# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 2124819'
loop_
_audit_author_name
_audit_author_address
'David Vicic'
;Lehigh University
United States of America
;
_audit_update_record             
;
2021-11-28 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H15 F11 N2 Ni'
_chemical_formula_weight         442.96

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   9.7161(12)
_cell_length_b                   9.6552(12)
_cell_length_c                   17.169(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.585(3)
_cell_angle_gamma                90
_cell_volume                     1600.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9923
_cell_measurement_theta_min      2.849
_cell_measurement_theta_max      24.625

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_F_000             888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.328
_shelx_estimated_absorpt_T_min   0.724
_shelx_estimated_absorpt_T_max   0.879
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.591216
_exptl_absorpt_correction_T_max  0.745112
_exptl_absorpt_process_details   Bruker
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3146
_diffrn_reflns_av_unetI/netI     0.1803
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.984
_diffrn_reflns_theta_max         24.716
_diffrn_reflns_theta_full        24.716
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3146
_reflns_number_gt                1994
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 4-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+22.4042P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3146
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2122
_refine_ls_R_factor_gt           0.1393
_refine_ls_wR_factor_ref         0.2933
_refine_ls_wR_factor_gt          0.2585
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.158
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.002

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 0.6018(2) 0.8126(3) 0.85202(14) 0.0218(6) Uani 1 1 d . . . . .
N1 N 0.5273(15) 0.9913(16) 0.8543(9) 0.026(4) Uani 1 1 d . . . . .
F1 F 0.6472(12) 0.9195(12) 1.0040(6) 0.043(3) Uani 1 1 d . . . . .
C1 C 0.711(2) 0.839(2) 0.9512(11) 0.032(5) Uani 1 1 d . . . . .
F2 F 0.8337(12) 0.9054(14) 0.9483(7) 0.051(4) Uani 1 1 d . . . . .
N2 N 0.3074(14) 0.2072(15) 0.5509(8) 0.020(3) Uiso 1 1 d . . . . .
C2 C 0.673(2) 0.6348(17) 0.8393(12) 0.029(5) Uani 1 1 d . . . . .
C3 C 0.640(2) 0.5802(19) 0.7564(11) 0.028(4) Uiso 1 1 d . . . . .
F3 F 0.7513(15) 0.7251(13) 0.9973(7) 0.064(4) Uani 1 1 d . . . . .
F4 F 0.8147(12) 0.6158(13) 0.8580(8) 0.053(4) Uani 1 1 d . . . . .
C4 C 0.499(2) 0.6365(18) 0.7269(11) 0.027(5) Uani 1 1 d . . . . .
F5 F 0.6155(14) 0.5364(12) 0.8865(7) 0.051(4) Uani 1 1 d . . . . .
C5 C 0.492(2) 0.7846(19) 0.7515(10) 0.029(5) Uani 1 1 d . . . . .
F6 F 0.6473(14) 0.4415(11) 0.7466(7) 0.049(3) Uani 1 1 d . . . . .
C6 C 0.4844(19) 1.101(2) 0.8489(10) 0.025(4) Uani 1 1 d . . . . .
F7 F 0.7283(12) 0.6384(13) 0.7097(7) 0.050(3) Uani 1 1 d . . . . .
C7 C 0.432(2) 1.2420(19) 0.8419(13) 0.037(5) Uani 1 1 d . . . . .
H7A H 0.342704 1.242842 0.809203 0.055 Uiso 1 1 calc R U . . .
H7B H 0.498205 1.300295 0.817793 0.055 Uiso 1 1 calc R U . . .
H7C H 0.420511 1.278082 0.894141 0.055 Uiso 1 1 calc R U . . .
F8 F 0.4002(12) 0.5625(12) 0.7622(7) 0.044(3) Uani 1 1 d . . . . .
C8 C 0.373(2) 0.212(2) 0.4768(14) 0.056(7) Uani 1 1 d . . . . .
H8A H 0.471646 0.191906 0.487860 0.084 Uiso 1 1 calc R U . . .
H8B H 0.360253 0.304963 0.453717 0.084 Uiso 1 1 calc R U . . .
H8C H 0.328670 0.143579 0.439993 0.084 Uiso 1 1 calc R U . . .
C9 C 0.159(2) 0.218(2) 0.5314(12) 0.043(6) Uani 1 1 d . . . . .
H9A H 0.113608 0.201587 0.578578 0.064 Uiso 1 1 calc R U . . .
H9B H 0.128366 0.148164 0.491691 0.064 Uiso 1 1 calc R U . . .
H9C H 0.135947 0.310382 0.510838 0.064 Uiso 1 1 calc R U . . .
F9 F 0.4639(13) 0.6150(13) 0.6473(7) 0.048(3) Uani 1 1 d . . . . .
C10 C 0.363(2) 0.321(2) 0.6015(12) 0.042(5) Uani 1 1 d . . . . .
H10A H 0.318999 0.321249 0.649983 0.062 Uiso 1 1 calc R U . . .
H10B H 0.344642 0.409558 0.574097 0.062 Uiso 1 1 calc R U . . .
H10C H 0.463506 0.309333 0.614155 0.062 Uiso 1 1 calc R U . . .
F10 F 0.3523(11) 0.8219(13) 0.7490(7) 0.045(3) Uani 1 1 d . . . . .
C11 C 0.339(2) 0.075(2) 0.5916(14) 0.051(6) Uani 1 1 d . . . . .
H11A H 0.310721 0.080779 0.644606 0.076 Uiso 1 1 calc R U . . .
H11B H 0.438295 0.057115 0.594856 0.076 Uiso 1 1 calc R U . . .
H11C H 0.287673 0.000543 0.562585 0.076 Uiso 1 1 calc R U . . .
F11 F 0.5383(12) 0.8629(11) 0.6924(6) 0.042(3) 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 C2 1.872(17) . ?
Ni1 N1 1.874(15) . ?
Ni1 C1 1.92(2) . ?
Ni1 C5 1.942(18) . ?
N1 C6 1.14(2) . ?
F1 C1 1.39(2) . ?
C1 F2 1.36(2) . ?
C1 F3 1.38(2) . ?
N2 C9 1.44(2) . ?
N2 C11 1.47(2) . ?
N2 C10 1.47(2) . ?
N2 C8 1.49(2) . ?
C2 F4 1.39(2) . ?
C2 F5 1.41(2) . ?
C2 C3 1.52(3) . ?
C3 F6 1.35(2) . ?
C3 F7 1.36(2) . ?
C3 C4 1.51(3) . ?
C4 F9 1.39(2) . ?
C4 F8 1.39(2) . ?
C4 C5 1.49(3) . ?
C5 F11 1.38(2) . ?
C5 F10 1.40(2) . ?
C6 C7 1.45(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
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
C2 Ni1 N1 174.5(8) . . ?
C2 Ni1 C1 93.0(9) . . ?
N1 Ni1 C1 92.0(8) . . ?
C2 Ni1 C5 86.6(8) . . ?
N1 Ni1 C5 88.4(7) . . ?
C1 Ni1 C5 179.6(8) . . ?
C6 N1 Ni1 173.9(16) . . ?
F2 C1 F3 101.7(16) . . ?
F2 C1 F1 102.5(15) . . ?
F3 C1 F1 100.9(14) . . ?
F2 C1 Ni1 115.3(13) . . ?
F3 C1 Ni1 119.7(14) . . ?
F1 C1 Ni1 114.3(13) . . ?
C9 N2 C11 108.5(16) . . ?
C9 N2 C10 112.1(15) . . ?
C11 N2 C10 109.1(15) . . ?
C9 N2 C8 108.1(15) . . ?
C11 N2 C8 110.6(17) . . ?
C10 N2 C8 108.4(15) . . ?
F4 C2 F5 103.0(14) . . ?
F4 C2 C3 105.5(15) . . ?
F5 C2 C3 104.5(15) . . ?
F4 C2 Ni1 117.6(13) . . ?
F5 C2 Ni1 112.1(12) . . ?
C3 C2 Ni1 112.8(12) . . ?
F6 C3 F7 106.9(15) . . ?
F6 C3 C4 111.9(16) . . ?
F7 C3 C4 105.4(15) . . ?
F6 C3 C2 116.9(16) . . ?
F7 C3 C2 109.3(16) . . ?
C4 C3 C2 106.0(15) . . ?
F9 C4 F8 104.5(15) . . ?
F9 C4 C5 114.1(14) . . ?
F8 C4 C5 108.3(16) . . ?
F9 C4 C3 112.8(16) . . ?
F8 C4 C3 108.4(15) . . ?
C5 C4 C3 108.6(16) . . ?
F11 C5 F10 103.4(14) . . ?
F11 C5 C4 106.7(14) . . ?
F10 C5 C4 108.2(17) . . ?
F11 C5 Ni1 112.6(13) . . ?
F10 C5 Ni1 115.1(12) . . ?
C4 C5 Ni1 110.3(13) . . ?
N1 C6 C7 179(2) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

_refine_diff_density_max         1.066
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.261

####################################################################### 
# 
# 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_Compound_6
_database_code_depnum_ccdc_archive 'CCDC 2141644'
loop_
_audit_author_name
_audit_author_address
'David Vicic'
;Lehigh University
United States of America
;
_audit_update_record             
;
2022-01-12 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H18 F4.50 N1.50 Ni0.50'
_chemical_formula_weight         322.15

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   8.515(3)
_cell_length_b                   34.457(9)
_cell_length_c                   10.433(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.227(11)
_cell_angle_gamma                90
_cell_volume                     2967.2(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    152(2)
_cell_measurement_reflns_used    9821
_cell_measurement_theta_min      3.025
_cell_measurement_theta_max      30.205

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_F_000             1336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.450
_exptl_absorpt_coefficient_mu    0.733
_shelx_estimated_absorpt_T_min   0.734
_shelx_estimated_absorpt_T_max   0.734
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   Multi-scan
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      152(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44945
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.017
_diffrn_reflns_theta_max         30.224
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             8185
_reflns_number_gt                7201
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+33.3473P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8185
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0860
_refine_ls_wR_factor_ref         0.2279
_refine_ls_wR_factor_gt          0.2243
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_restrained_S_all      1.199
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.78209(8) 0.64576(2) 0.44143(6) 0.01421(15) Uani 1 1 d . . . . .
F1 F 0.8083(5) 0.72833(10) 0.4139(4) 0.0333(8) Uani 1 1 d . . . . .
N1 N 0.6662(5) 0.57949(12) 0.2594(4) 0.0157(8) Uani 1 1 d . . . . .
C1 C 0.8240(7) 0.69848(15) 0.5056(5) 0.0208(10) Uani 1 1 d . . . . .
F2 F 0.7325(5) 0.71438(10) 0.5891(4) 0.0311(8) Uani 1 1 d . . . . .
N2 N 0.8241(5) 0.55993(12) 0.4415(4) 0.0166(8) Uani 1 1 d . . . . .
C2 C 0.8809(6) 0.65957(15) 0.2978(5) 0.0186(9) Uani 1 1 d . . . . .
F3 F 0.9793(4) 0.70316(11) 0.5812(4) 0.0340(8) Uani 1 1 d . . . . .
N3 N 0.3329(5) 0.75677(13) 0.4389(4) 0.0181(8) Uani 1 1 d . . . . .
C3 C 0.6807(7) 0.63428(15) 0.5865(5) 0.0201(10) Uani 1 1 d . . . . .
F4 F 1.0181(4) 0.68353(10) 0.3277(4) 0.0298(8) Uani 1 1 d . . . . .
C4 C 0.7542(6) 0.59311(14) 0.3788(4) 0.0140(8) Uani 1 1 d . . . . .
F5 F 0.7756(5) 0.67981(11) 0.1978(3) 0.0296(8) Uani 1 1 d . . . . .
C5 C 0.7799(7) 0.52703(15) 0.3618(5) 0.0201(10) Uani 1 1 d . . . . .
H5 H 0.813758 0.501058 0.383400 0.024 Uiso 1 1 calc R U . . .
C6 C 0.6806(7) 0.53948(15) 0.2492(5) 0.0210(10) Uani 1 1 d . . . . .
H6 H 0.629397 0.523847 0.175852 0.025 Uiso 1 1 calc R U . . .
F6 F 0.9368(4) 0.63022(10) 0.2287(3) 0.0264(7) Uani 1 1 d . . . . .
C7 C 0.5742(6) 0.60272(14) 0.1520(5) 0.0165(9) Uani 1 1 d . . . . .
F7 F 0.5440(4) 0.65646(10) 0.5892(3) 0.0270(7) Uani 1 1 d . . . . .
C8 C 0.4352(6) 0.62166(15) 0.1668(5) 0.0180(9) Uani 1 1 d . . . . .
F8 F 0.7822(5) 0.64094(12) 0.7101(3) 0.0334(8) Uani 1 1 d . . . . .
C9 C 0.3468(6) 0.64355(15) 0.0618(5) 0.0196(9) Uani 1 1 d . . . . .
H9 H 0.253432 0.657121 0.071780 0.023 Uiso 1 1 calc R U . . .
F9 F 0.6244(5) 0.59739(10) 0.5986(3) 0.0289(8) Uani 1 1 d . . . . .
C10 C 0.3918(7) 0.64613(15) -0.0583(5) 0.0210(10) Uani 1 1 d . . . . .
C12 C 0.6221(6) 0.60376(15) 0.0317(5) 0.0179(9) Uani 1 1 d . . . . .
C11 C 0.5293(7) 0.62576(15) -0.0705(5) 0.0195(10) Uani 1 1 d . . . . .
H11 H 0.560333 0.627026 -0.151834 0.023 Uiso 1 1 calc R U . . .
C13 C 0.3731(7) 0.61735(19) 0.2903(6) 0.0275(12) Uani 1 1 d . . . . .
H13A H 0.255905 0.621888 0.268299 0.041 Uiso 1 1 calc R U . . .
H13B H 0.427153 0.636312 0.356550 0.041 Uiso 1 1 calc R U . . .
H13C H 0.396116 0.591069 0.325834 0.041 Uiso 1 1 calc R U . . .
C14 C 0.2929(8) 0.66943(18) -0.1715(6) 0.0269(12) Uani 1 1 d . . . . .
H14A H 0.341310 0.667557 -0.247288 0.040 Uiso 1 1 calc R U . . .
H14B H 0.290796 0.696652 -0.144736 0.040 Uiso 1 1 calc R U . . .
H14C H 0.182031 0.659263 -0.196166 0.040 Uiso 1 1 calc R U . . .
C15 C 0.7671(7) 0.58157(18) 0.0077(6) 0.0261(12) Uani 1 1 d . . . . .
H15A H 0.826324 0.598112 -0.040793 0.039 Uiso 1 1 calc R U . . .
H15B H 0.729216 0.558203 -0.044313 0.039 Uiso 1 1 calc R U . . .
H15C H 0.839003 0.574117 0.092696 0.039 Uiso 1 1 calc R U . . .
C16 C 0.9232(6) 0.55653(14) 0.5739(5) 0.0161(9) Uani 1 1 d . . . . .
C17 C 1.0744(6) 0.57450(14) 0.6082(5) 0.0175(9) Uani 1 1 d . . . . .
C18 C 1.1699(7) 0.56970(15) 0.7368(5) 0.0194(10) Uani 1 1 d . . . . .
H18 H 1.272982 0.581901 0.761606 0.023 Uiso 1 1 calc R U . . .
C19 C 1.1166(7) 0.54727(15) 0.8298(5) 0.0220(11) Uani 1 1 d . . . . .
C20 C 0.9669(7) 0.52927(15) 0.7912(5) 0.0230(11) Uani 1 1 d . . . . .
H20 H 0.931050 0.513682 0.853549 0.028 Uiso 1 1 calc R U . . .
C21 C 0.8671(6) 0.53319(15) 0.6644(5) 0.0189(10) Uani 1 1 d . . . . .
C22 C 1.1425(7) 0.59798(18) 0.5120(6) 0.0266(12) Uani 1 1 d . . . . .
H22A H 1.261088 0.597097 0.538504 0.040 Uiso 1 1 calc R U . . .
H22B H 1.106061 0.624954 0.512233 0.040 Uiso 1 1 calc R U . . .
H22C H 1.104368 0.587106 0.423001 0.040 Uiso 1 1 calc R U . . .
C23 C 0.7064(8) 0.51254(18) 0.6313(6) 0.0293(12) Uani 1 1 d . . . . .
H23A H 0.671261 0.507847 0.712673 0.044 Uiso 1 1 calc R U . . .
H23B H 0.717428 0.487695 0.588652 0.044 Uiso 1 1 calc R U . . .
H23C H 0.625779 0.528623 0.571169 0.044 Uiso 1 1 calc R U . . .
C24 C 1.2207(9) 0.54265(19) 0.9679(6) 0.0316(13) Uani 1 1 d . . . . .
H24A H 1.226388 0.515151 0.992590 0.047 Uiso 1 1 calc R U . . .
H24B H 1.173535 0.557459 1.029489 0.047 Uiso 1 1 calc R U . . .
H24C H 1.329958 0.552345 0.971815 0.047 Uiso 1 1 calc R U . . .
C25 C 0.3635(7) 0.72809(17) 0.3393(6) 0.0258(11) Uani 1 1 d . . . . .
H25A H 0.356986 0.741337 0.255007 0.039 Uiso 1 1 calc R U . . .
H25B H 0.281851 0.707469 0.326447 0.039 Uiso 1 1 calc R U . . .
H25C H 0.471620 0.716768 0.371381 0.039 Uiso 1 1 calc R U . . .
C26 C 0.3375(7) 0.73562(17) 0.5655(6) 0.0254(11) Uani 1 1 d . . . . .
H26A H 0.311479 0.753673 0.629858 0.038 Uiso 1 1 calc R U . . .
H26B H 0.446084 0.724865 0.600853 0.038 Uiso 1 1 calc R U . . .
H26C H 0.257997 0.714498 0.548429 0.038 Uiso 1 1 calc R U . . .
C27 C 0.4607(7) 0.78784(17) 0.4609(6) 0.0284(12) Uani 1 1 d . . . . .
H27A H 0.437842 0.807259 0.522569 0.043 Uiso 1 1 calc R U . . .
H27B H 0.460410 0.800321 0.376485 0.043 Uiso 1 1 calc R U . . .
H27C H 0.567166 0.776197 0.498135 0.043 Uiso 1 1 calc R U . . .
C28 C 0.1697(7) 0.77516(17) 0.3911(6) 0.0253(11) Uani 1 1 d . . . . .
H28A H 0.145719 0.791026 0.461896 0.038 Uiso 1 1 calc R U . . .
H28B H 0.087219 0.754883 0.365675 0.038 Uiso 1 1 calc R U . . .
H28C H 0.169395 0.791611 0.314419 0.038 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 C4 1.923(5) . ?
Ni1 C1 1.939(5) . ?
Ni1 C2 1.949(5) . ?
Ni1 C3 1.959(5) . ?
F1 C1 1.389(6) . ?
N1 C4 1.369(6) . ?
N1 C6 1.390(6) . ?
N1 C7 1.442(6) . ?
C1 F3 1.373(6) . ?
C1 F2 1.414(6) . ?
N2 C4 1.378(6) . ?
N2 C5 1.402(6) . ?
N2 C16 1.436(6) . ?
C2 F5 1.385(6) . ?
C2 F6 1.392(6) . ?
C2 F4 1.402(6) . ?
N3 C28 1.497(7) . ?
N3 C26 1.500(7) . ?
N3 C25 1.503(7) . ?
N3 C27 1.504(7) . ?
C3 F9 1.375(6) . ?
C3 F8 1.384(6) . ?
C3 F7 1.398(6) . ?
C5 C6 1.338(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.393(7) . ?
C7 C12 1.411(6) . ?
C8 C9 1.389(7) . ?
C8 C13 1.515(7) . ?
C9 C10 1.400(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(7) . ?
C10 C14 1.503(7) . ?
C12 C11 1.386(7) . ?
C12 C15 1.525(7) . ?
C11 H11 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.394(7) . ?
C16 C21 1.410(7) . ?
C17 C18 1.397(7) . ?
C17 C22 1.511(7) . ?
C18 C19 1.401(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.386(8) . ?
C19 C24 1.503(8) . ?
C20 C21 1.393(8) . ?
C20 H20 0.9500 . ?
C21 C23 1.505(8) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 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
C4 Ni1 C1 176.6(2) . . ?
C4 Ni1 C2 90.6(2) . . ?
C1 Ni1 C2 87.7(2) . . ?
C4 Ni1 C3 91.8(2) . . ?
C1 Ni1 C3 90.0(2) . . ?
C2 Ni1 C3 177.5(2) . . ?
C4 N1 C6 111.7(4) . . ?
C4 N1 C7 126.0(4) . . ?
C6 N1 C7 122.2(4) . . ?
F3 C1 F1 103.0(4) . . ?
F3 C1 F2 101.5(4) . . ?
F1 C1 F2 99.4(4) . . ?
F3 C1 Ni1 112.2(4) . . ?
F1 C1 Ni1 118.5(4) . . ?
F2 C1 Ni1 119.6(4) . . ?
C4 N2 C5 111.6(4) . . ?
C4 N2 C16 127.5(4) . . ?
C5 N2 C16 120.9(4) . . ?
F5 C2 F6 102.5(4) . . ?
F5 C2 F4 102.8(4) . . ?
F6 C2 F4 99.8(4) . . ?
F5 C2 Ni1 112.4(3) . . ?
F6 C2 Ni1 119.2(3) . . ?
F4 C2 Ni1 117.8(3) . . ?
C28 N3 C26 108.7(4) . . ?
C28 N3 C25 110.6(4) . . ?
C26 N3 C25 108.5(4) . . ?
C28 N3 C27 109.1(4) . . ?
C26 N3 C27 110.5(4) . . ?
C25 N3 C27 109.4(4) . . ?
F9 C3 F8 102.7(4) . . ?
F9 C3 F7 101.1(4) . . ?
F8 C3 F7 102.9(4) . . ?
F9 C3 Ni1 119.1(3) . . ?
F8 C3 Ni1 113.2(4) . . ?
F7 C3 Ni1 115.6(3) . . ?
N1 C4 N2 102.9(4) . . ?
N1 C4 Ni1 128.8(4) . . ?
N2 C4 Ni1 128.2(4) . . ?
C6 C5 N2 106.3(4) . . ?
C6 C5 H5 126.8 . . ?
N2 C5 H5 126.8 . . ?
C5 C6 N1 107.4(4) . . ?
C5 C6 H6 126.3 . . ?
N1 C6 H6 126.3 . . ?
C8 C7 C12 121.7(5) . . ?
C8 C7 N1 119.2(4) . . ?
C12 C7 N1 119.0(4) . . ?
C9 C8 C7 118.5(4) . . ?
C9 C8 C13 119.3(5) . . ?
C7 C8 C13 122.1(5) . . ?
C8 C9 C10 121.7(5) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C11 C10 C9 118.0(5) . . ?
C11 C10 C14 121.1(5) . . ?
C9 C10 C14 120.9(5) . . ?
C11 C12 C7 117.6(5) . . ?
C11 C12 C15 118.6(4) . . ?
C7 C12 C15 123.8(5) . . ?
C12 C11 C10 122.4(5) . . ?
C12 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 121.7(5) . . ?
C17 C16 N2 119.9(4) . . ?
C21 C16 N2 118.4(5) . . ?
C16 C17 C18 118.5(5) . . ?
C16 C17 C22 123.2(5) . . ?
C18 C17 C22 118.3(5) . . ?
C17 C18 C19 121.3(5) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C20 C19 C18 118.5(5) . . ?
C20 C19 C24 121.0(5) . . ?
C18 C19 C24 120.5(5) . . ?
C19 C20 C21 122.4(5) . . ?
C19 C20 H20 118.8 . . ?
C21 C20 H20 118.8 . . ?
C20 C21 C16 117.6(5) . . ?
C20 C21 C23 118.7(5) . . ?
C16 C21 C23 123.7(5) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 H26A 109.5 . . ?
N3 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N3 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C27 H27A 109.5 . . ?
N3 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N3 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_refine_diff_density_max         1.779
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.143

