# Electronic Supplementary Material (ESI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_mo_krosi9_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2309035'
loop_
_audit_author_name
_audit_author_address
'Silva Maria Kronawitter'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2023-11-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_audit_creation_date             2021-12-15
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        DEPNidca3
_chemical_formula_moiety         'C6 N9 Ni, C9 H20 N'
_chemical_formula_sum            'C15 H20 N10 Ni'
_chemical_formula_weight         399.12
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   16.3161(17)
_cell_length_b                   12.1389(13)
_cell_length_c                   10.1679(11)
_cell_angle_alpha                90
_cell_angle_beta                 101.691(3)
_cell_angle_gamma                90
_cell_volume                     1972.1(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.65
_shelx_estimated_absorpt_T_max   0.935
_shelx_estimated_absorpt_T_min   0.844
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7173
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0570 before and 0.0418 after correction.
The Ratio of minimum to maximum transmission is 0.9623.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             832
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3.00 1.00 3.00 0.0200
0.00 1.00 2.00 0.0190
1.00 0.00 -1.00 0.0640
3.00 -1.00 -1.00 0.0450
-2.00 3.00 -4.00 0.0740
-2.00 1.00 0.00 0.0810
2.00 -3.00 4.00 0.0580
4.00 -3.00 -4.00 0.0280
1.00 -2.00 -4.00 0.0410
1.00 -2.00 -2.00 0.0270
-1.00 -2.00 -3.00 0.0410
4.00 3.00 -1.00 0.0740
-4.00 -4.00 1.00 0.0820
0.00 4.00 1.00 0.0740

_exptl_crystal_preparation       'wet chemistry'
_exptl_crystal_recrystallization_method 'wet chemistry'
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.068
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            48266
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.274
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3720
_reflns_number_total             4029
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         4029
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0355P)²+5.6162P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1159
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C18) = Uanis(C17)
Uanis(C15) = Uanis(C16) = Uanis(C10) = Uanis(C9)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,
 H15B), C17(H17A,H17B), C18(H18A,H18B)
3.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 1.000000 0.500000 0.500000 0.01719(13) Uani 1 2 d S . P . .
Ni2 Ni 0.500000 0.500000 0.500000 0.02016(14) Uani 1 2 d S . P . .
N1 N 0.94576(14) 0.64080(19) 0.4060(2) 0.0241(5) Uani 1 1 d . . . . .
N2 N 0.91332(16) 0.8315(2) 0.3326(3) 0.0295(6) Uani 1 1 d . . . . .
N3 N 0.98709(15) 0.9332(2) 0.1826(2) 0.0250(5) Uani 1 1 d . . . . .
N4 N 0.88341(14) 0.4281(2) 0.4904(2) 0.0247(5) Uani 1 1 d . . . . .
N5 N 0.76560(16) 0.3796(3) 0.5951(3) 0.0499(9) Uani 1 1 d . . . . .
N6 N 0.62705(16) 0.4664(2) 0.5475(3) 0.0343(6) Uani 1 1 d . . . . .
N7 N 0.47793(18) 0.3404(2) 0.5507(3) 0.0343(6) Uani 1 1 d . . . . .
N8 N 0.4944(3) 0.1426(3) 0.5935(3) 0.0769(15) Uani 1 1 d . . . . .
N9 N 0.49593(16) 0.0521(2) 0.8070(3) 0.0312(6) Uani 1 1 d . . . . .
N10 N 0.7602(2) 1.0111(3) 0.5660(3) 0.0573(11) Uani 1 1 d . . . . .
C1 C 0.82624(17) 0.4098(2) 0.5363(3) 0.0259(6) Uani 1 1 d . . . . .
C3 C 0.69299(18) 0.4293(3) 0.5650(3) 0.0308(7) Uani 1 1 d . . . . .
C4 C 0.4850(2) 0.2490(3) 0.5768(3) 0.0367(7) Uani 1 1 d . . . . .
C6 C 0.4943(2) 0.1000(3) 0.7108(3) 0.0329(7) Uani 1 1 d . . . . .
C7 C 0.93365(16) 0.7300(2) 0.3692(3) 0.0211(5) Uani 1 1 d . . . . .
C8 C 0.95436(16) 0.8815(2) 0.2519(3) 0.0210(5) Uani 1 1 d . . . . .
C9 C 0.8725(3) 1.1117(4) 0.4688(4) 0.0641(7) Uani 1 1 d . . . . .
H9A H 0.833263 1.118227 0.382356 0.096 Uiso 1 1 calc R U . . .
H9B H 0.907021 1.045711 0.468337 0.096 Uiso 1 1 calc R U . . .
H9C H 0.908491 1.176955 0.483512 0.096 Uiso 1 1 calc R U . . .
C10 C 0.8236(3) 1.1025(4) 0.5812(4) 0.0641(7) Uani 1 1 d . . . . .
H10A H 0.863951 1.091961 0.667157 0.077 Uiso 1 1 calc R U . . .
H10B H 0.794352 1.173244 0.587328 0.077 Uiso 1 1 calc R U . . .
C12 C 0.7159(3) 1.0155(5) 0.6868(4) 0.0718(7) Uani 1 1 d . . . . .
H12A H 0.759201 1.019831 0.770427 0.086 Uiso 1 1 calc R U . . .
H12B H 0.682386 1.083990 0.680416 0.086 Uiso 1 1 calc R U . . .
C13 C 0.6605(3) 0.9210(5) 0.6977(4) 0.0718(7) Uani 1 1 d . . . . .
H13A H 0.612757 0.921673 0.620042 0.086 Uiso 1 1 calc R U . . .
H13B H 0.637697 0.928954 0.780355 0.086 Uiso 1 1 calc R U . . .
C14 C 0.7059(3) 0.8111(5) 0.7016(4) 0.0718(7) Uani 1 1 d . . . . .
H14A H 0.665430 0.749977 0.698787 0.086 Uiso 1 1 calc R U . . .
H14B H 0.748192 0.805072 0.786096 0.086 Uiso 1 1 calc R U . . .
C15 C 0.6980(3) 1.0202(4) 0.4331(4) 0.0641(7) Uani 1 1 d . . . . .
H15A H 0.653179 0.965090 0.432436 0.077 Uiso 1 1 calc R U . . .
H15B H 0.727072 1.000922 0.359819 0.077 Uiso 1 1 calc R U . . .
C16 C 0.6574(3) 1.1331(4) 0.4029(4) 0.0641(7) Uani 1 1 d . . . . .
H16A H 0.700728 1.188207 0.399288 0.096 Uiso 1 1 calc R U . . .
H16B H 0.627297 1.152846 0.473774 0.096 Uiso 1 1 calc R U . . .
H16C H 0.617976 1.130684 0.316285 0.096 Uiso 1 1 calc R U . . .
C17 C 0.8055(3) 0.9010(5) 0.5731(4) 0.0718(7) Uani 1 1 d . . . . .
H17A H 0.830427 0.892951 0.492585 0.086 Uiso 1 1 calc R U . . .
H17B H 0.851784 0.900703 0.652914 0.086 Uiso 1 1 calc R U . . .
C18 C 0.7487(3) 0.8029(5) 0.5812(4) 0.0718(7) Uani 1 1 d . . . . .
H18A H 0.782237 0.734335 0.588604 0.086 Uiso 1 1 calc R U . . .
H18B H 0.705539 0.798662 0.497578 0.086 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 2.067(2) 3_766 ?
Ni1 N1 2.067(2) . ?
Ni1 N3 2.075(2) 4_576 ?
Ni1 N3 2.075(2) 2_745 ?
Ni1 N4 2.077(2) . ?
Ni1 N4 2.077(2) 3_766 ?
Ni2 N6 2.072(3) . ?
Ni2 N6 2.072(3) 3_666 ?
Ni2 N7 2.055(3) 3_666 ?
Ni2 N7 2.055(3) . ?
Ni2 N9 2.050(3) 2_656 ?
Ni2 N9 2.050(3) 4_565 ?
N1 C7 1.149(4) . ?
N2 C7 1.310(4) . ?
N2 C8 1.308(3) . ?
N3 C8 1.153(3) . ?
N4 C1 1.146(4) . ?
N5 C1 1.308(4) . ?
N5 C3 1.310(4) . ?
N6 C3 1.146(4) . ?
N7 C4 1.141(4) . ?
N8 C4 1.308(4) . ?
N8 C6 1.300(4) . ?
N9 C6 1.133(4) . ?
N10 C10 1.504(6) . ?
N10 C12 1.547(5) . ?
N10 C15 1.521(5) . ?
N10 C17 1.523(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 C10 1.524(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.480(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.522(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C18 1.531(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.525(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.521(8) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0 3_766 . ?
N1 Ni1 N3 91.20(9) . 2_745 ?
N1 Ni1 N3 88.80(9) 3_766 2_745 ?
N1 Ni1 N3 88.80(9) . 4_576 ?
N1 Ni1 N3 91.20(9) 3_766 4_576 ?
N1 Ni1 N4 91.34(9) . . ?
N1 Ni1 N4 88.66(9) 3_766 . ?
N1 Ni1 N4 91.34(9) 3_766 3_766 ?
N1 Ni1 N4 88.66(9) . 3_766 ?
N3 Ni1 N3 180.0 4_576 2_745 ?
N3 Ni1 N4 87.03(9) 2_745 3_766 ?
N3 Ni1 N4 92.97(9) 4_576 3_766 ?
N3 Ni1 N4 87.03(9) 4_576 . ?
N3 Ni1 N4 92.97(9) 2_745 . ?
N4 Ni1 N4 180.0 . 3_766 ?
N6 Ni2 N6 180.0 . 3_666 ?
N7 Ni2 N6 91.51(12) 3_666 . ?
N7 Ni2 N6 88.50(12) . . ?
N7 Ni2 N6 91.50(12) . 3_666 ?
N7 Ni2 N6 88.49(11) 3_666 3_666 ?
N7 Ni2 N7 180.0 . 3_666 ?
N9 Ni2 N6 90.05(11) 2_656 . ?
N9 Ni2 N6 89.95(11) 4_565 . ?
N9 Ni2 N6 89.95(11) 2_656 3_666 ?
N9 Ni2 N6 90.05(11) 4_565 3_666 ?
N9 Ni2 N7 91.39(11) 2_656 . ?
N9 Ni2 N7 91.39(11) 4_565 3_666 ?
N9 Ni2 N7 88.61(11) 4_565 . ?
N9 Ni2 N7 88.61(11) 2_656 3_666 ?
N9 Ni2 N9 180.0 4_565 2_656 ?
C7 N1 Ni1 163.4(2) . . ?
C8 N2 C7 118.9(2) . . ?
C8 N3 Ni1 154.6(2) . 2_755 ?
C1 N4 Ni1 151.1(2) . . ?
C1 N5 C3 119.7(3) . . ?
C3 N6 Ni2 167.7(3) . . ?
C4 N7 Ni2 163.8(3) . . ?
C6 N8 C4 119.4(3) . . ?
C6 N9 Ni2 167.2(3) . 2_646 ?
C10 N10 C12 108.4(3) . . ?
C10 N10 C15 111.1(4) . . ?
C10 N10 C17 109.0(3) . . ?
C15 N10 C12 111.6(3) . . ?
C15 N10 C17 109.7(3) . . ?
C17 N10 C12 107.0(4) . . ?
N4 C1 N5 173.7(3) . . ?
N6 C3 N5 173.5(3) . . ?
N7 C4 N8 173.8(4) . . ?
N9 C6 N8 172.5(4) . . ?
N1 C7 N2 174.3(3) . . ?
N3 C8 N2 174.5(3) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
N10 C10 C9 115.5(3) . . ?
N10 C10 H10A 108.4 . . ?
N10 C10 H10B 108.4 . . ?
C9 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
N10 C12 H12A 108.5 . . ?
N10 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C13 C12 N10 115.1(4) . . ?
C13 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
C12 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
C12 C13 C14 112.3(4) . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
C13 C14 C18 109.6(4) . . ?
H14A C14 H14B 108.2 . . ?
C18 C14 H14A 109.7 . . ?
C18 C14 H14B 109.7 . . ?
N10 C15 H15A 108.4 . . ?
N10 C15 H15B 108.4 . . ?
N10 C15 C16 115.4(3) . . ?
H15A C15 H15B 107.5 . . ?
C16 C15 H15A 108.4 . . ?
C16 C15 H15B 108.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N10 C17 H17A 108.9 . . ?
N10 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C18 C17 N10 113.2(4) . . ?
C18 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
C14 C18 H18A 109.2 . . ?
C14 C18 H18B 109.2 . . ?
C17 C18 C14 112.0(4) . . ?
C17 C18 H18A 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?

