) 0.0594(9) Uani 1 1 d . . . . .
H9 H 0.9298 1.1339 0.1107 0.071 Uiso 1 1 calc R U . . .
C10 C 0.8839(2) 1.01498(18) 0.1298(2) 0.0454(7) Uani 1 1 d . . . . .
C11 C 0.8050(3) 1.0197(2) 0.0638(3) 0.0633(10) Uani 1 1 d . . . . .
H11 H 0.7867 0.9608 0.0484 0.076 Uiso 1 1 calc R U . . .
C12 C 0.8283(4) 1.0638(3) -0.0221(3) 0.0888(14) Uani 1 1 d . . . . .
H12A H 0.8484 1.1213 -0.0089 0.133 Uiso 1 1 calc R U . . .
H12B H 0.7744 1.0654 -0.0621 0.133 Uiso 1 1 calc R U . . .
H12C H 0.8771 1.0331 -0.0505 0.133 Uiso 1 1 calc R U . . .
C13 C 0.7239(3) 1.0619(3) 0.1061(4) 0.0994(17) Uani 1 1 d . . . . .
H13A H 0.7080 1.0308 0.1595 0.149 Uiso 1 1 calc R U . . .
H13B H 0.6719 1.0622 0.0638 0.149 Uiso 1 1 calc R U . . .
H13C H 0.7399 1.1198 0.1223 0.149 Uiso 1 1 calc R U . . .
C14 C 0.9915(3) 0.8637(3) 0.3009(4) 0.113(2) Uani 1 1 d . . . . .
H14 H 0.9418 0.8221 0.2882 0.135 Uiso 1 1 calc R U . . .
C15 C 0.9936(5) 0.8827(5) 0.4000(5) 0.165(4) Uani 1 1 d . . . . .
H15A H 1.0449 0.9199 0.4149 0.247 Uiso 1 1 calc R U . . .
H15B H 1.0005 0.8302 0.4334 0.247 Uiso 1 1 calc R U . . .
H15C H 0.9368 0.9103 0.4154 0.247 Uiso 1 1 calc R U . . .
C16 C 1.0818(4) 0.8233(3) 0.2742(5) 0.133(2) Uani 1 1 d . . . . .
H16A H 1.0806 0.8143 0.2099 0.199 Uiso 1 1 calc R U . . .
H16B H 1.0897 0.7693 0.3047 0.199 Uiso 1 1 calc R U . . .
H16C H 1.1323 0.8607 0.2911 0.199 Uiso 1 1 calc R U . . .
C17 C 0.63131(18) 0.72327(17) 0.17182(18) 0.0363(6) Uani 1 1 d . . . . .
C18 C 0.6333(2) 0.64873(18) 0.2205(2) 0.0427(7) Uani 1 1 d . . . . .
C19 C 0.5516(2) 0.6066(2) 0.2301(2) 0.0581(9) Uani 1 1 d . . . . .
H19 H 0.5508 0.5559 0.2633 0.070 Uiso 1 1 calc R U . . .
C20 C 0.4718(2) 0.6371(2) 0.1925(3) 0.0649(10) Uani 1 1 d . . . . .
H20 H 0.4166 0.6076 0.2003 0.078 Uiso 1 1 calc R U . . .
C21 C 0.4715(2) 0.7097(2) 0.1438(3) 0.0612(9) Uani 1 1 d . . . . .
H21 H 0.4160 0.7296 0.1175 0.073 Uiso 1 1 calc R U . . .
C22 C 0.5514(2) 0.75510(19) 0.1319(2) 0.0466(7) Uani 1 1 d . . . . .
C23 C 0.7203(2) 0.6146(2) 0.2638(2) 0.0516(8) Uani 1 1 d . . . . .
H23 H 0.7724 0.6416 0.2341 0.062 Uiso 1 1 calc R U . . .
C24 C 0.7273(4) 0.6380(3) 0.3610(3) 0.0973(17) Uani 1 1 d . . . . .
H24A H 0.7267 0.6993 0.3669 0.146 Uiso 1 1 calc R U . . .
