# Electronic Supplementary Material (ESI) for ChemComm.
# 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. 
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data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1979878'
loop_
_audit_author_name
_audit_author_address
'Dr Hartmut Schubert'
;Eberhard Karls Universitaet Tuebingen
Germany
;
_audit_update_record             
;
2020-01-24 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H19 F3 N2 Ni O2 S'
_chemical_formula_weight         503.17

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   6.9629(8)
_cell_length_b                   27.163(3)
_cell_length_c                   11.1046(13)
_cell_angle_alpha                90
_cell_angle_beta                 96.720(7)
_cell_angle_gamma                90
_cell_volume                     2085.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7244
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.65

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_F_000             1032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.081
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6677
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21116
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.040
_diffrn_reflns_theta_max         27.912
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4950
_reflns_number_gt                3992
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+1.9412P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4950
_refine_ls_number_parameters     292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.0916
_refine_ls_wR_factor_gt          0.0854
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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 0.18589(4) 0.04452(2) 0.12727(2) 0.01153(9) Uani 1 1 d . . . . .
S1 S 0.27724(9) 0.09229(3) 0.36834(5) 0.02472(15) Uani 1 1 d . . . . .
F1 F -0.0339(4) 0.14632(9) 0.39065(17) 0.0870(10) Uani 1 1 d . . . . .
F2 F -0.0081(3) 0.08384(8) 0.50803(16) 0.0526(5) Uani 1 1 d . . . . .
F3 F 0.1791(4) 0.14524(7) 0.54885(16) 0.0684(7) Uani 1 1 d . . . . .
N2 N 0.2231(2) 0.02449(7) -0.02559(16) 0.0110(4) Uani 1 1 d . . . . .
C31 C 0.0467(5) 0.28532(9) -0.1079(3) 0.0324(7) Uani 1 1 d . . . . .
H31A H -0.077542 0.281674 -0.075478 0.049 Uiso 1 1 calc R U . . .
H31B H 0.041523 0.314020 -0.161671 0.049 Uiso 1 1 calc R U . . .
H31C H 0.149792 0.289908 -0.040835 0.049 Uiso 1 1 calc R U . . .
O1 O 0.1377(2) 0.06169(6) 0.28483(14) 0.0208(4) Uani 1 1 d . . . . .
N1 N 0.2531(3) -0.02577(7) 0.17065(17) 0.0145(4) Uani 1 1 d . . . . .
C30 C 0.0745(3) 0.19364(8) 0.0229(2) 0.0149(5) Uani 1 1 d . . . . .
H30 H 0.043249 0.223985 0.058422 0.018 Uiso 1 1 calc R U . . .
C1 C 0.2750(3) -0.05023(9) 0.2757(2) 0.0174(5) Uani 1 1 d . . . . .
H16 H 0.252363 -0.033499 0.347844 0.021 Uiso 1 1 calc R U . . .
C2 C 0.3304(3) -0.09990(9) 0.2827(2) 0.0215(5) Uani 1 1 d . . . . .
H15 H 0.344694 -0.116173 0.358911 0.026 Uiso 1 1 calc R U . . .
C3 C 0.3642(3) -0.12518(9) 0.1802(2) 0.0209(5) Uani 1 1 d . . . . .
H14 H 0.401130 -0.158855 0.185172 0.025 Uiso 1 1 calc R U . . .
C4 C 0.3435(3) -0.10056(8) 0.0670(2) 0.0172(5) Uani 1 1 d . . . . .
C5 C 0.2881(3) -0.05120(8) 0.0691(2) 0.0138(4) Uani 1 1 d . . . . .
C6 C 0.2705(3) -0.02323(8) -0.0401(2) 0.0131(4) Uani 1 1 d . . . . .
C7 C 0.2092(3) 0.05595(8) -0.11931(19) 0.0122(4) Uani 1 1 d . . . . .
C8 C 0.2421(3) 0.03854(8) -0.2350(2) 0.0147(5) Uani 1 1 d . . . . .
H4 H 0.231902 0.060491 -0.302026 0.018 Uiso 1 1 calc R U . . .
C9 C 0.2888(3) -0.01006(9) -0.2511(2) 0.0172(5) Uani 1 1 d . . . . .
H1 H 0.309607 -0.021587 -0.329252 0.021 Uiso 1 1 calc R U . . .
C10 C 0.3058(3) -0.04293(9) -0.1515(2) 0.0160(5) Uani 1 1 d . . . . .
C11 C 0.3593(3) -0.09403(9) -0.1518(2) 0.0195(5) Uani 1 1 d . . . . .
H2 H 0.382653 -0.109131 -0.225843 0.023 Uiso 1 1 calc R U . . .
C12 C 0.3771(3) -0.12129(9) -0.0479(2) 0.0199(5) Uani 1 1 d . . . . .
H3 H 0.412779 -0.154972 -0.051603 0.024 Uiso 1 1 calc R U . . .
C13 C 0.1610(3) 0.10510(8) -0.07780(19) 0.0116(4) Uani 1 1 d . . . . .
C14 C 0.1395(3) 0.10620(8) 0.04839(19) 0.0119(4) Uani 1 1 d . . . . .
C15 C 0.0930(3) 0.15133(8) 0.09535(19) 0.0140(4) Uani 1 1 d . . . . .
H13 H 0.073363 0.153618 0.178392 0.017 Uiso 1 1 calc R U . . .
C16 C 0.1004(3) 0.19269(8) -0.0998(2) 0.0144(5) Uani 1 1 d . . . . .
C17 C 0.1426(3) 0.14711(8) -0.14944(19) 0.0134(4) Uani 1 1 d . . . . .
H5 H 0.158689 0.144900 -0.233045 0.016 Uiso 1 1 calc R U . . .
C18 C 0.0877(3) 0.23902(9) -0.1793(2) 0.0184(5) Uani 1 1 d . . . . .
C19 C -0.0740(4) 0.23293(10) -0.2852(2) 0.0300(6) Uani 1 1 d . . . . .
H7 H -0.049110 0.203492 -0.331931 0.045 Uiso 1 1 calc R U . . .
H9 H -0.077329 0.261948 -0.337828 0.045 Uiso 1 1 calc R U . . .
H8 H -0.198667 0.229485 -0.253167 0.045 Uiso 1 1 calc R U . . .
C20 C 0.2799(4) 0.24658(9) -0.2317(2) 0.0245(5) Uani 1 1 d . . . . .
H12 H 0.304529 0.218343 -0.282651 0.037 Uiso 1 1 calc R U . . .
H11 H 0.385044 0.249559 -0.165277 0.037 Uiso 1 1 calc R U . . .
H10 H 0.272921 0.276681 -0.280707 0.037 Uiso 1 1 calc R U . . .
C21 C 0.0919(5) 0.11807(11) 0.4578(2) 0.0369(7) Uani 1 1 d . . . . .
O2 O 0.3900(3) 0.06222(9) 0.46032(19) 0.0505(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.8296(18) . ?
Ni1 O1 1.8784(16) . ?
Ni1 C14 1.901(2) . ?
Ni1 N1 2.0106(19) . ?
S1 O2 1.462(2) . ?
S1 O1 1.5111(18) . ?
S1 C21 1.855(3) . ?
F1 C21 1.327(3) . ?
F2 C21 1.323(4) . ?
F3 C21 1.339(4) . ?
N2 C7 1.341(3) . ?
N2 C6 1.352(3) . ?
C31 C18 1.532(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N1 C1 1.336(3) . ?
N1 C5 1.369(3) . ?
C30 C16 1.395(3) . ?
C30 C15 1.400(3) . ?
C30 H30 0.9500 . ?
C1 C2 1.403(3) . ?
C1 H16 0.9500 . ?
C2 C3 1.373(4) . ?
C2 H15 0.9500 . ?
C3 C4 1.416(3) . ?
C3 H14 0.9500 . ?
C4 C5 1.396(3) . ?
C4 C12 1.439(3) . ?
C5 C6 1.424(3) . ?
C6 C10 1.396(3) . ?
C7 C8 1.412(3) . ?
C7 C13 1.464(3) . ?
C8 C9 1.376(3) . ?
C8 H4 0.9500 . ?
C9 C10 1.415(3) . ?
C9 H1 0.9500 . ?
C10 C11 1.437(3) . ?
C11 C12 1.364(3) . ?
C11 H2 0.9500 . ?
C12 H3 0.9500 . ?
C13 C17 1.388(3) . ?
C13 C14 1.427(3) . ?
C14 C15 1.385(3) . ?
C15 H13 0.9500 . ?
C16 C17 1.400(3) . ?
C16 C18 1.534(3) . ?
C17 H5 0.9500 . ?
C18 C20 1.534(3) . ?
C18 C19 1.539(3) . ?
C19 H7 0.9800 . ?
C19 H9 0.9800 . ?
C19 H8 0.9800 . ?
C20 H12 0.9800 . ?
C20 H11 0.9800 . ?
C20 H10 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
N2 Ni1 O1 176.47(8) . . ?
N2 Ni1 C14 82.49(9) . . ?
O1 Ni1 C14 99.85(8) . . ?
N2 Ni1 N1 83.44(8) . . ?
O1 Ni1 N1 94.28(8) . . ?
C14 Ni1 N1 165.84(8) . . ?
O2 S1 O1 112.06(13) . . ?
O2 S1 C21 100.78(13) . . ?
O1 S1 C21 95.66(13) . . ?
C7 N2 C6 120.98(19) . . ?
C7 N2 Ni1 121.68(15) . . ?
C6 N2 Ni1 117.31(15) . . ?
C18 C31 H31A 109.5 . . ?
C18 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C18 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
S1 O1 Ni1 122.42(10) . . ?
C1 N1 C5 117.1(2) . . ?
C1 N1 Ni1 132.94(17) . . ?
C5 N1 Ni1 109.91(14) . . ?
C16 C30 C15 122.1(2) . . ?
C16 C30 H30 118.9 . . ?
C15 C30 H30 118.9 . . ?
N1 C1 C2 121.9(2) . . ?
N1 C1 H16 119.0 . . ?
C2 C1 H16 119.0 . . ?
C3 C2 C1 120.5(2) . . ?
C3 C2 H15 119.7 . . ?
C1 C2 H15 119.7 . . ?
C2 C3 C4 119.3(2) . . ?
C2 C3 H14 120.3 . . ?
C4 C3 H14 120.3 . . ?
C5 C4 C3 116.0(2) . . ?
C5 C4 C12 117.7(2) . . ?
C3 C4 C12 126.3(2) . . ?
N1 C5 C4 125.1(2) . . ?
N1 C5 C6 115.2(2) . . ?
C4 C5 C6 119.7(2) . . ?
N2 C6 C10 123.0(2) . . ?
N2 C6 C5 114.07(19) . . ?
C10 C6 C5 122.9(2) . . ?
N2 C7 C8 119.2(2) . . ?
N2 C7 C13 109.58(18) . . ?
C8 C7 C13 131.2(2) . . ?
C9 C8 C7 120.3(2) . . ?
C9 C8 H4 119.8 . . ?
C7 C8 H4 119.8 . . ?
C8 C9 C10 120.2(2) . . ?
C8 C9 H1 119.9 . . ?
C10 C9 H1 119.9 . . ?
C6 C10 C9 116.3(2) . . ?
C6 C10 C11 116.4(2) . . ?
C9 C10 C11 127.3(2) . . ?
C12 C11 C10 121.4(2) . . ?
C12 C11 H2 119.3 . . ?
C10 C11 H2 119.3 . . ?
C11 C12 C4 122.0(2) . . ?
C11 C12 H3 119.0 . . ?
C4 C12 H3 119.0 . . ?
C17 C13 C14 122.2(2) . . ?
C17 C13 C7 125.33(19) . . ?
C14 C13 C7 112.49(19) . . ?
C15 C14 C13 116.37(19) . . ?
C15 C14 Ni1 129.87(16) . . ?
C13 C14 Ni1 113.74(16) . . ?
C14 C15 C30 121.3(2) . . ?
C14 C15 H13 119.3 . . ?
C30 C15 H13 119.3 . . ?
C30 C16 C17 117.2(2) . . ?
C30 C16 C18 122.8(2) . . ?
C17 C16 C18 119.97(19) . . ?
C13 C17 C16 120.7(2) . . ?
C13 C17 H5 119.6 . . ?
C16 C17 H5 119.6 . . ?
C31 C18 C16 112.17(19) . . ?
C31 C18 C20 108.1(2) . . ?
C16 C18 C20 109.51(19) . . ?
C31 C18 C19 108.6(2) . . ?
C16 C18 C19 109.84(19) . . ?
C20 C18 C19 108.5(2) . . ?
C18 C19 H7 109.5 . . ?
C18 C19 H9 109.5 . . ?
H7 C19 H9 109.5 . . ?
C18 C19 H8 109.5 . . ?
H7 C19 H8 109.5 . . ?
H9 C19 H8 109.5 . . ?
C18 C20 H12 109.5 . . ?
C18 C20 H11 109.5 . . ?
H12 C20 H11 109.5 . . ?
C18 C20 H10 109.5 . . ?
H12 C20 H10 109.5 . . ?
H11 C20 H10 109.5 . . ?
F2 C21 F1 107.3(3) . . ?
F2 C21 F3 106.5(2) . . ?
F1 C21 F3 108.5(3) . . ?
F2 C21 S1 113.2(2) . . ?
F1 C21 S1 111.87(18) . . ?
F3 C21 S1 109.3(2) . . ?

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
C14 Ni1 N2 C7 1.02(17) . . . . ?
N1 Ni1 N2 C7 -177.35(17) . . . . ?
C14 Ni1 N2 C6 179.33(17) . . . . ?
N1 Ni1 N2 C6 0.96(15) . . . . ?
O2 S1 O1 Ni1 -102.60(14) . . . . ?
C21 S1 O1 Ni1 153.34(13) . . . . ?
C14 Ni1 O1 S1 -73.85(13) . . . . ?
N1 Ni1 O1 S1 105.18(12) . . . . ?
C5 N1 C1 C2 -0.3(3) . . . . ?
Ni1 N1 C1 C2 -177.55(16) . . . . ?
N1 C1 C2 C3 0.0(4) . . . . ?
C1 C2 C3 C4 0.3(3) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C2 C3 C4 C12 178.7(2) . . . . ?
C1 N1 C5 C4 0.4(3) . . . . ?
Ni1 N1 C5 C4 178.25(18) . . . . ?
C1 N1 C5 C6 -177.61(19) . . . . ?
Ni1 N1 C5 C6 0.2(2) . . . . ?
C3 C4 C5 N1 -0.1(3) . . . . ?
C12 C4 C5 N1 -179.1(2) . . . . ?
C3 C4 C5 C6 177.8(2) . . . . ?
C12 C4 C5 C6 -1.2(3) . . . . ?
C7 N2 C6 C10 -0.6(3) . . . . ?
Ni1 N2 C6 C10 -178.93(16) . . . . ?
C7 N2 C6 C5 177.23(19) . . . . ?
Ni1 N2 C6 C5 -1.1(2) . . . . ?
N1 C5 C6 N2 0.5(3) . . . . ?
C4 C5 C6 N2 -177.64(19) . . . . ?
N1 C5 C6 C10 178.4(2) . . . . ?
C4 C5 C6 C10 0.2(3) . . . . ?
C6 N2 C7 C8 0.9(3) . . . . ?
Ni1 N2 C7 C8 179.13(15) . . . . ?
C6 N2 C7 C13 -178.60(18) . . . . ?
Ni1 N2 C7 C13 -0.4(2) . . . . ?
N2 C7 C8 C9 -0.3(3) . . . . ?
C13 C7 C8 C9 179.0(2) . . . . ?
C7 C8 C9 C10 -0.5(3) . . . . ?
N2 C6 C10 C9 -0.2(3) . . . . ?
C5 C6 C10 C9 -177.9(2) . . . . ?
N2 C6 C10 C11 178.5(2) . . . . ?
C5 C6 C10 C11 0.9(3) . . . . ?
C8 C9 C10 C6 0.8(3) . . . . ?
C8 C9 C10 C11 -177.8(2) . . . . ?
C6 C10 C11 C12 -1.0(3) . . . . ?
C9 C10 C11 C12 177.6(2) . . . . ?
C10 C11 C12 C4 0.0(3) . . . . ?
C5 C4 C12 C11 1.1(3) . . . . ?
C3 C4 C12 C11 -177.8(2) . . . . ?
N2 C7 C13 C17 177.4(2) . . . . ?
C8 C7 C13 C17 -2.0(4) . . . . ?
N2 C7 C13 C14 -0.8(2) . . . . ?
C8 C7 C13 C14 179.8(2) . . . . ?
C17 C13 C14 C15 1.9(3) . . . . ?
C7 C13 C14 C15 -179.75(19) . . . . ?
C17 C13 C14 Ni1 -176.71(16) . . . . ?
C7 C13 C14 Ni1 1.6(2) . . . . ?
C13 C14 C15 C30 -1.9(3) . . . . ?
Ni1 C14 C15 C30 176.46(17) . . . . ?
C16 C30 C15 C14 0.4(3) . . . . ?
C15 C30 C16 C17 1.2(3) . . . . ?
C15 C30 C16 C18 -177.8(2) . . . . ?
C14 C13 C17 C16 -0.4(3) . . . . ?
C7 C13 C17 C16 -178.5(2) . . . . ?
C30 C16 C17 C13 -1.2(3) . . . . ?
C18 C16 C17 C13 177.8(2) . . . . ?
C30 C16 C18 C31 0.8(3) . . . . ?
C17 C16 C18 C31 -178.2(2) . . . . ?
C30 C16 C18 C20 120.8(2) . . . . ?
C17 C16 C18 C20 -58.2(3) . . . . ?
C30 C16 C18 C19 -120.2(2) . . . . ?
C17 C16 C18 C19 60.8(3) . . . . ?
O2 S1 C21 F2 -56.8(2) . . . . ?
O1 S1 C21 F2 57.0(2) . . . . ?
O2 S1 C21 F1 -178.2(3) . . . . ?
O1 S1 C21 F1 -64.4(3) . . . . ?
O2 S1 C21 F3 61.6(2) . . . . ?
O1 S1 C21 F3 175.42(19) . . . . ?