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
N10 C12 C13 C14 55.6(4) . . . . ?
N10 C17 C18 C14 -57.0(4) . . . . ?
C10 N10 C12 C13 -171.3(3) . . . . ?
C10 N10 C15 C16 -50.7(5) . . . . ?
C10 N10 C17 C18 170.8(3) . . . . ?
C12 N10 C10 C9 -179.0(3) . . . . ?
C12 N10 C15 C16 70.4(6) . . . . ?
C12 N10 C17 C18 53.8(4) . . . . ?
C12 C13 C14 C18 -53.2(5) . . . . ?
C13 C14 C18 C17 54.0(5) . . . . ?
C15 N10 C10 C9 -56.1(4) . . . . ?
C15 N10 C12 C13 66.1(5) . . . . ?
C15 N10 C17 C18 -67.5(5) . . . . ?
C17 N10 C10 C9 64.8(4) . . . . ?
C17 N10 C12 C13 -53.9(4) . . . . ?
C17 N10 C15 C16 -171.2(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_krosi100_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2309036'
loop_
_audit_author_name
_audit_author_address
'Silva Maria Kronawitter'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2023-11-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_audit_creation_date             2023-08-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        DEPNidca3_RT
_chemical_formula_moiety         'C6 N9 Ni, C9 H20 N'
_chemical_formula_sum            'C15 H20 N10 Ni'
_chemical_formula_weight         399.12
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   16.3871(7)
_cell_length_b                   12.2076(5)
_cell_length_c                   10.2673(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.250(2)
_cell_angle_gamma                90
_cell_volume                     2021.16(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      30.95
_cell_measurement_theta_min      2.53
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1416 before and 0.0888 after correction.
The Ratio of minimum to maximum transmission is 0.8742.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_preparation       'wet chemistry'
_exptl_crystal_recrystallization_method 'wet chemistry'
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            61583
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.032
_diffrn_reflns_theta_min         2.092
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_special_details          -
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3422
_reflns_number_total             6371
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         6371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      1.172
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0970P)²+1.1915P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.2452
_refine_special_details          -
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9b,H9a), C10(H10a,H10b), C11(H11a,H11b), C12(H12a,H12b), C13(H13a,H13b),
 C14(H14a,H14b), C15(H15a,H15b)
2.b Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C16(H16a,H16b,H16c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.500000 0.500000 0.500000 0.04676(19) Uani 1 2 d S . P . .
Ni2 Ni 0.000000 0.500000 0.500000 0.04702(19) Uani 1 2 d S . P . .
N1 N 0.5041(2) 0.0575(3) 0.1892(3) 0.0747(9) Uani 1 1 d . . . . .
N2 N 0.5212(2) 0.3432(3) 0.4417(3) 0.0755(9) Uani 1 1 d . . . . .
N3 N 0.3740(2) 0.4682(4) 0.4567(4) 0.0821(10) Uani 1 1 d . . . . .
N4 N 0.2377(2) 0.3857(5) 0.4123(6) 0.133(2) Uani 1 1 d . . . . .
N5 N 0.1172(2) 0.4341(3) 0.5056(4) 0.0727(9) Uani 1 1 d . . . . .
N6 N 0.0111(2) 0.9277(3) 0.8214(3) 0.0739(9) Uani 1 1 d . . . . .
N7 N 0.0507(2) 0.6392(3) 0.5961(3) 0.0712(9) Uani 1 1 d . . . . .
N8 N 0.0814(2) 0.8264(3) 0.6686(4) 0.0863(11) Uani 1 1 d . . . . .
N9 N 0.2381(3) 1.0140(4) 0.4409(5) 0.1081(18) Uani 1 1 d . . . . .
C1 C 0.5181(3) 0.2538(3) 0.4152(4) 0.0722(11) Uani 1 1 d . . . . .
C3 C 0.5091(3) 0.1058(3) 0.2815(4) 0.0700(10) Uani 1 1 d . . . . .
C4 C 0.3089(2) 0.4339(4) 0.4411(4) 0.0734(11) Uani 1 1 d . . . . .
C5 C 0.1756(2) 0.4163(3) 0.4656(4) 0.0712(10) Uani 1 1 d . . . . .
C6 C 0.0619(2) 0.7267(3) 0.6328(4) 0.0590(8) Uani 1 1 d . . . . .
C7 C 0.0428(2) 0.8759(3) 0.7518(4) 0.0621(9) Uani 1 1 d . . . . .
C8 C 0.1277(5) 1.1142(7) 0.5392(10) 0.161(3) Uani 1 1 d . . . . .
H8A H 0.093337 1.180378 0.527426 0.241 Uiso 1 1 calc R U . . .
H8B H 0.166331 1.118376 0.623767 0.241 Uiso 1 1 calc R U . . .
H8C H 0.092156 1.049680 0.539048 0.241 Uiso 1 1 calc R U . . .
C9 C 0.1754(5) 1.1055(7) 0.4292(8) 0.147(3) Uani 1 1 d . . . . .
H9B H 0.204651 1.175666 0.422841 0.177 Uiso 1 1 calc R U . . .
H9A H 0.135518 1.095704 0.345475 0.177 Uiso 1 1 calc R U . . .
N10 N 0.5167(5) 0.1480(3) 0.3982(4) 0.148(3) Uani 1 1 d . . . . .
C10 C 0.2803(5) 1.0206(9) 0.3206(7) 0.162(4) Uani 1 1 d . . . . .
H10A H 0.237241 1.024238 0.239764 0.194 Uiso 1 1 calc R U . . .
H10B H 0.313076 1.089073 0.325563 0.194 Uiso 1 1 calc R U . . .
C11 C 0.3356(5) 0.9267(11) 0.3092(7) 0.185(5) Uani 1 1 d . . . . .
H11A H 0.381531 0.926103 0.386274 0.222 Uiso 1 1 calc R U . . .
H11B H 0.360020 0.934987 0.228222 0.222 Uiso 1 1 calc R U . . .
C12 C 0.2886(5) 0.8181(9) 0.3033(7) 0.175(4) Uani 1 1 d . . . . .
H12A H 0.246714 0.814701 0.221014 0.210 Uiso 1 1 calc R U . . .
H12B H 0.327661 0.756349 0.302596 0.210 Uiso 1 1 calc R U . . .
C13 C 0.1915(4) 0.9057(6) 0.4334(6) 0.118(2) Uani 1 1 d . . . . .
H13A H 0.166112 0.897694 0.513471 0.142 Uiso 1 1 calc R U . . .
H13B H 0.146129 0.906971 0.355593 0.142 Uiso 1 1 calc R U . . .
C14 C 0.2460(5) 0.8086(7) 0.4229(7) 0.133(2) Uani 1 1 d . . . . .
H14A H 0.212122 0.740954 0.415288 0.160 Uiso 1 1 calc R U . . .
H14B H 0.288481 0.802958 0.504237 0.160 Uiso 1 1 calc R U . . .
C15 C 0.2989(4) 1.0223(5) 0.5706(5) 0.0986(17) Uani 1 1 d . . . . .
H15A H 0.268131 1.009740 0.643968 0.118 Uiso 1 1 calc R U . . .
H15B H 0.340044 0.962624 0.573485 0.118 Uiso 1 1 calc R U . . .
C16 C 0.3449(5) 1.1293(7) 0.5952(7) 0.141(3) Uani 1 1 d . . . . .
H16A H 0.387081 1.123265 0.675576 0.212 Uiso 1 1 calc R U . . .
H16B H 0.305863 1.187836 0.606369 0.212 Uiso 1 1 calc R U . . .
H16C H 0.371845 1.146286 0.519682 0.212 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 2.056(3) 2_655 ?
Ni1 N1 2.056(3) 4_566 ?
Ni1 N2 2.053(3) 3_666 ?
Ni1 N2 2.053(3) . ?
Ni1 N3 2.070(4) 3_666 ?
Ni1 N3 2.070(4) . ?
Ni2 N5 2.073(3) 3_566 ?
Ni2 N5 2.073(3) . ?
Ni2 N6 2.072(3) 2_546 ?
Ni2 N6 2.072(3) 4_575 ?
Ni2 N7 2.064(3) 3_566 ?
Ni2 N7 2.064(3) . ?
N1 C3 1.106(5) . ?
N2 C1 1.125(5) . ?
N3 C4 1.130(5) . ?
N4 C4 1.294(6) . ?
N4 C5 1.293(5) . ?
N5 C5 1.128(5) . ?
N6 C7 1.145(5) . ?
N7 C6 1.136(4) . ?
N8 C6 1.294(5) . ?
N8 C7 1.300(5) . ?
N9 C9 1.509(10) . ?
N9 C10 1.521(9) . ?
N9 C13 1.521(7) . ?
N9 C15 1.518(7) . ?
C1 N10 1.303(5) . ?
C3 N10 1.289(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C9 1.487(11) . ?
C9 H9B 0.9900 . ?
C9 H9A 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.479(13) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.529(12) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C14 1.520(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.500(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.507(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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 N1 180.0 4_566 2_655 ?
N1 Ni1 N3 90.15(15) 2_655 3_666 ?
N1 Ni1 N3 89.85(15) 4_566 3_666 ?
N1 Ni1 N3 89.85(15) 2_655 . ?
N1 Ni1 N3 90.15(15) 4_566 . ?
N2 Ni1 N1 91.23(14) . 2_655 ?
N2 Ni1 N1 91.23(14) 3_666 4_566 ?
N2 Ni1 N1 88.77(14) 3_666 2_655 ?
N2 Ni1 N1 88.77(14) . 4_566 ?
N2 Ni1 N2 180.0 . 3_666 ?
N2 Ni1 N3 91.32(16) . 3_666 ?
N2 Ni1 N3 88.68(16) 3_666 3_666 ?
N2 Ni1 N3 88.68(16) . . ?
N2 Ni1 N3 91.32(16) 3_666 . ?
N3 Ni1 N3 180.0(2) 3_666 . ?
N5 Ni2 N5 180.0 . 3_566 ?
N6 Ni2 N5 92.12(14) 2_546 . ?
N6 Ni2 N5 87.88(14) 4_575 . ?
N6 Ni2 N5 87.88(14) 2_546 3_566 ?
N6 Ni2 N5 92.12(14) 4_575 3_566 ?
N6 Ni2 N6 180.0 4_575 2_546 ?
N7 Ni2 N5 90.80(13) . . ?
N7 Ni2 N5 89.20(13) . 3_566 ?
N7 Ni2 N5 89.20(13) 3_566 . ?
N7 Ni2 N5 90.80(13) 3_566 3_566 ?
N7 Ni2 N6 91.11(14) 3_566 4_575 ?
N7 Ni2 N6 91.11(14) . 2_546 ?
N7 Ni2 N6 88.89(14) . 4_575 ?
N7 Ni2 N6 88.89(14) 3_566 2_546 ?
N7 Ni2 N7 180.0 3_566 . ?
C3 N1 Ni1 167.5(4) . 2_645 ?
C1 N2 Ni1 166.7(4) . . ?
C4 N3 Ni1 168.5(4) . . ?
C5 N4 C4 121.1(4) . . ?
C5 N5 Ni2 155.0(4) . . ?
C7 N6 Ni2 155.3(3) . 2_556 ?
C6 N7 Ni2 163.7(3) . . ?
C6 N8 C7 120.0(3) . . ?
C9 N9 C10 107.3(6) . . ?
C9 N9 C13 108.1(6) . . ?
C9 N9 C15 110.6(6) . . ?
C10 N9 C13 107.6(6) . . ?
C15 N9 C10 112.8(5) . . ?
C15 N9 C13 110.3(4) . . ?
N2 C1 N10 173.8(4) . . ?
N1 C3 N10 171.3(5) . . ?
N3 C4 N4 172.3(5) . . ?
N5 C5 N4 172.9(4) . . ?
N7 C6 N8 174.0(4) . . ?
N6 C7 N8 174.2(4) . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
N9 C9 H9B 108.3 . . ?
N9 C9 H9A 108.3 . . ?
C8 C9 N9 115.8(6) . . ?
C8 C9 H9B 108.3 . . ?
C8 C9 H9A 108.3 . . ?
H9B C9 H9A 107.4 . . ?
C3 N10 C1 121.1(4) . . ?
N9 C10 H10A 108.9 . . ?
N9 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 N9 113.3(6) . . ?
C11 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
C10 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
C10 C11 C12 111.3(7) . . ?
H11A C11 H11B 108.0 . . ?
C12 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
C14 C12 C11 109.6(6) . . ?
C14 C12 H12A 109.8 . . ?
C14 C12 H12B 109.8 . . ?
N9 C13 H13A 109.0 . . ?
N9 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 N9 113.0(6) . . ?
C14 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C12 C14 H14A 109.4 . . ?
C12 C14 H14B 109.4 . . ?
C13 C14 C12 111.2(7) . . ?
C13 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
N9 C15 H15A 108.3 . . ?
N9 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
C16 C15 N9 115.9(5) . . ?
C16 C15 H15A 108.3 . . ?
C16 C15 H15B 108.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

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
N9 C10 C11 C12 57.7(8) . . . . ?
N9 C13 C14 C12 -57.1(7) . . . . ?
C9 N9 C10 C11 -172.2(7) . . . . ?
C9 N9 C13 C14 171.1(6) . . . . ?
C9 N9 C15 C16 -56.3(8) . . . . ?
C10 N9 C9 C8 -179.2(7) . . . . ?
C10 N9 C13 C14 55.5(7) . . . . ?
C10 N9 C15 C16 63.9(9) . . . . ?
C10 C11 C12 C14 -55.1(10) . . . . ?
C11 C12 C14 C13 54.7(9) . . . . ?
C13 N9 C9 C8 65.0(8) . . . . ?
C13 N9 C10 C11 -56.1(8) . . . . ?
C13 N9 C15 C16 -175.8(6) . . . . ?
C15 N9 C9 C8 -55.8(8) . . . . ?
C15 N9 C10 C11 65.8(8) . . . . ?
C15 N9 C13 C14 -67.9(7) . . . . ?

