# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_felix122a
_database_code_depnum_ccdc_archive 'CCDC 1571580'
_audit_update_record             
;
2017-08-30 deposited with the CCDC.
2017-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H12 N2 Ni O5'
_chemical_formula_weight         358.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   21.7637(9)
_cell_length_b                   6.8956(3)
_cell_length_c                   18.7940(7)
_cell_angle_alpha                90
_cell_angle_beta                 101.478(3)
_cell_angle_gamma                90
_cell_volume                     2764.1(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    11650
_cell_measurement_theta_min      1.910
_cell_measurement_theta_max      26.005

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_F_000             1472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.433
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7360
_exptl_absorpt_correction_T_max  0.8440
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11650
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.910
_diffrn_reflns_theta_max         26.005
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2717
_reflns_number_gt                2151
_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       'X-Area (STOE, 2008)'
_computing_cell_refinement       'X-Area (STOE, 2008)'
_computing_data_reduction        'X-Area (STOE, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_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)+(0.0368P)²+9.8074P] 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         2717
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1121
_refine_ls_wR_factor_gt          0.1038
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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 0.31332(3) 0.44638(8) 0.48890(3) 0.03760(17) Uani 1 1 d . . . . .
O1 O 0.13958(15) 0.5996(5) 0.4860(2) 0.0538(9) Uani 1 1 d . . . . .
O2 O 0.23071(16) 0.5126(5) 0.45154(19) 0.0567(9) Uani 1 1 d . . . . .
O3 O 0.32847(17) 0.3928(5) 0.39748(18) 0.0567(9) Uani 1 1 d . . . . .
O4 O 0.40035(17) 0.2466(5) 0.34259(17) 0.0562(9) Uani 1 1 d . . . . .
O5 O 0.42399(15) 0.3401(5) 0.71764(17) 0.0470(8) Uani 1 1 d . . . . .
N1 N 0.29366(15) 0.4930(5) 0.5795(2) 0.0356(8) Uani 1 1 d . . . . .
N2 N 0.39612(16) 0.3701(5) 0.52342(18) 0.0352(8) Uani 1 1 d . . . . .
C1 C 0.23224(19) 0.5413(7) 0.5749(2) 0.0401(9) Uani 1 1 d . . . . .
C2 C 0.2076(2) 0.5758(8) 0.6352(3) 0.0528(12) Uani 1 1 d . . . . .
H2 H 0.1650 0.6130 0.6306 0.063 Uiso 1 1 calc R U . . .
C3 C 0.2458(2) 0.5558(9) 0.7028(3) 0.0634(14) Uani 1 1 d . . . . .
H3 H 0.2292 0.5732 0.7454 0.076 Uiso 1 1 calc R U . . .
C4 C 0.3081(2) 0.5102(8) 0.7079(3) 0.0528(13) Uani 1 1 d . . . . .
H4 H 0.3350 0.4994 0.7542 0.063 Uiso 1 1 calc R U . . .
C5 C 0.33149(19) 0.4801(6) 0.6454(2) 0.0371(9) Uani 1 1 d . . . . .
C6 C 0.40203(19) 0.4532(7) 0.6548(2) 0.0403(9) Uani 1 1 d . . . . .
C7 C 0.42923(19) 0.3722(6) 0.5923(2) 0.0362(9) Uani 1 1 d . . . . .
C8 C 0.4244(2) 0.3046(6) 0.4696(2) 0.0376(9) Uani 1 1 d . . . . .
C9 C 0.4854(2) 0.2402(6) 0.4827(2) 0.0403(10) Uani 1 1 d . . . . .
H9 H 0.5036 0.1928 0.4442 0.048 Uiso 1 1 calc R U . . .
C10 C 0.5196(2) 0.2456(7) 0.5529(3) 0.0437(10) Uani 1 1 d . . . . .
H10 H 0.5621 0.2043 0.5633 0.052 Uiso 1 1 calc R U . . .
C11 C 0.4914(2) 0.3114(6) 0.6073(2) 0.0407(10) Uani 1 1 d . . . . .
H11 H 0.5145 0.3156 0.6558 0.049 Uiso 1 1 calc R U . . .
C12 C 0.1960(2) 0.5548(7) 0.4991(2) 0.0426(10) Uani 1 1 d . . . . .
C13 C 0.3828(2) 0.3113(7) 0.3959(2) 0.0441(10) Uani 1 1 d . . . . .
C14 C 0.4037(3) 0.1425(7) 0.7096(3) 0.0551(13) Uani 1 1 d . . . . .
H14A H 0.3584 0.1382 0.6910 0.083 Uiso 1 1 calc R U . . .
H14B H 0.4136 0.0774 0.7569 0.083 Uiso 1 1 calc R U . . .
H14C H 0.4253 0.0765 0.6755 0.083 Uiso 1 1 calc R U . . .
C15 C 0.4317(2) 0.6583(6) 0.6734(3) 0.0450(11) Uani 1 1 d . . . . .
H15A H 0.4220 0.7038 0.7193 0.068 Uiso 1 1 calc R U . . .
H15B H 0.4145 0.7495 0.6345 0.068 Uiso 1 1 calc R U . . .
H15C H 0.4773 0.6502 0.6780 0.068 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 O3 1.850(3) . ?
Ni1 O2 1.853(3) . ?
Ni1 N1 1.863(4) . ?
Ni1 N2 1.865(4) . ?
O1 C12 1.243(5) . ?
O2 C12 1.312(5) . ?
O3 C13 1.314(6) . ?
O4 C13 1.226(5) . ?
O5 C6 1.416(5) . ?
O5 C14 1.431(6) . ?
N1 C5 1.347(6) . ?
N1 C1 1.364(5) . ?
N2 C7 1.350(5) . ?
N2 C8 1.361(5) . ?
C1 C2 1.366(6) . ?
C1 C12 1.488(6) . ?
C2 C3 1.379(7) . ?
C3 C4 1.375(7) . ?
C4 C5 1.387(6) . ?
C5 C6 1.521(6) . ?
C6 C7 1.524(6) . ?
C6 C15 1.565(6) . ?
C7 C11 1.390(6) . ?
C8 C9 1.376(6) . ?
C8 C13 1.496(6) . ?
C9 C10 1.380(7) . ?
C10 C11 1.370(6) . ?

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
O3 Ni1 O2 92.07(16) . . ?
O3 Ni1 N1 176.70(16) . . ?
O2 Ni1 N1 85.51(15) . . ?
O3 Ni1 N2 85.89(15) . . ?