####################################################################### 
# 
# 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_k453_a_a
_database_code_depnum_ccdc_archive 'CCDC 2103215'
loop_
_audit_author_name
_audit_author_address
'Sascha Schaefer'
;University of Cologne
Germany
;
_audit_update_record             
;
2022-01-25 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_k453_a_a            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.924 Why?
RESPONSE: Due to time constraints only a 180\% \f scan could be measured.
;
# Added during the CSD deposition process: Tuesday 25 January 2022 04:24 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22.14 H20 F13.03 N3 Ni'
_chemical_formula_weight         634.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0009 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0022 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0073 0.0048 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.2904 0.5913 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.9583(3)
_cell_length_b                   10.3755(5)
_cell_length_c                   12.8434(6)
_cell_angle_alpha                69.438(4)
_cell_angle_beta                 87.104(3)
_cell_angle_gamma                82.992(3)
_cell_volume                     1233.15(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6368
_cell_measurement_theta_min      1.8790
_cell_measurement_theta_max      28.0070

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_F_000             638
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.352
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.500
_diffrn_source                   "'U29 PETRA III undulator'"
_diffrn_measurement_device_type  
"'Kappa-diffractometer, P24 Beamline, DESY Hamburg (Germany)'"
_diffrn_measurement_method       "'φ scans'"
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27658
_diffrn_reflns_av_unetI/netI     0.1711
_diffrn_reflns_av_R_equivalents  0.1599
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.484
_diffrn_reflns_theta_max         31.501
_diffrn_reflns_theta_full        17.458
_diffrn_measured_fraction_theta_max 0.648
_diffrn_measured_fraction_theta_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.648
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.648
_diffrn_reflns_point_group_measured_fraction_full 0.924
_reflns_number_total             15287
_reflns_number_gt                6307
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0877P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         15287
_refine_ls_number_parameters     461
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1617
_refine_ls_wR_factor_gt          0.1497
_refine_ls_goodness_of_fit_ref   0.805
_refine_ls_restrained_S_all      0.813
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.53527(14) 0.62366(16) 0.83037(13) 0.0322(3) Uani 1 1 d . . . . .
N2 N 0.52032(13) 0.49167(16) 0.73721(13) 0.0302(3) Uani 1 1 d . . . . .
N3 N 0.94020(15) -0.03265(16) 0.28655(14) 0.0343(3) Uani 1 1 d . . . . .
C3 C 0.77425(18) 0.7324(2) 0.63987(16) 0.0393(4) Uani 1 1 d . . . . .
C4 C 0.61099(15) 0.55246(17) 0.77404(14) 0.0287(3) Uani 1 1 d . . . . .
C5 C 0.39880(17) 0.6067(2) 0.82974(18) 0.0387(4) Uani 1 1 d . . . . .
H5 H 0.328216 0.644971 0.863694 0.046 Uiso 1 1 calc R U . . .
C6 C 0.38895(16) 0.5249(2) 0.77111(18) 0.0368(4) Uani 1 1 d . . . . .
H6 H 0.310090 0.495557 0.755686 0.044 Uiso 1 1 calc R U . . .
C7 C 0.59020(17) 0.7075(2) 0.88086(15) 0.0330(3) Uani 1 1 d . . . . .
C8 C 0.53430(19) 0.8414(2) 0.86354(19) 0.0407(4) Uani 1 1 d . . . . .
C9 C 0.5861(2) 0.9273(2) 0.9069(2) 0.0458(5) Uani 1 1 d . . . . .
H9 H 0.545921 1.017213 0.893893 0.055 Uiso 1 1 calc R U . . .
F10 F 0.42359(14) 0.89174(15) 0.79719(15) 0.0589(4) Uani 1 1 d . . . . .
C10 C 0.6989(2) 0.8758(2) 0.96986(17) 0.0412(4) Uani 1 1 d . . . . .
F11 F 0.75173(16) 0.95898(16) 1.01375(13) 0.0561(4) Uani 1 1 d . . . . .
C11 C 0.7616(2) 0.7441(2) 0.99039(17) 0.0405(4) Uani 1 1 d . . . . .
H11 H 0.839214 0.712240 1.033468 0.049 Uiso 1 1 calc R U . . .
Ni1 Ni 0.80044(2) 0.54586(2) 0.75373(2) 0.02742(7) Uani 1 1 d . . . . .
F12 F 0.40668(12) 0.24908(14) 0.76894(12) 0.0469(3) Uani 1 1 d . . . . .
C12 C 0.70579(19) 0.6598(2) 0.94498(16) 0.0354(4) Uani 1 1 d . . . . .
H12 H 0.746505 0.570127 0.957738 0.043 Uiso 1 1 calc R U . . .
F13 F 0.65757(16) 0.17409(17) 0.47457(14) 0.0604(4) Uani 1 1 d . . . . .
C13 C 0.55465(16) 0.41044(19) 0.66927(15) 0.0313(3) Uani 1 1 d . . . . .
C14 C 0.49646(18) 0.2907(2) 0.68480(18) 0.0374(4) Uani 1 1 d . . . . .
C15 C 0.5279(2) 0.2108(2) 0.6204(2) 0.0454(5) Uani 1 1 d . . . . .
H15 H 0.486208 0.131339 0.631912 0.054 Uiso 1 1 calc R U . . .
C16 C 0.6230(2) 0.2519(3) 0.5381(2) 0.0447(5) Uani 1 1 d . . . . .
C17 C 0.68622(19) 0.3688(2) 0.51944(17) 0.0410(4) Uani 1 1 d . . . . .
H17 H 0.752096 0.393015 0.464196 0.049 Uiso 1 1 calc R U . . .
C18 C 0.65009(17) 0.4496(2) 0.58426(15) 0.0347(4) Uani 1 1 d . . . . .
H18 H 0.689783 0.530554 0.570986 0.042 Uiso 1 1 calc R U . . .
C19 C 0.9860(3) 0.0601(3) 0.1773(2) 0.0645(7) Uani 1 1 d . . . . .
H19A H 0.908679 0.109614 0.133147 0.097 Uiso 1 1 calc R U . . .
H19B H 1.039075 0.005906 0.139690 0.097 Uiso 1 1 calc R U . . .
H19C H 1.039879 0.124788 0.188393 0.097 Uiso 1 1 calc R U . . .
C20 C 1.0572(2) -0.1202(3) 0.3565(2) 0.0502(5) Uani 1 1 d . . . . .
H20A H 1.103318 -0.179407 0.319901 0.075 Uiso 1 1 calc R U . . .
H20B H 1.024127 -0.175838 0.427669 0.075 Uiso 1 1 calc R U . . .
H20C H 1.118735 -0.061330 0.366677 0.075 Uiso 1 1 calc R U . . .
C21 C 0.8495(2) -0.1265(2) 0.26847(18) 0.0379(4) Uani 1 1 d . . . . .
H21A H 0.776182 -0.072391 0.221294 0.057 Uiso 1 1 calc R U . . .
H21B H 0.814151 -0.181987 0.338687 0.057 Uiso 1 1 calc R U . . .
H21C H 0.899755 -0.185738 0.233741 0.057 Uiso 1 1 calc R U . . .
C22 C 0.8660(2) 0.0528(2) 0.34785(18) 0.0382(4) Uani 1 1 d . . . . .
H22A H 0.789765 0.107946 0.304935 0.057 Uiso 1 1 calc R U . . .
H22B H 0.925376 0.112451 0.359822 0.057 Uiso 1 1 calc R U . . .
H22C H 0.834976 -0.006881 0.418253 0.057 Uiso 1 1 calc R U . . .
C1 C 0.82106(19) 0.3614(2) 0.86702(16) 0.0379(4) Uani 1 1 d . . . . .
F1A F 0.8632(5) 0.2609(2) 0.8313(2) 0.0856(17) Uani 0.716(6) 1 d . U P A 1
F2A F 0.7111(3) 0.3227(3) 0.9351(3) 0.0561(9) Uani 0.716(6) 1 d . U P A 1
F3A F 0.9102(3) 0.3531(4) 0.9496(2) 0.0819(14) Uani 0.716(6) 1 d . U P A 1
F1B F 0.7572(12) 0.2560(7) 0.8271(7) 0.060(2) Uani 0.229(6) 1 d . U P A 2
F2B F 0.812(2) 0.3376(12) 0.9710(8) 0.126(6) Uani 0.229(6) 1 d . U P A 2
F3B F 0.9434(5) 0.2735(6) 0.8865(8) 0.056(2) Uani 0.229(6) 1 d . U P A 2
C23 C 0.7230(16) 0.2778(14) 0.9242(17) 0.029(3) Uani 0.141(3) 1 d . . P A 3
F14 F 0.7756(9) 0.1746(8) 1.0220(6) 0.038(2) Uani 0.141(3) 1 d . . P A 3
F15 F 0.6261(8) 0.3489(8) 0.9677(6) 0.036(2) Uani 0.141(3) 1 d . . P A 3
F16 F 0.6754(11) 0.2250(10) 0.8665(7) 0.043(2) Uani 0.141(3) 1 d . . P A 3
F7 F 0.83692(18) 0.82776(15) 0.65730(16) 0.0624(6) Uani 0.925(3) 1 d . . P B 4
F8 F 0.8119(2) 0.7322(2) 0.53631(14) 0.0773(7) Uani 0.925(3) 1 d . . P B 4
F9 F 0.64316(17) 0.79423(19) 0.61941(18) 0.0791(7) Uani 0.925(3) 1 d . . P B 4
C2A C 0.9965(4) 0.5440(4) 0.7402(4) 0.0330(8) Uani 0.737(6) 1 d . . P C 5
F4A F 1.07160(18) 0.4261(2) 0.7536(3) 0.0641(10) Uani 0.737(6) 1 d . U P C 5
F5A F 1.0445(4) 0.6363(5) 0.6417(3) 0.0697(11) Uani 0.737(6) 1 d . U P C 5
F6A F 1.0464(2) 0.5905(5) 0.8153(3) 0.0869(14) Uani 0.737(6) 1 d . U P C 5
C2B C 0.976(2) 0.538(3) 0.721(2) 0.089(8) Uani 0.263(6) 1 d . . P C 6
F4B F 1.0709(8) 0.4827(12) 0.8208(13) 0.126(6) Uani 0.263(6) 1 d . U P C 6
F5B F 1.0566(8) 0.6455(8) 0.6916(10) 0.060(3) Uani 0.263(6) 1 d . U P C 6
F6B F 1.0261(9) 0.4706(11) 0.6431(12) 0.110(5) Uani 0.263(6) 1 d . U P C 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
N1 C4 1.350(2) . ?
N1 C5 1.392(2) . ?
N1 C7 1.423(3) . ?
N2 C4 1.352(2) . ?
N2 C6 1.399(2) . ?
N2 C13 1.416(3) . ?
N3 C19 1.482(3) . ?
N3 C21 1.487(2) . ?
N3 C22 1.492(2) . ?
N3 C20 1.505(3) . ?
C3 F7 1.318(3) . ?
C3 F8 1.364(3) . ?
C3 F9 1.377(2) . ?
C3 Ni1 1.970(2) . ?
C4 Ni1 1.8877(15) . ?
C5 C6 1.332(3) . ?
C7 C8 1.377(3) . ?
C7 C12 1.385(2) . ?
C8 F10 1.362(2) . ?
C8 C9 1.364(3) . ?
C9 C10 1.357(3) . ?
C10 F11 1.350(3) . ?
C10 C11 1.373(3) . ?
C11 C12 1.387(3) . ?
Ni1 C2B 1.77(2) . ?
Ni1 C1 1.949(2) . ?
Ni1 C2A 1.950(4) . ?
F12 C14 1.350(2) . ?
F13 C16 1.343(3) . ?
C13 C14 1.381(3) . ?
C13 C18 1.392(2) . ?
C14 C15 1.365(3) . ?
C15 C16 1.369(3) . ?
C16 C17 1.375(3) . ?
C17 C18 1.383(3) . ?
C1 F2B 1.270(10) . ?
C1 F1A 1.297(3) . ?
C1 F2A 1.375(3) . ?
C1 F3A 1.389(3) . ?
C1 C23 1.390(15) . ?
C1 F3B 1.407(5) . ?
C1 F1B 1.569(8) . ?
C23 F16 1.208(18) . ?
C23 F15 1.359(19) . ?
C23 F14 1.41(2) . ?
C2A F4A 1.315(4) . ?
C2A F6A 1.357(6) . ?
C2A F5A 1.395(5) . ?
C2B F5B 1.39(2) . ?
C2B F6B 1.44(3) . ?
C2B F4B 1.53(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 N1 C5 111.41(16) . . ?
C4 N1 C7 123.25(14) . . ?
C5 N1 C7 125.33(16) . . ?
C4 N2 C6 111.01(16) . . ?
C4 N2 C13 123.88(14) . . ?
C6 N2 C13 125.06(15) . . ?
C19 N3 C21 109.15(19) . . ?
C19 N3 C22 109.18(18) . . ?
C21 N3 C22 109.98(15) . . ?
C19 N3 C20 111.8(2) . . ?
C21 N3 C20 108.28(16) . . ?
C22 N3 C20 108.44(16) . . ?
F7 C3 F8 106.86(19) . . ?
F7 C3 F9 103.1(2) . . ?
F8 C3 F9 100.06(19) . . ?
F7 C3 Ni1 115.93(13) . . ?
F8 C3 Ni1 112.24(17) . . ?
F9 C3 Ni1 116.94(14) . . ?
N1 C4 N2 104.23(14) . . ?
N1 C4 Ni1 125.84(13) . . ?
N2 C4 Ni1 129.93(14) . . ?
C6 C5 N1 106.70(16) . . ?
C5 C6 N2 106.65(15) . . ?
C8 C7 C12 117.39(19) . . ?
C8 C7 N1 121.28(17) . . ?
C12 C7 N1 121.25(17) . . ?
F10 C8 C9 118.38(18) . . ?
F10 C8 C7 118.17(19) . . ?
C9 C8 C7 123.42(19) . . ?
C10 C9 C8 117.1(2) . . ?
F11 C10 C9 118.1(2) . . ?
F11 C10 C11 118.72(19) . . ?
C9 C10 C11 123.2(2) . . ?
C10 C11 C12 118.00(18) . . ?
C2B Ni1 C4 173.9(8) . . ?
C2B Ni1 C1 92.4(8) . . ?
C4 Ni1 C1 89.58(7) . . ?
C4 Ni1 C2A 176.33(15) . . ?
C1 Ni1 C2A 90.35(15) . . ?
C2B Ni1 C3 89.2(8) . . ?
C4 Ni1 C3 88.87(7) . . ?
C1 Ni1 C3 178.44(8) . . ?
C2A Ni1 C3 91.20(15) . . ?
C7 C12 C11 120.89(19) . . ?
C14 C13 C18 117.88(19) . . ?
C14 C13 N2 121.89(16) . . ?
C18 C13 N2 120.23(16) . . ?
F12 C14 C15 118.38(18) . . ?
F12 C14 C13 118.65(19) . . ?
C15 C14 C13 122.95(19) . . ?
C14 C15 C16 117.5(2) . . ?
F13 C16 C15 118.9(2) . . ?
F13 C16 C17 118.7(2) . . ?
C15 C16 C17 122.4(2) . . ?
C16 C17 C18 118.79(19) . . ?
C17 C18 C13 120.40(19) . . ?
F1A C1 F2A 107.4(3) . . ?
F1A C1 F3A 106.5(3) . . ?
F2A C1 F3A 97.1(2) . . ?
F2B C1 F3B 88.3(8) . . ?
F2B C1 F1B 114.7(10) . . ?
F3B C1 F1B 89.2(5) . . ?
F2B C1 Ni1 124.3(5) . . ?
F1A C1 Ni1 115.56(17) . . ?
F2A C1 Ni1 116.56(16) . . ?
F3A C1 Ni1 111.67(18) . . ?
C23 C1 Ni1 129.8(7) . . ?
F3B C1 Ni1 123.4(3) . . ?
F1B C1 Ni1 110.5(3) . . ?
F16 C23 F15 112.0(13) . . ?
F16 C23 C1 111.4(16) . . ?
F15 C23 C1 111.2(9) . . ?
F16 C23 F14 109.9(11) . . ?
F15 C23 F14 100.6(14) . . ?
C1 C23 F14 111.3(12) . . ?
F4A C2A F6A 103.9(4) . . ?
F4A C2A F5A 104.4(3) . . ?
F6A C2A F5A 100.2(4) . . ?
F4A C2A Ni1 119.0(3) . . ?
F6A C2A Ni1 111.3(2) . . ?
F5A C2A Ni1 115.8(4) . . ?
F5B C2B F6B 100.1(17) . . ?
F5B C2B F4B 81.1(12) . . ?
F6B C2B F4B 107.2(17) . . ?
F5B C2B Ni1 127.4(18) . . ?
F6B C2B Ni1 118.8(12) . . ?
F4B C2B Ni1 115.4(16) . . ?