_olex2_exptl_crystal_mounting_method 'with a loop in oil'
_olex2_submission_original_sample_id DEPNidca3_300K
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_krosi102_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2309050'
loop_
_audit_author_name
_audit_author_address
'Silva Maria Kronawitter'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2023-11-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_audit_creation_date             2023-08-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        PEPNi_RT
_chemical_formula_moiety         'C6 N9 Ni, C10 H22 N'
_chemical_formula_sum            'C16 H22 N10 Ni'
_chemical_formula_weight         413.14
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   16.4756(7)
_cell_length_b                   11.9516(5)
_cell_length_c                   10.6587(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.9160(10)
_cell_angle_gamma                90
_cell_volume                     2028.08(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9560
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      24.09
_cell_measurement_theta_min      2.56
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.913
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1364 before and 0.0858 after correction.
The Ratio of minimum to maximum transmission is 0.8456.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_preparation       'wet chemistry'
_exptl_crystal_recrystallization_method 'wet chemistry'
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.032
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30600
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.149
_diffrn_reflns_theta_max         24.149
_diffrn_reflns_theta_min         2.131
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_special_details          -
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2108
_reflns_number_total             3184
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0606
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0946P)²+3.4933P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.2082
_refine_special_details          -
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H9C,H9D), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.000000 1.000000 0.500000 0.0408(3) Uani 1 2 d S . P . .
Ni2 Ni 0.500000 1.000000 0.500000 0.0364(3) Uani 1 2 d S . P . .
N1 N 0.1214(3) 1.0551(5) 0.5190(6) 0.0731(14) Uani 1 1 d . . . . .
N2 N 0.3718(3) 1.0263(4) 0.4535(5) 0.0587(12) Uani 1 1 d . . . . .
N3 N 0.4819(3) 0.8369(4) 0.4356(4) 0.0549(11) Uani 1 1 d . . . . .
N4 N 0.4659(4) 0.6404(4) 0.3733(5) 0.0832(19) Uani 1 1 d . . . . .
N5 N 0.4960(3) 0.5544(4) 0.1830(4) 0.0548(11) Uani 1 1 d . . . . .
N6 N 0.0436(3) 0.8524(4) 0.5898(5) 0.0672(14) Uani 1 1 d . . . . .
N7 N 0.0638(4) 0.6583(4) 0.6626(6) 0.0849(18) Uani 1 1 d . . . . .
N8 N 0.0048(3) 0.5700(4) 0.8242(5) 0.0706(14) Uani 1 1 d . . . . .
N9 N 0.7582(5) 0.4986(5) 0.5278(7) 0.101(3) Uani 1 1 d . . . . .
C1 C 0.1771(4) 1.0773(5) 0.4806(6) 0.0651(16) Uani 1 1 d . . . . .
C3 C 0.3080(4) 1.0625(5) 0.4474(5) 0.0554(14) Uani 1 1 d . . . . .
C4 C 0.4766(3) 0.7463(4) 0.4006(5) 0.0487(12) Uani 1 1 d . . . . .
C5 C 0.4835(3) 0.6009(4) 0.2699(5) 0.0463(12) Uani 1 1 d . . . . .
C6 C 0.0504(3) 0.7623(5) 0.6283(5) 0.0564(14) Uani 1 1 d . . . . .
C7 C 0.0310(4) 0.6173(4) 0.7490(5) 0.0568(14) Uani 1 1 d . . . . .
C8 C 0.6404(7) 0.6775(9) 0.7198(10) 0.137(4) Uani 1 1 d . . . . .
H8A H 0.625787 0.737848 0.658695 0.205 Uiso 1 1 calc R U . . .
H8B H 0.669742 0.706590 0.803043 0.205 Uiso 1 1 calc R U . . .
H8C H 0.590215 0.640131 0.727026 0.205 Uiso 1 1 calc R U . . .
C9 C 0.6929(14) 0.6003(11) 0.6762(16) 0.259(11) Uani 1 1 d . . . . .
H9A H 0.747706 0.622616 0.728765 0.311 Uiso 1 1 calc R U . . .
H9B H 0.680382 0.531832 0.716372 0.311 Uiso 1 1 calc R U . . .
N10 N 0.2365(3) 1.1148(6) 0.4326(8) 0.114(3) Uani 1 1 d . . . . .
C10 C 0.7095(13) 0.5668(11) 0.5904(18) 0.243(10) Uani 1 1 d . . . . .
H9C H 0.715718 0.637255 0.548666 0.292 Uiso 1 1 calc R U . . .
H9D H 0.654209 0.540819 0.543496 0.292 Uiso 1 1 calc R U . . .
C11 C 0.7746(13) 0.3914(13) 0.6132(12) 0.297(15) Uani 1 1 d . . . . .
H11A H 0.828331 0.402154 0.675837 0.357 Uiso 1 1 calc R U . . .
H11B H 0.732468 0.390309 0.662050 0.357 Uiso 1 1 calc R U . . .
C12 C 0.7761(8) 0.2922(10) 0.5663(11) 0.137(4) Uani 1 1 d . . . . .
H12A H 0.764649 0.239220 0.628464 0.164 Uiso 1 1 calc R U . . .
H12B H 0.832758 0.277700 0.559339 0.164 Uiso 1 1 calc R U . . .
C13 C 0.7183(7) 0.2689(9) 0.4403(12) 0.132(4) Uani 1 1 d . . . . .
H13A H 0.745601 0.218630 0.392431 0.158 Uiso 1 1 calc R U . . .
H13B H 0.669430 0.230677 0.454082 0.158 Uiso 1 1 calc R U . . .
C14 C 0.7019(10) 0.4681(13) 0.4020(12) 0.184(6) Uani 1 1 d . . . . .
H14A H 0.646856 0.497368 0.401184 0.220 Uiso 1 1 calc R U . . .
H14B H 0.720918 0.508994 0.336327 0.220 Uiso 1 1 calc R U . . .
C15 C 0.6911(12) 0.3663(13) 0.3631(12) 0.239(10) Uani 1 1 d . . . . .
H15A H 0.715917 0.360843 0.290068 0.287 Uiso 1 1 calc R U . . .
H15B H 0.631052 0.357451 0.327713 0.287 Uiso 1 1 calc R U . . .
C16 C 0.8347(8) 0.548(2) 0.5154(13) 0.298(16) Uani 1 1 d . . . . .
H16A H 0.855481 0.589183 0.595701 0.357 Uiso 1 1 calc R U . . .
H16B H 0.872696 0.485220 0.520325 0.357 Uiso 1 1 calc R U . . .
C17 C 0.8518(14) 0.6154(10) 0.4231(16) 0.243(10) Uani 1 1 d . . . . .
H17A H 0.901700 0.589481 0.401522 0.364 Uiso 1 1 calc R U . . .
H17B H 0.860326 0.690569 0.455521 0.364 Uiso 1 1 calc R U . . .
H17C H 0.805550 0.613772 0.346991 0.364 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 2.065(5) . ?
Ni1 N1 2.065(5) 3_576 ?
Ni1 N6 2.046(5) 3_576 ?
Ni1 N6 2.046(5) . ?
Ni1 N8 2.072(5) 2_556 ?
Ni1 N8 2.072(5) 4_575 ?
Ni2 N2 2.066(5) 3_676 ?
Ni2 N2 2.066(5) . ?
Ni2 N3 2.063(4) 3_676 ?
Ni2 N3 2.063(4) . ?
Ni2 N5 2.072(4) 2_655 ?
Ni2 N5 2.072(4) 4_576 ?
N1 C1 1.129(7) . ?
N2 C3 1.122(7) . ?
N3 C4 1.142(6) . ?
N4 C4 1.300(7) . ?
N4 C5 1.298(7) . ?
N5 C5 1.144(6) . ?
N6 C6 1.148(7) . ?
N7 C6 1.299(8) . ?
N7 C7 1.279(7) . ?
N8 C7 1.151(7) . ?
N9 C10 1.424(12) . ?
N9 C11 1.555(16) . ?
N9 C14 1.467(12) . ?
N9 C16 1.429(16) . ?
C1 N10 1.296(8) . ?
C3 N10 1.307(8) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 C9 1.422(15) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.096(14) . ?
C10 H9C 0.9700 . ?
C10 H9D 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.289(14) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.459(16) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C15 1.430(15) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.282(16) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.36(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0 3_576 . ?
N1 Ni1 N8 87.5(2) 3_576 2_556 ?
N1 Ni1 N8 92.5(2) . 2_556 ?
N1 Ni1 N8 87.5(2) . 4_575 ?
N1 Ni1 N8 92.5(2) 3_576 4_575 ?
N6 Ni1 N1 89.2(2) 3_576 . ?
N6 Ni1 N1 89.2(2) . 3_576 ?
N6 Ni1 N1 90.8(2) 3_576 3_576 ?
N6 Ni1 N1 90.8(2) . . ?
N6 Ni1 N6 180.0 . 3_576 ?
N6 Ni1 N8 89.1(2) . 4_575 ?
N6 Ni1 N8 90.9(2) . 2_556 ?
N6 Ni1 N8 90.9(2) 3_576 4_575 ?
N6 Ni1 N8 89.1(2) 3_576 2_556 ?
N8 Ni1 N8 180.0 4_575 2_556 ?
N2 Ni2 N2 180.0 3_676 . ?
N2 Ni2 N5 90.25(18) . 2_655 ?
N2 Ni2 N5 89.75(18) . 4_576 ?
N2 Ni2 N5 89.75(18) 3_676 2_655 ?
N2 Ni2 N5 90.25(18) 3_676 4_576 ?
N3 Ni2 N2 89.27(19) . 3_676 ?
N3 Ni2 N2 90.73(19) 3_676 3_676 ?
N3 Ni2 N2 90.73(19) . . ?
N3 Ni2 N2 89.26(19) 3_676 . ?
N3 Ni2 N3 180.0 3_676 . ?
N3 Ni2 N5 91.16(17) 3_676 4_576 ?
N3 Ni2 N5 88.84(17) 3_676 2_655 ?
N3 Ni2 N5 88.83(17) . 4_576 ?
N3 Ni2 N5 91.17(17) . 2_655 ?
N5 Ni2 N5 180.0 4_576 2_655 ?
C1 N1 Ni1 153.7(6) . . ?
C3 N2 Ni2 163.1(5) . . ?
C4 N3 Ni2 176.1(5) . . ?
C5 N4 C4 119.8(5) . . ?
C5 N5 Ni2 166.1(5) . 2_645 ?
C6 N6 Ni1 165.1(5) . . ?
C7 N7 C6 119.8(5) . . ?
C7 N8 Ni1 159.3(5) . 2_546 ?
C10 N9 C11 103.4(10) . . ?
C10 N9 C14 105.7(13) . . ?
C10 N9 C16 115.1(13) . . ?
C14 N9 C11 107.7(9) . . ?
C16 N9 C11 111.7(13) . . ?
C16 N9 C14 112.6(11) . . ?
N1 C1 N10 172.8(7) . . ?
N2 C3 N10 173.1(6) . . ?
N3 C4 N4 172.3(5) . . ?
N5 C5 N4 172.1(5) . . ?
N6 C6 N7 173.2(6) . . ?
N8 C7 N7 173.0(6) . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
C8 C9 H9A 100.8 . . ?
C8 C9 H9B 100.8 . . ?
H9A C9 H9B 104.4 . . ?
C10 C9 C8 144(2) . . ?
C10 C9 H9A 100.8 . . ?
C10 C9 H9B 100.8 . . ?
C1 N10 C3 122.5(6) . . ?
N9 C10 H9C 98.3 . . ?
N9 C10 H9D 98.3 . . ?
C9 C10 N9 153(2) . . ?
C9 C10 H9C 98.3 . . ?
C9 C10 H9D 98.3 . . ?
H9C C10 H9D 103.8 . . ?
N9 C11 H11A 106.5 . . ?
N9 C11 H11B 106.5 . . ?
H11A C11 H11B 106.5 . . ?
C12 C11 N9 123.3(11) . . ?
C12 C11 H11A 106.5 . . ?
C12 C11 H11B 106.5 . . ?
C11 C12 H12A 108.0 . . ?
C11 C12 H12B 108.0 . . ?
C11 C12 C13 117.3(10) . . ?
H12A C12 H12B 107.2 . . ?
C13 C12 H12A 108.0 . . ?
C13 C12 H12B 108.0 . . ?
C12 C13 H13A 108.7 . . ?
C12 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C15 C13 C12 114.1(8) . . ?
C15 C13 H13A 108.7 . . ?
C15 C13 H13B 108.7 . . ?
N9 C14 H14A 106.8 . . ?
N9 C14 H14B 106.8 . . ?
H14A C14 H14B 106.6 . . ?
C15 C14 N9 122.3(10) . . ?
C15 C14 H14A 106.8 . . ?
C15 C14 H14B 106.8 . . ?
C13 C15 H15A 105.8 . . ?
C13 C15 H15B 105.8 . . ?
C14 C15 C13 126.1(11) . . ?
C14 C15 H15A 105.8 . . ?
C14 C15 H15B 105.8 . . ?
H15A C15 H15B 106.2 . . ?
N9 C16 H16A 104.3 . . ?
N9 C16 H16B 104.3 . . ?
H16A C16 H16B 105.6 . . ?
C17 C16 N9 131.8(17) . . ?
C17 C16 H16A 104.3 . . ?
C17 C16 H16B 104.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

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
N9 C11 C12 C13 -35(3) . . . . ?
N9 C14 C15 C13 12(3) . . . . ?
C8 C9 C10 N9 175(2) . . . . ?
C10 N9 C11 C12 143(2) . . . . ?
C10 N9 C14 C15 -128(2) . . . . ?
C10 N9 C16 C17 -87(3) . . . . ?
C11 N9 C10 C9 37(5) . . . . ?
C11 N9 C14 C15 -18(2) . . . . ?
C11 N9 C16 C17 155(2) . . . . ?
C11 C12 C13 C15 23(2) . . . . ?
C12 C13 C15 C14 -12(3) . . . . ?
C14 N9 C10 C9 150(5) . . . . ?
C14 N9 C11 C12 31(2) . . . . ?
C14 N9 C16 C17 34(3) . . . . ?
C16 N9 C10 C9 -85(5) . . . . ?
C16 N9 C11 C12 -93(2) . . . . ?
C16 N9 C14 C15 106(2) . . . . ?