O2 Ni1 N2 177.31(16) . . ?
N1 Ni1 N2 96.46(15) . . ?
C12 O2 Ni1 116.3(3) . . ?
C13 O3 Ni1 115.7(3) . . ?
C6 O5 C14 113.0(4) . . ?
C5 N1 C1 119.0(4) . . ?
C5 N1 Ni1 128.3(3) . . ?
C1 N1 Ni1 112.7(3) . . ?
C7 N2 C8 118.8(4) . . ?
C7 N2 Ni1 128.7(3) . . ?
C8 N2 Ni1 112.5(3) . . ?
N1 C1 C2 122.1(4) . . ?
N1 C1 C12 113.6(4) . . ?
C2 C1 C12 124.3(4) . . ?
C1 C2 C3 118.8(4) . . ?
C4 C3 C2 119.5(5) . . ?
C3 C4 C5 119.8(5) . . ?
N1 C5 C4 120.6(4) . . ?
N1 C5 C6 122.2(4) . . ?
C4 C5 C6 116.8(4) . . ?
O5 C6 C5 109.3(3) . . ?
O5 C6 C7 108.8(3) . . ?
C5 C6 C7 119.5(4) . . ?
O5 C6 C15 104.9(3) . . ?
C5 C6 C15 106.1(4) . . ?
C7 C6 C15 107.3(4) . . ?
N2 C7 C11 120.2(4) . . ?
N2 C7 C6 121.9(4) . . ?
C11 C7 C6 117.8(4) . . ?
N2 C8 C9 122.5(4) . . ?
N2 C8 C13 113.5(4) . . ?
C9 C8 C13 124.1(4) . . ?
C8 C9 C10 118.7(4) . . ?
C11 C10 C9 119.0(4) . . ?
C10 C11 C7 120.7(4) . . ?
O1 C12 O2 126.9(4) . . ?
O1 C12 C1 121.3(4) . . ?
O2 C12 C1 111.8(4) . . ?
O4 C13 O3 127.0(4) . . ?
O4 C13 C8 121.0(4) . . ?
O3 C13 C8 111.9(4) . . ?

_refine_diff_density_max         0.556
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.071

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_felix129
_database_code_depnum_ccdc_archive 'CCDC 1571581'
_audit_update_record             
;
2017-08-30 deposited with the CCDC.
2017-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H60 N4 Ni2 O16'
_chemical_formula_weight         994.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   13.5292(9)
_cell_length_b                   13.8175(11)
_cell_length_c                   14.1756(11)
_cell_angle_alpha                92.609(7)
_cell_angle_beta                 100.302(6)
_cell_angle_gamma                116.725(6)
_cell_volume                     2304.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    17517
_cell_measurement_theta_min      1.475
_cell_measurement_theta_max      26.004

_exptl_crystal_description       block
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_F_000             1048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.890
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8064
_exptl_absorpt_correction_T_max  0.9093
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17517
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.475
_diffrn_reflns_theta_max         26.004
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             8835
_reflns_number_gt                6489
_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       'X-Area (STOE, 2008)'
_computing_cell_refinement       'X-Area (STOE, 2008)'
_computing_data_reduction        'X-Area (STOE, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_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)+(0.0584P)²+0.6521P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8835
_refine_ls_number_parameters     612
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1201
_refine_ls_wR_factor_gt          0.1092
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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 0.42525(4) 0.71923(4) 0.77541(3) 0.04142(12) Uani 1 1 d . . . . .
N1 N 0.4880(3) 0.8823(2) 0.81902(19) 0.0438(6) Uani 1 1 d . . . . .
C1 C 0.4034(3) 0.9063(3) 0.8299(2) 0.0465(8) Uani 1 1 d . . . . .
C2 C 0.4258(4) 1.0090(3) 0.8686(3) 0.0545(9) Uani 1 1 d . . . . .
H2 H 0.3655 1.0247 0.8749 0.065 Uiso 1 1 calc R U . . .
C3 C 0.5377(4) 1.0893(3) 0.8982(3) 0.0598(10) Uani 1 1 d . . . . .
H3 H 0.5556 1.1605 0.9264 0.072 Uiso 1 1 calc R U . . .
C4 C 0.6226(4) 1.0640(3) 0.8860(3) 0.0557(9) Uani 1 1 d . . . . .
H4 H 0.6998 1.1184 0.9053 0.067 Uiso 1 1 calc R U . . .
C5 C 0.5961(3) 0.9592(3) 0.8458(2) 0.0455(8) Uani 1 1 d . . . . .
C6 C 0.6903(3) 0.9387(3) 0.8177(3) 0.0487(8) Uani 1 1 d . . . . .
C7 C 0.6839(3) 0.8254(3) 0.8201(2) 0.0433(7) Uani 1 1 d . . . . .
C8 C 0.7841(3) 0.8174(3) 0.8341(3) 0.0491(8) Uani 1 1 d . . . . .
H8 H 0.8551 0.8820 0.8495 0.059 Uiso 1 1 calc R U . . .
C9 C 0.7808(3) 0.7160(3) 0.8258(2) 0.0486(8) Uani 1 1 d . . . . .
H9 H 0.8492 0.7102 0.8362 0.058 Uiso 1 1 calc R U . . .
C10 C 0.6775(3) 0.6235(3) 0.8023(2) 0.0440(8) Uani 1 1 d . . . . .
H10 H 0.6732 0.5529 0.7970 0.053 Uiso 1 1 calc R U . . .
C11 C 0.5799(3) 0.6351(3) 0.7863(2) 0.0413(7) Uani 1 1 d . . . . .
N2 N 0.5832(2) 0.7345(2) 0.79585(19) 0.0419(6) Uani 1 1 d . . . . .
C12 C 0.2849(3) 0.8136(3) 0.7949(3) 0.0494(8) Uani 1 1 d . . . . .
O1 O 0.2035(2) 0.8338(2) 0.7970(2) 0.0645(7) Uani 1 1 d . . . . .
O2 O 0.2748(2) 0.7215(2) 0.76675(17) 0.0480(6) Uani 1 1 d . . . . .
C13 C 0.4626(3) 0.5389(3) 0.7532(2) 0.0424(7) Uani 1 1 d . . . . .
O3 O 0.3786(2) 0.55787(19) 0.74007(16) 0.0441(5) Uani 1 1 d . . . . .
O4 O 0.4602(2) 0.44778(18) 0.74145(17) 0.0464(5) Uani 1 1 d . . . . .
C14 C 0.6970(4) 0.9660(3) 0.7136(3) 0.0567(9) Uani 1 1 d . . . . .
