#------------------------------------------------------------------------------
#$Date: 2016-03-21 03:24:52 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178431 $
#$URL: svn://www.crystallography.net/cod/cif/4/02/52/4025282.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4025282
loop_
_publ_author_name
'Daizong Lin'
'Guanghui Deng'
'Jiang Wang'
'Xiao Ding'
'Hualiang Jiang'
'Hong Liu'
_publ_section_title
;
 Efficient Synthesis of Symmetrical α,α-Disubstituted β-Amino Acids and
 α,α-Disubstituted Aldehydes via Dialkylation of Nucleophilic β-Alanine
 Equivalent
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1717
_journal_page_last               1722
_journal_paper_doi               10.1021/jo902699t
_journal_volume                  75
_journal_year                    2010
_chemical_formula_sum            'C36 H27 N5 Ni O7'
_chemical_formula_weight         700.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.978(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.273(2)
_cell_length_b                   11.4009(15)
_cell_length_c                   17.635(2)
_cell_measurement_reflns_used    1463
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.295
_cell_measurement_theta_min      4.375
_cell_volume                     3242.6(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1135
_diffrn_reflns_av_sigmaI/netI    0.1486
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17327
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79564
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.068
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.786
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.786
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0242P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                2999
_reflns_number_total             6360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo902699t_si_001.cif
_cod_data_source_block           cd2705
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3242.7(7)
_cod_database_code               4025282
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.25484(3) 0.41649(4) 0.57040(3) 0.04115(18) Uani 1 1 d . . .
O1 O 0.30414(19) 0.2371(3) 0.40133(17) 0.0630(9) Uani 1 1 d . . .
O2 O 0.24363(18) 0.5566(2) 0.61853(18) 0.0540(8) Uani 1 1 d . . .
O3 O 0.30885(19) 0.6782(2) 0.71844(19) 0.0708(10) Uani 1 1 d . . .
O4 O -0.1102(3) 0.5046(4) 0.7711(3) 0.1046(17) Uani 1 1 d . . .
O5 O -0.1096(2) 0.6632(4) 0.7082(3) 0.1069(19) Uani 1 1 d . . .
O6 O 0.5345(2) 0.1707(3) 0.5556(2) 0.0895(12) Uani 1 1 d . . .
O7 O 0.5097(2) 0.3366(3) 0.4946(2) 0.1004(13) Uani 1 1 d . . .
N1 N 0.27442(19) 0.2828(2) 0.51742(19) 0.0391(8) Uani 1 1 d . . .
N2 N 0.2696(2) 0.5010(3) 0.4843(2) 0.0484(9) Uani 1 1 d . . .
N3 N 0.23513(18) 0.3336(2) 0.6519(2) 0.0364(8) Uani 1 1 d . . .
N4 N -0.0759(3) 0.5779(5) 0.7449(3) 0.0948(16) Uani 1 1 d . . .
N5 N 0.5126(2) 0.2732(4) 0.5511(3) 0.0725(12) Uani 1 1 d . . .
C1 C 0.2900(3) 0.3051(4) 0.4487(3) 0.0450(11) Uani 1 1 d . . .
C2 C 0.2873(2) 0.4344(4) 0.4309(2) 0.0458(11) Uani 1 1 d . . .
C3 C 0.3019(3) 0.4800(4) 0.3654(3) 0.0606(13) Uani 1 1 d . . .
H3 H 0.3145 0.4312 0.3292 0.073 Uiso 1 1 calc R . .
C4 C 0.2975(3) 0.6007(4) 0.3542(3) 0.0714(15) Uani 1 1 d . . .
H4A H 0.3057 0.6349 0.3098 0.086 Uiso 1 1 calc R . .
C5 C 0.2807(3) 0.6679(4) 0.4110(3) 0.0798(16) Uani 1 1 d . . .
H5 H 0.2789 0.7491 0.4055 0.096 Uiso 1 1 calc R . .
C6 C 0.2665(3) 0.6185(4) 0.4752(3) 0.0695(15) Uani 1 1 d . . .
H6A H 0.2547 0.6658 0.5127 0.083 Uiso 1 1 calc R . .
C7 C 0.2833(2) 0.1670(3) 0.5493(2) 0.0399(10) Uani 1 1 d . . .