_olex2_exptl_crystal_mounting_method 'with a loop in oil'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_krosi103_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2309039'
loop_
_audit_author_name
_audit_author_address
'Silva Maria Kronawitter'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2023-11-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_audit_creation_date             2023-08-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 N9 Ni, C11 H24 N'
_chemical_formula_sum            'C17 H24 N10 Ni'
_chemical_formula_weight         427.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   16.346(2)
_cell_length_b                   12.0065(16)
_cell_length_c                   11.0462(17)
_cell_angle_alpha                90
_cell_angle_beta                 93.708(6)
_cell_angle_gamma                90
_cell_volume                     2163.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.50
_shelx_estimated_absorpt_T_max   0.905
_shelx_estimated_absorpt_T_min   0.864
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6183
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0815 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.8295.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3.00 1.00 -3.00 0.0490
-1.00 1.00 -3.00 0.0450
2.00 -2.00 -3.00 0.0610
-1.00 -2.00 -2.00 0.0680
3.00 2.00 -2.00 0.0550
0.00 -3.00 -1.00 0.0740
0.00 1.00 0.00 0.0590
0.00 -1.00 0.00 0.0740
0.00 1.00 1.00 0.0370
-2.00 -2.00 1.00 0.0410
1.00 3.00 2.00 0.0520
3.00 -3.00 2.00 0.0550
1.00 -3.00 2.00 0.0570
-1.00 2.00 2.00 0.0320

_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.111
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46500
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.402
_diffrn_reflns_theta_min         2.106
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3440
_reflns_number_total             4227
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.639
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.669
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.1450
_refine_ls_restrained_S_all      2.669
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5296
_refine_ls_wR_factor_ref         0.5445
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C19(H19A,H19B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.500000 0.000000 0.500000 0.0568(8) Uani 1 2 d S . P . .
Ni2 Ni 0.000000 0.000000 0.500000 0.0447(7) Uani 1 2 d S . P . .
N1 N 0.2571(5) 0.4927(6) 0.5140(10) 0.081(3) Uani 1 1 d . . . . .
N2 N 0.3868(3) 0.0773(5) 0.5049(7) 0.0804(18) Uani 1 1 d . . . . .
N3 N 0.1242(4) 0.0319(7) 0.5331(7) 0.0813(17) Uani 1 1 d . . . . .
N4 N -0.0146(4) 0.1561(4) 0.4233(5) 0.0719(15) Uani 1 1 d . . . . .
N5 N -0.0184(4) 0.4335(4) 0.1680(5) 0.0685(15) Uani 1 1 d . . . . .
N6 N 0.5359(4) 0.3929(7) 0.8683(7) 0.089(2) Uani 1 1 d . . . . .
N7 N 0.5477(4) 0.1120(5) 0.6256(7) 0.0852(19) Uani 1 1 d . . . . .
C1 C 0.3784(9) 0.3902(15) 0.6193(16) 0.164(6) Uani 1 1 d . . . . .
H1A H 0.398257 0.464690 0.633071 0.247 Uiso 1 1 calc R U . . .
H1B H 0.423646 0.341750 0.605851 0.247 Uiso 1 1 calc R U . . .
H1C H 0.351369 0.365160 0.688946 0.247 Uiso 1 1 calc R U . . .
N9 N -0.0207(8) 0.3515(5) 0.3680(7) 0.133(4) Uani 1 1 d . . . . .
N8 N 0.6059(4) 0.2697(7) 0.7365(9) 0.114(3) Uani 1 1 d . . . . .
C2 C 0.3178(8) 0.3887(13) 0.5079(14) 0.129(4) Uani 1 1 d . . . . .
H2 H 0.285623 0.319874 0.508772 0.155 Uiso 1 1 calc R U . . .
N10 N 0.2563(4) 0.1151(10) 0.5877(11) 0.136(4) Uani 1 1 d . . . . .
C3 C 0.2036(9) 0.4836(10) 0.3957(12) 0.115(4) Uani 1 1 d . . . . .
H3A H 0.171998 0.415275 0.396474 0.138 Uiso 1 1 calc R U . . .
H3B H 0.238512 0.479830 0.328104 0.138 Uiso 1 1 calc R U . . .
C4 C 0.1442(7) 0.5838(10) 0.3769(10) 0.112(3) Uani 1 1 d . . . . .
H4A H 0.114758 0.577517 0.298067 0.134 Uiso 1 1 calc R U . . .
H4B H 0.104273 0.581676 0.438165 0.134 Uiso 1 1 calc R U . . .
C5 C 0.3024(8) 0.6004(14) 0.5129(17) 0.148(5) Uani 1 1 d . . . . .
H5A H 0.338056 0.600674 0.446063 0.178 Uiso 1 1 calc R U . . .
H5B H 0.336444 0.607965 0.587745 0.178 Uiso 1 1 calc R U . . .
C6 C 0.2421(6) 0.7015(9) 0.4995(11) 0.109(3) Uani 1 1 d . . . . .
H6A H 0.208488 0.704095 0.568705 0.130 Uiso 1 1 calc R U . . .
H6B H 0.273111 0.770337 0.497875 0.130 Uiso 1 1 calc R U . . .
C7 C 0.1993(7) 0.4799(9) 0.6186(11) 0.098(3) Uani 1 1 d . . . . .
H7 H 0.156458 0.536059 0.602364 0.117 Uiso 1 1 calc R U . . .
C8 C 0.2419(9) 0.5142(12) 0.7352(11) 0.130(5) Uani 1 1 d . . . . .
H8A H 0.227941 0.463847 0.798086 0.195 Uiso 1 1 calc R U . . .
H8B H 0.225330 0.588314 0.755134 0.195 Uiso 1 1 calc R U . . .
H8C H 0.300092 0.512685 0.727717 0.195 Uiso 1 1 calc R U . . .
C19 C 0.1880(9) 0.6909(15) 0.3845(15) 0.162(6) Uani 1 1 d . . . . .
H19A H 0.148337 0.751110 0.380585 0.194 Uiso 1 1 calc R U . . .
H19B H 0.221268 0.697979 0.315310 0.194 Uiso 1 1 calc R U . . .
C9 C 0.1549(8) 0.3726(11) 0.6224(15) 0.143(5) Uani 1 1 d . . . . .
H9A H 0.172380 0.324657 0.559462 0.215 Uiso 1 1 calc R U . . .
H9B H 0.097051 0.385774 0.610167 0.215 Uiso 1 1 calc R U . . .
H9C H 0.166588 0.337918 0.699834 0.215 Uiso 1 1 calc R U . . .
C20 C 0.3645(9) 0.3899(14) 0.3979(13) 0.157(6) Uani 1 1 d . . . . .
H20A H 0.363709 0.316867 0.362396 0.236 Uiso 1 1 calc R U . . .
H20B H 0.420140 0.411421 0.419121 0.236 Uiso 1 1 calc R U . . .
H20C H 0.339993 0.442115 0.340595 0.236 Uiso 1 1 calc R U . . .
C10 C 0.3236(4) 0.0890(6) 0.5376(8) 0.077(2) Uani 1 1 d . . . . .
C12 C 0.1869(4) 0.0667(6) 0.5511(7) 0.076(2) Uani 1 1 d . . . . .
C13 C -0.0171(5) 0.2441(5) 0.3905(6) 0.0724(18) Uani 1 1 d . . . . .
C15 C -0.0185(4) 0.3881(5) 0.2579(6) 0.0664(17) Uani 1 1 d . . . . .
C16 C 0.5698(3) 0.1872(6) 0.6808(7) 0.0727(18) Uani 1 1 d . . . . .
C18 C 0.5650(4) 0.3321(6) 0.8043(7) 0.0709(17) 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 2.074(5) . ?
Ni1 N2 2.074(5) 3_656 ?
Ni1 N6 2.056(7) 4_565 ?
Ni1 N6 2.056(7) 2_646 ?
Ni1 N7 2.050(6) 3_656 ?
Ni1 N7 2.050(6) . ?
Ni2 N3 2.075(6) . ?
Ni2 N3 2.075(6) 3_556 ?
Ni2 N4 2.065(5) . ?
Ni2 N4 2.065(5) 3_556 ?
Ni2 N5 2.060(5) 2_545 ?
Ni2 N5 2.060(5) 4_566 ?
N1 C2 1.599(15) . ?
N1 C3 1.529(15) . ?
N1 C5 1.491(17) . ?
N1 C7 1.548(15) . ?
N2 C10 1.125(9) . ?
N3 C12 1.113(8) . ?
N4 C13 1.116(8) . ?
N5 C15 1.132(8) . ?
N6 C18 1.141(9) . ?
N7 C16 1.135(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.53(2) . ?
N9 C13 1.314(8) . ?
N9 C15 1.297(9) . ?
N8 C16 1.289(9) . ?
N8 C18 1.278(9) . ?
C2 H2 0.9800 . ?
C2 C20 1.476(18) . ?
N10 C10 1.300(10) . ?
N10 C12 1.316(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.551(15) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C19 1.47(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.565(19) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C19 1.507(19) . ?
C7 H7 0.9800 . ?
C7 C8 1.482(16) . ?
C7 C9 1.480(16) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N2 180.0 . 3_656 ?
N6 Ni1 N2 92.0(3) 2_646 3_656 ?
N6 Ni1 N2 92.0(3) 4_565 . ?
N6 Ni1 N2 88.0(3) 4_565 3_656 ?
N6 Ni1 N2 88.0(3) 2_646 . ?
N6 Ni1 N6 180.0 4_565 2_646 ?
N7 Ni1 N2 89.4(2) . . ?
N7 Ni1 N2 89.4(2) 3_656 3_656 ?
N7 Ni1 N2 90.6(2) 3_656 . ?
N7 Ni1 N2 90.6(2) . 3_656 ?
N7 Ni1 N6 92.6(3) . 2_646 ?
N7 Ni1 N6 87.4(3) . 4_565 ?
N7 Ni1 N6 92.6(3) 3_656 4_565 ?
N7 Ni1 N6 87.4(3) 3_656 2_646 ?
N7 Ni1 N7 180.0 3_656 . ?
N3 Ni2 N3 180.0 . 3_556 ?
N4 Ni2 N3 89.5(3) 3_556 3_556 ?
N4 Ni2 N3 90.5(3) 3_556 . ?
N4 Ni2 N3 89.5(3) . . ?
N4 Ni2 N3 90.5(3) . 3_556 ?
N4 Ni2 N4 180.0 3_556 . ?
N5 Ni2 N3 91.8(3) 2_545 . ?
N5 Ni2 N3 88.2(3) 2_545 3_556 ?
N5 Ni2 N3 88.2(3) 4_566 . ?
N5 Ni2 N3 91.8(3) 4_566 3_556 ?
N5 Ni2 N4 90.1(2) 2_545 . ?
N5 Ni2 N4 89.9(2) 2_545 3_556 ?
N5 Ni2 N4 90.1(2) 4_566 3_556 ?
N5 Ni2 N4 89.9(2) 4_566 . ?
N5 Ni2 N5 180.0 4_566 2_545 ?
C3 N1 C2 103.3(9) . . ?
C3 N1 C7 106.7(9) . . ?
C5 N1 C2 111.6(11) . . ?
C5 N1 C3 108.2(11) . . ?
C5 N1 C7 114.8(9) . . ?
C7 N1 C2 111.4(9) . . ?
C10 N2 Ni1 154.6(7) . . ?
C12 N3 Ni2 168.6(7) . . ?
C13 N4 Ni2 173.2(6) . . ?
C15 N5 Ni2 169.9(6) . 2 ?
C18 N6 Ni1 171.2(7) . 2_656 ?
C16 N7 Ni1 168.3(7) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C15 N9 C13 120.4(6) . . ?
C18 N8 C16 119.2(6) . . ?
N1 C2 H2 108.8 . . ?
C1 C2 N1 109.1(12) . . ?
C1 C2 H2 108.8 . . ?
C20 C2 N1 112.5(11) . . ?
C20 C2 C1 108.7(13) . . ?
C20 C2 H2 108.8 . . ?
C10 N10 C12 120.0(7) . . ?
N1 C3 H3A 109.2 . . ?
N1 C3 H3B 109.2 . . ?
N1 C3 C4 112.2(9) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C19 C4 C3 111.8(10) . . ?
C19 C4 H4A 109.3 . . ?
C19 C4 H4B 109.3 . . ?
N1 C5 H5A 109.4 . . ?
N1 C5 H5B 109.4 . . ?
N1 C5 C6 111.3(10) . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C19 C6 C5 110.2(12) . . ?
C19 C6 H6A 109.6 . . ?
C19 C6 H6B 109.6 . . ?
N1 C7 H7 105.0 . . ?
C8 C7 N1 110.2(10) . . ?
C8 C7 H7 105.0 . . ?
C9 C7 N1 115.5(10) . . ?
C9 C7 H7 105.0 . . ?
C9 C7 C8 114.9(12) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C19 C6 112.3(10) . . ?
C4 C19 H19A 109.1 . . ?
C4 C19 H19B 109.1 . . ?
C6 C19 H19A 109.1 . . ?
C6 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C20 H20A 109.5 . . ?
C2 C20 H20B 109.5 . . ?
C2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C10 N10 170.3(7) . . ?
N3 C12 N10 170.9(8) . . ?
N4 C13 N9 171.9(7) . . ?
N5 C15 N9 170.9(7) . . ?
N7 C16 N8 170.9(7) . . ?
N6 C18 N8 172.9(7) . . ?