H14A H 0.7053 1.0399 0.7102 0.085 Uiso 1 1 calc R U . . .
H14B H 0.6275 0.9130 0.6680 0.085 Uiso 1 1 calc R U . . .
H14C H 0.7626 0.9625 0.6967 0.085 Uiso 1 1 calc R U . . .
O5 O 0.7978(2) 1.0187(2) 0.87482(19) 0.0567(6) Uani 1 1 d . . . . .
C15 C 0.8145(4) 1.0092(4) 0.9772(3) 0.0626(10) Uani 1 1 d . . . . .
H15A H 0.7511 0.9423 0.9881 0.094 Uiso 1 1 calc R U . . .
H15B H 0.8179 1.0729 1.0138 0.094 Uiso 1 1 calc R U . . .
H15C H 0.8857 1.0058 0.9989 0.094 Uiso 1 1 calc R U . . .
O6 O 0.4202(2) 0.7319(2) 0.62841(17) 0.0582(7) Uani 1 1 d . . . . .
H6 H 0.4581 0.7080 0.6032 0.087 Uiso 1 1 d R U . . .
C16 C 0.3832(4) 0.7921(4) 0.5664(3) 0.0633(11) Uani 1 1 d . . . . .
H16A H 0.4251 0.8079 0.5137 0.076 Uiso 1 1 calc R U . . .
H16B H 0.4024 0.8629 0.6036 0.076 Uiso 1 1 calc R U . . .
C17 C 0.2601(4) 0.7350(4) 0.5228(3) 0.0797(13) Uani 1 1 d . . . . .
H17A H 0.2397 0.6635 0.4878 0.119 Uiso 1 1 calc R U . . .
H17B H 0.2412 0.7790 0.4776 0.119 Uiso 1 1 calc R U . . .
H17C H 0.2178 0.7249 0.5740 0.119 Uiso 1 1 calc R U . . .
O7 O 0.4216(2) 0.69253(19) 0.92231(16) 0.0479(6) Uani 1 1 d . . . . .
H7 H 0.4866 0.7212 0.9591 0.072 Uiso 1 1 d R U . . .
C18 C 0.3546(4) 0.5869(4) 0.9474(3) 0.0685(12) Uani 1 1 d . . . . .
H18A H 0.2798 0.5526 0.9011 0.082 Uiso 0.6 1 calc R U P A 1
H18B H 0.3919 0.5410 0.9379 0.082 Uiso 0.6 1 calc R U P A 1
H18C H 0.3111 0.5959 0.9933 0.082 Uiso 0.4 1 calc R U P B 2
H18D H 0.2987 0.5404 0.8879 0.082 Uiso 0.4 1 calc R U P B 2
C19 C 0.3353(7) 0.5836(7) 1.0434(5) 0.071(2) Uani 0.6 1 d . . P C 1
H19A H 0.2887 0.5075 1.0520 0.107 Uiso 0.6 1 calc R U P C 1
H19B H 0.4082 0.6146 1.0904 0.107 Uiso 0.6 1 calc R U P C 1
H19C H 0.2957 0.6263 1.0535 0.107 Uiso 0.6 1 calc R U P C 1
C19' C 0.4113(11) 0.5281(9) 0.9892(7) 0.073(3) Uani 0.4 1 d . . P C 2
H19D H 0.3553 0.4578 1.0026 0.109 Uiso 0.4 1 calc R U P C 2
H19E H 0.4525 0.5153 0.9440 0.109 Uiso 0.4 1 calc R U P C 2
H19F H 0.4650 0.5711 1.0498 0.109 Uiso 0.4 1 calc R U P C 2
Ni2 Ni 0.33713(4) 0.29320(3) 0.67883(3) 0.04061(12) Uani 1 1 d . . . . .
N21 N 0.2631(2) 0.3446(2) 0.56984(19) 0.0429(6) Uani 1 1 d . . . . .
C21 C 0.3259(3) 0.3757(3) 0.5019(2) 0.0439(7) Uani 1 1 d . . . . .
C22 C 0.3014(3) 0.4276(3) 0.4273(2) 0.0517(9) Uani 1 1 d . . . . .
H22 H 0.3483 0.4512 0.3818 0.062 Uiso 1 1 calc R U . . .
C23 C 0.2073(4) 0.4444(3) 0.4201(3) 0.0570(10) Uani 1 1 d . . . . .
H23 H 0.1883 0.4798 0.3694 0.068 Uiso 1 1 calc R U . . .
C24 C 0.1408(3) 0.4089(3) 0.4878(2) 0.0517(9) Uani 1 1 d . . . . .
H24 H 0.0739 0.4169 0.4819 0.062 Uiso 1 1 calc R U . . .
C25 C 0.1722(3) 0.3614(3) 0.5643(2) 0.0442(8) Uani 1 1 d . . . . .
C26 C 0.0903(3) 0.3149(3) 0.6329(2) 0.0457(8) Uani 1 1 d . . . . .
C27 C 0.1357(3) 0.3036(3) 0.7376(2) 0.0451(8) Uani 1 1 d . . . . .
C28 C 0.0715(4) 0.2995(3) 0.8058(3) 0.0580(10) Uani 1 1 d . . . . .
H28 H 0.0085 0.3137 0.7895 0.070 Uiso 1 1 calc R U . . .
C29 C 0.0996(4) 0.2750(4) 0.8964(3) 0.0655(11) Uani 1 1 d . . . . .
H29 H 0.0562 0.2716 0.9430 0.079 Uiso 1 1 calc R U . . .
C30 C 0.1922(4) 0.2553(4) 0.9187(3) 0.0599(10) Uani 1 1 d . . . . .
H30 H 0.2136 0.2387 0.9810 0.072 Uiso 1 1 calc R U . . .
C31 C 0.2526(3) 0.2600(3) 0.8492(2) 0.0477(8) Uani 1 1 d . . . . .
N22 N 0.2249(2) 0.2843(2) 0.75999(19) 0.0435(6) Uani 1 1 d . . . . .
C32 C 0.4213(3) 0.3462(3) 0.5113(3) 0.0473(8) Uani 1 1 d . . . . .
O21 O 0.4734(2) 0.3634(2) 0.44438(18) 0.0576(7) Uani 1 1 d . . . . .
O22 O 0.4403(2) 0.30422(19) 0.58580(17) 0.0465(5) Uani 1 1 d . . . . .
C33 C 0.3529(3) 0.2369(3) 0.8666(3) 0.0469(8) Uani 1 1 d . . . . .