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
_geom_hbond_publ_flag
C17 H5 F3 0.95 2.44 3.390(3) 174.9 1_554 yes
C15 H13 F1 0.95 2.56 3.497(3) 168.1 . yes
C15 H13 S1 0.95 2.92 3.535(2) 123.4 . yes
C8 H4 F2 0.95 2.61 3.395(3) 140.1 1_554 yes
C8 H4 F2 0.95 2.61 3.395(3) 140.1 1_554 yes
C8 H4 F2 0.95 2.61 3.395(3) 140.1 1_554 yes

_refine_diff_density_max         0.688
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.079


_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_AB16122019_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1979881'
loop_
_audit_author_name
_audit_author_address
'Dr Hartmut Schubert'
;Eberhard Karls Universitaet Tuebingen
Germany
;
_audit_update_record             
;
2020-01-24 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H30 F N2 Ni O2'
_chemical_formula_weight         528.27

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

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

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

_cell_length_a                   14.4635(13)
_cell_length_b                   6.9797(6)
_cell_length_c                   25.786(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.159(5)
_cell_angle_gamma                90
_cell_volume                     2562.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9041
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      27.85

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_F_000             1108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    0.795
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36036
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.331
_diffrn_reflns_theta_max         28.025
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6137
_reflns_number_gt                5002
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0501P)²+1.0844P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6137
_refine_ls_number_parameters     331
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0970
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.36162(2) 0.82323(3) 0.44813(2) 0.01580(8) Uani 1 1 d . . . . .
O1 O 0.28126(9) 0.90918(19) 0.38787(5) 0.0213(3) Uani 1 1 d . . . . .
F1 F 0.41223(11) 0.0758(2) 0.25905(5) 0.0493(4) Uani 1 1 d . . . . .
N2 N 0.48566(11) 0.8355(2) 0.42225(6) 0.0184(3) Uani 1 1 d . . . . .
N1 N 0.43699(10) 0.7517(2) 0.51007(5) 0.0159(3) Uani 1 1 d . . . . .
O2 O 0.30028(13) 0.6519(2) 0.33943(6) 0.0414(4) Uani 1 1 d . . . . .
C1 C 0.65227(13) 0.7755(3) 0.45756(7) 0.0200(4) Uani 1 1 d . . . . .
C2 C 0.46180(13) 0.6491(3) 0.59941(7) 0.0199(4) Uani 1 1 d . . . . .
H2 H 0.436886 0.618541 0.630110 0.024 Uiso 1 1 calc R U . . .
C3 C 0.55766(12) 0.7855(2) 0.46202(7) 0.0167(3) Uani 1 1 d . . . . .
C4 C 0.55638(14) 0.6360(3) 0.60042(7) 0.0209(4) Uani 1 1 d . . . . .
H4 H 0.596771 0.595953 0.631663 0.025 Uiso 1 1 calc R U . . .
C5 C 0.40059(13) 0.7076(2) 0.55311(7) 0.0169(3) Uani 1 1 d . . . . .
C6 C 0.69154(13) 0.6731(3) 0.54969(8) 0.0221(4) Uani 1 1 d . . . . .
H6 H 0.737400 0.635383 0.578959 0.027 Uiso 1 1 calc R U . . .
C7 C 0.71853(13) 0.7181(3) 0.50313(8) 0.0225(4) Uani 1 1 d . . . . .
H7 H 0.783247 0.711338 0.500750 0.027 Uiso 1 1 calc R U . . .
C8 C 0.52998(12) 0.7397(3) 0.51072(7) 0.0170(3) Uani 1 1 d . . . . .
C9 C 0.59427(13) 0.6822(3) 0.55490(7) 0.0190(4) Uani 1 1 d . . . . .
C10 C 0.50850(14) 0.8766(3) 0.37590(7) 0.0218(4) Uani 1 1 d . . . . .
H10 H 0.460188 0.911012 0.347475 0.026 Uiso 1 1 calc R U . . .
C11 C 0.67343(14) 0.8218(3) 0.40767(8) 0.0245(4) Uani 1 1 d . . . . .
H11 H 0.736534 0.819063 0.401964 0.029 Uiso 1 1 calc R U . . .
C12 C 0.29872(13) 0.7298(2) 0.54150(7) 0.0173(3) Uani 1 1 d . . . . .
C13 C 0.16918(13) 0.8179(3) 0.47464(7) 0.0209(4) Uani 1 1 d . . . . .
H13 H 0.144027 0.862842 0.440267 0.025 Uiso 1 1 calc R U . . .
C14 C 0.26546(13) 0.7916(2) 0.48889(7) 0.0177(4) Uani 1 1 d . . . . .
C15 C 0.60184(14) 0.8709(3) 0.36746(8) 0.0264(4) Uani 1 1 d . . . . .
H15 H 0.615511 0.901252 0.333697 0.032 Uiso 1 1 calc R U . . .
C16 C 0.23801(13) 0.6926(3) 0.57645(7) 0.0191(4) Uani 1 1 d . . . . .
H16 H 0.262837 0.651560 0.611252 0.023 Uiso 1 1 calc R U . . .
C17 C 0.26258(13) 0.8052(3) 0.34616(7) 0.0199(4) Uani 1 1 d . . . . .
C18 C 0.14123(13) 0.7146(3) 0.56125(7) 0.0200(4) Uani 1 1 d . . . . .
C19 C 0.18289(13) 0.8819(3) 0.30368(7) 0.0264(4) Uani 1 1 d . . . . .
C20 C 0.10890(13) 0.7795(3) 0.50988(7) 0.0224(4) Uani 1 1 d . . . . .
H20 H 0.043356 0.798090 0.498659 0.027 Uiso 1 1 calc R U . . .
C21 C 0.40821(17) 0.4156(3) 0.25987(7) 0.0323(5) Uani 1 1 d . . . . .
H21 H 0.345711 0.415305 0.266605 0.039 Uiso 1 1 calc R U . . .
C22 C 0.19599(15) 0.8147(3) 0.24908(7) 0.0316(5) Uani 1 1 d . . . . .
H22A H 0.200970 0.674658 0.248854 0.047 Uiso 1 1 calc R U . . .
H22B H 0.253463 0.871108 0.240475 0.047 Uiso 1 1 calc R U . . .
H22C H 0.141959 0.855084 0.222887 0.047 Uiso 1 1 calc R U . . .
C23 C -0.02802(14) 0.6843(3) 0.57569(9) 0.0316(5) Uani 1 1 d . . . . .
H23A H -0.042098 0.816772 0.564366 0.047 Uiso 1 1 calc R U . . .
H23B H -0.066469 0.648368 0.601865 0.047 Uiso 1 1 calc R U . . .
H23C H -0.042126 0.598698 0.545194 0.047 Uiso 1 1 calc R U . . .
C24 C 0.07599(14) 0.6673(3) 0.60009(8) 0.0277(4) Uani 1 1 d . . . . .
C25 C 0.45481(17) 0.5859(3) 0.25495(8) 0.0361(5) Uani 1 1 d . . . . .
H25 H 0.424029 0.704263 0.258449 0.043 Uiso 1 1 calc R U . . .
C26 C 0.45470(17) 0.2472(3) 0.25477(7) 0.0310(5) Uani 1 1 d . . . . .
C27 C 0.09349(16) 0.4589(4) 0.61928(10) 0.0434(6) Uani 1 1 d . . . . .
H27A H 0.080090 0.371643 0.589119 0.065 Uiso 1 1 calc R U . . .
H27B H 0.052305 0.428415 0.644511 0.065 Uiso 1 1 calc R U . . .
H27C H 0.159205 0.444401 0.636391 0.065 Uiso 1 1 calc R U . . .
C28 C 0.1764(2) 1.0986(4) 0.30549(10) 0.0617(9) Uani 1 1 d . . . . .
H28A H 0.124613 1.142496 0.278323 0.093 Uiso 1 1 calc R U . . .
H28B H 0.235453 1.154796 0.299073 0.093 Uiso 1 1 calc R U . . .
H28C H 0.164945 1.138583 0.340234 0.093 Uiso 1 1 calc R U . . .
C29 C 0.09656(18) 0.8052(5) 0.64723(9) 0.0502(7) Uani 1 1 d . . . . .
H29A H 0.162813 0.794618 0.663698 0.075 Uiso 1 1 calc R U . . .
H29B H 0.056858 0.771990 0.673016 0.075 Uiso 1 1 calc R U . . .
H29C H 0.083132 0.936936 0.635021 0.075 Uiso 1 1 calc R U . . .
C30 C 0.09327(18) 0.7909(7) 0.31620(10) 0.0833(14) Uani 1 1 d . . . . .
H30A H 0.038908 0.839003 0.291481 0.125 Uiso 1 1 calc R U . . .
H30B H 0.086478 0.824005 0.352272 0.125 Uiso 1 1 calc R U . . .
H30C H 0.096967 0.651378 0.312877 0.125 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 1.8371(14) . ?
Ni1 O1 1.8675(12) . ?
Ni1 C14 1.8983(18) . ?
Ni1 N2 2.0232(16) . ?
O1 C17 1.286(2) . ?
F1 C26 1.358(2) . ?
N2 C10 1.327(2) . ?
N2 C3 1.372(2) . ?
N1 C8 1.345(2) . ?
N1 C5 1.345(2) . ?
O2 C17 1.227(2) . ?
C1 C3 1.395(3) . ?
C1 C11 1.412(3) . ?
C1 C7 1.436(3) . ?
C2 C4 1.367(3) . ?
C2 C5 1.415(2) . ?
C2 H2 0.9500 . ?
C3 C8 1.420(2) . ?
C4 C9 1.417(3) . ?
C4 H4 0.9500 . ?
C5 C12 1.459(2) . ?
C6 C7 1.363(3) . ?
C6 C9 1.438(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.396(2) . ?
C10 C15 1.405(3) . ?
C10 H10 0.9500 . ?
C11 C15 1.373(3) . ?
C11 H11 0.9500 . ?
C12 C16 1.389(3) . ?
C12 C14 1.424(2) . ?
C13 C14 1.388(3) . ?
C13 C20 1.392(3) . ?
C13 H13 0.9500 . ?
C15 H15 0.9500 . ?
C16 C18 1.394(3) . ?
C16 H16 0.9500 . ?
C17 C19 1.539(2) . ?
C18 C20 1.400(3) . ?
C18 C24 1.528(3) . ?
C19 C28 1.516(4) . ?
C19 C22 1.527(3) . ?
C19 C30 1.528(3) . ?
C20 H20 0.9500 . ?
C21 C26 1.372(3) . ?
C21 C25 1.383(3) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.529(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C29 1.538(3) . ?
C24 C27 1.543(3) . ?
C25 C25 1.376(5) 2_655 ?
C25 H25 0.9500 . ?
C26 C26 1.375(5) 2_655 ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
N1 Ni1 O1 175.92(6) . . ?
N1 Ni1 C14 82.38(7) . . ?
O1 Ni1 C14 95.09(7) . . ?
N1 Ni1 N2 82.73(6) . . ?
O1 Ni1 N2 99.79(6) . . ?
C14 Ni1 N2 165.10(7) . . ?
C17 O1 Ni1 121.52(12) . . ?
C10 N2 C3 116.85(16) . . ?
C10 N2 Ni1 133.05(13) . . ?
C3 N2 Ni1 110.08(12) . . ?
C8 N1 C5 120.77(15) . . ?
C8 N1 Ni1 117.81(12) . . ?
C5 N1 Ni1 121.40(12) . . ?
C3 C1 C11 115.92(17) . . ?
C3 C1 C7 117.99(17) . . ?
C11 C1 C7 126.08(18) . . ?
C4 C2 C5 120.69(17) . . ?
C4 C2 H2 119.7 . . ?
C5 C2 H2 119.7 . . ?
N2 C3 C1 125.29(16) . . ?
N2 C3 C8 115.02(16) . . ?
C1 C3 C8 119.68(16) . . ?
C2 C4 C9 120.07(17) . . ?
C2 C4 H4 120.0 . . ?
C9 C4 H4 120.0 . . ?
N1 C5 C2 118.97(16) . . ?
N1 C5 C12 109.53(15) . . ?
C2 C5 C12 131.50(16) . . ?
C7 C6 C9 120.60(17) . . ?
C7 C6 H6 119.7 . . ?
C9 C6 H6 119.7 . . ?
C6 C7 C1 122.11(17) . . ?
C6 C7 H7 118.9 . . ?
C1 C7 H7 118.9 . . ?
N1 C8 C9 123.28(16) . . ?
N1 C8 C3 114.35(15) . . ?
C9 C8 C3 122.35(16) . . ?
C8 C9 C4 116.22(17) . . ?
C8 C9 C6 117.27(17) . . ?
C4 C9 C6 126.51(17) . . ?
N2 C10 C15 122.15(18) . . ?
N2 C10 H10 118.9 . . ?
C15 C10 H10 118.9 . . ?
C15 C11 C1 119.31(18) . . ?
C15 C11 H11 120.3 . . ?
C1 C11 H11 120.3 . . ?
C16 C12 C14 121.92(17) . . ?
C16 C12 C5 125.31(16) . . ?
C14 C12 C5 112.77(16) . . ?
C14 C13 C20 121.08(17) . . ?
C14 C13 H13 119.5 . . ?
C20 C13 H13 119.5 . . ?
C13 C14 C12 116.54(16) . . ?
C13 C14 Ni1 129.55(14) . . ?
C12 C14 Ni1 113.91(13) . . ?
C11 C15 C10 120.47(18) . . ?
C11 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
C12 C16 C18 121.01(17) . . ?
C12 C16 H16 119.5 . . ?
C18 C16 H16 119.5 . . ?
O2 C17 O1 125.25(17) . . ?
O2 C17 C19 119.88(17) . . ?
O1 C17 C19 114.80(16) . . ?
C16 C18 C20 116.93(17) . . ?
C16 C18 C24 119.83(16) . . ?
C20 C18 C24 123.23(17) . . ?
C28 C19 C22 110.69(18) . . ?
C28 C19 C30 110.4(3) . . ?
C22 C19 C30 108.3(2) . . ?
C28 C19 C17 111.57(19) . . ?
C22 C19 C17 110.48(16) . . ?
C30 C19 C17 105.16(18) . . ?
C13 C20 C18 122.47(18) . . ?
C13 C20 H20 118.8 . . ?
C18 C20 H20 118.8 . . ?
C26 C21 C25 118.2(2) . . ?
C26 C21 H21 120.9 . . ?
C25 C21 H21 120.9 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C24 C23 112.95(17) . . ?
C18 C24 C29 109.10(18) . . ?
C23 C24 C29 108.41(18) . . ?
C18 C24 C27 109.16(16) . . ?
C23 C24 C27 107.39(18) . . ?
C29 C24 C27 109.8(2) . . ?
C25 C25 C21 120.76(14) 2_655 . ?
C25 C25 H25 119.6 2_655 . ?
C21 C25 H25 119.6 . . ?
F1 C26 C21 120.7(2) . . ?
F1 C26 C26 118.26(12) . 2_655 ?
C21 C26 C26 121.05(13) . 2_655 ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C19 C28 H28A 109.5 . . ?
C19 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C19 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C19 C30 H30A 109.5 . . ?
C19 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C19 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_refine_diff_density_max         0.491
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.074


_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1979879'
loop_
_audit_author_name
_audit_author_address
'Dr Hartmut Schubert'
;Eberhard Karls Universitaet Tuebingen
Germany
;
_audit_update_record             
;
2020-01-24 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H37 N3 Ni O Si2'
_chemical_formula_weight         546.48