_refine_diff_density_max         1.479
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_Schaefer_NS_K03_0m
_database_code_depnum_ccdc_archive 'CCDC 2126925'
loop_
_audit_author_name
_audit_author_address
'Sascha Schaefer'
;University of Cologne
Germany
;
_audit_update_record             
;
2022-01-09 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H76 F14 N2 Ni2 O2 P4'
_chemical_formula_weight         1652.76

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.807(2)
_cell_length_b                   20.672(4)
_cell_length_c                   15.556(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.953(7)
_cell_angle_gamma                90
_cell_volume                     3782.6(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    8936
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      26.40

_exptl_crystal_description       column
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_F_000             1704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.667
_shelx_estimated_absorpt_T_min   0.912
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6992
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83345
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.970
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7749
_reflns_number_gt                6350
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0511P)²+3.9217P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7749
_refine_ls_number_parameters     487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.1056
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.07963(2) 0.94878(2) 0.51344(2) 0.01789(9) Uani 1 1 d . . . . .
P1 P 0.24317(5) 0.70817(3) 0.54357(4) 0.01605(13) Uani 1 1 d . . . . .
F1 F 0.00743(13) 1.01182(7) 0.57759(9) 0.0322(4) Uani 1 1 d . . . . .
O1 O 0.2685(2) 0.49473(13) 0.46544(17) 0.0608(7) Uani 1 1 d . . . . .
N1 N 0.35806(16) 0.67729(9) 0.51708(12) 0.0184(4) Uani 1 1 d . . . . .
C1 C -0.1412(3) 0.91212(15) 0.60735(18) 0.0393(7) Uani 1 1 d . . . . .
C2 C -0.1585(2) 0.89371(12) 0.43532(16) 0.0240(5) Uani 1 1 d . . . . .
F3 F -0.1138(3) 0.84738(9) 0.62096(13) 0.0835(9) Uani 1 1 d . . . . .
C3 C 0.13374(19) 0.70063(11) 0.45643(15) 0.0202(5) Uani 1 1 d . . . . .
F4 F -0.25523(19) 0.91254(15) 0.60853(13) 0.0860(9) Uani 1 1 d . . . . .
C4 C 0.0223(2) 0.71970(13) 0.46765(17) 0.0267(5) Uani 1 1 d . . . . .
H4 H 0.005395 0.740497 0.519477 0.032 Uiso 1 1 calc R U . . .
F5 F -0.22618(17) 0.84480(10) 0.45803(12) 0.0526(5) Uani 1 1 d . . . . .
C5 C -0.0633(2) 0.70810(13) 0.40278(17) 0.0295(6) Uani 1 1 d . . . . .
H5 H -0.139080 0.721025 0.410099 0.035 Uiso 1 1 calc R U . . .
F6 F -0.2247(2) 0.92547(9) 0.37461(15) 0.0720(8) Uani 1 1 d . . . . .
C6 C -0.0385(2) 0.67762(13) 0.32715(17) 0.0283(6) Uani 1 1 d . . . . .
H6 H -0.097582 0.669293 0.283152 0.034 Uiso 1 1 calc R U . . .
F7 F -0.08443(15) 0.86030(10) 0.38874(13) 0.0539(5) Uani 1 1 d . . . . .
C7 C 0.0719(2) 0.65930(13) 0.31550(16) 0.0268(5) Uani 1 1 d . . . . .
H7 H 0.088503 0.638929 0.263309 0.032 Uiso 1 1 calc R U . . .
C8 C 0.1582(2) 0.67065(12) 0.37994(16) 0.0225(5) Uani 1 1 d . . . . .
H8 H 0.233892 0.658011 0.371961 0.027 Uiso 1 1 calc R U . . .
C9 C 0.19377(18) 0.66327(11) 0.63179(14) 0.0183(5) Uani 1 1 d . . . . .
C10 C 0.21084(19) 0.59645(11) 0.63539(15) 0.0201(5) Uani 1 1 d . . . . .
H10 H 0.251697 0.575424 0.593407 0.024 Uiso 1 1 calc R U . . .
C15 C 0.25482(19) 0.79094(11) 0.57821(15) 0.0187(5) Uani 1 1 d . . . . .
C14 C 0.1330(2) 0.69366(12) 0.69343(15) 0.0222(5) Uani 1 1 d . . . . .
H14 H 0.120377 0.739022 0.690497 0.027 Uiso 1 1 calc R U . . .
C11 C 0.1674(2) 0.56099(12) 0.70106(16) 0.0237(5) Uani 1 1 d . . . . .
H11 H 0.178640 0.515501 0.703700 0.028 Uiso 1 1 calc R U . . .
C12 C 0.1076(2) 0.59140(13) 0.76297(16) 0.0263(5) Uani 1 1 d . . . . .
H12 H 0.078434 0.566792 0.807676 0.032 Uiso 1 1 calc R U . . .
C13 C 0.0909(2) 0.65768(13) 0.75910(16) 0.0258(5) Uani 1 1 d . . . . .
H13 H 0.050588 0.678617 0.801462 0.031 Uiso 1 1 calc R U . . .
C16 C 0.2058(2) 0.84190(12) 0.52964(17) 0.0266(5) Uani 1 1 d . . . . .
H16 H 0.160984 0.833722 0.477077 0.032 Uiso 1 1 calc R U . . .
C18 C 0.2875(2) 0.91710(13) 0.6358(2) 0.0347(6) Uani 1 1 d . . . . .
H18 H 0.297459 0.960343 0.655683 0.042 Uiso 1 1 calc R U . . .
C19 C 0.3373(2) 0.86663(12) 0.68384(17) 0.0272(5) Uani 1 1 d . . . . .
H19 H 0.382034 0.875168 0.736343 0.033 Uiso 1 1 calc R U . . .
C20 C 0.3216(2) 0.80373(12) 0.65498(15) 0.0217(5) Uani 1 1 d . . . . .
H20 H 0.356304 0.769027 0.687484 0.026 Uiso 1 1 calc R U . . .
C21 C 0.46824(18) 0.78774(11) 0.45374(15) 0.0179(4) Uani 1 1 d . . . . .
C22 C 0.4015(2) 0.79923(12) 0.37634(15) 0.0221(5) Uani 1 1 d . . . . .
H22 H 0.366806 0.764076 0.344761 0.026 Uiso 1 1 calc R U . . .
C23 C 0.3861(2) 0.86177(13) 0.34592(17) 0.0280(6) Uani 1 1 d . . . . .
H23 H 0.340805 0.869582 0.293469 0.034 Uiso 1 1 calc R U . . .
C24 C 0.4366(2) 0.91286(13) 0.39187(18) 0.0335(6) Uani 1 1 d . . . . .
H24 H 0.425596 0.955774 0.370936 0.040 Uiso 1 1 calc R U . . .
C25 C 0.5032(2) 0.90200(13) 0.46817(18) 0.0322(6) Uani 1 1 d . . . . .
H25 H 0.538363 0.937352 0.499037 0.039 Uiso 1 1 calc R U . . .
C26 C 0.5187(2) 0.83927(12) 0.49974(16) 0.0243(5) Uani 1 1 d . . . . .
H26 H 0.563602 0.831781 0.552467 0.029 Uiso 1 1 calc R U . . .
C27 C 0.58101(19) 0.70082(11) 0.58298(14) 0.0174(4) Uani 1 1 d . . . . .
C28 C 0.5540(2) 0.67108(11) 0.65912(15) 0.0213(5) Uani 1 1 d . . . . .
H28 H 0.479170 0.655505 0.664035 0.026 Uiso 1 1 calc R U . . .
C29 C 0.6363(2) 0.66426(12) 0.72752(16) 0.0261(5) Uani 1 1 d . . . . .
H29 H 0.617911 0.644232 0.779481 0.031 Uiso 1 1 calc R U . . .
C30 C 0.7456(2) 0.68672(12) 0.72004(16) 0.0263(5) Uani 1 1 d . . . . .
H30 H 0.802221 0.681640 0.766807 0.032 Uiso 1 1 calc R U . . .
C31 C 0.7729(2) 0.71647(12) 0.64489(16) 0.0240(5) Uani 1 1 d . . . . .
H31 H 0.847680 0.732312 0.640578 0.029 Uiso 1 1 calc R U . . .
C32 C 0.6915(2) 0.72326(12) 0.57595(16) 0.0219(5) Uani 1 1 d . . . . .
H32 H 0.710613 0.743088 0.524051 0.026 Uiso 1 1 calc R U . . .
C33 C 0.52674(18) 0.65625(11) 0.40901(14) 0.0180(5) Uani 1 1 d . . . . .
C34 C 0.5034(2) 0.58997(12) 0.40967(15) 0.0219(5) Uani 1 1 d . . . . .
H34 H 0.457988 0.572231 0.451337 0.026 Uiso 1 1 calc R U . . .
C35 C 0.5477(2) 0.55029(13) 0.34843(17) 0.0278(5) Uani 1 1 d . . . . .
H35 H 0.532922 0.505120 0.348775 0.033 Uiso 1 1 calc R U . . .
C36 C 0.6131(2) 0.57599(13) 0.28705(17) 0.0286(6) Uani 1 1 d . . . . .
H36 H 0.642308 0.548436 0.245349 0.034 Uiso 1 1 calc R U . . .
C37 C 0.6362(2) 0.64161(13) 0.28613(16) 0.0269(5) Uani 1 1 d . . . . .
H37 H 0.680963 0.659154 0.243900 0.032 Uiso 1 1 calc R U . . .
C38 C 0.5933(2) 0.68183(12) 0.34756(15) 0.0228(5) Uani 1 1 d . . . . .
H38 H 0.609506 0.726842 0.347506 0.027 Uiso 1 1 calc R U . . .
C39 C 0.2011(3) 0.44365(16) 0.4962(2) 0.0505(9) Uani 1 1 d . . . . .
H39A H 0.178448 0.454052 0.554448 0.061 Uiso 1 1 calc R U . . .
H39B H 0.244646 0.402655 0.499496 0.061 Uiso 1 1 calc R U . . .
C40 C 0.0970(3) 0.43744(17) 0.4324(2) 0.0478(8) Uani 1 1 d . . . . .
H40A H 0.028409 0.454043 0.457450 0.057 Uiso 1 1 calc R U . . .
H40B H 0.084025 0.391815 0.414950 0.057 Uiso 1 1 calc R U . . .
C41 C 0.1258(3) 0.4785(2) 0.3564(3) 0.0846(16) Uani 1 1 d . . . . .
H41A H 0.113489 0.453885 0.301797 0.101 Uiso 1 1 calc R U . . .
H41B H 0.078512 0.518086 0.351846 0.101 Uiso 1 1 calc R U . . .
C42 C 0.2481(3) 0.49515(17) 0.3750(2) 0.0505(8) Uani 1 1 d . . . . .
H42A H 0.296683 0.462888 0.348894 0.061 Uiso 1 1 calc R U . . .
H42B H 0.264169 0.538405 0.351652 0.061 Uiso 1 1 calc R U . . .
C17 C 0.2234(2) 0.90482(13) 0.5591(2) 0.0351(6) Uani 1 1 d . . . . .
H17 H 0.190841 0.939849 0.525995 0.042 Uiso 1 1 calc R U . . .
P2 P 0.47576(5) 0.70585(3) 0.49277(4) 0.01544(13) Uani 1 1 d . . . . .
F2 F -0.10356(16) 0.93824(8) 0.68587(10) 0.0403(4) 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 C1 1.849(3) . ?
Ni1 C2 1.856(2) . ?
Ni1 F1 1.8903(15) . ?
Ni1 F1 1.8984(15) 3_576 ?
Ni1 Ni1 2.8864(7) 3_576 ?
P1 N1 1.5855(19) . ?
P1 C9 1.795(2) . ?
P1 C15 1.796(2) . ?
P1 C3 1.797(2) . ?
O1 C42 1.406(4) . ?
O1 C39 1.429(4) . ?
N1 P2 1.5853(19) . ?
C1 F4 1.349(4) . ?
C1 F2 1.374(3) . ?
C1 F3 1.389(4) . ?
C2 F6 1.344(3) . ?
C2 F5 1.355(3) . ?
C2 F7 1.370(3) . ?
C3 C8 1.394(3) . ?
C3 C4 1.399(3) . ?
C4 C5 1.386(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.384(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.386(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C14 1.396(3) . ?
C9 C10 1.396(3) . ?
C10 C11 1.391(3) . ?
C10 H10 0.9500 . ?
C15 C16 1.393(3) . ?
C15 C20 1.398(3) . ?
C14 C13 1.390(3) . ?
C14 H14 0.9500 . ?
C11 C12 1.392(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C16 C17 1.388(4) . ?
C16 H16 0.9500 . ?
C18 C17 1.380(4) . ?
C18 C19 1.385(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.389(3) . ?
C21 C22 1.401(3) . ?
C21 P2 1.798(2) . ?
C22 C23 1.383(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.393(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.395(3) . ?
C27 C32 1.397(3) . ?
C27 P2 1.795(2) . ?
C28 C29 1.385(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.386(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.383(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.384(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.393(3) . ?
C33 C34 1.398(3) . ?
C33 P2 1.802(2) . ?
C34 C35 1.393(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.385(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.384(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.394(3) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.517(5) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.518(6) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.488(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C17 H17 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni1 C2 93.26(11) . . ?
C1 Ni1 F1 95.64(10) . . ?
C2 Ni1 F1 171.00(9) . . ?
C1 Ni1 F1 175.93(11) . 3_576 ?
C2 Ni1 F1 90.39(9) . 3_576 ?
F1 Ni1 F1 80.75(7) . 3_576 ?
C1 Ni1 Ni1 136.09(9) . 3_576 ?
C2 Ni1 Ni1 130.64(8) . 3_576 ?
F1 Ni1 Ni1 40.48(5) . 3_576 ?
F1 Ni1 Ni1 40.27(4) 3_576 3_576 ?
N1 P1 C9 109.41(11) . . ?
N1 P1 C15 114.62(10) . . ?
C9 P1 C15 106.55(11) . . ?
N1 P1 C3 110.15(11) . . ?
C9 P1 C3 105.77(11) . . ?
C15 P1 C3 109.91(11) . . ?
Ni1 F1 Ni1 99.26(7) . 3_576 ?
C42 O1 C39 106.7(2) . . ?
P2 N1 P1 134.37(13) . . ?
F4 C1 F2 103.4(2) . . ?
F4 C1 F3 102.9(3) . . ?
F2 C1 F3 101.0(2) . . ?
F4 C1 Ni1 118.0(2) . . ?
F2 C1 Ni1 114.99(18) . . ?
F3 C1 Ni1 114.4(2) . . ?
F6 C2 F5 103.1(2) . . ?
F6 C2 F7 103.5(2) . . ?
F5 C2 F7 100.3(2) . . ?
F6 C2 Ni1 112.89(17) . . ?
F5 C2 Ni1 124.12(18) . . ?
F7 C2 Ni1 110.42(16) . . ?
C8 C3 C4 119.9(2) . . ?
C8 C3 P1 119.63(18) . . ?
C4 C3 P1 120.27(18) . . ?
C5 C4 C3 119.7(2) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.1(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 120.4(2) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 120.0(2) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.0(2) . . ?
C7 C8 H8 120.0 . . ?
C3 C8 H8 120.0 . . ?
C14 C9 C10 119.9(2) . . ?
C14 C9 P1 120.85(18) . . ?
C10 C9 P1 119.13(18) . . ?
C11 C10 C9 119.3(2) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C16 C15 C20 119.8(2) . . ?
C16 C15 P1 122.72(19) . . ?
C20 C15 P1 117.34(18) . . ?
C13 C14 C9 120.1(2) . . ?
C13 C14 H14 119.9 . . ?
C9 C14 H14 119.9 . . ?
C10 C11 C12 120.7(2) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C12 C11 119.7(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 120.2(2) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C17 C16 C15 119.1(2) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C17 C18 C19 120.3(2) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 119.6(2) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C15 120.3(2) . . ?
C19 C20 H20 119.8 . . ?
C15 C20 H20 119.8 . . ?
C26 C21 C22 119.8(2) . . ?
C26 C21 P2 122.80(18) . . ?
C22 C21 P2 117.22(18) . . ?
C23 C22 C21 120.0(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 120.0(2) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 120.5(2) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C26 120.1(3) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 119.7(2) . . ?
C21 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C32 119.7(2) . . ?
C28 C27 P2 119.71(17) . . ?
C32 C27 P2 120.48(18) . . ?
C29 C28 C27 120.0(2) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 119.9(2) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C31 C30 C29 120.4(2) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C30 C31 C32 120.2(2) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C27 119.7(2) . . ?
C31 C32 H32 120.1 . . ?
C27 C32 H32 120.1 . . ?
C38 C33 C34 120.0(2) . . ?
C38 C33 P2 121.57(18) . . ?
C34 C33 P2 118.31(17) . . ?
C35 C34 C33 119.1(2) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C36 C35 C34 120.7(2) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C37 C36 C35 120.3(2) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C38 119.6(2) . . ?
C36 C37 H37 120.2 . . ?
C38 C37 H37 120.2 . . ?
C33 C38 C37 120.2(2) . . ?
C33 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
O1 C39 C40 106.6(3) . . ?
O1 C39 H39A 110.4 . . ?
C40 C39 H39A 110.4 . . ?
O1 C39 H39B 110.4 . . ?
C40 C39 H39B 110.4 . . ?
H39A C39 H39B 108.6 . . ?
C39 C40 C41 103.8(3) . . ?
C39 C40 H40A 111.0 . . ?
C41 C40 H40A 111.0 . . ?
C39 C40 H40B 111.0 . . ?
C41 C40 H40B 111.0 . . ?
H40A C40 H40B 109.0 . . ?
C42 C41 C40 104.8(3) . . ?
C42 C41 H41A 110.8 . . ?
C40 C41 H41A 110.8 . . ?
C42 C41 H41B 110.8 . . ?
C40 C41 H41B 110.8 . . ?
H41A C41 H41B 108.9 . . ?
O1 C42 C41 105.9(3) . . ?
O1 C42 H42A 110.6 . . ?
C41 C42 H42A 110.6 . . ?
O1 C42 H42B 110.6 . . ?
C41 C42 H42B 110.6 . . ?
H42A C42 H42B 108.7 . . ?
C18 C17 C16 120.8(3) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
N1 P2 C27 110.72(11) . . ?
N1 P2 C21 114.36(10) . . ?
C27 P2 C21 109.22(11) . . ?
N1 P2 C33 108.36(10) . . ?
C27 P2 C33 106.28(10) . . ?
C21 P2 C33 107.54(11) . . ?

