# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_cyprop
_database_code_depnum_ccdc_archive 'CCDC 1999299'
loop_
_audit_author_name
_audit_author_address
'Ksenia Paseshnichenko'
;Moscow State University
Russia
;
_audit_update_record             
;
2020-04-26 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;

####################################################################

# start Validation Reply Form
_vrf_PLAT234_cyprop              
;
PROBLEM: Large Hirshfeld Difference C19 --C20 . 0.18 Ang.
RESPONSE: The quality of structure determination is not extremely high
because the two-component twin was used for the diffraction experiment.
Thus the anisotropic displacement parameters are determined with
considerable errors
;
_vrf_PLAT341_cyprop              
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.00987 Ang.
RESPONSE: The quality of structure determination is not extremely high
because the two-component twin was used for the diffraction experiment.
;
_vrf_PLAT992_cyprop              
;
PROBLEM: Repd & Actual _reflns_number_gt Values Differ by 19 Check
RESPONSE: This number was assigned by SHELXL during the refinement
procedure
;
# end Validation Reply Form 

####################################################################

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
((1R,2S)-1-(((E)-(2-((((S)-1-Benzyl-2-pyrrolidinyl)carbonyl)amino)-phenyl)-(phenyl)methylidene)amine)-2-(methoxycarbonyl)cyclopropanecarboxylato-N,N',N'',O)-nickel(ii)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H29 N3 Ni O5'
_chemical_formula_sum            'C31 H29 N3 Ni O5'
_chemical_formula_weight         582.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.5849(2)
_cell_length_b                   10.7515(2)
_cell_length_c                   29.4255(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2715.99(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    292(2)
_cell_measurement_reflns_used    22841
_cell_measurement_theta_min      6.38
_cell_measurement_theta_max      69.89

_exptl_crystal_description       'platelike fragment'
_exptl_crystal_colour            red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             1216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.415
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      292(2)
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_type           CuK\a

_diffrn_detector                 Pilatus100K
_diffrn_detector_type            STOE
_diffrn_detector_area_resol_mean 5.81
_diffrn_source                   'Cu GeniX 3D'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_source_voltage           50
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_radiation_monochromator  none
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_measurement_device_type  'Stoe STADI VARI'
_diffrn_measurement_method       'rotation method'
_diffrn_measurement_details      '3039 frames, detector distance 42 mm'

_diffrn_reflns_number            32624
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         5.095
_diffrn_reflns_theta_max         69.783
_diffrn_reflns_theta_full        67.686
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             32624
_reflns_number_gt                29416
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_max     0.971
_reflns_Friedel_fraction_full    0.980

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'STOE X-AREA (Stoe & Cie, 2012)'
_computing_cell_refinement       'STOE X-AREA (Stoe & Cie, 2012)'
_computing_data_reduction        'STOE X-AREA (Stoe & Cie, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  'PLATON (Spek, 2009)'