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
N1 C3 C4 C19 54.4(15) . . . . ?
N1 C5 C6 C19 -58.4(15) . . . . ?
C2 N1 C3 C4 -174.9(11) . . . . ?
C2 N1 C5 C6 171.6(10) . . . . ?
C2 N1 C7 C8 81.4(12) . . . . ?
C2 N1 C7 C9 -50.9(15) . . . . ?
C3 N1 C2 C1 177.4(13) . . . . ?
C3 N1 C2 C20 56.7(15) . . . . ?
C3 N1 C5 C6 58.6(14) . . . . ?
C3 N1 C7 C8 -166.5(9) . . . . ?
C3 N1 C7 C9 61.2(13) . . . . ?
C3 C4 C19 C6 -53.0(15) . . . . ?
C5 N1 C2 C1 61.4(17) . . . . ?
C5 N1 C2 C20 -59.3(19) . . . . ?
C5 N1 C3 C4 -56.5(13) . . . . ?
C5 N1 C7 C8 -46.6(15) . . . . ?
C5 N1 C7 C9 -179.0(12) . . . . ?
C5 C6 C19 C4 54.6(14) . . . . ?
C7 N1 C2 C1 -68.4(15) . . . . ?
C7 N1 C2 C20 170.9(13) . . . . ?
C7 N1 C3 C4 67.5(12) . . . . ?
C7 N1 C5 C6 -60.5(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_krosi50_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2309049'
loop_
_audit_author_name
_audit_author_address
'Silva Maria Kronawitter'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2023-11-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_audit_creation_date             2021-12-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        PEPNidca3
_chemical_formula_moiety         'C6 N9 Ni, C10 H22 N'
_chemical_formula_sum            'C16 H22 N10 Ni'
_chemical_formula_weight         413.14
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   16.3743(14)
_cell_length_b                   11.9171(9)
_cell_length_c                   10.4761(8)
_cell_angle_alpha                90
_cell_angle_beta                 105.903(4)
_cell_angle_gamma                90
_cell_volume                     1966.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4697
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      2.59
_shelx_estimated_absorpt_T_max   0.893
_shelx_estimated_absorpt_T_min   0.848
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1003 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8665.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_preparation       'wet chemistry'
_exptl_crystal_recrystallization_method 'wet chemistry'
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.115
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32134
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.591
_diffrn_reflns_theta_min         2.143
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3384
_reflns_number_total             6028
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         6028
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0685
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0656P)²+5.9281P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1920
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004 within 2A
C12 \\sim C13 \\sim C14: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
C12A \\sim C13A \\sim C14A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11)
Uanis(C7A) = Uanis(C8A) = Uanis(C9A) = Uanis(C10A) = Uanis(C11A)
Uanis(C12) = Uanis(C13) = Uanis(C14)
Uanis(C12A) = Uanis(C13A) = Uanis(C14A)
Uanis(C7A) = Uanis(C7)
Uanis(C7A) = Uanis(C7) = Uanis(C11A) = Uanis(C11)
Uanis(C15A) = Uanis(C15)
Uanis(C12A) = Uanis(C13A) = Uanis(C14A)
Uanis(C12A) = Uanis(C12) = Uanis(C13A) = Uanis(C13) = Uanis(C14A) = Uanis(C14)
Uanis(C16) = Uanis(C16A)
Uanis(C15) = Uanis(C16)
Uanis(C16) = Uanis(C15A)
3. Rigid body (RIGU) restrains
 C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C7A, C8A, C9A, C10A, C11A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C12, C13, C14
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C12A, C13A, C14A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5)
 H9A(0.5) H9B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5)
 C7A(0.5) H7AA(0.5) H7AB(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) C9A(0.5) H9AA(0.5)
 H9AB(0.5) C10A(0.5) H10C(0.5) H10D(0.5) C11A(0.5) H11C(0.5) H11D(0.5) C12(0.5)
 H12A(0.5) H12B(0.5) C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5)
 H14C(0.5) C12A(0.5) H12C(0.5) H12D(0.5) C13A(0.5) H13C(0.5) H13D(0.5)
 C14A(0.5) H14D(0.5) H14E(0.5) H14F(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16A(0.5)
 H16A(0.5) H16B(0.5) H16C(0.5) C15A(0.5) H15C(0.5) H15D(0.5) C16(0.5) H16D(0.5)
 H16E(0.5) H16F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C7A(H7AA,H7AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10C,H10D), C11A(H11C,
 H11D), C12(H12A,H12B), C13(H13A,H13B), C12A(H12C,H12D), C13A(H13C,H13D),
 C15(H15A,H15B), C15A(H15C,H15D)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C16A(H16A,H16B,H16C), C16(H16D,
 H16E,H16F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.500000 0.500000 0.500000 0.01603(16) Uani 1 2 d S . P . .
Ni2 Ni 1.000000 0.500000 0.500000 0.01864(17) Uani 1 2 d S . P . .
N1 N 0.4823(2) 0.6659(3) 0.4414(3) 0.0226(7) Uani 1 1 d . . . . .
N2 N 0.4666(4) 0.8658(3) 0.3824(4) 0.0504(14) Uani 1 1 d . . . . .
N3 N 0.4980(2) 0.9518(3) 0.1888(3) 0.0209(7) Uani 1 1 d . . . . .
N4 N 0.6299(2) 0.5263(3) 0.5493(3) 0.0238(7) Uani 1 1 d . . . . .
N5 N 0.7672(3) 0.6173(3) 0.5775(5) 0.0407(10) Uani 1 1 d . . . . .
N6 N 0.8786(2) 0.5655(3) 0.4723(4) 0.0297(8) Uani 1 1 d . . . . .
N7 N 0.9897(2) 0.0665(3) 0.1769(4) 0.0299(8) Uani 1 1 d . . . . .
N8 N 0.9498(2) 0.3533(3) 0.4064(3) 0.0273(8) Uani 1 1 d . . . . .
N9 N 0.9242(3) 0.1575(3) 0.3354(4) 0.0347(9) Uani 1 1 d . . . . .
N10 N 0.7606(3) 0.9999(4) 0.5452(5) 0.0581(15) Uani 1 1 d . . . . .
C1 C 0.4765(3) 0.7577(3) 0.4088(4) 0.0260(9) Uani 1 1 d . . . . .
C2 C 0.4837(3) 0.9064(3) 0.2768(4) 0.0225(8) Uani 1 1 d . . . . .
C3 C 0.6948(3) 0.5645(3) 0.5576(4) 0.0213(8) Uani 1 1 d . . . . .
C4 C 0.8243(3) 0.5845(3) 0.5186(5) 0.0278(9) Uani 1 1 d . . . . .
C5 C 0.9413(3) 0.2625(4) 0.3698(4) 0.0244(8) Uani 1 1 d . . . . .
C6 C 0.9606(3) 0.1129(3) 0.2502(4) 0.0257(8) Uani 1 1 d . . . . .
C7 C 0.7528(7) 1.1173(9) 0.6318(9) 0.0374(4) Uani 0.5 1 d . U P A 1
H7A H 0.697316 1.118066 0.652480 0.045 Uiso 0.5 1 calc R U P A 1
H7B H 0.798096 1.117212 0.716769 0.045 Uiso 0.5 1 calc R U P A 1
C8 C 0.7610(7) 1.2220(10) 0.5529(10) 0.0374(4) Uani 0.5 1 d . U P A 1
H8A H 0.749529 1.288410 0.602130 0.045 Uiso 0.5 1 calc R U P A 1
H8B H 0.820427 1.227614 0.548400 0.045 Uiso 0.5 1 calc R U P A 1
C9 C 0.7167(8) 1.2258(12) 0.4460(10) 0.0374(4) Uani 0.5 1 d . U P A 1
H9A H 0.737239 1.288725 0.401335 0.045 Uiso 0.5 1 calc R U P A 1
H9B H 0.660009 1.248160 0.453834 0.045 Uiso 0.5 1 calc R U P A 1
C10 C 0.7015(7) 1.1223(9) 0.3451(9) 0.0374(4) Uani 0.5 1 d . U P A 1
H10A H 0.651323 1.135610 0.268803 0.045 Uiso 0.5 1 calc R U P A 1
H10B H 0.751746 1.110289 0.311395 0.045 Uiso 0.5 1 calc R U P A 1
C11 C 0.6866(7) 1.0176(9) 0.4287(10) 0.0374(4) Uani 0.5 1 d . U P A 1
H11A H 0.635067 1.029989 0.458891 0.045 Uiso 0.5 1 calc R U P A 1
H11B H 0.677363 0.949712 0.372020 0.045 Uiso 0.5 1 calc R U P A 1
C7A C 0.8247(6) 1.0820(9) 0.5821(9) 0.0374(4) Uani 0.5 1 d . U P A 2
H7AA H 0.860528 1.081283 0.519737 0.045 Uiso 0.5 1 calc R U P A 2
H7AB H 0.861381 1.066623 0.672544 0.045 Uiso 0.5 1 calc R U P A 2
C8A C 0.7801(7) 1.1996(10) 0.5782(10) 0.0374(4) Uani 0.5 1 d . U P A 2
H8AA H 0.823105 1.259924 0.590367 0.045 Uiso 0.5 1 calc R U P A 2
H8AB H 0.753118 1.204413 0.651782 0.045 Uiso 0.5 1 calc R U P A 2
C9A C 0.6989(8) 1.2194(12) 0.4185(10) 0.0374(4) Uani 0.5 1 d . U P A 2
H9AA H 0.653775 1.271122 0.428435 0.045 Uiso 0.5 1 calc R U P A 2
H9AB H 0.724577 1.249690 0.350392 0.045 Uiso 0.5 1 calc R U P A 2
C10A C 0.6663(7) 1.1107(9) 0.3842(9) 0.0374(4) Uani 0.5 1 d . U P A 2
H10C H 0.625502 1.097406 0.436968 0.045 Uiso 0.5 1 calc R U P A 2
H10D H 0.632111 1.115550 0.290432 0.045 Uiso 0.5 1 calc R U P A 2
C11A C 0.7136(7) 1.0120(9) 0.3937(9) 0.0374(4) Uani 0.5 1 d . U P A 2
H11C H 0.755004 1.017575 0.340486 0.045 Uiso 0.5 1 calc R U P A 2
H11D H 0.676035 0.946816 0.361980 0.045 Uiso 0.5 1 calc R U P A 2
C12 C 0.7420(8) 0.9012(9) 0.6359(11) 0.0417(6) Uani 0.5 1 d . U P A 3
H12A H 0.733290 0.831648 0.582142 0.050 Uiso 0.5 1 calc R U P A 3
H12B H 0.793971 0.890156 0.709762 0.050 Uiso 0.5 1 calc R U P A 3
C13 C 0.6696(7) 0.9118(8) 0.6946(11) 0.0417(6) Uani 0.5 1 d . U P A 3
H13A H 0.618765 0.937878 0.625809 0.050 Uiso 0.5 1 calc R U P A 3
H13B H 0.683329 0.968461 0.766450 0.050 Uiso 0.5 1 calc R U P A 3
C14 C 0.6507(9) 0.8014(10) 0.7496(12) 0.0417(6) Uani 0.5 1 d . U P A 3
H14A H 0.632162 0.747127 0.677070 0.062 Uiso 0.5 1 calc R U P A 3
H14B H 0.605661 0.811514 0.793720 0.062 Uiso 0.5 1 calc R U P A 3
H14C H 0.702071 0.773373 0.813786 0.062 Uiso 0.5 1 calc R U P A 3
C12A C 0.7257(8) 0.9493(9) 0.6303(11) 0.0417(6) Uani 0.5 1 d . U P A 4
H12C H 0.707628 1.009059 0.682303 0.050 Uiso 0.5 1 calc R U P A 4
H12D H 0.771479 0.906878 0.693068 0.050 Uiso 0.5 1 calc R U P A 4
C13A C 0.6548(7) 0.8737(9) 0.5859(10) 0.0417(6) Uani 0.5 1 d . U P A 4
H13C H 0.669189 0.812861 0.531440 0.050 Uiso 0.5 1 calc R U P A 4
H13D H 0.604683 0.914545 0.531311 0.050 Uiso 0.5 1 calc R U P A 4
C14A C 0.6349(9) 0.8227(10) 0.7157(11) 0.0417(6) Uani 0.5 1 d . U P A 4
H14D H 0.688142 0.800405 0.779724 0.062 Uiso 0.5 1 calc R U P A 4
H14E H 0.597927 0.757011 0.691001 0.062 Uiso 0.5 1 calc R U P A 4
H14F H 0.606373 0.879543 0.755823 0.062 Uiso 0.5 1 calc R U P A 4
C15 C 0.8275(7) 0.8829(10) 0.5228(11) 0.0439(13) Uani 0.5 1 d . . P A 5
H15A H 0.866223 0.866153 0.611307 0.053 Uiso 0.5 1 calc R U P A 5
H15B H 0.789659 0.817086 0.497317 0.053 Uiso 0.5 1 calc R U P A 5
C16A C 0.8791(8) 0.8870(11) 0.4318(13) 0.0439(13) Uani 0.5 1 d . . P A 5
H16A H 0.842483 0.894046 0.340854 0.066 Uiso 0.5 1 calc R U P A 5
H16B H 0.912631 0.817971 0.439656 0.066 Uiso 0.5 1 calc R U P A 5
H16C H 0.917317 0.951764 0.452723 0.066 Uiso 0.5 1 calc R U P A 5
C15A C 0.8431(7) 0.9920(9) 0.5348(11) 0.0439(13) Uani 0.5 1 d . . P A 6
H15C H 0.883382 0.989425 0.624547 0.053 Uiso 0.5 1 calc R U P A 6
H15D H 0.856588 1.058930 0.488362 0.053 Uiso 0.5 1 calc R U P A 6
C16 C 0.8527(8) 0.8890(11) 0.4600(13) 0.0439(13) Uani 0.5 1 d . . P A 6
H16D H 0.804626 0.882840 0.380462 0.066 Uiso 0.5 1 calc R U P A 6
H16E H 0.854239 0.823018 0.516353 0.066 Uiso 0.5 1 calc R U P A 6
H16F H 0.905717 0.893376 0.433795 0.066 Uiso 0.5 1 calc R U P A 6