C8 C 0.3356(2) 0.0833(4) 0.5332(2) 0.0504(11) Uani 1 1 d . . .
H8 H 0.3644 0.1038 0.4996 0.060 Uiso 1 1 calc R . .
C9 C 0.3451(3) -0.0264(4) 0.5654(3) 0.0645(14) Uani 1 1 d . . .
H9 H 0.3796 -0.0798 0.5531 0.077 Uiso 1 1 calc R . .
C10 C 0.3041(3) -0.0590(4) 0.6161(3) 0.0647(14) Uani 1 1 d . . .
H10 H 0.3100 -0.1344 0.6375 0.078 Uiso 1 1 calc R . .
C11 C 0.2537(3) 0.0223(3) 0.6348(2) 0.0541(12) Uani 1 1 d . . .
H11 H 0.2268 0.0015 0.6701 0.065 Uiso 1 1 calc R . .
C12 C 0.2430(2) 0.1348(3) 0.6012(2) 0.0379(10) Uani 1 1 d . . .
C13 C 0.1913(2) 0.2188(3) 0.6299(2) 0.0393(10) Uani 1 1 d . . .
H13 H 0.1874 0.1858 0.6797 0.047 Uiso 1 1 calc R . .
C14 C 0.1023(3) 0.2394(4) 0.5705(3) 0.0511(12) Uani 1 1 d . . .
C15 C 0.0626(3) 0.1596(5) 0.5132(3) 0.0806(16) Uani 1 1 d . . .
H15 H 0.0918 0.0951 0.5054 0.097 Uiso 1 1 calc R . .
C16 C -0.0207(3) 0.1714(6) 0.4656(3) 0.101(2) Uani 1 1 d . . .
H16 H -0.0469 0.1141 0.4275 0.121 Uiso 1 1 calc R . .
C17 C -0.0640(3) 0.2667(7) 0.4745(4) 0.106(2) Uani 1 1 d . . .
H17 H -0.1195 0.2762 0.4422 0.127 Uiso 1 1 calc R . .
C18 C -0.0243(4) 0.3476(6) 0.5317(5) 0.112(3) Uani 1 1 d . . .
H18 H -0.0533 0.4125 0.5393 0.130 Uiso 1 1 calc R . .
C19 C 0.0591(3) 0.3352(5) 0.5790(4) 0.110(3) Uani 1 1 d . . .
H19 H 0.0856 0.3927 0.6168 0.124 Uiso 1 1 calc R . .
C20 C 0.2843(3) 0.5788(4) 0.6933(3) 0.0509(11) Uani 1 1 d . . .
C21 C 0.3010(2) 0.4806(3) 0.7567(2) 0.0396(10) Uani 1 1 d . . .
C22 C 0.2557(2) 0.3679(3) 0.7246(3) 0.0372(10) Uani 1 1 d . . .
H22 H 0.2419 0.3204 0.7607 0.045 Uiso 1 1 calc R . .
C23 C 0.2751(2) 0.5251(3) 0.8269(2) 0.0495(11) Uani 1 1 d . . .
H23A H 0.2945 0.4697 0.8715 0.059 Uiso 1 1 calc R . .
H23B H 0.3024 0.5994 0.8460 0.059 Uiso 1 1 calc R . .
C24 C 0.1832(3) 0.5413(4) 0.8043(3) 0.0472(11) Uani 1 1 d . . .
C25 C 0.1402(3) 0.6310(4) 0.7568(3) 0.0779(16) Uani 1 1 d . . .
H25 H 0.1686 0.6856 0.7374 0.093 Uiso 1 1 calc R . .
C26 C 0.0546(3) 0.6433(5) 0.7364(3) 0.0918(19) Uani 1 1 d . . .
H26 H 0.0261 0.7049 0.7036 0.110 Uiso 1 1 calc R . .
C27 C 0.0148(3) 0.5647(5) 0.7649(3) 0.0683(14) Uani 1 1 d . . .
C28 C 0.0549(3) 0.4741(5) 0.8120(3) 0.0809(17) Uani 1 1 d . . .
H28 H 0.0259 0.4199 0.8309 0.097 Uiso 1 1 calc R . .
C29 C 0.1383(3) 0.4631(4) 0.8314(3) 0.0720(15) Uani 1 1 d . . .