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 Ni1 F1 Ni1 178.11(12) . . . 3_576 ?
F1 Ni1 F1 Ni1 0.0 3_576 . . 3_576 ?
C9 P1 N1 P2 -136.84(17) . . . . ?
C15 P1 N1 P2 -17.3(2) . . . . ?
C3 P1 N1 P2 107.29(18) . . . . ?
C2 Ni1 C1 F4 -58.6(3) . . . . ?
F1 Ni1 C1 F4 120.1(2) . . . . ?
Ni1 Ni1 C1 F4 121.8(2) 3_576 . . . ?
C2 Ni1 C1 F2 178.9(2) . . . . ?
F1 Ni1 C1 F2 -2.4(3) . . . . ?
Ni1 Ni1 C1 F2 -0.7(3) 3_576 . . . ?
C2 Ni1 C1 F3 62.6(2) . . . . ?
F1 Ni1 C1 F3 -118.7(2) . . . . ?
Ni1 Ni1 C1 F3 -116.9(2) 3_576 . . . ?
C1 Ni1 C2 F6 122.1(2) . . . . ?
F1 Ni1 C2 F6 -59.7(2) 3_576 . . . ?
Ni1 Ni1 C2 F6 -58.4(2) 3_576 . . . ?
C1 Ni1 C2 F5 -3.6(2) . . . . ?
F1 Ni1 C2 F5 174.6(2) 3_576 . . . ?
Ni1 Ni1 C2 F5 175.92(16) 3_576 . . . ?
C1 Ni1 C2 F7 -122.6(2) . . . . ?
F1 Ni1 C2 F7 55.64(18) 3_576 . . . ?
Ni1 Ni1 C2 F7 57.0(2) 3_576 . . . ?
N1 P1 C3 C8 0.1(2) . . . . ?
C9 P1 C3 C8 -118.0(2) . . . . ?
C15 P1 C3 C8 127.31(19) . . . . ?
N1 P1 C3 C4 174.69(19) . . . . ?
C9 P1 C3 C4 56.6(2) . . . . ?
C15 P1 C3 C4 -58.1(2) . . . . ?
C8 C3 C4 C5 0.6(4) . . . . ?
P1 C3 C4 C5 -174.0(2) . . . . ?
C3 C4 C5 C6 0.1(4) . . . . ?
C4 C5 C6 C7 -0.8(4) . . . . ?
C5 C6 C7 C8 0.8(4) . . . . ?
C6 C7 C8 C3 -0.1(4) . . . . ?
C4 C3 C8 C7 -0.6(4) . . . . ?
P1 C3 C8 C7 174.06(19) . . . . ?
N1 P1 C9 C14 148.65(19) . . . . ?
C15 P1 C9 C14 24.2(2) . . . . ?
C3 P1 C9 C14 -92.7(2) . . . . ?
N1 P1 C9 C10 -35.2(2) . . . . ?
C15 P1 C9 C10 -159.62(18) . . . . ?
C3 P1 C9 C10 83.4(2) . . . . ?
C14 C9 C10 C11 -0.4(3) . . . . ?
P1 C9 C10 C11 -176.60(18) . . . . ?
N1 P1 C15 C16 110.1(2) . . . . ?
C9 P1 C15 C16 -128.7(2) . . . . ?
C3 P1 C15 C16 -14.6(2) . . . . ?
N1 P1 C15 C20 -66.3(2) . . . . ?
C9 P1 C15 C20 54.9(2) . . . . ?
C3 P1 C15 C20 169.06(17) . . . . ?
C10 C9 C14 C13 1.0(3) . . . . ?
P1 C9 C14 C13 177.08(19) . . . . ?
C9 C10 C11 C12 -0.1(4) . . . . ?
C10 C11 C12 C13 0.2(4) . . . . ?
C11 C12 C13 C14 0.4(4) . . . . ?
C9 C14 C13 C12 -1.0(4) . . . . ?
C20 C15 C16 C17 -0.7(4) . . . . ?
P1 C15 C16 C17 -177.0(2) . . . . ?
C17 C18 C19 C20 -0.6(4) . . . . ?
C18 C19 C20 C15 -0.7(4) . . . . ?
C16 C15 C20 C19 1.3(3) . . . . ?
P1 C15 C20 C19 177.80(18) . . . . ?
C26 C21 C22 C23 0.0(3) . . . . ?
P2 C21 C22 C23 175.67(18) . . . . ?
C21 C22 C23 C24 0.0(4) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C23 C24 C25 C26 -0.7(4) . . . . ?
C22 C21 C26 C25 -0.5(4) . . . . ?
P2 C21 C26 C25 -175.8(2) . . . . ?
C24 C25 C26 C21 0.8(4) . . . . ?
C32 C27 C28 C29 0.4(3) . . . . ?
P2 C27 C28 C29 176.92(19) . . . . ?
C27 C28 C29 C30 -0.3(4) . . . . ?
C28 C29 C30 C31 0.6(4) . . . . ?
C29 C30 C31 C32 -0.9(4) . . . . ?
C30 C31 C32 C27 1.0(4) . . . . ?
C28 C27 C32 C31 -0.7(3) . . . . ?
P2 C27 C32 C31 -177.22(18) . . . . ?
C38 C33 C34 C35 0.1(3) . . . . ?
P2 C33 C34 C35 -176.32(18) . . . . ?
C33 C34 C35 C36 -0.6(4) . . . . ?
C34 C35 C36 C37 0.5(4) . . . . ?
C35 C36 C37 C38 0.1(4) . . . . ?
C34 C33 C38 C37 0.5(3) . . . . ?
P2 C33 C38 C37 176.81(18) . . . . ?
C36 C37 C38 C33 -0.6(4) . . . . ?
C42 O1 C39 C40 -30.0(4) . . . . ?
O1 C39 C40 C41 11.7(4) . . . . ?
C39 C40 C41 C42 9.4(5) . . . . ?
C39 O1 C42 C41 36.3(4) . . . . ?
C40 C41 C42 O1 -27.9(5) . . . . ?
C19 C18 C17 C16 1.3(4) . . . . ?
C15 C16 C17 C18 -0.6(4) . . . . ?
P1 N1 P2 C27 100.58(18) . . . . ?
P1 N1 P2 C21 -23.3(2) . . . . ?
P1 N1 P2 C33 -143.23(17) . . . . ?
C28 C27 P2 N1 3.5(2) . . . . ?
C32 C27 P2 N1 179.95(18) . . . . ?
C28 C27 P2 C21 130.26(19) . . . . ?
C32 C27 P2 C21 -53.3(2) . . . . ?
C28 C27 P2 C33 -114.00(19) . . . . ?
C32 C27 P2 C33 62.5(2) . . . . ?
C26 C21 P2 N1 111.9(2) . . . . ?
C22 C21 P2 N1 -63.6(2) . . . . ?
C26 C21 P2 C27 -12.8(2) . . . . ?
C22 C21 P2 C27 171.71(17) . . . . ?
C26 C21 P2 C33 -127.7(2) . . . . ?
C22 C21 P2 C33 56.8(2) . . . . ?
C38 C33 P2 N1 149.69(19) . . . . ?
C34 C33 P2 N1 -33.9(2) . . . . ?
C38 C33 P2 C27 -91.3(2) . . . . ?
C34 C33 P2 C27 85.11(19) . . . . ?
C38 C33 P2 C21 25.6(2) . . . . ?
C34 C33 P2 C21 -158.02(18) . . . . ?

_refine_diff_density_max         0.695
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.068


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF, n-pentane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_Schaefer_RJ_P_37_0m
_database_code_depnum_ccdc_archive 'CCDC 2095551'
loop_
_audit_author_name
_audit_author_address
'Sascha Schaefer'
;University of Cologne
Germany
;
_audit_update_record             
;
2022-01-22 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H47 F9 N3 Ni P'
_chemical_formula_weight         950.58

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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+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                   19.9610(11)
_cell_length_b                   11.2347(6)
_cell_length_c                   40.329(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.043(2)
_cell_angle_gamma                90
_cell_volume                     8975.8(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9760
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      29.27

_exptl_crystal_description       hexagon
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             3936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.544
_shelx_estimated_absorpt_T_min   0.963
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source.source            'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement.device       'KAPPA diffractometer'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            137625
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_theta_min         2.035
_diffrn_reflns_theta_max         29.599
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12599
_reflns_number_gt                10876
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+16.6147P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12599
_refine_ls_number_parameters     621
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0957
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.28951(2) 0.58068(2) 0.65206(2) 0.01101(5) Uani 1 1 d . . . . .
P1 P 0.50538(2) 0.23890(4) 0.53634(2) 0.01331(9) Uani 1 1 d . . . . .
F1 F 0.23915(7) 0.46822(10) 0.70779(3) 0.0253(3) Uani 1 1 d . . . . .
N1 N 0.35913(7) 0.70849(13) 0.71097(4) 0.0134(3) Uani 1 1 d . . . . .
C1 C 0.24523(9) 0.45454(16) 0.67405(5) 0.0169(3) Uani 1 1 d . . . . .
F2 F 0.27425(7) 0.34296(10) 0.67400(3) 0.0251(3) Uani 1 1 d . . . . .
N2 N 0.25133(7) 0.73033(13) 0.70688(4) 0.0132(3) Uani 1 1 d . . . . .
F3 F 0.17918(6) 0.43286(13) 0.66091(4) 0.0349(3) Uani 1 1 d . . . . .
N3 N 0.24594(15) 0.4926(2) 0.42787(7) 0.0585(8) Uani 1 1 d . . . . .
C3 C 0.33273(9) 0.70594(16) 0.62897(4) 0.0149(3) Uani 1 1 d . . . . .
C4 C 0.30074(9) 0.67480(15) 0.69191(4) 0.0121(3) Uani 1 1 d . . . . .
C5 C 0.34574(10) 0.78367(16) 0.73689(4) 0.0171(4) Uani 1 1 d . . . . .
H5 H 0.378062 0.818310 0.753334 0.020 Uiso 1 1 calc R U . . .
C6 C 0.27869(10) 0.79774(16) 0.73420(4) 0.0164(3) Uani 1 1 d . . . . .
H6 H 0.254411 0.844757 0.748257 0.020 Uiso 1 1 calc R U . . .
F7 F 0.30126(6) 0.73787(10) 0.59788(3) 0.0224(2) Uani 1 1 d . . . . .
C7 C 0.42700(9) 0.67920(16) 0.70506(4) 0.0148(3) Uani 1 1 d . . . . .
F8 F 0.34176(6) 0.81748(9) 0.64413(3) 0.0189(2) Uani 1 1 d . . . . .
C8 C 0.47042(9) 0.77089(17) 0.69784(5) 0.0174(4) Uani 1 1 d . . . . .
F9 F 0.39779(6) 0.68044(11) 0.62275(3) 0.0255(3) Uani 1 1 d . . . . .
C9 C 0.53558(10) 0.74118(19) 0.69171(5) 0.0216(4) Uani 1 1 d . . . . .
H9 H 0.565117 0.802368 0.686162 0.026 Uiso 1 1 calc R U . . .
C10 C 0.55840(10) 0.6240(2) 0.69351(5) 0.0233(4) Uani 1 1 d . . . . .
C11 C 0.51504(10) 0.53657(19) 0.70186(5) 0.0239(4) Uani 1 1 d . . . . .
H11 H 0.530531 0.456573 0.703381 0.029 Uiso 1 1 calc R U . . .
C12 C 0.44913(10) 0.56104(17) 0.70819(5) 0.0186(4) Uani 1 1 d . . . . .
C13 C 0.45091(10) 0.90050(17) 0.69749(5) 0.0226(4) Uani 1 1 d . . . . .
H13A H 0.478381 0.944788 0.683155 0.034 Uiso 1 1 calc R U . . .
H13B H 0.458583 0.932322 0.720268 0.034 Uiso 1 1 calc R U . . .
H13C H 0.403072 0.908687 0.688832 0.034 Uiso 1 1 calc R U . . .
C14 C 0.62985(11) 0.5951(2) 0.68716(6) 0.0343(5) Uani 1 1 d . . . . .
H14A H 0.650033 0.539217 0.704191 0.051 Uiso 1 1 calc R U . . .
H14B H 0.656649 0.668373 0.688174 0.051 Uiso 1 1 calc R U . . .
H14C H 0.629081 0.558982 0.664993 0.051 Uiso 1 1 calc R U . . .
C15 C 0.40560(11) 0.46317(18) 0.71894(6) 0.0252(4) Uani 1 1 d . . . . .
H15A H 0.378185 0.429782 0.699317 0.038 Uiso 1 1 calc R U . . .
H15B H 0.375920 0.495090 0.734427 0.038 Uiso 1 1 calc R U . . .
H15C H 0.434229 0.400616 0.730118 0.038 Uiso 1 1 calc R U . . .
C16 C 0.17926(9) 0.71958(15) 0.69850(4) 0.0138(3) Uani 1 1 d . . . . .
C17 C 0.14177(10) 0.67174(16) 0.72261(5) 0.0166(3) Uani 1 1 d . . . . .
C18 C 0.07167(10) 0.66561(17) 0.71474(5) 0.0193(4) Uani 1 1 d . . . . .
H18 H 0.045648 0.631973 0.730590 0.023 Uiso 1 1 calc R U . . .
C19 C 0.03868(10) 0.70688(17) 0.68462(5) 0.0198(4) Uani 1 1 d . . . . .
C20 C 0.07756(10) 0.75541(17) 0.66190(5) 0.0189(4) Uani 1 1 d . . . . .
H20 H 0.055633 0.784242 0.641216 0.023 Uiso 1 1 calc R U . . .
C21 C 0.14759(9) 0.76367(16) 0.66814(5) 0.0160(3) Uani 1 1 d . . . . .
C22 C 0.17394(11) 0.62815(18) 0.75627(5) 0.0216(4) Uani 1 1 d . . . . .
H22A H 0.218841 0.595982 0.754137 0.032 Uiso 1 1 calc R U . . .
H22B H 0.145766 0.565659 0.764357 0.032 Uiso 1 1 calc R U . . .
H22C H 0.178072 0.694524 0.772157 0.032 Uiso 1 1 calc R U . . .
C23 C -0.03699(10) 0.7003(2) 0.67609(6) 0.0280(5) Uani 1 1 d . . . . .
H23A H -0.054422 0.778746 0.668726 0.042 Uiso 1 1 calc R U . . .
H23B H -0.057436 0.675613 0.695875 0.042 Uiso 1 1 calc R U . . .
H23C H -0.048239 0.642302 0.658117 0.042 Uiso 1 1 calc R U . . .
C24 C 0.18528(10) 0.82049(19) 0.64227(5) 0.0216(4) Uani 1 1 d . . . . .
H24A H 0.200146 0.758836 0.627610 0.032 Uiso 1 1 calc R U . . .
H24B H 0.224717 0.862951 0.653345 0.032 Uiso 1 1 calc R U . . .
H24C H 0.155591 0.876753 0.628978 0.032 Uiso 1 1 calc R U . . .
C25 C 0.57429(9) 0.22485(16) 0.51225(5) 0.0156(3) Uani 1 1 d . . . . .
C26 C 0.62543(10) 0.14130(17) 0.52012(5) 0.0186(4) Uani 1 1 d . . . . .
H26 H 0.624215 0.089089 0.538563 0.022 Uiso 1 1 calc R U . . .
C27 C 0.67808(10) 0.13525(19) 0.50072(5) 0.0235(4) Uani 1 1 d . . . . .
H27 H 0.712909 0.078142 0.505846 0.028 Uiso 1 1 calc R U . . .
C28 C 0.68036(10) 0.2115(2) 0.47397(5) 0.0241(4) Uani 1 1 d . . . . .
H28 H 0.716587 0.206357 0.460805 0.029 Uiso 1 1 calc R U . . .
C29 C 0.62990(11) 0.2957(2) 0.46630(5) 0.0240(4) Uani 1 1 d . . . . .
H29 H 0.631932 0.348688 0.448082 0.029 Uiso 1 1 calc R U . . .
C30 C 0.57657(10) 0.30248(18) 0.48523(5) 0.0207(4) Uani 1 1 d . . . . .
H30 H 0.541739 0.359454 0.479908 0.025 Uiso 1 1 calc R U . . .
C31 C 0.51701(9) 0.36802(16) 0.56238(5) 0.0156(3) Uani 1 1 d . . . . .
C32 C 0.47362(10) 0.38364(17) 0.58690(5) 0.0196(4) Uani 1 1 d . . . . .
H32 H 0.439449 0.326576 0.589339 0.024 Uiso 1 1 calc R U . . .
C33 C 0.48077(11) 0.48235(18) 0.60749(5) 0.0233(4) Uani 1 1 d . . . . .
H33 H 0.451580 0.493163 0.624162 0.028 Uiso 1 1 calc R U . . .
C34 C 0.53046(11) 0.56531(18) 0.60379(5) 0.0263(4) Uani 1 1 d . . . . .
H34 H 0.534725 0.633656 0.617762 0.032 Uiso 1 1 calc R U . . .
C35 C 0.57412(11) 0.54994(18) 0.57993(6) 0.0257(4) Uani 1 1 d . . . . .
H35 H 0.608464 0.607010 0.577829 0.031 Uiso 1 1 calc R U . . .
C36 C 0.56766(10) 0.45079(17) 0.55904(5) 0.0201(4) Uani 1 1 d . . . . .
H36 H 0.597502 0.439772 0.542667 0.024 Uiso 1 1 calc R U . . .
C37 C 0.49869(9) 0.11371(15) 0.56325(4) 0.0148(3) Uani 1 1 d . . . . .
C38 C 0.44067(10) 0.04275(17) 0.56015(5) 0.0177(4) Uani 1 1 d . . . . .
H38 H 0.404834 0.058140 0.542919 0.021 Uiso 1 1 calc R U . . .
C39 C 0.43574(10) -0.05046(17) 0.58242(5) 0.0215(4) Uani 1 1 d . . . . .
H39 H 0.396170 -0.098180 0.580628 0.026 Uiso 1 1 calc R U . . .
C40 C 0.48860(11) -0.07377(18) 0.60726(5) 0.0233(4) Uani 1 1 d . . . . .
H40 H 0.485323 -0.138362 0.622176 0.028 Uiso 1 1 calc R U . . .
C41 C 0.54626(11) -0.00341(18) 0.61048(5) 0.0224(4) Uani 1 1 d . . . . .
H41 H 0.582258 -0.020011 0.627527 0.027 Uiso 1 1 calc R U . . .
C42 C 0.55123(10) 0.09112(17) 0.58879(5) 0.0185(4) Uani 1 1 d . . . . .
H42 H 0.590196 0.140415 0.591258 0.022 Uiso 1 1 calc R U . . .
C43 C 0.42998(9) 0.25047(16) 0.50742(5) 0.0157(3) Uani 1 1 d . . . . .
C44 C 0.37864(10) 0.33126(18) 0.51215(5) 0.0209(4) Uani 1 1 d . . . . .
H44 H 0.383870 0.385349 0.530394 0.025 Uiso 1 1 calc R U . . .
C45 C 0.32003(11) 0.3311(2) 0.48980(6) 0.0271(4) Uani 1 1 d . . . . .
H45 H 0.285153 0.386391 0.492640 0.033 Uiso 1 1 calc R U . . .
C46 C 0.31167(11) 0.25159(19) 0.46341(5) 0.0252(4) Uani 1 1 d . . . . .
H46 H 0.270734 0.251321 0.448657 0.030 Uiso 1 1 calc R U . . .
C47 C 0.36281(11) 0.17210(18) 0.45835(5) 0.0229(4) Uani 1 1 d . . . . .
H47 H 0.357246 0.118330 0.440040 0.027 Uiso 1 1 calc R U . . .
C48 C 0.42213(10) 0.17199(17) 0.48032(5) 0.0200(4) Uani 1 1 d . . . . .
H48 H 0.457471 0.118421 0.476913 0.024 Uiso 1 1 calc R U . . .
C49 C 0.20840(15) 0.4036(2) 0.36912(8) 0.0444(7) Uani 1 1 d . . . . .
H49A H 0.170600 0.449806 0.357892 0.067 Uiso 1 1 calc R U . . .
H49B H 0.194331 0.320692 0.371377 0.067 Uiso 1 1 calc R U . . .
H49C H 0.246393 0.406602 0.355885 0.067 Uiso 1 1 calc R U . . .
C50 C 0.22904(13) 0.4535(2) 0.40214(7) 0.0368(6) Uani 1 1 d . . . . .
C2A C 0.27163(17) 0.4970(3) 0.60962(8) 0.0167(6) Uani 0.832(3) 1 d . . P A 1
F4A F 0.25660(16) 0.3777(3) 0.60888(8) 0.0310(7) Uani 0.832(3) 1 d . U P A 1
F5A F 0.3210(2) 0.4999(6) 0.58833(15) 0.0265(8) Uani 0.832(3) 1 d . U P A 1
F6A F 0.21575(7) 0.54414(14) 0.59016(4) 0.0263(4) Uani 0.832(3) 1 d . . P A 1
C2B C 0.2919(9) 0.4687(18) 0.6167(4) 0.026(4) Uani 0.168(3) 1 d . . P A 2
F4B F 0.2336(7) 0.3964(17) 0.6091(5) 0.038(4) Uani 0.168(3) 1 d . U P A 2
F5B F 0.3042(11) 0.507(3) 0.5845(7) 0.027(4) Uani 0.168(3) 1 d . U P A 2
F6B F 0.3410(4) 0.3791(6) 0.6233(2) 0.029(2) Uani 0.168(3) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C2B 1.91(2) . ?
Ni1 C4 1.9140(17) . ?
Ni1 C1 1.9411(19) . ?
Ni1 C3 1.9465(18) . ?
Ni1 C2A 1.947(3) . ?
P1 C25 1.7856(18) . ?
P1 C31 1.7893(19) . ?
P1 C37 1.7915(18) . ?
P1 C43 1.7922(19) . ?
F1 C1 1.389(2) . ?
N1 C4 1.369(2) . ?
N1 C5 1.395(2) . ?
N1 C7 1.442(2) . ?
C1 F2 1.381(2) . ?
C1 F3 1.381(2) . ?
N2 C4 1.368(2) . ?
N2 C6 1.392(2) . ?
N2 C16 1.442(2) . ?
N3 C50 1.139(4) . ?
C3 F7 1.379(2) . ?
C3 F9 1.382(2) . ?
C3 F8 1.396(2) . ?
C5 C6 1.339(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.400(3) . ?
C7 C12 1.400(3) . ?
C8 C9 1.394(3) . ?
C8 C13 1.507(3) . ?
C9 C10 1.392(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(3) . ?
C10 C14 1.515(3) . ?
C11 C12 1.398(3) . ?
C11 H11 0.9500 . ?
C12 C15 1.498(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.398(3) . ?
C16 C17 1.405(2) . ?
C17 C18 1.398(3) . ?
C17 C22 1.510(3) . ?
C18 C19 1.389(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(3) . ?
C19 C23 1.509(3) . ?
C20 C21 1.393(3) . ?
C20 H20 0.9500 . ?
C21 C24 1.501(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.394(3) . ?
C25 C30 1.401(3) . ?
C26 C27 1.387(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.383(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.389(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.386(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.392(3) . ?
C31 C32 1.403(3) . ?
C32 C33 1.382(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.382(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.386(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.393(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.399(3) . ?
C37 C42 1.400(3) . ?
C38 C39 1.391(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.388(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.389(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.387(3) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C48 1.398(3) . ?
C43 C44 1.399(3) . ?
C44 C45 1.387(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.384(3) . ?
C45 H45 0.9500 . ?
C46 C47 1.390(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.389(3) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C50 1.457(4) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C2A F4A 1.373(4) . ?
C2A F5A 1.385(7) . ?
C2A F6A 1.388(3) . ?
C2B F6B 1.41(2) . ?
C2B F5B 1.42(3) . ?
C2B F4B 1.42(3) . ?