O23 O 0.4008(2) 0.24125(19) 0.79661(17) 0.0466(5) Uani 1 1 d . . . . .
O24 O 0.3807(2) 0.2155(2) 0.94890(17) 0.0553(6) Uani 1 1 d . . . . .
C34 C -0.0005(3) 0.2002(3) 0.5843(3) 0.0546(9) Uani 1 1 d . . . . .
H34A H -0.0586 0.1708 0.6224 0.082 Uiso 1 1 calc R U . . .
H34B H 0.0347 0.1522 0.5804 0.082 Uiso 1 1 calc R U . . .
H34C H -0.0356 0.2043 0.5188 0.082 Uiso 1 1 calc R U . . .
O25 O 0.0294(2) 0.3759(2) 0.63559(18) 0.0516(6) Uani 1 1 d . . . . .
O26 O 0.2253(2) 0.12695(19) 0.61894(17) 0.0498(6) Uani 1 1 d . . . . .
H26 H 0.2163 0.0911 0.6658 0.075 Uiso 1 1 d R U . . .
C35 C 0.0994(4) 0.4889(3) 0.6784(3) 0.0567(9) Uani 1 1 d . . . . .
H35A H 0.1325 0.4925 0.7467 0.085 Uiso 1 1 calc R U . . .
H35B H 0.0529 0.5268 0.6738 0.085 Uiso 1 1 calc R U . . .
H35C H 0.1603 0.5241 0.6439 0.085 Uiso 1 1 calc R U . . .
C36 C 0.2450(4) 0.0699(3) 0.5436(3) 0.0617(10) Uani 1 1 d . . . . .
H36A H 0.2662 0.1167 0.4923 0.074 Uiso 1 1 calc R U . . .
H36B H 0.1738 0.0026 0.5144 0.074 Uiso 1 1 calc R U . . .
C37 C 0.3362(5) 0.0395(4) 0.5790(4) 0.0826(14) Uani 1 1 d . . . . .
H37A H 0.4064 0.1055 0.6097 0.124 Uiso 1 1 calc R U . . .
H37B H 0.3491 0.0042 0.5243 0.124 Uiso 1 1 calc R U . . .
H37C H 0.3132 -0.0112 0.6264 0.124 Uiso 1 1 calc R U . . .
O41 O 0.1622(2) 1.0036(2) 0.7594(2) 0.0575(6) Uani 1 1 d . . . . .
H41 H 0.1820 0.9542 0.7654 0.086 Uiso 1 1 calc R U . . .
C41 C 0.0436(3) 0.9587(4) 0.7563(3) 0.0566(9) Uani 1 1 d . . . . .
H41A H 0.0244 1.0192 0.7649 0.068 Uiso 1 1 calc R U . . .
H41B H 0.0261 0.9162 0.8108 0.068 Uiso 1 1 calc R U . . .
C42 C -0.0281(4) 0.8862(4) 0.6635(3) 0.0748(13) Uani 1 1 d . . . . .
H42A H -0.1085 0.8575 0.6649 0.112 Uiso 1 1 calc R U . . .
H42B H -0.0124 0.9282 0.6093 0.112 Uiso 1 1 calc R U . . .
H42C H -0.0107 0.8251 0.6552 0.112 Uiso 1 1 calc R U . . .
O51 O 0.6631(4) 0.3715(4) 0.6947(4) 0.0882(16) Uani 0.7 1 d . . P D 1
H51 H 0.5965 0.3564 0.6671 0.132 Uiso 0.7 1 calc R U P D 1
C51 C 0.6646(16) 0.2828(18) 0.7237(16) 0.064(4) Uani 0.7 1 d . . P D 1
H51A H 0.6279 0.2220 0.6691 0.076 Uiso 0.7 1 calc R U P D 1
H51B H 0.6224 0.2603 0.7758 0.076 Uiso 0.7 1 calc R U P D 1
O51' O 0.6502(10) 0.3531(10) 0.8083(8) 0.082(3) Uiso 0.3 1 d . . P D 2
H51' H 0.5847 0.3162 0.8177 0.123 Uiso 0.3 1 d R U P D 2
C51' C 0.668(5) 0.286(5) 0.739(4) 0.085(19) Uiso 0.3 1 d . . P D 2
H51C H 0.6476 0.3019 0.6727 0.102 Uiso 0.3 1 calc R U P D 2
H51D H 0.6176 0.2077 0.7407 0.102 Uiso 0.3 1 calc R U P D 2
C52 C 0.7859(4) 0.3079(4) 0.7606(4) 0.0740(12) Uani 1 1 d . . . . .
H52A H 0.7885 0.2427 0.7825 0.111 Uiso 0.7 1 calc R U P D 1
H52B H 0.8269 0.3296 0.7086 0.111 Uiso 0.7 1 calc R U P D 1
H52C H 0.8214 0.3678 0.8149 0.111 Uiso 0.7 1 calc R U P D 1
H52D H 0.7969 0.2620 0.7131 0.111 Uiso 0.3 1 calc R U P D 2
H52E H 0.8350 0.3852 0.7578 0.111 Uiso 0.3 1 calc R U P D 2
H52F H 0.8051 0.2912 0.8257 0.111 Uiso 0.3 1 calc R U P D 2
O61 O 0.0278(4) 0.7273(4) 0.8897(4) 0.0846(14) Uani 0.75 1 d . . P E 1
H61 H 0.0776 0.7599 0.8584 0.127 Uiso 0.75 1 calc R U P E 1
O61' O -0.0031(12) 0.6650(12) 0.8054(10) 0.079(3) Uiso 0.25 1 d . . P E 2
H61' H 0.0575 0.7240 0.8137 0.118 Uiso 0.25 1 calc R U P E 2
C61 C -0.0008(5) 0.6150(4) 0.8803(4) 0.0828(14) Uani 1 1 d . . . . .
H61A H -0.0698 0.5753 0.9058 0.099 Uiso 0.75 1 calc R U P E 1
H61B H -0.0201 0.5867 0.8105 0.099 Uiso 0.75 1 calc R U P E 1
H61C H -0.0036 0.5442 0.8595 0.099 Uiso 0.25 1 calc R U P E 2
H61D H -0.0698 0.5987 0.9051 0.099 Uiso 0.25 1 calc R U P E 2
C62 C 0.0835(7) 0.5908(7) 0.9275(6) 0.091(2) Uani 0.75 1 d . . P E 1
H62A H 0.0561 0.5115 0.9170 0.136 Uiso 0.75 1 calc R U P E 1
H62B H 0.1517 0.6276 0.9016 0.136 Uiso 0.75 1 calc R U P E 1
H62C H 0.1019 0.6162 0.9971 0.136 Uiso 0.75 1 calc R U P E 1
C62' C 0.107(2) 0.682(2) 0.9661(17) 0.099(7) Uiso 0.25 1 d . . P E 2
H62D H 0.1028 0.6385 1.0197 0.148 Uiso 0.25 1 calc R U P E 2
H62E H 0.1762 0.6965 0.9430 0.148 Uiso 0.25 1 calc R U P E 2
H62F H 0.1100 0.7510 0.9886 0.148 Uiso 0.25 1 calc R U P E 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 N2 2.015(3) . ?