H24B H 0.7841 0.6157 0.3874 0.146 Uiso 1 1 calc R U . . .
H24C H 0.6757 0.6141 0.3915 0.146 Uiso 1 1 calc R U . . .
C25 C 0.7295(3) 0.5199(3) 0.2527(3) 0.0765(12) Uani 1 1 d . . . . .
H25A H 0.6805 0.4915 0.2834 0.115 Uiso 1 1 calc R U . . .
H25B H 0.7883 0.5015 0.2782 0.115 Uiso 1 1 calc R U . . .
H25C H 0.7255 0.5056 0.1895 0.115 Uiso 1 1 calc R U . . .
C26 C 0.5485(2) 0.8356(2) 0.0777(3) 0.0618(10) Uani 1 1 d . . . . .
H26 H 0.6123 0.8563 0.0731 0.074 Uiso 1 1 calc R U . . .
C27 C 0.4945(4) 0.9035(3) 0.1243(4) 0.1048(17) Uani 1 1 d . . . . .
H27A H 0.4313 0.8851 0.1288 0.157 Uiso 1 1 calc R U . . .
H27B H 0.4963 0.9557 0.0900 0.157 Uiso 1 1 calc R U . . .
H27C H 0.5211 0.9131 0.1839 0.157 Uiso 1 1 calc R U . . .
C28 C 0.5099(3) 0.8213(3) -0.0159(3) 0.0878(13) Uani 1 1 d . . . . .
H28A H 0.5456 0.7781 -0.0451 0.132 Uiso 1 1 calc R U . . .
H28B H 0.5127 0.8739 -0.0496 0.132 Uiso 1 1 calc R U . . .
H28C H 0.4466 0.8029 -0.0134 0.132 Uiso 1 1 calc R U . . .
C29 C 0.70822(19) 0.96772(17) 0.36952(18) 0.0366(6) Uani 1 1 d . . . . .
C30 C 0.6356(2) 0.91468(18) 0.36655(19) 0.0406(7) Uani 1 1 d . . . . .
C31 C 0.7247(2) 1.04344(18) 0.4232(2) 0.0408(7) Uani 1 1 d . . . . .
C32 C 0.7839(3) 1.1045(2) 0.3931(3) 0.0623(9) Uani 1 1 d . . . . .
H32 H 0.8145 1.0951 0.3396 0.075 Uiso 1 1 calc R U . . .
C33 C 0.7990(3) 1.1779(3) 0.4392(3) 0.0826(13) Uani 1 1 d . . . . .
H33 H 0.8389 1.2189 0.4167 0.099 Uiso 1 1 calc R U . . .
C34 C 0.7566(3) 1.1924(2) 0.5176(3) 0.0758(12) Uani 1 1 d . . . . .
H34 H 0.7670 1.2434 0.5491 0.091 Uiso 1 1 calc R U . . .
C35 C 0.7000(3) 1.1332(2) 0.5495(3) 0.0656(10) Uani 1 1 d . . . . .
H35 H 0.6711 1.1428 0.6039 0.079 Uiso 1 1 calc R U . . .
C36 C 0.6840(2) 1.0592(2) 0.5036(2) 0.0544(8) Uani 1 1 d . . . . .
H36 H 0.6446 1.0183 0.5273 0.065 Uiso 1 1 calc R U . . .
C37 C 0.5497(2) 0.9175(2) 0.4160(2) 0.0592(9) Uani 1 1 d . . . . .
H37A H 0.4999 0.8942 0.3787 0.089 Uiso 1 1 calc R U . . .
H37B H 0.5358 0.9758 0.4312 0.089 Uiso 1 1 calc R U . . .
H37C H 0.5570 0.8841 0.4704 0.089 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 O1 1.7958(19) . ?
Ni1 O2 1.814(2) . ?
Ni1 N2 1.850(2) . ?
Ni1 N1 1.851(2) . ?
O1 C29 1.341(3) . ?
O2 C30 1.333(3) . ?