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
C2B Ni1 C4 169.0(5) . . ?
C2B Ni1 C1 85.1(6) . . ?
C4 Ni1 C1 91.88(8) . . ?
C2B Ni1 C3 93.8(6) . . ?
C4 Ni1 C3 89.38(7) . . ?
C1 Ni1 C3 178.59(8) . . ?
C4 Ni1 C2A 174.23(11) . . ?
C1 Ni1 C2A 90.24(11) . . ?
C3 Ni1 C2A 88.45(11) . . ?
C25 P1 C31 109.75(9) . . ?
C25 P1 C37 112.32(9) . . ?
C31 P1 C37 107.15(8) . . ?
C25 P1 C43 107.09(9) . . ?
C31 P1 C43 111.19(8) . . ?
C37 P1 C43 109.40(9) . . ?
C4 N1 C5 111.10(15) . . ?
C4 N1 C7 126.63(15) . . ?
C5 N1 C7 122.16(15) . . ?
F2 C1 F3 102.73(14) . . ?
F2 C1 F1 100.89(14) . . ?
F3 C1 F1 101.62(15) . . ?
F2 C1 Ni1 116.58(13) . . ?
F3 C1 Ni1 114.85(12) . . ?
F1 C1 Ni1 117.77(12) . . ?
C4 N2 C6 111.29(15) . . ?
C4 N2 C16 127.64(15) . . ?
C6 N2 C16 120.96(15) . . ?
F7 C3 F9 102.86(14) . . ?
F7 C3 F8 100.64(13) . . ?
F9 C3 F8 101.05(14) . . ?
F7 C3 Ni1 116.35(12) . . ?
F9 C3 Ni1 114.72(12) . . ?
F8 C3 Ni1 118.70(12) . . ?
N2 C4 N1 103.67(14) . . ?
N2 C4 Ni1 127.29(13) . . ?
N1 C4 Ni1 128.93(13) . . ?
C6 C5 N1 107.00(16) . . ?
C6 C5 H5 126.5 . . ?
N1 C5 H5 126.5 . . ?
C5 C6 N2 106.93(16) . . ?
C5 C6 H6 126.5 . . ?
N2 C6 H6 126.5 . . ?
C8 C7 C12 121.34(17) . . ?
C8 C7 N1 118.99(16) . . ?
C12 C7 N1 119.60(16) . . ?
C9 C8 C7 118.41(18) . . ?
C9 C8 C13 118.39(18) . . ?
C7 C8 C13 123.17(17) . . ?
C10 C9 C8 121.58(19) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C11 C10 C9 118.39(18) . . ?
C11 C10 C14 121.4(2) . . ?
C9 C10 C14 120.2(2) . . ?
C10 C11 C12 122.54(19) . . ?
C10 C11 H11 118.7 . . ?
C12 C11 H11 118.7 . . ?
C11 C12 C7 117.63(18) . . ?
C11 C12 C15 120.04(18) . . ?
C7 C12 C15 122.29(18) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C16 C17 121.32(17) . . ?
C21 C16 N2 120.44(16) . . ?
C17 C16 N2 118.07(16) . . ?
C18 C17 C16 117.71(17) . . ?
C18 C17 C22 119.44(17) . . ?
C16 C17 C22 122.85(17) . . ?
C19 C18 C17 122.43(18) . . ?
C19 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
C20 C19 C18 117.81(18) . . ?
C20 C19 C23 119.70(19) . . ?
C18 C19 C23 122.49(19) . . ?
C19 C20 C21 122.60(18) . . ?
C19 C20 H20 118.7 . . ?
C21 C20 H20 118.7 . . ?
C20 C21 C16 118.08(17) . . ?
C20 C21 C24 118.69(17) . . ?
C16 C21 C24 123.22(17) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 120.22(17) . . ?
C26 C25 P1 121.81(15) . . ?
C30 C25 P1 117.96(14) . . ?
C27 C26 C25 119.27(18) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C28 C27 C26 120.63(19) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 120.24(19) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 119.97(19) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C25 119.66(19) . . ?
C29 C30 H30 120.2 . . ?
C25 C30 H30 120.2 . . ?
C36 C31 C32 120.20(17) . . ?
C36 C31 P1 121.87(15) . . ?
C32 C31 P1 117.92(14) . . ?
C33 C32 C31 119.77(19) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C32 C33 C34 119.91(19) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.76(19) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C34 C35 C36 120.0(2) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C31 C36 C35 119.33(19) . . ?
C31 C36 H36 120.3 . . ?
C35 C36 H36 120.3 . . ?
C38 C37 C42 119.98(17) . . ?
C38 C37 P1 121.03(14) . . ?
C42 C37 P1 118.90(14) . . ?
C39 C38 C37 119.65(18) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C40 C39 C38 120.03(18) . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C40 C41 120.53(18) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C42 C41 C40 119.94(19) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C37 119.84(18) . . ?
C41 C42 H42 120.1 . . ?
C37 C42 H42 120.1 . . ?
C48 C43 C44 120.13(17) . . ?
C48 C43 P1 117.89(14) . . ?
C44 C43 P1 121.93(15) . . ?
C45 C44 C43 118.97(19) . . ?
C45 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C46 C45 C44 120.9(2) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C47 120.41(19) . . ?
C45 C46 H46 119.8 . . ?
C47 C46 H46 119.8 . . ?
C48 C47 C46 119.40(19) . . ?
C48 C47 H47 120.3 . . ?
C46 C47 H47 120.3 . . ?
C47 C48 C43 120.21(18) . . ?
C47 C48 H48 119.9 . . ?
C43 C48 H48 119.9 . . ?
C50 C49 H49A 109.5 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C50 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N3 C50 C49 179.2(3) . . ?
F4A C2A F5A 100.4(4) . . ?
F4A C2A F6A 101.7(3) . . ?
F5A C2A F6A 102.9(3) . . ?
F4A C2A Ni1 120.4(2) . . ?
F5A C2A Ni1 117.8(3) . . ?
F6A C2A Ni1 111.15(19) . . ?
F6B C2B F5B 101.4(16) . . ?
F6B C2B F4B 99.5(15) . . ?
F5B C2B F4B 101.9(18) . . ?
F6B C2B Ni1 114.3(10) . . ?
F5B C2B Ni1 120.4(18) . . ?
F4B C2B Ni1 116.3(13) . . ?

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
C6 N2 C4 N1 0.77(19) . . . . ?
C16 N2 C4 N1 -175.46(16) . . . . ?
C6 N2 C4 Ni1 -175.81(13) . . . . ?
C16 N2 C4 Ni1 8.0(3) . . . . ?
C5 N1 C4 N2 -0.42(19) . . . . ?
C7 N1 C4 N2 -176.72(16) . . . . ?
C5 N1 C4 Ni1 176.09(13) . . . . ?
C7 N1 C4 Ni1 -0.2(3) . . . . ?
C4 N1 C5 C6 -0.1(2) . . . . ?
C7 N1 C5 C6 176.41(16) . . . . ?
N1 C5 C6 N2 0.5(2) . . . . ?
C4 N2 C6 C5 -0.9(2) . . . . ?
C16 N2 C6 C5 175.67(16) . . . . ?
C4 N1 C7 C8 115.6(2) . . . . ?
C5 N1 C7 C8 -60.3(2) . . . . ?
C4 N1 C7 C12 -67.3(2) . . . . ?
C5 N1 C7 C12 116.73(19) . . . . ?
C12 C7 C8 C9 3.9(3) . . . . ?
N1 C7 C8 C9 -179.10(16) . . . . ?
C12 C7 C8 C13 -173.95(18) . . . . ?
N1 C7 C8 C13 3.0(3) . . . . ?
C7 C8 C9 C10 -1.7(3) . . . . ?
C13 C8 C9 C10 176.26(18) . . . . ?
C8 C9 C10 C11 -0.5(3) . . . . ?
C8 C9 C10 C14 -179.17(19) . . . . ?
C9 C10 C11 C12 0.7(3) . . . . ?
C14 C10 C11 C12 179.33(19) . . . . ?
C10 C11 C12 C7 1.4(3) . . . . ?
C10 C11 C12 C15 -176.72(19) . . . . ?
C8 C7 C12 C11 -3.8(3) . . . . ?
N1 C7 C12 C11 179.31(16) . . . . ?
C8 C7 C12 C15 174.31(18) . . . . ?
N1 C7 C12 C15 -2.6(3) . . . . ?
C4 N2 C16 C21 -67.5(2) . . . . ?
C6 N2 C16 C21 116.61(19) . . . . ?
C4 N2 C16 C17 117.04(19) . . . . ?
C6 N2 C16 C17 -58.9(2) . . . . ?
C21 C16 C17 C18 2.3(3) . . . . ?
N2 C16 C17 C18 177.73(16) . . . . ?
C21 C16 C17 C22 -177.29(17) . . . . ?
N2 C16 C17 C22 -1.9(3) . . . . ?
C16 C17 C18 C19 -1.3(3) . . . . ?
C22 C17 C18 C19 178.32(18) . . . . ?
C17 C18 C19 C20 0.1(3) . . . . ?
C17 C18 C19 C23 179.99(18) . . . . ?
C18 C19 C20 C21 0.2(3) . . . . ?
C23 C19 C20 C21 -179.71(18) . . . . ?
C19 C20 C21 C16 0.8(3) . . . . ?
C19 C20 C21 C24 -178.53(18) . . . . ?
C17 C16 C21 C20 -2.1(3) . . . . ?
N2 C16 C21 C20 -177.37(16) . . . . ?
C17 C16 C21 C24 177.21(17) . . . . ?
N2 C16 C21 C24 1.9(3) . . . . ?
C31 P1 C25 C26 104.15(16) . . . . ?
C37 P1 C25 C26 -14.92(19) . . . . ?
C43 P1 C25 C26 -135.05(16) . . . . ?
C31 P1 C25 C30 -74.61(17) . . . . ?
C37 P1 C25 C30 166.32(15) . . . . ?
C43 P1 C25 C30 46.20(17) . . . . ?
C30 C25 C26 C27 -0.6(3) . . . . ?
P1 C25 C26 C27 -179.34(15) . . . . ?
C25 C26 C27 C28 0.4(3) . . . . ?
C26 C27 C28 C29 0.3(3) . . . . ?
C27 C28 C29 C30 -0.8(3) . . . . ?
C28 C29 C30 C25 0.6(3) . . . . ?
C26 C25 C30 C29 0.1(3) . . . . ?
P1 C25 C30 C29 178.86(15) . . . . ?
C25 P1 C31 C36 9.17(19) . . . . ?
C37 P1 C31 C36 131.37(16) . . . . ?
C43 P1 C31 C36 -109.13(16) . . . . ?
C25 P1 C31 C32 -170.20(14) . . . . ?
C37 P1 C31 C32 -48.00(17) . . . . ?
C43 P1 C31 C32 71.50(16) . . . . ?
C36 C31 C32 C33 0.8(3) . . . . ?
P1 C31 C32 C33 -179.83(15) . . . . ?
C31 C32 C33 C34 0.2(3) . . . . ?
C32 C33 C34 C35 -1.0(3) . . . . ?
C33 C34 C35 C36 0.9(3) . . . . ?
C32 C31 C36 C35 -0.9(3) . . . . ?
P1 C31 C36 C35 179.72(15) . . . . ?
C34 C35 C36 C31 0.1(3) . . . . ?
C25 P1 C37 C38 -119.45(16) . . . . ?
C31 P1 C37 C38 119.96(16) . . . . ?
C43 P1 C37 C38 -0.68(18) . . . . ?
C25 P1 C37 C42 63.86(17) . . . . ?
C31 P1 C37 C42 -56.73(17) . . . . ?
C43 P1 C37 C42 -177.37(14) . . . . ?
C42 C37 C38 C39 -0.4(3) . . . . ?
P1 C37 C38 C39 -177.01(15) . . . . ?
C37 C38 C39 C40 -0.9(3) . . . . ?
C38 C39 C40 C41 1.1(3) . . . . ?
C39 C40 C41 C42 0.1(3) . . . . ?
C40 C41 C42 C37 -1.4(3) . . . . ?
C38 C37 C42 C41 1.5(3) . . . . ?
P1 C37 C42 C41 178.24(15) . . . . ?
C25 P1 C43 C48 44.89(17) . . . . ?
C31 P1 C43 C48 164.78(15) . . . . ?
C37 P1 C43 C48 -77.08(17) . . . . ?
C25 P1 C43 C44 -137.90(16) . . . . ?
C31 P1 C43 C44 -18.02(19) . . . . ?
C37 P1 C43 C44 100.13(17) . . . . ?
C48 C43 C44 C45 0.6(3) . . . . ?
P1 C43 C44 C45 -176.52(16) . . . . ?
C43 C44 C45 C46 0.8(3) . . . . ?
C44 C45 C46 C47 -1.6(3) . . . . ?
C45 C46 C47 C48 0.9(3) . . . . ?
C46 C47 C48 C43 0.6(3) . . . . ?
C44 C43 C48 C47 -1.3(3) . . . . ?
P1 C43 C48 C47 175.92(15) . . . . ?