Ni1 O2 2.031(3) . ?
Ni1 O3 2.035(2) . ?
Ni1 N1 2.036(3) . ?
Ni1 O6 2.090(2) . ?
Ni1 O7 2.137(2) . ?
N1 C5 1.334(5) . ?
N1 C1 1.357(5) . ?
C1 C2 1.375(5) . ?
C1 C12 1.506(5) . ?
C2 C3 1.385(6) . ?
C3 C4 1.378(6) . ?
C4 C5 1.390(5) . ?
C5 C6 1.536(5) . ?
C6 O5 1.430(4) . ?
C6 C7 1.531(5) . ?
C6 C14 1.548(5) . ?
C7 N2 1.344(4) . ?
C7 C8 1.388(5) . ?
C8 C9 1.382(5) . ?
C9 C10 1.373(5) . ?
C10 C11 1.380(5) . ?
C11 N2 1.355(4) . ?
C11 C13 1.512(5) . ?
C12 O2 1.256(4) . ?
C12 O1 1.256(4) . ?
C13 O4 1.247(4) . ?
C13 O3 1.261(4) . ?
O4 Ni2 2.055(2) . ?
O5 C15 1.449(4) . ?
O6 C16 1.414(4) . ?
C16 C17 1.478(7) . ?
O7 C18 1.433(5) . ?
C18 C19' 1.428(12) . ?
C18 C19 1.430(8) . ?
Ni2 N21 2.020(3) . ?
Ni2 N22 2.028(3) . ?
Ni2 O23 2.048(2) . ?
Ni2 O22 2.049(2) . ?
Ni2 O26 2.127(2) . ?
N21 C25 1.340(4) . ?
N21 C21 1.355(4) . ?
C21 C22 1.378(5) . ?
C21 C32 1.506(5) . ?
C22 C23 1.382(6) . ?
C23 C24 1.387(5) . ?
C24 C25 1.392(5) . ?
C25 C26 1.546(5) . ?
C26 O25 1.422(4) . ?
C26 C34 1.530(5) . ?
C26 C27 1.544(5) . ?
C27 N22 1.337(5) . ?
C27 C28 1.398(5) . ?
C28 C29 1.375(5) . ?
C29 C30 1.384(6) . ?
C30 C31 1.375(5) . ?
C31 N22 1.354(4) . ?
C31 C33 1.510(5) . ?
C32 O21 1.250(4) . ?
C32 O22 1.269(4) . ?
C33 O24 1.251(4) . ?
C33 O23 1.268(4) . ?
O25 C35 1.443(5) . ?
O26 C36 1.431(5) . ?
C36 C37 1.489(7) . ?
O41 C41 1.428(5) . ?
C41 C42 1.492(6) . ?
O51 C51 1.32(2) . ?
C51 C52 1.50(2) . ?
O51' C51' 1.44(6) . ?
C51' C52 1.46(6) . ?
O61 C61 1.414(6) . ?
O61' C61 1.296(13) . ?
C61 C62 1.398(9) . ?
C61 C62' 1.59(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
N2 Ni1 O2 172.77(11) . . ?
N2 Ni1 O3 83.07(10) . . ?
O2 Ni1 O3 103.48(10) . . ?
N2 Ni1 N1 91.30(12) . . ?
O2 Ni1 N1 82.02(11) . . ?
O3 Ni1 N1 173.87(11) . . ?
N2 Ni1 O6 90.76(11) . . ?
O2 Ni1 O6 92.64(10) . . ?
O3 Ni1 O6 86.90(10) . . ?
N1 Ni1 O6 95.64(11) . . ?
N2 Ni1 O7 90.38(10) . . ?
O2 Ni1 O7 86.74(10) . . ?
O3 Ni1 O7 88.81(9) . . ?
N1 Ni1 O7 88.80(10) . . ?
O6 Ni1 O7 175.39(11) . . ?
C5 N1 C1 120.2(3) . . ?
C5 N1 Ni1 128.6(2) . . ?
C1 N1 Ni1 110.8(2) . . ?
N1 C1 C2 121.6(4) . . ?
N1 C1 C12 115.3(3) . . ?
C2 C1 C12 123.0(4) . . ?
C1 C2 C3 118.8(4) . . ?
C4 C3 C2 118.9(4) . . ?
C3 C4 C5 120.4(4) . . ?
N1 C5 C4 120.1(4) . . ?
N1 C5 C6 120.3(3) . . ?
C4 C5 C6 119.0(3) . . ?
O5 C6 C7 108.7(3) . . ?
O5 C6 C5 109.1(3) . . ?
C7 C6 C5 119.7(3) . . ?
O5 C6 C14 103.2(3) . . ?
C7 C6 C14 107.2(3) . . ?
C5 C6 C14 107.7(3) . . ?
N2 C7 C8 120.2(3) . . ?
N2 C7 C6 120.4(3) . . ?
C8 C7 C6 118.7(3) . . ?
C9 C8 C7 120.2(3) . . ?
C10 C9 C8 119.2(3) . . ?
C9 C10 C11 118.8(3) . . ?
N2 C11 C10 122.0(3) . . ?
N2 C11 C13 115.2(3) . . ?
C10 C11 C13 122.8(3) . . ?
C7 N2 C11 119.6(3) . . ?
C7 N2 Ni1 129.4(2) . . ?
C11 N2 Ni1 110.9(2) . . ?
O2 C12 O1 124.9(4) . . ?
O2 C12 C1 117.4(3) . . ?
O1 C12 C1 117.7(3) . . ?
C12 O2 Ni1 113.9(2) . . ?
O4 C13 O3 126.9(3) . . ?
O4 C13 C11 115.0(3) . . ?
O3 C13 C11 118.1(3) . . ?
C13 O3 Ni1 112.3(2) . . ?
C13 O4 Ni2 134.5(2) . . ?
C6 O5 C15 114.3(3) . . ?