_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 2.067(3) . ?
Ni1 N1 2.067(3) 3_666 ?
Ni1 N3 2.069(3) 2_645 ?
Ni1 N3 2.069(3) 4_576 ?
Ni1 N4 2.070(4) . ?
Ni1 N4 2.070(4) 3_666 ?
Ni2 N6 2.081(3) . ?
Ni2 N6 2.081(3) 3_766 ?
Ni2 N7 2.065(3) 2_755 ?
Ni2 N7 2.065(3) 4_566 ?
Ni2 N8 2.061(3) 3_766 ?
Ni2 N8 2.061(3) . ?
N1 C1 1.142(5) . ?
N2 C1 1.318(5) . ?
N2 C2 1.306(5) . ?
N3 C2 1.147(5) . ?
N4 C3 1.138(5) . ?
N5 C3 1.308(5) . ?
N5 C4 1.313(6) . ?
N6 C4 1.145(5) . ?
N7 C6 1.150(5) . ?
N8 C5 1.144(5) . ?
N9 C5 1.310(5) . ?
N9 C6 1.314(5) . ?
N10 C7 1.691(11) . ?
N10 C11 1.481(11) . ?
N10 C7A 1.410(10) . ?
N10 C11A 1.569(11) . ?
N10 C12 1.593(11) . ?
N10 C12A 1.328(11) . ?
N10 C15 1.828(12) . ?
N10 C15A 1.389(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.523(15) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.157(14) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.599(15) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.581(15) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C7A C8A 1.576(15) . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C8A C9A 1.845(14) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
C9A C10A 1.409(16) . ?
C10A H10C 0.9900 . ?
C10A H10D 0.9900 . ?
C10A C11A 1.398(15) . ?
C11A H11C 0.9900 . ?
C11A H11D 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.483(14) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.503(15) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C12A C13A 1.442(15) . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C13A C14A 1.603(14) . ?
C14A H14D 0.9800 . ?
C14A H14E 0.9800 . ?
C14A H14F 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16A 1.438(13) . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C15A C16 1.487(17) . ?
C16 H16D 0.9800 . ?
C16 H16E 0.9800 . ?
C16 H16F 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 N1 180.00(5) . 3_666 ?
N1 Ni1 N3 88.89(12) 3_666 2_645 ?
N1 Ni1 N3 88.89(12) . 4_576 ?
N1 Ni1 N3 91.11(12) 3_666 4_576 ?
N1 Ni1 N3 91.11(12) . 2_645 ?
N1 Ni1 N4 91.15(14) 3_666 . ?
N1 Ni1 N4 91.14(14) . 3_666 ?
N1 Ni1 N4 88.86(14) . . ?
N1 Ni1 N4 88.85(14) 3_666 3_666 ?
N3 Ni1 N3 180.0 4_576 2_645 ?
N3 Ni1 N4 90.24(13) 4_576 . ?
N3 Ni1 N4 89.76(13) 4_576 3_666 ?
N3 Ni1 N4 89.76(13) 2_645 . ?
N3 Ni1 N4 90.24(13) 2_645 3_666 ?
N4 Ni1 N4 180.0 . 3_666 ?
N6 Ni2 N6 180.00(18) 3_766 . ?
N7 Ni2 N6 87.66(15) 2_755 3_766 ?
N7 Ni2 N6 92.34(15) 4_566 3_766 ?
N7 Ni2 N6 87.66(15) 4_566 . ?
N7 Ni2 N6 92.34(15) 2_755 . ?
N7 Ni2 N7 180.0 4_566 2_755 ?
N8 Ni2 N6 90.62(15) 3_766 3_766 ?
N8 Ni2 N6 89.38(15) . 3_766 ?
N8 Ni2 N6 90.62(15) . . ?
N8 Ni2 N6 89.38(15) 3_766 . ?
N8 Ni2 N7 91.07(14) . 2_755 ?
N8 Ni2 N7 88.93(14) . 4_566 ?
N8 Ni2 N7 88.93(14) 3_766 2_755 ?
N8 Ni2 N7 91.07(14) 3_766 4_566 ?
N8 Ni2 N8 180.0 3_766 . ?
C1 N1 Ni1 176.7(3) . . ?
C2 N2 C1 119.8(4) . . ?
C2 N3 Ni1 163.7(3) . 2_655 ?
C3 N4 Ni1 162.6(3) . . ?
C3 N5 C4 120.9(4) . . ?
C4 N6 Ni2 146.9(4) . . ?
C6 N7 Ni2 159.2(4) . 2_745 ?
C5 N8 Ni2 163.3(4) . . ?
C5 N9 C6 118.1(4) . . ?
C11 N10 C7 99.2(6) . . ?
C7A N10 C11A 109.6(6) . . ?
N1 C1 N2 173.7(4) . . ?
N3 C2 N2 173.6(4) . . ?
N4 C3 N5 172.8(4) . . ?
N6 C4 N5 173.1(5) . . ?
N8 C5 N9 173.0(4) . . ?
N7 C6 N9 175.0(5) . . ?
N10 C7 H7A 109.5 . . ?
N10 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 N10 110.8(7) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C7 C8 H8A 108.4 . . ?
C7 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
C9 C8 C7 115.7(12) . . ?
C9 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
C8 C9 H9A 106.5 . . ?
C8 C9 H9B 106.5 . . ?
C8 C9 C10 123.5(13) . . ?
H9A C9 H9B 106.5 . . ?
C10 C9 H9A 106.5 . . ?
C10 C9 H9B 106.5 . . ?
C9 C10 H10A 110.7 . . ?
C9 C10 H10B 110.7 . . ?
H10A C10 H10B 108.8 . . ?
C11 C10 C9 105.2(8) . . ?
C11 C10 H10A 110.7 . . ?
C11 C10 H10B 110.7 . . ?
N10 C11 C10 110.7(8) . . ?
N10 C11 H11A 109.5 . . ?
N10 C11 H11B 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
N10 C7A H7AA 110.2 . . ?
N10 C7A H7AB 110.2 . . ?
N10 C7A C8A 107.7(8) . . ?
H7AA C7A H7AB 108.5 . . ?
C8A C7A H7AA 110.2 . . ?
C8A C7A H7AB 110.2 . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
C7A C8A C9A 110.6(8) . . ?
H8AA C8A H8AB 108.1 . . ?
C9A C8A H8AA 109.5 . . ?
C9A C8A H8AB 109.5 . . ?
C8A C9A H9AA 111.0 . . ?
C8A C9A H9AB 111.0 . . ?
H9AA C9A H9AB 109.0 . . ?
C10A C9A C8A 104.0(10) . . ?
C10A C9A H9AA 111.0 . . ?
C10A C9A H9AB 111.0 . . ?
C9A C10A H10C 105.7 . . ?
C9A C10A H10D 105.7 . . ?
H10C C10A H10D 106.2 . . ?
C11A C10A C9A 126.3(10) . . ?
C11A C10A H10C 105.7 . . ?
C11A C10A H10D 105.7 . . ?
N10 C11A H11C 110.8 . . ?
N10 C11A H11D 110.8 . . ?
C10A C11A N10 104.9(8) . . ?
C10A C11A H11C 110.8 . . ?
C10A C11A H11D 110.8 . . ?
H11C C11A H11D 108.8 . . ?
N10 C12 H12A 107.5 . . ?
N10 C12 H12B 107.5 . . ?
H12A C12 H12B 107.0 . . ?
C13 C12 N10 119.3(9) . . ?
C13 C12 H12A 107.5 . . ?
C13 C12 H12B 107.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 C14 110.9(9) . . ?
H13A C13 H13B 108.1 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N10 C12A H12C 106.9 . . ?
N10 C12A H12D 106.9 . . ?
N10 C12A C13A 121.6(9) . . ?
H12C C12A H12D 106.7 . . ?
C13A C12A H12C 106.9 . . ?
C13A C12A H12D 106.9 . . ?
C12A C13A H13C 110.3 . . ?
C12A C13A H13D 110.3 . . ?
C12A C13A C14A 107.2(9) . . ?
H13C C13A H13D 108.5 . . ?
C14A C13A H13C 110.3 . . ?
C14A C13A H13D 110.3 . . ?
C13A C14A H14D 109.5 . . ?
C13A C14A H14E 109.5 . . ?
C13A C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
N10 C15 H15A 106.6 . . ?
N10 C15 H15B 106.6 . . ?
H15A C15 H15B 106.6 . . ?
C16A C15 N10 122.8(8) . . ?
C16A C15 H15A 106.6 . . ?
C16A C15 H15B 106.6 . . ?
C15 C16A H16A 109.5 . . ?
C15 C16A H16B 109.5 . . ?
C15 C16A H16C 109.5 . . ?
H16A C16A H16B 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
N10 C15A H15C 109.6 . . ?
N10 C15A H15D 109.6 . . ?
N10 C15A C16 110.1(10) . . ?
H15C C15A H15D 108.2 . . ?
C16 C15A H15C 109.6 . . ?
C16 C15A H15D 109.6 . . ?
C15A C16 H16D 109.5 . . ?
C15A C16 H16E 109.5 . . ?
C15A C16 H16F 109.5 . . ?
H16D C16 H16E 109.5 . . ?
H16D C16 H16F 109.5 . . ?
H16E C16 H16F 109.5 . . ?

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
N10 C7 C8 C9 51.7(15) . . . . ?
N10 C7A C8A C9A -50.7(10) . . . . ?
N10 C12 C13 C14 167.1(9) . . . . ?
N10 C12A C13A C14A 175.9(10) . . . . ?
C7 N10 C11 C10 66.6(9) . . . . ?
C7 C8 C9 C10 -44.8(19) . . . . ?
C8 C9 C10 C11 45.8(17) . . . . ?
C9 C10 C11 N10 -58.5(11) . . . . ?
C11 N10 C7 C8 -61.0(9) . . . . ?
C7A N10 C11A C10A -71.2(10) . . . . ?
C7A C8A C9A C10A 33.8(12) . . . . ?
C8A C9A C10A C11A -43.9(14) . . . . ?
C9A C10A C11A N10 61.4(14) . . . . ?
C11A N10 C7A C8A 70.1(9) . . . . ?

_olex2_exptl_crystal_mounting_method 'with a loop in oil '
_olex2_submission_original_sample_id PEPNidca3
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_krosi27_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2309042'
loop_
_audit_author_name
_audit_author_address
'Silva Maria Kronawitter'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2023-11-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_audit_creation_date             2021-08-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        DPPNidca3
_chemical_formula_moiety         'C6 N9 Ni, C11 H24 N'
_chemical_formula_sum            'C17 H24 N10 Ni'
_chemical_formula_weight         427.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.1198(15)
_cell_length_b                   12.3344(10)
_cell_length_c                   10.2007(9)
_cell_angle_alpha                90
_cell_angle_beta                 110.800(3)
_cell_angle_gamma                90
_cell_volume                     2013.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.55
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6527
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1799 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.8759.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_preparation       'mild solution synthesis in water'
_exptl_crystal_recrystallization_method 'mild solution synthesis in water'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22253
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.085
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1622
_reflns_number_total             1847
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL n/a (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         1847
_refine_ls_number_restraints     153
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0473
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0545P)²+11.8809P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1226
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim N1 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8
\\sim C9 \\sim C10 \\sim C11: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
2. Rigid body (RIGU) restrains
 C1, C2, C3, N1, C4, C5, C6, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) N1(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5) H10A(0.5) H10B(0.5)
 C11(0.5) H11A(0.5) H11B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.750000 0.250000 0.500000 0.0143(2) Uani 1 2 d S . P . .
N2 N 0.62694(17) 0.2031(2) 0.4043(3) 0.0233(6) Uani 1 1 d . . . . .
N3 N 0.500000 0.1127(3) 0.250000 0.0303(10) Uani 1 2 d S T P . .
N4 N 0.71424(17) 0.4012(2) 0.5452(3) 0.0225(6) Uani 1 1 d . . . . .
N5 N 0.6979(2) 0.5956(2) 0.5819(3) 0.0315(8) Uani 1 1 d . . . . .
N6 N 0.74834(18) 0.6892(2) 0.8083(3) 0.0236(6) Uani 1 1 d . . . . .
C1 C 0.3620(13) 0.0649(15) 0.4239(17) 0.056(3) Uani 0.5 1 d . U P A -1
H1A H 0.312651 0.082998 0.341917 0.084 Uiso 0.5 1 calc R U P A -1
H1B H 0.346788 0.010844 0.481142 0.084 Uiso 0.5 1 calc R U P A -1
H1C H 0.405618 0.035358 0.392854 0.084 Uiso 0.5 1 calc R U P A -1
C2 C 0.3930(8) 0.1627(9) 0.5073(11) 0.0590(15) Uani 0.5 1 d . U P A -1
H2A H 0.404920 0.218014 0.446595 0.071 Uiso 0.5 1 calc R U P A -1
H2B H 0.348214 0.191687 0.537645 0.071 Uiso 0.5 1 calc R U P A -1
C3 C 0.4612(7) 0.1485(9) 0.6198(12) 0.0543(13) Uani 0.5 1 d . U P A -1
H3A H 0.507286 0.126134 0.588439 0.065 Uiso 0.5 1 calc R U P A -1
H3B H 0.450946 0.088014 0.675447 0.065 Uiso 0.5 1 calc R U P A -1
N1 N 0.4925(7) 0.2549(5) 0.7236(7) 0.0450(9) Uani 0.5 1 d . U P A -1
C4 C 0.6319(9) 0.0806(11) 1.0476(13) 0.0311(17) Uani 0.5 1 d . U P A -1
H4A H 0.647008 0.028017 0.988586 0.047 Uiso 0.5 1 calc R U P A -1
H4B H 0.623163 0.042653 1.125702 0.047 Uiso 0.5 1 calc R U P A -1
H4C H 0.677115 0.133556 1.084606 0.047 Uiso 0.5 1 calc R U P A -1
C5 C 0.5537(5) 0.1376(6) 0.9626(8) 0.0259(11) Uani 0.5 1 d . U P A -1
H5A H 0.535740 0.188147 1.021864 0.031 Uiso 0.5 1 calc R U P A -1
H5B H 0.508194 0.084838 0.919368 0.031 Uiso 0.5 1 calc R U P A -1
C6 C 0.5752(5) 0.2019(6) 0.8457(8) 0.0292(10) Uani 0.5 1 d . U P A -1
H6A H 0.603346 0.152063 0.800500 0.035 Uiso 0.5 1 calc R U P A -1
H6B H 0.614932 0.260752 0.890854 0.035 Uiso 0.5 1 calc R U P A -1
C7 C 0.5248(7) 0.3386(9) 0.6371(10) 0.0440(11) Uani 0.5 1 d . U P A -1
H7A H 0.566728 0.302439 0.605704 0.053 Uiso 0.5 1 calc R U P A -1
H7B H 0.477398 0.360548 0.552447 0.053 Uiso 0.5 1 calc R U P A -1
C8 C 0.5625(6) 0.4362(8) 0.7175(9) 0.0420(11) Uani 0.5 1 d . U P A -1
H8A H 0.575571 0.488070 0.654093 0.050 Uiso 0.5 1 calc R U P A -1
H8B H 0.615896 0.415757 0.791676 0.050 Uiso 0.5 1 calc R U P A -1
C9 C 0.5081(6) 0.4924(7) 0.7849(8) 0.0431(12) Uani 0.5 1 d . U P A -1
H9A H 0.457657 0.522172 0.711683 0.052 Uiso 0.5 1 calc R U P A -1
H9B H 0.539090 0.553140 0.844051 0.052 Uiso 0.5 1 calc R U P A -1
C10 C 0.4825(6) 0.4104(9) 0.8750(9) 0.0437(11) Uani 0.5 1 d . U P A -1
H10A H 0.532866 0.384576 0.951958 0.052 Uiso 0.5 1 calc R U P A -1
H10B H 0.445336 0.446025 0.917432 0.052 Uiso 0.5 1 calc R U P A -1
C11 C 0.4382(6) 0.3161(8) 0.7881(10) 0.0451(11) Uani 0.5 1 d . U P A -1
H11A H 0.387510 0.342431 0.712284 0.054 Uiso 0.5 1 calc R U P A -1
H11B H 0.420153 0.265819 0.847502 0.054 Uiso 0.5 1 calc R U P A -1
C12 C 0.56599(19) 0.1661(3) 0.3294(3) 0.0197(7) Uani 1 1 d . . . . .
C13 C 0.7092(2) 0.4918(3) 0.5694(3) 0.0209(7) Uani 1 1 d . . . . .
C14 C 0.72624(19) 0.6409(3) 0.7059(3) 0.0187(7) 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 2.065(3) . ?
Ni1 N2 2.065(3) 7_656 ?
Ni1 N4 2.066(3) . ?
Ni1 N4 2.066(3) 7_656 ?
Ni1 N6 2.085(3) 4_646 ?
Ni1 N6 2.085(3) 6_565 ?
N2 C12 1.147(4) . ?
N3 C12 1.310(4) . ?
N3 C12 1.310(4) 2_655 ?
N4 C13 1.154(4) . ?
N5 C13 1.309(5) . ?
N5 C14 1.309(4) . ?
N6 C14 1.143(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.462(18) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.327(15) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 N1 1.652(13) . ?
N1 C6 1.653(12) . ?
N1 C7 1.580(11) . ?
N1 C11 1.516(14) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4 C5 1.489(16) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.580(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.471(13) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.509(14) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.531(11) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.496(13) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N2 180.0 . 7_656 ?
N2 Ni1 N4 91.42(11) 7_656 7_656 ?
N2 Ni1 N4 88.58(11) . 7_656 ?
N2 Ni1 N4 88.58(11) 7_656 . ?
N2 Ni1 N4 91.42(11) . . ?
N2 Ni1 N6 89.17(11) . 6_565 ?
N2 Ni1 N6 90.83(11) . 4_646 ?
N2 Ni1 N6 90.83(11) 7_656 6_565 ?
N2 Ni1 N6 89.17(11) 7_656 4_646 ?
N4 Ni1 N4 180.0 . 7_656 ?
N4 Ni1 N6 88.73(11) . 6_565 ?
N4 Ni1 N6 91.27(11) . 4_646 ?
N4 Ni1 N6 88.73(11) 7_656 4_646 ?
N4 Ni1 N6 91.27(11) 7_656 6_565 ?
N6 Ni1 N6 180.0 6_565 4_646 ?
C12 N2 Ni1 163.9(3) . . ?
C12 N3 C12 119.6(4) 2_655 . ?
C13 N4 Ni1 166.5(3) . . ?
C14 N5 C13 119.7(3) . . ?
C14 N6 Ni1 159.0(3) . 4_656 ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.5 . . ?
C3 C2 C1 114.9(13) . . ?
C3 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
C2 C3 H3A 108.3 . . ?
C2 C3 H3B 108.3 . . ?
C2 C3 N1 115.8(10) . . ?
H3A C3 H3B 107.4 . . ?
N1 C3 H3A 108.3 . . ?
N1 C3 H3B 108.3 . . ?
C3 N1 C6 99.4(7) . . ?
C7 N1 C3 105.0(7) . . ?
C7 N1 C6 107.6(8) . . ?
C11 N1 C3 124.4(9) . . ?
C11 N1 C6 111.3(6) . . ?
C11 N1 C7 107.9(7) . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
C4 C5 H5A 110.6 . . ?
C4 C5 H5B 110.6 . . ?
C4 C5 C6 105.9(7) . . ?
H5A C5 H5B 108.7 . . ?
C6 C5 H5A 110.6 . . ?
C6 C5 H5B 110.6 . . ?
N1 C6 H6A 108.9 . . ?
N1 C6 H6B 108.9 . . ?
C5 C6 N1 113.6(6) . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
N1 C7 H7A 108.9 . . ?
N1 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 N1 113.3(7) . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
C7 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
C7 C8 C9 114.2(8) . . ?
H8A C8 H8B 107.6 . . ?
C9 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
C8 C9 H9A 109.9 . . ?
C8 C9 H9B 109.9 . . ?
C8 C9 C10 109.0(8) . . ?
H9A C9 H9B 108.3 . . ?
C10 C9 H9A 109.9 . . ?
C10 C9 H9B 109.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C11 C10 C9 110.5(7) . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
N1 C11 H11A 109.1 . . ?
N1 C11 H11B 109.1 . . ?
C10 C11 N1 112.6(8) . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N2 C12 N3 173.3(4) . . ?
N4 C13 N5 173.4(4) . . ?
N6 C14 N5 173.8(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 N1 -174.5(13) . . . . ?
C2 C3 N1 C6 179.4(10) . . . . ?
C2 C3 N1 C7 -69.3(13) . . . . ?
C2 C3 N1 C11 55.4(13) . . . . ?
C3 N1 C6 C5 -84.3(8) . . . . ?
C3 N1 C7 C8 -174.9(9) . . . . ?
C3 N1 C11 C10 -178.8(8) . . . . ?
N1 C7 C8 C9 -52.3(12) . . . . ?
C4 C5 C6 N1 170.5(7) . . . . ?
C6 N1 C7 C8 -69.6(11) . . . . ?
C6 N1 C11 C10 62.6(9) . . . . ?
C7 N1 C6 C5 166.5(7) . . . . ?
C7 N1 C11 C10 -55.3(9) . . . . ?
C7 C8 C9 C10 54.5(10) . . . . ?
C8 C9 C10 C11 -57.5(10) . . . . ?
C9 C10 C11 N1 61.2(11) . . . . ?
C11 N1 C6 C5 48.5(8) . . . . ?
C11 N1 C7 C8 50.6(10) . . . . ?