N1 C1 1.313(4) . ?
N1 C5 1.449(3) . ?
N2 C2 1.316(3) . ?
N2 C17 1.451(3) . ?
C1 C2 1.438(4) . ?
C1 C3 1.495(4) . ?
C2 C4 1.496(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.384(5) . ?
C5 C10 1.403(4) . ?
C6 C7 1.395(5) . ?
C6 C14 1.508(5) . ?
C7 C8 1.358(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.374(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.506(5) . ?
C11 C12 1.523(5) . ?
C11 C13 1.529(6) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.525(9) . ?
C14 C16 1.542(8) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.395(4) . ?
C17 C22 1.398(4) . ?
C18 C19 1.390(4) . ?
C18 C23 1.518(4) . ?
C19 C20 1.375(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.369(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.398(4) . ?
C21 H21 0.9500 . ?
C22 C26 1.519(5) . ?
C23 C24 1.511(5) . ?
C23 C25 1.523(5) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.520(6) . ?
C26 C27 1.527(6) . ?
C26 H26 1.0000 . ?
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 C30 1.362(4) . ?
C29 C31 1.467(4) . ?
C30 C37 1.492(4) . ?
C31 C32 1.392(5) . ?
C31 C36 1.394(4) . ?
C32 C33 1.373(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.376(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.357(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.382(5) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O2 86.45(8) . . ?
O1 Ni1 N2 176.68(9) . . ?
O2 Ni1 N2 96.67(9) . . ?
O1 Ni1 N1 93.71(9) . . ?
O2 Ni1 N1 178.59(10) . . ?
N2 Ni1 N1 83.14(10) . . ?
C29 O1 Ni1 112.50(17) . . ?
C30 O2 Ni1 111.85(17) . . ?
C1 N1 C5 122.8(2) . . ?
C1 N1 Ni1 115.75(19) . . ?
C5 N1 Ni1 121.13(18) . . ?
C2 N2 C17 121.8(2) . . ?
C2 N2 Ni1 115.50(19) . . ?
C17 N2 Ni1 122.65(17) . . ?
N1 C1 C2 112.7(2) . . ?
N1 C1 C3 123.7(3) . . ?
C2 C1 C3 123.6(3) . . ?
N2 C2 C1 112.9(3) . . ?
N2 C2 C4 124.0(3) . . ?
C1 C2 C4 123.1(3) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 122.3(3) . . ?
C6 C5 N1 119.2(3) . . ?
C10 C5 N1 118.3(3) . . ?
C5 C6 C7 117.9(3) . . ?
C5 C6 C14 122.0(3) . . ?
C7 C6 C14 120.1(3) . . ?
C8 C7 C6 121.1(4) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C9 120.3(3) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C10 121.5(3) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C9 C10 C5 116.9(3) . . ?
C9 C10 C11 120.5(3) . . ?
C5 C10 C11 122.5(3) . . ?
C10 C11 C12 113.1(3) . . ?
C10 C11 C13 110.0(3) . . ?
C12 C11 C13 110.8(4) . . ?
C10 C11 H11 107.6 . . ?
C12 C11 H11 107.6 . . ?
C13 C11 H11 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6 C14 C15 111.4(5) . . ?
C6 C14 C16 111.1(4) . . ?
C15 C14 C16 110.5(5) . . ?
C6 C14 H14 107.9 . . ?
C15 C14 H14 107.9 . . ?
C16 C14 H14 107.9 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C22 122.4(3) . . ?
C18 C17 N2 119.2(2) . . ?
C22 C17 N2 118.3(3) . . ?
C19 C18 C17 117.6(3) . . ?
C19 C18 C23 120.2(3) . . ?
C17 C18 C23 122.2(3) . . ?
C20 C19 C18 121.1(3) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C21 C20 C19 120.4(3) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 121.2(3) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 H21 119.4 . . ?
C21 C22 C17 117.2(3) . . ?
C21 C22 C26 119.8(3) . . ?
C17 C22 C26 123.0(3) . . ?
C24 C23 C18 110.9(3) . . ?