_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1380P)²+0.0712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1901 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         32624
_refine_ls_number_parameters     363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.1840
_refine_ls_wR_factor_gt          0.1799
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.32035(9) 0.47250(8) 0.38427(3) 0.0471(3) Uani 1 1 d . . . . .
O1 O 0.1821(5) 0.3375(4) 0.38113(16) 0.0582(9) Uani 1 1 d . . . . .
O2 O 0.1869(6) 0.1308(4) 0.3734(2) 0.0787(14) Uani 1 1 d . . . . .
O3 O 0.7237(5) 0.3355(5) 0.33271(17) 0.0692(12) Uani 1 1 d . . . . .
O4 O 0.5803(7) 0.3376(5) 0.26927(18) 0.0769(13) Uani 1 1 d . . . . .
O5 O 0.4875(7) 0.8066(5) 0.3651(2) 0.0843(17) Uani 1 1 d . . . . .
N1 N 0.4710(5) 0.3568(4) 0.39904(16) 0.0447(9) Uani 1 1 d . . . . .
N2 N 0.4517(5) 0.6077(4) 0.39363(17) 0.0498(10) Uani 1 1 d . . . . .
N3 N 0.1663(5) 0.5921(4) 0.36480(18) 0.0544(10) Uani 1 1 d . . . . .
C1 C 0.2523(7) 0.2311(5) 0.3775(2) 0.0561(13) Uani 1 1 d . . . . .
C2 C 0.4259(6) 0.2414(5) 0.3769(2) 0.0493(12) Uani 1 1 d . . . . .
C3 C 0.5881(6) 0.3702(4) 0.42601(18) 0.0439(10) Uani 1 1 d . . . . .
C4 C 0.6299(5) 0.4938(4) 0.44331(19) 0.0462(11) Uani 1 1 d . . . . .
C5 C 0.7360(7) 0.4969(5) 0.4801(2) 0.0571(13) Uani 1 1 d . . . . .
H5 H 0.771950 0.422404 0.492248 0.068 Uiso 1 1 calc R U . . .
C6 C 0.7874(8) 0.6076(6) 0.4985(3) 0.0674(16) Uani 1 1 d . . . . .
H6 H 0.854989 0.608463 0.523138 0.081 Uiso 1 1 calc R U . . .
C7 C 0.7359(9) 0.7166(6) 0.4793(3) 0.0703(17) Uani 1 1 d . . . . .
H7 H 0.773249 0.791904 0.490432 0.084 Uiso 1 1 calc R U . . .
C8 C 0.6312(7) 0.7175(5) 0.4442(3) 0.0607(14) Uani 1 1 d . . . . .
H8 H 0.598203 0.793319 0.432462 0.073 Uiso 1 1 calc R U . . .
C9 C 0.5724(6) 0.6072(5) 0.4254(2) 0.0484(11) Uani 1 1 d . . . . .
C10 C 0.4104(8) 0.7115(5) 0.3694(2) 0.0599(14) Uani 1 1 d . . . . .
C11 C 0.2549(7) 0.7022(5) 0.3466(2) 0.0575(13) Uani 1 1 d . . . . .
H11 H 0.270527 0.691586 0.313858 0.069 Uiso 1 1 calc R U . . .
C12 C 0.1509(9) 0.8154(6) 0.3547(3) 0.076(2) Uani 1 1 d . . . . .
H12A H 0.093264 0.836188 0.327426 0.092 Uiso 1 1 calc R U . . .
H12B H 0.212865 0.886802 0.363645 0.092 Uiso 1 1 calc R U . . .
C13 C 0.0393(11) 0.7779(8) 0.3931(3) 0.088(2) Uani 1 1 d . . . . .
H13A H -0.067964 0.781682 0.382848 0.106 Uiso 1 1 calc R U . . .
H13B H 0.051517 0.832597 0.419076 0.106 Uiso 1 1 calc R U . . .
C14 C 0.0846(9) 0.6441(6) 0.4055(3) 0.0687(16) Uani 1 1 d . . . . .
H14A H 0.153048 0.643386 0.431717 0.082 Uiso 1 1 calc R U . . .
H14B H -0.007417 0.595412 0.412479 0.082 Uiso 1 1 calc R U . . .
C15 C 0.0431(7) 0.5481(7) 0.3317(3) 0.0665(16) Uani 1 1 d . . . . .
H15A H -0.000476 0.470854 0.343046 0.080 Uiso 1 1 calc R U . . .
H15B H -0.040159 0.609046 0.331062 0.080 Uiso 1 1 calc R U . . .
C16 C 0.0993(8) 0.5273(7) 0.2838(2) 0.0664(15) Uani 1 1 d . . . . .
C17 C 0.1917(12) 0.4258(9) 0.2722(3) 0.087(2) Uani 1 1 d . . . . .
H17 H 0.223952 0.370590 0.294619 0.104 Uiso 1 1 calc R U . . .
C18 C 0.2363(13) 0.4060(11) 0.2274(3) 0.097(3) Uani 1 1 d . . . . .
H18 H 0.302376 0.340062 0.220558 0.116 Uiso 1 1 calc R U . . .
C19 C 0.1856(13) 0.4805(11) 0.1936(3) 0.100(3) Uani 1 1 d . . . . .
H19 H 0.212849 0.464045 0.163595 0.120 Uiso 1 1 calc R U . . .
C20 C 0.0931(14) 0.5811(12) 0.2040(3) 0.110(4) Uani 1 1 d . . . . .