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
H H 0.0000 0.0000 '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                   11.9534(7)
_cell_length_b                   13.7247(7)
_cell_length_c                   17.1253(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.5720(10)
_cell_angle_gamma                90
_cell_volume                     2804.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9799
_cell_measurement_theta_min      3.87
_cell_measurement_theta_max      30.50

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_F_000             1160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.803
_shelx_estimated_absorpt_T_min   0.6744
_shelx_estimated_absorpt_T_max   0.7461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44954
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.208
_diffrn_reflns_theta_max         30.503
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8514
_reflns_number_gt                7630
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0486P)²+0.8267P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8514
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0856
_refine_ls_wR_factor_gt          0.0787
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.65138(2) 0.39135(2) 0.33747(2) 0.01133(5) Uani 1 1 d . . . . .
Si2 Si 0.85027(3) 0.26637(2) 0.38441(2) 0.01373(7) Uani 1 1 d . . . . .
Si1 Si 0.80187(3) 0.32561(2) 0.21250(2) 0.01640(7) Uani 1 1 d . . . . .
O1 O 0.75264(7) 0.48993(6) 0.34372(6) 0.02092(18) Uani 1 1 d . . . . .
N3 N 0.54162(8) 0.29055(7) 0.32859(6) 0.01330(17) Uani 1 1 d . . . . .
N2 N 0.53399(8) 0.47013(7) 0.37393(5) 0.01139(16) Uani 1 1 d . . . . .
N1 N 0.76669(8) 0.30575(7) 0.30640(6) 0.01275(17) Uani 1 1 d . . . . .
C2 C 0.44086(10) 0.60361(8) 0.43259(7) 0.0157(2) Uani 1 1 d . . . . .
H2 H 0.443442 0.668853 0.451154 0.019 Uiso 1 1 calc R U . . .
C3 C 0.63553(10) 0.72478(8) 0.40443(7) 0.0147(2) Uani 1 1 d . . . . .
H3 H 0.568553 0.752447 0.421727 0.018 Uiso 1 1 calc R U . . .
C4 C 0.44122(9) 0.31935(8) 0.35455(6) 0.01337(19) Uani 1 1 d . . . . .
C5 C 0.43754(9) 0.41736(8) 0.38096(6) 0.01255(19) Uani 1 1 d . . . . .
C6 C 0.34642(10) 0.25874(9) 0.35597(7) 0.0164(2) Uani 1 1 d . . . . .
C7 C 0.34535(10) 0.55038(9) 0.43971(7) 0.0168(2) Uani 1 1 d . . . . .
H7 H 0.282861 0.578384 0.463042 0.020 Uiso 1 1 calc R U . . .
C8 C 0.24705(10) 0.29772(10) 0.38718(8) 0.0202(2) Uani 1 1 d . . . . .
H8 H 0.182047 0.258082 0.388580 0.024 Uiso 1 1 calc R U . . .
C9 C 0.35778(10) 0.16324(9) 0.32711(7) 0.0195(2) Uani 1 1 d . . . . .
H9 H 0.296330 0.119265 0.326007 0.023 Uiso 1 1 calc R U . . .
C10 C 0.53738(9) 0.56412(8) 0.39797(6) 0.01201(19) Uani 1 1 d . . . . .
C11 C 0.61569(11) 0.92767(9) 0.44864(9) 0.0239(3) Uani 1 1 d . . . . .
H11A H 0.549563 0.911887 0.414259 0.036 Uiso 1 1 calc R U . . .
H11B H 0.618321 0.998083 0.458068 0.036 Uiso 1 1 calc R U . . .
H11C H 0.611378 0.893339 0.498539 0.036 Uiso 1 1 calc R U . . .
C12 C 0.54985(10) 0.19965(9) 0.30206(7) 0.0166(2) Uani 1 1 d . . . . .
H12 H 0.619085 0.178325 0.283655 0.020 Uiso 1 1 calc R U . . .
C13 C 0.72192(10) 0.89586(8) 0.40956(7) 0.0171(2) Uani 1 1 d . . . . .
C14 C 0.34036(9) 0.45323(9) 0.41205(7) 0.0148(2) Uani 1 1 d . . . . .
C15 C 0.24466(10) 0.39072(9) 0.41481(8) 0.0195(2) Uani 1 1 d . . . . .
H15 H 0.178528 0.414516 0.436240 0.023 Uiso 1 1 calc R U . . .
C16 C 0.67216(13) 0.36716(12) 0.15353(8) 0.0286(3) Uani 1 1 d . . . . .
H16A H 0.613302 0.317812 0.156378 0.043 Uiso 1 1 calc R U . . .
H16B H 0.689665 0.376371 0.098870 0.043 Uiso 1 1 calc R U . . .
H16C H 0.646098 0.428896 0.174689 0.043 Uiso 1 1 calc R U . . .
C17 C 0.45909(11) 0.13453(9) 0.30055(7) 0.0193(2) Uani 1 1 d . . . . .
H17 H 0.467631 0.070311 0.281093 0.023 Uiso 1 1 calc R U . . .
C18 C 0.72489(13) 0.94726(10) 0.32973(8) 0.0261(3) Uani 1 1 d . . . . .
H18A H 0.792781 0.927885 0.304446 0.039 Uiso 1 1 calc R U . . .
H18B H 0.725118 1.018002 0.337485 0.039 Uiso 1 1 calc R U . . .
H18C H 0.658677 0.928569 0.296476 0.039 Uiso 1 1 calc R U . . .
C19 C 0.72576(10) 0.78538(8) 0.39589(7) 0.0163(2) Uani 1 1 d . . . . .
C20 C 0.82486(10) 0.74192(9) 0.37098(9) 0.0222(3) Uani 1 1 d . . . . .
H20 H 0.889040 0.781392 0.364944 0.027 Uiso 1 1 calc R U . . .
C21 C 0.93684(11) 0.36408(10) 0.43631(8) 0.0230(2) Uani 1 1 d . . . . .
H21A H 0.982262 0.397381 0.398776 0.034 Uiso 1 1 calc R U . . .
H21B H 0.986168 0.334463 0.477575 0.034 Uiso 1 1 calc R U . . .
H21C H 0.887145 0.411247 0.459589 0.034 Uiso 1 1 calc R U . . .
C22 C 0.63714(9) 0.62275(8) 0.38872(6) 0.01275(19) Uani 1 1 d . . . . .
C23 C 0.95271(11) 0.16977(10) 0.35646(8) 0.0218(2) Uani 1 1 d . . . . .
H23A H 0.911825 0.115997 0.330061 0.033 Uiso 1 1 calc R U . . .
H23B H 0.994013 0.145280 0.403661 0.033 Uiso 1 1 calc R U . . .
H23C H 1.005509 0.197860 0.321138 0.033 Uiso 1 1 calc R U . . .
C24 C 0.76040(11) 0.20995(9) 0.45868(7) 0.0194(2) Uani 1 1 d . . . . .
H24A H 0.713403 0.260315 0.480580 0.029 Uiso 1 1 calc R U . . .
H24B H 0.808455 0.180506 0.500743 0.029 Uiso 1 1 calc R U . . .
H24C H 0.712559 0.159636 0.433406 0.029 Uiso 1 1 calc R U . . .
C25 C 0.73680(9) 0.58139(8) 0.36253(7) 0.0157(2) Uani 1 1 d . . . . .
C26 C 0.82367(11) 0.92776(10) 0.46309(9) 0.0250(3) Uani 1 1 d . . . . .
H26A H 0.822868 0.893306 0.513171 0.037 Uiso 1 1 calc R U . . .
H26B H 0.819989 0.998149 0.472197 0.037 Uiso 1 1 calc R U . . .
H26C H 0.892891 0.912123 0.437949 0.037 Uiso 1 1 calc R U . . .
C27 C 0.85143(11) 0.20944(11) 0.16746(7) 0.0225(3) Uani 1 1 d . . . . .
H27A H 0.922950 0.189671 0.193842 0.034 Uiso 1 1 calc R U . . .
H27B H 0.861526 0.220097 0.111754 0.034 Uiso 1 1 calc R U . . .
H27C H 0.795623 0.158082 0.173345 0.034 Uiso 1 1 calc R U . . .
C28 C 0.83024(10) 0.64408(9) 0.35537(9) 0.0228(3) Uani 1 1 d . . . . .
H28 H 0.898453 0.617416 0.339296 0.027 Uiso 1 1 calc R U . . .
C29 C 0.91383(14) 0.41917(12) 0.20051(10) 0.0361(4) Uani 1 1 d . . . . .
H29A H 0.889490 0.481931 0.220847 0.054 Uiso 1 1 calc R U . . .
H29B H 0.927417 0.425888 0.144926 0.054 Uiso 1 1 calc R U . . .
H29C H 0.983084 0.398597 0.229507 0.054 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 1.8141(9) . ?
Ni1 N3 1.9061(10) . ?
Ni1 N2 1.9071(9) . ?
Ni1 N1 1.9117(9) . ?
Si2 N1 1.7054(10) . ?
Si2 C24 1.8819(13) . ?
Si2 C21 1.8827(13) . ?
Si2 C23 1.8866(13) . ?
Si1 N1 1.7093(10) . ?
Si1 C29 1.8752(16) . ?
Si1 C27 1.8828(13) . ?
Si1 C16 1.8851(14) . ?
O1 C25 1.3126(14) . ?
N3 C12 1.3334(15) . ?
N3 C4 1.3641(14) . ?
N2 C10 1.3540(14) . ?
N2 C5 1.3733(14) . ?
C2 C7 1.3672(16) . ?
C2 C10 1.4358(15) . ?
C2 H2 0.9500 . ?
C3 C19 1.3769(16) . ?
C3 C22 1.4264(15) . ?
C3 H3 0.9500 . ?
C4 C6 1.4072(15) . ?
C4 C5 1.4207(15) . ?
C5 C14 1.3972(15) . ?
C6 C9 1.4103(17) . ?
C6 C8 1.4358(17) . ?
C7 C14 1.4151(17) . ?
C7 H7 0.9500 . ?
C8 C15 1.3623(18) . ?
C8 H8 0.9500 . ?
C9 C17 1.3775(18) . ?
C9 H9 0.9500 . ?
C10 C22 1.4554(15) . ?
C11 C13 1.5352(18) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C17 1.4046(16) . ?
C12 H12 0.9500 . ?
C13 C19 1.5355(16) . ?
C13 C26 1.5402(18) . ?
C13 C18 1.5407(18) . ?
C14 C15 1.4329(16) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.4156(17) . ?
C20 C28 1.3715(17) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C25 1.4174(15) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C28 1.4212(16) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 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 N3 178.00(4) . . ?
O1 Ni1 N2 93.42(4) . . ?
N3 Ni1 N2 85.46(4) . . ?
O1 Ni1 N1 89.13(4) . . ?
N3 Ni1 N1 92.09(4) . . ?
N2 Ni1 N1 175.95(4) . . ?
N1 Si2 C24 109.19(5) . . ?
N1 Si2 C21 114.96(6) . . ?
C24 Si2 C21 107.11(6) . . ?
N1 Si2 C23 112.44(5) . . ?
C24 Si2 C23 106.81(6) . . ?
C21 Si2 C23 105.90(6) . . ?
N1 Si1 C29 115.55(7) . . ?
N1 Si1 C27 110.64(5) . . ?
C29 Si1 C27 106.87(7) . . ?
N1 Si1 C16 108.06(6) . . ?
C29 Si1 C16 107.64(8) . . ?
C27 Si1 C16 107.82(6) . . ?
C25 O1 Ni1 128.45(8) . . ?
C12 N3 C4 117.85(10) . . ?
C12 N3 Ni1 129.88(8) . . ?
C4 N3 Ni1 112.26(7) . . ?
C10 N2 C5 119.02(9) . . ?
C10 N2 Ni1 129.13(8) . . ?
C5 N2 Ni1 111.63(7) . . ?
Si2 N1 Si1 128.40(6) . . ?
Si2 N1 Ni1 111.97(5) . . ?
Si1 N1 Ni1 112.81(5) . . ?
C7 C2 C10 122.14(11) . . ?
C7 C2 H2 118.9 . . ?
C10 C2 H2 118.9 . . ?
C19 C3 C22 123.58(11) . . ?
C19 C3 H3 118.2 . . ?
C22 C3 H3 118.2 . . ?
N3 C4 C6 124.07(11) . . ?
N3 C4 C5 115.05(10) . . ?
C6 C4 C5 120.88(10) . . ?
N2 C5 C14 124.76(10) . . ?
N2 C5 C4 115.38(10) . . ?
C14 C5 C4 119.86(10) . . ?
C4 C6 C9 116.62(11) . . ?
C4 C6 C8 118.16(11) . . ?
C9 C6 C8 125.21(11) . . ?
C2 C7 C14 119.45(10) . . ?
C2 C7 H7 120.3 . . ?
C14 C7 H7 120.3 . . ?
C15 C8 C6 120.93(11) . . ?
C15 C8 H8 119.5 . . ?
C6 C8 H8 119.5 . . ?
C17 C9 C6 119.17(11) . . ?
C17 C9 H9 120.4 . . ?
C6 C9 H9 120.4 . . ?
N2 C10 C2 118.41(10) . . ?
N2 C10 C22 120.18(10) . . ?
C2 C10 C22 121.41(10) . . ?
C13 C11 H11A 109.5 . . ?
C13 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C13 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C17 121.90(11) . . ?
N3 C12 H12 119.1 . . ?
C17 C12 H12 119.1 . . ?
C11 C13 C19 112.38(10) . . ?
C11 C13 C26 107.68(11) . . ?
C19 C13 C26 109.97(10) . . ?
C11 C13 C18 108.79(11) . . ?
C19 C13 C18 108.32(10) . . ?
C26 C13 C18 109.69(11) . . ?
C5 C14 C7 116.15(10) . . ?
C5 C14 C15 119.08(11) . . ?
C7 C14 C15 124.76(11) . . ?
C8 C15 C14 121.03(11) . . ?
C8 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C9 C17 C12 120.38(11) . . ?
C9 C17 H17 119.8 . . ?
C12 C17 H17 119.8 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C3 C19 C20 116.96(10) . . ?
C3 C19 C13 123.31(11) . . ?
C20 C19 C13 119.71(10) . . ?
C28 C20 C19 121.43(11) . . ?
C28 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C22 C3 118.32(10) . . ?
C25 C22 C10 121.57(10) . . ?
C3 C22 C10 120.10(10) . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O1 C25 C22 126.69(10) . . ?
O1 C25 C28 115.57(10) . . ?
C22 C25 C28 117.74(10) . . ?
C13 C26 H26A 109.5 . . ?
C13 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C13 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si1 C27 H27A 109.5 . . ?
Si1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C20 C28 C25 121.96(11) . . ?
C20 C28 H28 119.0 . . ?
C25 C28 H28 119.0 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

_refine_diff_density_max         0.525
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1979882'
loop_
_audit_author_name
_audit_author_address
'Dr Hartmut Schubert'
;Eberhard Karls Universitaet Tuebingen
Germany
;
_audit_update_record             
;
2020-01-24 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H55.50 N4.50 Ni1.50 Si3'
_chemical_formula_weight         795.74

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'

_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                   23.5957(7)
_cell_length_b                   13.6797(4)
_cell_length_c                   26.9113(8)
_cell_angle_alpha                90
_cell_angle_beta                 101.4330(10)
_cell_angle_gamma                90
_cell_volume                     8514.1(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9756
_cell_measurement_theta_min      3.24
_cell_measurement_theta_max      28.29