C24 C23 C25 110.3(3) . . ?
C18 C23 C25 112.6(3) . . ?
C24 C23 H23 107.6 . . ?
C18 C23 H23 107.6 . . ?
C25 C23 H23 107.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 C28 112.1(3) . . ?
C22 C26 C27 110.7(4) . . ?
C28 C26 C27 110.4(3) . . ?
C22 C26 H26 107.8 . . ?
C28 C26 H26 107.8 . . ?
C27 C26 H26 107.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O1 C29 C30 114.2(2) . . ?
O1 C29 C31 115.7(2) . . ?
C30 C29 C31 129.9(3) . . ?
O2 C30 C29 114.9(2) . . ?
O2 C30 C37 115.0(2) . . ?
C29 C30 C37 130.1(3) . . ?
C32 C31 C36 116.8(3) . . ?
C32 C31 C29 119.1(3) . . ?
C36 C31 C29 124.1(3) . . ?
C33 C32 C31 121.4(4) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C32 C33 C34 120.5(4) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C35 C34 C33 119.4(4) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 120.6(4) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 121.2(3) . . ?
C35 C36 H36 119.4 . . ?
C31 C36 H36 119.4 . . ?
C30 C37 H37A 109.5 . . ?
C30 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C30 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

_refine_diff_density_max         0.747
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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 1500225'
_audit_update_record             
;
2016-08-20 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H50 N2 Ni O2'
_chemical_formula_weight         673.55

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   10.5244(19)
_cell_length_b                   18.501(3)
_cell_length_c                   19.839(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3862.9(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8797
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      24.58

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   0.3987
_exptl_transmission_factor_max   0.7452
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.537
_shelx_estimated_absorpt_T_min   0.855
_shelx_estimated_absorpt_T_max   0.877
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 'fine-focus sealed tube'
_diffrn_reflns_number            23502
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.505
_diffrn_reflns_theta_max         24.707
_diffrn_reflns_theta_full        24.707
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6554
_reflns_number_gt                5341
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.995

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_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)+(0.0539P)²+0.4086P] 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 
;
 Flack x determined using 2030 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6554
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0894
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.973
_refine_ls_shift/su_max          0.010
_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 0.12854(5) 0.59696(3) 0.81716(2) 0.04169(16) Uani 1 1 d . . . . .
O1 O 0.1206(3) 0.60578(14) 0.90787(12) 0.0503(7) Uani 1 1 d . . . . .
O2 O 0.1599(3) 0.69278(14) 0.81422(13) 0.0502(7) Uani 1 1 d . . . . .
N1 N 0.0923(3) 0.49921(15) 0.81684(16) 0.0377(7) Uani 1 1 d . . . . .
N2 N 0.1492(3) 0.58206(16) 0.72493(14) 0.0380(8) Uani 1 1 d . . . . .
C1 C 0.0946(4) 0.4671(2) 0.75801(19) 0.0405(10) Uani 1 1 d . . . . .
C2 C 0.1339(4) 0.5156(2) 0.70422(17) 0.0404(9) Uani 1 1 d . . . . .
C3 C 0.0632(5) 0.3896(2) 0.7467(2) 0.0565(12) Uani 1 1 d . . . . .
H3A H 0.1416 0.3610 0.7466 0.085 Uiso 1 1 calc R U . . .
H3B H 0.0200 0.3843 0.7032 0.085 Uiso 1 1 calc R U . . .
H3C H 0.0073 0.3726 0.7829 0.085 Uiso 1 1 calc R U . . .
C4 C 0.1551(5) 0.4907(2) 0.6338(2) 0.0600(13) Uani 1 1 d . . . . .
H4A H 0.0734 0.4783 0.6131 0.090 Uiso 1 1 calc R U . . .
H4B H 0.2102 0.4480 0.6340 0.090 Uiso 1 1 calc R U . . .
H4C H 0.1957 0.5294 0.6078 0.090 Uiso 1 1 calc R U . . .