C16 O6 Ni1 131.7(2) . . ?
O6 C16 C17 113.8(4) . . ?
C18 O7 Ni1 122.1(2) . . ?
C19' C18 O7 118.3(6) . . ?
C19 C18 O7 116.9(5) . . ?
N21 Ni2 N22 92.44(11) . . ?
N21 Ni2 O23 174.39(11) . . ?
N22 Ni2 O23 81.95(11) . . ?
N21 Ni2 O22 82.03(10) . . ?
N22 Ni2 O22 174.38(10) . . ?
O23 Ni2 O22 103.58(10) . . ?
N21 Ni2 O4 94.86(10) . . ?
N22 Ni2 O4 95.86(11) . . ?
O23 Ni2 O4 85.56(9) . . ?
O22 Ni2 O4 85.69(10) . . ?
N21 Ni2 O26 90.79(10) . . ?
N22 Ni2 O26 88.06(11) . . ?
O23 Ni2 O26 89.23(10) . . ?
O22 Ni2 O26 90.97(10) . . ?
O4 Ni2 O26 172.97(10) . . ?
C25 N21 C21 119.9(3) . . ?
C25 N21 Ni2 128.4(2) . . ?
C21 N21 Ni2 111.2(2) . . ?
N21 C21 C22 122.1(3) . . ?
N21 C21 C32 115.5(3) . . ?
C22 C21 C32 122.3(3) . . ?
C21 C22 C23 118.5(3) . . ?
C22 C23 C24 119.3(3) . . ?
C23 C24 C25 119.8(4) . . ?
N21 C25 C24 120.2(3) . . ?
N21 C25 C26 121.5(3) . . ?
C24 C25 C26 117.8(3) . . ?
O25 C26 C34 104.2(3) . . ?
O25 C26 C27 109.0(3) . . ?
C34 C26 C27 106.6(3) . . ?
O25 C26 C25 108.7(3) . . ?
C34 C26 C25 107.0(3) . . ?
C27 C26 C25 120.2(3) . . ?
N22 C27 C28 120.4(3) . . ?
N22 C27 C26 121.5(3) . . ?
C28 C27 C26 117.6(3) . . ?
C29 C28 C27 120.0(4) . . ?
C28 C29 C30 119.0(4) . . ?
C31 C30 C29 118.9(3) . . ?
N22 C31 C30 122.0(3) . . ?
N22 C31 C33 115.7(3) . . ?
C30 C31 C33 122.3(3) . . ?
C27 N22 C31 119.7(3) . . ?
C27 N22 Ni2 128.7(2) . . ?
C31 N22 Ni2 111.6(2) . . ?
O21 C32 O22 125.8(3) . . ?
O21 C32 C21 117.2(3) . . ?
O22 C32 C21 117.0(3) . . ?
C32 O22 Ni2 113.1(2) . . ?
O24 C33 O23 126.3(4) . . ?
O24 C33 C31 116.7(3) . . ?
O23 C33 C31 117.0(3) . . ?
C33 O23 Ni2 113.4(2) . . ?
C26 O25 C35 114.1(3) . . ?
C36 O26 Ni2 123.1(2) . . ?
O26 C36 C37 112.7(3) . . ?
O41 C41 C42 112.6(3) . . ?
O51 C51 C52 108.4(13) . . ?
O51' C51' C52 110(4) . . ?
C62 C61 O61 115.3(6) . . ?
O61' C61 C62' 114.4(12) . . ?

_refine_diff_density_max         0.346
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.055

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_felix127
_database_code_depnum_ccdc_archive 'CCDC 1571582'
_audit_update_record             
;
2017-08-30 deposited with the CCDC.
2017-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32.50 H29.50 N5.50 Ni O5'
_chemical_formula_weight         635.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   11.4677(2)
_cell_length_b                   16.1148(4)
_cell_length_c                   15.6428(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.183(2)
_cell_angle_gamma                90
_cell_volume                     2890.77(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    35572
_cell_measurement_theta_min      1.814
_cell_measurement_theta_max      27.899

_exptl_crystal_description       block
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_F_000             1324
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.724
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8554
_exptl_absorpt_correction_T_max  0.9375
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35572
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.814
_diffrn_reflns_theta_max         27.899
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6890
_reflns_number_gt                6048
_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       'X-Area (STOE, 2008)'
_computing_cell_refinement       'X-Area (STOE, 2008)'
_computing_data_reduction        'X-Area (STOE, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_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)+(0.0395P)²+1.5578P] 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         6890
_refine_ls_number_parameters     399
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0861
_refine_ls_wR_factor_gt          0.0829
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.59304(2) 0.27893(2) 0.76934(2) 0.02283(7) Uani 1 1 d . . . . .
N1 N 0.66974(11) 0.39237(8) 0.76200(8) 0.0234(3) Uani 1 1 d . . . . .
C1 C 0.78450(14) 0.38528(10) 0.74417(10) 0.0268(3) Uani 1 1 d . . . . .
C2 C 0.85189(15) 0.45364(12) 0.72459(12) 0.0346(4) Uani 1 1 d . . . . .
H2 H 0.9323 0.4475 0.7116 0.042 Uiso 1 1 calc R U . . .
C3 C 0.80041(17) 0.53122(12) 0.72420(13) 0.0384(4) Uani 1 1 d . . . . .
H3 H 0.8449 0.5790 0.7100 0.046 Uiso 1 1 calc R U . . .
C4 C 0.68372(16) 0.53864(10) 0.74459(12) 0.0330(4) Uani 1 1 d . . . . .
H4 H 0.6476 0.5917 0.7459 0.040 Uiso 1 1 calc R U . . .
C5 C 0.61925(14) 0.46725(9) 0.76335(10) 0.0254(3) Uani 1 1 d . . . . .
C6 C 0.49409(14) 0.47823(9) 0.79701(10) 0.0263(3) Uani 1 1 d . . . . .
C7 C 0.40179(14) 0.41063(9) 0.77983(10) 0.0240(3) Uani 1 1 d . . . . .
C8 C 0.28444(15) 0.43419(11) 0.78236(11) 0.0311(3) Uani 1 1 d . . . . .
H8 H 0.2636 0.4908 0.7894 0.037 Uiso 1 1 calc R U . . .
C9 C 0.19934(15) 0.37398(12) 0.77443(12) 0.0342(4) Uani 1 1 d . . . . .
H9 H 0.1193 0.3890 0.7766 0.041 Uiso 1 1 calc R U . . .