H29 H 0.1657 0.4008 0.8641 0.086 Uiso 1 1 calc R . .
C30 C 0.3950(2) 0.4536(3) 0.7935(3) 0.0516(12) Uani 1 1 d . . .
H30A H 0.4241 0.5245 0.8184 0.062 Uiso 1 1 calc R . .
H30B H 0.4044 0.3954 0.8360 0.062 Uiso 1 1 calc R . .
C31 C 0.4314(2) 0.4095(4) 0.7335(3) 0.0492(11) Uani 1 1 d . . .
C32 C 0.4470(2) 0.2904(4) 0.7296(3) 0.0547(12) Uani 1 1 d . . .
H32 H 0.4390 0.2396 0.7675 0.066 Uiso 1 1 calc R . .
C33 C 0.4742(2) 0.2459(4) 0.6704(3) 0.0583(13) Uani 1 1 d . . .
H33 H 0.4838 0.1660 0.6679 0.070 Uiso 1 1 calc R . .
C34 C 0.4868(2) 0.3206(4) 0.6160(3) 0.0543(12) Uani 1 1 d . . .
C35 C 0.4748(3) 0.4405(4) 0.6191(3) 0.0630(14) Uani 1 1 d . . .
H35 H 0.4852 0.4909 0.5823 0.076 Uiso 1 1 calc R . .
C36 C 0.4474(3) 0.4830(4) 0.6776(3) 0.0573(13) Uani 1 1 d . . .
H36 H 0.4393 0.5633 0.6802 0.069 Uiso 1 1 calc R . .
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'
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 Ni O2 90.35(13) . . ?
N3 Ni N1 95.02(13) . . ?
O2 Ni N1 173.74(13) . . ?
N3 Ni N2 177.31(14) . . ?
O2 Ni N2 89.71(14) . . ?
N1 Ni N2 85.07(14) . . ?
C20 O2 Ni 122.4(3) . . ?
C1 N1 C7 119.9(3) . . ?
C1 N1 Ni 114.9(3) . . ?
C7 N1 Ni 124.8(3) . . ?
C2 N2 C6 119.5(4) . . ?
C2 N2 Ni 114.3(3) . . ?
C6 N2 Ni 126.2(3) . . ?
C22 N3 C13 117.9(3) . . ?
C22 N3 Ni 124.5(3) . . ?
C13 N3 Ni 117.6(2) . . ?
O5 N4 O4 123.9(6) . . ?
O5 N4 C27 118.5(6) . . ?
O4 N4 C27 117.4(5) . . ?
O6 N5 O7 122.8(5) . . ?
O6 N5 C34 118.3(5) . . ?
O7 N5 C34 118.9(5) . . ?
O1 C1 N1 129.9(4) . . ?
O1 C1 C2 118.4(4) . . ?
N1 C1 C2 111.7(4) . . ?
N2 C2 C3 122.7(4) . . ?
N2 C2 C1 114.1(4) . . ?
C3 C2 C1 123.2(4) . . ?
C2 C3 C4 118.6(4) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 117.7(4) . . ?
C5 C4 H4A 121.2 . . ?
C3 C4 H4A 121.2 . . ?
C6 C5 C4 121.6(4) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
N2 C6 C5 119.9(5) . . ?
N2 C6 H6A 120.0 . . ?
C5 C6 H6A 120.0 . . ?
C12 C7 C8 117.7(4) . . ?
C12 C7 N1 119.8(3) . . ?
C8 C7 N1 122.4(4) . . ?
C9 C8 C7 122.0(4) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C8 C9 C10 120.4(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C11 119.1(4) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C10 C11 C12 120.7(4) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C7 C12 C11 120.1(4) . . ?
C7 C12 C13 123.4(3) . . ?
C11 C12 C13 116.4(4) . . ?
N3 C13 C12 109.7(3) . . ?
N3 C13 C14 109.5(3) . . ?
C12 C13 C14 115.8(3) . . ?
N3 C13 H13 107.2 . . ?
C12 C13 H13 107.2 . . ?
C14 C13 H13 107.2 . . ?
C15 C14 C19 118.1(5) . . ?
C15 C14 C13 121.5(4) . . ?
C19 C14 C13 120.1(4) . . ?
C14 C15 C16 121.7(5) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C17 C16 C15 120.1(6) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 118.4(6) . . ?