C5 C 0.0597(4) 0.4600(2) 0.87746(19) 0.0393(9) Uani 1 1 d . . . . .
C6 C -0.0664(4) 0.4585(2) 0.8982(2) 0.0488(10) Uani 1 1 d . . . . .
C7 C -0.0927(5) 0.4233(3) 0.9584(2) 0.0645(13) Uani 1 1 d . . . . .
H7 H -0.1778 0.4218 0.9744 0.077 Uiso 1 1 calc R U . . .
C8 C 0.0011(6) 0.3908(3) 0.9952(2) 0.0723(15) Uani 1 1 d . . . . .
H8 H -0.0194 0.3667 1.0361 0.087 Uiso 1 1 calc R U . . .
C9 C 0.1235(6) 0.3927(3) 0.9734(2) 0.0656(12) Uani 1 1 d . . . . .
H9 H 0.1874 0.3695 0.9994 0.079 Uiso 1 1 calc R U . . .
C10 C 0.1579(4) 0.4278(2) 0.9141(2) 0.0512(11) Uani 1 1 d . . . . .
C11 C -0.1718(4) 0.4958(3) 0.8589(3) 0.0626(13) Uani 1 1 d . . . . .
H11 H -0.1406 0.5030 0.8118 0.075 Uiso 1 1 calc R U . . .
C12 C -0.2926(5) 0.4496(4) 0.8551(3) 0.094(2) Uani 1 1 d . . . . .
H12A H -0.2722 0.4025 0.8351 0.141 Uiso 1 1 calc R U . . .
H12B H -0.3560 0.4742 0.8271 0.141 Uiso 1 1 calc R U . . .
H12C H -0.3269 0.4425 0.9005 0.141 Uiso 1 1 calc R U . . .
C13 C -0.2000(7) 0.5700(4) 0.8882(4) 0.113(2) Uani 1 1 d . . . . .
H13A H -0.2292 0.5648 0.9349 0.169 Uiso 1 1 calc R U . . .
H13B H -0.2664 0.5935 0.8614 0.169 Uiso 1 1 calc R U . . .
H13C H -0.1227 0.5995 0.8872 0.169 Uiso 1 1 calc R U . . .
C14 C 0.2954(5) 0.4332(3) 0.8930(3) 0.0655(14) Uani 1 1 d . . . . .
H14 H 0.2972 0.4568 0.8477 0.079 Uiso 1 1 calc R U . . .
C15 C 0.3686(6) 0.4819(4) 0.9412(4) 0.111(2) Uani 1 1 d . . . . .
H15A H 0.3222 0.5274 0.9474 0.166 Uiso 1 1 calc R U . . .
H15B H 0.4529 0.4921 0.9225 0.166 Uiso 1 1 calc R U . . .
H15C H 0.3778 0.4577 0.9849 0.166 Uiso 1 1 calc R U . . .
C16 C 0.3590(7) 0.3597(4) 0.8858(4) 0.110(2) Uani 1 1 d . . . . .
H16A H 0.3563 0.3343 0.9291 0.166 Uiso 1 1 calc R U . . .
H16B H 0.4476 0.3663 0.8719 0.166 Uiso 1 1 calc R U . . .
H16C H 0.3140 0.3312 0.8516 0.166 Uiso 1 1 calc R U . . .
C17 C 0.1914(4) 0.6384(2) 0.68003(19) 0.0406(9) Uani 1 1 d . . . . .
C18 C 0.1003(5) 0.6731(2) 0.6400(2) 0.0504(11) Uani 1 1 d . . . . .
C19 C 0.1430(6) 0.7298(3) 0.6000(2) 0.0666(13) Uani 1 1 d . . . . .
H19 H 0.0845 0.7550 0.5721 0.080 Uiso 1 1 calc R U . . .
C20 C 0.2691(7) 0.7499(3) 0.6003(3) 0.0744(16) Uani 1 1 d . . . . .
H20 H 0.2966 0.7886 0.5724 0.089 Uiso 1 1 calc R U . . .