_exptl_crystal_description       prism
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             3384
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.576
_exptl_crystal_size_mid          0.434
_exptl_crystal_size_min          0.226
_exptl_absorpt_coefficient_mu    0.788
_shelx_estimated_absorpt_T_min   0.659
_shelx_estimated_absorpt_T_max   0.842
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8170
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            106842
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.677
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             21075
_reflns_number_gt                17698
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0462P)²+4.3064P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         21075
_refine_ls_number_parameters     946
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0958
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
Ni3 Ni 0.84458(2) -0.05112(2) 0.50700(2) 0.01116(5) Uani 1 1 d . . . . .
Ni1 Ni 0.50563(2) 0.56202(2) 0.33880(2) 0.01094(5) Uani 1 1 d . . . . .
Ni2 Ni 0.82678(2) 0.44843(2) 0.33263(2) 0.01039(5) Uani 1 1 d . . . . .
Si1 Si 0.47653(2) 0.66666(3) 0.43051(2) 0.01282(8) Uani 1 1 d . . . . .
Si6 Si 0.80847(2) -0.15294(3) 0.59770(2) 0.01321(8) Uani 1 1 d . . . . .
Si5 Si 0.72022(2) -0.11337(3) 0.49974(2) 0.01677(9) Uani 1 1 d . . . . .
Si3 Si 0.95164(2) 0.38265(3) 0.34034(2) 0.01718(9) Uani 1 1 d . . . . .
Si4 Si 0.86069(2) 0.34022(3) 0.24412(2) 0.01498(8) Uani 1 1 d . . . . .
Si2 Si 0.38296(2) 0.64229(3) 0.33564(2) 0.02114(9) Uani 1 1 d . . . . .
N9 N 0.56222(5) 0.50189(8) 0.31078(4) 0.0121(2) Uani 1 1 d . . . . .
N6 N 0.76919(5) 0.50688(8) 0.36005(4) 0.0115(2) Uani 1 1 d . . . . .
N3 N 0.90100(5) 0.00345(9) 0.47663(4) 0.0127(2) Uani 1 1 d . . . . .
N7 N 0.79979(5) 0.32732(8) 0.36657(4) 0.0126(2) Uani 1 1 d . . . . .
N8 N 0.53476(5) 0.68284(9) 0.30543(4) 0.0142(2) Uani 1 1 d . . . . .
N4 N 0.86917(5) -0.17515(9) 0.47375(4) 0.0142(2) Uani 1 1 d . . . . .
N1 N 0.78746(5) -0.11125(8) 0.53713(4) 0.0132(2) Uani 1 1 d . . . . .
C14 C 0.87614(6) 0.14603(10) 0.51158(5) 0.0134(3) Uani 1 1 d . . . . .
C15 C 0.79820(6) 0.74546(10) 0.31266(5) 0.0141(3) Uani 1 1 d . . . . .
H15 H 0.771138 0.788378 0.323097 0.017 Uiso 1 1 calc R U . . .
N2 N 0.45106(5) 0.62767(8) 0.36996(4) 0.0132(2) Uani 1 1 d . . . . .
C17 C 0.74472(6) 0.18689(11) 0.41714(6) 0.0175(3) Uani 1 1 d . . . . .
H17 H 0.726715 0.138417 0.433997 0.021 Uiso 1 1 calc R U . . .
C18 C 0.79753(6) 0.64650(10) 0.32450(5) 0.0121(3) Uani 1 1 d . . . . .
C19 C 0.71233(6) 0.64428(10) 0.37322(5) 0.0146(3) Uani 1 1 d . . . . .
H19 H 0.704283 0.712130 0.368882 0.018 Uiso 1 1 calc R U . . .
C20 C 0.61785(6) 0.36264(10) 0.29770(5) 0.0153(3) Uani 1 1 d . . . . .
H20 H 0.625493 0.294722 0.302382 0.018 Uiso 1 1 calc R U . . .
C21 C 0.53169(6) 0.36254(10) 0.34517(5) 0.0127(3) Uani 1 1 d . . . . .
C22 C 0.87774(6) 0.24612(10) 0.52237(5) 0.0161(3) Uani 1 1 d . . . . .
H22 H 0.904867 0.286722 0.510443 0.019 Uiso 1 1 calc R U . . .
N5 N 0.88409(5) 0.38524(8) 0.30387(4) 0.0136(2) Uani 1 1 d . . . . .
C24 C 0.57253(6) 0.40595(10) 0.31724(5) 0.0128(3) Uani 1 1 d . . . . .
C25 C 0.49319(6) 0.43197(10) 0.35978(5) 0.0128(3) Uani 1 1 d . . . . .
C26 C 0.58988(7) 0.82027(11) 0.25306(6) 0.0191(3) Uani 1 1 d . . . . .
H26 H 0.607762 0.867616 0.235411 0.023 Uiso 1 1 calc R U . . .
C27 C 0.83632(6) 0.57787(10) 0.30963(5) 0.0123(3) Uani 1 1 d . . . . .
C28 C 0.91354(6) 0.09884(10) 0.48183(5) 0.0135(3) Uani 1 1 d . . . . .
C29 C 0.52935(6) 0.26338(10) 0.35601(5) 0.0143(3) Uani 1 1 d . . . . .
H29 H 0.556488 0.220013 0.346021 0.017 Uiso 1 1 calc R U . . .
C30 C 0.79105(6) 0.16321(11) 0.39520(6) 0.0174(3) Uani 1 1 d . . . . .
H30 H 0.805186 0.098017 0.397024 0.021 Uiso 1 1 calc R U . . .
C31 C 0.75776(6) 0.60239(10) 0.35326(5) 0.0121(3) Uani 1 1 d . . . . .
C32 C 0.69138(6) 0.48564(10) 0.40576(5) 0.0138(3) Uani 1 1 d . . . . .
C33 C 0.67951(6) 0.58691(11) 0.39904(5) 0.0158(3) Uani 1 1 d . . . . .
H33 H 0.648941 0.615425 0.412322 0.019 Uiso 1 1 calc R U . . .
C34 C 0.91797(7) -0.31943(11) 0.42045(6) 0.0209(3) Uani 1 1 d . . . . .
H34 H 0.933749 -0.369044 0.402547 0.025 Uiso 1 1 calc R U . . .
C35 C 0.66093(6) 0.41640(11) 0.43088(5) 0.0170(3) Uani 1 1 d . . . . .
H35 H 0.629159 0.437823 0.444910 0.020 Uiso 1 1 calc R U . . .
C36 C 0.66992(6) 0.58756(11) 0.23807(6) 0.0185(3) Uani 1 1 d . . . . .
H36 H 0.700938 0.564809 0.223416 0.022 Uiso 1 1 calc R U . . .
C37 C 0.95787(6) 0.13805(11) 0.45932(6) 0.0178(3) Uani 1 1 d . . . . .
H37 H 0.967202 0.205557 0.463034 0.021 Uiso 1 1 calc R U . . .
C38 C 0.65110(6) 0.41875(11) 0.27180(5) 0.0165(3) Uani 1 1 d . . . . .
H38 H 0.681590 0.389349 0.258768 0.020 Uiso 1 1 calc R U . . .
C39 C 0.83721(6) 0.08038(10) 0.52843(5) 0.0138(3) Uani 1 1 d . . . . .
C40 C 1.00053(6) -0.09311(12) 0.39864(6) 0.0215(3) Uani 1 1 d . . . . .
H40 H 1.030608 -0.073214 0.382055 0.026 Uiso 1 1 calc R U . . .
C41 C 0.67684(6) 0.32046(11) 0.43495(6) 0.0175(3) Uani 1 1 d . . . . .
H41 H 0.655964 0.276444 0.451907 0.021 Uiso 1 1 calc R U . . .
C42 C 0.54517(7) 0.84644(11) 0.27655(6) 0.0190(3) Uani 1 1 d . . . . .
H42 H 0.532261 0.912344 0.275232 0.023 Uiso 1 1 calc R U . . .
C43 C 0.93005(6) -0.05522(10) 0.45011(5) 0.0141(3) Uani 1 1 d . . . . .
C44 C 0.87498(6) 0.61539(10) 0.28152(5) 0.0152(3) Uani 1 1 d . . . . .
H44 H 0.901061 0.572346 0.269776 0.018 Uiso 1 1 calc R U . . .
C45 C 0.65465(6) 0.68367(12) 0.23359(6) 0.0194(3) Uani 1 1 d . . . . .
H45 H 0.674965 0.726321 0.215408 0.023 Uiso 1 1 calc R U . . .
C46 C 0.48766(6) 0.22661(10) 0.38136(5) 0.0143(3) Uani 1 1 d . . . . .
C47 C 0.87620(6) 0.71527(10) 0.27020(5) 0.0163(3) Uani 1 1 d . . . . .
H47 H 0.903677 0.738192 0.251464 0.020 Uiso 1 1 calc R U . . .
C48 C 0.51859(6) 0.77591(10) 0.30246(5) 0.0166(3) Uani 1 1 d . . . . .
H48 H 0.487957 0.795694 0.318391 0.020 Uiso 1 1 calc R U . . .
C49 C 0.63989(6) 0.51992(11) 0.26462(5) 0.0143(3) Uani 1 1 d . . . . .
C50 C 0.85116(6) -0.26730(11) 0.47260(5) 0.0173(3) Uani 1 1 d . . . . .
H50 H 0.821296 -0.284028 0.490107 0.021 Uiso 1 1 calc R U . . .
C51 C 0.97398(6) -0.02213(11) 0.42624(5) 0.0170(3) Uani 1 1 d . . . . .
C52 C 0.73732(6) 0.45019(10) 0.38509(5) 0.0119(3) Uani 1 1 d . . . . .
C53 C 0.72451(6) 0.28426(10) 0.41416(5) 0.0145(3) Uani 1 1 d . . . . .
C54 C 0.81738(6) 0.23505(10) 0.37018(5) 0.0154(3) Uani 1 1 d . . . . .
H54 H 0.849081 0.216843 0.355236 0.018 Uiso 1 1 calc R U . . .
C55 C 0.98764(6) 0.07830(12) 0.43192(6) 0.0196(3) Uani 1 1 d . . . . .
H55 H 1.017397 0.104884 0.416862 0.024 Uiso 1 1 calc R U . . .
C56 C 0.87474(7) -0.34105(11) 0.44634(6) 0.0206(3) Uani 1 1 d . . . . .
H56 H 0.860734 -0.406133 0.446493 0.025 Uiso 1 1 calc R U . . .
C57 C 0.93852(6) -0.22245(11) 0.42090(5) 0.0178(3) Uani 1 1 d . . . . .
C58 C 0.79808(6) 0.41212(12) 0.20857(6) 0.0203(3) Uani 1 1 d . . . . .
H58A H 0.765247 0.406148 0.225690 0.030 Uiso 1 1 calc R U . . .
H58B H 0.787106 0.386800 0.173931 0.030 Uiso 1 1 calc R U . . .
H58C H 0.809104 0.481035 0.207492 0.030 Uiso 1 1 calc R U . . .
C59 C 0.80135(7) 0.22274(11) 0.56738(6) 0.0195(3) Uani 1 1 d . . . . .
H59 H 0.774971 0.248461 0.586484 0.023 Uiso 1 1 calc R U . . .
C60 C 0.80030(6) 0.12230(11) 0.55717(6) 0.0170(3) Uani 1 1 d . . . . .
H60 H 0.773889 0.081747 0.570075 0.020 Uiso 1 1 calc R U . . .
C61 C 0.75417(6) 0.35047(10) 0.38885(5) 0.0121(3) Uani 1 1 d . . . . .
C62 C 0.44966(6) 0.29437(11) 0.39601(6) 0.0168(3) Uani 1 1 d . . . . .
H62 H 0.420837 0.271649 0.413340 0.020 Uiso 1 1 calc R U . . .
C63 C 0.83833(6) 0.78240(10) 0.28556(5) 0.0147(3) Uani 1 1 d . . . . .
C64 C 0.57914(6) 0.65741(10) 0.28211(5) 0.0132(3) Uani 1 1 d . . . . .
C65 C 0.59454(6) 0.55735(10) 0.28561(5) 0.0131(3) Uani 1 1 d . . . . .
C66 C 0.60859(6) 0.72227(11) 0.25566(5) 0.0159(3) Uani 1 1 d . . . . .
C67 C 0.42023(7) 0.66464(12) 0.47131(6) 0.0230(3) Uani 1 1 d . . . . .
H67A H 0.390402 0.713508 0.458911 0.035 Uiso 1 1 calc R U . . .
H67B H 0.438477 0.679716 0.506437 0.035 Uiso 1 1 calc R U . . .
H67C H 0.402512 0.599630 0.469793 0.035 Uiso 1 1 calc R U . . .
C68 C 0.87186(6) -0.08239(11) 0.63304(6) 0.0185(3) Uani 1 1 d . . . . .
H68A H 0.904781 -0.090498 0.616203 0.028 Uiso 1 1 calc R U . . .
H68B H 0.882246 -0.106799 0.667897 0.028 Uiso 1 1 calc R U . . .
H68C H 0.861725 -0.012971 0.633501 0.028 Uiso 1 1 calc R U . . .
C69 C 0.84002(6) 0.28693(10) 0.55040(5) 0.0171(3) Uani 1 1 d . . . . .
C70 C 0.94808(7) 0.39592(12) 0.40943(6) 0.0234(3) Uani 1 1 d . . . . .
H70A H 0.932917 0.460711 0.415242 0.035 Uiso 1 1 calc R U . . .
H70B H 0.986930 0.388421 0.430220 0.035 Uiso 1 1 calc R U . . .
H70C H 0.922558 0.345510 0.418718 0.035 Uiso 1 1 calc R U . . .
C71 C 0.91237(6) -0.15437(10) 0.44816(5) 0.0141(3) Uani 1 1 d . . . . .
C72 C 0.45265(6) 0.39477(10) 0.38598(5) 0.0156(3) Uani 1 1 d . . . . .
H72 H 0.426461 0.438217 0.397300 0.019 Uiso 1 1 calc R U . . .
C73 C 0.53823(6) 0.58959(11) 0.46358(6) 0.0186(3) Uani 1 1 d . . . . .
H73A H 0.526031 0.521051 0.463064 0.028 Uiso 1 1 calc R U . . .
H73B H 0.550107 0.611511 0.498773 0.028 Uiso 1 1 calc R U . . .
H73C H 0.570821 0.595877 0.446192 0.028 Uiso 1 1 calc R U . . .
C74 C 0.48611(8) 0.05681(11) 0.34542(6) 0.0241(3) Uani 1 1 d . . . . .
H74A H 0.521077 0.071105 0.332255 0.036 Uiso 1 1 calc R U . . .
H74B H 0.451899 0.073582 0.319753 0.036 Uiso 1 1 calc R U . . .
H74C H 0.485160 -0.012917 0.353569 0.036 Uiso 1 1 calc R U . . .
C75 C 0.48642(6) 0.11720(10) 0.39335(6) 0.0161(3) Uani 1 1 d . . . . .
C76 C 0.98330(7) -0.18831(12) 0.39589(6) 0.0219(3) Uani 1 1 d . . . . .
H76 H 1.001290 -0.233255 0.376987 0.026 Uiso 1 1 calc R U . . .
C77 C 0.68126(7) -0.23150(13) 0.50582(7) 0.0276(4) Uani 1 1 d . . . . .
H77A H 0.704286 -0.286314 0.497250 0.041 Uiso 1 1 calc R U . . .
H77B H 0.643565 -0.230783 0.482644 0.041 Uiso 1 1 calc R U . . .
H77C H 0.675647 -0.238905 0.540747 0.041 Uiso 1 1 calc R U . . .
C78 C 0.72451(7) -0.10102(12) 0.43072(6) 0.0241(3) Uani 1 1 d . . . . .