C16 C17 H17 120.8 . . ?
C18 C17 H17 120.8 . . ?
C17 C18 C19 121.1(6) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C14 C19 C18 120.5(6) . . ?
C14 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
O3 C20 O2 122.9(4) . . ?
O3 C20 C21 117.2(4) . . ?
O2 C20 C21 119.8(4) . . ?
C22 C21 C20 114.3(3) . . ?
C22 C21 C23 108.7(3) . . ?
C20 C21 C23 108.1(3) . . ?
C22 C21 C30 108.3(3) . . ?
C20 C21 C30 110.2(3) . . ?
C23 C21 C30 106.9(3) . . ?
N3 C22 C21 124.4(4) . . ?
N3 C22 H22 117.8 . . ?
C21 C22 H22 117.8 . . ?
C24 C23 C21 114.2(3) . . ?
C24 C23 H23A 108.7 . . ?
C21 C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
C21 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
C25 C24 C29 116.7(4) . . ?
C25 C24 C23 123.2(4) . . ?
C29 C24 C23 120.1(4) . . ?
C24 C25 C26 121.9(5) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
C27 C26 C25 118.4(5) . . ?
C27 C26 H26 120.8 . . ?
C25 C26 H26 120.8 . . ?
C26 C27 C28 121.7(5) . . ?
C26 C27 N4 119.0(5) . . ?
C28 C27 N4 119.3(5) . . ?
C27 C28 C29 119.3(5) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C28 C29 C24 122.0(5) . . ?
C28 C29 H29 119.0 . . ?
C24 C29 H29 119.0 . . ?
C31 C30 C21 114.4(3) . . ?
C31 C30 H30A 108.6 . . ?
C21 C30 H30A 108.6 . . ?
C31 C30 H30B 108.6 . . ?
C21 C30 H30B 108.6 . . ?
H30A C30 H30B 107.6 . . ?
C32 C31 C36 117.5(4) . . ?
C32 C31 C30 120.0(4) . . ?
C36 C31 C30 122.5(4) . . ?
C33 C32 C31 121.2(4) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C34 C33 C32 119.1(4) . . ?
C34 C33 H33 120.4 . . ?
C32 C33 H33 120.4 . . ?
C33 C34 C35 121.8(4) . . ?
C33 C34 N5 119.2(4) . . ?
C35 C34 N5 119.0(4) . . ?
C36 C35 C34 118.3(4) . . ?
C36 C35 H35 120.8 . . ?
C34 C35 H35 120.8 . . ?
C35 C36 C31 122.0(4) . . ?
C35 C36 H36 119.0 . . ?
C31 C36 H36 119.0 . . ?
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
Ni N3 1.851(3) . ?
Ni O2 1.851(3) . ?
Ni N1 1.881(3) . ?
Ni N2 1.890(3) . ?
O1 C1 1.227(4) . ?
O2 C20 1.278(5) . ?
O3 C20 1.235(5) . ?
O4 N4 1.207(5) . ?
O5 N4 1.198(5) . ?
O6 N5 1.222(5) . ?
O7 N5 1.217(5) . ?
N1 C1 1.356(5) . ?
N1 C7 1.421(4) . ?
N2 C2 1.329(5) . ?
N2 C6 1.348(5) . ?
N3 C22 1.264(4) . ?
N3 C13 1.492(4) . ?
N4 C27 1.485(6) . ?
N5 C34 1.471(5) . ?
C1 C2 1.505(5) . ?
C2 C3 1.368(5) . ?
C3 C4 1.388(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.371(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.363(6) . ?
C5 H5 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C12 1.385(5) . ?
C7 C8 1.410(5) . ?
C8 C9 1.359(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.375(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.390(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.398(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.513(5) . ?
C13 C14 1.537(5) . ?
C13 H13 0.9800 . ?
C14 C15 1.350(6) . ?
C14 C19 1.360(6) . ?
C15 C16 1.389(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.360(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.358(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.390(7) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.535(5) . ?
C21 C22 1.505(5) . ?
C21 C23 1.545(5) . ?
C21 C30 1.548(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.502(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.361(5) . ?
C24 C29 1.376(5) . ?
C25 C26 1.398(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.333(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.350(6) . ?
C28 C29 1.362(6) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.498(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.390(5) . ?