C21 C 0.3547(5) 0.7149(3) 0.6400(2) 0.0644(13) Uani 1 1 d . . . . .
H21 H 0.4411 0.7296 0.6393 0.077 Uiso 1 1 calc R U . . .
C22 C 0.3183(4) 0.6582(2) 0.6816(2) 0.0495(10) Uani 1 1 d . . . . .
C23 C -0.0398(5) 0.6529(3) 0.6432(2) 0.0603(13) Uani 1 1 d . . . . .
H23 H -0.0448 0.6014 0.6583 0.072 Uiso 1 1 calc R U . . .
C24 C -0.1082(7) 0.6579(4) 0.5754(3) 0.099(2) Uani 1 1 d . . . . .
H24A H -0.1069 0.7081 0.5595 0.148 Uiso 1 1 calc R U . . .
H24B H -0.1964 0.6419 0.5807 0.148 Uiso 1 1 calc R U . . .
H24C H -0.0651 0.6270 0.5425 0.148 Uiso 1 1 calc R U . . .
C25 C -0.1090(6) 0.6980(4) 0.6949(3) 0.108(2) Uani 1 1 d . . . . .
H25A H -0.0605 0.6984 0.7371 0.162 Uiso 1 1 calc R U . . .
H25B H -0.1933 0.6774 0.7030 0.162 Uiso 1 1 calc R U . . .
H25C H -0.1179 0.7476 0.6782 0.162 Uiso 1 1 calc R U . . .
C26 C 0.4141(5) 0.6205(3) 0.7264(2) 0.0636(14) Uani 1 1 d . . . . .
H26 H 0.3648 0.5871 0.7562 0.076 Uiso 1 1 calc R U . . .
C27 C 0.4840(7) 0.6713(5) 0.7718(4) 0.128(3) Uani 1 1 d . . . . .
H27A H 0.5308 0.7066 0.7445 0.193 Uiso 1 1 calc R U . . .
H27B H 0.5439 0.6440 0.7998 0.193 Uiso 1 1 calc R U . . .
H27C H 0.4233 0.6966 0.8008 0.193 Uiso 1 1 calc R U . . .
C28 C 0.5057(8) 0.5744(5) 0.6877(4) 0.133(3) Uani 1 1 d . . . . .
H28A H 0.4592 0.5356 0.6649 0.200 Uiso 1 1 calc R U . . .
H28B H 0.5679 0.5534 0.7188 0.200 Uiso 1 1 calc R U . . .
H28C H 0.5497 0.6041 0.6541 0.200 Uiso 1 1 calc R U . . .
C29 C 0.1478(4) 0.6736(2) 0.9275(2) 0.0457(10) Uani 1 1 d . . . . .
C30 C 0.1625(4) 0.7223(2) 0.8763(2) 0.0460(10) Uani 1 1 d . . . . .
C31 C 0.1627(4) 0.6842(2) 1.0007(2) 0.0521(12) Uani 1 1 d . . . . .
C32 C 0.0781(5) 0.6538(3) 1.0448(2) 0.0760(16) Uani 1 1 d . . . . .
H32 H 0.0103 0.6250 1.0281 0.091 Uiso 1 1 calc R U . . .
C33 C 0.0910(7) 0.6649(4) 1.1148(3) 0.097(2) Uani 1 1 d . . . . .
H33 H 0.0297 0.6461 1.1452 0.116 Uiso 1 1 calc R U . . .
C34 C 0.1937(8) 0.7032(4) 1.1382(3) 0.098(2) Uani 1 1 d . . . . .
H34 H 0.2039 0.7103 1.1853 0.118 Uiso 1 1 calc R U . . .
C35 C 0.2795(8) 0.7309(3) 1.0955(3) 0.090(2) Uani 1 1 d . . . . .
H35 H 0.3503 0.7569 1.1126 0.108 Uiso 1 1 calc R U . . .
C36 C 0.2658(5) 0.7220(3) 1.0270(3) 0.0686(14) Uani 1 1 d . . . . .
H36 H 0.3274 0.7420 0.9974 0.082 Uiso 1 1 calc R U . . .