H20 H 0.059462 0.634229 0.181079 0.132 Uiso 1 1 calc R U . . .
C21 C 0.0493(10) 0.6036(8) 0.2494(3) 0.086(2) Uani 1 1 d . . . . .
H21 H -0.014323 0.671115 0.256145 0.104 Uiso 1 1 calc R U . . .
C22 C 0.6792(7) 0.2608(5) 0.44303(18) 0.0470(10) Uani 1 1 d . . . . .
C23 C 0.8304(7) 0.2381(5) 0.4306(2) 0.0538(12) Uani 1 1 d . . . . .
H23 H 0.881774 0.292688 0.411192 0.065 Uiso 1 1 calc R U . . .
C24 C 0.9067(8) 0.1337(6) 0.4470(3) 0.0670(16) Uani 1 1 d . . . . .
H24 H 1.008158 0.116688 0.437829 0.080 Uiso 1 1 calc R U . . .
C25 C 0.8323(9) 0.0553(6) 0.4768(3) 0.0745(19) Uani 1 1 d . . . . .
H25 H 0.884289 -0.013914 0.488118 0.089 Uiso 1 1 calc R U . . .
C26 C 0.6821(10) 0.0785(7) 0.4899(3) 0.0747(17) Uani 1 1 d . . . . .
H26 H 0.632884 0.025348 0.510257 0.090 Uiso 1 1 calc R U . . .
C27 C 0.6028(8) 0.1811(6) 0.4728(2) 0.0580(13) Uani 1 1 d . . . . .
H27 H 0.500133 0.196176 0.481242 0.070 Uiso 1 1 calc R U . . .
C28 C 0.4909(7) 0.2161(6) 0.3283(2) 0.0589(13) Uani 1 1 d . . . . .
H28 H 0.416020 0.186277 0.305673 0.071 Uiso 1 1 calc R U . . .
C29 C 0.5240(7) 0.1306(5) 0.3675(2) 0.0588(14) Uani 1 1 d . . . . .
H29A H 0.473120 0.050027 0.367518 0.071 Uiso 1 1 calc R U . . .
H29B H 0.628981 0.130289 0.379708 0.071 Uiso 1 1 calc R U . . .
C30 C 0.6137(8) 0.3014(6) 0.3117(2) 0.0588(13) Uani 1 1 d . . . . .
C31 C 0.6800(14) 0.4359(11) 0.2514(3) 0.106(3) Uani 1 1 d . . . . .
H31A H 0.657887 0.512355 0.266987 0.160 Uiso 1 1 calc R U . . .
H31B H 0.660556 0.446128 0.219530 0.160 Uiso 1 1 calc R U . . .
H31C H 0.787213 0.413860 0.256052 0.160 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 N1 1.847(4) . ?
Ni1 N2 1.860(4) . ?
Ni1 O1 1.877(4) . ?
Ni1 N3 1.932(5) . ?
O1 C1 1.298(7) . ?
O2 C1 1.222(8) . ?
O3 C30 1.187(8) . ?
O4 C30 1.338(8) . ?
O4 C31 1.457(11) . ?
O5 C10 1.224(8) . ?
N1 C3 1.289(7) . ?
N1 C2 1.454(7) . ?
N2 C10 1.371(8) . ?
N2 C9 1.396(8) . ?
N3 C14 1.496(9) . ?
N3 C11 1.505(7) . ?
N3 C15 1.513(8) . ?
C1 C2 1.494(8) . ?
C2 C29 1.485(8) . ?
C2 C28 1.558(8) . ?
C3 C4 1.467(7) . ?
C3 C22 1.498(7) . ?
C4 C5 1.415(8) . ?
C4 C9 1.417(7) . ?
C5 C6 1.380(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.373(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.369(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.401(8) . ?
C8 H8 0.9300 . ?
C10 C11 1.497(9) . ?
C11 C12 1.528(8) . ?
C11 H11 0.9800 . ?
C12 C13 1.534(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.534(10) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.506(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C21 1.373(10) . ?
C16 C17 1.392(12) . ?
C17 C18 1.389(13) . ?
C17 H17 0.9300 . ?
C18 C19 1.349(15) . ?
C18 H18 0.9300 . ?
C19 C20 1.377(17) . ?
C19 H19 0.9300 . ?
C20 C21 1.409(16) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.371(9) . ?
C22 C27 1.391(8) . ?
C23 C24 1.387(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.373(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.369(13) . ?
C25 H25 0.9300 . ?
C26 C27 1.389(9) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C30 1.480(9) . ?
C28 C29 1.503(9) . ?
C28 H28 0.9800 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 93.83(18) . . ?
N1 Ni1 O1 86.20(18) . . ?
N2 Ni1 O1 174.1(2) . . ?
N1 Ni1 N3 176.3(2) . . ?
N2 Ni1 N3 86.5(2) . . ?
O1 Ni1 N3 93.86(19) . . ?
C1 O1 Ni1 113.1(4) . . ?
C30 O4 C31 114.9(6) . . ?
C3 N1 C2 125.4(5) . . ?
C3 N1 Ni1 128.0(4) . . ?