H78A H 0.741276 -0.037409 0.425106 0.036 Uiso 1 1 calc R U . . .
H78B H 0.685600 -0.105975 0.409763 0.036 Uiso 1 1 calc R U . . .
H78C H 0.748882 -0.153277 0.421473 0.036 Uiso 1 1 calc R U . . .
C79 C 0.83967(7) 0.39679(11) 0.56167(6) 0.0204(3) Uani 1 1 d . . . . .
C80 C 0.83829(6) 0.89168(10) 0.27282(6) 0.0168(3) Uani 1 1 d . . . . .
C81 C 0.98986(8) 0.26430(13) 0.33361(7) 0.0305(4) Uani 1 1 d . . . . .
H81A H 0.965160 0.209448 0.339217 0.046 Uiso 1 1 calc R U . . .
H81B H 1.026152 0.261878 0.358677 0.046 Uiso 1 1 calc R U . . .
H81C H 0.998204 0.259861 0.299428 0.046 Uiso 1 1 calc R U . . .
C82 C 0.91830(7) 0.34012(14) 0.20472(6) 0.0274(4) Uani 1 1 d . . . . .
H82A H 0.936266 0.404908 0.206090 0.041 Uiso 1 1 calc R U . . .
H82B H 0.900866 0.324173 0.169499 0.041 Uiso 1 1 calc R U . . .
H82C H 0.947759 0.291221 0.218043 0.041 Uiso 1 1 calc R U . . .
C83 C 0.84036(8) 0.95242(11) 0.32096(6) 0.0265(4) Uani 1 1 d . . . . .
H83A H 0.806707 0.936827 0.335771 0.040 Uiso 1 1 calc R U . . .
H83B H 0.839848 1.022118 0.312454 0.040 Uiso 1 1 calc R U . . .
H83C H 0.875849 0.937193 0.345459 0.040 Uiso 1 1 calc R U . . .
C84 C 0.38145(8) 0.61822(13) 0.26647(6) 0.0300(4) Uani 1 1 d . . . . .
H84A H 0.410417 0.659214 0.255001 0.045 Uiso 1 1 calc R U . . .
H84B H 0.342997 0.633735 0.246676 0.045 Uiso 1 1 calc R U . . .
H84C H 0.390153 0.549192 0.261737 0.045 Uiso 1 1 calc R U . . .
C85 C 0.50502(8) 0.79601(12) 0.43295(6) 0.0269(4) Uani 1 1 d . . . . .
H85A H 0.537342 0.799397 0.415088 0.040 Uiso 1 1 calc R U . . .
H85B H 0.518347 0.815600 0.468373 0.040 Uiso 1 1 calc R U . . .
H85C H 0.474145 0.840128 0.416671 0.040 Uiso 1 1 calc R U . . .
C86 C 0.74971(7) -0.14612(13) 0.63581(6) 0.0241(3) Uani 1 1 d . . . . .
H86A H 0.734028 -0.079600 0.634153 0.036 Uiso 1 1 calc R U . . .
H86B H 0.765736 -0.163062 0.671189 0.036 Uiso 1 1 calc R U . . .
H86C H 0.718786 -0.192145 0.621922 0.036 Uiso 1 1 calc R U . . .
C87 C 0.83223(9) -0.28466(12) 0.60097(6) 0.0296(4) Uani 1 1 d . . . . .
H87A H 0.800366 -0.325761 0.583624 0.044 Uiso 1 1 calc R U . . .
H87B H 0.843224 -0.304808 0.636529 0.044 Uiso 1 1 calc R U . . .
H87C H 0.865473 -0.291917 0.584469 0.044 Uiso 1 1 calc R U . . .
C88 C 0.35505(8) 0.76997(15) 0.34135(7) 0.0369(5) Uani 1 1 d . . . . .
H88A H 0.353783 0.783484 0.376880 0.055 Uiso 1 1 calc R U . . .
H88B H 0.316061 0.775831 0.320622 0.055 Uiso 1 1 calc R U . . .
H88C H 0.380769 0.817020 0.329534 0.055 Uiso 1 1 calc R U . . .
C89 C 0.54020(7) 0.09149(12) 0.43333(7) 0.0274(4) Uani 1 1 d . . . . .
H89A H 0.539487 0.021788 0.441590 0.041 Uiso 1 1 calc R U . . .
H89B H 0.540482 0.130274 0.464000 0.041 Uiso 1 1 calc R U . . .
H89C H 0.575007 0.105983 0.419966 0.041 Uiso 1 1 calc R U . . .
C90 C 0.89196(9) 0.44997(12) 0.54702(7) 0.0337(4) Uani 1 1 d . . . . .
H90A H 0.890101 0.443442 0.510468 0.051 Uiso 1 1 calc R U . . .
H90B H 0.927949 0.420755 0.565475 0.051 Uiso 1 1 calc R U . . .
H90C H 0.890899 0.519360 0.555846 0.051 Uiso 1 1 calc R U . . .
C91 C 0.84257(8) 0.41467(12) 0.61814(6) 0.0265(3) Uani 1 1 d . . . . .
H91A H 0.843683 0.485147 0.624786 0.040 Uiso 1 1 calc R U . . .
H91B H 0.877510 0.384039 0.637714 0.040 Uiso 1 1 calc R U . . .
H91C H 0.808386 0.386279 0.628161 0.040 Uiso 1 1 calc R U . . .
C92 C 1.00151(7) 0.48226(14) 0.32684(7) 0.0286(4) Uani 1 1 d . . . . .
H92A H 1.002313 0.482745 0.290573 0.043 Uiso 1 1 calc R U . . .
H92B H 1.040576 0.470308 0.346366 0.043 Uiso 1 1 calc R U . . .
H92C H 0.987613 0.545584 0.336560 0.043 Uiso 1 1 calc R U . . .
C93 C 0.43257(7) 0.08883(12) 0.41406(7) 0.0265(4) Uani 1 1 d . . . . .
H93A H 0.432699 0.018157 0.420052 0.040 Uiso 1 1 calc R U . . .
H93B H 0.397755 0.106763 0.389366 0.040 Uiso 1 1 calc R U . . .
H93C H 0.432883 0.123450 0.445999 0.040 Uiso 1 1 calc R U . . .
C94 C 0.89060(8) 0.92041(12) 0.24997(7) 0.0276(4) Uani 1 1 d . . . . .
H94A H 0.889886 0.991018 0.243711 0.041 Uiso 1 1 calc R U . . .
H94B H 0.888991 0.885456 0.217936 0.041 Uiso 1 1 calc R U . . .
H94C H 0.926324 0.903108 0.273683 0.041 Uiso 1 1 calc R U . . .
C95 C 0.67145(7) -0.01217(13) 0.51295(7) 0.0272(4) Uani 1 1 d . . . . .
H95A H 0.670346 -0.011463 0.549161 0.041 Uiso 1 1 calc R U . . .
H95B H 0.632355 -0.022860 0.493194 0.041 Uiso 1 1 calc R U . . .
H95C H 0.686194 0.050610 0.503385 0.041 Uiso 1 1 calc R U . . .
C96 C 0.78468(9) 0.44169(13) 0.53099(7) 0.0388(5) Uani 1 1 d . . . . .
H96A H 0.750921 0.409313 0.539732 0.058 Uiso 1 1 calc R U . . .
H96B H 0.784114 0.433081 0.494741 0.058 Uiso 1 1 calc R U . . .
H96C H 0.783606 0.511586 0.538739 0.058 Uiso 1 1 calc R U . . .
C97 C 0.78318(8) 0.91590(13) 0.23433(7) 0.0318(4) Uani 1 1 d . . . . .
H97A H 0.749332 0.900692 0.248940 0.048 Uiso 1 1 calc R U . . .
H97B H 0.781943 0.876960 0.203565 0.048 Uiso 1 1 calc R U . . .
H97C H 0.782963 0.985574 0.225816 0.048 Uiso 1 1 calc R U . . .
C98 C 0.83358(10) 0.21085(12) 0.24431(7) 0.0385(5) Uani 1 1 d . . . . .
H98A H 0.864804 0.168501 0.261671 0.058 Uiso 1 1 calc R U . . .
H98B H 0.820696 0.188371 0.209312 0.058 Uiso 1 1 calc R U . . .
H98C H 0.801117 0.208328 0.262037 0.058 Uiso 1 1 calc R U . . .
C99 C 0.32697(8) 0.56003(18) 0.35436(8) 0.0447(5) Uani 1 1 d . . . . .
H99A H 0.334052 0.492441 0.345170 0.067 Uiso 1 1 calc R U . . .
H99B H 0.288427 0.580386 0.336622 0.067 Uiso 1 1 calc R U . . .
H99C H 0.329227 0.564366 0.391047 0.067 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
Ni3 N3 1.8517(11) . ?
Ni3 N1 1.8932(11) . ?
Ni3 C39 1.9075(14) . ?
Ni3 N4 2.0547(12) . ?
Ni1 N9 1.8511(11) . ?
Ni1 N2 1.8963(11) . ?
Ni1 C25 1.9068(14) . ?
Ni1 N8 2.0628(12) . ?
Ni2 N6 1.8515(11) . ?
Ni2 N5 1.8946(11) . ?
Ni2 C27 1.9038(14) . ?
Ni2 N7 2.0531(11) . ?
Si1 N2 1.7066(12) . ?
Si1 C73 1.8734(15) . ?
Si1 C67 1.8839(15) . ?
Si1 C85 1.8894(16) . ?
Si6 N1 1.7054(12) . ?
Si6 C68 1.8733(15) . ?
Si6 C86 1.8832(15) . ?
Si6 C87 1.8839(16) . ?
Si5 N1 1.7022(12) . ?
Si5 C95 1.8787(17) . ?
Si5 C77 1.8822(16) . ?
Si5 C78 1.8876(16) . ?
Si3 N5 1.6985(12) . ?
Si3 C81 1.8793(17) . ?
Si3 C92 1.8823(17) . ?
Si3 C70 1.8865(16) . ?
Si4 N5 1.7082(13) . ?
Si4 C58 1.8721(16) . ?
Si4 C98 1.8821(17) . ?
Si4 C82 1.8825(16) . ?
Si2 N2 1.6990(12) . ?
Si2 C99 1.8786(19) . ?
Si2 C84 1.8837(18) . ?
Si2 C88 1.8838(19) . ?
N9 C24 1.3399(18) . ?
N9 C65 1.3494(17) . ?
N6 C31 1.3393(17) . ?
N6 C52 1.3497(17) . ?
N3 C28 1.3393(18) . ?
N3 C43 1.3479(17) . ?
N7 C54 1.3263(18) . ?
N7 C61 1.3692(17) . ?
N8 C48 1.3269(18) . ?
N8 C64 1.3681(17) . ?
N4 C50 1.3288(18) . ?
N4 C71 1.3682(17) . ?
C14 C22 1.3986(19) . ?
C14 C39 1.4216(19) . ?
C14 C28 1.4550(19) . ?
C15 C18 1.3915(19) . ?
C15 C63 1.3992(19) . ?
C15 H15 0.9500 . ?
C17 C30 1.380(2) . ?
C17 C53 1.412(2) . ?
C17 H17 0.9500 . ?
C18 C27 1.4230(18) . ?
C18 C31 1.4600(18) . ?
C19 C33 1.3826(19) . ?
C19 C31 1.4122(18) . ?
C19 H19 0.9500 . ?
C20 C38 1.381(2) . ?
C20 C24 1.4121(18) . ?
C20 H20 0.9500 . ?
C21 C29 1.3909(19) . ?
C21 C25 1.4226(18) . ?
C21 C24 1.4606(18) . ?
C22 C69 1.393(2) . ?
C22 H22 0.9500 . ?
C25 C72 1.3922(18) . ?
C26 C42 1.380(2) . ?
C26 C66 1.409(2) . ?
C26 H26 0.9500 . ?
C27 C44 1.3931(18) . ?
C28 C37 1.4141(19) . ?
C29 C46 1.3973(19) . ?
C29 H29 0.9500 . ?
C30 C54 1.4038(19) . ?
C30 H30 0.9500 . ?
C32 C52 1.3995(18) . ?
C32 C33 1.418(2) . ?
C32 C35 1.4364(19) . ?
C33 H33 0.9500 . ?
C34 C56 1.377(2) . ?
C34 C57 1.412(2) . ?
C34 H34 0.9500 . ?
C35 C41 1.363(2) . ?
C35 H35 0.9500 . ?
C36 C45 1.362(2) . ?
C36 C49 1.4385(19) . ?
C36 H36 0.9500 . ?
C37 C55 1.382(2) . ?
C37 H37 0.9500 . ?
C38 C49 1.415(2) . ?
C38 H38 0.9500 . ?
C39 C60 1.3973(19) . ?
C40 C76 1.362(2) . ?
C40 C51 1.439(2) . ?
C40 H40 0.9500 . ?
C41 C53 1.4398(19) . ?
C41 H41 0.9500 . ?
C42 C48 1.408(2) . ?
C42 H42 0.9500 . ?
C43 C51 1.3988(19) . ?
C43 C71 1.417(2) . ?
C44 C47 1.4014(19) . ?
C44 H44 0.9500 . ?
C45 C66 1.438(2) . ?
C45 H45 0.9500 . ?
C46 C62 1.3995(19) . ?
C46 C75 1.5325(19) . ?
C47 C63 1.400(2) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C65 1.4021(18) . ?
C50 C56 1.408(2) . ?
C50 H50 0.9500 . ?
C51 C55 1.412(2) . ?
C52 C61 1.4188(19) . ?
C53 C61 1.4011(18) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C71 1.4021(19) . ?
C57 C76 1.439(2) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.400(2) . ?
C59 C69 1.406(2) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C62 C72 1.404(2) . ?
C62 H62 0.9500 . ?
C63 C80 1.5337(19) . ?
C64 C66 1.4048(19) . ?
C64 C65 1.4145(19) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 C79 1.534(2) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C72 H72 0.9500 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C75 1.531(2) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C89 1.533(2) . ?
C75 C93 1.535(2) . ?
C76 H76 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 C96 1.523(2) . ?
C79 C91 1.527(2) . ?
C79 C90 1.549(2) . ?
C80 C97 1.530(2) . ?
C80 C83 1.532(2) . ?
C80 C94 1.535(2) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?
C98 H98A 0.9800 . ?
C98 H98B 0.9800 . ?
C98 H98C 0.9800 . ?
C99 H99A 0.9800 . ?
C99 H99B 0.9800 . ?
C99 H99C 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 Ni3 N1 177.98(5) . . ?
N3 Ni3 C39 82.53(5) . . ?
N1 Ni3 C39 99.49(5) . . ?
N3 Ni3 N4 81.43(5) . . ?
N1 Ni3 N4 96.55(5) . . ?
C39 Ni3 N4 163.94(5) . . ?
N9 Ni1 N2 176.72(5) . . ?
N9 Ni1 C25 82.64(5) . . ?
N2 Ni1 C25 98.80(5) . . ?
N9 Ni1 N8 81.33(5) . . ?
N2 Ni1 N8 97.30(5) . . ?
C25 Ni1 N8 163.87(5) . . ?
N6 Ni2 N5 178.16(5) . . ?
N6 Ni2 C27 82.62(5) . . ?
N5 Ni2 C27 98.71(5) . . ?
N6 Ni2 N7 81.62(5) . . ?
N5 Ni2 N7 97.06(5) . . ?
C27 Ni2 N7 164.22(5) . . ?
N2 Si1 C73 111.78(6) . . ?
N2 Si1 C67 113.35(7) . . ?
C73 Si1 C67 106.64(7) . . ?
N2 Si1 C85 112.42(7) . . ?
C73 Si1 C85 105.84(8) . . ?
C67 Si1 C85 106.30(8) . . ?
N1 Si6 C68 111.38(6) . . ?
N1 Si6 C86 113.46(7) . . ?
C68 Si6 C86 107.34(7) . . ?
N1 Si6 C87 113.08(7) . . ?
C68 Si6 C87 105.59(8) . . ?
C86 Si6 C87 105.45(8) . . ?
N1 Si5 C95 114.19(7) . . ?
N1 Si5 C77 112.17(7) . . ?
C95 Si5 C77 106.75(8) . . ?
N1 Si5 C78 110.77(7) . . ?
C95 Si5 C78 105.94(8) . . ?
C77 Si5 C78 106.55(8) . . ?