_refine_diff_density_max         0.486
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.066


_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 2124820'
loop_
_audit_author_name
_audit_author_address
'David Vicic'
;Lehigh University
United States of America
;
_audit_update_record             
;
2021-11-28 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H15 F13 N2 Ni'
_chemical_formula_weight         492.97

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   9.6856(7)
_cell_length_b                   14.9509(10)
_cell_length_c                   13.1346(9)
_cell_angle_alpha                90
_cell_angle_beta                 108.190(2)
_cell_angle_gamma                90
_cell_volume                     1807.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9575
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      29.85

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.201
_shelx_estimated_absorpt_T_min   0.804
_shelx_estimated_absorpt_T_max   0.889
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   Bruker
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33720
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.177
_diffrn_reflns_theta_max         30.699
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5111
_reflns_number_gt                4163
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0375P)²+1.4117P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0067(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5111
_refine_ls_number_parameters     259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0879
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.74940(2) 0.38418(2) 0.35996(2) 0.02236(8) Uani 1 1 d . . . . .
F1 F 0.73513(13) 0.48802(8) 0.18083(9) 0.0358(3) Uani 1 1 d . . . . .
N1 N 0.81100(17) 0.50205(10) 0.40458(12) 0.0284(3) Uani 1 1 d . . . . .
C1 C 0.7822(2) 0.40266(12) 0.22193(14) 0.0276(4) Uani 1 1 d . . . . .
N2 N 0.14803(16) 0.04208(11) 0.31655(12) 0.0283(3) Uani 1 1 d . . . . .
F2 F 0.70771(15) 0.34746(9) 0.13747(9) 0.0418(3) Uani 1 1 d . . . . .
C2 C 0.9375(2) 0.40003(14) 0.21868(16) 0.0358(4) Uani 1 1 d . . . . .
F3 F 0.99757(16) 0.31950(10) 0.24724(12) 0.0531(4) Uani 1 1 d . . . . .
C3 C 0.6901(2) 0.26360(12) 0.32930(15) 0.0272(4) Uani 1 1 d . . . . .
F4 F 0.94958(15) 0.41808(10) 0.12124(10) 0.0477(3) Uani 1 1 d . . . . .
C4 C 0.6882(2) 0.21481(12) 0.43128(16) 0.0319(4) Uani 1 1 d . . . . .
F5 F 1.02156(14) 0.45897(10) 0.28678(11) 0.0486(3) Uani 1 1 d . . . . .
C5 C 0.6297(2) 0.27974(15) 0.49656(18) 0.0392(5) Uani 1 1 d . . . . .
C6 C 0.7041(2) 0.36923(13) 0.49221(16) 0.0320(4) Uani 1 1 d . . . . .
F6 F 0.55076(13) 0.25672(9) 0.25838(10) 0.0429(3) Uani 1 1 d . . . . .
F7 F 0.77229(14) 0.21043(7) 0.28432(10) 0.0388(3) Uani 1 1 d . . . . .
C7 C 0.8437(2) 0.57245(12) 0.43521(14) 0.0290(4) Uani 1 1 d . . . . .
F8 F 0.82730(13) 0.19429(8) 0.48996(10) 0.0402(3) Uani 1 1 d . . . . .
C8 C 0.8819(3) 0.66283(13) 0.47346(17) 0.0412(5) Uani 1 1 d . . . . .
H8A H 0.966327 0.661307 0.538316 0.062 Uiso 1 1 calc R U . . .
H8B H 0.799615 0.690510 0.489941 0.062 Uiso 1 1 calc R U . . .
H8C H 0.905473 0.697795 0.417994 0.062 Uiso 1 1 calc R U . . .
C9 C 0.0269(3) 0.0954(2) 0.2469(3) 0.0612(8) Uani 1 1 d . . . . .
H9A H -0.065382 0.065270 0.240339 0.092 Uiso 1 1 calc R U . . .
H9B H 0.038732 0.101365 0.175778 0.092 Uiso 1 1 calc R U . . .
H9C H 0.026852 0.154823 0.278273 0.092 Uiso 1 1 calc R U . . .
F9 F 0.61314(15) 0.13670(8) 0.41433(12) 0.0445(3) Uani 1 1 d . . . . .
C10 C 0.2887(2) 0.08922(17) 0.3310(2) 0.0459(5) Uani 1 1 d . . . . .
H10A H 0.368780 0.052513 0.375390 0.069 Uiso 1 1 calc R U . . .
H10B H 0.287790 0.146859 0.366372 0.069 Uiso 1 1 calc R U . . .
H10C H 0.301775 0.099245 0.260909 0.069 Uiso 1 1 calc R U . . .
F10 F 0.6484(2) 0.24818(10) 0.59676(12) 0.0616(4) Uani 1 1 d . . . . .
C11 C 0.1494(3) -0.04598(19) 0.2620(3) 0.0647(8) Uani 1 1 d . . . . .
H11A H 0.228925 -0.083014 0.306447 0.097 Uiso 1 1 calc R U . . .
H11B H 0.163425 -0.035687 0.192186 0.097 Uiso 1 1 calc R U . . .
H11C H 0.056652 -0.076738 0.251669 0.097 Uiso 1 1 calc R U . . .
F11 F 0.48368(16) 0.28778(11) 0.44739(14) 0.0593(4) Uani 1 1 d . . . . .
C12 C 0.1273(3) 0.0241(2) 0.4210(2) 0.0664(8) Uani 1 1 d . . . . .
H12A H 0.211114 -0.009070 0.466564 0.100 Uiso 1 1 calc R U . . .
H12B H 0.038855 -0.011442 0.410329 0.100 Uiso 1 1 calc R U . . .
H12C H 0.117988 0.080861 0.455616 0.100 Uiso 1 1 calc R U . . .
F12 F 0.61525(18) 0.43497(9) 0.51243(12) 0.0553(4) Uani 1 1 d . . . . .
F13 F 0.82644(17) 0.37167(9) 0.58186(10) 0.0485(3) 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 1.8938(15) . ?
Ni1 C3 1.8967(18) . ?
Ni1 C6 1.9330(19) . ?
Ni1 C1 1.9556(18) . ?
F1 C1 1.405(2) . ?
N1 C7 1.136(2) . ?
C1 F2 1.390(2) . ?
C1 C2 1.518(3) . ?
N2 C12 1.472(3) . ?
N2 C9 1.476(3) . ?
N2 C10 1.492(3) . ?
N2 C11 1.501(3) . ?
C2 F5 1.336(3) . ?
C2 F3 1.339(2) . ?
C2 F4 1.348(2) . ?
C3 F7 1.381(2) . ?
C3 F6 1.384(2) . ?
C3 C4 1.531(3) . ?
C4 F9 1.356(2) . ?
C4 F8 1.362(2) . ?
C4 C5 1.517(3) . ?
C5 F10 1.356(3) . ?
C5 F11 1.364(3) . ?
C5 C6 1.529(3) . ?
C6 F12 1.385(2) . ?
C6 F13 1.386(2) . ?
C7 C8 1.449(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 C3 174.49(7) . . ?
N1 Ni1 C6 88.14(7) . . ?
C3 Ni1 C6 86.69(8) . . ?
N1 Ni1 C1 91.65(7) . . ?
C3 Ni1 C1 93.64(8) . . ?
C6 Ni1 C1 176.16(8) . . ?
C7 N1 Ni1 176.21(16) . . ?
F2 C1 F1 101.96(14) . . ?
F2 C1 C2 103.55(15) . . ?
F1 C1 C2 102.62(15) . . ?
F2 C1 Ni1 117.50(12) . . ?
F1 C1 Ni1 110.92(12) . . ?
C2 C1 Ni1 118.14(13) . . ?
C12 N2 C9 111.3(2) . . ?
C12 N2 C10 110.62(18) . . ?
C9 N2 C10 109.98(18) . . ?
C12 N2 C11 108.0(2) . . ?
C9 N2 C11 107.5(2) . . ?
C10 N2 C11 109.36(18) . . ?
F5 C2 F3 106.54(18) . . ?
F5 C2 F4 106.74(17) . . ?
F3 C2 F4 106.68(16) . . ?
F5 C2 C1 111.48(16) . . ?
F3 C2 C1 111.29(17) . . ?
F4 C2 C1 113.69(17) . . ?
F7 C3 F6 103.91(14) . . ?
F7 C3 C4 105.44(15) . . ?
F6 C3 C4 106.11(15) . . ?
F7 C3 Ni1 117.47(12) . . ?
F6 C3 Ni1 112.36(12) . . ?
C4 C3 Ni1 110.66(12) . . ?
F9 C4 F8 106.47(15) . . ?
F9 C4 C5 111.61(16) . . ?
F8 C4 C5 107.61(17) . . ?
F9 C4 C3 114.77(17) . . ?
F8 C4 C3 108.78(15) . . ?
C5 C4 C3 107.37(16) . . ?
F10 C5 F11 107.16(17) . . ?
F10 C5 C4 111.44(18) . . ?
F11 C5 C4 107.68(18) . . ?
F10 C5 C6 114.76(19) . . ?
F11 C5 C6 109.64(18) . . ?
C4 C5 C6 105.98(15) . . ?
F12 C6 F13 103.65(16) . . ?
F12 C6 C5 106.60(16) . . ?
F13 C6 C5 106.21(16) . . ?
F12 C6 Ni1 114.78(13) . . ?
F13 C6 Ni1 112.73(14) . . ?
C5 C6 Ni1 112.13(13) . . ?
N1 C7 C8 178.7(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_refine_diff_density_max         0.790
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_Schaefer_SB01_0m
_database_code_depnum_ccdc_archive 'CCDC 2118416'
loop_
_audit_author_name
_audit_author_address
'Sascha Schaefer'
;University of Cologne
Germany
;
_audit_update_record             
;
2022-01-09 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H18 F15 N3 Ni'
_chemical_formula_weight         668.10

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'
F F 0.0171 0.0103 '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'

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

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

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

_cell_length_a                   15.9285(11)
_cell_length_b                   9.6940(6)
_cell_length_c                   16.2880(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.067(2)
_cell_angle_gamma                90
_cell_volume                     2505.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9962
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      25.84

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_F_000             1336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.905
_shelx_estimated_absorpt_T_min   0.899
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42484
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.447
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5140
_reflns_number_gt                4046
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1109P)²+5.8698P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5140
_refine_ls_number_parameters     402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.2004
_refine_ls_wR_factor_gt          0.1861
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.24827(4) 0.43413(5) 0.66659(3) 0.0345(2) Uani 1 1 d . . . . .
F1 F 0.2034(3) 0.1610(3) 0.7093(3) 0.0794(12) Uani 1 1 d . . . . .
N1 N 0.1227(2) 0.5562(4) 0.5427(2) 0.0372(8) Uani 1 1 d . . . . .
C1 C 0.1715(4) 0.2920(5) 0.7007(3) 0.0497(12) Uani 1 1 d . . . . .
F2 F 0.1369(2) 0.3173(4) 0.77362(18) 0.0591(8) Uani 1 1 d . . . . .
N2 N 0.1785(3) 0.3703(4) 0.5008(2) 0.0399(9) Uani 1 1 d . . . . .
C2 C 0.3228(4) 0.4044(6) 0.7636(3) 0.0525(13) Uani 1 1 d . . . . .
F3 F 0.0961(2) 0.2707(4) 0.6471(2) 0.0759(11) Uani 1 1 d . . . . .
N3 N 0.6184(3) 0.4326(4) 0.6730(3) 0.0438(9) Uani 1 1 d . . . . .
C3 C 0.3188(3) 0.5808(5) 0.6312(3) 0.0457(11) Uani 1 1 d . . . . .
F4 F 0.2993(2) 0.3151(4) 0.8241(2) 0.0712(10) Uani 1 1 d . . . . .
C4 C 0.1786(3) 0.4562(5) 0.5673(3) 0.0362(9) Uani 1 1 d . . . . .
F5 F 0.3407(3) 0.5141(4) 0.8122(2) 0.0871(13) Uani 1 1 d . . . . .
C5 C 0.0889(3) 0.5349(6) 0.4615(3) 0.0448(11) Uani 1 1 d . . . . .
H5 H 0.049389 0.592209 0.430530 0.054 Uiso 1 1 calc R U . . .
F6 F 0.3972(2) 0.3418(4) 0.7467(2) 0.0680(10) Uani 1 1 d . . . . .
C6 C 0.1226(3) 0.4189(6) 0.4360(3) 0.0457(12) Uani 1 1 d . . . . .
H6 H 0.111069 0.376810 0.383547 0.055 Uiso 1 1 calc R U . . .
C7 C 0.0998(3) 0.6666(5) 0.5948(3) 0.0366(9) Uani 1 1 d . . . . .
C8 C 0.1040(3) 0.6463(5) 0.6794(3) 0.0410(10) Uani 1 1 d . . . . .
H8 H 0.120407 0.559479 0.702668 0.049 Uiso 1 1 calc R U . . .
C9 C 0.0839(3) 0.7539(5) 0.7289(3) 0.0460(11) Uani 1 1 d . . . . .
F10 F 0.0886(2) 0.7368(3) 0.81102(18) 0.0628(9) Uani 1 1 d . . . . .
C10 C 0.0583(3) 0.8792(5) 0.6961(3) 0.0474(11) Uani 1 1 d . . . . .
F11 F 0.0398(2) 0.9830(3) 0.7461(2) 0.0620(9) Uani 1 1 d . . . . .
C11 C 0.0528(4) 0.8964(5) 0.6128(4) 0.0517(13) Uani 1 1 d . . . . .
F12 F 0.0261(3) 1.0183(4) 0.5816(2) 0.0768(11) Uani 1 1 d . . . . .
C12 C 0.0729(3) 0.7919(5) 0.5604(3) 0.0453(11) Uani 1 1 d . . . . .
H12 H 0.068437 0.805361 0.502417 0.054 Uiso 1 1 calc R U . . .
F13 F 0.4320(2) 0.1130(3) 0.56847(19) 0.0532(7) Uani 1 1 d . . . . .
C13 C 0.2254(3) 0.2451(5) 0.5005(3) 0.0410(10) Uani 1 1 d . . . . .
F14 F 0.3606(2) -0.1161(3) 0.4999(2) 0.0619(9) Uani 1 1 d . . . . .
C14 C 0.3076(3) 0.2420(5) 0.5357(3) 0.0401(10) Uani 1 1 d . . . . .
H14 H 0.333156 0.322672 0.559748 0.048 Uiso 1 1 calc R U . . .
F15 F 0.2000(2) -0.1083(4) 0.4313(2) 0.0709(10) Uani 1 1 d . . . . .
C15 C 0.3521(3) 0.1184(5) 0.5355(3) 0.0441(11) Uani 1 1 d . . . . .
C16 C 0.3155(4) 0.0007(5) 0.5001(3) 0.0487(12) Uani 1 1 d . . . . .
C17 C 0.2336(4) 0.0089(6) 0.4658(3) 0.0522(13) Uani 1 1 d . . . . .
C18 C 0.1878(3) 0.1271(6) 0.4656(3) 0.0481(12) Uani 1 1 d . . . . .
H18 H 0.131053 0.129005 0.442102 0.058 Uiso 1 1 calc R U . . .
C19 C 0.6024(4) 0.4785(6) 0.7582(3) 0.0551(13) Uani 1 1 d . . . . .
H19A H 0.637043 0.559626 0.773354 0.083 Uiso 1 1 calc R U . . .
H19B H 0.616995 0.403717 0.797350 0.083 Uiso 1 1 calc R U . . .
H19C H 0.542705 0.502026 0.759418 0.083 Uiso 1 1 calc R U . . .
C20 C 0.5647(4) 0.3135(6) 0.6485(4) 0.0635(16) Uani 1 1 d . . . . .
H20A H 0.505383 0.338566 0.651236 0.095 Uiso 1 1 calc R U . . .
H20B H 0.579000 0.236196 0.685860 0.095 Uiso 1 1 calc R U . . .
H20C H 0.573846 0.286540 0.591978 0.095 Uiso 1 1 calc R U . . .
C21 C 0.5983(6) 0.5480(6) 0.6152(4) 0.074(2) Uani 1 1 d . . . . .
H21A H 0.607461 0.518845 0.559120 0.110 Uiso 1 1 calc R U . . .
H21B H 0.634830 0.626810 0.630866 0.110 Uiso 1 1 calc R U . . .
H21C H 0.539221 0.574947 0.617413 0.110 Uiso 1 1 calc R U . . .
C22 C 0.7079(4) 0.3892(9) 0.6713(4) 0.0752(19) Uani 1 1 d . . . . .
H22A H 0.717272 0.356095 0.616018 0.113 Uiso 1 1 calc R U . . .
H22B H 0.720409 0.315006 0.711400 0.113 Uiso 1 1 calc R U . . .
H22C H 0.744995 0.467987 0.685416 0.113 Uiso 1 1 calc R U . . .
F7A F 0.3973(4) 0.6055(10) 0.6748(5) 0.063(3) Uani 0.61(2) 1 d . . P A 1
F8A F 0.2838(6) 0.7099(11) 0.6378(8) 0.059(3) Uani 0.61(2) 1 d . . P A 1
F9A F 0.3389(9) 0.5772(10) 0.5536(5) 0.063(3) Uani 0.61(2) 1 d . . P A 1
F7B F 0.4032(7) 0.5507(13) 0.6130(19) 0.101(10) Uani 0.39(2) 1 d . . P A 2
F8B F 0.3182(17) 0.7036(18) 0.6598(12) 0.081(6) Uani 0.39(2) 1 d . . P A 2
F9B F 0.2994(13) 0.619(2) 0.5399(11) 0.070(4) Uani 0.39(2) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C4 1.891(4) . ?
Ni1 C2 1.913(5) . ?
Ni1 C3 1.931(5) . ?
Ni1 C1 1.955(5) . ?
F1 C1 1.370(6) . ?
N1 C4 1.352(6) . ?
N1 C5 1.400(6) . ?
N1 C7 1.432(6) . ?
C1 F2 1.374(5) . ?
C1 F3 1.437(7) . ?
N2 C4 1.367(6) . ?
N2 C6 1.401(6) . ?
N2 C13 1.425(6) . ?
C2 F5 1.342(6) . ?
C2 F6 1.381(6) . ?
C2 F4 1.386(7) . ?
N3 C20 1.472(7) . ?
N3 C21 1.479(7) . ?
N3 C22 1.489(8) . ?
N3 C19 1.499(6) . ?
C3 F8B 1.278(18) . ?
C3 F9A 1.331(10) . ?
C3 F8A 1.378(11) . ?
C3 F7A 1.403(8) . ?
C3 F7B 1.432(15) . ?
C3 F9B 1.54(2) . ?
C5 C6 1.328(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.388(6) . ?
C7 C12 1.390(7) . ?
C8 C9 1.373(7) . ?
C8 H8 0.9500 . ?
C9 F10 1.343(5) . ?
C9 C10 1.375(7) . ?
C10 F11 1.344(6) . ?
C10 C11 1.362(8) . ?
C11 F12 1.341(6) . ?
C11 C12 1.380(8) . ?
C12 H12 0.9500 . ?
F13 C15 1.337(6) . ?
C13 C14 1.382(7) . ?
C13 C18 1.389(7) . ?
F14 C16 1.341(6) . ?
C14 C15 1.393(7) . ?
C14 H14 0.9500 . ?
F15 C17 1.356(6) . ?
C15 C16 1.383(7) . ?
C16 C17 1.376(8) . ?
C17 C18 1.358(8) . ?
C18 H18 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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
C4 Ni1 C2 176.6(2) . . ?
C4 Ni1 C3 88.5(2) . . ?
C2 Ni1 C3 91.3(2) . . ?
C4 Ni1 C1 89.3(2) . . ?
C2 Ni1 C1 90.9(2) . . ?
C3 Ni1 C1 176.9(2) . . ?
C4 N1 C5 111.2(4) . . ?
C4 N1 C7 123.7(4) . . ?
C5 N1 C7 125.0(4) . . ?
F1 C1 F2 104.6(4) . . ?
F1 C1 F3 102.2(4) . . ?
F2 C1 F3 100.0(4) . . ?
F1 C1 Ni1 116.5(4) . . ?
F2 C1 Ni1 115.4(4) . . ?
F3 C1 Ni1 116.0(3) . . ?
C4 N2 C6 110.4(4) . . ?
C4 N2 C13 124.0(4) . . ?
C6 N2 C13 125.6(4) . . ?
F5 C2 F6 108.9(5) . . ?
F5 C2 F4 97.7(4) . . ?
F6 C2 F4 99.0(4) . . ?
F5 C2 Ni1 116.9(4) . . ?
F6 C2 Ni1 112.5(4) . . ?
F4 C2 Ni1 119.6(4) . . ?
C20 N3 C21 109.4(5) . . ?
C20 N3 C22 107.9(5) . . ?
C21 N3 C22 110.9(5) . . ?
C20 N3 C19 110.0(4) . . ?
C21 N3 C19 108.6(4) . . ?
C22 N3 C19 110.0(5) . . ?
F9A C3 F8A 103.4(7) . . ?
F9A C3 F7A 101.9(6) . . ?
F8A C3 F7A 98.8(6) . . ?
F8B C3 F7B 107.6(12) . . ?
F8B C3 F9B 97.1(11) . . ?
F7B C3 F9B 87.7(10) . . ?
F8B C3 Ni1 123.6(12) . . ?
F9A C3 Ni1 117.3(5) . . ?
F8A C3 Ni1 113.3(5) . . ?
F7A C3 Ni1 119.4(4) . . ?
F7B C3 Ni1 119.5(5) . . ?
F9B C3 Ni1 113.1(7) . . ?
N1 C4 N2 104.3(4) . . ?
N1 C4 Ni1 131.0(3) . . ?
N2 C4 Ni1 124.6(4) . . ?
C6 C5 N1 106.7(4) . . ?
C6 C5 H5 126.6 . . ?
N1 C5 H5 126.6 . . ?
C5 C6 N2 107.3(4) . . ?
C5 C6 H6 126.4 . . ?
N2 C6 H6 126.4 . . ?
C8 C7 C12 120.7(4) . . ?
C8 C7 N1 119.3(4) . . ?
C12 C7 N1 120.0(4) . . ?
C9 C8 C7 118.8(4) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
F10 C9 C8 119.7(4) . . ?
F10 C9 C10 119.0(4) . . ?
C8 C9 C10 121.3(5) . . ?
F11 C10 C11 121.0(5) . . ?
F11 C10 C9 119.9(5) . . ?
C11 C10 C9 119.1(5) . . ?
F12 C11 C10 118.4(5) . . ?
F12 C11 C12 119.7(5) . . ?
C10 C11 C12 121.9(5) . . ?
C11 C12 C7 118.2(5) . . ?
C11 C12 H12 120.9 . . ?
C7 C12 H12 120.9 . . ?
C14 C13 C18 120.7(5) . . ?
C14 C13 N2 119.6(4) . . ?
C18 C13 N2 119.7(5) . . ?
C13 C14 C15 118.8(4) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
F13 C15 C16 119.1(5) . . ?
F13 C15 C14 119.9(4) . . ?
C16 C15 C14 121.0(5) . . ?
F14 C16 C17 122.5(5) . . ?
F14 C16 C15 119.4(5) . . ?
C17 C16 C15 118.1(5) . . ?
F15 C17 C18 120.9(5) . . ?
F15 C17 C16 116.4(5) . . ?
C18 C17 C16 122.7(5) . . ?
C17 C18 C13 118.8(5) . . ?
C17 C18 H18 120.6 . . ?
C13 C18 H18 120.6 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 H21A 109.5 . . ?
N3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 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
C5 N1 C4 N2 -0.9(5) . . . . ?
C7 N1 C4 N2 177.2(4) . . . . ?
C5 N1 C4 Ni1 176.2(3) . . . . ?
C7 N1 C4 Ni1 -5.7(6) . . . . ?
C6 N2 C4 N1 0.2(5) . . . . ?
C13 N2 C4 N1 -176.5(4) . . . . ?
C6 N2 C4 Ni1 -177.2(3) . . . . ?
C13 N2 C4 Ni1 6.2(6) . . . . ?
C3 Ni1 C4 N1 -73.5(4) . . . . ?
C1 Ni1 C4 N1 104.2(4) . . . . ?
C3 Ni1 C4 N2 103.1(4) . . . . ?
C1 Ni1 C4 N2 -79.2(4) . . . . ?
C4 N1 C5 C6 1.3(5) . . . . ?
C7 N1 C5 C6 -176.8(4) . . . . ?
N1 C5 C6 N2 -1.2(5) . . . . ?
C4 N2 C6 C5 0.7(5) . . . . ?
C13 N2 C6 C5 177.2(4) . . . . ?
C4 N1 C7 C8 -28.0(6) . . . . ?
C5 N1 C7 C8 149.9(5) . . . . ?
C4 N1 C7 C12 152.7(4) . . . . ?
C5 N1 C7 C12 -29.4(7) . . . . ?
C12 C7 C8 C9 -2.3(7) . . . . ?
N1 C7 C8 C9 178.3(4) . . . . ?
C7 C8 C9 F10 -179.2(5) . . . . ?
C7 C8 C9 C10 1.4(8) . . . . ?
F10 C9 C10 F11 1.2(8) . . . . ?
C8 C9 C10 F11 -179.4(5) . . . . ?
F10 C9 C10 C11 -179.4(5) . . . . ?
C8 C9 C10 C11 -0.1(8) . . . . ?
F11 C10 C11 F12 -1.9(8) . . . . ?
C9 C10 C11 F12 178.7(5) . . . . ?
F11 C10 C11 C12 178.9(5) . . . . ?
C9 C10 C11 C12 -0.5(9) . . . . ?
F12 C11 C12 C7 -179.6(5) . . . . ?
C10 C11 C12 C7 -0.4(8) . . . . ?
C8 C7 C12 C11 1.8(7) . . . . ?
N1 C7 C12 C11 -178.9(4) . . . . ?
C4 N2 C13 C14 -43.1(6) . . . . ?
C6 N2 C13 C14 140.8(5) . . . . ?
C4 N2 C13 C18 136.1(5) . . . . ?
C6 N2 C13 C18 -40.0(6) . . . . ?
C18 C13 C14 C15 0.3(6) . . . . ?
N2 C13 C14 C15 179.4(4) . . . . ?
C13 C14 C15 F13 179.3(4) . . . . ?
C13 C14 C15 C16 0.5(7) . . . . ?
F13 C15 C16 F14 0.2(7) . . . . ?
C14 C15 C16 F14 179.1(4) . . . . ?
F13 C15 C16 C17 -179.4(4) . . . . ?
C14 C15 C16 C17 -0.5(7) . . . . ?
F14 C16 C17 F15 0.0(7) . . . . ?
C15 C16 C17 F15 179.6(4) . . . . ?
F14 C16 C17 C18 -179.7(4) . . . . ?
C15 C16 C17 C18 -0.2(7) . . . . ?
F15 C17 C18 C13 -178.9(4) . . . . ?
C16 C17 C18 C13 0.9(7) . . . . ?
C14 C13 C18 C17 -0.9(7) . . . . ?
N2 C13 C18 C17 179.9(4) . . . . ?