C10 C 0.23074(14) 0.29178(11) 0.76325(11) 0.0299(3) Uani 1 1 d . . . . .
H10 H 0.1731 0.2499 0.7570 0.036 Uiso 1 1 calc R U . . .
C11 C 0.34789(13) 0.27225(9) 0.76144(10) 0.0241(3) Uani 1 1 d . . . . .
N2 N 0.43148(11) 0.33071(8) 0.77050(8) 0.0224(3) Uani 1 1 d . . . . .
C12 C 0.83488(14) 0.29804(11) 0.75048(11) 0.0290(3) Uani 1 1 d . . . . .
O1 O 0.94142(11) 0.28992(9) 0.74327(10) 0.0412(3) Uani 1 1 d . . . . .
O2 O 0.76150(10) 0.24040(7) 0.76457(8) 0.0312(3) Uani 1 1 d . . . . .
C13 C 0.39076(14) 0.18300(10) 0.75191(11) 0.0267(3) Uani 1 1 d . . . . .
O3 O 0.49908(10) 0.17196(7) 0.76717(8) 0.0284(2) Uani 1 1 d . . . . .
O4 O 0.31902(12) 0.12983(8) 0.73186(10) 0.0402(3) Uani 1 1 d . . . . .
C14 C 0.50285(17) 0.48865(11) 0.89439(11) 0.0334(4) Uani 1 1 d . . . . .
H14A H 0.5564 0.5343 0.9078 0.050 Uiso 1 1 calc R U . . .
H14B H 0.5322 0.4372 0.9199 0.050 Uiso 1 1 calc R U . . .
H14C H 0.4255 0.5012 0.9176 0.050 Uiso 1 1 calc R U . . .
O5 O 0.44959(11) 0.55557(7) 0.76836(8) 0.0319(3) Uani 1 1 d . . . . .
C15 C 0.42906(18) 0.56156(12) 0.67822(12) 0.0381(4) Uani 1 1 d . . . . .
H15A H 0.5028 0.5544 0.6476 0.057 Uiso 1 1 calc R U . . .
H15B H 0.3961 0.6162 0.6648 0.057 Uiso 1 1 calc R U . . .
H15C H 0.3742 0.5182 0.6605 0.057 Uiso 1 1 calc R U . . .
N21 N 0.58489(12) 0.26871(8) 0.62872(9) 0.0278(3) Uani 1 1 d . . . . .
C21 C 0.65316(17) 0.21290(11) 0.58970(12) 0.0367(4) Uani 1 1 d . . . . .
H21 H 0.7111 0.1852 0.6225 0.044 Uiso 1 1 calc R U . . .
C22 C 0.6428(2) 0.19385(13) 0.50344(13) 0.0441(5) Uani 1 1 d . . . . .
H22 H 0.6942 0.1549 0.4779 0.053 Uiso 1 1 calc R U . . .
C23 C 0.55758(19) 0.23183(13) 0.45521(13) 0.0424(4) Uani 1 1 d . . . . .
H23 H 0.5478 0.2187 0.3964 0.051 Uiso 1 1 calc R U . . .
C24 C 0.48691(18) 0.28932(13) 0.49433(12) 0.0397(4) Uani 1 1 d . . . . .
H24 H 0.4274 0.3170 0.4630 0.048 Uiso 1 1 calc R U . . .
C25 C 0.50404(16) 0.30617(11) 0.58037(11) 0.0337(4) Uani 1 1 d . . . . .
H25 H 0.4556 0.3466 0.6065 0.040 Uiso 1 1 calc R U . . .
N31 N 0.59690(12) 0.27661(8) 0.90624(9) 0.0278(3) Uani 1 1 d . . . . .
C31 C 0.68733(17) 0.30548(12) 0.95194(12) 0.0362(4) Uani 1 1 d . . . . .
H31 H 0.7573 0.3190 0.9227 0.043 Uiso 1 1 calc R U . . .
C32 C 0.6836(2) 0.31653(13) 1.03967(13) 0.0453(5) Uani 1 1 d . . . . .
H32 H 0.7496 0.3373 1.0696 0.054 Uiso 1 1 calc R U . . .
C33 C 0.5829(2) 0.29702(12) 1.08296(13) 0.0440(5) Uani 1 1 d . . . . .
H33 H 0.5772 0.3056 1.1429 0.053 Uiso 1 1 calc R U . . .
C34 C 0.49075(19) 0.26478(13) 1.03731(13) 0.0424(4) Uani 1 1 d . . . . .
H34 H 0.4210 0.2489 1.0655 0.051 Uiso 1 1 calc R U . . .
C35 C 0.50101(16) 0.25573(12) 0.94984(12) 0.0347(4) Uani 1 1 d . . . . .
H35 H 0.4367 0.2335 0.9190 0.042 Uiso 1 1 calc R U . . .
N41 N 0.3008(2) 0.45114(14) 0.48580(15) 0.0664(6) Uani 1 1 d . . . . .
C41 C 0.2158(2) 0.41421(14) 0.52855(16) 0.0539(6) Uani 1 1 d . . . . .
H41 H 0.2167 0.3553 0.5308 0.065 Uiso 1 1 calc R U . . .
C42 C 0.1274(2) 0.45378(15) 0.56948(17) 0.0554(6) Uani 1 1 d . . . . .
H42 H 0.0698 0.4234 0.5998 0.066 Uiso 1 1 calc R U . . .
C43 C 0.1237(2) 0.53902(17) 0.5657(2) 0.0709(8) Uani 1 1 d . . . . .
H43 H 0.0643 0.5696 0.5938 0.085 Uiso 1 1 calc R U . . .
C44 C 0.2108(3) 0.57902(15) 0.5186(2) 0.0755(9) Uani 1 1 d . . . . .
H44 H 0.2114 0.6377 0.5132 0.091 Uiso 1 1 calc R U . . .
C45 C 0.2946(3) 0.53204(18) 0.48097(17) 0.0674(7) Uani 1 1 d . . . . .
H45 H 0.3527 0.5600 0.4488 0.081 Uiso 1 1 calc R U . . .
N51 N 0.8934(2) 0.47402(14) 0.03138(17) 0.0638(6) Uani 0.5 1 d . . P A 1
C51 C 0.8934(2) 0.47402(14) 0.03138(17) 0.0638(6) Uani 0.5 1 d . . P A 2
H51 H 0.8201 0.4566 0.0531 0.077 Uiso 0.5 1 calc R U P A 2
C52 C 0.9883(3) 0.48085(15) 0.08348(17) 0.0616(7) Uani 1 1 d . . . . .