N5 Si3 C81 112.06(7) . . ?
N5 Si3 C92 115.11(7) . . ?
C81 Si3 C92 105.95(8) . . ?
N5 Si3 C70 110.33(7) . . ?
C81 Si3 C70 107.09(8) . . ?
C92 Si3 C70 105.79(8) . . ?
N5 Si4 C58 111.51(6) . . ?
N5 Si4 C98 112.52(7) . . ?
C58 Si4 C98 105.14(9) . . ?
N5 Si4 C82 113.32(7) . . ?
C58 Si4 C82 107.30(7) . . ?
C98 Si4 C82 106.54(9) . . ?
N2 Si2 C99 115.04(8) . . ?
N2 Si2 C84 110.32(7) . . ?
C99 Si2 C84 106.48(9) . . ?
N2 Si2 C88 111.91(8) . . ?
C99 Si2 C88 104.92(10) . . ?
C84 Si2 C88 107.72(8) . . ?
C24 N9 C65 120.64(12) . . ?
C24 N9 Ni1 120.64(9) . . ?
C65 N9 Ni1 118.67(9) . . ?
C31 N6 C52 120.78(12) . . ?
C31 N6 Ni2 120.70(9) . . ?
C52 N6 Ni2 118.45(9) . . ?
C28 N3 C43 120.70(12) . . ?
C28 N3 Ni3 120.66(9) . . ?
C43 N3 Ni3 118.63(10) . . ?
C54 N7 C61 116.74(12) . . ?
C54 N7 Ni2 132.87(10) . . ?
C61 N7 Ni2 110.39(9) . . ?
C48 N8 C64 116.97(12) . . ?
C48 N8 Ni1 132.72(10) . . ?
C64 N8 Ni1 110.32(9) . . ?
C50 N4 C71 116.87(12) . . ?
C50 N4 Ni3 132.61(10) . . ?
C71 N4 Ni3 110.51(9) . . ?
Si5 N1 Si6 128.29(7) . . ?
Si5 N1 Ni3 114.43(6) . . ?
Si6 N1 Ni3 117.26(6) . . ?
C22 C14 C39 123.01(13) . . ?
C22 C14 C28 123.65(13) . . ?
C39 C14 C28 113.33(12) . . ?
C18 C15 C63 120.68(13) . . ?
C18 C15 H15 119.7 . . ?
C63 C15 H15 119.7 . . ?
Si2 N2 Si1 126.75(7) . . ?
Si2 N2 Ni1 117.86(7) . . ?
Si1 N2 Ni1 115.39(6) . . ?
C30 C17 C53 118.98(13) . . ?
C30 C17 H17 120.5 . . ?
C53 C17 H17 120.5 . . ?
C15 C18 C27 122.71(12) . . ?
C15 C18 C31 124.13(12) . . ?
C27 C18 C31 113.16(12) . . ?
C33 C19 C31 120.25(13) . . ?
C33 C19 H19 119.9 . . ?
C31 C19 H19 119.9 . . ?
C38 C20 C24 120.17(13) . . ?
C38 C20 H20 119.9 . . ?
C24 C20 H20 119.9 . . ?
C29 C21 C25 122.61(12) . . ?
C29 C21 C24 124.20(12) . . ?
C25 C21 C24 113.17(12) . . ?
C69 C22 C14 120.73(13) . . ?
C69 C22 H22 119.6 . . ?
C14 C22 H22 119.6 . . ?
Si3 N5 Si4 128.87(7) . . ?
Si3 N5 Ni2 115.95(7) . . ?
Si4 N5 Ni2 115.17(6) . . ?
N9 C24 C20 119.62(12) . . ?
N9 C24 C21 110.09(12) . . ?
C20 C24 C21 130.29(13) . . ?
C72 C25 C21 115.88(12) . . ?
C72 C25 Ni1 130.74(11) . . ?
C21 C25 Ni1 113.37(10) . . ?
C42 C26 C66 118.98(13) . . ?
C42 C26 H26 120.5 . . ?
C66 C26 H26 120.5 . . ?
C44 C27 C18 115.88(12) . . ?
C44 C27 Ni2 130.66(10) . . ?
C18 C27 Ni2 113.45(10) . . ?
N3 C28 C37 119.45(13) . . ?
N3 C28 C14 110.14(12) . . ?
C37 C28 C14 130.41(13) . . ?
C21 C29 C46 120.97(13) . . ?
C21 C29 H29 119.5 . . ?
C46 C29 H29 119.5 . . ?
C17 C30 C54 120.28(13) . . ?
C17 C30 H30 119.9 . . ?
C54 C30 H30 119.9 . . ?
N6 C31 C19 119.43(12) . . ?
N6 C31 C18 110.03(11) . . ?
C19 C31 C18 130.54(13) . . ?
C52 C32 C33 115.91(12) . . ?
C52 C32 C35 117.24(13) . . ?
C33 C32 C35 126.85(13) . . ?
C19 C33 C32 120.17(13) . . ?
C19 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C56 C34 C57 119.03(14) . . ?
C56 C34 H34 120.5 . . ?
C57 C34 H34 120.5 . . ?
C41 C35 C32 121.14(13) . . ?
C41 C35 H35 119.4 . . ?
C32 C35 H35 119.4 . . ?
C45 C36 C49 121.14(13) . . ?
C45 C36 H36 119.4 . . ?
C49 C36 H36 119.4 . . ?
C55 C37 C28 120.09(14) . . ?
C55 C37 H37 120.0 . . ?
C28 C37 H37 120.0 . . ?
C20 C38 C49 120.20(13) . . ?
C20 C38 H38 119.9 . . ?
C49 C38 H38 119.9 . . ?
C60 C39 C14 115.49(13) . . ?
C60 C39 Ni3 131.19(11) . . ?
C14 C39 Ni3 113.32(10) . . ?
C76 C40 C51 121.16(14) . . ?
C76 C40 H40 119.4 . . ?
C51 C40 H40 119.4 . . ?
C35 C41 C53 121.59(13) . . ?
C35 C41 H41 119.2 . . ?
C53 C41 H41 119.2 . . ?
C26 C42 C48 120.32(14) . . ?
C26 C42 H42 119.8 . . ?
C48 C42 H42 119.8 . . ?
N3 C43 C51 123.45(13) . . ?
N3 C43 C71 114.38(12) . . ?
C51 C43 C71 122.17(13) . . ?
C27 C44 C47 121.41(13) . . ?
C27 C44 H44 119.3 . . ?
C47 C44 H44 119.3 . . ?
C36 C45 C66 121.73(13) . . ?
C36 C45 H45 119.1 . . ?
C66 C45 H45 119.1 . . ?
C29 C46 C62 116.83(13) . . ?
C29 C46 C75 119.94(12) . . ?
C62 C46 C75 123.20(13) . . ?
C63 C47 C44 122.25(13) . . ?
C63 C47 H47 118.9 . . ?
C44 C47 H47 118.9 . . ?
N8 C48 C42 122.42(13) . . ?
N8 C48 H48 118.8 . . ?
C42 C48 H48 118.8 . . ?
C65 C49 C38 116.04(13) . . ?
C65 C49 C36 117.11(13) . . ?
C38 C49 C36 126.85(13) . . ?
N4 C50 C56 122.35(14) . . ?
N4 C50 H50 118.8 . . ?
C56 C50 H50 118.8 . . ?
C43 C51 C55 116.04(13) . . ?
C43 C51 C40 117.17(14) . . ?
C55 C51 C40 126.79(14) . . ?
N6 C52 C32 123.46(13) . . ?
N6 C52 C61 114.34(12) . . ?
C32 C52 C61 122.21(12) . . ?
C61 C53 C17 116.23(13) . . ?
C61 C53 C41 118.06(13) . . ?
C17 C53 C41 125.71(13) . . ?
N7 C54 C30 122.65(13) . . ?
N7 C54 H54 118.7 . . ?
C30 C54 H54 118.7 . . ?
C37 C55 C51 120.26(13) . . ?
C37 C55 H55 119.9 . . ?
C51 C55 H55 119.9 . . ?
C34 C56 C50 120.42(14) . . ?
C34 C56 H56 119.8 . . ?
C50 C56 H56 119.8 . . ?
C71 C57 C34 116.28(14) . . ?
C71 C57 C76 118.00(14) . . ?
C34 C57 C76 125.73(14) . . ?
Si4 C58 H58A 109.5 . . ?
Si4 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
Si4 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C60 C59 C69 122.44(14) . . ?
C60 C59 H59 118.8 . . ?
C69 C59 H59 118.8 . . ?
C39 C60 C59 121.50(13) . . ?
C39 C60 H60 119.3 . . ?
C59 C60 H60 119.3 . . ?
N7 C61 C53 125.11(13) . . ?
N7 C61 C52 115.13(12) . . ?
C53 C61 C52 119.76(12) . . ?
C46 C62 C72 122.30(13) . . ?
C46 C62 H62 118.8 . . ?
C72 C62 H62 118.8 . . ?
C15 C63 C47 117.04(13) . . ?
C15 C63 C80 119.88(13) . . ?
C47 C63 C80 123.07(13) . . ?
N8 C64 C66 124.91(13) . . ?
N8 C64 C65 115.18(12) . . ?
C66 C64 C65 119.90(13) . . ?
N9 C65 C49 123.32(13) . . ?
N9 C65 C64 114.46(12) . . ?
C49 C65 C64 122.22(13) . . ?
C64 C66 C26 116.40(13) . . ?
C64 C66 C45 117.88(13) . . ?
C26 C66 C45 125.72(13) . . ?
Si1 C67 H67A 109.5 . . ?
Si1 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
Si1 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
Si6 C68 H68A 109.5 . . ?
Si6 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
Si6 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C22 C69 C59 116.82(13) . . ?
C22 C69 C79 121.94(13) . . ?
C59 C69 C79 121.23(13) . . ?
Si3 C70 H70A 109.5 . . ?
Si3 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
Si3 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
N4 C71 C57 125.06(13) . . ?
N4 C71 C43 115.05(12) . . ?
C57 C71 C43 119.89(13) . . ?
C25 C72 C62 121.37(13) . . ?
C25 C72 H72 119.3 . . ?
C62 C72 H72 119.3 . . ?
Si1 C73 H73A 109.5 . . ?
Si1 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
Si1 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C75 C74 H74A 109.5 . . ?
C75 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C75 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C74 C75 C46 110.29(12) . . ?
C74 C75 C89 109.43(13) . . ?
C46 C75 C89 108.91(12) . . ?
C74 C75 C93 107.67(13) . . ?
C46 C75 C93 112.03(12) . . ?
C89 C75 C93 108.46(13) . . ?
C40 C76 C57 121.60(14) . . ?
C40 C76 H76 119.2 . . ?
C57 C76 H76 119.2 . . ?
Si5 C77 H77A 109.5 . . ?
Si5 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
Si5 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
Si5 C78 H78A 109.5 . . ?
Si5 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
Si5 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C96 C79 C91 109.90(14) . . ?
C96 C79 C69 108.99(13) . . ?
C91 C79 C69 110.66(13) . . ?
C96 C79 C90 107.98(15) . . ?
C91 C79 C90 107.29(13) . . ?
C69 C79 C90 111.97(13) . . ?
C97 C80 C83 109.60(14) . . ?
C97 C80 C63 108.98(12) . . ?
C83 C80 C63 109.95(12) . . ?
C97 C80 C94 108.44(13) . . ?
C83 C80 C94 107.85(13) . . ?
C63 C80 C94 111.98(12) . . ?
Si3 C81 H81A 109.5 . . ?
Si3 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
Si3 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
Si4 C82 H82A 109.5 . . ?
Si4 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
Si4 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C80 C83 H83A 109.5 . . ?
C80 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C80 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
Si2 C84 H84A 109.5 . . ?
Si2 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
Si2 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
Si1 C85 H85A 109.5 . . ?
Si1 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
Si1 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
Si6 C86 H86A 109.5 . . ?
Si6 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
Si6 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
Si6 C87 H87A 109.5 . . ?
Si6 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
Si6 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
Si2 C88 H88A 109.5 . . ?
Si2 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
Si2 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C75 C89 H89A 109.5 . . ?
C75 C89 H89B 109.5 . . ?
H89A C89 H89B 109.5 . . ?
C75 C89 H89C 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C79 C90 H90A 109.5 . . ?
C79 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
C79 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C79 C91 H91A 109.5 . . ?
C79 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C79 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
Si3 C92 H92A 109.5 . . ?
Si3 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
Si3 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C75 C93 H93A 109.5 . . ?
C75 C93 H93B 109.5 . . ?
H93A C93 H93B 109.5 . . ?
C75 C93 H93C 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C80 C94 H94A 109.5 . . ?
C80 C94 H94B 109.5 . . ?
H94A C94 H94B 109.5 . . ?
C80 C94 H94C 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
Si5 C95 H95A 109.5 . . ?
Si5 C95 H95B 109.5 . . ?
H95A C95 H95B 109.5 . . ?
Si5 C95 H95C 109.5 . . ?
H95A C95 H95C 109.5 . . ?
H95B C95 H95C 109.5 . . ?
C79 C96 H96A 109.5 . . ?
C79 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C79 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
C80 C97 H97A 109.5 . . ?
C80 C97 H97B 109.5 . . ?
H97A C97 H97B 109.5 . . ?
C80 C97 H97C 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
Si4 C98 H98A 109.5 . . ?
Si4 C98 H98B 109.5 . . ?
H98A C98 H98B 109.5 . . ?
Si4 C98 H98C 109.5 . . ?
H98A C98 H98C 109.5 . . ?
H98B C98 H98C 109.5 . . ?
Si2 C99 H99A 109.5 . . ?
Si2 C99 H99B 109.5 . . ?
H99A C99 H99B 109.5 . . ?
Si2 C99 H99C 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 109.5 . . ?