_refine_diff_density_max         1.635
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.108


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF, n-pentane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_Schaefer_SS113_0m
_database_code_depnum_ccdc_archive 'CCDC 2133045'
loop_
_audit_author_name
_audit_author_address
'Sascha Schaefer'
;University of Cologne
Germany
;
_audit_update_record             
;
2022-01-11 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31.21 H33.31 F16.94 N3 Ni O2'


_chemical_formula_weight         862.57

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

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

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

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

_cell_length_a                   8.5261(3)
_cell_length_b                   13.2144(5)
_cell_length_c                   16.9930(6)
_cell_angle_alpha                104.8370(10)
_cell_angle_beta                 91.5500(10)
_cell_angle_gamma                105.7390(10)
_cell_volume                     1771.72(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9265
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      26.20

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_F_000             876
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.671
_shelx_estimated_absorpt_T_min   0.948
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            78752
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.337
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7250
_reflns_number_gt                6394
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0631P)²+1.8678P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7250
_refine_ls_number_parameters     640
_refine_ls_number_restraints     207
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1177
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N2 N 0.4956(2) 0.66684(16) 0.69531(11) 0.0295(4) Uani 1 1 d . . . . .
C2 C 0.3622(4) 0.2637(2) 0.63292(19) 0.0444(6) Uani 1 1 d . . . . .
N3 N 0.7213(3) 0.28283(16) 0.91124(12) 0.0322(4) Uani 1 1 d . . . . .
C3 C 0.2377(4) 0.3780(3) 0.80955(19) 0.0547(8) Uani 1 1 d D . . . .
C4 C 0.1756(4) 0.5649(3) 0.79134(18) 0.0535(8) Uani 1 1 d . . . . .
C5 C 0.3765(3) 0.56898(19) 0.67400(13) 0.0285(5) Uani 1 1 d . . . . .
C6 C 0.4040(3) 0.6490(2) 0.56926(14) 0.0326(5) Uani 1 1 d . . . . .
H6 H 0.387076 0.659970 0.516938 0.039 Uiso 1 1 calc R U . . .
C7 C 0.5120(3) 0.7166(2) 0.63164(14) 0.0333(5) Uani 1 1 d . . . . .
H7 H 0.585826 0.785234 0.632462 0.040 Uiso 1 1 calc R U . . .
C8 C 0.1969(3) 0.4669(2) 0.54655(13) 0.0301(5) Uani 1 1 d . . . . .
C9 C 0.2178(3) 0.4248(2) 0.46521(14) 0.0307(5) Uani 1 1 d . . . . .
H9 H 0.310778 0.458429 0.441677 0.037 Uiso 1 1 calc R U . . .
C10 C 0.1005(3) 0.3330(2) 0.41958(14) 0.0353(5) Uani 1 1 d . . . . .
C11 C -0.0352(3) 0.2833(2) 0.45234(16) 0.0396(6) Uani 1 1 d . . . . .
F12 F 0.1192(2) 0.28773(15) 0.34154(9) 0.0508(4) Uani 1 1 d . . . . .
C12 C -0.0547(3) 0.3299(3) 0.53288(17) 0.0442(6) Uani 1 1 d . . . . .
F13 F -0.1474(2) 0.19267(14) 0.40729(11) 0.0529(4) Uani 1 1 d . . . . .
C20 C 0.7626(4) 0.4017(2) 0.91693(18) 0.0465(7) Uani 1 1 d . . . . .
H20A H 0.862125 0.423072 0.890316 0.070 Uiso 1 1 calc R U . . .
H20B H 0.781030 0.443845 0.974624 0.070 Uiso 1 1 calc R U . . .
H20C H 0.671822 0.416369 0.889608 0.070 Uiso 1 1 calc R U . . .
C21 C 0.6908(4) 0.2184(2) 0.82297(16) 0.0443(6) Uani 1 1 d . . . . .
H21A H 0.597525 0.231773 0.796705 0.066 Uiso 1 1 calc R U . . .
H21B H 0.666379 0.140288 0.819168 0.066 Uiso 1 1 calc R U . . .
H21C H 0.788403 0.240857 0.795329 0.066 Uiso 1 1 calc R U . . .
C22 C 0.8590(4) 0.2588(3) 0.95153(17) 0.0439(6) Uani 1 1 d . . . . .
H22A H 0.829612 0.180737 0.948351 0.066 Uiso 1 1 calc R U . . .
H22B H 0.880539 0.301658 1.009054 0.066 Uiso 1 1 calc R U . . .
H22C H 0.957401 0.278194 0.923691 0.066 Uiso 1 1 calc R U . . .
C23 C 0.5695(3) 0.2511(2) 0.95244(17) 0.0425(6) Uani 1 1 d . . . . .
H23A H 0.480209 0.269338 0.926972 0.064 Uiso 1 1 calc R U . . .
H23B H 0.590426 0.290931 1.010655 0.064 Uiso 1 1 calc R U . . .
H23C H 0.538708 0.172314 0.946615 0.064 Uiso 1 1 calc R U . . .
C24 C 0.3418(4) 0.9271(3) 0.9036(2) 0.0541(7) Uani 1 1 d . . . . .
H24A H 0.365967 0.970249 0.961728 0.065 Uiso 1 1 calc R U . . .
H24B H 0.377221 0.860280 0.897602 0.065 Uiso 1 1 calc R U . . .
C25 C 0.1611(4) 0.8965(3) 0.8777(2) 0.0526(7) Uani 1 1 d . . . . .
H25A H 0.113022 0.816160 0.860739 0.063 Uiso 1 1 calc R U . . .
H25B H 0.102947 0.928523 0.922819 0.063 Uiso 1 1 calc R U . . .
C26 C 0.1515(5) 0.9436(4) 0.8071(3) 0.0841(13) Uani 1 1 d . . . . .
H26A H 0.070724 0.891160 0.762123 0.101 Uiso 1 1 calc R U . . .
H26B H 0.119944 1.012232 0.824165 0.101 Uiso 1 1 calc R U . . .
C27 C 0.3206(5) 0.9650(4) 0.7809(2) 0.0739(11) Uani 1 1 d . . . . .
H27A H 0.332603 0.899765 0.740087 0.089 Uiso 1 1 calc R U . . .
H27B H 0.344889 1.027274 0.756363 0.089 Uiso 1 1 calc R U . . .
F2 F 0.5660(2) 0.37540(15) 0.73214(11) 0.0502(4) Uani 1 1 d . . . . .
Ni1 Ni 0.30579(4) 0.47055(3) 0.73819(2) 0.03093(10) Uani 1 1 d . . . . .
F1 F 0.5301(2) 0.42327(14) 0.62287(11) 0.0518(4) Uani 1 1 d . . . . .
N1 N 0.3206(2) 0.55909(16) 0.59589(11) 0.0292(4) Uani 1 1 d . . . . .
C1 C 0.4399(3) 0.3804(2) 0.68103(15) 0.0342(5) Uani 1 1 d . . . . .
C13 C 0.0586(3) 0.4216(2) 0.58076(15) 0.0412(6) Uani 1 1 d . . . . .
H13 H 0.042661 0.453127 0.635725 0.049 Uiso 1 1 calc R U . . .
F14 F -0.1914(2) 0.28416(18) 0.56405(11) 0.0636(5) Uani 1 1 d . . . . .
C14 C 0.5911(3) 0.71400(19) 0.77328(13) 0.0293(5) Uani 1 1 d . . . . .
F15 F 0.7476(3) 0.63372(14) 0.93950(11) 0.0667(6) Uani 1 1 d . . . . .
C15 C 0.6256(3) 0.6469(2) 0.81764(15) 0.0385(6) Uani 1 1 d . . . . .
H15 H 0.590118 0.569644 0.796328 0.046 Uiso 1 1 calc R U . . .
F16 F 0.85325(19) 0.85191(13) 0.99946(9) 0.0437(4) Uani 1 1 d . . . . .
C16 C 0.7129(3) 0.6954(2) 0.89360(16) 0.0406(6) Uani 1 1 d . . . . .
F17 F 0.7949(2) 0.98023(12) 0.90783(10) 0.0490(4) Uani 1 1 d . . . . .
C17 C 0.7683(3) 0.8071(2) 0.92488(14) 0.0344(5) Uani 1 1 d . . . . .
C18 C 0.7367(3) 0.87069(19) 0.87785(15) 0.0329(5) Uani 1 1 d . . . . .
C19 C 0.6472(3) 0.82679(19) 0.80226(15) 0.0321(5) Uani 1 1 d . . . . .
H19 H 0.624730 0.872353 0.770996 0.038 Uiso 1 1 calc R U . . .
F3A F 0.4752(5) 0.2194(3) 0.5924(3) 0.0482(9) Uani 0.635(6) 1 d . U P A 1
F4A F 0.2452(5) 0.2538(3) 0.5782(2) 0.0524(10) Uani 0.635(6) 1 d . U P A 1
F5A F 0.3026(4) 0.1992(2) 0.68126(19) 0.0491(8) Uani 0.635(6) 1 d . U P A 1
F6A F 0.0881(5) 0.3014(3) 0.7816(2) 0.0593(9) Uani 0.794(3) 1 d . U P B 1
F7A F 0.3381(3) 0.3302(3) 0.83336(17) 0.0571(7) Uani 0.794(3) 1 d . U P B 1
F8A F 0.1959(3) 0.4342(2) 0.88699(13) 0.0640(7) Uani 0.794(3) 1 d . U P B 1
F9A F 0.0155(4) 0.5160(3) 0.8001(2) 0.0630(9) Uani 0.794(3) 1 d . . P B 1
F10A F 0.1439(4) 0.6402(2) 0.74675(16) 0.0516(6) Uani 0.794(3) 1 d . . P B 1
F11A F 0.2399(4) 0.6374(3) 0.86382(16) 0.0651(8) Uani 0.794(3) 1 d . . P B 1
O2A_1 O 0.6945(3) 0.9826(2) 0.67546(15) 0.0640(6) Uani 0.656(10) 1 d . U P C 1
C28A_1 C 0.6100(13) 1.0006(12) 0.6124(6) 0.0604(18) Uani 0.656(10) 1 d D U P C
1
H28A_1 H 0.568971 1.064714 0.633439 0.073 Uiso 0.656(10) 1 calc R U P C 1
H28B_1 H 0.514982 0.936117 0.588214 0.073 Uiso 0.656(10) 1 calc R U P C 1
C29A_1 C 0.7222(11) 1.0205(7) 0.5499(5) 0.075(2) Uani 0.656(10) 1 d D U P C 1
H29A_1 H 0.693672 1.069493 0.520183 0.090 Uiso 0.656(10) 1 calc R U P C 1
H29B_1 H 0.723638 0.951376 0.510205 0.090 Uiso 0.656(10) 1 calc R U P C 1
C30A_1 C 0.8907(9) 1.0774(7) 0.6059(4) 0.089(2) Uani 0.656(10) 1 d D U P C 1
H30A_1 H 0.985163 1.069322 0.574870 0.107 Uiso 0.656(10) 1 calc R U P C 1
H30B_1 H 0.904384 1.155955 0.631597 0.107 Uiso 0.656(10) 1 calc R U P C 1
C31A_1 C 0.8696(16) 1.0157(11) 0.6657(7) 0.077(2) Uani 0.656(10) 1 d D U P C 1
H31A_1 H 0.932716 1.061293 0.718549 0.093 Uiso 0.656(10) 1 calc R U P C 1
H31B_1 H 0.909077 0.950560 0.646764 0.093 Uiso 0.656(10) 1 calc R U P C 1
F5B F 0.449(3) 0.1983(15) 0.6226(12) 0.094(5) Uani 0.206(3) 1 d . U P A 2
F3B F 0.331(3) 0.2656(13) 0.5555(11) 0.101(4) Uani 0.206(3) 1 d . U P A 2
F4B F 0.219(2) 0.2197(13) 0.6457(12) 0.121(5) Uani 0.206(3) 1 d . U P A 2
F6B F 0.0999(19) 0.3236(13) 0.8207(8) 0.060(3) Uani 0.206(3) 1 d . U P B 2
F7B F 0.2905(15) 0.2683(9) 0.7868(9) 0.078(3) Uani 0.206(3) 1 d D U P B 2
F8B F 0.3378(14) 0.4056(11) 0.8864(6) 0.072(3) Uani 0.206(3) 1 d . U P B 2
F10B F 0.2872(12) 0.6662(9) 0.8321(7) 0.059(3) Uani 0.206(3) 1 d . . P B 2
F11B F 0.1585(9) 0.5327(6) 0.8824(4) 0.0405(19) Uani 0.206(3) 1 d . . P B 2
F18 F 0.0515(14) 0.5983(10) 0.7089(6) 0.061(3) Uani 0.206(3) 1 d . . P B 2
F19 F -0.0296(13) 0.6239(10) 0.8297(6) 0.074(3) Uani 0.206(3) 1 d . . P B 2
F20 F -0.0745(11) 0.4563(9) 0.7497(6) 0.063(3) Uani 0.206(3) 1 d . . P B 2
C32 C 0.032(2) 0.5558(19) 0.7745(12) 0.053(5) Uani 0.206(3) 1 d . . P B 2
O1 O 0.4270(2) 0.98985(16) 0.85307(13) 0.0488(5) Uani 1 1 d . . . . .
O2B_2 O 0.6945(3) 0.9826(2) 0.67546(15) 0.0640(6) Uani 0.344(10) 1 d . U P C 2
C31B_2 C 0.858(3) 1.006(2) 0.6851(12) 0.073(3) Uani 0.344(10) 1 d D U P C 2
H31A_2 H 0.893004 0.957137 0.712853 0.088 Uiso 0.344(10) 1 calc R U P C 2
H31B_2 H 0.909506 1.082967 0.716189 0.088 Uiso 0.344(10) 1 calc R U P C 2
C30B_2 C 0.8959(19) 0.9835(14) 0.5940(9) 0.090(4) Uani 0.344(10) 1 d D U P C 2
H30B_2 H 0.981021 0.954100 0.572799 0.108 Uiso 0.344(10) 1 calc R U P C 2
C29B_2 C 0.798(3) 1.0100(17) 0.5537(12) 0.091(4) Uani 0.344(10) 1 d D U P C 2
H29B_2 H 0.818395 1.032548 0.505187 0.110 Uiso 0.344(10) 1 calc R U P C 2
C28B_2 C 0.639(3) 1.000(3) 0.5959(15) 0.074(3) Uani 0.344(10) 1 d D U P C 2
H28A_2 H 0.604080 1.067354 0.605208 0.088 Uiso 0.344(10) 1 calc R U P C 2
H28B_2 H 0.548213 0.936687 0.564113 0.088 Uiso 0.344(10) 1 calc R U P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N2 C5 1.365(3) . ?
N2 C7 1.394(3) . ?
N2 C14 1.432(3) . ?
C2 F4B 1.252(16) . ?
C2 F5B 1.266(18) . ?
C2 F4A 1.301(4) . ?
C2 F5A 1.344(4) . ?
C2 F3B 1.344(17) . ?
C2 F3A 1.371(5) . ?
C2 C1 1.502(4) . ?
N3 C22 1.489(3) . ?
N3 C20 1.490(3) . ?
N3 C23 1.499(3) . ?
N3 C21 1.499(3) . ?
C3 F6B 1.247(15) . ?
C3 F7A 1.304(4) . ?
C3 F6A 1.377(5) . ?
C3 F8A 1.442(4) . ?
C3 F8B 1.446(10) . ?
C3 F7B 1.590(8) . ?
C3 Ni1 1.928(3) . ?
C4 C32 1.216(18) . ?
C4 F11A 1.345(4) . ?
C4 F9A 1.372(4) . ?
C4 F10B 1.405(11) . ?
C4 F10A 1.469(4) . ?
C4 F11B 1.706(7) . ?
C4 Ni1 1.957(3) . ?
C5 N1 1.360(3) . ?
C5 Ni1 1.893(2) . ?
C6 C7 1.336(3) . ?
C6 N1 1.399(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.386(4) . ?
C8 C9 1.388(3) . ?
C8 N1 1.425(3) . ?
C9 C10 1.375(4) . ?
C9 H9 0.9500 . ?
C10 F12 1.341(3) . ?
C10 C11 1.375(4) . ?
C11 F13 1.344(3) . ?
C11 C12 1.384(4) . ?
C12 F14 1.349(3) . ?
C12 C13 1.372(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 O1 1.423(4) . ?
C24 C25 1.505(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.497(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.495(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 O1 1.417(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
F2 C1 1.390(3) . ?
Ni1 C1 1.969(3) . ?
F1 C1 1.407(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(3) . ?
C14 C19 1.385(3) . ?
F15 C16 1.343(3) . ?
C15 C16 1.377(3) . ?
C15 H15 0.9500 . ?
F16 C17 1.347(3) . ?
C16 C17 1.376(4) . ?
F17 C18 1.349(3) . ?
C17 C18 1.368(4) . ?
C18 C19 1.376(3) . ?
C19 H19 0.9500 . ?
O2A_1 C28A_1 1.380(11) . ?
O2A_1 C31A_1 1.464(13) . ?
C28A_1 C29A_1 1.474(9) . ?
C28A_1 H28A_1 0.9900 . ?
C28A_1 H28B_1 0.9900 . ?
C29A_1 C30A_1 1.584(11) . ?
C29A_1 H29A_1 0.9900 . ?
C29A_1 H29B_1 0.9900 . ?
C30A_1 C31A_1 1.443(11) . ?
C30A_1 H30A_1 0.9900 . ?
C30A_1 H30B_1 0.9900 . ?
C31A_1 H31A_1 0.9900 . ?
C31A_1 H31B_1 0.9900 . ?
F18 C32 1.37(3) . ?
F19 C32 1.347(18) . ?
F20 C32 1.33(3) . ?
O2B_2 C31B_2 1.34(3) . ?
O2B_2 C28B_2 1.51(3) . ?
C31B_2 C30B_2 1.561(19) . ?
C31B_2 H31A_2 0.9900 . ?
C31B_2 H31B_2 0.9900 . ?
C30B_2 C29B_2 1.24(3) . ?
C30B_2 H30B_2 0.9500 . ?
C29B_2 C28B_2 1.55(2) . ?
C29B_2 H29B_2 0.9500 . ?
C28B_2 H28A_2 0.9900 . ?
C28B_2 H28B_2 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
C5 N2 C7 111.45(19) . . ?
C5 N2 C14 124.77(19) . . ?
C7 N2 C14 123.8(2) . . ?
F4B C2 F5B 112.2(13) . . ?
F4A C2 F5A 108.7(3) . . ?
F4B C2 F3B 98.4(13) . . ?
F5B C2 F3B 100.9(12) . . ?
F4A C2 F3A 107.1(3) . . ?
F5A C2 F3A 104.9(3) . . ?
F4B C2 C1 117.0(7) . . ?
F5B C2 C1 118.3(9) . . ?
F4A C2 C1 112.5(3) . . ?
F5A C2 C1 112.2(3) . . ?
F3B C2 C1 106.2(7) . . ?
F3A C2 C1 111.0(3) . . ?
C22 N3 C20 110.2(2) . . ?
C22 N3 C23 109.7(2) . . ?
C20 N3 C23 109.1(2) . . ?
C22 N3 C21 109.2(2) . . ?
C20 N3 C21 109.4(2) . . ?
C23 N3 C21 109.2(2) . . ?
F7A C3 F6A 108.7(3) . . ?
F7A C3 F8A 101.2(3) . . ?
F6A C3 F8A 98.4(3) . . ?
F6B C3 F8B 105.3(8) . . ?
F6B C3 F7B 88.6(9) . . ?
F8B C3 F7B 86.1(8) . . ?
F6B C3 Ni1 132.1(7) . . ?
F7A C3 Ni1 119.9(2) . . ?
F6A C3 Ni1 112.6(2) . . ?
F8A C3 Ni1 113.5(2) . . ?
F8B C3 Ni1 117.1(5) . . ?
F7B C3 Ni1 114.5(4) . . ?
F11A C4 F9A 106.5(3) . . ?
C32 C4 F10B 121.7(11) . . ?
F11A C4 F10A 99.1(3) . . ?
F9A C4 F10A 97.3(3) . . ?
C32 C4 F11B 98.1(12) . . ?
F10B C4 F11B 89.2(6) . . ?
C32 C4 Ni1 128.1(8) . . ?
F11A C4 Ni1 117.4(3) . . ?
F9A C4 Ni1 117.7(3) . . ?
F10B C4 Ni1 106.6(5) . . ?
F10A C4 Ni1 115.59(19) . . ?
F11B C4 Ni1 100.4(3) . . ?
N1 C5 N2 103.65(19) . . ?
N1 C5 Ni1 128.24(17) . . ?
N2 C5 Ni1 128.11(16) . . ?
C7 C6 N1 106.8(2) . . ?
C7 C6 H6 126.6 . . ?
N1 C6 H6 126.6 . . ?
C6 C7 N2 106.8(2) . . ?
C6 C7 H7 126.6 . . ?
N2 C7 H7 126.6 . . ?
C13 C8 C9 121.5(2) . . ?
C13 C8 N1 119.3(2) . . ?
C9 C8 N1 119.1(2) . . ?
C10 C9 C8 118.2(2) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
F12 C10 C11 118.2(2) . . ?
F12 C10 C9 120.0(2) . . ?
C11 C10 C9 121.8(2) . . ?
F13 C11 C10 121.1(2) . . ?
F13 C11 C12 120.6(3) . . ?
C10 C11 C12 118.3(2) . . ?
F14 C12 C13 119.5(3) . . ?
F14 C12 C11 118.4(3) . . ?
C13 C12 C11 122.0(3) . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N3 C21 H21A 109.5 . . ?
N3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O1 C24 C25 108.3(3) . . ?
O1 C24 H24A 110.0 . . ?
C25 C24 H24A 110.0 . . ?
O1 C24 H24B 110.0 . . ?
C25 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
C26 C25 C24 104.1(3) . . ?
C26 C25 H25A 110.9 . . ?
C24 C25 H25A 110.9 . . ?
C26 C25 H25B 110.9 . . ?
C24 C25 H25B 110.9 . . ?
H25A C25 H25B 109.0 . . ?
C27 C26 C25 104.5(3) . . ?
C27 C26 H26A 110.9 . . ?
C25 C26 H26A 110.9 . . ?
C27 C26 H26B 110.9 . . ?
C25 C26 H26B 110.9 . . ?
H26A C26 H26B 108.9 . . ?
O1 C27 C26 105.5(3) . . ?
O1 C27 H27A 110.6 . . ?
C26 C27 H27A 110.6 . . ?
O1 C27 H27B 110.6 . . ?
C26 C27 H27B 110.6 . . ?
H27A C27 H27B 108.8 . . ?
C5 Ni1 C3 176.43(12) . . ?
C5 Ni1 C4 87.60(12) . . ?
C3 Ni1 C4 90.17(15) . . ?
C5 Ni1 C1 89.52(10) . . ?
C3 Ni1 C1 92.71(13) . . ?
C4 Ni1 C1 177.12(12) . . ?
C5 N1 C6 111.38(19) . . ?
C5 N1 C8 124.2(2) . . ?
C6 N1 C8 124.38(19) . . ?
F2 C1 F1 100.38(19) . . ?
F2 C1 C2 104.3(2) . . ?
F1 C1 C2 101.6(2) . . ?
F2 C1 Ni1 113.29(17) . . ?
F1 C1 Ni1 114.01(16) . . ?
C2 C1 Ni1 120.76(18) . . ?
C12 C13 C8 118.0(2) . . ?
C12 C13 H13 121.0 . . ?
C8 C13 H13 121.0 . . ?
C15 C14 C19 121.6(2) . . ?
C15 C14 N2 119.8(2) . . ?
C19 C14 N2 118.6(2) . . ?
C16 C15 C14 118.1(2) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
F15 C16 C17 117.8(2) . . ?
F15 C16 C15 120.3(2) . . ?
C17 C16 C15 121.9(2) . . ?
F16 C17 C18 121.4(2) . . ?
F16 C17 C16 120.4(2) . . ?
C18 C17 C16 118.2(2) . . ?
F17 C18 C17 118.1(2) . . ?
F17 C18 C19 119.5(2) . . ?
C17 C18 C19 122.4(2) . . ?
C18 C19 C14 117.8(2) . . ?
C18 C19 H19 121.1 . . ?
C14 C19 H19 121.1 . . ?
C28A_1 O2A_1 C31A_1 108.3(6) . . ?
O2A_1 C28A_1 C29A_1 108.5(8) . . ?
O2A_1 C28A_1 H28A_1 110.0 . . ?
C29A_1 C28A_1 H28A_1 110.0 . . ?
O2A_1 C28A_1 H28B_1 110.0 . . ?
C29A_1 C28A_1 H28B_1 110.0 . . ?
H28A_1 C28A_1 H28B_1 108.4 . . ?
C28A_1 C29A_1 C30A_1 100.3(7) . . ?
C28A_1 C29A_1 H29A_1 111.7 . . ?
C30A_1 C29A_1 H29A_1 111.7 . . ?
C28A_1 C29A_1 H29B_1 111.7 . . ?
C30A_1 C29A_1 H29B_1 111.7 . . ?
H29A_1 C29A_1 H29B_1 109.5 . . ?
C31A_1 C30A_1 C29A_1 100.5(7) . . ?
C31A_1 C30A_1 H30A_1 111.7 . . ?
C29A_1 C30A_1 H30A_1 111.7 . . ?
C31A_1 C30A_1 H30B_1 111.7 . . ?
C29A_1 C30A_1 H30B_1 111.7 . . ?
H30A_1 C30A_1 H30B_1 109.4 . . ?
C30A_1 C31A_1 O2A_1 107.4(9) . . ?
C30A_1 C31A_1 H31A_1 110.2 . . ?
O2A_1 C31A_1 H31A_1 110.2 . . ?
C30A_1 C31A_1 H31B_1 110.2 . . ?
O2A_1 C31A_1 H31B_1 110.2 . . ?
H31A_1 C31A_1 H31B_1 108.5 . . ?
C4 C32 F20 119.2(17) . . ?
C4 C32 F19 114.1(14) . . ?
F20 C32 F19 110.8(17) . . ?
C4 C32 F18 97.3(17) . . ?
F20 C32 F18 108.0(14) . . ?
F19 C32 F18 105.4(17) . . ?
C27 O1 C24 106.8(3) . . ?
C31B_2 O2B_2 C28B_2 110.6(13) . . ?
O2B_2 C31B_2 C30B_2 100.6(16) . . ?
O2B_2 C31B_2 H31A_2 111.6 . . ?
C30B_2 C31B_2 H31A_2 111.6 . . ?
O2B_2 C31B_2 H31B_2 111.6 . . ?
C30B_2 C31B_2 H31B_2 111.6 . . ?
H31A_2 C31B_2 H31B_2 109.4 . . ?
C29B_2 C30B_2 C31B_2 109.6(16) . . ?
C29B_2 C30B_2 H30B_2 125.2 . . ?
C31B_2 C30B_2 H30B_2 125.2 . . ?
C30B_2 C29B_2 C28B_2 108.1(18) . . ?
C30B_2 C29B_2 H29B_2 125.9 . . ?
C28B_2 C29B_2 H29B_2 125.9 . . ?
O2B_2 C28B_2 C29B_2 100.2(17) . . ?
O2B_2 C28B_2 H28A_2 111.7 . . ?
C29B_2 C28B_2 H28A_2 111.7 . . ?
O2B_2 C28B_2 H28B_2 111.7 . . ?
C29B_2 C28B_2 H28B_2 111.7 . . ?
H28A_2 C28B_2 H28B_2 109.5 . . ?