H52 H 0.9815 0.4672 0.1423 0.074 Uiso 1 1 calc R U . A 1
C53 C 1.0934(3) 0.50716(16) 0.05223(17) 0.0600(6) Uani 1 1 d . . . . .
H53 H 1.1581 0.5123 0.0900 0.072 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 O2 2.0308(12) . ?
Ni1 N1 2.0322(13) . ?
Ni1 N2 2.0322(13) . ?
Ni1 O3 2.0330(11) . ?
Ni1 N31 2.1422(14) . ?
Ni1 N21 2.2075(14) . ?
N1 C5 1.339(2) . ?
N1 C1 1.351(2) . ?
C1 C2 1.381(2) . ?
C1 C12 1.523(2) . ?
C2 C3 1.383(3) . ?
C3 C4 1.382(3) . ?
C4 C5 1.399(2) . ?
C5 C6 1.541(2) . ?
C6 O5 1.4188(18) . ?
C6 C14 1.535(2) . ?
C6 C7 1.542(2) . ?
C7 N2 1.3401(19) . ?
C7 C8 1.399(2) . ?
C8 C9 1.381(3) . ?
C9 C10 1.384(3) . ?
C10 C11 1.380(2) . ?
C11 N2 1.3511(19) . ?
C11 C13 1.528(2) . ?
C12 O1 1.234(2) . ?
C12 O2 1.273(2) . ?
C13 O4 1.228(2) . ?
C13 O3 1.277(2) . ?
O5 C15 1.432(2) . ?
N21 C25 1.339(2) . ?
N21 C21 1.341(2) . ?
C21 C22 1.389(3) . ?
C22 C23 1.376(3) . ?
C23 C24 1.376(3) . ?
C24 C25 1.386(3) . ?
N31 C35 1.339(2) . ?
N31 C31 1.341(2) . ?
C31 C32 1.385(3) . ?
C32 C33 1.377(3) . ?
C33 C34 1.375(3) . ?
C34 C35 1.381(3) . ?
N41 C45 1.308(3) . ?
N41 C41 1.325(3) . ?
C41 C42 1.360(3) . ?
C42 C43 1.376(4) . ?
C43 C44 1.400(5) . ?
C44 C45 1.359(4) . ?
N51 C53 1.352(4) 3_765 ?
N51 C52 1.362(4) . ?
C52 C53 1.369(4) . ?
C53 C51 1.352(4) 3_765 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 N1 82.01(5) . . ?
O2 Ni1 N2 173.37(5) . . ?
N1 Ni1 N2 91.48(5) . . ?
O2 Ni1 O3 104.15(5) . . ?
N1 Ni1 O3 172.43(5) . . ?
N2 Ni1 O3 82.25(5) . . ?
O2 Ni1 N31 90.85(5) . . ?
N1 Ni1 N31 93.70(5) . . ?
N2 Ni1 N31 90.81(5) . . ?
O3 Ni1 N31 90.64(5) . . ?
O2 Ni1 N21 88.73(5) . . ?
N1 Ni1 N21 91.59(5) . . ?
N2 Ni1 N21 90.22(5) . . ?
O3 Ni1 N21 84.22(5) . . ?
N31 Ni1 N21 174.58(5) . . ?
C5 N1 C1 120.08(13) . . ?
C5 N1 Ni1 128.52(11) . . ?
C1 N1 Ni1 110.96(10) . . ?
N1 C1 C2 121.65(15) . . ?
N1 C1 C12 115.74(14) . . ?
C2 C1 C12 122.57(15) . . ?
C1 C2 C3 118.89(16) . . ?
C4 C3 C2 119.41(16) . . ?
C3 C4 C5 119.34(16) . . ?
N1 C5 C4 120.60(15) . . ?
N1 C5 C6 120.82(13) . . ?
C4 C5 C6 118.09(14) . . ?
O5 C6 C14 103.87(13) . . ?
O5 C6 C5 109.11(13) . . ?
C14 C6 C5 107.07(14) . . ?
O5 C6 C7 108.64(13) . . ?
C14 C6 C7 107.03(13) . . ?
C5 C6 C7 119.94(13) . . ?
N2 C7 C8 120.57(15) . . ?
N2 C7 C6 121.57(13) . . ?
C8 C7 C6 117.59(14) . . ?
C9 C8 C7 119.09(15) . . ?
C8 C9 C10 119.98(15) . . ?
C11 C10 C9 118.32(15) . . ?
N2 C11 C10 121.95(14) . . ?
N2 C11 C13 116.00(13) . . ?
C10 C11 C13 122.03(14) . . ?
C7 N2 C11 120.07(13) . . ?
C7 N2 Ni1 128.86(11) . . ?
C11 N2 Ni1 111.06(10) . . ?
O1 C12 O2 126.41(16) . . ?
O1 C12 C1 117.86(15) . . ?
O2 C12 C1 115.71(14) . . ?
C12 O2 Ni1 114.38(10) . . ?
O4 C13 O3 126.97(15) . . ?
O4 C13 C11 117.80(15) . . ?
O3 C13 C11 115.23(13) . . ?
C13 O3 Ni1 113.60(10) . . ?
C6 O5 C15 115.35(13) . . ?
C25 N21 C21 116.73(16) . . ?
C25 N21 Ni1 123.81(11) . . ?
C21 N21 Ni1 118.73(12) . . ?
N21 C21 C22 122.86(19) . . ?
C23 C22 C21 119.51(18) . . ?
C24 C23 C22 118.30(19) . . ?
C23 C24 C25 118.81(19) . . ?
N21 C25 C24 123.78(17) . . ?
C35 N31 C31 116.79(16) . . ?
C35 N31 Ni1 119.95(12) . . ?
C31 N31 Ni1 122.71(12) . . ?
N31 C31 C32 123.12(19) . . ?
C33 C32 C31 119.14(19) . . ?
C34 C33 C32 118.36(19) . . ?
C33 C34 C35 119.11(19) . . ?
N31 C35 C34 123.41(18) . . ?
C45 N41 C41 115.9(2) . . ?
N41 C41 C42 125.3(2) . . ?
C41 C42 C43 118.1(2) . . ?
C42 C43 C44 117.4(3) . . ?
C45 C44 C43 118.6(2) . . ?
N41 C45 C44 124.7(3) . . ?
C53 N51 C52 118.0(2) 3_765 . ?
N51 C52 C53 120.9(2) . . ?
C51 C53 C52 121.1(3) 3_765 . ?

_refine_diff_density_max         0.492
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.050

_shelxl_version_number           2014-3