_refine_diff_density_max         0.729
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.068


_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1979880'
loop_
_audit_author_name
_audit_author_address
'Dr Hartmut Schubert'
;Eberhard Karls Universitaet Tuebingen
Germany
;
_audit_update_record             
;
2020-01-24 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H70 F6 N4 Ni2 O11 S2'
_chemical_formula_weight         1342.72

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8801(10)
_cell_length_b                   14.0913(11)
_cell_length_c                   17.4958(13)
_cell_angle_alpha                81.586(2)
_cell_angle_beta                 77.019(3)
_cell_angle_gamma                84.657(3)
_cell_volume                     3055.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9273
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      29.59

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.537
_exptl_crystal_size_mid          0.408
_exptl_crystal_size_min          0.330
_exptl_absorpt_coefficient_mu    0.766
_shelx_estimated_absorpt_T_min   0.684
_shelx_estimated_absorpt_T_max   0.786
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.9507
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56171
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.631
_diffrn_reflns_theta_max         29.597
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             17069
_reflns_number_gt                14723
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0563P)²+4.9510P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17069
_refine_ls_number_parameters     824
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1235
_refine_ls_wR_factor_gt          0.1162
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.65251(2) 0.13900(2) 0.75072(2) 0.01206(6) Uani 1 1 d . . . A 1
Ni1 Ni 0.67768(2) 0.24388(2) 0.58238(2) 0.01306(6) Uani 1 1 d . . . B 1
S1 S 0.83853(4) 0.05623(4) 0.61320(3) 0.01380(14) Uani 0.8075(19) 1 d . . P A 1
S2 S 0.25744(7) 0.63858(5) 0.80925(5) 0.0486(2) Uani 1 1 d . . . . .
O1 O 0.72475(10) 0.26061(9) 0.67915(8) 0.0134(2) Uani 1 1 d . . . . .
O8 O 0.79668(11) 0.33262(11) 0.50529(8) 0.0182(3) Uani 1 1 d . . . . .
O9 O 0.57856(12) 0.01378(10) 0.80998(8) 0.0201(3) Uani 1 1 d . . . . .
O2 O 0.57227(10) 0.15178(9) 0.66447(8) 0.0138(2) Uani 1 1 d . . . . .
O4 O 0.77265(12) 0.04761(10) 0.69572(8) 0.0206(3) Uani 1 1 d . . . . .
O3 O 0.79202(14) 0.13263(11) 0.55877(9) 0.0267(3) Uani 1 1 d . . . . .
N1 N 0.54228(12) 0.22675(11) 0.81304(9) 0.0123(3) Uani 1 1 d . . . . .
N2 N 0.72668(12) 0.14355(11) 0.84235(9) 0.0139(3) Uani 1 1 d . . . . .
N4 N 0.56976(12) 0.35781(11) 0.59502(9) 0.0130(3) Uani 1 1 d . . . . .
O7 O 0.03281(17) 0.95944(14) 0.82031(12) 0.0407(5) Uani 1 1 d . . . . .
N3 N 0.60482(14) 0.22822(12) 0.49281(9) 0.0168(3) Uani 1 1 d . . . . .
O5 O 0.34361(18) 0.58062(14) 0.83523(13) 0.0420(5) Uani 1 1 d . . . . .
O6 O 0.2195(2) 0.72046(15) 0.84995(13) 0.0509(6) Uani 1 1 d . . . . .
F2 F 0.8411(3) -0.0586(2) 0.50532(17) 0.0587(8) Uani 0.8075(19) 1 d . . P A 1
C1 C 0.49737(15) 0.35879(13) 0.54901(10) 0.0140(3) Uani 1 1 d . . . . .
C2 C 0.57894(14) 0.25691(13) 0.87201(10) 0.0128(3) Uani 1 1 d . . . . .
C3 C 0.39846(15) 0.34646(14) 0.83239(11) 0.0157(3) Uani 1 1 d . . . . .
H3 H 0.336981 0.378356 0.816501 0.019 Uiso 1 1 calc R U . . .
C4 C 0.46148(15) 0.48239(14) 0.65921(11) 0.0163(3) Uani 1 1 d . . . . .
H4 H 0.449213 0.523883 0.698947 0.020 Uiso 1 1 calc R U . . .
C5 C 0.45161(14) 0.26721(13) 0.79429(10) 0.0131(3) Uani 1 1 d . . . . .
C6 C 0.51667(16) 0.28943(14) 0.49354(11) 0.0160(3) Uani 1 1 d . . . . .
C7 C 0.40674(15) 0.22740(13) 0.73575(10) 0.0136(3) Uani 1 1 d . . . . .
C8 C 0.67635(15) 0.20984(13) 0.88975(10) 0.0137(3) Uani 1 1 d . . . . .
C9 C 0.38898(16) 0.48389(14) 0.61247(12) 0.0178(4) Uani 1 1 d . . . . .
H9 H 0.327261 0.526909 0.619428 0.021 Uiso 1 1 calc R U . . .
C10 C 0.86002(16) 0.11514(15) 0.92082(12) 0.0201(4) Uani 1 1 d . . . . .
H10 H 0.923191 0.079974 0.930895 0.024 Uiso 1 1 calc R U . . .
C11 C 0.71660(14) 0.34562(13) 0.70592(10) 0.0130(3) Uani 1 1 d . . . . .
C12 C 0.71567(15) 0.23373(14) 0.95273(11) 0.0159(3) Uani 1 1 d . . . . .
C13 C 0.81661(15) 0.09793(14) 0.85759(12) 0.0172(3) Uani 1 1 d . . . . .
H13 H 0.852750 0.052042 0.824494 0.021 Uiso 1 1 calc R U . . .
C14 C 0.81046(16) 0.18314(15) 0.96791(12) 0.0200(4) Uani 1 1 d . . . . .
H14 H 0.839635 0.196072 1.010315 0.024 Uiso 1 1 calc R U . . .
C15 C 0.55526(14) 0.41912(13) 0.64881(10) 0.0128(3) Uani 1 1 d . . . . .
C16 C 0.52659(15) 0.33010(13) 0.91562(11) 0.0148(3) Uani 1 1 d . . . . .
C17 C 0.33438(16) 0.41812(15) 0.50224(12) 0.0203(4) Uani 1 1 d . . . . .
H17 H 0.273904 0.462489 0.504158 0.024 Uiso 1 1 calc R U . . .
C18 C 0.40584(15) 0.42155(14) 0.55393(11) 0.0162(3) Uani 1 1 d . . . . .
C19 C 0.29650(15) 0.24592(14) 0.73924(11) 0.0162(3) Uani 1 1 d . . . . .
H19 H 0.257275 0.283953 0.777912 0.019 Uiso 1 1 calc R U . . .
C20 C 0.43522(16) 0.37712(14) 0.89179(11) 0.0165(3) Uani 1 1 d . . . . .
H20 H 0.399199 0.429980 0.916870 0.020 Uiso 1 1 calc R U . . .
C21 C 0.63796(15) 0.50448(13) 0.73224(11) 0.0143(3) Uani 1 1 d . . . . .
H21 H 0.584339 0.554447 0.726535 0.017 Uiso 1 1 calc R U . . .
F3 F 0.8016(3) -0.13005(16) 0.62492(16) 0.0694(9) Uani 0.8075(19) 1 d . . P A 1
F1 F 0.6846(2) -0.03590(19) 0.57745(14) 0.0577(7) Uani 0.8075(19) 1 d . . P A 1
C24 C 0.24113(16) 0.21232(14) 0.68992(12) 0.0178(4) Uani 1 1 d . . . . .
C25 C 0.79103(16) 0.44351(14) 0.78274(12) 0.0180(4) Uani 1 1 d . . . . .
H25 H 0.844363 0.450545 0.810857 0.022 Uiso 1 1 calc R U . . .
C26 C 0.71181(15) 0.51726(14) 0.77595(11) 0.0157(3) Uani 1 1 d . . . . .
C27 C 0.79255(15) 0.36040(14) 0.74894(11) 0.0166(3) Uani 1 1 d . . . . .
H27 H 0.847014 0.311367 0.755016 0.020 Uiso 1 1 calc R U . . .
C28 C 0.56928(16) 0.35383(14) 0.97895(11) 0.0176(4) Uani 1 1 d . . . . .
H28 H 0.533799 0.403235 1.008595 0.021 Uiso 1 1 calc R U . . .
O11 O 0.2852(2) 0.0886(2) 0.99593(17) 0.0668(7) Uani 1 1 d . . . . .
C30 C 0.46635(15) 0.17058(13) 0.67769(11) 0.0142(3) Uani 1 1 d . . . . .
C31 C 0.35241(17) 0.35186(16) 0.45044(12) 0.0220(4) Uani 1 1 d . . . . .
H31 H 0.303650 0.350008 0.417296 0.026 Uiso 1 1 calc R U . . .
C32 C 0.65928(17) 0.30725(15) 0.99746(11) 0.0188(4) Uani 1 1 d . . . . .
H32 H 0.685048 0.323499 1.040362 0.023 Uiso 1 1 calc R U . . .
C33 C 0.44368(17) 0.28513(15) 0.44529(11) 0.0197(4) Uani 1 1 d . . . . .
C34 C 0.62279(18) 0.16068(15) 0.44513(12) 0.0220(4) Uani 1 1 d . . . . .
H34 H 0.684429 0.117905 0.444471 0.026 Uiso 1 1 calc R U . . .
C35 C 0.63773(14) 0.42123(13) 0.69553(10) 0.0132(3) Uani 1 1 d . . . . .
C36 C 0.12119(16) 0.24029(15) 0.69752(12) 0.0201(4) Uani 1 1 d . . . . .
C37 C 0.30086(16) 0.15521(15) 0.63446(12) 0.0192(4) Uani 1 1 d . . . . .
H37 H 0.266436 0.129988 0.599848 0.023 Uiso 1 1 calc R U . . .
C38 C 0.40959(16) 0.13481(14) 0.62920(11) 0.0170(3) Uani 1 1 d . . . . .
H38 H 0.447248 0.095057 0.591291 0.020 Uiso 1 1 calc R U . . .
C39 C 0.70914(17) 0.60797(14) 0.81571(12) 0.0188(4) Uani 1 1 d . . . . .
C40 C 0.83903(18) 0.30582(18) 0.42675(12) 0.0250(4) Uani 1 1 d . . . . .
H40A H 0.784821 0.319538 0.393806 0.030 Uiso 1 1 calc R U . . .
H40B H 0.862006 0.236603 0.429553 0.030 Uiso 1 1 calc R U . . .
C41 C 0.10736(18) 0.34474(17) 0.65968(16) 0.0290(5) Uani 1 1 d . . . . .
H41A H 0.142539 0.386584 0.684767 0.043 Uiso 1 1 calc R U . . .
H41B H 0.031153 0.364508 0.667099 0.043 Uiso 1 1 calc R U . . .
H41C H 0.139575 0.349837 0.603001 0.043 Uiso 1 1 calc R U . . .
C42 C 0.55364(19) 0.15031(17) 0.39554(12) 0.0254(4) Uani 1 1 d . . . . .
H42 H 0.568376 0.100992 0.362254 0.030 Uiso 1 1 calc R U . . .
C43 C 0.5482(2) -0.05671(15) 0.76778(13) 0.0252(4) Uani 1 1 d . . . . .
H43A H 0.601713 -0.111918 0.763462 0.030 Uiso 1 1 calc R U . . .
H43B H 0.541119 -0.027811 0.713961 0.030 Uiso 1 1 calc R U . . .
C44 C 0.46486(19) 0.21187(17) 0.39560(12) 0.0246(4) Uani 1 1 d . . . . .
H44 H 0.417602 0.205372 0.362345 0.029 Uiso 1 1 calc R U . . .
C45 C 0.88655(18) 0.3554(2) 0.53537(13) 0.0296(5) Uani 1 1 d . . . . .
H45A H 0.906329 0.301427 0.573491 0.036 Uiso 1 1 calc R U . . .
H45B H 0.868363 0.413673 0.562385 0.036 Uiso 1 1 calc R U . . .
O10 O 0.2689(3) 0.6558(3) 0.72469(17) 0.1032(15) Uani 1 1 d . . . . .
C47 C 0.1473(2) 0.9497(2) 0.8015(2) 0.0437(7) Uani 1 1 d . . . . .
H47A H 0.174217 0.905268 0.843012 0.052 Uiso 1 1 calc R U . . .
H47B H 0.177457 1.012900 0.797086 0.052 Uiso 1 1 calc R U . . .
C48 C 0.6050(2) 0.67005(16) 0.81536(14) 0.0271(5) Uani 1 1 d . . . . .
H48A H 0.544138 0.630836 0.839160 0.041 Uiso 1 1 calc R U . . .
H48B H 0.601347 0.695579 0.760775 0.041 Uiso 1 1 calc R U . . .
H48C H 0.603002 0.723429 0.845930 0.041 Uiso 1 1 calc R U . . .
C49 C 0.71794(19) 0.57862(16) 0.90227(12) 0.0244(4) Uani 1 1 d . . . . .
H49A H 0.661520 0.535649 0.929078 0.037 Uiso 1 1 calc R U . . .
H49B H 0.710086 0.636160 0.928978 0.037 Uiso 1 1 calc R U . . .
H49C H 0.787830 0.545327 0.903950 0.037 Uiso 1 1 calc R U . . .
C50 C 0.8036(2) 0.66764(18) 0.77188(15) 0.0332(5) Uani 1 1 d . . . . .
H50A H 0.801935 0.725704 0.796986 0.050 Uiso 1 1 calc R U . . .
H50B H 0.798540 0.685898 0.716534 0.050 Uiso 1 1 calc R U . . .
H50C H 0.870688 0.629411 0.774138 0.050 Uiso 1 1 calc R U . . .
C51 C 0.0673(2) 0.17571(19) 0.65734(19) 0.0373(6) Uani 1 1 d . . . . .
H51A H -0.009249 0.194172 0.665687 0.056 Uiso 1 1 calc R U . . .
H51B H 0.077848 0.108607 0.680017 0.056 Uiso 1 1 calc R U . . .
H51C H 0.098780 0.182867 0.600502 0.056 Uiso 1 1 calc R U . . .
C52 C 0.06458(18) 0.2327(2) 0.78525(15) 0.0372(6) Uani 1 1 d . . . . .
H52A H 0.093362 0.278138 0.811255 0.056 Uiso 1 1 calc R U . . .
H52B H 0.076454 0.167138 0.810881 0.056 Uiso 1 1 calc R U . . .
H52C H -0.012159 0.247853 0.789542 0.056 Uiso 1 1 calc R U . . .
C53 C 0.4535(2) -0.08165(18) 0.90103(17) 0.0374(6) Uani 1 1 d . . . . .
H53A H 0.492371 -0.139911 0.922252 0.045 Uiso 1 1 calc R U . . .
H53B H 0.383004 -0.072903 0.936939 0.045 Uiso 1 1 calc R U . . .
F4 F 0.0570(3) 0.6041(3) 0.8267(3) 0.1454(19) Uani 1 1 d . . . . .
C55 C 0.1155(3) 0.1592(2) 0.98960(18) 0.0437(7) Uani 1 1 d . . . . .
H55A H 0.072197 0.191092 0.951939 0.052 Uiso 1 1 calc R U . . .
H55B H 0.069205 0.121216 1.034249 0.052 Uiso 1 1 calc R U . . .
C56 C 0.0006(3) 0.8810(2) 0.7904(2) 0.0519(8) Uani 1 1 d . . . . .
H56A H -0.073224 0.894011 0.782075 0.062 Uiso 1 1 calc R U . . .
H56B H 0.003480 0.821331 0.827716 0.062 Uiso 1 1 calc R U . . .
C57 C 0.2081(3) 0.0980(3) 0.94960(19) 0.0528(8) Uani 1 1 d . . . . .
H57A H 0.184938 0.034054 0.945972 0.063 Uiso 1 1 calc R U . . .
H57B H 0.237693 0.128990 0.895493 0.063 Uiso 1 1 calc R U . . .
C58 C 0.4417(2) -0.0880(2) 0.81723(19) 0.0384(6) Uani 1 1 d . . . . .
H58A H 0.429852 -0.154456 0.810638 0.046 Uiso 1 1 calc R U . . .
H58B H 0.382112 -0.044285 0.803353 0.046 Uiso 1 1 calc R U . . .
C59 C 0.9324(2) 0.3664(2) 0.39356(16) 0.0418(7) Uani 1 1 d . . . . .
H59A H 0.909355 0.430957 0.370053 0.050 Uiso 1 1 calc R U . . .
H59B H 0.985435 0.335483 0.352847 0.050 Uiso 1 1 calc R U . . .
C60 C 0.5178(3) 0.00685(19) 0.89020(15) 0.0398(7) Uani 1 1 d . . . . .
H60A H 0.469736 0.065158 0.898668 0.048 Uiso 1 1 calc R U . . .
H60B H 0.565799 -0.000934 0.927959 0.048 Uiso 1 1 calc R U . . .
C61 C 0.1782(3) 0.9101(2) 0.7234(2) 0.0517(9) Uani 1 1 d . . . . .
H61A H 0.235440 0.858270 0.724362 0.062 Uiso 1 1 calc R U . . .
H61B H 0.203046 0.961321 0.679648 0.062 Uiso 1 1 calc R U . . .
C62 C 0.2719(3) 0.1659(3) 1.0385(2) 0.0577(9) Uani 1 1 d . . . . .
H62A H 0.336488 0.203228 1.023615 0.069 Uiso 1 1 calc R U . . .
H62B H 0.258957 0.143373 1.095914 0.069 Uiso 1 1 calc R U . . .
C63 C 0.9773(3) 0.3724(4) 0.46459(18) 0.0708(14) Uani 1 1 d . . . . .
H63A H 1.004645 0.436477 0.461531 0.085 Uiso 1 1 calc R U . . .
H63B H 1.036440 0.322895 0.468043 0.085 Uiso 1 1 calc R U . . .
F6 F 0.1668(3) 0.4823(2) 0.8064(4) 0.166(2) Uani 1 1 d . . . . .
F5 F 0.1310(3) 0.5341(3) 0.9182(3) 0.1418(17) Uani 1 1 d . . . . .
C66 C 0.7880(4) -0.0484(2) 0.57871(18) 0.0416(9) Uani 0.8075(19) 1 d . . P A 1
C67 C 0.0768(4) 0.8716(3) 0.7141(2) 0.0620(10) Uani 1 1 d . . . . .
H67A H 0.049855 0.909696 0.669626 0.074 Uiso 1 1 calc R U . . .
H67B H 0.089031 0.803565 0.704531 0.074 Uiso 1 1 calc R U . . .
C68 C 0.1730(3) 0.2297(3) 1.0176(2) 0.0527(8) Uani 1 1 d . . . . .
H68A H 0.128517 0.255849 1.064636 0.063 Uiso 1 1 calc R U . . .
H68B H 0.195256 0.283364 0.975431 0.063 Uiso 1 1 calc R U . . .
C69 C 0.1502(3) 0.5632(3) 0.8390(3) 0.0624(9) Uani 1 1 d . . . . .
S3 S 0.7480(4) 0.0302(4) 0.6102(4) 0.0624(9) Uani 0.1925(19) 1 d . . P A 2
C70 C 0.8698(17) -0.0391(14) 0.5775(15) 0.0624(9) Uani 0.1925(19) 1 d . . P A 2
F7 F 0.9599(8) 0.0076(9) 0.5829(7) 0.061(3) Uani 0.1925(19) 1 d . . P A 2
F8 F 0.8790(7) -0.1237(5) 0.6217(5) 0.0286(17) Uani 0.1925(19) 1 d . . P A 2
F9 F 0.8957(7) -0.0500(8) 0.5046(7) 0.035(2) Uani 0.1925(19) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 O2 1.9911(13) . ?
Ni2 N1 2.0262(15) . ?
Ni2 N2 2.0534(16) . ?
Ni2 O4 2.0740(14) . ?
Ni2 O9 2.1047(14) . ?
Ni2 O1 2.1250(13) . ?
Ni1 O1 1.9732(13) . ?
Ni1 N4 2.0269(16) . ?
Ni1 N3 2.0461(17) . ?
Ni1 O3 2.0696(15) . ?
Ni1 O2 2.1207(13) . ?
Ni1 O8 2.1601(14) . ?
S1 O4 1.4955(15) . ?
S1 O3 1.5037(16) . ?
S1 C66 1.891(4) . ?
S2 O5 1.4334(19) . ?
S2 O6 1.434(2) . ?
S2 O10 1.440(3) . ?
S2 C69 1.759(5) . ?
O1 C11 1.336(2) . ?
O8 C40 1.451(2) . ?
O8 C45 1.454(3) . ?
O9 C60 1.440(3) . ?
O9 C43 1.450(2) . ?
O2 C30 1.339(2) . ?
O4 S3 1.654(6) . ?
O3 S3 1.660(6) . ?
N1 C5 1.338(2) . ?
N1 C2 1.361(2) . ?
N2 C13 1.333(2) . ?
N2 C8 1.361(2) . ?
N4 C15 1.340(2) . ?
N4 C1 1.360(2) . ?
O7 C56 1.421(4) . ?
O7 C47 1.435(4) . ?
N3 C34 1.327(3) . ?
N3 C6 1.359(3) . ?
F2 C66 1.334(4) . ?
C1 C18 1.401(3) . ?
C1 C6 1.443(3) . ?
C2 C16 1.404(2) . ?
C2 C8 1.439(3) . ?
C3 C20 1.372(3) . ?
C3 C5 1.425(2) . ?
C3 H3 0.9500 . ?
C4 C9 1.370(3) . ?
C4 C15 1.427(3) . ?
C4 H4 0.9500 . ?
C5 C7 1.481(2) . ?
C6 C33 1.408(3) . ?
C7 C19 1.409(3) . ?
C7 C30 1.427(3) . ?
C8 C12 1.405(2) . ?
C9 C18 1.413(3) . ?
C9 H9 0.9500 . ?
C10 C14 1.373(3) . ?
C10 C13 1.406(3) . ?
C10 H10 0.9500 . ?
C11 C27 1.408(3) . ?
C11 C35 1.423(2) . ?
C12 C14 1.413(3) . ?
C12 C32 1.433(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C35 1.483(2) . ?
C16 C20 1.412(3) . ?
C16 C28 1.435(3) . ?
C17 C31 1.364(3) . ?
C17 C18 1.436(3) . ?
C17 H17 0.9500 . ?
C19 C24 1.391(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.386(3) . ?
C21 C35 1.418(2) . ?
C21 H21 0.9500 . ?
F3 C66 1.328(4) . ?
F1 C66 1.332(5) . ?
C24 C37 1.400(3) . ?
C24 C36 1.539(3) . ?
C25 C27 1.384(3) . ?
C25 C26 1.399(3) . ?
C25 H25 0.9500 . ?
C26 C39 1.536(3) . ?
C27 H27 0.9500 . ?
C28 C32 1.358(3) . ?
C28 H28 0.9500 . ?
O11 C62 1.384(4) . ?
O11 C57 1.402(5) . ?
C30 C38 1.407(3) . ?
C31 C33 1.430(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C44 1.414(3) . ?
C34 C42 1.406(3) . ?
C34 H34 0.9500 . ?
C36 C51 1.526(3) . ?
C36 C41 1.535(3) . ?
C36 C52 1.537(3) . ?
C37 C38 1.388(3) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C48 1.532(3) . ?
C39 C50 1.536(3) . ?
C39 C49 1.537(3) . ?
C40 C59 1.498(3) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C44 1.369(3) . ?
C42 H42 0.9500 . ?
C43 C58 1.513(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44 0.9500 . ?
C45 C63 1.507(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C47 C61 1.507(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C58 1.524(4) . ?
C53 C60 1.526(3) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
F4 C69 1.330(4) . ?
C55 C68 1.488(4) . ?
C55 C57 1.505(5) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C67 1.483(5) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C63 1.499(4) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 C67 1.509(6) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C68 1.570(5) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
F6 C69 1.328(5) . ?
F5 C69 1.360(6) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
S3 C70 1.79(2) . ?
C70 F9 1.27(3) . ?
C70 F8 1.33(2) . ?
C70 F7 1.41(2) . ?