C31 C36 1.395(5) . ?
C32 C33 1.387(5) . ?
C32 H32 0.9300 . ?
C33 C34 1.357(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.386(6) . ?
C35 C36 1.369(5) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C35 H35 O7 0.93 2.41 3.306(6) 162.1 3_666
C11 H11 O4 0.93 2.58 3.447(6) 156.3 2_546
C10 H10 O3 0.93 2.57 3.484(5) 166.2 1_545
C22 H22 O1 0.93 2.41 3.159(5) 137.1 4_566
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Ni O2 C20 52.3(3) . . . . ?
N1 Ni O2 C20 -97.0(13) . . . . ?
N2 Ni O2 C20 -130.4(3) . . . . ?
N3 Ni N1 C1 178.2(3) . . . . ?
O2 Ni N1 C1 -32.7(14) . . . . ?
N2 Ni N1 C1 0.9(3) . . . . ?
N3 Ni N1 C7 -9.6(3) . . . . ?
O2 Ni N1 C7 139.5(12) . . . . ?
N2 Ni N1 C7 173.1(3) . . . . ?
N3 Ni N2 C2 -93(3) . . . . ?
O2 Ni N2 C2 175.3(3) . . . . ?
N1 Ni N2 C2 -1.3(3) . . . . ?
N3 Ni N2 C6 89(3) . . . . ?
O2 Ni N2 C6 -2.3(4) . . . . ?
N1 Ni N2 C6 -178.8(4) . . . . ?
O2 Ni N3 C22 -32.1(3) . . . . ?
N1 Ni N3 C22 144.7(3) . . . . ?
N2 Ni N3 C22 -123(3) . . . . ?
O2 Ni N3 C13 147.4(2) . . . . ?
N1 Ni N3 C13 -35.8(3) . . . . ?
N2 Ni N3 C13 56(3) . . . . ?
C7 N1 C1 O1 8.1(7) . . . . ?
Ni N1 C1 O1 -179.3(4) . . . . ?
C7 N1 C1 C2 -173.0(3) . . . . ?
Ni N1 C1 C2 -0.4(4) . . . . ?
C6 N2 C2 C3 -0.8(7) . . . . ?
Ni N2 C2 C3 -178.5(3) . . . . ?
C6 N2 C2 C1 179.1(4) . . . . ?
Ni N2 C2 C1 1.4(5) . . . . ?
O1 C1 C2 N2 178.4(4) . . . . ?
N1 C1 C2 N2 -0.7(5) . . . . ?
O1 C1 C2 C3 -1.7(6) . . . . ?
N1 C1 C2 C3 179.3(4) . . . . ?
N2 C2 C3 C4 -0.4(7) . . . . ?
C1 C2 C3 C4 179.7(4) . . . . ?
C2 C3 C4 C5 1.6(7) . . . . ?
C3 C4 C5 C6 -1.7(8) . . . . ?
C2 N2 C6 C5 0.7(7) . . . . ?
Ni N2 C6 C5 178.2(4) . . . . ?
C4 C5 C6 N2 0.6(8) . . . . ?
C1 N1 C7 C12 -158.8(4) . . . . ?
Ni N1 C7 C12 29.4(5) . . . . ?
C1 N1 C7 C8 24.4(6) . . . . ?
Ni N1 C7 C8 -147.4(3) . . . . ?
C12 C7 C8 C9 1.6(6) . . . . ?
N1 C7 C8 C9 178.5(4) . . . . ?
C7 C8 C9 C10 -0.7(7) . . . . ?
C8 C9 C10 C11 -0.9(7) . . . . ?
C9 C10 C11 C12 1.6(7) . . . . ?
C8 C7 C12 C11 -1.0(6) . . . . ?
N1 C7 C12 C11 -177.9(4) . . . . ?
C8 C7 C12 C13 174.3(3) . . . . ?
N1 C7 C12 C13 -2.7(6) . . . . ?
C10 C11 C12 C7 -0.6(6) . . . . ?
C10 C11 C12 C13 -176.2(4) . . . . ?
C22 N3 C13 C12 -118.1(4) . . . . ?
Ni N3 C13 C12 62.4(4) . . . . ?
C22 N3 C13 C14 113.8(4) . . . . ?
Ni N3 C13 C14 -65.7(4) . . . . ?