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
C7 N2 C5 N1 0.3(2) . . . . ?
C14 N2 C5 N1 179.6(2) . . . . ?
C7 N2 C5 Ni1 -179.55(17) . . . . ?
C14 N2 C5 Ni1 -0.3(3) . . . . ?
N1 C6 C7 N2 0.9(3) . . . . ?
C5 N2 C7 C6 -0.8(3) . . . . ?
C14 N2 C7 C6 179.9(2) . . . . ?
C13 C8 C9 C10 -2.8(4) . . . . ?
N1 C8 C9 C10 177.3(2) . . . . ?
C8 C9 C10 F12 -177.8(2) . . . . ?
C8 C9 C10 C11 0.3(4) . . . . ?
F12 C10 C11 F13 -0.8(4) . . . . ?
C9 C10 C11 F13 -178.9(2) . . . . ?
F12 C10 C11 C12 179.9(2) . . . . ?
C9 C10 C11 C12 1.9(4) . . . . ?
F13 C11 C12 F14 -2.2(4) . . . . ?
C10 C11 C12 F14 177.0(2) . . . . ?
F13 C11 C12 C13 179.2(3) . . . . ?
C10 C11 C12 C13 -1.6(4) . . . . ?
O1 C24 C25 C26 1.8(4) . . . . ?
C24 C25 C26 C27 17.4(4) . . . . ?
C25 C26 C27 O1 -31.1(5) . . . . ?
N1 C5 Ni1 C4 -99.7(2) . . . . ?
N2 C5 Ni1 C4 80.1(2) . . . . ?
N1 C5 Ni1 C1 80.0(2) . . . . ?
N2 C5 Ni1 C1 -100.1(2) . . . . ?
N2 C5 N1 C6 0.2(2) . . . . ?
Ni1 C5 N1 C6 -179.90(17) . . . . ?
N2 C5 N1 C8 178.1(2) . . . . ?
Ni1 C5 N1 C8 -2.0(3) . . . . ?
C7 C6 N1 C5 -0.7(3) . . . . ?
C7 C6 N1 C8 -178.6(2) . . . . ?
C13 C8 N1 C5 43.3(3) . . . . ?
C9 C8 N1 C5 -136.8(2) . . . . ?
C13 C8 N1 C6 -139.1(2) . . . . ?
C9 C8 N1 C6 40.8(3) . . . . ?
F4B C2 C1 F2 113.0(14) . . . . ?
F5B C2 C1 F2 -26.0(12) . . . . ?
F4A C2 C1 F2 -176.7(3) . . . . ?
F5A C2 C1 F2 60.4(3) . . . . ?
F3B C2 C1 F2 -138.4(10) . . . . ?
F3A C2 C1 F2 -56.7(3) . . . . ?
F4B C2 C1 F1 -143.0(14) . . . . ?
F5B C2 C1 F1 78.0(12) . . . . ?
F4A C2 C1 F1 -72.7(3) . . . . ?
F5A C2 C1 F1 164.4(2) . . . . ?
F3B C2 C1 F1 -34.4(10) . . . . ?
F3A C2 C1 F1 47.3(3) . . . . ?
F4B C2 C1 Ni1 -15.7(14) . . . . ?
F5B C2 C1 Ni1 -154.8(12) . . . . ?
F4A C2 C1 Ni1 54.6(4) . . . . ?
F5A C2 C1 Ni1 -68.4(3) . . . . ?
F3B C2 C1 Ni1 92.9(10) . . . . ?
F3A C2 C1 Ni1 174.6(2) . . . . ?
F14 C12 C13 C8 -179.5(2) . . . . ?
C11 C12 C13 C8 -0.9(4) . . . . ?
C9 C8 C13 C12 3.1(4) . . . . ?
N1 C8 C13 C12 -177.0(2) . . . . ?
C5 N2 C14 C15 30.4(3) . . . . ?
C7 N2 C14 C15 -150.4(2) . . . . ?
C5 N2 C14 C19 -149.8(2) . . . . ?
C7 N2 C14 C19 29.4(3) . . . . ?
C19 C14 C15 C16 2.4(4) . . . . ?
N2 C14 C15 C16 -177.8(2) . . . . ?
C14 C15 C16 F15 179.1(3) . . . . ?
C14 C15 C16 C17 -1.3(4) . . . . ?
F15 C16 C17 F16 -0.5(4) . . . . ?
C15 C16 C17 F16 179.9(3) . . . . ?
F15 C16 C17 C18 178.6(3) . . . . ?
C15 C16 C17 C18 -1.0(4) . . . . ?
F16 C17 C18 F17 0.8(4) . . . . ?
C16 C17 C18 F17 -178.3(2) . . . . ?
F16 C17 C18 C19 -178.6(2) . . . . ?
C16 C17 C18 C19 2.3(4) . . . . ?
F17 C18 C19 C14 179.3(2) . . . . ?
C17 C18 C19 C14 -1.3(4) . . . . ?
C15 C14 C19 C18 -1.2(4) . . . . ?
N2 C14 C19 C18 179.0(2) . . . . ?
C31A_1 O2A_1 C28A_1 C29A_1 13.4(12) . . . . ?
O2A_1 C28A_1 C29A_1 C30A_1 -31.6(10) . . . . ?
C28A_1 C29A_1 C30A_1 C31A_1 37.5(11) . . . . ?
C29A_1 C30A_1 C31A_1 O2A_1 -31.2(11) . . . . ?
C28A_1 O2A_1 C31A_1 C30A_1 13.0(12) . . . . ?
F10B C4 C32 F20 -167.8(12) . . . . ?
F11B C4 C32 F20 -73.7(17) . . . . ?
Ni1 C4 C32 F20 36(3) . . . . ?
F10B C4 C32 F19 -34(3) . . . . ?
F11B C4 C32 F19 60(2) . . . . ?
Ni1 C4 C32 F19 170.6(11) . . . . ?
F10B C4 C32 F18 76.8(13) . . . . ?
F11B C4 C32 F18 171.0(10) . . . . ?
Ni1 C4 C32 F18 -78.9(17) . . . . ?
C26 C27 O1 C24 32.9(4) . . . . ?
C25 C24 O1 C27 -21.7(4) . . . . ?
C28B_2 O2B_2 C31B_2 C30B_2 -26(2) . . . . ?
O2B_2 C31B_2 C30B_2 C29B_2 35(2) . . . . ?
C31B_2 C30B_2 C29B_2 C28B_2 -27(2) . . . . ?
C31B_2 O2B_2 C28B_2 C29B_2 13(2) . . . . ?
C30B_2 C29B_2 C28B_2 O2B_2 10(2) . . . . ?

_refine_diff_density_max         0.966
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.063


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF, n-pentane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