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 Ni2 N1 91.62(6) . . ?
O2 Ni2 N2 172.47(6) . . ?
N1 Ni2 N2 81.78(6) . . ?
O2 Ni2 O4 93.76(6) . . ?
N1 Ni2 O4 174.61(6) . . ?
N2 Ni2 O4 92.86(6) . . ?
O2 Ni2 O9 93.35(6) . . ?
N1 Ni2 O9 93.14(6) . . ?
N2 Ni2 O9 90.64(6) . . ?
O4 Ni2 O9 86.32(6) . . ?
O2 Ni2 O1 81.15(5) . . ?
N1 Ni2 O1 90.17(6) . . ?
N2 Ni2 O1 95.18(6) . . ?
O4 Ni2 O1 90.89(6) . . ?
O9 Ni2 O1 173.67(5) . . ?
O1 Ni1 N4 91.76(6) . . ?
O1 Ni1 N3 170.89(6) . . ?
N4 Ni1 N3 82.25(7) . . ?
O1 Ni1 O3 91.84(6) . . ?
N4 Ni1 O3 174.79(6) . . ?
N3 Ni1 O3 94.61(7) . . ?
O1 Ni1 O2 81.67(5) . . ?
N4 Ni1 O2 91.79(6) . . ?
N3 Ni1 O2 91.61(6) . . ?
O3 Ni1 O2 92.45(6) . . ?
O1 Ni1 O8 93.94(5) . . ?
N4 Ni1 O8 91.74(6) . . ?
N3 Ni1 O8 93.11(6) . . ?
O3 Ni1 O8 84.26(6) . . ?
O2 Ni1 O8 174.44(5) . . ?
O4 S1 O3 112.04(9) . . ?
O4 S1 C66 98.39(13) . . ?
O3 S1 C66 95.54(14) . . ?
O5 S2 O6 115.49(12) . . ?
O5 S2 O10 114.45(16) . . ?
O6 S2 O10 115.22(15) . . ?
O5 S2 C69 103.25(17) . . ?
O6 S2 C69 103.31(18) . . ?
O10 S2 C69 102.6(3) . . ?
C11 O1 Ni1 122.44(11) . . ?
C11 O1 Ni2 121.45(11) . . ?
Ni1 O1 Ni2 96.44(6) . . ?
C40 O8 C45 107.21(16) . . ?
C40 O8 Ni1 116.77(12) . . ?
C45 O8 Ni1 118.75(12) . . ?
C60 O9 C43 110.89(17) . . ?
C60 O9 Ni2 123.01(13) . . ?
C43 O9 Ni2 122.04(12) . . ?
C30 O2 Ni2 122.09(11) . . ?
C30 O2 Ni1 121.24(11) . . ?
Ni2 O2 Ni1 96.04(5) . . ?
S1 O4 Ni2 130.91(9) . . ?
S1 O3 Ni1 131.14(9) . . ?
C5 N1 C2 119.93(15) . . ?
C5 N1 Ni2 127.39(12) . . ?
C2 N1 Ni2 111.69(12) . . ?
C13 N2 C8 118.13(16) . . ?
C13 N2 Ni2 130.27(13) . . ?
C8 N2 Ni2 111.42(12) . . ?
C15 N4 C1 119.96(16) . . ?
C15 N4 Ni1 127.69(13) . . ?
C1 N4 Ni1 111.62(12) . . ?
C56 O7 C47 104.6(2) . . ?
C34 N3 C6 118.80(18) . . ?
C34 N3 Ni1 129.27(15) . . ?
C6 N3 Ni1 111.12(12) . . ?
N4 C1 C18 123.63(17) . . ?
N4 C1 C6 117.05(17) . . ?
C18 C1 C6 119.30(17) . . ?
N1 C2 C16 123.47(17) . . ?
N1 C2 C8 117.17(16) . . ?
C16 C2 C8 119.36(16) . . ?
C20 C3 C5 120.63(17) . . ?
C20 C3 H3 119.7 . . ?
C5 C3 H3 119.7 . . ?
C9 C4 C15 120.64(18) . . ?
C9 C4 H4 119.7 . . ?
C15 C4 H4 119.7 . . ?
N1 C5 C3 119.45(16) . . ?
N1 C5 C7 119.46(16) . . ?
C3 C5 C7 121.07(16) . . ?
N3 C6 C33 122.96(18) . . ?
N3 C6 C1 117.00(17) . . ?
C33 C6 C1 120.00(18) . . ?
C19 C7 C30 118.14(17) . . ?
C19 C7 C5 116.99(16) . . ?
C30 C7 C5 124.86(16) . . ?
N2 C8 C12 123.25(17) . . ?
N2 C8 C2 116.57(16) . . ?
C12 C8 C2 120.18(17) . . ?
C4 C9 C18 120.08(18) . . ?
C4 C9 H9 120.0 . . ?
C18 C9 H9 120.0 . . ?
C14 C10 C13 119.54(18) . . ?
C14 C10 H10 120.2 . . ?
C13 C10 H10 120.2 . . ?
O1 C11 C27 116.46(16) . . ?
O1 C11 C35 125.83(16) . . ?
C27 C11 C35 117.70(16) . . ?
C8 C12 C14 117.14(18) . . ?
C8 C12 C32 119.24(18) . . ?
C14 C12 C32 123.62(18) . . ?
N2 C13 C10 122.47(18) . . ?
N2 C13 H13 118.8 . . ?
C10 C13 H13 118.8 . . ?
C10 C14 C12 119.42(18) . . ?
C10 C14 H14 120.3 . . ?
C12 C14 H14 120.3 . . ?
N4 C15 C4 119.36(16) . . ?
N4 C15 C35 119.51(16) . . ?
C4 C15 C35 121.12(16) . . ?
C2 C16 C20 116.26(17) . . ?
C2 C16 C28 119.20(17) . . ?
C20 C16 C28 124.53(17) . . ?
C31 C17 C18 120.71(19) . . ?
C31 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C1 C18 C9 116.25(17) . . ?
C1 C18 C17 119.75(18) . . ?
C9 C18 C17 123.99(18) . . ?
C24 C19 C7 124.49(18) . . ?
C24 C19 H19 117.8 . . ?
C7 C19 H19 117.8 . . ?
C3 C20 C16 119.97(17) . . ?
C3 C20 H20 120.0 . . ?
C16 C20 H20 120.0 . . ?
C26 C21 C35 123.86(17) . . ?
C26 C21 H21 118.1 . . ?
C35 C21 H21 118.1 . . ?
C19 C24 C37 116.34(18) . . ?
C19 C24 C36 119.71(18) . . ?
C37 C24 C36 123.93(18) . . ?
C27 C25 C26 120.71(18) . . ?
C27 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C25 117.23(17) . . ?
C21 C26 C39 122.57(18) . . ?
C25 C26 C39 120.21(17) . . ?
C25 C27 C11 122.61(18) . . ?
C25 C27 H27 118.7 . . ?
C11 C27 H27 118.7 . . ?
C32 C28 C16 121.47(18) . . ?
C32 C28 H28 119.3 . . ?
C16 C28 H28 119.3 . . ?
C62 O11 C57 109.3(3) . . ?
O2 C30 C38 118.02(16) . . ?
O2 C30 C7 124.75(16) . . ?
C38 C30 C7 117.19(17) . . ?
C17 C31 C33 120.95(18) . . ?
C17 C31 H31 119.5 . . ?
C33 C31 H31 119.5 . . ?
C28 C32 C12 120.48(17) . . ?
C28 C32 H32 119.8 . . ?
C12 C32 H32 119.8 . . ?
C6 C33 C44 116.7(2) . . ?
C6 C33 C31 119.23(19) . . ?
C44 C33 C31 124.00(19) . . ?
N3 C34 C42 122.2(2) . . ?
N3 C34 H34 118.9 . . ?
C42 C34 H34 118.9 . . ?
C21 C35 C11 117.82(16) . . ?
C21 C35 C15 117.65(16) . . ?
C11 C35 C15 124.54(16) . . ?
C51 C36 C41 109.01(19) . . ?
C51 C36 C52 108.0(2) . . ?
C41 C36 C52 108.7(2) . . ?
C51 C36 C24 112.27(19) . . ?
C41 C36 C24 108.86(17) . . ?
C52 C36 C24 109.99(17) . . ?
C38 C37 C24 121.08(18) . . ?
C38 C37 H37 119.5 . . ?
C24 C37 H37 119.5 . . ?
C37 C38 C30 122.73(18) . . ?
C37 C38 H38 118.6 . . ?
C30 C38 H38 118.6 . . ?
C48 C39 C50 109.03(19) . . ?
C48 C39 C26 111.85(17) . . ?
C50 C39 C26 109.31(17) . . ?
C48 C39 C49 107.91(17) . . ?
C50 C39 C49 109.35(18) . . ?
C26 C39 C49 109.36(16) . . ?
O8 C40 C59 104.68(19) . . ?
O8 C40 H40A 110.8 . . ?
C59 C40 H40A 110.8 . . ?
O8 C40 H40B 110.8 . . ?
C59 C40 H40B 110.8 . . ?
H40A C40 H40B 108.9 . . ?
C36 C41 H41A 109.5 . . ?
C36 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C36 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C44 C42 C34 119.5(2) . . ?
C44 C42 H42 120.3 . . ?
C34 C42 H42 120.3 . . ?
O9 C43 C58 104.56(19) . . ?
O9 C43 H43A 110.8 . . ?
C58 C43 H43A 110.8 . . ?
O9 C43 H43B 110.8 . . ?
C58 C43 H43B 110.8 . . ?
H43A C43 H43B 108.9 . . ?
C42 C44 C33 119.84(19) . . ?
C42 C44 H44 120.1 . . ?
C33 C44 H44 120.1 . . ?
O8 C45 C63 106.29(19) . . ?
O8 C45 H45A 110.5 . . ?
C63 C45 H45A 110.5 . . ?
O8 C45 H45B 110.5 . . ?
C63 C45 H45B 110.5 . . ?
H45A C45 H45B 108.7 . . ?
O7 C47 C61 106.2(3) . . ?
O7 C47 H47A 110.5 . . ?
C61 C47 H47A 110.5 . . ?
O7 C47 H47B 110.5 . . ?
C61 C47 H47B 110.5 . . ?
H47A C47 H47B 108.7 . . ?
C39 C48 H48A 109.5 . . ?
C39 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C39 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C39 C49 H49A 109.5 . . ?
C39 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C39 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C39 C50 H50A 109.5 . . ?
C39 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C39 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C36 C51 H51A 109.5 . . ?
C36 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C36 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C36 C52 H52A 109.5 . . ?
C36 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C36 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C58 C53 C60 102.8(2) . . ?
C58 C53 H53A 111.2 . . ?
C60 C53 H53A 111.2 . . ?
C58 C53 H53B 111.2 . . ?
C60 C53 H53B 111.2 . . ?
H53A C53 H53B 109.1 . . ?
C68 C55 C57 100.7(3) . . ?
C68 C55 H55A 111.6 . . ?
C57 C55 H55A 111.6 . . ?
C68 C55 H55B 111.6 . . ?
C57 C55 H55B 111.6 . . ?
H55A C55 H55B 109.4 . . ?
O7 C56 C67 105.8(3) . . ?
O7 C56 H56A 110.6 . . ?
C67 C56 H56A 110.6 . . ?
O7 C56 H56B 110.6 . . ?
C67 C56 H56B 110.6 . . ?
H56A C56 H56B 108.7 . . ?
O11 C57 C55 106.8(3) . . ?
O11 C57 H57A 110.4 . . ?
C55 C57 H57A 110.4 . . ?
O11 C57 H57B 110.4 . . ?
C55 C57 H57B 110.4 . . ?
H57A C57 H57B 108.6 . . ?
C43 C58 C53 102.5(2) . . ?
C43 C58 H58A 111.3 . . ?
C53 C58 H58A 111.3 . . ?
C43 C58 H58B 111.3 . . ?
C53 C58 H58B 111.3 . . ?
H58A C58 H58B 109.2 . . ?
C40 C59 C63 103.1(2) . . ?
C40 C59 H59A 111.1 . . ?
C63 C59 H59A 111.1 . . ?
C40 C59 H59B 111.1 . . ?
C63 C59 H59B 111.1 . . ?
H59A C59 H59B 109.1 . . ?
O9 C60 C53 105.3(2) . . ?
O9 C60 H60A 110.7 . . ?
C53 C60 H60A 110.7 . . ?
O9 C60 H60B 110.7 . . ?
C53 C60 H60B 110.7 . . ?
H60A C60 H60B 108.8 . . ?
C47 C61 C67 104.3(2) . . ?
C47 C61 H61A 110.9 . . ?
C67 C61 H61A 110.9 . . ?
C47 C61 H61B 110.9 . . ?
C67 C61 H61B 110.9 . . ?
H61A C61 H61B 108.9 . . ?
O11 C62 C68 106.6(3) . . ?
O11 C62 H62A 110.4 . . ?
C68 C62 H62A 110.4 . . ?
O11 C62 H62B 110.4 . . ?
C68 C62 H62B 110.4 . . ?
H62A C62 H62B 108.6 . . ?
C59 C63 C45 106.2(2) . . ?
C59 C63 H63A 110.5 . . ?
C45 C63 H63A 110.5 . . ?
C59 C63 H63B 110.5 . . ?
C45 C63 H63B 110.5 . . ?
H63A C63 H63B 108.7 . . ?
F3 C66 F1 107.3(3) . . ?
F3 C66 F2 108.3(3) . . ?
F1 C66 F2 107.4(3) . . ?
F3 C66 S1 111.7(3) . . ?
F1 C66 S1 112.6(2) . . ?
F2 C66 S1 109.5(3) . . ?
C56 C67 C61 104.6(3) . . ?
C56 C67 H67A 110.8 . . ?
C61 C67 H67A 110.8 . . ?
C56 C67 H67B 110.8 . . ?
C61 C67 H67B 110.8 . . ?
H67A C67 H67B 108.9 . . ?
C55 C68 C62 101.7(3) . . ?
C55 C68 H68A 111.4 . . ?
C62 C68 H68A 111.4 . . ?
C55 C68 H68B 111.4 . . ?
C62 C68 H68B 111.4 . . ?
H68A C68 H68B 109.3 . . ?
F6 C69 F4 107.1(3) . . ?
F6 C69 F5 104.6(5) . . ?
F4 C69 F5 104.0(4) . . ?
F6 C69 S2 113.9(4) . . ?
F4 C69 S2 114.8(3) . . ?
F5 C69 S2 111.4(3) . . ?
O4 S3 O3 97.3(3) . . ?
O4 S3 C70 96.6(7) . . ?
O3 S3 C70 94.4(8) . . ?
F9 C70 F8 109.8(15) . . ?
F9 C70 F7 99.0(18) . . ?
F8 C70 F7 103.3(14) . . ?
F9 C70 S3 117.5(14) . . ?
F8 C70 S3 113.9(17) . . ?
F7 C70 S3 111.5(12) . . ?

_refine_diff_density_max         2.198
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.088