_olex2_date_sample_data_collection 2021-08-02
_olex2_submission_original_sample_id KroSi27
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_krosi104_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2309043'
loop_
_audit_author_name
_audit_author_address
'Silva Maria Kronawitter'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2023-11-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_audit_creation_date             2023-08-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        DPPNidca_RT
_chemical_formula_moiety         'C6 N9 Ni, C11 H24 N'
_chemical_formula_sum            'C17 H24 N10 Ni'
_chemical_formula_weight         427.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.3196(5)
_cell_length_b                   12.3357(3)
_cell_length_c                   10.4909(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.9170(10)
_cell_angle_gamma                90
_cell_volume                     2079.38(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.54
_shelx_estimated_absorpt_T_max   0.930
_shelx_estimated_absorpt_T_min   0.817
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1075 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.9389.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             896
_exptl_crystal_preparation       'wet chemistry'
_exptl_crystal_recrystallization_method 'wet chemistry'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.077
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            52302
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.145
_diffrn_reflns_theta_min         2.081
_diffrn_ambient_temperature      300.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_special_details          -
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2191
_reflns_number_total             2803
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.736
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2803
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0592
_refine_ls_restrained_S_all      1.180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1272P)²+3.9689P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.2271
_refine_special_details          -
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H8A(0.5) H8B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5B,H5A), C7(H7A,H7B), C8(H8A,H8B)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.250000 0.250000 0.500000 0.0349(2) Uani 1 2 d S . P . .
N1 N 0.1264(2) 0.2917(3) 0.4062(4) 0.0581(8) Uani 1 1 d . . . . .
N2 N 0.2812(2) 0.4008(3) 0.4472(3) 0.0567(8) Uani 1 1 d . . . . .
N3 N 0.3009(3) 0.5917(3) 0.4056(4) 0.0793(14) Uani 1 1 d . . . . .
N4 N 0.2540(2) 0.6843(3) 0.1851(3) 0.0565(8) Uani 1 1 d . . . . .
N5 N 0.000000 0.3770(5) 0.250000 0.082(2) Uani 1 2 d S T P . .
C1 C 0.6331(6) 0.9225(7) 1.0589(8) 0.116(3) Uani 1 1 d . . . . .
H1A H 0.650757 0.976776 1.010046 0.174 Uiso 1 1 calc R U . . .
H1B H 0.678588 0.874240 1.104503 0.174 Uiso 1 1 calc R U . . .
H1C H 0.615602 0.956752 1.125774 0.174 Uiso 1 1 calc R U . . .
C2 C 0.5602(14) 0.8579(10) 0.9571(15) 0.237(10) Uani 1 1 d . . . . .
H2A H 0.543925 0.804319 1.010088 0.285 Uiso 1 1 calc R U . . .
H2B H 0.513779 0.907689 0.919868 0.285 Uiso 1 1 calc R U . . .
N6 N 0.500000 0.7438(6) 0.750000 0.094(3) Uani 1 2 d S T P . .
C3 C 0.5676(9) 0.8091(12) 0.8570(10) 0.192(7) Uani 1 1 d . . . . .
H3A H 0.614418 0.760154 0.896048 0.230 Uiso 1 1 calc R U . . .
H3B H 0.585043 0.863454 0.806477 0.230 Uiso 1 1 calc R U . . .
C5 C 0.4588(10) 0.6650(11) 0.8284(17) 0.219(8) Uani 1 1 d . . . . .
H5B H 0.489015 0.675882 0.926033 0.263 Uiso 1 1 calc R U . . .
H5A H 0.402610 0.691144 0.808279 0.263 Uiso 1 1 calc R U . . .
C7 C 0.4537(12) 0.5675(9) 0.809(2) 0.257(10) Uani 1 1 d . . . . .
H7A H 0.395761 0.553235 0.753947 0.308 Uiso 1 1 calc R U . . .
H7B H 0.464134 0.535032 0.898271 0.308 Uiso 1 1 calc R U . . .
C8 C 0.500000 0.5063(11) 0.750000 0.155(6) Uani 1 2 d S T P . .
H8A H 0.537880 0.459779 0.820215 0.186 Uiso 0.5 1 calc R U P . .
H8B H 0.462121 0.459777 0.679786 0.186 Uiso 0.5 1 calc R U P . .
C9 C 0.2874(3) 0.4891(3) 0.4200(4) 0.0501(8) Uani 1 1 d . . . . .
C10 C 0.2736(2) 0.6361(3) 0.2841(4) 0.0474(8) Uani 1 1 d . . . . .
C11 C 0.0651(2) 0.3255(3) 0.3307(4) 0.0510(8) 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 N1 2.060(3) 7_556 ?
Ni1 N1 2.060(3) . ?
Ni1 N2 2.070(3) 7_556 ?
Ni1 N2 2.070(3) . ?
Ni1 N4 2.081(3) 6_566 ?
Ni1 N4 2.081(3) 4_545 ?
N1 C11 1.139(5) . ?
N2 C9 1.141(5) . ?
N3 C9 1.305(5) . ?
N3 C10 1.304(5) . ?
N4 C10 1.133(5) . ?
N5 C11 1.296(4) . ?
N5 C11 1.296(4) 2 ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.538(17) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.259(17) . ?
N6 C3 1.516(11) . ?
N6 C3 1.516(10) 2_656 ?
N6 C5 1.603(12) 2_656 ?
N6 C5 1.603(12) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 C7 1.217(14) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.404(14) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0(2) 7_556 . ?
N1 Ni1 N2 91.35(16) 7_556 . ?
N1 Ni1 N2 88.65(16) 7_556 7_556 ?
N1 Ni1 N2 88.65(16) . . ?
N1 Ni1 N2 91.35(16) . 7_556 ?
N1 Ni1 N4 89.14(15) 7_556 6_566 ?
N1 Ni1 N4 90.86(15) 7_556 4_545 ?
N1 Ni1 N4 90.86(15) . 6_566 ?
N1 Ni1 N4 89.14(15) . 4_545 ?
N2 Ni1 N2 180.0 7_556 . ?
N2 Ni1 N4 88.76(14) 7_556 4_545 ?
N2 Ni1 N4 88.76(14) . 6_566 ?
N2 Ni1 N4 91.24(14) . 4_545 ?
N2 Ni1 N4 91.24(14) 7_556 6_566 ?
N4 Ni1 N4 180.0 6_566 4_545 ?
C11 N1 Ni1 162.7(4) . . ?
C9 N2 Ni1 169.5(4) . . ?
C10 N3 C9 120.4(4) . . ?
C10 N4 Ni1 162.5(4) . 4 ?
C11 N5 C11 121.3(5) 2 . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2A 107.1 . . ?
C1 C2 H2B 107.1 . . ?
H2A C2 H2B 106.8 . . ?
C3 C2 C1 120.9(16) . . ?
C3 C2 H2A 107.1 . . ?
C3 C2 H2B 107.1 . . ?
C3 N6 C3 115.8(13) 2_656 . ?
C3 N6 C5 109.4(11) 2_656 . ?
C3 N6 C5 109.4(10) . 2_656 ?
C3 N6 C5 108.1(7) . . ?
C3 N6 C5 108.1(7) 2_656 2_656 ?
C5 N6 C5 105.4(9) . 2_656 ?
C2 C3 N6 125.5(15) . . ?
C2 C3 H3A 106.0 . . ?
C2 C3 H3B 106.0 . . ?
N6 C3 H3A 106.0 . . ?
N6 C3 H3B 106.0 . . ?
H3A C3 H3B 106.3 . . ?
N6 C5 H5B 106.8 . . ?
N6 C5 H5A 106.8 . . ?
H5B C5 H5A 106.6 . . ?
C7 C5 N6 122.1(9) . . ?
C7 C5 H5B 106.8 . . ?
C7 C5 H5A 106.8 . . ?
C5 C7 H7A 105.8 . . ?
C5 C7 H7B 105.8 . . ?
C5 C7 C8 126.0(11) . . ?
H7A C7 H7B 106.2 . . ?
C8 C7 H7A 105.8 . . ?
C8 C7 H7B 105.8 . . ?
C7 C8 C7 114.8(12) 2_656 . ?
C7 C8 H8A 108.6 2_656 . ?
C7 C8 H8A 108.6 . . ?
C7 C8 H8B 108.6 . . ?
C7 C8 H8B 108.6 2_656 . ?
H8A C8 H8B 107.5 . . ?
N2 C9 N3 172.5(4) . . ?
N4 C10 N3 172.9(4) . . ?
N1 C11 N5 172.1(5) . . ?

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
C1 C2 C3 N6 -179.6(9) . . . . ?
N6 C5 C7 C8 18(4) . . . . ?
C3 N6 C3 C2 75.7(17) 2_656 . . . ?
C3 N6 C5 C7 107(2) 2_656 . . . ?
C3 N6 C5 C7 -126(2) . . . . ?
C5 N6 C3 C2 -47.5(19) . . . . ?
C5 N6 C3 C2 -161.8(15) 2_656 . . . ?
C5 N6 C5 C7 -8.8(17) 2_656 . . . ?
C5 C7 C8 C7 -10(2) . . . 2_656 ?