C37 C 0.1815(4) 0.8009(2) 0.8797(2) 0.0511(11) Uani 1 1 d . . . . .
C38 C 0.1316(6) 0.8433(3) 0.9316(2) 0.0690(13) Uani 1 1 d . . . . .
H38 H 0.0842 0.8212 0.9667 0.083 Uiso 1 1 calc R U . . .
C39 C 0.1505(7) 0.9170(3) 0.9321(3) 0.092(2) Uani 1 1 d . . . . .
H39 H 0.1166 0.9449 0.9681 0.110 Uiso 1 1 calc R U . . .
C40 C 0.2163(8) 0.9503(3) 0.8825(4) 0.105(2) Uani 1 1 d . . . . .
H40 H 0.2300 1.0010 0.8840 0.126 Uiso 1 1 calc R U . . .
C41 C 0.2627(6) 0.9103(3) 0.8301(4) 0.0941(19) Uani 1 1 d . . . . .
H41 H 0.3078 0.9338 0.7949 0.113 Uiso 1 1 calc R U . . .
C42 C 0.2452(5) 0.8356(3) 0.8275(3) 0.0674(13) Uani 1 1 d . . . . .
H42 H 0.2765 0.8087 0.7903 0.081 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 O2 1.804(3) . ?
Ni1 O1 1.809(2) . ?
Ni1 N1 1.848(3) . ?
Ni1 N2 1.863(3) . ?
O1 C29 1.345(5) . ?
O2 C30 1.347(4) . ?
N1 C1 1.310(5) . ?
N1 C5 1.446(5) . ?
N2 C2 1.307(5) . ?
N2 C17 1.441(5) . ?
C1 C2 1.454(5) . ?
C1 C3 1.487(6) . ?
C2 C4 1.488(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.390(6) . ?
C5 C10 1.398(6) . ?
C6 C7 1.388(6) . ?
C6 C11 1.521(6) . ?
C7 C8 1.367(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.360(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(6) . ?
C9 H9 0.9500 . ?
C10 C14 1.509(7) . ?
C11 C13 1.521(8) . ?
C11 C12 1.534(8) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.523(8) . ?
C14 C15 1.523(7) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C22 1.386(6) . ?
C17 C18 1.401(6) . ?
C18 C19 1.389(6) . ?
C18 C23 1.523(7) . ?
C19 C20 1.379(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.361(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(6) . ?
C21 H21 0.9500 . ?
C22 C26 1.514(6) . ?
C23 C25 1.509(7) . ?
C23 C24 1.529(6) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.496(8) . ?
C26 C28 1.497(7) . ?
C26 H26 1.0000 . ?
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 C30 1.365(6) . ?
C29 C31 1.474(6) . ?
C30 C37 1.470(6) . ?
C31 C32 1.369(7) . ?
C31 C36 1.393(7) . ?
C32 C33 1.410(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.374(10) . ?
C33 H33 0.9500 . ?
C34 C35 1.340(10) . ?
C34 H34 0.9500 . ?
C35 C36 1.375(7) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.391(7) . ?
C37 C38 1.395(6) . ?
C38 C39 1.377(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.353(9) . ?
C39 H39 0.9500 . ?
C40 C41 1.365(9) . ?
C40 H40 0.9500 . ?
C41 C42 1.395(7) . ?
C41 H41 0.9500 . ?
C42 H42 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
O2 Ni1 O1 87.24(12) . . ?
O2 Ni1 N1 177.54(14) . . ?
O1 Ni1 N1 94.71(13) . . ?
O2 Ni1 N2 95.30(13) . . ?
O1 Ni1 N2 174.74(15) . . ?
N1 Ni1 N2 82.87(14) . . ?
C29 O1 Ni1 111.2(2) . . ?
C30 O2 Ni1 111.8(2) . . ?
C1 N1 C5 121.2(3) . . ?
C1 N1 Ni1 116.3(3) . . ?
C5 N1 Ni1 122.5(2) . . ?