C7 C12 C13 N3 -43.1(5) . . . . ?
C11 C12 C13 N3 132.3(4) . . . . ?
C7 C12 C13 C14 81.4(5) . . . . ?
C11 C12 C13 C14 -103.2(4) . . . . ?
N3 C13 C14 C15 148.6(4) . . . . ?
C12 C13 C14 C15 23.9(6) . . . . ?
N3 C13 C14 C19 -36.8(6) . . . . ?
C12 C13 C14 C19 -161.4(4) . . . . ?
C19 C14 C15 C16 -2.2(8) . . . . ?
C13 C14 C15 C16 172.6(5) . . . . ?
C14 C15 C16 C17 1.7(9) . . . . ?
C15 C16 C17 C18 -1.2(10) . . . . ?
C16 C17 C18 C19 1.3(12) . . . . ?
C15 C14 C19 C18 2.2(10) . . . . ?
C13 C14 C19 C18 -172.6(6) . . . . ?
C17 C18 C19 C14 -1.8(12) . . . . ?
Ni O2 C20 O3 145.8(3) . . . . ?
Ni O2 C20 C21 -37.0(5) . . . . ?
O3 C20 C21 C22 168.8(3) . . . . ?
O2 C20 C21 C22 -8.6(5) . . . . ?
O3 C20 C21 C23 47.6(5) . . . . ?
O2 C20 C21 C23 -129.7(4) . . . . ?
O3 C20 C21 C30 -69.0(5) . . . . ?
O2 C20 C21 C30 113.7(4) . . . . ?
C13 N3 C22 C21 179.2(3) . . . . ?
Ni N3 C22 C21 -1.3(5) . . . . ?
C20 C21 C22 N3 29.1(5) . . . . ?
C23 C21 C22 N3 150.0(4) . . . . ?
C30 C21 C22 N3 -94.2(4) . . . . ?
C22 C21 C23 C24 -56.0(4) . . . . ?
C20 C21 C23 C24 68.6(4) . . . . ?
C30 C21 C23 C24 -172.7(3) . . . . ?
C21 C23 C24 C25 -73.3(5) . . . . ?
C21 C23 C24 C29 106.3(5) . . . . ?
C29 C24 C25 C26 -0.1(7) . . . . ?
C23 C24 C25 C26 179.6(4) . . . . ?
C24 C25 C26 C27 0.3(9) . . . . ?
C25 C26 C27 C28 -0.5(9) . . . . ?
C25 C26 C27 N4 178.9(5) . . . . ?
O5 N4 C27 C26 -4.9(9) . . . . ?
O4 N4 C27 C26 179.3(6) . . . . ?
O5 N4 C27 C28 174.6(6) . . . . ?
O4 N4 C27 C28 -1.3(8) . . . . ?
C26 C27 C28 C29 0.5(9) . . . . ?
N4 C27 C28 C29 -178.9(5) . . . . ?
C27 C28 C29 C24 -0.3(8) . . . . ?
C25 C24 C29 C28 0.1(7) . . . . ?
C23 C24 C29 C28 -179.6(4) . . . . ?
C22 C21 C30 C31 63.3(4) . . . . ?
C20 C21 C30 C31 -62.5(4) . . . . ?
C23 C21 C30 C31 -179.8(3) . . . . ?
C21 C30 C31 C32 -101.6(5) . . . . ?
C21 C30 C31 C36 75.4(5) . . . . ?
C36 C31 C32 C33 -2.5(6) . . . . ?
C30 C31 C32 C33 174.6(4) . . . . ?
C31 C32 C33 C34 0.8(7) . . . . ?
C32 C33 C34 C35 1.4(7) . . . . ?
C32 C33 C34 N5 -177.7(4) . . . . ?
O6 N5 C34 C33 -11.3(7) . . . . ?
O7 N5 C34 C33 167.2(5) . . . . ?
O6 N5 C34 C35 169.6(4) . . . . ?
O7 N5 C34 C35 -11.9(7) . . . . ?
C33 C34 C35 C36 -1.8(7) . . . . ?
N5 C34 C35 C36 177.3(4) . . . . ?
C34 C35 C36 C31 0.0(7) . . . . ?
C32 C31 C36 C35 2.1(7) . . . . ?
C30 C31 C36 C35 -175.0(4) . . . . ?