_olex2_exptl_crystal_mounting_method 'with a loop in oil '
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mo_krosi21_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2309038'
loop_
_audit_author_name
_audit_author_address
'Silva Maria Kronawitter'
;Technical University of Munich
Germany
;
_audit_update_record             
;
2023-11-20 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_audit_creation_date             2021-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        KroSI21
_chemical_formula_moiety         'C6 N9 Ni, C11 H24 N'
_chemical_formula_sum            'C17 H24 N10 Ni'
_chemical_formula_weight         427.17
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   16.1247(8)
_cell_length_b                   11.9812(5)
_cell_length_c                   10.8829(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.986(2)
_cell_angle_gamma                90
_cell_volume                     2091.04(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.67
_cell_measurement_theta_min      2.54
_shelx_estimated_absorpt_T_max   0.891
_shelx_estimated_absorpt_T_min   0.792
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0402 after correction.
The Ratio of minimum to maximum transmission is 0.9317.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4.00 -1.00 1.00 0.0620
-4.00 1.00 -1.00 0.0470
4.00 4.00 3.00 0.0860
-1.00 2.00 -3.00 0.1210
3.00 -1.00 -4.00 0.1310
-1.00 -2.00 -1.00 0.0820
-4.00 -3.00 -2.00 0.0490
-4.00 5.00 1.00 0.0600
-4.00 -5.00 4.00 0.0930
-2.00 -1.00 0.00 0.0530
-4.00 1.00 1.00 0.0460
4.00 -1.00 -1.00 0.1020

_exptl_crystal_preparation       'mild solution synthesis'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.124
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0080
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            96894
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.312
_diffrn_reflns_theta_min         2.122
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4842
_reflns_number_total             5203
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0237
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0276P)²+1.1502P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0644
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7B,H7A), C8(H8A,H8B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 1.000000 1.000000 0.500000 0.01408(6) Uani 1 2 d S . P . .
Ni2 Ni 0.500000 1.000000 0.500000 0.01394(6) Uani 1 2 d S . P . .
N2 N 0.88909(6) 1.09075(8) 0.49754(9) 0.02122(19) Uani 1 1 d . . . . .
N3 N 0.94483(6) 0.89056(9) 0.36949(9) 0.0233(2) Uani 1 1 d . . . . .
N4 N 0.88667(6) 0.71731(9) 0.27562(11) 0.0282(2) Uani 1 1 d . . . . .
N5 N 0.95730(6) 0.59915(9) 0.13431(9) 0.0232(2) Uani 1 1 d . . . . .
N6 N 0.62596(6) 1.03102(10) 0.54451(9) 0.0248(2) Uani 1 1 d . . . . .
N7 N 0.52079(6) 0.56114(8) 0.82903(9) 0.02047(19) Uani 1 1 d . . . . .
N8 N 0.51364(7) 0.84059(8) 0.57005(9) 0.0243(2) Uani 1 1 d . . . . .
N18 N 0.51188(8) 0.64103(9) 0.62045(9) 0.0307(2) Uani 1 1 d . . . . .
N19 N 0.76455(7) 1.10954(11) 0.60815(10) 0.0315(2) Uani 1 1 d . . . . .
C12 C 0.92143(7) 0.80830(10) 0.32361(10) 0.0192(2) Uani 1 1 d . . . . .
C13 C 0.92717(7) 0.65748(9) 0.20040(10) 0.0190(2) Uani 1 1 d . . . . .
C14 C 0.82857(7) 1.09576(9) 0.54536(10) 0.0195(2) Uani 1 1 d . . . . .
C16 C 0.69217(7) 1.06519(10) 0.56857(10) 0.0219(2) Uani 1 1 d . . . . .
C17 C 0.51335(7) 0.74881(10) 0.59990(10) 0.0204(2) Uani 1 1 d . . . . .
C19 C 0.51661(7) 0.60414(9) 0.73416(10) 0.0185(2) Uani 1 1 d . . . . .
N1 N 0.24674(6) 0.51248(8) 0.47951(9) 0.01968(19) Uani 1 1 d . . . . .
C1 C 0.12534(9) 0.60295(13) 0.58076(13) 0.0336(3) Uani 1 1 d . . . . .
H1A H 0.095466 0.673671 0.586564 0.050 Uiso 1 1 calc R U . . .
H1B H 0.158257 0.587341 0.659745 0.050 Uiso 1 1 calc R U . . .
H1C H 0.085102 0.542554 0.561424 0.050 Uiso 1 1 calc R U . . .
C2 C 0.18350(8) 0.61120(11) 0.47843(11) 0.0249(2) Uani 1 1 d . . . . .
H2 H 0.216975 0.680985 0.493965 0.030 Uiso 1 1 calc R U . . .
C3 C 0.20156(7) 0.40180(10) 0.47710(11) 0.0247(2) Uani 1 1 d . . . . .
H3A H 0.166594 0.394269 0.397184 0.030 Uiso 1 1 calc R U . . .
H3B H 0.164012 0.401149 0.543494 0.030 Uiso 1 1 calc R U . . .
C4 C 0.26059(8) 0.30134(11) 0.49418(12) 0.0268(2) Uani 1 1 d . . . . .
H4A H 0.227557 0.231638 0.493183 0.032 Uiso 1 1 calc R U . . .
H4B H 0.295748 0.298271 0.424914 0.032 Uiso 1 1 calc R U . . .
C5 C 0.31618(8) 0.31015(11) 0.61624(12) 0.0299(3) Uani 1 1 d . . . . .
H5A H 0.281531 0.303436 0.685813 0.036 Uiso 1 1 calc R U . . .
H5B H 0.356903 0.248042 0.622490 0.036 Uiso 1 1 calc R U . . .
C6 C 0.13016(8) 0.62669(12) 0.35529(12) 0.0296(3) Uani 1 1 d . . . . .
H6A H 0.101229 0.556718 0.331903 0.044 Uiso 1 1 calc R U . . .
H6B H 0.165937 0.647517 0.291508 0.044 Uiso 1 1 calc R U . . .
H6C H 0.089056 0.685782 0.363382 0.044 Uiso 1 1 calc R U . . .
C7 C 0.30297(8) 0.51929(11) 0.60146(11) 0.0248(2) Uani 1 1 d . . . . .
H7B H 0.336207 0.588791 0.601830 0.030 Uiso 1 1 calc R U . . .
H7A H 0.267387 0.524260 0.670094 0.030 Uiso 1 1 calc R U . . .
C8 C 0.36247(8) 0.42061(11) 0.62551(11) 0.0261(2) Uani 1 1 d . . . . .
H8A H 0.404008 0.421816 0.564656 0.031 Uiso 1 1 calc R U . . .
H8B H 0.392830 0.427896 0.709003 0.031 Uiso 1 1 calc R U . . .
C9 C 0.30377(7) 0.51981(11) 0.37210(11) 0.0237(2) Uani 1 1 d . . . . .
H9 H 0.352864 0.471084 0.397905 0.028 Uiso 1 1 calc R U . . .
C10 C 0.26542(8) 0.47273(12) 0.24865(11) 0.0281(3) Uani 1 1 d . . . . .
H10A H 0.216965 0.517812 0.217762 0.042 Uiso 1 1 calc R U . . .
H10B H 0.247827 0.395452 0.260072 0.042 Uiso 1 1 calc R U . . .
H10C H 0.306849 0.474701 0.188896 0.042 Uiso 1 1 calc R U . . .
C11 C 0.33941(8) 0.63608(12) 0.35719(13) 0.0319(3) Uani 1 1 d . . . . .
H11A H 0.381967 0.633136 0.299211 0.048 Uiso 1 1 calc R U . . .
H11B H 0.364611 0.663109 0.437529 0.048 Uiso 1 1 calc R U . . .
H11C H 0.294617 0.686842 0.325210 0.048 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 N2 2.0907(10) . ?
Ni1 N2 2.0907(10) 3_776 ?
Ni1 N3 2.0650(10) 3_776 ?
Ni1 N3 2.0651(10) . ?
Ni1 N5 2.0571(10) 2_755 ?
Ni1 N5 2.0571(10) 4_576 ?
Ni2 N6 2.0719(10) 3_676 ?
Ni2 N6 2.0718(10) . ?
Ni2 N7 2.0594(9) 2_656 ?
Ni2 N7 2.0594(9) 4_575 ?
Ni2 N8 2.0597(10) . ?
Ni2 N8 2.0597(10) 3_676 ?
N2 C14 1.1544(15) . ?
N3 C12 1.1506(15) . ?
N4 C12 1.3093(15) . ?
N4 C13 1.3122(15) . ?
N5 C13 1.1466(15) . ?
N6 C16 1.1479(16) . ?
N7 C19 1.1496(15) . ?
N8 C17 1.1467(15) . ?
N18 C17 1.3112(15) . ?
N18 C19 1.3088(15) . ?
N19 C14 1.3065(15) . ?
N19 C16 1.3135(15) . ?
N1 C2 1.5609(15) . ?
N1 C3 1.5120(15) . ?
N1 C7 1.5294(15) . ?
N1 C9 1.5632(15) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.5321(18) . ?
C2 H2 1.0000 . ?
C2 C6 1.5264(16) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.5337(17) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.5267(18) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C8 1.5176(18) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 C8 1.5279(17) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9 1.0000 . ?
C9 C10 1.5272(17) . ?
C9 C11 1.5221(18) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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 N2 180.0 3_776 . ?
N3 Ni1 N2 90.85(4) 3_776 3_776 ?
N3 Ni1 N2 90.85(4) . . ?
N3 Ni1 N2 89.15(4) 3_776 . ?
N3 Ni1 N2 89.15(4) . 3_776 ?
N3 Ni1 N3 180.00(5) 3_776 . ?
N5 Ni1 N2 87.72(4) 4_576 . ?
N5 Ni1 N2 92.28(4) 4_576 3_776 ?
N5 Ni1 N2 87.72(4) 2_755 3_776 ?
N5 Ni1 N2 92.28(4) 2_755 . ?
N5 Ni1 N3 91.72(4) 4_576 3_776 ?
N5 Ni1 N3 88.28(4) 4_576 . ?
N5 Ni1 N3 91.72(4) 2_755 . ?
N5 Ni1 N3 88.28(4) 2_755 3_776 ?
N5 Ni1 N5 180.0 4_576 2_755 ?
N6 Ni2 N6 180.0 . 3_676 ?
N7 Ni2 N6 91.55(4) 2_656 3_676 ?
N7 Ni2 N6 88.45(4) 4_575 3_676 ?
N7 Ni2 N6 91.55(4) 4_575 . ?
N7 Ni2 N6 88.45(4) 2_656 . ?
N7 Ni2 N7 180.0 4_575 2_656 ?
N7 Ni2 N8 89.05(4) 4_575 . ?
N7 Ni2 N8 90.95(4) 4_575 3_676 ?
N7 Ni2 N8 89.05(4) 2_656 3_676 ?
N7 Ni2 N8 90.95(4) 2_656 . ?
N8 Ni2 N6 90.89(4) 3_676 3_676 ?
N8 Ni2 N6 89.11(4) 3_676 . ?
N8 Ni2 N6 90.89(4) . . ?
N8 Ni2 N6 89.11(4) . 3_676 ?
N8 Ni2 N8 180.00(6) 3_676 . ?
C14 N2 Ni1 141.58(9) . . ?
C12 N3 Ni1 160.16(10) . . ?
C12 N4 C13 118.91(10) . . ?
C13 N5 Ni1 173.14(10) . 2_745 ?
C16 N6 Ni2 169.43(11) . . ?
C19 N7 Ni2 166.18(9) . 2_646 ?
C17 N8 Ni2 172.13(10) . . ?
C19 N18 C17 119.58(10) . . ?
C14 N19 C16 120.06(10) . . ?
N3 C12 N4 173.58(12) . . ?
N5 C13 N4 174.43(12) . . ?
N2 C14 N19 173.48(12) . . ?
N6 C16 N19 173.02(12) . . ?
N8 C17 N18 173.40(12) . . ?
N7 C19 N18 173.11(12) . . ?
C2 N1 C9 112.74(9) . . ?
C3 N1 C2 110.57(9) . . ?
C3 N1 C7 107.63(9) . . ?
C3 N1 C9 110.86(9) . . ?
C7 N1 C2 107.09(9) . . ?
C7 N1 C9 107.71(9) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C2 H2 107.0 . . ?
C1 C2 N1 113.24(10) . . ?
C1 C2 H2 107.0 . . ?
C6 C2 N1 113.99(10) . . ?
C6 C2 C1 108.33(10) . . ?
C6 C2 H2 107.0 . . ?
N1 C3 H3A 108.9 . . ?
N1 C3 H3B 108.9 . . ?
N1 C3 C4 113.23(10) . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C5 C4 C3 110.60(11) . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C4 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C8 C5 C4 110.99(10) . . ?
C8 C5 H5A 109.4 . . ?
C8 C5 H5B 109.4 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7B 108.7 . . ?
N1 C7 H7A 108.7 . . ?
H7B C7 H7A 107.6 . . ?
C8 C7 N1 114.34(10) . . ?
C8 C7 H7B 108.7 . . ?
C8 C7 H7A 108.7 . . ?
C5 C8 C7 111.58(10) . . ?
C5 C8 H8A 109.3 . . ?
C5 C8 H8B 109.3 . . ?
C7 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
N1 C9 H9 105.5 . . ?
C10 C9 N1 114.92(10) . . ?
C10 C9 H9 105.5 . . ?
C11 C9 N1 112.91(10) . . ?
C11 C9 H9 105.5 . . ?
C11 C9 C10 111.53(11) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

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
N1 C3 C4 C5 58.25(13) . . . . ?
N1 C7 C8 C5 -53.93(14) . . . . ?
C2 N1 C3 C4 -172.86(10) . . . . ?
C2 N1 C7 C8 173.11(10) . . . . ?
C2 N1 C9 C10 -83.55(12) . . . . ?
C2 N1 C9 C11 45.91(13) . . . . ?
C3 N1 C2 C1 53.40(13) . . . . ?
C3 N1 C2 C6 -71.05(13) . . . . ?
C3 N1 C7 C8 54.21(13) . . . . ?
C3 N1 C9 C10 41.01(13) . . . . ?
C3 N1 C9 C11 170.48(10) . . . . ?
C3 C4 C5 C8 -54.49(14) . . . . ?
C4 C5 C8 C7 52.50(14) . . . . ?
C7 N1 C2 C1 -63.58(13) . . . . ?
C7 N1 C2 C6 171.97(10) . . . . ?
C7 N1 C3 C4 -56.21(12) . . . . ?
C7 N1 C9 C10 158.52(10) . . . . ?
C7 N1 C9 C11 -72.01(12) . . . . ?
C9 N1 C2 C1 178.14(10) . . . . ?
C9 N1 C2 C6 53.69(13) . . . . ?
C9 N1 C3 C4 61.34(12) . . . . ?
C9 N1 C7 C8 -65.38(13) . . . . ?

_olex2_submission_original_sample_id DIPNidca3
_olex2_submission_special_instructions 'No special instructions were received'