C2 N2 C17 121.6(3) . . ?
C2 N2 Ni1 115.7(2) . . ?
C17 N2 Ni1 122.4(2) . . ?
N1 C1 C2 112.2(3) . . ?
N1 C1 C3 124.6(4) . . ?
C2 C1 C3 123.2(3) . . ?
N2 C2 C1 112.6(3) . . ?
N2 C2 C4 124.6(4) . . ?
C1 C2 C4 122.7(4) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 122.9(4) . . ?
C6 C5 N1 118.9(4) . . ?
C10 C5 N1 118.1(4) . . ?
C7 C6 C5 117.0(4) . . ?
C7 C6 C11 120.5(4) . . ?
C5 C6 C11 122.4(4) . . ?
C8 C7 C6 121.5(5) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 121.9(5) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C9 C10 C5 116.5(4) . . ?
C9 C10 C14 121.0(4) . . ?
C5 C10 C14 122.4(4) . . ?
C13 C11 C6 110.9(5) . . ?
C13 C11 C12 111.1(5) . . ?
C6 C11 C12 112.2(4) . . ?
C13 C11 H11 107.5 . . ?
C6 C11 H11 107.5 . . ?
C12 C11 H11 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 C16 112.8(5) . . ?
C10 C14 C15 110.5(5) . . ?
C16 C14 C15 111.4(5) . . ?
C10 C14 H14 107.3 . . ?
C16 C14 H14 107.3 . . ?
C15 C14 H14 107.3 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 123.4(4) . . ?
C22 C17 N2 118.3(4) . . ?
C18 C17 N2 118.1(3) . . ?
C19 C18 C17 116.7(4) . . ?
C19 C18 C23 121.5(4) . . ?
C17 C18 C23 121.7(4) . . ?
C20 C19 C18 120.8(5) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C21 C20 C19 120.7(5) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 121.5(5) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C17 C22 C21 116.9(4) . . ?
C17 C22 C26 122.2(4) . . ?
C21 C22 C26 120.9(4) . . ?
C25 C23 C18 111.1(4) . . ?
C25 C23 C24 109.7(5) . . ?
C18 C23 C24 113.8(4) . . ?
C25 C23 H23 107.3 . . ?
C18 C23 H23 107.3 . . ?
C24 C23 H23 107.3 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C28 110.5(6) . . ?
C27 C26 C22 113.0(5) . . ?
C28 C26 C22 113.0(4) . . ?
C27 C26 H26 106.6 . . ?
C28 C26 H26 106.6 . . ?
C22 C26 H26 106.6 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O1 C29 C30 115.1(3) . . ?
O1 C29 C31 115.5(4) . . ?
C30 C29 C31 129.3(4) . . ?
O2 C30 C29 114.3(4) . . ?
O2 C30 C37 116.5(4) . . ?
C29 C30 C37 129.2(4) . . ?
C32 C31 C36 118.2(4) . . ?
C32 C31 C29 120.4(4) . . ?
C36 C31 C29 121.3(4) . . ?
C31 C32 C33 120.4(6) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C34 C33 C32 119.0(6) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C35 C34 C33 120.9(6) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C34 C35 C36 120.6(6) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 120.8(6) . . ?
C35 C36 H36 119.6 . . ?
C31 C36 H36 119.6 . . ?
C42 C37 C38 118.1(5) . . ?
C42 C37 C30 119.2(4) . . ?
C38 C37 C30 122.7(4) . . ?
C39 C38 C37 120.5(6) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C40 C39 C38 121.3(6) . . ?
C40 C39 H39 119.4 . . ?
C38 C39 H39 119.4 . . ?
C39 C40 C41 119.3(6) . . ?
C39 C40 H40 120.3 . . ?
C41 C40 H40 120.3 . . ?
C40 C41 C42 121.2(6) . . ?
C40 C41 H41 119.4 . . ?
C42 C41 H41 119.4 . . ?
C37 C42 C41 119.6(5) . . ?
C37 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?

_refine_diff_density_max         0.383
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.040