C2 N1 Ni1 106.4(3) . . ?
C10 N2 C9 122.9(5) . . ?
C10 N2 Ni1 113.7(4) . . ?
C9 N2 Ni1 123.1(4) . . ?
C14 N3 C11 103.2(5) . . ?
C14 N3 C15 107.7(5) . . ?
C11 N3 C15 111.8(5) . . ?
C14 N3 Ni1 109.4(4) . . ?
C11 N3 Ni1 106.4(3) . . ?
C15 N3 Ni1 117.4(4) . . ?
O2 C1 O1 125.0(6) . . ?
O2 C1 C2 121.5(6) . . ?
O1 C1 C2 113.5(5) . . ?
N1 C2 C29 128.1(5) . . ?
N1 C2 C1 108.9(5) . . ?
C29 C2 C1 120.6(5) . . ?
N1 C2 C28 117.7(4) . . ?
C29 C2 C28 59.1(4) . . ?
C1 C2 C28 110.9(5) . . ?
N1 C3 C4 120.4(5) . . ?
N1 C3 C22 121.7(4) . . ?
C4 C3 C22 117.8(4) . . ?
C5 C4 C9 119.2(5) . . ?
C5 C4 C3 116.4(4) . . ?
C9 C4 C3 124.4(5) . . ?
C6 C5 C4 121.7(6) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C7 C6 C5 118.2(6) . . ?
C7 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C8 C7 C6 121.7(6) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C7 C8 C9 121.9(6) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
N2 C9 C8 121.9(5) . . ?
N2 C9 C4 120.7(5) . . ?
C8 C9 C4 117.2(5) . . ?
O5 C10 N2 126.4(6) . . ?
O5 C10 C11 119.4(6) . . ?
N2 C10 C11 114.2(5) . . ?
C10 C11 N3 110.1(5) . . ?
C10 C11 C12 113.4(6) . . ?
N3 C11 C12 106.0(5) . . ?
C10 C11 H11 109.1 . . ?
N3 C11 H11 109.1 . . ?
C12 C11 H11 109.1 . . ?
C11 C12 C13 105.7(6) . . ?
C11 C12 H12A 110.6 . . ?
C13 C12 H12A 110.6 . . ?
C11 C12 H12B 110.6 . . ?
C13 C12 H12B 110.6 . . ?
H12A C12 H12B 108.7 . . ?
C12 C13 C14 105.2(6) . . ?
C12 C13 H13A 110.7 . . ?
C14 C13 H13A 110.7 . . ?
C12 C13 H13B 110.7 . . ?
C14 C13 H13B 110.7 . . ?
H13A C13 H13B 108.8 . . ?
N3 C14 C13 106.2(6) . . ?
N3 C14 H14A 110.5 . . ?
C13 C14 H14A 110.5 . . ?
N3 C14 H14B 110.5 . . ?
C13 C14 H14B 110.5 . . ?
H14A C14 H14B 108.7 . . ?
C16 C15 N3 115.1(5) . . ?
C16 C15 H15A 108.5 . . ?
N3 C15 H15A 108.5 . . ?
C16 C15 H15B 108.5 . . ?
N3 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C21 C16 C17 117.7(8) . . ?
C21 C16 C15 120.1(8) . . ?
C17 C16 C15 122.0(6) . . ?
C18 C17 C16 120.7(8) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C19 C18 C17 121.3(11) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 119.2(9) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C19 C20 C21 120.0(8) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C16 C21 C20 120.9(10) . . ?
C16 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C23 C22 C27 120.3(5) . . ?
C23 C22 C3 123.0(5) . . ?
C27 C22 C3 116.7(5) . . ?
C22 C23 C24 119.9(6) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 119.9(6) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C26 C25 C24 120.4(6) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 120.3(7) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C22 119.1(6) . . ?
C26 C27 H27 120.5 . . ?
C22 C27 H27 120.5 . . ?
C30 C28 C29 119.9(6) . . ?
C30 C28 C2 116.8(5) . . ?
C29 C28 C2 58.0(4) . . ?
C30 C28 H28 116.5 . . ?
C29 C28 H28 116.4 . . ?
C2 C28 H28 116.5 . . ?
C2 C29 C28 62.9(4) . . ?
C2 C29 H29A 117.5 . . ?
C28 C29 H29A 117.5 . . ?
C2 C29 H29B 117.5 . . ?
C28 C29 H29B 117.5 . . ?
H29A C29 H29B 114.6 . . ?
O3 C30 O4 124.5(6) . . ?
O3 C30 C28 125.8(6) . . ?
O4 C30 C28 109.6(6) . . ?
O4 C31 H31A 109.5 . . ?
O4 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O4 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

_refine_diff_density_max         0.473
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.043


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
